# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_PEA-Mn_293K
_database_code_depnum_ccdc_archive 'CCDC 2411272'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Mn, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cl4 Mn N2'
_chemical_formula_weight         441.11
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'-x-1/2, -y, z-1/2'

_cell_length_a                   7.2039(3)
_cell_length_b                   7.2919(3)
_cell_length_c                   39.3912(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2069.22(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8216
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.8968
_exptl_absorpt_correction_T_min  0.7322
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale pink'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.144
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            19429
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         3.011
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2188
_reflns_number_total             2357
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0565
_refine_ls_restrained_S_all      1.385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+5.4436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1121
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C4(H4), C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mn01 Mn 0.000000 0.000000 0.500000 0.02300(18) Uani 1 2 d S . P . .
Cl1 Cl 0.23587(11) 0.26394(11) 0.50544(2) 0.0319(2) Uani 1 1 d . . . . .
Cl2 Cl 0.03522(13) 0.00823(14) 0.43732(2) 0.0373(2) Uani 1 1 d . . . . .
N1 N 0.5084(5) 0.0155(5) 0.55865(7) 0.0399(8) Uani 1 1 d . . . . .
H1A H 0.448965 -0.057376 0.544146 0.048 Uiso 1 1 calc R U . . .
H1B H 0.630257 0.004751 0.555538 0.048 Uiso 1 1 calc R U . . .
H1C H 0.474396 0.131280 0.555102 0.048 Uiso 1 1 calc R U . . .
C1 C 0.4607(7) -0.0382(6) 0.59406(10) 0.0446(10) Uani 1 1 d . . . . .
H1D H 0.507249 -0.160733 0.598507 0.054 Uiso 1 1 calc R U . . .
H1E H 0.326817 -0.040532 0.596636 0.054 Uiso 1 1 calc R U . . .
C3 C 0.5159(7) 0.0279(6) 0.65529(10) 0.0506(11) Uani 1 1 d . . . . .
C7 C 0.3627(9) 0.0400(9) 0.70934(14) 0.0754(17) Uani 1 1 d . . . . .
H7 H 0.270553 0.089704 0.723082 0.090 Uiso 1 1 calc R U . . .
C8 C 0.3766(9) 0.0928(8) 0.67571(13) 0.0677(15) Uani 1 1 d . . . . .
H8 H 0.289812 0.173971 0.666788 0.081 Uiso 1 1 calc R U . . .
C2 C 0.5418(9) 0.0919(7) 0.61914(11) 0.0611(14) Uani 1 1 d . . . . .
H2A H 0.483607 0.210990 0.616421 0.073 Uiso 1 1 calc R U . . .
H2B H 0.673322 0.106018 0.614580 0.073 Uiso 1 1 calc R U . . .
C4 C 0.6342(9) -0.0986(9) 0.66929(13) 0.0765(18) Uani 1 1 d . . . . .
H4 H 0.728702 -0.147847 0.656032 0.092 Uiso 1 1 calc R U . . .
C6 C 0.4834(10) -0.0840(9) 0.72221(13) 0.0796(19) Uani 1 1 d . . . . .
H6 H 0.473279 -0.119995 0.744782 0.095 Uiso 1 1 calc R U . . .
C5 C 0.6161(10) -0.1547(9) 0.70283(15) 0.083(2) Uani 1 1 d . . . . .
H5 H 0.696973 -0.241767 0.711707 0.100 Uiso 1 1 calc R 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
Mn01 Cl1 2.5747(8) 6_566 ?
Mn01 Cl1 2.5763(8) 5_556 ?
Mn01 Cl1 2.5763(8) . ?
Mn01 Cl1 2.5747(8) 2_545 ?
Mn01 Cl2 2.4826(9) . ?
Mn01 Cl2 2.4827(9) 5_556 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.489(5) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.489(6) . ?
C3 C8 1.371(7) . ?
C3 C2 1.510(6) . ?
C3 C4 1.371(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.383(7) . ?
C7 C6 1.353(9) . ?
C8 H8 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 H4 0.9300 . ?
C4 C5 1.389(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.328(9) . ?
C5 H5 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
Cl1 Mn01 Cl1 180.00(4) 6_566 2_545 ?
Cl1 Mn01 Cl1 180.00(4) 5_556 . ?
Cl1 Mn01 Cl1 89.707(5) 6_566 . ?
Cl1 Mn01 Cl1 89.708(5) 2_545 5_556 ?
Cl1 Mn01 Cl1 90.292(5) 6_566 5_556 ?
Cl1 Mn01 Cl1 90.293(5) 2_545 . ?
Cl2 Mn01 Cl1 90.16(3) 5_556 . ?
Cl2 Mn01 Cl1 88.66(3) . 6_566 ?
Cl2 Mn01 Cl1 88.66(3) 5_556 2_545 ?
Cl2 Mn01 Cl1 91.34(3) 5_556 6_566 ?
Cl2 Mn01 Cl1 90.16(3) . 5_556 ?
Cl2 Mn01 Cl1 89.84(3) . . ?
Cl2 Mn01 Cl1 91.34(3) . 2_545 ?
Cl2 Mn01 Cl1 89.84(3) 5_556 5_556 ?
Cl2 Mn01 Cl2 180.0 . 5_556 ?
Mn01 Cl1 Mn01 168.50(4) 2 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 H1E 109.4 . . ?
N1 C1 C2 111.3(4) . . ?
H1D C1 H1E 108.0 . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
C8 C3 C2 122.5(5) . . ?
C8 C3 C4 116.8(5) . . ?
C4 C3 C2 120.7(5) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.9(6) . . ?
C3 C8 C7 121.3(5) . . ?
C3 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C1 C2 C3 112.3(4) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C3 C4 H4 119.3 . . ?
C3 C4 C5 121.5(6) . . ?
C5 C4 H4 119.3 . . ?
C7 C6 H6 119.8 . . ?
C5 C6 C7 120.5(5) . . ?
C5 C6 H6 119.8 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(6) . . ?
C6 C5 H5 120.0 . . ?

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 C1 C2 C3 -172.9(4) . . . . ?
C3 C4 C5 C6 -0.8(11) . . . . ?
C7 C6 C5 C4 1.3(11) . . . . ?
C8 C3 C2 C1 -98.7(6) . . . . ?
C8 C3 C4 C5 -1.5(9) . . . . ?
C8 C7 C6 C5 0.4(10) . . . . ?
C2 C3 C8 C7 -176.1(5) . . . . ?
C2 C3 C4 C5 177.9(6) . . . . ?
C4 C3 C8 C7 3.3(9) . . . . ?
C4 C3 C2 C1 81.9(7) . . . . ?
C6 C7 C8 C3 -2.9(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PEA-Mn_433K
_database_code_depnum_ccdc_archive 'CCDC 2411274'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_vrf_PLAT043_PEA-Mn_433K         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      24.19 Check 
RESPONSE: We were not able to include hydrogen atoms due to
disorder generated by the mirror and C4 axis. Manual addition was also failed.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Mn, 4(C4 N0.5)'
_chemical_formula_sum            'C16 H24 Cl4 Mn N2'
_chemical_formula_weight         441.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H32N2MnCl4
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.16257(7)
_cell_length_b                   5.16257(7)
_cell_length_c                   39.9478(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1064.69(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7926
_cell_measurement_temperature    433.00(10)
_cell_measurement_theta_max      30.0540
_cell_measurement_theta_min      2.0170
_shelx_estimated_absorpt_T_max   0.901
_shelx_estimated_absorpt_T_min   0.696
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale pink'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 0 -8 0.1464
7 0 13 0.1457
0 -7 -10 0.1556
0 7 10 0.1705
0 0 -56 0.0378
0 0 -1 0.0490

_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.095
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.2057 -0.0386 -7.9075 -0.2157 -0.0373 0.9758
7.0944 0.0112 12.5694 0.2073 -0.0465 -0.9772
-0.0613 -7.1641 -10.0740 -0.9594 0.2297 -0.1638
0.0806 7.1632 10.1067 0.9598 -0.2298 0.1611
-0.0049 0.0511 -56.3097 0.0240 0.9820 0.1872
-0.0004 0.0007 -0.9965 0.0004 0.0174 0.0033

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            11678
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.205
_diffrn_reflns_theta_min         2.039
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      433.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  -7.00   0.50    3.00    --  -23.03 112.00 -49.00  150
  2  ω     12.00  64.00   0.50    3.00    --   24.44-112.00-141.00  104
  3  ω   -121.00 -39.00   0.50    3.00    --  -23.03 178.00 -30.00  164
  4  ω     14.00  56.00   0.50    3.00    --  -23.03  38.00  30.00   84
  5  ω     31.00  59.00   0.50    3.00    --  -23.03  19.00-180.00   56
  6  ω    -10.00  16.00   0.50    3.00    --  -23.03  19.00-180.00   52
  7  ω    -31.00  -5.00   0.50    3.00    --  -23.03  38.00  30.00   52
  8  ω    -17.00  59.00   0.50    3.00    --  -23.03  19.00 -60.00  152
  9  ω    -11.00  29.00   0.50    3.00    --  -23.03 -99.00-150.00   80
 10  ω    -16.00  53.00   0.50    3.00    --  -23.03  19.00 120.00  138
 11  ω    -17.00  15.00   0.50    3.00    --  -23.03 -99.00  30.00   64
 12  ω    -17.00  10.00   0.50    3.00    --  -23.03 -99.00 -90.00   54
 13  ω   -112.00 -39.00   0.50    3.00    --  -23.03 -77.00-180.00  146
 14  ω    -17.00  14.00   0.50    3.00    --  -23.03 -77.00-180.00   62
 15  ω    -57.00  62.00   0.50    3.00    --   24.44 -57.00-180.00  238
 16  ω     57.00  91.00   0.50    3.00    --   24.44  57.00 120.00   68
 17  ω    -15.00  50.00   0.50    3.00    --   24.44  57.00 120.00  130
 18  ω    -16.00 106.00   0.50    3.00    --   24.44  77.00-180.00  244
 19  ω     -4.00 103.00   0.50    3.00    --   24.44  57.00   0.00  214
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295498000
_diffrn_orient_matrix_UB_12      0.1340956000
_diffrn_orient_matrix_UB_13      -0.0003078000
_diffrn_orient_matrix_UB_21      0.0243660000
_diffrn_orient_matrix_UB_22      -0.0077314000
_diffrn_orient_matrix_UB_23      -0.0174489000
_diffrn_orient_matrix_UB_31      -0.1319609000
_diffrn_orient_matrix_UB_32      0.0286136000
_diffrn_orient_matrix_UB_33      -0.0032870000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                505
_reflns_number_total             544
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         544
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0811P)²+0.0124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1045
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C1-C2
 1.54 with sigma of 0.02
 C3-C5
 2.4 with sigma of 0.04
 C4-C6
 2.4 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C4 \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
3. Others
 Fixed Sof: C2(0.125) C4(0.25) C5(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mn01 Mn 0.500000 0.500000 0.500000 0.0477(2) Uani 1 16 d S T P . .
Cl1 Cl 0.000000 0.500000 0.500000 0.0705(3) Uani 1 8 d S T P . .
Cl2 Cl 0.500000 0.500000 0.43855(2) 0.0852(3) Uani 1 8 d S T P . .
N1 N 0.000000 0.000000 0.44316(8) 0.0833(10) Uani 1 8 d S T P . .
C1 C 0.000000 0.000000 0.40783(14) 0.152(3) Uani 1 8 d DS T P . .
C6 C 0.000000 0.000000 0.2836(4) 0.35(3) Uani 1 8 d DS T P . .
C2 C 0.000000 -0.172(3) 0.3849(2) 0.128(4) Uani 0.25 2 d DS T P . .
C3 C 0.000000 0.000000 0.34917(19) 0.215(8) Uani 1 8 d DS T P . .
C4 C -0.165(3) 0.165(3) 0.3319(3) 0.347(19) Uani 0.5 2 d DS TU P . .
C5 C -0.158(5) 0.158(5) 0.2981(3) 0.38(2) Uani 0.5 2 d DS TU P . .


_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
Mn01 Cl1 2.58128(3) 3_665 ?
Mn01 Cl1 2.58128(3) . ?
Mn01 Cl1 2.58128(3) 3_655 ?
Mn01 Cl1 2.58128(3) 1_655 ?
Mn01 Cl2 2.4548(8) 17_666 ?
Mn01 Cl2 2.4549(8) . ?
N1 C1 1.412(6) . ?
C1 C2 1.276(12) 4 ?
C1 C2 1.276(12) 3 ?
C1 C2 1.276(12) 2 ?
C1 C2 1.276(12) . ?
C6 C5 1.29(3) . ?
C6 C5 1.29(3) 3 ?
C6 C5 1.29(3) 2 ?
C6 C5 1.29(3) 4 ?
C2 C2 1.26(2) 3 ?
C2 C2 1.78(3) 2 ?
C2 C2 1.26(2) 4 ?
C2 C3 1.684(14) . ?
C3 C4 1.39(2) 3 ?
C3 C4 1.39(2) 4 ?
C3 C4 1.39(2) 2 ?
C3 C4 1.39(2) . ?
C4 C4 1.71(3) 4 ?
C4 C4 1.71(3) 3 ?
C4 C5 1.352(13) . ?
C5 C5 1.63(5) 3 ?
C5 C5 1.63(5) 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
Cl1 Mn01 Cl1 180.0 . 1_655 ?
Cl1 Mn01 Cl1 90.0 . 3_655 ?
Cl1 Mn01 Cl1 90.0 1_655 3_665 ?
Cl1 Mn01 Cl1 90.0 . 3_665 ?
Cl1 Mn01 Cl1 90.0 1_655 3_655 ?
Cl1 Mn01 Cl1 180.0 3_655 3_665 ?
Cl2 Mn01 Cl1 90.0 . 3_655 ?
Cl2 Mn01 Cl1 90.0 . 1_655 ?
Cl2 Mn01 Cl1 90.0 17_666 . ?
Cl2 Mn01 Cl1 90.0 . 3_665 ?
Cl2 Mn01 Cl1 90.0 17_666 3_665 ?
Cl2 Mn01 Cl1 90.0 17_666 3_655 ?
Cl2 Mn01 Cl1 90.0 . . ?
Cl2 Mn01 Cl1 90.0 17_666 1_655 ?
Cl2 Mn01 Cl2 180.0 17_666 . ?
Mn01 Cl1 Mn01 180.0 1_455 . ?
C2 C1 N1 135.8(7) 2 . ?
C2 C1 N1 135.8(7) . . ?
C2 C1 N1 135.8(7) 4 . ?
C2 C1 N1 135.8(7) 3 . ?
C2 C1 C2 59.1(8) 3 . ?
C2 C1 C2 88.5(13) 4 3 ?
C2 C1 C2 88.5(13) 2 . ?
C2 C1 C2 59.1(8) 4 . ?
C2 C1 C2 59.1(8) 4 2 ?
C2 C1 C2 59.1(8) 3 2 ?
C5 C6 C5 78.4(9) . 4 ?
C5 C6 C5 127(2) 4 3 ?
C5 C6 C5 78.4(9) 3 2 ?
C5 C6 C5 78.4(9) 4 2 ?
C5 C6 C5 127(2) . 2 ?
C5 C6 C5 78.4(9) . 3 ?
C1 C2 C2 45.8(7) . 2 ?
C1 C2 C3 103.9(10) . . ?
C2 C2 C1 60.4(4) 4 . ?
C2 C2 C1 60.4(4) 3 . ?
C2 C2 C2 45.000(5) 3 2 ?
C2 C2 C2 45.000(6) 4 2 ?
C2 C2 C2 90.000(12) 3 4 ?
C2 C2 C3 68.1(3) 3 . ?
C2 C2 C3 68.1(3) 4 . ?
C3 C2 C2 58.1(5) . 2 ?
C2 C3 C2 43.9(6) . 4 ?
C2 C3 C2 43.9(6) 2 3 ?
C2 C3 C2 43.9(6) 2 4 ?
C2 C3 C2 63.8(10) . 2 ?
C2 C3 C2 43.9(6) . 3 ?
C2 C3 C2 63.8(10) 3 4 ?
C4 C3 C2 138.2(7) 3 3 ?
C4 C3 C2 138.2(7) 4 4 ?
C4 C3 C2 95.5(8) . 2 ?
C4 C3 C2 95.5(8) 4 3 ?
C4 C3 C2 138.2(7) 4 . ?
C4 C3 C2 95.5(8) 2 3 ?
C4 C3 C2 95.5(8) 4 2 ?
C4 C3 C2 95.5(8) 3 4 ?
C4 C3 C2 138.2(7) 2 2 ?
C4 C3 C2 138.2(7) 2 4 ?
C4 C3 C2 95.5(8) . 4 ?
C4 C3 C2 138.2(7) . . ?
C4 C3 C2 138.2(7) 3 2 ?
C4 C3 C2 138.2(7) . 3 ?
C4 C3 C2 95.5(8) 3 . ?
C4 C3 C2 95.5(8) 2 . ?
C4 C3 C4 75.8(7) . 4 ?
C4 C3 C4 75.7(7) 3 2 ?
C4 C3 C4 120.5(15) . 2 ?
C4 C3 C4 75.8(7) . 3 ?
C4 C3 C4 75.7(7) 4 2 ?
C4 C3 C4 120.5(15) 3 4 ?
C3 C4 C4 52.1(3) . 3 ?
C3 C4 C4 52.1(3) . 4 ?
C4 C4 C4 90.001(9) 4 3 ?
C5 C4 C3 117.4(18) . . ?
C5 C4 C4 88.4(10) . 3 ?
C5 C4 C4 88.4(10) . 4 ?
C6 C5 C4 119(2) . . ?
C6 C5 C5 50.8(5) . 3 ?
C6 C5 C5 50.8(5) . 4 ?
C4 C5 C5 91.6(10) . 4 ?
C4 C5 C5 91.6(10) . 3 ?
C5 C5 C5 89.999(12) 4 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 C1 C2 C2 -125.6(3) . . . 3 ?
N1 C1 C2 C2 180.000(7) . . . 2 ?
N1 C1 C2 C2 125.6(3) . . . 4 ?
N1 C1 C2 C3 180.000(5) . . . . ?
C1 C2 C3 C2 -49.67(15) . . . 4 ?
C1 C2 C3 C2 49.67(14) . . . 3 ?
C1 C2 C3 C2 0.000(2) . . . 2 ?
C1 C2 C3 C4 -141.9(3) . . . 3 ?
C1 C2 C3 C4 -67.1(8) . . . . ?
C1 C2 C3 C4 141.9(3) . . . 2 ?
C1 C2 C3 C4 67.1(8) . . . 4 ?
C2 C1 C2 C2 -54.4(3) 2 . . 4 ?
C2 C1 C2 C2 -108.8(6) 3 . . 4 ?
C2 C1 C2 C2 54.4(3) 4 . . 2 ?
C2 C1 C2 C2 54.4(3) 2 . . 3 ?
C2 C1 C2 C2 -54.4(3) 3 . . 2 ?
C2 C1 C2 C2 108.8(6) 4 . . 3 ?
C2 C1 C2 C3 -54.4(3) 3 . . . ?
C2 C1 C2 C3 54.4(3) 4 . . . ?
C2 C1 C2 C3 0.000(2) 2 . . . ?
C2 C2 C3 C2 49.67(14) 2 . . 3 ?
C2 C2 C3 C2 -49.67(14) 3 . . 2 ?
C2 C2 C3 C2 -99.3(3) 3 . . 4 ?
C2 C2 C3 C2 -49.67(15) 2 . . 4 ?
C2 C2 C3 C2 99.3(3) 4 . . 3 ?
C2 C2 C3 C2 49.67(14) 4 . . 2 ?
C2 C2 C3 C4 -17.5(7) 4 . . . ?
C2 C2 C3 C4 67.1(8) 2 . . 4 ?
C2 C2 C3 C4 92.2(3) 3 . . 2 ?
C2 C2 C3 C4 -141.9(3) 2 . . 3 ?
C2 C2 C3 C4 -168.4(3) 4 . . 2 ?
C2 C2 C3 C4 116.8(9) 4 . . 4 ?
C2 C2 C3 C4 -67.1(8) 2 . . . ?
C2 C2 C3 C4 -116.8(9) 3 . . . ?
C2 C2 C3 C4 168.4(3) 3 . . 3 ?
C2 C2 C3 C4 17.5(7) 3 . . 4 ?
C2 C2 C3 C4 141.9(3) 2 . . 2 ?
C2 C2 C3 C4 -92.2(3) 4 . . 3 ?
C2 C3 C4 C4 150.5(12) . . . 4 ?
C2 C3 C4 C4 -150.5(12) 3 . . 3 ?
C2 C3 C4 C4 -138.4(6) 2 . . 3 ?
C2 C3 C4 C4 -82.3(7) . . . 3 ?
C2 C3 C4 C4 138.4(6) 4 . . 4 ?
C2 C3 C4 C4 -94.3(6) 4 . . 3 ?
C2 C3 C4 C4 94.3(6) 2 . . 4 ?
C2 C3 C4 C4 82.3(7) 3 . . 4 ?
C2 C3 C4 C5 145.9(8) 3 . . . ?
C2 C3 C4 C5 -157.9(3) 4 . . . ?
C2 C3 C4 C5 157.9(3) 2 . . . ?
C2 C3 C4 C5 -145.9(8) . . . . ?
C3 C4 C5 C6 0.000(4) . . . . ?
C3 C4 C5 C5 -45.02(2) . . . 4 ?
C3 C4 C5 C5 45.02(2) . . . 3 ?
C4 C3 C4 C4 -63.6(5) 2 . . 4 ?
C4 C3 C4 C4 63.6(5) 2 . . 3 ?
C4 C3 C4 C4 -127.2(10) 3 . . 4 ?
C4 C3 C4 C4 127.2(10) 4 . . 3 ?
C4 C3 C4 C5 -63.6(5) 3 . . . ?
C4 C3 C4 C5 0.000(3) 2 . . . ?
C4 C3 C4 C5 63.6(5) 4 . . . ?
C4 C4 C5 C6 -45.02(3) 3 . . . ?
C4 C4 C5 C6 45.02(3) 4 . . . ?
C4 C4 C5 C5 -90.05(5) 3 . . 4 ?
C4 C4 C5 C5 -0.001(12) 3 . . 3 ?
C4 C4 C5 C5 0.001(14) 4 . . 4 ?
C4 C4 C5 C5 90.05(5) 4 . . 3 ?
C5 C6 C5 C4 -65.8(8) 4 . . . ?
C5 C6 C5 C4 65.8(8) 3 . . . ?
C5 C6 C5 C4 0.000(4) 2 . . . ?
C5 C6 C5 C5 -131.7(17) 4 . . 3 ?
C5 C6 C5 C5 131.7(17) 3 . . 4 ?
C5 C6 C5 C5 -65.8(8) 2 . . 3 ?
C5 C6 C5 C5 65.8(8) 2 . . 4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.672
_oxdiff_exptl_absorpt_empirical_full_min 0.527
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PEA-Cu_293K
_database_code_depnum_ccdc_archive 'CCDC 2411275'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Cu, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cl4 Cu N2'
_chemical_formula_weight         449.71
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'-x-1/2, -y, z-1/2'

_cell_length_a                   7.2924(8)
_cell_length_b                   7.3280(8)
_cell_length_c                   38.583(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2061.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.64
_shelx_estimated_absorpt_T_max   0.743
_shelx_estimated_absorpt_T_min   0.544
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  0.78705
_exptl_absorpt_correction_T_min  0.61272
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            20160
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.578
_diffrn_reflns_theta_min         2.986
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2269
_reflns_number_total             2371
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.712
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0700
_refine_ls_restrained_S_all      1.323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+10.0628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1792
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C4(H4), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Cu01 Cu 0.000000 0.000000 0.500000 0.0240(2) Uani 1 2 d S . P . .
Cl2 Cl 0.02867(18) -0.01207(18) 0.44081(3) 0.0381(3) Uani 1 1 d . . . . .
Cl1 Cl 0.28364(14) 0.27609(15) 0.50523(3) 0.0308(3) Uani 1 1 d . . . . .
N1 N 0.5121(6) -0.0046(7) 0.55509(12) 0.0396(11) Uani 1 1 d . . . . .
H1A H 0.471566 0.083331 0.541140 0.048 Uiso 1 1 calc R U . . .
H1B H 0.458215 -0.109551 0.549537 0.048 Uiso 1 1 calc R U . . .
H1C H 0.632985 -0.015718 0.552725 0.048 Uiso 1 1 calc R U . . .
C1 C 0.4680(9) 0.0425(9) 0.59157(16) 0.0491(14) Uani 1 1 d . . . . .
H1D H 0.513349 0.164134 0.596516 0.059 Uiso 1 1 calc R U . . .
H1E H 0.335834 0.043992 0.594433 0.059 Uiso 1 1 calc R U . . .
C3 C 0.5202(11) -0.0274(10) 0.65355(17) 0.0610(19) Uani 1 1 d . . . . .
C5 C 0.3678(14) -0.0473(13) 0.7088(2) 0.082(3) Uani 1 1 d . . . . .
H5 H 0.278703 -0.100820 0.722760 0.098 Uiso 1 1 calc R U . . .
C8 C 0.6303(15) 0.1024(14) 0.6682(2) 0.089(3) Uani 1 1 d . . . . .
H8 H 0.718979 0.160340 0.654832 0.107 Uiso 1 1 calc R U . . .
C4 C 0.3809(13) -0.0950(12) 0.67389(19) 0.075(2) Uani 1 1 d . . . . .
H4 H 0.294441 -0.173328 0.664259 0.089 Uiso 1 1 calc R U . . .
C2 C 0.5478(14) -0.0863(11) 0.61654(17) 0.072(2) Uani 1 1 d . . . . .
H2A H 0.678115 -0.097904 0.612018 0.086 Uiso 1 1 calc R U . . .
H2B H 0.492342 -0.205378 0.613235 0.086 Uiso 1 1 calc R U . . .
C6 C 0.4834(14) 0.0754(15) 0.72225(18) 0.082(3) Uani 1 1 d . . . . .
H6 H 0.472959 0.108602 0.745425 0.099 Uiso 1 1 calc R U . . .
C7 C 0.6107(15) 0.1487(14) 0.7031(2) 0.088(3) Uani 1 1 d . . . . .
H7 H 0.690141 0.233698 0.712847 0.105 Uiso 1 1 calc R 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
Cu01 Cl2 2.2950(13) . ?
Cu01 Cl2 2.2950(13) 5_556 ?
Cu01 Cl1 2.9004(11) 5_556 ?
Cu01 Cl1 2.2853(10) 2_545 ?
Cu01 Cl1 2.9004(11) . ?
Cu01 Cl1 2.2853(10) 6_566 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.484(8) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.469(9) . ?
C3 C8 1.368(11) . ?
C3 C4 1.376(11) . ?
C3 C2 1.505(9) . ?
C5 H5 0.9300 . ?
C5 C4 1.396(11) . ?
C5 C6 1.337(14) . ?
C8 H8 0.9300 . ?
C8 C7 1.395(11) . ?
C4 H4 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C7 1.303(13) . ?
C7 H7 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
Cl2 Cu01 Cl2 180.0 5_556 . ?
Cl2 Cu01 Cl1 91.78(4) . . ?
Cl2 Cu01 Cl1 91.78(4) 5_556 5_556 ?
Cl2 Cu01 Cl1 88.22(4) 5_556 . ?
Cl2 Cu01 Cl1 88.22(4) . 5_556 ?
Cl1 Cu01 Cl2 89.85(4) 6_566 5_556 ?
Cl1 Cu01 Cl2 90.15(4) 6_566 . ?
Cl1 Cu01 Cl2 89.85(4) 2_545 . ?
Cl1 Cu01 Cl2 90.15(4) 2_545 5_556 ?
Cl1 Cu01 Cl1 90.133(12) 6_566 5_556 ?
Cl1 Cu01 Cl1 89.867(12) 6_566 . ?
Cl1 Cu01 Cl1 89.867(12) 2_545 5_556 ?
Cl1 Cu01 Cl1 90.133(12) 2_545 . ?
Cl1 Cu01 Cl1 180.00(6) 6_566 2_545 ?
Cl1 Cu01 Cl1 180.0 5_556 . ?
Cu01 Cl1 Cu01 170.78(5) 2 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 109.0 . . ?
N1 C1 H1E 109.0 . . ?
H1D C1 H1E 107.8 . . ?
C2 C1 N1 112.8(6) . . ?
C2 C1 H1D 109.0 . . ?
C2 C1 H1E 109.0 . . ?
C8 C3 C4 116.6(7) . . ?
C8 C3 C2 120.9(8) . . ?
C4 C3 C2 122.5(8) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C6 C5 C4 120.0(8) . . ?
C3 C8 H8 119.7 . . ?
C3 C8 C7 120.5(8) . . ?
C7 C8 H8 119.7 . . ?
C3 C4 C5 120.7(8) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C1 C2 C3 112.6(6) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.5(8) . . ?
C7 C6 H6 119.8 . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.3(9) . . ?
C6 C7 H7 119.3 . . ?

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 C1 C2 C3 173.8(6) . . . . ?
C3 C8 C7 C6 -2.6(17) . . . . ?
C5 C6 C7 C8 0.1(17) . . . . ?
C8 C3 C4 C5 -7.0(13) . . . . ?
C8 C3 C2 C1 -79.8(11) . . . . ?
C4 C3 C8 C7 6.0(15) . . . . ?
C4 C3 C2 C1 97.8(10) . . . . ?
C4 C5 C6 C7 -1.2(16) . . . . ?
C2 C3 C8 C7 -176.3(9) . . . . ?
C2 C3 C4 C5 175.2(8) . . . . ?
C6 C5 C4 C3 4.8(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: distilled water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PEA-Mn_393K
_database_code_depnum_ccdc_archive 'CCDC 2411273'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Mn, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cl4 Mn N2'
_chemical_formula_weight         441.11
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'B b c m'
_space_group_name_Hall           '-B 2 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y-1/2, z-1/2'
'x, -y-1/2, z-1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y-1/2, z'
'x+1/2, -y-1/2, z'

_cell_length_a                   7.2822(13)
_cell_length_b                   7.3039(13)
_cell_length_c                   39.910(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2122.7(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4425
_cell_measurement_temperature    393(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   0.825
_shelx_estimated_absorpt_T_min   0.693
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.6954
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale pink'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.178
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            10068
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         3.984
_diffrn_ambient_temperature      393(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                975
_reflns_number_total             1221
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1221
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.262
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+4.1985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1323
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C1-C2
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C4) = Uanis(C5)
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5) H1E(0.5) C2(0.5) H2A(0.5)
 H2B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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 0.000000 0.500000 0.0351(3) Uani 1 4 d S T P . .
Cl1 Cl 0.25286(12) 0.24725(13) 0.500000 0.0563(3) Uani 1 2 d S T P . .
Cl2 Cl 0.000000 0.000000 0.56182(3) 0.0686(4) Uani 1 2 d S T P . .
N1 N 0.000000 0.500000 0.55769(9) 0.0639(10) Uani 1 2 d S T P C .
H1A H -0.109631 0.535366 0.550254 0.077 Uiso 0.5 1 calc R U P A -1
H1B H 0.024096 0.387656 0.550254 0.077 Uiso 0.5 1 calc R U P A -1
H1C H 0.085534 0.576978 0.550254 0.077 Uiso 0.5 1 calc R U P A -1
C1 C 0.000000 0.500000 0.59273(17) 0.131(3) Uani 1 2 d DS TU P . .
H1D H 0.129487 0.484645 0.597691 0.157 Uiso 0.5 1 calc R U P B -1
H1E H -0.025229 0.627556 0.597691 0.157 Uiso 0.5 1 calc R U P B -1
C6 C 0.000000 0.500000 0.7189(2) 0.194(7) Uani 1 2 d S T P . .
H6 H 0.000000 0.500003 0.742228 0.232 Uiso 1 2 calc R U P . .
C3 C 0.000000 0.500000 0.65256(18) 0.158(5) Uani 1 2 d S T P . .
C5 C -0.1157(15) 0.6039(15) 0.7041(2) 0.199(3) Uani 1 1 d . . . . .
H5 H -0.196543 0.677041 0.716197 0.239 Uiso 1 1 calc R U . . .
C4 C -0.1165(15) 0.6036(15) 0.66978(19) 0.199(3) Uani 1 1 d . . . . .
H4 H -0.199890 0.677090 0.658353 0.239 Uiso 1 1 calc R U . . .
C2 C -0.072(2) 0.4220(19) 0.6167(2) 0.130(5) Uani 0.5 1 d D U P C -1
H2A H -0.046548 0.291972 0.615418 0.156 Uiso 0.5 1 calc R U P C -1
H2B H -0.204491 0.437865 0.615418 0.156 Uiso 0.5 1 calc R U P C -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
Mn1 Cl1 2.5781(9) 15 ?
Mn1 Cl1 2.5792(9) . ?
Mn1 Cl1 2.5792(9) 9_556 ?
Mn1 Cl1 2.5781(9) 7_455 ?
Mn1 Cl2 2.4673(12) . ?
Mn1 Cl2 2.4674(12) 9_556 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.399(8) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.233(9) . ?
C6 H6 0.9300 . ?
C6 C5 1.279(9) . ?
C6 C5 1.279(9) 2_565 ?
C3 C4 1.328(9) 2_565 ?
C3 C4 1.328(9) . ?
C3 C2 1.627(11) . ?
C5 H5 0.9300 . ?
C5 C4 1.370(10) . ?
C4 H4 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 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
Cl1 Mn1 Cl1 180.0 15 7_455 ?
Cl1 Mn1 Cl1 89.830(15) 7_455 . ?
Cl1 Mn1 Cl1 90.170(15) 15 . ?
Cl1 Mn1 Cl1 180.0 . 9_556 ?
Cl1 Mn1 Cl1 90.171(15) 7_455 9_556 ?
Cl1 Mn1 Cl1 89.829(15) 15 9_556 ?
Cl2 Mn1 Cl1 90.0 . 9_556 ?
Cl2 Mn1 Cl1 90.0 . 15 ?
Cl2 Mn1 Cl1 90.0 9_556 . ?
Cl2 Mn1 Cl1 90.0 9_556 9_556 ?
Cl2 Mn1 Cl1 90.0 9_556 15 ?
Cl2 Mn1 Cl1 90.0 9_556 7_455 ?
Cl2 Mn1 Cl1 90.0 . . ?
Cl2 Mn1 Cl1 90.0 . 7_455 ?
Cl2 Mn1 Cl2 180.0 . 9_556 ?
Mn1 Cl1 Mn1 178.71(4) 7 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 101.8 . . ?
N1 C1 H1E 101.8 . . ?
H1D C1 H1E 104.7 . . ?
C2 C1 N1 141.0(5) . . ?
C2 C1 H1D 101.8 . . ?
C2 C1 H1E 101.8 . . ?
C5 C6 H6 117.6 . . ?
C5 C6 H6 117.6 2_565 . ?
C5 C6 C5 124.9(11) 2_565 . ?
C4 C3 C4 117.7(9) 2_565 . ?
C4 C3 C2 116.6(8) . . ?
C4 C3 C2 117.5(8) 2_565 . ?
C6 C5 H5 121.2 . . ?
C6 C5 C4 117.7(9) . . ?
C4 C5 H5 121.2 . . ?
C3 C4 C5 121.0(8) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C1 C2 C3 112.5(8) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?

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 C1 C2 C3 180.000(1) . . . . ?
C6 C5 C4 C3 -0.5(15) . . . . ?
C5 C6 C5 C4 0.2(7) 2_565 . . . ?
C4 C3 C4 C5 0.3(8) 2_565 . . . ?
C4 C3 C2 C1 107.0(13) . . . . ?
C4 C3 C2 C1 -105.2(13) 2_565 . . . ?
C2 C3 C4 C5 148.0(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PEA-Cu_393K
_database_code_depnum_ccdc_archive 'CCDC 2411276'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Cu, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cl4 Cu N2'
_chemical_formula_weight         449.71
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'B b c m'
_space_group_name_Hall           '-B 2 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y-1/2, z-1/2'
'x, -y-1/2, z-1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y-1/2, z'
'x+1/2, -y-1/2, z'

_cell_length_a                   7.3448(2)
_cell_length_b                   7.3896(2)
_cell_length_c                   39.0232(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2117.99(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6667
_cell_measurement_temperature    393(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.76
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.82104
_exptl_absorpt_correction_T_min  0.71407
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            10175
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         3.132
_diffrn_ambient_temperature      393(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1124
_reflns_number_total             1247
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1247
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.210
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0672P)²+1.8157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1149
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C1-C2
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C6)
Uanis(C4) = Uanis(C5)
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1E(0.5) H1D(0.5) C2(0.5) H2A(0.5)
 H2B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1E,H1D), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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 0.0424(2) Uani 1 4 d S T P . .
Cl2 Cl 0.000000 0.000000 0.55851(3) 0.0720(3) Uani 1 2 d S T P . .
Cl1 Cl 0.22025(10) 0.21853(11) 0.500000 0.0603(3) Uani 1 2 d S T P . .
N1 N 0.000000 0.500000 0.55433(9) 0.0674(9) Uani 1 2 d S T P C .
H1A H -0.103706 0.547635 0.546727 0.081 Uiso 0.5 1 calc R U P A -1
H1B H 0.010348 0.386915 0.546727 0.081 Uiso 0.5 1 calc R U P A -1
H1C H 0.093358 0.565450 0.546728 0.081 Uiso 0.5 1 calc R U P A -1
C1 C 0.000000 0.500000 0.59050(16) 0.135(3) Uani 1 2 d DS T P . .
H1E H -0.128429 0.515084 0.595537 0.162 Uiso 0.5 1 calc R U P B -1
H1D H 0.024973 0.373881 0.595537 0.162 Uiso 0.5 1 calc R U P B -1
C6 C 0.000000 0.500000 0.7193(2) 0.194(6) Uani 1 2 d S T P . .
H6 H 0.000004 0.499997 0.743104 0.232 Uiso 1 2 calc R U P . .
C5 C -0.1136(14) 0.6029(13) 0.70460(16) 0.207(3) Uani 1 1 d . . . . .
H5 H -0.192971 0.676058 0.716959 0.249 Uiso 1 1 calc R U . . .
C3 C 0.000000 0.500000 0.6513(2) 0.194(6) Uani 1 2 d S T P . .
C4 C -0.1131(14) 0.6005(14) 0.66920(16) 0.207(3) Uani 1 1 d . . . . .
H4 H -0.196148 0.672918 0.657554 0.249 Uiso 1 1 calc R U . . .
C2 C 0.0702(19) 0.5753(19) 0.6147(2) 0.149(5) Uani 0.5 1 d D . P C -1
H2A H 0.044568 0.703869 0.613319 0.179 Uiso 0.5 1 calc R U P C -1
H2B H 0.201094 0.559791 0.613319 0.179 Uiso 0.5 1 calc R U P C -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
Cu1 Cl2 2.2831(11) 9_556 ?
Cu1 Cl2 2.2831(11) . ?
Cu1 Cl1 2.9237(8) 8_545 ?
Cu1 Cl1 2.2857(8) 9_556 ?
Cu1 Cl1 2.2857(8) . ?
Cu1 Cl1 2.9237(8) 7_455 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.411(8) . ?
C1 H1E 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.211(8) . ?
C6 H6 0.9300 . ?
C6 C5 1.266(8) . ?
C6 C5 1.266(8) 2_565 ?
C5 H5 0.9300 . ?
C5 C4 1.381(9) . ?
C3 C4 1.315(8) 2_565 ?
C3 C4 1.315(8) . ?
C3 C2 1.617(11) . ?
C4 H4 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 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
Cl2 Cu1 Cl2 180.0 9_556 . ?
Cl2 Cu1 Cl1 90.0 . . ?
Cl2 Cu1 Cl1 90.0 9_556 . ?
Cl2 Cu1 Cl1 90.0 . 7_455 ?
Cl2 Cu1 Cl1 90.0 9_556 8_545 ?
Cl2 Cu1 Cl1 90.0 9_556 9_556 ?
Cl2 Cu1 Cl1 90.0 . 8_545 ?
Cl2 Cu1 Cl1 90.0 . 9_556 ?
Cl2 Cu1 Cl1 90.0 9_556 7_455 ?
Cl1 Cu1 Cl1 90.299(5) 9_556 7_455 ?
Cl1 Cu1 Cl1 89.701(5) . 7_455 ?
Cl1 Cu1 Cl1 180.0 7_455 8_545 ?
Cl1 Cu1 Cl1 180.0 . 9_556 ?
Cl1 Cu1 Cl1 89.701(5) 9_556 8_545 ?
Cl1 Cu1 Cl1 90.299(5) . 8_545 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1E 101.7 . . ?
N1 C1 H1D 101.7 . . ?
H1E C1 H1D 104.7 . . ?
C2 C1 N1 141.2(5) . . ?
C2 C1 H1E 101.7 . . ?
C2 C1 H1D 101.7 . . ?
C5 C6 H6 116.9 2_565 . ?
C5 C6 H6 116.9 . . ?
C5 C6 C5 126.2(9) . 2_565 ?
C6 C5 H5 121.9 . . ?
C6 C5 C4 116.3(7) . . ?
C4 C5 H5 121.9 . . ?
C4 C3 C4 115.8(9) 2_565 . ?
C4 C3 C2 117.5(8) 2_565 . ?
C4 C3 C2 118.4(8) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 C5 122.7(7) . . ?
C3 C4 H4 118.7 . . ?
C1 C2 C3 113.3(8) . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?

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
N1 C1 C2 C3 180.000(1) . . . . ?
C6 C5 C4 C3 -1.1(14) . . . . ?
C5 C6 C5 C4 0.5(7) 2_565 . . . ?
C4 C3 C4 C5 0.5(7) 2_565 . . . ?
C4 C3 C2 C1 -105.6(13) . . . . ?
C4 C3 C2 C1 107.2(13) 2_565 . . . ?
C2 C3 C4 C5 -147.2(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: distilled water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PEA-Fe_453K
_database_code_depnum_ccdc_archive 'CCDC 2411280'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_vrf_PLAT043_PEA-Fe_453K         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      24.19 Check 
RESPONSE: We were not able to include hydrogen atoms due to
disorder generated by the mirror and C4 axis. Manual addition was also failed.
;
_audit_creation_date             2024-04-19
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Fe, 4(C4 N0.5)'
_chemical_formula_sum            'C16 H24 Cl4 Fe N2'
_chemical_formula_weight         442.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H24N2FeCl4
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.17610(10)
_cell_length_b                   5.17610(10)
_cell_length_c                   39.7194(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1064.16(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6646
_cell_measurement_temperature    453(2)
_cell_measurement_theta_max      30.0870
_cell_measurement_theta_min      3.0670
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.839
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'slightly brown'
_exptl_crystal_colour_modifier   slightly
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0067
0 0 -1 0.0489
-1 0 1 0.0706
1 0 -1 0.0669
0 -1 0 0.0767
0 1 0 0.0489

_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0001 0.0000 1.0001 -0.0110 0.0004 0.0141
-0.0001 -0.0000 -1.0001 0.0110 -0.0004 -0.0141
-1.0000 -0.0002 1.0007 -0.0200 -0.1363 0.0111
1.0000 0.0002 -1.0007 0.0200 0.1363 -0.0111
-0.0002 -0.9999 0.0001 0.1076 -0.0089 0.0843
0.0002 0.9999 -0.0001 -0.1076 0.0089 -0.0843

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0048
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            10205
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.077
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      453(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -90.00   9.00   0.50    4.00    --  -22.93 -52.00 -74.00  198
  2  ω    -41.00  58.00   0.50    4.00    --  -22.93  52.00  70.00  198
  3  ω     30.00  71.00   0.50    4.00    --   24.50  52.00  70.00   82
  4  ω    -42.00  42.00   0.50    4.00    --   24.50 -52.00 -74.00  168
  5  ω    -89.00 -50.00   0.50    4.00    --  -22.93-178.00  30.00   78
  6  ω    -17.00  31.00   0.50    4.00    --  -22.93 -99.00-150.00   96
  7  ω   -110.00 -54.00   0.50    4.00    --  -22.93-178.00  60.00  112
  8  ω   -118.00 -92.00   0.50    4.00    --  -22.93-178.00  30.00   52
  9  ω     -2.00  57.00   0.50    4.00    --  -22.93  19.00  30.00  118
 10  ω    -17.00  32.00   0.50    4.00    --  -22.93 -99.00 150.00   98
 11  ω    -21.00   8.00   0.50    4.00    --   24.50  77.00-120.00   58
 12  ω     -6.00  76.00   0.50    4.00    --   24.50 -99.00 -60.00  164
 13  ω    -15.00 103.00   0.50    4.00    --   24.50  57.00 120.00  236
 14  ω    -15.00 105.00   0.50    4.00    --   24.50  19.00  60.00  240
 15  ω     78.00 106.00   0.50    4.00    --   24.50  77.00-120.00   56
 16  ω     12.00  61.00   0.50    4.00    --   24.50  77.00-120.00   98
 17  ω     74.00 106.00   0.50    4.00    --   24.50  52.00  70.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089858000
_diffrn_orient_matrix_UB_12      -0.1076375000
_diffrn_orient_matrix_UB_13      -0.0109856000
_diffrn_orient_matrix_UB_21      0.1367116000
_diffrn_orient_matrix_UB_22      0.0088868000
_diffrn_orient_matrix_UB_23      0.0004101000
_diffrn_orient_matrix_UB_31      0.0029964000
_diffrn_orient_matrix_UB_32      -0.0843159000
_diffrn_orient_matrix_UB_33      0.0140743000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                420
_reflns_number_total             433
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         433
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.211
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0689P)²+0.0089P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C4-C6
 2.36 with sigma of 0.04
2. Others
 Fixed Sof: C2(0.125) C4(0.25) C5(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe01 Fe 0.500000 0.500000 0.500000 0.0508(3) Uani 1 16 d S T P . .
Cl1 Cl 0.000000 0.500000 0.500000 0.0687(3) Uani 1 8 d S T P . .
Cl2 Cl 0.500000 0.500000 0.44023(2) 0.0802(3) Uani 1 8 d S T P . .
N1 N 0.000000 0.000000 0.44514(9) 0.0806(10) Uani 1 8 d S T P . .
C1 C 0.000000 0.000000 0.40891(16) 0.148(4) Uani 1 8 d S T P . .
C3 C 0.000000 0.000000 0.3499(2) 0.214(8) Uani 1 8 d S T P . .
C2 C 0.000000 -0.149(3) 0.3867(3) 0.123(5) Uani 0.25 2 d S T P . .
C6 C 0.000000 0.000000 0.2832(5) 0.40(3) Uani 1 8 d DS T P . .
C4 C -0.157(3) 0.157(3) 0.3323(3) 0.336(19) Uani 0.5 2 d DS T P . .
C5 C -0.149(6) 0.149(6) 0.2990(3) 0.43(3) Uani 0.5 2 d S T P . .


_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
Fe01 Cl1 2.58805(5) 3_665 ?
Fe01 Cl1 2.58805(5) . ?
Fe01 Cl1 2.58805(5) 3_655 ?
Fe01 Cl1 2.58805(5) 1_655 ?
Fe01 Cl2 2.3738(9) . ?
Fe01 Cl2 2.3738(9) 17_666 ?
N1 C1 1.439(8) . ?
C1 C2 1.173(13) 3 ?
C1 C2 1.173(13) . ?
C1 C2 1.173(13) 4 ?
C1 C2 1.173(13) 2 ?
C3 C2 1.651(14) 2 ?
C3 C2 1.651(14) 3 ?
C3 C2 1.651(14) 4 ?
C3 C2 1.651(14) . ?
C3 C4 1.34(2) 2 ?
C3 C4 1.34(2) 4 ?
C3 C4 1.34(2) 3 ?
C3 C4 1.34(2) . ?
C2 C2 1.54(3) 2 ?
C2 C2 1.09(2) 3 ?
C2 C2 1.09(2) 4 ?
C6 C5 1.26(3) 3 ?
C6 C5 1.26(3) 4 ?
C6 C5 1.26(3) . ?
C6 C5 1.26(3) 2 ?
C4 C4 1.62(4) 4 ?
C4 C4 1.62(4) 3 ?
C4 C5 1.324(13) . ?
C5 C5 1.54(6) 3 ?
C5 C5 1.54(6) 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
Cl1 Fe01 Cl1 180.0 . 1_655 ?
Cl1 Fe01 Cl1 90.0 . 3_655 ?
Cl1 Fe01 Cl1 90.0 1_655 3_665 ?
Cl1 Fe01 Cl1 90.0 . 3_665 ?
Cl1 Fe01 Cl1 90.0 1_655 3_655 ?
Cl1 Fe01 Cl1 180.0 3_655 3_665 ?
Cl2 Fe01 Cl1 90.0 . 3_655 ?
Cl2 Fe01 Cl1 90.0 17_666 . ?
Cl2 Fe01 Cl1 90.0 17_666 1_655 ?
Cl2 Fe01 Cl1 90.0 . 3_665 ?
Cl2 Fe01 Cl1 90.0 . 1_655 ?
Cl2 Fe01 Cl1 90.0 17_666 3_655 ?
Cl2 Fe01 Cl1 90.0 . . ?
Cl2 Fe01 Cl1 90.0 17_666 3_665 ?
Cl2 Fe01 Cl2 180.0 17_666 . ?
Fe01 Cl1 Fe01 180.0 1_455 . ?
C2 C1 N1 138.9(7) 2 . ?
C2 C1 N1 138.9(7) . . ?
C2 C1 N1 138.9(7) 4 . ?
C2 C1 N1 138.9(7) 3 . ?
C2 C1 C2 55.5(8) 3 . ?
C2 C1 C2 55.5(8) 3 2 ?
C2 C1 C2 82.3(13) 4 3 ?
C2 C1 C2 55.5(8) 4 . ?
C2 C1 C2 55.5(8) 4 2 ?
C2 C1 C2 82.3(13) 2 . ?
C2 C3 C2 38.6(7) . 3 ?
C2 C3 C2 38.6(7) . 4 ?
C2 C3 C2 38.6(7) 2 3 ?
C2 C3 C2 55.7(10) 3 4 ?
C2 C3 C2 38.6(7) 2 4 ?
C2 C3 C2 55.7(10) . 2 ?
C4 C3 C2 138.0(8) 2 4 ?
C4 C3 C2 100.3(9) 4 3 ?
C4 C3 C2 100.3(9) 4 2 ?
C4 C3 C2 100.3(9) . 2 ?
C4 C3 C2 138.0(8) 4 . ?
C4 C3 C2 138.0(8) 3 2 ?
C4 C3 C2 100.3(9) 2 . ?
C4 C3 C2 137.9(8) . . ?
C4 C3 C2 100.3(9) . 4 ?
C4 C3 C2 137.9(8) . 3 ?
C4 C3 C2 138.0(8) 4 4 ?
C4 C3 C2 100.3(9) 3 4 ?
C4 C3 C2 138.0(8) 2 2 ?
C4 C3 C2 100.3(9) 3 . ?
C4 C3 C2 100.3(9) 2 3 ?
C4 C3 C2 138.0(8) 3 3 ?
C4 C3 C4 74.3(8) . 4 ?
C4 C3 C4 117.2(16) . 2 ?
C4 C3 C4 117.2(17) 3 4 ?
C4 C3 C4 74.3(8) 4 2 ?
C4 C3 C4 74.3(8) 3 2 ?
C4 C3 C4 74.3(8) . 3 ?
C1 C2 C3 111.0(10) . . ?
C1 C2 C2 48.9(7) . 2 ?
C2 C2 C1 62.3(4) 4 . ?
C2 C2 C1 62.3(4) 3 . ?
C2 C2 C3 70.7(3) 4 . ?
C2 C2 C3 62.1(5) 2 . ?
C2 C2 C3 70.7(3) 3 . ?
C2 C2 C2 90.001(11) 3 4 ?
C2 C2 C2 45.001(6) 4 2 ?
C2 C2 C2 45.001(6) 3 2 ?
C5 C6 C5 120(3) 4 3 ?
C5 C6 C5 75.7(12) 4 2 ?
C5 C6 C5 75.7(12) 3 2 ?
C5 C6 C5 120(3) 2 . ?
C5 C6 C5 75.7(12) 4 . ?
C5 C6 C5 75.7(12) 3 . ?
C3 C4 C4 52.9(4) . 4 ?
C3 C4 C4 52.9(4) . 3 ?
C4 C4 C4 89.999(11) 4 3 ?
C5 C4 C3 119(2) . . ?
C5 C4 C4 88.3(14) . 3 ?
C5 C4 C4 88.3(14) . 4 ?
C6 C5 C4 122(3) . . ?
C6 C5 C5 52.2(6) . 3 ?
C6 C5 C5 52.2(6) . 4 ?
C4 C5 C5 91.7(15) . 4 ?
C4 C5 C5 91.7(15) . 3 ?
C5 C5 C5 90.000(14) 4 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 C1 C2 C3 180.000(5) . . . . ?
N1 C1 C2 C2 127.0(3) . . . 4 ?
N1 C1 C2 C2 180.000(7) . . . 2 ?
N1 C1 C2 C2 -127.0(3) . . . 3 ?
C3 C4 C5 C6 0.000(4) . . . . ?
C3 C4 C5 C5 -45.03(3) . . . 4 ?
C3 C4 C5 C5 45.03(3) . . . 3 ?
C2 C1 C2 C3 53.0(3) 4 . . . ?
C2 C1 C2 C3 0.000(2) 2 . . . ?
C2 C1 C2 C3 -53.0(3) 3 . . . ?
C2 C1 C2 C2 -53.0(3) 2 . . 4 ?
C2 C1 C2 C2 106.0(6) 4 . . 3 ?
C2 C1 C2 C2 53.0(3) 4 . . 2 ?
C2 C1 C2 C2 -106.0(6) 3 . . 4 ?
C2 C1 C2 C2 -53.0(3) 3 . . 2 ?
C2 C1 C2 C2 53.0(3) 2 . . 3 ?
C2 C3 C2 C1 0.000(2) 2 . . . ?
C2 C3 C2 C1 48.52(13) 3 . . . ?
C2 C3 C2 C1 -48.52(13) 4 . . . ?
C2 C3 C2 C2 -97.0(3) 4 . . 3 ?
C2 C3 C2 C2 97.0(3) 3 . . 4 ?
C2 C3 C2 C2 -48.52(13) 2 . . 3 ?
C2 C3 C2 C2 48.52(14) 2 . . 4 ?
C2 C3 C2 C2 -48.52(12) 4 . . 2 ?
C2 C3 C2 C2 48.52(13) 3 . . 2 ?
C2 C3 C4 C4 88.0(7) 3 . . 4 ?
C2 C3 C4 C4 -97.9(6) 4 . . 3 ?
C2 C3 C4 C4 -137.1(7) 2 . . 3 ?
C2 C3 C4 C4 -88.0(7) . . . 3 ?
C2 C3 C4 C4 137.1(7) 4 . . 4 ?
C2 C3 C4 C4 97.9(6) 2 . . 4 ?
C2 C3 C4 C4 147.1(12) . . . 4 ?
C2 C3 C4 C4 -147.1(12) 3 . . 3 ?
C2 C3 C4 C5 150.4(8) 3 . . . ?
C2 C3 C4 C5 -150.4(8) . . . . ?
C2 C3 C4 C5 160.4(3) 2 . . . ?
C2 C3 C4 C5 -160.4(3) 4 . . . ?
C4 C3 C2 C1 -64.3(8) . . . . ?
C4 C3 C2 C1 -142.2(3) 3 . . . ?
C4 C3 C2 C1 64.3(8) 4 . . . ?
C4 C3 C2 C1 142.2(3) 2 . . . ?
C4 C3 C2 C2 15.8(7) 4 . . 3 ?
C4 C3 C2 C2 169.3(3) 3 . . 3 ?
C4 C3 C2 C2 -15.8(7) . . . 4 ?
C4 C3 C2 C2 -112.8(9) . . . 3 ?
C4 C3 C2 C2 64.3(8) 4 . . 2 ?
C4 C3 C2 C2 -64.3(8) . . . 2 ?
C4 C3 C2 C2 93.6(3) 2 . . 3 ?
C4 C3 C2 C2 -93.6(3) 3 . . 4 ?
C4 C3 C2 C2 -169.3(3) 2 . . 4 ?
C4 C3 C2 C2 112.8(9) 4 . . 4 ?
C4 C3 C2 C2 -142.2(3) 3 . . 2 ?
C4 C3 C2 C2 142.2(3) 2 . . 2 ?
C4 C3 C4 C4 62.5(6) 2 . . 3 ?
C4 C3 C4 C4 -62.5(6) 2 . . 4 ?
C4 C3 C4 C4 125.0(11) 4 . . 3 ?
C4 C3 C4 C4 -125.0(11) 3 . . 4 ?
C4 C3 C4 C5 -62.5(6) 3 . . . ?
C4 C3 C4 C5 62.5(6) 4 . . . ?
C4 C3 C4 C5 0.000(3) 2 . . . ?
C4 C4 C5 C6 -45.03(4) 3 . . . ?
C4 C4 C5 C6 45.03(5) 4 . . . ?
C4 C4 C5 C5 90.05(7) 4 . . 3 ?
C4 C4 C5 C5 0.000(17) 4 . . 4 ?
C4 C4 C5 C5 0.001(14) 3 . . 3 ?
C4 C4 C5 C5 -90.05(8) 3 . . 4 ?
C5 C6 C5 C4 -63.5(10) 4 . . . ?
C5 C6 C5 C4 63.5(10) 3 . . . ?
C5 C6 C5 C4 0.000(6) 2 . . . ?
C5 C6 C5 C5 -127.1(19) 4 . . 3 ?
C5 C6 C5 C5 127.1(19) 3 . . 4 ?
C5 C6 C5 C5 -63.5(10) 2 . . 3 ?
C5 C6 C5 C5 63.5(10) 2 . . 4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.731
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_PEA-Fe_373K
_database_code_depnum_ccdc_archive 'CCDC 2411279'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_audit_creation_date             2024-03-04
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Fe, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cl4 Fe N2'
_chemical_formula_weight         442.02
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'B b c m'
_space_group_name_Hall           '-B 2 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y-1/2, z-1/2'
'x, -y-1/2, z-1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y-1/2, z'
'x+1/2, -y-1/2, z'

_cell_length_a                   7.2427(2)
_cell_length_b                   7.2798(2)
_cell_length_c                   39.4455(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2079.78(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4286
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.80
_shelx_estimated_absorpt_T_max   0.897
_shelx_estimated_absorpt_T_min   0.678
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.93716
_exptl_absorpt_correction_T_min  0.74064
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'slightly brown'
_exptl_crystal_colour_modifier   slightly
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            9468
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.099
_diffrn_ambient_temperature      373(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                885
_reflns_number_total             1214
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1214
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.174
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0456P)²+5.8508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1189
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C1-C2
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C5)
4. Rigid body (RIGU) restrains
 C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5) H1E(0.5) C2(0.5) H2A(0.5)
 H2B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C5(H5)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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 0.000000 0.000000 0.500000 0.0309(2) Uani 1 4 d S T P . .
Cl1 Cl 0.25205(14) 0.24827(16) 0.500000 0.0460(3) Uani 1 2 d S T P . .
Cl2 Cl 0.000000 0.000000 0.43962(3) 0.0557(3) Uani 1 2 d S T P . .
N1 N 0.000000 0.500000 0.55610(9) 0.0519(9) Uani 1 2 d S T P D .
H1A H -0.111817 0.530165 0.548583 0.062 Uiso 0.5 1 calc R U P A -1
H1B H 0.029651 0.388575 0.548583 0.062 Uiso 0.5 1 calc R U P A -1
H1C H 0.082166 0.581260 0.548583 0.062 Uiso 0.5 1 calc R U P A -1
C1 C 0.000000 0.500000 0.59168(16) 0.119(3) Uani 1 2 d DS T P . .
H1D H -0.130236 0.514868 0.596715 0.143 Uiso 0.5 1 calc R U P B -1
H1E H 0.025979 0.372164 0.596715 0.143 Uiso 0.5 1 calc R U P B -1
C4 C -0.1180(12) 0.6047(12) 0.66981(17) 0.152(2) Uani 1 1 d . . . . .
H4 H -0.201363 0.678934 0.658256 0.182 Uiso 1 1 calc R U . C -1
C3 C 0.000000 0.500000 0.65231(17) 0.144(4) Uani 1 2 d S T P . .
C6 C 0.000000 0.500000 0.7197(2) 0.153(5) Uani 1 2 d S T P . .
H6 H -0.000001 0.500001 0.743231 0.184 Uiso 1 2 calc R U P . .
C5 C -0.1176(12) 0.6039(12) 0.70423(17) 0.152(2) Uani 1 1 d . . . . .
H5 H -0.199930 0.676468 0.716398 0.182 Uiso 1 1 calc R U . . .
C2 C 0.0727(19) 0.5788(17) 0.6159(2) 0.114(4) Uani 0.5 1 d D . P D -1
H2A H 0.046055 0.709144 0.614556 0.137 Uiso 0.5 1 calc R U P D -1
H2B H 0.205531 0.563461 0.614556 0.137 Uiso 0.5 1 calc R U P D -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
Fe1 Cl1 2.5658(10) 15 ?
Fe1 Cl1 2.5689(11) 9_556 ?
Fe1 Cl1 2.5689(11) . ?
Fe1 Cl1 2.5658(10) 7_455 ?
Fe1 Cl2 2.3815(10) 9_556 ?
Fe1 Cl2 2.3815(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.403(7) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.233(9) . ?
C4 H4 0.9300 . ?
C4 C3 1.337(7) . ?
C4 C5 1.358(8) . ?
C3 C2 1.633(11) . ?
C6 H6 0.9300 . ?
C6 C5 1.291(8) . ?
C6 C5 1.291(8) 2_565 ?
C5 H5 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 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
Cl1 Fe1 Cl1 180.0 15 7_455 ?
Cl1 Fe1 Cl1 90.293(2) 7_455 9_556 ?
Cl1 Fe1 Cl1 89.707(2) 15 9_556 ?
Cl1 Fe1 Cl1 180.0 9_556 . ?
Cl1 Fe1 Cl1 89.707(2) 7_455 . ?
Cl1 Fe1 Cl1 90.293(2) 15 . ?
Cl2 Fe1 Cl1 90.000(1) 9_556 . ?
Cl2 Fe1 Cl1 90.0 9_556 15 ?
Cl2 Fe1 Cl1 90.0 . 9_556 ?
Cl2 Fe1 Cl1 90.0 . . ?
Cl2 Fe1 Cl1 90.0 . 15 ?
Cl2 Fe1 Cl1 90.0 . 7_455 ?
Cl2 Fe1 Cl1 90.000(1) 9_556 9_556 ?
Cl2 Fe1 Cl1 90.0 9_556 7_455 ?
Cl2 Fe1 Cl2 180.0 9_556 . ?
Fe1 Cl1 Fe1 179.13(5) 7 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 101.8 . . ?
N1 C1 H1E 101.8 . . ?
H1D C1 H1E 104.7 . . ?
C2 C1 N1 140.8(5) . . ?
C2 C1 H1D 101.8 . . ?
C2 C1 H1E 101.8 . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.9(7) . . ?
C5 C4 H4 119.6 . . ?
C4 C3 C4 117.8(8) 2_565 . ?
C4 C3 C2 117.4(7) . . ?
C4 C3 C2 116.6(7) 2_565 . ?
C5 C6 H6 118.1 2_565 . ?
C5 C6 H6 118.1 . . ?
C5 C6 C5 123.8(9) 2_565 . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.3(7) . . ?
C6 C5 H5 120.8 . . ?
C1 C2 C3 112.4(8) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?

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
N1 C1 C2 C3 180.000(1) . . . . ?
C4 C3 C2 C1 -105.4(11) . . . . ?
C4 C3 C2 C1 106.7(11) 2_565 . . . ?
C3 C4 C5 C6 0.2(13) . . . . ?
C5 C4 C3 C4 -0.1(6) . . . 2_565 ?
C5 C4 C3 C2 -147.6(8) . . . . ?
C5 C6 C5 C4 -0.1(6) 2_565 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_PEA-Fe_293K
_database_code_depnum_ccdc_archive 'CCDC 2411278'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Fe, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cl4 Fe N2'
_chemical_formula_weight         442.02
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'-x-1/2, -y, z-1/2'

_cell_length_a                   7.1717(3)
_cell_length_b                   7.2827(3)
_cell_length_c                   39.0900(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2041.64(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6672
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.80
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.632
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.94919
_exptl_absorpt_correction_T_min  0.70783
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'slightly brown'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   slightly
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            18415
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         3.026
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2094
_reflns_number_total             2338
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.465
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0876
_refine_ls_restrained_S_all      1.465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+16.4649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.1935
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C8(H8), C4(H4), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe01 Fe 0.000000 0.000000 0.500000 0.0229(3) Uani 1 2 d S . P . .
Cl1 Cl 0.2580(2) 0.2418(2) 0.50430(4) 0.0305(4) Uani 1 1 d . . . . .
Cl2 Cl 0.0281(2) -0.0060(3) 0.43907(4) 0.0358(4) Uani 1 1 d . . . . .
N1 N 0.5063(8) -0.0104(9) 0.55681(13) 0.0364(13) Uani 1 1 d . . . . .
H1A H 0.444005 0.063541 0.542729 0.044 Uiso 1 1 calc R U . . .
H1B H 0.471521 -0.126064 0.553171 0.044 Uiso 1 1 calc R U . . .
H1C H 0.628075 0.000650 0.552956 0.044 Uiso 1 1 calc R U . . .
C1 C 0.4651(12) 0.0407(11) 0.59267(18) 0.0445(19) Uani 1 1 d . . . . .
H1D H 0.518471 0.160404 0.597436 0.053 Uiso 1 1 calc R U . . .
H1E H 0.331130 0.049668 0.595670 0.053 Uiso 1 1 calc R U . . .
C3 C 0.5172(14) -0.0354(10) 0.65417(19) 0.048(2) Uani 1 1 d . . . . .
C6 C 0.4879(17) 0.0702(17) 0.7217(2) 0.073(3) Uani 1 1 d . . . . .
H6 H 0.479629 0.104203 0.744540 0.087 Uiso 1 1 calc R U . . .
C5 C 0.3643(17) -0.0525(15) 0.7087(3) 0.071(3) Uani 1 1 d . . . . .
H5 H 0.271623 -0.102222 0.722492 0.086 Uiso 1 1 calc R U . . .
C2 C 0.5404(17) -0.0941(13) 0.6172(2) 0.063(3) Uani 1 1 d . . . . .
H2A H 0.671925 -0.112404 0.612504 0.076 Uiso 1 1 calc R U . . .
H2B H 0.477673 -0.210718 0.613825 0.076 Uiso 1 1 calc R U . . .
C8 C 0.6344(17) 0.0917(16) 0.6687(2) 0.076(3) Uani 1 1 d . . . . .
H8 H 0.726769 0.145301 0.655325 0.091 Uiso 1 1 calc R U . . .
C4 C 0.3778(16) -0.1030(15) 0.6745(2) 0.067(3) Uani 1 1 d . . . . .
H4 H 0.290928 -0.183824 0.665256 0.080 Uiso 1 1 calc R U . . .
C7 C 0.6190(19) 0.1417(17) 0.7023(3) 0.081(4) Uani 1 1 d . . . . .
H7 H 0.701831 0.226570 0.711558 0.097 Uiso 1 1 calc R 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
Fe01 Cl1 2.5645(15) 6_566 ?
Fe01 Cl1 2.5597(15) . ?
Fe01 Cl1 2.5645(15) 2_545 ?
Fe01 Cl1 2.5597(15) 5_556 ?
Fe01 Cl2 2.3905(15) 5_556 ?
Fe01 Cl2 2.3905(15) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.480(8) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.475(11) . ?
C3 C2 1.517(11) . ?
C3 C8 1.373(13) . ?
C3 C4 1.368(13) . ?
C6 H6 0.9300 . ?
C6 C5 1.357(15) . ?
C6 C7 1.314(16) . ?
C5 H5 0.9300 . ?
C5 C4 1.390(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C8 H8 0.9300 . ?
C8 C7 1.368(13) . ?
C4 H4 0.9300 . ?
C7 H7 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
Cl1 Fe01 Cl1 180.0 . 5_556 ?
Cl1 Fe01 Cl1 89.374(6) 5_556 2_545 ?
Cl1 Fe01 Cl1 90.627(6) . 2_545 ?
Cl1 Fe01 Cl1 180.00(7) 2_545 6_566 ?
Cl1 Fe01 Cl1 89.373(6) . 6_566 ?
Cl1 Fe01 Cl1 90.626(6) 5_556 6_566 ?
Cl2 Fe01 Cl1 90.98(6) 5_556 5_556 ?
Cl2 Fe01 Cl1 90.30(5) . 6_566 ?
Cl2 Fe01 Cl1 89.70(5) . 2_545 ?
Cl2 Fe01 Cl1 89.70(5) 5_556 6_566 ?
Cl2 Fe01 Cl1 89.03(6) 5_556 . ?
Cl2 Fe01 Cl1 89.02(6) . 5_556 ?
Cl2 Fe01 Cl1 90.30(5) 5_556 2_545 ?
Cl2 Fe01 Cl1 90.97(6) . . ?
Cl2 Fe01 Cl2 180.00(9) 5_556 . ?
Fe01 Cl1 Fe01 171.62(7) . 2 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 N1 112.0(7) . . ?
C2 C1 H1D 109.2 . . ?
C2 C1 H1E 109.2 . . ?
C8 C3 C2 121.2(9) . . ?
C4 C3 C2 122.1(9) . . ?
C4 C3 C8 116.7(8) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C7 C6 C5 120.9(9) . . ?
C6 C5 H5 120.4 . . ?
C6 C5 C4 119.2(10) . . ?
C4 C5 H5 120.4 . . ?
C1 C2 C3 113.1(7) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C3 C8 H8 119.1 . . ?
C7 C8 C3 121.8(10) . . ?
C7 C8 H8 119.1 . . ?
C3 C4 C5 120.9(10) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C7 C8 120.3(11) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?

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 C1 C2 C3 174.2(8) . . . . ?
C3 C8 C7 C6 -1(2) . . . . ?
C6 C5 C4 C3 2.2(17) . . . . ?
C5 C6 C7 C8 -1(2) . . . . ?
C2 C3 C8 C7 -177.9(11) . . . . ?
C2 C3 C4 C5 177.4(10) . . . . ?
C8 C3 C2 C1 -78.4(13) . . . . ?
C8 C3 C4 C5 -3.8(16) . . . . ?
C4 C3 C2 C1 100.4(11) . . . . ?
C4 C3 C8 C7 3.3(17) . . . . ?
C7 C6 C5 C4 0.2(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_PEA-Cu_433K
_database_code_depnum_ccdc_archive 'CCDC 2411277'
loop_
_audit_author_name
_audit_author_address
'Naoto Tsuchiya'
;Hiroshima University
Japan
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-01-17 downloaded from the CCDC.
;
_vrf_PLAT043_PEA-Cu_433K         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      24.18 Check 
RESPONSE: We were not able to include hydrogen atoms due to
disorder generated by the mirror and C4 axis. Manual addition was also failed.
;
_vrf_PLAT242_PEA-Cu_433K         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cu1 Check 
RESPONSE: The bond length of Cu and bridged Cl ions have the same by
considering the symmetry of C4 axis parallel to the c axis. However, the
competition between the Jahn-Teller effect of the Cu ion and the crystalline
symmetry gave the distorted shape of the thermal ellipsoid of the bridged Cl
atom, resulting in the low Ueq value of the neighboring Cu ion.
;

_audit_creation_date             2024-06-26
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Cu, 4(C4 N0.5)'
_chemical_formula_sum            'C16 H24 Cl4 Cu N2'
_chemical_formula_weight         449.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H24N2Cu1Cl4
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.23790(10)
_cell_length_b                   5.23790(10)
_cell_length_c                   39.1329(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1073.63(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16338
_cell_measurement_temperature    432.99(10)
_cell_measurement_theta_max      28.4190
_cell_measurement_theta_min      3.0920
_shelx_estimated_absorpt_T_max   0.742
_shelx_estimated_absorpt_T_min   0.612
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             462
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 3 0.3000
-7 0 -7 0.0200
0 0 55 0.1318
0 0 -55 0.0650
0 -7 14 0.3000
0 7 -7 0.0400

_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.21
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.9868 -0.0015 2.9957 0.8382 0.4266 0.1188
-6.9867 0.0017 -6.9903 -0.8327 -0.4264 -0.1910
-0.0663 -0.0499 55.1990 -0.0805 -0.0123 0.9967
0.0255 0.0618 -55.2003 0.0749 0.0112 -0.9971
0.3558 -7.1410 13.7497 0.4593 -0.8421 0.2827
-0.2997 7.3132 -7.2085 -0.4720 0.8661 -0.1648

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            21351
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         2.082
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      432.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00 100.00   0.50    1.00    --   17.44   5.00  90.00  262
  2  ω    -80.00  39.00   0.50    1.00    --   17.44  -5.00 -86.00  238
  3  ω    -18.00  74.00   0.50    1.00    --   17.44 -99.00 -60.00  184
  4  ω    -18.00  74.00   0.50    1.00    --   17.44 -99.00  60.00  184
  5  ω    -18.00  74.00   0.50    1.00    --   17.44 -99.00-150.00  184
  6  ω   -118.00  39.00   0.50    1.00    --  -19.94  -5.00 -86.00  314
  7  ω    -18.00  37.00   0.50    1.00    --  -19.94 -99.00  30.00  110
  8  ω   -101.00  18.00   0.50    1.00    --  -19.94 -57.00 -90.00  238
  9  ω   -101.00  18.00   0.50    1.00    --  -19.94 -57.00  30.00  238
 10  ω   -101.00  18.00   0.50    1.00    --  -19.94 -57.00 150.00  238
 11  ω    -18.00  37.00   0.50    1.00    --  -19.94 -99.00 150.00  110
 12  ω    -31.00  63.00   0.50    1.00    --  -19.94   5.00  90.00  188
 13  ω   -119.00 -42.00   0.50    1.00    --  -19.94-178.00-120.00  154
 14  ω     47.00 100.00   0.50    1.00    --   17.44 178.00-120.00  106
 15  ω     44.00 100.00   0.50    1.00    --   17.44-178.00 -30.00  112
 16  ω     47.00 100.00   0.50    1.00    --   17.44 178.00  90.00  106
 17  ω    -39.00 100.00   0.50    1.00    --   17.44  38.00 120.00  278
 18  ω    -18.00  37.00   0.50    1.00    --  -19.94 -99.00 120.00  110
 19  ω   -119.00  -1.00   0.50    1.00    --  -19.94   0.00-120.00  236
 20  ω   -119.00  63.00   0.50    1.00    --  -19.94   0.00-150.00  364
 21  ω   -119.00  63.00   0.50    1.00    --  -19.94   0.00-180.00  364
 22  ω    -18.00  37.00   0.50    1.00    --  -19.94 -99.00 -90.00  110
 23  ω    -22.00  63.00   0.50    1.00    --  -19.94  19.00  90.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1205356000
_diffrn_orient_matrix_UB_12      -0.0609490000
_diffrn_orient_matrix_UB_13      -0.0013686000
_diffrn_orient_matrix_UB_21      0.0611037000
_diffrn_orient_matrix_UB_22      0.1208906000
_diffrn_orient_matrix_UB_23      -0.0000400000
_diffrn_orient_matrix_UB_31      0.0092619000
_diffrn_orient_matrix_UB_32      -0.0043454000
_diffrn_orient_matrix_UB_33      0.0180633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                424
_reflns_number_total             435
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         435
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0774
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1035P)²+3.8796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2170
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C5-C6
 1.39 with sigma of 0.02
2. Rigid body (RIGU) restrains
 C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu1, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C5(0.25) C2(0.125) C4(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.0596(8) Uani 1 16 d S T P . .
Cl2 Cl 0.500000 0.500000 0.44185(10) 0.0955(14) Uani 1 8 d S T P . .
Cl1 Cl 0.000000 0.500000 0.500000 0.136(2) Uani 1 8 d S T P . .
C1 C 0.000000 0.000000 0.4097(5) 0.154(12) Uani 1 8 d S T P . .
N1 N 0.000000 0.000000 0.4468(3) 0.087(4) Uani 1 8 d S T P . .
C3 C 0.000000 0.000000 0.3513(7) 0.23(2) Uani 1 8 d S T P . .
C6 C 0.000000 0.000000 0.2852(16) 0.35(7) Uani 1 8 d DS T P . .
C5 C 0.174(6) 0.174(6) 0.2981(11) 0.42(7) Uani 0.5 2 d DS T P . .
C2 C 0.000000 -0.146(9) 0.3888(8) 0.14(2) Uani 0.25 2 d S T P . .
C4 C 0.157(9) 0.157(9) 0.3350(9) 0.35(4) Uani 0.5 2 d S T P . .


_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
Cu1 Cl2 2.276(4) . ?
Cu1 Cl2 2.276(4) 17_666 ?
Cu1 Cl1 2.61895(5) 1_655 ?
Cu1 Cl1 2.61895(5) . ?
Cu1 Cl1 2.61895(5) 3_655 ?
Cu1 Cl1 2.61895(5) 3_665 ?
C1 N1 1.45(2) . ?
C1 C2 1.12(4) 2 ?
C1 C2 1.12(4) 4 ?
C1 C2 1.12(4) . ?
C1 C2 1.12(4) 3 ?
C3 C2 1.65(4) 3 ?
C3 C2 1.65(4) 2 ?
C3 C2 1.65(4) 4 ?
C3 C2 1.65(4) . ?
C3 C4 1.33(6) . ?
C3 C4 1.33(6) 3 ?
C3 C4 1.33(6) 4 ?
C3 C4 1.33(6) 2 ?
C6 C5 1.38(2) 2 ?
C6 C5 1.38(2) 3 ?
C6 C5 1.38(2) 4 ?
C6 C5 1.38(2) . ?
C5 C5 1.82(6) 4 ?
C5 C5 1.82(6) 3 ?
C5 C4 1.45(5) . ?
C2 C2 1.08(7) 3 ?
C2 C2 1.53(10) 2 ?
C2 C2 1.08(7) 4 ?
C4 C4 1.65(10) 4 ?
C4 C4 1.65(10) 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
Cl2 Cu1 Cl2 180.0 . 17_666 ?
Cl2 Cu1 Cl1 90.0 . 1_655 ?
Cl2 Cu1 Cl1 90.0 . . ?
Cl2 Cu1 Cl1 90.0 17_666 . ?
Cl2 Cu1 Cl1 90.0 17_666 3_665 ?
Cl2 Cu1 Cl1 90.0 . 3_655 ?
Cl2 Cu1 Cl1 90.0 17_666 1_655 ?
Cl2 Cu1 Cl1 90.0 . 3_665 ?
Cl2 Cu1 Cl1 90.0 17_666 3_655 ?
Cl1 Cu1 Cl1 180.0 . 1_655 ?
Cl1 Cu1 Cl1 90.0 1_655 3_655 ?
Cl1 Cu1 Cl1 90.0 3_665 1_655 ?
Cl1 Cu1 Cl1 90.0 . 3_655 ?
Cl1 Cu1 Cl1 180.0 3_665 3_655 ?
Cl1 Cu1 Cl1 90.0 3_665 . ?
Cu1 Cl1 Cu1 180.0 1_455 . ?
C2 C1 N1 137(2) . . ?
C2 C1 N1 137(2) 2 . ?
C2 C1 N1 137(2) 4 . ?
C2 C1 N1 137(2) 3 . ?
C2 C1 C2 58(3) 3 . ?
C2 C1 C2 58(3) 3 2 ?
C2 C1 C2 86(5) 4 3 ?
C2 C1 C2 58(3) 4 . ?
C2 C1 C2 58(3) 4 2 ?
C2 C1 C2 86(5) 2 . ?
C2 C3 C2 55(3) . 2 ?
C2 C3 C2 38(2) . 4 ?
C2 C3 C2 38(2) 3 2 ?
C2 C3 C2 38(2) 2 4 ?
C2 C3 C2 55(3) 3 4 ?
C2 C3 C2 38(2) . 3 ?
C4 C3 C2 135(2) . 4 ?
C4 C3 C2 98(2) 3 2 ?
C4 C3 C2 135(2) 3 3 ?
C4 C3 C2 135(2) 2 3 ?
C4 C3 C2 135(2) 3 . ?
C4 C3 C2 98(2) 4 3 ?
C4 C3 C2 135(2) . . ?
C4 C3 C2 98(2) 2 . ?
C4 C3 C2 98(2) 2 4 ?
C4 C3 C2 135(2) 2 2 ?
C4 C3 C2 98(2) 3 4 ?
C4 C3 C2 135(2) 4 4 ?
C4 C3 C2 98(2) . 3 ?
C4 C3 C2 98(2) 4 . ?
C4 C3 C2 98(2) . 2 ?
C4 C3 C2 135(2) 4 2 ?
C4 C3 C4 77(2) 2 4 ?
C4 C3 C4 123(5) 2 . ?
C4 C3 C4 123(5) 4 3 ?
C4 C3 C4 77(2) 3 . ?
C4 C3 C4 77(2) 4 . ?
C4 C3 C4 77(2) 2 3 ?
C5 C6 C5 82(3) . 4 ?
C5 C6 C5 82(3) 2 4 ?
C5 C6 C5 82(3) . 3 ?
C5 C6 C5 137(8) . 2 ?
C5 C6 C5 137(8) 4 3 ?
C5 C6 C5 82(3) 2 3 ?
C6 C5 C5 48.8(14) . 3 ?
C6 C5 C5 48.8(14) . 4 ?
C6 C5 C4 106(6) . . ?
C5 C5 C5 90.000(14) 4 3 ?
C4 C5 C5 87(2) . 3 ?
C4 C5 C5 87(2) . 4 ?
C1 C2 C3 109(4) . . ?
C1 C2 C2 47(2) . 2 ?
C2 C2 C1 61.2(14) 3 . ?
C2 C2 C1 61.2(14) 4 . ?
C2 C2 C3 70.9(10) 3 . ?
C2 C2 C3 70.9(10) 4 . ?
C2 C2 C3 62.5(16) 2 . ?
C2 C2 C2 45.000(19) 3 2 ?
C2 C2 C2 45.000(18) 4 2 ?
C2 C2 C2 90.00(4) 3 4 ?
C3 C4 C5 123(5) . . ?
C3 C4 C4 51.6(10) . 3 ?
C3 C4 C4 51.6(10) . 4 ?
C5 C4 C4 93(2) . 3 ?
C5 C4 C4 93(2) . 4 ?
C4 C4 C4 90.000(3) 4 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 C1 C2 C3 180.000(16) . . . . ?
N1 C1 C2 C2 126.2(10) . . . 4 ?
N1 C1 C2 C2 180.00(2) . . . 2 ?
N1 C1 C2 C2 -126.2(10) . . . 3 ?
C6 C5 C4 C3 0.000(5) . . . . ?
C6 C5 C4 C4 45.10(14) . . . 4 ?
C6 C5 C4 C4 -45.10(13) . . . 3 ?
C5 C6 C5 C5 70(3) 2 . . 4 ?
C5 C6 C5 C5 -70(3) 2 . . 3 ?
C5 C6 C5 C5 140(7) 3 . . 4 ?
C5 C6 C5 C5 -140(7) 4 . . 3 ?
C5 C6 C5 C4 70(3) 3 . . . ?
C5 C6 C5 C4 0.000(1) 2 . . . ?
C5 C6 C5 C4 -70(3) 4 . . . ?
C5 C5 C4 C3 -45.10(14) 4 . . . ?
C5 C5 C4 C3 45.10(13) 3 . . . ?
C5 C5 C4 C4 90.2(3) 3 . . 4 ?
C5 C5 C4 C4 0.000(13) 3 . . 3 ?
C5 C5 C4 C4 0.000(11) 4 . . 4 ?
C5 C5 C4 C4 -90.2(3) 4 . . 3 ?
C2 C1 C2 C3 53.8(10) 4 . . . ?
C2 C1 C2 C3 0.000(7) 2 . . . ?
C2 C1 C2 C3 -53.8(10) 3 . . . ?
C2 C1 C2 C2 -108(2) 3 . . 4 ?
C2 C1 C2 C2 53.8(10) 4 . . 2 ?
C2 C1 C2 C2 -53.8(10) 3 . . 2 ?
C2 C1 C2 C2 -53.8(11) 2 . . 4 ?
C2 C1 C2 C2 108(2) 4 . . 3 ?
C2 C1 C2 C2 53.8(11) 2 . . 3 ?
C2 C3 C2 C1 0.000(10) 2 . . . ?
C2 C3 C2 C1 -48.4(4) 4 . . . ?
C2 C3 C2 C1 48.4(4) 3 . . . ?
C2 C3 C2 C2 96.9(8) 3 . . 4 ?
C2 C3 C2 C2 -48.4(4) 4 . . 2 ?
C2 C3 C2 C2 48.4(4) 2 . . 4 ?
C2 C3 C2 C2 -48.4(4) 2 . . 3 ?
C2 C3 C2 C2 -96.9(8) 4 . . 3 ?
C2 C3 C2 C2 48.4(4) 3 . . 2 ?
C2 C3 C4 C5 -160.7(10) 2 . . . ?
C2 C3 C4 C5 -152(2) 4 . . . ?
C2 C3 C4 C5 160.7(10) 3 . . . ?
C2 C3 C4 C5 152(2) . . . . ?
C2 C3 C4 C4 143(4) 4 . . 4 ?
C2 C3 C4 C4 -88(2) 4 . . 3 ?
C2 C3 C4 C4 -96.3(17) 2 . . 3 ?
C2 C3 C4 C4 88(2) . . . 4 ?
C2 C3 C4 C4 -143(4) . . . 3 ?
C2 C3 C4 C4 96.3(17) 3 . . 4 ?
C2 C3 C4 C4 -135(2) 3 . . 3 ?
C2 C3 C4 C4 135(2) 2 . . 4 ?
C4 C3 C2 C1 141.2(8) 4 . . . ?
C4 C3 C2 C1 62(2) . . . . ?
C4 C3 C2 C1 -62(2) 3 . . . ?
C4 C3 C2 C1 -141.2(8) 2 . . . ?
C4 C3 C2 C2 14(2) . . . 3 ?
C4 C3 C2 C2 110(3) . . . 4 ?
C4 C3 C2 C2 -141.2(8) 2 . . 2 ?
C4 C3 C2 C2 -62(2) 3 . . 2 ?
C4 C3 C2 C2 62(2) . . . 2 ?
C4 C3 C2 C2 92.7(8) 4 . . 3 ?
C4 C3 C2 C2 -13.6(19) 3 . . 4 ?
C4 C3 C2 C2 -170.4(10) 4 . . 4 ?
C4 C3 C2 C2 141.2(8) 4 . . 2 ?
C4 C3 C2 C2 170.4(10) 2 . . 3 ?
C4 C3 C2 C2 -92.7(8) 2 . . 4 ?
C4 C3 C2 C2 -110(3) 3 . . 3 ?
C4 C3 C4 C5 -64.4(17) 3 . . . ?
C4 C3 C4 C5 0.000(2) 2 . . . ?
C4 C3 C4 C5 64.4(17) 4 . . . ?
C4 C3 C4 C4 -64.4(17) 2 . . 4 ?
C4 C3 C4 C4 64.4(17) 2 . . 3 ?
C4 C3 C4 C4 129(3) 4 . . 3 ?
C4 C3 C4 C4 -129(3) 3 . . 4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.037
_oxdiff_exptl_absorpt_empirical_full_min 0.388
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: distilled water'
_exptl_crystal_preparation       'Magnetic properties'
