# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px139
_database_code_depnum_ccdc_archive 'CCDC 2061069'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-04-08
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        1-cyclopropyl-5H-tetrazole
_chemical_name_common            1-cyclopropyl-5H-tetrazole
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 N4'
_chemical_formula_sum            'C4 H6 N4'
_chemical_formula_weight         110.13

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   4.9091(9)
_cell_length_b                   6.6220(8)
_cell_length_c                   8.103(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.75(2)
_cell_angle_gamma                90
_cell_volume                     259.60(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    112(2)
_cell_measurement_reflns_used    604
_cell_measurement_theta_min      3.0510
_cell_measurement_theta_max      30.6150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.491
_exptl_crystal_size_min          0.138
_exptl_absorpt_coefficient_mu    0.099
_shelx_estimated_absorpt_T_min   0.952
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      112(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            2494
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.998
_diffrn_reflns_theta_max         30.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1571
_reflns_number_gt                1319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+0.0286P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 508 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;

_refine_ls_abs_structure_Flack   -1.7(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1571
_refine_ls_number_parameters     97
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0791454000
_diffrn_orient_matrix_UB_12      0.0652377000
_diffrn_orient_matrix_UB_13      -0.0592351000
_diffrn_orient_matrix_UB_21      0.0364076000
_diffrn_orient_matrix_UB_22      -0.0581407000
_diffrn_orient_matrix_UB_23      -0.0663170000
_diffrn_orient_matrix_UB_31      -0.1178577000
_diffrn_orient_matrix_UB_32      -0.0618478000
_diffrn_orient_matrix_UB_33      0.0003758000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00 -44.00   1.00    5.00    --  -28.86-178.00  60.00   52
  2  ω      1.00  83.00   1.00    5.00    --   29.79  37.00   0.00   82
  3  ω     52.00 109.00   1.00    5.00    --   29.79 178.00 150.00   57
  4  ω    -19.00  84.00   1.00    5.00    --   29.79 -19.00-120.00  103
  5  ω    -35.00 106.00   1.00    5.00    --   29.79  19.00 -90.00  141
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.7620(4) 0.5082(3) 0.7961(3) 0.0214(4) Uani 1 1 d . . . . .
N3 N 0.9406(4) 0.2153(3) 0.8019(3) 0.0282(5) Uani 1 1 d . . . . .
N2 N 0.9554(4) 0.3950(3) 0.7382(3) 0.0270(5) Uani 1 1 d . . . . .
N4 N 0.7394(4) 0.2090(3) 0.9007(3) 0.0267(5) Uani 1 1 d . . . . .
C1 C 0.6349(5) 0.3923(3) 0.8943(3) 0.0239(5) Uani 1 1 d . . . . .
C2 C 0.7265(5) 0.7212(4) 0.7584(3) 0.0215(5) Uani 1 1 d . . . . .
C3 C 0.4450(5) 0.7927(4) 0.6817(4) 0.0256(5) Uani 1 1 d . . . . .
C4 C 0.6725(6) 0.7852(4) 0.5794(4) 0.0274(6) Uani 1 1 d . . . . .
H4A H 0.763(5) 0.911(4) 0.553(4) 0.023(7) Uiso 1 1 d . . . . .
H3A H 0.384(5) 0.922(4) 0.713(4) 0.027(7) Uiso 1 1 d . . . . .
H3B H 0.301(6) 0.693(5) 0.663(4) 0.032(8) Uiso 1 1 d . . . . .
H4B H 0.666(6) 0.688(5) 0.503(4) 0.040(9) Uiso 1 1 d . . . . .
H2 H 0.837(5) 0.796(4) 0.834(4) 0.022(7) Uiso 1 1 d . . . . .
H1 H 0.488(7) 0.442(4) 0.946(4) 0.041(9) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.335(3) . ?
N1 N2 1.354(3) . ?
N1 C2 1.447(3) . ?
N3 N2 1.303(3) . ?
N3 N4 1.374(3) . ?
N4 C1 1.315(3) . ?
C1 H1 0.95(3) . ?
C2 C4 1.491(4) . ?
C2 C3 1.493(3) . ?
C2 H2 0.90(3) . ?
C3 C4 1.500(4) . ?
C3 H3A 0.95(3) . ?
C3 H3B 0.96(3) . ?
C4 H4A 0.98(3) . ?
C4 H4B 0.89(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 N2 108.29(19) . . ?
C1 N1 C2 129.4(2) . . ?
N2 N1 C2 122.2(2) . . ?
N2 N3 N4 110.61(19) . . ?
N3 N2 N1 106.2(2) . . ?
C1 N4 N3 105.3(2) . . ?
N4 C1 N1 109.6(2) . . ?
N4 C1 H1 128.4(18) . . ?
N1 C1 H1 122.0(18) . . ?
N1 C2 C4 118.5(2) . . ?
N1 C2 C3 117.8(2) . . ?
C4 C2 C3 60.36(18) . . ?
N1 C2 H2 110.9(18) . . ?
C4 C2 H2 119.7(18) . . ?
C3 C2 H2 121.4(17) . . ?
C2 C3 C4 59.78(17) . . ?
C2 C3 H3A 118.9(17) . . ?
C4 C3 H3A 118.1(18) . . ?
C2 C3 H3B 116.8(17) . . ?
C4 C3 H3B 118.8(17) . . ?
H3A C3 H3B 114(2) . . ?
C2 C4 C3 59.86(17) . . ?
C2 C4 H4A 116.1(17) . . ?
C3 C4 H4A 119.9(15) . . ?
C2 C4 H4B 117(2) . . ?
C3 C4 H4B 118(2) . . ?
H4A C4 H4B 115(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 N3 N2 N1 0.1(3) . . . . ?
C1 N1 N2 N3 0.1(3) . . . . ?
C2 N1 N2 N3 176.8(2) . . . . ?
N2 N3 N4 C1 -0.2(3) . . . . ?
N3 N4 C1 N1 0.3(3) . . . . ?
N2 N1 C1 N4 -0.2(3) . . . . ?
C2 N1 C1 N4 -176.7(2) . . . . ?
C1 N1 C2 C4 -127.9(3) . . . . ?
N2 N1 C2 C4 56.1(3) . . . . ?
C1 N1 C2 C3 -58.3(3) . . . . ?
N2 N1 C2 C3 125.7(2) . . . . ?
N1 C2 C3 C4 -108.7(3) . . . . ?
N1 C2 C4 C3 107.6(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N4 0.95(3) 2.53(3) 3.401(3) 153(2) 2_657




_refine_diff_density_max         0.208
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.043

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px226
_database_code_depnum_ccdc_archive 'CCDC 2061075'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-12
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'dinitrato di(1-cyclobutyl-5H-tetrazolyl copper(II)'
_chemical_name_common            
'dinitrato di(1-cyclobutyl-5H-tetrazolyl copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H20 Cu N10 O6'
_chemical_formula_sum            'C12 H20 Cu N10 O6'
_chemical_formula_weight         463.92

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.4782(13)
_cell_length_b                   6.3738(3)
_cell_length_c                   9.7644(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.052(6)
_cell_angle_gamma                90
_cell_volume                     900.49(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    1248
_cell_measurement_theta_min      3.7890
_cell_measurement_theta_max      27.1340

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.271
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_F_000             478
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            4777
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.816
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1833
_reflns_number_gt                1429
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1833
_refine_ls_number_parameters     173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1371
_refine_ls_wR_factor_gt          0.1220
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0369315000
_diffrn_orient_matrix_UB_12      0.0549541000
_diffrn_orient_matrix_UB_13      -0.0295755000
_diffrn_orient_matrix_UB_21      0.0161366000
_diffrn_orient_matrix_UB_22      0.0321220000
_diffrn_orient_matrix_UB_23      0.0661805000
_diffrn_orient_matrix_UB_31      0.0278624000
_diffrn_orient_matrix_UB_32      -0.0913412000
_diffrn_orient_matrix_UB_33      0.0054646000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  50.00   1.00   25.00    --  -20.37  57.00   0.00   94
  2  ω    -90.00   3.00   1.00   25.00    --  -20.37 -57.00-150.00   93
  3  ω     -2.00  92.00   1.00   25.00    --   21.23  57.00 120.00   94
  4  ω    -12.00  31.00   1.00   25.00    --   21.23  77.00-150.00   43
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.500000 0.500000 0.500000 0.0213(2) Uani 1 2 d S . P . .
O1 O 0.57688(18) 0.2484(4) 0.4612(2) 0.0241(6) Uani 1 1 d . . . . .
O2 O 0.53070(18) 0.3550(4) 0.2583(2) 0.0289(6) Uani 1 1 d . . . . .
O3 O 0.63834(18) 0.1168(4) 0.2805(2) 0.0307(6) Uani 1 1 d . . . . .
N5 N 0.5827(2) 0.2378(4) 0.3285(3) 0.0235(7) Uani 1 1 d . . . . .
N1 N 0.6114(2) 0.6748(4) 0.4921(3) 0.0229(7) Uani 1 1 d . . . . .
N4 N 0.7235(2) 0.8823(4) 0.5425(3) 0.0228(7) Uani 1 1 d . . . . .
N2 N 0.6841(2) 0.6314(4) 0.4111(3) 0.0277(7) Uani 1 1 d . . . . .
N3 N 0.7520(2) 0.7548(5) 0.4407(3) 0.0267(7) Uani 1 1 d . . . . .
C1 C 0.6390(3) 0.8325(5) 0.5720(3) 0.0229(8) Uani 1 1 d . . . . .
C2 C 0.7854(3) 1.0447(6) 0.6009(4) 0.0252(8) Uani 1 1 d . . . . .
C3 C 0.8728(3) 0.9598(7) 0.6702(5) 0.0321(9) Uani 1 1 d . . . . .
C6 C 0.8199(3) 1.1989(6) 0.4951(4) 0.0331(9) Uani 1 1 d . . . . .
C4 C 0.9425(3) 1.1385(7) 0.6667(4) 0.0349(10) Uani 1 1 d . . . . .
C5 C 0.8968(4) 1.3092(7) 0.5759(5) 0.0414(11) Uani 1 1 d . . . . .
H6A H 0.774(3) 1.287(6) 0.454(3) 0.016(9) Uiso 1 1 d . . . . .
H2 H 0.751(2) 1.106(5) 0.662(4) 0.014(8) Uiso 1 1 d . . . . .
H6B H 0.838(3) 1.131(7) 0.419(5) 0.048(14) Uiso 1 1 d . . . . .
H5A H 0.944(4) 1.382(7) 0.525(5) 0.058(15) Uiso 1 1 d . . . . .
H1 H 0.610(2) 0.893(5) 0.632(3) 0.009(8) Uiso 1 1 d . . . . .
H3A H 0.894(3) 0.854(7) 0.624(5) 0.042(13) Uiso 1 1 d . . . . .
H5B H 0.872(3) 1.416(8) 0.625(5) 0.046(13) Uiso 1 1 d . . . . .
H4A H 0.958(3) 1.187(7) 0.760(4) 0.042(12) Uiso 1 1 d . . . . .
H4B H 0.998(4) 1.089(8) 0.629(5) 0.056(14) Uiso 1 1 d . . . . .
H3B H 0.870(4) 0.908(9) 0.750(6) 0.077(18) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.964(3) 3_666 ?
Cu1 N1 1.964(3) . ?
Cu1 O1 1.996(2) . ?
Cu1 O1 1.996(2) 3_666 ?
O1 N5 1.303(3) . ?
O2 N5 1.248(4) . ?
O3 N5 1.221(4) . ?
N1 C1 1.325(4) . ?
N1 N2 1.367(4) . ?
N4 C1 1.305(5) . ?
N4 N3 1.360(4) . ?
N4 C2 1.471(5) . ?
N2 N3 1.284(4) . ?
C1 H1 0.83(3) . ?
C2 C3 1.513(6) . ?
C2 C6 1.523(5) . ?
C2 H2 0.88(4) . ?
C3 C4 1.523(6) . ?
C3 H3A 0.87(5) . ?
C3 H3B 0.85(6) . ?
C6 C5 1.515(6) . ?
C6 H6A 0.95(4) . ?
C6 H6B 0.91(5) . ?
C4 C5 1.538(6) . ?
C4 H4A 0.98(4) . ?
C4 H4B 0.95(5) . ?
C5 H5A 0.97(5) . ?
C5 H5B 0.91(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 180.0 3_666 . ?
N1 Cu1 O1 90.93(11) 3_666 . ?
N1 Cu1 O1 89.07(11) . . ?
N1 Cu1 O1 89.07(11) 3_666 3_666 ?
N1 Cu1 O1 90.93(11) . 3_666 ?
O1 Cu1 O1 180.0 . 3_666 ?
N5 O1 Cu1 106.65(19) . . ?
O3 N5 O2 124.0(3) . . ?
O3 N5 O1 118.8(3) . . ?
O2 N5 O1 117.1(3) . . ?
C1 N1 N2 105.8(3) . . ?
C1 N1 Cu1 129.6(3) . . ?
N2 N1 Cu1 123.9(2) . . ?
C1 N4 N3 109.1(3) . . ?
C1 N4 C2 130.5(3) . . ?
N3 N4 C2 120.4(3) . . ?
N3 N2 N1 110.2(3) . . ?
N2 N3 N4 106.2(3) . . ?
N4 C1 N1 108.7(3) . . ?
N4 C1 H1 123(2) . . ?
N1 C1 H1 128(2) . . ?
N4 C2 C3 114.2(3) . . ?
N4 C2 C6 113.7(3) . . ?
C3 C2 C6 104.2(3) . . ?
N4 C2 H2 103(2) . . ?
C3 C2 H2 110(2) . . ?
C6 C2 H2 112(2) . . ?
C2 C3 C4 105.5(3) . . ?
C2 C3 H3A 111(3) . . ?
C4 C3 H3A 109(3) . . ?
C2 C3 H3B 119(4) . . ?
C4 C3 H3B 112(4) . . ?
H3A C3 H3B 102(5) . . ?
C5 C6 C2 101.5(3) . . ?
C5 C6 H6A 116(2) . . ?
C2 C6 H6A 115(2) . . ?
C5 C6 H6B 115(3) . . ?
C2 C6 H6B 111(3) . . ?
H6A C6 H6B 99(3) . . ?
C3 C4 C5 105.7(3) . . ?
C3 C4 H4A 110(3) . . ?
C5 C4 H4A 113(2) . . ?
C3 C4 H4B 110(3) . . ?
C5 C4 H4B 111(3) . . ?
H4A C4 H4B 107(4) . . ?
C6 C5 C4 105.3(3) . . ?
C6 C5 H5A 118(3) . . ?
C4 C5 H5A 110(3) . . ?
C6 C5 H5B 109(3) . . ?
C4 C5 H5B 113(3) . . ?
H5A C5 H5B 101(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 N5 O3 168.3(2) . . . . ?
Cu1 O1 N5 O2 -11.0(3) . . . . ?
C1 N1 N2 N3 0.4(4) . . . . ?
Cu1 N1 N2 N3 -171.1(2) . . . . ?
N1 N2 N3 N4 -0.3(4) . . . . ?
C1 N4 N3 N2 0.1(4) . . . . ?
C2 N4 N3 N2 -179.9(3) . . . . ?
N3 N4 C1 N1 0.2(4) . . . . ?
C2 N4 C1 N1 -179.9(3) . . . . ?
N2 N1 C1 N4 -0.3(4) . . . . ?
Cu1 N1 C1 N4 170.5(2) . . . . ?
C1 N4 C2 C3 117.7(4) . . . . ?
N3 N4 C2 C3 -62.3(4) . . . . ?
C1 N4 C2 C6 -122.9(4) . . . . ?
N3 N4 C2 C6 57.1(5) . . . . ?
N4 C2 C3 C4 156.1(3) . . . . ?
C6 C2 C3 C4 31.5(4) . . . . ?
N4 C2 C6 C5 -167.2(4) . . . . ?
C3 C2 C6 C5 -42.3(4) . . . . ?
C2 C3 C4 C5 -8.3(4) . . . . ?
C2 C6 C5 C4 36.9(5) . . . . ?
C3 C4 C5 C6 -18.1(5) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C6 H6A N2 0.95(4) 2.58(4) 3.468(5) 156(3) 1_565




_refine_diff_density_max         1.259
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.122

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px177
_database_code_depnum_ccdc_archive 'CCDC 2061076'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-05-07
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'dichlorato tetrakis(1-cyclopentyl)tetrazole copper(II)'
_chemical_name_common            
'dichlorato tetrakis(1-cyclopentyl)tetrazole copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 Cl2 Cu N16 O6'
_chemical_formula_sum            'C24 H40 Cl2 Cu N16 O6'
_chemical_formula_weight         783.16

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/a'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'

_space_group_crystal_system      monoclinic

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   21.6878(12)
_cell_length_b                   6.4701(5)
_cell_length_c                   24.9341(13)
_cell_angle_alpha                90
_cell_angle_beta                 104.209(4)
_cell_angle_gamma                90
_cell_volume                     3391.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    127(2)
_cell_measurement_reflns_used    5503
_cell_measurement_theta_min      2.3280
_cell_measurement_theta_max      31.7880

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.557
_exptl_crystal_size_mid          0.537
_exptl_crystal_size_min          0.218
_exptl_absorpt_coefficient_mu    0.866
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_F_000             1628
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      127(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            14134
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.234
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3468
_reflns_number_gt                3120
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+4.5096P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3468
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0534059000
_diffrn_orient_matrix_UB_12      -0.0130494000
_diffrn_orient_matrix_UB_13      0.0079166000
_diffrn_orient_matrix_UB_21      0.0158073000
_diffrn_orient_matrix_UB_22      0.0330176000
_diffrn_orient_matrix_UB_23      -0.0300574000
_diffrn_orient_matrix_UB_31      -0.0108573000
_diffrn_orient_matrix_UB_32      0.0349979000
_diffrn_orient_matrix_UB_33      0.0233919000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00 -39.00   1.00    5.00    --  -28.86-178.00-150.00   32
  2  ω   -108.00 -72.00   1.00    5.00    --  -28.86-178.00 150.00   36
  3  ω    -12.00  59.00   1.00    5.00    --   29.64 -99.00  90.00   71
  4  ω     67.00  93.00   1.00    5.00    --   29.64-178.00  90.00   26
  5  ω    -20.00  74.00   1.00    5.00    --   29.64 -99.00-180.00   94
  6  ω     41.00  66.00   1.00    5.00    --   29.64 -99.00   0.00   25
  7  ω     15.00  97.00   1.00    5.00    --   29.64  57.00   0.00   82
  8  ω    -36.00   2.00   1.00    5.00    --   29.64 -57.00 120.00   38
  9  ω    -13.00 101.00   1.00    5.00    --   29.64  19.00 -60.00  114
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.500000 0.500000 0.500000 0.01533(10) Uani 1 2 d S . P . .
Cl1 Cl 0.63848(2) 0.22661(7) 0.52204(2) 0.02171(12) Uani 1 1 d . . . . .
O1 O 0.56962(6) 0.2132(2) 0.52196(5) 0.0216(3) Uani 1 1 d . . . . .
O2 O 0.64183(9) 0.2099(3) 0.46408(7) 0.0460(5) Uani 1 1 d . . . . .
O3 O 0.66897(6) 0.0415(2) 0.55202(6) 0.0274(3) Uani 1 1 d . . . . .
N1 N 0.54910(7) 0.6696(2) 0.56352(6) 0.0173(3) Uani 1 1 d . . . . .
N2 N 0.60062(7) 0.5989(3) 0.60213(6) 0.0233(3) Uani 1 1 d . . . . .
N3 N 0.61785(8) 0.7366(2) 0.64053(7) 0.0239(4) Uani 1 1 d . . . . .
N4 N 0.57772(7) 0.8979(2) 0.62694(6) 0.0175(3) Uani 1 1 d . . . . .
N5 N 0.55224(7) 0.6144(2) 0.44982(6) 0.0171(3) Uani 1 1 d . . . . .
N6 N 0.54134(7) 0.5663(3) 0.39479(6) 0.0242(4) Uani 1 1 d . . . . .
N7 N 0.58817(7) 0.6296(3) 0.37600(6) 0.0247(4) Uani 1 1 d . . . . .
N8 N 0.63061(7) 0.7187(2) 0.41869(6) 0.0174(3) Uani 1 1 d . . . . .
C1 C 0.53593(8) 0.8542(3) 0.57986(7) 0.0173(4) Uani 1 1 d . . . . .
H1 H 0.502225 0.941237 0.561122 0.021 Uiso 1 1 calc R U . . .
C2 C 0.58440(9) 1.0879(3) 0.66035(7) 0.0205(4) Uani 1 1 d . . . . .
H2 H 0.565769 1.205594 0.635679 0.025 Uiso 1 1 calc R U . . .
C3 C 0.55179(10) 1.0769(4) 0.70788(8) 0.0291(5) Uani 1 1 d . . . . .
H3A H 0.561532 0.945341 0.728477 0.035 Uiso 1 1 calc R U . . .
H3B H 0.505099 1.091488 0.694387 0.035 Uiso 1 1 calc R U . . .
C4 C 0.58076(12) 1.2617(4) 0.74382(9) 0.0410(6) Uani 1 1 d . . . . .
H4A H 0.584798 1.231001 0.783427 0.049 Uiso 1 1 calc R U . . .
H4B H 0.553665 1.385705 0.733643 0.049 Uiso 1 1 calc R U . . .
C5 C 0.64663(11) 1.2980(3) 0.73286(8) 0.0309(5) Uani 1 1 d . . . . .
H5A H 0.649896 1.440543 0.719357 0.037 Uiso 1 1 calc R U . . .
H5B H 0.680477 1.277294 0.767154 0.037 Uiso 1 1 calc R U . . .
C6 C 0.65313(10) 1.1397(3) 0.68864(8) 0.0281(4) Uani 1 1 d . . . . .
H6A H 0.675389 1.200294 0.662136 0.034 Uiso 1 1 calc R U . . .
H6B H 0.676520 1.015348 0.705732 0.034 Uiso 1 1 calc R U . . .
C7 C 0.60770(8) 0.7082(3) 0.46322(7) 0.0164(3) Uani 1 1 d . . . . .
H7 H 0.627952 0.759675 0.498865 0.020 Uiso 1 1 calc R U . . .
C8 C 0.69333(8) 0.7965(3) 0.41453(7) 0.0190(4) Uani 1 1 d . . . . .
H8 H 0.711195 0.893666 0.445641 0.023 Uiso 1 1 calc R U . . .
C9 C 0.73848(9) 0.6172(3) 0.41510(9) 0.0278(4) Uani 1 1 d . . . . .
H9A H 0.731411 0.506731 0.440397 0.033 Uiso 1 1 calc R U . . .
H9B H 0.783310 0.663357 0.426755 0.033 Uiso 1 1 calc R U . . .
C10 C 0.72221(11) 0.5420(4) 0.35523(11) 0.0432(6) Uani 1 1 d . . . . .
H10A H 0.759819 0.477831 0.346122 0.052 Uiso 1 1 calc R U . . .
H10B H 0.687403 0.439010 0.349007 0.052 Uiso 1 1 calc R U . . .
C11 C 0.70153(12) 0.7334(4) 0.32005(9) 0.0437(6) Uani 1 1 d . . . . .
H11A H 0.662423 0.704555 0.290880 0.052 Uiso 1 1 calc R U . . .
H11B H 0.735364 0.777481 0.302144 0.052 Uiso 1 1 calc R U . . .
C12 C 0.68905(10) 0.9019(3) 0.35916(8) 0.0282(4) Uani 1 1 d . . . . .
H12A H 0.721227 1.012994 0.363127 0.034 Uiso 1 1 calc R U . . .
H12B H 0.646325 0.962973 0.344809 0.034 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.0048(15) 5_666 ?
Cu1 N1 2.0048(15) . ?
Cu1 N5 2.0231(14) . ?
Cu1 N5 2.0231(14) 5_666 ?
Cu1 O1 2.3699(13) 5_666 ?
Cu1 O1 2.3699(13) . ?
Cl1 O2 1.4687(16) . ?
Cl1 O3 1.4789(14) . ?
Cl1 O1 1.4954(13) . ?
N1 C1 1.315(2) . ?
N1 N2 1.363(2) . ?
N2 N3 1.294(2) . ?
N3 N4 1.348(2) . ?
N4 C1 1.326(2) . ?
N4 C2 1.472(2) . ?
N5 C7 1.315(2) . ?
N5 N6 1.370(2) . ?
N6 N7 1.285(2) . ?
N7 N8 1.353(2) . ?
N8 C7 1.325(2) . ?
N8 C8 1.478(2) . ?
C1 H1 0.9500 . ?
C2 C6 1.522(3) . ?
C2 C3 1.523(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.533(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.537(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.537(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C8 C9 1.515(3) . ?
C8 C12 1.522(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.527(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.520(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.531(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 180.0 5_666 . ?
N1 Cu1 N5 88.93(6) 5_666 . ?
N1 Cu1 N5 91.08(6) . . ?
N1 Cu1 N5 91.07(6) 5_666 5_666 ?
N1 Cu1 N5 88.92(6) . 5_666 ?
N5 Cu1 N5 180.00(8) . 5_666 ?
N1 Cu1 O1 93.52(5) 5_666 5_666 ?
N1 Cu1 O1 86.48(5) . 5_666 ?
N5 Cu1 O1 89.56(5) . 5_666 ?
N5 Cu1 O1 90.44(5) 5_666 5_666 ?
N1 Cu1 O1 86.48(5) 5_666 . ?
N1 Cu1 O1 93.52(5) . . ?
N5 Cu1 O1 90.43(5) . . ?
N5 Cu1 O1 89.56(5) 5_666 . ?
O1 Cu1 O1 180.0 5_666 . ?
O2 Cl1 O3 108.29(9) . . ?
O2 Cl1 O1 106.55(9) . . ?
O3 Cl1 O1 106.04(8) . . ?
Cl1 O1 Cu1 122.31(7) . . ?
C1 N1 N2 106.79(14) . . ?
C1 N1 Cu1 128.90(12) . . ?
N2 N1 Cu1 123.97(12) . . ?
N3 N2 N1 109.22(15) . . ?
N2 N3 N4 107.21(14) . . ?
C1 N4 N3 108.44(15) . . ?
C1 N4 C2 129.07(16) . . ?
N3 N4 C2 122.45(14) . . ?
C7 N5 N6 106.35(14) . . ?
C7 N5 Cu1 128.90(12) . . ?
N6 N5 Cu1 123.44(12) . . ?
N7 N6 N5 109.56(15) . . ?
N6 N7 N8 107.17(14) . . ?
C7 N8 N7 108.32(15) . . ?
C7 N8 C8 128.14(15) . . ?
N7 N8 C8 123.37(14) . . ?
N1 C1 N4 108.34(16) . . ?
N1 C1 H1 125.8 . . ?
N4 C1 H1 125.8 . . ?
N4 C2 C6 113.30(15) . . ?
N4 C2 C3 113.67(16) . . ?
C6 C2 C3 103.81(15) . . ?
N4 C2 H2 108.6 . . ?
C6 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C2 C3 C4 102.50(18) . . ?
C2 C3 H3A 111.3 . . ?
C4 C3 H3A 111.3 . . ?
C2 C3 H3B 111.3 . . ?
C4 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C3 C4 C5 106.31(17) . . ?
C3 C4 H4A 110.5 . . ?
C5 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
C5 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C6 C5 C4 106.18(17) . . ?
C6 C5 H5A 110.5 . . ?
C4 C5 H5A 110.5 . . ?
C6 C5 H5B 110.5 . . ?
C4 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C2 C6 C5 103.15(17) . . ?
C2 C6 H6A 111.1 . . ?
C5 C6 H6A 111.1 . . ?
C2 C6 H6B 111.1 . . ?
C5 C6 H6B 111.1 . . ?
H6A C6 H6B 109.1 . . ?
N5 C7 N8 108.60(15) . . ?
N5 C7 H7 125.7 . . ?
N8 C7 H7 125.7 . . ?
N8 C8 C9 110.05(15) . . ?
N8 C8 C12 111.33(15) . . ?
C9 C8 C12 104.29(16) . . ?
N8 C8 H8 110.3 . . ?
C9 C8 H8 110.3 . . ?
C12 C8 H8 110.3 . . ?
C8 C9 C10 103.95(17) . . ?
C8 C9 H9A 111.0 . . ?
C10 C9 H9A 111.0 . . ?
C8 C9 H9B 111.0 . . ?
C10 C9 H9B 111.0 . . ?
H9A C9 H9B 109.0 . . ?
C11 C10 C9 105.60(18) . . ?
C11 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
C11 C10 H10B 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.8 . . ?
C10 C11 C12 106.60(17) . . ?
C10 C11 H11A 110.4 . . ?
C12 C11 H11A 110.4 . . ?
C10 C11 H11B 110.4 . . ?
C12 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C8 C12 C11 106.13(18) . . ?
C8 C12 H12A 110.5 . . ?
C11 C12 H12A 110.5 . . ?
C8 C12 H12B 110.5 . . ?
C11 C12 H12B 110.5 . . ?
H12A C12 H12B 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cl1 O1 Cu1 -80.10(10) . . . . ?
O3 Cl1 O1 Cu1 164.69(8) . . . . ?
C1 N1 N2 N3 0.1(2) . . . . ?
Cu1 N1 N2 N3 -173.75(12) . . . . ?
N1 N2 N3 N4 -0.2(2) . . . . ?
N2 N3 N4 C1 0.3(2) . . . . ?
N2 N3 N4 C2 -177.69(16) . . . . ?
C7 N5 N6 N7 -0.3(2) . . . . ?
Cu1 N5 N6 N7 -168.30(13) . . . . ?
N5 N6 N7 N8 0.5(2) . . . . ?
N6 N7 N8 C7 -0.4(2) . . . . ?
N6 N7 N8 C8 175.16(16) . . . . ?
N2 N1 C1 N4 0.12(19) . . . . ?
Cu1 N1 C1 N4 173.51(12) . . . . ?
N3 N4 C1 N1 -0.2(2) . . . . ?
C2 N4 C1 N1 177.54(16) . . . . ?
C1 N4 C2 C6 -145.44(18) . . . . ?
N3 N4 C2 C6 32.1(2) . . . . ?
C1 N4 C2 C3 96.4(2) . . . . ?
N3 N4 C2 C3 -86.1(2) . . . . ?
N4 C2 C3 C4 165.15(17) . . . . ?
C6 C2 C3 C4 41.6(2) . . . . ?
C2 C3 C4 C5 -26.9(2) . . . . ?
C3 C4 C5 C6 2.6(2) . . . . ?
N4 C2 C6 C5 -163.87(16) . . . . ?
C3 C2 C6 C5 -40.1(2) . . . . ?
C4 C5 C6 C2 22.8(2) . . . . ?
N6 N5 C7 N8 0.1(2) . . . . ?
Cu1 N5 C7 N8 167.14(12) . . . . ?
N7 N8 C7 N5 0.2(2) . . . . ?
C8 N8 C7 N5 -175.09(16) . . . . ?
C7 N8 C8 C9 99.0(2) . . . . ?
N7 N8 C8 C9 -75.7(2) . . . . ?
C7 N8 C8 C12 -145.90(18) . . . . ?
N7 N8 C8 C12 39.4(2) . . . . ?
N8 C8 C9 C10 82.54(19) . . . . ?
C12 C8 C9 C10 -37.0(2) . . . . ?
C8 C9 C10 C11 32.1(2) . . . . ?
C9 C10 C11 C12 -14.8(2) . . . . ?
N8 C8 C12 C11 -90.71(19) . . . . ?
C9 C8 C12 C11 27.9(2) . . . . ?
C10 C11 C12 C8 -8.1(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.338
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.061

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px206
_database_code_depnum_ccdc_archive 'CCDC 2061071'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-05-29
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'dinitrato tris(1-cyclobutyl-5H-tetrazolyl) copper(II)'
_chemical_name_common            
'dinitrato tris(1-cyclobutyl-5H-tetrazolyl) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 Cu N14 O6'
_chemical_formula_sum            'C15 H24 Cu N14 O6'
_chemical_formula_weight         560.02

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I a'
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'I -2ya'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'

_cell_length_a                   10.4489(4)
_cell_length_b                   13.0298(5)
_cell_length_c                   17.6353(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.235(4)
_cell_angle_gamma                90
_cell_volume                     2346.46(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    8379
_cell_measurement_theta_min      2.5390
_cell_measurement_theta_max      31.8950

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.198
_exptl_absorpt_coefficient_mu    0.995
_shelx_estimated_absorpt_T_min   0.700
_shelx_estimated_absorpt_T_max   0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_F_000             1156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            23149
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.959
_diffrn_reflns_theta_max         30.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7161
_reflns_number_gt                6720
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0276P)²+0.4941P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;

_refine_ls_abs_structure_Flack   0.381(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7161
_refine_ls_number_parameters     422
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0604
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0522833000
_diffrn_orient_matrix_UB_12      -0.0350506000
_diffrn_orient_matrix_UB_13      0.0010553000
_diffrn_orient_matrix_UB_21      0.0182433000
_diffrn_orient_matrix_UB_22      0.0055921000
_diffrn_orient_matrix_UB_23      0.0408972000
_diffrn_orient_matrix_UB_31      -0.0419517000
_diffrn_orient_matrix_UB_32      -0.0412392000
_diffrn_orient_matrix_UB_33      0.0046261000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00 -46.00   1.00   12.00    --  -28.70 153.00 109.00   57
  2  ω    -54.00  37.00   1.00   12.00    --  -28.70  77.00 -30.00   91
  3  ω    -61.00  30.00   1.00   12.00    --  -28.70  77.00  60.00   91
  4  ω     39.00 102.00   1.00   12.00    --   29.64 178.00-150.00   63
  5  ω    -21.00  12.00   1.00   12.00    --   29.64 110.00 -88.81   33
  6  ω      6.00  82.00   1.00   12.00    --   29.64  57.00  30.00   76
  7  ω    -41.00  -1.00   1.00   12.00    --   29.64 -57.00-180.00   40
  8  ω      6.00 100.00   1.00   12.00    --   29.64  57.00 120.00   94
  9  ω    -33.00  -4.00   1.00   12.00    --   29.64 130.00  68.25   29
 10  ω     -3.00 103.00   1.00   12.00    --   29.64  37.00 -30.00  106
 11  ω      6.00 100.00   1.00   12.00    --   29.64  57.00-150.00   94
 12  ω    -43.00  59.00   1.00   12.00    --   29.64 -37.00-150.00  102
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.50122(2) 0.77815(2) 0.51765(2) 0.01276(6) Uani 1 1 d . . . . .
O1 O 0.6803(2) 0.78398(14) 0.58558(14) 0.0195(5) Uani 1 1 d . . . . .
O5 O 0.1818(2) 0.86830(19) 0.37649(14) 0.0279(5) Uani 1 1 d . . . . .
O3 O 0.6350(2) 0.94679(16) 0.57867(13) 0.0281(5) Uani 1 1 d . . . . .
O6 O 0.3399(2) 0.93130(16) 0.46513(13) 0.0257(5) Uani 1 1 d . . . . .
N8 N 0.4967(2) 0.44505(13) 0.51364(16) 0.0132(3) Uani 1 1 d . . . . .
O4 O 0.3243(2) 0.76667(15) 0.44666(13) 0.0173(4) Uani 1 1 d . . . . .
N14 N 0.2805(2) 0.85768(18) 0.42877(14) 0.0167(4) Uani 1 1 d . . . . .
N9 N 0.4184(2) 0.78053(15) 0.61068(15) 0.0133(5) Uani 1 1 d . . . . .
O2 O 0.8204(2) 0.89399(18) 0.64722(14) 0.0296(5) Uani 1 1 d . . . . .
N13 N 0.7119(2) 0.87711(18) 0.60448(14) 0.0180(5) Uani 1 1 d . . . . .
N12 N 0.3321(2) 0.81243(17) 0.70864(12) 0.0152(4) Uani 1 1 d . . . . .
N5 N 0.5204(2) 0.60900(15) 0.51369(14) 0.0152(4) Uani 1 1 d . . . . .
N6 N 0.6343(2) 0.56306(17) 0.50768(14) 0.0180(4) Uani 1 1 d . . . . .
N1 N 0.5772(2) 0.80583(18) 0.42367(14) 0.0161(4) Uani 1 1 d . . . . .
N4 N 0.6807(2) 0.85993(17) 0.33882(12) 0.0171(4) Uani 1 1 d . . . . .
N3 N 0.6254(2) 0.76960(17) 0.31303(13) 0.0196(4) Uani 1 1 d . . . . .
N11 N 0.3450(2) 0.70958(17) 0.70441(13) 0.0197(4) Uani 1 1 d . . . . .
N10 N 0.3967(2) 0.69075(17) 0.64576(13) 0.0185(4) Uani 1 1 d . . . . .
N7 N 0.6215(2) 0.46457(16) 0.50771(13) 0.0184(4) Uani 1 1 d . . . . .
N2 N 0.5632(2) 0.73664(17) 0.36429(13) 0.0202(4) Uani 1 1 d . . . . .
C7 C 0.4480(2) 0.33960(18) 0.51304(15) 0.0158(4) Uani 1 1 d . . . . .
C3 C 0.8627(3) 0.8570(2) 0.26039(16) 0.0228(5) Uani 1 1 d . . . . .
C1 C 0.6496(3) 0.8812(2) 0.40634(15) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.7633(3) 0.91736(19) 0.29550(15) 0.0187(5) Uani 1 1 d . . . . .
C15 C 0.3300(3) 0.9600(3) 0.80493(18) 0.0261(6) Uani 1 1 d . . . . .
C6 C 0.4369(2) 0.53476(18) 0.51716(14) 0.0148(4) Uani 1 1 d . . . . .
C4 C 0.8317(3) 0.9322(2) 0.19082(17) 0.0231(5) Uani 1 1 d . . . . .
C12 C 0.2753(3) 0.8579(2) 0.76984(15) 0.0195(5) Uani 1 1 d . . . . .
C10 C 0.4688(4) 0.2693(2) 0.4473(2) 0.0299(8) Uani 1 1 d . . . . .
C13 C 0.1383(3) 0.9068(2) 0.74697(19) 0.0265(6) Uani 1 1 d . . . . .
C9 C 0.4948(5) 0.1820(2) 0.5084(3) 0.0381(9) Uani 1 1 d . . . . .
C11 C 0.3774(3) 0.8548(2) 0.65069(15) 0.0165(5) Uani 1 1 d . . . . .
C5 C 0.7006(3) 0.9571(3) 0.21427(19) 0.0250(6) Uani 1 1 d . . . . .
C8 C 0.5256(4) 0.2639(3) 0.5722(2) 0.0298(8) Uani 1 1 d . . . . .
C14 C 0.1887(4) 0.9892(3) 0.8094(2) 0.0358(7) Uani 1 1 d . . . . .
H7 H 0.363(3) 0.347(3) 0.5189(19) 0.027(9) Uiso 1 1 d . . . . .
H3A H 0.945(4) 0.856(3) 0.286(2) 0.036(11) Uiso 1 1 d . . . . .
H2 H 0.810(3) 0.969(2) 0.3314(18) 0.019(8) Uiso 1 1 d . . . . .
H1 H 0.680(3) 0.937(2) 0.4353(17) 0.013(7) Uiso 1 1 d . . . . .
H8A H 0.502(4) 0.260(3) 0.620(2) 0.034(10) Uiso 1 1 d . . . . .
H15A H 0.387(4) 0.956(3) 0.846(2) 0.032(10) Uiso 1 1 d . . . . .
H9A H 0.410(4) 0.150(3) 0.504(2) 0.031(9) Uiso 1 1 d . . . . .
H9B H 0.546(4) 0.137(3) 0.504(2) 0.042(11) Uiso 1 1 d . . . . .
H4A H 0.821(3) 0.899(3) 0.142(2) 0.026(8) Uiso 1 1 d . . . . .
H5A H 0.639(3) 0.910(3) 0.1894(19) 0.019(8) Uiso 1 1 d . . . . .
H3B H 0.838(4) 0.785(3) 0.246(2) 0.038(10) Uiso 1 1 d . . . . .
H10A H 0.552(4) 0.290(3) 0.432(2) 0.036(10) Uiso 1 1 d . . . . .
H13A H 0.116(3) 0.934(3) 0.694(2) 0.028(9) Uiso 1 1 d . . . . .
H12 H 0.281(3) 0.810(3) 0.8074(19) 0.023(8) Uiso 1 1 d . . . . .
H13B H 0.055(4) 0.866(4) 0.749(3) 0.046(12) Uiso 1 1 d . . . . .
H4B H 0.889(3) 0.989(3) 0.198(2) 0.029(9) Uiso 1 1 d . . . . .
H11 H 0.377(3) 0.923(2) 0.6404(18) 0.015(7) Uiso 1 1 d . . . . .
H15B H 0.355(3) 1.002(3) 0.7699(19) 0.022(8) Uiso 1 1 d . . . . .
H6 H 0.357(3) 0.548(2) 0.5241(17) 0.007(7) Uiso 1 1 d . . . . .
H8B H 0.604(4) 0.285(3) 0.585(2) 0.033(10) Uiso 1 1 d . . . . .
H5B H 0.676(4) 1.026(4) 0.215(2) 0.052(12) Uiso 1 1 d . . . . .
H10B H 0.379(4) 0.270(3) 0.400(3) 0.046(11) Uiso 1 1 d . . . . .
H14A H 0.155(4) 1.059(3) 0.794(2) 0.042(10) Uiso 1 1 d . . . . .
H14B H 0.172(4) 0.977(3) 0.856(3) 0.047(12) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.998(2) . ?
Cu1 O4 2.006(2) . ?
Cu1 N9 2.011(3) . ?
Cu1 N1 2.016(2) . ?
Cu1 N5 2.216(2) . ?
O1 N13 1.283(3) . ?
O5 N14 1.237(3) . ?
O3 N13 1.233(3) . ?
O6 N14 1.244(3) . ?
N8 C6 1.333(3) . ?
N8 N7 1.354(3) . ?
N8 C7 1.464(3) . ?
O4 N14 1.286(3) . ?
N9 C11 1.321(3) . ?
N9 N10 1.365(3) . ?
O2 N13 1.241(3) . ?
N12 C11 1.333(3) . ?
N12 N11 1.350(3) . ?
N12 C12 1.463(3) . ?
N5 C6 1.313(3) . ?
N5 N6 1.356(3) . ?
N6 N7 1.290(3) . ?
N1 C1 1.315(4) . ?
N1 N2 1.366(3) . ?
N4 C1 1.328(3) . ?
N4 N3 1.347(3) . ?
N4 C2 1.473(3) . ?
N3 N2 1.293(3) . ?
N11 N10 1.288(3) . ?
C7 C10 1.529(4) . ?
C7 C8 1.536(4) . ?
C7 H7 0.92(3) . ?
C3 C2 1.534(4) . ?
C3 C4 1.550(4) . ?
C3 H3A 0.88(4) . ?
C3 H3B 1.00(4) . ?
C1 H1 0.91(3) . ?
C2 C5 1.533(4) . ?
C2 H2 0.99(3) . ?
C15 C12 1.526(4) . ?
C15 C14 1.543(5) . ?
C15 H15A 0.84(4) . ?
C15 H15B 0.90(3) . ?
C6 H6 0.89(3) . ?
C4 C5 1.546(4) . ?
C4 H4A 0.94(4) . ?
C4 H4B 0.95(4) . ?
C12 C13 1.540(4) . ?
C12 H12 0.90(3) . ?
C10 C9 1.550(6) . ?
C10 H10A 1.00(4) . ?
C10 H10B 1.12(5) . ?
C13 C14 1.548(4) . ?
C13 H13A 0.97(4) . ?
C13 H13B 1.02(4) . ?
C9 C8 1.535(6) . ?
C9 H9A 0.97(4) . ?
C9 H9B 0.81(4) . ?
C11 H11 0.90(3) . ?
C5 H5A 0.93(3) . ?
C5 H5B 0.94(5) . ?
C8 H8A 0.93(4) . ?
C8 H8B 0.85(4) . ?
C14 H14A 0.99(4) . ?
C14 H14B 0.89(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O4 177.23(9) . . ?
O1 Cu1 N9 91.18(10) . . ?
O4 Cu1 N9 90.65(10) . . ?
O1 Cu1 N1 90.25(10) . . ?
O4 Cu1 N1 88.36(9) . . ?
N9 Cu1 N1 168.66(9) . . ?
O1 Cu1 N5 88.69(8) . . ?
O4 Cu1 N5 89.07(8) . . ?
N9 Cu1 N5 95.66(8) . . ?
N1 Cu1 N5 95.62(9) . . ?
N13 O1 Cu1 110.37(18) . . ?
C6 N8 N7 107.87(18) . . ?
C6 N8 C7 131.2(2) . . ?
N7 N8 C7 120.9(2) . . ?
N14 O4 Cu1 108.49(17) . . ?
O5 N14 O6 123.0(2) . . ?
O5 N14 O4 118.9(2) . . ?
O6 N14 O4 118.1(2) . . ?
C11 N9 N10 106.4(2) . . ?
C11 N9 Cu1 133.74(18) . . ?
N10 N9 Cu1 119.89(16) . . ?
O3 N13 O2 122.2(2) . . ?
O3 N13 O1 119.3(3) . . ?
O2 N13 O1 118.5(2) . . ?
C11 N12 N11 108.2(2) . . ?
C11 N12 C12 131.5(2) . . ?
N11 N12 C12 120.2(2) . . ?
C6 N5 N6 106.34(19) . . ?
C6 N5 Cu1 131.76(16) . . ?
N6 N5 Cu1 121.89(15) . . ?
N7 N6 N5 110.2(2) . . ?
C1 N1 N2 106.7(2) . . ?
C1 N1 Cu1 132.13(19) . . ?
N2 N1 Cu1 121.04(17) . . ?
C1 N4 N3 108.4(2) . . ?
C1 N4 C2 129.8(2) . . ?
N3 N4 C2 121.7(2) . . ?
N2 N3 N4 107.3(2) . . ?
N10 N11 N12 107.3(2) . . ?
N11 N10 N9 109.8(2) . . ?
N6 N7 N8 106.79(19) . . ?
N3 N2 N1 109.2(2) . . ?
N8 C7 C10 117.6(2) . . ?
N8 C7 C8 117.7(2) . . ?
C10 C7 C8 89.5(2) . . ?
N8 C7 H7 104(2) . . ?
C10 C7 H7 116(2) . . ?
C8 C7 H7 112(2) . . ?
C2 C3 C4 87.1(2) . . ?
C2 C3 H3A 118(3) . . ?
C4 C3 H3A 116(3) . . ?
C2 C3 H3B 115(2) . . ?
C4 C3 H3B 113(2) . . ?
H3A C3 H3B 107(4) . . ?
N1 C1 N4 108.3(2) . . ?
N1 C1 H1 128.4(18) . . ?
N4 C1 H1 123.1(19) . . ?
N4 C2 C5 118.3(2) . . ?
N4 C2 C3 118.1(2) . . ?
C5 C2 C3 89.3(2) . . ?
N4 C2 H2 106.6(18) . . ?
C5 C2 H2 115.1(18) . . ?
C3 C2 H2 108.8(18) . . ?
C12 C15 C14 87.5(2) . . ?
C12 C15 H15A 115(3) . . ?
C14 C15 H15A 119(3) . . ?
C12 C15 H15B 113(2) . . ?
C14 C15 H15B 108(2) . . ?
H15A C15 H15B 113(3) . . ?
N5 C6 N8 108.8(2) . . ?
N5 C6 H6 120.9(19) . . ?
N8 C6 H6 130.2(19) . . ?
C5 C4 C3 88.3(2) . . ?
C5 C4 H4A 113(2) . . ?
C3 C4 H4A 113(2) . . ?
C5 C4 H4B 112(2) . . ?
C3 C4 H4B 112(2) . . ?
H4A C4 H4B 116(3) . . ?
N12 C12 C15 118.5(2) . . ?
N12 C12 C13 118.3(2) . . ?
C15 C12 C13 89.6(2) . . ?
N12 C12 H12 107(2) . . ?
C15 C12 H12 110(2) . . ?
C13 C12 H12 113(2) . . ?
C7 C10 C9 86.8(3) . . ?
C7 C10 H10A 108(2) . . ?
C9 C10 H10A 110(2) . . ?
C7 C10 H10B 109(2) . . ?
C9 C10 H10B 122(2) . . ?
H10A C10 H10B 116(3) . . ?
C12 C13 C14 86.7(2) . . ?
C12 C13 H13A 115(2) . . ?
C14 C13 H13A 114(2) . . ?
C12 C13 H13B 122(3) . . ?
C14 C13 H13B 120(3) . . ?
H13A C13 H13B 101(3) . . ?
C8 C9 C10 88.8(2) . . ?
C8 C9 H9A 114(2) . . ?
C10 C9 H9A 104(2) . . ?
C8 C9 H9B 122(3) . . ?
C10 C9 H9B 119(3) . . ?
H9A C9 H9B 107(3) . . ?
N9 C11 N12 108.3(2) . . ?
N9 C11 H11 126.6(19) . . ?
N12 C11 H11 125.1(19) . . ?
C2 C5 C4 87.2(2) . . ?
C2 C5 H5A 110(2) . . ?
C4 C5 H5A 107.7(19) . . ?
C2 C5 H5B 112(3) . . ?
C4 C5 H5B 117(2) . . ?
H5A C5 H5B 118(3) . . ?
C9 C8 C7 87.1(3) . . ?
C9 C8 H8A 125(2) . . ?
C7 C8 H8A 117(3) . . ?
C9 C8 H8B 117(3) . . ?
C7 C8 H8B 109(3) . . ?
H8A C8 H8B 102(4) . . ?
C15 C14 C13 88.7(2) . . ?
C15 C14 H14A 120(2) . . ?
C13 C14 H14A 113(2) . . ?
C15 C14 H14B 112(3) . . ?
C13 C14 H14B 115(3) . . ?
H14A C14 H14B 107(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O4 N14 O5 169.32(19) . . . . ?
Cu1 O4 N14 O6 -10.7(3) . . . . ?
Cu1 O1 N13 O3 -1.8(3) . . . . ?
Cu1 O1 N13 O2 179.5(2) . . . . ?
C6 N5 N6 N7 -0.2(3) . . . . ?
Cu1 N5 N6 N7 179.00(17) . . . . ?
C1 N4 N3 N2 -0.6(3) . . . . ?
C2 N4 N3 N2 177.8(2) . . . . ?
C11 N12 N11 N10 0.1(3) . . . . ?
C12 N12 N11 N10 179.8(2) . . . . ?
N12 N11 N10 N9 0.0(3) . . . . ?
C11 N9 N10 N11 -0.1(3) . . . . ?
Cu1 N9 N10 N11 179.08(18) . . . . ?
N5 N6 N7 N8 0.2(3) . . . . ?
C6 N8 N7 N6 -0.1(3) . . . . ?
C7 N8 N7 N6 178.2(2) . . . . ?
N4 N3 N2 N1 0.4(3) . . . . ?
C1 N1 N2 N3 0.0(3) . . . . ?
Cu1 N1 N2 N3 -176.97(19) . . . . ?
C6 N8 C7 C10 126.8(4) . . . . ?
N7 N8 C7 C10 -51.1(4) . . . . ?
C6 N8 C7 C8 -128.0(3) . . . . ?
N7 N8 C7 C8 54.2(4) . . . . ?
N2 N1 C1 N4 -0.4(3) . . . . ?
Cu1 N1 C1 N4 176.13(19) . . . . ?
N3 N4 C1 N1 0.6(3) . . . . ?
C2 N4 C1 N1 -177.6(3) . . . . ?
C1 N4 C2 C5 -118.8(3) . . . . ?
N3 N4 C2 C5 63.2(3) . . . . ?
C1 N4 C2 C3 135.5(3) . . . . ?
N3 N4 C2 C3 -42.6(4) . . . . ?
C4 C3 C2 N4 143.5(2) . . . . ?
C4 C3 C2 C5 21.4(2) . . . . ?
N6 N5 C6 N8 0.2(3) . . . . ?
Cu1 N5 C6 N8 -178.9(2) . . . . ?
N7 N8 C6 N5 -0.1(3) . . . . ?
C7 N8 C6 N5 -178.1(3) . . . . ?
C2 C3 C4 C5 -21.2(2) . . . . ?
C11 N12 C12 C15 -36.4(4) . . . . ?
N11 N12 C12 C15 144.0(3) . . . . ?
C11 N12 C12 C13 70.0(4) . . . . ?
N11 N12 C12 C13 -109.6(3) . . . . ?
C14 C15 C12 N12 143.0(3) . . . . ?
C14 C15 C12 C13 20.6(2) . . . . ?
N8 C7 C10 C9 142.2(3) . . . . ?
C8 C7 C10 C9 20.9(3) . . . . ?
N12 C12 C13 C14 -143.0(3) . . . . ?
C15 C12 C13 C14 -20.5(2) . . . . ?
C7 C10 C9 C8 -20.9(3) . . . . ?
N10 N9 C11 N12 0.1(3) . . . . ?
Cu1 N9 C11 N12 -178.8(2) . . . . ?
N11 N12 C11 N9 -0.2(3) . . . . ?
C12 N12 C11 N9 -179.8(2) . . . . ?
N4 C2 C5 C4 -143.3(2) . . . . ?
C3 C2 C5 C4 -21.4(2) . . . . ?
C3 C4 C5 C2 21.2(2) . . . . ?
C10 C9 C8 C7 20.8(3) . . . . ?
N8 C7 C8 C9 -142.3(3) . . . . ?
C10 C7 C8 C9 -21.1(3) . . . . ?
C12 C15 C14 C13 -20.5(2) . . . . ?
C12 C13 C14 C15 20.3(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.416
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.050

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px215
_database_code_depnum_ccdc_archive 'CCDC 2061074'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-04
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        'hexakis(1-cyclopropyl)iron(II) perchlorate'
_chemical_name_common            'hexakis(1-cyclopropyl)iron(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C24 H36 Fe N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Fe N24 O8'
_chemical_formula_weight         915.52

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.7309(7)
_cell_length_b                   10.7309(7)
_cell_length_c                   29.207(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2912.7(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    107(2)
_cell_measurement_reflns_used    1967
_cell_measurement_theta_min      2.3010
_cell_measurement_theta_max      28.4180

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.152
_exptl_absorpt_coefficient_mu    0.605
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      107(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            5417
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.300
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1341
_reflns_number_gt                1169
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+4.2453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1341
_refine_ls_number_parameters     114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0425468000
_diffrn_orient_matrix_UB_12      -0.0299954000
_diffrn_orient_matrix_UB_13      -0.0199042000
_diffrn_orient_matrix_UB_21      0.0444685000
_diffrn_orient_matrix_UB_22      -0.0283819000
_diffrn_orient_matrix_UB_23      -0.0066094000
_diffrn_orient_matrix_UB_31      -0.0451872000
_diffrn_orient_matrix_UB_32      -0.0642234000
_diffrn_orient_matrix_UB_33      0.0122100000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  39.00   1.00   25.00    --  -20.37  77.00 150.00   92
  2  ω     -2.00  89.00   1.00   25.00    --   21.23  57.00  60.00   91
  3  ω     -9.00  25.00   1.00   25.00    --   21.23  77.00 -90.00   34
  4  ω    -49.00  45.00   1.00   25.00    --   21.23 -57.00 -90.00   94
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.000000 1.000000 0.500000 0.01151(16) Uani 1 6 d S T P . .
Cl1 Cl 0.333333 0.666667 0.51199(2) 0.01787(18) Uani 1 3 d S T P . .
N1 N 0.82550(14) 0.89057(15) 0.46043(4) 0.0146(3) Uani 1 1 d . . . . .
O1 O 0.28756(16) 0.52447(14) 0.49491(5) 0.0319(4) Uani 1 1 d . . . . .
N4 N 0.64715(15) 0.73149(15) 0.42116(5) 0.0155(3) Uani 1 1 d . . . . .
N2 N 0.77920(16) 0.95699(16) 0.43063(5) 0.0204(3) Uani 1 1 d . . . . .
O2 O 0.333333 0.666667 0.56067(8) 0.0412(7) Uani 1 3 d S T P . .
N3 N 0.67156(16) 0.86194(16) 0.40719(5) 0.0214(3) Uani 1 1 d . . . . .
C1 C 0.74125(17) 0.75107(18) 0.45390(6) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.52388(19) 0.59922(18) 0.40517(6) 0.0182(4) Uani 1 1 d . . . . .
C3 C 0.4986(2) 0.5804(2) 0.35486(6) 0.0243(4) Uani 1 1 d . . . . .
C4 C 0.5497(2) 0.4932(2) 0.38024(7) 0.0244(4) Uani 1 1 d . . . . .
H1 H 0.748(2) 0.678(2) 0.4677(7) 0.021(5) Uiso 1 1 d . . . . .
H2 H 0.449(2) 0.569(2) 0.4237(7) 0.021(5) Uiso 1 1 d . . . . .
H3A H 0.401(2) 0.536(2) 0.3448(7) 0.027(5) Uiso 1 1 d . . . . .
H4A H 0.484(2) 0.392(2) 0.3862(7) 0.030(6) Uiso 1 1 d . . . . .
H4B H 0.645(2) 0.517(2) 0.3757(6) 0.020(5) Uiso 1 1 d . . . . .
H3B H 0.565(2) 0.656(2) 0.3360(7) 0.028(5) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.0055(14) 12_656 ?
Fe1 N1 2.0055(14) 3_675 ?
Fe1 N1 2.0055(14) 10_776 ?
Fe1 N1 2.0055(14) . ?
Fe1 N1 2.0055(14) 11_566 ?
Fe1 N1 2.0055(14) 2_765 ?
Cl1 O2 1.422(2) . ?
Cl1 O1 1.4383(13) 3_565 ?
Cl1 O1 1.4383(14) 2_665 ?
Cl1 O1 1.4383(13) . ?
N1 C1 1.320(2) . ?
N1 N2 1.3662(19) . ?
N4 C1 1.329(2) . ?
N4 N3 1.352(2) . ?
N4 C2 1.451(2) . ?
N2 N3 1.290(2) . ?
C1 H1 0.92(2) . ?
C2 C4 1.489(3) . ?
C2 C3 1.490(2) . ?
C2 H2 0.89(2) . ?
C3 C4 1.496(3) . ?
C3 H3A 0.95(2) . ?
C3 H3B 0.94(2) . ?
C4 H4A 0.97(2) . ?
C4 H4B 0.93(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 180.0 12_656 3_675 ?
N1 Fe1 N1 90.11(5) 12_656 10_776 ?
N1 Fe1 N1 89.89(5) 3_675 10_776 ?
N1 Fe1 N1 89.89(5) 12_656 . ?
N1 Fe1 N1 90.11(5) 3_675 . ?
N1 Fe1 N1 180.0 10_776 . ?
N1 Fe1 N1 90.11(5) 12_656 11_566 ?
N1 Fe1 N1 89.89(5) 3_675 11_566 ?
N1 Fe1 N1 90.11(5) 10_776 11_566 ?
N1 Fe1 N1 89.89(5) . 11_566 ?
N1 Fe1 N1 89.89(5) 12_656 2_765 ?
N1 Fe1 N1 90.11(5) 3_675 2_765 ?
N1 Fe1 N1 89.89(5) 10_776 2_765 ?
N1 Fe1 N1 90.11(5) . 2_765 ?
N1 Fe1 N1 180.00(6) 11_566 2_765 ?
O2 Cl1 O1 110.28(6) . 3_565 ?
O2 Cl1 O1 110.28(6) . 2_665 ?
O1 Cl1 O1 108.65(6) 3_565 2_665 ?
O2 Cl1 O1 110.28(6) . . ?
O1 Cl1 O1 108.65(6) 3_565 . ?
O1 Cl1 O1 108.65(6) 2_665 . ?
C1 N1 N2 106.15(13) . . ?
C1 N1 Fe1 131.07(11) . . ?
N2 N1 Fe1 122.57(11) . . ?
C1 N4 N3 108.36(14) . . ?
C1 N4 C2 129.44(15) . . ?
N3 N4 C2 121.72(13) . . ?
N3 N2 N1 109.93(14) . . ?
N2 N3 N4 106.97(13) . . ?
N1 C1 N4 108.58(15) . . ?
N1 C1 H1 127.3(12) . . ?
N4 C1 H1 124.0(13) . . ?
N4 C2 C4 118.57(16) . . ?
N4 C2 C3 117.73(15) . . ?
C4 C2 C3 60.32(13) . . ?
N4 C2 H2 112.0(13) . . ?
C4 C2 H2 120.4(13) . . ?
C3 C2 H2 118.8(13) . . ?
C2 C3 C4 59.83(12) . . ?
C2 C3 H3A 116.9(12) . . ?
C4 C3 H3A 119.5(13) . . ?
C2 C3 H3B 116.9(13) . . ?
C4 C3 H3B 118.0(13) . . ?
H3A C3 H3B 114.7(17) . . ?
C2 C4 C3 59.86(12) . . ?
C2 C4 H4A 117.2(13) . . ?
C3 C4 H4A 120.0(13) . . ?
C2 C4 H4B 117.1(12) . . ?
C3 C4 H4B 116.8(12) . . ?
H4A C4 H4B 114.9(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.14(18) . . . . ?
Fe1 N1 N2 N3 175.43(11) . . . . ?
N1 N2 N3 N4 -0.65(18) . . . . ?
C1 N4 N3 N2 0.93(18) . . . . ?
C2 N4 N3 N2 173.62(15) . . . . ?
N2 N1 C1 N4 0.45(18) . . . . ?
Fe1 N1 C1 N4 -174.29(11) . . . . ?
N3 N4 C1 N1 -0.86(18) . . . . ?
C2 N4 C1 N1 -172.80(15) . . . . ?
C1 N4 C2 C4 -68.5(2) . . . . ?
N3 N4 C2 C4 120.45(18) . . . . ?
C1 N4 C2 C3 -138.00(18) . . . . ?
N3 N4 C2 C3 51.0(2) . . . . ?
N4 C2 C3 C4 108.80(18) . . . . ?
N4 C2 C4 C3 -107.42(18) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.337
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.051

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px217
_database_code_depnum_ccdc_archive 'CCDC 2061073'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-05
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'hexakis(1-cyclopropyl-5H-tetrazolyl)manganese(II) diperchlorate'
_chemical_name_common            
'hexakis(1-cyclopropyl-5H-tetrazolyl)manganese(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C24 H36 Mn N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Mn N24 O8'
_chemical_formula_weight         914.61

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.8880(6)
_cell_length_b                   10.8880(6)
_cell_length_c                   29.5174(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3030.4(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    106(2)
_cell_measurement_reflns_used    1240
_cell_measurement_theta_min      2.5280
_cell_measurement_theta_max      30.1090

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.642
_exptl_crystal_size_mid          0.594
_exptl_crystal_size_min          0.142
_exptl_absorpt_coefficient_mu    0.535
_shelx_estimated_absorpt_T_min   0.725
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_F_000             1413
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      106(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            2261
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.070
_diffrn_reflns_theta_max         26.328
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1385
_reflns_number_gt                1240
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²+2.7176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1385
_refine_ls_number_parameters     114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0734
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0409365000
_diffrn_orient_matrix_UB_12      0.0084596000
_diffrn_orient_matrix_UB_13      0.0196922000
_diffrn_orient_matrix_UB_21      0.0631017000
_diffrn_orient_matrix_UB_22      0.0412100000
_diffrn_orient_matrix_UB_23      -0.0125853000
_diffrn_orient_matrix_UB_31      -0.0019232000
_diffrn_orient_matrix_UB_32      0.0622747000
_diffrn_orient_matrix_UB_33      0.0056583000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  -3.00   1.00   30.00    --  -24.42 -57.00-180.00   67
  2  ω    -24.00  39.00   1.00   30.00    --   25.20 -57.00 -90.00   63
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.666667 0.333333 0.333333 0.01444(16) Uani 1 6 d S T P . .
Cl1 Cl 0.333333 0.666667 0.32421(2) 0.01978(18) Uani 1 3 d S T P . .
N4 N 0.38038(13) 0.41233(13) 0.41608(4) 0.0176(3) Uani 1 1 d . . . . .
O1 O 0.42915(14) 0.62244(14) 0.34103(5) 0.0345(3) Uani 1 1 d . . . . .
N1 N 0.53711(14) 0.39488(13) 0.37699(4) 0.0186(3) Uani 1 1 d . . . . .
N3 N 0.50839(14) 0.51123(15) 0.43185(5) 0.0234(3) Uani 1 1 d . . . . .
O2 O 0.333333 0.666667 0.27611(7) 0.0456(7) Uani 1 3 d S T P . .
N2 N 0.60225(14) 0.50008(14) 0.40845(5) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.40019(16) 0.34322(16) 0.38253(5) 0.0189(3) Uani 1 1 d . . . . .
C2 C 0.25087(16) 0.40580(18) 0.43134(5) 0.0202(3) Uani 1 1 d . . . . .
C3 C 0.22800(19) 0.40598(19) 0.48121(6) 0.0253(4) Uani 1 1 d . . . . .
C4 C 0.14224(19) 0.2737(2) 0.45415(6) 0.0276(4) Uani 1 1 d . . . . .
H2 H 0.2199(18) 0.4518(19) 0.4116(6) 0.019(4) Uiso 1 1 d . . . . .
H3A H 0.298(2) 0.409(2) 0.5007(7) 0.028(5) Uiso 1 1 d . . . . .
H1 H 0.327(2) 0.270(2) 0.3678(6) 0.022(4) Uiso 1 1 d . . . . .
H4A H 0.046(2) 0.2448(19) 0.4471(7) 0.028(5) Uiso 1 1 d . . . . .
H3B H 0.187(2) 0.460(2) 0.4900(6) 0.027(5) Uiso 1 1 d . . . . .
H4B H 0.163(2) 0.200(2) 0.4574(7) 0.034(5) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N1 2.2461(13) . ?
Mn1 N1 2.2461(13) 3_665 ?
Mn1 N1 2.2461(13) 2_655 ?
Mn1 N1 2.2461(13) 17 ?
Mn1 N1 2.2461(13) 18_545 ?
Mn1 N1 2.2462(13) 16_655 ?
Cl1 O2 1.420(2) . ?
Cl1 O1 1.4383(12) 3_565 ?
Cl1 O1 1.4383(12) . ?
Cl1 O1 1.4384(12) 2_665 ?
N4 C1 1.325(2) . ?
N4 N3 1.3483(19) . ?
N4 C2 1.4478(19) . ?
N1 C1 1.314(2) . ?
N1 N2 1.3655(19) . ?
N3 N2 1.2884(19) . ?
C1 H1 0.906(19) . ?
C2 C4 1.490(2) . ?
C2 C3 1.493(2) . ?
C2 H2 0.935(18) . ?
C3 C4 1.497(3) . ?
C3 H3A 0.95(2) . ?
C3 H3B 0.94(2) . ?
C4 H4A 0.96(2) . ?
C4 H4B 0.95(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mn1 N1 90.36(5) . 3_665 ?
N1 Mn1 N1 90.36(5) . 2_655 ?
N1 Mn1 N1 90.36(5) 3_665 2_655 ?
N1 Mn1 N1 89.65(5) . 17 ?
N1 Mn1 N1 89.64(5) 3_665 17 ?
N1 Mn1 N1 180.0 2_655 17 ?
N1 Mn1 N1 89.64(5) . 18_545 ?
N1 Mn1 N1 180.0 3_665 18_545 ?
N1 Mn1 N1 89.64(5) 2_655 18_545 ?
N1 Mn1 N1 90.36(5) 17 18_545 ?
N1 Mn1 N1 180.0 . 16_655 ?
N1 Mn1 N1 89.64(5) 3_665 16_655 ?
N1 Mn1 N1 89.64(5) 2_655 16_655 ?
N1 Mn1 N1 90.35(5) 17 16_655 ?
N1 Mn1 N1 90.35(5) 18_545 16_655 ?
O2 Cl1 O1 110.18(6) . 3_565 ?
O2 Cl1 O1 110.18(6) . . ?
O1 Cl1 O1 108.75(6) 3_565 . ?
O2 Cl1 O1 110.18(6) . 2_665 ?
O1 Cl1 O1 108.75(6) 3_565 2_665 ?
O1 Cl1 O1 108.75(6) . 2_665 ?
C1 N4 N3 108.34(13) . . ?
C1 N4 C2 129.48(14) . . ?
N3 N4 C2 121.62(13) . . ?
C1 N1 N2 106.06(13) . . ?
C1 N1 Mn1 133.70(11) . . ?
N2 N1 Mn1 120.01(9) . . ?
N2 N3 N4 106.95(12) . . ?
N3 N2 N1 109.86(12) . . ?
N1 C1 N4 108.77(14) . . ?
N1 C1 H1 128.9(12) . . ?
N4 C1 H1 122.3(12) . . ?
N4 C2 C4 118.13(14) . . ?
N4 C2 C3 117.76(14) . . ?
C4 C2 C3 60.22(12) . . ?
N4 C2 H2 112.5(11) . . ?
C4 C2 H2 118.3(11) . . ?
C3 C2 H2 120.6(11) . . ?
C2 C3 C4 59.79(11) . . ?
C2 C3 H3A 117.8(12) . . ?
C4 C3 H3A 117.3(12) . . ?
C2 C3 H3B 114.0(12) . . ?
C4 C3 H3B 119.3(12) . . ?
H3A C3 H3B 116.4(17) . . ?
C2 C4 C3 59.98(11) . . ?
C2 C4 H4A 115.4(11) . . ?
C3 C4 H4A 119.1(11) . . ?
C2 C4 H4B 117.1(13) . . ?
C3 C4 H4B 117.8(13) . . ?
H4A C4 H4B 115.7(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 -0.63(17) . . . . ?
C2 N4 N3 N2 -172.84(14) . . . . ?
N4 N3 N2 N1 0.44(17) . . . . ?
C1 N1 N2 N3 -0.08(18) . . . . ?
Mn1 N1 N2 N3 -175.34(10) . . . . ?
N2 N1 C1 N4 -0.32(17) . . . . ?
Mn1 N1 C1 N4 174.00(10) . . . . ?
N3 N4 C1 N1 0.59(17) . . . . ?
C2 N4 C1 N1 171.99(14) . . . . ?
C1 N4 C2 C4 69.9(2) . . . . ?
N3 N4 C2 C4 -119.73(17) . . . . ?
C1 N4 C2 C3 139.07(17) . . . . ?
N3 N4 C2 C3 -50.5(2) . . . . ?
N4 C2 C3 C4 -108.22(17) . . . . ?
N4 C2 C4 C3 107.61(17) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.329
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.049

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px189
_database_code_depnum_ccdc_archive 'CCDC 2061070'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-05-15
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'aqua tetrakis(1-cyclopentyl-5H-tetrazole) copper(II) diperchlorate'
_chemical_name_common            
'aqua tetrakis(1-cyclopentyl-5H-tetrazole) copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H84 Cu2 N32 O2, 4(Cl O4)'
_chemical_formula_sum            'C48 H84 Cl4 Cu2 N32 O18'
_chemical_formula_weight         1666.35

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0187(5)
_cell_length_b                   12.6481(8)
_cell_length_c                   13.4478(8)
_cell_angle_alpha                86.257(5)
_cell_angle_beta                 73.006(5)
_cell_angle_gamma                82.596(5)
_cell_volume                     1776.63(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    4768
_cell_measurement_theta_min      2.1360
_cell_measurement_theta_max      31.6830

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.188
_exptl_absorpt_coefficient_mu    0.838
_shelx_estimated_absorpt_T_min   0.713
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             866
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            20438
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.946
_diffrn_reflns_theta_max         32.302
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11483
_reflns_number_gt                8487
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²+0.1170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11483
_refine_ls_number_parameters     617
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1416
_refine_ls_wR_factor_gt          0.1171
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0256660000
_diffrn_orient_matrix_UB_12      0.0322600000
_diffrn_orient_matrix_UB_13      0.0441773000
_diffrn_orient_matrix_UB_21      -0.0046552000
_diffrn_orient_matrix_UB_22      -0.0463956000
_diffrn_orient_matrix_UB_23      0.0328793000
_diffrn_orient_matrix_UB_31      0.0625395000
_diffrn_orient_matrix_UB_32      0.0027337000
_diffrn_orient_matrix_UB_33      0.0034279000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -83.00   1.00   10.00    --  -28.86 178.00-180.00   26
  2  ω   -104.00 -51.00   1.00   10.00    --  -28.86-178.00 -30.00   53
  3  ω   -101.00 -63.00   1.00   10.00    --  -28.86 178.00 120.00   38
  4  ω     21.00 100.00   1.00   10.00    --   29.64  57.00  30.00   79
  5  ω     82.00 112.00   1.00   10.00    --   29.64-178.00  60.00   30
  6  ω     53.00  95.00   1.00   10.00    --   29.64  57.00-180.00   42
  7  ω      6.00  91.00   1.00   10.00    --   29.64-127.00 178.00   85
  8  ω    -46.00  83.00   1.00   10.00    --   29.64 -19.00-150.00  129
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.14002(2) 0.56081(2) 0.55231(2) 0.01350(8) Uani 1 1 d . . . . .
Cl1 Cl 0.47690(5) 0.59100(5) 0.74416(5) 0.02205(13) Uani 1 1 d . . . . .
Cl2 Cl 0.50226(5) 0.81527(5) 0.37152(5) 0.02453(13) Uani 1 1 d . . . . .
O1 O 0.36354(16) 0.54739(15) 0.51397(15) 0.0205(4) Uani 1 1 d . . . . .
O2 O 0.50523(17) 0.48332(15) 0.70457(14) 0.0274(4) Uani 1 1 d . . . . .
N12 N 0.23881(16) 0.27294(15) 0.40539(14) 0.0139(3) Uani 1 1 d . . . . .
N5 N 0.14182(17) 0.65179(15) 0.42326(15) 0.0156(4) Uani 1 1 d . . . . .
N9 N 0.16531(17) 0.42622(15) 0.47149(14) 0.0144(3) Uani 1 1 d . . . . .
N13 N 0.12852(17) 0.46887(15) 0.68081(14) 0.0150(4) Uani 1 1 d . . . . .
O5 O 0.45430(19) 0.66365(16) 0.66156(16) 0.0318(4) Uani 1 1 d . . . . .
N11 N 0.14166(17) 0.31151(16) 0.36698(15) 0.0164(4) Uani 1 1 d . . . . .
N1 N 0.14078(17) 0.68757(15) 0.63593(14) 0.0145(3) Uani 1 1 d . . . . .
N8 N 0.17530(18) 0.71798(17) 0.26769(15) 0.0183(4) Uani 1 1 d . . . . .
O3 O 0.36467(19) 0.59487(19) 0.83122(17) 0.0406(5) Uani 1 1 d . . . . .
O4 O 0.5840(2) 0.6167(2) 0.77382(17) 0.0432(6) Uani 1 1 d . . . . .
N10 N 0.09746(17) 0.40415(16) 0.40677(15) 0.0157(4) Uani 1 1 d . . . . .
N4 N 0.19139(17) 0.82325(16) 0.69680(15) 0.0167(4) Uani 1 1 d . . . . .
N16 N 0.16206(18) 0.39216(16) 0.81855(15) 0.0180(4) Uani 1 1 d . . . . .
N3 N 0.11822(19) 0.76939(17) 0.77842(16) 0.0208(4) Uani 1 1 d . . . . .
N2 N 0.08843(18) 0.68825(17) 0.74143(15) 0.0197(4) Uani 1 1 d . . . . .
N14 N 0.0178(2) 0.43485(19) 0.74260(17) 0.0264(5) Uani 1 1 d . . . . .
N6 N 0.0581(2) 0.74075(18) 0.42357(17) 0.0287(5) Uani 1 1 d . . . . .
N7 N 0.0780(2) 0.78126(19) 0.33019(18) 0.0300(5) Uani 1 1 d . . . . .
C13 C 0.2524(2) 0.34335(18) 0.46926(18) 0.0166(4) Uani 1 1 d . . . . .
H13 H 0.314044 0.335553 0.506819 0.020 Uiso 1 1 calc R U . . .
N15 N 0.0374(2) 0.3890(2) 0.82629(17) 0.0283(5) Uani 1 1 d . . . . .
C7 C 0.2130(2) 0.6392(2) 0.32599(18) 0.0180(4) Uani 1 1 d . . . . .
H7 H 0.279704 0.583340 0.301901 0.022 Uiso 1 1 calc R U . . .
C19 C 0.2157(2) 0.44160(19) 0.73007(18) 0.0172(4) Uani 1 1 d . . . . .
H19 H 0.302407 0.455217 0.705982 0.021 Uiso 1 1 calc R U . . .
C1 C 0.2042(2) 0.77171(18) 0.61040(17) 0.0157(4) Uani 1 1 d . . . . .
H1 H 0.250924 0.792043 0.542069 0.019 Uiso 1 1 calc R U . . .
C20 C 0.2183(2) 0.3493(2) 0.90153(19) 0.0200(5) Uani 1 1 d . . . . .
O6 O 0.3798(3) 0.7945(3) 0.3726(2) 0.0847(12) Uani 1 1 d . . . . .
C2 C 0.2465(2) 0.91968(19) 0.71155(19) 0.0195(4) Uani 1 1 d . . . . .
C14 C 0.3128(2) 0.16620(19) 0.38009(19) 0.0194(4) Uani 1 1 d . . . . .
C6 C 0.1433(3) 1.0144(2) 0.7387(2) 0.0239(5) Uani 1 1 d . . . . .
C5 C 0.0782(3) 0.9991(2) 0.8553(2) 0.0296(6) Uani 1 1 d . . . . .
H5B H 0.006606 0.960996 0.867020 0.036 Uiso 1 1 d R U . . .
H5A H 0.035203 1.071872 0.888605 0.036 Uiso 1 1 d R U . . .
C23 C 0.2080(3) 0.3269(3) 1.0794(2) 0.0309(6) Uani 1 1 d . . . . .
C4 C 0.1820(3) 0.9410(2) 0.9011(2) 0.0324(6) Uani 1 1 d . . . . .
C8 C 0.2183(2) 0.7430(2) 0.15418(19) 0.0239(5) Uani 1 1 d . . . . .
C12 C 0.2876(3) 0.6438(3) 0.0926(2) 0.0314(6) Uani 1 1 d . . . . .
C3 C 0.2965(3) 0.9046(2) 0.8077(2) 0.0280(6) Uani 1 1 d . . . . .
C24 C 0.1579(3) 0.4037(3) 1.0046(2) 0.0298(6) Uani 1 1 d . . . . .
C18 C 0.3045(3) 0.1275(2) 0.2778(2) 0.0303(6) Uani 1 1 d . . . . .
C22 C 0.2023(3) 0.2165(3) 1.0416(2) 0.0344(7) Uani 1 1 d . . . . .
C9 C 0.3154(3) 0.8248(3) 0.1292(2) 0.0323(6) Uani 1 1 d . . . . .
O8A O 0.5343(10) 0.9001(9) 0.4107(13) 0.080(5) Uani 0.308(8) 1 d . . P A 1
O7A O 0.5706(10) 0.8193(15) 0.2578(8) 0.096(6) Uani 0.308(8) 1 d . . P A 1
O9A O 0.5439(13) 0.7159(10) 0.4101(15) 0.091(6) Uani 0.308(8) 1 d . . P A 1
O8B O 0.4795(4) 0.8531(4) 0.4778(3) 0.0537(15) Uani 0.692(8) 1 d . . P A 2
O7B O 0.5311(4) 0.8994(4) 0.3013(4) 0.0676(19) Uani 0.692(8) 1 d . . P A 2
O9B O 0.6074(6) 0.7356(4) 0.3545(4) 0.0671(19) Uani 0.692(8) 1 d . . P A 2
C21 C 0.2056(4) 0.2321(2) 0.9262(3) 0.0472(9) Uani 1 1 d . . . . .
H21A H 0.279219 0.187377 0.881607 0.057 Uiso 1 1 calc R U . . .
H21B H 0.125976 0.213238 0.915411 0.057 Uiso 1 1 calc R U . . .
C15 C 0.2540(4) 0.0837(3) 0.4599(3) 0.0502(10) Uani 1 1 d . . . . .
C11 C 0.4285(3) 0.6548(3) 0.0691(3) 0.0416(8) Uani 1 1 d . . . . .
C17 C 0.1827(4) 0.0744(3) 0.3053(4) 0.0611(13) Uani 1 1 d . . . . .
H17A H 0.112802 0.123001 0.288796 0.073 Uiso 1 1 calc R U . . .
H17B H 0.195899 0.008273 0.266133 0.073 Uiso 1 1 calc R U . . .
C10 C 0.4323(3) 0.7739(3) 0.0477(3) 0.0487(9) Uani 1 1 d . . . . .
H10A H 0.427106 0.793787 -0.023492 0.058 Uiso 1 1 calc R U . . .
H10B H 0.511817 0.796192 0.055622 0.058 Uiso 1 1 calc R U . . .
C16 C 0.1508(5) 0.0494(5) 0.4201(6) 0.094(2) Uani 1 1 d . . . . .
H12A H 0.270(3) 0.577(3) 0.125(3) 0.033(8) Uiso 1 1 d . . . . .
H20 H 0.302(3) 0.365(2) 0.875(2) 0.020(7) Uiso 1 1 d . . . . .
H6A H 0.182(3) 1.074(2) 0.725(2) 0.022(7) Uiso 1 1 d . . . . .
H14 H 0.399(3) 0.179(3) 0.378(2) 0.030(8) Uiso 1 1 d . . . . .
H23A H 0.296(3) 0.336(3) 1.075(3) 0.036(9) Uiso 1 1 d . . . . .
H6B H 0.092(3) 1.016(2) 0.693(2) 0.021(7) Uiso 1 1 d . . . . .
H8 H 0.145(3) 0.772(2) 0.138(2) 0.028(8) Uiso 1 1 d . . . . .
H22A H 0.276(3) 0.167(3) 1.050(3) 0.040(9) Uiso 1 1 d . . . . .
H24A H 0.181(3) 0.467(3) 1.000(3) 0.049(11) Uiso 1 1 d . . . . .
H11A H 0.458(4) 0.647(3) 0.127(3) 0.056(11) Uiso 1 1 d . . . . .
H1A H 0.402(3) 0.551(3) 0.456(3) 0.026(8) Uiso 1 1 d . . . . .
H24B H 0.062(3) 0.405(3) 1.021(3) 0.041(9) Uiso 1 1 d . . . . .
H2 H 0.313(3) 0.930(2) 0.649(2) 0.024(7) Uiso 1 1 d . . . . .
H1B H 0.395(3) 0.583(3) 0.541(3) 0.035(9) Uiso 1 1 d . . . . .
H9A H 0.277(3) 0.891(3) 0.108(3) 0.035(9) Uiso 1 1 d . . . . .
H23B H 0.162(4) 0.335(4) 1.146(3) 0.069(13) Uiso 1 1 d . . . . .
H15A H 0.317(4) 0.026(4) 0.462(3) 0.061(12) Uiso 1 1 d . . . . .
H9B H 0.342(3) 0.836(3) 0.185(3) 0.046(10) Uiso 1 1 d . . . . .
H11B H 0.486(4) 0.614(3) 0.013(3) 0.057(11) Uiso 1 1 d . . . . .
H4A H 0.148(3) 0.881(3) 0.946(2) 0.028(8) Uiso 1 1 d . . . . .
H12B H 0.263(3) 0.648(2) 0.029(2) 0.025(8) Uiso 1 1 d . . . . .
H3A H 0.331(3) 0.831(3) 0.814(2) 0.027(8) Uiso 1 1 d . . . . .
H4B H 0.204(3) 0.988(3) 0.947(3) 0.040(9) Uiso 1 1 d . . . . .
H15B H 0.222(4) 0.106(3) 0.526(3) 0.053(11) Uiso 1 1 d . . . . .
H22B H 0.130(4) 0.192(4) 1.078(4) 0.073(14) Uiso 1 1 d . . . . .
H16A H 0.062(9) 0.061(7) 0.449(7) 0.20(4) Uiso 1 1 d . . . . .
H16B H 0.163(5) -0.014(5) 0.430(4) 0.080(17) Uiso 1 1 d . . . . .
H3B H 0.362(3) 0.954(3) 0.793(3) 0.046(10) Uiso 1 1 d . . . . .
H18A H 0.310(3) 0.183(3) 0.229(3) 0.035(9) Uiso 1 1 d . . . . .
H18B H 0.365(3) 0.081(3) 0.258(3) 0.042(10) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N13 2.0005(19) . ?
Cu1 N5 2.0152(19) . ?
Cu1 N1 2.0197(19) . ?
Cu1 N9 2.0246(18) . ?
Cu1 O1 2.3499(16) . ?
Cl1 O4 1.4309(19) . ?
Cl1 O3 1.431(2) . ?
Cl1 O5 1.452(2) . ?
Cl1 O2 1.457(2) . ?
Cl2 O8A 1.354(8) . ?
Cl2 O7B 1.381(4) . ?
Cl2 O9A 1.401(10) . ?
Cl2 O6 1.403(2) . ?
Cl2 O9B 1.409(4) . ?
Cl2 O8B 1.478(4) . ?
Cl2 O7A 1.495(10) . ?
O1 H1A 0.77(3) . ?
O1 H1B 0.77(4) . ?
N12 C13 1.328(3) . ?
N12 N11 1.344(2) . ?
N12 C14 1.489(3) . ?
N5 C7 1.321(3) . ?
N5 N6 1.359(3) . ?
N9 C13 1.322(3) . ?
N9 N10 1.364(2) . ?
N13 C19 1.318(3) . ?
N13 N14 1.363(3) . ?
N11 N10 1.296(3) . ?
N1 C1 1.320(3) . ?
N1 N2 1.367(3) . ?
N8 C7 1.327(3) . ?
N8 N7 1.355(3) . ?
N8 C8 1.486(3) . ?
N4 C1 1.332(3) . ?
N4 N3 1.358(3) . ?
N4 C2 1.479(3) . ?
N16 C19 1.320(3) . ?
N16 N15 1.352(3) . ?
N16 C20 1.470(3) . ?
N3 N2 1.287(3) . ?
N14 N15 1.294(3) . ?
N6 N7 1.293(3) . ?
C13 H13 0.9500 . ?
C7 H7 0.9500 . ?
C19 H19 0.9500 . ?
C1 H1 0.9500 . ?
C20 C21 1.512(4) . ?
C20 C24 1.518(4) . ?
C20 H20 0.93(3) . ?
C2 C6 1.525(3) . ?
C2 C3 1.539(4) . ?
C2 H2 0.95(3) . ?
C14 C15 1.511(4) . ?
C14 C18 1.521(4) . ?
C14 H14 0.98(3) . ?
C6 C5 1.532(4) . ?
C6 H6A 0.89(3) . ?
C6 H6B 0.95(3) . ?
C5 C4 1.537(4) . ?
C5 H5B 0.9461 . ?
C5 H5A 1.0443 . ?
C23 C24 1.522(4) . ?
C23 C22 1.530(5) . ?
C23 H23A 0.98(3) . ?
C23 H23B 0.90(4) . ?
C4 C3 1.543(4) . ?
C4 H4A 0.98(3) . ?
C4 H4B 0.98(3) . ?
C8 C9 1.536(4) . ?
C8 C12 1.536(4) . ?
C8 H8 0.92(3) . ?
C12 C11 1.514(4) . ?
C12 H12A 0.95(3) . ?
C12 H12B 0.97(3) . ?
C3 H3A 0.97(3) . ?
C3 H3B 0.99(4) . ?
C24 H24A 0.86(4) . ?
C24 H24B 1.02(3) . ?
C18 C17 1.517(5) . ?
C18 H18A 0.92(4) . ?
C18 H18B 0.82(4) . ?
C22 C21 1.543(4) . ?
C22 H22A 0.99(3) . ?
C22 H22B 0.89(5) . ?
C9 C10 1.527(5) . ?
C9 H9A 0.95(3) . ?
C9 H9B 0.91(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C15 C16 1.510(8) . ?
C15 H15A 0.94(4) . ?
C15 H15B 0.90(4) . ?
C11 C10 1.518(5) . ?
C11 H11A 0.93(4) . ?
C11 H11B 0.97(4) . ?
C17 C16 1.501(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C16 H16A 0.94(9) . ?
C16 H16B 0.81(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N13 Cu1 N5 176.85(7) . . ?
N13 Cu1 N1 88.46(8) . . ?
N5 Cu1 N1 92.76(8) . . ?
N13 Cu1 N9 88.25(8) . . ?
N5 Cu1 N9 90.94(8) . . ?
N1 Cu1 N9 171.39(7) . . ?
N13 Cu1 O1 91.08(7) . . ?
N5 Cu1 O1 91.92(7) . . ?
N1 Cu1 O1 84.94(7) . . ?
N9 Cu1 O1 87.17(7) . . ?
O4 Cl1 O3 111.03(14) . . ?
O4 Cl1 O5 110.31(13) . . ?
O3 Cl1 O5 110.05(13) . . ?
O4 Cl1 O2 108.86(13) . . ?
O3 Cl1 O2 108.55(13) . . ?
O5 Cl1 O2 107.97(12) . . ?
O8A Cl2 O9A 114.6(8) . . ?
O8A Cl2 O6 127.8(5) . . ?
O7B Cl2 O6 105.8(2) . . ?
O9A Cl2 O6 98.5(4) . . ?
O7B Cl2 O9B 110.0(3) . . ?
O6 Cl2 O9B 122.7(3) . . ?
O7B Cl2 O8B 109.0(3) . . ?
O6 Cl2 O8B 101.9(2) . . ?
O9B Cl2 O8B 106.6(2) . . ?
O8A Cl2 O7A 105.1(9) . . ?
O9A Cl2 O7A 106.5(10) . . ?
O6 Cl2 O7A 102.5(5) . . ?
Cu1 O1 H1A 118(2) . . ?
Cu1 O1 H1B 120(2) . . ?
H1A O1 H1B 104(3) . . ?
C13 N12 N11 108.87(17) . . ?
C13 N12 C14 127.76(18) . . ?
N11 N12 C14 123.34(18) . . ?
C7 N5 N6 106.73(18) . . ?
C7 N5 Cu1 130.61(16) . . ?
N6 N5 Cu1 122.60(15) . . ?
C13 N9 N10 106.42(18) . . ?
C13 N9 Cu1 126.88(14) . . ?
N10 N9 Cu1 126.69(14) . . ?
C19 N13 N14 106.53(19) . . ?
C19 N13 Cu1 128.95(16) . . ?
N14 N13 Cu1 123.93(14) . . ?
N10 N11 N12 106.96(17) . . ?
C1 N1 N2 106.53(18) . . ?
C1 N1 Cu1 130.81(15) . . ?
N2 N1 Cu1 121.65(15) . . ?
C7 N8 N7 108.14(19) . . ?
C7 N8 C8 132.0(2) . . ?
N7 N8 C8 119.8(2) . . ?
N11 N10 N9 109.62(17) . . ?
C1 N4 N3 108.21(19) . . ?
C1 N4 C2 130.0(2) . . ?
N3 N4 C2 121.70(19) . . ?
C19 N16 N15 108.65(18) . . ?
C19 N16 C20 129.23(19) . . ?
N15 N16 C20 122.1(2) . . ?
N2 N3 N4 107.08(18) . . ?
N3 N2 N1 109.83(19) . . ?
N15 N14 N13 109.51(18) . . ?
N7 N6 N5 109.5(2) . . ?
N6 N7 N8 107.2(2) . . ?
N9 C13 N12 108.12(18) . . ?
N9 C13 H13 125.9 . . ?
N12 C13 H13 125.9 . . ?
N14 N15 N16 106.82(19) . . ?
N5 C7 N8 108.4(2) . . ?
N5 C7 H7 125.8 . . ?
N8 C7 H7 125.8 . . ?
N13 C19 N16 108.48(19) . . ?
N13 C19 H19 125.8 . . ?
N16 C19 H19 125.8 . . ?
N1 C1 N4 108.3(2) . . ?
N1 C1 H1 125.8 . . ?
N4 C1 H1 125.8 . . ?
N16 C20 C21 113.1(2) . . ?
N16 C20 C24 113.7(2) . . ?
C21 C20 C24 104.9(2) . . ?
N16 C20 H20 102.2(17) . . ?
C21 C20 H20 114.0(18) . . ?
C24 C20 H20 109.0(17) . . ?
N4 C2 C6 110.86(19) . . ?
N4 C2 C3 110.4(2) . . ?
C6 C2 C3 103.4(2) . . ?
N4 C2 H2 106.3(18) . . ?
C6 C2 H2 114.2(18) . . ?
C3 C2 H2 111.8(17) . . ?
N12 C14 C15 110.0(2) . . ?
N12 C14 C18 111.59(19) . . ?
C15 C14 C18 104.1(3) . . ?
N12 C14 H14 102.9(18) . . ?
C15 C14 H14 115.5(18) . . ?
C18 C14 H14 113.0(18) . . ?
C2 C6 C5 104.7(2) . . ?
C2 C6 H6A 107.8(18) . . ?
C5 C6 H6A 111.6(19) . . ?
C2 C6 H6B 108.3(18) . . ?
C5 C6 H6B 117.6(18) . . ?
H6A C6 H6B 106(3) . . ?
C6 C5 C4 105.8(2) . . ?
C6 C5 H5B 111.3 . . ?
C4 C5 H5B 112.8 . . ?
C6 C5 H5A 110.8 . . ?
C4 C5 H5A 115.1 . . ?
H5B C5 H5A 101.2 . . ?
C24 C23 C22 103.9(2) . . ?
C24 C23 H23A 111(2) . . ?
C22 C23 H23A 110.0(19) . . ?
C24 C23 H23B 113(3) . . ?
C22 C23 H23B 112(3) . . ?
H23A C23 H23B 107(3) . . ?
C5 C4 C3 106.3(2) . . ?
C5 C4 H4A 109.8(17) . . ?
C3 C4 H4A 112.4(18) . . ?
C5 C4 H4B 111(2) . . ?
C3 C4 H4B 113(2) . . ?
H4A C4 H4B 105(3) . . ?
N8 C8 C9 111.1(2) . . ?
N8 C8 C12 111.5(2) . . ?
C9 C8 C12 105.7(2) . . ?
N8 C8 H8 104.9(19) . . ?
C9 C8 H8 110(2) . . ?
C12 C8 H8 114.3(19) . . ?
C11 C12 C8 105.1(3) . . ?
C11 C12 H12A 110.2(19) . . ?
C8 C12 H12A 117(2) . . ?
C11 C12 H12B 110.0(18) . . ?
C8 C12 H12B 106.8(18) . . ?
H12A C12 H12B 107(3) . . ?
C2 C3 C4 106.0(2) . . ?
C2 C3 H3A 109.8(17) . . ?
C4 C3 H3A 113.0(18) . . ?
C2 C3 H3B 103(2) . . ?
C4 C3 H3B 111(2) . . ?
H3A C3 H3B 113(3) . . ?
C20 C24 C23 101.9(2) . . ?
C20 C24 H24A 109(3) . . ?
C23 C24 H24A 115(2) . . ?
C20 C24 H24B 107.7(19) . . ?
C23 C24 H24B 110(2) . . ?
H24A C24 H24B 112(3) . . ?
C17 C18 C14 105.4(3) . . ?
C17 C18 H18A 116(2) . . ?
C14 C18 H18A 111(2) . . ?
C17 C18 H18B 108(3) . . ?
C14 C18 H18B 107(2) . . ?
H18A C18 H18B 110(3) . . ?
C23 C22 C21 106.2(2) . . ?
C23 C22 H22A 110(2) . . ?
C21 C22 H22A 111(2) . . ?
C23 C22 H22B 110(3) . . ?
C21 C22 H22B 110(3) . . ?
H22A C22 H22B 110(4) . . ?
C10 C9 C8 105.7(3) . . ?
C10 C9 H9A 115(2) . . ?
C8 C9 H9A 109.6(19) . . ?
C10 C9 H9B 106(2) . . ?
C8 C9 H9B 112(2) . . ?
H9A C9 H9B 108(3) . . ?
C20 C21 C22 104.9(2) . . ?
C20 C21 H21A 110.8 . . ?
C22 C21 H21A 110.8 . . ?
C20 C21 H21B 110.8 . . ?
C22 C21 H21B 110.8 . . ?
H21A C21 H21B 108.8 . . ?
C16 C15 C14 104.1(4) . . ?
C16 C15 H15A 111(3) . . ?
C14 C15 H15A 109(3) . . ?
C16 C15 H15B 111(2) . . ?
C14 C15 H15B 116(3) . . ?
H15A C15 H15B 105(3) . . ?
C12 C11 C10 102.6(3) . . ?
C12 C11 H11A 114(2) . . ?
C10 C11 H11A 100(3) . . ?
C12 C11 H11B 117(2) . . ?
C10 C11 H11B 112(2) . . ?
H11A C11 H11B 110(3) . . ?
C16 C17 C18 105.9(3) . . ?
C16 C17 H17A 110.6 . . ?
C18 C17 H17A 110.6 . . ?
C16 C17 H17B 110.6 . . ?
C18 C17 H17B 110.6 . . ?
H17A C17 H17B 108.7 . . ?
C11 C10 C9 104.3(3) . . ?
C11 C10 H10A 110.9 . . ?
C9 C10 H10A 110.9 . . ?
C11 C10 H10B 110.9 . . ?
C9 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
C17 C16 C15 108.3(3) . . ?
C17 C16 H16A 109(5) . . ?
C15 C16 H16A 129(5) . . ?
C17 C16 H16B 110(4) . . ?
C15 C16 H16B 99(4) . . ?
H16A C16 H16B 101(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 N12 N11 N10 0.2(2) . . . . ?
C14 N12 N11 N10 178.4(2) . . . . ?
N12 N11 N10 N9 -0.2(2) . . . . ?
C13 N9 N10 N11 0.1(2) . . . . ?
Cu1 N9 N10 N11 178.79(15) . . . . ?
C1 N4 N3 N2 0.0(2) . . . . ?
C2 N4 N3 N2 -177.92(19) . . . . ?
N4 N3 N2 N1 -0.1(2) . . . . ?
C1 N1 N2 N3 0.2(2) . . . . ?
Cu1 N1 N2 N3 169.91(15) . . . . ?
C19 N13 N14 N15 0.2(3) . . . . ?
Cu1 N13 N14 N15 -171.69(17) . . . . ?
C7 N5 N6 N7 -0.4(3) . . . . ?
Cu1 N5 N6 N7 -177.85(17) . . . . ?
N5 N6 N7 N8 0.4(3) . . . . ?
C7 N8 N7 N6 -0.2(3) . . . . ?
C8 N8 N7 N6 178.5(2) . . . . ?
N10 N9 C13 N12 0.1(2) . . . . ?
Cu1 N9 C13 N12 -178.64(14) . . . . ?
N11 N12 C13 N9 -0.2(2) . . . . ?
C14 N12 C13 N9 -178.3(2) . . . . ?
N13 N14 N15 N16 -0.6(3) . . . . ?
C19 N16 N15 N14 0.8(3) . . . . ?
C20 N16 N15 N14 178.5(2) . . . . ?
N6 N5 C7 N8 0.3(3) . . . . ?
Cu1 N5 C7 N8 177.45(15) . . . . ?
N7 N8 C7 N5 -0.1(3) . . . . ?
C8 N8 C7 N5 -178.6(2) . . . . ?
N14 N13 C19 N16 0.3(3) . . . . ?
Cu1 N13 C19 N16 171.65(15) . . . . ?
N15 N16 C19 N13 -0.7(3) . . . . ?
C20 N16 C19 N13 -178.2(2) . . . . ?
N2 N1 C1 N4 -0.2(2) . . . . ?
Cu1 N1 C1 N4 -168.62(14) . . . . ?
N3 N4 C1 N1 0.2(2) . . . . ?
C2 N4 C1 N1 177.8(2) . . . . ?
C19 N16 C20 C21 -124.1(3) . . . . ?
N15 N16 C20 C21 58.7(3) . . . . ?
C19 N16 C20 C24 116.3(3) . . . . ?
N15 N16 C20 C24 -60.9(3) . . . . ?
C1 N4 C2 C6 109.7(3) . . . . ?
N3 N4 C2 C6 -73.0(3) . . . . ?
C1 N4 C2 C3 -136.4(2) . . . . ?
N3 N4 C2 C3 41.0(3) . . . . ?
C13 N12 C14 C15 85.8(3) . . . . ?
N11 N12 C14 C15 -92.0(3) . . . . ?
C13 N12 C14 C18 -159.1(2) . . . . ?
N11 N12 C14 C18 23.1(3) . . . . ?
N4 C2 C6 C5 80.6(2) . . . . ?
C3 C2 C6 C5 -37.7(3) . . . . ?
C2 C6 C5 C4 30.3(3) . . . . ?
C6 C5 C4 C3 -10.8(3) . . . . ?
C7 N8 C8 C9 -96.6(3) . . . . ?
N7 N8 C8 C9 85.0(3) . . . . ?
C7 N8 C8 C12 20.9(3) . . . . ?
N7 N8 C8 C12 -157.4(2) . . . . ?
N8 C8 C12 C11 -100.4(3) . . . . ?
C9 C8 C12 C11 20.4(3) . . . . ?
N4 C2 C3 C4 -87.7(2) . . . . ?
C6 C2 C3 C4 30.9(3) . . . . ?
C5 C4 C3 C2 -12.4(3) . . . . ?
N16 C20 C24 C23 165.9(2) . . . . ?
C21 C20 C24 C23 41.8(3) . . . . ?
C22 C23 C24 C20 -39.7(3) . . . . ?
N12 C14 C18 C17 -85.2(3) . . . . ?
C15 C14 C18 C17 33.3(3) . . . . ?
C24 C23 C22 C21 23.4(3) . . . . ?
N8 C8 C9 C10 125.7(3) . . . . ?
C12 C8 C9 C10 4.6(3) . . . . ?
N16 C20 C21 C22 -151.7(2) . . . . ?
C24 C20 C21 C22 -27.2(3) . . . . ?
C23 C22 C21 C20 2.2(3) . . . . ?
N12 C14 C15 C16 85.7(3) . . . . ?
C18 C14 C15 C16 -33.9(3) . . . . ?
C8 C12 C11 C10 -37.6(3) . . . . ?
C14 C18 C17 C16 -19.5(4) . . . . ?
C12 C11 C10 C9 40.4(3) . . . . ?
C8 C9 C10 C11 -27.8(3) . . . . ?
C18 C17 C16 C15 -1.8(5) . . . . ?
C14 C15 C16 C17 22.3(5) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.681
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.110

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px179
_database_code_depnum_ccdc_archive 'CCDC 2061072'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-05-08
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'hexakis(1-cyclopropyl)tetrazole copper(II) perchlorate'
_chemical_name_common            
'hexakis(1-cyclopropyl)tetrazole copper(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H36 Cu N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Cu N24 O8'
_chemical_formula_weight         923.21

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.7417(15)
_cell_length_b                   10.7417(15)
_cell_length_c                   29.826(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2980.4(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    1599
_cell_measurement_theta_min      2.2780
_cell_measurement_theta_max      27.3040

_exptl_crystal_description       hexagon
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.051
_exptl_absorpt_coefficient_mu    0.761
_shelx_estimated_absorpt_T_min   0.722
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             1425
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      115(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            7345
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.1733
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.048
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1363
_reflns_number_gt                1124
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1363
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0953
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0625424000
_diffrn_orient_matrix_UB_12      -0.0028348000
_diffrn_orient_matrix_UB_13      -0.0097772000
_diffrn_orient_matrix_UB_21      -0.0379852000
_diffrn_orient_matrix_UB_22      -0.0712740000
_diffrn_orient_matrix_UB_23      -0.0112092000
_diffrn_orient_matrix_UB_31      -0.0164940000
_diffrn_orient_matrix_UB_32      -0.0006169000
_diffrn_orient_matrix_UB_33      -0.0370889000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -39.00   1.00   25.00    --  -20.37-178.00 120.00   26
  2  ω     23.00  50.00   1.00   25.00    --  -20.37  57.00-150.00   27
  3  ω    -49.00  40.00   1.00   25.00    --   21.39 -57.00 -60.00   89
  4  ω     -9.00  36.00   1.00   25.00    --   21.39  77.00  60.00   45
  5  ω    -10.00  26.00   1.00   25.00    --   21.39  77.00 -60.00   36
  6  ω     -1.00  92.00   1.00   25.00    --   21.39  37.00-150.00   93
  7  ω      4.00  92.00   1.00   25.00    --   21.39  57.00  90.00   88
  8  ω     33.00  64.00   1.00   25.00    --   21.39 -99.00-180.00   31
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.000000 0.000000 0.500000 0.0183(2) Uani 1 6 d S T P . .
N1 N 0.1844(2) 0.1182(2) 0.54115(7) 0.0267(5) Uani 1 1 d . . . . .
N2 N 0.2233(2) 0.0521(2) 0.57272(8) 0.0341(6) Uani 1 1 d . . . . .
N3 N 0.3287(2) 0.1470(2) 0.59662(8) 0.0362(6) Uani 1 1 d . . . . .
N4 N 0.3586(2) 0.2772(2) 0.58074(7) 0.0274(5) Uani 1 1 d . . . . .
C1 C 0.2707(3) 0.2575(2) 0.54717(9) 0.0274(6) Uani 1 1 d . . . . .
H1 H 0.269574 0.331534 0.530072 0.033 Uiso 1 1 calc R U . . .
C2 C 0.4823(3) 0.4087(3) 0.59670(9) 0.0305(6) Uani 1 1 d . . . . .
H2 H 0.570996 0.448015 0.577859 0.037 Uiso 1 1 calc R U . . .
C3 C 0.5049(3) 0.4289(3) 0.64600(10) 0.0353(7) Uani 1 1 d . . . . .
H3A H 0.605038 0.477844 0.657212 0.042 Uiso 1 1 calc R U . . .
H3B H 0.433888 0.352192 0.665786 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4567(3) 0.5165(3) 0.62013(9) 0.0353(7) Uani 1 1 d . . . . .
H4A H 0.355907 0.493892 0.623936 0.042 Uiso 1 1 calc R U . . .
H4B H 0.527082 0.619563 0.615361 0.042 Uiso 1 1 calc R U . . .
Cl1 Cl 0.666667 0.333333 0.49056(4) 0.0243(3) Uani 1 3 d S T P . .
O1 O 0.666667 0.333333 0.44273(12) 0.0516(10) Uani 1 3 d S T P . .
O2 O 0.70482(19) 0.47336(18) 0.50722(7) 0.0408(5) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.128(2) . ?
Cu1 N1 2.128(2) 11_556 ?
Cu1 N1 2.128(2) 2 ?
Cu1 N1 2.128(2) 10_556 ?
Cu1 N1 2.128(2) 12_556 ?
Cu1 N1 2.128(2) 3 ?
N1 C1 1.320(3) . ?
N1 N2 1.364(3) . ?
N2 N3 1.294(3) . ?
N3 N4 1.354(3) . ?
N4 C1 1.319(3) . ?
N4 C2 1.453(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.488(4) . ?
C2 C4 1.492(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.496(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
Cl1 O1 1.427(4) . ?
Cl1 O2 1.4355(17) 3_665 ?
Cl1 O2 1.4355(18) 2_655 ?
Cl1 O2 1.4356(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 89.95(8) . 11_556 ?
N1 Cu1 N1 90.05(8) . 2 ?
N1 Cu1 N1 180.00(9) 11_556 2 ?
N1 Cu1 N1 180.00(9) . 10_556 ?
N1 Cu1 N1 90.05(8) 11_556 10_556 ?
N1 Cu1 N1 89.95(8) 2 10_556 ?
N1 Cu1 N1 89.95(8) . 12_556 ?
N1 Cu1 N1 90.05(8) 11_556 12_556 ?
N1 Cu1 N1 89.95(8) 2 12_556 ?
N1 Cu1 N1 90.05(8) 10_556 12_556 ?
N1 Cu1 N1 90.05(8) . 3 ?
N1 Cu1 N1 89.95(8) 11_556 3 ?
N1 Cu1 N1 90.05(8) 2 3 ?
N1 Cu1 N1 89.95(8) 10_556 3 ?
N1 Cu1 N1 180.00(8) 12_556 3 ?
C1 N1 N2 105.8(2) . . ?
C1 N1 Cu1 132.14(17) . . ?
N2 N1 Cu1 121.56(15) . . ?
N3 N2 N1 110.19(19) . . ?
N2 N3 N4 106.4(2) . . ?
C1 N4 N3 108.6(2) . . ?
C1 N4 C2 129.7(2) . . ?
N3 N4 C2 121.2(2) . . ?
N4 C1 N1 109.0(2) . . ?
N4 C1 H1 125.5 . . ?
N1 C1 H1 125.5 . . ?
N4 C2 C3 117.9(2) . . ?
N4 C2 C4 118.3(2) . . ?
C3 C2 C4 60.26(18) . . ?
N4 C2 H2 116.2 . . ?
C3 C2 H2 116.2 . . ?
C4 C2 H2 116.2 . . ?
C2 C3 C4 59.98(17) . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3B 117.8 . . ?
C4 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C2 C4 C3 59.76(17) . . ?
C2 C4 H4A 117.8 . . ?
C3 C4 H4A 117.8 . . ?
C2 C4 H4B 117.8 . . ?
C3 C4 H4B 117.8 . . ?
H4A C4 H4B 114.9 . . ?
O1 Cl1 O2 110.24(9) . 3_665 ?
O1 Cl1 O2 110.24(9) . 2_655 ?
O2 Cl1 O2 108.69(9) 3_665 2_655 ?
O1 Cl1 O2 110.25(9) . . ?
O2 Cl1 O2 108.69(9) 3_665 . ?
O2 Cl1 O2 108.68(9) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.3(3) . . . . ?
Cu1 N1 N2 N3 -173.07(15) . . . . ?
N1 N2 N3 N4 0.5(3) . . . . ?
N2 N3 N4 C1 -0.6(3) . . . . ?
N2 N3 N4 C2 -173.2(2) . . . . ?
N3 N4 C1 N1 0.4(3) . . . . ?
C2 N4 C1 N1 172.2(2) . . . . ?
N2 N1 C1 N4 -0.1(3) . . . . ?
Cu1 N1 C1 N4 171.62(16) . . . . ?
C1 N4 C2 C3 140.7(3) . . . . ?
N3 N4 C2 C3 -48.5(3) . . . . ?
C1 N4 C2 C4 71.3(3) . . . . ?
N3 N4 C2 C4 -117.9(3) . . . . ?
N4 C2 C3 C4 -108.4(2) . . . . ?
N4 C2 C4 C3 107.8(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 O2 0.95 2.26 3.209(3) 172.8 10_666




_refine_diff_density_max         0.457
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.068

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px216
_database_code_depnum_ccdc_archive 'CCDC 2061077'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-05
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'hexakis(1-cyclopropyl-5H-tetrazolyl)zinc(II) diperchlorate'
_chemical_name_common            
'hexakis(1-cyclopropyl-5H-tetrazolyl)zinc(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C24 H36 N24 Zn, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 N24 O8 Zn'
_chemical_formula_weight         925.04

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.7815(5)
_cell_length_b                   10.7815(5)
_cell_length_c                   29.5910(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2978.8(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    107(2)
_cell_measurement_reflns_used    1294
_cell_measurement_theta_min      2.3220
_cell_measurement_theta_max      27.3560

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.174
_exptl_absorpt_coefficient_mu    0.830
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70278
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             1428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      107(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            6902
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_sigmaI/netI    0.1346
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.514
_diffrn_reflns_theta_max         26.355
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1362
_reflns_number_gt                1081
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1362
_refine_ls_number_parameters     114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0402825000
_diffrn_orient_matrix_UB_12      -0.0360724000
_diffrn_orient_matrix_UB_13      0.0194699000
_diffrn_orient_matrix_UB_21      -0.0510781000
_diffrn_orient_matrix_UB_22      -0.0560931000
_diffrn_orient_matrix_UB_23      -0.0138226000
_diffrn_orient_matrix_UB_31      0.0392678000
_diffrn_orient_matrix_UB_32      -0.0364179000
_diffrn_orient_matrix_UB_33      0.0019993000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     23.00 103.00   1.00   50.00    --   29.64-147.00 -60.00   80
  2  ω     19.00  99.00   1.00   50.00    --   29.64  57.00 150.00   80
  3  ω     69.00 112.00   1.00   50.00    --   29.64-178.00 150.00   43
  4  ω    -20.00  64.00   1.00   50.00    --   29.64 -99.00 -30.00   84
  5  ω    -26.00  92.00   1.00   50.00    --   29.64  19.00 120.00  118
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.000000 1.000000 0.500000 0.0140(2) Uani 1 6 d S T P . .
Cl1 Cl 0.666667 0.333333 0.49070(3) 0.0182(3) Uani 1 3 d S T P . .
O1 O 0.52603(18) 0.2907(2) 0.50736(6) 0.0320(5) Uani 1 1 d . . . . .
N4 N 0.7200(2) 0.6393(2) 0.58151(7) 0.0161(5) Uani 1 1 d . . . . .
N1 N 0.8785(2) 0.8138(2) 0.54200(7) 0.0160(4) Uani 1 1 d . . . . .
N3 N 0.8496(2) 0.6686(2) 0.59720(7) 0.0211(5) Uani 1 1 d . . . . .
O2 O 0.666667 0.333333 0.44285(11) 0.0418(9) Uani 1 3 d S T P . .
N2 N 0.9443(2) 0.7741(2) 0.57346(7) 0.0214(5) Uani 1 1 d . . . . .
C3 C 0.5678(3) 0.4929(3) 0.64670(9) 0.0240(6) Uani 1 1 d . . . . .
C1 C 0.7403(3) 0.7290(2) 0.54790(8) 0.0160(5) Uani 1 1 d . . . . .
C2 C 0.5891(3) 0.5164(3) 0.59718(8) 0.0185(5) Uani 1 1 d . . . . .
C4 C 0.4811(3) 0.5411(3) 0.62053(9) 0.0257(6) Uani 1 1 d . . . . .
H3A H 0.525(3) 0.397(3) 0.6561(8) 0.020(7) Uiso 1 1 d . . . . .
H3B H 0.645(3) 0.562(3) 0.6660(9) 0.024(7) Uiso 1 1 d . . . . .
H4A H 0.388(3) 0.476(3) 0.6129(8) 0.020(7) Uiso 1 1 d . . . . .
H2 H 0.563(3) 0.440(3) 0.5782(8) 0.018(7) Uiso 1 1 d . . . . .
H4B H 0.502(3) 0.640(3) 0.6231(9) 0.038(8) Uiso 1 1 d . . . . .
H1 H 0.665(3) 0.728(3) 0.5329(8) 0.015(6) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.1589(19) . ?
Zn1 N1 2.1589(19) 11_566 ?
Zn1 N1 2.1589(19) 2_765 ?
Zn1 N1 2.1589(19) 12_656 ?
Zn1 N1 2.1589(19) 3_675 ?
Zn1 N1 2.1589(19) 10_776 ?
Cl1 O2 1.416(3) . ?
Cl1 O1 1.4341(18) 2_655 ?
Cl1 O1 1.4341(18) 3_665 ?
Cl1 O1 1.4341(18) . ?
N4 C1 1.327(3) . ?
N4 N3 1.351(3) . ?
N4 C2 1.447(3) . ?
N1 C1 1.314(3) . ?
N1 N2 1.362(3) . ?
N3 N2 1.292(3) . ?
C3 C2 1.485(4) . ?
C3 C4 1.493(4) . ?
C3 H3A 0.94(3) . ?
C3 H3B 0.98(3) . ?
C1 H1 0.92(2) . ?
C2 C4 1.488(4) . ?
C2 H2 0.92(3) . ?
C4 H4A 0.92(3) . ?
C4 H4B 0.98(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N1 89.83(7) . 11_566 ?
N1 Zn1 N1 90.17(7) . 2_765 ?
N1 Zn1 N1 180.0 11_566 2_765 ?
N1 Zn1 N1 89.83(7) . 12_656 ?
N1 Zn1 N1 90.17(7) 11_566 12_656 ?
N1 Zn1 N1 89.83(7) 2_765 12_656 ?
N1 Zn1 N1 90.17(7) . 3_675 ?
N1 Zn1 N1 89.83(7) 11_566 3_675 ?
N1 Zn1 N1 90.17(7) 2_765 3_675 ?
N1 Zn1 N1 180.00(8) 12_656 3_675 ?
N1 Zn1 N1 180.00(11) . 10_776 ?
N1 Zn1 N1 90.17(7) 11_566 10_776 ?
N1 Zn1 N1 89.83(7) 2_765 10_776 ?
N1 Zn1 N1 90.17(7) 12_656 10_776 ?
N1 Zn1 N1 89.83(7) 3_675 10_776 ?
O2 Cl1 O1 110.11(8) . 2_655 ?
O2 Cl1 O1 110.11(8) . 3_665 ?
O1 Cl1 O1 108.82(9) 2_655 3_665 ?
O2 Cl1 O1 110.12(8) . . ?
O1 Cl1 O1 108.82(9) 2_655 . ?
O1 Cl1 O1 108.82(9) 3_665 . ?
C1 N4 N3 108.24(19) . . ?
C1 N4 C2 129.6(2) . . ?
N3 N4 C2 121.67(19) . . ?
C1 N1 N2 106.16(19) . . ?
C1 N1 Zn1 132.34(17) . . ?
N2 N1 Zn1 121.08(14) . . ?
N2 N3 N4 106.76(18) . . ?
N3 N2 N1 109.99(18) . . ?
C2 C3 C4 59.96(18) . . ?
C2 C3 H3A 115.5(15) . . ?
C4 C3 H3A 119.1(16) . . ?
C2 C3 H3B 116.5(15) . . ?
C4 C3 H3B 118.8(15) . . ?
H3A C3 H3B 115(2) . . ?
N1 C1 N4 108.8(2) . . ?
N1 C1 H1 129.2(16) . . ?
N4 C1 H1 121.9(16) . . ?
N4 C2 C3 118.0(2) . . ?
N4 C2 C4 118.5(2) . . ?
C3 C2 C4 60.30(18) . . ?
N4 C2 H2 110.2(16) . . ?
C3 C2 H2 119.9(16) . . ?
C4 C2 H2 122.2(16) . . ?
C2 C4 C3 59.75(18) . . ?
C2 C4 H4A 113.7(16) . . ?
C3 C4 H4A 119.8(16) . . ?
C2 C4 H4B 117.3(17) . . ?
C3 C4 H4B 119.9(17) . . ?
H4A C4 H4B 115(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 0.4(2) . . . . ?
C2 N4 N3 N2 173.2(2) . . . . ?
N4 N3 N2 N1 -0.6(2) . . . . ?
C1 N1 N2 N3 0.6(3) . . . . ?
Zn1 N1 N2 N3 174.02(15) . . . . ?
N2 N1 C1 N4 -0.3(3) . . . . ?
Zn1 N1 C1 N4 -172.68(15) . . . . ?
N3 N4 C1 N1 -0.1(3) . . . . ?
C2 N4 C1 N1 -172.1(2) . . . . ?
C1 N4 C2 C3 -139.8(3) . . . . ?
N3 N4 C2 C3 49.1(3) . . . . ?
C1 N4 C2 C4 -70.3(3) . . . . ?
N3 N4 C2 C4 118.6(3) . . . . ?
C4 C3 C2 N4 108.6(3) . . . . ?
N4 C2 C4 C3 -107.7(3) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.468
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.071

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px178
_database_code_depnum_ccdc_archive 'CCDC 2061081'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-05-08
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'hexakis(1-cyclopropyl-5H-tetrazolyl)copper(II) dichlorate'
_chemical_name_common            
'hexakis(1-cyclopropyl-5H-tetrazolyl)copper(II) dichlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H36 Cu N24, 2(Cl O3)'
_chemical_formula_sum            'C24 H36 Cl2 Cu N24 O6'
_chemical_formula_weight         891.21

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.9182(10)
_cell_length_b                   10.9182(10)
_cell_length_c                   28.166(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2907.8(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    127(2)
_cell_measurement_reflns_used    2269
_cell_measurement_theta_min      2.3000
_cell_measurement_theta_max      30.7420

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.774
_shelx_estimated_absorpt_T_min   0.816
_shelx_estimated_absorpt_T_max   0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82974
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_F_000             1377
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      127(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            7265
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.272
_diffrn_reflns_theta_max         26.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1328
_reflns_number_gt                1148
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²+1.1875P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1328
_refine_ls_number_parameters     111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0797
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0169621000
_diffrn_orient_matrix_UB_12      -0.0386090000
_diffrn_orient_matrix_UB_13      -0.0215741000
_diffrn_orient_matrix_UB_21      0.0572538000
_diffrn_orient_matrix_UB_22      -0.0122326000
_diffrn_orient_matrix_UB_23      0.0035118000
_diffrn_orient_matrix_UB_31      -0.0454715000
_diffrn_orient_matrix_UB_32      -0.0632897000
_diffrn_orient_matrix_UB_33      0.0124462000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00 -82.00   1.00   50.00    --  -28.86-178.00  30.00   26
  2  ω     45.00 100.00   1.00   50.00    --   29.64  57.00  60.00   55
  3  ω     43.00  74.00   1.00   50.00    --   29.64 -99.00-180.00   31
  4  ω     -4.00  41.00   1.00   50.00    --   29.64  82.00  51.00   45
  5  ω    -32.00  40.00   1.00   50.00    --   29.64 -77.00-150.00   72
  6  ω     -3.00  79.00   1.00   50.00    --   29.64  37.00-180.00   82
  7  ω    -38.00  53.00   1.00   50.00    --   29.64 -57.00 -90.00   91
  8  ω     44.00  95.00   1.00   50.00    --   29.64  57.00   0.00   51
  9  ω     87.00 112.00   1.00   50.00    --   29.64-178.00  30.00   25
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.000000 0.000000 0.500000 0.01588(16) Uani 1 6 d S T P . .
Cl1 Cl 0.666667 0.333333 0.48065(2) 0.0232(2) Uani 1 3 d S T P . .
O1 O 0.72579(16) 0.47772(14) 0.50025(5) 0.0366(4) Uani 1 1 d . . . . .
N4 N 0.18220(16) 0.12116(16) 0.54277(5) 0.0236(3) Uani 1 1 d . . . . .
N1 N 0.36097(17) 0.28257(16) 0.58042(5) 0.0248(3) Uani 1 1 d . . . . .
N2 N 0.33566(19) 0.15666(17) 0.59788(6) 0.0329(4) Uani 1 1 d . . . . .
N3 N 0.22738(18) 0.05991(17) 0.57516(6) 0.0306(4) Uani 1 1 d . . . . .
C1 C 0.2669(2) 0.2583(2) 0.54660(7) 0.0255(4) Uani 1 1 d . . . . .
C2 C 0.4847(2) 0.4139(2) 0.59421(7) 0.0279(4) Uani 1 1 d . . . . .
C3 C 0.5092(3) 0.4471(2) 0.64567(7) 0.0334(5) Uani 1 1 d . . . . .
C4 C 0.4622(3) 0.5271(2) 0.61475(8) 0.0342(5) Uani 1 1 d . . . . .
H2 H 0.560(3) 0.438(2) 0.5746(8) 0.037(6) Uiso 1 1 d . . . . .
H3A H 0.444(2) 0.380(2) 0.6652(7) 0.024(5) Uiso 1 1 d . . . . .
H1 H 0.267(2) 0.330(2) 0.5309(7) 0.023(5) Uiso 1 1 d . . . . .
H3B H 0.600(3) 0.487(2) 0.6555(7) 0.033(6) Uiso 1 1 d . . . . .
H4A H 0.371(3) 0.511(3) 0.6191(7) 0.038(6) Uiso 1 1 d . . . . .
H4B H 0.521(3) 0.615(3) 0.6072(8) 0.037(6) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.1275(16) 10_556 ?
Cu1 N4 2.1275(16) 12_556 ?
Cu1 N4 2.1275(16) 3 ?
Cu1 N4 2.1275(16) 2 ?
Cu1 N4 2.1275(16) 11_556 ?
Cu1 N4 2.1276(16) . ?
Cl1 O1 1.4796(14) 3_665 ?
Cl1 O1 1.4796(14) 2_655 ?
Cl1 O1 1.4796(14) . ?
N4 C1 1.313(2) . ?
N4 N3 1.361(2) . ?
N1 C1 1.327(3) . ?
N1 N2 1.352(2) . ?
N1 C2 1.447(3) . ?
N2 N3 1.294(2) . ?
C1 H1 0.90(2) . ?
C2 C3 1.486(3) . ?
C2 C4 1.493(3) . ?
C2 H2 0.91(2) . ?
C3 C4 1.495(3) . ?
C3 H3A 0.91(2) . ?
C3 H3B 0.91(2) . ?
C4 H4A 0.93(2) . ?
C4 H4B 0.87(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N4 91.10(5) 10_556 12_556 ?
N4 Cu1 N4 88.90(5) 10_556 3 ?
N4 Cu1 N4 180.00(6) 12_556 3 ?
N4 Cu1 N4 88.90(5) 10_556 2 ?
N4 Cu1 N4 88.90(5) 12_556 2 ?
N4 Cu1 N4 91.10(5) 3 2 ?
N4 Cu1 N4 91.10(5) 10_556 11_556 ?
N4 Cu1 N4 91.10(5) 12_556 11_556 ?
N4 Cu1 N4 88.90(5) 3 11_556 ?
N4 Cu1 N4 180.00(6) 2 11_556 ?
N4 Cu1 N4 180.00(9) 10_556 . ?
N4 Cu1 N4 88.90(5) 12_556 . ?
N4 Cu1 N4 91.10(5) 3 . ?
N4 Cu1 N4 91.10(5) 2 . ?
N4 Cu1 N4 88.90(5) 11_556 . ?
O1 Cl1 O1 106.92(6) 3_665 2_655 ?
O1 Cl1 O1 106.92(6) 3_665 . ?
O1 Cl1 O1 106.92(6) 2_655 . ?
C1 N4 N3 106.47(16) . . ?
C1 N4 Cu1 131.45(13) . . ?
N3 N4 Cu1 122.00(12) . . ?
C1 N1 N2 108.30(16) . . ?
C1 N1 C2 129.52(16) . . ?
N2 N1 C2 121.65(16) . . ?
N3 N2 N1 106.80(15) . . ?
N2 N3 N4 109.76(15) . . ?
N4 C1 N1 108.66(16) . . ?
N4 C1 H1 130.4(13) . . ?
N1 C1 H1 120.9(13) . . ?
N1 C2 C3 117.96(17) . . ?
N1 C2 C4 117.77(17) . . ?
C3 C2 C4 60.24(14) . . ?
N1 C2 H2 112.6(14) . . ?
C3 C2 H2 119.5(15) . . ?
C4 C2 H2 119.5(15) . . ?
C2 C3 C4 60.11(14) . . ?
C2 C3 H3A 115.1(13) . . ?
C4 C3 H3A 117.9(13) . . ?
C2 C3 H3B 115.8(14) . . ?
C4 C3 H3B 120.6(15) . . ?
H3A C3 H3B 115.5(19) . . ?
C2 C4 C3 59.64(14) . . ?
C2 C4 H4A 120.1(15) . . ?
C3 C4 H4A 117.7(15) . . ?
C2 C4 H4B 118.7(15) . . ?
C3 C4 H4B 120.3(16) . . ?
H4A C4 H4B 112(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.8(2) . . . . ?
C2 N1 N2 N3 -173.14(16) . . . . ?
N1 N2 N3 N4 0.4(2) . . . . ?
C1 N4 N3 N2 0.1(2) . . . . ?
Cu1 N4 N3 N2 -177.03(12) . . . . ?
N3 N4 C1 N1 -0.6(2) . . . . ?
Cu1 N4 C1 N1 176.15(11) . . . . ?
N2 N1 C1 N4 0.8(2) . . . . ?
C2 N1 C1 N4 172.39(17) . . . . ?
C1 N1 C2 C3 134.5(2) . . . . ?
N2 N1 C2 C3 -54.9(2) . . . . ?
C1 N1 C2 C4 65.3(3) . . . . ?
N2 N1 C2 C4 -124.10(19) . . . . ?
N1 C2 C3 C4 -107.7(2) . . . . ?
N1 C2 C4 C3 108.0(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.318
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.058

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px213
_database_code_depnum_ccdc_archive 'CCDC 2061078'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-02
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'dinitrato di(1-cyclopropyl-5H-tetrazolyl) copper(II)'
_chemical_name_common            
'dinitrato di(1-cyclopropyl-5H-tetrazolyl) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H24 Cu2 N20 O12'
_chemical_formula_sum            'C16 H24 Cu2 N20 O12'
_chemical_formula_weight         815.63

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   19.4982(5)
_cell_length_b                   15.0587(5)
_cell_length_c                   20.7916(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6104.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6205
_cell_measurement_theta_min      2.4670
_cell_measurement_theta_max      27.4590

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    1.486
_shelx_estimated_absorpt_T_min   0.669
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_F_000             3312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            56214
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_sigmaI/netI    0.1371
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.489
_diffrn_reflns_theta_max         32.346
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             18817
_reflns_number_gt                12571
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_max     0.776
_reflns_Friedel_fraction_full    0.934

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0338P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;

_refine_ls_abs_structure_Flack   0.505(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         18817
_refine_ls_number_parameters     902
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1121
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0060541000
_diffrn_orient_matrix_UB_12      0.0362963000
_diffrn_orient_matrix_UB_13      0.0209853000
_diffrn_orient_matrix_UB_21      0.0108908000
_diffrn_orient_matrix_UB_22      0.0298734000
_diffrn_orient_matrix_UB_23      -0.0243337000
_diffrn_orient_matrix_UB_31      -0.0341740000
_diffrn_orient_matrix_UB_32      0.0030689000
_diffrn_orient_matrix_UB_33      -0.0114526000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  52.00   1.00   50.00    --   29.64 -57.00-120.00   90
  2  ω    -19.00  71.00   1.00   50.00    --   29.64 -99.00 120.00   90
  3  ω      6.00  99.00   1.00   50.00    --   29.64  57.00  30.00   93
  4  ω     76.00 112.00   1.00   50.00    --   29.64-178.00 -30.00   36
  5  ω    -43.00  46.00   1.00   50.00    --   29.64 -37.00 120.00   89
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.67034(4) 0.60706(5) 0.38864(3) 0.01570(16) Uani 1 1 d . . . . .
Cu3 Cu 0.42908(4) 0.63628(5) 0.62798(3) 0.01650(16) Uani 1 1 d . . . . .
Cu4 Cu 0.17234(4) 0.61905(5) 0.61639(3) 0.01623(16) Uani 1 1 d . . . . .
Cu1 Cu 0.92428(4) 0.65987(5) 0.36433(4) 0.01652(16) Uani 1 1 d . . . . .
O22 O 0.2087(2) 0.5059(3) 0.6525(2) 0.0174(10) Uani 1 1 d . . . . .
O19 O 0.1314(2) 0.7327(3) 0.5855(2) 0.0182(9) Uani 1 1 d . . . . .
O13 O 0.3813(2) 0.7266(3) 0.5750(2) 0.0180(9) Uani 1 1 d . . . . .
O10 O 0.7077(2) 0.5025(3) 0.3412(2) 0.0185(10) Uani 1 1 d . . . . .
O1 O 0.8700(2) 0.7439(3) 0.4164(2) 0.0183(9) Uani 1 1 d . . . . .
O4 O 0.9903(2) 0.5906(3) 0.3127(2) 0.0228(10) Uani 1 1 d . . . . .
O16 O 0.4863(2) 0.5551(3) 0.6799(2) 0.0217(10) Uani 1 1 d . . . . .
O2 O 0.7884(2) 0.6552(3) 0.3857(2) 0.0233(10) Uani 1 1 d . . . . .
O14 O 0.2908(2) 0.6580(3) 0.6107(2) 0.0222(10) Uani 1 1 d . . . . .
O7 O 0.6176(2) 0.7008(3) 0.4329(2) 0.0217(10) Uani 1 1 d . . . . .
O20 O 0.0383(2) 0.8103(3) 0.5856(2) 0.0238(10) Uani 1 1 d . . . . .
O11 O 0.6694(3) 0.3711(3) 0.3171(2) 0.0298(12) Uani 1 1 d . . . . .
O15 O 0.2813(2) 0.7852(3) 0.5622(2) 0.0278(11) Uani 1 1 d . . . . .
N40 N 0.1601(3) 0.4472(4) 0.6522(3) 0.0200(12) Uani 1 1 d . . . . .
O18 O 0.3844(2) 0.4994(3) 0.6936(2) 0.0292(12) Uani 1 1 d . . . . .
N19 N 0.5529(3) 0.7026(4) 0.4181(2) 0.0200(12) Uani 1 1 d . . . . .
O24 O 0.1723(3) 0.3739(3) 0.6758(2) 0.0266(11) Uani 1 1 d . . . . .
O9 O 0.5222(2) 0.7736(3) 0.4292(2) 0.0275(11) Uani 1 1 d . . . . .
N29 N 0.3153(3) 0.7233(4) 0.5824(2) 0.0177(11) Uani 1 1 d . . . . .
O3 O 0.7636(2) 0.7826(4) 0.4296(2) 0.0304(12) Uani 1 1 d . . . . .
N5 N 0.9358(3) 0.5778(4) 0.4386(2) 0.0177(11) Uani 1 1 d . . . . .
O8 O 0.5259(2) 0.6381(3) 0.3942(3) 0.0336(12) Uani 1 1 d . . . . .
N1 N 0.9061(3) 0.7338(4) 0.2872(2) 0.0173(11) Uani 1 1 d . . . . .
N2 N 0.8455(3) 0.7775(4) 0.2772(2) 0.0202(12) Uani 1 1 d . . . . .
N9 N 0.8045(3) 0.7271(4) 0.4105(2) 0.0188(11) Uani 1 1 d . . . . .
N18 N 0.7072(3) 0.5213(4) 0.5733(2) 0.0198(12) Uani 1 1 d . . . . .
O23 O 0.1043(2) 0.4664(3) 0.6283(3) 0.0381(13) Uani 1 1 d . . . . .
O12 O 0.6043(2) 0.4643(3) 0.3681(3) 0.0377(13) Uani 1 1 d . . . . .
N35 N 0.1613(3) 0.6598(4) 0.7054(3) 0.0189(11) Uani 1 1 d . . . . .
N12 N 0.6080(3) 0.7281(4) 0.2926(2) 0.0207(12) Uani 1 1 d . . . . .
N24 N 0.4372(3) 0.4985(4) 0.4587(2) 0.0213(12) Uani 1 1 d . . . . .
O21 O 0.0333(2) 0.6684(3) 0.6043(2) 0.0303(12) Uani 1 1 d . . . . .
O5 O 0.9863(3) 0.4673(4) 0.2577(2) 0.0414(15) Uani 1 1 d . . . . .
N14 N 0.6653(3) 0.7093(4) 0.2065(2) 0.0201(11) Uani 1 1 d . . . . .
N38 N 0.1649(3) 0.6693(4) 0.8083(2) 0.0200(11) Uani 1 1 d . . . . .
N11 N 0.6570(3) 0.6658(4) 0.3044(2) 0.0176(11) Uani 1 1 d . . . . .
N15 N 0.6940(3) 0.5539(4) 0.4735(2) 0.0183(11) Uani 1 1 d . . . . .
O6 O 0.8936(3) 0.5228(3) 0.2983(2) 0.0299(12) Uani 1 1 d . . . . .
N34 N 0.1718(3) 0.5631(4) 0.4251(2) 0.0194(11) Uani 1 1 d . . . . .
O17 O 0.4738(3) 0.4289(4) 0.7292(2) 0.0367(13) Uani 1 1 d . . . . .
N28 N 0.4279(3) 0.7790(4) 0.7950(2) 0.0211(12) Uani 1 1 d . . . . .
N31 N 0.1810(3) 0.5770(4) 0.5275(3) 0.0213(12) Uani 1 1 d . . . . .
N8 N 0.9448(3) 0.5208(4) 0.5323(2) 0.0184(12) Uani 1 1 d . . . . .
N10 N 0.9557(3) 0.5247(4) 0.2881(3) 0.0259(13) Uani 1 1 d . . . . .
N39 N 0.0652(3) 0.7369(4) 0.5920(2) 0.0183(11) Uani 1 1 d . . . . .
N6 N 0.9589(3) 0.4929(4) 0.4335(3) 0.0284(14) Uani 1 1 d . . . . .
N25 N 0.4178(3) 0.7117(4) 0.7052(2) 0.0182(11) Uani 1 1 d . . . . .
N36 N 0.1168(3) 0.7237(4) 0.7257(3) 0.0241(12) Uani 1 1 d . . . . .
N4 N 0.9067(3) 0.7940(4) 0.1937(2) 0.0188(11) Uani 1 1 d . . . . .
N37 N 0.1191(3) 0.7296(4) 0.7876(3) 0.0270(13) Uani 1 1 d . . . . .
N26 N 0.3620(3) 0.7649(4) 0.7143(3) 0.0245(13) Uani 1 1 d . . . . .
N3 N 0.8454(3) 0.8132(4) 0.2207(3) 0.0214(12) Uani 1 1 d . . . . .
N13 N 0.6130(3) 0.7547(4) 0.2338(3) 0.0247(13) Uani 1 1 d . . . . .
N21 N 0.4346(3) 0.5559(4) 0.5527(2) 0.0173(11) Uani 1 1 d . . . . .
N20 N 0.6591(3) 0.4431(4) 0.3417(3) 0.0235(13) Uani 1 1 d . . . . .
N7 N 0.9643(4) 0.4580(4) 0.4903(3) 0.0323(15) Uani 1 1 d . . . . .
N27 N 0.3674(3) 0.8058(4) 0.7682(3) 0.0271(13) Uani 1 1 d . . . . .
N22 N 0.4598(3) 0.4717(4) 0.5559(3) 0.0311(15) Uani 1 1 d . . . . .
C9 C 0.6917(3) 0.6553(4) 0.2508(3) 0.0194(14) Uani 1 1 d . . . . .
H9 H 0.729216 0.615952 0.244706 0.023 Uiso 1 1 calc R U . . .
C25 C 0.1503(3) 0.6075(4) 0.4755(3) 0.0206(13) Uani 1 1 d . . . . .
H25 H 0.117661 0.654297 0.474703 0.025 Uiso 1 1 calc R U . . .
N30 N 0.4477(3) 0.4922(4) 0.7019(2) 0.0227(13) Uani 1 1 d . . . . .
C5 C 0.9277(3) 0.5937(4) 0.5004(3) 0.0186(13) Uani 1 1 d . . . . .
H5 H 0.912229 0.647817 0.518882 0.022 Uiso 1 1 calc R U . . .
C1 C 0.9420(3) 0.7449(4) 0.2341(3) 0.0192(13) Uani 1 1 d . . . . .
H1 H 0.986369 0.721212 0.226272 0.023 Uiso 1 1 calc R U . . .
N16 N 0.7384(3) 0.4852(5) 0.4790(3) 0.0386(17) Uani 1 1 d . . . . .
N32 N 0.2242(4) 0.5127(5) 0.5070(3) 0.046(2) Uani 1 1 d . . . . .
N23 N 0.4612(3) 0.4362(4) 0.4998(3) 0.0295(14) Uani 1 1 d . . . . .
C17 C 0.4217(3) 0.5713(5) 0.4913(3) 0.0210(14) Uani 1 1 d . . . . .
H17 H 0.404480 0.625080 0.473665 0.025 Uiso 1 1 calc R U . . .
C6 C 0.9475(3) 0.5053(4) 0.6009(3) 0.0205(14) Uani 1 1 d . . . . .
H6 H 0.994216 0.504256 0.620686 0.025 Uiso 1 1 calc R U . . .
C30 C 0.1797(4) 0.6543(5) 0.8759(3) 0.0252(15) Uani 1 1 d . . . . .
H30 H 0.190327 0.591560 0.888184 0.030 Uiso 1 1 calc R U . . .
C14 C 0.7047(3) 0.5135(5) 0.6422(3) 0.0255(15) Uani 1 1 d . . . . .
H14 H 0.720908 0.455337 0.659699 0.031 Uiso 1 1 calc R U . . .
N17 N 0.7460(3) 0.4644(5) 0.5388(3) 0.0373(17) Uani 1 1 d . . . . .
N33 N 0.2183(4) 0.5029(5) 0.4450(3) 0.0420(19) Uani 1 1 d . . . . .
C7 C 0.8959(3) 0.4453(5) 0.6302(3) 0.0270(15) Uani 1 1 d . . . . .
H7A H 0.910658 0.407468 0.666601 0.032 Uiso 1 1 calc R U . . .
H7B H 0.861277 0.418077 0.601447 0.032 Uiso 1 1 calc R U . . .
C8 C 0.8923(4) 0.5431(5) 0.6410(3) 0.0281(17) Uani 1 1 d . . . . .
H8A H 0.855323 0.576456 0.618963 0.034 Uiso 1 1 calc R U . . .
H8B H 0.904686 0.565851 0.684093 0.034 Uiso 1 1 calc R U . . .
C21 C 0.4573(3) 0.7214(4) 0.7558(3) 0.0197(14) Uani 1 1 d . . . . .
H21 H 0.499732 0.692095 0.763035 0.024 Uiso 1 1 calc R U . . .
C22 C 0.4521(3) 0.8119(5) 0.8565(3) 0.0283(16) Uani 1 1 d . . . . .
H22 H 0.486776 0.860856 0.855151 0.034 Uiso 1 1 calc R U . . .
C29 C 0.1902(3) 0.6269(5) 0.7575(3) 0.0204(14) Uani 1 1 d . . . . .
H29 H 0.223417 0.580780 0.758498 0.024 Uiso 1 1 calc R U . . .
C13 C 0.6756(3) 0.5753(5) 0.5325(3) 0.0215(14) Uani 1 1 d . . . . .
H13 H 0.644922 0.621664 0.543911 0.026 Uiso 1 1 calc R U . . .
C15 C 0.6486(3) 0.5557(5) 0.6790(3) 0.0295(17) Uani 1 1 d . . . . .
H15A H 0.630169 0.523223 0.716679 0.035 Uiso 1 1 calc R U . . .
H15B H 0.614298 0.590804 0.654827 0.035 Uiso 1 1 calc R U . . .
C16 C 0.7192(4) 0.5914(5) 0.6836(3) 0.0293(17) Uani 1 1 d . . . . .
H16A H 0.728926 0.648756 0.662166 0.035 Uiso 1 1 calc R U . . .
H16B H 0.744800 0.581165 0.724028 0.035 Uiso 1 1 calc R U . . .
C27 C 0.2091(4) 0.5813(5) 0.3100(3) 0.0282(16) Uani 1 1 d . . . . .
H27A H 0.257088 0.573450 0.324617 0.034 Uiso 1 1 calc R U . . .
H27B H 0.202990 0.623675 0.274074 0.034 Uiso 1 1 calc R U . . .
C23 C 0.4579(4) 0.7481(6) 0.9106(3) 0.0349(19) Uani 1 1 d . . . . .
H23A H 0.495767 0.756887 0.941730 0.042 Uiso 1 1 calc R U . . .
H23B H 0.445781 0.685361 0.902195 0.042 Uiso 1 1 calc R U . . .
C26 C 0.1545(3) 0.5757(5) 0.3585(3) 0.0261(14) Uani 1 1 d . . . . .
H26 H 0.114072 0.615081 0.350585 0.031 Uiso 1 1 calc R U . . .
C19 C 0.3946(4) 0.5382(5) 0.3479(3) 0.0288(17) Uani 1 1 d . . . . .
H19A H 0.411965 0.551880 0.304299 0.035 Uiso 1 1 calc R U . . .
H19B H 0.368514 0.586743 0.368717 0.035 Uiso 1 1 calc R U . . .
C18 C 0.4372(4) 0.4803(5) 0.3897(3) 0.0261(15) Uani 1 1 d . . . . .
H18 H 0.481120 0.457828 0.370813 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9467(4) 0.7546(6) 0.0830(3) 0.0344(19) Uani 1 1 d . . . . .
H3A H 0.982896 0.770208 0.051623 0.041 Uiso 1 1 calc R U . . .
H3B H 0.947747 0.692268 0.098202 0.041 Uiso 1 1 calc R U . . .
C31 C 0.2171(4) 0.7238(6) 0.9125(3) 0.0356(18) Uani 1 1 d . . . . .
H31A H 0.250443 0.704267 0.945470 0.043 Uiso 1 1 calc R U . . .
H31B H 0.229642 0.779074 0.889501 0.043 Uiso 1 1 calc R U . . .
C12 C 0.6321(4) 0.7108(5) 0.0913(3) 0.0320(18) Uani 1 1 d . . . . .
H12A H 0.586890 0.688163 0.105391 0.038 Uiso 1 1 calc R U . . .
H12B H 0.630764 0.752010 0.054242 0.038 Uiso 1 1 calc R U . . .
C4 C 0.8784(4) 0.7979(6) 0.0758(3) 0.0356(19) Uani 1 1 d . . . . .
H4A H 0.837203 0.762423 0.086409 0.043 Uiso 1 1 calc R U . . .
H4B H 0.872348 0.840353 0.039837 0.043 Uiso 1 1 calc R U . . .
C10 C 0.6853(3) 0.7262(5) 0.1415(3) 0.0279(16) Uani 1 1 d . . . . .
H10 H 0.717166 0.777319 0.134372 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6919(4) 0.6505(5) 0.0969(3) 0.0322(18) Uani 1 1 d . . . . .
H11A H 0.683736 0.590199 0.114261 0.039 Uiso 1 1 calc R U . . .
H11B H 0.727581 0.654005 0.063145 0.039 Uiso 1 1 calc R U . . .
C2 C 0.9246(3) 0.8248(4) 0.1300(3) 0.0250(14) Uani 1 1 d . . . . .
H2 H 0.947448 0.884072 0.126708 0.030 Uiso 1 1 calc R U . . .
C32 C 0.1437(4) 0.7070(6) 0.9247(3) 0.038(2) Uani 1 1 d . . . . .
H32A H 0.131132 0.677259 0.965486 0.046 Uiso 1 1 calc R U . . .
H32B H 0.110347 0.752007 0.909561 0.046 Uiso 1 1 calc R U . . .
C20 C 0.3732(4) 0.4454(5) 0.3616(4) 0.0331(17) Uani 1 1 d . . . . .
H20A H 0.333688 0.436264 0.390757 0.040 Uiso 1 1 calc R U . . .
H20B H 0.377121 0.401415 0.326366 0.040 Uiso 1 1 calc R U . . .
C28 C 0.1623(5) 0.5022(6) 0.3129(3) 0.041(2) Uani 1 1 d . . . . .
H28A H 0.127364 0.495848 0.278643 0.049 Uiso 1 1 calc R U . . .
H28B H 0.181449 0.445634 0.329176 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4014(4) 0.8151(6) 0.9099(3) 0.039(2) Uani 1 1 d . . . . .
H24A H 0.354359 0.793680 0.901036 0.047 Uiso 1 1 calc R U . . .
H24B H 0.404353 0.865219 0.940578 0.047 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu2 O7 1.975(4) . ?
Cu2 N11 1.980(5) . ?
Cu2 N15 1.991(5) . ?
Cu2 O10 1.996(4) . ?
Cu2 O2 2.414(4) . ?
Cu3 O16 1.975(4) . ?
Cu3 N25 1.979(5) . ?
Cu3 N21 1.981(5) . ?
Cu3 O13 1.983(4) . ?
Cu4 N35 1.961(5) . ?
Cu4 N31 1.961(5) . ?
Cu4 O22 1.992(4) . ?
Cu4 O19 1.995(4) . ?
Cu4 O14 2.386(4) . ?
Cu1 O1 1.974(4) . ?
Cu1 O4 1.974(4) . ?
Cu1 N1 1.984(5) . ?
Cu1 N5 1.991(5) . ?
O22 N40 1.296(7) . ?
O19 N39 1.301(6) . ?
O13 N29 1.296(6) . ?
O10 N20 1.303(7) . ?
O1 N9 1.308(7) . ?
O4 N10 1.304(7) . ?
O16 N30 1.293(7) . ?
O2 N9 1.240(7) . ?
O14 N29 1.242(7) . ?
O7 N19 1.299(6) . ?
O20 N39 1.231(7) . ?
O11 N20 1.216(7) . ?
O15 N29 1.218(7) . ?
N40 O24 1.230(7) . ?
N40 O23 1.231(7) . ?
O18 N30 1.252(7) . ?
N19 O8 1.211(7) . ?
N19 O9 1.248(7) . ?
O3 N9 1.222(7) . ?
N5 C5 1.316(8) . ?
N5 N6 1.360(8) . ?
N1 C1 1.318(8) . ?
N1 N2 1.369(7) . ?
N2 N3 1.292(7) . ?
N18 C13 1.326(8) . ?
N18 N17 1.349(7) . ?
N18 C14 1.439(8) . ?
O12 N20 1.243(7) . ?
N35 C29 1.318(8) . ?
N35 N36 1.363(7) . ?
N12 N13 1.289(7) . ?
N12 N11 1.360(7) . ?
N24 C17 1.324(8) . ?
N24 N23 1.352(8) . ?
N24 C18 1.460(8) . ?
O21 N39 1.231(7) . ?
O5 N10 1.227(7) . ?
N14 C9 1.332(8) . ?
N14 N13 1.353(7) . ?
N14 C10 1.429(8) . ?
N38 C29 1.330(8) . ?
N38 N37 1.345(7) . ?
N38 C30 1.453(8) . ?
N11 C9 1.313(8) . ?
N15 C13 1.319(8) . ?
N15 N16 1.355(8) . ?
O6 N10 1.230(7) . ?
N34 C25 1.312(8) . ?
N34 N33 1.348(8) . ?
N34 C26 1.437(8) . ?
O17 N30 1.220(7) . ?
N28 C21 1.321(8) . ?
N28 N27 1.365(8) . ?
N28 C22 1.451(8) . ?
N31 C25 1.317(8) . ?
N31 N32 1.354(8) . ?
N8 C5 1.326(8) . ?
N8 N7 1.342(8) . ?
N8 C6 1.447(8) . ?
N6 N7 1.297(8) . ?
N25 C21 1.312(8) . ?
N25 N26 1.364(7) . ?
N36 N37 1.289(7) . ?
N4 C1 1.314(8) . ?
N4 N3 1.352(7) . ?
N4 C2 1.445(8) . ?
N26 N27 1.284(7) . ?
N21 C17 1.323(7) . ?
N21 N22 1.361(8) . ?
N22 N23 1.283(8) . ?
C9 H9 0.9500 . ?
C25 H25 0.9500 . ?
C5 H5 0.9500 . ?
C1 H1 0.9500 . ?
N16 N17 1.289(8) . ?
N32 N33 1.302(8) . ?
C17 H17 0.9500 . ?
C6 C8 1.474(9) . ?
C6 C7 1.483(9) . ?
C6 H6 1.0000 . ?
C30 C32 1.467(10) . ?
C30 C31 1.485(10) . ?
C30 H30 1.0000 . ?
C14 C15 1.478(9) . ?
C14 C16 1.481(10) . ?
C14 H14 1.0000 . ?
C7 C8 1.492(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C21 H21 0.9500 . ?
C22 C23 1.484(10) . ?
C22 C24 1.487(10) . ?
C22 H22 1.0000 . ?
C29 H29 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.482(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C27 C26 1.471(9) . ?
C27 C28 1.502(11) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C23 C24 1.493(11) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C26 C28 1.466(10) . ?
C26 H26 1.0000 . ?
C19 C18 1.484(10) . ?
C19 C20 1.487(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C18 C20 1.475(9) . ?
C18 H18 1.0000 . ?
C3 C4 1.491(11) . ?
C3 C2 1.502(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C31 C32 1.475(11) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C12 C11 1.481(11) . ?
C12 C10 1.490(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C4 C2 1.499(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C10 C11 1.476(10) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C2 H2 1.0000 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Cu2 N11 91.4(2) . . ?
O7 Cu2 N15 89.7(2) . . ?
N11 Cu2 N15 173.7(2) . . ?
O7 Cu2 O10 169.97(18) . . ?
N11 Cu2 O10 87.89(19) . . ?
N15 Cu2 O10 92.1(2) . . ?
O7 Cu2 O2 107.09(18) . . ?
N11 Cu2 O2 88.22(19) . . ?
N15 Cu2 O2 85.55(19) . . ?
O10 Cu2 O2 82.89(17) . . ?
O16 Cu3 N25 88.6(2) . . ?
O16 Cu3 N21 91.3(2) . . ?
N25 Cu3 N21 176.0(2) . . ?
O16 Cu3 O13 173.34(19) . . ?
N25 Cu3 O13 90.2(2) . . ?
N21 Cu3 O13 90.4(2) . . ?
N35 Cu4 N31 178.5(2) . . ?
N35 Cu4 O22 87.2(2) . . ?
N31 Cu4 O22 92.8(2) . . ?
N35 Cu4 O19 89.5(2) . . ?
N31 Cu4 O19 90.4(2) . . ?
O22 Cu4 O19 175.95(18) . . ?
N35 Cu4 O14 94.4(2) . . ?
N31 Cu4 O14 87.1(2) . . ?
O22 Cu4 O14 83.39(16) . . ?
O19 Cu4 O14 99.21(16) . . ?
O1 Cu1 O4 170.71(19) . . ?
O1 Cu1 N1 89.3(2) . . ?
O4 Cu1 N1 88.4(2) . . ?
O1 Cu1 N5 91.85(19) . . ?
O4 Cu1 N5 91.2(2) . . ?
N1 Cu1 N5 174.6(2) . . ?
N40 O22 Cu4 108.8(4) . . ?
N39 O19 Cu4 113.9(4) . . ?
N29 O13 Cu3 112.0(4) . . ?
N20 O10 Cu2 105.8(4) . . ?
N9 O1 Cu1 110.3(4) . . ?
N10 O4 Cu1 106.2(4) . . ?
N30 O16 Cu3 108.6(4) . . ?
N9 O2 Cu2 119.5(4) . . ?
N29 O14 Cu4 126.2(4) . . ?
N19 O7 Cu2 114.2(4) . . ?
O24 N40 O23 122.9(6) . . ?
O24 N40 O22 118.0(5) . . ?
O23 N40 O22 119.1(5) . . ?
O8 N19 O9 123.8(6) . . ?
O8 N19 O7 120.2(5) . . ?
O9 N19 O7 116.0(5) . . ?
O15 N29 O14 124.0(6) . . ?
O15 N29 O13 118.0(5) . . ?
O14 N29 O13 117.9(5) . . ?
C5 N5 N6 106.7(5) . . ?
C5 N5 Cu1 129.1(4) . . ?
N6 N5 Cu1 124.0(4) . . ?
C1 N1 N2 105.6(5) . . ?
C1 N1 Cu1 130.9(5) . . ?
N2 N1 Cu1 123.1(4) . . ?
N3 N2 N1 109.9(5) . . ?
O3 N9 O2 124.6(6) . . ?
O3 N9 O1 118.3(6) . . ?
O2 N9 O1 117.1(5) . . ?
C13 N18 N17 108.1(5) . . ?
C13 N18 C14 132.1(6) . . ?
N17 N18 C14 119.8(5) . . ?
C29 N35 N36 106.4(5) . . ?
C29 N35 Cu4 127.6(5) . . ?
N36 N35 Cu4 125.8(4) . . ?
N13 N12 N11 109.4(5) . . ?
C17 N24 N23 109.2(5) . . ?
C17 N24 C18 131.2(6) . . ?
N23 N24 C18 119.4(6) . . ?
C9 N14 N13 108.0(5) . . ?
C9 N14 C10 131.1(6) . . ?
N13 N14 C10 120.9(5) . . ?
C29 N38 N37 108.4(5) . . ?
C29 N38 C30 128.4(6) . . ?
N37 N38 C30 123.2(5) . . ?
C9 N11 N12 107.0(5) . . ?
C9 N11 Cu2 128.9(4) . . ?
N12 N11 Cu2 124.1(4) . . ?
C13 N15 N16 106.3(5) . . ?
C13 N15 Cu2 131.5(5) . . ?
N16 N15 Cu2 122.1(4) . . ?
C25 N34 N33 108.2(5) . . ?
C25 N34 C26 128.8(6) . . ?
N33 N34 C26 122.9(5) . . ?
C21 N28 N27 108.5(5) . . ?
C21 N28 C22 128.8(6) . . ?
N27 N28 C22 122.7(6) . . ?
C25 N31 N32 105.9(5) . . ?
C25 N31 Cu4 128.4(5) . . ?
N32 N31 Cu4 125.6(4) . . ?
C5 N8 N7 109.2(5) . . ?
C5 N8 C6 129.4(6) . . ?
N7 N8 C6 121.3(5) . . ?
O5 N10 O6 123.5(6) . . ?
O5 N10 O4 119.1(6) . . ?
O6 N10 O4 117.3(6) . . ?
O20 N39 O21 124.1(6) . . ?
O20 N39 O19 117.1(5) . . ?
O21 N39 O19 118.9(5) . . ?
N7 N6 N5 109.6(5) . . ?
C21 N25 N26 106.9(5) . . ?
C21 N25 Cu3 130.5(5) . . ?
N26 N25 Cu3 122.6(4) . . ?
N37 N36 N35 109.7(5) . . ?
C1 N4 N3 108.5(5) . . ?
C1 N4 C2 129.7(6) . . ?
N3 N4 C2 121.7(5) . . ?
N36 N37 N38 107.2(5) . . ?
N27 N26 N25 109.8(5) . . ?
N2 N3 N4 106.7(5) . . ?
N12 N13 N14 107.3(5) . . ?
C17 N21 N22 106.2(5) . . ?
C17 N21 Cu3 130.2(5) . . ?
N22 N21 Cu3 123.4(4) . . ?
O11 N20 O12 123.9(6) . . ?
O11 N20 O10 119.2(6) . . ?
O12 N20 O10 116.9(6) . . ?
N6 N7 N8 106.5(6) . . ?
N26 N27 N28 106.5(5) . . ?
N23 N22 N21 110.6(6) . . ?
N11 C9 N14 108.3(6) . . ?
N11 C9 H9 125.9 . . ?
N14 C9 H9 125.9 . . ?
N34 C25 N31 109.4(6) . . ?
N34 C25 H25 125.3 . . ?
N31 C25 H25 125.3 . . ?
O17 N30 O18 122.9(6) . . ?
O17 N30 O16 119.6(6) . . ?
O18 N30 O16 117.4(5) . . ?
N5 C5 N8 107.9(6) . . ?
N5 C5 H5 126.1 . . ?
N8 C5 H5 126.1 . . ?
N4 C1 N1 109.2(6) . . ?
N4 C1 H1 125.4 . . ?
N1 C1 H1 125.4 . . ?
N17 N16 N15 109.9(5) . . ?
N33 N32 N31 109.8(6) . . ?
N22 N23 N24 106.2(6) . . ?
N21 C17 N24 107.8(6) . . ?
N21 C17 H17 126.1 . . ?
N24 C17 H17 126.1 . . ?
N8 C6 C8 117.9(6) . . ?
N8 C6 C7 118.6(6) . . ?
C8 C6 C7 60.6(5) . . ?
N8 C6 H6 116.1 . . ?
C8 C6 H6 116.1 . . ?
C7 C6 H6 116.1 . . ?
N38 C30 C32 119.3(6) . . ?
N38 C30 C31 118.9(6) . . ?
C32 C30 C31 60.0(5) . . ?
N38 C30 H30 115.8 . . ?
C32 C30 H30 115.8 . . ?
C31 C30 H30 115.8 . . ?
N18 C14 C15 120.4(6) . . ?
N18 C14 C16 120.5(6) . . ?
C15 C14 C16 60.1(5) . . ?
N18 C14 H14 115.0 . . ?
C15 C14 H14 115.0 . . ?
C16 C14 H14 115.0 . . ?
N16 N17 N18 107.1(5) . . ?
N32 N33 N34 106.7(6) . . ?
C6 C7 C8 59.4(4) . . ?
C6 C7 H7A 117.8 . . ?
C8 C7 H7A 117.8 . . ?
C6 C7 H7B 117.8 . . ?
C8 C7 H7B 117.8 . . ?
H7A C7 H7B 115.0 . . ?
C6 C8 C7 60.0(5) . . ?
C6 C8 H8A 117.8 . . ?
C7 C8 H8A 117.8 . . ?
C6 C8 H8B 117.8 . . ?
C7 C8 H8B 117.8 . . ?
H8A C8 H8B 114.9 . . ?
N25 C21 N28 108.3(6) . . ?
N25 C21 H21 125.9 . . ?
N28 C21 H21 125.9 . . ?
N28 C22 C23 118.1(6) . . ?
N28 C22 C24 116.9(6) . . ?
C23 C22 C24 60.3(5) . . ?
N28 C22 H22 116.6 . . ?
C23 C22 H22 116.6 . . ?
C24 C22 H22 116.6 . . ?
N35 C29 N38 108.3(6) . . ?
N35 C29 H29 125.8 . . ?
N38 C29 H29 125.8 . . ?
N15 C13 N18 108.6(6) . . ?
N15 C13 H13 125.7 . . ?
N18 C13 H13 125.7 . . ?
C14 C15 C16 60.1(5) . . ?
C14 C15 H15A 117.8 . . ?
C16 C15 H15A 117.8 . . ?
C14 C15 H15B 117.8 . . ?
C16 C15 H15B 117.8 . . ?
H15A C15 H15B 114.9 . . ?
C14 C16 C15 59.8(5) . . ?
C14 C16 H16A 117.8 . . ?
C15 C16 H16A 117.8 . . ?
C14 C16 H16B 117.8 . . ?
C15 C16 H16B 117.8 . . ?
H16A C16 H16B 114.9 . . ?
C26 C27 C28 59.1(5) . . ?
C26 C27 H27A 117.9 . . ?
C28 C27 H27A 117.9 . . ?
C26 C27 H27B 117.9 . . ?
C28 C27 H27B 117.9 . . ?
H27A C27 H27B 115.0 . . ?
C22 C23 C24 60.0(5) . . ?
C22 C23 H23A 117.8 . . ?
C24 C23 H23A 117.8 . . ?
C22 C23 H23B 117.8 . . ?
C24 C23 H23B 117.8 . . ?
H23A C23 H23B 114.9 . . ?
N34 C26 C28 120.0(6) . . ?
N34 C26 C27 119.8(6) . . ?
C28 C26 C27 61.5(5) . . ?
N34 C26 H26 115.0 . . ?
C28 C26 H26 115.0 . . ?
C27 C26 H26 115.0 . . ?
C18 C19 C20 59.5(5) . . ?
C18 C19 H19A 117.8 . . ?
C20 C19 H19A 117.8 . . ?
C18 C19 H19B 117.8 . . ?
C20 C19 H19B 117.8 . . ?
H19A C19 H19B 115.0 . . ?
N24 C18 C20 117.1(6) . . ?
N24 C18 C19 117.6(6) . . ?
C20 C18 C19 60.3(5) . . ?
N24 C18 H18 116.7 . . ?
C20 C18 H18 116.7 . . ?
C19 C18 H18 116.7 . . ?
C4 C3 C2 60.1(5) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C32 C31 C30 59.4(5) . . ?
C32 C31 H31A 117.8 . . ?
C30 C31 H31A 117.8 . . ?
C32 C31 H31B 117.8 . . ?
C30 C31 H31B 117.8 . . ?
H31A C31 H31B 115.0 . . ?
C11 C12 C10 59.6(5) . . ?
C11 C12 H12A 117.8 . . ?
C10 C12 H12A 117.8 . . ?
C11 C12 H12B 117.8 . . ?
C10 C12 H12B 117.8 . . ?
H12A C12 H12B 115.0 . . ?
C3 C4 C2 60.3(5) . . ?
C3 C4 H4A 117.7 . . ?
C2 C4 H4A 117.7 . . ?
C3 C4 H4B 117.7 . . ?
C2 C4 H4B 117.7 . . ?
H4A C4 H4B 114.9 . . ?
N14 C10 C11 118.7(6) . . ?
N14 C10 C12 116.4(6) . . ?
C11 C10 C12 59.9(5) . . ?
N14 C10 H10 116.6 . . ?
C11 C10 H10 116.6 . . ?
C12 C10 H10 116.6 . . ?
C10 C11 C12 60.5(5) . . ?
C10 C11 H11A 117.7 . . ?
C12 C11 H11A 117.7 . . ?
C10 C11 H11B 117.7 . . ?
C12 C11 H11B 117.7 . . ?
H11A C11 H11B 114.8 . . ?
N4 C2 C4 117.2(6) . . ?
N4 C2 C3 116.1(6) . . ?
C4 C2 C3 59.6(5) . . ?
N4 C2 H2 117.2 . . ?
C4 C2 H2 117.2 . . ?
C3 C2 H2 117.2 . . ?
C30 C32 C31 60.6(5) . . ?
C30 C32 H32A 117.7 . . ?
C31 C32 H32A 117.7 . . ?
C30 C32 H32B 117.7 . . ?
C31 C32 H32B 117.7 . . ?
H32A C32 H32B 114.8 . . ?
C18 C20 C19 60.2(5) . . ?
C18 C20 H20A 117.8 . . ?
C19 C20 H20A 117.8 . . ?
C18 C20 H20B 117.8 . . ?
C19 C20 H20B 117.8 . . ?
H20A C20 H20B 114.9 . . ?
C26 C28 C27 59.4(5) . . ?
C26 C28 H28A 117.8 . . ?
C27 C28 H28A 117.8 . . ?
C26 C28 H28B 117.8 . . ?
C27 C28 H28B 117.8 . . ?
H28A C28 H28B 115.0 . . ?
C22 C24 C23 59.7(5) . . ?
C22 C24 H24A 117.8 . . ?
C23 C24 H24A 117.8 . . ?
C22 C24 H24B 117.8 . . ?
C23 C24 H24B 117.8 . . ?
H24A C24 H24B 114.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu4 O22 N40 O24 -176.6(4) . . . . ?
Cu4 O22 N40 O23 3.9(7) . . . . ?
Cu2 O7 N19 O8 19.2(7) . . . . ?
Cu2 O7 N19 O9 -159.9(4) . . . . ?
Cu4 O14 N29 O15 12.7(8) . . . . ?
Cu4 O14 N29 O13 -168.8(4) . . . . ?
Cu3 O13 N29 O15 166.6(4) . . . . ?
Cu3 O13 N29 O14 -12.1(6) . . . . ?
C1 N1 N2 N3 -0.2(7) . . . . ?
Cu1 N1 N2 N3 -173.9(4) . . . . ?
Cu2 O2 N9 O3 -10.2(8) . . . . ?
Cu2 O2 N9 O1 169.9(3) . . . . ?
Cu1 O1 N9 O3 -166.4(4) . . . . ?
Cu1 O1 N9 O2 13.6(6) . . . . ?
N13 N12 N11 C9 -0.1(7) . . . . ?
N13 N12 N11 Cu2 179.0(4) . . . . ?
Cu1 O4 N10 O5 -174.3(5) . . . . ?
Cu1 O4 N10 O6 3.9(6) . . . . ?
Cu4 O19 N39 O20 166.4(4) . . . . ?
Cu4 O19 N39 O21 -13.1(6) . . . . ?
C5 N5 N6 N7 0.3(8) . . . . ?
Cu1 N5 N6 N7 176.6(5) . . . . ?
C29 N35 N36 N37 0.5(7) . . . . ?
Cu4 N35 N36 N37 175.4(4) . . . . ?
N35 N36 N37 N38 -0.3(7) . . . . ?
C29 N38 N37 N36 0.1(7) . . . . ?
C30 N38 N37 N36 -177.8(6) . . . . ?
C21 N25 N26 N27 0.4(7) . . . . ?
Cu3 N25 N26 N27 179.5(4) . . . . ?
N1 N2 N3 N4 -0.8(7) . . . . ?
C1 N4 N3 N2 1.6(7) . . . . ?
C2 N4 N3 N2 -179.4(6) . . . . ?
N11 N12 N13 N14 0.3(7) . . . . ?
C9 N14 N13 N12 -0.4(7) . . . . ?
C10 N14 N13 N12 -177.8(6) . . . . ?
Cu2 O10 N20 O11 -178.0(5) . . . . ?
Cu2 O10 N20 O12 1.6(7) . . . . ?
N5 N6 N7 N8 -0.2(8) . . . . ?
C5 N8 N7 N6 -0.1(8) . . . . ?
C6 N8 N7 N6 -177.3(6) . . . . ?
N25 N26 N27 N28 -0.1(7) . . . . ?
C21 N28 N27 N26 -0.3(7) . . . . ?
C22 N28 N27 N26 179.5(6) . . . . ?
C17 N21 N22 N23 -1.3(8) . . . . ?
Cu3 N21 N22 N23 -176.3(5) . . . . ?
N12 N11 C9 N14 -0.1(7) . . . . ?
Cu2 N11 C9 N14 -179.2(4) . . . . ?
N13 N14 C9 N11 0.3(7) . . . . ?
C10 N14 C9 N11 177.4(6) . . . . ?
N33 N34 C25 N31 -0.7(8) . . . . ?
C26 N34 C25 N31 -177.4(6) . . . . ?
N32 N31 C25 N34 1.5(8) . . . . ?
Cu4 N31 C25 N34 177.8(4) . . . . ?
Cu3 O16 N30 O17 171.7(5) . . . . ?
Cu3 O16 N30 O18 -8.0(6) . . . . ?
N6 N5 C5 N8 -0.3(7) . . . . ?
Cu1 N5 C5 N8 -176.4(4) . . . . ?
N7 N8 C5 N5 0.3(7) . . . . ?
C6 N8 C5 N5 177.2(6) . . . . ?
N3 N4 C1 N1 -1.7(7) . . . . ?
C2 N4 C1 N1 179.3(6) . . . . ?
N2 N1 C1 N4 1.2(7) . . . . ?
Cu1 N1 C1 N4 174.2(4) . . . . ?
C13 N15 N16 N17 1.1(8) . . . . ?
Cu2 N15 N16 N17 178.6(5) . . . . ?
C25 N31 N32 N33 -1.8(9) . . . . ?
Cu4 N31 N32 N33 -178.2(6) . . . . ?
N21 N22 N23 N24 0.8(8) . . . . ?
C17 N24 N23 N22 0.0(8) . . . . ?
C18 N24 N23 N22 175.5(6) . . . . ?
N22 N21 C17 N24 1.3(7) . . . . ?
Cu3 N21 C17 N24 175.8(4) . . . . ?
N23 N24 C17 N21 -0.8(8) . . . . ?
C18 N24 C17 N21 -175.6(6) . . . . ?
C5 N8 C6 C8 40.5(10) . . . . ?
N7 N8 C6 C8 -143.0(7) . . . . ?
C5 N8 C6 C7 110.3(8) . . . . ?
N7 N8 C6 C7 -73.1(8) . . . . ?
C29 N38 C30 C32 -177.6(7) . . . . ?
N37 N38 C30 C32 -0.2(10) . . . . ?
C29 N38 C30 C31 112.6(8) . . . . ?
N37 N38 C30 C31 -70.0(9) . . . . ?
C13 N18 C14 C15 15.8(11) . . . . ?
N17 N18 C14 C15 -161.8(7) . . . . ?
C13 N18 C14 C16 -55.2(10) . . . . ?
N17 N18 C14 C16 127.2(7) . . . . ?
N15 N16 N17 N18 -1.3(9) . . . . ?
C13 N18 N17 N16 1.0(8) . . . . ?
C14 N18 N17 N16 179.2(6) . . . . ?
N31 N32 N33 N34 1.4(10) . . . . ?
C25 N34 N33 N32 -0.5(9) . . . . ?
C26 N34 N33 N32 176.4(7) . . . . ?
N8 C6 C7 C8 -107.8(7) . . . . ?
N8 C6 C8 C7 108.8(7) . . . . ?
N26 N25 C21 N28 -0.6(7) . . . . ?
Cu3 N25 C21 N28 -179.5(4) . . . . ?
N27 N28 C21 N25 0.6(7) . . . . ?
C22 N28 C21 N25 -179.2(6) . . . . ?
C21 N28 C22 C23 -65.4(9) . . . . ?
N27 N28 C22 C23 114.9(7) . . . . ?
C21 N28 C22 C24 -134.4(7) . . . . ?
N27 N28 C22 C24 45.8(9) . . . . ?
N36 N35 C29 N38 -0.4(7) . . . . ?
Cu4 N35 C29 N38 -175.2(4) . . . . ?
N37 N38 C29 N35 0.2(7) . . . . ?
C30 N38 C29 N35 177.9(6) . . . . ?
N16 N15 C13 N18 -0.4(8) . . . . ?
Cu2 N15 C13 N18 -177.7(5) . . . . ?
N17 N18 C13 N15 -0.3(8) . . . . ?
C14 N18 C13 N15 -178.2(6) . . . . ?
N18 C14 C15 C16 -109.9(7) . . . . ?
N18 C14 C16 C15 109.8(7) . . . . ?
N28 C22 C23 C24 -106.6(7) . . . . ?
C25 N34 C26 C28 -157.2(7) . . . . ?
N33 N34 C26 C28 26.6(10) . . . . ?
C25 N34 C26 C27 130.5(7) . . . . ?
N33 N34 C26 C27 -45.8(10) . . . . ?
C28 C27 C26 N34 110.2(8) . . . . ?
C17 N24 C18 C20 -90.4(9) . . . . ?
N23 N24 C18 C20 95.3(8) . . . . ?
C17 N24 C18 C19 -21.6(11) . . . . ?
N23 N24 C18 C19 164.2(6) . . . . ?
C20 C19 C18 N24 -107.1(7) . . . . ?
N38 C30 C31 C32 109.1(7) . . . . ?
C9 N14 C10 C11 54.4(10) . . . . ?
N13 N14 C10 C11 -128.9(7) . . . . ?
C9 N14 C10 C12 122.9(8) . . . . ?
N13 N14 C10 C12 -60.4(9) . . . . ?
C11 C12 C10 N14 -109.4(7) . . . . ?
N14 C10 C11 C12 105.6(7) . . . . ?
C1 N4 C2 C4 121.0(8) . . . . ?
N3 N4 C2 C4 -57.9(9) . . . . ?
C1 N4 C2 C3 53.5(9) . . . . ?
N3 N4 C2 C3 -125.4(6) . . . . ?
C3 C4 C2 N4 -105.7(7) . . . . ?
C4 C3 C2 N4 107.6(7) . . . . ?
N38 C30 C32 C31 -108.4(7) . . . . ?
N24 C18 C20 C19 107.9(7) . . . . ?
N34 C26 C28 C27 -109.9(7) . . . . ?
N28 C22 C24 C23 108.7(7) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.775
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.120

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px231
_database_code_depnum_ccdc_archive 'CCDC 2061080'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-17
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'aqua(tetrakis(1-cyclopropyl-5H-tetrazolyl)copper(II) diperchlorate'
_chemical_name_common            
'aqua(tetrakis(1-cyclopropyl-5H-tetrazolyl)copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H68 Cu2 N32 O2, 4(Cl O4)'
_chemical_formula_sum            'C40 H68 Cl4 Cu2 N32 O18'
_chemical_formula_weight         1554.14

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.0836(7)
_cell_length_b                   11.1197(5)
_cell_length_c                   17.2721(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.681(4)
_cell_angle_gamma                90
_cell_volume                     3274.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    111(2)
_cell_measurement_reflns_used    2316
_cell_measurement_theta_min      2.1610
_cell_measurement_theta_max      24.8030

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.091
_exptl_absorpt_coefficient_mu    0.903
_shelx_estimated_absorpt_T_min   0.810
_shelx_estimated_absorpt_T_max   0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_F_000             1604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      111(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            18424
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.1257
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.180
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6677
_reflns_number_gt                4331
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+1.6112P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6677
_refine_ls_number_parameters     472
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0374236000
_diffrn_orient_matrix_UB_12      -0.0039346000
_diffrn_orient_matrix_UB_13      -0.0153867000
_diffrn_orient_matrix_UB_21      0.0144105000
_diffrn_orient_matrix_UB_22      -0.0320005000
_diffrn_orient_matrix_UB_23      0.0334791000
_diffrn_orient_matrix_UB_31      -0.0110764000
_diffrn_orient_matrix_UB_32      -0.0550372000
_diffrn_orient_matrix_UB_33      -0.0183300000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  50.00   1.00   35.00    --  -20.37  57.00  60.00   94
  2  ω    -91.00   3.00   1.00   35.00    --  -20.37 -57.00 -90.00   94
  3  ω     -2.00  92.00   1.00   35.00    --   21.23  57.00-180.00   94
  4  ω    -12.00  33.00   1.00   35.00    --   21.23  77.00 -90.00   45
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.53865(3) 0.19577(4) 0.01862(3) 0.01552(14) Uani 1 1 d . . . . .
O1 O 0.4981(2) 0.3758(3) -0.0278(2) 0.0284(8) Uani 1 1 d . . . . .
N1 N 0.65639(18) 0.3136(3) 0.21900(18) 0.0167(7) Uani 1 1 d . . . . .
N2 N 0.71581(18) 0.2675(3) 0.1812(2) 0.0227(8) Uani 1 1 d . . . . .
N3 N 0.68730(18) 0.2324(3) 0.11418(19) 0.0198(8) Uani 1 1 d . . . . .
N4 N 0.60845(17) 0.2559(3) 0.10739(18) 0.0155(7) Uani 1 1 d . . . . .
N5 N 0.33874(18) 0.1711(3) 0.13798(18) 0.0161(7) Uani 1 1 d . . . . .
N6 N 0.39231(18) 0.1290(3) 0.19318(19) 0.0217(8) Uani 1 1 d . . . . .
N7 N 0.45929(19) 0.1315(3) 0.16327(19) 0.0219(8) Uani 1 1 d . . . . .
N8 N 0.45090(17) 0.1749(3) 0.08880(18) 0.0165(7) Uani 1 1 d . . . . .
N12 N 0.47138(17) 0.1267(3) -0.07041(18) 0.0150(7) Uani 1 1 d . . . . .
N13 N 0.73908(18) 0.2182(3) -0.10146(18) 0.0177(8) Uani 1 1 d . . . . .
N14 N 0.70914(19) 0.1113(3) -0.1253(2) 0.0253(8) Uani 1 1 d . . . . .
N15 N 0.64318(19) 0.0982(3) -0.0934(2) 0.0256(8) Uani 1 1 d . . . . .
N16 N 0.63012(17) 0.1953(3) -0.04861(18) 0.0169(7) Uani 1 1 d . . . . .
C1 C 0.5917(2) 0.3076(3) 0.1728(2) 0.0176(9) Uani 1 1 d . . . . .
H1 H 0.541466 0.335907 0.184917 0.021 Uiso 1 1 calc R U . . .
C2 C 0.6700(2) 0.3651(4) 0.2968(2) 0.0236(10) Uani 1 1 d . . . . .
H2 H 0.722547 0.339443 0.319967 0.028 Uiso 1 1 calc R U . . .
C3 C 0.6078(3) 0.3461(4) 0.3554(3) 0.0314(11) Uani 1 1 d . . . . .
H3A H 0.621665 0.283586 0.394765 0.038 Uiso 1 1 calc R U . . .
H3B H 0.554256 0.333422 0.331431 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6237(3) 0.4747(4) 0.3838(3) 0.0380(12) Uani 1 1 d . . . . .
H4A H 0.661272 0.480065 0.429709 0.046 Uiso 1 1 calc R U . . .
H4B H 0.575572 0.521642 0.391600 0.046 Uiso 1 1 calc R U . . .
C5 C 0.6602(3) 0.5008(4) 0.3065(2) 0.0322(11) Uani 1 1 d . . . . .
H5A H 0.623526 0.538104 0.266789 0.039 Uiso 1 1 calc R U . . .
H5B H 0.710312 0.545601 0.312128 0.039 Uiso 1 1 calc R U . . .
C6 C 0.3755(2) 0.1982(3) 0.0752(2) 0.0162(8) Uani 1 1 d . . . . .
H6 H 0.351650 0.229197 0.028203 0.019 Uiso 1 1 calc R U . . .
C7 C 0.2557(2) 0.1817(4) 0.1533(2) 0.0224(10) Uani 1 1 d . . . . .
H7 H 0.244359 0.134515 0.200629 0.027 Uiso 1 1 calc R U . . .
C8 C 0.1946(2) 0.1534(4) 0.0869(3) 0.0351(12) Uani 1 1 d . . . . .
H8A H 0.213889 0.164937 0.034513 0.042 Uiso 1 1 calc R U . . .
H8B H 0.168947 0.074117 0.091363 0.042 Uiso 1 1 calc R U . . .
C9 C 0.1464(3) 0.2591(5) 0.1151(3) 0.0450(14) Uani 1 1 d . . . . .
H9A H 0.124703 0.311954 0.072857 0.054 Uiso 1 1 calc R U . . .
H9B H 0.105285 0.235240 0.149901 0.054 Uiso 1 1 calc R U . . .
C10 C 0.2210(2) 0.3081(4) 0.1577(3) 0.0338(11) Uani 1 1 d . . . . .
H10A H 0.248741 0.369306 0.128143 0.041 Uiso 1 1 calc R U . . .
H10B H 0.213562 0.335885 0.211224 0.041 Uiso 1 1 calc R U . . .
C16 C 0.6901(2) 0.2687(4) -0.0547(2) 0.0185(9) Uani 1 1 d . . . . .
H16 H 0.697004 0.344469 -0.029797 0.022 Uiso 1 1 calc R U . . .
C17 C 0.8168(2) 0.2548(4) -0.1247(2) 0.0205(9) Uani 1 1 d . . . . .
H17 H 0.823159 0.229462 -0.179475 0.025 Uiso 1 1 calc R U . . .
C18 C 0.8430(2) 0.3847(4) -0.1137(3) 0.0248(10) Uani 1 1 d . . . . .
H18A H 0.820559 0.425893 -0.069375 0.030 Uiso 1 1 calc R U . . .
H18B H 0.837199 0.434110 -0.161422 0.030 Uiso 1 1 calc R U . . .
C19 C 0.9258(2) 0.3346(4) -0.0959(3) 0.0303(11) Uani 1 1 d . . . . .
H19A H 0.955430 0.375637 -0.052366 0.036 Uiso 1 1 calc R U . . .
H19B H 0.957354 0.328844 -0.141830 0.036 Uiso 1 1 calc R U . . .
C20 C 0.8884(2) 0.2145(4) -0.0730(3) 0.0322(11) Uani 1 1 d . . . . .
H20A H 0.915088 0.142119 -0.091896 0.039 Uiso 1 1 calc R U . . .
H20B H 0.878835 0.207614 -0.017259 0.039 Uiso 1 1 calc R U . . .
Cl1 Cl 0.09325(6) 0.01252(10) 0.29933(7) 0.0304(3) Uani 1 1 d . . . . .
O3 O 0.0927(2) -0.0245(3) 0.3795(2) 0.0658(12) Uani 1 1 d . . . . .
Cl2 Cl 0.71880(6) 0.59393(9) 0.08619(6) 0.0255(3) Uani 1 1 d . . . . .
O7 O 0.7552(2) 0.5657(3) 0.16000(19) 0.0545(11) Uani 1 1 d . . . . .
O8 O 0.7737(3) 0.5802(4) 0.0297(2) 0.0820(15) Uani 1 1 d . . . . .
O10 O 0.69283(19) 0.7164(3) 0.08563(18) 0.0398(9) Uani 1 1 d . . . . .
N9 N 0.41538(17) 0.1015(3) -0.18372(18) 0.0152(7) Uani 1 1 d . . . . .
N11 N 0.42066(18) 0.0330(3) -0.06882(19) 0.0184(8) Uani 1 1 d . . . . .
N10 N 0.38622(18) 0.0167(3) -0.13707(19) 0.0195(8) Uani 1 1 d . . . . .
C11 C 0.4671(2) 0.1673(3) -0.1421(2) 0.0170(9) Uani 1 1 d . . . . .
H11 H 0.496185 0.232765 -0.160776 0.020 Uiso 1 1 calc R U . . .
C12 C 0.3939(2) 0.0973(4) -0.2672(2) 0.0182(9) Uani 1 1 d . . . . .
H12 H 0.336575 0.079713 -0.276124 0.022 Uiso 1 1 calc R U . . .
C13 C 0.4162(2) 0.2024(4) -0.3180(2) 0.0255(10) Uani 1 1 d . . . . .
H13A H 0.463562 0.246686 -0.298084 0.031 Uiso 1 1 calc R U . . .
H13B H 0.372398 0.258017 -0.332404 0.031 Uiso 1 1 calc R U . . .
C15 C 0.4409(2) 0.0124(4) -0.3157(2) 0.0263(10) Uani 1 1 d . . . . .
H15A H 0.414409 -0.064903 -0.328499 0.032 Uiso 1 1 calc R U . . .
H15B H 0.495699 -0.000333 -0.295065 0.032 Uiso 1 1 calc R U . . .
C14 C 0.4317(3) 0.1079(4) -0.3807(2) 0.0314(11) Uani 1 1 d . . . . .
H14A H 0.480134 0.122463 -0.407766 0.038 Uiso 1 1 calc R U . . .
H14B H 0.386312 0.093724 -0.418229 0.038 Uiso 1 1 calc R U . . .
O4A O 0.1635(3) 0.0674(7) 0.2908(3) 0.068(3) Uani 0.753(9) 1 d . . P A 1
O5A O 0.0850(3) -0.0963(5) 0.2585(4) 0.063(2) Uani 0.753(9) 1 d . . P A 1
O6A O 0.0272(3) 0.0850(5) 0.2857(3) 0.059(2) Uani 0.753(9) 1 d . . P A 1
O9A O 0.6511(4) 0.5152(6) 0.0764(5) 0.071(2) Uani 0.753(9) 1 d . . P A 1
O4B O 0.0982(12) 0.1467(12) 0.2950(7) 0.050(7) Uani 0.247(9) 1 d . . P A 2
O5B O 0.1603(14) -0.0213(18) 0.2564(13) 0.089(9) Uani 0.247(9) 1 d . . P A 2
O6B O 0.0326(14) -0.016(2) 0.2398(14) 0.128(13) Uani 0.247(9) 1 d . . P A 2
O9B O 0.6640(14) 0.534(2) 0.0385(16) 0.071(2) Uani 0.247(9) 1 d . . P A 2
H1B H 0.521(2) 0.415(4) -0.050(2) 0.017(14) Uiso 1 1 d . . . . .
H1C H 0.445(4) 0.396(6) -0.032(4) 0.10(2) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 1.996(3) . ?
Cu1 N8 2.001(3) . ?
Cu1 N16 2.006(3) . ?
Cu1 N12 2.012(3) . ?
Cu1 O1 2.249(3) . ?
O1 H1B 0.71(4) . ?
O1 H1C 0.93(6) . ?
N1 C1 1.322(4) . ?
N1 N2 1.343(4) . ?
N1 C2 1.466(5) . ?
N2 N3 1.287(4) . ?
N3 N4 1.370(4) . ?
N4 C1 1.316(5) . ?
N5 C6 1.322(5) . ?
N5 N6 1.362(4) . ?
N5 C7 1.465(5) . ?
N6 N7 1.286(4) . ?
N7 N8 1.372(4) . ?
N8 C6 1.320(5) . ?
N12 C11 1.315(5) . ?
N12 N11 1.356(4) . ?
N13 C16 1.325(5) . ?
N13 N14 1.348(4) . ?
N13 C17 1.468(5) . ?
N14 N15 1.294(4) . ?
N15 N16 1.355(4) . ?
N16 C16 1.320(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.528(6) . ?
C2 C5 1.528(6) . ?
C2 H2 1.0000 . ?
C3 C4 1.530(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.537(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6 0.9500 . ?
C7 C10 1.529(6) . ?
C7 C8 1.533(6) . ?
C7 H7 1.0000 . ?
C8 C9 1.533(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.531(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C16 H16 0.9500 . ?
C17 C18 1.521(5) . ?
C17 C20 1.535(5) . ?
C17 H17 1.0000 . ?
C18 C19 1.534(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.543(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
Cl1 O4A 1.363(5) . ?
Cl1 O6A 1.395(4) . ?
Cl1 O5A 1.403(5) . ?
Cl1 O6B 1.446(16) . ?
Cl1 O3 1.446(4) . ?
Cl1 O5B 1.454(16) . ?
Cl1 O4B 1.497(13) . ?
Cl2 O9B 1.38(3) . ?
Cl2 O8 1.405(4) . ?
Cl2 O7 1.418(3) . ?
Cl2 O10 1.432(3) . ?
Cl2 O9A 1.452(7) . ?
N9 C11 1.324(4) . ?
N9 N10 1.355(4) . ?
N9 C12 1.465(5) . ?
N11 N10 1.296(4) . ?
C11 H11 0.9500 . ?
C12 C15 1.525(5) . ?
C12 C13 1.525(5) . ?
C12 H12 1.0000 . ?
C13 C14 1.544(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C15 C14 1.546(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N8 90.42(12) . . ?
N4 Cu1 N16 89.79(12) . . ?
N8 Cu1 N16 172.83(13) . . ?
N4 Cu1 N12 176.94(13) . . ?
N8 Cu1 N12 90.31(12) . . ?
N16 Cu1 N12 89.11(12) . . ?
N4 Cu1 O1 97.51(13) . . ?
N8 Cu1 O1 95.36(13) . . ?
N16 Cu1 O1 91.71(14) . . ?
N12 Cu1 O1 85.39(12) . . ?
Cu1 O1 H1B 125(3) . . ?
Cu1 O1 H1C 121(4) . . ?
H1B O1 H1C 111(5) . . ?
C1 N1 N2 108.4(3) . . ?
C1 N1 C2 130.6(3) . . ?
N2 N1 C2 120.9(3) . . ?
N3 N2 N1 107.4(3) . . ?
N2 N3 N4 109.4(3) . . ?
C1 N4 N3 106.1(3) . . ?
C1 N4 Cu1 130.9(3) . . ?
N3 N4 Cu1 122.5(2) . . ?
C6 N5 N6 108.6(3) . . ?
C6 N5 C7 130.3(3) . . ?
N6 N5 C7 121.1(3) . . ?
N7 N6 N5 106.7(3) . . ?
N6 N7 N8 110.0(3) . . ?
C6 N8 N7 106.1(3) . . ?
C6 N8 Cu1 129.1(3) . . ?
N7 N8 Cu1 124.8(2) . . ?
C11 N12 N11 106.6(3) . . ?
C11 N12 Cu1 125.7(3) . . ?
N11 N12 Cu1 127.7(2) . . ?
C16 N13 N14 108.5(3) . . ?
C16 N13 C17 131.8(3) . . ?
N14 N13 C17 119.5(3) . . ?
N15 N14 N13 107.0(3) . . ?
N14 N15 N16 109.5(3) . . ?
C16 N16 N15 106.9(3) . . ?
C16 N16 Cu1 133.0(3) . . ?
N15 N16 Cu1 119.7(2) . . ?
N4 C1 N1 108.7(3) . . ?
N4 C1 H1 125.6 . . ?
N1 C1 H1 125.6 . . ?
N1 C2 C3 118.5(3) . . ?
N1 C2 C5 118.3(3) . . ?
C3 C2 C5 88.8(3) . . ?
N1 C2 H2 109.9 . . ?
C3 C2 H2 109.9 . . ?
C5 C2 H2 109.9 . . ?
C2 C3 C4 88.1(3) . . ?
C2 C3 H3A 114.0 . . ?
C4 C3 H3A 114.0 . . ?
C2 C3 H3B 114.0 . . ?
C4 C3 H3B 114.0 . . ?
H3A C3 H3B 111.2 . . ?
C3 C4 C5 88.4(3) . . ?
C3 C4 H4A 113.9 . . ?
C5 C4 H4A 113.9 . . ?
C3 C4 H4B 113.9 . . ?
C5 C4 H4B 113.9 . . ?
H4A C4 H4B 111.1 . . ?
C2 C5 C4 87.8(3) . . ?
C2 C5 H5A 114.0 . . ?
C4 C5 H5A 114.0 . . ?
C2 C5 H5B 114.0 . . ?
C4 C5 H5B 114.0 . . ?
H5A C5 H5B 111.2 . . ?
N8 C6 N5 108.6(3) . . ?
N8 C6 H6 125.7 . . ?
N5 C6 H6 125.7 . . ?
N5 C7 C10 117.7(3) . . ?
N5 C7 C8 117.9(3) . . ?
C10 C7 C8 88.8(3) . . ?
N5 C7 H7 110.2 . . ?
C10 C7 H7 110.2 . . ?
C8 C7 H7 110.2 . . ?
C9 C8 C7 87.6(3) . . ?
C9 C8 H8A 114.1 . . ?
C7 C8 H8A 114.1 . . ?
C9 C8 H8B 114.1 . . ?
C7 C8 H8B 114.1 . . ?
H8A C8 H8B 111.2 . . ?
C10 C9 C8 88.7(3) . . ?
C10 C9 H9A 113.9 . . ?
C8 C9 H9A 113.9 . . ?
C10 C9 H9B 113.9 . . ?
C8 C9 H9B 113.9 . . ?
H9A C9 H9B 111.1 . . ?
C7 C10 C9 87.8(3) . . ?
C7 C10 H10A 114.0 . . ?
C9 C10 H10A 114.0 . . ?
C7 C10 H10B 114.0 . . ?
C9 C10 H10B 114.0 . . ?
H10A C10 H10B 111.2 . . ?
N16 C16 N13 108.1(3) . . ?
N16 C16 H16 126.0 . . ?
N13 C16 H16 126.0 . . ?
N13 C17 C18 119.6(3) . . ?
N13 C17 C20 117.5(3) . . ?
C18 C17 C20 89.3(3) . . ?
N13 C17 H17 109.7 . . ?
C18 C17 H17 109.7 . . ?
C20 C17 H17 109.7 . . ?
C17 C18 C19 86.6(3) . . ?
C17 C18 H18A 114.2 . . ?
C19 C18 H18A 114.2 . . ?
C17 C18 H18B 114.2 . . ?
C19 C18 H18B 114.2 . . ?
H18A C18 H18B 111.4 . . ?
C18 C19 C20 88.5(3) . . ?
C18 C19 H19A 113.9 . . ?
C20 C19 H19A 113.9 . . ?
C18 C19 H19B 113.9 . . ?
C20 C19 H19B 113.9 . . ?
H19A C19 H19B 111.1 . . ?
C17 C20 C19 85.8(3) . . ?
C17 C20 H20A 114.4 . . ?
C19 C20 H20A 114.4 . . ?
C17 C20 H20B 114.4 . . ?
C19 C20 H20B 114.4 . . ?
H20A C20 H20B 111.5 . . ?
O4A Cl1 O6A 115.6(4) . . ?
O4A Cl1 O5A 113.1(4) . . ?
O6A Cl1 O5A 111.1(3) . . ?
O4A Cl1 O3 106.9(3) . . ?
O6A Cl1 O3 105.7(3) . . ?
O5A Cl1 O3 103.3(3) . . ?
O6B Cl1 O3 124.8(10) . . ?
O6B Cl1 O5B 97.6(16) . . ?
O3 Cl1 O5B 118.0(9) . . ?
O6B Cl1 O4B 102.8(12) . . ?
O3 Cl1 O4B 109.6(5) . . ?
O5B Cl1 O4B 100.6(10) . . ?
O9B Cl2 O8 89.5(12) . . ?
O9B Cl2 O7 132.2(8) . . ?
O8 Cl2 O7 109.0(2) . . ?
O9B Cl2 O10 105.0(10) . . ?
O8 Cl2 O10 108.6(2) . . ?
O7 Cl2 O10 109.5(2) . . ?
O8 Cl2 O9A 114.6(4) . . ?
O7 Cl2 O9A 105.8(3) . . ?
O10 Cl2 O9A 109.1(3) . . ?
C11 N9 N10 108.6(3) . . ?
C11 N9 C12 132.0(3) . . ?
N10 N9 C12 119.0(3) . . ?
N10 N11 N12 110.0(3) . . ?
N11 N10 N9 106.3(3) . . ?
N12 C11 N9 108.5(3) . . ?
N12 C11 H11 125.8 . . ?
N9 C11 H11 125.8 . . ?
N9 C12 C15 116.9(3) . . ?
N9 C12 C13 119.1(3) . . ?
C15 C12 C13 89.9(3) . . ?
N9 C12 H12 109.8 . . ?
C15 C12 H12 109.8 . . ?
C13 C12 H12 109.8 . . ?
C12 C13 C14 86.7(3) . . ?
C12 C13 H13A 114.2 . . ?
C14 C13 H13A 114.2 . . ?
C12 C13 H13B 114.2 . . ?
C14 C13 H13B 114.2 . . ?
H13A C13 H13B 111.4 . . ?
C12 C15 C14 86.6(3) . . ?
C12 C15 H15A 114.2 . . ?
C14 C15 H15A 114.2 . . ?
C12 C15 H15B 114.2 . . ?
C14 C15 H15B 114.2 . . ?
H15A C15 H15B 111.4 . . ?
C13 C14 C15 88.4(3) . . ?
C13 C14 H14A 113.9 . . ?
C15 C14 H14A 113.9 . . ?
C13 C14 H14B 113.9 . . ?
C15 C14 H14B 113.9 . . ?
H14A C14 H14B 111.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -1.2(4) . . . . ?
C2 N1 N2 N3 -178.2(3) . . . . ?
N1 N2 N3 N4 0.3(4) . . . . ?
N2 N3 N4 C1 0.7(4) . . . . ?
N2 N3 N4 Cu1 -171.5(2) . . . . ?
C6 N5 N6 N7 0.1(4) . . . . ?
C7 N5 N6 N7 -179.3(3) . . . . ?
N5 N6 N7 N8 0.0(4) . . . . ?
N6 N7 N8 C6 -0.1(4) . . . . ?
N6 N7 N8 Cu1 179.9(2) . . . . ?
C16 N13 N14 N15 0.2(4) . . . . ?
C17 N13 N14 N15 176.3(3) . . . . ?
N13 N14 N15 N16 -0.4(4) . . . . ?
N14 N15 N16 C16 0.5(4) . . . . ?
N14 N15 N16 Cu1 -173.2(2) . . . . ?
N3 N4 C1 N1 -1.4(4) . . . . ?
Cu1 N4 C1 N1 169.8(3) . . . . ?
N2 N1 C1 N4 1.6(4) . . . . ?
C2 N1 C1 N4 178.3(4) . . . . ?
C1 N1 C2 C3 40.6(6) . . . . ?
N2 N1 C2 C3 -143.1(4) . . . . ?
C1 N1 C2 C5 -64.7(6) . . . . ?
N2 N1 C2 C5 111.6(4) . . . . ?
N1 C2 C3 C4 -141.7(4) . . . . ?
C5 C2 C3 C4 -19.8(3) . . . . ?
C2 C3 C4 C5 19.7(4) . . . . ?
N1 C2 C5 C4 141.7(4) . . . . ?
C3 C2 C5 C4 19.8(3) . . . . ?
C3 C4 C5 C2 -19.7(4) . . . . ?
N7 N8 C6 N5 0.2(4) . . . . ?
Cu1 N8 C6 N5 -179.8(2) . . . . ?
N6 N5 C6 N8 -0.2(4) . . . . ?
C7 N5 C6 N8 179.1(3) . . . . ?
C6 N5 C7 C10 -67.0(6) . . . . ?
N6 N5 C7 C10 112.2(4) . . . . ?
C6 N5 C7 C8 37.6(6) . . . . ?
N6 N5 C7 C8 -143.2(4) . . . . ?
N5 C7 C8 C9 -140.9(4) . . . . ?
C10 C7 C8 C9 -19.9(3) . . . . ?
C7 C8 C9 C10 19.8(3) . . . . ?
N5 C7 C10 C9 141.1(4) . . . . ?
C8 C7 C10 C9 19.9(3) . . . . ?
C8 C9 C10 C7 -19.9(3) . . . . ?
N15 N16 C16 N13 -0.4(4) . . . . ?
Cu1 N16 C16 N13 172.1(3) . . . . ?
N14 N13 C16 N16 0.1(4) . . . . ?
C17 N13 C16 N16 -175.4(4) . . . . ?
C16 N13 C17 C18 -18.5(6) . . . . ?
N14 N13 C17 C18 166.4(4) . . . . ?
C16 N13 C17 C20 87.6(5) . . . . ?
N14 N13 C17 C20 -87.5(5) . . . . ?
N13 C17 C18 C19 145.1(4) . . . . ?
C20 C17 C18 C19 23.6(3) . . . . ?
C17 C18 C19 C20 -23.4(3) . . . . ?
N13 C17 C20 C19 -146.8(4) . . . . ?
C18 C17 C20 C19 -23.4(3) . . . . ?
C18 C19 C20 C17 23.2(3) . . . . ?
C11 N12 N11 N10 -0.2(4) . . . . ?
Cu1 N12 N11 N10 178.3(2) . . . . ?
N12 N11 N10 N9 0.1(4) . . . . ?
C11 N9 N10 N11 0.0(4) . . . . ?
C12 N9 N10 N11 173.2(3) . . . . ?
N11 N12 C11 N9 0.2(4) . . . . ?
Cu1 N12 C11 N9 -178.3(2) . . . . ?
N10 N9 C11 N12 -0.1(4) . . . . ?
C12 N9 C11 N12 -172.1(3) . . . . ?
C11 N9 C12 C15 88.4(5) . . . . ?
N10 N9 C12 C15 -83.0(4) . . . . ?
C11 N9 C12 C13 -17.8(6) . . . . ?
N10 N9 C12 C13 170.8(3) . . . . ?
N9 C12 C13 C14 142.9(3) . . . . ?
C15 C12 C13 C14 21.8(3) . . . . ?
N9 C12 C15 C14 -144.7(3) . . . . ?
C13 C12 C15 C14 -21.8(3) . . . . ?
C12 C13 C14 C15 -21.5(3) . . . . ?
C12 C15 C14 C13 21.5(3) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?




_refine_diff_density_max         0.542
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.095

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px224
_database_code_depnum_ccdc_archive 'CCDC 2061079'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-11
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'dinitrato tetrakis(1-cyclobutyl-5H-tetrazolyl) copper(II)'
_chemical_name_common            
'dinitrato tetrakis(1-cyclobutyl-5H-tetrazolyl) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 Cl2 Cu N16 O6'
_chemical_formula_sum            'C20 H32 Cl2 Cu N16 O6'
_chemical_formula_weight         727.05

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.7946(4)
_cell_length_b                   18.1424(12)
_cell_length_c                   12.4720(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.844(6)
_cell_angle_gamma                90
_cell_volume                     1526.47(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2648
_cell_measurement_theta_min      2.7690
_cell_measurement_theta_max      31.2080

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.408
_exptl_crystal_size_min          0.154
_exptl_absorpt_coefficient_mu    0.956
_shelx_estimated_absorpt_T_min   0.530
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_F_000             750
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            10086
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.991
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3135
_reflns_number_gt                2587
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0358P)²+0.7271P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3135
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0883964000
_diffrn_orient_matrix_UB_12      0.0007939000
_diffrn_orient_matrix_UB_13      -0.0249934000
_diffrn_orient_matrix_UB_21      -0.0287224000
_diffrn_orient_matrix_UB_22      0.0343403000
_diffrn_orient_matrix_UB_23      -0.0242268000
_diffrn_orient_matrix_UB_31      0.0491187000
_diffrn_orient_matrix_UB_32      0.0186562000
_diffrn_orient_matrix_UB_33      0.0455206000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  22.00   1.00   40.00    --  -28.70 -19.00 -30.00  106
  2  ω     67.00 112.00   1.00   40.00    --   29.64-178.00-180.00   45
  3  ω    -41.00  53.00   1.00   40.00    --   29.64 -57.00 150.00   94
  4  ω     22.00  74.00   1.00   40.00    --   29.64 -99.00 -30.00   52
  5  ω      6.00  98.00   1.00   40.00    --   29.64  57.00 -60.00   92
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.000000 0.500000 0.500000 0.01378(11) Uani 1 2 d S . P . .
Cl1 Cl 0.65926(8) 0.62324(3) 0.39087(4) 0.01851(13) Uani 1 1 d . . . . .
O2 O 0.5007(2) 0.67446(9) 0.41566(13) 0.0229(4) Uani 1 1 d . . . . .
O1 O 0.6974(2) 0.57159(8) 0.48485(12) 0.0204(4) Uani 1 1 d . . . . .
O3 O 0.5782(3) 0.57823(10) 0.29678(13) 0.0306(4) Uani 1 1 d . . . . .
N1 N 0.9617(3) 0.47705(10) 0.65525(14) 0.0152(4) Uani 1 1 d . . . . .
N5 N 0.8316(3) 0.41313(10) 0.44945(14) 0.0153(4) Uani 1 1 d . . . . .
N4 N 0.8819(3) 0.42886(10) 0.80113(14) 0.0158(4) Uani 1 1 d . . . . .
N2 N 1.0422(3) 0.51767(10) 0.74233(14) 0.0196(4) Uani 1 1 d . . . . .
N8 N 0.6302(3) 0.34257(10) 0.35294(14) 0.0167(4) Uani 1 1 d . . . . .
N3 N 0.9949(3) 0.48905(10) 0.83004(14) 0.0199(4) Uani 1 1 d . . . . .
N6 N 0.8955(3) 0.34212(10) 0.46151(15) 0.0195(4) Uani 1 1 d . . . . .
N7 N 0.7739(3) 0.29947(10) 0.40336(15) 0.0211(4) Uani 1 1 d . . . . .
C1 C 0.8637(3) 0.42269(12) 0.69437(17) 0.0157(4) Uani 1 1 d . . . . .
C6 C 0.6653(3) 0.41160(13) 0.38279(17) 0.0172(4) Uani 1 1 d . . . . .
C2 C 0.7950(3) 0.38399(13) 0.88098(18) 0.0194(5) Uani 1 1 d . . . . .
C7 C 0.4723(3) 0.30876(13) 0.27754(18) 0.0195(5) Uani 1 1 d . . . . .
C5 C 0.9266(4) 0.36182(15) 0.98449(19) 0.0251(5) Uani 1 1 d . . . . .
C9 C 0.1649(4) 0.29710(16) 0.2307(2) 0.0319(6) Uani 1 1 d . . . . .
C4 C 0.7389(4) 0.36877(15) 1.0427(2) 0.0310(6) Uani 1 1 d . . . . .
C3 C 0.6502(4) 0.41980(16) 0.9506(2) 0.0284(6) Uani 1 1 d . . . . .
C8 C 0.3147(4) 0.36018(16) 0.2210(3) 0.0341(6) Uani 1 1 d . . . . .
C10 C 0.3086(4) 0.26499(17) 0.3237(2) 0.0295(6) Uani 1 1 d . . . . .
H5A H 1.014(3) 0.3995(14) 1.0050(18) 0.019(6) Uiso 1 1 d . . . . .
H2 H 0.741(3) 0.3436(12) 0.8439(18) 0.009(5) Uiso 1 1 d . . . . .
H6 H 0.585(3) 0.4529(14) 0.3621(19) 0.019(6) Uiso 1 1 d . . . . .
H3A H 0.688(4) 0.4690(16) 0.964(2) 0.028(7) Uiso 1 1 d . . . . .
H7 H 0.539(4) 0.2784(15) 0.224(2) 0.032(7) Uiso 1 1 d . . . . .
H3B H 0.517(4) 0.4144(14) 0.927(2) 0.026(7) Uiso 1 1 d . . . . .
H4A H 0.667(4) 0.3230(15) 1.039(2) 0.032(7) Uiso 1 1 d . . . . .
H5B H 0.990(4) 0.3139(15) 0.982(2) 0.026(7) Uiso 1 1 d . . . . .
H10A H 0.328(4) 0.2123(16) 0.329(2) 0.028(7) Uiso 1 1 d . . . . .
H10B H 0.282(4) 0.2809(15) 0.388(2) 0.030(7) Uiso 1 1 d . . . . .
H1 H 0.792(4) 0.3859(14) 0.657(2) 0.022(6) Uiso 1 1 d . . . . .
H8A H 0.292(4) 0.4011(18) 0.272(3) 0.051(9) Uiso 1 1 d . . . . .
H9A H 0.149(3) 0.2660(14) 0.171(2) 0.022(6) Uiso 1 1 d . . . . .
H8B H 0.336(5) 0.3778(18) 0.153(3) 0.059(10) Uiso 1 1 d . . . . .
H9B H 0.033(4) 0.3101(15) 0.246(2) 0.032(7) Uiso 1 1 d . . . . .
H4B H 0.753(4) 0.3885(15) 1.109(2) 0.034(8) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N5 2.0047(17) . ?
Cu1 N5 2.0047(17) 3_766 ?
Cu1 N1 2.0274(17) 3_766 ?
Cu1 N1 2.0274(17) . ?
Cu1 O1 2.4201(15) 3_766 ?
Cu1 O1 2.4201(15) . ?
Cl1 O3 1.4807(17) . ?
Cl1 O2 1.4832(16) . ?
Cl1 O1 1.4988(15) . ?
N1 C1 1.316(3) . ?
N1 N2 1.371(2) . ?
N5 C6 1.321(3) . ?
N5 N6 1.362(2) . ?
N4 C1 1.327(3) . ?
N4 N3 1.359(2) . ?
N4 C2 1.464(3) . ?
N2 N3 1.286(3) . ?
N8 C6 1.320(3) . ?
N8 N7 1.347(3) . ?
N8 C7 1.474(3) . ?
N6 N7 1.290(3) . ?
C1 H1 0.92(3) . ?
C6 H6 0.94(2) . ?
C2 C3 1.532(3) . ?
C2 C5 1.534(3) . ?
C2 H2 0.92(2) . ?
C7 C8 1.528(3) . ?
C7 C10 1.533(3) . ?
C7 H7 1.01(3) . ?
C5 C4 1.546(4) . ?
C5 H5A 0.92(3) . ?
C5 H5B 0.97(3) . ?
C9 C10 1.539(4) . ?
C9 C8 1.546(4) . ?
C9 H9A 0.93(3) . ?
C9 H9B 0.96(3) . ?
C4 C3 1.541(4) . ?
C4 H4A 0.96(3) . ?
C4 H4B 0.90(3) . ?
C3 H3A 0.94(3) . ?
C3 H3B 0.92(3) . ?
C8 H8A 1.00(3) . ?
C8 H8B 0.94(3) . ?
C10 H10A 0.97(3) . ?
C10 H10B 0.89(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Cu1 N5 180.0 . 3_766 ?
N5 Cu1 N1 89.68(7) . 3_766 ?
N5 Cu1 N1 90.31(7) 3_766 3_766 ?
N5 Cu1 N1 90.31(7) . . ?
N5 Cu1 N1 89.69(7) 3_766 . ?
N1 Cu1 N1 180.0 3_766 . ?
N5 Cu1 O1 92.89(6) . 3_766 ?
N5 Cu1 O1 87.11(6) 3_766 3_766 ?
N1 Cu1 O1 88.87(6) 3_766 3_766 ?
N1 Cu1 O1 91.13(6) . 3_766 ?
N5 Cu1 O1 87.11(6) . . ?
N5 Cu1 O1 92.89(6) 3_766 . ?
N1 Cu1 O1 91.13(6) 3_766 . ?
N1 Cu1 O1 88.87(6) . . ?
O1 Cu1 O1 180.00(4) 3_766 . ?
O3 Cl1 O2 107.45(9) . . ?
O3 Cl1 O1 106.76(10) . . ?
O2 Cl1 O1 106.91(9) . . ?
Cl1 O1 Cu1 117.56(8) . . ?
C1 N1 N2 106.33(17) . . ?
C1 N1 Cu1 129.50(15) . . ?
N2 N1 Cu1 124.16(14) . . ?
C6 N5 N6 106.70(18) . . ?
C6 N5 Cu1 128.89(15) . . ?
N6 N5 Cu1 123.10(13) . . ?
C1 N4 N3 108.45(18) . . ?
C1 N4 C2 129.67(19) . . ?
N3 N4 C2 121.83(17) . . ?
N3 N2 N1 109.88(17) . . ?
C6 N8 N7 108.81(17) . . ?
C6 N8 C7 131.93(19) . . ?
N7 N8 C7 119.25(18) . . ?
N2 N3 N4 106.82(17) . . ?
N7 N6 N5 109.31(17) . . ?
N6 N7 N8 107.12(17) . . ?
N1 C1 N4 108.52(19) . . ?
N1 C1 H1 128.3(16) . . ?
N4 C1 H1 123.2(16) . . ?
N8 C6 N5 108.1(2) . . ?
N8 C6 H6 126.6(14) . . ?
N5 C6 H6 125.3(14) . . ?
N4 C2 C3 119.2(2) . . ?
N4 C2 C5 118.5(2) . . ?
C3 C2 C5 89.06(18) . . ?
N4 C2 H2 105.6(14) . . ?
C3 C2 H2 112.4(14) . . ?
C5 C2 H2 111.8(14) . . ?
N8 C7 C8 117.23(19) . . ?
N8 C7 C10 118.79(19) . . ?
C8 C7 C10 89.4(2) . . ?
N8 C7 H7 107.3(15) . . ?
C8 C7 H7 111.9(15) . . ?
C10 C7 H7 111.5(15) . . ?
C2 C5 C4 86.73(19) . . ?
C2 C5 H5A 109.3(15) . . ?
C4 C5 H5A 110.5(15) . . ?
C2 C5 H5B 114.9(15) . . ?
C4 C5 H5B 118.9(15) . . ?
H5A C5 H5B 114(2) . . ?
C10 C9 C8 88.54(19) . . ?
C10 C9 H9A 112.1(15) . . ?
C8 C9 H9A 113.4(15) . . ?
C10 C9 H9B 117.9(16) . . ?
C8 C9 H9B 117.9(16) . . ?
H9A C9 H9B 107(2) . . ?
C3 C4 C5 88.30(19) . . ?
C3 C4 H4A 109.6(16) . . ?
C5 C4 H4A 110.7(16) . . ?
C3 C4 H4B 116.0(18) . . ?
C5 C4 H4B 117.5(18) . . ?
H4A C4 H4B 112(2) . . ?
C2 C3 C4 87.0(2) . . ?
C2 C3 H3A 108.8(17) . . ?
C4 C3 H3A 111.4(16) . . ?
C2 C3 H3B 116.5(16) . . ?
C4 C3 H3B 117.1(16) . . ?
H3A C3 H3B 113(2) . . ?
C7 C8 C9 86.8(2) . . ?
C7 C8 H8A 108.0(17) . . ?
C9 C8 H8A 110.3(18) . . ?
C7 C8 H8B 117(2) . . ?
C9 C8 H8B 120(2) . . ?
H8A C8 H8B 112(3) . . ?
C7 C10 C9 86.8(2) . . ?
C7 C10 H10A 115.8(16) . . ?
C9 C10 H10A 119.6(15) . . ?
C7 C10 H10B 113.8(17) . . ?
C9 C10 H10B 112.2(18) . . ?
H10A C10 H10B 108(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Cl1 O1 Cu1 80.82(11) . . . . ?
O2 Cl1 O1 Cu1 -164.41(9) . . . . ?
C1 N1 N2 N3 0.0(2) . . . . ?
Cu1 N1 N2 N3 -178.92(14) . . . . ?
N1 N2 N3 N4 0.0(2) . . . . ?
C1 N4 N3 N2 0.0(2) . . . . ?
C2 N4 N3 N2 -177.66(19) . . . . ?
C6 N5 N6 N7 0.7(2) . . . . ?
Cu1 N5 N6 N7 -167.23(14) . . . . ?
N5 N6 N7 N8 0.1(2) . . . . ?
C6 N8 N7 N6 -0.9(2) . . . . ?
C7 N8 N7 N6 178.09(18) . . . . ?
N2 N1 C1 N4 -0.1(2) . . . . ?
Cu1 N1 C1 N4 178.82(14) . . . . ?
N3 N4 C1 N1 0.1(2) . . . . ?
C2 N4 C1 N1 177.4(2) . . . . ?
N7 N8 C6 N5 1.4(2) . . . . ?
C7 N8 C6 N5 -177.4(2) . . . . ?
N6 N5 C6 N8 -1.3(2) . . . . ?
Cu1 N5 C6 N8 165.73(14) . . . . ?
C1 N4 C2 C3 -116.8(3) . . . . ?
N3 N4 C2 C3 60.3(3) . . . . ?
C1 N4 C2 C5 136.8(2) . . . . ?
N3 N4 C2 C5 -46.1(3) . . . . ?
C6 N8 C7 C8 -0.2(4) . . . . ?
N7 N8 C7 C8 -179.0(2) . . . . ?
C6 N8 C7 C10 -105.9(3) . . . . ?
N7 N8 C7 C10 75.3(3) . . . . ?
N4 C2 C5 C4 145.5(2) . . . . ?
C3 C2 C5 C4 22.39(19) . . . . ?
C2 C5 C4 C3 -22.26(19) . . . . ?
N4 C2 C3 C4 -144.9(2) . . . . ?
C5 C2 C3 C4 -22.46(19) . . . . ?
C5 C4 C3 C2 22.28(19) . . . . ?
N8 C7 C8 C9 -144.2(2) . . . . ?
C10 C7 C8 C9 -21.8(2) . . . . ?
C10 C9 C8 C7 21.7(2) . . . . ?
N8 C7 C10 C9 143.0(2) . . . . ?
C8 C7 C10 C9 21.9(2) . . . . ?
C8 C9 C10 C7 -21.6(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.383
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.065

_shelxl_version_number           ?





####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px
_database_code_depnum_ccdc_archive 'CCDC 2061083'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-10-02
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) zinc(II) diperchlorate'
_chemical_name_common            
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) zinc(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H44 N16 O2 Zn, 2(Cl O4)'
_chemical_formula_sum            'C24 H44 Cl2 N16 O10 Zn'
_chemical_formula_weight         853.02

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9914(8)
_cell_length_b                   11.9384(9)
_cell_length_c                   14.9946(11)
_cell_angle_alpha                112.552(7)
_cell_angle_beta                 90.350(6)
_cell_angle_gamma                96.674(6)
_cell_volume                     1802.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    3597
_cell_measurement_theta_min      2.4490
_cell_measurement_theta_max      30.8320

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.905
_shelx_estimated_absorpt_T_min   0.742
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      101(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            16058
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.862
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7369
_reflns_number_gt                5411
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0960P)²+3.5349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7369
_refine_ls_number_parameters     493
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1950
_refine_ls_wR_factor_gt          0.1702
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0034480000
_diffrn_orient_matrix_UB_12      0.0416216000
_diffrn_orient_matrix_UB_13      0.0489808000
_diffrn_orient_matrix_UB_21      -0.0649300000
_diffrn_orient_matrix_UB_22      -0.0080727000
_diffrn_orient_matrix_UB_23      0.0003613000
_diffrn_orient_matrix_UB_31      0.0025606000
_diffrn_orient_matrix_UB_32      -0.0490976000
_diffrn_orient_matrix_UB_33      0.0152421000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00 -39.00   1.00   22.00    --  -23.68-178.00 -60.00   30
  2  ω    -31.00  -4.00   1.00   22.00    --   24.78 131.00  43.38   27
  3  ω    -39.00  -3.00   1.00   22.00    --   24.78 -77.00-150.00   36
  4  ω     53.00  94.00   1.00   22.00    --   24.78 178.00 150.00   41
  5  ω    -20.00  64.00   1.00   22.00    --   24.78 -99.00 150.00   84
  6  ω    -29.00  -3.00   1.00   22.00    --   24.78 126.00 -69.56   26
  7  ω    -43.00  37.00   1.00   22.00    --   24.78 -37.00-120.00   80
  8  ω     20.00  52.00   1.00   22.00    --   24.78 -77.00-150.00   32
  9  ω    -20.00  12.00   1.00   22.00    --   24.78 -57.00-150.00   32
 10  ω      9.00  92.00   1.00   22.00    --   24.78  57.00   0.00   83
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.500000 1.000000 0.500000 0.01741(19) Uani 1 2 d S . P . .
O1 O 0.6029(3) 0.8608(3) 0.4969(3) 0.0241(7) Uani 1 1 d . . . . .
N1 N 0.1746(3) 0.9138(3) 0.6324(3) 0.0194(8) Uani 1 1 d . . . . .
N2 N 0.2027(4) 0.7991(3) 0.5869(3) 0.0244(8) Uani 1 1 d . . . . .
N3 N 0.3041(3) 0.8089(3) 0.5452(3) 0.0222(8) Uani 1 1 d . . . . .
N4 N 0.3425(3) 0.9279(3) 0.5610(3) 0.0188(7) Uani 1 1 d . . . . .
N5 N 0.3645(3) 0.8306(3) 0.2055(3) 0.0236(8) Uani 1 1 d . . . . .
N6 N 0.2891(4) 0.7721(4) 0.2493(3) 0.0322(10) Uani 1 1 d . . . . .
N7 N 0.3287(4) 0.8136(4) 0.3389(3) 0.0281(9) Uani 1 1 d . . . . .
N8 N 0.4283(3) 0.9002(3) 0.3552(3) 0.0208(8) Uani 1 1 d . . . . .
C1 C 0.2603(4) 0.9907(4) 0.6156(3) 0.0212(9) Uani 1 1 d . . . . .
H1A H 0.262063 1.076954 0.639118 0.025 Uiso 1 1 calc R U . . .
C2 C 0.0644(4) 0.9346(4) 0.6894(3) 0.0252(10) Uani 1 1 d . . . . .
H2A H 0.061020 0.887955 0.732485 0.030 Uiso 1 1 calc R U . . .
C3 C 0.0629(5) 1.0706(4) 0.7496(4) 0.0316(11) Uani 1 1 d . . . . .
H3A H 0.019472 1.082454 0.809589 0.038 Uiso 1 1 calc R U . . .
H3B H 0.147587 1.113459 0.767312 0.038 Uiso 1 1 calc R U . . .
C4 C -0.0046(5) 1.1184(5) 0.6851(5) 0.0449(15) Uani 1 1 d . . . . .
H4A H 0.047212 1.127884 0.634017 0.054 Uiso 1 1 calc R U . A 1
H4B H -0.035193 1.196889 0.722836 0.054 Uiso 1 1 calc R U . A 1
C6 C -0.0528(5) 0.8972(5) 0.6232(4) 0.0363(12) Uani 1 1 d . . . . .
H6A H -0.031719 0.862032 0.554724 0.044 Uiso 1 1 calc R U . B 1
H6B H -0.107715 0.834407 0.636663 0.044 Uiso 1 1 calc R U . B 1
C7 C 0.4481(4) 0.9071(4) 0.2704(3) 0.0235(9) Uani 1 1 d . . . . .
H7 H 0.512284 0.959024 0.258174 0.028 Uiso 1 1 calc R U . . .
C8 C 0.3461(5) 0.8022(5) 0.0996(3) 0.0321(11) Uani 1 1 d . . . . .
H8 H 0.391457 0.868218 0.082538 0.039 Uiso 1 1 calc R U . . .
C9 C 0.2127(6) 0.7829(6) 0.0685(4) 0.0449(14) Uani 1 1 d . . . . .
H9A H 0.199860 0.813842 0.017103 0.054 Uiso 1 1 calc R U . . .
H9B H 0.163484 0.824822 0.123808 0.054 Uiso 1 1 calc R U . . .
C10 C 0.1779(13) 0.6448(11) 0.0307(8) 0.130(6) Uani 1 1 d . . . . .
H10A H 0.112689 0.624542 0.069280 0.156 Uiso 1 1 calc R U . . .
H10B H 0.145792 0.613967 -0.037440 0.156 Uiso 1 1 calc R U . . .
C11 C 0.279(2) 0.5895(8) 0.0366(7) 0.147(8) Uani 1 1 d . . . . .
H11A H 0.279972 0.512293 -0.020526 0.176 Uiso 1 1 calc R U . . .
H11B H 0.279651 0.571316 0.095689 0.176 Uiso 1 1 calc R U . . .
C12 C 0.3862(9) 0.6790(10) 0.0399(5) 0.096(4) Uani 1 1 d . . . . .
H12A H 0.405332 0.673538 -0.025927 0.115 Uiso 1 1 calc R U . . .
H12B H 0.459442 0.665156 0.071127 0.115 Uiso 1 1 calc R U . . .
Zn2 Zn 0.500000 0.500000 0.500000 0.01881(19) Uani 1 2 d S . P . .
O2 O 0.4329(3) 0.6141(3) 0.4374(3) 0.0222(7) Uani 1 1 d . . . . .
N9 N 0.3551(3) 0.2380(3) 0.2194(3) 0.0223(8) Uani 1 1 d . . . . .
N10 N 0.3491(4) 0.1633(3) 0.2677(3) 0.0257(8) Uani 1 1 d . . . . .
N11 N 0.3992(4) 0.2270(3) 0.3532(3) 0.0222(8) Uani 1 1 d . . . . .
N12 N 0.4376(3) 0.3437(3) 0.3628(3) 0.0210(8) Uani 1 1 d . . . . .
N13 N 0.8356(4) 0.4869(3) 0.3631(3) 0.0268(9) Uani 1 1 d . . . . .
N14 N 0.8583(4) 0.5996(3) 0.4357(3) 0.0286(9) Uani 1 1 d . . . . .
N15 N 0.7603(4) 0.6175(3) 0.4831(3) 0.0261(9) Uani 1 1 d . . . . .
N16 N 0.6731(3) 0.5171(3) 0.4433(3) 0.0213(8) Uani 1 1 d . . . . .
C13 C 0.4105(4) 0.3472(4) 0.2781(3) 0.0231(9) Uani 1 1 d . . . . .
H13 H 0.427642 0.416529 0.261673 0.028 Uiso 1 1 calc R U . . .
C14 C 0.3065(5) 0.1937(5) 0.1175(4) 0.0337(12) Uani 1 1 d . . . . .
H14 H 0.361147 0.133416 0.078772 0.040 Uiso 1 1 calc R U . C 1
C15 C 0.1791(5) 0.1227(5) 0.1023(4) 0.0377(12) Uani 1 1 d . . . . .
H15A H 0.183610 0.033597 0.075000 0.045 Uiso 1 1 calc R U . . .
H15B H 0.138271 0.144205 0.164250 0.045 Uiso 1 1 calc R U . . .
C16 C 0.1097(6) 0.1584(8) 0.0326(6) 0.065(2) Uani 1 1 d . . . . .
H16A H 0.084052 0.085722 -0.027227 0.078 Uiso 1 1 calc R U . . .
H16B H 0.035371 0.193552 0.061981 0.078 Uiso 1 1 calc R U . . .
C17 C 0.1913(8) 0.2491(8) 0.0102(7) 0.084(3) Uani 1 1 d . . . . .
H17A H 0.149379 0.321834 0.020534 0.100 Uiso 1 1 calc R U . D 1
H17B H 0.211476 0.214072 -0.058555 0.100 Uiso 1 1 calc R U . D 1
C19 C 0.7232(4) 0.4386(4) 0.3698(3) 0.0242(10) Uani 1 1 d . . . . .
H19 H 0.684770 0.360071 0.328246 0.029 Uiso 1 1 calc R U . . .
C20 C 0.9243(5) 0.4343(5) 0.2878(4) 0.0400(13) Uani 1 1 d . . . . .
H20 H 0.881508 0.363792 0.231503 0.048 Uiso 1 1 calc R U . . .
C21 C 1.0253(6) 0.3936(5) 0.3312(5) 0.0453(15) Uani 1 1 d . . . . .
H21A H 0.993233 0.359681 0.378410 0.054 Uiso 1 1 calc R U . . .
H21B H 1.065286 0.330671 0.280395 0.054 Uiso 1 1 calc R U . . .
C22 C 1.1116(5) 0.5048(5) 0.3791(4) 0.0409(13) Uani 1 1 d . . . . .
H22A H 1.195578 0.483753 0.382399 0.049 Uiso 1 1 calc R U . . .
H22B H 1.087808 0.549807 0.445766 0.049 Uiso 1 1 calc R U . . .
C23 C 1.1071(5) 0.5838(5) 0.3186(4) 0.0364(12) Uani 1 1 d . . . . .
H23A H 1.104928 0.670544 0.361377 0.044 Uiso 1 1 calc R U . . .
H23B H 1.180206 0.578409 0.279670 0.044 Uiso 1 1 calc R U . . .
C24 C 0.9908(5) 0.5339(5) 0.2529(4) 0.0380(12) Uani 1 1 d . . . . .
H24A H 1.010688 0.496496 0.184208 0.046 Uiso 1 1 calc R U . . .
H24B H 0.939064 0.599231 0.260821 0.046 Uiso 1 1 calc R U . . .
Cl2 Cl 0.63194(11) 0.63298(10) 0.23744(8) 0.0263(3) Uani 1 1 d . . . . .
O7 O 0.5032(3) 0.6161(3) 0.2568(3) 0.0369(8) Uani 1 1 d . . . . .
O8 O 0.6766(4) 0.5166(3) 0.2014(3) 0.0479(11) Uani 1 1 d . . . . .
O9 O 0.6456(4) 0.6887(4) 0.1698(3) 0.0500(11) Uani 1 1 d . . . . .
O10 O 0.7006(3) 0.7115(3) 0.3279(3) 0.0355(8) Uani 1 1 d . . . . .
Cl1 Cl 0.67163(11) 0.10205(10) 0.14848(8) 0.0290(3) Uani 1 1 d . . . . .
O3 O 0.7980(4) 0.1437(4) 0.1469(3) 0.0489(10) Uani 1 1 d . . . . .
C5A C -0.1157(9) 1.0066(8) 0.6410(7) 0.032(2) Uiso 0.542(9) 1 d . . P E 1
H5A1 H -0.180085 1.012843 0.687968 0.038 Uiso 0.542(9) 1 calc R U P E 1
H5A2 H -0.153017 1.005027 0.580244 0.038 Uiso 0.542(9) 1 calc R U P E 1
C18A C 0.3138(13) 0.2885(11) 0.0773(9) 0.046(3) Uiso 0.542(9) 1 d . . P E 1
H18A H 0.387326 0.287197 0.039359 0.055 Uiso 0.542(9) 1 calc R U P E 1
H18B H 0.314706 0.370956 0.128862 0.055 Uiso 0.542(9) 1 calc R U P E 1
O4A O 0.6239(6) 0.1495(5) 0.2446(4) 0.0274(17) Uiso 0.542(9) 1 d . . P E 1
O5A O 0.6544(11) -0.0321(11) 0.1254(9) 0.081(3) Uiso 0.542(9) 1 d . . P E 1
O6A O 0.5969(12) 0.1239(13) 0.0826(10) 0.095(4) Uiso 0.542(9) 1 d . . P E 1
C5B C -0.0539(13) 1.0132(12) 0.5944(10) 0.047(3) Uiso 0.458(9) 1 d . . P E 2
H5B1 H -0.000824 1.007098 0.540096 0.056 Uiso 0.458(9) 1 calc R U P E 2
H5B2 H -0.138218 1.021258 0.576172 0.056 Uiso 0.458(9) 1 calc R U P E 2
C18B C 0.2697(10) 0.3105(9) 0.0959(7) 0.019(2) Uiso 0.458(9) 1 d . . P E 2
H18C H 0.225544 0.364715 0.149546 0.023 Uiso 0.458(9) 1 calc R U P E 2
H18D H 0.342789 0.358664 0.084114 0.023 Uiso 0.458(9) 1 calc R U P E 2
O4B O 0.6155(13) 0.2007(13) 0.2048(10) 0.089(4) Uiso 0.458(9) 1 d . . P E 2
O5B O 0.6747(10) 0.0050(10) 0.1827(9) 0.060(3) Uiso 0.458(9) 1 d . . P E 2
O6B O 0.6186(9) 0.0517(9) 0.0526(7) 0.046(3) Uiso 0.458(9) 1 d . . P E 2
H2B H 0.390(5) 0.679(5) 0.478(4) 0.024(13) Uiso 1 1 d . . . . .
H2C H 0.455(5) 0.620(5) 0.395(4) 0.024(16) Uiso 1 1 d . . . . .
H1C H 0.594(6) 0.841(6) 0.549(5) 0.053(19) Uiso 1 1 d . . . . .
H1B H 0.620(5) 0.828(5) 0.457(4) 0.022(18) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.103(3) . ?
Zn1 O1 2.103(3) 2_676 ?
Zn1 N8 2.129(4) . ?
Zn1 N8 2.129(4) 2_676 ?
Zn1 N4 2.203(3) . ?
Zn1 N4 2.203(3) 2_676 ?
O1 H1C 0.90(7) . ?
O1 H1B 0.62(6) . ?
N1 C1 1.332(5) . ?
N1 N2 1.349(5) . ?
N1 C2 1.476(6) . ?
N2 N3 1.296(5) . ?
N3 N4 1.362(5) . ?
N4 C1 1.320(6) . ?
N5 C7 1.318(6) . ?
N5 N6 1.352(5) . ?
N5 C8 1.498(6) . ?
N6 N7 1.293(5) . ?
N7 N8 1.366(5) . ?
N8 C7 1.323(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.527(6) . ?
C2 C6 1.534(7) . ?
C2 H2A 1.0000 . ?
C3 C4 1.525(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5B 1.498(14) . ?
C4 C5A 1.626(11) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C5A 1.483(11) . ?
C6 C5B 1.602(14) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C8 C9 1.501(8) . ?
C8 C12 1.518(10) . ?
C8 H8 1.0000 . ?
C9 C10 1.523(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.377(19) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.481(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Zn2 N16 2.109(4) . ?
Zn2 N16 2.109(4) 2_666 ?
Zn2 O2 2.118(3) . ?
Zn2 O2 2.118(3) 2_666 ?
Zn2 N12 2.219(4) 2_666 ?
Zn2 N12 2.219(4) . ?
O2 H2B 0.96(6) . ?
O2 H2C 0.70(5) . ?
N9 C13 1.332(6) . ?
N9 N10 1.343(5) . ?
N9 C14 1.485(6) . ?
N10 N11 1.294(5) . ?
N11 N12 1.360(5) . ?
N12 C13 1.320(6) . ?
N13 C19 1.322(6) . ?
N13 N14 1.361(5) . ?
N13 C20 1.494(7) . ?
N14 N15 1.287(5) . ?
N15 N16 1.375(5) . ?
N16 C19 1.315(6) . ?
C13 H13 0.9500 . ?
C14 C18A 1.468(12) . ?
C14 C15 1.518(7) . ?
C14 C18B 1.641(11) . ?
C14 H14 1.0000 . ?
C15 C16 1.503(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.466(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18B 1.431(13) . ?
C17 C18A 1.587(15) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C19 H19 0.9500 . ?
C20 C21 1.500(8) . ?
C20 C24 1.582(8) . ?
C20 H20 1.0000 . ?
C21 C22 1.464(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.544(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.521(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
Cl2 O9 1.412(4) . ?
Cl2 O8 1.432(4) . ?
Cl2 O7 1.453(4) . ?
Cl2 O10 1.461(4) . ?
Cl1 O4B 1.376(15) . ?
Cl1 O6A 1.399(13) . ?
Cl1 O6B 1.419(9) . ?
Cl1 O3 1.423(4) . ?
Cl1 O5B 1.440(11) . ?
Cl1 O4A 1.458(6) . ?
Cl1 O5A 1.491(11) . ?
C5A H5A1 0.9900 . ?
C5A H5A2 0.9900 . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C5B H5B1 0.9900 . ?
C5B H5B2 0.9900 . ?
C18B H18C 0.9900 . ?
C18B H18D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 180.0 . 2_676 ?
O1 Zn1 N8 92.55(15) . . ?
O1 Zn1 N8 87.45(15) 2_676 . ?
O1 Zn1 N8 87.45(15) . 2_676 ?
O1 Zn1 N8 92.55(15) 2_676 2_676 ?
N8 Zn1 N8 180.0 . 2_676 ?
O1 Zn1 N4 92.84(14) . . ?
O1 Zn1 N4 87.16(14) 2_676 . ?
N8 Zn1 N4 92.87(13) . . ?
N8 Zn1 N4 87.13(13) 2_676 . ?
O1 Zn1 N4 87.16(14) . 2_676 ?
O1 Zn1 N4 92.84(14) 2_676 2_676 ?
N8 Zn1 N4 87.13(13) . 2_676 ?
N8 Zn1 N4 92.87(13) 2_676 2_676 ?
N4 Zn1 N4 180.0 . 2_676 ?
Zn1 O1 H1C 113(4) . . ?
Zn1 O1 H1B 117(5) . . ?
H1C O1 H1B 127(7) . . ?
C1 N1 N2 108.3(3) . . ?
C1 N1 C2 131.8(4) . . ?
N2 N1 C2 119.9(3) . . ?
N3 N2 N1 106.4(3) . . ?
N2 N3 N4 110.8(3) . . ?
C1 N4 N3 105.3(3) . . ?
C1 N4 Zn1 127.0(3) . . ?
N3 N4 Zn1 127.6(3) . . ?
C7 N5 N6 108.5(4) . . ?
C7 N5 C8 130.7(4) . . ?
N6 N5 C8 120.7(4) . . ?
N7 N6 N5 106.6(4) . . ?
N6 N7 N8 110.3(3) . . ?
C7 N8 N7 105.4(4) . . ?
C7 N8 Zn1 135.7(3) . . ?
N7 N8 Zn1 118.5(3) . . ?
N4 C1 N1 109.2(4) . . ?
N4 C1 H1A 125.4 . . ?
N1 C1 H1A 125.4 . . ?
N1 C2 C3 111.1(4) . . ?
N1 C2 C6 111.1(4) . . ?
C3 C2 C6 104.3(4) . . ?
N1 C2 H2A 110.1 . . ?
C3 C2 H2A 110.1 . . ?
C6 C2 H2A 110.1 . . ?
C4 C3 C2 105.3(4) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C5B C4 C3 109.2(6) . . ?
C3 C4 C5A 99.0(5) . . ?
C3 C4 H4A 112.0 . . ?
C5A C4 H4A 112.0 . . ?
C3 C4 H4B 112.0 . . ?
C5A C4 H4B 112.0 . . ?
H4A C4 H4B 109.6 . . ?
C5A C6 C2 109.1(5) . . ?
C2 C6 C5B 101.4(6) . . ?
C5A C6 H6A 109.9 . . ?
C2 C6 H6A 109.9 . . ?
C5A C6 H6B 109.9 . . ?
C2 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N5 C7 N8 109.2(4) . . ?
N5 C7 H7 125.4 . . ?
N8 C7 H7 125.4 . . ?
N5 C8 C9 111.8(4) . . ?
N5 C8 C12 110.7(5) . . ?
C9 C8 C12 102.1(5) . . ?
N5 C8 H8 110.6 . . ?
C9 C8 H8 110.6 . . ?
C12 C8 H8 110.6 . . ?
C8 C9 C10 104.3(7) . . ?
C8 C9 H9A 110.9 . . ?
C10 C9 H9A 110.9 . . ?
C8 C9 H9B 110.9 . . ?
C10 C9 H9B 110.9 . . ?
H9A C9 H9B 108.9 . . ?
C11 C10 C9 109.9(9) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C10 C11 C12 105.2(7) . . ?
C10 C11 H11A 110.7 . . ?
C12 C11 H11A 110.7 . . ?
C10 C11 H11B 110.7 . . ?
C12 C11 H11B 110.7 . . ?
H11A C11 H11B 108.8 . . ?
C11 C12 C8 104.2(7) . . ?
C11 C12 H12A 110.9 . . ?
C8 C12 H12A 110.9 . . ?
C11 C12 H12B 110.9 . . ?
C8 C12 H12B 110.9 . . ?
H12A C12 H12B 108.9 . . ?
N16 Zn2 N16 180.0(2) . 2_666 ?
N16 Zn2 O2 91.10(13) . . ?
N16 Zn2 O2 88.90(13) 2_666 . ?
N16 Zn2 O2 88.90(13) . 2_666 ?
N16 Zn2 O2 91.10(13) 2_666 2_666 ?
O2 Zn2 O2 180.00(15) . 2_666 ?
N16 Zn2 N12 90.80(14) . 2_666 ?
N16 Zn2 N12 89.20(14) 2_666 2_666 ?
O2 Zn2 N12 92.83(13) . 2_666 ?
O2 Zn2 N12 87.17(13) 2_666 2_666 ?
N16 Zn2 N12 89.20(14) . . ?
N16 Zn2 N12 90.80(14) 2_666 . ?
O2 Zn2 N12 87.17(13) . . ?
O2 Zn2 N12 92.83(13) 2_666 . ?
N12 Zn2 N12 180.00(17) 2_666 . ?
Zn2 O2 H2B 117(3) . . ?
Zn2 O2 H2C 124(5) . . ?
H2B O2 H2C 116(5) . . ?
C13 N9 N10 108.1(4) . . ?
C13 N9 C14 130.7(4) . . ?
N10 N9 C14 121.1(4) . . ?
N11 N10 N9 106.8(3) . . ?
N10 N11 N12 110.6(3) . . ?
C13 N12 N11 105.4(4) . . ?
C13 N12 Zn2 127.7(3) . . ?
N11 N12 Zn2 126.1(3) . . ?
C19 N13 N14 108.4(4) . . ?
C19 N13 C20 128.0(4) . . ?
N14 N13 C20 123.6(4) . . ?
N15 N14 N13 106.8(4) . . ?
N14 N15 N16 109.8(4) . . ?
C19 N16 N15 106.1(4) . . ?
C19 N16 Zn2 130.0(3) . . ?
N15 N16 Zn2 123.8(3) . . ?
N12 C13 N9 109.1(4) . . ?
N12 C13 H13 125.5 . . ?
N9 C13 H13 125.5 . . ?
C18A C14 N9 114.2(6) . . ?
C18A C14 C15 112.2(7) . . ?
N9 C14 C15 112.2(4) . . ?
N9 C14 C18B 108.8(5) . . ?
C15 C14 C18B 97.8(5) . . ?
C18A C14 H14 105.8 . . ?
N9 C14 H14 105.8 . . ?
C15 C14 H14 105.8 . . ?
C16 C15 C14 106.0(5) . . ?
C16 C15 H15A 110.5 . . ?
C14 C15 H15A 110.5 . . ?
C16 C15 H15B 110.5 . . ?
C14 C15 H15B 110.5 . . ?
H15A C15 H15B 108.7 . . ?
C17 C16 C15 107.8(6) . . ?
C17 C16 H16A 110.1 . . ?
C15 C16 H16A 110.1 . . ?
C17 C16 H16B 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.5 . . ?
C18B C17 C16 103.9(7) . . ?
C16 C17 C18A 110.1(7) . . ?
C16 C17 H17A 109.6 . . ?
C18A C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C18A C17 H17B 109.6 . . ?
H17A C17 H17B 108.2 . . ?
N16 C19 N13 109.0(4) . . ?
N16 C19 H19 125.5 . . ?
N13 C19 H19 125.5 . . ?
N13 C20 C21 109.2(5) . . ?
N13 C20 C24 111.7(4) . . ?
C21 C20 C24 104.9(4) . . ?
N13 C20 H20 110.3 . . ?
C21 C20 H20 110.3 . . ?
C24 C20 H20 110.3 . . ?
C22 C21 C20 104.6(4) . . ?
C22 C21 H21A 110.8 . . ?
C20 C21 H21A 110.8 . . ?
C22 C21 H21B 110.8 . . ?
C20 C21 H21B 110.8 . . ?
H21A C21 H21B 108.9 . . ?
C21 C22 C23 107.1(5) . . ?
C21 C22 H22A 110.3 . . ?
C23 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
C23 C22 H22B 110.3 . . ?
H22A C22 H22B 108.6 . . ?
C24 C23 C22 106.6(4) . . ?
C24 C23 H23A 110.4 . . ?
C22 C23 H23A 110.4 . . ?
C24 C23 H23B 110.4 . . ?
C22 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
C23 C24 C20 103.7(4) . . ?
C23 C24 H24A 111.0 . . ?
C20 C24 H24A 111.0 . . ?
C23 C24 H24B 111.0 . . ?
C20 C24 H24B 111.0 . . ?
H24A C24 H24B 109.0 . . ?
O9 Cl2 O8 110.8(3) . . ?
O9 Cl2 O7 109.7(2) . . ?
O8 Cl2 O7 109.1(2) . . ?
O9 Cl2 O10 109.6(3) . . ?
O8 Cl2 O10 109.0(2) . . ?
O7 Cl2 O10 108.7(2) . . ?
O4B Cl1 O6B 110.5(7) . . ?
O4B Cl1 O3 107.9(6) . . ?
O6A Cl1 O3 113.1(5) . . ?
O6B Cl1 O3 109.1(4) . . ?
O4B Cl1 O5B 116.8(8) . . ?
O6B Cl1 O5B 108.8(6) . . ?
O3 Cl1 O5B 103.3(5) . . ?
O6A Cl1 O4A 110.1(6) . . ?
O3 Cl1 O4A 113.4(3) . . ?
O6A Cl1 O5A 108.0(7) . . ?
O3 Cl1 O5A 110.0(5) . . ?
O4A Cl1 O5A 101.4(5) . . ?
C6 C5A C4 102.7(6) . . ?
C6 C5A H5A1 111.2 . . ?
C4 C5A H5A1 111.2 . . ?
C6 C5A H5A2 111.2 . . ?
C4 C5A H5A2 111.2 . . ?
H5A1 C5A H5A2 109.1 . . ?
C14 C18A C17 101.7(8) . . ?
C14 C18A H18A 111.4 . . ?
C17 C18A H18A 111.4 . . ?
C14 C18A H18B 111.4 . . ?
C17 C18A H18B 111.4 . . ?
H18A C18A H18B 109.3 . . ?
C4 C5B C6 103.2(8) . . ?
C4 C5B H5B1 111.1 . . ?
C6 C5B H5B1 111.1 . . ?
C4 C5B H5B2 111.1 . . ?
C6 C5B H5B2 111.1 . . ?
H5B1 C5B H5B2 109.1 . . ?
C17 C18B C14 100.8(7) . . ?
C17 C18B H18C 111.6 . . ?
C14 C18B H18C 111.6 . . ?
C17 C18B H18D 111.6 . . ?
C14 C18B H18D 111.6 . . ?
H18C C18B H18D 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.8(5) . . . . ?
C2 N1 N2 N3 -178.5(4) . . . . ?
N1 N2 N3 N4 -1.0(5) . . . . ?
N2 N3 N4 C1 0.8(5) . . . . ?
N2 N3 N4 Zn1 -175.0(3) . . . . ?
C7 N5 N6 N7 -0.4(5) . . . . ?
C8 N5 N6 N7 178.8(4) . . . . ?
N5 N6 N7 N8 0.9(5) . . . . ?
N6 N7 N8 C7 -1.1(5) . . . . ?
N6 N7 N8 Zn1 172.8(3) . . . . ?
N3 N4 C1 N1 -0.2(5) . . . . ?
Zn1 N4 C1 N1 175.6(3) . . . . ?
N2 N1 C1 N4 -0.3(5) . . . . ?
C2 N1 C1 N4 178.9(4) . . . . ?
C1 N1 C2 C3 -9.8(7) . . . . ?
N2 N1 C2 C3 169.3(4) . . . . ?
C1 N1 C2 C6 105.8(5) . . . . ?
N2 N1 C2 C6 -75.1(5) . . . . ?
N1 C2 C3 C4 90.1(5) . . . . ?
C6 C2 C3 C4 -29.7(5) . . . . ?
C2 C3 C4 C5B 6.1(8) . . . . ?
C2 C3 C4 C5A 42.7(6) . . . . ?
N1 C2 C6 C5A -117.4(6) . . . . ?
C3 C2 C6 C5A 2.4(6) . . . . ?
N1 C2 C6 C5B -79.4(7) . . . . ?
C3 C2 C6 C5B 40.4(7) . . . . ?
N6 N5 C7 N8 -0.4(5) . . . . ?
C8 N5 C7 N8 -179.4(4) . . . . ?
N7 N8 C7 N5 0.9(5) . . . . ?
Zn1 N8 C7 N5 -171.5(3) . . . . ?
C7 N5 C8 C9 -141.6(5) . . . . ?
N6 N5 C8 C9 39.4(6) . . . . ?
C7 N5 C8 C12 105.3(7) . . . . ?
N6 N5 C8 C12 -73.7(7) . . . . ?
N5 C8 C9 C10 -95.4(6) . . . . ?
C12 C8 C9 C10 23.0(7) . . . . ?
C8 C9 C10 C11 -1.3(10) . . . . ?
C9 C10 C11 C12 -21.9(11) . . . . ?
C10 C11 C12 C8 36.6(10) . . . . ?
N5 C8 C12 C11 82.8(7) . . . . ?
C9 C8 C12 C11 -36.4(8) . . . . ?
C13 N9 N10 N11 0.3(5) . . . . ?
C14 N9 N10 N11 179.4(4) . . . . ?
N9 N10 N11 N12 0.6(5) . . . . ?
N10 N11 N12 C13 -1.2(5) . . . . ?
N10 N11 N12 Zn2 168.7(3) . . . . ?
C19 N13 N14 N15 -0.8(5) . . . . ?
C20 N13 N14 N15 176.4(4) . . . . ?
N13 N14 N15 N16 0.6(5) . . . . ?
N14 N15 N16 C19 -0.2(5) . . . . ?
N14 N15 N16 Zn2 177.1(3) . . . . ?
N11 N12 C13 N9 1.3(5) . . . . ?
Zn2 N12 C13 N9 -168.4(3) . . . . ?
N10 N9 C13 N12 -1.1(5) . . . . ?
C14 N9 C13 N12 179.9(4) . . . . ?
C13 N9 C14 C18A -4.5(10) . . . . ?
N10 N9 C14 C18A 176.6(7) . . . . ?
C13 N9 C14 C15 -133.6(5) . . . . ?
N10 N9 C14 C15 47.5(6) . . . . ?
C13 N9 C14 C18B -26.5(8) . . . . ?
N10 N9 C14 C18B 154.6(5) . . . . ?
C18A C14 C15 C16 11.2(9) . . . . ?
N9 C14 C15 C16 141.4(5) . . . . ?
C18B C14 C15 C16 27.4(7) . . . . ?
C14 C15 C16 C17 -1.7(9) . . . . ?
C15 C16 C17 C18B -29.7(10) . . . . ?
C15 C16 C17 C18A -7.5(11) . . . . ?
N15 N16 C19 N13 -0.3(5) . . . . ?
Zn2 N16 C19 N13 -177.3(3) . . . . ?
N14 N13 C19 N16 0.7(5) . . . . ?
C20 N13 C19 N16 -176.4(5) . . . . ?
C19 N13 C20 C21 -107.9(6) . . . . ?
N14 N13 C20 C21 75.4(6) . . . . ?
C19 N13 C20 C24 136.5(5) . . . . ?
N14 N13 C20 C24 -40.2(7) . . . . ?
N13 C20 C21 C22 -83.3(5) . . . . ?
C24 C20 C21 C22 36.6(6) . . . . ?
C20 C21 C22 C23 -33.0(6) . . . . ?
C21 C22 C23 C24 16.3(6) . . . . ?
C22 C23 C24 C20 6.1(6) . . . . ?
N13 C20 C24 C23 92.3(5) . . . . ?
C21 C20 C24 C23 -25.9(6) . . . . ?
C2 C6 C5A C4 23.7(7) . . . . ?
C3 C4 C5A C6 -40.4(7) . . . . ?
N9 C14 C18A C17 -144.0(7) . . . . ?
C15 C14 C18A C17 -14.9(11) . . . . ?
C16 C17 C18A C14 13.7(12) . . . . ?
C3 C4 C5B C6 18.7(10) . . . . ?
C2 C6 C5B C4 -36.2(9) . . . . ?
C16 C17 C18B C14 46.2(9) . . . . ?
N9 C14 C18B C17 -162.3(7) . . . . ?
C15 C14 C18B C17 -45.6(8) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         1.700
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.121

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_yv363
_database_code_depnum_ccdc_archive 'CCDC 2061086'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-25
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'diazido 1-cyclopropyl-5H-tetrazolyl copper(II)'
_chemical_name_common            
'diazido 1-cyclopropyl-5H-tetrazolyl copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 Cu N10'
_chemical_formula_sum            'C4 H6 Cu N10'
_chemical_formula_weight         257.73

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.5870(3)
_cell_length_b                   6.9121(4)
_cell_length_c                   13.0900(7)
_cell_angle_alpha                96.426(2)
_cell_angle_beta                 99.436(2)
_cell_angle_gamma                110.441(2)
_cell_volume                     459.38(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    7870
_cell_measurement_theta_min      3.2095
_cell_measurement_theta_max      30.5269

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.362
_shelx_estimated_absorpt_T_min   0.911
_shelx_estimated_absorpt_T_max   0.933
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_F_000             258
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            9544
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.209
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1867
_reflns_number_gt                1760
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²+0.3133P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1867
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0470
_refine_ls_wR_factor_gt          0.0459
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24789(4) 0.56857(3) 0.45402(2) 0.01105(8) Uani 1 1 d . . . . .
N1 N 0.3307(3) 0.5666(2) 0.31083(11) 0.0132(3) Uani 1 1 d . . . . .
N6 N 0.7264(3) 0.9096(2) 0.54932(10) 0.0119(3) Uani 1 1 d . . . . .
N5 N 0.6234(3) 0.7232(2) 0.52023(11) 0.0130(3) Uani 1 1 d . . . . .
N9 N -0.2696(3) 0.2709(2) 0.33216(11) 0.0170(3) Uani 1 1 d . . . . .
N8 N -0.1353(3) 0.4020(2) 0.40883(11) 0.0135(3) Uani 1 1 d . . . . .
N4 N 0.5204(3) 0.6204(2) 0.18155(11) 0.0151(3) Uani 1 1 d . . . . .
N7 N 0.8346(3) 1.0885(2) 0.57798(13) 0.0221(3) Uani 1 1 d . . . . .
N2 N 0.1485(3) 0.4851(3) 0.21893(11) 0.0209(3) Uani 1 1 d . . . . .
N3 N 0.2608(3) 0.5169(3) 0.14035(12) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.5595(3) 0.6494(3) 0.28571(13) 0.0136(3) Uani 1 1 d . . . . .
N10 N -0.4028(3) 0.1504(3) 0.26033(14) 0.0385(5) Uani 1 1 d . . . . .
C2 C 0.7064(3) 0.6762(3) 0.11422(14) 0.0186(4) Uani 1 1 d . . . . .
C4 C 0.9320(4) 0.8811(3) 0.14720(16) 0.0259(4) Uani 1 1 d . . . . .
C3 C 0.7135(4) 0.8528(3) 0.05705(16) 0.0260(4) Uani 1 1 d . . . . .
H1 H 0.711(4) 0.709(3) 0.3307(16) 0.020(5) Uiso 1 1 d . . . . .
H2 H 0.729(4) 0.558(3) 0.0812(16) 0.020(5) Uiso 1 1 d . . . . .
H4A H 1.088(5) 0.883(3) 0.1331(17) 0.029(6) Uiso 1 1 d . . . . .
H3A H 0.737(4) 0.839(4) -0.0087(19) 0.033(6) Uiso 1 1 d . . . . .
H3B H 0.596(4) 0.918(4) 0.0689(17) 0.029(6) Uiso 1 1 d . . . . .
H4B H 0.944(4) 0.968(3) 0.2091(17) 0.025(5) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N5 1.9814(14) . ?
Cu1 N8 1.9924(14) . ?
Cu1 N1 2.0026(13) . ?
Cu1 N8 2.0095(14) 2_566 ?
Cu1 N5 2.4050(14) 2_666 ?
N1 C1 1.319(2) . ?
N1 N2 1.359(2) . ?
N6 N7 1.155(2) . ?
N6 N5 1.1986(19) . ?
N9 N10 1.137(2) . ?
N9 N8 1.211(2) . ?
N4 C1 1.326(2) . ?
N4 N3 1.356(2) . ?
N4 C2 1.450(2) . ?
N2 N3 1.291(2) . ?
C1 H1 0.88(2) . ?
C2 C4 1.489(3) . ?
C2 C3 1.494(3) . ?
C2 H2 0.94(2) . ?
C4 C3 1.493(3) . ?
C4 H4A 0.92(2) . ?
C4 H4B 0.93(2) . ?
C3 H3A 0.89(2) . ?
C3 H3B 0.94(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Cu1 N8 171.31(6) . . ?
N5 Cu1 N1 90.39(6) . . ?
N8 Cu1 N1 97.85(6) . . ?
N5 Cu1 N8 93.22(6) . 2_566 ?
N8 Cu1 N8 79.01(6) . 2_566 ?
N1 Cu1 N8 171.35(6) . 2_566 ?
N5 Cu1 N5 80.44(5) . 2_666 ?
N8 Cu1 N5 96.43(5) . 2_666 ?
N1 Cu1 N5 92.03(5) . 2_666 ?
N8 Cu1 N5 96.32(5) 2_566 2_666 ?
C1 N1 N2 106.86(13) . . ?
C1 N1 Cu1 128.68(12) . . ?
N2 N1 Cu1 124.37(11) . . ?
N7 N6 N5 177.41(16) . . ?
N6 N5 Cu1 125.29(11) . . ?
N6 N5 Cu1 134.34(11) . 2_666 ?
Cu1 N5 Cu1 99.56(5) . 2_666 ?
N10 N9 N8 177.52(18) . . ?
N9 N8 Cu1 133.17(11) . . ?
N9 N8 Cu1 123.35(11) . 2_566 ?
Cu1 N8 Cu1 100.99(6) . 2_566 ?
C1 N4 N3 108.66(14) . . ?
C1 N4 C2 130.13(15) . . ?
N3 N4 C2 121.18(14) . . ?
N3 N2 N1 109.78(14) . . ?
N2 N3 N4 106.68(14) . . ?
N1 C1 N4 108.02(15) . . ?
N1 C1 H1 125.4(13) . . ?
N4 C1 H1 126.6(13) . . ?
N4 C2 C4 118.24(16) . . ?
N4 C2 C3 117.78(16) . . ?
C4 C2 C3 60.08(13) . . ?
N4 C2 H2 111.8(13) . . ?
C4 C2 H2 120.0(13) . . ?
C3 C2 H2 120.1(12) . . ?
C2 C4 C3 60.12(13) . . ?
C2 C4 H4A 116.3(14) . . ?
C3 C4 H4A 118.6(14) . . ?
C2 C4 H4B 118.4(13) . . ?
C3 C4 H4B 116.5(13) . . ?
H4A C4 H4B 115.7(19) . . ?
C4 C3 C2 59.80(13) . . ?
C4 C3 H3A 119.9(15) . . ?
C2 C3 H3A 117.1(15) . . ?
C4 C3 H3B 117.3(14) . . ?
C2 C3 H3B 116.1(14) . . ?
H3A C3 H3B 115(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.1(2) . . . . ?
Cu1 N1 N2 N3 176.75(12) . . . . ?
N1 N2 N3 N4 0.1(2) . . . . ?
C1 N4 N3 N2 -0.06(19) . . . . ?
C2 N4 N3 N2 178.33(15) . . . . ?
N2 N1 C1 N4 0.10(18) . . . . ?
Cu1 N1 C1 N4 -176.61(11) . . . . ?
N3 N4 C1 N1 -0.03(19) . . . . ?
C2 N4 C1 N1 -178.22(16) . . . . ?
C1 N4 C2 C4 -39.1(3) . . . . ?
N3 N4 C2 C4 142.85(17) . . . . ?
C1 N4 C2 C3 -108.2(2) . . . . ?
N3 N4 C2 C3 73.8(2) . . . . ?
N4 C2 C4 C3 -107.54(18) . . . . ?
N4 C2 C3 C4 108.29(19) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.393
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.056

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px234
_database_code_depnum_ccdc_archive 'CCDC 2061084'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-19
_audit_creation_method           SHELXL-2018/1


_chemical_name_systematic        'diazido 1-cyclobutyl-5H-tetrazolyl copper(II)'
_chemical_name_common            'diazido 1-cyclobutyl-5H-tetrazolyl copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H8 Cu N10'
_chemical_formula_sum            'C5 H8 Cu N10'
_chemical_formula_weight         271.75

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'




_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.1598(14)
_cell_length_b                   6.2457(3)
_cell_length_c                   10.8574(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.305(6)
_cell_angle_gamma                90
_cell_volume                     1004.40(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    106(2)
_cell_measurement_reflns_used    1395
_cell_measurement_theta_min      2.8050
_cell_measurement_theta_max      27.3230

_exptl_crystal_description       platelet
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    2.166
_shelx_estimated_absorpt_T_min   0.479
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_F_000             548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      106(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            6720
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.750
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2055
_reflns_number_gt                1547
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0395P)²+0.9872P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2055
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0027156000
_diffrn_orient_matrix_UB_12      0.0121211000
_diffrn_orient_matrix_UB_13      -0.0656579000
_diffrn_orient_matrix_UB_21      -0.0465888000
_diffrn_orient_matrix_UB_22      0.0248373000
_diffrn_orient_matrix_UB_23      -0.0087053000
_diffrn_orient_matrix_UB_31      0.0107995000
_diffrn_orient_matrix_UB_32      0.1101245000
_diffrn_orient_matrix_UB_33      0.0091758000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  78.00   1.00   25.00    --   21.23  57.00  60.00   65
  2  ω     -9.00  36.00   1.00   25.00    --   21.23  77.00  30.00   45
  3  ω    -11.00  27.00   1.00   25.00    --   21.23  77.00 150.00   38
  4  ω    -47.00  34.00   1.00   25.00    --   21.23 -57.00 150.00   81
  5  ω    -40.00  97.00   1.00   25.00    --   21.23  19.00 -30.00  137
  6  ω     23.00  64.00   1.00   25.00    --   21.23 -99.00 -90.00   41
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.03919(4) 0.04591(7) 0.14243(4) 0.01502(17) Uani 1 1 d . . . . .
N1 N 0.2681(2) 0.0725(5) 0.4202(3) 0.0170(8) Uani 1 1 d . . . . .
N2 N 0.3058(3) 0.0237(6) 0.3221(3) 0.0233(8) Uani 1 1 d . . . . .
N3 N 0.2406(3) 0.0058(6) 0.2245(3) 0.0248(9) Uani 1 1 d . . . . .
N4 N 0.1601(2) 0.0403(5) 0.2568(3) 0.0131(7) Uani 1 1 d . . . . .
N6 N -0.0143(2) 0.1763(5) 0.2784(3) 0.0154(7) Uani 1 1 d . . . . .
N7 N -0.0563(2) 0.0569(5) 0.3320(3) 0.0169(7) Uani 1 1 d . . . . .
N9 N -0.0776(2) 0.0528(5) 0.0150(3) 0.0161(7) Uani 1 1 d . . . . .
N10 N -0.1503(2) 0.0702(5) 0.0429(3) 0.0155(7) Uani 1 1 d . . . . .
N11 N -0.2177(3) 0.0885(6) 0.0718(3) 0.0265(9) Uani 1 1 d . . . . .
C1 C 0.1799(3) 0.0819(6) 0.3793(4) 0.0171(9) Uani 1 1 d . . . . .
H1 H 0.137301 0.113421 0.429557 0.021 Uiso 1 1 calc R U . . .
C2 C 0.3215(3) 0.1000(6) 0.5479(4) 0.0211(10) Uani 1 1 d . . . . .
H2 H 0.280907 0.140466 0.605705 0.025 Uiso 1 1 calc R U . . .
C3 C 0.4022(3) 0.2520(7) 0.5678(4) 0.0288(11) Uani 1 1 d . . . . .
H3A H 0.390340 0.394454 0.600894 0.035 Uiso 1 1 calc R U . . .
H3B H 0.430395 0.265097 0.493907 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4513(3) 0.0939(7) 0.6701(4) 0.0290(11) Uani 1 1 d . . . . .
H4A H 0.514880 0.065402 0.666284 0.035 Uiso 1 1 calc R U . . .
H4B H 0.445831 0.131029 0.756847 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3845(3) -0.0803(7) 0.6071(4) 0.0274(11) Uani 1 1 d . . . . .
H5A H 0.407267 -0.169606 0.545211 0.033 Uiso 1 1 calc R U . . .
H5B H 0.360176 -0.170027 0.667296 0.033 Uiso 1 1 calc R U . . .
N8 N -0.0971(3) -0.0537(5) 0.3840(3) 0.0274(9) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 1.983(3) . ?
Cu1 N9 2.002(3) . ?
Cu1 N6 2.002(3) . ?
Cu1 N9 2.016(3) 3 ?
N1 C1 1.318(5) . ?
N1 N2 1.346(5) . ?
N1 C2 1.459(5) . ?
N2 N3 1.292(5) . ?
N3 N4 1.357(5) . ?
N4 C1 1.326(5) . ?
N6 N7 1.208(4) . ?
N7 N8 1.152(5) . ?
N9 N10 1.209(5) . ?
N10 N11 1.137(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.527(6) . ?
C2 C5 1.527(6) . ?
C2 H2 1.0000 . ?
C3 C4 1.553(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.544(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N9 175.22(13) . . ?
N4 Cu1 N6 90.63(13) . . ?
N9 Cu1 N6 93.64(13) . . ?
N4 Cu1 N9 97.47(13) . 3 ?
N9 Cu1 N9 78.06(15) . 3 ?
N6 Cu1 N9 170.00(13) . 3 ?
C1 N1 N2 108.4(3) . . ?
C1 N1 C2 129.2(3) . . ?
N2 N1 C2 122.4(4) . . ?
N3 N2 N1 106.8(3) . . ?
N2 N3 N4 110.4(3) . . ?
C1 N4 N3 105.5(3) . . ?
C1 N4 Cu1 127.3(3) . . ?
N3 N4 Cu1 127.1(3) . . ?
N7 N6 Cu1 116.3(2) . . ?
N8 N7 N6 178.8(4) . . ?
N10 N9 Cu1 123.2(3) . . ?
N10 N9 Cu1 133.2(3) . 3 ?
Cu1 N9 Cu1 101.94(15) . 3 ?
N11 N10 N9 178.4(4) . . ?
N1 C1 N4 109.0(4) . . ?
N1 C1 H1 125.5 . . ?
N4 C1 H1 125.5 . . ?
N1 C2 C3 118.2(3) . . ?
N1 C2 C5 118.9(3) . . ?
C3 C2 C5 89.3(3) . . ?
N1 C2 H2 109.6 . . ?
C3 C2 H2 109.6 . . ?
C5 C2 H2 109.6 . . ?
C2 C3 C4 87.3(3) . . ?
C2 C3 H3A 114.1 . . ?
C4 C3 H3A 114.1 . . ?
C2 C3 H3B 114.1 . . ?
C4 C3 H3B 114.1 . . ?
H3A C3 H3B 111.3 . . ?
C5 C4 C3 87.8(3) . . ?
C5 C4 H4A 114.0 . . ?
C3 C4 H4A 114.0 . . ?
C5 C4 H4B 114.0 . . ?
C3 C4 H4B 114.0 . . ?
H4A C4 H4B 111.2 . . ?
C2 C5 C4 87.6(3) . . ?
C2 C5 H5A 114.0 . . ?
C4 C5 H5A 114.0 . . ?
C2 C5 H5B 114.0 . . ?
C4 C5 H5B 114.0 . . ?
H5A C5 H5B 111.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.4(4) . . . . ?
C2 N1 N2 N3 178.5(3) . . . . ?
N1 N2 N3 N4 -0.5(4) . . . . ?
N2 N3 N4 C1 0.5(4) . . . . ?
N2 N3 N4 Cu1 176.9(3) . . . . ?
N2 N1 C1 N4 -0.1(4) . . . . ?
C2 N1 C1 N4 -178.0(3) . . . . ?
N3 N4 C1 N1 -0.2(4) . . . . ?
Cu1 N4 C1 N1 -176.6(2) . . . . ?
C1 N1 C2 C3 -130.8(4) . . . . ?
N2 N1 C2 C3 51.5(5) . . . . ?
C1 N1 C2 C5 122.9(5) . . . . ?
N2 N1 C2 C5 -54.8(5) . . . . ?
N1 C2 C3 C4 -143.9(4) . . . . ?
C5 C2 C3 C4 -21.1(3) . . . . ?
C2 C3 C4 C5 20.9(3) . . . . ?
N1 C2 C5 C4 143.5(4) . . . . ?
C3 C2 C5 C4 21.2(3) . . . . ?
C3 C4 C5 C2 -20.8(3) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N8 0.95 2.27 3.096(5) 145.5 3_556




_refine_diff_density_max         1.461
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.120

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px241
_database_code_depnum_ccdc_archive 'CCDC 2061087'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-06-25
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        triclinic
_chemical_name_common            'P -1'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C32 H52 Cu2 N32 O2, 4(N O3)'
_chemical_formula_sum            'C32 H52 Cu2 N36 O14'
_chemical_formula_weight         1292.17

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2105(7)
_cell_length_b                   11.3324(8)
_cell_length_c                   11.4691(7)
_cell_angle_alpha                104.328(6)
_cell_angle_beta                 106.897(5)
_cell_angle_gamma                91.541(5)
_cell_volume                     1343.09(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    2446
_cell_measurement_theta_min      2.2460
_cell_measurement_theta_max      28.5550

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.888
_shelx_estimated_absorpt_T_min   0.665
_shelx_estimated_absorpt_T_max   0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_F_000             666
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            7859
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.909
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5412
_reflns_number_gt                4547
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0319P)²+0.5581P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5412
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0601000000
_diffrn_orient_matrix_UB_12      -0.0261007000
_diffrn_orient_matrix_UB_13      -0.0419041000
_diffrn_orient_matrix_UB_21      -0.0151668000
_diffrn_orient_matrix_UB_22      0.0588180000
_diffrn_orient_matrix_UB_23      -0.0067354000
_diffrn_orient_matrix_UB_31      0.0240992000
_diffrn_orient_matrix_UB_32      -0.0089634000
_diffrn_orient_matrix_UB_33      -0.0519304000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  39.00   1.00    5.00    --   21.39  77.00 120.00   50
  2  ω     -2.00  92.00   1.00    5.00    --   21.39  57.00  60.00   94
  3  ω     -2.00  89.00   1.00    5.00    --   21.39  57.00 -60.00   91
  4  ω    -49.00  45.00   1.00    5.00    --   21.39 -57.00 150.00   94
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.42016(3) 0.44063(3) 0.12689(2) 0.01350(9) Uani 1 1 d . . . . .
O2 O 0.49729(16) 0.30333(15) 0.47002(15) 0.0204(4) Uani 1 1 d . . . . .
O1 O 0.46371(17) 0.48045(19) 0.33663(16) 0.0208(4) Uani 1 1 d . . . . .
O3 O 0.61568(16) 0.19475(16) 0.37627(15) 0.0235(4) Uani 1 1 d . . . . .
O7 O 0.24657(17) 0.36591(18) 0.56279(17) 0.0279(4) Uani 1 1 d . . . . .
O4 O 0.65778(16) 0.23455(16) 0.58017(15) 0.0241(4) Uani 1 1 d . . . . .
O6 O 0.24308(18) 0.51705(17) 0.47829(17) 0.0313(5) Uani 1 1 d . . . . .
N16 N 0.10303(17) 0.60409(18) 0.14503(17) 0.0148(4) Uani 1 1 d . . . . .
N13 N 0.27012(17) 0.53222(18) 0.11805(17) 0.0146(4) Uani 1 1 d . . . . .
N5 N 0.56895(17) 0.34700(17) 0.13210(17) 0.0142(4) Uani 1 1 d . . . . .
N1 N 0.52616(17) 0.59896(18) 0.15666(17) 0.0139(4) Uani 1 1 d . . . . .
N4 N 0.62201(18) 0.77864(17) 0.25110(17) 0.0148(4) Uani 1 1 d . . . . .
N9 N 0.31472(17) 0.28784(18) 0.11203(17) 0.0146(4) Uani 1 1 d . . . . .
O5 O 0.19545(18) 0.33174(18) 0.35884(16) 0.0315(5) Uani 1 1 d . . . . .
N3 N 0.68081(18) 0.72582(18) 0.16734(17) 0.0169(4) Uani 1 1 d . . . . .
N8 N 0.74717(18) 0.27833(18) 0.18225(18) 0.0165(4) Uani 1 1 d . . . . .
N12 N 0.23928(18) 0.13515(18) 0.15670(18) 0.0164(4) Uani 1 1 d . . . . .
N21 N 0.59223(19) 0.24405(18) 0.47531(18) 0.0177(4) Uani 1 1 d . . . . .
N7 N 0.67496(19) 0.19878(19) 0.07345(19) 0.0210(5) Uani 1 1 d . . . . .
N14 N 0.21833(19) 0.58689(18) 0.02515(18) 0.0185(4) Uani 1 1 d . . . . .
N2 N 0.62222(18) 0.61746(18) 0.11042(17) 0.0158(4) Uani 1 1 d . . . . .
N15 N 0.11746(19) 0.63026(19) 0.04029(18) 0.0199(5) Uani 1 1 d . . . . .
N20 N 0.22849(18) 0.40407(19) 0.46627(19) 0.0194(4) Uani 1 1 d . . . . .
N10 N 0.18900(19) 0.26554(19) 0.05145(19) 0.0206(5) Uani 1 1 d . . . . .
N11 N 0.14301(18) 0.1737(2) 0.07792(19) 0.0212(5) Uani 1 1 d . . . . .
N6 N 0.56816(19) 0.24095(19) 0.04388(18) 0.0192(4) Uani 1 1 d . . . . .
C1 C 0.5281(2) 0.7008(2) 0.2433(2) 0.0149(5) Uani 1 1 d . . . . .
C14 C -0.0014(2) 0.6452(2) 0.1887(2) 0.0189(5) Uani 1 1 d . . . . .
C9 C 0.3429(2) 0.2060(2) 0.1770(2) 0.0153(5) Uani 1 1 d . . . . .
C13 C 0.1975(2) 0.5439(2) 0.1911(2) 0.0164(5) Uani 1 1 d . . . . .
C4 C 0.6536(3) 0.9268(3) 0.4610(2) 0.0255(6) Uani 1 1 d . . . . .
C5 C 0.6809(2) 0.3677(2) 0.2167(2) 0.0163(5) Uani 1 1 d . . . . .
C2 C 0.6597(2) 0.9028(2) 0.3298(2) 0.0217(5) Uani 1 1 d . . . . .
C6 C 0.8766(2) 0.2611(3) 0.2389(2) 0.0230(6) Uani 1 1 d . . . . .
C10 C 0.2180(2) 0.0438(2) 0.2183(2) 0.0203(5) Uani 1 1 d . . . . .
C3 C 0.7780(3) 0.9274(3) 0.4375(2) 0.0258(6) Uani 1 1 d . . . . .
C15 C 0.0235(3) 0.7423(3) 0.3092(3) 0.0273(6) Uani 1 1 d . . . . .
C12 C 0.1516(3) -0.0766(3) 0.1360(3) 0.0312(7) Uani 1 1 d . . . . .
C11 C 0.2887(3) -0.0658(2) 0.2052(3) 0.0256(6) Uani 1 1 d . . . . .
C16 C -0.0177(3) 0.6138(3) 0.3008(3) 0.0299(7) Uani 1 1 d . . . . .
C7 C 0.9146(3) 0.2523(4) 0.3707(3) 0.0429(9) Uani 1 1 d . . . . .
C8 C 0.9010(3) 0.1410(3) 0.2657(4) 0.0425(9) Uani 1 1 d . . . . .
H5 H 0.708(2) 0.430(2) 0.287(2) 0.014(6) Uiso 1 1 d . . . . .
H10 H 0.204(2) 0.078(2) 0.296(2) 0.015(6) Uiso 1 1 d . . . . .
H14 H -0.073(2) 0.647(2) 0.120(2) 0.011(6) Uiso 1 1 d . . . . .
H1 H 0.474(2) 0.717(2) 0.296(2) 0.020(7) Uiso 1 1 d . . . . .
H6 H 0.931(2) 0.295(2) 0.207(2) 0.015(6) Uiso 1 1 d . . . . .
H13 H 0.206(2) 0.516(2) 0.260(2) 0.014(6) Uiso 1 1 d . . . . .
H2 H 0.635(2) 0.963(3) 0.286(2) 0.025(7) Uiso 1 1 d . . . . .
H11A H 0.345(3) -0.066(3) 0.159(3) 0.028(7) Uiso 1 1 d . . . . .
H4A H 0.633(3) 0.860(3) 0.489(3) 0.029(7) Uiso 1 1 d . . . . .
H16A H -0.098(3) 0.596(3) 0.299(3) 0.034(8) Uiso 1 1 d . . . . .
H3A H 0.824(3) 0.861(3) 0.450(3) 0.031(8) Uiso 1 1 d . . . . .
H12A H 0.129(2) -0.087(2) 0.045(3) 0.025(7) Uiso 1 1 d . . . . .
H16B H 0.037(3) 0.572(3) 0.340(3) 0.028(8) Uiso 1 1 d . . . . .
H15A H 0.106(3) 0.769(2) 0.353(2) 0.021(7) Uiso 1 1 d . . . . .
H12B H 0.098(2) -0.112(3) 0.171(2) 0.024(7) Uiso 1 1 d . . . . .
H15B H -0.033(3) 0.801(3) 0.314(3) 0.037(8) Uiso 1 1 d . . . . .
H1A H 0.470(2) 0.428(3) 0.369(3) 0.020(8) Uiso 1 1 d . . . . .
H11B H 0.313(2) -0.096(2) 0.268(3) 0.021(7) Uiso 1 1 d . . . . .
H4B H 0.627(2) 1.000(3) 0.492(2) 0.025(7) Uiso 1 1 d . . . . .
H9 H 0.418(3) 0.196(2) 0.226(2) 0.023(7) Uiso 1 1 d . . . . .
H3B H 0.822(3) 1.001(3) 0.454(3) 0.028(7) Uiso 1 1 d . . . . .
H7A H 0.854(3) 0.258(3) 0.407(3) 0.047(10) Uiso 1 1 d . . . . .
H1B H 0.481(3) 0.549(4) 0.394(3) 0.055(11) Uiso 1 1 d . . . . .
H7B H 0.996(3) 0.289(3) 0.425(3) 0.052(10) Uiso 1 1 d . . . . .
H8A H 0.833(3) 0.085(3) 0.241(3) 0.050(10) Uiso 1 1 d . . . . .
H8B H 0.978(3) 0.108(3) 0.249(3) 0.061(11) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N13 1.9909(19) . ?
Cu1 N5 1.9951(19) . ?
Cu1 N9 2.0127(19) . ?
Cu1 N1 2.0235(19) . ?
Cu1 O1 2.2354(17) . ?
O2 N21 1.268(2) . ?
O1 H1A 0.77(3) . ?
O1 H1B 0.86(4) . ?
O3 N21 1.240(2) . ?
O7 N20 1.251(2) . ?
O4 N21 1.246(2) . ?
O6 N20 1.254(3) . ?
N16 C13 1.326(3) . ?
N16 N15 1.358(2) . ?
N16 C14 1.447(3) . ?
N13 C13 1.315(3) . ?
N13 N14 1.357(2) . ?
N5 C5 1.317(3) . ?
N5 N6 1.364(3) . ?
N1 C1 1.318(3) . ?
N1 N2 1.364(3) . ?
N4 C1 1.324(3) . ?
N4 N3 1.349(3) . ?
N4 C2 1.446(3) . ?
N9 C9 1.318(3) . ?
N9 N10 1.363(3) . ?
O5 N20 1.243(3) . ?
N3 N2 1.295(3) . ?
N8 C5 1.322(3) . ?
N8 N7 1.357(3) . ?
N8 C6 1.447(3) . ?
N12 C9 1.322(3) . ?
N12 N11 1.351(3) . ?
N12 C10 1.441(3) . ?
N7 N6 1.285(3) . ?
N14 N15 1.285(3) . ?
N10 N11 1.288(3) . ?
C1 H1 0.96(3) . ?
C14 C16 1.473(3) . ?
C14 C15 1.486(4) . ?
C14 H14 0.95(2) . ?
C9 H9 0.90(3) . ?
C13 H13 0.90(2) . ?
C4 C2 1.484(3) . ?
C4 C3 1.496(4) . ?
C4 H4A 0.94(3) . ?
C4 H4B 0.91(3) . ?
C5 H5 0.90(3) . ?
C2 C3 1.490(4) . ?
C2 H2 0.94(3) . ?
C6 C7 1.477(4) . ?
C6 C8 1.483(4) . ?
C6 H6 0.92(2) . ?
C10 C12 1.486(4) . ?
C10 C11 1.491(4) . ?
C10 H10 0.94(2) . ?
C3 H3A 0.94(3) . ?
C3 H3B 0.90(3) . ?
C15 C16 1.487(4) . ?
C15 H15A 0.91(3) . ?
C15 H15B 0.94(3) . ?
C12 C11 1.497(4) . ?
C12 H12A 0.97(3) . ?
C12 H12B 0.95(3) . ?
C11 H11A 0.93(3) . ?
C11 H11B 0.85(2) . ?
C16 H16A 0.92(3) . ?
C16 H16B 0.87(3) . ?
C7 C8 1.482(5) . ?
C7 H7A 0.89(3) . ?
C7 H7B 0.95(3) . ?
C8 H8A 0.90(4) . ?
C8 H8B 1.00(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N13 Cu1 N5 178.85(8) . . ?
N13 Cu1 N9 89.35(8) . . ?
N5 Cu1 N9 90.24(8) . . ?
N13 Cu1 N1 89.48(8) . . ?
N5 Cu1 N1 91.01(8) . . ?
N9 Cu1 N1 175.32(7) . . ?
N13 Cu1 O1 90.08(7) . . ?
N5 Cu1 O1 90.99(7) . . ?
N9 Cu1 O1 87.85(7) . . ?
N1 Cu1 O1 87.62(7) . . ?
Cu1 O1 H1A 121(2) . . ?
Cu1 O1 H1B 131(2) . . ?
H1A O1 H1B 108(3) . . ?
C13 N16 N15 108.36(19) . . ?
C13 N16 C14 131.81(19) . . ?
N15 N16 C14 119.80(18) . . ?
C13 N13 N14 107.15(18) . . ?
C13 N13 Cu1 128.35(15) . . ?
N14 N13 Cu1 124.30(14) . . ?
C5 N5 N6 106.69(19) . . ?
C5 N5 Cu1 129.91(17) . . ?
N6 N5 Cu1 123.36(14) . . ?
C1 N1 N2 106.27(19) . . ?
C1 N1 Cu1 124.55(15) . . ?
N2 N1 Cu1 128.30(15) . . ?
C1 N4 N3 108.99(19) . . ?
C1 N4 C2 128.9(2) . . ?
N3 N4 C2 122.05(19) . . ?
C9 N9 N10 106.34(19) . . ?
C9 N9 Cu1 128.26(16) . . ?
N10 N9 Cu1 123.94(14) . . ?
N2 N3 N4 106.41(18) . . ?
C5 N8 N7 108.72(19) . . ?
C5 N8 C6 130.1(2) . . ?
N7 N8 C6 121.1(2) . . ?
C9 N12 N11 108.64(18) . . ?
C9 N12 C10 129.4(2) . . ?
N11 N12 C10 121.26(19) . . ?
O3 N21 O4 121.8(2) . . ?
O3 N21 O2 119.44(18) . . ?
O4 N21 O2 118.75(19) . . ?
N6 N7 N8 106.69(19) . . ?
N15 N14 N13 109.58(17) . . ?
N3 N2 N1 109.99(19) . . ?
N14 N15 N16 106.94(17) . . ?
O5 N20 O7 121.0(2) . . ?
O5 N20 O6 119.7(2) . . ?
O7 N20 O6 119.4(2) . . ?
N11 N10 N9 109.85(18) . . ?
N10 N11 N12 106.77(18) . . ?
N7 N6 N5 109.78(19) . . ?
N1 C1 N4 108.3(2) . . ?
N1 C1 H1 127.7(16) . . ?
N4 C1 H1 123.9(16) . . ?
N16 C14 C16 119.3(2) . . ?
N16 C14 C15 119.0(2) . . ?
C16 C14 C15 60.35(19) . . ?
N16 C14 H14 111.3(14) . . ?
C16 C14 H14 120.1(14) . . ?
C15 C14 H14 118.4(15) . . ?
N9 C9 N12 108.4(2) . . ?
N9 C9 H9 128.3(17) . . ?
N12 C9 H9 123.3(17) . . ?
N13 C13 N16 108.0(2) . . ?
N13 C13 H13 128.9(15) . . ?
N16 C13 H13 123.2(15) . . ?
C2 C4 C3 60.02(17) . . ?
C2 C4 H4A 118.6(17) . . ?
C3 C4 H4A 114.9(17) . . ?
C2 C4 H4B 116.0(16) . . ?
C3 C4 H4B 118.5(17) . . ?
H4A C4 H4B 117(2) . . ?
N5 C5 N8 108.1(2) . . ?
N5 C5 H5 126.9(16) . . ?
N8 C5 H5 124.9(16) . . ?
N4 C2 C4 116.6(2) . . ?
N4 C2 C3 118.3(2) . . ?
C4 C2 C3 60.40(18) . . ?
N4 C2 H2 113.7(17) . . ?
C4 C2 H2 118.0(17) . . ?
C3 C2 H2 119.8(17) . . ?
N8 C6 C7 117.8(2) . . ?
N8 C6 C8 116.9(2) . . ?
C7 C6 C8 60.1(2) . . ?
N8 C6 H6 113.2(15) . . ?
C7 C6 H6 121.3(15) . . ?
C8 C6 H6 117.5(15) . . ?
N12 C10 C12 117.2(2) . . ?
N12 C10 C11 118.1(2) . . ?
C12 C10 C11 60.37(19) . . ?
N12 C10 H10 112.3(15) . . ?
C12 C10 H10 120.7(15) . . ?
C11 C10 H10 119.2(15) . . ?
C2 C3 C4 59.58(18) . . ?
C2 C3 H3A 118.1(18) . . ?
C4 C3 H3A 117.2(17) . . ?
C2 C3 H3B 115.2(17) . . ?
C4 C3 H3B 118.0(18) . . ?
H3A C3 H3B 117(2) . . ?
C14 C15 C16 59.41(18) . . ?
C14 C15 H15A 116.0(17) . . ?
C16 C15 H15A 115.6(17) . . ?
C14 C15 H15B 118.3(19) . . ?
C16 C15 H15B 119.0(19) . . ?
H15A C15 H15B 116(3) . . ?
C10 C12 C11 59.98(18) . . ?
C10 C12 H12A 116.4(16) . . ?
C11 C12 H12A 116.7(15) . . ?
C10 C12 H12B 113.2(17) . . ?
C11 C12 H12B 115.6(15) . . ?
H12A C12 H12B 120(2) . . ?
C10 C11 C12 59.66(18) . . ?
C10 C11 H11A 114.8(17) . . ?
C12 C11 H11A 117.8(17) . . ?
C10 C11 H11B 118.6(18) . . ?
C12 C11 H11B 119.3(17) . . ?
H11A C11 H11B 115(2) . . ?
C14 C16 C15 60.24(18) . . ?
C14 C16 H16A 116.8(17) . . ?
C15 C16 H16A 118.1(19) . . ?
C14 C16 H16B 118.6(18) . . ?
C15 C16 H16B 117.9(19) . . ?
H16A C16 H16B 115(2) . . ?
C6 C7 C8 60.2(2) . . ?
C6 C7 H7A 116(2) . . ?
C8 C7 H7A 116(2) . . ?
C6 C7 H7B 118.6(19) . . ?
C8 C7 H7B 120(2) . . ?
H7A C7 H7B 115(3) . . ?
C7 C8 C6 59.7(2) . . ?
C7 C8 H8A 120(2) . . ?
C6 C8 H8A 116(2) . . ?
C7 C8 H8B 119(2) . . ?
C6 C8 H8B 115(2) . . ?
H8A C8 H8B 115(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 0.0(2) . . . . ?
C2 N4 N3 N2 -178.09(19) . . . . ?
C5 N8 N7 N6 0.4(2) . . . . ?
C6 N8 N7 N6 -176.97(19) . . . . ?
C13 N13 N14 N15 -0.2(3) . . . . ?
Cu1 N13 N14 N15 175.08(16) . . . . ?
N4 N3 N2 N1 -0.3(2) . . . . ?
C1 N1 N2 N3 0.5(2) . . . . ?
Cu1 N1 N2 N3 -169.00(14) . . . . ?
N13 N14 N15 N16 0.2(3) . . . . ?
C13 N16 N15 N14 -0.2(3) . . . . ?
C14 N16 N15 N14 178.1(2) . . . . ?
C9 N9 N10 N11 -0.4(3) . . . . ?
Cu1 N9 N10 N11 -167.58(16) . . . . ?
N9 N10 N11 N12 0.0(3) . . . . ?
C9 N12 N11 N10 0.3(3) . . . . ?
C10 N12 N11 N10 171.6(2) . . . . ?
N8 N7 N6 N5 -0.3(2) . . . . ?
C5 N5 N6 N7 0.1(2) . . . . ?
Cu1 N5 N6 N7 -177.73(14) . . . . ?
N2 N1 C1 N4 -0.5(2) . . . . ?
Cu1 N1 C1 N4 169.50(13) . . . . ?
N3 N4 C1 N1 0.3(2) . . . . ?
C2 N4 C1 N1 178.2(2) . . . . ?
C13 N16 C14 C16 -3.6(4) . . . . ?
N15 N16 C14 C16 178.6(2) . . . . ?
C13 N16 C14 C15 66.7(4) . . . . ?
N15 N16 C14 C15 -111.1(3) . . . . ?
N10 N9 C9 N12 0.6(3) . . . . ?
Cu1 N9 C9 N12 167.05(15) . . . . ?
N11 N12 C9 N9 -0.6(3) . . . . ?
C10 N12 C9 N9 -170.9(2) . . . . ?
N14 N13 C13 N16 0.1(3) . . . . ?
Cu1 N13 C13 N16 -174.95(16) . . . . ?
N15 N16 C13 N13 0.1(3) . . . . ?
C14 N16 C13 N13 -177.9(2) . . . . ?
N6 N5 C5 N8 0.2(2) . . . . ?
Cu1 N5 C5 N8 177.76(14) . . . . ?
N7 N8 C5 N5 -0.3(2) . . . . ?
C6 N8 C5 N5 176.7(2) . . . . ?
C1 N4 C2 C4 39.8(3) . . . . ?
N3 N4 C2 C4 -142.5(2) . . . . ?
C1 N4 C2 C3 108.9(3) . . . . ?
N3 N4 C2 C3 -73.5(3) . . . . ?
C3 C4 C2 N4 109.1(3) . . . . ?
C5 N8 C6 C7 60.0(4) . . . . ?
N7 N8 C6 C7 -123.4(3) . . . . ?
C5 N8 C6 C8 128.6(3) . . . . ?
N7 N8 C6 C8 -54.7(3) . . . . ?
C9 N12 C10 C12 -132.8(3) . . . . ?
N11 N12 C10 C12 57.9(3) . . . . ?
C9 N12 C10 C11 -63.7(3) . . . . ?
N11 N12 C10 C11 127.1(3) . . . . ?
N4 C2 C3 C4 -106.1(3) . . . . ?
N16 C14 C15 C16 -109.2(2) . . . . ?
N12 C10 C12 C11 108.5(3) . . . . ?
N12 C10 C11 C12 -107.0(3) . . . . ?
N16 C14 C16 C15 108.7(3) . . . . ?
N8 C6 C7 C8 106.6(3) . . . . ?
N8 C6 C8 C7 -108.2(3) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O2 0.77(3) 2.01(3) 2.781(2) 174(3) .




_refine_diff_density_max         0.336
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.067

_shelxl_version_number           ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px326
_database_code_depnum_ccdc_archive 'CCDC 2061082'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-09-23
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) iron(II) diperchlorate'
_chemical_name_common            
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) iron(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H44 Mn N16 O2, 2(Cl O4)'
_chemical_formula_sum            'C24 H44 Cl2 Mn N16 O10'
_chemical_formula_weight         842.59

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7162(4)
_cell_length_b                   11.9386(6)
_cell_length_c                   15.5566(7)
_cell_angle_alpha                68.044(4)
_cell_angle_beta                 79.661(4)
_cell_angle_gamma                77.005(4)
_cell_volume                     1788.58(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    106(2)
_cell_measurement_reflns_used    3778
_cell_measurement_theta_min      2.2870
_cell_measurement_theta_max      28.8860

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.595
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             878
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      106(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            12525
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.961
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             7870
_reflns_number_gt                6124
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0604P)²+3.5768P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7870
_refine_ls_number_parameters     497
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1514
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0603530000
_diffrn_orient_matrix_UB_12      0.0134712000
_diffrn_orient_matrix_UB_13      -0.0176131000
_diffrn_orient_matrix_UB_21      -0.0253737000
_diffrn_orient_matrix_UB_22      -0.0398680000
_diffrn_orient_matrix_UB_23      0.0430237000
_diffrn_orient_matrix_UB_31      -0.0194962000
_diffrn_orient_matrix_UB_32      0.0495884000
_diffrn_orient_matrix_UB_33      0.0168143000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  11.00   1.00   10.00    --  -15.28 -77.00  30.00   50
  2  ω     -3.00  85.00   1.00   10.00    --   16.22  37.00   0.00   88
  3  ω    -20.00  55.00   1.00   10.00    --   16.22 -99.00-180.00   75
  4  ω    -54.00  39.00   1.00   10.00    --   16.22 -19.00-180.00   93
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.000000 1.000000 0.000000 0.01846(16) Uani 1 2 d S . P . .
O1 O -0.1055(2) 0.8654(2) 0.00102(18) 0.0233(5) Uani 1 1 d . . . . .
N1 N -0.1428(3) 0.9223(3) 0.29377(19) 0.0260(6) Uani 1 1 d . . . . .
N2 N -0.2315(3) 1.0199(3) 0.2542(2) 0.0290(6) Uani 1 1 d . . . . .
N3 N -0.2004(3) 1.0528(3) 0.16561(19) 0.0272(6) Uani 1 1 d . . . . .
N4 N -0.0915(3) 0.9775(2) 0.14606(18) 0.0231(6) Uani 1 1 d . . . . .
N5 N 0.3529(3) 0.7822(2) 0.11893(18) 0.0218(5) Uani 1 1 d . . . . .
N6 N 0.3294(3) 0.7026(2) 0.08353(19) 0.0231(6) Uani 1 1 d . . . . .
N7 N 0.2197(3) 0.7490(2) 0.04946(18) 0.0221(5) Uani 1 1 d . . . . .
N8 N 0.1709(3) 0.8578(2) 0.06219(19) 0.0228(6) Uani 1 1 d . . . . .
C1 C -0.0587(3) 0.8976(3) 0.2270(2) 0.0252(7) Uani 1 1 d . . . . .
H1 H 0.013437 0.832896 0.236026 0.030 Uiso 1 1 calc R U . . .
C2 C -0.1441(4) 0.8598(4) 0.3961(2) 0.0381(9) Uani 1 1 d . . . . .
H2 H -0.061908 0.800548 0.410849 0.046 Uiso 1 1 calc R U . . .
C3 C -0.2582(6) 0.7919(5) 0.4351(3) 0.0640(15) Uani 1 1 d . . . . .
H3A H -0.288428 0.773830 0.385952 0.077 Uiso 1 1 calc R U . . .
H3B H -0.234827 0.714089 0.486680 0.077 Uiso 1 1 calc R U . . .
C5 C -0.2951(5) 0.9497(6) 0.4995(4) 0.0621(13) Uani 1 1 d . . . . .
H5A H -0.288842 0.912071 0.567429 0.075 Uiso 1 1 calc R U . . .
H5B H -0.343204 1.034514 0.485774 0.075 Uiso 1 1 calc R U . . .
C6 C -0.1632(4) 0.9502(4) 0.4471(3) 0.0419(9) Uani 1 1 d . . . . .
H6A H -0.096989 0.925387 0.490749 0.050 Uiso 1 1 calc R U . . .
H6B H -0.155681 1.033445 0.401940 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2551(3) 0.8751(3) 0.1056(2) 0.0245(7) Uani 1 1 d . . . . .
H7 H 0.247158 0.943597 0.124569 0.029 Uiso 1 1 calc R U . . .
C8 C 0.4719(3) 0.7609(3) 0.1631(2) 0.0283(7) Uani 1 1 d . . . . .
H8 H 0.523296 0.678002 0.168277 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5526(3) 0.8595(3) 0.1099(3) 0.0315(8) Uani 1 1 d . . . . .
H9A H 0.645324 0.825322 0.114083 0.038 Uiso 1 1 calc R U . . .
H9B H 0.537010 0.894810 0.043356 0.038 Uiso 1 1 calc R U . . .
C10 C 0.5115(4) 0.9555(4) 0.1546(3) 0.0472(11) Uani 1 1 d . . . . .
H10A H 0.580231 1.004287 0.143066 0.057 Uiso 1 1 calc R U . . .
H10B H 0.432241 1.011518 0.130583 0.057 Uiso 1 1 calc R U . . .
C11 C 0.4880(7) 0.8855(6) 0.2540(4) 0.0795(18) Uani 1 1 d . . . . .
H11A H 0.423617 0.935295 0.285378 0.095 Uiso 1 1 calc R U . . .
H11B H 0.568724 0.861139 0.283948 0.095 Uiso 1 1 calc R U . . .
C12 C 0.4386(4) 0.7740(5) 0.2608(3) 0.0556(13) Uani 1 1 d . . . . .
H12A H 0.344278 0.783989 0.278184 0.067 Uiso 1 1 calc R U . . .
H12B H 0.480257 0.700221 0.308592 0.067 Uiso 1 1 calc R U . . .
Mn2 Mn 1.000000 0.500000 0.000000 0.01655(15) Uani 1 2 d S . P . .
O2 O 1.0843(2) 0.6658(2) -0.05644(18) 0.0236(5) Uani 1 1 d . . . . .
N9 N 0.6231(2) 0.6723(2) -0.10075(18) 0.0204(5) Uani 1 1 d . . . . .
N10 N 0.6190(3) 0.7104(3) -0.02898(19) 0.0251(6) Uani 1 1 d . . . . .
N11 N 0.7290(3) 0.6668(3) 0.00354(19) 0.0243(6) Uani 1 1 d . . . . .
N12 N 0.8058(2) 0.5991(2) -0.04568(17) 0.0195(5) Uani 1 1 d . . . . .
N13 N 0.8783(3) 0.5101(2) 0.28403(18) 0.0231(6) Uani 1 1 d . . . . .
N14 N 0.8668(3) 0.6310(2) 0.23483(18) 0.0256(6) Uani 1 1 d . . . . .
N15 N 0.9070(3) 0.6413(2) 0.14960(18) 0.0228(6) Uani 1 1 d . . . . .
N16 N 0.9450(2) 0.5286(2) 0.14123(17) 0.0196(5) Uani 1 1 d . . . . .
C13 C 0.7372(3) 0.6042(3) -0.1099(2) 0.0207(6) Uani 1 1 d . . . . .
H13 H 0.764997 0.565434 -0.155092 0.025 Uiso 1 1 calc R U . . .
C14 C 0.5089(3) 0.7026(3) -0.1508(2) 0.0236(7) Uani 1 1 d . . . . .
H14 H 0.445611 0.767536 -0.132695 0.028 Uiso 1 1 calc R U . . .
C15 C 0.5398(4) 0.7493(4) -0.2569(2) 0.0370(9) Uani 1 1 d . . . . .
H15A H 0.535674 0.839307 -0.281430 0.044 Uiso 1 1 calc R U . . .
H15B H 0.626792 0.709908 -0.275286 0.044 Uiso 1 1 calc R U . . .
C16 C 0.4368(4) 0.7142(4) -0.2931(3) 0.0443(10) Uani 1 1 d . . . . .
H16A H 0.375875 0.788304 -0.324609 0.053 Uiso 1 1 calc R U . . .
H16B H 0.476885 0.672893 -0.338372 0.053 Uiso 1 1 calc R U . . .
C17 C 0.3682(5) 0.6303(6) -0.2118(3) 0.0612(14) Uani 1 1 d . . . . .
H17A H 0.361580 0.557051 -0.225007 0.073 Uiso 1 1 calc R U . . .
H17B H 0.280062 0.672205 -0.198443 0.073 Uiso 1 1 calc R U . . .
C18 C 0.4438(3) 0.5924(3) -0.1284(3) 0.0323(8) Uani 1 1 d . . . . .
H18A H 0.507941 0.516962 -0.123624 0.039 Uiso 1 1 calc R U . . .
H18B H 0.385821 0.579022 -0.069527 0.039 Uiso 1 1 calc R U . . .
C19 C 0.9270(3) 0.4495(3) 0.2261(2) 0.0215(6) Uani 1 1 d . . . . .
H19 H 0.945794 0.362776 0.243069 0.026 Uiso 1 1 calc R U . . .
C20 C 0.8434(4) 0.4668(4) 0.3864(2) 0.0401(10) Uani 1 1 d . . . . .
H20 H 0.872350 0.523038 0.410039 0.048 Uiso 1 1 calc R U . . .
C21 C 0.6962(4) 0.4803(4) 0.4103(3) 0.0406(9) Uani 1 1 d . . . . .
H21A H 0.651997 0.497227 0.354927 0.049 Uiso 1 1 calc R U . . .
H21B H 0.661948 0.545963 0.436954 0.049 Uiso 1 1 calc R U . . .
C24 C 0.9126(6) 0.3405(5) 0.4348(3) 0.0631(14) Uani 1 1 d . . . . .
H24A H 0.987574 0.314983 0.394701 0.076 Uiso 1 1 calc R U . . .
H24B H 0.940692 0.333046 0.494240 0.076 Uiso 1 1 calc R U . . .
Cl1 Cl 0.19574(9) 0.54410(8) 0.33132(6) 0.0300(2) Uani 1 1 d . . . . .
O3 O 0.1616(3) 0.6733(3) 0.2931(3) 0.0718(11) Uani 1 1 d . . . . .
O4 O 0.3310(3) 0.5157(3) 0.3367(3) 0.0790(13) Uani 1 1 d . . . . .
O5 O 0.1631(3) 0.4881(4) 0.2749(3) 0.0682(11) Uani 1 1 d . . . . .
O6 O 0.1319(5) 0.5016(4) 0.4201(2) 0.0927(15) Uani 1 1 d . . . . .
Cl2 Cl 0.11297(7) 0.11538(7) 0.25186(5) 0.02308(17) Uani 1 1 d . . . . .
O7 O 0.1223(3) -0.0071(2) 0.3155(2) 0.0431(7) Uani 1 1 d . . . . .
O8 O -0.0201(2) 0.1646(2) 0.23189(16) 0.0283(5) Uani 1 1 d . . . . .
O9 O 0.1551(3) 0.1919(3) 0.28853(18) 0.0375(6) Uani 1 1 d . . . . .
O10 O 0.1910(2) 0.1170(2) 0.16500(16) 0.0307(5) Uani 1 1 d . . . . .
C4B C -0.3595(7) 0.8794(8) 0.4696(6) 0.115(3) Uani 1 1 d . . . . .
H4B1 H -0.412712 0.934464 0.419088 0.138 Uiso 1 1 calc R U . . .
H4B2 H -0.416616 0.833510 0.522217 0.138 Uiso 1 1 calc R U . . .
C22B C 0.6830(7) 0.3493(6) 0.4851(3) 0.099(3) Uani 1 1 d . . . . .
H22A H 0.605264 0.320780 0.480578 0.119 Uiso 1 1 calc R U . . .
H22B H 0.683521 0.346308 0.549472 0.119 Uiso 1 1 calc R U . . .
C23B C 0.8135(7) 0.2748(6) 0.4493(6) 0.101(3) Uani 1 1 d . . . . .
H23A H 0.834013 0.192078 0.496471 0.121 Uiso 1 1 calc R U . . .
H23B H 0.803039 0.265480 0.390537 0.121 Uiso 1 1 calc R U . . .
H22 H 1.067(4) 0.724(4) -0.105(3) 0.031(11) Uiso 1 1 d . . . . .
H12 H -0.123(4) 0.860(4) -0.049(3) 0.037(11) Uiso 1 1 d . . . . .
H11 H -0.105(4) 0.801(4) 0.042(3) 0.034(11) Uiso 1 1 d . . . . .
H21 H 1.119(5) 0.690(4) -0.029(4) 0.055(15) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.157(2) 2_575 ?
Mn1 O1 2.157(2) . ?
Mn1 N4 2.249(3) . ?
Mn1 N4 2.249(3) 2_575 ?
Mn1 N8 2.276(3) 2_575 ?
Mn1 N8 2.276(3) . ?
O1 H12 0.86(5) . ?
O1 H11 0.79(5) . ?
N1 C1 1.324(4) . ?
N1 N2 1.347(4) . ?
N1 C2 1.483(4) . ?
N2 N3 1.287(4) . ?
N3 N4 1.367(4) . ?
N4 C1 1.315(4) . ?
N5 C7 1.324(4) . ?
N5 N6 1.349(3) . ?
N5 C8 1.484(4) . ?
N6 N7 1.296(4) . ?
N7 N8 1.360(4) . ?
N8 C7 1.312(4) . ?
C1 H1 0.9500 . ?
C2 C6 1.523(6) . ?
C2 C3 1.526(6) . ?
C2 H2 1.0000 . ?
C3 C4B 1.503(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 C4B 1.437(8) . ?
C5 C6 1.500(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C8 C9 1.514(5) . ?
C8 C12 1.555(6) . ?
C8 H8 1.0000 . ?
C9 C10 1.501(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.463(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.502(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Mn2 O2 2.173(2) 2_765 ?
Mn2 O2 2.173(2) . ?
Mn2 N12 2.243(3) . ?
Mn2 N12 2.243(3) 2_765 ?
Mn2 N16 2.302(2) 2_765 ?
Mn2 N16 2.302(2) . ?
O2 H22 0.84(4) . ?
O2 H21 0.77(5) . ?
N9 C13 1.325(4) . ?
N9 N10 1.344(4) . ?
N9 C14 1.472(4) . ?
N10 N11 1.288(4) . ?
N11 N12 1.361(4) . ?
N12 C13 1.319(4) . ?
N13 C19 1.327(4) . ?
N13 N14 1.346(4) . ?
N13 C20 1.484(4) . ?
N14 N15 1.287(4) . ?
N15 N16 1.363(4) . ?
N16 C19 1.315(4) . ?
C13 H13 0.9500 . ?
C14 C18 1.523(5) . ?
C14 C15 1.530(5) . ?
C14 H14 1.0000 . ?
C15 C16 1.523(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.481(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.522(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
C20 C24 1.497(6) . ?
C20 C21 1.540(6) . ?
C20 H20 1.0000 . ?
C21 C22B 1.582(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C24 C23B 1.396(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
Cl1 O6 1.388(3) . ?
Cl1 O5 1.412(3) . ?
Cl1 O3 1.416(3) . ?
Cl1 O4 1.423(3) . ?
Cl2 O7 1.420(3) . ?
Cl2 O9 1.425(2) . ?
Cl2 O10 1.452(2) . ?
Cl2 O8 1.456(2) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C22B C23B 1.609(10) . ?
C22B H22A 0.9900 . ?
C22B H22B 0.9900 . ?
C23B H23A 0.9900 . ?
C23B H23B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 180.0 2_575 . ?
O1 Mn1 N4 92.00(9) 2_575 . ?
O1 Mn1 N4 88.00(9) . . ?
O1 Mn1 N4 88.00(9) 2_575 2_575 ?
O1 Mn1 N4 92.00(9) . 2_575 ?
N4 Mn1 N4 180.0 . 2_575 ?
O1 Mn1 N8 93.96(9) 2_575 2_575 ?
O1 Mn1 N8 86.04(9) . 2_575 ?
N4 Mn1 N8 91.79(10) . 2_575 ?
N4 Mn1 N8 88.21(10) 2_575 2_575 ?
O1 Mn1 N8 86.04(9) 2_575 . ?
O1 Mn1 N8 93.96(9) . . ?
N4 Mn1 N8 88.21(10) . . ?
N4 Mn1 N8 91.79(10) 2_575 . ?
N8 Mn1 N8 180.0 2_575 . ?
Mn1 O1 H12 123(3) . . ?
Mn1 O1 H11 123(3) . . ?
H12 O1 H11 109(4) . . ?
C1 N1 N2 108.6(3) . . ?
C1 N1 C2 128.5(3) . . ?
N2 N1 C2 122.9(3) . . ?
N3 N2 N1 106.8(3) . . ?
N2 N3 N4 110.0(3) . . ?
C1 N4 N3 105.9(3) . . ?
C1 N4 Mn1 131.2(2) . . ?
N3 N4 Mn1 122.9(2) . . ?
C7 N5 N6 108.2(3) . . ?
C7 N5 C8 129.7(3) . . ?
N6 N5 C8 122.1(3) . . ?
N7 N6 N5 106.5(2) . . ?
N6 N7 N8 110.4(2) . . ?
C7 N8 N7 105.6(3) . . ?
C7 N8 Mn1 125.2(2) . . ?
N7 N8 Mn1 128.3(2) . . ?
N4 C1 N1 108.6(3) . . ?
N4 C1 H1 125.7 . . ?
N1 C1 H1 125.7 . . ?
N1 C2 C6 112.1(3) . . ?
N1 C2 C3 110.5(4) . . ?
C6 C2 C3 104.8(3) . . ?
N1 C2 H2 109.8 . . ?
C6 C2 H2 109.8 . . ?
C3 C2 H2 109.8 . . ?
C4B C3 C2 104.0(4) . . ?
C4B C3 H3A 110.9 . . ?
C2 C3 H3A 110.9 . . ?
C4B C3 H3B 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 109.0 . . ?
C4B C5 C6 107.1(4) . . ?
C4B C5 H5A 110.3 . . ?
C6 C5 H5A 110.3 . . ?
C4B C5 H5B 110.3 . . ?
C6 C5 H5B 110.3 . . ?
H5A C5 H5B 108.6 . . ?
C5 C6 C2 107.3(4) . . ?
C5 C6 H6A 110.2 . . ?
C2 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
C2 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
N8 C7 N5 109.4(3) . . ?
N8 C7 H7 125.3 . . ?
N5 C7 H7 125.3 . . ?
N5 C8 C9 111.4(3) . . ?
N5 C8 C12 110.7(3) . . ?
C9 C8 C12 103.2(3) . . ?
N5 C8 H8 110.5 . . ?
C9 C8 H8 110.5 . . ?
C12 C8 H8 110.5 . . ?
C10 C9 C8 105.9(3) . . ?
C10 C9 H9A 110.5 . . ?
C8 C9 H9A 110.5 . . ?
C10 C9 H9B 110.5 . . ?
C8 C9 H9B 110.5 . . ?
H9A C9 H9B 108.7 . . ?
C11 C10 C9 104.2(4) . . ?
C11 C10 H10A 110.9 . . ?
C9 C10 H10A 110.9 . . ?
C11 C10 H10B 110.9 . . ?
C9 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
C10 C11 C12 106.7(4) . . ?
C10 C11 H11A 110.4 . . ?
C12 C11 H11A 110.4 . . ?
C10 C11 H11B 110.4 . . ?
C12 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C11 C12 C8 106.7(4) . . ?
C11 C12 H12A 110.4 . . ?
C8 C12 H12A 110.4 . . ?
C11 C12 H12B 110.4 . . ?
C8 C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
O2 Mn2 O2 180.0 2_765 . ?
O2 Mn2 N12 86.45(9) 2_765 . ?
O2 Mn2 N12 93.55(9) . . ?
O2 Mn2 N12 93.55(9) 2_765 2_765 ?
O2 Mn2 N12 86.45(9) . 2_765 ?
N12 Mn2 N12 180.0 . 2_765 ?
O2 Mn2 N16 90.18(9) 2_765 2_765 ?
O2 Mn2 N16 89.82(9) . 2_765 ?
N12 Mn2 N16 88.76(9) . 2_765 ?
N12 Mn2 N16 91.24(9) 2_765 2_765 ?
O2 Mn2 N16 89.82(9) 2_765 . ?
O2 Mn2 N16 90.18(9) . . ?
N12 Mn2 N16 91.24(9) . . ?
N12 Mn2 N16 88.76(9) 2_765 . ?
N16 Mn2 N16 180.0 2_765 . ?
Mn2 O2 H22 125(3) . . ?
Mn2 O2 H21 126(4) . . ?
H22 O2 H21 107(4) . . ?
C13 N9 N10 108.6(2) . . ?
C13 N9 C14 130.9(3) . . ?
N10 N9 C14 120.4(2) . . ?
N11 N10 N9 106.9(2) . . ?
N10 N11 N12 110.1(2) . . ?
C13 N12 N11 106.0(2) . . ?
C13 N12 Mn2 135.1(2) . . ?
N11 N12 Mn2 118.79(19) . . ?
C19 N13 N14 108.3(3) . . ?
C19 N13 C20 131.5(3) . . ?
N14 N13 C20 120.1(3) . . ?
N15 N14 N13 106.6(2) . . ?
N14 N15 N16 110.6(2) . . ?
C19 N16 N15 105.4(2) . . ?
C19 N16 Mn2 130.8(2) . . ?
N15 N16 Mn2 123.32(19) . . ?
N12 C13 N9 108.5(3) . . ?
N12 C13 H13 125.8 . . ?
N9 C13 H13 125.8 . . ?
N9 C14 C18 112.7(3) . . ?
N9 C14 C15 113.2(3) . . ?
C18 C14 C15 105.3(3) . . ?
N9 C14 H14 108.5 . . ?
C18 C14 H14 108.5 . . ?
C15 C14 H14 108.5 . . ?
C16 C15 C14 104.8(3) . . ?
C16 C15 H15A 110.8 . . ?
C14 C15 H15A 110.8 . . ?
C16 C15 H15B 110.8 . . ?
C14 C15 H15B 110.8 . . ?
H15A C15 H15B 108.9 . . ?
C17 C16 C15 107.4(3) . . ?
C17 C16 H16A 110.2 . . ?
C15 C16 H16A 110.2 . . ?
C17 C16 H16B 110.2 . . ?
C15 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C16 C17 C18 108.2(3) . . ?
C16 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C17 C18 C14 102.3(3) . . ?
C17 C18 H18A 111.3 . . ?
C14 C18 H18A 111.3 . . ?
C17 C18 H18B 111.3 . . ?
C14 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
N16 C19 N13 109.1(3) . . ?
N16 C19 H19 125.5 . . ?
N13 C19 H19 125.5 . . ?
N13 C20 C24 112.8(3) . . ?
N13 C20 C21 110.9(3) . . ?
C24 C20 C21 112.9(4) . . ?
N13 C20 H20 106.6 . . ?
C24 C20 H20 106.6 . . ?
C21 C20 H20 106.6 . . ?
C20 C21 C22B 101.1(4) . . ?
C20 C21 H21A 111.6 . . ?
C22B C21 H21A 111.6 . . ?
C20 C21 H21B 111.6 . . ?
C22B C21 H21B 111.6 . . ?
H21A C21 H21B 109.4 . . ?
C23B C24 C20 99.2(5) . . ?
C23B C24 H24A 111.9 . . ?
C20 C24 H24A 111.9 . . ?
C23B C24 H24B 111.9 . . ?
C20 C24 H24B 111.9 . . ?
H24A C24 H24B 109.6 . . ?
O6 Cl1 O5 109.3(2) . . ?
O6 Cl1 O3 109.5(3) . . ?
O5 Cl1 O3 110.8(3) . . ?
O6 Cl1 O4 109.5(3) . . ?
O5 Cl1 O4 110.1(2) . . ?
O3 Cl1 O4 107.6(2) . . ?
O7 Cl2 O9 111.33(18) . . ?
O7 Cl2 O10 109.46(17) . . ?
O9 Cl2 O10 109.28(15) . . ?
O7 Cl2 O8 109.76(15) . . ?
O9 Cl2 O8 108.85(15) . . ?
O10 Cl2 O8 108.10(14) . . ?
C5 C4B C3 107.8(6) . . ?
C5 C4B H4B1 110.2 . . ?
C3 C4B H4B1 110.2 . . ?
C5 C4B H4B2 110.2 . . ?
C3 C4B H4B2 110.2 . . ?
H4B1 C4B H4B2 108.5 . . ?
C21 C22B C23B 97.4(4) . . ?
C21 C22B H22A 112.3 . . ?
C23B C22B H22A 112.3 . . ?
C21 C22B H22B 112.3 . . ?
C23B C22B H22B 112.3 . . ?
H22A C22B H22B 109.9 . . ?
C24 C23B C22B 108.1(4) . . ?
C24 C23B H23A 110.1 . . ?
C22B C23B H23A 110.1 . . ?
C24 C23B H23B 110.1 . . ?
C22B C23B H23B 110.1 . . ?
H23A C23B H23B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.2(4) . . . . ?
C2 N1 N2 N3 178.5(3) . . . . ?
N1 N2 N3 N4 0.0(4) . . . . ?
N2 N3 N4 C1 0.2(4) . . . . ?
N2 N3 N4 Mn1 -179.7(2) . . . . ?
C7 N5 N6 N7 0.4(3) . . . . ?
C8 N5 N6 N7 -179.1(3) . . . . ?
N5 N6 N7 N8 -0.1(3) . . . . ?
N6 N7 N8 C7 -0.2(3) . . . . ?
N6 N7 N8 Mn1 169.5(2) . . . . ?
N3 N4 C1 N1 -0.3(3) . . . . ?
Mn1 N4 C1 N1 179.6(2) . . . . ?
N2 N1 C1 N4 0.3(4) . . . . ?
C2 N1 C1 N4 -178.3(3) . . . . ?
C1 N1 C2 C6 131.1(4) . . . . ?
N2 N1 C2 C6 -47.2(5) . . . . ?
C1 N1 C2 C3 -112.3(4) . . . . ?
N2 N1 C2 C3 69.3(4) . . . . ?
N1 C2 C3 C4B -96.8(5) . . . . ?
C6 C2 C3 C4B 24.2(6) . . . . ?
C4B C5 C6 C2 -9.0(7) . . . . ?
N1 C2 C6 C5 110.0(4) . . . . ?
C3 C2 C6 C5 -9.9(5) . . . . ?
N7 N8 C7 N5 0.5(4) . . . . ?
Mn1 N8 C7 N5 -169.6(2) . . . . ?
N6 N5 C7 N8 -0.6(4) . . . . ?
C8 N5 C7 N8 178.9(3) . . . . ?
C7 N5 C8 C9 -62.4(5) . . . . ?
N6 N5 C8 C9 117.0(3) . . . . ?
C7 N5 C8 C12 51.8(5) . . . . ?
N6 N5 C8 C12 -128.7(3) . . . . ?
N5 C8 C9 C10 92.6(4) . . . . ?
C12 C8 C9 C10 -26.2(4) . . . . ?
C8 C9 C10 C11 37.2(5) . . . . ?
C9 C10 C11 C12 -32.9(6) . . . . ?
C10 C11 C12 C8 16.5(6) . . . . ?
N5 C8 C12 C11 -113.1(4) . . . . ?
C9 C8 C12 C11 6.2(5) . . . . ?
C13 N9 N10 N11 0.6(3) . . . . ?
C14 N9 N10 N11 177.3(3) . . . . ?
N9 N10 N11 N12 -0.5(3) . . . . ?
N10 N11 N12 C13 0.2(3) . . . . ?
N10 N11 N12 Mn2 -176.0(2) . . . . ?
C19 N13 N14 N15 0.5(4) . . . . ?
C20 N13 N14 N15 178.1(3) . . . . ?
N13 N14 N15 N16 0.1(3) . . . . ?
N14 N15 N16 C19 -0.6(3) . . . . ?
N14 N15 N16 Mn2 172.0(2) . . . . ?
N11 N12 C13 N9 0.2(3) . . . . ?
Mn2 N12 C13 N9 175.4(2) . . . . ?
N10 N9 C13 N12 -0.5(3) . . . . ?
C14 N9 C13 N12 -176.7(3) . . . . ?
C13 N9 C14 C18 69.2(4) . . . . ?
N10 N9 C14 C18 -106.7(3) . . . . ?
C13 N9 C14 C15 -50.1(5) . . . . ?
N10 N9 C14 C15 134.0(3) . . . . ?
N9 C14 C15 C16 152.2(3) . . . . ?
C18 C14 C15 C16 28.7(4) . . . . ?
C14 C15 C16 C17 -10.8(5) . . . . ?
C15 C16 C17 C18 -11.2(5) . . . . ?
C16 C17 C18 C14 28.5(5) . . . . ?
N9 C14 C18 C17 -158.6(3) . . . . ?
C15 C14 C18 C17 -34.8(4) . . . . ?
N15 N16 C19 N13 0.9(3) . . . . ?
Mn2 N16 C19 N13 -171.0(2) . . . . ?
N14 N13 C19 N16 -0.9(4) . . . . ?
C20 N13 C19 N16 -178.1(3) . . . . ?
C19 N13 C20 C24 22.4(6) . . . . ?
N14 N13 C20 C24 -154.6(4) . . . . ?
C19 N13 C20 C21 -105.4(4) . . . . ?
N14 N13 C20 C21 77.6(4) . . . . ?
N13 C20 C21 C22B 131.6(3) . . . . ?
C24 C20 C21 C22B 3.8(5) . . . . ?
N13 C20 C24 C23B -102.0(5) . . . . ?
C21 C20 C24 C23B 24.7(6) . . . . ?
C6 C5 C4B C3 25.0(8) . . . . ?
C2 C3 C4B C5 -31.0(7) . . . . ?
C20 C21 C22B C23B -26.5(4) . . . . ?
C20 C24 C23B C22B -43.7(6) . . . . ?
C21 C22B C23B C24 46.8(6) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         1.724
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.091

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px324
_database_code_depnum_ccdc_archive 'CCDC 2061088'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-09-23
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) iron(II) diperchlorate'
_chemical_name_common            
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) iron(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C24 H42 Fe N16 O2, C24 H44 Fe N16 O2, 4(Cl O4)'
_chemical_formula_sum            'C48 H86 Cl4 Fe2 N32 O20'
_chemical_formula_weight         1684.98

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9841(4)
_cell_length_b                   11.8637(5)
_cell_length_c                   15.0067(9)
_cell_angle_alpha                112.565(5)
_cell_angle_beta                 90.518(4)
_cell_angle_gamma                96.245(3)
_cell_volume                     1792.38(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    109(2)
_cell_measurement_reflns_used    4427
_cell_measurement_theta_min      2.3000
_cell_measurement_theta_max      30.1290

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.646
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             878
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      109(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            19528
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.868
_diffrn_reflns_theta_max         30.887
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9842
_reflns_number_gt                7128
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²+3.4562P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9842
_refine_ls_number_parameters     518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1709
_refine_ls_wR_factor_gt          0.1482
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0650477000
_diffrn_orient_matrix_UB_12      0.0080103000
_diffrn_orient_matrix_UB_13      0.0019378000
_diffrn_orient_matrix_UB_21      -0.0012670000
_diffrn_orient_matrix_UB_22      -0.0018672000
_diffrn_orient_matrix_UB_23      -0.0478148000
_diffrn_orient_matrix_UB_31      -0.0001163000
_diffrn_orient_matrix_UB_32      0.0647070000
_diffrn_orient_matrix_UB_33      0.0183800000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00 -20.00   1.00   12.00    --   20.19 -57.00 -30.00   27
  2  ω     -5.00  37.00   1.00   12.00    --   20.19 -57.00 -30.00   42
  3  ω     -7.00  31.00   1.00   12.00    --   20.19  77.00-150.00   38
  4  ω     -7.00  31.00   1.00   12.00    --   20.19  77.00  90.00   38
  5  ω    -44.00  37.00   1.00   12.00    --   20.19 -57.00-150.00   81
  6  ω     -7.00  34.00   1.00   12.00    --   20.19  77.00 -30.00   41
  7  ω    -47.00  37.00   1.00   12.00    --   20.19 -57.00  90.00   84
  8  ω    -44.00   4.00   1.00   12.00    --   20.19 -37.00 -30.00   48
  9  ω     66.00  91.00   1.00   12.00    --   20.19 178.00   0.00   25
 10  ω     32.00  57.00   1.00   12.00    --   20.19  57.00 120.00   25
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.500000 0.500000 0.01381(13) Uani 1 2 d S . P . .
O1 O 0.3971(2) 0.6387(2) 0.50256(18) 0.0195(4) Uani 1 1 d . . . . .
N4 N 0.4277(2) 0.3977(2) 0.35158(18) 0.0179(5) Uani 1 1 d . . . . .
N3 N 0.3269(3) 0.3127(3) 0.3362(2) 0.0277(6) Uani 1 1 d . . . . .
N2 N 0.2889(3) 0.2695(3) 0.2464(2) 0.0298(7) Uani 1 1 d . . . . .
N1 N 0.3641(2) 0.3264(2) 0.20184(18) 0.0208(5) Uani 1 1 d . . . . .
N8 N 0.3417(2) 0.4266(2) 0.56202(18) 0.0162(5) Uani 1 1 d . . . . .
N7 N 0.3008(2) 0.3066(2) 0.54203(18) 0.0180(5) Uani 1 1 d . . . . .
N6 N 0.1999(2) 0.2973(2) 0.58401(19) 0.0201(5) Uani 1 1 d . . . . .
N5 N 0.1740(2) 0.4128(2) 0.63259(18) 0.0173(5) Uani 1 1 d . . . . .
C1 C 0.4490(3) 0.4044(3) 0.2669(2) 0.0191(6) Uani 1 1 d . . . . .
C7 C 0.2610(3) 0.4902(3) 0.6184(2) 0.0185(6) Uani 1 1 d . . . . .
H7 H 0.264490 0.577264 0.644660 0.022 Uiso 1 1 calc R U . . .
C8 C 0.0632(3) 0.4343(3) 0.6900(2) 0.0217(6) Uani 1 1 d . . . . .
H8 H 0.059652 0.386946 0.732733 0.026 Uiso 1 1 calc R U . . .
C11 C -0.0042(4) 0.6194(4) 0.6865(4) 0.0456(11) Uani 1 1 d . . . . .
H11A H 0.048097 0.629926 0.636241 0.055 Uiso 1 1 calc R U . A 1
H11B H -0.035258 0.698193 0.724798 0.055 Uiso 1 1 calc R U . A 1
C12 C 0.0624(3) 0.5701(3) 0.7500(3) 0.0299(8) Uani 1 1 d . . . . .
H12A H 0.019023 0.582290 0.809936 0.036 Uiso 1 1 calc R U . . .
H12B H 0.147193 0.612195 0.767656 0.036 Uiso 1 1 calc R U . . .
C9 C -0.0527(3) 0.3975(3) 0.6233(3) 0.0321(8) Uani 1 1 d . . . . .
H9A H -0.031248 0.361652 0.554922 0.039 Uiso 1 1 calc R U . B 1
H9B H -0.108741 0.335317 0.636605 0.039 Uiso 1 1 calc R U . B 1
Fe2 Fe 0.500000 1.000000 0.500000 0.01484(14) Uani 1 2 d S . P . .
O2 O 0.4331(2) 1.1136(2) 0.43791(18) 0.0196(4) Uani 1 1 d . . . . .
N12 N 0.6770(2) 1.0174(2) 0.44178(18) 0.0182(5) Uani 1 1 d . . . . .
N11 N 0.7639(2) 1.1171(2) 0.4817(2) 0.0228(5) Uani 1 1 d . . . . .
N10 N 0.8621(2) 1.0985(2) 0.4346(2) 0.0243(6) Uani 1 1 d . . . . .
N9 N 0.8393(2) 0.9855(2) 0.3626(2) 0.0244(6) Uani 1 1 d . . . . .
N16 N 0.4378(2) 0.8410(2) 0.36152(18) 0.0183(5) Uani 1 1 d . . . . .
N15 N 0.3949(2) 0.7256(2) 0.35359(18) 0.0185(5) Uani 1 1 d . . . . .
N14 N 0.3449(3) 0.6612(2) 0.26799(19) 0.0217(5) Uani 1 1 d . . . . .
N13 N 0.3550(2) 0.7349(2) 0.21836(18) 0.0194(5) Uani 1 1 d . . . . .
C13 C 0.7270(3) 0.9378(3) 0.3688(2) 0.0212(6) Uani 1 1 d . . . . .
H13 H 0.688701 0.858954 0.327313 0.025 Uiso 1 1 calc R U . . .
C14 C 0.9274(3) 0.9315(4) 0.2874(3) 0.0377(9) Uani 1 1 d . . . . .
H14 H 0.884588 0.860136 0.231676 0.045 Uiso 1 1 calc R U . . .
C15 C 0.9936(4) 1.0318(4) 0.2507(3) 0.0363(8) Uani 1 1 d . . . . .
H15A H 1.014095 0.993369 0.182282 0.044 Uiso 1 1 calc R U . . .
H15B H 0.941406 1.097377 0.257861 0.044 Uiso 1 1 calc R U . . .
C16 C 1.1087(3) 1.0818(4) 0.3172(3) 0.0330(8) Uani 1 1 d . . . . .
H16A H 1.105497 1.168917 0.359834 0.040 Uiso 1 1 calc R U . . .
H16B H 1.182159 1.076787 0.278798 0.040 Uiso 1 1 calc R U . . .
C17 C 1.1150(4) 1.0039(4) 0.3778(3) 0.0389(9) Uani 1 1 d . . . . .
H17A H 1.199388 0.982872 0.380710 0.047 Uiso 1 1 calc R U . . .
H17B H 1.091959 1.049924 0.444535 0.047 Uiso 1 1 calc R U . . .
C18 C 1.0290(4) 0.8914(4) 0.3313(3) 0.0410(9) Uani 1 1 d . . . . .
H18A H 0.997594 0.858715 0.379325 0.049 Uiso 1 1 calc R U . . .
H18B H 1.068963 0.827280 0.280928 0.049 Uiso 1 1 calc R U . . .
C19 C 0.4124(3) 0.8435(3) 0.2761(2) 0.0193(6) Uani 1 1 d . . . . .
H19 H 0.432090 0.912088 0.258700 0.023 Uiso 1 1 calc R U . . .
C20 C 0.3068(3) 0.6909(3) 0.1173(2) 0.0302(8) Uani 1 1 d . . . . .
H20 H 0.364315 0.637979 0.073667 0.036 Uiso 1 1 calc R U . . .
C21 C 0.1797(4) 0.6201(4) 0.1014(3) 0.0376(9) Uani 1 1 d . . . . .
H21A H 0.184568 0.530435 0.072731 0.045 Uiso 1 1 calc R U . . .
H21B H 0.139360 0.640208 0.163402 0.045 Uiso 1 1 calc R U . . .
C22 C 0.1094(4) 0.6581(6) 0.0337(4) 0.0578(13) Uani 1 1 d . . . . .
H22A H 0.082695 0.585633 -0.026185 0.069 Uiso 1 1 calc R U . . .
H22B H 0.035525 0.693594 0.064353 0.069 Uiso 1 1 calc R U . . .
C23 C 0.1892(5) 0.7502(6) 0.0104(4) 0.0646(15) Uani 1 1 d . . . . .
H23A H 0.142758 0.817012 0.009962 0.077 Uiso 1 1 calc R U . . .
H23B H 0.223000 0.711730 -0.053790 0.077 Uiso 1 1 calc R U . . .
C24 C 0.2894(6) 0.7991(5) 0.0876(4) 0.072(2) Uani 1 1 d . . . . .
H24A H 0.265984 0.869833 0.143161 0.087 Uiso 1 1 calc R U . . .
H24B H 0.365719 0.825739 0.062778 0.087 Uiso 1 1 calc R U . . .
Cl1 Cl 0.66699(8) 0.60210(8) 0.15042(6) 0.02609(18) Uani 1 1 d . . . . .
O4 O 0.7933(3) 0.6399(3) 0.1478(2) 0.0470(8) Uani 1 1 d . . . . .
Cl2 Cl 0.63248(7) 0.13451(7) 0.23944(5) 0.02221(16) Uani 1 1 d . . . . .
O7 O 0.5045(2) 0.1148(2) 0.25916(19) 0.0328(6) Uani 1 1 d . . . . .
O8 O 0.6999(2) 0.2124(2) 0.32945(18) 0.0309(5) Uani 1 1 d . . . . .
O9 O 0.6801(3) 0.0194(2) 0.2020(2) 0.0431(7) Uani 1 1 d . . . . .
O10 O 0.6430(3) 0.1943(3) 0.1733(2) 0.0429(7) Uani 1 1 d . . . . .
C10A C -0.1134(6) 0.5096(6) 0.6413(6) 0.0446(18) Uani 0.649(6) 1 d . . P C 1
H10A H -0.179014 0.516264 0.687193 0.054 Uiso 0.649(6) 1 calc R U P C 1
H10B H -0.149085 0.509274 0.580348 0.054 Uiso 0.649(6) 1 calc R U P C 1
O3A O 0.6166(6) 0.6628(6) 0.2410(5) 0.058(2) Uiso 0.649(6) 1 d . . P C 1
O5A O 0.5987(6) 0.5926(11) 0.0718(5) 0.094(3) Uani 0.649(6) 1 d . . P C 1
O6A O 0.6647(6) 0.4708(5) 0.1410(6) 0.072(2) Uani 0.649(6) 1 d . . P C 1
C10B C -0.0517(9) 0.5126(11) 0.5927(8) 0.032(3) Uani 0.351(6) 1 d . . P C 2
H10C H 0.003934 0.506064 0.539857 0.039 Uiso 0.351(6) 1 calc R U P C 2
H10D H -0.135088 0.521132 0.572326 0.039 Uiso 0.351(6) 1 calc R U P C 2
O3B O 0.6307(7) 0.6380(7) 0.2501(5) 0.0188(16) Uiso 0.351(6) 1 d . . P C 2
O5B O 0.6166(12) 0.6978(17) 0.1248(15) 0.097(6) Uani 0.351(6) 1 d . . P C 2
O6B O 0.6081(13) 0.4897(10) 0.0959(11) 0.072(2) Uani 0.351(6) 1 d . . P C 2
C2 C 0.3471(3) 0.2972(3) 0.0968(2) 0.0282(7) Uani 1 1 d . . . . .
H2 H 0.394006 0.362091 0.079198 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2128(4) 0.2805(4) 0.0655(3) 0.0397(10) Uani 1 1 d . . . . .
H3A H 0.164561 0.325482 0.120527 0.048 Uiso 1 1 calc R U . . .
H3B H 0.201470 0.310907 0.013398 0.048 Uiso 1 1 calc R U . . .
C6 C 0.3848(6) 0.1713(6) 0.0379(3) 0.077(2) Uani 1 1 d . . . . .
H6A H 0.404582 0.164420 -0.028120 0.092 Uiso 1 1 calc R U . . .
H6B H 0.457180 0.155830 0.069364 0.092 Uiso 1 1 calc R U . . .
C5 C 0.2760(12) 0.0841(5) 0.0351(4) 0.123(4) Uani 1 1 d . . . . .
H5A H 0.275186 0.006081 -0.022023 0.147 Uiso 1 1 calc R U . . .
H5B H 0.275808 0.065837 0.094139 0.147 Uiso 1 1 calc R U . . .
C4 C 0.1739(8) 0.1440(8) 0.0294(6) 0.116(4) Uani 1 1 d . . . . .
H4A H 0.108780 0.126781 0.069221 0.139 Uiso 1 1 calc R U . . .
H4B H 0.140637 0.113016 -0.038328 0.139 Uiso 1 1 calc R U . . .
H1B H 0.370(3) 0.688(4) 0.550(3) 0.022(10) Uiso 1 1 d . . . . .
H1A H 0.402(4) 0.658(4) 0.462(3) 0.034(12) Uiso 1 1 d . . . . .
H2B H 0.460(4) 1.117(4) 0.389(4) 0.041(13) Uiso 1 1 d . . . . .
H2A H 0.401(4) 1.162(4) 0.464(3) 0.035(13) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.085(2) 2_666 ?
Fe1 O1 2.085(2) . ?
Fe1 N4 2.179(2) . ?
Fe1 N4 2.179(2) 2_666 ?
Fe1 N8 2.230(2) . ?
Fe1 N8 2.230(2) 2_666 ?
N4 C1 1.324(4) . ?
N4 N3 1.368(4) . ?
N3 N2 1.291(4) . ?
N2 N1 1.348(4) . ?
N1 C1 1.335(4) . ?
N1 C2 1.484(4) . ?
N8 C7 1.319(4) . ?
N8 N7 1.359(3) . ?
N7 N6 1.295(4) . ?
N6 N5 1.347(3) . ?
N5 C7 1.328(4) . ?
N5 C8 1.485(4) . ?
C8 C12 1.515(5) . ?
C8 C9 1.529(5) . ?
C11 C12 1.515(6) . ?
C11 C10B 1.528(12) . ?
C11 C10A 1.601(8) . ?
C9 C10A 1.485(7) . ?
C9 C10B 1.598(11) . ?
Fe2 O2 2.096(2) . ?
Fe2 O2 2.096(2) 2_676 ?
Fe2 N12 2.161(3) 2_676 ?
Fe2 N12 2.161(3) . ?
Fe2 N16 2.242(2) . ?
Fe2 N16 2.242(2) 2_676 ?
N12 C13 1.313(4) . ?
N12 N11 1.367(4) . ?
N11 N10 1.287(4) . ?
N10 N9 1.356(4) . ?
N9 C13 1.320(4) . ?
N9 C14 1.490(5) . ?
N16 C19 1.322(4) . ?
N16 N15 1.359(3) . ?
N15 N14 1.295(4) . ?
N14 N13 1.346(4) . ?
N13 C19 1.329(4) . ?
N13 C20 1.473(4) . ?
C14 C18 1.499(6) . ?
C14 C15 1.602(6) . ?
C15 C16 1.519(5) . ?
C16 C17 1.530(5) . ?
C17 C18 1.470(6) . ?
C20 C21 1.515(5) . ?
C20 C24 1.541(6) . ?
C21 C22 1.498(6) . ?
C22 C23 1.475(7) . ?
C23 C24 1.487(7) . ?
Cl1 O5A 1.353(5) . ?
Cl1 O6B 1.353(12) . ?
Cl1 O4 1.417(3) . ?
Cl1 O3A 1.422(7) . ?
Cl1 O3B 1.461(7) . ?
Cl1 O5B 1.488(10) . ?
Cl1 O6A 1.506(6) . ?
Cl2 O9 1.423(3) . ?
Cl2 O10 1.423(3) . ?
Cl2 O8 1.450(3) . ?
Cl2 O7 1.452(3) . ?
C2 C3 1.512(5) . ?
C2 C6 1.520(6) . ?
C3 C4 1.507(9) . ?
C6 C5 1.483(11) . ?
C5 C4 1.409(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 180.0 2_666 . ?
O1 Fe1 N4 92.65(9) 2_666 . ?
O1 Fe1 N4 87.35(9) . . ?
O1 Fe1 N4 87.35(9) 2_666 2_666 ?
O1 Fe1 N4 92.65(9) . 2_666 ?
N4 Fe1 N4 180.00(12) . 2_666 ?
O1 Fe1 N8 92.57(9) 2_666 . ?
O1 Fe1 N8 87.43(9) . . ?
N4 Fe1 N8 93.30(9) . . ?
N4 Fe1 N8 86.70(9) 2_666 . ?
O1 Fe1 N8 87.43(9) 2_666 2_666 ?
O1 Fe1 N8 92.57(9) . 2_666 ?
N4 Fe1 N8 86.70(9) . 2_666 ?
N4 Fe1 N8 93.30(9) 2_666 2_666 ?
N8 Fe1 N8 180.0 . 2_666 ?
C1 N4 N3 106.2(2) . . ?
C1 N4 Fe1 135.5(2) . . ?
N3 N4 Fe1 117.80(19) . . ?
N2 N3 N4 109.9(3) . . ?
N3 N2 N1 107.1(3) . . ?
C1 N1 N2 108.6(3) . . ?
C1 N1 C2 130.1(3) . . ?
N2 N1 C2 121.4(3) . . ?
C7 N8 N7 105.5(2) . . ?
C7 N8 Fe1 126.9(2) . . ?
N7 N8 Fe1 127.29(18) . . ?
N6 N7 N8 110.6(2) . . ?
N7 N6 N5 106.4(2) . . ?
C7 N5 N6 108.4(2) . . ?
C7 N5 C8 131.6(3) . . ?
N6 N5 C8 120.0(2) . . ?
N4 C1 N1 108.2(3) . . ?
N8 C7 N5 109.0(3) . . ?
N5 C8 C12 110.8(3) . . ?
N5 C8 C9 110.5(3) . . ?
C12 C8 C9 104.8(3) . . ?
C12 C11 C10B 109.0(4) . . ?
C12 C11 C10A 99.4(4) . . ?
C11 C12 C8 105.5(3) . . ?
C10A C9 C8 108.1(4) . . ?
C8 C9 C10B 101.4(4) . . ?
O2 Fe2 O2 180.00(12) . 2_676 ?
O2 Fe2 N12 89.15(10) . 2_676 ?
O2 Fe2 N12 90.85(10) 2_676 2_676 ?
O2 Fe2 N12 90.85(10) . . ?
O2 Fe2 N12 89.15(10) 2_676 . ?
N12 Fe2 N12 180.0 2_676 . ?
O2 Fe2 N16 87.25(9) . . ?
O2 Fe2 N16 92.75(9) 2_676 . ?
N12 Fe2 N16 90.90(9) 2_676 . ?
N12 Fe2 N16 89.10(9) . . ?
O2 Fe2 N16 92.75(9) . 2_676 ?
O2 Fe2 N16 87.25(9) 2_676 2_676 ?
N12 Fe2 N16 89.10(9) 2_676 2_676 ?
N12 Fe2 N16 90.90(9) . 2_676 ?
N16 Fe2 N16 180.00(11) . 2_676 ?
C13 N12 N11 106.2(3) . . ?
C13 N12 Fe2 129.7(2) . . ?
N11 N12 Fe2 123.97(19) . . ?
N10 N11 N12 109.9(2) . . ?
N11 N10 N9 106.5(2) . . ?
C13 N9 N10 108.6(3) . . ?
C13 N9 C14 127.6(3) . . ?
N10 N9 C14 123.7(3) . . ?
C19 N16 N15 105.3(2) . . ?
C19 N16 Fe2 128.0(2) . . ?
N15 N16 Fe2 125.43(19) . . ?
N14 N15 N16 110.6(2) . . ?
N15 N14 N13 106.7(2) . . ?
C19 N13 N14 108.1(2) . . ?
C19 N13 C20 130.6(3) . . ?
N14 N13 C20 121.3(3) . . ?
N12 C13 N9 108.7(3) . . ?
N9 C14 C18 109.0(3) . . ?
N9 C14 C15 111.7(3) . . ?
C18 C14 C15 105.0(3) . . ?
C16 C15 C14 102.7(3) . . ?
C15 C16 C17 107.7(3) . . ?
C18 C17 C16 107.4(4) . . ?
C17 C18 C14 104.3(3) . . ?
N16 C19 N13 109.2(3) . . ?
N13 C20 C21 112.5(3) . . ?
N13 C20 C24 111.3(3) . . ?
C21 C20 C24 103.8(3) . . ?
C22 C21 C20 106.4(3) . . ?
C23 C22 C21 108.8(4) . . ?
C22 C23 C24 105.7(4) . . ?
C23 C24 C20 104.9(4) . . ?
O5A Cl1 O4 113.9(3) . . ?
O6B Cl1 O4 125.0(5) . . ?
O5A Cl1 O3A 115.6(5) . . ?
O4 Cl1 O3A 114.1(3) . . ?
O6B Cl1 O3B 109.4(6) . . ?
O4 Cl1 O3B 110.8(3) . . ?
O6B Cl1 O5B 110.1(10) . . ?
O4 Cl1 O5B 98.2(5) . . ?
O3B Cl1 O5B 100.0(7) . . ?
O5A Cl1 O6A 103.6(5) . . ?
O4 Cl1 O6A 103.2(3) . . ?
O3A Cl1 O6A 104.6(4) . . ?
O9 Cl2 O10 111.26(19) . . ?
O9 Cl2 O8 109.01(16) . . ?
O10 Cl2 O8 109.20(17) . . ?
O9 Cl2 O7 109.27(18) . . ?
O10 Cl2 O7 109.62(16) . . ?
O8 Cl2 O7 108.43(15) . . ?
C9 C10A C11 103.6(4) . . ?
C11 C10B C9 101.8(6) . . ?
N1 C2 C3 111.5(3) . . ?
N1 C2 C6 110.8(3) . . ?
C3 C2 C6 102.0(4) . . ?
C4 C3 C2 105.1(5) . . ?
C5 C6 C2 104.2(5) . . ?
C4 C5 C6 105.3(5) . . ?
C5 C4 C3 109.3(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 0.2(4) . . . . ?
Fe1 N4 N3 N2 173.7(2) . . . . ?
N4 N3 N2 N1 -0.4(4) . . . . ?
N3 N2 N1 C1 0.4(4) . . . . ?
N3 N2 N1 C2 179.4(3) . . . . ?
C7 N8 N7 N6 0.1(3) . . . . ?
Fe1 N8 N7 N6 -173.88(19) . . . . ?
N8 N7 N6 N5 -0.1(3) . . . . ?
N7 N6 N5 C7 0.1(3) . . . . ?
N7 N6 N5 C8 -179.3(3) . . . . ?
N3 N4 C1 N1 0.1(3) . . . . ?
Fe1 N4 C1 N1 -171.7(2) . . . . ?
N2 N1 C1 N4 -0.3(4) . . . . ?
C2 N1 C1 N4 -179.1(3) . . . . ?
N7 N8 C7 N5 0.0(3) . . . . ?
Fe1 N8 C7 N5 173.99(19) . . . . ?
N6 N5 C7 N8 0.0(3) . . . . ?
C8 N5 C7 N8 179.3(3) . . . . ?
C7 N5 C8 C12 -7.7(5) . . . . ?
N6 N5 C8 C12 171.6(3) . . . . ?
C7 N5 C8 C9 107.9(4) . . . . ?
N6 N5 C8 C9 -72.8(4) . . . . ?
C10B C11 C12 C8 4.4(6) . . . . ?
C10A C11 C12 C8 41.9(4) . . . . ?
N5 C8 C12 C11 89.9(3) . . . . ?
C9 C8 C12 C11 -29.2(4) . . . . ?
N5 C8 C9 C10A -116.6(4) . . . . ?
C12 C8 C9 C10A 2.8(5) . . . . ?
N5 C8 C9 C10B -77.9(5) . . . . ?
C12 C8 C9 C10B 41.5(5) . . . . ?
C13 N12 N11 N10 0.2(3) . . . . ?
Fe2 N12 N11 N10 176.4(2) . . . . ?
N12 N11 N10 N9 0.3(3) . . . . ?
N11 N10 N9 C13 -0.6(4) . . . . ?
N11 N10 N9 C14 176.2(3) . . . . ?
C19 N16 N15 N14 -0.5(3) . . . . ?
Fe2 N16 N15 N14 167.8(2) . . . . ?
N16 N15 N14 N13 0.1(3) . . . . ?
N15 N14 N13 C19 0.4(3) . . . . ?
N15 N14 N13 C20 -179.8(3) . . . . ?
N11 N12 C13 N9 -0.6(4) . . . . ?
Fe2 N12 C13 N9 -176.5(2) . . . . ?
N10 N9 C13 N12 0.7(4) . . . . ?
C14 N9 C13 N12 -175.9(3) . . . . ?
C13 N9 C14 C18 -108.9(4) . . . . ?
N10 N9 C14 C18 74.9(4) . . . . ?
C13 N9 C14 C15 135.4(4) . . . . ?
N10 N9 C14 C15 -40.8(5) . . . . ?
N9 C14 C15 C16 91.8(4) . . . . ?
C18 C14 C15 C16 -26.3(4) . . . . ?
C14 C15 C16 C17 6.8(4) . . . . ?
C15 C16 C17 C18 15.5(4) . . . . ?
C16 C17 C18 C14 -32.4(4) . . . . ?
N9 C14 C18 C17 -83.5(4) . . . . ?
C15 C14 C18 C17 36.3(4) . . . . ?
N15 N16 C19 N13 0.7(3) . . . . ?
Fe2 N16 C19 N13 -167.2(2) . . . . ?
N14 N13 C19 N16 -0.7(4) . . . . ?
C20 N13 C19 N16 179.5(3) . . . . ?
C19 N13 C20 C21 -135.4(4) . . . . ?
N14 N13 C20 C21 44.9(4) . . . . ?
C19 N13 C20 C24 -19.4(6) . . . . ?
N14 N13 C20 C24 160.9(4) . . . . ?
N13 C20 C21 C22 140.1(4) . . . . ?
C24 C20 C21 C22 19.6(5) . . . . ?
C20 C21 C22 C23 -1.0(6) . . . . ?
C21 C22 C23 C24 -18.9(7) . . . . ?
C22 C23 C24 C20 31.0(7) . . . . ?
N13 C20 C24 C23 -152.6(4) . . . . ?
C21 C20 C24 C23 -31.3(6) . . . . ?
C8 C9 C10A C11 22.9(6) . . . . ?
C12 C11 C10A C9 -39.5(6) . . . . ?
C12 C11 C10B C9 20.7(7) . . . . ?
C8 C9 C10B C11 -37.5(6) . . . . ?
C1 N1 C2 C3 -140.9(4) . . . . ?
N2 N1 C2 C3 40.4(5) . . . . ?
C1 N1 C2 C6 106.3(5) . . . . ?
N2 N1 C2 C6 -72.4(5) . . . . ?
N1 C2 C3 C4 -94.9(5) . . . . ?
C6 C2 C3 C4 23.4(5) . . . . ?
N1 C2 C6 C5 82.5(5) . . . . ?
C3 C2 C6 C5 -36.2(5) . . . . ?
C2 C6 C5 C4 36.0(6) . . . . ?
C6 C5 C4 C3 -21.0(7) . . . . ?
C2 C3 C4 C5 -2.1(7) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         1.723
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.107

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_px273
_database_code_depnum_ccdc_archive 'CCDC 2061085'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             2020-07-27
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
' diazido 1-cyclopropyl-5H-tetrazole copper(II) '
_chemical_name_common            ' 1-cyclopropyl-5H-tetrazole copper(II) azide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H20 Cu2 N20'
_chemical_formula_sum            'C12 H20 Cu2 N20'
_chemical_formula_weight         571.56

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2935(15)
_cell_length_b                   10.817(2)
_cell_length_c                   16.387(3)
_cell_angle_alpha                75.106(16)
_cell_angle_beta                 82.860(18)
_cell_angle_gamma                89.884(17)
_cell_volume                     1069.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    112(2)
_cell_measurement_reflns_used    637
_cell_measurement_theta_min      3.7270
_cell_measurement_theta_max      24.3490

_exptl_crystal_description       platelet
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.039
_shelx_estimated_absorpt_T_min   0.580
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_F_000             580
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      112(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            6103
_diffrn_reflns_av_unetI/netI     0.1819
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.1598
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.594
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4320
_reflns_number_gt                2317
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4320
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.1643
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0388119000
_diffrn_orient_matrix_UB_12      -0.0201491000
_diffrn_orient_matrix_UB_13      0.0440207000
_diffrn_orient_matrix_UB_21      -0.1061015000
_diffrn_orient_matrix_UB_22      -0.0023825000
_diffrn_orient_matrix_UB_23      -0.0100322000
_diffrn_orient_matrix_UB_31      0.0122573000
_diffrn_orient_matrix_UB_32      -0.0647847000
_diffrn_orient_matrix_UB_33      -0.0010751000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  50.00   1.00   70.00    --  -20.37  57.00 -30.00   94
  2  ω    -90.00   3.00   1.00   70.00    --  -20.37 -57.00-180.00   93
  3  ω     -2.00  92.00   1.00   70.00    --   21.23  57.00  90.00   94
  4  ω    -12.00  29.00   1.00   70.00    --   21.23  77.00-180.00   41
;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.94451(16) 0.11514(9) 0.53909(7) 0.0173(3) Uani 1 1 d . . . . .
Cu2 Cu 0.47259(15) 0.38363(9) 0.46317(7) 0.0172(3) Uani 1 1 d . . . . .
N4 N 0.9410(10) 0.1475(6) 0.6525(5) 0.0148(16) Uani 1 1 d . . . . .
N3 N 0.8853(11) 0.0644(6) 0.7287(5) 0.0226(18) Uani 1 1 d . . . . .
N2 N 0.8987(10) 0.1178(6) 0.7906(5) 0.0210(18) Uani 1 1 d . . . . .
N1 N 0.9662(10) 0.2398(6) 0.7523(5) 0.0150(16) Uani 1 1 d . . . . .
N5 N 0.8366(11) 0.2920(7) 0.4914(5) 0.0232(18) Uani 1 1 d . . . . .
N6 N 0.9719(10) 0.3722(6) 0.4513(5) 0.0167(17) Uani 1 1 d . . . . .
N7 N 1.0934(11) 0.4496(7) 0.4144(5) 0.029(2) Uani 1 1 d . . . . .
N8 N 0.9681(10) 0.0686(6) 0.4283(5) 0.0182(17) Uani 1 1 d . . . . .
N9 N 0.9785(10) 0.1473(7) 0.3601(5) 0.0190(18) Uani 1 1 d . . . . .
N10 N 0.9819(11) 0.2219(7) 0.2968(5) 0.0271(19) Uani 1 1 d . . . . .
N14 N 0.5226(9) 0.3494(6) 0.3489(4) 0.0130(15) Uani 1 1 d . . . . .
N13 N 0.6087(11) 0.4332(6) 0.2744(5) 0.0218(18) Uani 1 1 d . . . . .
N12 N 0.6085(10) 0.3796(6) 0.2118(5) 0.0182(17) Uani 1 1 d . . . . .
N11 N 0.5239(10) 0.2625(6) 0.2449(5) 0.0182(17) Uani 1 1 d . . . . .
N15 N 0.5744(10) 0.5675(6) 0.4259(5) 0.0164(17) Uani 1 1 d . . . . .
N16 N 0.5333(10) 0.6441(7) 0.3617(5) 0.0161(17) Uani 1 1 d . . . . .
N17 N 0.5034(11) 0.7198(7) 0.3009(6) 0.027(2) Uani 1 1 d . . . . .
C1 C 0.9865(11) 0.2555(8) 0.6699(6) 0.018(2) Uani 1 1 d . . . . .
H1 H 1.028014 0.333591 0.628604 0.022 Uiso 1 1 calc R U . . .
C2 C 0.9921(13) 0.3332(8) 0.8040(6) 0.022(2) Uani 1 1 d . . . . .
H2 H 1.062622 0.412888 0.764740 0.027 Uiso 1 1 calc R U . . .
C3 C 1.1241(15) 0.2892(9) 0.8740(7) 0.035(3) Uani 1 1 d . . . . .
H3A H 1.278481 0.302801 0.852291 0.042 Uiso 1 1 calc R U . . .
H3B H 1.095246 0.197100 0.901872 0.042 Uiso 1 1 calc R U . . .
C4 C 1.0582(15) 0.3701(9) 0.9363(6) 0.036(3) Uani 1 1 d . . . . .
H4A H 1.173289 0.433673 0.934000 0.043 Uiso 1 1 calc R U . . .
H4B H 1.029321 0.315196 0.995216 0.043 Uiso 1 1 calc R U . . .
C5 C 0.8554(15) 0.4375(10) 0.9087(7) 0.043(3) Uani 1 1 d . . . . .
H5A H 0.886247 0.529591 0.881505 0.051 Uiso 1 1 calc R U . . .
H5B H 0.743376 0.428717 0.958106 0.051 Uiso 1 1 calc R U . . .
C6 C 0.7831(15) 0.3690(11) 0.8444(7) 0.046(3) Uani 1 1 d . . . . .
H6A H 0.691142 0.292396 0.873578 0.056 Uiso 1 1 calc R U . . .
H6B H 0.704975 0.427156 0.801943 0.056 Uiso 1 1 calc R U . . .
C7 C 0.4733(12) 0.2437(8) 0.3274(6) 0.0167(19) Uani 1 1 d . . . . .
H7 H 0.411620 0.167057 0.365508 0.020 Uiso 1 1 calc R U . . .
C8 C 0.5018(13) 0.1707(8) 0.1934(6) 0.024(2) Uani 1 1 d . . . . .
H8 H 0.427099 0.090935 0.230821 0.028 Uiso 1 1 calc R U . . .
C9 C 0.7140(15) 0.1355(10) 0.1515(7) 0.045(3) Uani 1 1 d . . . . .
H9A H 0.806204 0.212386 0.123239 0.054 Uiso 1 1 calc R U . . .
H9B H 0.792071 0.075811 0.193141 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6415(16) 0.0718(11) 0.0875(8) 0.050(3) Uani 1 1 d . . . . .
H10A H 0.613389 -0.020805 0.113551 0.061 Uiso 1 1 calc R U . . .
H10B H 0.753455 0.082500 0.037887 0.061 Uiso 1 1 calc R U . . .
C11 C 0.4389(15) 0.1351(9) 0.0598(7) 0.036(3) Uani 1 1 d . . . . .
H11A H 0.323574 0.070173 0.065549 0.043 Uiso 1 1 calc R U . . .
H11B H 0.464385 0.186015 -0.000264 0.043 Uiso 1 1 calc R U . . .
C12 C 0.3784(15) 0.2211(9) 0.1185(7) 0.034(3) Uani 1 1 d . . . . .
H12A H 0.420726 0.311377 0.089744 0.041 Uiso 1 1 calc R U . . .
H12B H 0.222218 0.215280 0.137299 0.041 Uiso 1 1 calc R U . . .
N19 N 0.4427(11) 0.1294(7) 0.5507(5) 0.0188(17) Uani 1 1 d . . . . .
N18 N 0.3308(10) 0.2100(7) 0.5141(5) 0.0215(17) Uani 1 1 d . . . . .
N20 N 0.5456(11) 0.0496(7) 0.5868(5) 0.028(2) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 1.976(7) . ?
Cu1 N8 1.994(7) . ?
Cu1 N8 2.015(7) 2_756 ?
Cu1 N5 2.023(7) . ?
Cu2 N14 1.989(7) . ?
Cu2 N15 2.006(6) . ?
Cu2 N15 2.008(7) 2_666 ?
Cu2 N18 2.009(7) . ?
N4 C1 1.311(9) . ?
N4 N3 1.343(9) . ?
N3 N2 1.302(9) . ?
N2 N1 1.352(9) . ?
N1 C1 1.308(10) . ?
N1 C2 1.496(9) . ?
N5 N6 1.216(9) . ?
N6 N7 1.131(9) . ?
N8 N9 1.212(10) . ?
N9 N10 1.138(10) . ?
N14 C7 1.327(9) . ?
N14 N13 1.369(9) . ?
N13 N12 1.302(9) . ?
N12 N11 1.327(8) . ?
N11 C7 1.312(10) . ?
N11 C8 1.476(9) . ?
N15 N16 1.216(10) . ?
N16 N17 1.151(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.479(12) . ?
C2 C6 1.494(12) . ?
C2 H2 1.0000 . ?
C3 C4 1.528(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.528(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.545(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C8 C12 1.515(12) . ?
C8 C9 1.518(12) . ?
C8 H8 1.0000 . ?
C9 C10 1.508(12) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.510(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.518(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N19 N20 1.160(9) . ?
N19 N18 1.204(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N8 174.3(3) . . ?
N4 Cu1 N8 97.1(3) . 2_756 ?
N8 Cu1 N8 77.7(3) . 2_756 ?
N4 Cu1 N5 91.1(3) . . ?
N8 Cu1 N5 94.2(3) . . ?
N8 Cu1 N5 171.0(3) 2_756 . ?
N14 Cu2 N15 96.6(3) . . ?
N14 Cu2 N15 175.6(3) . 2_666 ?
N15 Cu2 N15 79.1(3) . 2_666 ?
N14 Cu2 N18 91.2(3) . . ?
N15 Cu2 N18 169.9(3) . . ?
N15 Cu2 N18 93.0(3) 2_666 . ?
C1 N4 N3 105.0(7) . . ?
C1 N4 Cu1 127.6(6) . . ?
N3 N4 Cu1 127.3(5) . . ?
N2 N3 N4 111.4(7) . . ?
N3 N2 N1 105.2(7) . . ?
C1 N1 N2 108.4(6) . . ?
C1 N1 C2 130.9(7) . . ?
N2 N1 C2 120.6(7) . . ?
N6 N5 Cu1 115.8(5) . . ?
N7 N6 N5 177.8(8) . . ?
N9 N8 Cu1 123.1(5) . . ?
N9 N8 Cu1 132.1(6) . 2_756 ?
Cu1 N8 Cu1 102.3(3) . 2_756 ?
N10 N9 N8 178.0(9) . . ?
C7 N14 N13 105.2(7) . . ?
C7 N14 Cu2 128.0(6) . . ?
N13 N14 Cu2 126.7(5) . . ?
N12 N13 N14 109.6(6) . . ?
N13 N12 N11 106.8(7) . . ?
C7 N11 N12 109.5(6) . . ?
C7 N11 C8 127.7(7) . . ?
N12 N11 C8 122.7(7) . . ?
N16 N15 Cu2 124.8(5) . . ?
N16 N15 Cu2 118.7(5) . 2_666 ?
Cu2 N15 Cu2 100.9(3) . 2_666 ?
N17 N16 N15 176.7(8) . . ?
N1 C1 N4 110.0(8) . . ?
N1 C1 H1 125.0 . . ?
N4 C1 H1 125.0 . . ?
C3 C2 C6 105.8(8) . . ?
C3 C2 N1 114.9(7) . . ?
C6 C2 N1 112.8(6) . . ?
C3 C2 H2 107.7 . . ?
C6 C2 H2 107.7 . . ?
N1 C2 H2 107.7 . . ?
C2 C3 C4 105.2(8) . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 C5 106.2(7) . . ?
C3 C4 H4A 110.5 . . ?
C5 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
C5 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C4 C5 C6 104.7(7) . . ?
C4 C5 H5A 110.8 . . ?
C6 C5 H5A 110.8 . . ?
C4 C5 H5B 110.8 . . ?
C6 C5 H5B 110.8 . . ?
H5A C5 H5B 108.9 . . ?
C2 C6 C5 102.0(7) . . ?
C2 C6 H6A 111.4 . . ?
C5 C6 H6A 111.4 . . ?
C2 C6 H6B 111.4 . . ?
C5 C6 H6B 111.4 . . ?
H6A C6 H6B 109.2 . . ?
N11 C7 N14 108.8(7) . . ?
N11 C7 H7 125.6 . . ?
N14 C7 H7 125.6 . . ?
N11 C8 C12 113.8(7) . . ?
N11 C8 C9 113.7(6) . . ?
C12 C8 C9 102.9(8) . . ?
N11 C8 H8 108.7 . . ?
C12 C8 H8 108.7 . . ?
C9 C8 H8 108.7 . . ?
C10 C9 C8 101.6(7) . . ?
C10 C9 H9A 111.5 . . ?
C8 C9 H9A 111.5 . . ?
C10 C9 H9B 111.5 . . ?
C8 C9 H9B 111.5 . . ?
H9A C9 H9B 109.3 . . ?
C9 C10 C11 107.3(8) . . ?
C9 C10 H10A 110.3 . . ?
C11 C10 H10A 110.3 . . ?
C9 C10 H10B 110.3 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
C10 C11 C12 105.5(7) . . ?
C10 C11 H11A 110.6 . . ?
C12 C11 H11A 110.6 . . ?
C10 C11 H11B 110.6 . . ?
C12 C11 H11B 110.6 . . ?
H11A C11 H11B 108.8 . . ?
C8 C12 C11 104.4(7) . . ?
C8 C12 H12A 110.9 . . ?
C11 C12 H12A 110.9 . . ?
C8 C12 H12B 110.9 . . ?
C11 C12 H12B 110.9 . . ?
H12A C12 H12B 108.9 . . ?
N20 N19 N18 178.2(9) . . ?
N19 N18 Cu2 115.4(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 -0.9(9) . . . . ?
Cu1 N4 N3 N2 -179.2(5) . . . . ?
N4 N3 N2 N1 -0.2(9) . . . . ?
N3 N2 N1 C1 1.2(8) . . . . ?
N3 N2 N1 C2 177.5(7) . . . . ?
C7 N14 N13 N12 0.5(8) . . . . ?
Cu2 N14 N13 N12 -177.2(5) . . . . ?
N14 N13 N12 N11 -0.1(8) . . . . ?
N13 N12 N11 C7 -0.4(9) . . . . ?
N13 N12 N11 C8 -178.4(7) . . . . ?
N2 N1 C1 N4 -1.9(9) . . . . ?
C2 N1 C1 N4 -177.7(7) . . . . ?
N3 N4 C1 N1 1.7(9) . . . . ?
Cu1 N4 C1 N1 180.0(5) . . . . ?
C1 N1 C2 C3 -132.6(10) . . . . ?
N2 N1 C2 C3 52.1(11) . . . . ?
C1 N1 C2 C6 106.0(11) . . . . ?
N2 N1 C2 C6 -69.4(10) . . . . ?
C6 C2 C3 C4 -33.3(10) . . . . ?
N1 C2 C3 C4 -158.5(7) . . . . ?
C2 C3 C4 C5 12.1(11) . . . . ?
C3 C4 C5 C6 12.6(12) . . . . ?
C3 C2 C6 C5 40.8(10) . . . . ?
N1 C2 C6 C5 167.3(8) . . . . ?
C4 C5 C6 C2 -32.2(12) . . . . ?
N12 N11 C7 N14 0.7(9) . . . . ?
C8 N11 C7 N14 178.6(7) . . . . ?
N13 N14 C7 N11 -0.7(8) . . . . ?
Cu2 N14 C7 N11 177.0(5) . . . . ?
C7 N11 C8 C12 126.7(10) . . . . ?
N12 N11 C8 C12 -55.6(11) . . . . ?
C7 N11 C8 C9 -115.9(10) . . . . ?
N12 N11 C8 C9 61.7(11) . . . . ?
N11 C8 C9 C10 -165.9(8) . . . . ?
C12 C8 C9 C10 -42.5(10) . . . . ?
C8 C9 C10 C11 31.5(12) . . . . ?
C9 C10 C11 C12 -8.4(13) . . . . ?
N11 C8 C12 C11 161.4(8) . . . . ?
C9 C8 C12 C11 38.0(9) . . . . ?
C10 C11 C12 C8 -18.2(11) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N7 0.95 2.42 3.199(11) 139.1 2_766




_refine_diff_density_max         1.462
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.158

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_yv333
_database_code_depnum_ccdc_archive 'CCDC 2061089'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'hexakis(1-cyclopropyl-5H-tetrazolyl)iron(II) diperchlorate'
_chemical_name_common            
'hexakis(1-cyclopropyl-5H-tetrazolyl)iron(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C24 H36 Fe N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Fe N24 O8'
_chemical_formula_weight         915.52

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.83930(10)
_cell_length_b                   10.83930(10)
_cell_length_c                   30.1945(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3072.28(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      3.4633
_cell_measurement_theta_max      30.4238

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.574
_shelx_estimated_absorpt_T_min   0.894
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7089
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            19341
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.555
_diffrn_reflns_theta_max         26.343
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1401
_reflns_number_gt                1328
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1096P)²+5.1691P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.043(4)
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1401
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1712
_refine_ls_wR_factor_gt          0.1651
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.000000 1.000000 0.500000 0.0288(4) Uani 1 6 d S T P . .
Cl1 Cl 0.333333 0.666667 0.51062(4) 0.0470(4) Uani 1 3 d S T P . .
N4 N 0.7213(2) 0.6405(2) 0.58097(7) 0.0377(6) Uani 1 1 d . . . . .
N1 N 0.8780(2) 0.8127(2) 0.54200(7) 0.0365(6) Uani 1 1 d . . . . .
N3 N 0.8493(3) 0.6714(3) 0.59657(10) 0.0587(8) Uani 1 1 d . . . . .
C1 C 0.7416(3) 0.7270(3) 0.54745(9) 0.0401(6) Uani 1 1 d . . . . .
N2 N 0.9432(3) 0.7752(3) 0.57328(10) 0.0559(8) Uani 1 1 d . . . . .
C2 C 0.5912(3) 0.5191(3) 0.59677(10) 0.0468(7) Uani 1 1 d . . . . .
C4 C 0.4857(4) 0.5440(5) 0.61983(14) 0.0655(10) Uani 1 1 d . . . . .
C3 C 0.5703(4) 0.4970(4) 0.64513(10) 0.0575(9) Uani 1 1 d . . . . .
H3A H 0.522482 0.399809 0.656012 0.069 Uiso 1 1 calc R U . . .
H3B H 0.644501 0.565943 0.664363 0.069 Uiso 1 1 calc R U . . .
O1 O 0.2358(5) 0.5301(4) 0.49415(17) 0.1250(17) Uani 1 1 d . . . . .
O2 O 0.333333 0.666667 0.5559(2) 0.160(4) Uani 1 3 d S T P . .
H1 H 0.676(4) 0.723(4) 0.5339(13) 0.051(9) Uiso 1 1 d . . . . .
H4A H 0.513(5) 0.624(6) 0.6205(16) 0.072(14) Uiso 1 1 d . . . . .
H2 H 0.570(5) 0.439(5) 0.5783(15) 0.069(12) Uiso 1 1 d . . . . .
H4B H 0.390(5) 0.472(5) 0.6107(15) 0.074(12) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.190(2) . ?
Fe1 N1 2.190(2) 11_566 ?
Fe1 N1 2.190(2) 2_765 ?
Fe1 N1 2.190(2) 12_656 ?
Fe1 N1 2.190(2) 3_675 ?
Fe1 N1 2.190(2) 10_776 ?
Cl1 O2 1.368(6) . ?
Cl1 O1 1.411(4) 3_565 ?
Cl1 O1 1.411(4) . ?
Cl1 O1 1.411(4) 2_665 ?
N4 C1 1.321(3) . ?
N4 N3 1.340(3) . ?
N4 C2 1.447(3) . ?
N1 C1 1.305(3) . ?
N1 N2 1.357(3) . ?
N3 N2 1.285(4) . ?
C1 H1 0.81(4) . ?
C2 C4 1.474(5) . ?
C2 C3 1.479(4) . ?
C2 H2 0.96(4) . ?
C4 C3 1.467(6) . ?
C4 H4A 0.76(5) . ?
C4 H4B 0.98(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 90.18(8) . 11_566 ?
N1 Fe1 N1 89.82(8) . 2_765 ?
N1 Fe1 N1 180.0 11_566 2_765 ?
N1 Fe1 N1 90.18(8) . 12_656 ?
N1 Fe1 N1 89.82(8) 11_566 12_656 ?
N1 Fe1 N1 90.18(8) 2_765 12_656 ?
N1 Fe1 N1 89.82(8) . 3_675 ?
N1 Fe1 N1 90.18(8) 11_566 3_675 ?
N1 Fe1 N1 89.82(8) 2_765 3_675 ?
N1 Fe1 N1 180.00(9) 12_656 3_675 ?
N1 Fe1 N1 180.0 . 10_776 ?
N1 Fe1 N1 89.82(8) 11_566 10_776 ?
N1 Fe1 N1 90.18(8) 2_765 10_776 ?
N1 Fe1 N1 89.82(8) 12_656 10_776 ?
N1 Fe1 N1 90.18(8) 3_675 10_776 ?
O2 Cl1 O1 110.6(2) . 3_565 ?
O2 Cl1 O1 110.6(2) . . ?
O1 Cl1 O1 108.3(2) 3_565 . ?
O2 Cl1 O1 110.6(2) . 2_665 ?
O1 Cl1 O1 108.3(2) 3_565 2_665 ?
O1 Cl1 O1 108.3(2) . 2_665 ?
C1 N4 N3 107.9(2) . . ?
C1 N4 C2 129.7(2) . . ?
N3 N4 C2 121.9(2) . . ?
C1 N1 N2 105.9(2) . . ?
C1 N1 Fe1 132.60(18) . . ?
N2 N1 Fe1 121.14(16) . . ?
N2 N3 N4 107.1(2) . . ?
N1 C1 N4 109.2(2) . . ?
N1 C1 H1 129(3) . . ?
N4 C1 H1 122(3) . . ?
N3 N2 N1 109.9(2) . . ?
N4 C2 C4 118.8(3) . . ?
N4 C2 C3 118.3(3) . . ?
C4 C2 C3 59.6(3) . . ?
N4 C2 H2 108(3) . . ?
C4 C2 H2 126(3) . . ?
C3 C2 H2 119(3) . . ?
C3 C4 C2 60.4(2) . . ?
C3 C4 H4A 115(4) . . ?
C2 C4 H4A 109(4) . . ?
C3 C4 H4B 118(3) . . ?
C2 C4 H4B 110(3) . . ?
H4A C4 H4B 125(5) . . ?
C4 C3 C2 60.1(2) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 0.9(4) . . . . ?
C2 N4 N3 N2 173.8(3) . . . . ?
N2 N1 C1 N4 0.7(3) . . . . ?
Fe1 N1 C1 N4 -171.89(18) . . . . ?
N3 N4 C1 N1 -1.0(3) . . . . ?
C2 N4 C1 N1 -173.1(3) . . . . ?
N4 N3 N2 N1 -0.5(4) . . . . ?
C1 N1 N2 N3 -0.1(4) . . . . ?
Fe1 N1 N2 N3 173.5(2) . . . . ?
C1 N4 C2 C4 -72.1(4) . . . . ?
N3 N4 C2 C4 116.7(4) . . . . ?
C1 N4 C2 C3 -141.0(3) . . . . ?
N3 N4 C2 C3 47.8(4) . . . . ?
N4 C2 C4 C3 -107.7(3) . . . . ?
N4 C2 C3 C4 108.6(4) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?





_refine_diff_density_max         0.933
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.195

_shelxl_version_number           ?


