# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1526244'

_audit_update_record             
;
2017-01-08 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
_publcif_datablock.id            {69e981f3-9788-4bad-9c83-fc473afe6f90}
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (C24H30N6Zn),(Cl),(ClO4)
_chemical_formula_sum            'C24 H30 Cl2 N6 O4 Zn'
_chemical_formula_weight         602.81

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'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   13.9000(5)
_cell_length_b                   13.9000(5)
_cell_length_c                   45.0290(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7534.5(6)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    44094
_cell_measurement_theta_min      3.23
_cell_measurement_theta_max      27.41

_exptl_crystal_description       chunk
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_F_000             3744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.236
_shelx_estimated_absorpt_T_min   0.748
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8646
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrystalClear SM 1.4.0 (Rigaku/MSC Inc., 2008).
;
_exptl_special_details           
;
 T.Higashi, Empirical Absorption Correction, 2001
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           40.0000
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_detector       RX
_diffrn_measurement_device       RAXIS-RAPID
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       dtprofit.ref
_diffrn_measurement_details      
;
 scan:  N=1,PHI=180.0,CHI=0.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                 
 scan:  N=2,PHI=0.0,CHI=0.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                   
 scan:  N=3,PHI=90.0,CHI=40.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                 
 scan:  N=4,PHI=180.0,CHI=40.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                
 Orientation Matrix:
    UB11  0.0687 UB12  0.0153 UB13  0.0110
    UB21  0.0415 UB22  0.0747 UB23 -0.0096
    UB31 -0.0214 UB32  0.0329 UB33  0.0167
    Matrix type: 'd*Trek'
;
_diffrn_reflns_number            72365
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         3.230
_diffrn_reflns_theta_max         27.472
_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             1924
_reflns_number_gt                1614
_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       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.'
_computing_publication_material  ?
_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)+(0.1034P)²+20.5149P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1924
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1812
_refine_ls_wR_factor_gt          0.1697
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.3333 0.6667 0.05435(2) 0.0344(3) Uani 1 3 d S T P . .
N2 N 0.3191(2) 0.5259(2) 0.02730(5) 0.0416(6) Uani 1 1 d . . . . .
N1 N 0.4091(2) 0.5976(2) 0.08252(5) 0.0364(6) Uani 1 1 d . . . . .
H1N H 0.4891 0.6441 0.0790 0.044 Uiso 1 1 d R U . . .
C8 C 0.2908(3) 0.5047(3) -0.00163(7) 0.0496(8) Uani 1 1 d . . . . .
H8 H 0.2622 0.5446 -0.0111 0.060 Uiso 1 1 calc R U . . .
C7 C 0.3022(3) 0.4269(3) -0.01792(8) 0.0578(9) Uani 1 1 d . . . . .
H7 H 0.2816 0.4146 -0.0378 0.069 Uiso 1 1 calc R U . . .
C6 C 0.3446(4) 0.3679(4) -0.00415(9) 0.0626(10) Uani 1 1 d . . . . .
H6 H 0.3541 0.3158 -0.0147 0.075 Uiso 1 1 calc R U . . .
C5 C 0.3731(3) 0.3869(3) 0.02565(8) 0.0535(8) Uani 1 1 d . . . . .
H5 H 0.4013 0.3474 0.0354 0.064 Uiso 1 1 calc R U . . .
C4 C 0.3585(3) 0.4670(3) 0.04074(7) 0.0407(7) Uani 1 1 d . . . . .
C3 C 0.3820(3) 0.4855(3) 0.07374(7) 0.0469(8) Uani 1 1 d . . . . .
H3A H 0.3174 0.4316 0.0847 0.056 Uiso 1 1 calc R U . . .
H3B H 0.4437 0.4743 0.0787 0.056 Uiso 1 1 calc R U . . .
C1 C 0.3951(2) 0.6052(3) 0.11513(6) 0.0383(7) Uani 1 1 d . . . . .
H1 H 0.4313 0.5694 0.1253 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4546(3) 0.7276(3) 0.12453(7) 0.0414(7) Uani 1 1 d . . . . .
H2A H 0.4626 0.7316 0.1460 0.050 Uiso 1 1 calc R U . . .
H2B H 0.5286 0.7647 0.1160 0.050 Uiso 1 1 calc R U . . .
Cl2 Cl 0.6667 0.71459(12) 0.0833 0.0628(4) Uani 1 2 d S T P . .
Cl1 Cl 0.3333 0.6667 -0.0833 0.1073(15) Uani 1 6 d S T P . .
O1 O 0.3333 0.6667 -0.0561(6) 0.276(10) Uiso 1 3 d S . P . .
O2 O 0.2138(19) 0.5512(19) -0.0686(5) 0.465(11) Uiso 1 1 d . . . . .


_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.
;

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 2.157(3) . ?
Zn1 N1 2.157(3) 2_665 ?
Zn1 N1 2.157(3) 3_565 ?
Zn1 N2 2.228(3) . ?
Zn1 N2 2.228(3) 3_565 ?
Zn1 N2 2.228(3) 2_665 ?
N2 C4 1.336(4) . ?
N2 C8 1.350(4) . ?
N1 C3 1.462(4) . ?
N1 C1 1.492(4) . ?
N1 H1N 0.9801 . ?
C8 C7 1.380(5) . ?
C8 H8 0.9300 . ?
C7 C6 1.373(6) . ?
C7 H7 0.9300 . ?
C6 C5 1.386(5) . ?
C6 H6 0.9300 . ?
C5 C4 1.403(4) . ?
C5 H5 0.9300 . ?
C4 C3 1.516(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 C2 1.531(4) 3_565 ?
C1 C2 1.533(4) . ?
C1 H1 0.9800 . ?
C2 C1 1.531(4) 2_665 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
Cl1 O1 1.22(3) . ?
Cl1 O1 1.22(3) 10_564 ?
Cl1 O2 1.763(19) 11_554 ?
Cl1 O2 1.763(19) 12_454 ?
Cl1 O2 1.763(19) 3_565 ?
Cl1 O2 1.763(19) 2_665 ?
Cl1 O2 1.763(19) . ?
Cl1 O2 1.763(19) 10_564 ?
O1 O2 1.728(18) 3_565 ?
O1 O2 1.728(18) 2_665 ?
O1 O2 1.729(18) . ?
O2 O2 1.33(4) 12_454 ?

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 88.92(10) . 2_665 ?
N1 Zn1 N1 88.93(10) . 3_565 ?
N1 Zn1 N1 88.92(10) 2_665 3_565 ?
N1 Zn1 N2 77.24(10) . . ?
N1 Zn1 N2 160.72(10) 2_665 . ?
N1 Zn1 N2 103.98(10) 3_565 . ?
N1 Zn1 N2 160.72(10) . 3_565 ?
N1 Zn1 N2 103.98(10) 2_665 3_565 ?
N1 Zn1 N2 77.25(10) 3_565 3_565 ?
N2 Zn1 N2 92.95(9) . 3_565 ?
N1 Zn1 N2 103.98(10) . 2_665 ?
N1 Zn1 N2 77.25(10) 2_665 2_665 ?
N1 Zn1 N2 160.72(10) 3_565 2_665 ?
N2 Zn1 N2 92.95(9) . 2_665 ?
N2 Zn1 N2 92.95(9) 3_565 2_665 ?
C4 N2 C8 117.8(3) . . ?
C4 N2 Zn1 114.02(19) . . ?
C8 N2 Zn1 127.4(2) . . ?
C3 N1 C1 111.7(2) . . ?
C3 N1 Zn1 113.10(19) . . ?
C1 N1 Zn1 115.91(19) . . ?
C3 N1 H1N 105.3 . . ?
C1 N1 H1N 104.8 . . ?
Zn1 N1 H1N 104.9 . . ?
N2 C8 C7 123.3(4) . . ?
N2 C8 H8 118.4 . . ?
C7 C8 H8 118.4 . . ?
C6 C7 C8 118.7(3) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
C7 C6 C5 119.4(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C5 C4 118.6(3) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N2 C4 C5 122.2(3) . . ?
N2 C4 C3 117.4(3) . . ?
C5 C4 C3 120.3(3) . . ?
N1 C3 C4 111.4(2) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
N1 C1 C2 112.5(2) . 3_565 ?
N1 C1 C2 109.5(2) . . ?
C2 C1 C2 111.3(3) 3_565 . ?
N1 C1 H1 107.8 . . ?
C2 C1 H1 107.8 3_565 . ?
C2 C1 H1 107.8 . . ?
C1 C2 C1 114.0(3) 2_665 . ?
C1 C2 H2A 108.7 2_665 . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 2_665 . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
O1 Cl1 O1 180.0 . 10_564 ?
O1 Cl1 O2 112.0(6) . 11_554 ?
O1 Cl1 O2 68.0(6) 10_564 11_554 ?
O1 Cl1 O2 112.0(6) . 12_454 ?
O1 Cl1 O2 68.0(6) 10_564 12_454 ?
O2 Cl1 O2 106.8(7) 11_554 12_454 ?
O1 Cl1 O2 68.0(6) . 3_565 ?
O1 Cl1 O2 112.0(6) 10_564 3_565 ?
O2 Cl1 O2 122(2) 11_554 3_565 ?
O2 Cl1 O2 128(2) 12_454 3_565 ?
O1 Cl1 O2 68.0(6) . 2_665 ?
O1 Cl1 O2 112.0(6) 10_564 2_665 ?
O2 Cl1 O2 44.2(13) 11_554 2_665 ?
O2 Cl1 O2 122(2) 12_454 2_665 ?
O2 Cl1 O2 106.8(7) 3_565 2_665 ?
O1 Cl1 O2 68.0(6) . . ?
O1 Cl1 O2 112.0(6) 10_564 . ?
O2 Cl1 O2 128(2) 11_554 . ?
O2 Cl1 O2 44.2(13) 12_454 . ?
O2 Cl1 O2 106.8(7) 3_565 . ?
O2 Cl1 O2 106.8(7) 2_665 . ?
O1 Cl1 O2 112.0(6) . 10_564 ?
O1 Cl1 O2 68.0(6) 10_564 10_564 ?
O2 Cl1 O2 106.8(7) 11_554 10_564 ?
O2 Cl1 O2 106.8(7) 12_454 10_564 ?
O2 Cl1 O2 44.2(13) 3_565 10_564 ?
O2 Cl1 O2 128(2) 2_665 10_564 ?
O2 Cl1 O2 122(2) . 10_564 ?
Cl1 O1 O2 71.0(12) . 3_565 ?
Cl1 O1 O2 71.0(12) . 2_665 ?
O2 O1 O2 109.9(12) 3_565 2_665 ?
Cl1 O1 O2 71.0(12) . . ?
O2 O1 O2 109.9(12) 3_565 . ?
O2 O1 O2 109.9(12) 2_665 . ?
O2 O2 O1 108.9(13) 12_454 . ?
O2 O2 Cl1 67.9(6) 12_454 . ?
O1 O2 Cl1 41.1(11) . . ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1526245'
_audit_update_record             
;
2017-01-08 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT245_3                   
;
PROBLEM: U(iso) H1W     Smaller than U(eq) O1W     by ...      0.276 AngSq
RESPONSE: Disordered water molecule.
;
_vrf_PLAT420_3                   
;
PROBLEM: D-H Without Acceptor       O1W    --  H1W    ...     Please Check
RESPONSE: Disordered water molecule.
;
# Added during the CSD deposition process: Sunday 08 January 2017 01:44 PM
# end Validation Reply Form


_publcif_datablock.id            {362ad4eb-882e-42f7-8544-7531065e0d36}

_audit_creation_date             2016-12-05T19:40:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#==============================================================================

# CHEMICAL DATA

_chemical_formula_moiety         'C24 H30 Cu N6, 2(Cl O4), H2 O'
_chemical_formula_sum            'C24 H32 Cl2 Cu N6 O9'
_chemical_formula_weight         682.99

#==============================================================================

# CRYSTAL DATA

_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'


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_cell_length_a                   8.5315(16)
_cell_length_b                   14.200(6)
_cell_length_c                   24.011(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.230(10)
_cell_angle_gamma                90
_cell_volume                     2871.3(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      9.7
_cell_measurement_theta_max      16.1
_cell_measurement_temperature    293(2)
_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        Fourier smoothing - Window value   5
;
_exptl_absorpt_correction_T_min  0.7362
_exptl_absorpt_correction_T_max  0.8631

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'profiled omega/2theta scans'
_diffrn_reflns_number            8665
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_theta_min         2.694
_diffrn_reflns_theta_max         25.975
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_standards_number         3
_diffrn_standards_interval_count 255
_diffrn_standards_interval_time  11
_diffrn_standards_decay_%        5
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -7 10
3 -5 4
4 -1 -4


#==============================================================================

# STRUCTURE SOLUTION

_atom_sites_solution_hydrogens   mixed

#==============================================================================

# REFINEMENT DATA

_reflns_number_total             5615
_reflns_number_gt                4436
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0874
_refine_ls_wR_factor_ref         0.2322
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_number_reflns         5615
_refine_ls_number_parameters     394
_refine_ls_number_restraints     5
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0940P)²+11.8288P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
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 0 '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 0.006 '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'

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
C1 C 0.6465(7) 0.6523(5) 0.8954(3) 0.0540(15) Uani 1 1 d . . . . .
H1C H 0.5993 0.6507 0.9300 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5122(7) 0.6634(5) 0.8457(3) 0.0564(16) Uani 1 1 d . . . . .
H2A H 0.4307 0.6174 0.8496 0.068 Uiso 1 1 calc R U . . .
H2B H 0.4657 0.7254 0.8478 0.068 Uiso 1 1 calc R U . . .
C1A C 0.5586(7) 0.6521(5) 0.7884(3) 0.0527(15) Uani 1 1 d . . . . .
H1A1 H 0.4617 0.6488 0.7603 0.063 Uiso 1 1 calc R U . . .
C2A C 0.6516(8) 0.5619(5) 0.7856(3) 0.0571(16) Uani 1 1 d . . . . .
H2A1 H 0.6952 0.5620 0.7507 0.069 Uiso 1 1 calc R U . . .
H2A2 H 0.5781 0.5094 0.7839 0.069 Uiso 1 1 calc R U . . .
C1B C 0.7872(7) 0.5443(4) 0.8344(3) 0.0510(14) Uani 1 1 d . . . . .
H1B1 H 0.8207 0.4785 0.8323 0.061 Uiso 1 1 calc R U . . .
C2B C 0.7352(8) 0.5593(5) 0.8915(3) 0.0600(17) Uani 1 1 d . . . . .
H2B2 H 0.8281 0.5581 0.9206 0.072 Uiso 1 1 calc R U . . .
H2B1 H 0.6667 0.5076 0.8986 0.072 Uiso 1 1 calc R U . . .
C3 C 0.6962(8) 0.8222(5) 0.9151(3) 0.0577(16) Uani 1 1 d . . . . .
H3A H 0.6828 0.8217 0.9545 0.069 Uiso 1 1 calc R U . . .
H3B H 0.5926 0.8310 0.8923 0.069 Uiso 1 1 calc R U . . .
C4 C 0.8039(8) 0.9019(5) 0.9049(3) 0.0545(15) Uani 1 1 d . . . . .
C5 C 0.8165(10) 0.9845(6) 0.9357(4) 0.075(2) Uani 1 1 d . . . . .
H5 H 0.7592 0.9928 0.9652 0.090 Uiso 1 1 calc R U . . .
C6 C 0.9147(12) 1.0537(6) 0.9220(4) 0.087(3) Uani 1 1 d . . . . .
H6 H 0.9249 1.1097 0.9423 0.105 Uiso 1 1 calc R U . . .
C7 C 0.9976(10) 1.0410(5) 0.8788(3) 0.073(2) Uani 1 1 d . . . . .
H7 H 1.0643 1.0880 0.8691 0.088 Uiso 1 1 calc R U . . .
C8 C 0.9811(9) 0.9573(5) 0.8494(3) 0.0589(16) Uani 1 1 d . . . . .
H8 H 1.0378 0.9483 0.8198 0.071 Uiso 1 1 calc R U . . .
C3A C 0.6781(8) 0.7461(5) 0.7179(3) 0.0603(17) Uani 1 1 d . . . . .
H3A2 H 0.6071 0.7937 0.6990 0.072 Uiso 1 1 calc R U . . .
H3A1 H 0.6519 0.6867 0.6987 0.072 Uiso 1 1 calc R U . . .
C4A C 0.8473(8) 0.7721(5) 0.7127(2) 0.0499(14) Uani 1 1 d . . . . .
C5A C 0.8863(9) 0.7886(6) 0.6605(3) 0.0646(18) Uani 1 1 d . . . . .
H5A H 0.8089 0.7870 0.6285 0.078 Uiso 1 1 calc R U . . .
C6A C 1.0411(10) 0.8074(7) 0.6562(3) 0.076(2) Uani 1 1 d . . . . .
H6A H 1.0698 0.8180 0.6209 0.092 Uiso 1 1 calc R U . . .
C7A C 1.1530(9) 0.8106(6) 0.7032(3) 0.073(2) Uani 1 1 d . . . . .
H7A H 1.2584 0.8238 0.7006 0.088 Uiso 1 1 calc R U . . .
C8A C 1.1087(8) 0.7943(5) 0.7547(3) 0.0580(16) Uani 1 1 d . . . . .
H8A H 1.1853 0.7957 0.7869 0.070 Uiso 1 1 calc R U . . .
C3B C 1.0786(8) 0.5715(5) 0.8627(3) 0.0628(18) Uani 1 1 d . . . . .
H3B1 H 1.1533 0.5570 0.8374 0.075 Uiso 1 1 calc R U . . .
H3B2 H 1.0574 0.5136 0.8815 0.075 Uiso 1 1 calc R U . . .
C4B C 1.1545(7) 0.6409(5) 0.9062(3) 0.0493(14) Uani 1 1 d . . . . .
C5B C 1.2527(8) 0.6065(5) 0.9540(3) 0.0599(17) Uani 1 1 d . . . . .
H5B H 1.2622 0.5422 0.9610 0.072 Uiso 1 1 calc R U . . .
C6B C 1.3352(9) 0.6707(7) 0.9906(3) 0.075(2) Uani 1 1 d . . . . .
H6B H 1.4027 0.6503 1.0226 0.090 Uiso 1 1 calc R U . . .
C7B C 1.3167(9) 0.7646(6) 0.9794(3) 0.068(2) Uani 1 1 d . . . . .
H7B H 1.3712 0.8088 1.0037 0.082 Uiso 1 1 calc R U . . .
C8B C 1.2179(8) 0.7927(5) 0.9324(3) 0.0591(16) Uani 1 1 d . . . . .
H8B H 1.2059 0.8569 0.9253 0.071 Uiso 1 1 calc R U . . .
N1 N 0.7639(6) 0.7316(4) 0.9006(2) 0.0456(11) Uani 1 1 d D . . . .
N1A N 0.6504(6) 0.7375(4) 0.7765(2) 0.0474(11) Uani 1 1 d D . . . .
N1B N 0.9267(6) 0.6058(4) 0.8284(2) 0.0481(12) Uani 1 1 d D . . . .
N2 N 0.8850(6) 0.8881(4) 0.8625(2) 0.0491(12) Uani 1 1 d . . . . .
N2A N 0.9548(6) 0.7760(4) 0.7597(2) 0.0454(11) Uani 1 1 d . . . . .
N2B N 1.1361(6) 0.7318(4) 0.8953(2) 0.0495(12) Uani 1 1 d . . . . .
O1W O 0.410(2) 0.067(2) 0.9521(9) 0.326(13) Uani 1 1 d D . . . .
O7 O 0.9984(19) 0.6449(11) 1.0923(7) 0.281(10) Uani 1 1 d . . . . .
O6 O 0.9499(9) 0.7397(6) 1.0155(3) 0.118(3) Uani 1 1 d . . . . .
O8 O 0.856(2) 0.7486(12) 1.0951(8) 0.288(12) Uani 1 1 d . . . . .
O5 O 0.7541(10) 0.6363(6) 1.0381(3) 0.130(3) Uani 1 1 d . . . . .
O2 O 0.2860(9) 1.0304(6) 0.7663(3) 0.120(3) Uani 1 1 d . . . . .
O3 O 0.4908(12) 0.9295(7) 0.7644(5) 0.161(4) Uani 1 1 d . . . . .
O1 O 0.5383(11) 1.0633(7) 0.8107(5) 0.168(4) Uani 1 1 d . . . . .
O4 O 0.3951(10) 0.9450(9) 0.8425(4) 0.180(5) Uani 1 1 d . . . . .
Cl2 Cl 0.8898(3) 0.68645(14) 1.05675(7) 0.0703(5) Uani 1 1 d . . . . .
Cl1 Cl 0.4253(2) 0.99478(13) 0.79793(8) 0.0641(5) Uani 1 1 d . . . . .
Cu1 Cu 0.88028(8) 0.75076(5) 0.83447(3) 0.0409(2) Uani 1 1 d . . . . .
H1 H 0.834(6) 0.721(5) 0.9316(17) 0.049 Uiso 1 1 d D U . . .
H1A H 0.583(6) 0.780(4) 0.787(3) 0.049 Uiso 1 1 d D U . . .
H1W H 0.374(9) 0.123(3) 0.953(3) 0.049 Uiso 1 1 d D U . . .
H1B H 0.931(7) 0.602(5) 0.7910(10) 0.049 Uiso 1 1 d D U . . .
H2W H 0.400(8) 0.012(2) 0.937(3) 0.049 Uiso 1 1 d D U . . .


_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.
;

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
C1 N1 1.499(8) . ?
C1 C2 1.524(9) . ?
C1 C2B 1.532(10) . ?
C2 C1A 1.501(9) . ?
C1A N1A 1.495(8) . ?
C1A C2A 1.514(10) . ?
C2A C1B 1.529(9) . ?
C1B N1B 1.502(8) . ?
C1B C2B 1.523(9) . ?
C3 N1 1.474(8) . ?
C3 C4 1.503(10) . ?
C4 N2 1.334(8) . ?
C4 C5 1.382(10) . ?
C5 C6 1.366(12) . ?
C6 C7 1.358(12) . ?
C7 C8 1.377(10) . ?
C8 N2 1.349(8) . ?
C3A N1A 1.469(8) . ?
C3A C4A 1.514(9) . ?
C4A N2A 1.336(8) . ?
C4A C5A 1.368(9) . ?
C5A C6A 1.368(11) . ?
C6A C7A 1.358(11) . ?
C7A C8A 1.368(9) . ?
C8A N2A 1.362(8) . ?
C3B N1B 1.500(8) . ?
C3B C4B 1.505(9) . ?
C4B N2B 1.321(8) . ?
C4B C5B 1.397(9) . ?
C5B C6B 1.378(11) . ?
C6B C7B 1.363(12) . ?
C7B C8B 1.356(10) . ?
C8B N2B 1.353(8) . ?
N1 Cu1 2.022(5) . ?
N1A Cu1 2.223(5) . ?
N1B Cu1 2.105(5) . ?
N2 Cu1 2.061(5) . ?
N2A Cu1 2.031(5) . ?
N2B Cu1 2.438(5) . ?
O7 Cl2 1.297(11) . ?
O6 Cl2 1.406(7) . ?
O8 Cl2 1.340(11) . ?
O5 Cl2 1.372(7) . ?
O2 Cl1 1.398(6) . ?
O3 Cl1 1.402(9) . ?
O1 Cl1 1.369(8) . ?
O4 Cl1 1.341(7) . ?

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 C1 C2 113.3(5) . . ?
N1 C1 C2B 108.9(5) . . ?
C2 C1 C2B 111.0(6) . . ?
C1A C2 C1 115.5(5) . . ?
N1A C1A C2 108.2(5) . . ?
N1A C1A C2A 112.6(5) . . ?
C2 C1A C2A 110.3(6) . . ?
C1A C2A C1B 116.3(5) . . ?
N1B C1B C2B 110.7(5) . . ?
N1B C1B C2A 110.3(5) . . ?
C2B C1B C2A 111.8(5) . . ?
C1B C2B C1 113.2(5) . . ?
N1 C3 C4 110.2(5) . . ?
N2 C4 C5 121.9(7) . . ?
N2 C4 C3 114.8(5) . . ?
C5 C4 C3 123.3(7) . . ?
C6 C5 C4 118.7(8) . . ?
C7 C6 C5 120.3(8) . . ?
C6 C7 C8 118.8(8) . . ?
N2 C8 C7 121.8(7) . . ?
N1A C3A C4A 113.6(5) . . ?
N2A C4A C5A 122.1(6) . . ?
N2A C4A C3A 118.4(5) . . ?
C5A C4A C3A 119.5(6) . . ?
C6A C5A C4A 118.9(7) . . ?
C7A C6A C5A 120.1(7) . . ?
C6A C7A C8A 119.1(7) . . ?
N2A C8A C7A 121.5(6) . . ?
N1B C3B C4B 113.9(5) . . ?
N2B C4B C5B 122.8(6) . . ?
N2B C4B C3B 118.5(6) . . ?
C5B C4B C3B 118.5(6) . . ?
C6B C5B C4B 118.0(7) . . ?
C7B C6B C5B 119.4(7) . . ?
C8B C7B C6B 119.3(7) . . ?
N2B C8B C7B 123.1(7) . . ?
C3 N1 C1 113.2(5) . . ?
C3 N1 Cu1 109.2(4) . . ?
C1 N1 Cu1 116.2(4) . . ?
C3A N1A C1A 114.8(5) . . ?
C3A N1A Cu1 109.4(4) . . ?
C1A N1A Cu1 112.7(4) . . ?
C3B N1B C1B 112.8(5) . . ?
C3B N1B Cu1 115.8(4) . . ?
C1B N1B Cu1 113.7(4) . . ?
C4 N2 C8 118.6(6) . . ?
C4 N2 Cu1 113.8(4) . . ?
C8 N2 Cu1 126.5(4) . . ?
C4A N2A C8A 118.3(5) . . ?
C4A N2A Cu1 118.0(4) . . ?
C8A N2A Cu1 123.7(4) . . ?
C4B N2B C8B 117.5(6) . . ?
C4B N2B Cu1 107.0(4) . . ?
C8B N2B Cu1 129.9(4) . . ?
O7 Cl2 O8 93.3(12) . . ?
O7 Cl2 O5 117.0(7) . . ?
O8 Cl2 O5 107.5(8) . . ?
O7 Cl2 O6 114.0(9) . . ?
O8 Cl2 O6 105.8(8) . . ?
O5 Cl2 O6 115.7(5) . . ?
O4 Cl1 O1 114.5(8) . . ?
O4 Cl1 O2 111.6(5) . . ?
O1 Cl1 O2 111.8(6) . . ?
O4 Cl1 O3 104.8(8) . . ?
O1 Cl1 O3 105.5(7) . . ?
O2 Cl1 O3 108.0(6) . . ?
N1 Cu1 N2A 168.9(2) . . ?
N1 Cu1 N2 81.8(2) . . ?
N2A Cu1 N2 97.4(2) . . ?
N1 Cu1 N1B 92.5(2) . . ?
N2A Cu1 N1B 91.3(2) . . ?
N2 Cu1 N1B 162.4(2) . . ?
N1 Cu1 N1A 89.2(2) . . ?
N2A Cu1 N1A 80.28(19) . . ?
N2 Cu1 N1A 104.7(2) . . ?
N1B Cu1 N1A 91.8(2) . . ?
N1 Cu1 N2B 91.13(19) . . ?
N2A Cu1 N2B 99.91(19) . . ?
N2 Cu1 N2B 86.59(19) . . ?
N1B Cu1 N2B 76.88(19) . . ?
N1A Cu1 N2B 168.64(19) . . ?
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
N1 H1 O6 0.89(2) 2.11(3) 2.957(8) 158(6) .
N1A H1A O3 0.90(2) 2.29(5) 3.042(11) 141(5) .
N1B H1B O1 0.91(2) 2.56(3) 3.454(13) 170(6) 2_646
O1W H2W O4 0.86(2) 2.46(6) 3.140(19) 136(6) 1_545


####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1526243'

_audit_update_record             
;
2017-01-08 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
_publcif_datablock.id            {d163bc37-05fa-4ff3-b805-2192bb3d9edc}
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         2(ClO4),(O),(C24H30N6Zn)
_chemical_formula_sum            'C24 H30 Cl2 N6 O9 Zn'
_chemical_formula_weight         682.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_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                   8.5454(2)
_cell_length_b                   14.1957(3)
_cell_length_c                   24.2629(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.2980(10)
_cell_angle_gamma                90
_cell_volume                     2895.87(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15340
_cell_measurement_theta_min      6.51
_cell_measurement_theta_max      68.12

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.415
_shelx_estimated_absorpt_T_min   0.280
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrystalClear SM 1.4.0 (Rigaku/MSC Inc., 2008).
;
_exptl_absorpt_correction_T_min  0.5159
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_special_details   
;
 T.Higashi, Empirical Absorption Correction, 2001
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Sealed Tube'
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           40.0000
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_detector       RX
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_measurement_details      
;
 scan:  N=1,PHI=270.0,CHI=40.0,OMEGA=5.0,185.0,5.0,COUPLE=0.00                 
 scan:  N=2,PHI=180.0,CHI=40.0,OMEGA=144.0,234.0,5.0,COUPLE=0.00               
 scan:  N=3,PHI=270.0,CHI=15.0,OMEGA=5.0,155.0,5.0,COUPLE=0.00                 
 scan:  N=4,PHI=0.0,CHI=40.0,OMEGA=72.0,117.0,5.0,COUPLE=0.00                  
 scan:  N=5,PHI=0.0,CHI=0.0,OMEGA=20.0,200.0,5.0,COUPLE=0.00                   
 Orientation Matrix:
    UB11  0.0493 UB12 -0.0582 UB13 -0.0126
    UB21 -0.0714 UB22  0.0048 UB23 -0.0373
    UB31  0.0814 UB32  0.0394 UB33 -0.0141
    Matrix type: 'd*Trek'
;
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            20821
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         6.506
_diffrn_reflns_theta_max         58.920
_diffrn_reflns_theta_full        58.920
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             4076
_reflns_number_gt                3202
_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       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.'
_computing_publication_material  ?
_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)+(0.0681P)²+2.9952P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4076
_refine_ls_number_parameters     406
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1537
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

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 0.60797(7) 0.25246(4) 0.16529(2) 0.0481(2) Uani 1 1 d . . . A 1
Cl1 Cl 0.42810(16) 0.00178(9) 0.29583(5) 0.0709(4) Uani 1 1 d . . . B 1
Cl2 Cl 0.1137(2) 0.31725(10) 0.44568(5) 0.0840(5) Uani 1 1 d D . . C 1
O1 O 0.5448(6) 0.0681(4) 0.3104(3) 0.154(2) Uani 1 1 d . . . B 1
O2 O 0.2962(6) 0.0385(4) 0.2611(2) 0.1397(19) Uani 1 1 d . . . B 1
O3 O 0.4947(7) -0.0697(4) 0.2665(3) 0.158(2) Uani 1 1 d . . . B 1
O4 O 0.3855(6) -0.0426(5) 0.3414(2) 0.165(3) Uani 1 1 d . . . B 1
O5 O 0.2458(6) 0.3726(4) 0.4624(2) 0.145(2) Uani 1 1 d D . . C 1
O6 O 0.0454(10) 0.2638(7) 0.4843(3) 0.068(3) Uani 0.504(15) 1 d D . P C 1
O7 O -0.0267(16) 0.3575(13) 0.4139(10) 0.213(11) Uani 0.504(15) 1 d D . P C 1
O8 O 0.166(3) 0.2478(12) 0.4115(12) 0.258(16) Uani 0.504(15) 1 d D . P C 1
O9A O 0.4033(17) 0.1065(12) 0.4416(6) 0.170(5) Uiso 0.5 1 d . . P D 1
O5B O 0.0354(17) 0.3765(16) 0.4777(7) 0.273(17) Uani 0.496(15) 1 d D . P C 2
O6B O 0.174(4) 0.2298(9) 0.4648(10) 0.35(2) Uani 0.496(15) 1 d D . P C 2
O7B O 0.0657(16) 0.3191(11) 0.3903(3) 0.106(5) Uani 0.496(15) 1 d D . P C 2
O9B O 0.4029(17) 0.0426(12) 0.4562(6) 0.167(5) Uiso 0.5 1 d . . P D 1
N1 N 0.7444(4) 0.2367(3) 0.09884(15) 0.0528(9) Uani 1 1 d . . . A 1
H1 H 0.6671 0.2184 0.0657 0.063 Uiso 1 1 calc R U . A 1
N2 N 0.6165(5) 0.3961(3) 0.13660(15) 0.0584(10) Uani 1 1 d . . . A 1
N1A N 0.8322(4) 0.2430(3) 0.22369(15) 0.0547(10) Uani 1 1 d . . . A 1
H1A H 0.8922 0.2995 0.2172 0.066 Uiso 1 1 calc R U . A 1
N2A N 0.5317(4) 0.2831(3) 0.24257(14) 0.0526(9) Uani 1 1 d . . . A 1
N1B N 0.5787(4) 0.1018(3) 0.16976(15) 0.0579(10) Uani 1 1 d . . . A 1
H1B H 0.5595 0.0894 0.2077 0.070 Uiso 1 1 calc R U . A 1
N2B N 0.3803(4) 0.2311(3) 0.10637(15) 0.0516(9) Uani 1 1 d . . . A 1
C1 C 0.8644(6) 0.1604(4) 0.10687(19) 0.0636(13) Uani 1 1 d . . . A 1
H1C H 0.9162 0.1595 0.0739 0.076 Uiso 1 1 calc R U . A 1
C2 C 0.9927(5) 0.1746(4) 0.1582(2) 0.0692(14) Uani 1 1 d . . . A 1
H2A H 1.0355 0.2377 0.1571 0.083 Uiso 1 1 calc R U . A 1
H2B H 1.0784 0.1305 0.1565 0.083 Uiso 1 1 calc R U . A 1
C3 C 0.8075(6) 0.3291(3) 0.0846(2) 0.0674(13) Uani 1 1 d . . . A 1
H3A H 0.8185 0.3293 0.0455 0.081 Uiso 1 1 calc R U . A 1
H3B H 0.9120 0.3390 0.1071 0.081 Uiso 1 1 calc R U . A 1
C4 C 0.6980(6) 0.4078(3) 0.0951(2) 0.0629(13) Uani 1 1 d . . . A 1
C5 C 0.6885(8) 0.4903(4) 0.0641(2) 0.0869(18) Uani 1 1 d . . . A 1
H5 H 0.7456 0.4970 0.0352 0.104 Uiso 1 1 calc R U . A 1
C6 C 0.5933(9) 0.5618(4) 0.0770(3) 0.098(2) Uani 1 1 d . . . A 1
H6 H 0.5853 0.6176 0.0565 0.117 Uiso 1 1 calc R U . A 1
C7 C 0.5100(8) 0.5512(4) 0.1198(2) 0.0856(17) Uani 1 1 d . . . A 1
H7 H 0.4453 0.5992 0.1291 0.103 Uiso 1 1 calc R U . A 1
C8 C 0.5247(6) 0.4678(4) 0.1487(2) 0.0708(14) Uani 1 1 d . . . A 1
H8 H 0.4687 0.4603 0.1779 0.085 Uiso 1 1 calc R U . A 1
C1A C 0.9353(5) 0.1612(4) 0.21399(19) 0.0620(13) Uani 1 1 d . . . A 1
H1A1 H 1.0289 0.1613 0.2439 0.074 Uiso 1 1 calc R U . A 1
C2A C 0.8527(6) 0.0673(3) 0.2155(2) 0.0643(13) Uani 1 1 d . . . A 1
H2A1 H 0.8054 0.0647 0.2489 0.077 Uiso 1 1 calc R U . A 1
H2A2 H 0.9320 0.0177 0.2184 0.077 Uiso 1 1 calc R U . A 1
C3A C 0.8090(6) 0.2492(4) 0.28243(19) 0.0692(14) Uani 1 1 d . . . A 1
H3A1 H 0.8843 0.2942 0.3021 0.083 Uiso 1 1 calc R U . A 1
H3A2 H 0.8321 0.1883 0.3002 0.083 Uiso 1 1 calc R U . A 1
C4A C 0.6419(6) 0.2787(3) 0.28823(18) 0.0520(11) Uani 1 1 d . . . A 1
C5A C 0.6087(7) 0.2968(4) 0.34111(19) 0.0682(14) Uani 1 1 d . . . A 1
H5A H 0.6888 0.2947 0.3726 0.082 Uiso 1 1 calc R U . A 1
C6A C 0.4551(8) 0.3177(4) 0.3460(2) 0.0844(17) Uani 1 1 d . . . A 1
H6A H 0.4298 0.3299 0.3810 0.101 Uiso 1 1 calc R U . A 1
C7A C 0.3400(7) 0.3206(4) 0.2994(2) 0.0775(15) Uani 1 1 d . . . A 1
H7A H 0.2352 0.3343 0.3020 0.093 Uiso 1 1 calc R U . A 1
C8A C 0.3823(6) 0.3028(4) 0.2484(2) 0.0639(13) Uani 1 1 d . . . A 1
H8A H 0.3036 0.3046 0.2165 0.077 Uiso 1 1 calc R U . A 1
C1B C 0.7238(6) 0.0472(3) 0.16476(19) 0.0620(12) Uani 1 1 d . . . A 1
H1B1 H 0.6968 -0.0198 0.1657 0.074 Uiso 1 1 calc R U . A 1
C2B C 0.7830(6) 0.0658(4) 0.1099(2) 0.0687(14) Uani 1 1 d . . . A 1
H2B1 H 0.8570 0.0163 0.1045 0.082 Uiso 1 1 calc R U . A 1
H2B2 H 0.6932 0.0620 0.0792 0.082 Uiso 1 1 calc R U . A 1
C3B C 0.4346(6) 0.0682(3) 0.1318(2) 0.0777(16) Uani 1 1 d . . . A 1
H3B1 H 0.3609 0.0436 0.1544 0.093 Uiso 1 1 calc R U . A 1
H3B2 H 0.4643 0.0165 0.1097 0.093 Uiso 1 1 calc R U . A 1
C4B C 0.3511(5) 0.1407(3) 0.09322(17) 0.0546(11) Uani 1 1 d . . . A 1
C5B C 0.2422(6) 0.1139(4) 0.0464(2) 0.0720(14) Uani 1 1 d . . . A 1
H5B H 0.2243 0.0505 0.0378 0.086 Uiso 1 1 calc R U . A 1
C6B C 0.1619(7) 0.1820(5) 0.0133(2) 0.0856(18) Uani 1 1 d . . . A 1
H6B H 0.0905 0.1653 -0.0188 0.103 Uiso 1 1 calc R U . A 1
C7B C 0.1862(6) 0.2753(5) 0.0273(2) 0.0784(16) Uani 1 1 d . . . A 1
H7B H 0.1291 0.3224 0.0059 0.094 Uiso 1 1 calc R U . A 1
C8B C 0.2960(6) 0.2966(4) 0.0733(2) 0.0643(13) Uani 1 1 d . . . A 1
H8B H 0.3140 0.3597 0.0826 0.077 Uiso 1 1 calc R U . A 1


_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.
;

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 N2A 2.137(3) . ?
Zn1 N1B 2.158(4) . ?
Zn1 N2 2.160(4) . ?
Zn1 N1 2.164(3) . ?
Zn1 N1A 2.174(4) . ?
Zn1 N2B 2.219(4) . ?
Cl1 O1 1.371(5) . ?
Cl1 O4 1.378(4) . ?
Cl1 O2 1.383(4) . ?
Cl1 O3 1.416(5) . ?
Cl2 O5 1.376(4) . ?
Cl2 O8 1.411(8) . ?
Cl2 O6 1.410(6) . ?
Cl2 O7 1.424(8) . ?
O9A O9B 0.975(17) . ?
N1 C1 1.480(6) . ?
N1 C3 1.482(6) . ?
N1 H1 0.9800 . ?
N2 C4 1.333(6) . ?
N2 C8 1.349(6) . ?
N1A C3A 1.476(6) . ?
N1A C1A 1.501(6) . ?
N1A H1A 0.9800 . ?
N2A C4A 1.321(5) . ?
N2A C8A 1.340(6) . ?
N1B C3B 1.479(6) . ?
N1B C1B 1.485(6) . ?
N1B H1B 0.9800 . ?
N2B C4B 1.335(6) . ?
N2B C8B 1.349(6) . ?
C1 C2 1.517(7) . ?
C1 C2B 1.520(7) . ?
C1 H1C 0.9800 . ?
C2 C1A 1.533(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.508(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.386(7) . ?
C5 C6 1.371(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.369(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.369(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C1A C2A 1.512(7) . ?
C1A H1A1 0.9800 . ?
C2A C1B 1.524(6) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C3A C4A 1.519(7) . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C4A C5A 1.387(6) . ?
C5A C6A 1.372(7) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.360(7) . ?
C6A H6A 0.9300 . ?
C7A C8A 1.373(7) . ?
C7A H7A 0.9300 . ?
C8A H8A 0.9300 . ?
C1B C2B 1.529(6) . ?
C1B H1B1 0.9800 . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
C3B C4B 1.486(6) . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C4B C5B 1.386(6) . ?
C5B C6B 1.362(8) . ?
C5B H5B 0.9300 . ?
C6B C7B 1.374(8) . ?
C6B H6B 0.9300 . ?
C7B C8B 1.358(7) . ?
C7B H7B 0.9300 . ?
C8B H8B 0.9300 . ?

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
N2A Zn1 N1B 95.82(14) . . ?
N2A Zn1 N2 97.11(14) . . ?
N1B Zn1 N2 164.27(13) . . ?
N2A Zn1 N1 164.67(15) . . ?
N1B Zn1 N1 91.00(14) . . ?
N2 Zn1 N1 78.69(14) . . ?
N2A Zn1 N1A 79.19(14) . . ?
N1B Zn1 N1A 90.13(14) . . ?
N2 Zn1 N1A 101.06(14) . . ?
N1 Zn1 N1A 87.11(14) . . ?
N2A Zn1 N2B 102.91(14) . . ?
N1B Zn1 N2B 78.51(14) . . ?
N2 Zn1 N2B 89.87(14) . . ?
N1 Zn1 N2B 91.89(14) . . ?
N1A Zn1 N2B 168.59(14) . . ?
O1 Cl1 O4 113.1(4) . . ?
O1 Cl1 O2 112.0(4) . . ?
O4 Cl1 O2 111.0(4) . . ?
O1 Cl1 O3 106.4(4) . . ?
O4 Cl1 O3 105.3(4) . . ?
O2 Cl1 O3 108.7(3) . . ?
O5 Cl2 O8 104.1(9) . . ?
O5 Cl2 O6 121.8(4) . . ?
O8 Cl2 O6 103.1(9) . . ?
O5 Cl2 O7 119.9(7) . . ?
O8 Cl2 O7 106.7(15) . . ?
O6 Cl2 O7 99.6(9) . . ?
C1 N1 C3 114.0(4) . . ?
C1 N1 Zn1 115.5(3) . . ?
C3 N1 Zn1 110.4(3) . . ?
C1 N1 H1 105.3 . . ?
C3 N1 H1 105.3 . . ?
Zn1 N1 H1 105.3 . . ?
C4 N2 C8 118.2(4) . . ?
C4 N2 Zn1 114.4(3) . . ?
C8 N2 Zn1 126.0(3) . . ?
C3A N1A C1A 112.4(3) . . ?
C3A N1A Zn1 111.8(3) . . ?
C1A N1A Zn1 114.8(3) . . ?
C3A N1A H1A 105.7 . . ?
C1A N1A H1A 105.7 . . ?
Zn1 N1A H1A 105.7 . . ?
C4A N2A C8A 118.1(4) . . ?
C4A N2A Zn1 116.3(3) . . ?
C8A N2A Zn1 125.6(3) . . ?
C3B N1B C1B 113.3(4) . . ?
C3B N1B Zn1 112.3(3) . . ?
C1B N1B Zn1 114.0(3) . . ?
C3B N1B H1B 105.4 . . ?
C1B N1B H1B 105.4 . . ?
Zn1 N1B H1B 105.4 . . ?
C4B N2B C8B 117.6(4) . . ?
C4B N2B Zn1 113.0(3) . . ?
C8B N2B Zn1 127.0(3) . . ?
N1 C1 C2 113.1(4) . . ?
N1 C1 C2B 109.9(4) . . ?
C2 C1 C2B 110.3(4) . . ?
N1 C1 H1C 107.8 . . ?
C2 C1 H1C 107.8 . . ?
C2B C1 H1C 107.8 . . ?
C1 C2 C1A 114.2(4) . . ?
C1 C2 H2A 108.7 . . ?
C1A C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C1A C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N1 C3 C4 110.7(4) . . ?
N1 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N2 C4 C5 121.8(5) . . ?
N2 C4 C3 117.3(4) . . ?
C5 C4 C3 120.8(5) . . ?
C6 C5 C4 118.9(6) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C7 C6 C5 120.0(5) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C8 C7 C6 118.1(6) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
N2 C8 C7 123.0(5) . . ?
N2 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
N1A C1A C2A 112.9(4) . . ?
N1A C1A C2 109.4(4) . . ?
C2A C1A C2 110.7(4) . . ?
N1A C1A H1A1 107.9 . . ?
C2A C1A H1A1 107.9 . . ?
C2 C1A H1A1 107.9 . . ?
C1A C2A C1B 114.8(4) . . ?
C1A C2A H2A1 108.6 . . ?
C1B C2A H2A1 108.6 . . ?
C1A C2A H2A2 108.6 . . ?
C1B C2A H2A2 108.6 . . ?
H2A1 C2A H2A2 107.6 . . ?
N1A C3A C4A 113.4(4) . . ?
N1A C3A H3A1 108.9 . . ?
C4A C3A H3A1 108.9 . . ?
N1A C3A H3A2 108.9 . . ?
C4A C3A H3A2 108.9 . . ?
H3A1 C3A H3A2 107.7 . . ?
N2A C4A C5A 122.3(5) . . ?
N2A C4A C3A 118.5(4) . . ?
C5A C4A C3A 119.2(4) . . ?
C6A C5A C4A 118.5(5) . . ?
C6A C5A H5A 120.7 . . ?
C4A C5A H5A 120.7 . . ?
C7A C6A C5A 119.7(5) . . ?
C7A C6A H6A 120.1 . . ?
C5A C6A H6A 120.1 . . ?
C6A C7A C8A 118.4(5) . . ?
C6A C7A H7A 120.8 . . ?
C8A C7A H7A 120.8 . . ?
N2A C8A C7A 122.9(5) . . ?
N2A C8A H8A 118.5 . . ?
C7A C8A H8A 118.5 . . ?
N1B C1B C2A 109.3(4) . . ?
N1B C1B C2B 113.1(4) . . ?
C2A C1B C2B 111.5(4) . . ?
N1B C1B H1B1 107.6 . . ?
C2A C1B H1B1 107.6 . . ?
C2B C1B H1B1 107.6 . . ?
C1 C2B C1B 114.8(4) . . ?
C1 C2B H2B1 108.6 . . ?
C1B C2B H2B1 108.6 . . ?
C1 C2B H2B2 108.6 . . ?
C1B C2B H2B2 108.6 . . ?
H2B1 C2B H2B2 107.5 . . ?
N1B C3B C4B 114.9(4) . . ?
N1B C3B H3B1 108.5 . . ?
C4B C3B H3B1 108.5 . . ?
N1B C3B H3B2 108.5 . . ?
C4B C3B H3B2 108.5 . . ?
H3B1 C3B H3B2 107.5 . . ?
N2B C4B C5B 121.9(5) . . ?
N2B C4B C3B 117.8(4) . . ?
C5B C4B C3B 120.2(5) . . ?
C6B C5B C4B 118.9(5) . . ?
C6B C5B H5B 120.6 . . ?
C4B C5B H5B 120.6 . . ?
C5B C6B C7B 120.0(5) . . ?
C5B C6B H6B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
C8B C7B C6B 118.0(5) . . ?
C8B C7B H7B 121.0 . . ?
C6B C7B H7B 121.0 . . ?
N2B C8B C7B 123.5(5) . . ?
N2B C8B H8B 118.2 . . ?
C7B C8B H8B 118.2 . . ?

_refine_diff_density_max         0.415
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1526246'
_audit_update_record             
;
2017-01-08 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_4                   
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: Shift of disordered solvent atoms.
;
_vrf_PLAT080_4                   
;
PROBLEM: Maximum Shift/Error ............................       2.59 Why ?
RESPONSE: Disordered solvent atoms
;
_vrf_PLAT245_4                   
;
PROBLEM: U(iso) H21A    Smaller than U(eq) O2W     by ...      0.617 AngSq
RESPONSE: Disordered solvent water
;
_vrf_PLAT411_4                   
;
PROBLEM: Short Inter H...H Contact  H12A   ..  H70A    ..       1.47 Ang.
RESPONSE: Solvent water hydrogen, it is a disordered molecule.
;
_vrf_PLAT413_4                   
;
PROBLEM: Short Inter XH3 .. XHn     H2B    ..  H13B    ..       1.85 Ang.
RESPONSE: Solvent water hydrogen, it is a disordered molecule.
;
_vrf_PLAT415_4                   
;
PROBLEM: Short Inter D-H..H-X       H4     ..  H13B    ..       1.66 Ang.
RESPONSE: Solvent water hydrogen, it is a disordered molecule.
;
_vrf_PLAT482_4                   
;
PROBLEM: Small D-H..A Angle Rep for O11    ..  CL3     ..      11.00 Degree
RESPONSE: Chloride is the counter ion, electrostatic interaction.
;
_vrf_PLAT728_4                   
;
PROBLEM: D-H..A  Calc     109(19), Rep       11.00 Dev...      98.00 Degree
RESPONSE: Disordered solvent molecule.
;
# Added during the CSD deposition process: Sunday 08 January 2017 01:44 PM
# end Validation Reply Form

_publcif_datablock.id            {323cb2f9-b221-40f0-9a7c-3100bf0d038b}

_audit_creation_date             2016-07-08T15:13:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#==============================================================================

# CHEMICAL DATA
_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'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'


_chemical_name_systematic        ?
_chemical_formula_moiety         
'C144 H198 Cl11 Cu11 N42, 6(C2 H6 O), 11(Cl), 6(H2O)'
_chemical_formula_sum            'C156 H246 Cl22 Cu11 N42 O12'
_chemical_formula_weight         4380.77
_chemical_absolute_configuration unk

#==============================================================================

# CRYSTAL DATA

_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I 2 3'
_space_group_name_Hall           'I 2 2 3'
_cell_length_a                   26.85010(10)
_cell_length_b                   26.85010(10)
_cell_length_c                   26.85010(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19357.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9060
_exptl_absorpt_coefficient_mu    4.599
_cell_measurement_reflns_used    30575
_cell_measurement_theta_min      3.2680
_cell_measurement_theta_max      73.2610
_exptl_absorpt_correction_T_min  0.63038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_number            73532
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_theta_min         3.292
_diffrn_reflns_theta_max         73.746
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.5908
_diffrn_measurement_method       'ω scans'

# STRUCTURE SOLUTION

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_atom_sites_solution_hydrogens   mixed

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_reflns_number_total             6505
_reflns_number_gt                6034
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0837
_refine_ls_wR_factor_ref         0.2415
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_restrained_S_all      1.09
_refine_ls_number_reflns         6505
_refine_ls_number_parameters     381
_refine_ls_number_restraints     5
_refine_ls_number_constraints    0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1878P)²+9.7076P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max          2.593
_refine_ls_shift/su_mean         0.02
_refine_diff_density_max         1.688
_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C2 0.2419(4) 0.0852(4) 0.5505(4) 0.080(3) Uani d 1 . . C
H2A 0.2575 0.0527 0.548 0.096 Uiso calc 1 . . H
H2B 0.2631 0.1059 0.5712 0.096 Uiso calc 1 . . H
C3 0.1935(4) 0.0796(4) 0.5751(5) 0.085(3) Uani d 1 . . C
H3A 0.1983 0.0707 0.6098 0.102 Uiso calc 1 . . H
H3B 0.1746 0.0533 0.5592 0.102 Uiso calc 1 . . H
C5 0.2867(3) 0.1315(4) 0.4846(4) 0.081(3) Uani d 1 . . C
H5A 0.2884 0.1334 0.4485 0.098 Uiso calc 1 . . H
H5B 0.3144 0.1113 0.4961 0.098 Uiso calc 1 . . H
C6 0.2909(3) 0.1840(3) 0.5067(5) 0.079(2) Uani d 1 . . C
H6A 0.2955 0.1819 0.5425 0.095 Uiso calc 1 . . H
H6B 0.3195 0.201 0.4927 0.095 Uiso calc 1 . . H
C8 0.2227(4) 0.0698(4) 0.4646(4) 0.085(3) Uani d 1 . . C
H8A 0.1981 0.0487 0.4806 0.102 Uiso calc 1 . . H
H8B 0.2509 0.0491 0.4555 0.102 Uiso calc 1 . . H
C9 0.2007(5) 0.0919(5) 0.4187(4) 0.095(4) Uani d 1 . . C
H9A 0.2271 0.1044 0.3976 0.114 Uiso calc 1 . . H
H9B 0.183 0.0662 0.4004 0.114 Uiso calc 1 . . H
C12 0.209(2) 0.2229(11) 0.6310(13) 0.45(6) Uani d 1 . . C
H12A 0.2149 0.2345 0.5972 0.537 Uiso calc 1 . . H
H12B 0.1746 0.2126 0.6326 0.537 Uiso calc 1 . . H
C13 0.2389(5) 0.1785(10) 0.6373(6) 0.142(8) Uani d 1 . . C
H13A 0.2722 0.1877 0.6465 0.213 Uiso calc 1 . . H
H13B 0.2396 0.1602 0.6066 0.213 Uiso calc 1 . . H
H13C 0.2245 0.1582 0.6629 0.213 Uiso calc 1 . . H
C20 0.1136(3) 0.1186(4) 0.4223(4) 0.069(2) Uani d 1 . . C
H20A 0.0926 0.1464 0.432 0.083 Uiso calc 1 . . H
H20B 0.1054 0.0907 0.4438 0.083 Uiso calc 1 . . H
C22 0.0676(3) 0.0668(3) 0.3597(3) 0.0633(18) Uani d 1 . . C
H22 0.0542 0.0494 0.3865 0.076 Uiso calc 1 . . H
C23 0.1015(3) 0.1046(3) 0.3694(4) 0.0619(18) Uani d 1 . . C
C24 0.1234(3) 0.1274(4) 0.3274(4) 0.071(2) Uani d 1 . . C
H24 0.1476 0.1518 0.3319 0.085 Uiso calc 1 . . H
C25 0.1092(5) 0.1139(5) 0.2796(4) 0.084(3) Uani d 1 . . C
H25 0.1224 0.1301 0.252 0.101 Uiso calc 1 . . H
C26 0.0745(4) 0.0755(4) 0.2737(3) 0.074(2) Uani d 1 . . C
H26 0.0665 0.0647 0.2418 0.088 Uiso calc 1 . . H
C30 0.1129(3) 0.1210(4) 0.5825(4) 0.071(2) Uani d 1 . . C
H30A 0.0995 0.0959 0.5602 0.085 Uiso calc 1 . . H
H30B 0.0959 0.1521 0.5753 0.085 Uiso calc 1 . . H
C32 0.0670(3) 0.0681(4) 0.6441(3) 0.0654(19) Uani d 1 . . C
H32 0.053 0.0521 0.6167 0.079 Uiso calc 1 . . H
C33 0.1015(3) 0.1061(4) 0.6352(3) 0.0646(18) Uani d 1 . . C
C34 0.1211(5) 0.1297(5) 0.6750(4) 0.092(3) Uani d 1 . . C
H34 0.1425 0.1566 0.6709 0.111 Uiso calc 1 . . H
C35 0.1086(6) 0.1130(7) 0.7222(5) 0.107(5) Uani d 1 . . C
H35 0.1242 0.1267 0.7499 0.128 Uiso calc 1 . . H
C36 0.0744(4) 0.0775(5) 0.7282(4) 0.083(3) Uani d 1 . . C
H36 0.0648 0.0689 0.7604 0.1 Uiso calc 1 . . H
C70 0.2412(5) 0.2612(4) 0.5160(5) 0.098(3) Uani d 1 . . C
H70A 0.2314 0.2578 0.5506 0.117 Uiso calc 1 . . H
H70B 0.2141 0.2778 0.4989 0.117 Uiso calc 1 . . H
C72 0.3019(6) 0.3099(6) 0.5585(7) 0.114(4) Uani d 1 . . C
H72 0.2859 0.2984 0.587 0.137 Uiso calc 1 . . H
C73 0.2851(5) 0.2945(4) 0.5143(5) 0.093(3) Uani d 1 . . C
C74 0.3076(9) 0.3131(7) 0.4711(9) 0.141(7) Uani d 1 . . C
H74 0.2964 0.3043 0.4395 0.169 Uiso calc 1 . . H
C75 0.3493(14) 0.3468(8) 0.4781(9) 0.166(11) Uani d 1 . . C
H75 0.3665 0.3615 0.4519 0.199 Uiso calc 1 . . H
C76 0.3604(7) 0.3546(7) 0.5255(7) 0.118(5) Uani d 1 . . C
H76 0.3886 0.3743 0.5299 0.142 Uiso calc 1 . . H
N1 0.23903(19) 0.10774(19) 0.4995(3) 0.0576(11) Uani d 1 . . N
N4 0.1661(3) 0.1273(3) 0.5716(2) 0.0608(15) Uani d 1 . . N
H4 0.1795 0.149 0.5977 0.073 Uiso calc 1 . . H
N7 0.2455(3) 0.2118(3) 0.4955(5) 0.089(2) Uani d 1 . . N
H7 0.2477 0.2177 0.4595 0.107 Uiso calc 1 . . H
N10 0.1663(3) 0.1324(3) 0.4305(3) 0.0658(16) Uani d 1 . . N
H10 0.1736 0.1592 0.4068 0.079 Uiso calc 1 . . H
N21 0.0527(3) 0.0539(3) 0.3128(3) 0.0683(17) Uani d 1 . . N
N31 0.0530(3) 0.0533(3) 0.6895(3) 0.0657(16) Uani d 1 . . N
N71 0.3415(5) 0.3416(4) 0.5642(5) 0.106(3) Uani d 1 . . N
O1W 0.3397(9) 0 0.5 0.206(11) Uani d 1 . . O
O2W 0 0 0.0899(16) 0.74(10) Uani d 1 . . O
O11 0.2138(13) 0.2655(9) 0.6627(11) 0.232(11) Uani d 1 . . O
Cl1 0.12676(7) 0.21857(7) 0.50315(10) 0.0771(5) Uani d 1 . . Cl
Cl2 0 0 0.20812(8) 0.0814(7) Uani d 1 . . Cl
Cl3 0.3113(2) 0.3113(2) 0.6887(2) 0.152(3) Uani d 1 . . Cl
Cl4 0.09504(11) 0 0.5 0.0935(8) Uani d 1 . . Cl
Cl5 0.2306(3) 0.2186(3) 0.3726(2) 0.185(3) Uani d 1 . . Cl
Cl6 0 0 0.440(2) 0.86(10) Uani d 0.6667 . . Cl
Cu1 0.18552(3) 0.16063(3) 0.50221(5) 0.0573(3) Uani d 1 . . Cu
Cu2 0 0 0.30045(4) 0.0607(4) Uani d 1 . . Cu
Cu3 0.36386(12) 0.36386(12) 0.63614(12) 0.1277(13) Uani d 1 . . Cu
H11 0.221(12) 0.278(11) 0.691(6) 0.192 Uiso d 1 . . H
H11A 0.3080(11) 0 0.5 0.153 Uiso d 1 . . H
H11B 0.3714(11) 0 0.5 0.153 Uiso d 1 . . H
H21A -0.020(7) -0.025(6) 0.095(9) 0.153 Uiso d 1 . . H



#==============================================================================

# MOLECULAR GEOMETRY

_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.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C2 C3 . 1.466(14) ?
C2 N1 . 1.499(11) ?
C2 H2A . 0.97 ?
C2 H2B . 0.97 ?
C3 N4 . 1.481(12) ?
C3 H3A . 0.97 ?
C3 H3B . 0.97 ?
C5 N1 . 1.486(11) ?
C5 C6 . 1.534(14) ?
C5 H5A . 0.97 ?
C5 H5B . 0.97 ?
C6 N7 . 1.462(11) ?
C6 H6A . 0.97 ?
C6 H6B . 0.97 ?
C8 N1 . 1.453(13) ?
C8 C9 . 1.489(16) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
C9 N10 . 1.462(11) ?
C9 H9A . 0.97 ?
C9 H9B . 0.97 ?
C12 O11 . 1.43(3) ?
C12 C13 . 1.445(14) ?
C12 H12A . 0.97 ?
C12 H12B . 0.97 ?
C13 H13A . 0.96 ?
C13 H13B . 0.96 ?
C13 H13C . 0.96 ?
C20 N10 . 1.481(13) ?
C20 C23 . 1.505(13) ?
C20 H20A . 0.97 ?
C20 H20B . 0.97 ?
C22 N21 . 1.367(11) ?
C22 C23 . 1.386(12) ?
C22 H22 . 0.9302 ?
C23 C24 . 1.413(13) ?
C24 C25 . 1.387(15) ?
C24 H24 . 0.93 ?
C25 C26 . 1.398(15) ?
C25 H25 . 0.9301 ?
C26 N21 . 1.333(12) ?
C26 H26 . 0.9299 ?
C30 N4 . 1.468(11) ?
C30 C33 . 1.502(13) ?
C30 H30A . 0.97 ?
C30 H30B . 0.97 ?
C32 N31 . 1.336(12) ?
C32 C33 . 1.398(14) ?
C32 H32 . 0.9299 ?
C33 C34 . 1.349(15) ?
C34 C35 . 1.384(19) ?
C34 H34 . 0.93 ?
C35 C36 . 1.34(2) ?
C35 H35 . 0.9298 ?
C36 N31 . 1.353(13) ?
C36 H36 . 0.9301 ?
C70 N7 . 1.439(14) ?
C70 C73 . 1.481(17) ?
C70 H70A . 0.97 ?
C70 H70B . 0.97 ?
C72 C73 . 1.33(2) ?
C72 N71 . 1.37(2) ?
C72 H72 . 0.9303 ?
C73 C74 . 1.40(3) ?
C74 C75 . 1.45(4) ?
C74 H74 . 0.9298 ?
C75 C76 . 1.32(3) ?
C75 H75 . 0.9298 ?
C76 N71 . 1.21(2) ?
C76 H76 . 0.9298 ?
N1 Cu1 . 2.021(4) ?
N4 Cu1 . 2.132(6) ?
N4 H4 . 0.98 ?
N7 Cu1 . 2.125(8) ?
N7 H7 . 0.98 ?
N10 Cu1 . 2.131(8) ?
N10 H10 . 0.98 ?
N21 Cu2 . 2.051(8) ?
N31 Cu2 3_556 2.037(8) ?
N71 Cu3 . 2.109(13) ?
O1W H11A . 0.850(14) ?
O1W H11B . 0.853(14) ?
O2W H21A . 0.87(4) ?
O11 H11 . 0.85(3) ?
Cl1 Cu1 . 2.2159(15) ?
Cl2 Cu2 . 2.479(2) ?
Cl3 Cu3 . 2.443(11) ?
Cu2 N31 4_556 2.037(8) ?
Cu2 N31 3_556 2.037(8) ?
Cu2 N21 2 2.051(8) ?
Cu3 N71 12_566 2.109(13) ?
Cu3 N71 11_656 2.109(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
C3 C2 N1 114.0(8) . . ?
C3 C2 H2A 108.8 . . ?
N1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
N1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 N4 108.9(8) . . ?
C2 C3 H3A 109.9 . . ?
N4 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
N4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N1 C5 C6 110.7(7) . . ?
N1 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N7 C6 C5 109.1(7) . . ?
N7 C6 H6A 109.8 . . ?
C5 C6 H6A 109.9 . . ?
N7 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N1 C8 C9 112.0(9) . . ?
N1 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
N1 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N10 C9 C8 111.6(8) . . ?
N10 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
N10 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 108 . . ?
O11 C12 C13 123(3) . . ?
O11 C12 H12A 106.6 . . ?
C13 C12 H12A 106.6 . . ?
O11 C12 H12B 106.6 . . ?
C13 C12 H12B 106.6 . . ?
H12A C12 H12B 106.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N10 C20 C23 114.2(7) . . ?
N10 C20 H20A 108.7 . . ?
C23 C20 H20A 108.7 . . ?
N10 C20 H20B 108.7 . . ?
C23 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
N21 C22 C23 123.4(8) . . ?
N21 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C22 C23 C24 116.2(8) . . ?
C22 C23 C20 120.1(8) . . ?
C24 C23 C20 123.7(8) . . ?
C25 C24 C23 120.7(8) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 118.7(8) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
N21 C26 C25 121.6(8) . . ?
N21 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
N4 C30 C33 114.5(7) . . ?
N4 C30 H30A 108.6 . . ?
C33 C30 H30A 108.6 . . ?
N4 C30 H30B 108.6 . . ?
C33 C30 H30B 108.6 . . ?
H30A C30 H30B 107.6 . . ?
N31 C32 C33 123.9(8) . . ?
N31 C32 H32 118 . . ?
C33 C32 H32 118 . . ?
C34 C33 C32 117.7(9) . . ?
C34 C33 C30 122.9(9) . . ?
C32 C33 C30 119.3(8) . . ?
C33 C34 C35 118.7(12) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.6 . . ?
C36 C35 C34 120.5(11) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 N31 122.8(10) . . ?
C35 C36 H36 118.6 . . ?
N31 C36 H36 118.6 . . ?
N7 C70 C73 118.8(10) . . ?
N7 C70 H70A 107.6 . . ?
C73 C70 H70A 107.6 . . ?
N7 C70 H70B 107.6 . . ?
C73 C70 H70B 107.6 . . ?
H70A C70 H70B 107.1 . . ?
C73 C72 N71 123.7(16) . . ?
C73 C72 H72 118.2 . . ?
N71 C72 H72 118.2 . . ?
C72 C73 C74 118.7(14) . . ?
C72 C73 C70 115.4(13) . . ?
C74 C73 C70 125.7(12) . . ?
C73 C74 C75 116.5(17) . . ?
C73 C74 H74 121.7 . . ?
C75 C74 H74 121.8 . . ?
C76 C75 C74 113(2) . . ?
C76 C75 H75 123.3 . . ?
C74 C75 H75 123.3 . . ?
N71 C76 C75 133(2) . . ?
N71 C76 H76 113.3 . . ?
C75 C76 H76 113.3 . . ?
C8 N1 C5 112.8(8) . . ?
C8 N1 C2 108.8(8) . . ?
C5 N1 C2 112.1(7) . . ?
C8 N1 Cu1 107.5(5) . . ?
C5 N1 Cu1 108.7(4) . . ?
C2 N1 Cu1 106.8(5) . . ?
C30 N4 C3 111.8(8) . . ?
C30 N4 Cu1 117.4(5) . . ?
C3 N4 Cu1 107.3(5) . . ?
C30 N4 H4 106.6 . . ?
C3 N4 H4 106.6 . . ?
Cu1 N4 H4 106.6 . . ?
C70 N7 C6 117.2(10) . . ?
C70 N7 Cu1 120.2(7) . . ?
C6 N7 Cu1 106.5(6) . . ?
C70 N7 H7 103.6 . . ?
C6 N7 H7 103.6 . . ?
Cu1 N7 H7 103.6 . . ?
C9 N10 C20 112.6(9) . . ?
C9 N10 Cu1 107.9(6) . . ?
C20 N10 Cu1 117.1(6) . . ?
C9 N10 H10 106.2 . . ?
C20 N10 H10 106.2 . . ?
Cu1 N10 H10 106.2 . . ?
C26 N21 C22 119.1(8) . . ?
C26 N21 Cu2 118.9(6) . . ?
C22 N21 Cu2 121.9(6) . . ?
C32 N31 C36 116.1(8) . . ?
C32 N31 Cu2 121.8(6) . 3_556 ?
C36 N31 Cu2 122.0(7) . 3_556 ?
C76 N71 C72 114.1(15) . . ?
C76 N71 Cu3 125.9(12) . . ?
C72 N71 Cu3 120.0(11) . . ?
H11A O1W H11B 180 . . ?
C12 O11 H11 150(10) . . ?
N1 Cu1 N7 85.0(2) . . ?
N1 Cu1 N10 83.7(3) . . ?
N7 Cu1 N10 109.6(5) . . ?
N1 Cu1 N4 84.8(3) . . ?
N7 Cu1 N4 122.1(5) . . ?
N10 Cu1 N4 125.5(3) . . ?
N1 Cu1 Cl1 178.6(2) . . ?
N7 Cu1 Cl1 94.9(2) . . ?
N10 Cu1 Cl1 95.0(2) . . ?
N4 Cu1 Cl1 96.3(2) . . ?
N31 Cu2 N31 164.7(4) 4_556 3_556 ?
N31 Cu2 N21 88.0(2) 4_556 . ?
N31 Cu2 N21 89.6(2) 3_556 . ?
N31 Cu2 N21 89.6(2) 4_556 2 ?
N31 Cu2 N21 88.0(2) 3_556 2 ?
N21 Cu2 N21 161.5(4) . 2 ?
N31 Cu2 Cl2 97.6(2) 4_556 . ?
N31 Cu2 Cl2 97.6(2) 3_556 . ?
N21 Cu2 Cl2 99.3(2) . . ?
N21 Cu2 Cl2 99.3(2) 2 . ?
N71 Cu3 N71 116.1(2) 12_566 11_656 ?
N71 Cu3 N71 116.1(2) 12_566 . ?
N71 Cu3 N71 116.1(2) 11_656 . ?
N71 Cu3 Cl3 101.6(3) 12_566 . ?
N71 Cu3 Cl3 101.6(3) 11_656 . ?
N71 Cu3 Cl3 101.6(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
N1 C2 C3 N4 -49.2(14) . . . . ?
N1 C5 C6 N7 -50.8(12) . . . . ?
N1 C8 C9 N10 -45.0(15) . . . . ?
N21 C22 C23 C24 -4.5(14) . . . . ?
N21 C22 C23 C20 176.3(9) . . . . ?
N10 C20 C23 C22 143.4(9) . . . . ?
N10 C20 C23 C24 -35.7(12) . . . . ?
C22 C23 C24 C25 3.2(15) . . . . ?
C20 C23 C24 C25 -177.6(10) . . . . ?
C23 C24 C25 C26 -3.1(18) . . . . ?
C24 C25 C26 N21 4.3(19) . . . . ?
N31 C32 C33 C34 -1.1(15) . . . . ?
N31 C32 C33 C30 -177.5(8) . . . . ?
N4 C30 C33 C34 49.0(15) . . . . ?
N4 C30 C33 C32 -134.8(9) . . . . ?
C32 C33 C34 C35 4.2(19) . . . . ?
C30 C33 C34 C35 -179.6(12) . . . . ?
C33 C34 C35 C36 -6(2) . . . . ?
C34 C35 C36 N31 5(2) . . . . ?
N71 C72 C73 C74 -3(2) . . . . ?
N71 C72 C73 C70 -178.7(13) . . . . ?
N7 C70 C73 C72 -119.7(14) . . . . ?
N7 C70 C73 C74 65(2) . . . . ?
C72 C73 C74 C75 2(2) . . . . ?
C70 C73 C74 C75 177.7(16) . . . . ?
C73 C74 C75 C76 1(3) . . . . ?
C74 C75 C76 N71 -5(4) . . . . ?
C9 C8 N1 C5 -76.6(10) . . . . ?
C9 C8 N1 C2 158.4(9) . . . . ?
C9 C8 N1 Cu1 43.1(11) . . . . ?
C6 C5 N1 C8 154.8(8) . . . . ?
C6 C5 N1 C2 -82.1(9) . . . . ?
C6 C5 N1 Cu1 35.7(9) . . . . ?
C3 C2 N1 C8 -78.0(10) . . . . ?
C3 C2 N1 C5 156.6(9) . . . . ?
C3 C2 N1 Cu1 37.8(11) . . . . ?
C33 C30 N4 C3 66.0(12) . . . . ?
C33 C30 N4 Cu1 -169.4(7) . . . . ?
C2 C3 N4 C30 163.9(9) . . . . ?
C2 C3 N4 Cu1 33.9(12) . . . . ?
C73 C70 N7 C6 43.2(18) . . . . ?
C73 C70 N7 Cu1 175.1(10) . . . . ?
C5 C6 N7 C70 176.2(10) . . . . ?
C5 C6 N7 Cu1 38.4(12) . . . . ?
C8 C9 N10 C20 -107.8(11) . . . . ?
C8 C9 N10 Cu1 23.0(13) . . . . ?
C23 C20 N10 C9 -60.7(11) . . . . ?
C23 C20 N10 Cu1 173.4(6) . . . . ?
C25 C26 N21 C22 -5.5(17) . . . . ?
C25 C26 N21 Cu2 177.2(9) . . . . ?
C23 C22 N21 C26 5.7(15) . . . . ?
C23 C22 N21 Cu2 -177.1(7) . . . . ?
C33 C32 N31 C36 -0.1(14) . . . . ?
C33 C32 N31 Cu2 176.9(7) . . . 3_556 ?
C35 C36 N31 C32 -2.0(18) . . . . ?
C35 C36 N31 Cu2 -179.0(12) . . . 3_556 ?
C75 C76 N71 C72 4(4) . . . . ?
C75 C76 N71 Cu3 -175(2) . . . . ?
C73 C72 N71 C76 0(2) . . . . ?
C73 C72 N71 Cu3 179.1(11) . . . . ?

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
C2 H2A Cl1 0.97 2.67 3.308(8) 123.6 22
C8 H8B Cl1 0.97 2.66 3.422(10) 135.7 20_545
C13 H13B N4 0.96 2.36 2.969(16) 121.1 .
C13 H13C Cl5 0.96 2.51 3.08(2) 117.6 22
C20 H20A Cl1 0.97 2.87 3.471(10) 120.9 .
C20 H20B Cl4 0.97 2.88 3.838(10) 170.5 .
C22 H22 Cl6 0.93 2.44 3.34(4) 163.6 .
C25 H25 Cl3 0.93 2.92 3.814(10) 161.6 14_554
C26 H26 Cl2 0.93 2.65 3.349(9) 132.4 .
C30 H30B Cl1 0.97 2.76 3.396(10) 123.6 .
C32 H32 Cl6 0.93 2.51 3.42(4) 164.9 3_556
C36 H36 Cl2 0.93 2.68 3.352(12) 130.1 3_556
C70 H70B Cl1 0.97 2.84 3.297(13) 110 .
C72 H72 Cl3 0.93 2.84 3.505(19) 129.8 .
N7 H7 Cl5 0.98 2.38 3.327(16) 163 .
N10 H10 Cl5 0.98 2.39 3.279(11) 150 .
O11 H11 Cl3 0.85(3) 2.6(3) 2.98(3) 11E1(3) .



loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?

