# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_cu1
_database_code_depnum_ccdc_archive 'CCDC 1949216'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H11 Cl3 Cu N3 O3, N O3, H2 O'
_chemical_formula_sum            'C12 H13 Cl3 Cu N4 O7'
_chemical_formula_weight         495.15

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   20.3976(15)
_cell_length_b                   14.1980(7)
_cell_length_c                   13.6387(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.840(6)
_cell_angle_gamma                90
_cell_volume                     3612.8(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4537
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7560
_cell_measurement_theta_min      3.5580

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_F_000             1992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.698
_shelx_estimated_absorpt_T_min   0.728
_shelx_estimated_absorpt_T_max   0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            12202
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.336
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             3178
_reflns_number_gt                2683
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0726P)²+3.6876P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3178
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1070
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.31826(2) -0.42175(3) 0.08743(3) 0.03995(17) Uani 1 1 d . . . . .
Cl1 Cl -0.49644(5) -0.18176(8) 0.02218(13) 0.0918(5) Uani 1 1 d . . . . .
N1 N -0.23190(12) -0.34620(17) 0.12231(19) 0.0336(5) Uani 1 1 d . . . . .
O1 O -0.37637(11) -0.31100(16) 0.0613(2) 0.0541(6) Uani 1 1 d . . . . .
C1 C -0.35595(16) -0.2229(2) 0.0771(2) 0.0388(7) Uani 1 1 d . . . . .
O1W O -0.48742(15) -0.6116(2) 0.1046(3) 0.0978(12) Uani 1 1 d . . . . .
H1WA H -0.5015 -0.6495 0.0511 0.147 Uiso 1 1 d R U . . .
H1WB H -0.4671 -0.6461 0.1594 0.147 Uiso 1 1 d R U . . .
Cl2 Cl -0.29723(6) 0.08894(6) 0.12584(8) 0.0565(3) Uani 1 1 d . . . . .
N2 N -0.17168(13) -0.39911(19) 0.1435(2) 0.0399(6) Uani 1 1 d . . . . .
H2A H -0.1307 -0.3731 0.1579 0.048 Uiso 1 1 calc R U . . .
O2 O -0.38045(12) -0.46282(19) -0.0788(2) 0.0583(7) Uani 1 1 d . . . . .
H2B H -0.4201 -0.4333 -0.1104 0.087 Uiso 1 1 d R U . . .
H2C H -0.3926 -0.5215 -0.0896 0.087 Uiso 1 1 d R U . . .
C2 C -0.40716(17) -0.1507(2) 0.0603(3) 0.0477(8) Uani 1 1 d . . . . .
Cl3 Cl -0.33848(6) -0.66507(7) 0.07360(10) 0.0664(3) Uani 1 1 d . . . . .
N3 N -0.24561(13) -0.52759(18) 0.11357(19) 0.0371(6) Uani 1 1 d . . . . .
O3 O -0.38030(13) -0.47786(18) 0.1560(2) 0.0566(6) Uani 1 1 d . . . . .
H3A H -0.3635 -0.4669 0.2196 0.085 Uiso 1 1 d R U . . .
H3D H -0.4144 -0.5178 0.1408 0.085 Uiso 1 1 d R U . . .
C3 C -0.38975(19) -0.0569(2) 0.0746(3) 0.0479(8) Uani 1 1 d . . . . .
H3B H -0.4253 -0.0118 0.0621 0.058 Uiso 1 1 calc R U . . .
C4 C -0.31892(18) -0.0303(2) 0.1077(3) 0.0413(7) Uani 1 1 d . . . . .
C5 C -0.26644(17) -0.0965(2) 0.1266(2) 0.0385(7) Uani 1 1 d . . . . .
H5A H -0.2188 -0.0779 0.1500 0.046 Uiso 1 1 calc R U . . .
N5 N -0.5000 -0.3704(3) 0.2500 0.0679(14) Uani 1 2 d DS T P . .
C6 C -0.28425(15) -0.1923(2) 0.1106(2) 0.0325(6) Uani 1 1 d . . . . .
C7 C -0.22556(15) -0.2560(2) 0.1308(2) 0.0361(7) Uani 1 1 d . . . . .
H7A H -0.1799 -0.2305 0.1513 0.043 Uiso 1 1 calc R U . . .
C8 C -0.17891(16) -0.4942(2) 0.1409(2) 0.0364(7) Uani 1 1 d . . . . .
C9 C -0.11930(19) -0.5533(3) 0.1639(3) 0.0506(8) Uani 1 1 d . . . . .
H9A H -0.0739 -0.5282 0.1812 0.061 Uiso 1 1 calc R U . . .
C10 C -0.1296(2) -0.6483(3) 0.1602(3) 0.0544(9) Uani 1 1 d . . . . .
H10A H -0.0909 -0.6888 0.1758 0.065 Uiso 1 1 calc R U . . .
C11 C -0.19743(19) -0.6844(2) 0.1334(3) 0.0520(9) Uani 1 1 d . . . . .
H11A H -0.2051 -0.7490 0.1312 0.062 Uiso 1 1 calc R U . . .
C12 C -0.25282(18) -0.6226(2) 0.1103(3) 0.0437(7) Uani 1 1 d . . . . .
O7 O -0.4242(3) -0.3699(4) 0.2830(5) 0.0610(13) Uani 0.5 1 d D . P . .
O6 O -0.4734(7) -0.3839(10) 0.3365(11) 0.154(6) Uani 0.5 1 d D . P . .
O8 O -0.5136(8) -0.3545(10) 0.3190(16) 0.157(6) Uani 0.5 1 d D . P . .
N4 N 0.0000 -0.3006(4) 0.2500 0.0898(18) Uani 1 2 d S T P . .
O4 O 0.0000 -0.3867(4) 0.2500 0.129(2) Uani 1 2 d S T P . .
O5 O -0.05609(15) -0.2580(3) 0.2240(4) 0.1211(16) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.914(2) . ?
Cu1 N1 1.950(2) . ?
Cu1 O3 2.017(2) . ?
Cu1 N3 2.038(3) . ?
Cu1 O2 2.183(2) . ?
Cl1 C2 1.736(3) . ?
N1 C7 1.287(4) . ?
N1 N2 1.368(3) . ?
O1 C1 1.308(4) . ?
C1 C6 1.413(4) . ?
C1 C2 1.414(4) . ?
O1W H1WA 0.8573 . ?
O1W H1WB 0.8497 . ?
Cl2 C4 1.742(3) . ?
N2 C8 1.356(4) . ?
N2 H2A 0.8600 . ?
O2 H2B 0.8562 . ?
O2 H2C 0.8643 . ?
C2 C3 1.372(5) . ?
Cl3 C12 1.720(3) . ?
N3 C8 1.344(4) . ?
N3 C12 1.356(4) . ?
O3 H3A 0.8082 . ?
O3 H3D 0.8560 . ?
C3 C4 1.381(5) . ?
C3 H3B 0.9300 . ?
C4 C5 1.369(5) . ?
C5 C6 1.402(4) . ?
C5 H5A 0.9300 . ?
N5 O6 1.098(13) 2_455 ?
N5 O6 1.098(13) . ?
N5 O8 1.107(13) 2_455 ?
N5 O8 1.107(13) . ?
N5 O7 1.424(5) . ?
N5 O7 1.424(5) 2_455 ?
C6 C7 1.436(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.404(4) . ?
C9 C10 1.364(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.378(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.362(5) . ?
C11 H11A 0.9300 . ?
O7 O8 1.471(19) 2_455 ?
O7 O6 1.47(2) . ?
O6 O8 0.863(13) . ?
O8 O7 1.471(19) 2_455 ?
N4 O5 1.214(4) 2 ?
N4 O5 1.214(4) . ?
N4 O4 1.222(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 91.36(9) . . ?
O1 Cu1 O3 87.34(11) . . ?
N1 Cu1 O3 141.12(10) . . ?
O1 Cu1 N3 171.92(10) . . ?
N1 Cu1 N3 80.90(10) . . ?
O3 Cu1 N3 100.13(10) . . ?
O1 Cu1 O2 88.26(10) . . ?
N1 Cu1 O2 119.26(10) . . ?
O3 Cu1 O2 99.55(10) . . ?
N3 Cu1 O2 93.50(10) . . ?
C7 N1 N2 118.6(2) . . ?
C7 N1 Cu1 128.1(2) . . ?
N2 N1 Cu1 113.27(19) . . ?
C1 O1 Cu1 128.5(2) . . ?
O1 C1 C6 124.5(3) . . ?
O1 C1 C2 120.1(3) . . ?
C6 C1 C2 115.4(3) . . ?
H1WA O1W H1WB 105.2 . . ?
C8 N2 N1 117.5(2) . . ?
C8 N2 H2A 121.2 . . ?
N1 N2 H2A 121.2 . . ?
Cu1 O2 H2B 115.2 . . ?
Cu1 O2 H2C 116.1 . . ?
H2B O2 H2C 103.8 . . ?
C3 C2 C1 123.3(3) . . ?
C3 C2 Cl1 118.0(2) . . ?
C1 C2 Cl1 118.7(3) . . ?
C8 N3 C12 116.4(3) . . ?
C8 N3 Cu1 111.8(2) . . ?
C12 N3 Cu1 131.8(2) . . ?
Cu1 O3 H3A 110.4 . . ?
Cu1 O3 H3D 138.7 . . ?
H3A O3 H3D 109.7 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 Cl2 120.4(3) . . ?
C3 C4 Cl2 119.0(3) . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
O6 N5 O6 159.9(15) 2_455 . ?
O6 N5 O8 46.1(8) 2_455 2_455 ?
O6 N5 O8 139.9(10) . 2_455 ?
O6 N5 O8 139.9(10) 2_455 . ?
O6 N5 O8 46.1(8) . . ?
O8 N5 O8 156.5(17) 2_455 . ?
O6 N5 O7 110.0(9) 2_455 . ?
O6 N5 O7 70.1(9) . . ?
O8 N5 O7 69.8(9) 2_455 . ?
O8 N5 O7 110.1(9) . . ?
O6 N5 O7 70.1(9) 2_455 2_455 ?
O6 N5 O7 110.0(9) . 2_455 ?
O8 N5 O7 110.1(9) 2_455 2_455 ?
O8 N5 O7 69.8(9) . 2_455 ?
O7 N5 O7 179.4(6) . 2_455 ?
C5 C6 C1 121.2(3) . . ?
C5 C6 C7 116.0(3) . . ?
C1 C6 C7 122.8(3) . . ?
N1 C7 C6 124.3(3) . . ?
N1 C7 H7A 117.8 . . ?
C6 C7 H7A 117.8 . . ?
N3 C8 N2 116.5(3) . . ?
N3 C8 C9 122.6(3) . . ?
N2 C8 C9 120.9(3) . . ?
C10 C9 C8 118.4(3) . . ?
C10 C9 H9A 120.8 . . ?
C8 C9 H9A 120.8 . . ?
C9 C10 C11 120.1(3) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C12 C11 C10 118.2(3) . . ?
C12 C11 H11A 120.9 . . ?
C10 C11 H11A 120.9 . . ?
N3 C12 C11 124.3(3) . . ?
N3 C12 Cl3 116.2(2) . . ?
C11 C12 Cl3 119.5(3) . . ?
N5 O7 O8 44.9(4) . 2_455 ?
N5 O7 O6 44.5(4) . . ?
O8 O7 O6 89.4(6) 2_455 . ?
O8 O6 N5 67.5(16) . . ?
O8 O6 O7 124(2) . . ?
N5 O6 O7 65.4(10) . . ?
O6 O8 N5 66.4(13) . . ?
O6 O8 O7 123.2(18) . 2_455 ?
N5 O8 O7 65.3(10) . 2_455 ?
O5 N4 O5 120.2(6) 2 . ?
O5 N4 O4 119.9(3) 2 . ?
O5 N4 O4 119.9(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O1 0.86 2.41 2.994(4) 126.3 5_445
O1W H1WA Cl1 0.86 2.59 3.354(4) 149.0 5_445
O1W H1WB O5 0.85 2.16 2.983(6) 163.0 4_445
N2 H2A O5 0.86 2.17 2.947(4) 150.9 .
N2 H2A O4 0.86 2.45 3.208(3) 146.8 .
O2 H2B O1W 0.86 2.02 2.782(4) 147.1 5_445
O2 H2C O6 0.86 2.05 2.810(10) 146.6 6_545
O2 H2C O7 0.86 2.22 2.938(7) 141.0 6_545
O2 H2C Cl3 0.86 2.89 3.444(3) 123.7 .
O3 H3A O7 0.81 2.25 2.722(6) 118.1 .
O3 H3D O1W 0.86 1.91 2.762(4) 176.9 .

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.063

_shelxl_version_number           2014-3



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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1949217'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Cl4 Cu N6 O2, 2(H2 O), N O3'
_chemical_formula_sum            'C24 H22 Cl4 Cu N7 O7'
_chemical_formula_weight         725.84

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 2'
_space_group_name_Hall           'I 2y'

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

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

_cell_length_a                   21.2421(12)
_cell_length_b                   7.1200(3)
_cell_length_c                   22.4062(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.875(6)
_cell_angle_gamma                90
_cell_volume                     3049.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2338
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.7230
_cell_measurement_theta_min      3.7360

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             1472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.121
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            10307
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.395
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.948
_reflns_number_total             5920
_reflns_number_gt                3929
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_max     0.875
_reflns_Friedel_fraction_full    0.899

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+2.8168P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1321 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5920
_refine_ls_number_parameters     395
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1462
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.33067(5) 0.01454(15) 0.50567(4) 0.0540(3) Uani 1 1 d . . . . .
Cl1 Cl 0.42933(16) -0.1130(4) 0.42768(14) 0.0823(8) Uani 1 1 d . . . . .
N1 N 0.4168(4) 0.1397(10) 0.5745(3) 0.0511(18) Uani 1 1 d . . . . .
C1 C 0.4461(4) 0.0471(14) 0.6329(4) 0.051(2) Uani 1 1 d . . . . .
O1 O 0.2000(4) -0.3959(12) 0.6179(4) 0.0848(17) Uani 1 1 d . U . . .
H1 H 0.1678 -0.4527 0.6207 0.127 Uiso 1 1 calc R U . . .
O2 O 0.0950(4) -0.0041(12) 0.5496(3) 0.085(2) Uani 1 1 d . U . . .
H2 H 0.0943 -0.1177 0.5553 0.127 Uiso 1 1 calc R U . . .
N2 N 0.4136(4) -0.1140(12) 0.6369(4) 0.064(2) Uani 1 1 d . . . . .
H2A H 0.4309 -0.1804 0.6726 0.077 Uiso 1 1 calc R U . . .
C2 C 0.5058(5) 0.1125(16) 0.6865(5) 0.069(3) Uani 1 1 d . . . . .
H2B H 0.5254 0.0440 0.7257 0.082 Uiso 1 1 calc R U . . .
Cl2 Cl 0.40897(16) 0.4152(4) 0.49582(17) 0.0911(10) Uani 1 1 d . . . . .
Cl3 Cl 0.17134(16) -0.4343(4) 0.34494(11) 0.0826(9) Uani 1 1 d . . . . .
N3 N 0.3524(4) -0.1711(11) 0.5836(3) 0.0505(18) Uani 1 1 d . . . . .
C3 C 0.5348(6) 0.2756(18) 0.6812(6) 0.083(3) Uani 1 1 d . . . . .
H3 H 0.5742 0.3213 0.7170 0.100 Uiso 1 1 calc R U . . .
O3 O -0.0039(5) -0.1368(15) 0.4087(5) 0.101(3) Uani 1 1 d G . . . .
H3A H -0.0160 -0.0249 0.3954 0.151 Uiso 1 1 d G U . . .
H3B H 0.0169 -0.1752 0.3861 0.151 Uiso 1 1 d G U . . .
Cl4 Cl 0.37214(16) 0.2947(5) 0.72718(13) 0.0897(10) Uani 1 1 d . . . . .
N4 N 0.3040(4) -0.0055(11) 0.4075(3) 0.0514(17) Uani 1 1 d . . . . .
C4 C 0.5060(6) 0.3752(17) 0.6223(7) 0.086(4) Uani 1 1 d . . . . .
H4 H 0.5251 0.4884 0.6174 0.103 Uiso 1 1 calc R U . . .
O4 O 0.4218(5) 0.0074(16) 0.8739(5) 0.113(3) Uani 1 1 d G . . . .
H4A H 0.4340 0.1180 0.8694 0.169 Uiso 1 1 d G U . . .
H4B H 0.4256 -0.0646 0.8455 0.169 Uiso 1 1 d G U . . .
C5 C 0.4479(5) 0.2991(14) 0.5714(5) 0.060(2) Uani 1 1 d . . . . .
N5 N 0.1966(4) 0.0834(11) 0.4003(3) 0.058(2) Uani 1 1 d . . . . .
H5 H 0.1527 0.1041 0.3774 0.069 Uiso 1 1 calc R U . . .
O5 O 0.4526(5) -0.2532(16) 0.7761(4) 0.119(3) Uani 1 1 d . . . . .
N6 N 0.2262(4) 0.0911(10) 0.4688(3) 0.0522(18) Uani 1 1 d . . . . .
C6 C 0.3439(5) -0.0482(12) 0.3761(4) 0.054(2) Uani 1 1 d . . . . .
O6 O 0.5419(5) -0.3046(12) 0.7525(4) 0.0903(17) Uani 1 1 d . U . . .
C7 C 0.3201(6) -0.0477(15) 0.3086(5) 0.075(3) Uani 1 1 d . . . . .
H7 H 0.3493 -0.0782 0.2890 0.090 Uiso 1 1 calc R U . . .
N7 N 0.5138(7) -0.3214(15) 0.7911(5) 0.092(3) Uani 1 1 d . U . . .
O7 O 0.5455(6) -0.4124(17) 0.8387(6) 0.142(4) Uani 1 1 d . U . . .
C8 C 0.2513(5) -0.0004(16) 0.2711(4) 0.068(3) Uani 1 1 d . . . . .
H8 H 0.2334 -0.0021 0.2251 0.082 Uiso 1 1 calc R U . . .
C9 C 0.2088(5) 0.0488(13) 0.2993(4) 0.060(2) Uani 1 1 d . . . . .
H9 H 0.1627 0.0850 0.2737 0.072 Uiso 1 1 calc R U . . .
C10 C 0.2375(5) 0.0431(12) 0.3696(4) 0.048(2) Uani 1 1 d . . . . .
C11 C 0.1830(5) 0.1001(13) 0.4946(4) 0.058(2) Uani 1 1 d . . . . .
H11 H 0.1353 0.0972 0.4669 0.070 Uiso 1 1 calc R U . . .
C12 C 0.2064(5) 0.1147(12) 0.5664(4) 0.050(2) Uani 1 1 d . . . . .
C13 C 0.1594(5) 0.0670(14) 0.5927(4) 0.062(3) Uani 1 1 d . . . . .
C14 C 0.1780(6) 0.0816(17) 0.6586(5) 0.078(3) Uani 1 1 d . . . . .
H14 H 0.1466 0.0450 0.6752 0.093 Uiso 1 1 calc R U . . .
C15 C 0.2441(7) 0.1513(16) 0.7022(5) 0.077(3) Uani 1 1 d . . . . .
H15 H 0.2570 0.1624 0.7474 0.093 Uiso 1 1 calc R U . . .
C16 C 0.2893(6) 0.2030(14) 0.6752(4) 0.063(3) Uani 1 1 d . . . . .
C17 C 0.2713(5) 0.1838(12) 0.6091(4) 0.051(2) Uani 1 1 d . . . . .
H17 H 0.3030 0.2175 0.5926 0.062 Uiso 1 1 calc R U . . .
C18 C 0.3133(5) -0.2874(12) 0.5952(4) 0.052(2) Uani 1 1 d . . . . .
H18 H 0.3260 -0.3284 0.6384 0.063 Uiso 1 1 calc R U . . .
C19 C 0.2483(4) -0.3569(11) 0.5411(4) 0.046(2) Uani 1 1 d . . . . .
C20 C 0.2408(5) -0.3686(12) 0.4769(4) 0.054(2) Uani 1 1 d . . . . .
H20 H 0.2787 -0.3397 0.4683 0.065 Uiso 1 1 calc R U . . .
C21 C 0.1787(5) -0.4220(13) 0.4255(4) 0.055(2) Uani 1 1 d . . . . .
C22 C 0.1226(5) -0.4662(16) 0.4380(4) 0.070(3) Uani 1 1 d . . . . .
H22 H 0.0803 -0.5009 0.4032 0.084 Uiso 1 1 calc R U . . .
C23 C 0.1289(5) -0.4593(16) 0.5020(4) 0.065(3) Uani 1 1 d . . . . .
H23 H 0.0910 -0.4914 0.5102 0.078 Uiso 1 1 calc R U . . .
C24 C 0.1922(5) -0.4041(12) 0.5545(4) 0.051(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.015(7) . ?
Cu1 N4 2.022(6) . ?
Cu1 N6 2.074(8) . ?
Cu1 N3 2.075(7) . ?
Cl1 C6 1.735(9) . ?
N1 C5 1.329(12) . ?
N1 C1 1.351(10) . ?
C1 N2 1.362(12) . ?
C1 C2 1.391(11) . ?
O1 C24 1.358(10) . ?
O1 H1 0.8200 . ?
O2 C13 1.381(11) . ?
O2 H2 0.8200 . ?
N2 N3 1.389(9) . ?
N2 H2A 0.8600 . ?
C2 C3 1.344(15) . ?
C2 H2B 0.9300 . ?
Cl2 C5 1.737(10) . ?
Cl3 C21 1.745(9) . ?
N3 C18 1.278(11) . ?
C3 C4 1.383(15) . ?
C3 H3 0.9300 . ?
O3 H3A 0.8499 . ?
O3 H3B 0.8498 . ?
Cl4 C16 1.758(11) . ?
N4 C10 1.338(10) . ?
N4 C6 1.351(11) . ?
C4 C5 1.374(14) . ?
C4 H4 0.9300 . ?
O4 H4A 0.8493 . ?
O4 H4B 0.8497 . ?
N5 C10 1.354(11) . ?
N5 N6 1.381(9) . ?
N5 H5 0.8600 . ?
O5 N7 1.288(14) . ?
N6 C11 1.284(12) . ?
C6 C7 1.370(12) . ?
O6 N7 1.254(13) . ?
C7 C8 1.372(13) . ?
C7 H7 0.9300 . ?
N7 O7 1.176(13) . ?
C8 C9 1.354(13) . ?
C8 H8 0.9300 . ?
C9 C10 1.418(10) . ?
C9 H9 0.9300 . ?
C11 C12 1.466(12) . ?
C11 H11 0.9300 . ?
C12 C17 1.380(12) . ?
C12 C13 1.405(12) . ?
C13 C14 1.355(13) . ?
C14 C15 1.405(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.392(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.365(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.469(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.379(12) . ?
C19 C24 1.391(12) . ?
C20 C21 1.372(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.373(13) . ?
C22 C23 1.382(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.401(11) . ?
C23 H23 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
N1 Cu1 N4 126.4(3) . . ?
N1 Cu1 N6 130.2(3) . . ?
N4 Cu1 N6 80.9(3) . . ?
N1 Cu1 N3 81.0(3) . . ?
N4 Cu1 N3 136.4(3) . . ?
N6 Cu1 N3 108.0(3) . . ?
C5 N1 C1 116.0(8) . . ?
C5 N1 Cu1 130.0(6) . . ?
C1 N1 Cu1 114.0(6) . . ?
N1 C1 N2 116.3(7) . . ?
N1 C1 C2 122.2(9) . . ?
N2 C1 C2 121.5(8) . . ?
C24 O1 H1 109.5 . . ?
C13 O2 H2 109.5 . . ?
C1 N2 N3 120.1(7) . . ?
C1 N2 H2A 120.0 . . ?
N3 N2 H2A 120.0 . . ?
C3 C2 C1 119.5(10) . . ?
C3 C2 H2B 120.2 . . ?
C1 C2 H2B 120.2 . . ?
C18 N3 N2 117.5(7) . . ?
C18 N3 Cu1 131.3(6) . . ?
N2 N3 Cu1 108.6(5) . . ?
C2 C3 C4 119.9(10) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
H3A O3 H3B 104.5 . . ?
C10 N4 C6 117.1(7) . . ?
C10 N4 Cu1 113.0(5) . . ?
C6 N4 Cu1 129.8(6) . . ?
C5 C4 C3 116.8(11) . . ?
C5 C4 H4 121.6 . . ?
C3 C4 H4 121.6 . . ?
H4A O4 H4B 109.6 . . ?
N1 C5 C4 125.5(10) . . ?
N1 C5 Cl2 114.9(7) . . ?
C4 C5 Cl2 119.6(9) . . ?
C10 N5 N6 119.4(7) . . ?
C10 N5 H5 120.3 . . ?
N6 N5 H5 120.3 . . ?
C11 N6 N5 115.8(7) . . ?
C11 N6 Cu1 133.2(6) . . ?
N5 N6 Cu1 108.7(5) . . ?
N4 C6 C7 124.1(9) . . ?
N4 C6 Cl1 115.1(6) . . ?
C7 C6 Cl1 120.7(8) . . ?
C6 C7 C8 117.3(10) . . ?
C6 C7 H7 121.4 . . ?
C8 C7 H7 121.4 . . ?
O7 N7 O6 115.0(14) . . ?
O7 N7 O5 123.9(13) . . ?
O6 N7 O5 120.9(9) . . ?
C9 C8 C7 121.7(8) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 117.3(9) . . ?
C8 C9 H9 121.3 . . ?
C10 C9 H9 121.3 . . ?
N4 C10 N5 117.7(7) . . ?
N4 C10 C9 122.4(8) . . ?
N5 C10 C9 119.9(8) . . ?
N6 C11 C12 122.2(8) . . ?
N6 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C17 C12 C13 118.3(8) . . ?
C17 C12 C11 122.9(8) . . ?
C13 C12 C11 118.7(8) . . ?
C14 C13 O2 121.3(9) . . ?
C14 C13 C12 121.0(9) . . ?
O2 C13 C12 117.6(8) . . ?
C13 C14 C15 120.8(10) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C16 117.5(9) . . ?
C14 C15 H15 121.3 . . ?
C16 C15 H15 121.3 . . ?
C17 C16 C15 121.7(10) . . ?
C17 C16 Cl4 118.8(8) . . ?
C15 C16 Cl4 119.4(8) . . ?
C16 C17 C12 120.6(9) . . ?
C16 C17 H17 119.7 . . ?
C12 C17 H17 119.7 . . ?
N3 C18 C19 120.6(8) . . ?
N3 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C24 119.3(8) . . ?
C20 C19 C18 121.4(8) . . ?
C24 C19 C18 119.2(8) . . ?
C21 C20 C19 121.6(9) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C22 119.6(8) . . ?
C20 C21 Cl3 120.1(8) . . ?
C22 C21 Cl3 120.3(7) . . ?
C21 C22 C23 120.2(8) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C24 120.3(9) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
O1 C24 C19 119.3(8) . . ?
O1 C24 C23 121.7(9) . . ?
C19 C24 C23 118.9(8) . . ?

_refine_diff_density_max         0.665
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_1011s48-1
_database_code_depnum_ccdc_archive 'CCDC 2072362'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C23 H14.50 Br Cl0.50 Cu N6 O), C H4 O'
_chemical_formula_sum            'C93 H62 Br4 Cl2 Cu4 N24 O5'
_chemical_formula_weight         2240.37

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   12.9230(11)
_cell_length_b                   13.3034(7)
_cell_length_c                   14.0758(8)
_cell_angle_alpha                85.644(4)
_cell_angle_beta                 71.862(7)
_cell_angle_gamma                72.048(6)
_cell_volume                     2187.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3217
_cell_measurement_theta_min      3.6820
_cell_measurement_theta_max      24.6350

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_F_000             1118
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    2.918
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.83920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            15472
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.366
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             7677
_reflns_number_gt                4205
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0589P)²+1.2568P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7677
_refine_ls_number_parameters     615
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1783
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.30404(7) 0.25618(6) 0.93927(7) 0.0414(3) Uani 1 1 d . . . . .
Br1 Br 0.10441(8) -0.14445(7) 1.27944(8) 0.0697(3) Uani 1 1 d . . . . .
O1 O 0.1725(4) 0.2400(4) 1.0427(4) 0.0476(13) Uani 1 1 d . . . . .
Cl1 Cl 0.3799(5) 0.4197(4) 0.7628(5) 0.110(3) Uani 0.500(7) 1 d D . P A 2
N1 N 0.5538(5) 0.3093(5) 0.6739(5) 0.0516(17) Uani 1 1 d . . . . .
C1 C 0.2278(7) -0.0329(6) 1.1293(6) 0.049(2) Uani 1 1 d . . . . .
H1 H 0.2852 -0.0974 1.1178 0.059 Uiso 1 1 calc R U . . .
O3 O 0.2053(17) 1.0253(13) 0.5200(15) 0.144(7) Uani 0.5 1 d D U P . .
H3B H 0.2723 0.9926 0.4928 0.216 Uiso 0.5 1 calc R U P . .
Cu2 Cu 0.67803(7) 0.68618(6) 0.43726(7) 0.0410(3) Uani 1 1 d . . . . .
Br2 Br 0.79915(8) 1.11664(7) 0.09625(7) 0.0640(3) Uani 1 1 d . . . . .
O2 O 0.7903(4) 0.7122(4) 0.3182(4) 0.0475(13) Uani 1 1 d . . . . .
Cl2 Cl 0.5917(4) 0.4871(4) 0.5668(4) 0.086(2) Uani 0.500(7) 1 d D . P A 2
N2 N 0.4302(5) 0.2497(5) 0.8143(5) 0.0426(15) Uani 1 1 d . . . . .
C2 C 0.1270(7) -0.0241(6) 1.2024(6) 0.051(2) Uani 1 1 d . . . . .
N3 N 0.4888(5) 0.0712(5) 0.8587(5) 0.0520(17) Uani 1 1 d . . . . .
C3 C 0.0414(7) 0.0712(6) 1.2207(6) 0.055(2) Uani 1 1 d . . . . .
H3A H -0.0274 0.0768 1.2704 0.067 Uiso 1 1 calc R U . . .
N4 N 0.3851(5) 0.1068(5) 0.9335(5) 0.0421(15) Uani 1 1 d . . . . .
C4 C 0.0577(7) 0.1569(6) 1.1660(6) 0.051(2) Uani 1 1 d . . . . .
H4 H -0.0013 0.2202 1.1789 0.062 Uiso 1 1 calc R U . . .
N5 N 0.3839(5) 0.3278(5) 1.0357(5) 0.0506(17) Uani 1 1 d . . . . .
C5 C 0.1604(6) 0.1536(6) 1.0906(6) 0.0416(18) Uani 1 1 d . . . . .
N6 N 0.2202(5) 0.4132(4) 0.9452(4) 0.0397(14) Uani 1 1 d . . . . .
C6 C 0.2460(6) 0.0541(5) 1.0712(6) 0.0415(18) Uani 1 1 d . . . . .
N7 N 0.4169(5) 0.5875(5) 0.6605(5) 0.0457(16) Uani 1 1 d . . . . .
C7 C 0.3535(6) 0.0360(6) 0.9930(6) 0.0459(19) Uani 1 1 d . . . . .
H7 H 0.4040 -0.0321 0.9849 0.055 Uiso 1 1 calc R U . . .
N8 N 0.5355(5) 0.6661(4) 0.5337(5) 0.0426(16) Uani 1 1 d . . . . .
C8 C 0.5076(6) 0.1490(6) 0.7982(6) 0.0453(19) Uani 1 1 d . . . . .
N9 N 0.4671(5) 0.8470(4) 0.5076(5) 0.0487(17) Uani 1 1 d . . . . .
C9 C 0.6089(6) 0.1302(7) 0.7173(6) 0.053(2) Uani 1 1 d . . . . .
H9 H 0.6608 0.0628 0.7050 0.064 Uiso 1 1 calc R U . . .
N10 N 0.5720(5) 0.8256(4) 0.4361(4) 0.0396(15) Uani 1 1 d . . . . .
C10 C 0.6295(7) 0.2089(7) 0.6592(6) 0.060(2) Uani 1 1 d . . . . .
H10 H 0.6973 0.1961 0.6068 0.071 Uiso 1 1 calc R U . . .
N11 N 0.7878(5) 0.5433(4) 0.4473(4) 0.0389(14) Uani 1 1 d . . . . .
C11 C 0.4550(7) 0.3241(6) 0.7519(6) 0.053(2) Uani 1 1 d D . . . .
H11 H 0.4019 0.3910 0.7615 0.063 Uiso 0.500(7) 1 calc R U P A 1
N12 N 0.7366(6) 0.7083(5) 0.5724(5) 0.0516(17) Uani 1 1 d . . . . .
C12 C 0.1429(6) 0.4544(6) 0.8977(6) 0.052(2) Uani 1 1 d . . . . .
H12 H 0.1292 0.4108 0.8575 0.062 Uiso 1 1 calc R U . . .
C13 C 0.0819(6) 0.5619(6) 0.9067(6) 0.050(2) Uani 1 1 d . . . . .
H13 H 0.0265 0.5886 0.8745 0.060 Uiso 1 1 calc R U . . .
C14 C 0.1035(7) 0.6271(6) 0.9626(6) 0.053(2) Uani 1 1 d . . . . .
H14 H 0.0619 0.6984 0.9696 0.063 Uiso 1 1 calc R U . . .
C15 C 0.1877(6) 0.5878(5) 1.0095(6) 0.0445(19) Uani 1 1 d . . . . .
C16 C 0.2440(6) 0.4777(5) 1.0004(6) 0.0407(18) Uani 1 1 d . . . . .
C17 C 0.3306(6) 0.4337(6) 1.0465(6) 0.047(2) Uani 1 1 d . . . . .
C18 C 0.4635(8) 0.2877(7) 1.0810(7) 0.069(3) Uani 1 1 d . . . . .
H18 H 0.5016 0.2157 1.0727 0.083 Uiso 1 1 calc R U . . .
C19 C 0.4933(8) 0.3461(8) 1.1398(8) 0.084(3) Uani 1 1 d . . . . .
H19 H 0.5481 0.3131 1.1712 0.101 Uiso 1 1 calc R U . . .
C20 C 0.4416(8) 0.4524(8) 1.1511(8) 0.081(3) Uani 1 1 d . . . . .
H20 H 0.4620 0.4929 1.1891 0.097 Uiso 1 1 calc R U . . .
C21 C 0.3574(7) 0.5000(6) 1.1048(6) 0.054(2) Uani 1 1 d . . . . .
C22 C 0.2967(7) 0.6095(6) 1.1145(7) 0.062(2) Uani 1 1 d . . . . .
H22 H 0.3129 0.6528 1.1533 0.075 Uiso 1 1 calc R U . . .
C23 C 0.2168(8) 0.6518(6) 1.0693(7) 0.061(2) Uani 1 1 d . . . . .
H23 H 0.1792 0.7240 1.0765 0.074 Uiso 1 1 calc R U . . .
C24 C 0.5155(6) 0.5814(5) 0.5851(6) 0.045(2) Uani 1 1 d D . . . .
H24 H 0.5708 0.5160 0.5687 0.055 Uiso 0.500(7) 1 calc R U P A 1
C25 C 0.3341(7) 0.6820(6) 0.6829(6) 0.052(2) Uani 1 1 d . . . . .
H25 H 0.2666 0.6861 0.7338 0.062 Uiso 1 1 calc R U . . .
C26 C 0.3472(6) 0.7680(6) 0.6339(6) 0.048(2) Uani 1 1 d . . . . .
H26 H 0.2894 0.8321 0.6490 0.057 Uiso 1 1 calc R U . . .
C27 C 0.4523(6) 0.7605(6) 0.5573(6) 0.0419(18) Uani 1 1 d . . . . .
C28 C 0.5912(6) 0.9014(6) 0.3794(6) 0.0446(19) Uani 1 1 d . . . . .
H28 H 0.5346 0.9663 0.3924 0.054 Uiso 1 1 calc R U . . .
C29 C 0.6926(6) 0.8958(5) 0.2974(5) 0.0387(17) Uani 1 1 d . . . . .
C30 C 0.6983(7) 0.9886(6) 0.2443(6) 0.048(2) Uani 1 1 d . . . . .
H30 H 0.6368 1.0498 0.2614 0.058 Uiso 1 1 calc R U . . .
C31 C 0.7946(7) 0.9891(6) 0.1670(6) 0.0453(19) Uani 1 1 d . . . . .
C32 C 0.8858(7) 0.8987(6) 0.1391(6) 0.055(2) Uani 1 1 d . . . . .
H32 H 0.9502 0.8998 0.0864 0.066 Uiso 1 1 calc R U . . .
C33 C 0.8810(6) 0.8076(6) 0.1895(6) 0.052(2) Uani 1 1 d . . . . .
H33 H 0.9423 0.7467 0.1686 0.062 Uiso 1 1 calc R U . . .
C34 C 0.7864(6) 0.8016(6) 0.2724(6) 0.0414(18) Uani 1 1 d . . . . .
C35 C 0.7064(8) 0.7897(8) 0.6352(8) 0.078(3) Uani 1 1 d . . . . .
H35 H 0.6604 0.8548 0.6218 0.093 Uiso 1 1 calc R U . . .
C36 C 0.7412(10) 0.7804(9) 0.7195(8) 0.089(3) Uani 1 1 d . . . . .
H36 H 0.7194 0.8390 0.7613 0.107 Uiso 1 1 calc R U . . .
C37 C 0.8066(9) 0.6871(9) 0.7415(7) 0.079(3) Uani 1 1 d . . . . .
H37 H 0.8305 0.6812 0.7982 0.095 Uiso 1 1 calc R U . . .
C38 C 0.8381(7) 0.6004(8) 0.6795(7) 0.058(2) Uani 1 1 d . . . . .
C39 C 0.9079(8) 0.4962(9) 0.6949(7) 0.071(3) Uani 1 1 d . . . . .
H39 H 0.9334 0.4853 0.7509 0.085 Uiso 1 1 calc R U . . .
C40 C 0.9371(8) 0.4151(8) 0.6319(8) 0.072(3) Uani 1 1 d . . . . .
H40 H 0.9846 0.3499 0.6431 0.086 Uiso 1 1 calc R U . . .
C41 C 0.8954(7) 0.4278(7) 0.5463(7) 0.056(2) Uani 1 1 d . . . . .
C42 C 0.9208(7) 0.3454(6) 0.4813(8) 0.065(3) Uani 1 1 d . . . . .
H42 H 0.9645 0.2784 0.4928 0.078 Uiso 1 1 calc R U . . .
C43 C 0.8820(7) 0.3621(6) 0.4002(7) 0.062(3) Uani 1 1 d . . . . .
H43 H 0.8996 0.3075 0.3548 0.075 Uiso 1 1 calc R U . . .
C44 C 0.8156(6) 0.4628(6) 0.3875(6) 0.051(2) Uani 1 1 d . . . . .
H44 H 0.7889 0.4739 0.3322 0.061 Uiso 1 1 calc R U . . .
C45 C 0.8281(6) 0.5269(6) 0.5272(6) 0.0423(18) Uani 1 1 d . . . . .
C46 C 0.8001(6) 0.6132(6) 0.5946(6) 0.0435(19) Uani 1 1 d . . . . .
C47 C 0.135(2) 0.957(2) 0.530(2) 0.169(12) Uani 0.5 1 d D U P . .
H47A H 0.0884 0.9583 0.5977 0.253 Uiso 0.5 1 calc R U P . .
H47B H 0.1832 0.8860 0.5101 0.253 Uiso 0.5 1 calc R U P . .
H47C H 0.0873 0.9809 0.4870 0.253 Uiso 0.5 1 calc R U 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 O1 1.921(5) . ?
Cu1 N4 1.934(6) . ?
Cu1 N2 1.977(6) . ?
Cu1 N6 2.029(6) . ?
Cu1 N5 2.344(6) . ?
Br1 C2 1.911(8) . ?
O1 C5 1.315(8) . ?
Cl1 C11 1.326(7) . ?
N1 C10 1.376(9) . ?
N1 C11 1.371(9) . ?
C1 C2 1.364(11) . ?
C1 C6 1.403(10) . ?
O3 C47 1.443(10) . ?
Cu2 O2 1.934(5) . ?
Cu2 N10 1.939(6) . ?
Cu2 N8 2.000(6) . ?
Cu2 N11 2.017(6) . ?
Cu2 N12 2.322(6) . ?
Br2 C31 1.909(8) . ?
O2 C34 1.303(8) . ?
Cl2 C24 1.319(7) . ?
N2 C11 1.320(9) . ?
N2 C8 1.387(9) . ?
C2 C3 1.380(10) . ?
N3 C8 1.323(9) . ?
N3 N4 1.391(8) . ?
C3 C4 1.361(10) . ?
N4 C7 1.287(9) . ?
C4 C5 1.408(10) . ?
N5 C18 1.329(10) . ?
N5 C17 1.361(8) . ?
C5 C6 1.419(9) . ?
N6 C12 1.330(9) . ?
N6 C16 1.360(8) . ?
C6 C7 1.443(10) . ?
N7 C25 1.358(9) . ?
N7 C24 1.365(9) . ?
N8 C24 1.341(9) . ?
N8 C27 1.361(8) . ?
C8 C9 1.409(10) . ?
N9 C27 1.335(8) . ?
N9 N10 1.374(7) . ?
C9 C10 1.320(10) . ?
N10 C28 1.275(8) . ?
N11 C44 1.303(8) . ?
N11 C45 1.356(9) . ?
N12 C35 1.333(10) . ?
N12 C46 1.353(9) . ?
C12 C13 1.397(10) . ?
C13 C14 1.356(10) . ?
C14 C15 1.392(11) . ?
C15 C16 1.415(9) . ?
C15 C23 1.442(10) . ?
C16 C17 1.417(10) . ?
C17 C21 1.430(10) . ?
C18 C19 1.384(11) . ?
C19 C20 1.363(11) . ?
C20 C21 1.401(11) . ?
C21 C22 1.420(10) . ?
C22 C23 1.336(11) . ?
C25 C26 1.320(10) . ?
C26 C27 1.428(10) . ?
C28 C29 1.437(9) . ?
C29 C30 1.403(9) . ?
C29 C34 1.424(9) . ?
C30 C31 1.376(10) . ?
C31 C32 1.378(10) . ?
C32 C33 1.366(10) . ?
C33 C34 1.422(10) . ?
C35 C36 1.379(13) . ?
C36 C37 1.345(13) . ?
C37 C38 1.379(12) . ?
C38 C46 1.408(11) . ?
C38 C39 1.445(12) . ?
C39 C40 1.334(12) . ?
C40 C41 1.444(12) . ?
C41 C42 1.374(11) . ?
C41 C45 1.397(10) . ?
C42 C43 1.362(12) . ?
C43 C44 1.384(10) . ?
C45 C46 1.430(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N4 93.1(2) . . ?
O1 Cu1 N2 166.0(2) . . ?
N4 Cu1 N2 80.3(3) . . ?
O1 Cu1 N6 87.3(2) . . ?
N4 Cu1 N6 179.5(2) . . ?
N2 Cu1 N6 99.4(2) . . ?
O1 Cu1 N5 99.2(2) . . ?
N4 Cu1 N5 103.3(2) . . ?
N2 Cu1 N5 94.3(2) . . ?
N6 Cu1 N5 76.4(2) . . ?
C5 O1 Cu1 127.6(4) . . ?
C10 N1 C11 116.9(7) . . ?
C2 C1 C6 120.7(7) . . ?
O2 Cu2 N10 92.5(2) . . ?
O2 Cu2 N8 163.7(2) . . ?
N10 Cu2 N8 79.8(2) . . ?
O2 Cu2 N11 89.5(2) . . ?
N10 Cu2 N11 176.4(2) . . ?
N8 Cu2 N11 99.0(2) . . ?
O2 Cu2 N12 106.8(2) . . ?
N10 Cu2 N12 99.8(2) . . ?
N8 Cu2 N12 88.8(2) . . ?
N11 Cu2 N12 76.8(2) . . ?
C34 O2 Cu2 126.9(4) . . ?
C11 N2 C8 117.9(6) . . ?
C11 N2 Cu1 131.3(5) . . ?
C8 N2 Cu1 110.6(5) . . ?
C1 C2 C3 120.3(8) . . ?
C1 C2 Br1 119.7(6) . . ?
C3 C2 Br1 120.0(6) . . ?
C8 N3 N4 110.3(6) . . ?
C4 C3 C2 119.9(8) . . ?
C7 N4 N3 115.9(6) . . ?
C7 N4 Cu1 126.6(5) . . ?
N3 N4 Cu1 117.5(5) . . ?
C3 C4 C5 122.6(7) . . ?
C18 N5 C17 117.3(7) . . ?
C18 N5 Cu1 134.4(5) . . ?
C17 N5 Cu1 108.2(5) . . ?
O1 C5 C4 119.8(6) . . ?
O1 C5 C6 123.8(7) . . ?
C4 C5 C6 116.4(7) . . ?
C12 N6 C16 119.3(6) . . ?
C12 N6 Cu1 122.4(5) . . ?
C16 N6 Cu1 118.4(5) . . ?
C1 C6 C5 119.9(7) . . ?
C1 C6 C7 116.7(6) . . ?
C5 C6 C7 123.4(7) . . ?
C25 N7 C24 119.2(6) . . ?
N4 C7 C6 125.1(7) . . ?
C24 N8 C27 117.8(6) . . ?
C24 N8 Cu2 131.2(5) . . ?
C27 N8 Cu2 110.4(4) . . ?
N3 C8 N2 121.0(7) . . ?
N3 C8 C9 119.6(7) . . ?
N2 C8 C9 119.4(7) . . ?
C27 N9 N10 111.5(6) . . ?
C10 C9 C8 119.5(8) . . ?
C28 N10 N9 116.4(6) . . ?
C28 N10 Cu2 126.9(5) . . ?
N9 N10 Cu2 116.6(5) . . ?
C9 C10 N1 122.0(7) . . ?
C44 N11 C45 117.3(7) . . ?
C44 N11 Cu2 124.8(6) . . ?
C45 N11 Cu2 117.6(5) . . ?
Cl1 C11 N2 119.1(7) . . ?
Cl1 C11 N1 116.6(7) . . ?
N2 C11 N1 124.3(7) . . ?
C35 N12 C46 118.4(8) . . ?
C35 N12 Cu2 132.1(6) . . ?
C46 N12 Cu2 108.7(5) . . ?
N6 C12 C13 121.5(7) . . ?
C14 C13 C12 119.9(7) . . ?
C13 C14 C15 120.3(7) . . ?
C14 C15 C16 117.3(7) . . ?
C14 C15 C23 123.8(7) . . ?
C16 C15 C23 118.9(8) . . ?
N6 C16 C15 121.7(7) . . ?
N6 C16 C17 118.8(6) . . ?
C15 C16 C17 119.5(7) . . ?
N5 C17 C16 118.2(6) . . ?
N5 C17 C21 121.9(7) . . ?
C16 C17 C21 119.8(7) . . ?
N5 C18 C19 124.3(8) . . ?
C20 C19 C18 119.4(9) . . ?
C19 C20 C21 119.2(8) . . ?
C20 C21 C22 123.3(8) . . ?
C20 C21 C17 117.8(7) . . ?
C22 C21 C17 118.9(8) . . ?
C23 C22 C21 121.5(8) . . ?
C22 C23 C15 121.3(7) . . ?
Cl2 C24 N8 121.6(7) . . ?
Cl2 C24 N7 116.0(7) . . ?
N8 C24 N7 122.4(6) . . ?
C26 C25 N7 121.5(7) . . ?
C25 C26 C27 118.4(7) . . ?
N9 C27 N8 120.3(6) . . ?
N9 C27 C26 119.1(6) . . ?
N8 C27 C26 120.6(7) . . ?
N10 C28 C29 125.9(7) . . ?
C30 C29 C34 120.5(7) . . ?
C30 C29 C28 117.4(6) . . ?
C34 C29 C28 122.1(7) . . ?
C31 C30 C29 120.1(7) . . ?
C30 C31 C32 121.0(7) . . ?
C30 C31 Br2 119.0(6) . . ?
C32 C31 Br2 120.0(6) . . ?
C33 C32 C31 119.5(7) . . ?
C32 C33 C34 122.9(7) . . ?
O2 C34 C33 118.9(6) . . ?
O2 C34 C29 125.1(7) . . ?
C33 C34 C29 115.9(7) . . ?
N12 C35 C36 122.0(10) . . ?
C37 C36 C35 120.4(9) . . ?
C36 C37 C38 119.5(10) . . ?
C37 C38 C46 118.3(9) . . ?
C37 C38 C39 124.8(9) . . ?
C46 C38 C39 116.9(8) . . ?
C40 C39 C38 122.5(9) . . ?
C39 C40 C41 120.4(9) . . ?
C42 C41 C45 118.1(9) . . ?
C42 C41 C40 122.2(9) . . ?
C45 C41 C40 119.7(8) . . ?
C43 C42 C41 120.0(8) . . ?
C42 C43 C44 117.8(8) . . ?
N11 C44 C43 124.7(8) . . ?
N11 C45 C41 122.0(7) . . ?
N11 C45 C46 119.1(7) . . ?
C41 C45 C46 118.8(7) . . ?
N12 C46 C38 121.4(7) . . ?
N12 C46 C45 117.0(7) . . ?
C38 C46 C45 121.6(8) . . ?

_refine_diff_density_max         1.050
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.113

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 1949223'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C24 H16 Br2 Cl2 Co N6 O2), C H4 O'
_chemical_formula_sum            'C97 H68 Br8 Cl8 Co4 N24 O9'
_chemical_formula_weight         2872.27

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'
Br Br -0.2901 2.4595 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.2469(5)
_cell_length_b                   13.4344(6)
_cell_length_c                   20.9301(9)
_cell_angle_alpha                88.404(4)
_cell_angle_beta                 80.376(4)
_cell_angle_gamma                79.353(4)
_cell_volume                     2791.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5719
_cell_measurement_theta_min      3.6360
_cell_measurement_theta_max      27.6700

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_F_000             1414
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    3.703
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.71299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            18233
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.344
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.955
_reflns_number_total             9651
_reflns_number_gt                7293
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²+1.9142P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9651
_refine_ls_number_parameters     685
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1047
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.32411(5) 0.11996(4) 0.12467(2) 0.02957(14) Uani 1 1 d . . . . .
Br1 Br 0.10539(5) 0.27690(4) 0.02231(2) 0.05224(15) Uani 1 1 d . . . . .
Br2 Br 0.04674(7) -0.02414(5) 0.18353(3) 0.0824(2) Uani 1 1 d . . . . .
Cl1 Cl 0.74433(15) 0.48156(12) -0.03178(7) 0.0756(4) Uani 1 1 d . . . . .
Cl2 Cl 0.75557(16) -0.14962(12) 0.34639(7) 0.0767(4) Uani 1 1 d . . . . .
O1 O 0.4100(3) 0.2405(2) 0.13976(12) 0.0371(7) Uani 1 1 d . . . . .
O2 O 0.4766(3) -0.0009(2) 0.12980(12) 0.0394(7) Uani 1 1 d . . . . .
N4 N 0.2735(3) 0.1046(2) 0.22452(15) 0.0338(8) Uani 1 1 d . . . . .
N1 N 0.3998(3) 0.1337(2) 0.02761(14) 0.0310(7) Uani 1 1 d . . . . .
N6 N 0.1206(3) 0.2162(3) 0.14883(16) 0.0346(8) Uani 1 1 d . . . . .
C13 C 0.0380(4) 0.2680(3) 0.1118(2) 0.0388(10) Uani 1 1 d . . . . .
N5 N 0.1542(3) 0.1634(3) 0.25247(16) 0.0393(8) Uani 1 1 d . . . . .
H5 H 0.1312 0.1670 0.2939 0.047 Uiso 1 1 calc R U . . .
N3 N 0.2208(3) 0.0178(3) 0.07461(16) 0.0368(8) Uani 1 1 d . . . . .
C4 C 0.4832(4) 0.2939(3) 0.09886(18) 0.0302(8) Uani 1 1 d . . . . .
C18 C 0.3450(4) 0.0541(3) 0.26383(19) 0.0391(10) Uani 1 1 d . . . . .
H18 H 0.3106 0.0598 0.3079 0.047 Uiso 1 1 calc R U . . .
C17 C 0.0735(4) 0.2156(3) 0.2129(2) 0.0360(9) Uani 1 1 d . . . . .
N2 N 0.3688(4) 0.0643(3) -0.01235(16) 0.0400(8) Uani 1 1 d . . . . .
H2 H 0.4078 0.0575 -0.0521 0.048 Uiso 1 1 calc R U . . .
C2 C 0.5268(4) 0.3768(3) 0.1218(2) 0.0443(11) Uani 1 1 d . . . . .
H2A H 0.5033 0.3931 0.1656 0.053 Uiso 1 1 calc R U . . .
C12 C 0.1292(5) -0.0389(4) 0.0956(2) 0.0463(11) Uani 1 1 d . . . . .
C3 C 0.6412(4) 0.4112(3) 0.0175(2) 0.0449(11) Uani 1 1 d . . . . .
C20 C 0.5339(4) -0.0344(3) 0.17988(18) 0.0337(9) Uani 1 1 d . . . . .
C7 C 0.4765(4) 0.1937(3) -0.00008(19) 0.0374(10) Uani 1 1 d . . . . .
H7 H 0.5070 0.1853 -0.0444 0.045 Uiso 1 1 calc R U . . .
C19 C 0.4744(4) -0.0106(3) 0.24502(19) 0.0359(9) Uani 1 1 d . . . . .
C24 C 0.5420(5) -0.0496(3) 0.2954(2) 0.0436(11) Uani 1 1 d . . . . .
H24 H 0.5013 -0.0349 0.3380 0.052 Uiso 1 1 calc R U . . .
C16 C -0.0537(4) 0.2661(4) 0.2405(2) 0.0483(11) Uani 1 1 d . . . . .
H16 H -0.0824 0.2659 0.2850 0.058 Uiso 1 1 calc R U . . .
C5 C 0.5984(4) 0.3322(4) -0.0069(2) 0.0436(11) Uani 1 1 d . . . . .
H5A H 0.6230 0.3174 -0.0509 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6609(4) -0.0990(3) 0.1704(2) 0.0444(11) Uani 1 1 d . . . . .
H21 H 0.7013 -0.1184 0.1284 0.053 Uiso 1 1 calc R U . . .
C22 C 0.7271(5) -0.1341(4) 0.2204(2) 0.0493(11) Uani 1 1 d . . . . .
H22 H 0.8120 -0.1748 0.2119 0.059 Uiso 1 1 calc R U . . .
C1 C 0.6035(4) 0.4355(3) 0.0816(2) 0.0457(11) Uani 1 1 d . . . . .
H1 H 0.6293 0.4910 0.0983 0.055 Uiso 1 1 calc R U . . .
C6 C 0.5187(4) 0.2726(3) 0.03203(19) 0.0345(9) Uani 1 1 d . . . . .
C23 C 0.6679(5) -0.1092(3) 0.2830(2) 0.0456(11) Uani 1 1 d . . . . .
C9 C 0.2433(5) -0.0602(3) -0.0300(2) 0.0466(11) Uani 1 1 d . . . . .
H9 H 0.2841 -0.0663 -0.0732 0.056 Uiso 1 1 calc R U . . .
C8 C 0.2766(4) 0.0075(3) 0.01175(19) 0.0360(9) Uani 1 1 d . . . . .
C11 C 0.0894(5) -0.1066(4) 0.0582(2) 0.0558(13) Uani 1 1 d . . . . .
H11 H 0.0240 -0.1439 0.0754 0.067 Uiso 1 1 calc R U . . .
C14 C -0.0900(5) 0.3177(4) 0.1336(2) 0.0512(12) Uani 1 1 d . . . . .
H14 H -0.1442 0.3511 0.1052 0.061 Uiso 1 1 calc R U . . .
C10 C 0.1492(5) -0.1169(4) -0.0051(3) 0.0587(14) Uani 1 1 d . . . . .
H10 H 0.1257 -0.1628 -0.0316 0.070 Uiso 1 1 calc R U . . .
C15 C -0.1357(5) 0.3165(4) 0.1993(3) 0.0572(14) Uani 1 1 d . . . . .
H15 H -0.2221 0.3497 0.2160 0.069 Uiso 1 1 calc R U . . .
Br4 Br 0.38334(5) 0.21507(4) 0.50075(2) 0.05031(14) Uani 1 1 d . . . . .
Co2 Co 0.18673(5) 0.36068(4) 0.38510(2) 0.02851(14) Uani 1 1 d . . . . .
Br3 Br 0.47723(6) 0.49470(5) 0.32396(3) 0.0740(2) Uani 1 1 d . . . . .
Cl4 Cl -0.27323(13) 0.03545(11) 0.55271(7) 0.0642(4) Uani 1 1 d . . . . .
Cl3 Cl -0.17941(17) 0.61984(12) 0.13360(7) 0.0749(4) Uani 1 1 d . . . . .
O4 O 0.1083(3) 0.2334(2) 0.37634(12) 0.0366(6) Uani 1 1 d . U . . .
N9 N 0.2507(3) 0.3648(2) 0.28601(15) 0.0318(7) Uani 1 1 d . . . . .
N10 N 0.1005(3) 0.3625(2) 0.48192(14) 0.0304(7) Uani 1 1 d . . . . .
O3 O 0.0331(3) 0.4760(2) 0.37031(12) 0.0385(7) Uani 1 1 d . . . . .
N7 N 0.3882(3) 0.2614(2) 0.37075(16) 0.0334(8) Uani 1 1 d . . . . .
C37 C 0.4611(4) 0.2108(3) 0.4122(2) 0.0401(10) Uani 1 1 d . . . . .
N12 N 0.2867(3) 0.4707(3) 0.43131(15) 0.0350(8) Uani 1 1 d . . . . .
N8 N 0.3712(3) 0.3019(3) 0.26412(16) 0.0397(8) Uani 1 1 d . . . . .
H8 H 0.3998 0.2933 0.2233 0.048 Uiso 1 1 calc R U . . .
N11 N 0.1286(3) 0.4377(3) 0.51806(16) 0.0365(8) Uani 1 1 d . . . . .
H11A H 0.0856 0.4505 0.5567 0.044 Uiso 1 1 calc R U . . .
C25 C 0.3819(4) 0.5240(3) 0.4092(2) 0.0426(10) Uani 1 1 d . . . . .
C41 C 0.4437(4) 0.2537(3) 0.30794(19) 0.0350(9) Uani 1 1 d . . . . .
C36 C 0.0250(4) 0.1904(3) 0.41789(19) 0.0310(9) Uani 1 1 d . . . . .
C43 C 0.0626(4) 0.4790(3) 0.25379(18) 0.0360(9) Uani 1 1 d . . . . .
C35 C -0.0200(4) 0.1041(3) 0.3991(2) 0.0377(10) Uani 1 1 d . . . . .
H35 H 0.0105 0.0791 0.3573 0.045 Uiso 1 1 calc R U . . .
C46 C -0.1892(5) 0.6045(4) 0.2637(2) 0.0504(12) Uani 1 1 d . . . . .
H46 H -0.2739 0.6453 0.2671 0.060 Uiso 1 1 calc R U . . .
C31 C -0.0219(4) 0.2246(3) 0.48280(19) 0.0330(9) Uani 1 1 d . . . . .
C47 C -0.1380(5) 0.5703(4) 0.3184(2) 0.0458(11) Uani 1 1 d . . . . .
H47 H -0.1888 0.5897 0.3587 0.055 Uiso 1 1 calc R U . . .
C48 C -0.0114(4) 0.5068(3) 0.31590(18) 0.0330(9) Uani 1 1 d . . . . .
C32 C -0.1125(4) 0.1749(3) 0.5236(2) 0.0400(10) Uani 1 1 d . . . . .
H32 H -0.1435 0.1976 0.5660 0.048 Uiso 1 1 calc R U . . .
C44 C 0.0093(5) 0.5172(3) 0.1987(2) 0.0441(11) Uani 1 1 d . . . . .
H44 H 0.0596 0.5006 0.1579 0.053 Uiso 1 1 calc R U . . .
C34 C -0.1069(4) 0.0558(3) 0.4402(2) 0.0431(11) Uani 1 1 d . . . . .
H34 H -0.1326 -0.0020 0.4267 0.052 Uiso 1 1 calc R U . . .
C30 C 0.0182(4) 0.3073(3) 0.51122(19) 0.0345(9) Uani 1 1 d . . . . .
H30 H -0.0179 0.3226 0.5544 0.041 Uiso 1 1 calc R U . . .
C33 C -0.1559(4) 0.0939(3) 0.5022(2) 0.0415(10) Uani 1 1 d . . . . .
C40 C 0.5728(4) 0.1985(4) 0.2857(2) 0.0495(12) Uani 1 1 d . . . . .
H40 H 0.6078 0.1944 0.2417 0.059 Uiso 1 1 calc R U . . .
C29 C 0.2235(4) 0.4908(3) 0.49250(19) 0.0343(9) Uani 1 1 d . . . . .
C28 C 0.2544(5) 0.5654(3) 0.5307(2) 0.0428(10) Uani 1 1 d . . . . .
H28 H 0.2089 0.5783 0.5728 0.051 Uiso 1 1 calc R U . . .
C27 C 0.3510(5) 0.6175(4) 0.5051(2) 0.0517(12) Uani 1 1 d . . . . .
H27 H 0.3724 0.6670 0.5297 0.062 Uiso 1 1 calc R U . . .
C45 C -0.1141(5) 0.5779(4) 0.2033(2) 0.0465(11) Uani 1 1 d . . . . .
C39 C 0.6453(5) 0.1513(4) 0.3302(3) 0.0571(13) Uani 1 1 d . . . . .
H39 H 0.7324 0.1161 0.3170 0.069 Uiso 1 1 calc R U . . .
C26 C 0.4179(5) 0.5980(4) 0.4429(2) 0.0511(12) Uani 1 1 d . . . . .
H26 H 0.4847 0.6334 0.4244 0.061 Uiso 1 1 calc R U . . .
C38 C 0.5885(5) 0.1558(4) 0.3955(3) 0.0556(13) Uani 1 1 d . . . . .
H38 H 0.6353 0.1227 0.4267 0.067 Uiso 1 1 calc R U . . .
C42 C 0.1911(4) 0.4118(3) 0.24227(18) 0.0365(10) Uani 1 1 d . . . . .
H42 H 0.2338 0.4018 0.1995 0.044 Uiso 1 1 calc R U . . .
O5 O 0.2761(8) -0.2696(5) 0.2440(3) 0.0694(17) Uani 0.5 1 d D U P . .
H5B H 0.2480 -0.2088 0.2401 0.104 Uiso 0.5 1 d R U P . .
C49 C 0.172(3) -0.287(3) 0.2972(11) 0.292(18) Uani 0.5 1 d D U P . .
H49A H 0.1082 -0.2244 0.3057 0.438 Uiso 0.5 1 d R U P . .
H49B H 0.2109 -0.3064 0.3353 0.438 Uiso 0.5 1 d R U P . .
H49C H 0.1264 -0.3385 0.2861 0.438 Uiso 0.5 1 d R U 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
Co1 O1 2.036(3) . ?
Co1 O2 2.049(3) . ?
Co1 N1 2.066(3) . ?
Co1 N4 2.081(3) . ?
Co1 N6 2.228(3) . ?
Co1 N3 2.256(3) . ?
Br1 C13 1.893(4) . ?
Br2 C12 1.892(4) . ?
Cl1 C3 1.739(4) . ?
Cl2 C23 1.744(5) . ?
O1 C4 1.327(4) . ?
O2 C20 1.314(5) . ?
N4 C18 1.289(5) . ?
N4 N5 1.375(5) . ?
N1 C7 1.288(5) . ?
N1 N2 1.383(4) . ?
N6 C13 1.332(5) . ?
N6 C17 1.347(5) . ?
C13 C14 1.367(6) . ?
N5 C17 1.358(5) . ?
N5 H5 0.8600 . ?
N3 C12 1.328(5) . ?
N3 C8 1.344(5) . ?
C4 C2 1.398(5) . ?
C4 C6 1.409(5) . ?
C18 C19 1.445(6) . ?
C18 H18 0.9300 . ?
C17 C16 1.391(6) . ?
N2 C8 1.347(5) . ?
N2 H2 0.8600 . ?
C2 C1 1.385(6) . ?
C2 H2A 0.9300 . ?
C12 C11 1.374(6) . ?
C3 C5 1.362(6) . ?
C3 C1 1.365(7) . ?
C20 C21 1.411(6) . ?
C20 C19 1.416(5) . ?
C7 C6 1.438(6) . ?
C7 H7 0.9300 . ?
C19 C24 1.394(6) . ?
C24 C23 1.375(6) . ?
C24 H24 0.9300 . ?
C16 C15 1.380(7) . ?
C16 H16 0.9300 . ?
C5 C6 1.398(5) . ?
C5 H5A 0.9300 . ?
C21 C22 1.366(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.371(6) . ?
C22 H22 0.9300 . ?
C1 H1 0.9300 . ?
C9 C10 1.364(7) . ?
C9 C8 1.402(6) . ?
C9 H9 0.9300 . ?
C11 C10 1.363(7) . ?
C11 H11 0.9300 . ?
C14 C15 1.377(7) . ?
C14 H14 0.9300 . ?
C10 H10 0.9300 . ?
C15 H15 0.9300 . ?
Br4 C37 1.890(4) . ?
Co2 O4 2.044(3) . ?
Co2 O3 2.052(3) . ?
Co2 N10 2.070(3) . ?
Co2 N9 2.070(3) . ?
Co2 N7 2.220(3) . ?
Co2 N12 2.267(3) . ?
Br3 C25 1.899(4) . ?
Cl4 C33 1.749(4) . ?
Cl3 C45 1.742(4) . ?
O4 C36 1.314(4) . ?
N9 C42 1.274(5) . ?
N9 N8 1.377(5) . ?
N10 C30 1.293(5) . ?
N10 N11 1.378(4) . ?
O3 C48 1.324(5) . ?
N7 C37 1.330(5) . ?
N7 C41 1.341(5) . ?
C37 C38 1.369(6) . ?
N12 C25 1.329(5) . ?
N12 C29 1.346(5) . ?
N8 C41 1.353(5) . ?
N8 H8 0.8600 . ?
N11 C29 1.342(5) . ?
N11 H11A 0.8600 . ?
C25 C26 1.373(6) . ?
C41 C40 1.402(6) . ?
C36 C35 1.411(5) . ?
C36 C31 1.422(5) . ?
C43 C44 1.402(6) . ?
C43 C48 1.413(5) . ?
C43 C42 1.440(6) . ?
C35 C34 1.372(6) . ?
C35 H35 0.9300 . ?
C46 C47 1.372(6) . ?
C46 C45 1.383(7) . ?
C46 H46 0.9300 . ?
C31 C32 1.403(5) . ?
C31 C30 1.430(6) . ?
C47 C48 1.408(6) . ?
C47 H47 0.9300 . ?
C32 C33 1.362(6) . ?
C32 H32 0.9300 . ?
C44 C45 1.363(6) . ?
C44 H44 0.9300 . ?
C34 C33 1.385(6) . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C40 C39 1.357(7) . ?
C40 H40 0.9300 . ?
C29 C28 1.410(6) . ?
C28 C27 1.347(7) . ?
C28 H28 0.9300 . ?
C27 C26 1.375(7) . ?
C27 H27 0.9300 . ?
C39 C38 1.391(7) . ?
C39 H39 0.9300 . ?
C26 H26 0.9300 . ?
C38 H38 0.9300 . ?
C42 H42 0.9300 . ?
O5 C49 1.455(10) . ?
O5 H5B 0.8200 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O2 102.83(12) . . ?
O1 Co1 N1 86.53(11) . . ?
O2 Co1 N1 88.77(12) . . ?
O1 Co1 N4 89.26(11) . . ?
O2 Co1 N4 86.15(12) . . ?
N1 Co1 N4 172.54(13) . . ?
O1 Co1 N6 89.97(11) . . ?
O2 Co1 N6 157.89(12) . . ?
N1 Co1 N6 110.20(13) . . ?
N4 Co1 N6 75.93(13) . . ?
O1 Co1 N3 159.22(12) . . ?
O2 Co1 N3 88.37(12) . . ?
N1 Co1 N3 76.14(12) . . ?
N4 Co1 N3 109.14(12) . . ?
N6 Co1 N3 85.44(12) . . ?
C4 O1 Co1 131.1(2) . . ?
C20 O2 Co1 128.9(2) . . ?
C18 N4 N5 116.1(3) . . ?
C18 N4 Co1 128.1(3) . . ?
N5 N4 Co1 115.4(3) . . ?
C7 N1 N2 116.0(3) . . ?
C7 N1 Co1 129.4(3) . . ?
N2 N1 Co1 114.5(2) . . ?
C13 N6 C17 116.4(3) . . ?
C13 N6 Co1 131.9(3) . . ?
C17 N6 Co1 111.6(3) . . ?
N6 C13 C14 125.1(4) . . ?
N6 C13 Br1 117.3(3) . . ?
C14 C13 Br1 117.5(4) . . ?
C17 N5 N4 118.2(3) . . ?
C17 N5 H5 120.9 . . ?
N4 N5 H5 120.9 . . ?
C12 N3 C8 116.3(3) . . ?
C12 N3 Co1 133.4(3) . . ?
C8 N3 Co1 109.9(3) . . ?
O1 C4 C2 119.6(3) . . ?
O1 C4 C6 123.3(3) . . ?
C2 C4 C6 117.1(4) . . ?
N4 C18 C19 125.3(4) . . ?
N4 C18 H18 117.4 . . ?
C19 C18 H18 117.4 . . ?
N6 C17 N5 118.4(3) . . ?
N6 C17 C16 123.2(4) . . ?
N5 C17 C16 118.4(4) . . ?
C8 N2 N1 119.1(3) . . ?
C8 N2 H2 120.4 . . ?
N1 N2 H2 120.4 . . ?
C1 C2 C4 122.4(4) . . ?
C1 C2 H2A 118.8 . . ?
C4 C2 H2A 118.8 . . ?
N3 C12 C11 125.0(4) . . ?
N3 C12 Br2 117.2(3) . . ?
C11 C12 Br2 117.9(3) . . ?
C5 C3 C1 119.7(4) . . ?
C5 C3 Cl1 121.1(4) . . ?
C1 C3 Cl1 119.2(3) . . ?
O2 C20 C21 120.1(3) . . ?
O2 C20 C19 123.7(4) . . ?
C21 C20 C19 116.2(4) . . ?
N1 C7 C6 125.2(4) . . ?
N1 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
C24 C19 C20 120.0(4) . . ?
C24 C19 C18 116.1(4) . . ?
C20 C19 C18 123.9(4) . . ?
C23 C24 C19 121.1(4) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
C15 C16 C17 117.6(4) . . ?
C15 C16 H16 121.2 . . ?
C17 C16 H16 121.2 . . ?
C3 C5 C6 122.2(4) . . ?
C3 C5 H5A 118.9 . . ?
C6 C5 H5A 118.9 . . ?
C22 C21 C20 122.8(4) . . ?
C22 C21 H21 118.6 . . ?
C20 C21 H21 118.6 . . ?
C21 C22 C23 119.8(4) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C3 C1 C2 119.5(4) . . ?
C3 C1 H1 120.3 . . ?
C2 C1 H1 120.3 . . ?
C5 C6 C4 118.9(4) . . ?
C5 C6 C7 116.7(4) . . ?
C4 C6 C7 124.4(3) . . ?
C22 C23 C24 120.0(4) . . ?
C22 C23 Cl2 119.7(4) . . ?
C24 C23 Cl2 120.3(3) . . ?
C10 C9 C8 117.9(4) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
N3 C8 N2 118.8(3) . . ?
N3 C8 C9 122.8(4) . . ?
N2 C8 C9 118.4(4) . . ?
C10 C11 C12 117.6(4) . . ?
C10 C11 H11 121.2 . . ?
C12 C11 H11 121.2 . . ?
C13 C14 C15 117.3(5) . . ?
C13 C14 H14 121.3 . . ?
C15 C14 H14 121.3 . . ?
C11 C10 C9 120.5(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C14 C15 C16 120.3(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
O4 Co2 O3 103.30(12) . . ?
O4 Co2 N10 86.88(11) . . ?
O3 Co2 N10 88.11(12) . . ?
O4 Co2 N9 91.35(11) . . ?
O3 Co2 N9 86.11(12) . . ?
N10 Co2 N9 173.39(13) . . ?
O4 Co2 N7 87.21(12) . . ?
O3 Co2 N7 159.76(12) . . ?
N10 Co2 N7 109.97(13) . . ?
N9 Co2 N7 76.27(13) . . ?
O4 Co2 N12 157.65(12) . . ?
O3 Co2 N12 90.45(12) . . ?
N10 Co2 N12 75.90(12) . . ?
N9 Co2 N12 107.30(12) . . ?
N7 Co2 N12 85.46(12) . . ?
C36 O4 Co2 130.5(2) . . ?
C42 N9 N8 115.6(3) . . ?
C42 N9 Co2 129.5(3) . . ?
N8 N9 Co2 114.8(2) . . ?
C30 N10 N11 116.7(3) . . ?
C30 N10 Co2 128.6(3) . . ?
N11 N10 Co2 114.5(2) . . ?
C48 O3 Co2 129.6(2) . . ?
C37 N7 C41 116.3(3) . . ?
C37 N7 Co2 132.2(3) . . ?
C41 N7 Co2 111.6(3) . . ?
N7 C37 C38 124.9(4) . . ?
N7 C37 Br4 117.5(3) . . ?
C38 C37 Br4 117.5(4) . . ?
C25 N12 C29 116.2(3) . . ?
C25 N12 Co2 133.9(3) . . ?
C29 N12 Co2 109.6(2) . . ?
C41 N8 N9 118.9(3) . . ?
C41 N8 H8 120.6 . . ?
N9 N8 H8 120.6 . . ?
C29 N11 N10 119.6(3) . . ?
C29 N11 H11A 120.2 . . ?
N10 N11 H11A 120.2 . . ?
N12 C25 C26 125.5(4) . . ?
N12 C25 Br3 117.3(3) . . ?
C26 C25 Br3 117.1(3) . . ?
N7 C41 N8 118.0(3) . . ?
N7 C41 C40 123.2(4) . . ?
N8 C41 C40 118.7(4) . . ?
O4 C36 C35 119.8(3) . . ?
O4 C36 C31 123.4(3) . . ?
C35 C36 C31 116.7(3) . . ?
C44 C43 C48 119.3(4) . . ?
C44 C43 C42 116.3(4) . . ?
C48 C43 C42 124.4(4) . . ?
C34 C35 C36 122.6(4) . . ?
C34 C35 H35 118.7 . . ?
C36 C35 H35 118.7 . . ?
C47 C46 C45 119.7(4) . . ?
C47 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
C32 C31 C36 119.6(4) . . ?
C32 C31 C30 115.9(4) . . ?
C36 C31 C30 124.6(4) . . ?
C46 C47 C48 122.4(4) . . ?
C46 C47 H47 118.8 . . ?
C48 C47 H47 118.8 . . ?
O3 C48 C47 119.9(3) . . ?
O3 C48 C43 123.1(4) . . ?
C47 C48 C43 117.0(4) . . ?
C33 C32 C31 121.1(4) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C45 C44 C43 121.8(4) . . ?
C45 C44 H44 119.1 . . ?
C43 C44 H44 119.1 . . ?
C35 C34 C33 119.3(4) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
N10 C30 C31 125.4(4) . . ?
N10 C30 H30 117.3 . . ?
C31 C30 H30 117.3 . . ?
C32 C33 C34 120.6(4) . . ?
C32 C33 Cl4 120.5(3) . . ?
C34 C33 Cl4 118.9(3) . . ?
C39 C40 C41 118.2(4) . . ?
C39 C40 H40 120.9 . . ?
C41 C40 H40 120.9 . . ?
N11 C29 N12 118.9(3) . . ?
N11 C29 C28 119.1(4) . . ?
N12 C29 C28 122.1(4) . . ?
C27 C28 C29 118.8(4) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C28 C27 C26 120.3(4) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C44 C45 C46 119.8(4) . . ?
C44 C45 Cl3 120.3(4) . . ?
C46 C45 Cl3 119.9(4) . . ?
C40 C39 C38 119.6(4) . . ?
C40 C39 H39 120.2 . . ?
C38 C39 H39 120.2 . . ?
C25 C26 C27 117.1(4) . . ?
C25 C26 H26 121.5 . . ?
C27 C26 H26 121.5 . . ?
C37 C38 C39 117.7(5) . . ?
C37 C38 H38 121.2 . . ?
C39 C38 H38 121.2 . . ?
N9 C42 C43 125.2(4) . . ?
N9 C42 H42 117.4 . . ?
C43 C42 H42 117.4 . . ?
C49 O5 H5B 96.3 . . ?
O5 C49 H49A 108.2 . . ?
O5 C49 H49B 109.7 . . ?
H49A C49 H49B 109.5 . . ?
O5 C49 H49C 110.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5 O4 0.86 1.92 2.719(4) 153.2 .
N2 H2 O2 0.86 1.93 2.756(4) 161.0 2_655
C2 H2A N8 0.93 2.67 3.357(6) 131.3 .
C24 H24 Cl4 0.93 2.99 3.827(5) 151.3 2_556
C21 H21 N2 0.93 2.69 3.384(5) 132.1 2_655
N8 H8 O1 0.86 1.88 2.695(4) 156.6 .
N11 H11A O3 0.86 1.95 2.774(4) 159.9 2_566
O5 H5B Br2 0.82 3.25 3.987(8) 150.6 .

_refine_diff_density_max         0.902
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.083

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_17
_database_code_depnum_ccdc_archive 'CCDC 1949224'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C97 H68 Br16 Co4 N24 O9'
_chemical_formula_weight         3227.87

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.3047(5)
_cell_length_b                   13.6173(8)
_cell_length_c                   21.1711(8)
_cell_angle_alpha                89.131(4)
_cell_angle_beta                 80.042(4)
_cell_angle_gamma                78.773(5)
_cell_volume                     2869.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4979
_cell_measurement_theta_min      3.6850
_cell_measurement_theta_max      26.7810

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    6.202
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.44365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            18226
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.326
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             10024
_reflns_number_gt                6983
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0499P)²+2.9476P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10024
_refine_ls_number_parameters     697
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1197
_refine_ls_wR_factor_gt          0.1047
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br3 Br 0.38616(6) 0.72131(5) -0.00087(3) 0.04876(18) Uani 1 1 d . . . . .
Co1 Co 0.18759(7) 0.86125(5) -0.11493(3) 0.02714(18) Uani 1 1 d . . . . .
Co2 Co 0.32389(7) 0.61863(5) -0.37499(3) 0.02848(18) Uani 1 1 d . . . . .
Br7 Br 0.10170(7) 0.77181(5) -0.47489(3) 0.05177(19) Uani 1 1 d . . . . .
Br2 Br -0.28019(7) 0.53793(6) 0.05413(4) 0.0654(2) Uani 1 1 d . . . . .
Br6 Br 0.75155(8) 0.97912(6) -0.53238(4) 0.0705(2) Uani 1 1 d . . . . .
Br1 Br 0.47337(8) 0.99414(6) -0.17663(3) 0.0716(3) Uani 1 1 d . . . . .
Br8 Br 0.05348(9) 0.47424(7) -0.31562(3) 0.0800(3) Uani 1 1 d . . . . .
Br4 Br -0.18231(8) 1.11714(6) -0.36943(3) 0.0671(2) Uani 1 1 d . . . . .
Br5 Br 0.76791(9) 0.35293(6) -0.15294(4) 0.0725(3) Uani 1 1 d . . . . .
O3 O 0.4091(4) 0.7372(3) -0.35956(16) 0.0357(9) Uani 1 1 d . . . . .
O2 O 0.1104(4) 0.7365(3) -0.12449(16) 0.0347(9) Uani 1 1 d . . . . .
N7 N 0.1193(4) 0.7138(3) -0.3498(2) 0.0326(11) Uani 1 1 d . . . . .
N6 N 0.2515(4) 0.8623(3) -0.2131(2) 0.0306(11) Uani 1 1 d . . . . .
N3 N 0.1014(4) 0.8641(3) -0.01881(19) 0.0274(10) Uani 1 1 d . . . . .
O4 O 0.4779(4) 0.4991(3) -0.37107(17) 0.0400(10) Uani 1 1 d . U . . .
N4 N 0.3899(4) 0.7626(3) -0.1296(2) 0.0298(10) Uani 1 1 d . . . . .
O1 O 0.0330(4) 0.9751(3) -0.12880(16) 0.0356(9) Uani 1 1 d . . . . .
N8 N 0.1552(4) 0.6644(4) -0.2473(2) 0.0360(12) Uani 1 1 d . . . . .
H8A H 0.1329 0.6688 -0.2063 0.043 Uiso 1 1 calc R U . . .
N9 N 0.2752(4) 0.6054(3) -0.2759(2) 0.0308(11) Uani 1 1 d . . . . .
N5 N 0.3718(4) 0.7994(4) -0.2357(2) 0.0354(12) Uani 1 1 d . . . . .
H5 H 0.3996 0.7899 -0.2763 0.042 Uiso 1 1 calc R U . . .
N12 N 0.3985(4) 0.6318(3) -0.47137(18) 0.0301(11) Uani 1 1 d . . . . .
C13 C 0.4647(5) 0.7139(4) -0.0888(3) 0.0359(14) Uani 1 1 d . . . . .
C42 C 0.3474(6) 0.5577(4) -0.2375(3) 0.0364(14) Uani 1 1 d . . . . .
H42 H 0.3139 0.5658 -0.1938 0.044 Uiso 1 1 calc R U . . .
C1 C 0.3801(6) 1.0236(4) -0.0913(3) 0.0409(15) Uani 1 1 d . . . . .
C19 C 0.0622(5) 0.9761(4) -0.2446(2) 0.0331(13) Uani 1 1 d . . . . .
N1 N 0.2857(4) 0.9705(3) -0.0695(2) 0.0350(11) Uani 1 1 d . . . . .
C36 C 0.4804(5) 0.7903(4) -0.3997(2) 0.0300(12) Uani 1 1 d . . . . .
C12 C 0.0296(5) 0.6928(4) -0.0823(2) 0.0286(12) Uani 1 1 d . . . . .
N2 N 0.1296(4) 0.9384(4) 0.0176(2) 0.0356(11) Uani 1 1 d . . . . .
H2 H 0.0876 0.9507 0.0563 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0158(6) 0.6080(5) -0.1018(3) 0.0393(14) Uani 1 1 d . . . . .
H11 H 0.0142 0.5834 -0.1436 0.047 Uiso 1 1 calc R U . . .
C33 C 0.6379(6) 0.9049(5) -0.4801(3) 0.0415(15) Uani 1 1 d . . . . .
C9 C -0.1511(5) 0.5987(5) 0.0005(3) 0.0376(14) Uani 1 1 d . . . . .
N10 N 0.2229(5) 0.5170(4) -0.4243(2) 0.0370(12) Uani 1 1 d . . . . .
C8 C -0.1096(5) 0.6791(5) 0.0216(3) 0.0397(15) Uani 1 1 d . . . . .
H8 H -0.1418 0.7026 0.0634 0.048 Uiso 1 1 calc R U . . .
C37 C 0.0353(6) 0.7651(5) -0.3853(3) 0.0391(14) Uani 1 1 d . . . . .
C48 C 0.5361(6) 0.4656(4) -0.3221(2) 0.0323(13) Uani 1 1 d . . . . .
C25 C 0.1328(6) 0.4606(5) -0.4034(3) 0.0446(16) Uani 1 1 d . . . . .
C10 C -0.1023(6) 0.5609(5) -0.0611(3) 0.0421(15) Uani 1 1 d . . . . .
H10 H -0.1279 0.5041 -0.0749 0.051 Uiso 1 1 calc R U . . .
C7 C -0.0189(5) 0.7275(4) -0.0186(2) 0.0312(13) Uani 1 1 d . . . . .
C4 C 0.2545(6) 1.0641(5) 0.0299(3) 0.0426(15) Uani 1 1 d . . . . .
H4 H 0.2099 1.0769 0.0719 0.051 Uiso 1 1 calc R U . . .
C40 C -0.0549(6) 0.7670(5) -0.2579(3) 0.0472(17) Uani 1 1 d . . . . .
H40 H -0.0827 0.7686 -0.2137 0.057 Uiso 1 1 calc R U . . .
C23 C -0.1356(6) 1.0694(5) -0.1798(3) 0.0457(16) Uani 1 1 d . . . . .
H23 H -0.1854 1.0914 -0.1399 0.055 Uiso 1 1 calc R U . . .
C18 C 0.1902(6) 0.9077(4) -0.2563(2) 0.0331(13) Uani 1 1 d . . . . .
H18 H 0.2319 0.8955 -0.2988 0.040 Uiso 1 1 calc R U . . .
N11 N 0.3677(5) 0.5639(4) -0.5112(2) 0.0392(12) Uani 1 1 d . . . . .
H11A H 0.4059 0.5577 -0.5508 0.047 Uiso 1 1 calc R U . . .
C22 C -0.1876(6) 1.1023(5) -0.2338(3) 0.0454(16) Uani 1 1 d . . . . .
H22 H -0.2724 1.1430 -0.2300 0.054 Uiso 1 1 calc R U . . .
C5 C 0.2224(5) 0.9910(4) -0.0075(2) 0.0308(13) Uani 1 1 d . . . . .
C35 C 0.5241(6) 0.8727(4) -0.3765(3) 0.0394(15) Uani 1 1 d . . . . .
H35 H 0.5001 0.8894 -0.3330 0.047 Uiso 1 1 calc R U . . .
C20 C 0.0100(6) 1.0128(4) -0.2990(3) 0.0382(14) Uani 1 1 d . . . . .
H20 H 0.0598 0.9949 -0.3396 0.046 Uiso 1 1 calc R U . . .
C17 C 0.4464(5) 0.7525(4) -0.1925(3) 0.0324(13) Uani 1 1 d . . . . .
C47 C 0.6623(6) 0.4017(5) -0.3322(3) 0.0444(16) Uani 1 1 d . . . . .
H47 H 0.7020 0.3813 -0.3739 0.053 Uiso 1 1 calc R U . . .
C30 C 0.4753(5) 0.6906(4) -0.4988(2) 0.0348(14) Uani 1 1 d . . . . .
H30 H 0.5064 0.6814 -0.5427 0.042 Uiso 1 1 calc R U . . .
C24 C -0.0109(5) 1.0041(4) -0.1822(2) 0.0310(13) Uani 1 1 d . . . . .
C32 C 0.5962(6) 0.8270(5) -0.5051(3) 0.0412(15) Uani 1 1 d . . . . .
H32 H 0.6215 0.8120 -0.5487 0.049 Uiso 1 1 calc R U . . .
C41 C 0.0729(5) 0.7156(4) -0.2862(3) 0.0346(14) Uani 1 1 d . . . . .
C21 C -0.1127(6) 1.0743(4) -0.2935(3) 0.0410(15) Uani 1 1 d . . . . .
C3 C 0.3494(6) 1.1154(5) 0.0050(3) 0.0496(17) Uani 1 1 d . . . . .
H3 H 0.3699 1.1645 0.0296 0.060 Uiso 1 1 calc R U . . .
C45 C 0.6704(6) 0.3946(5) -0.2208(3) 0.0429(15) Uani 1 1 d . . . . .
C31 C 0.5162(5) 0.7690(4) -0.4667(2) 0.0311(13) Uani 1 1 d . . . . .
C44 C 0.5456(6) 0.4551(4) -0.2080(3) 0.0389(15) Uani 1 1 d . . . . .
H44 H 0.5059 0.4716 -0.1657 0.047 Uiso 1 1 calc R U . . .
C28 C 0.2426(6) 0.4406(5) -0.5289(3) 0.0456(16) Uani 1 1 d . . . . .
H28 H 0.2821 0.4347 -0.5720 0.055 Uiso 1 1 calc R U . . .
C38 C -0.0929(6) 0.8146(5) -0.3639(3) 0.0495(17) Uani 1 1 d . . . . .
H38 H -0.1479 0.8464 -0.3916 0.059 Uiso 1 1 calc R U . . .
C29 C 0.2775(6) 0.5073(4) -0.4879(3) 0.0356(14) Uani 1 1 d . . . . .
C43 C 0.4776(6) 0.4919(4) -0.2567(2) 0.0322(13) Uani 1 1 d . . . . .
C16 C 0.5742(6) 0.6991(5) -0.2140(3) 0.0434(16) Uani 1 1 d . . . . .
H16 H 0.6096 0.6944 -0.2576 0.052 Uiso 1 1 calc R U . . .
C26 C 0.0924(7) 0.3946(5) -0.4406(3) 0.0569(19) Uani 1 1 d . . . . .
H26 H 0.0282 0.3577 -0.4234 0.068 Uiso 1 1 calc R U . . .
C39 C -0.1365(6) 0.8145(5) -0.2974(3) 0.0543(18) Uani 1 1 d . . . . .
H39 H -0.2229 0.8476 -0.2801 0.065 Uiso 1 1 calc R U . . .
C6 C 0.0201(5) 0.8106(4) 0.0098(2) 0.0349(14) Uani 1 1 d . . . . .
H6 H -0.0169 0.8267 0.0525 0.042 Uiso 1 1 calc R U . . .
C15 C 0.6471(7) 0.6536(5) -0.1707(3) 0.0560(19) Uani 1 1 d . . . . .
H15 H 0.7340 0.6181 -0.1843 0.067 Uiso 1 1 calc R U . . .
C27 C 0.1511(7) 0.3850(5) -0.5050(3) 0.0545(18) Uani 1 1 d . . . . .
H27 H 0.1272 0.3403 -0.5316 0.065 Uiso 1 1 calc R U . . .
C34 C 0.6010(6) 0.9293(5) -0.4158(3) 0.0453(16) Uani 1 1 d . . . . .
H34 H 0.6276 0.9834 -0.3990 0.054 Uiso 1 1 calc R U . . .
C46 C 0.7301(6) 0.3677(5) -0.2831(3) 0.0460(16) Uani 1 1 d . . . . .
H46 H 0.8150 0.3271 -0.2919 0.055 Uiso 1 1 calc R U . . .
C2 C 0.4174(6) 1.0950(5) -0.0578(3) 0.0520(17) Uani 1 1 d . . . . .
H2A H 0.4849 1.1286 -0.0759 0.062 Uiso 1 1 calc R U . . .
C14 C 0.5918(6) 0.6600(5) -0.1058(3) 0.0517(17) Uani 1 1 d . . . . .
H14 H 0.6397 0.6288 -0.0752 0.062 Uiso 1 1 calc R U . . .
O5 O 0.2780(9) 0.2260(7) -0.2557(4) 0.061(2) Uani 0.5 1 d D U P . .
H5B H 0.308(3) 0.249(5) -0.2251(11) 0.091 Uiso 0.5 1 d D U P . .
C49 C 0.413(2) 0.231(3) -0.2940(14) 0.098(12) Uani 0.25 1 d D U P . .
H49A H 0.4019 0.2690 -0.3320 0.147 Uiso 0.25 1 calc R U P . .
H49B H 0.4622 0.2636 -0.2687 0.147 Uiso 0.25 1 calc R U P . .
H49C H 0.4622 0.1649 -0.3058 0.147 Uiso 0.25 1 calc R U P . .
C50 C 0.160(2) 0.207(2) -0.2071(11) 0.060(7) Uani 0.25 1 d D U P . .
H50A H 0.0778 0.2383 -0.2209 0.090 Uiso 0.25 1 calc R U P . .
H50B H 0.1634 0.1366 -0.2033 0.090 Uiso 0.25 1 calc R U P . .
H50C H 0.1634 0.2353 -0.1662 0.090 Uiso 0.25 1 calc R U 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
Br3 C13 1.894(5) . ?
Co1 O2 2.038(4) . ?
Co1 O1 2.053(4) . ?
Co1 N6 2.069(4) . ?
Co1 N3 2.072(4) . ?
Co1 N4 2.224(4) . ?
Co1 N1 2.263(5) . ?
Co2 O3 2.038(4) . ?
Co2 O4 2.052(4) . ?
Co2 N12 2.071(4) . ?
Co2 N9 2.083(4) . ?
Co2 N7 2.231(5) . ?
Co2 N10 2.251(5) . ?
Br7 C37 1.910(6) . ?
Br2 C9 1.903(5) . ?
Br6 C33 1.897(6) . ?
Br1 C1 1.902(6) . ?
Br8 C25 1.893(6) . ?
Br4 C21 1.909(6) . ?
Br5 C45 1.910(6) . ?
O3 C36 1.325(6) . ?
O2 C12 1.329(6) . ?
N7 C37 1.333(7) . ?
N7 C41 1.346(6) . ?
N6 C18 1.284(7) . ?
N6 N5 1.376(6) . ?
N3 C6 1.285(7) . ?
N3 N2 1.385(6) . ?
O4 C48 1.318(6) . ?
N4 C13 1.338(7) . ?
N4 C17 1.355(6) . ?
O1 C24 1.316(6) . ?
N8 C41 1.371(7) . ?
N8 N9 1.382(6) . ?
N9 C42 1.282(7) . ?
N5 C17 1.368(7) . ?
N12 C30 1.295(7) . ?
N12 N11 1.379(6) . ?
C13 C14 1.362(8) . ?
C42 C43 1.457(8) . ?
C1 N1 1.338(7) . ?
C1 C2 1.364(8) . ?
C19 C20 1.399(8) . ?
C19 C24 1.422(7) . ?
C19 C18 1.444(8) . ?
N1 C5 1.368(6) . ?
C36 C35 1.411(8) . ?
C36 C31 1.422(7) . ?
C12 C7 1.410(7) . ?
C12 C11 1.419(8) . ?
N2 C5 1.337(7) . ?
C11 C10 1.374(8) . ?
C33 C32 1.366(8) . ?
C33 C34 1.375(8) . ?
C9 C8 1.358(8) . ?
C9 C10 1.382(8) . ?
N10 C25 1.332(7) . ?
N10 C29 1.364(7) . ?
C8 C7 1.406(7) . ?
C37 C38 1.364(8) . ?
C48 C47 1.401(8) . ?
C48 C43 1.431(7) . ?
C25 C26 1.372(8) . ?
C7 C6 1.443(8) . ?
C4 C3 1.341(8) . ?
C4 C5 1.404(8) . ?
C40 C39 1.357(9) . ?
C40 C41 1.402(8) . ?
C23 C22 1.377(8) . ?
C23 C24 1.407(8) . ?
N11 C29 1.346(7) . ?
C22 C21 1.379(8) . ?
C35 C34 1.381(8) . ?
C20 C21 1.361(8) . ?
C17 C16 1.378(8) . ?
C47 C46 1.375(8) . ?
C30 C31 1.441(8) . ?
C32 C31 1.401(7) . ?
C3 C2 1.396(8) . ?
C45 C44 1.371(8) . ?
C45 C46 1.380(8) . ?
C44 C43 1.379(8) . ?
C28 C27 1.349(9) . ?
C28 C29 1.403(8) . ?
C38 C39 1.401(9) . ?
C16 C15 1.352(9) . ?
C26 C27 1.389(9) . ?
C15 C14 1.391(9) . ?
O5 C49 1.501(10) . ?
O5 C50 1.511(10) . ?

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
O2 Co1 O1 102.72(16) . . ?
O2 Co1 N6 90.40(15) . . ?
O1 Co1 N6 86.39(15) . . ?
O2 Co1 N3 87.10(15) . . ?
O1 Co1 N3 88.25(15) . . ?
N6 Co1 N3 173.44(17) . . ?
O2 Co1 N4 87.62(15) . . ?
O1 Co1 N4 159.95(15) . . ?
N6 Co1 N4 76.28(17) . . ?
N3 Co1 N4 109.64(16) . . ?
O2 Co1 N1 158.38(16) . . ?
O1 Co1 N1 90.52(16) . . ?
N6 Co1 N1 107.63(17) . . ?
N3 Co1 N1 76.17(16) . . ?
N4 Co1 N1 85.29(16) . . ?
O3 Co2 O4 102.31(16) . . ?
O3 Co2 N12 86.51(15) . . ?
O4 Co2 N12 89.02(16) . . ?
O3 Co2 N9 88.57(15) . . ?
O4 Co2 N9 86.11(16) . . ?
N12 Co2 N9 172.20(18) . . ?
O3 Co2 N7 90.54(16) . . ?
O4 Co2 N7 157.78(16) . . ?
N12 Co2 N7 110.02(17) . . ?
N9 Co2 N7 76.05(17) . . ?
O3 Co2 N10 159.70(16) . . ?
O4 Co2 N10 88.27(17) . . ?
N12 Co2 N10 76.27(17) . . ?
N9 Co2 N10 109.63(17) . . ?
N7 Co2 N10 85.43(16) . . ?
C36 O3 Co2 131.4(3) . . ?
C12 O2 Co1 130.1(3) . . ?
C37 N7 C41 115.5(5) . . ?
C37 N7 Co2 132.5(4) . . ?
C41 N7 Co2 111.9(4) . . ?
C18 N6 N5 115.3(4) . . ?
C18 N6 Co1 129.1(3) . . ?
N5 N6 Co1 115.4(3) . . ?
C6 N3 N2 116.8(4) . . ?
C6 N3 Co1 128.5(4) . . ?
N2 N3 Co1 114.6(3) . . ?
C48 O4 Co2 129.4(3) . . ?
C13 N4 C17 115.6(4) . . ?
C13 N4 Co1 132.5(3) . . ?
C17 N4 Co1 111.8(4) . . ?
C24 O1 Co1 129.3(3) . . ?
C41 N8 N9 118.1(4) . . ?
C42 N9 N8 115.7(4) . . ?
C42 N9 Co2 128.6(3) . . ?
N8 N9 Co2 115.4(3) . . ?
C17 N5 N6 118.7(4) . . ?
C30 N12 N11 115.9(4) . . ?
C30 N12 Co2 129.4(4) . . ?
N11 N12 Co2 114.6(3) . . ?
N4 C13 C14 125.1(5) . . ?
N4 C13 Br3 116.9(4) . . ?
C14 C13 Br3 118.0(5) . . ?
N9 C42 C43 125.3(5) . . ?
N1 C1 C2 126.2(5) . . ?
N1 C1 Br1 116.6(4) . . ?
C2 C1 Br1 117.2(5) . . ?
C20 C19 C24 120.5(5) . . ?
C20 C19 C18 116.1(5) . . ?
C24 C19 C18 123.3(5) . . ?
C1 N1 C5 115.7(5) . . ?
C1 N1 Co1 134.4(4) . . ?
C5 N1 Co1 109.6(4) . . ?
O3 C36 C35 120.0(5) . . ?
O3 C36 C31 123.2(5) . . ?
C35 C36 C31 116.8(5) . . ?
O2 C12 C7 123.9(5) . . ?
O2 C12 C11 119.3(5) . . ?
C7 C12 C11 116.8(5) . . ?
C5 N2 N3 119.8(4) . . ?
C10 C11 C12 122.3(5) . . ?
C32 C33 C34 120.4(5) . . ?
C32 C33 Br6 120.9(4) . . ?
C34 C33 Br6 118.6(5) . . ?
C8 C9 C10 120.4(5) . . ?
C8 C9 Br2 120.8(4) . . ?
C10 C9 Br2 118.8(5) . . ?
C25 N10 C29 116.2(5) . . ?
C25 N10 Co2 133.5(4) . . ?
C29 N10 Co2 110.0(4) . . ?
C9 C8 C7 121.5(5) . . ?
N7 C37 C38 126.6(5) . . ?
N7 C37 Br7 116.8(4) . . ?
C38 C37 Br7 116.6(5) . . ?
O4 C48 C47 120.5(5) . . ?
O4 C48 C43 123.4(5) . . ?
C47 C48 C43 116.2(5) . . ?
N10 C25 C26 125.1(6) . . ?
N10 C25 Br8 117.1(4) . . ?
C26 C25 Br8 117.8(5) . . ?
C11 C10 C9 119.4(6) . . ?
C8 C7 C12 119.6(5) . . ?
C8 C7 C6 116.3(5) . . ?
C12 C7 C6 124.1(5) . . ?
C3 C4 C5 120.0(6) . . ?
C39 C40 C41 117.5(6) . . ?
C22 C23 C24 123.1(5) . . ?
N6 C18 C19 125.7(5) . . ?
C29 N11 N12 119.6(4) . . ?
C23 C22 C21 119.3(6) . . ?
N2 C5 N1 118.5(5) . . ?
N2 C5 C4 120.0(5) . . ?
N1 C5 C4 121.4(5) . . ?
C34 C35 C36 122.5(5) . . ?
C21 C20 C19 121.0(5) . . ?
N4 C17 N5 117.3(5) . . ?
N4 C17 C16 123.2(6) . . ?
N5 C17 C16 119.5(5) . . ?
C46 C47 C48 123.0(5) . . ?
N12 C30 C31 125.1(5) . . ?
O1 C24 C23 120.2(5) . . ?
O1 C24 C19 124.1(5) . . ?
C23 C24 C19 115.6(5) . . ?
C33 C32 C31 121.7(5) . . ?
N7 C41 N8 118.1(5) . . ?
N7 C41 C40 123.5(6) . . ?
N8 C41 C40 118.4(5) . . ?
C20 C21 C22 120.4(5) . . ?
C20 C21 Br4 119.1(4) . . ?
C22 C21 Br4 120.5(5) . . ?
C4 C3 C2 119.9(6) . . ?
C44 C45 C46 120.3(6) . . ?
C44 C45 Br5 120.4(4) . . ?
C46 C45 Br5 119.2(5) . . ?
C32 C31 C36 119.2(5) . . ?
C32 C31 C30 116.7(5) . . ?
C36 C31 C30 124.2(5) . . ?
C45 C44 C43 121.4(5) . . ?
C27 C28 C29 119.0(6) . . ?
C37 C38 C39 115.7(6) . . ?
N11 C29 N10 118.2(5) . . ?
N11 C29 C28 119.7(5) . . ?
N10 C29 C28 122.1(5) . . ?
C44 C43 C48 120.0(5) . . ?
C44 C43 C42 116.5(5) . . ?
C48 C43 C42 123.5(5) . . ?
C15 C16 C17 118.9(6) . . ?
C25 C26 C27 117.5(6) . . ?
C40 C39 C38 121.1(6) . . ?
N3 C6 C7 125.6(5) . . ?
C16 C15 C14 119.8(6) . . ?
C28 C27 C26 120.0(6) . . ?
C33 C34 C35 119.3(6) . . ?
C47 C46 C45 119.1(6) . . ?
C1 C2 C3 116.8(6) . . ?
C13 C14 C15 117.3(6) . . ?
C49 O5 C50 167.4(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8A O2 0.86 1.93 2.725(5) 153.0 .
N5 H5 O3 0.86 1.89 2.707(5) 157.4 .
N2 H2 O1 0.86 1.95 2.773(5) 158.6 2_575
N11 H11A O4 0.86 1.94 2.763(5) 160.3 2_664

_refine_diff_density_max         1.485
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.102

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_co
_database_code_depnum_ccdc_archive 'CCDC 1949221'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' 2(C24 H16 Cl4 Co N6 O2), 0.5(H2 O) '
_chemical_formula_sum            'C48 H33 Cl8 Co2 N12 O4.50'
_chemical_formula_weight         1251.32

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.0897(9)
_cell_length_b                   12.3484(7)
_cell_length_c                   13.2790(9)
_cell_angle_alpha                63.242(6)
_cell_angle_beta                 71.896(7)
_cell_angle_gamma                78.893(6)
_cell_volume                     1401.44(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3528
_cell_measurement_theta_min      3.8570
_cell_measurement_theta_max      28.9740

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            RED
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_F_000             631
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.027
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.539
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            8796
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.370
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4975
_reflns_number_gt                4294
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+6.5667P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4975
_refine_ls_number_parameters     340
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1418
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.93292(6) 0.24976(5) 0.01312(5) 0.03281(18) Uani 1 1 d . . . . .
Cl2 Cl 0.64105(14) 0.20999(12) 0.25993(11) 0.0533(3) Uani 1 1 d . . . . .
Cl1 Cl 0.67791(19) 0.32957(13) -0.15794(15) 0.0732(5) Uani 1 1 d . . . . .
Cl4 Cl 1.2219(2) 0.04588(17) 0.52504(14) 0.0808(5) Uani 1 1 d . . . . .
Cl3 Cl 1.5116(2) 0.2871(2) -0.50457(17) 0.1054(8) Uani 1 1 d . . . . .
O2 O 1.0447(3) 0.1128(3) 0.1178(3) 0.0404(7) Uani 1 1 d . . . . .
N4 N 0.9256(4) 0.3418(3) 0.1123(3) 0.0335(8) Uani 1 1 d . . . . .
N3 N 0.9600(4) 0.1608(3) -0.0930(3) 0.0356(8) Uani 1 1 d . . . . .
O1 O 1.0897(4) 0.3564(3) -0.1134(3) 0.0440(8) Uani 1 1 d . . . . .
N6 N 0.7756(4) 0.4050(3) -0.0405(3) 0.0382(9) Uani 1 1 d . . . . .
N5 N 0.8562(4) 0.4551(3) 0.0776(3) 0.0415(9) Uani 1 1 d . . . . .
H5 H 0.8604 0.5045 0.1057 0.050 Uiso 1 1 calc R U . . .
N2 N 0.8667(4) 0.0735(3) -0.0533(4) 0.0422(9) Uani 1 1 d . . . . .
H2 H 0.8765 0.0271 -0.0882 0.051 Uiso 1 1 calc R U . . .
N1 N 0.7548(4) 0.1323(3) 0.0961(3) 0.0366(8) Uani 1 1 d . . . . .
C20 C 1.0804(4) 0.1015(4) 0.2098(4) 0.0344(9) Uani 1 1 d . . . . .
C18 C 0.9805(5) 0.3102(4) 0.1978(4) 0.0401(11) Uani 1 1 d . . . . .
H18 H 0.9725 0.3665 0.2283 0.048 Uiso 1 1 calc R U . . .
C6 C 1.0557(5) 0.1718(4) -0.1866(4) 0.0426(11) Uani 1 1 d . . . . .
H6 H 1.0532 0.1226 -0.2222 0.051 Uiso 1 1 calc R U . . .
C17 C 0.7813(5) 0.4872(4) -0.0017(4) 0.0371(10) Uani 1 1 d . . . . .
C4 C 0.7595(5) 0.0621(4) 0.0414(4) 0.0402(11) Uani 1 1 d . . . . .
C16 C 0.7121(5) 0.6029(4) -0.0388(5) 0.0472(12) Uani 1 1 d . . . . .
H16 H 0.7183 0.6578 -0.0106 0.057 Uiso 1 1 calc R U . . .
C5 C 0.6468(5) 0.1195(4) 0.1893(4) 0.0439(11) Uani 1 1 d . . . . .
C13 C 0.6948(5) 0.4382(4) -0.1144(4) 0.0461(12) Uani 1 1 d . . . . .
C23 C 1.1646(5) 0.0674(5) 0.4057(4) 0.0466(12) Uani 1 1 d . . . . .
C21 C 1.1481(5) -0.0078(4) 0.2746(5) 0.0458(12) Uani 1 1 d . . . . .
H21 H 1.1658 -0.0709 0.2512 0.055 Uiso 1 1 calc R U . . .
C19 C 1.0534(5) 0.1946(4) 0.2503(4) 0.0359(10) Uani 1 1 d . . . . .
C12 C 1.1829(5) 0.3381(4) -0.2006(4) 0.0421(11) Uani 1 1 d . . . . .
C7 C 1.1666(5) 0.2536(4) -0.2412(4) 0.0424(11) Uani 1 1 d . . . . .
C24 C 1.0985(5) 0.1741(4) 0.3478(4) 0.0461(12) Uani 1 1 d . . . . .
H24 H 1.0826 0.2354 0.3734 0.055 Uiso 1 1 calc R U . . .
C22 C 1.1892(5) -0.0256(5) 0.3706(5) 0.0489(12) Uani 1 1 d . . . . .
H22 H 1.2329 -0.0993 0.4113 0.059 Uiso 1 1 calc R U . . .
C11 C 1.3056(6) 0.4022(5) -0.2572(5) 0.0583(15) Uani 1 1 d . . . . .
H11 H 1.3197 0.4568 -0.2315 0.070 Uiso 1 1 calc R U . . .
C8 C 1.2694(6) 0.2431(5) -0.3370(5) 0.0569(14) Uani 1 1 d . . . . .
H8 H 1.2572 0.1904 -0.3657 0.068 Uiso 1 1 calc R U . . .
C3 C 0.6571(6) -0.0190(5) 0.0774(5) 0.0574(14) Uani 1 1 d . . . . .
H3 H 0.6626 -0.0660 0.0375 0.069 Uiso 1 1 calc R U . . .
C14 C 0.6242(6) 0.5494(5) -0.1560(5) 0.0584(14) Uani 1 1 d . . . . .
H14 H 0.5708 0.5679 -0.2083 0.070 Uiso 1 1 calc R U . . .
C10 C 1.4052(7) 0.3877(6) -0.3486(5) 0.0671(17) Uani 1 1 d . . . . .
H10 H 1.4851 0.4313 -0.3832 0.081 Uiso 1 1 calc R U . . .
C15 C 0.6358(6) 0.6328(5) -0.1168(5) 0.0571(14) Uani 1 1 d . . . . .
H15 H 0.5912 0.7098 -0.1441 0.069 Uiso 1 1 calc R U . . .
C2 C 0.5485(6) -0.0274(5) 0.1727(6) 0.0698(18) Uani 1 1 d . . . . .
H2A H 0.4787 -0.0801 0.1978 0.084 Uiso 1 1 calc R U . . .
C1 C 0.5426(6) 0.0424(5) 0.2315(6) 0.0620(15) Uani 1 1 d . . . . .
H1 H 0.4706 0.0370 0.2972 0.074 Uiso 1 1 calc R U . . .
C9 C 1.3862(7) 0.3079(5) -0.3891(5) 0.0646(16) Uani 1 1 d . . . . .
O1W O 1.0000 0.5000 -0.5000 0.138(6) Uani 0.5 2 d S U P . .
H1WA H 0.9269 0.5293 -0.4641 0.207 Uiso 0.25 1 d R U P . .
H1WB H 1.0649 0.5473 -0.5185 0.207 Uiso 0.25 1 d R U 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
Co1 O2 2.046(3) . ?
Co1 O1 2.054(3) . ?
Co1 N4 2.070(3) . ?
Co1 N3 2.075(3) . ?
Co1 N1 2.209(4) . ?
Co1 N6 2.237(4) . ?
Cl2 C5 1.737(5) . ?
Cl1 C13 1.736(5) . ?
Cl4 C23 1.746(5) . ?
Cl3 C9 1.744(5) . ?
O2 C20 1.319(5) . ?
N4 C18 1.288(6) . ?
N4 N5 1.379(5) . ?
N3 C6 1.285(6) . ?
N3 N2 1.378(5) . ?
O1 C12 1.324(5) . ?
N6 C13 1.342(6) . ?
N6 C17 1.345(5) . ?
N5 C17 1.357(6) . ?
N5 H5 0.8600 . ?
N2 C4 1.352(6) . ?
N2 H2 0.8600 . ?
N1 C5 1.340(6) . ?
N1 C4 1.346(6) . ?
C20 C21 1.412(6) . ?
C20 C19 1.426(6) . ?
C18 C19 1.443(6) . ?
C18 H18 0.9300 . ?
C6 C7 1.439(7) . ?
C6 H6 0.9300 . ?
C17 C16 1.402(6) . ?
C4 C3 1.400(7) . ?
C16 C15 1.358(7) . ?
C16 H16 0.9300 . ?
C5 C1 1.366(7) . ?
C13 C14 1.373(7) . ?
C23 C24 1.357(7) . ?
C23 C22 1.377(7) . ?
C21 C22 1.373(7) . ?
C21 H21 0.9300 . ?
C19 C24 1.405(6) . ?
C12 C11 1.410(7) . ?
C12 C7 1.427(6) . ?
C7 C8 1.410(7) . ?
C24 H24 0.9300 . ?
C22 H22 0.9300 . ?
C11 C10 1.373(7) . ?
C11 H11 0.9300 . ?
C8 C9 1.366(8) . ?
C8 H8 0.9300 . ?
C3 C2 1.370(8) . ?
C3 H3 0.9300 . ?
C14 C15 1.383(8) . ?
C14 H14 0.9300 . ?
C10 C9 1.382(8) . ?
C10 H10 0.9300 . ?
C15 H15 0.9300 . ?
C2 C1 1.384(8) . ?
C2 H2A 0.9300 . ?
C1 H1 0.9300 . ?
O1W H1WA 0.8580 . ?
O1W H1WB 0.8659 . ?

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
O2 Co1 O1 101.11(14) . . ?
O2 Co1 N4 86.81(13) . . ?
O1 Co1 N4 88.63(13) . . ?
O2 Co1 N3 91.52(13) . . ?
O1 Co1 N3 86.66(13) . . ?
N4 Co1 N3 174.61(15) . . ?
O2 Co1 N1 88.84(13) . . ?
O1 Co1 N1 160.29(13) . . ?
N4 Co1 N1 109.05(14) . . ?
N3 Co1 N1 76.01(14) . . ?
O2 Co1 N6 159.29(13) . . ?
O1 Co1 N6 90.04(14) . . ?
N4 Co1 N6 75.96(13) . . ?
N3 Co1 N6 106.64(14) . . ?
N1 Co1 N6 86.08(13) . . ?
C20 O2 Co1 130.7(3) . . ?
C18 N4 N5 116.3(3) . . ?
C18 N4 Co1 129.3(3) . . ?
N5 N4 Co1 114.4(3) . . ?
C6 N3 N2 116.1(4) . . ?
C6 N3 Co1 128.8(3) . . ?
N2 N3 Co1 115.0(3) . . ?
C12 O1 Co1 129.5(3) . . ?
C13 N6 C17 116.0(4) . . ?
C13 N6 Co1 132.8(3) . . ?
C17 N6 Co1 110.4(3) . . ?
C17 N5 N4 118.9(3) . . ?
C17 N5 H5 120.5 . . ?
N4 N5 H5 120.5 . . ?
C4 N2 N3 118.7(4) . . ?
C4 N2 H2 120.7 . . ?
N3 N2 H2 120.7 . . ?
C5 N1 C4 116.3(4) . . ?
C5 N1 Co1 131.5(3) . . ?
C4 N1 Co1 112.2(3) . . ?
O2 C20 C21 120.1(4) . . ?
O2 C20 C19 123.5(4) . . ?
C21 C20 C19 116.3(4) . . ?
N4 C18 C19 125.4(4) . . ?
N4 C18 H18 117.3 . . ?
C19 C18 H18 117.3 . . ?
N3 C6 C7 125.6(4) . . ?
N3 C6 H6 117.2 . . ?
C7 C6 H6 117.2 . . ?
N6 C17 N5 117.9(4) . . ?
N6 C17 C16 122.8(4) . . ?
N5 C17 C16 119.3(4) . . ?
N1 C4 N2 117.7(4) . . ?
N1 C4 C3 122.7(5) . . ?
N2 C4 C3 119.5(4) . . ?
C15 C16 C17 118.5(5) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N1 C5 C1 125.4(5) . . ?
N1 C5 Cl2 116.2(4) . . ?
C1 C5 Cl2 118.4(4) . . ?
N6 C13 C14 125.3(5) . . ?
N6 C13 Cl1 116.4(3) . . ?
C14 C13 Cl1 118.2(4) . . ?
C24 C23 C22 120.6(4) . . ?
C24 C23 Cl4 120.6(4) . . ?
C22 C23 Cl4 118.7(4) . . ?
C22 C21 C20 123.2(4) . . ?
C22 C21 H21 118.4 . . ?
C20 C21 H21 118.4 . . ?
C24 C19 C20 119.0(4) . . ?
C24 C19 C18 117.0(4) . . ?
C20 C19 C18 124.0(4) . . ?
O1 C12 C11 120.4(4) . . ?
O1 C12 C7 122.8(4) . . ?
C11 C12 C7 116.8(4) . . ?
C8 C7 C12 118.8(5) . . ?
C8 C7 C6 116.7(4) . . ?
C12 C7 C6 124.4(4) . . ?
C23 C24 C19 121.8(4) . . ?
C23 C24 H24 119.1 . . ?
C19 C24 H24 119.1 . . ?
C21 C22 C23 119.0(5) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C10 C11 C12 122.9(5) . . ?
C10 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C9 C8 C7 122.0(5) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C2 C3 C4 118.3(5) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C13 C14 C15 117.0(5) . . ?
C13 C14 H14 121.5 . . ?
C15 C14 H14 121.5 . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C16 C15 C14 120.4(5) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C3 C2 C1 120.1(5) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C5 C1 C2 117.3(5) . . ?
C5 C1 H1 121.4 . . ?
C2 C1 H1 121.4 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 Cl3 119.6(4) . . ?
C10 C9 Cl3 120.6(5) . . ?
H1WA O1W H1WB 104.6 . . ?

_refine_diff_density_max         1.462
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.096

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_cu
_database_code_depnum_ccdc_archive 'CCDC 1949219'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Br2 Cl2 Cu N6 O2, N O3, 2(H2 O) '
_chemical_formula_sum            'C24 H22 Br2 Cl2 Cu N7 O7'
_chemical_formula_weight         814.74

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   23.057(3)
_cell_length_b                   7.2192(6)
_cell_length_c                   22.309(2)
_cell_angle_alpha                90
_cell_angle_beta                 123.604(17)
_cell_angle_gamma                90
_cell_volume                     3092.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2193
_cell_measurement_theta_min      3.7290
_cell_measurement_theta_max      19.9820

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_F_000             1616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    3.516
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_T_max  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            9684
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.365
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.905
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.904
_reflns_number_total             4880
_reflns_number_gt                3065
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.903

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1093P)²+3.7919P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4880
_refine_ls_number_parameters     397
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.2065
_refine_ls_wR_factor_gt          0.1643
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.32393(9) -0.8418(3) -0.32175(9) 0.0644(5) Uani 1 1 d . . . . .
Br1 Br -0.42733(12) -0.7169(3) -0.50256(9) 0.1032(8) Uani 1 1 d . . . . .
Br2 Br -0.40078(11) -1.2483(3) -0.41352(11) 0.1061(8) Uani 1 1 d . . . . .
Cl2 Cl -0.3696(3) -1.1276(8) -0.1445(3) 0.0987(17) Uani 1 1 d . . . . .
C5 C -0.4406(8) -0.865(3) -0.3094(7) 0.065(4) Uani 1 1 d . . . . .
C11 C -0.1725(9) -0.404(2) -0.2487(9) 0.068(4) Uani 1 1 d . . . . .
N2 N -0.4078(6) -0.712(2) -0.2730(7) 0.077(4) Uani 1 1 d . . . . .
H2 H -0.4251 -0.6463 -0.2545 0.092 Uiso 1 1 calc R U . . .
N3 N -0.3465(6) -0.6592(19) -0.2647(6) 0.059(3) Uani 1 1 d . . . . .
C7 C -0.2421(8) -0.476(2) -0.2033(8) 0.059(4) Uani 1 1 d . . . . .
N6 N -0.2959(7) -0.827(2) -0.3930(6) 0.068(3) Uani 1 1 d . . . . .
C19 C -0.2017(8) -0.942(2) -0.1379(7) 0.056(4) Uani 1 1 d . . . . .
C8 C -0.1882(8) -0.423(2) -0.1360(8) 0.063(4) Uani 1 1 d . . . . .
O2 O -0.1966(8) -0.435(2) -0.0796(8) 0.108(3) Uani 1 1 d . U . . .
H2A H -0.1769 -0.3475 -0.0522 0.162 Uiso 1 1 calc R U . . .
C22 C -0.2447(10) -0.977(3) -0.0451(10) 0.083(5) Uani 1 1 d . . . . .
H22 H -0.2597 -0.9833 -0.0142 0.099 Uiso 1 1 calc R U . . .
C18 C -0.1786(8) -0.927(2) -0.1865(8) 0.063(4) Uani 1 1 d . . . . .
H18 H -0.1310 -0.9222 -0.1669 0.076 Uiso 1 1 calc R U . . .
C12 C -0.2353(8) -0.460(2) -0.2617(8) 0.059(4) Uani 1 1 d . . . . .
H12 H -0.2724 -0.4878 -0.3082 0.071 Uiso 1 1 calc R U . . .
N5 N -0.1896(7) -0.912(2) -0.2931(7) 0.072(4) Uani 1 1 d . . . . .
H5 H -0.1456 -0.9295 -0.2724 0.086 Uiso 1 1 calc R U . . .
C20 C -0.1588(9) -0.888(3) -0.0660(9) 0.072(4) Uani 1 1 d . U . . .
C17 C -0.2311(9) -0.876(2) -0.3652(8) 0.063(4) Uani 1 1 d . . . . .
C23 C -0.2887(9) -1.033(3) -0.1148(8) 0.067(4) Uani 1 1 d . . . . .
C16 C -0.1992(10) -0.886(3) -0.4041(9) 0.081(5) Uani 1 1 d . . . . .
H16 H -0.1526 -0.9180 -0.3821 0.097 Uiso 1 1 calc R U . . .
N4 N -0.2199(7) -0.9193(17) -0.2537(6) 0.059(3) Uani 1 1 d . . . . .
C9 C -0.1256(7) -0.368(3) -0.1254(8) 0.069(4) Uani 1 1 d . . . . .
H9 H -0.0886 -0.3354 -0.0795 0.083 Uiso 1 1 calc R U . . .
C24 C -0.2680(8) -1.018(2) -0.1606(8) 0.066(4) Uani 1 1 d . . . . .
H24 H -0.2976 -1.0571 -0.2079 0.079 Uiso 1 1 calc R U . . .
C1 C -0.4432(10) -1.121(3) -0.3732(8) 0.077(5) Uani 1 1 d . . . . .
C4 C -0.5012(9) -0.933(3) -0.3168(10) 0.088(6) Uani 1 1 d . . . . .
H4 H -0.5221 -0.8628 -0.2988 0.106 Uiso 1 1 calc R U . . .
N1 N -0.4120(6) -0.9641(18) -0.3400(6) 0.065(3) Uani 1 1 d . . . . .
C2 C -0.5005(10) -1.194(3) -0.3774(11) 0.099(6) Uani 1 1 d . . . . .
H2B H -0.5191 -1.3076 -0.3992 0.118 Uiso 1 1 calc R U . . .
C15 C -0.2414(11) -0.846(3) -0.4764(10) 0.092(6) Uani 1 1 d . . . . .
H15 H -0.2235 -0.8546 -0.5047 0.111 Uiso 1 1 calc R U . . .
C13 C -0.3342(9) -0.787(2) -0.4651(8) 0.073(5) Uani 1 1 d . . . . .
C6 C -0.3090(7) -0.544(2) -0.2149(8) 0.059(4) Uani 1 1 d . . . . .
H6 H -0.3231 -0.5018 -0.1856 0.071 Uiso 1 1 calc R U . . .
C10 C -0.1178(8) -0.362(3) -0.1814(10) 0.082(5) Uani 1 1 d . . . . .
H10 H -0.0750 -0.3304 -0.1736 0.098 Uiso 1 1 calc R U . . .
C21 C -0.1795(10) -0.912(3) -0.0193(9) 0.087(6) Uani 1 1 d . . . . .
H21 H -0.1493 -0.8833 0.0293 0.105 Uiso 1 1 calc R U . . .
C3 C -0.5295(11) -1.091(3) -0.3480(11) 0.096(6) Uani 1 1 d . . . . .
H3 H -0.5687 -1.1342 -0.3504 0.115 Uiso 1 1 calc R U . . .
Cl1 Cl -0.1642(3) -0.3953(8) -0.3224(3) 0.0964(15) Uani 1 1 d . . . . .
C14 C -0.3092(13) -0.794(3) -0.5074(10) 0.101(7) Uani 1 1 d . . . . .
H14 H -0.3372 -0.7640 -0.5560 0.121 Uiso 1 1 calc R U . . .
O3 O -0.0792(9) -0.329(3) 0.0480(7) 0.113(5) Uani 1 1 d G . . . .
H3A H -0.0696 -0.4120 0.0794 0.170 Uiso 1 1 d G U . . .
H3B H -0.0823 -0.2242 0.0634 0.170 Uiso 1 1 d G U . . .
O4 O -0.0078(6) -0.688(3) 0.0878(7) 0.114(5) Uani 1 1 d G . . . .
H4A H 0.0309 -0.7090 0.0927 0.171 Uiso 1 1 d G U . . .
H4B H -0.0035 -0.7367 0.1247 0.171 Uiso 1 1 d G U . . .
O5 O -0.4491(9) -0.578(3) -0.1720(8) 0.128(6) Uani 1 1 d . . . . .
N7 N -0.5076(11) -0.506(3) -0.2153(11) 0.094(5) Uani 1 1 d . U . . .
O6 O -0.5336(9) -0.512(3) -0.2803(11) 0.145(6) Uani 1 1 d . . . . .
O7 O -0.5422(8) -0.414(2) -0.2018(8) 0.113(3) Uani 1 1 d . U . . .
O1 O -0.0942(6) -0.819(3) -0.0458(6) 0.107(5) Uani 1 1 d . . . . .
H1 H -0.0677 -0.8225 -0.0019 0.160 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
Cu1 N6 2.023(10) . ?
Cu1 N1 2.037(13) . ?
Cu1 N4 2.084(13) . ?
Cu1 N3 2.088(12) . ?
Br1 C13 1.892(18) . ?
Br2 C1 1.891(18) . ?
Cl2 C23 1.737(18) . ?
C5 N2 1.33(2) . ?
C5 N1 1.380(19) . ?
C5 C4 1.40(2) . ?
C11 C10 1.36(2) . ?
C11 C12 1.37(2) . ?
C11 Cl1 1.759(13) . ?
N2 N3 1.375(16) . ?
N2 H2 0.8600 . ?
N3 C6 1.268(18) . ?
C7 C8 1.37(2) . ?
C7 C12 1.400(18) . ?
C7 C6 1.498(19) . ?
N6 C17 1.309(19) . ?
N6 C13 1.372(18) . ?
C19 C20 1.40(2) . ?
C19 C24 1.43(2) . ?
C19 C18 1.452(19) . ?
C8 O2 1.377(17) . ?
C8 C9 1.38(2) . ?
O2 H2A 0.8200 . ?
C22 C21 1.36(3) . ?
C22 C23 1.37(2) . ?
C22 H22 0.9300 . ?
C18 N4 1.256(17) . ?
C18 H18 0.9300 . ?
C12 H12 0.9300 . ?
N5 C17 1.367(19) . ?
N5 N4 1.392(15) . ?
N5 H5 0.8600 . ?
C20 C21 1.38(2) . ?
C20 O1 1.39(2) . ?
C17 C16 1.417(19) . ?
C23 C24 1.351(19) . ?
C16 C15 1.38(2) . ?
C16 H16 0.9300 . ?
C9 C10 1.36(2) . ?
C9 H9 0.9300 . ?
C24 H24 0.9300 . ?
C1 N1 1.33(2) . ?
C1 C2 1.38(3) . ?
C4 C3 1.31(3) . ?
C4 H4 0.9300 . ?
C2 C3 1.38(3) . ?
C2 H2B 0.9300 . ?
C15 C14 1.36(3) . ?
C15 H15 0.9300 . ?
C13 C14 1.35(2) . ?
C6 H6 0.9300 . ?
C10 H10 0.9300 . ?
C21 H21 0.9300 . ?
C3 H3 0.9300 . ?
C14 H14 0.9300 . ?
O3 H3A 0.8518 . ?
O3 H3B 0.8504 . ?
O4 H4A 0.8499 . ?
O4 H4B 0.8499 . ?
O5 N7 1.26(2) . ?
N7 O7 1.20(2) . ?
N7 O6 1.23(2) . ?
O1 H1 0.8200 . ?

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
N6 Cu1 N1 125.6(5) . . ?
N6 Cu1 N4 81.2(5) . . ?
N1 Cu1 N4 130.3(5) . . ?
N6 Cu1 N3 137.9(5) . . ?
N1 Cu1 N3 80.7(5) . . ?
N4 Cu1 N3 107.5(4) . . ?
N2 C5 N1 117.7(13) . . ?
N2 C5 C4 123.6(15) . . ?
N1 C5 C4 118.7(16) . . ?
C10 C11 C12 121.7(13) . . ?
C10 C11 Cl1 120.8(12) . . ?
C12 C11 Cl1 117.5(13) . . ?
C5 N2 N3 120.5(13) . . ?
C5 N2 H2 119.7 . . ?
N3 N2 H2 119.7 . . ?
C6 N3 N2 116.9(11) . . ?
C6 N3 Cu1 131.9(9) . . ?
N2 N3 Cu1 109.0(10) . . ?
C8 C7 C12 119.6(13) . . ?
C8 C7 C6 120.3(12) . . ?
C12 C7 C6 120.0(13) . . ?
C17 N6 C13 115.9(12) . . ?
C17 N6 Cu1 113.1(9) . . ?
C13 N6 Cu1 130.9(12) . . ?
C20 C19 C24 116.9(13) . . ?
C20 C19 C18 121.1(14) . . ?
C24 C19 C18 121.9(13) . . ?
C7 C8 O2 118.8(13) . . ?
C7 C8 C9 119.6(12) . . ?
O2 C8 C9 121.5(14) . . ?
C8 O2 H2A 109.5 . . ?
C21 C22 C23 122.4(15) . . ?
C21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
N4 C18 C19 123.1(15) . . ?
N4 C18 H18 118.5 . . ?
C19 C18 H18 118.5 . . ?
C11 C12 C7 118.5(14) . . ?
C11 C12 H12 120.8 . . ?
C7 C12 H12 120.8 . . ?
C17 N5 N4 118.8(13) . . ?
C17 N5 H5 120.6 . . ?
N4 N5 H5 120.6 . . ?
C21 C20 O1 123.9(15) . . ?
C21 C20 C19 120.9(16) . . ?
O1 C20 C19 115.1(13) . . ?
N6 C17 N5 118.7(11) . . ?
N6 C17 C16 124.6(14) . . ?
N5 C17 C16 116.6(16) . . ?
C24 C23 C22 119.0(16) . . ?
C24 C23 Cl2 119.9(12) . . ?
C22 C23 Cl2 121.1(12) . . ?
C15 C16 C17 115.8(17) . . ?
C15 C16 H16 122.1 . . ?
C17 C16 H16 122.1 . . ?
C18 N4 N5 116.2(13) . . ?
C18 N4 Cu1 133.4(10) . . ?
N5 N4 Cu1 107.9(9) . . ?
C10 C9 C8 120.6(14) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C23 C24 C19 121.5(14) . . ?
C23 C24 H24 119.3 . . ?
C19 C24 H24 119.3 . . ?
N1 C1 C2 124.4(18) . . ?
N1 C1 Br2 114.6(14) . . ?
C2 C1 Br2 121.0(16) . . ?
C3 C4 C5 123(2) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 H4 118.7 . . ?
C1 N1 C5 117.2(15) . . ?
C1 N1 Cu1 130.8(12) . . ?
C5 N1 Cu1 111.9(10) . . ?
C1 C2 C3 118(2) . . ?
C1 C2 H2B 121.2 . . ?
C3 C2 H2B 121.2 . . ?
C14 C15 C16 121.5(15) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C14 C13 N6 124.4(18) . . ?
C14 C13 Br1 121.4(14) . . ?
N6 C13 Br1 114.3(11) . . ?
N3 C6 C7 120.3(12) . . ?
N3 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C11 C10 C9 119.7(14) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C22 C21 C20 119.1(16) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C4 C3 C2 119.4(19) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C13 C14 C15 117.8(17) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
H3A O3 H3B 109.6 . . ?
H4A O4 H4B 104.5 . . ?
O7 N7 O6 111(2) . . ?
O7 N7 O5 128(2) . . ?
O6 N7 O5 120.6(19) . . ?
C20 O1 H1 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C5 N2 N3 -2(2) . . . . ?
C4 C5 N2 N3 176.5(15) . . . . ?
C5 N2 N3 C6 -161.9(15) . . . . ?
C5 N2 N3 Cu1 3.5(17) . . . . ?
C12 C7 C8 O2 178.4(14) . . . . ?
C6 C7 C8 O2 1(2) . . . . ?
C12 C7 C8 C9 -5(2) . . . . ?
C6 C7 C8 C9 177.1(15) . . . . ?
C20 C19 C18 N4 -157.9(16) . . . . ?
C24 C19 C18 N4 24(2) . . . . ?
C10 C11 C12 C7 0(2) . . . . ?
Cl1 C11 C12 C7 177.1(12) . . . . ?
C8 C7 C12 C11 5(2) . . . . ?
C6 C7 C12 C11 -177.9(15) . . . . ?
C24 C19 C20 C21 2(2) . . . . ?
C18 C19 C20 C21 -176.7(16) . . . . ?
C24 C19 C20 O1 178.6(15) . . . . ?
C18 C19 C20 O1 0(2) . . . . ?
C13 N6 C17 N5 177.8(14) . . . . ?
Cu1 N6 C17 N5 -6.0(19) . . . . ?
C13 N6 C17 C16 1(2) . . . . ?
Cu1 N6 C17 C16 177.1(13) . . . . ?
N4 N5 C17 N6 8(2) . . . . ?
N4 N5 C17 C16 -174.5(14) . . . . ?
C21 C22 C23 C24 -2(3) . . . . ?
C21 C22 C23 Cl2 176.5(16) . . . . ?
N6 C17 C16 C15 -2(3) . . . . ?
N5 C17 C16 C15 -178.8(16) . . . . ?
C19 C18 N4 N5 -177.6(13) . . . . ?
C19 C18 N4 Cu1 23(2) . . . . ?
C17 N5 N4 C18 -170.4(15) . . . . ?
C17 N5 N4 Cu1 -5.9(16) . . . . ?
C7 C8 C9 C10 2(3) . . . . ?
O2 C8 C9 C10 178.0(17) . . . . ?
C22 C23 C24 C19 -1(3) . . . . ?
Cl2 C23 C24 C19 -179.6(13) . . . . ?
C20 C19 C24 C23 1(2) . . . . ?
C18 C19 C24 C23 179.3(16) . . . . ?
N2 C5 C4 C3 -174.5(19) . . . . ?
N1 C5 C4 C3 4(3) . . . . ?
C2 C1 N1 C5 -2(2) . . . . ?
Br2 C1 N1 C5 -180.0(10) . . . . ?
C2 C1 N1 Cu1 175.4(14) . . . . ?
Br2 C1 N1 Cu1 -2.7(18) . . . . ?
N2 C5 N1 C1 176.8(14) . . . . ?
C4 C5 N1 C1 -2(2) . . . . ?
N2 C5 N1 Cu1 -1.0(17) . . . . ?
C4 C5 N1 Cu1 -179.4(12) . . . . ?
N1 C1 C2 C3 3(3) . . . . ?
Br2 C1 C2 C3 -178.7(15) . . . . ?
C17 C16 C15 C14 2(3) . . . . ?
C17 N6 C13 C14 0(2) . . . . ?
Cu1 N6 C13 C14 -175.6(14) . . . . ?
C17 N6 C13 Br1 -179.8(12) . . . . ?
Cu1 N6 C13 Br1 4.8(19) . . . . ?
N2 N3 C6 C7 -178.8(13) . . . . ?
Cu1 N3 C6 C7 20(2) . . . . ?
C8 C7 C6 N3 -151.3(16) . . . . ?
C12 C7 C6 N3 31(2) . . . . ?
C12 C11 C10 C9 -3(3) . . . . ?
Cl1 C11 C10 C9 179.4(14) . . . . ?
C8 C9 C10 C11 2(3) . . . . ?
C23 C22 C21 C20 5(3) . . . . ?
O1 C20 C21 C22 178.7(19) . . . . ?
C19 C20 C21 C22 -5(3) . . . . ?
C5 C4 C3 C2 -2(3) . . . . ?
C1 C2 C3 C4 -1(3) . . . . ?
N6 C13 C14 C15 1(3) . . . . ?
Br1 C13 C14 C15 -179.9(15) . . . . ?
C16 C15 C14 C13 -2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O5 0.86 2.25 3.049(19) 154.5 .
N2 H2 O6 0.86 2.44 3.16(2) 142.8 .
N2 H2 N7 0.86 2.69 3.53(2) 164.4 .
O2 H2A O3 0.82 2.12 2.74(2) 131.4 .
N5 H5 O7 0.86 2.01 2.83(2) 161.7 3_545
O3 H3A O4 0.85 2.40 2.93(3) 121.5 .
O3 H3A Cl2 0.85 2.96 3.671(17) 142.6 4_455
O3 H3B O5 0.85 2.36 3.06(2) 140.0 4_455
O4 H4A O1 0.85 2.35 3.120(19) 150.1 2
O4 H4B O7 0.85 1.92 2.68(2) 148.7 4_445
O1 H1 O4 0.82 1.95 2.680(19) 148.1 .

_refine_diff_density_max         0.902
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.092

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_CU
_database_code_depnum_ccdc_archive 'CCDC 1949218'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Br2 Cl2 Cu N6 O2, N O3, 2(H2 O)'
_chemical_formula_sum            'C24 H22 Br2 Cl2 Cu N7 O7'
_chemical_formula_weight         814.74

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 2'
_space_group_name_Hall           'I 2y'

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

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

_cell_length_a                   22.6667(10)
_cell_length_b                   7.2097(4)
_cell_length_c                   21.1442(13)
_cell_angle_alpha                90
_cell_angle_beta                 115.478(6)
_cell_angle_gamma                90
_cell_volume                     3119.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3081
_cell_measurement_theta_min      3.7200
_cell_measurement_theta_max      25.0120

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_F_000             1616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    3.487
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            10066
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.356
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             5079
_reflns_number_gt                3710
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.985

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.615(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5079
_refine_ls_number_parameters     384
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.99499(4) 0.24954(14) 0.17055(5) 0.0507(3) Uani 1 1 d . . . . .
Br1 Br 1.15604(4) 0.70298(16) 0.33215(6) 0.0851(4) Uani 1 1 d . . . . .
Br2 Br 0.77465(5) -0.05262(18) 0.12405(6) 0.0858(4) Uani 1 1 d . . . . .
N6 N 1.0918(3) 0.2772(9) 0.1958(4) 0.0466(17) Uani 1 1 d . . . . .
C11 C 1.0691(4) 0.6852(13) 0.3232(5) 0.057(2) Uani 1 1 d . . . . .
N3 N 0.9165(3) 0.4283(10) 0.1484(3) 0.0451(16) Uani 1 1 d . . . . .
C16 C 1.1983(3) 0.2271(14) 0.2906(5) 0.060(2) Uani 1 1 d . . . . .
H16 H 1.2236 0.1942 0.3371 0.072 Uiso 1 1 calc R U . . .
N1 N 0.9283(3) 0.1247(10) 0.0846(3) 0.0477(17) Uani 1 1 d . . . . .
C12 C 1.0202(4) 0.6277(11) 0.2602(4) 0.046(2) Uani 1 1 d . . . . .
H12 H 1.0296 0.6013 0.2225 0.055 Uiso 1 1 calc R U . . .
N2 N 0.8656(3) 0.3729(11) 0.0874(3) 0.056(2) Uani 1 1 d . . . . .
H2 H 0.8302 0.4370 0.0698 0.067 Uiso 1 1 calc R U . . .
C5 C 0.8713(3) 0.2172(13) 0.0551(4) 0.046(2) Uani 1 1 d . . . . .
N4 N 1.0320(3) 0.1746(10) 0.2752(3) 0.0440(17) Uani 1 1 d . . . . .
C20 C 0.8952(4) 0.0713(12) 0.2316(5) 0.052(2) Uani 1 1 d . . . . .
H20 H 0.9119 0.0368 0.2001 0.062 Uiso 1 1 calc R U . . .
C7 C 0.9559(4) 0.6092(11) 0.2533(4) 0.0434(19) Uani 1 1 d . . . . .
N5 N 1.1000(3) 0.1827(11) 0.3033(4) 0.0559(19) Uani 1 1 d . . . . .
H5 H 1.1230 0.1581 0.3469 0.067 Uiso 1 1 calc R U . . .
C21 C 0.8287(4) 0.0522(13) 0.2129(5) 0.053(2) Uani 1 1 d . . . . .
C8 C 0.9425(4) 0.6594(11) 0.3097(4) 0.048(2) Uani 1 1 d . . . . .
C1 C 0.9313(4) -0.0340(15) 0.0540(5) 0.060(2) Uani 1 1 d . . . . .
C18 C 1.0068(4) 0.1594(12) 0.3174(5) 0.052(2) Uani 1 1 d . . . . .
H18 H 1.0345 0.1597 0.3650 0.062 Uiso 1 1 calc R U . . .
C10 C 1.0555(4) 0.7289(14) 0.3789(5) 0.065(3) Uani 1 1 d . . . . .
H10 H 1.0891 0.7672 0.4210 0.078 Uiso 1 1 calc R U . . .
O1 O 0.8796(3) 0.6469(9) 0.3015(3) 0.0655(17) Uani 1 1 d . . . . .
C9 C 0.9933(4) 0.7166(14) 0.3730(4) 0.062(2) Uani 1 1 d . . . . .
H9 H 0.9847 0.7461 0.4110 0.075 Uiso 1 1 calc R U . . .
C17 C 1.1297(3) 0.2291(13) 0.2625(4) 0.048(2) Uani 1 1 d . . . . .
C14 C 1.1881(5) 0.3283(15) 0.1791(6) 0.072(3) Uani 1 1 d . . . . .
H14 H 1.2071 0.3644 0.1499 0.086 Uiso 1 1 calc R U . . .
C15 C 1.2261(4) 0.2747(15) 0.2479(6) 0.071(3) Uani 1 1 d . . . . .
H15 H 1.2714 0.2716 0.2648 0.085 Uiso 1 1 calc R U . . .
C13 C 1.1216(4) 0.3262(13) 0.1559(5) 0.054(2) Uani 1 1 d . . . . .
C6 C 0.9049(4) 0.5420(12) 0.1883(4) 0.050(2) Uani 1 1 d . . . . .
H6 H 0.8622 0.5825 0.1750 0.060 Uiso 1 1 calc R U . . .
O2 O 0.9536(3) 0.2604(12) 0.4072(3) 0.080(2) Uani 1 1 d . . . . .
H2A H 0.9346 0.3367 0.4204 0.120 Uiso 1 1 calc DR U . . .
C22 C 0.8042(4) 0.1014(15) 0.2593(6) 0.071(3) Uani 1 1 d . . . . .
H22 H 0.7599 0.0865 0.2471 0.085 Uiso 1 1 calc R U . . .
C19 C 0.9367(4) 0.1413(12) 0.2966(5) 0.050(2) Uani 1 1 d . . . . .
C24 C 0.9109(4) 0.1907(14) 0.3425(5) 0.062(2) Uani 1 1 d . . . . .
Cl2 Cl 1.07100(12) 0.3873(4) 0.07077(14) 0.0803(8) Uani 1 1 d . . . . .
Cl1 Cl 1.00592(15) -0.1492(4) 0.09398(16) 0.0910(9) Uani 1 1 d . . . . .
C3 C 0.8244(6) -0.0073(18) -0.0352(6) 0.080(3) Uani 1 1 d . . . . .
H3 H 0.7898 -0.0522 -0.0752 0.096 Uiso 1 1 calc R U . . .
C2 C 0.8823(6) -0.1048(16) -0.0047(5) 0.079(3) Uani 1 1 d . . . . .
H2B H 0.8877 -0.2161 -0.0238 0.095 Uiso 1 1 calc R U . . .
C23 C 0.8449(5) 0.1736(17) 0.3244(6) 0.076(3) Uani 1 1 d . . . . .
H23 H 0.8279 0.2098 0.3555 0.092 Uiso 1 1 calc R U . . .
C4 C 0.8188(4) 0.1540(16) -0.0060(5) 0.067(3) Uani 1 1 d . . . . .
H4 H 0.7805 0.2229 -0.0262 0.080 Uiso 1 1 calc R U . . .
O4 O 0.8699(5) 0.7463(15) 0.4218(5) 0.107(3) Uani 1 1 d G . . . .
H4A H 0.8689 0.6303 0.4286 0.160 Uiso 1 1 d G U . . .
H4B H 0.8410 0.8001 0.4309 0.160 Uiso 1 1 d G U . . .
O3 O 0.9068(3) 0.3860(12) 0.4966(2) 0.093(2) Uani 1 1 d G . . . .
N7 N 0.7118(2) 0.5753(7) -0.0133(2) 0.086(3) Uani 1 1 d G U . . .
O6 O 0.7252(2) 0.4962(7) 0.0444(2) 0.113(3) Uani 1 1 d G . . . .
O7 O 0.7501(2) 0.5777(12) -0.0397(2) 0.113(3) Uani 1 1 d G . . . .
O5 O 0.6587(3) 0.6515(11) -0.0464(2) 0.133(3) Uani 1 1 d G U . . .
H1 H 0.8652 0.6895 0.3222 0.199 Uiso 1 1 d G U . . .
H3B H 0.8881 0.2810 0.4907 0.199 Uiso 1 1 d DR U . . .
H3A H 0.9409 0.3770 0.5352 0.199 Uiso 1 1 d 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
Cu1 N1 2.009(7) . ?
Cu1 N6 2.034(6) . ?
Cu1 N4 2.071(7) . ?
Cu1 N3 2.081(6) . ?
Br1 C11 1.901(8) . ?
Br2 C21 1.903(9) . ?
N6 C13 1.333(10) . ?
N6 C17 1.344(10) . ?
C11 C10 1.376(12) . ?
C11 C12 1.380(11) . ?
N3 C6 1.282(10) . ?
N3 N2 1.369(8) . ?
C16 C15 1.350(12) . ?
C16 C17 1.404(10) . ?
C16 H16 0.9300 . ?
N1 C5 1.344(10) . ?
N1 C1 1.331(12) . ?
C12 C7 1.407(11) . ?
C12 H12 0.9300 . ?
N2 C5 1.350(11) . ?
N2 H2 0.8600 . ?
C5 C4 1.403(11) . ?
N4 C18 1.256(10) . ?
N4 N5 1.393(8) . ?
C20 C19 1.385(12) . ?
C20 C21 1.392(11) . ?
C20 H20 0.9300 . ?
C7 C8 1.398(11) . ?
C7 C6 1.447(11) . ?
N5 C17 1.346(10) . ?
N5 H5 0.8600 . ?
C21 C22 1.365(13) . ?
C8 O1 1.363(9) . ?
C8 C9 1.400(11) . ?
C1 C2 1.360(13) . ?
C1 Cl1 1.742(9) . ?
C18 C19 1.460(11) . ?
C18 H18 0.9300 . ?
C10 C9 1.363(11) . ?
C10 H10 0.9300 . ?
O1 H1 0.7180 . ?
C9 H9 0.9300 . ?
C14 C13 1.370(11) . ?
C14 C15 1.389(13) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C13 Cl2 1.725(9) . ?
C6 H6 0.9300 . ?
O2 C24 1.387(11) . ?
O2 H2A 0.8200 . ?
C22 C23 1.387(14) . ?
C22 H22 0.9300 . ?
C19 C24 1.377(12) . ?
C24 C23 1.382(12) . ?
C3 C2 1.380(14) . ?
C3 C4 1.348(15) . ?
C3 H3 0.9300 . ?
C2 H2B 0.9300 . ?
C23 H23 0.9300 . ?
C4 H4 0.9300 . ?
O4 H4A 0.8501 . ?
O4 H4B 0.8497 . ?
O3 H3B 0.8501 . ?
O3 H3A 0.8507 . ?
N7 O7 1.2192 . ?
N7 O5 1.2304 . ?
N7 O6 1.2604 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N6 126.1(3) . . ?
N1 Cu1 N4 130.6(3) . . ?
N6 Cu1 N4 81.3(3) . . ?
N1 Cu1 N3 80.5(3) . . ?
N6 Cu1 N3 136.1(3) . . ?
N4 Cu1 N3 108.4(2) . . ?
C13 N6 C17 117.6(6) . . ?
C13 N6 Cu1 130.0(6) . . ?
C17 N6 Cu1 112.3(5) . . ?
C10 C11 C12 120.7(8) . . ?
C10 C11 Br1 120.2(7) . . ?
C12 C11 Br1 119.0(7) . . ?
C6 N3 N2 118.5(6) . . ?
C6 N3 Cu1 130.2(5) . . ?
N2 N3 Cu1 108.9(5) . . ?
C15 C16 C17 117.7(9) . . ?
C15 C16 H16 121.1 . . ?
C17 C16 H16 121.1 . . ?
C5 N1 C1 116.2(7) . . ?
C5 N1 Cu1 113.4(6) . . ?
C1 N1 Cu1 130.4(6) . . ?
C11 C12 C7 119.7(8) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
C5 N2 N3 119.6(7) . . ?
C5 N2 H2 120.2 . . ?
N3 N2 H2 120.2 . . ?
N1 C5 N2 117.4(7) . . ?
N1 C5 C4 122.1(9) . . ?
N2 C5 C4 120.5(8) . . ?
C18 N4 N5 117.3(7) . . ?
C18 N4 Cu1 133.0(5) . . ?
N5 N4 Cu1 108.1(5) . . ?
C19 C20 C21 120.5(9) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C8 C7 C12 118.8(7) . . ?
C8 C7 C6 121.3(7) . . ?
C12 C7 C6 119.9(7) . . ?
C17 N5 N4 120.2(6) . . ?
C17 N5 H5 119.9 . . ?
N4 N5 H5 119.9 . . ?
C22 C21 C20 119.8(9) . . ?
C22 C21 Br2 121.7(7) . . ?
C20 C21 Br2 118.5(7) . . ?
O1 C8 C7 118.2(7) . . ?
O1 C8 C9 121.8(8) . . ?
C7 C8 C9 120.0(8) . . ?
N1 C1 C2 125.0(9) . . ?
N1 C1 Cl1 114.7(7) . . ?
C2 C1 Cl1 120.3(8) . . ?
N4 C18 C19 124.3(8) . . ?
N4 C18 H18 117.9 . . ?
C19 C18 H18 117.9 . . ?
C11 C10 C9 120.7(8) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C8 O1 H1 128.2 . . ?
C10 C9 C8 120.0(9) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
N5 C17 N6 117.8(6) . . ?
N5 C17 C16 119.6(8) . . ?
N6 C17 C16 122.5(8) . . ?
C13 C14 C15 117.6(9) . . ?
C13 C14 H14 121.2 . . ?
C15 C14 H14 121.2 . . ?
C16 C15 C14 120.8(8) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C14 C13 N6 123.7(9) . . ?
C14 C13 Cl2 120.3(8) . . ?
N6 C13 Cl2 116.0(6) . . ?
N3 C6 C7 122.2(7) . . ?
N3 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C24 O2 H2A 109.5 . . ?
C23 C22 C21 120.6(8) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C19 C20 118.7(8) . . ?
C24 C19 C18 120.1(9) . . ?
C20 C19 C18 121.2(8) . . ?
C19 C24 C23 121.4(10) . . ?
C19 C24 O2 117.4(8) . . ?
C23 C24 O2 121.2(9) . . ?
C2 C3 C4 118.9(10) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C1 C2 C3 118.3(10) . . ?
C1 C2 H2B 120.8 . . ?
C3 C2 H2B 120.8 . . ?
C22 C23 C24 119.0(9) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C3 C4 C5 119.5(10) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
H4A O4 H4B 109.5 . . ?
H3B O3 H3A 105.2 . . ?
O7 N7 O5 116.6 . . ?
O7 N7 O6 121.9 . . ?
O5 N7 O6 121.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O6 0.86 2.24 3.043(8) 154.5 .
N2 H2 O7 0.86 2.46 3.195(9) 143.2 .
N5 H5 O5 0.86 2.04 2.877(9) 163.3 3_545
O2 H2A O3 0.82 2.00 2.692(9) 142.2 .
O4 H4A O3 0.85 2.20 2.968(12) 150.0 .
O4 H4B O6 0.85 2.28 3.12(3) 168.7 4_655
O1 H1 O4 0.72 2.10 2.742(10) 148.7 .
O3 H3B O5 0.85 2.11 2.742(17) 130.6 4_645
O3 H3A O2 0.85 2.32 3.070(9) 146.5 2_756

_refine_diff_density_max         0.529
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.064

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_20
_database_code_depnum_ccdc_archive 'CCDC 1949220'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Br4 Cu N6 O2, N O3, 2(H2 O)'
_chemical_formula_sum            'C24 H22 Br4 Cu N7 O7'
_chemical_formula_weight         903.64

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   23.2906(18)
_cell_length_b                   7.2893(5)
_cell_length_c                   22.5828(17)
_cell_angle_alpha                90
_cell_angle_beta                 124.599(11)
_cell_angle_gamma                90
_cell_volume                     3155.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2906
_cell_measurement_theta_min      3.5000
_cell_measurement_theta_max      23.5140

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.809
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            10157
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.288
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.899
_reflns_number_total             4447
_reflns_number_gt                3499
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.898

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0879P)²+14.7529P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4447
_refine_ls_number_parameters     391
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1592
_refine_ls_wR_factor_gt          0.1384
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.32259(8) 0.4216(2) 0.32111(8) 0.0538(4) Uani 1 1 d . . . . .
Br1 Br 0.16100(10) 0.8737(3) 0.32026(11) 0.0897(6) Uani 1 1 d . . . . .
Br4 Br 0.37270(9) 0.1163(3) 0.14959(9) 0.0865(6) Uani 1 1 d . . . . .
N3 N 0.2958(6) 0.4450(16) 0.3922(5) 0.055(3) Uani 1 1 d . . . . .
C23 C 0.1700(7) 0.855(2) 0.2414(8) 0.058(3) Uani 1 1 d . . . . .
C4 C 0.2003(8) 0.386(2) 0.4040(8) 0.066(4) Uani 1 1 d . . . . .
H4 H 0.1544 0.3501 0.3833 0.080 Uiso 1 1 calc R U . . .
C6 C 0.1771(7) 0.332(2) 0.1863(7) 0.055(3) Uani 1 1 d . . . . .
H6 H 0.1293 0.3328 0.1656 0.066 Uiso 1 1 calc R U . . .
N5 N 0.4070(5) 0.5466(18) 0.2747(6) 0.063(3) Uani 1 1 d . . . . .
H5 H 0.4251 0.6114 0.2575 0.076 Uiso 1 1 calc R U . . .
N4 N 0.4098(5) 0.2978(16) 0.3402(5) 0.054(3) Uani 1 1 d . . . . .
O1 O 0.1968(5) 0.8211(15) 0.0769(5) 0.064(2) Uani 1 1 d . . . . .
H1 H 0.1703 0.8920 0.0444 0.096 Uiso 1 1 calc R U . . .
C9 C 0.2854(7) 0.223(2) 0.1154(7) 0.055(3) Uani 1 1 d . . . . .
C24 C 0.2330(6) 0.7965(18) 0.2559(7) 0.049(3) Uani 1 1 d . . . . .
H24 H 0.2695 0.7677 0.3027 0.059 Uiso 1 1 calc R U . . .
C17 C 0.4387(6) 0.390(2) 0.3117(6) 0.051(3) Uani 1 1 d . . . . .
N6 N 0.3452(5) 0.6009(16) 0.2651(5) 0.048(2) Uani 1 1 d . . . . .
N1 N 0.2184(5) 0.3458(15) 0.2537(5) 0.048(2) Uani 1 1 d . . . . .
C8 C 0.2643(7) 0.2403(18) 0.1608(7) 0.052(3) Uani 1 1 d . . . . .
H8 H 0.2939 0.1996 0.2080 0.062 Uiso 1 1 calc R U . . .
C10 C 0.2402(9) 0.279(3) 0.0444(9) 0.077(5) Uani 1 1 d . . . . .
H10 H 0.2539 0.2689 0.0131 0.092 Uiso 1 1 calc R U . . .
C16 C 0.5000(7) 0.330(2) 0.3208(8) 0.069(4) Uani 1 1 d . . . . .
H16 H 0.5211 0.3995 0.3037 0.082 Uiso 1 1 calc R U . . .
N2 N 0.1888(6) 0.3537(18) 0.2915(6) 0.061(3) Uani 1 1 d . . . . .
H2 H 0.1449 0.3329 0.2702 0.074 Uiso 1 1 calc R U . . .
C21 C 0.1239(7) 0.890(2) 0.1179(8) 0.064(4) Uani 1 1 d . . . . .
H21 H 0.0868 0.9206 0.0716 0.077 Uiso 1 1 calc R U . . .
C5 C 0.2292(7) 0.395(2) 0.3634(7) 0.054(3) Uani 1 1 d . . . . .
C18 C 0.3060(6) 0.7095(19) 0.2120(7) 0.052(3) Uani 1 1 d . . . . .
H18 H 0.3189 0.7428 0.1813 0.062 Uiso 1 1 calc R U . . .
C20 C 0.1863(6) 0.8315(19) 0.1300(7) 0.053(3) Uani 1 1 d . . . . .
C12 C 0.1556(7) 0.367(2) 0.0667(7) 0.066(4) Uani 1 1 d . . . . .
C1 C 0.3336(8) 0.485(2) 0.4620(8) 0.067(4) Uani 1 1 d . . . . .
C22 C 0.1163(7) 0.903(2) 0.1744(9) 0.070(4) Uani 1 1 d . . . . .
H22 H 0.0746 0.9439 0.1662 0.084 Uiso 1 1 calc R U . . .
C7 C 0.2013(7) 0.315(2) 0.1393(7) 0.054(3) Uani 1 1 d . . . . .
O2 O 0.0921(5) 0.436(2) 0.0453(6) 0.095(4) Uani 1 1 d . U . . .
H2A H 0.0815 0.5196 0.0165 0.143 Uiso 1 1 calc R U . . .
C2 C 0.3105(11) 0.482(3) 0.5054(9) 0.087(5) Uani 1 1 d . . . . .
H2B H 0.3396 0.5111 0.5540 0.104 Uiso 1 1 calc R U . . .
C11 C 0.1761(9) 0.347(2) 0.0200(8) 0.074(4) Uani 1 1 d . . . . .
H11 H 0.1459 0.3815 -0.0280 0.089 Uiso 1 1 calc R U . . .
Br2 Br 0.42761(10) 0.5527(3) 0.50129(8) 0.0911(6) Uani 1 1 d . . . . .
C19 C 0.2416(6) 0.7806(18) 0.1997(7) 0.051(3) Uani 1 1 d . . . . .
C14 C 0.4990(8) 0.070(3) 0.3826(9) 0.085(5) Uani 1 1 d . . . . .
H14 H 0.5177 -0.0404 0.4065 0.102 Uiso 1 1 calc R U . . .
C13 C 0.4412(8) 0.143(2) 0.3736(7) 0.065(4) Uani 1 1 d . . . . .
Br3 Br 0.39680(11) 0.0168(3) 0.41192(10) 0.1002(7) Uani 1 1 d . . . . .
C3 C 0.2421(11) 0.434(3) 0.4740(9) 0.083(5) Uani 1 1 d . . . . .
H3 H 0.2241 0.4334 0.5017 0.099 Uiso 1 1 calc R U . . .
C15 C 0.5287(9) 0.168(3) 0.3547(9) 0.084(5) Uani 1 1 d . . . . .
H15 H 0.5684 0.1243 0.3592 0.101 Uiso 1 1 calc R U . . .
N7 N 0.0050(9) 0.246(2) 0.2170(9) 0.084(4) Uani 1 1 d . U . . .
O5 O -0.0509(6) 0.163(2) 0.1760(7) 0.106(5) Uani 1 1 d . . . . .
O6 O 0.0298(8) 0.250(2) 0.2816(10) 0.121(5) Uani 1 1 d . . . . .
O7 O 0.0406(7) 0.323(3) 0.2007(8) 0.130(5) Uani 1 1 d . U . . .
O4 O 0.0800(6) 0.923(2) -0.0523(6) 0.104(4) Uani 1 1 d . . . . .
H4A H 0.0546 0.9758 -0.0929 0.156 Uiso 1 1 d R U . . .
H4B H 0.0591 0.8194 -0.0675 0.156 Uiso 1 1 d R U . . .
O3 O 0.0065(5) 0.566(2) -0.0887(5) 0.088(4) Uani 1 1 d . . . . .
H3A H 0.0024 0.5259 -0.1263 0.131 Uiso 1 1 d R U . . .
H3B H -0.0337 0.5514 -0.0968 0.131 Uiso 1 1 d 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
Cu1 N4 2.032(11) . ?
Cu1 N3 2.034(10) . ?
Cu1 N1 2.078(10) . ?
Cu1 N6 2.084(10) . ?
Br1 C23 1.913(13) . ?
Br4 C9 1.885(14) . ?
N3 C1 1.328(17) . ?
N3 C5 1.349(17) . ?
C23 C22 1.35(2) . ?
C23 C24 1.376(18) . ?
C4 C3 1.35(2) . ?
C4 C5 1.412(17) . ?
C4 H4 0.9300 . ?
C6 N1 1.262(16) . ?
C6 C7 1.463(17) . ?
C6 H6 0.9300 . ?
N5 C17 1.360(18) . ?
N5 N6 1.385(13) . ?
N5 H5 0.8600 . ?
N4 C13 1.326(18) . ?
N4 C17 1.344(17) . ?
O1 C20 1.356(16) . ?
O1 H1 0.8200 . ?
C9 C8 1.371(17) . ?
C9 C10 1.39(2) . ?
C24 C19 1.398(18) . ?
C24 H24 0.9300 . ?
C17 C16 1.395(17) . ?
N6 C18 1.286(15) . ?
N1 N2 1.369(13) . ?
C8 C7 1.370(19) . ?
C8 H8 0.9300 . ?
C10 C11 1.36(2) . ?
C10 H10 0.9300 . ?
C16 C15 1.35(2) . ?
C16 H16 0.9300 . ?
N2 C5 1.368(16) . ?
N2 H2 0.8600 . ?
C21 C20 1.385(18) . ?
C21 C22 1.39(2) . ?
C21 H21 0.9300 . ?
C18 C19 1.458(17) . ?
C18 H18 0.9300 . ?
C20 C19 1.403(18) . ?
C12 O2 1.364(18) . ?
C12 C11 1.39(2) . ?
C12 C7 1.408(19) . ?
C1 C2 1.36(2) . ?
C1 Br2 1.904(17) . ?
C22 H22 0.9300 . ?
O2 H2A 0.8200 . ?
C2 C3 1.37(3) . ?
C2 H2B 0.9300 . ?
C11 H11 0.9300 . ?
C14 C13 1.35(2) . ?
C14 C15 1.37(3) . ?
C14 H14 0.9300 . ?
C13 Br3 1.917(16) . ?
C3 H3 0.9300 . ?
C15 H15 0.9300 . ?
N7 O7 1.216(19) . ?
N7 O6 1.228(19) . ?
N7 O5 1.244(19) . ?
O4 H4A 0.8510 . ?
O4 H4B 0.8553 . ?
O3 H3A 0.8514 . ?
O3 H3B 0.8506 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N3 126.0(4) . . ?
N4 Cu1 N1 130.4(4) . . ?
N3 Cu1 N1 81.1(4) . . ?
N4 Cu1 N6 80.9(4) . . ?
N3 Cu1 N6 136.3(5) . . ?
N1 Cu1 N6 108.4(4) . . ?
C1 N3 C5 116.0(12) . . ?
C1 N3 Cu1 131.4(10) . . ?
C5 N3 Cu1 112.3(8) . . ?
C22 C23 C24 122.0(13) . . ?
C22 C23 Br1 120.2(10) . . ?
C24 C23 Br1 117.8(11) . . ?
C3 C4 C5 117.3(15) . . ?
C3 C4 H4 121.4 . . ?
C5 C4 H4 121.4 . . ?
N1 C6 C7 122.6(12) . . ?
N1 C6 H6 118.7 . . ?
C7 C6 H6 118.7 . . ?
C17 N5 N6 119.3(11) . . ?
C17 N5 H5 120.4 . . ?
N6 N5 H5 120.4 . . ?
C13 N4 C17 115.6(12) . . ?
C13 N4 Cu1 131.5(11) . . ?
C17 N4 Cu1 112.8(9) . . ?
C20 O1 H1 109.5 . . ?
C8 C9 C10 118.5(13) . . ?
C8 C9 Br4 119.6(10) . . ?
C10 C9 Br4 121.8(10) . . ?
C23 C24 C19 119.5(12) . . ?
C23 C24 H24 120.2 . . ?
C19 C24 H24 120.2 . . ?
N4 C17 N5 118.0(11) . . ?
N4 C17 C16 121.5(13) . . ?
N5 C17 C16 120.5(13) . . ?
C18 N6 N5 116.5(10) . . ?
C18 N6 Cu1 131.5(8) . . ?
N5 N6 Cu1 108.9(8) . . ?
C6 N1 N2 116.6(11) . . ?
C6 N1 Cu1 132.7(9) . . ?
N2 N1 Cu1 108.9(8) . . ?
C7 C8 C9 122.6(13) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C11 C10 C9 120.9(14) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C15 C16 C17 119.4(16) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C5 N2 N1 119.9(10) . . ?
C5 N2 H2 120.1 . . ?
N1 N2 H2 120.1 . . ?
C20 C21 C22 120.5(13) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
N3 C5 N2 117.4(11) . . ?
N3 C5 C4 122.6(12) . . ?
N2 C5 C4 120.0(13) . . ?
N6 C18 C19 120.3(11) . . ?
N6 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
O1 C20 C21 122.7(12) . . ?
O1 C20 C19 117.8(11) . . ?
C21 C20 C19 119.6(12) . . ?
O2 C12 C11 122.6(13) . . ?
O2 C12 C7 117.6(12) . . ?
C11 C12 C7 119.8(13) . . ?
N3 C1 C2 125.8(16) . . ?
N3 C1 Br2 114.9(11) . . ?
C2 C1 Br2 119.3(13) . . ?
C23 C22 C21 119.5(12) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C8 C7 C12 118.0(12) . . ?
C8 C7 C6 123.6(12) . . ?
C12 C7 C6 118.3(12) . . ?
C12 O2 H2A 109.5 . . ?
C1 C2 C3 116.7(15) . . ?
C1 C2 H2B 121.6 . . ?
C3 C2 H2B 121.6 . . ?
C10 C11 C12 120.1(14) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C24 C19 C20 118.9(11) . . ?
C24 C19 C18 121.3(12) . . ?
C20 C19 C18 119.8(12) . . ?
C13 C14 C15 116.5(17) . . ?
C13 C14 H14 121.7 . . ?
C15 C14 H14 121.7 . . ?
N4 C13 C14 126.9(16) . . ?
N4 C13 Br3 113.5(12) . . ?
C14 C13 Br3 119.5(13) . . ?
C4 C3 C2 121.6(14) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C16 C15 C14 119.9(16) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
O7 N7 O6 114.0(18) . . ?
O7 N7 O5 127.0(17) . . ?
O6 N7 O5 119.0(18) . . ?
H4A O4 H4B 94.5 . . ?
H3A O3 H3B 105.0 . . ?

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
C22 C23 C24 C19 -2(2) . . . . ?
Br1 C23 C24 C19 179.8(10) . . . . ?
C13 N4 C17 N5 177.7(12) . . . . ?
Cu1 N4 C17 N5 -0.5(15) . . . . ?
C13 N4 C17 C16 -3.6(18) . . . . ?
Cu1 N4 C17 C16 178.1(11) . . . . ?
N6 N5 C17 N4 -2.8(18) . . . . ?
N6 N5 C17 C16 178.5(12) . . . . ?
C17 N5 N6 C18 -157.7(12) . . . . ?
C17 N5 N6 Cu1 4.5(14) . . . . ?
C7 C6 N1 N2 -177.6(12) . . . . ?
C7 C6 N1 Cu1 20(2) . . . . ?
C10 C9 C8 C7 -2(2) . . . . ?
Br4 C9 C8 C7 -179.4(11) . . . . ?
C8 C9 C10 C11 -1(2) . . . . ?
Br4 C9 C10 C11 176.8(13) . . . . ?
N4 C17 C16 C15 5(2) . . . . ?
N5 C17 C16 C15 -176.7(14) . . . . ?
C6 N1 N2 C5 -170.7(13) . . . . ?
Cu1 N1 N2 C5 -4.0(15) . . . . ?
C1 N3 C5 N2 179.7(13) . . . . ?
Cu1 N3 C5 N2 -5.9(16) . . . . ?
C1 N3 C5 C4 1(2) . . . . ?
Cu1 N3 C5 C4 175.2(11) . . . . ?
N1 N2 C5 N3 6.9(19) . . . . ?
N1 N2 C5 C4 -174.2(13) . . . . ?
C3 C4 C5 N3 1(2) . . . . ?
C3 C4 C5 N2 -178.1(14) . . . . ?
N5 N6 C18 C19 -177.1(12) . . . . ?
Cu1 N6 C18 C19 26(2) . . . . ?
C22 C21 C20 O1 -178.3(14) . . . . ?
C22 C21 C20 C19 2(2) . . . . ?
C5 N3 C1 C2 -1(2) . . . . ?
Cu1 N3 C1 C2 -174.3(12) . . . . ?
C5 N3 C1 Br2 179.4(10) . . . . ?
Cu1 N3 C1 Br2 6.3(17) . . . . ?
C24 C23 C22 C21 1(2) . . . . ?
Br1 C23 C22 C21 179.5(12) . . . . ?
C20 C21 C22 C23 -1(2) . . . . ?
C9 C8 C7 C12 3(2) . . . . ?
C9 C8 C7 C6 178.9(13) . . . . ?
O2 C12 C7 C8 178.1(14) . . . . ?
C11 C12 C7 C8 -2(2) . . . . ?
O2 C12 C7 C6 2(2) . . . . ?
C11 C12 C7 C6 -178.1(14) . . . . ?
N1 C6 C7 C8 27(2) . . . . ?
N1 C6 C7 C12 -157.1(15) . . . . ?
N3 C1 C2 C3 0(3) . . . . ?
Br2 C1 C2 C3 179.3(13) . . . . ?
C9 C10 C11 C12 2(3) . . . . ?
O2 C12 C11 C10 179.6(17) . . . . ?
C7 C12 C11 C10 0(3) . . . . ?
C23 C24 C19 C20 2.4(19) . . . . ?
C23 C24 C19 C18 -176.6(13) . . . . ?
O1 C20 C19 C24 177.7(12) . . . . ?
C21 C20 C19 C24 -2(2) . . . . ?
O1 C20 C19 C18 -3.4(19) . . . . ?
C21 C20 C19 C18 176.6(13) . . . . ?
N6 C18 C19 C24 25(2) . . . . ?
N6 C18 C19 C20 -153.5(13) . . . . ?
C17 N4 C13 C14 1(2) . . . . ?
Cu1 N4 C13 C14 178.9(12) . . . . ?
C17 N4 C13 Br3 -179.3(9) . . . . ?
Cu1 N4 C13 Br3 -1.4(15) . . . . ?
C15 C14 C13 N4 0(2) . . . . ?
C15 C14 C13 Br3 -179.1(12) . . . . ?
C5 C4 C3 C2 -2(3) . . . . ?
C1 C2 C3 C4 2(3) . . . . ?
C17 C16 C15 C14 -3(2) . . . . ?
C13 C14 C15 C16 0(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4 O6 0.93 2.58 3.45(2) 156.8 .
C6 H6 O7 0.93 2.60 3.375(18) 141.0 .
N5 H5 N7 0.86 2.68 3.52(2) 165.7 3
N5 H5 O5 0.86 2.24 3.024(17) 151.7 3
N5 H5 O6 0.86 2.40 3.148(18) 145.7 3
O1 H1 O4 0.82 2.01 2.729(14) 146.7 .
C16 H16 Br1 0.93 3.07 3.770(14) 133.6 3_545
C16 H16 O6 0.93 2.64 3.37(3) 136.6 3
N2 H2 O7 0.86 2.01 2.852(17) 165.6 .
O2 H2A O3 0.82 2.02 2.678(15) 136.4 .
C2 H2B Br1 0.93 3.02 3.687(15) 130.0 4_546
C11 H11 Br4 0.93 3.05 3.855(15) 145.7 4
O4 H4A O5 0.85 2.28 3.03(2) 146.7 2_565
O4 H4B O3 0.86 2.12 2.96(2) 169.5 .
O3 H3A O7 0.85 2.03 2.755(19) 143.0 2
O3 H3B O2 0.85 2.39 3.111(16) 143.0 2

_refine_diff_density_max         0.936
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.084

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_CU_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2072365'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C23H17ClCuN6O2, 2(C23H15ClCuN6O), CH4O, 6(H2O)'
_chemical_formula_sum            'C70 H63 Cl3 Cu3 N18 O11'
_chemical_formula_weight         1629.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0147 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3292 0.5397 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -2.8874 3.6899 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   20.5906(5)
_cell_length_b                   12.3240(2)
_cell_length_c                   28.4849(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.204(2)
_cell_angle_gamma                90
_cell_volume                     6941.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17793
_cell_measurement_theta_min      2.9170
_cell_measurement_theta_max      60.0480

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_F_000             3340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    6.011
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_T_max  0.382
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.3415
_diffrn_radiation_type           GaK\a
_diffrn_source                   'micro-focus metaljet'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            55337
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.936
_diffrn_reflns_theta_max         60.650
_diffrn_reflns_theta_full        53.543
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             15483
_reflns_number_gt                11304
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²+8.7473P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15483
_refine_ls_number_parameters     976
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1319
_refine_ls_wR_factor_gt          0.1185
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu3 Cu 1.40935(2) 0.73558(4) 0.87691(2) 0.02274(11) Uani 1 1 d . . . . .
Cu2 Cu 0.75192(2) 0.55105(4) 0.59509(2) 0.02726(12) Uani 1 1 d . . . . .
Cu1 Cu 0.89161(2) 0.54258(4) 0.84072(2) 0.02879(12) Uani 1 1 d . . . . .
Cl1 Cl 1.05858(4) 0.50856(7) 0.82347(3) 0.03073(17) Uani 1 1 d . . . . .
Cl3 Cl 1.57865(4) 0.80392(7) 0.87540(3) 0.03563(19) Uani 1 1 d . . . . .
Cl2 Cl 0.89180(5) 0.54502(8) 0.53893(3) 0.0449(2) Uani 1 1 d . . . . .
O3 O 1.35858(10) 0.74436(17) 0.92477(8) 0.0271(5) Uani 1 1 d . . . . .
O2 O 0.65392(11) 0.54071(18) 0.57662(8) 0.0312(5) Uani 1 1 d . . . . .
N14 N 1.48989(12) 0.6971(2) 0.93313(9) 0.0227(5) Uani 1 1 d . . . . .
O1 O 0.82860(13) 0.4623(2) 0.86699(10) 0.0460(7) Uani 1 1 d . . . . .
N4 N 0.94352(13) 0.6141(2) 0.79575(9) 0.0265(6) Uani 1 1 d . . . . .
N12 N 0.75866(14) 0.5120(2) 0.66218(10) 0.0292(6) Uani 1 1 d . . . . .
N13 N 1.41627(13) 0.5552(2) 0.86651(9) 0.0262(6) Uani 1 1 d . . . . .
N1 N 0.96682(13) 0.4654(2) 0.88990(9) 0.0278(6) Uani 1 1 d . . . . .
N18 N 1.32858(14) 0.7543(2) 0.82291(10) 0.0297(6) Uani 1 1 d . . . . .
N7 N 0.76271(13) 0.7325(2) 0.60205(9) 0.0263(6) Uani 1 1 d . . . . .
N16 N 1.45289(13) 0.7784(2) 0.82328(9) 0.0265(6) Uani 1 1 d . . . . .
N3 N 1.03240(13) 0.6605(2) 0.76007(9) 0.0292(6) Uani 1 1 d . . . . .
N10 N 0.85326(14) 0.5133(2) 0.61879(9) 0.0301(6) Uani 1 1 d . . . . .
N11 N 0.82191(14) 0.4830(2) 0.69159(10) 0.0321(6) Uani 1 1 d . . . . .
N5 N 0.83857(14) 0.7066(2) 0.76912(10) 0.0318(6) Uani 1 1 d . . . . .
N6 N 0.82045(14) 0.6337(2) 0.80037(10) 0.0301(6) Uani 1 1 d . . . . .
N8 N 0.74283(14) 0.5944(2) 0.52554(9) 0.0302(6) Uani 1 1 d . . . . .
N17 N 1.33834(15) 0.7679(3) 0.77690(10) 0.0374(7) Uani 1 1 d . . . . .
N15 N 1.53718(15) 0.8203(3) 0.78265(11) 0.0395(7) Uani 1 1 d . . . . .
N2 N 0.93286(17) 0.6747(2) 0.89922(11) 0.0409(7) Uani 1 1 d . . . . .
C16 C 0.90134(16) 0.6917(3) 0.76738(11) 0.0272(7) Uani 1 1 d . . . . .
N9 N 0.97004(16) 0.4930(3) 0.62153(12) 0.0435(7) Uani 1 1 d . . . . .
C58 C 1.46850(15) 0.5145(2) 0.90219(11) 0.0228(6) Uani 1 1 d . . . . .
C50 C 1.48462(16) 0.4040(3) 0.90661(11) 0.0268(7) Uani 1 1 d . . . . .
C56 C 1.52432(16) 0.7665(3) 0.96670(11) 0.0271(7) Uani 1 1 d . . . . .
H56A H 1.5119 0.8409 0.9636 0.033 Uiso 1 1 calc R U . . .
C57 C 1.50757(15) 0.5903(3) 0.93782(11) 0.0234(6) Uani 1 1 d . . . . .
C54 C 1.59585(15) 0.6274(3) 1.01144(12) 0.0301(7) Uani 1 1 d . . . . .
H54A H 1.6319 0.6044 1.0384 0.036 Uiso 1 1 calc R U . . .
C69 C 1.29224(15) 0.7420(2) 0.91600(12) 0.0264(7) Uani 1 1 d . . . . .
C51 C 1.54003(17) 0.3675(3) 0.94625(12) 0.0311(7) Uani 1 1 d . . . . .
H51A H 1.5517 0.2927 0.9488 0.037 Uiso 1 1 calc R U . . .
C25 C 0.77608(16) 0.9124(3) 0.63529(13) 0.0319(7) Uani 1 1 d . . . . .
H25A H 0.7820 0.9577 0.6632 0.038 Uiso 1 1 calc R U . . .
C27 C 0.76306(15) 0.8880(3) 0.54970(12) 0.0282(7) Uani 1 1 d . . . . .
C26 C 0.77269(16) 0.9560(3) 0.59055(13) 0.0313(7) Uani 1 1 d . . . . .
H26A H 0.7768 1.0322 0.5871 0.038 Uiso 1 1 calc R U . . .
C28 C 0.75859(15) 0.7755(3) 0.55733(11) 0.0258(6) Uani 1 1 d . . . . .
C13 C 1.00512(16) 0.6061(3) 0.78903(11) 0.0260(6) Uani 1 1 d . . . . .
C29 C 0.74826(15) 0.7018(3) 0.51699(11) 0.0271(7) Uani 1 1 d . . . . .
C55 C 1.57789(15) 0.7348(3) 1.00637(11) 0.0287(7) Uani 1 1 d . . . . .
H55A H 1.6015 0.7869 1.0295 0.034 Uiso 1 1 calc R U . . .
C41 C 0.64043(18) 0.5354(3) 0.65832(12) 0.0311(7) Uani 1 1 d . . . . .
C53 C 1.56088(15) 0.5515(3) 0.97676(11) 0.0267(7) Uani 1 1 d . . . . .
C5 C 1.00451(16) 0.5230(3) 0.92852(11) 0.0287(7) Uani 1 1 d . . . . .
C40 C 0.71044(18) 0.5151(3) 0.68297(12) 0.0320(7) Uani 1 1 d . . . . .
H40A H 0.7221 0.5031 0.7172 0.038 Uiso 1 1 calc R U . . .
C68 C 1.26480(17) 0.7422(3) 0.95627(13) 0.0313(7) Uani 1 1 d . . . . .
H68A H 1.2944 0.7434 0.9885 0.038 Uiso 1 1 calc R U . . .
C46 C 0.61510(17) 0.5415(2) 0.60634(12) 0.0295(7) Uani 1 1 d . . . . .
C33 C 0.74385(16) 0.7427(3) 0.47010(12) 0.0326(8) Uani 1 1 d . . . . .
C52 C 1.57567(16) 0.4380(3) 0.97986(12) 0.0306(7) Uani 1 1 d . . . . .
H52A H 1.6114 0.4117 1.0062 0.037 Uiso 1 1 calc R U . . .
C49 C 1.44315(18) 0.3337(3) 0.87160(12) 0.0325(8) Uani 1 1 d . . . . .
H49A H 1.4520 0.2579 0.8730 0.039 Uiso 1 1 calc R U . . .
C4 C 1.05887(16) 0.4759(3) 0.96425(12) 0.0328(8) Uani 1 1 d . . . . .
C59 C 1.51568(17) 0.8003(3) 0.82060(12) 0.0303(7) Uani 1 1 d . . . . .
C39 C 0.86825(17) 0.4838(3) 0.66789(12) 0.0302(7) Uani 1 1 d . . . . .
C15 C 0.92723(18) 0.7559(3) 0.73511(12) 0.0336(8) Uani 1 1 d . . . . .
H15B H 0.9000 0.8103 0.7155 0.040 Uiso 1 1 calc R U . . .
C47 C 1.37817(17) 0.4869(3) 0.83426(11) 0.0293(7) Uani 1 1 d . . . . .
H47A H 1.3413 0.5150 0.8092 0.035 Uiso 1 1 calc R U . . .
C65 C 1.17606(17) 0.7352(3) 0.86348(14) 0.0360(8) Uani 1 1 d . . . . .
H65A H 1.1456 0.7319 0.8316 0.043 Uiso 1 1 calc R U . . .
C17 C 0.75896(16) 0.6399(3) 0.80261(12) 0.0318(7) Uani 1 1 d . . . . .
H17B H 0.7312 0.6950 0.7838 0.038 Uiso 1 1 calc R U . . .
C48 C 1.39038(18) 0.3751(3) 0.83584(12) 0.0325(7) Uani 1 1 d . . . . .
H48A H 1.3622 0.3284 0.8122 0.039 Uiso 1 1 calc R U . . .
C24 C 0.77061(16) 0.7994(3) 0.63934(12) 0.0296(7) Uani 1 1 d . . . . .
H24A H 0.7727 0.7697 0.6705 0.036 Uiso 1 1 calc R U . . .
C1 C 0.98021(17) 0.3615(3) 0.88640(12) 0.0299(7) Uani 1 1 d . . . . .
H1A H 0.9524 0.3207 0.8601 0.036 Uiso 1 1 calc R U . . .
C18 C 0.72887(17) 0.5703(3) 0.83115(12) 0.0314(7) Uani 1 1 d . . . . .
C14 C 0.99108(18) 0.7383(3) 0.73285(12) 0.0339(8) Uani 1 1 d . . . . .
H14A H 1.0081 0.7818 0.7114 0.041 Uiso 1 1 calc R U . . .
C62 C 1.40265(18) 0.7814(3) 0.77923(12) 0.0336(8) Uani 1 1 d . . . . .
C34 C 0.74637(16) 0.8575(3) 0.46330(13) 0.0356(8) Uani 1 1 d . . . . .
H34A H 0.7413 0.8856 0.4314 0.043 Uiso 1 1 calc R U . . .
C63 C 1.26672(16) 0.7467(3) 0.82475(12) 0.0325(8) Uani 1 1 d . . . . .
H63A H 1.2322 0.7460 0.7946 0.039 Uiso 1 1 calc R U . . .
C6 C 0.98718(19) 0.6344(3) 0.93343(12) 0.0352(8) Uani 1 1 d . . . . .
C2 C 1.03364(18) 0.3091(3) 0.91978(13) 0.0357(8) Uani 1 1 d . . . . .
H2A H 1.0427 0.2347 0.9156 0.043 Uiso 1 1 calc R U . . .
C64 C 1.24609(16) 0.7394(3) 0.86890(12) 0.0298(7) Uani 1 1 d . . . . .
C67 C 1.19558(19) 0.7407(3) 0.94972(15) 0.0382(8) Uani 1 1 d . . . . .
H67A H 1.1787 0.7431 0.9775 0.046 Uiso 1 1 calc R U . . .
C35 C 0.75582(16) 0.9261(3) 0.50112(13) 0.0338(8) Uani 1 1 d . . . . .
H35A H 0.7578 1.0019 0.4955 0.041 Uiso 1 1 calc R U . . .
C3 C 1.07282(17) 0.3665(3) 0.95862(12) 0.0356(8) Uani 1 1 d . . . . .
H3B H 1.1094 0.3320 0.9817 0.043 Uiso 1 1 calc R U . . .
C45 C 0.54427(17) 0.5488(3) 0.58650(13) 0.0326(7) Uani 1 1 d . . . . .
H45A H 0.5257 0.5500 0.5520 0.039 Uiso 1 1 calc R U . . .
C44 C 0.50150(19) 0.5542(3) 0.61574(14) 0.0388(8) Uani 1 1 d . . . . .
H44A H 0.4541 0.5588 0.6011 0.047 Uiso 1 1 calc R U . . .
C42 C 0.5950(2) 0.5428(3) 0.68714(14) 0.0385(8) Uani 1 1 d . . . . .
H42A H 0.6122 0.5407 0.7217 0.046 Uiso 1 1 calc R U . . .
C32 C 0.73527(18) 0.6672(3) 0.43172(13) 0.0394(9) Uani 1 1 d . . . . .
H32A H 0.7332 0.6914 0.3997 0.047 Uiso 1 1 calc R U . . .
C19 C 0.65975(17) 0.5885(3) 0.82774(13) 0.0361(8) Uani 1 1 d . . . . .
H19A H 0.6366 0.6469 0.8083 0.043 Uiso 1 1 calc R U . . .
C23 C 0.76357(17) 0.4843(3) 0.86020(12) 0.0340(8) Uani 1 1 d . . . . .
C20 C 0.62542(19) 0.5232(3) 0.85202(14) 0.0431(9) Uani 1 1 d . . . . .
H20A H 0.5793 0.5369 0.8500 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6593(2) 0.4370(3) 0.87951(14) 0.0430(9) Uani 1 1 d . . . . .
H21A H 0.6356 0.3904 0.8956 0.052 Uiso 1 1 calc R U . . .
C43 C 0.5265(2) 0.5529(3) 0.66663(15) 0.0410(9) Uani 1 1 d . . . . .
H43A H 0.4967 0.5590 0.6867 0.049 Uiso 1 1 calc R U . . .
C66 C 1.15061(18) 0.7358(3) 0.90357(15) 0.0405(9) Uani 1 1 d . . . . .
H66A H 1.1032 0.7329 0.8995 0.049 Uiso 1 1 calc R U . . .
C22 C 0.72636(19) 0.4175(3) 0.88401(13) 0.0382(8) Uani 1 1 d . . . . .
H22A H 0.7483 0.3582 0.9034 0.046 Uiso 1 1 calc R U . . .
C38 C 0.93582(18) 0.4537(3) 0.69304(13) 0.0371(8) Uani 1 1 d . . . . .
H38A H 0.9468 0.4293 0.7260 0.044 Uiso 1 1 calc R U . . .
C12 C 1.09458(18) 0.5407(4) 1.00550(13) 0.0439(10) Uani 1 1 d . . . . .
H12A H 1.1302 0.5087 1.0303 0.053 Uiso 1 1 calc R U . . .
C10 C 1.0246(2) 0.6954(3) 0.97381(14) 0.0435(9) Uani 1 1 d . . . . .
C36 C 0.90644(19) 0.5136(3) 0.60054(13) 0.0358(8) Uani 1 1 d . . . . .
C37 C 0.9835(2) 0.4604(3) 0.66942(14) 0.0434(9) Uani 1 1 d . . . . .
H37A H 1.0286 0.4418 0.6865 0.052 Uiso 1 1 calc R U . . .
C60 C 1.4871(2) 0.8206(4) 0.73938(14) 0.0498(10) Uani 1 1 d . . . . .
H60A H 1.4994 0.8348 0.7102 0.060 Uiso 1 1 calc R U . . .
C30 C 0.7336(2) 0.5258(3) 0.48811(13) 0.0421(9) Uani 1 1 d . . . . .
H30A H 0.7293 0.4506 0.4939 0.050 Uiso 1 1 calc R U . . .
C11 C 1.0788(2) 0.6444(4) 1.00973(14) 0.0471(10) Uani 1 1 d . . . . .
H11B H 1.1039 0.6852 1.0371 0.056 Uiso 1 1 calc R U . . .
C61 C 1.4217(2) 0.8020(4) 0.73565(13) 0.0479(10) Uani 1 1 d . . . . .
H61A H 1.3888 0.8026 0.7047 0.057 Uiso 1 1 calc R U . . .
C31 C 0.7300(2) 0.5600(4) 0.44053(13) 0.0467(10) Uani 1 1 d . . . . .
H31A H 0.7239 0.5087 0.4148 0.056 Uiso 1 1 calc R U . . .
C7 C 0.9149(3) 0.7766(3) 0.90399(16) 0.0543(12) Uani 1 1 d . . . . .
H7A H 0.8770 0.8055 0.8801 0.065 Uiso 1 1 calc R U . . .
C9 C 1.0037(3) 0.8029(4) 0.97742(17) 0.0604(14) Uani 1 1 d . . . . .
H9B H 1.0274 0.8473 1.0040 0.072 Uiso 1 1 calc R U . . .
C8 C 0.9492(3) 0.8435(4) 0.94273(18) 0.0686(16) Uani 1 1 d . . . . .
H8A H 0.9349 0.9161 0.9448 0.082 Uiso 1 1 calc R U . . .
O5 O 0.59857(13) 0.3954(2) 0.49972(9) 0.0414(6) Uani 1 1 d . . . . .
O8 O 0.77018(13) 0.9094(2) 0.75161(9) 0.0426(6) Uani 1 1 d . . . . .
O6 O 0.87208(14) 0.3796(2) 0.78238(9) 0.0471(7) Uani 1 1 d . . . . .
O7 O 1.0834(2) 0.5905(4) 0.5967(3) 0.161(3) Uani 1 1 d . . . . .
H7C H 1.0466 0.5746 0.6032 0.242 Uiso 1 1 d R U . . .
H7D H 1.1130 0.5908 0.6243 0.242 Uiso 1 1 d R U . . .
H8D H 0.7955 0.9560 0.7697 0.242 Uiso 1 1 d R U . . .
H8C H 0.7898 0.8490 0.7593 0.242 Uiso 1 1 d R U . . .
H6D H 0.8437 0.3401 0.7906 0.242 Uiso 1 1 d R U . . .
H5C H 0.6107 0.4475 0.5198 0.242 Uiso 1 1 d R U . . .
H6C H 0.8487 0.4162 0.7577 0.242 Uiso 1 1 d R U . . .
H5D H 0.6116 0.3384 0.5157 0.242 Uiso 1 1 d R U . . .
O1W O 1.1981(5) 0.6822(8) 0.5864(3) 0.098(3) Uani 0.467(4) 1 d . . P . .
H1WA H 1.1689 0.6355 0.5721 0.146 Uiso 0.467(4) 1 d R U P . .
H1WB H 1.2232 0.6913 0.5676 0.146 Uiso 0.467(4) 1 d R U P . .
O1W' O 1.3391(3) 0.6859(4) 0.57845(18) 0.0455(14) Uani 0.533(4) 1 d . . P A 1
H1WC H 1.3718 0.6464 0.5759 0.068 Uiso 0.533(4) 1 d R U P A 1
H1WD H 1.3283 0.7236 0.5525 0.068 Uiso 0.533(4) 1 d R U P A 1
O9 O 0.67841(16) 0.9138(3) 0.80715(13) 0.0771(11) Uani 1 1 d . . . . .
H9C H 0.6402 0.8861 0.7927 0.116 Uiso 1 1 d R U . . .
H9D H 0.6992 0.9171 0.7853 0.116 Uiso 1 1 d R U . . .
H10A H 1.1493 0.6417 0.7071 0.116 Uiso 1 1 d R U . . .
H10B H 1.1142 0.6084 0.7379 0.116 Uiso 1 1 d R U . . .
O10 O 1.14505(14) 0.5890(2) 0.72512(12) 0.0550(8) Uani 1 1 d . . . . .
C70 C 1.3430(5) 0.5890(7) 0.6693(3) 0.059(3) Uani 0.467(4) 1 d D . P A 2
C70A H 1.3822 0.6369 0.6737 0.088 Uiso 0.467(4) 1 calc R U P A 2
C70B H 1.3294 0.5618 0.6356 0.088 Uiso 0.467(4) 1 calc R U P A 2
C70C H 1.3549 0.5277 0.6920 0.088 Uiso 0.467(4) 1 calc R U P A 2
O11 O 1.2917(3) 0.6443(5) 0.6782(2) 0.0511(17) Uani 0.467(4) 1 d D . P A 2
H11C H 1.3128 0.6707 0.7044 0.077 Uiso 0.467(4) 1 d R U P A 2
C70' C 1.2293(3) 0.7345(5) 0.6945(2) 0.0298(15) Uani 0.533(4) 1 d D . P A 1
C70D H 1.2543 0.8018 0.6936 0.045 Uiso 0.533(4) 1 calc R U P A 1
C70E H 1.2585 0.6721 0.6936 0.045 Uiso 0.533(4) 1 calc R U P A 1
C70F H 1.2153 0.7321 0.7246 0.045 Uiso 0.533(4) 1 calc R U P A 1
O11' O 1.1705(3) 0.7308(5) 0.6529(2) 0.0619(17) Uani 0.533(4) 1 d D . P A 1
H11F H 1.1636 0.7457 0.6235 0.093 Uiso 0.533(4) 1 d R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu3 N18 1.939(3) . ?
Cu3 O3 1.939(2) . ?
Cu3 N14 2.014(2) . ?
Cu3 N16 2.045(3) . ?
Cu3 N13 2.252(3) . ?
Cu2 N12 1.938(3) . ?
Cu2 O2 1.942(2) . ?
Cu2 N8 2.009(3) . ?
Cu2 N10 2.059(3) . ?
Cu2 N7 2.251(3) . ?
Cu1 O1 1.940(3) . ?
Cu1 N6 1.946(3) . ?
Cu1 N1 2.014(3) . ?
Cu1 N4 2.079(3) . ?
Cu1 N2 2.315(3) . ?
Cl1 C13 1.737(3) . ?
Cl3 C59 1.729(3) . ?
Cl2 C36 1.740(4) . ?
O3 C69 1.318(4) . ?
O2 C46 1.316(4) . ?
N14 C56 1.330(4) . ?
N14 C57 1.363(4) . ?
O1 C23 1.326(4) . ?
N4 C13 1.338(4) . ?
N4 C16 1.390(4) . ?
N12 C40 1.291(4) . ?
N12 N11 1.385(4) . ?
N13 C47 1.329(4) . ?
N13 C58 1.354(4) . ?
N1 C1 1.320(4) . ?
N1 C5 1.356(4) . ?
N18 C63 1.293(4) . ?
N18 N17 1.390(4) . ?
N7 C24 1.318(4) . ?
N7 C28 1.360(4) . ?
N16 C59 1.344(4) . ?
N16 C62 1.386(4) . ?
N3 C13 1.305(4) . ?
N3 C14 1.369(4) . ?
N10 C36 1.337(5) . ?
N10 C39 1.393(4) . ?
N11 C39 1.314(4) . ?
N5 C16 1.320(4) . ?
N5 N6 1.388(4) . ?
N6 C17 1.288(4) . ?
N8 C30 1.332(4) . ?
N8 C29 1.356(4) . ?
N17 C62 1.318(4) . ?
N15 C59 1.301(4) . ?
N15 C60 1.369(5) . ?
N2 C7 1.327(5) . ?
N2 C6 1.356(5) . ?
C16 C15 1.424(5) . ?
N9 C36 1.304(5) . ?
N9 C37 1.374(5) . ?
C58 C50 1.399(4) . ?
C58 C57 1.447(4) . ?
C50 C49 1.414(5) . ?
C50 C51 1.435(4) . ?
C56 C55 1.396(4) . ?
C57 C53 1.408(4) . ?
C54 C55 1.371(5) . ?
C54 C53 1.404(5) . ?
C69 C64 1.412(5) . ?
C69 C68 1.413(5) . ?
C51 C52 1.349(5) . ?
C25 C26 1.367(5) . ?
C25 C24 1.404(5) . ?
C27 C26 1.403(5) . ?
C27 C28 1.410(4) . ?
C27 C35 1.429(5) . ?
C28 C29 1.433(5) . ?
C29 C33 1.407(4) . ?
C41 C42 1.410(5) . ?
C41 C46 1.428(5) . ?
C41 C40 1.438(5) . ?
C53 C52 1.429(5) . ?
C5 C4 1.411(5) . ?
C5 C6 1.435(5) . ?
C68 C67 1.385(5) . ?
C46 C45 1.412(5) . ?
C33 C32 1.409(5) . ?
C33 C34 1.431(5) . ?
C49 C48 1.364(5) . ?
C4 C3 1.397(5) . ?
C4 C12 1.441(5) . ?
C39 C38 1.425(5) . ?
C15 C14 1.352(5) . ?
C47 C48 1.399(5) . ?
C65 C66 1.383(5) . ?
C65 C64 1.408(5) . ?
C17 C18 1.435(5) . ?
C1 C2 1.395(5) . ?
C18 C23 1.411(5) . ?
C18 C19 1.417(5) . ?
C62 C61 1.425(5) . ?
C34 C35 1.340(5) . ?
C63 C64 1.438(5) . ?
C6 C10 1.409(5) . ?
C2 C3 1.370(5) . ?
C67 C66 1.382(5) . ?
C45 C44 1.372(5) . ?
C44 C43 1.396(5) . ?
C42 C43 1.374(5) . ?
C32 C31 1.354(6) . ?
C19 C20 1.378(5) . ?
C23 C22 1.419(5) . ?
C20 C21 1.387(6) . ?
C21 C22 1.371(5) . ?
C38 C37 1.338(5) . ?
C12 C11 1.333(6) . ?
C10 C9 1.406(6) . ?
C10 C11 1.431(6) . ?
C60 C61 1.340(6) . ?
C30 C31 1.402(5) . ?
C7 C8 1.401(7) . ?
C9 C8 1.365(7) . ?
C70 O11 1.338(8) . ?
C70' O11' 1.441(6) . ?

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
N18 Cu3 O3 92.28(11) . . ?
N18 Cu3 N14 173.03(11) . . ?
O3 Cu3 N14 86.57(9) . . ?
N18 Cu3 N16 80.47(11) . . ?
O3 Cu3 N16 161.08(10) . . ?
N14 Cu3 N16 102.67(10) . . ?
N18 Cu3 N13 94.85(11) . . ?
O3 Cu3 N13 102.36(9) . . ?
N14 Cu3 N13 78.71(10) . . ?
N16 Cu3 N13 95.69(10) . . ?
N12 Cu2 O2 91.94(11) . . ?
N12 Cu2 N8 178.40(12) . . ?
O2 Cu2 N8 86.93(10) . . ?
N12 Cu2 N10 80.41(11) . . ?
O2 Cu2 N10 162.76(10) . . ?
N8 Cu2 N10 100.98(11) . . ?
N12 Cu2 N7 100.47(10) . . ?
O2 Cu2 N7 99.12(9) . . ?
N8 Cu2 N7 78.61(10) . . ?
N10 Cu2 N7 97.46(10) . . ?
O1 Cu1 N6 92.73(11) . . ?
O1 Cu1 N1 87.59(11) . . ?
N6 Cu1 N1 171.62(11) . . ?
O1 Cu1 N4 165.42(11) . . ?
N6 Cu1 N4 79.84(11) . . ?
N1 Cu1 N4 101.59(10) . . ?
O1 Cu1 N2 103.38(11) . . ?
N6 Cu1 N2 94.80(12) . . ?
N1 Cu1 N2 77.00(11) . . ?
N4 Cu1 N2 89.82(10) . . ?
C69 O3 Cu3 126.8(2) . . ?
C46 O2 Cu2 126.6(2) . . ?
C56 N14 C57 118.4(3) . . ?
C56 N14 Cu3 125.2(2) . . ?
C57 N14 Cu3 116.3(2) . . ?
C23 O1 Cu1 126.6(2) . . ?
C13 N4 C16 115.5(3) . . ?
C13 N4 Cu1 136.7(2) . . ?
C16 N4 Cu1 107.7(2) . . ?
C40 N12 N11 116.4(3) . . ?
C40 N12 Cu2 126.3(2) . . ?
N11 N12 Cu2 117.2(2) . . ?
C47 N13 C58 118.4(3) . . ?
C47 N13 Cu3 132.0(2) . . ?
C58 N13 Cu3 109.5(2) . . ?
C1 N1 C5 119.0(3) . . ?
C1 N1 Cu1 122.8(2) . . ?
C5 N1 Cu1 118.2(2) . . ?
C63 N18 N17 116.8(3) . . ?
C63 N18 Cu3 126.6(2) . . ?
N17 N18 Cu3 116.4(2) . . ?
C24 N7 C28 118.2(3) . . ?
C24 N7 Cu2 132.8(2) . . ?
C28 N7 Cu2 109.0(2) . . ?
C59 N16 C62 115.5(3) . . ?
C59 N16 Cu3 136.4(2) . . ?
C62 N16 Cu3 108.1(2) . . ?
C13 N3 C14 114.1(3) . . ?
C36 N10 C39 114.5(3) . . ?
C36 N10 Cu2 137.5(2) . . ?
C39 N10 Cu2 108.0(2) . . ?
C39 N11 N12 112.5(3) . . ?
C16 N5 N6 112.0(3) . . ?
C17 N6 N5 115.9(3) . . ?
C17 N6 Cu1 126.4(2) . . ?
N5 N6 Cu1 117.4(2) . . ?
C30 N8 C29 118.4(3) . . ?
C30 N8 Cu2 125.0(2) . . ?
C29 N8 Cu2 116.5(2) . . ?
C62 N17 N18 112.1(3) . . ?
C59 N15 C60 113.7(3) . . ?
C7 N2 C6 118.1(4) . . ?
C7 N2 Cu1 133.0(3) . . ?
C6 N2 Cu1 108.8(2) . . ?
N5 C16 N4 122.2(3) . . ?
N5 C16 C15 119.6(3) . . ?
N4 C16 C15 118.2(3) . . ?
C36 N9 C37 114.2(3) . . ?
N13 C58 C50 123.2(3) . . ?
N13 C58 C57 117.2(3) . . ?
C50 C58 C57 119.6(3) . . ?
C58 C50 C49 116.8(3) . . ?
C58 C50 C51 119.5(3) . . ?
C49 C50 C51 123.6(3) . . ?
N14 C56 C55 123.0(3) . . ?
N14 C57 C53 122.2(3) . . ?
N14 C57 C58 118.3(3) . . ?
C53 C57 C58 119.5(3) . . ?
C55 C54 C53 119.9(3) . . ?
O3 C69 C64 124.6(3) . . ?
O3 C69 C68 118.3(3) . . ?
C64 C69 C68 117.1(3) . . ?
C52 C51 C50 120.8(3) . . ?
C26 C25 C24 118.8(3) . . ?
C26 C27 C28 117.4(3) . . ?
C26 C27 C35 124.0(3) . . ?
C28 C27 C35 118.6(3) . . ?
C25 C26 C27 119.8(3) . . ?
N7 C28 C27 122.5(3) . . ?
N7 C28 C29 117.4(3) . . ?
C27 C28 C29 120.1(3) . . ?
N3 C13 N4 130.2(3) . . ?
N3 C13 Cl1 113.3(2) . . ?
N4 C13 Cl1 116.5(2) . . ?
N8 C29 C33 122.3(3) . . ?
N8 C29 C28 118.4(3) . . ?
C33 C29 C28 119.3(3) . . ?
C54 C55 C56 118.9(3) . . ?
C42 C41 C46 119.4(3) . . ?
C42 C41 C40 117.7(3) . . ?
C46 C41 C40 122.8(3) . . ?
C54 C53 C57 117.5(3) . . ?
C54 C53 C52 123.4(3) . . ?
C57 C53 C52 119.1(3) . . ?
N1 C5 C4 121.9(3) . . ?
N1 C5 C6 118.6(3) . . ?
C4 C5 C6 119.5(3) . . ?
N12 C40 C41 125.2(3) . . ?
C67 C68 C69 121.4(3) . . ?
O2 C46 C45 119.2(3) . . ?
O2 C46 C41 123.7(3) . . ?
C45 C46 C41 117.1(3) . . ?
C29 C33 C32 117.4(3) . . ?
C29 C33 C34 119.2(3) . . ?
C32 C33 C34 123.3(3) . . ?
C51 C52 C53 121.5(3) . . ?
C48 C49 C50 119.7(3) . . ?
C3 C4 C5 117.5(3) . . ?
C3 C4 C12 123.6(3) . . ?
C5 C4 C12 118.8(4) . . ?
N15 C59 N16 129.9(3) . . ?
N15 C59 Cl3 113.7(3) . . ?
N16 C59 Cl3 116.4(2) . . ?
N11 C39 N10 121.9(3) . . ?
N11 C39 C38 119.1(3) . . ?
N10 C39 C38 119.0(3) . . ?
C14 C15 C16 119.1(3) . . ?
N13 C47 C48 122.4(3) . . ?
C66 C65 C64 121.5(3) . . ?
N6 C17 C18 125.3(3) . . ?
C49 C48 C47 119.4(3) . . ?
N7 C24 C25 123.3(3) . . ?
N1 C1 C2 122.6(3) . . ?
C23 C18 C19 119.6(3) . . ?
C23 C18 C17 123.6(3) . . ?
C19 C18 C17 116.8(3) . . ?
C15 C14 N3 123.0(3) . . ?
N17 C62 N16 121.9(3) . . ?
N17 C62 C61 119.7(3) . . ?
N16 C62 C61 118.4(3) . . ?
C35 C34 C33 121.2(3) . . ?
N18 C63 C64 125.1(3) . . ?
N2 C6 C10 123.0(4) . . ?
N2 C6 C5 117.3(3) . . ?
C10 C6 C5 119.7(3) . . ?
C3 C2 C1 119.1(3) . . ?
C65 C64 C69 120.2(3) . . ?
C65 C64 C63 116.7(3) . . ?
C69 C64 C63 123.0(3) . . ?
C66 C67 C68 121.3(4) . . ?
C34 C35 C27 121.6(3) . . ?
C2 C3 C4 119.8(3) . . ?
C44 C45 C46 121.8(3) . . ?
C45 C44 C43 121.1(3) . . ?
C43 C42 C41 121.9(3) . . ?
C31 C32 C33 120.0(3) . . ?
C20 C19 C18 121.3(4) . . ?
O1 C23 C18 124.3(3) . . ?
O1 C23 C22 118.0(3) . . ?
C18 C23 C22 117.6(3) . . ?
C19 C20 C21 118.9(3) . . ?
C22 C21 C20 121.5(4) . . ?
C42 C43 C44 118.6(4) . . ?
C67 C66 C65 118.6(3) . . ?
C21 C22 C23 121.1(4) . . ?
C37 C38 C39 118.8(3) . . ?
C11 C12 C4 121.5(4) . . ?
C9 C10 C6 116.9(4) . . ?
C9 C10 C11 123.7(4) . . ?
C6 C10 C11 119.3(4) . . ?
N9 C36 N10 130.4(3) . . ?
N9 C36 Cl2 112.0(3) . . ?
N10 C36 Cl2 117.6(3) . . ?
C38 C37 N9 123.0(3) . . ?
C61 C60 N15 124.0(3) . . ?
N8 C30 C31 122.7(4) . . ?
C12 C11 C10 121.2(4) . . ?
C60 C61 C62 118.4(4) . . ?
C32 C31 C30 119.2(4) . . ?
N2 C7 C8 122.9(5) . . ?
C8 C9 C10 119.9(4) . . ?
C9 C8 C7 119.1(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C55 H55A O2 0.95 2.58 3.515(4) 167.0 4_676
C68 H68A O1W' 0.95 2.62 3.502(6) 155.0 4_576
C15 H15B Cl1 0.95 2.91 3.583(3) 129.1 2_756
C1 H1A O6 0.95 2.47 3.179(4) 131.0 .
C2 H2A Cl2 0.95 2.83 3.650(4) 145.8 2_746
C45 H45A O5 0.95 2.66 3.335(4) 128.6 3_666
C22 H22A O1W 0.95 2.42 3.288(11) 152.5 2_746
C38 H38A O6 0.95 2.59 3.301(5) 131.9 .
C8 H8A O7 0.95 2.43 3.250(7) 144.2 2_756
O7 H7C N9 0.85 2.06 2.882(6) 163.6 .
O7 H7D O11' 0.85 2.12 2.676(8) 122.6 .
O8 H8D O10 0.85 2.03 2.782(4) 148.1 2_756
O8 H8C N5 0.85 2.00 2.844(4) 172.6 .
O6 H6D O11' 0.84 2.18 2.904(7) 143.9 2_746
O5 H5C O2 0.85 1.98 2.812(3) 165.5 .
O6 H6C N11 0.86 1.99 2.809(4) 159.2 .
O5 H5D O3 0.84 2.00 2.795(3) 156.8 2_746
O1W H1WA O7 0.85 2.14 2.707(10) 123.7 .
O1W H1WB O1W' 0.85 2.32 2.976(10) 134.2 .
O1W' H1WC O5 0.85 2.45 3.034(5) 126.4 3_766
O9 H9C N15 0.85 2.21 3.023(5) 158.9 1_455
O9 H9D O8 0.85 1.96 2.783(4) 162.3 .
O10 H10A O11' 0.85 2.04 2.857(7) 162.1 .
O10 H10B N3 0.85 2.06 2.904(4) 172.7 .
O11 H11C N17 0.82 2.32 3.106(7) 161.5 .
O11' H11F O1W 0.83 1.63 2.206(11) 124.4 .

_refine_diff_density_max         1.085
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.073

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_911L19
_database_code_depnum_ccdc_archive 'CCDC 2072364'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C25.735 H21.21 Cl0.265 Cu N6 O2.735), CH4O, 5.5(H2O)'
_chemical_formula_sum            'C103.94 H99.82 Cl1.06 Cu4 N24 O17.44'
_chemical_formula_weight         2256.00

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.2555(5)
_cell_length_b                   15.0401(7)
_cell_length_c                   17.0183(7)
_cell_angle_alpha                88.110(4)
_cell_angle_beta                 87.004(4)
_cell_angle_gamma                83.153(4)
_cell_volume                     2601.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3797
_cell_measurement_theta_min      3.5360
_cell_measurement_theta_max      23.1470

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_F_000             1165
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.912
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            17108
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.410
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             9123
_reflns_number_gt                5485
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0697P)²+2.9863P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9123
_refine_ls_number_parameters     716
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1867
_refine_ls_wR_factor_gt          0.1510
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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 0.49374(6) 0.69404(5) 0.82230(4) 0.0454(2) Uani 1 1 d . . . . .
O1 O 0.3064(3) 0.6923(2) 0.8339(2) 0.0513(9) Uani 1 1 d . . . . .
N1 N 0.8720(5) 0.7240(4) 0.7025(3) 0.0713(16) Uani 1 1 d . . . . .
Cl1 Cl 0.735(7) 0.6172(19) 0.6859(7) 0.107(2) Uani 0.265(13) 1 d D . P A 2
O11 O 0.731(6) 0.6094(17) 0.6953(6) 0.107(2) Uani 0.735(13) 1 d D . P A 1
C54 C 0.8194(13) 0.5770(9) 0.6346(8) 0.132(6) Uani 0.735(13) 1 d . . P A 1
H54A H 0.7738 0.5465 0.5979 0.198 Uiso 0.735(13) 1 calc R U P A 1
H54B H 0.8884 0.5361 0.6561 0.198 Uiso 0.735(13) 1 calc R U P A 1
H54C H 0.8565 0.6262 0.6081 0.198 Uiso 0.735(13) 1 calc R U P A 1
C1 C 0.7586(6) 0.6946(5) 0.7236(4) 0.0632(17) Uani 1 1 d D . . . .
Cu2 Cu 0.47845(8) 0.17249(5) 0.69554(4) 0.0597(3) Uani 1 1 d . . . . .
O2 O 0.0743(3) 0.6456(3) 0.8596(2) 0.0584(11) Uani 1 1 d . . . . .
N2 N 0.6631(4) 0.7331(3) 0.7734(2) 0.0491(12) Uani 1 1 d . . . . .
C2 C 0.8889(7) 0.8028(6) 0.7335(4) 0.077(2) Uani 1 1 d . . . . .
H2 H 0.9670 0.8263 0.7196 0.093 Uiso 1 1 calc R U . . .
Cl2 Cl 0.223(6) 0.3333(8) 0.6305(15) 0.106(2) Uani 0.265(13) 1 d D . P A 2
O12 O 0.237(6) 0.3193(8) 0.6342(12) 0.106(2) Uani 0.735(13) 1 d D . P A 1
C55 C 0.157(2) 0.3905(17) 0.6035(12) 0.198(9) Uani 0.735(13) 1 d . . P A 1
H55A H 0.1982 0.4443 0.6065 0.297 Uiso 0.735(13) 1 calc R U P A 1
H55B H 0.0744 0.3969 0.6331 0.297 Uiso 0.735(13) 1 calc R U P A 1
H55C H 0.1428 0.3798 0.5495 0.297 Uiso 0.735(13) 1 calc R U P A 1
O3 O 0.6638(4) 0.1682(3) 0.6725(2) 0.0620(11) Uani 1 1 d . . . . .
N3 N 0.5954(5) 0.8573(3) 0.8524(3) 0.0562(12) Uani 1 1 d . . . . .
C3 C 0.8034(6) 0.8502(5) 0.7824(4) 0.0703(18) Uani 1 1 d . . . . .
H3A H 0.8203 0.9047 0.8015 0.084 Uiso 1 1 calc R U . . .
N4 N 0.4830(4) 0.8131(3) 0.8616(2) 0.0455(11) Uani 1 1 d . . . . .
O4 O 0.9003(4) 0.1533(3) 0.6080(2) 0.0694(12) Uani 1 1 d . . . . .
C4 C 0.6839(5) 0.8125(4) 0.8040(3) 0.0529(15) Uani 1 1 d . . . . .
N5 N 0.5877(4) 0.6207(3) 0.9295(2) 0.0454(11) Uani 1 1 d . . . . .
C5 C 0.3840(6) 0.8558(4) 0.9004(3) 0.0492(14) Uani 1 1 d . . . . .
H5 H 0.3963 0.9095 0.9229 0.059 Uiso 1 1 calc R U . . .
O5 O 0.1650(6) 0.6713(5) 0.6824(3) 0.136(3) Uani 1 1 d . . . . .
H5A H 0.2468 0.6763 0.6820 0.204 Uiso 1 1 d R U . . .
H5B H 0.1278 0.7217 0.6977 0.204 Uiso 1 1 d R U . . .
N6 N 0.5102(4) 0.5661(3) 0.7907(2) 0.0480(11) Uani 1 1 d . . . . .
O6 O 0.6794(5) 0.9387(3) 0.9953(2) 0.0940(16) Uani 1 1 d . . . . .
H6A H 0.6533 0.9091 1.0352 0.141 Uiso 1 1 d R U . . .
H6B H 0.6286 0.9283 0.9590 0.141 Uiso 1 1 d R U . . .
C6 C 0.2560(6) 0.8253(4) 0.9108(3) 0.0499(14) Uani 1 1 d . . . . .
N7 N 0.0894(7) 0.3083(5) 0.7471(5) 0.106(2) Uani 1 1 d . U . . .
C7 C 0.1580(6) 0.8801(5) 0.9541(3) 0.0657(18) Uani 1 1 d . . . . .
H7 H 0.1782 0.9330 0.9748 0.079 Uiso 1 1 calc R U . . .
O7 O 0.2912(13) 0.5940(8) 0.5472(6) 0.137(5) Uani 0.5 1 d . . P . .
H7A H 0.2589 0.5714 0.5085 0.205 Uiso 0.5 1 d R U P . .
H7B H 0.2982 0.6478 0.5324 0.205 Uiso 0.5 1 d R U P . .
N8 N 0.3089(6) 0.2324(4) 0.7428(3) 0.0717(16) Uani 1 1 d . . . . .
C8 C 0.0339(7) 0.8562(5) 0.9657(4) 0.0716(19) Uani 1 1 d . . . . .
H8 H -0.0300 0.8930 0.9940 0.086 Uiso 1 1 calc R U . . .
N9 N 0.3938(8) 0.1575(5) 0.8556(3) 0.090(2) Uani 1 1 d . . . . .
C9 C 0.0032(6) 0.7778(5) 0.9358(3) 0.0615(17) Uani 1 1 d . . . . .
H9 H -0.0807 0.7611 0.9453 0.074 Uiso 1 1 calc R U . . .
N10 N 0.5059(7) 0.1467(4) 0.8071(3) 0.0729(17) Uani 1 1 d . . . . .
C10 C 0.0951(5) 0.7242(4) 0.8921(3) 0.0495(14) Uani 1 1 d . . . . .
O10 O 0.7432(14) 0.3321(8) 0.5944(7) 0.121(4) Uani 0.5 1 d D U P . .
H10 H 0.7422 0.3684 0.5574 0.182 Uiso 0.5 1 calc R U P . .
N11 N 0.3925(5) 0.0415(3) 0.6767(3) 0.0536(12) Uani 1 1 d . . . . .
C11 C 0.2246(5) 0.7471(4) 0.8771(3) 0.0460(13) Uani 1 1 d . . . . .
N12 N 0.4456(5) 0.1794(4) 0.5793(3) 0.0600(14) Uani 1 1 d . . . . .
C12 C -0.0417(6) 0.6050(5) 0.8826(4) 0.0707(19) Uani 1 1 d . . . . .
H12A H -0.1193 0.6426 0.8659 0.085 Uiso 1 1 calc R U . . .
H12B H -0.0489 0.5969 0.9394 0.085 Uiso 1 1 calc R U . . .
C13 C -0.0299(7) 0.5179(5) 0.8446(5) 0.099(3) Uani 1 1 d . . . . .
H13A H -0.0135 0.5263 0.7889 0.149 Uiso 1 1 calc R U . . .
H13B H -0.1101 0.4914 0.8541 0.149 Uiso 1 1 calc R U . . .
H13C H 0.0417 0.4791 0.8658 0.149 Uiso 1 1 calc R U . . .
C14 C 0.4668(6) 0.5391(5) 0.7248(4) 0.0641(17) Uani 1 1 d . . . . .
H14 H 0.4190 0.5805 0.6924 0.077 Uiso 1 1 calc R U . . .
C15 C 0.4913(7) 0.4497(6) 0.7027(4) 0.081(2) Uani 1 1 d . . . . .
H15 H 0.4590 0.4326 0.6561 0.097 Uiso 1 1 calc R U . . .
C16 C 0.5610(7) 0.3880(5) 0.7480(4) 0.076(2) Uani 1 1 d . . . . .
H16 H 0.5799 0.3291 0.7320 0.091 Uiso 1 1 calc R U . . .
C17 C 0.6040(6) 0.4138(4) 0.8187(4) 0.0551(15) Uani 1 1 d . . . . .
C18 C 0.5751(5) 0.5035(4) 0.8385(3) 0.0430(13) Uani 1 1 d . . . . .
C19 C 0.6148(5) 0.5327(4) 0.9125(3) 0.0430(13) Uani 1 1 d . . . . .
C20 C 0.6203(5) 0.6475(4) 0.9984(3) 0.0550(15) Uani 1 1 d . . . . .
H20 H 0.6028 0.7079 1.0100 0.066 Uiso 1 1 calc R U . . .
C21 C 0.6797(6) 0.5884(5) 1.0541(3) 0.0617(17) Uani 1 1 d . . . . .
H21 H 0.6993 0.6095 1.1024 0.074 Uiso 1 1 calc R U . . .
C22 C 0.7089(6) 0.5013(5) 1.0386(4) 0.0652(18) Uani 1 1 d . . . . .
H22 H 0.7495 0.4621 1.0757 0.078 Uiso 1 1 calc R U . . .
C23 C 0.6777(5) 0.4693(4) 0.9656(3) 0.0526(15) Uani 1 1 d . . . . .
C24 C 0.7067(6) 0.3789(5) 0.9416(4) 0.0705(19) Uani 1 1 d . . . . .
H24 H 0.7504 0.3372 0.9755 0.085 Uiso 1 1 calc R U . . .
C25 C 0.6735(7) 0.3519(4) 0.8724(4) 0.0697(18) Uani 1 1 d . . . . .
H25 H 0.6955 0.2925 0.8587 0.084 Uiso 1 1 calc R U . . .
C26 C 0.2096(8) 0.2847(5) 0.7132(5) 0.083(2) Uani 1 1 d D . . . .
C27 C 0.0787(10) 0.2707(6) 0.8231(6) 0.107(3) Uani 1 1 d . U . . .
H27 H -0.0026 0.2817 0.8500 0.128 Uiso 1 1 calc R U . . .
C28 C 0.1702(10) 0.2224(6) 0.8597(5) 0.105(3) Uani 1 1 d . U . . .
H28 H 0.1546 0.2012 0.9109 0.126 Uiso 1 1 calc R U . . .
C29 C 0.2935(9) 0.2026(5) 0.8207(4) 0.079(2) Uani 1 1 d . . . . .
C30 C 0.6169(10) 0.1124(5) 0.8362(4) 0.083(2) Uani 1 1 d . . . . .
H30 H 0.6136 0.0939 0.8889 0.100 Uiso 1 1 calc R U . . .
C31 C 0.7418(8) 0.1007(4) 0.7956(3) 0.0680(18) Uani 1 1 d . . . . .
C32 C 0.8532(10) 0.0637(5) 0.8369(4) 0.091(3) Uani 1 1 d . . . . .
H32 H 0.8426 0.0469 0.8898 0.110 Uiso 1 1 calc R U . . .
C33 C 0.9743(9) 0.0525(6) 0.8007(5) 0.093(3) Uani 1 1 d . . . . .
H33 H 1.0452 0.0240 0.8274 0.111 Uiso 1 1 calc R U . . .
C34 C 0.9920(7) 0.0828(5) 0.7258(4) 0.080(2) Uani 1 1 d . . . . .
H34 H 1.0764 0.0772 0.7024 0.096 Uiso 1 1 calc R U . . .
C35 C 0.8893(6) 0.1213(4) 0.6834(3) 0.0614(16) Uani 1 1 d . . . . .
C36 C 0.7602(7) 0.1319(4) 0.7159(3) 0.0565(16) Uani 1 1 d . . . . .
C37 C 1.0266(7) 0.1489(6) 0.5689(4) 0.095(3) Uani 1 1 d . . . . .
H37A H 1.0646 0.0870 0.5642 0.113 Uiso 1 1 calc R U . . .
H37B H 1.0847 0.1800 0.5986 0.113 Uiso 1 1 calc R U . . .
C38 C 1.0106(8) 0.1920(7) 0.4895(4) 0.121(4) Uani 1 1 d . . . . .
H38A H 1.0954 0.1927 0.4628 0.181 Uiso 1 1 calc R U . . .
H38B H 0.9691 0.2524 0.4948 0.181 Uiso 1 1 calc R U . . .
H38C H 0.9571 0.1588 0.4596 0.181 Uiso 1 1 calc R U . . .
C39 C 0.3656(7) -0.0241(4) 0.7262(4) 0.0657(17) Uani 1 1 d . . . . .
H39 H 0.3867 -0.0209 0.7784 0.079 Uiso 1 1 calc R U . . .
C40 C 0.3075(7) -0.0972(5) 0.7040(4) 0.0714(18) Uani 1 1 d . . . . .
H40 H 0.2885 -0.1414 0.7409 0.086 Uiso 1 1 calc R U . . .
C41 C 0.2785(6) -0.1037(5) 0.6272(4) 0.0678(17) Uani 1 1 d . . . . .
H41 H 0.2407 -0.1529 0.6112 0.081 Uiso 1 1 calc R U . . .
C42 C 0.3059(6) -0.0361(5) 0.5725(3) 0.0608(17) Uani 1 1 d . . . . .
C43 C 0.3614(5) 0.0370(4) 0.6005(3) 0.0525(15) Uani 1 1 d . . . . .
C44 C 0.3918(5) 0.1102(4) 0.5494(3) 0.0534(15) Uani 1 1 d . . . . .
C45 C 0.4763(7) 0.2448(5) 0.5314(4) 0.075(2) Uani 1 1 d . . . . .
H45 H 0.5148 0.2916 0.5515 0.090 Uiso 1 1 calc R U . . .
C46 C 0.4529(8) 0.2464(6) 0.4506(4) 0.091(3) Uani 1 1 d . . . . .
H46 H 0.4742 0.2939 0.4180 0.109 Uiso 1 1 calc R U . . .
C47 C 0.3989(8) 0.1778(7) 0.4215(4) 0.089(3) Uani 1 1 d . . . . .
H47 H 0.3832 0.1789 0.3681 0.106 Uiso 1 1 calc R U . . .
C48 C 0.3659(6) 0.1056(5) 0.4681(3) 0.071(2) Uani 1 1 d . . . . .
C49 C 0.3102(7) 0.0289(6) 0.4428(4) 0.075(2) Uani 1 1 d . . . . .
H49 H 0.2934 0.0257 0.3898 0.089 Uiso 1 1 calc R U . . .
C50 C 0.2815(7) -0.0374(5) 0.4910(4) 0.074(2) Uani 1 1 d . . . . .
H50 H 0.2451 -0.0854 0.4715 0.089 Uiso 1 1 calc R U . . .
C53 C 0.8415(13) 0.3495(11) 0.6474(9) 0.106(5) Uani 0.5 1 d D U P . .
H53A H 0.9260 0.3216 0.6287 0.159 Uiso 0.5 1 calc R U P . .
H53B H 0.8203 0.3256 0.6989 0.159 Uiso 0.5 1 calc R U P . .
H53C H 0.8437 0.4130 0.6501 0.159 Uiso 0.5 1 calc R U P . .
O1W O 0.529(2) 0.5288(16) 0.5062(14) 0.110(8) Uani 0.25 1 d . U P . .
H1WA H 0.5985 0.5490 0.5183 0.165 Uiso 0.25 1 d R U P . .
H1WB H 0.5485 0.4758 0.4901 0.165 Uiso 0.25 1 d R U 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 N4 1.921(5) . ?
Cu1 O1 1.925(3) . ?
Cu1 N6 2.001(5) . ?
Cu1 N2 2.028(4) . ?
Cu1 N5 2.295(4) . ?
O1 C11 1.317(6) . ?
N1 C1 1.321(8) . ?
N1 C2 1.346(9) . ?
Cl1 C1 1.40(2) . ?
O11 C54 1.40(4) . ?
O11 C1 1.447(10) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C1 N2 1.351(7) . ?
Cu2 O3 1.915(4) . ?
Cu2 N10 1.953(6) . ?
Cu2 N8 2.002(6) . ?
Cu2 N12 2.022(5) . ?
Cu2 N11 2.290(5) . ?
O2 C10 1.365(7) . ?
O2 C12 1.432(7) . ?
N2 C4 1.362(7) . ?
C2 C3 1.336(9) . ?
C2 H2 0.9300 . ?
Cl2 C26 1.57(2) . ?
O12 C55 1.38(4) . ?
O12 C26 1.452(10) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
O3 C36 1.320(7) . ?
N3 C4 1.329(7) . ?
N3 N4 1.397(6) . ?
C3 C4 1.436(8) . ?
C3 H3A 0.9300 . ?
N4 C5 1.297(6) . ?
O4 C35 1.359(7) . ?
O4 C37 1.420(7) . ?
N5 C20 1.325(7) . ?
N5 C19 1.358(6) . ?
C5 C6 1.441(8) . ?
C5 H5 0.9300 . ?
O5 H5A 0.8502 . ?
O5 H5B 0.8496 . ?
N6 C14 1.321(7) . ?
N6 C18 1.359(6) . ?
O6 H6A 0.8487 . ?
O6 H6B 0.8573 . ?
C6 C11 1.404(8) . ?
C6 C7 1.413(7) . ?
N7 C26 1.346(9) . ?
N7 C27 1.399(11) . ?
C7 C8 1.366(9) . ?
C7 H7 0.9300 . ?
O7 H7A 0.8502 . ?
O7 H7B 0.8500 . ?
N8 C26 1.322(9) . ?
N8 C29 1.392(9) . ?
C8 C9 1.376(9) . ?
C8 H8 0.9300 . ?
N9 C29 1.320(10) . ?
N9 N10 1.376(8) . ?
C9 C10 1.371(8) . ?
C9 H9 0.9300 . ?
N10 C30 1.308(9) . ?
C10 C11 1.419(7) . ?
O10 C53 1.440(9) . ?
O10 H10 0.8200 . ?
N11 C39 1.320(7) . ?
N11 C43 1.359(7) . ?
N12 C45 1.314(7) . ?
N12 C44 1.360(8) . ?
C12 C13 1.471(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.399(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.350(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.396(7) . ?
C17 C25 1.436(8) . ?
C18 C19 1.440(7) . ?
C19 C23 1.414(7) . ?
C20 C21 1.392(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.341(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.412(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.426(9) . ?
C24 C25 1.332(9) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C27 C28 1.290(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.403(10) . ?
C28 H28 0.9300 . ?
C30 C31 1.418(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.420(10) . ?
C31 C36 1.431(8) . ?
C32 C33 1.352(10) . ?
C32 H32 0.9300 . ?
C33 C34 1.351(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.369(9) . ?
C34 H34 0.9300 . ?
C35 C36 1.402(8) . ?
C37 C38 1.489(9) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.384(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.364(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.400(9) . ?
C41 H41 0.9300 . ?
C42 C43 1.403(8) . ?
C42 C50 1.423(8) . ?
C43 C44 1.434(8) . ?
C44 C48 1.427(8) . ?
C45 C46 1.407(10) . ?
C45 H45 0.9300 . ?
C46 C47 1.347(11) . ?
C46 H46 0.9300 . ?
C47 C48 1.388(10) . ?
C47 H47 0.9300 . ?
C48 C49 1.435(10) . ?
C49 C50 1.320(10) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
O1W O1W 1.13(4) 2_666 ?
O1W H1WA 0.8498 . ?
O1W H1WB 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 O1 92.62(17) . . ?
N4 Cu1 N6 174.94(17) . . ?
O1 Cu1 N6 88.47(16) . . ?
N4 Cu1 N2 79.69(19) . . ?
O1 Cu1 N2 155.46(16) . . ?
N6 Cu1 N2 101.24(18) . . ?
N4 Cu1 N5 96.97(16) . . ?
O1 Cu1 N5 108.42(15) . . ?
N6 Cu1 N5 78.01(17) . . ?
N2 Cu1 N5 95.70(16) . . ?
C11 O1 Cu1 125.5(4) . . ?
C1 N1 C2 114.3(6) . . ?
C54 O11 C1 113(3) . . ?
O11 C54 H54A 109.4 . . ?
O11 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O11 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N1 C1 N2 127.4(7) . . ?
N1 C1 Cl1 115(3) . . ?
N2 C1 Cl1 118(3) . . ?
N1 C1 O11 119(2) . . ?
N2 C1 O11 113(2) . . ?
O3 Cu2 N10 91.4(2) . . ?
O3 Cu2 N8 151.2(2) . . ?
N10 Cu2 N8 79.9(3) . . ?
O3 Cu2 N12 90.45(18) . . ?
N10 Cu2 N12 171.3(2) . . ?
N8 Cu2 N12 102.3(2) . . ?
O3 Cu2 N11 114.96(17) . . ?
N10 Cu2 N11 94.19(19) . . ?
N8 Cu2 N11 93.21(19) . . ?
N12 Cu2 N11 77.31(19) . . ?
C10 O2 C12 119.7(5) . . ?
C1 N2 C4 116.6(5) . . ?
C1 N2 Cu1 133.8(5) . . ?
C4 N2 Cu1 109.4(3) . . ?
C3 C2 N1 125.8(7) . . ?
C3 C2 H2 117.1 . . ?
N1 C2 H2 117.1 . . ?
C55 O12 C26 120(3) . . ?
O12 C55 H55A 107.1 . . ?
O12 C55 H55B 110.7 . . ?
H55A C55 H55B 109.5 . . ?
O12 C55 H55C 110.6 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C36 O3 Cu2 127.9(4) . . ?
C4 N3 N4 110.0(5) . . ?
C2 C3 C4 116.4(7) . . ?
C2 C3 H3A 121.8 . . ?
C4 C3 H3A 121.8 . . ?
C5 N4 N3 115.5(5) . . ?
C5 N4 Cu1 126.8(4) . . ?
N3 N4 Cu1 117.5(3) . . ?
C35 O4 C37 119.2(5) . . ?
N3 C4 N2 121.8(5) . . ?
N3 C4 C3 118.8(6) . . ?
N2 C4 C3 119.4(6) . . ?
C20 N5 C19 118.7(5) . . ?
C20 N5 Cu1 133.5(4) . . ?
C19 N5 Cu1 107.8(3) . . ?
N4 C5 C6 124.2(5) . . ?
N4 C5 H5 117.9 . . ?
C6 C5 H5 117.9 . . ?
H5A O5 H5B 104.5 . . ?
C14 N6 C18 118.0(5) . . ?
C14 N6 Cu1 124.1(4) . . ?
C18 N6 Cu1 117.8(3) . . ?
H6A O6 H6B 104.5 . . ?
C11 C6 C7 119.8(6) . . ?
C11 C6 C5 123.0(5) . . ?
C7 C6 C5 117.2(6) . . ?
C26 N7 C27 111.1(8) . . ?
C8 C7 C6 120.6(7) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
H7A O7 H7B 104.5 . . ?
C26 N8 C29 117.3(6) . . ?
C26 N8 Cu2 133.2(5) . . ?
C29 N8 Cu2 109.1(5) . . ?
C7 C8 C9 120.2(6) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C29 N9 N10 112.5(6) . . ?
C10 C9 C8 120.6(6) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C30 N10 N9 119.4(6) . . ?
C30 N10 Cu2 125.2(5) . . ?
N9 N10 Cu2 115.0(5) . . ?
O2 C10 C9 125.1(6) . . ?
O2 C10 C11 113.7(5) . . ?
C9 C10 C11 121.2(6) . . ?
C53 O10 H10 109.5 . . ?
C39 N11 C43 118.4(6) . . ?
C39 N11 Cu2 131.6(4) . . ?
C43 N11 Cu2 110.0(4) . . ?
O1 C11 C6 125.2(5) . . ?
O1 C11 C10 117.3(5) . . ?
C6 C11 C10 117.5(5) . . ?
C45 N12 C44 118.8(6) . . ?
C45 N12 Cu2 124.1(5) . . ?
C44 N12 Cu2 117.1(4) . . ?
O2 C12 C13 107.1(5) . . ?
O2 C12 H12A 110.3 . . ?
C13 C12 H12A 110.3 . . ?
O2 C12 H12B 110.3 . . ?
C13 C12 H12B 110.3 . . ?
H12A C12 H12B 108.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 121.4(6) . . ?
N6 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 120.9(6) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 118.9(6) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C16 C17 C18 117.8(6) . . ?
C16 C17 C25 122.8(6) . . ?
C18 C17 C25 119.3(6) . . ?
N6 C18 C17 122.8(5) . . ?
N6 C18 C19 117.5(5) . . ?
C17 C18 C19 119.7(5) . . ?
N5 C19 C23 122.0(5) . . ?
N5 C19 C18 118.4(5) . . ?
C23 C19 C18 119.6(5) . . ?
N5 C20 C21 122.3(6) . . ?
N5 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C22 C21 C20 120.3(6) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 119.7(6) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C19 117.0(6) . . ?
C22 C23 C24 124.9(6) . . ?
C19 C23 C24 118.2(6) . . ?
C25 C24 C23 122.5(6) . . ?
C25 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
C24 C25 C17 120.6(6) . . ?
C24 C25 H25 119.7 . . ?
C17 C25 H25 119.7 . . ?
N8 C26 N7 128.1(8) . . ?
N8 C26 O12 114(2) . . ?
N7 C26 O12 118(2) . . ?
N8 C26 Cl2 122(2) . . ?
N7 C26 Cl2 110(2) . . ?
C28 C27 N7 126.6(8) . . ?
C28 C27 H27 116.7 . . ?
N7 C27 H27 116.7 . . ?
C27 C28 C29 118.5(9) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 H28 120.7 . . ?
N9 C29 N8 119.9(6) . . ?
N9 C29 C28 122.0(8) . . ?
N8 C29 C28 118.1(9) . . ?
N10 C30 C31 126.6(6) . . ?
N10 C30 H30 116.7 . . ?
C31 C30 H30 116.7 . . ?
C30 C31 C32 119.1(6) . . ?
C30 C31 C36 121.6(7) . . ?
C32 C31 C36 119.0(7) . . ?
C33 C32 C31 121.1(6) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C34 C33 C32 119.8(8) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 122.0(7) . . ?
C33 C34 H34 119.0 . . ?
C35 C34 H34 119.0 . . ?
O4 C35 C34 125.0(6) . . ?
O4 C35 C36 113.6(5) . . ?
C34 C35 C36 121.4(6) . . ?
O3 C36 C35 119.5(5) . . ?
O3 C36 C31 124.0(6) . . ?
C35 C36 C31 116.5(6) . . ?
O4 C37 C38 107.8(6) . . ?
O4 C37 H37A 110.1 . . ?
C38 C37 H37A 110.1 . . ?
O4 C37 H37B 110.1 . . ?
C38 C37 H37B 110.1 . . ?
H37A C37 H37B 108.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N11 C39 C40 123.2(6) . . ?
N11 C39 H39 118.4 . . ?
C40 C39 H39 118.4 . . ?
C41 C40 C39 119.1(6) . . ?
C41 C40 H40 120.4 . . ?
C39 C40 H40 120.4 . . ?
C40 C41 C42 119.8(6) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 H41 120.1 . . ?
C41 C42 C43 117.3(5) . . ?
C41 C42 C50 124.1(7) . . ?
C43 C42 C50 118.6(6) . . ?
N11 C43 C42 122.2(6) . . ?
N11 C43 C44 116.1(6) . . ?
C42 C43 C44 121.6(5) . . ?
N12 C44 C48 123.0(6) . . ?
N12 C44 C43 119.4(5) . . ?
C48 C44 C43 117.6(6) . . ?
N12 C45 C46 122.1(8) . . ?
N12 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C47 C46 C45 118.7(7) . . ?
C47 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
C46 C47 C48 122.5(7) . . ?
C46 C47 H47 118.7 . . ?
C48 C47 H47 118.7 . . ?
C47 C48 C44 114.9(8) . . ?
C47 C48 C49 126.9(7) . . ?
C44 C48 C49 118.3(6) . . ?
C50 C49 C48 123.2(6) . . ?
C50 C49 H49 118.4 . . ?
C48 C49 H49 118.4 . . ?
C49 C50 C42 120.7(7) . . ?
C49 C50 H50 119.7 . . ?
C42 C50 H50 119.7 . . ?
O10 C53 H53A 109.5 . . ?
O10 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
O10 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O1W O1W H1WA 151.3 2_666 . ?
O1W O1W H1WB 44.8 2_666 . ?
H1WA O1W H1WB 108.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B N1 0.85 2.62 3.019(8) 110.4 1_455
O7 H7B O10 0.85 2.22 2.643(16) 110.3 2_666
O10 H10 O7 0.82 1.89 2.643(16) 153.1 2_666
C15 H15 Cl2 0.93 3.05 3.71(7) 129.8 .
C45 H45 O10 0.93 2.63 3.409(16) 141.2 .
O1W H1WB O7 0.85 1.93 2.60(3) 135.0 2_666
O6 H6A N9 0.85 2.14 2.986(7) 172.3 2_667
O6 H6B N3 0.86 2.20 2.971(7) 149.8 .

_refine_diff_density_max         0.772
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.070

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1949222'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C24 H16 Br2 Cl2 Co N6 O2), 0.5(H2O)'
_chemical_formula_sum            'C48 H33 Br4 Cl4 Co2 N12 O4.50 '
_chemical_formula_weight         1429.12

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'
Br Br -0.2901 2.4595 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.0668(8)
_cell_length_b                   12.2845(7)
_cell_length_c                   13.5174(8)
_cell_angle_alpha                63.376(6)
_cell_angle_beta                 71.616(6)
_cell_angle_gamma                79.004(5)
_cell_volume                     1415.73(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3436
_cell_measurement_theta_min      3.494
_cell_measurement_theta_max      27.1860

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_F_000             703
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.650
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            9727
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.494
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             4941
_reflns_number_gt                3815
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+4.9927P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4941
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1246
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.43280(7) 0.25058(6) 0.01223(6) 0.02854(19) Uani 1 1 d . . . . .
Br1 Br 0.72688(9) 0.04521(8) 0.52106(6) 0.0713(3) Uani 1 1 d . . . . .
Br2 Br 1.02233(10) 0.27932(8) -0.50359(7) 0.0857(3) Uani 1 1 d . . . . .
Cl1 Cl 0.13920(17) 0.21273(14) 0.25354(13) 0.0493(4) Uani 1 1 d . . . . .
Cl2 Cl 0.1844(2) 0.33117(15) -0.15811(17) 0.0701(6) Uani 1 1 d . . . . .
O2 O 0.5435(4) 0.1145(3) 0.1141(3) 0.0359(9) Uani 1 1 d . . . . .
N6 N 0.4246(4) 0.3424(3) 0.1099(3) 0.0287(9) Uani 1 1 d . . . . .
O1 O 0.5909(4) 0.3560(3) -0.1120(3) 0.0399(9) Uani 1 1 d . . . . .
N1 N 0.4596(5) 0.1604(4) -0.0905(4) 0.0312(10) Uani 1 1 d . . . . .
C20 C 0.2807(6) 0.4881(4) -0.0011(4) 0.0334(12) Uani 1 1 d . . . . .
N3 N 0.2535(5) 0.1334(4) 0.0946(4) 0.0318(10) Uani 1 1 d . . . . .
N5 N 0.3554(5) 0.4551(4) 0.0770(4) 0.0379(11) Uani 1 1 d . . . . .
H5 H 0.3591 0.5042 0.1054 0.046 Uiso 1 1 calc R U . . .
C18 C 0.5797(5) 0.1029(4) 0.2038(4) 0.0307(11) Uani 1 1 d . . . . .
N2 N 0.3662(5) 0.0723(4) -0.0510(4) 0.0360(10) Uani 1 1 d . . . . .
H2 H 0.3768 0.0247 -0.0845 0.043 Uiso 1 1 calc R U . . .
C5 C 0.6836(6) 0.3379(5) -0.1980(4) 0.0363(12) Uani 1 1 d . . . . .
C17 C 0.5521(6) 0.1956(5) 0.2439(4) 0.0326(12) Uani 1 1 d . . . . .
C8 C 0.2580(6) 0.0622(4) 0.0411(5) 0.0344(12) Uani 1 1 d . . . . .
C7 C 0.5557(6) 0.1713(5) -0.1826(5) 0.0376(13) Uani 1 1 d . . . . .
H7 H 0.5529 0.1216 -0.2174 0.045 Uiso 1 1 calc R U . . .
C9 C 0.1559(7) -0.0186(5) 0.0760(6) 0.0515(16) Uani 1 1 d . . . . .
H9 H 0.1620 -0.0662 0.0371 0.062 Uiso 1 1 calc R U . . .
N4 N 0.2771(5) 0.4054(4) -0.0405(4) 0.0339(10) Uani 1 1 d . . . . .
C12 C 0.1450(6) 0.1212(5) 0.1854(5) 0.0394(13) Uani 1 1 d . . . . .
C24 C 0.1989(7) 0.4400(5) -0.1141(5) 0.0437(14) Uani 1 1 d . . . . .
C16 C 0.5971(6) 0.1757(5) 0.3392(5) 0.0401(13) Uani 1 1 d . . . . .
H16 H 0.5812 0.2373 0.3645 0.048 Uiso 1 1 calc R U . . .
C19 C 0.4800(6) 0.3112(5) 0.1932(4) 0.0367(13) Uani 1 1 d . . . . .
H19 H 0.4727 0.3679 0.2229 0.044 Uiso 1 1 calc R U . . .
C6 C 0.8041(7) 0.4026(6) -0.2548(5) 0.0541(17) Uani 1 1 d . . . . .
H6 H 0.8173 0.4592 -0.2311 0.065 Uiso 1 1 calc R U . . .
C3 C 0.7684(7) 0.2408(5) -0.3298(5) 0.0488(15) Uani 1 1 d . . . . .
H3 H 0.7560 0.1867 -0.3566 0.059 Uiso 1 1 calc R U . . .
C13 C 0.6461(6) -0.0062(5) 0.2663(5) 0.0405(13) Uani 1 1 d . . . . .
H13 H 0.6632 -0.0695 0.2431 0.049 Uiso 1 1 calc R U . . .
C14 C 0.6872(6) -0.0239(5) 0.3605(5) 0.0444(14) Uani 1 1 d . . . . .
H14 H 0.7308 -0.0978 0.4003 0.053 Uiso 1 1 calc R U . . .
C2 C 0.8841(7) 0.3055(6) -0.3820(5) 0.0539(17) Uani 1 1 d . . . . .
C15 C 0.6625(6) 0.0698(5) 0.3947(5) 0.0422(14) Uani 1 1 d . . . . .
C4 C 0.6665(6) 0.2528(5) -0.2365(4) 0.0366(12) Uani 1 1 d . . . . .
C22 C 0.1367(7) 0.6316(6) -0.1132(6) 0.0565(17) Uani 1 1 d . . . . .
H22 H 0.0913 0.7086 -0.1394 0.068 Uiso 1 1 calc R U . . .
C23 C 0.1273(7) 0.5491(5) -0.1531(6) 0.0554(17) Uani 1 1 d . . . . .
H23 H 0.0744 0.5674 -0.2044 0.066 Uiso 1 1 calc R U . . .
C1 C 0.9055(7) 0.3869(6) -0.3448(6) 0.0589(18) Uani 1 1 d . . . . .
H1 H 0.9862 0.4303 -0.3794 0.071 Uiso 1 1 calc R U . . .
C10 C 0.0463(8) -0.0261(6) 0.1690(6) 0.0611(18) Uani 1 1 d . . . . .
H10 H -0.0239 -0.0789 0.1935 0.073 Uiso 1 1 calc R U . . .
C21 C 0.2114(6) 0.6022(5) -0.0361(5) 0.0446(14) Uani 1 1 d . . . . .
H21 H 0.2159 0.6571 -0.0075 0.054 Uiso 1 1 calc R U . . .
C11 C 0.0391(7) 0.0446(6) 0.2270(6) 0.0554(17) Uani 1 1 d . . . . .
H11 H -0.0340 0.0400 0.2910 0.067 Uiso 1 1 calc R U . . .
O1W O 0.5000 0.5000 -0.5000 0.180(14) Uani 0.5 2 d S . P . .
H1WB H 0.4424 0.4445 -0.4807 0.270 Uiso 0.25 1 d R U P . .
H1WA H 0.4330 0.5717 -0.4969 0.270 Uiso 0.25 1 d R U 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
Co1 O2 2.031(3) . ?
Co1 O1 2.045(4) . ?
Co1 N6 2.062(4) . ?
Co1 N1 2.063(4) . ?
Co1 N3 2.203(4) . ?
Co1 N4 2.222(4) . ?
Br1 C15 1.895(5) . ?
Br2 C2 1.898(6) . ?
Cl1 C12 1.728(6) . ?
Cl2 C24 1.733(6) . ?
O2 C18 1.315(6) . ?
N6 C19 1.286(6) . ?
N6 N5 1.369(6) . ?
O1 C5 1.320(6) . ?
N1 C7 1.283(7) . ?
N1 N2 1.376(6) . ?
C20 N4 1.353(6) . ?
C20 N5 1.357(7) . ?
C20 C21 1.384(7) . ?
N3 C12 1.332(7) . ?
N3 C8 1.349(6) . ?
N5 H5 0.8600 . ?
C18 C13 1.399(7) . ?
C18 C17 1.417(7) . ?
N2 C8 1.346(7) . ?
N2 H2 0.8600 . ?
C5 C6 1.388(8) . ?
C5 C4 1.416(7) . ?
C17 C16 1.402(7) . ?
C17 C19 1.435(7) . ?
C8 C9 1.388(8) . ?
C7 C4 1.427(8) . ?
C7 H7 0.9300 . ?
C9 C10 1.366(9) . ?
C9 H9 0.9300 . ?
N4 C24 1.333(7) . ?
C12 C11 1.367(8) . ?
C24 C23 1.354(8) . ?
C16 C15 1.342(8) . ?
C16 H16 0.9300 . ?
C19 H19 0.9300 . ?
C6 C1 1.382(8) . ?
C6 H6 0.9300 . ?
C3 C2 1.348(9) . ?
C3 C4 1.399(8) . ?
C3 H3 0.9300 . ?
C13 C14 1.374(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.378(8) . ?
C14 H14 0.9300 . ?
C2 C1 1.379(9) . ?
C22 C21 1.354(9) . ?
C22 C23 1.373(9) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C1 H1 0.9300 . ?
C10 C11 1.388(9) . ?
C10 H10 0.9300 . ?
C21 H21 0.9300 . ?
C11 H11 0.9300 . ?
O1W H1WB 0.8741 . ?
O1W H1WA 1.0104 . ?

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
O2 Co1 O1 100.81(16) . . ?
O2 Co1 N6 86.71(14) . . ?
O1 Co1 N6 89.20(15) . . ?
O2 Co1 N1 91.29(15) . . ?
O1 Co1 N1 86.68(15) . . ?
N6 Co1 N1 175.01(18) . . ?
O2 Co1 N3 88.92(15) . . ?
O1 Co1 N3 160.40(15) . . ?
N6 Co1 N3 108.47(16) . . ?
N1 Co1 N3 76.03(16) . . ?
O2 Co1 N4 159.52(15) . . ?
O1 Co1 N4 90.21(16) . . ?
N6 Co1 N4 76.14(15) . . ?
N1 Co1 N4 106.66(16) . . ?
N3 Co1 N4 86.04(16) . . ?
C18 O2 Co1 131.1(3) . . ?
C19 N6 N5 116.1(4) . . ?
C19 N6 Co1 129.3(3) . . ?
N5 N6 Co1 114.6(3) . . ?
C5 O1 Co1 129.8(3) . . ?
C7 N1 N2 116.0(4) . . ?
C7 N1 Co1 128.6(3) . . ?
N2 N1 Co1 115.3(3) . . ?
N4 C20 N5 117.3(4) . . ?
N4 C20 C21 122.9(5) . . ?
N5 C20 C21 119.8(5) . . ?
C12 N3 C8 116.1(5) . . ?
C12 N3 Co1 131.8(3) . . ?
C8 N3 Co1 112.1(3) . . ?
C20 N5 N6 119.1(4) . . ?
C20 N5 H5 120.4 . . ?
N6 N5 H5 120.4 . . ?
O2 C18 C13 119.9(4) . . ?
O2 C18 C17 123.3(4) . . ?
C13 C18 C17 116.8(5) . . ?
C8 N2 N1 118.5(4) . . ?
C8 N2 H2 120.8 . . ?
N1 N2 H2 120.8 . . ?
O1 C5 C6 120.5(5) . . ?
O1 C5 C4 122.5(5) . . ?
C6 C5 C4 117.0(5) . . ?
C16 C17 C18 119.2(5) . . ?
C16 C17 C19 116.6(4) . . ?
C18 C17 C19 124.2(4) . . ?
N2 C8 N3 117.6(5) . . ?
N2 C8 C9 119.3(5) . . ?
N3 C8 C9 123.0(5) . . ?
N1 C7 C4 125.8(4) . . ?
N1 C7 H7 117.1 . . ?
C4 C7 H7 117.1 . . ?
C10 C9 C8 118.2(6) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
C24 N4 C20 115.4(4) . . ?
C24 N4 Co1 133.1(3) . . ?
C20 N4 Co1 110.7(3) . . ?
N3 C12 C11 125.6(5) . . ?
N3 C12 Cl1 116.0(4) . . ?
C11 C12 Cl1 118.3(5) . . ?
N4 C24 C23 125.9(5) . . ?
N4 C24 Cl2 115.8(4) . . ?
C23 C24 Cl2 118.3(5) . . ?
C15 C16 C17 121.4(5) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
N6 C19 C17 125.1(4) . . ?
N6 C19 H19 117.4 . . ?
C17 C19 H19 117.4 . . ?
C1 C6 C5 123.2(5) . . ?
C1 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
C2 C3 C4 122.0(5) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C14 C13 C18 122.8(5) . . ?
C14 C13 H13 118.6 . . ?
C18 C13 H13 118.6 . . ?
C13 C14 C15 118.7(5) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C3 C2 C1 120.5(6) . . ?
C3 C2 Br2 119.7(5) . . ?
C1 C2 Br2 119.7(5) . . ?
C16 C15 C14 121.1(5) . . ?
C16 C15 Br1 121.1(4) . . ?
C14 C15 Br1 117.8(4) . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 C7 116.3(5) . . ?
C5 C4 C7 124.7(5) . . ?
C21 C22 C23 120.7(6) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 116.8(6) . . ?
C24 C23 H23 121.6 . . ?
C22 C23 H23 121.6 . . ?
C2 C1 C6 118.4(6) . . ?
C2 C1 H1 120.8 . . ?
C6 C1 H1 120.8 . . ?
C9 C10 C11 120.4(6) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C22 C21 C20 118.3(5) . . ?
C22 C21 H21 120.9 . . ?
C20 C21 H21 120.9 . . ?
C12 C11 C10 116.7(6) . . ?
C12 C11 H11 121.7 . . ?
C10 C11 H11 121.7 . . ?
H1WB O1W H1WA 101.8 . . ?

_refine_diff_density_max         1.936
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.099

_shelxl_version_number           2014-3



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

data_1
_database_code_depnum_ccdc_archive 'CCDC 2072363'
loop_
_audit_author_name
_audit_author_address
'shuhua zhang'
;Guangdong University of Petrochemical Technology
China
;
_audit_update_record             
;
2021-12-07 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C25 H20 Cu N6 O3), 9(H2 O)'
_chemical_formula_sum            'C100 H98 Cu4 N24 O21'
_chemical_formula_weight         2226.18

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   16.3685(6)
_cell_length_b                   19.8394(5)
_cell_length_c                   17.3180(5)
_cell_angle_alpha                90
_cell_angle_beta                 117.660(4)
_cell_angle_gamma                90
_cell_volume                     4981.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8189
_cell_measurement_theta_min      3.5430
_cell_measurement_theta_max      25.5760

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_F_000             2300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.927
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.74155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            33470
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.355
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             16474
_reflns_number_gt                12519
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.974

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0489P)²+2.0316P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5

_chemical_absolute_configuration ?
_refine_ls_number_reflns         16474
_refine_ls_number_parameters     1356
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.50208(6) 0.52331(5) 0.43857(5) 0.0389(2) Uani 1 1 d . . . . .
Cu4 Cu 0.94179(6) 0.72939(4) 0.93248(5) 0.0404(2) Uani 1 1 d . . . . .
Cu3 Cu 0.78100(6) 0.52346(5) 1.06256(5) 0.0413(2) Uani 1 1 d . . . . .
Cu1 Cu -0.21841(6) 0.21277(4) 0.43597(5) 0.0404(2) Uani 1 1 d . . . . .
O5 O 0.6026(3) 0.5676(3) 0.4305(3) 0.0444(13) Uani 1 1 d . . . . .
O8 O 0.6750(4) 0.5515(3) 1.0744(3) 0.0470(14) Uani 1 1 d . . . . .
O6 O 0.7060(4) 0.6167(3) 0.3654(3) 0.0629(16) Uani 1 1 d . . . . .
O2 O -0.1118(4) 0.1780(3) 0.4298(3) 0.0498(13) Uani 1 1 d . . . . .
N4 N -0.1413(5) 0.2639(3) 0.5410(4) 0.0438(16) Uani 1 1 d . . . . .
O10 O 0.7397(4) 0.6807(3) 0.9116(3) 0.0532(14) Uani 1 1 d . . . . .
N22 N 1.0293(4) 0.7771(3) 1.0353(4) 0.0422(15) Uani 1 1 d . . . . .
O1 O -0.4293(4) 0.1569(3) 0.3875(3) 0.0557(14) Uani 1 1 d . U . . .
N23 N 0.8477(4) 0.6901(3) 0.8178(3) 0.0373(14) Uani 1 1 d . . . . .
N18 N 0.8622(4) 0.5683(3) 1.1777(4) 0.0386(14) Uani 1 1 d . . . . .
O3 O -0.0056(4) 0.1424(3) 0.3628(4) 0.0682(18) Uani 1 1 d . . . . .
N5 N -0.2977(4) 0.1664(3) 0.3224(4) 0.0372(14) Uani 1 1 d . . . . .
O11 O 1.0369(4) 0.6856(3) 0.9174(3) 0.0528(14) Uani 1 1 d . . . . .
N12 N 0.4116(4) 0.5630(3) 0.3242(4) 0.0394(14) Uani 1 1 d . . . . .
N17 N 0.8358(5) 0.4337(4) 1.1532(4) 0.0546(18) Uani 1 1 d . . . . .
C6 C -0.0588(6) 0.2842(4) 0.5623(5) 0.048(2) Uani 1 1 d . . . . .
H6 H -0.0327 0.3156 0.6070 0.057 Uiso 1 1 calc R U . . .
N20 N 0.8622(4) 0.7490(3) 0.9899(4) 0.0412(16) Uani 1 1 d . . . . .
C32 C 0.7227(5) 0.4927(4) 0.5258(4) 0.0419(18) Uani 1 1 d . . . . .
N21 N 0.9945(4) 0.8104(3) 1.0843(4) 0.0456(16) Uani 1 1 d . . . . .
N11 N 0.4641(4) 0.4323(3) 0.3455(4) 0.0448(15) Uani 1 1 d . . . . .
O9 O 0.9837(5) 0.5870(4) 1.1041(4) 0.0694(18) Uani 1 1 d . U . . .
N3 N -0.1829(5) 0.2867(4) 0.5896(4) 0.0511(18) Uani 1 1 d . . . . .
N14 N 0.8679(4) 0.5185(4) 1.0102(4) 0.0452(15) Uani 1 1 d . . . . .
N10 N 0.5860(5) 0.4762(3) 0.5436(3) 0.0423(16) Uani 1 1 d . . . . .
N9 N 0.5498(5) 0.4456(3) 0.5924(4) 0.0478(17) Uani 1 1 d . . . . .
N8 N 0.4185(4) 0.5042(3) 0.4926(4) 0.0404(15) Uani 1 1 d . . . . .
N19 N 0.7297(5) 0.7519(4) 1.0124(4) 0.0537(18) Uani 1 1 d . . . . .
N16 N 0.7038(5) 0.4747(3) 0.9553(4) 0.0449(16) Uani 1 1 d . . . . .
N7 N 0.2795(5) 0.5014(4) 0.5058(4) 0.0563(19) Uani 1 1 d . . . . .
N24 N 0.8995(4) 0.8205(3) 0.8414(4) 0.0439(15) Uani 1 1 d . . . . .
N2 N -0.3077(4) 0.2246(3) 0.4846(4) 0.0456(15) Uani 1 1 d . . . . .
N15 N 0.7461(6) 0.4538(4) 0.9061(4) 0.0547(19) Uani 1 1 d . . . . .
N1 N -0.4510(5) 0.2205(4) 0.4903(5) 0.060(2) Uani 1 1 d . . . . .
C27 C 0.3317(5) 0.5231(4) 0.4720(4) 0.0457(18) Uani 1 1 d . . . . .
O7 O 0.5690(4) 0.5820(3) 1.1421(4) 0.0642(17) Uani 1 1 d . . . . .
C57 C 0.5966(5) 0.5207(4) 1.0418(4) 0.0427(17) Uani 1 1 d . . . . .
C44 C 0.3676(5) 0.5202(4) 0.2560(4) 0.0371(15) Uani 1 1 d . . . . .
C62 C 0.9528(6) 0.5420(4) 1.0342(5) 0.053(2) Uani 1 1 d . . . . .
C81 C 1.1169(5) 0.7852(4) 1.0590(5) 0.0437(19) Uani 1 1 d . . . . .
H81 H 1.1498 0.8154 1.1039 0.052 Uiso 1 1 calc R U . . .
C37 C 0.6855(5) 0.5423(4) 0.4598(4) 0.0414(19) Uani 1 1 d . . . . .
C43 C 0.3954(5) 0.4504(4) 0.2680(4) 0.0407(17) Uani 1 1 d . . . . .
C74 C 0.9098(4) 0.5267(5) 1.2464(4) 0.0399(18) Uani 1 1 d . . . . .
N6 N -0.2721(5) 0.3013(3) 0.3411(4) 0.0532(18) Uani 1 1 d . . . . .
C12 C -0.0336(5) 0.2114(4) 0.4593(4) 0.0450(19) Uani 1 1 d . . . . .
N13 N 1.0088(5) 0.5288(4) 1.0020(5) 0.067(2) Uani 1 1 d . . . . .
C56 C 0.5673(6) 0.4728(4) 0.9742(5) 0.048(2) Uani 1 1 d . . . . .
C5 C -0.2696(6) 0.2659(4) 0.5569(5) 0.047(2) Uani 1 1 d . . . . .
C31 C 0.6718(6) 0.4647(4) 0.5668(4) 0.0423(19) Uani 1 1 d . . . . .
H31 H 0.7032 0.4360 0.6139 0.051 Uiso 1 1 calc R U . . .
C78 C 0.7714(7) 0.8008(4) 1.0734(5) 0.059(2) Uani 1 1 d . . . . .
H78 H 0.7380 0.8202 1.0988 0.070 Uiso 1 1 calc R U . . .
C94 C 0.8056(4) 0.7323(4) 0.7509(4) 0.0363(16) Uani 1 1 d . . . . .
C79 C 0.8583(6) 0.8227(4) 1.0993(5) 0.054(2) Uani 1 1 d . . . . .
H79 H 0.8848 0.8551 1.1428 0.065 Uiso 1 1 calc R U . . .
O12 O 1.1401(4) 0.6121(4) 0.8734(4) 0.093(2) Uani 1 1 d . . . . .
C33 C 0.8136(6) 0.4687(4) 0.5533(5) 0.055(2) Uani 1 1 d . . . . .
H33 H 0.8372 0.4352 0.5957 0.066 Uiso 1 1 calc R U . . .
C93 C 0.8316(5) 0.8025(4) 0.7619(4) 0.0409(18) Uani 1 1 d . . . . .
C30 C 0.4617(6) 0.4614(4) 0.5622(5) 0.046(2) Uani 1 1 d . . . . .
C48 C 0.2979(5) 0.5424(5) 0.1747(4) 0.050(2) Uani 1 1 d . . . . .
C95 C 0.8279(6) 0.6251(4) 0.8054(5) 0.053(2) Uani 1 1 d . . . . .
H95 H 0.8587 0.5955 0.8516 0.063 Uiso 1 1 calc R U . . .
C36 C 0.7440(5) 0.5673(4) 0.4270(5) 0.049(2) Uani 1 1 d . . . . .
C18 C -0.3441(5) 0.2061(4) 0.2517(4) 0.0413(18) Uani 1 1 d . . . . .
C73 C 0.8738(6) 0.6339(4) 1.1891(5) 0.051(2) Uani 1 1 d . . . . .
H73 H 0.8403 0.6621 1.1420 0.061 Uiso 1 1 calc R U . . .
C7 C -0.0042(5) 0.2620(4) 0.5221(5) 0.046(2) Uani 1 1 d . . . . .
C4 C -0.3258(7) 0.2854(5) 0.5953(6) 0.059(2) Uani 1 1 d . . . . .
H4 H -0.3024 0.3124 0.6449 0.071 Uiso 1 1 calc R U . . .
C77 C 0.7775(5) 0.7305(4) 0.9744(4) 0.0422(17) Uani 1 1 d . . . . .
C60 C 0.8866(8) 0.4618(5) 0.8961(6) 0.070(3) Uani 1 1 d . . . . .
H60 H 0.8646 0.4345 0.8468 0.084 Uiso 1 1 calc R U . . .
C55 C 0.4774(6) 0.4428(5) 0.9423(6) 0.062(3) Uani 1 1 d . . . . .
H55 H 0.4579 0.4112 0.8976 0.075 Uiso 1 1 calc R U . . .
C3 C -0.4145(8) 0.2638(5) 0.5581(6) 0.065(3) Uani 1 1 d . . . . .
H3A H -0.4525 0.2798 0.5807 0.078 Uiso 1 1 calc R U . . .
C70 C 0.9723(5) 0.5524(5) 1.3285(5) 0.051(2) Uani 1 1 d . . . . .
C89 C 0.9270(6) 0.8835(4) 0.8527(5) 0.055(2) Uani 1 1 d . . . . .
H89 H 0.9724 0.8967 0.9074 0.066 Uiso 1 1 calc R U . . .
C80 C 0.9078(6) 0.7946(4) 1.0579(4) 0.046(2) Uani 1 1 d . . . . .
C19 C -0.3308(6) 0.2772(4) 0.2613(5) 0.049(2) Uani 1 1 d . . . . .
C92 C 0.7898(6) 0.8481(5) 0.6932(5) 0.054(2) Uani 1 1 d . . . . .
C98 C 0.7371(5) 0.7104(5) 0.6680(4) 0.050(2) Uani 1 1 d . . . . .
C52 C 0.5340(5) 0.5365(4) 1.0757(5) 0.047(2) Uani 1 1 d . . . . .
C45 C 0.3911(6) 0.6276(4) 0.3127(5) 0.051(2) Uani 1 1 d . . . . .
H45 H 0.4215 0.6570 0.3592 0.061 Uiso 1 1 calc R U . . .
C11 C 0.0276(6) 0.1927(5) 0.4246(5) 0.054(2) Uani 1 1 d . . . . .
C8 C 0.0820(6) 0.2936(5) 0.5488(6) 0.062(2) Uani 1 1 d . . . . .
H8 H 0.1009 0.3276 0.5905 0.075 Uiso 1 1 calc R U . . .
C35 C 0.8325(6) 0.5427(5) 0.4563(5) 0.062(2) Uani 1 1 d . . . . .
H35 H 0.8694 0.5597 0.4331 0.074 Uiso 1 1 calc R U . . .
C38 C 0.7585(6) 0.6399(5) 0.3239(5) 0.071(3) Uani 1 1 d . . . . .
H38A H 0.7249 0.6745 0.2826 0.106 Uiso 1 1 calc R U . . .
H38B H 0.7697 0.6030 0.2941 0.106 Uiso 1 1 calc R U . . .
H38C H 0.8163 0.6577 0.3670 0.106 Uiso 1 1 calc R U . . .
C14 C -0.3074(6) 0.1002(4) 0.3136(5) 0.053(2) Uani 1 1 d . . . . .
H14 H -0.2733 0.0732 0.3619 0.063 Uiso 1 1 calc R U . . .
C42 C 0.3538(6) 0.4057(4) 0.1978(5) 0.056(2) Uani 1 1 d . . . . .
C75 C 0.8957(6) 0.4550(4) 1.2334(5) 0.047(2) Uani 1 1 d . . . . .
C49 C 0.2540(6) 0.4952(6) 0.1065(5) 0.067(3) Uani 1 1 d . . . . .
H49 H 0.2063 0.5095 0.0537 0.081 Uiso 1 1 calc R U . . .
C47 C 0.2793(6) 0.6122(5) 0.1657(5) 0.061(2) Uani 1 1 d . . . . .
H47 H 0.2349 0.6295 0.1130 0.073 Uiso 1 1 calc R U . . .
C82 C 1.1649(5) 0.7510(4) 1.0207(4) 0.0451(19) Uani 1 1 d . . . . .
C90 C 0.8919(8) 0.9314(5) 0.7872(6) 0.080(3) Uani 1 1 d . . . . .
H90 H 0.9150 0.9751 0.7974 0.096 Uiso 1 1 calc R U . . .
C83 C 1.2605(6) 0.7644(5) 1.0542(5) 0.057(2) Uani 1 1 d . . . . .
H83 H 1.2874 0.7977 1.0965 0.068 Uiso 1 1 calc R U . . .
C84 C 1.3136(6) 0.7304(6) 1.0268(5) 0.070(3) Uani 1 1 d . . . . .
H84 H 1.3759 0.7405 1.0493 0.085 Uiso 1 1 calc R U . . .
C67 C 0.9443(6) 0.4128(4) 1.3056(6) 0.056(2) Uani 1 1 d . . . . .
C71 C 0.9830(6) 0.6224(5) 1.3375(6) 0.064(3) Uani 1 1 d . . . . .
H71 H 1.0239 0.6410 1.3909 0.077 Uiso 1 1 calc R U . . .
C72 C 0.9342(6) 0.6627(5) 1.2688(6) 0.067(3) Uani 1 1 d . . . . .
H72 H 0.9406 0.7093 1.2744 0.080 Uiso 1 1 calc R U . . .
C39 C 0.4949(7) 0.3700(4) 0.3568(6) 0.067(3) Uani 1 1 d . . . . .
H39 H 0.5427 0.3574 0.4106 0.080 Uiso 1 1 calc R U . . .
C9 C 0.1379(7) 0.2747(6) 0.5138(7) 0.079(3) Uani 1 1 d . . . . .
H9A H 0.1943 0.2960 0.5312 0.095 Uiso 1 1 calc R U . . .
C86 C 1.1832(6) 0.6644(5) 0.9312(5) 0.059(2) Uani 1 1 d . . . . .
C59 C 0.8300(7) 0.4776(4) 0.9373(5) 0.052(2) Uani 1 1 d . . . . .
C91 C 0.8233(8) 0.9136(5) 0.7077(6) 0.080(3) Uani 1 1 d . . . . .
H91 H 0.7989 0.9452 0.6631 0.096 Uiso 1 1 calc R U . . .
C87 C 1.1249(5) 0.7009(4) 0.9549(4) 0.049(2) Uani 1 1 d . . . . .
C24 C -0.4389(7) 0.2888(7) 0.1062(6) 0.083(3) Uani 1 1 d . . . . .
H24 H -0.4697 0.3162 0.0576 0.100 Uiso 1 1 calc R U . . .
C58 C 0.6217(6) 0.4549(4) 0.9324(5) 0.054(2) Uani 1 1 d . . . . .
H58 H 0.5949 0.4264 0.8844 0.064 Uiso 1 1 calc R U . . .
C61 C 0.9710(8) 0.4873(5) 0.9307(7) 0.076(3) Uani 1 1 d . . . . .
H61 H 1.0075 0.4760 0.9045 0.091 Uiso 1 1 calc R U . . .
C100 C 0.7205(6) 0.8236(6) 0.6127(5) 0.069(3) Uani 1 1 d . . . . .
H100 H 0.6925 0.8537 0.5666 0.083 Uiso 1 1 calc R U . . .
C46 C 0.3259(6) 0.6535(5) 0.2335(5) 0.063(2) Uani 1 1 d . . . . .
H46 H 0.3144 0.6996 0.2274 0.076 Uiso 1 1 calc R U . . .
C99 C 0.6935(6) 0.7598(6) 0.5998(5) 0.069(3) Uani 1 1 d . . . . .
H99 H 0.6458 0.7467 0.5462 0.083 Uiso 1 1 calc R U . . .
C29 C 0.4089(7) 0.4356(5) 0.6019(5) 0.059(2) Uani 1 1 d . . . . .
H29 H 0.4348 0.4053 0.6480 0.070 Uiso 1 1 calc R U . . .
C28 C 0.3233(7) 0.4556(5) 0.5721(6) 0.066(3) Uani 1 1 d . . . . .
H28 H 0.2894 0.4373 0.5978 0.080 Uiso 1 1 calc R U . . .
C50 C 0.2798(7) 0.4292(6) 0.1164(5) 0.072(3) Uani 1 1 d . . . . .
H50 H 0.2497 0.3992 0.0705 0.087 Uiso 1 1 calc R U . . .
C54 C 0.4207(7) 0.4600(5) 0.9768(6) 0.072(3) Uani 1 1 d . . . . .
H54 H 0.3624 0.4408 0.9550 0.086 Uiso 1 1 calc R U . . .
C10 C 0.1100(6) 0.2221(5) 0.4505(6) 0.066(2) Uani 1 1 d . . . . .
H10 H 0.1485 0.2084 0.4274 0.079 Uiso 1 1 calc R U . . .
C85 C 1.2745(6) 0.6807(6) 0.9654(6) 0.074(3) Uani 1 1 d . . . . .
H85 H 1.3112 0.6575 0.9465 0.089 Uiso 1 1 calc R U . . .
C23 C -0.3786(7) 0.3187(6) 0.1895(6) 0.071(3) Uani 1 1 d . . . . .
C97 C 0.7183(6) 0.6410(5) 0.6584(6) 0.063(3) Uani 1 1 d . . . . .
H97 H 0.6749 0.6239 0.6051 0.076 Uiso 1 1 calc R U . . .
C34 C 0.8667(6) 0.4937(5) 0.5189(5) 0.064(3) Uani 1 1 d . . . . .
H34 H 0.9263 0.4776 0.5378 0.077 Uiso 1 1 calc R U . . .
C25 C -0.4507(6) 0.2234(7) 0.0985(6) 0.081(3) Uani 1 1 d . . . . .
H25 H -0.4915 0.2058 0.0444 0.097 Uiso 1 1 calc R U . . .
C41 C 0.3868(8) 0.3397(5) 0.2110(6) 0.081(3) Uani 1 1 d . . . . .
H41 H 0.3609 0.3080 0.1664 0.097 Uiso 1 1 calc R U . . .
C17 C -0.4036(5) 0.1777(6) 0.1697(5) 0.061(3) Uani 1 1 d . . . . .
C15 C -0.3659(7) 0.0694(5) 0.2357(6) 0.070(3) Uani 1 1 d . . . . .
H15 H -0.3729 0.0228 0.2328 0.084 Uiso 1 1 calc R U . . .
C20 C -0.2607(8) 0.3672(5) 0.3522(7) 0.080(3) Uani 1 1 d . . . . .
H20 H -0.2218 0.3844 0.4071 0.096 Uiso 1 1 calc R U . . .
C68 C 1.0067(7) 0.4417(6) 1.3881(6) 0.074(3) Uani 1 1 d . . . . .
H68 H 1.0383 0.4133 1.4355 0.089 Uiso 1 1 calc R U . . .
C21 C -0.3072(11) 0.4119(5) 0.2814(9) 0.114(5) Uani 1 1 d . . . . .
H21 H -0.2985 0.4581 0.2900 0.137 Uiso 1 1 calc R U . . .
C13 C 0.0475(7) 0.1258(6) 0.3190(6) 0.085(3) Uani 1 1 d . . . . .
H13A H 0.0158 0.0919 0.2758 0.127 Uiso 1 1 calc R U . . .
H13B H 0.1067 0.1090 0.3606 0.127 Uiso 1 1 calc R U . . .
H13C H 0.0555 0.1654 0.2914 0.127 Uiso 1 1 calc R U . . .
C2 C -0.3957(5) 0.2037(4) 0.4581(5) 0.051(2) Uani 1 1 d . . . . .
C53 C 0.4498(6) 0.5062(5) 1.0444(6) 0.063(3) Uani 1 1 d . . . . .
H53 H 0.4114 0.5166 1.0688 0.075 Uiso 1 1 calc R U . . .
C96 C 0.7630(7) 0.5995(5) 0.7261(6) 0.069(3) Uani 1 1 d . . . . .
H96 H 0.7505 0.5536 0.7200 0.082 Uiso 1 1 calc R U . . .
C64 C 0.8234(8) 0.3684(5) 1.1433(7) 0.083(3) Uani 1 1 d . . . . .
H64 H 0.7818 0.3526 1.0884 0.099 Uiso 1 1 calc R U . . .
C69 C 1.0204(6) 0.5072(6) 1.3987(6) 0.072(3) Uani 1 1 d . . . . .
H69 H 1.0622 0.5241 1.4529 0.086 Uiso 1 1 calc R U . . .
C16 C -0.4124(7) 0.1070(6) 0.1648(7) 0.072(3) Uani 1 1 d . . . . .
H16 H -0.4508 0.0865 0.1119 0.087 Uiso 1 1 calc R U . . .
C40 C 0.4575(9) 0.3219(5) 0.2897(7) 0.089(3) Uani 1 1 d . . . . .
H40 H 0.4809 0.2782 0.2989 0.106 Uiso 1 1 calc R U . . .
C22 C -0.3633(10) 0.3878(7) 0.2026(9) 0.105(4) Uani 1 1 d . . . . .
H22 H -0.3926 0.4173 0.1560 0.126 Uiso 1 1 calc R U . . .
C66 C 0.9285(9) 0.3446(6) 1.2887(8) 0.088(3) Uani 1 1 d . . . . .
H66 H 0.9604 0.3139 1.3333 0.106 Uiso 1 1 calc R U . . .
C51 C 0.5128(7) 0.6015(6) 1.1808(6) 0.093(4) Uani 1 1 d . . . . .
H51A H 0.4549 0.6182 1.1366 0.139 Uiso 1 1 calc R U . . .
H51B H 0.5434 0.6362 1.2232 0.139 Uiso 1 1 calc R U . . .
H51C H 0.5022 0.5632 1.2089 0.139 Uiso 1 1 calc R U . . .
C65 C 0.8677(9) 0.3212(5) 1.2086(8) 0.097(4) Uani 1 1 d . . . . .
H65 H 0.8562 0.2753 1.1981 0.117 Uiso 1 1 calc R U . . .
O18 O 0.6507(4) 0.3733(3) 0.7523(3) 0.0630(16) Uani 1 1 d G . . . .
H18A H 0.6853 0.3995 0.7933 0.094 Uiso 1 1 d G U . . .
H18B H 0.6165 0.3965 0.7075 0.094 Uiso 1 1 d G U . . .
O19 O 0.6331(6) 0.7021(4) 1.1017(5) 0.087(2) Uani 1 1 d G . . . .
H19A H 0.6318 0.6606 1.1130 0.131 Uiso 1 1 d G U . . .
H19B H 0.6637 0.7036 1.0733 0.131 Uiso 1 1 d G U . . .
O4 O 0.2944(4) 0.5705(3) 0.4054(3) 0.0522(14) Uani 1 1 d . . . . .
C88 C 1.1915(9) 0.5729(7) 0.8443(8) 0.135(5) Uani 1 1 d . U . . .
H88A H 1.1528 0.5385 0.8057 0.202 Uiso 1 1 calc R U . . .
H88B H 1.2422 0.5524 0.8933 0.202 Uiso 1 1 calc R U . . .
H88C H 1.2148 0.6011 0.8138 0.202 Uiso 1 1 calc R U . . .
O17 O 0.5164(5) 0.2932(4) 0.7596(4) 0.098(2) Uani 1 1 d . . . . .
H17A H 0.5376 0.3270 0.7448 0.147 Uiso 1 1 d R U . . .
H17B H 0.4905 0.2640 0.7196 0.147 Uiso 1 1 d R U . . .
O14 O -0.1085(5) 0.0223(4) 0.3787(4) 0.105(2) Uani 1 1 d . . . . .
H14A H -0.0713 0.0437 0.3631 0.157 Uiso 1 1 d R U . . .
H14B H -0.1264 0.0574 0.3983 0.157 Uiso 1 1 d R U . . .
O16 O 0.3611(6) 0.3073(4) 0.7866(7) 0.136(3) Uani 1 1 d . . . . .
H16A H 0.4167 0.3106 0.7959 0.204 Uiso 1 1 d R U . . .
H16B H 0.3613 0.2740 0.8175 0.204 Uiso 1 1 d R U . . .
O15 O -0.0534(6) -0.0741(5) 0.2872(6) 0.133(3) Uani 1 1 d . . . . .
H15A H -0.0178 -0.0746 0.2638 0.200 Uiso 1 1 d R U . . .
H15B H -0.0906 -0.0411 0.2733 0.200 Uiso 1 1 d R U . . .
C26 C 0.2089(6) 0.5929(5) 0.3801(6) 0.079(3) Uani 1 1 d . . . . .
H26A H 0.1946 0.6276 0.3372 0.118 Uiso 1 1 calc R U . . .
H26B H 0.2044 0.6108 0.4296 0.118 Uiso 1 1 calc R U . . .
H26C H 0.1660 0.5563 0.3556 0.118 Uiso 1 1 calc R U . . .
C63 C 1.0558(8) 0.6157(6) 1.1293(7) 0.089(3) Uani 1 1 d . U . . .
H63A H 1.1052 0.5852 1.1631 0.134 Uiso 1 1 calc R U . . .
H63B H 1.0574 0.6533 1.1649 0.134 Uiso 1 1 calc R U . . .
H63C H 1.0627 0.6315 1.0803 0.134 Uiso 1 1 calc R U . . .
C76 C 0.6571(7) 0.6557(5) 0.8929(6) 0.076(3) Uani 1 1 d . . . . .
H76A H 0.6410 0.6212 0.8493 0.115 Uiso 1 1 calc R U . . .
H76B H 0.6119 0.6910 0.8713 0.115 Uiso 1 1 calc R U . . .
H76C H 0.6588 0.6367 0.9446 0.115 Uiso 1 1 calc R U . . .
C1 C -0.5097(7) 0.1328(6) 0.3600(7) 0.089(3) Uani 1 1 d . U . . .
H1A H -0.5177 0.0958 0.3215 0.134 Uiso 1 1 calc R U . . .
H1B H -0.5544 0.1671 0.3292 0.134 Uiso 1 1 calc R U . . .
H1C H -0.5178 0.1173 0.4086 0.134 Uiso 1 1 calc R U . . .
O1W O -0.2367(7) -0.0842(5) 0.2584(6) 0.158(4) Uani 1 1 d . . . . .
H1WA H -0.2803 -0.1024 0.2648 0.237 Uiso 1 1 d R U . . .
H1WB H -0.2022 -0.1170 0.2606 0.237 Uiso 1 1 d R U . . .
O13 O 0.0862(4) -0.1320(3) 0.2568(3) 0.0680(18) Uani 1 1 d . . . . .
H13F H 0.1071 -0.1593 0.2995 0.102 Uiso 1 1 d R U . . .
H13G H 0.0678 -0.1538 0.2094 0.102 Uiso 1 1 d R U . . .
O20 O 0.5879(4) 0.7110(4) 0.3878(4) 0.092(2) Uani 1 1 d . . . . .
H20A H 0.5663 0.6725 0.3880 0.137 Uiso 1 1 d R U . . .
H20B H 0.6300 0.7057 0.3732 0.137 Uiso 1 1 d 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
Cu2 O5 1.926(5) . ?
Cu2 N10 1.936(6) . ?
Cu2 N12 2.003(6) . ?
Cu2 N8 2.020(6) . ?
Cu2 N11 2.306(6) . ?
Cu4 O11 1.904(5) . ?
Cu4 N22 1.936(6) . ?
Cu4 N20 2.010(6) . ?
Cu4 N23 2.020(5) . ?
Cu4 N24 2.285(6) . ?
Cu3 O8 1.922(5) . ?
Cu3 N16 1.950(6) . ?
Cu3 N14 2.013(6) . ?
Cu3 N18 2.018(6) . ?
Cu3 N17 2.266(7) . ?
Cu1 O2 1.925(5) . ?
Cu1 N4 1.948(6) . ?
Cu1 N5 2.007(6) . ?
Cu1 N2 2.011(6) . ?
Cu1 N6 2.283(7) . ?
O5 C37 1.309(8) . ?
O8 C57 1.290(8) . ?
O6 C36 1.366(9) . ?
O6 C38 1.430(9) . ?
O2 C12 1.315(9) . ?
N4 C6 1.289(10) . ?
N4 N3 1.382(8) . ?
O10 C76 1.333(10) . ?
O10 C77 1.384(9) . ?
N22 C81 1.306(9) . ?
N22 N21 1.388(8) . ?
O1 C1 1.266(11) . ?
O1 C2 1.425(10) . ?
N23 C95 1.322(9) . ?
N23 C94 1.334(8) . ?
N18 C73 1.316(10) . ?
N18 C74 1.358(9) . ?
O3 C11 1.377(10) . ?
O3 C13 1.432(9) . ?
N5 C14 1.323(10) . ?
N5 C18 1.354(9) . ?
O11 C87 1.312(9) . ?
N12 C45 1.317(10) . ?
N12 C44 1.358(9) . ?
N17 C64 1.310(11) . ?
N17 C75 1.344(10) . ?
C6 C7 1.433(11) . ?
N20 C77 1.336(9) . ?
N20 C80 1.396(9) . ?
C32 C37 1.414(10) . ?
C32 C33 1.418(11) . ?
C32 C31 1.435(10) . ?
N21 C80 1.312(10) . ?
N11 C39 1.315(10) . ?
N11 C43 1.338(9) . ?
O9 C63 1.195(11) . ?
O9 C62 1.397(10) . ?
N3 C5 1.326(10) . ?
N14 C62 1.336(10) . ?
N14 C59 1.382(10) . ?
N10 C31 1.289(10) . ?
N10 N9 1.379(8) . ?
N9 C30 1.324(10) . ?
N8 C27 1.348(9) . ?
N8 C30 1.372(10) . ?
N19 C77 1.305(9) . ?
N19 C78 1.361(10) . ?
N16 C58 1.273(10) . ?
N16 N15 1.387(9) . ?
N7 C27 1.312(10) . ?
N7 C28 1.378(12) . ?
N24 C89 1.312(10) . ?
N24 C93 1.356(9) . ?
N2 C2 1.357(9) . ?
N2 C5 1.381(10) . ?
N15 C59 1.309(11) . ?
N1 C2 1.309(9) . ?
N1 C3 1.350(12) . ?
C27 O4 1.390(9) . ?
O7 C52 1.362(9) . ?
O7 C51 1.420(10) . ?
C57 C56 1.408(11) . ?
C57 C52 1.432(11) . ?
C44 C48 1.410(9) . ?
C44 C43 1.443(11) . ?
C62 N13 1.301(10) . ?
C81 C82 1.415(10) . ?
C37 C36 1.410(10) . ?
C43 C42 1.400(10) . ?
C74 C70 1.406(10) . ?
C74 C75 1.441(12) . ?
N6 C20 1.322(11) . ?
N6 C19 1.354(10) . ?
C12 C7 1.392(11) . ?
C12 C11 1.435(11) . ?
N13 C61 1.369(13) . ?
C56 C58 1.430(12) . ?
C56 C55 1.439(12) . ?
C5 C4 1.416(11) . ?
C78 C79 1.349(11) . ?
C94 C98 1.419(9) . ?
C94 C93 1.442(10) . ?
C79 C80 1.422(11) . ?
O12 C86 1.385(11) . ?
O12 C88 1.401(11) . ?
C33 C34 1.357(11) . ?
C93 C92 1.396(10) . ?
C30 C29 1.426(11) . ?
C48 C47 1.411(12) . ?
C48 C49 1.413(12) . ?
C95 C96 1.384(11) . ?
C36 C35 1.383(11) . ?
C18 C17 1.413(10) . ?
C18 C19 1.425(12) . ?
C73 C72 1.393(11) . ?
C7 C8 1.413(11) . ?
C4 C3 1.356(13) . ?
C60 C61 1.324(13) . ?
C60 C59 1.442(12) . ?
C55 C54 1.360(13) . ?
C70 C71 1.399(13) . ?
C70 C69 1.419(12) . ?
C89 C90 1.383(12) . ?
C19 C23 1.391(11) . ?
C92 C91 1.387(13) . ?
C92 C100 1.414(12) . ?
C98 C97 1.403(12) . ?
C98 C99 1.442(12) . ?
C52 C53 1.365(11) . ?
C45 C46 1.387(11) . ?
C11 C10 1.342(11) . ?
C8 C9 1.364(13) . ?
C35 C34 1.367(11) . ?
C14 C15 1.383(12) . ?
C42 C41 1.395(13) . ?
C42 C50 1.445(12) . ?
C75 C67 1.405(11) . ?
C49 C50 1.361(13) . ?
C47 C46 1.341(12) . ?
C82 C83 1.419(11) . ?
C82 C87 1.423(11) . ?
C90 C91 1.358(13) . ?
C83 C84 1.349(12) . ?
C84 C85 1.371(13) . ?
C67 C66 1.383(14) . ?
C67 C68 1.435(13) . ?
C71 C72 1.347(12) . ?
C39 C40 1.405(13) . ?
C9 C10 1.425(13) . ?
C86 C85 1.366(12) . ?
C86 C87 1.402(11) . ?
C24 C25 1.309(15) . ?
C24 C23 1.444(14) . ?
C100 C99 1.326(13) . ?
C29 C28 1.311(13) . ?
C54 C53 1.385(12) . ?
C23 C22 1.393(16) . ?
C97 C96 1.338(12) . ?
C25 C17 1.433(13) . ?
C41 C40 1.363(14) . ?
C17 C16 1.409(14) . ?
C15 C16 1.332(13) . ?
C20 C21 1.413(14) . ?
C68 C69 1.319(14) . ?
C21 C22 1.331(17) . ?
C64 C65 1.386(14) . ?
C66 C65 1.360(16) . ?
O4 C26 1.334(10) . ?

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
O5 Cu2 N10 91.8(2) . . ?
O5 Cu2 N12 90.7(2) . . ?
N10 Cu2 N12 174.3(3) . . ?
O5 Cu2 N8 154.7(2) . . ?
N10 Cu2 N8 79.2(3) . . ?
N12 Cu2 N8 100.6(2) . . ?
O5 Cu2 N11 105.6(2) . . ?
N10 Cu2 N11 97.0(2) . . ?
N12 Cu2 N11 77.3(2) . . ?
N8 Cu2 N11 99.0(2) . . ?
O11 Cu4 N22 92.6(3) . . ?
O11 Cu4 N20 156.3(2) . . ?
N22 Cu4 N20 79.8(3) . . ?
O11 Cu4 N23 89.3(2) . . ?
N22 Cu4 N23 173.3(3) . . ?
N20 Cu4 N23 100.8(2) . . ?
O11 Cu4 N24 105.7(2) . . ?
N22 Cu4 N24 96.1(2) . . ?
N20 Cu4 N24 97.5(2) . . ?
N23 Cu4 N24 77.2(2) . . ?
O8 Cu3 N16 91.6(3) . . ?
O8 Cu3 N14 157.5(2) . . ?
N16 Cu3 N14 80.1(3) . . ?
O8 Cu3 N18 88.9(2) . . ?
N16 Cu3 N18 176.3(3) . . ?
N14 Cu3 N18 100.8(2) . . ?
O8 Cu3 N17 103.9(2) . . ?
N16 Cu3 N17 98.2(3) . . ?
N14 Cu3 N17 97.9(3) . . ?
N18 Cu3 N17 78.2(3) . . ?
O2 Cu1 N4 91.6(2) . . ?
O2 Cu1 N5 88.4(2) . . ?
N4 Cu1 N5 175.5(3) . . ?
O2 Cu1 N2 156.8(2) . . ?
N4 Cu1 N2 80.2(3) . . ?
N5 Cu1 N2 101.5(2) . . ?
O2 Cu1 N6 106.9(2) . . ?
N4 Cu1 N6 97.9(3) . . ?
N5 Cu1 N6 77.9(2) . . ?
N2 Cu1 N6 95.7(2) . . ?
C37 O5 Cu2 124.4(5) . . ?
C57 O8 Cu3 125.4(5) . . ?
C36 O6 C38 117.4(6) . . ?
C12 O2 Cu1 122.8(5) . . ?
C6 N4 N3 118.0(7) . . ?
C6 N4 Cu1 124.7(5) . . ?
N3 N4 Cu1 116.8(5) . . ?
C76 O10 C77 119.2(7) . . ?
C81 N22 N21 116.8(6) . . ?
C81 N22 Cu4 125.8(5) . . ?
N21 N22 Cu4 117.2(5) . . ?
C1 O1 C2 119.2(7) . . ?
C95 N23 C94 118.8(6) . . ?
C95 N23 Cu4 123.7(5) . . ?
C94 N23 Cu4 117.5(5) . . ?
C73 N18 C74 119.0(7) . . ?
C73 N18 Cu3 124.6(5) . . ?
C74 N18 Cu3 116.4(5) . . ?
C11 O3 C13 117.4(7) . . ?
C14 N5 C18 119.0(7) . . ?
C14 N5 Cu1 123.8(5) . . ?
C18 N5 Cu1 117.1(5) . . ?
C87 O11 Cu4 127.4(5) . . ?
C45 N12 C44 118.8(6) . . ?
C45 N12 Cu2 123.5(5) . . ?
C44 N12 Cu2 117.7(5) . . ?
C64 N17 C75 116.2(8) . . ?
C64 N17 Cu3 134.3(7) . . ?
C75 N17 Cu3 109.4(5) . . ?
N4 C6 C7 124.9(7) . . ?
C77 N20 C80 116.5(6) . . ?
C77 N20 Cu4 134.3(5) . . ?
C80 N20 Cu4 109.1(5) . . ?
C37 C32 C33 119.8(7) . . ?
C37 C32 C31 122.6(7) . . ?
C33 C32 C31 117.6(7) . . ?
C80 N21 N22 111.0(6) . . ?
C39 N11 C43 119.2(7) . . ?
C39 N11 Cu2 132.2(6) . . ?
C43 N11 Cu2 108.6(5) . . ?
C63 O9 C62 121.3(8) . . ?
C5 N3 N4 111.7(6) . . ?
C62 N14 C59 116.7(7) . . ?
C62 N14 Cu3 133.9(6) . . ?
C59 N14 Cu3 109.2(6) . . ?
C31 N10 N9 116.5(6) . . ?
C31 N10 Cu2 125.0(5) . . ?
N9 N10 Cu2 118.0(5) . . ?
C30 N9 N10 110.6(6) . . ?
C27 N8 C30 117.1(7) . . ?
C27 N8 Cu2 133.0(5) . . ?
C30 N8 Cu2 109.9(5) . . ?
C77 N19 C78 114.9(7) . . ?
C58 N16 N15 118.1(7) . . ?
C58 N16 Cu3 125.0(6) . . ?
N15 N16 Cu3 116.5(6) . . ?
C27 N7 C28 113.2(8) . . ?
C89 N24 C93 117.8(7) . . ?
C89 N24 Cu4 132.7(5) . . ?
C93 N24 Cu4 109.5(5) . . ?
C2 N2 C5 116.8(7) . . ?
C2 N2 Cu1 133.3(5) . . ?
C5 N2 Cu1 109.8(5) . . ?
C59 N15 N16 111.5(7) . . ?
C2 N1 C3 114.8(8) . . ?
N7 C27 N8 127.9(8) . . ?
N7 C27 O4 117.7(7) . . ?
N8 C27 O4 114.3(7) . . ?
C52 O7 C51 117.9(7) . . ?
O8 C57 C56 124.7(7) . . ?
O8 C57 C52 118.2(7) . . ?
C56 C57 C52 117.1(7) . . ?
N12 C44 C48 122.1(8) . . ?
N12 C44 C43 118.0(6) . . ?
C48 C44 C43 119.9(7) . . ?
N13 C62 N14 129.4(9) . . ?
N13 C62 O9 117.2(8) . . ?
N14 C62 O9 113.4(7) . . ?
N22 C81 C82 124.1(7) . . ?
O5 C37 C36 119.1(7) . . ?
O5 C37 C32 124.0(7) . . ?
C36 C37 C32 116.9(7) . . ?
N11 C43 C42 122.9(7) . . ?
N11 C43 C44 117.7(6) . . ?
C42 C43 C44 119.3(7) . . ?
N18 C74 C70 121.2(8) . . ?
N18 C74 C75 118.6(6) . . ?
C70 C74 C75 120.2(7) . . ?
C20 N6 C19 118.9(8) . . ?
C20 N6 Cu1 132.5(7) . . ?
C19 N6 Cu1 108.5(5) . . ?
O2 C12 C7 126.0(7) . . ?
O2 C12 C11 116.7(7) . . ?
C7 C12 C11 117.2(7) . . ?
C62 N13 C61 113.2(8) . . ?
C57 C56 C58 122.5(8) . . ?
C57 C56 C55 119.5(8) . . ?
C58 C56 C55 118.0(8) . . ?
N3 C5 N2 121.0(7) . . ?
N3 C5 C4 121.0(8) . . ?
N2 C5 C4 118.0(8) . . ?
N10 C31 C32 125.2(7) . . ?
C79 C78 N19 124.1(8) . . ?
N23 C94 C98 122.3(7) . . ?
N23 C94 C93 119.3(6) . . ?
C98 C94 C93 118.4(7) . . ?
C78 C79 C80 117.7(8) . . ?
C86 O12 C88 119.1(9) . . ?
C34 C33 C32 121.0(8) . . ?
N24 C93 C92 122.7(8) . . ?
N24 C93 C94 116.2(6) . . ?
C92 C93 C94 121.1(7) . . ?
N9 C30 N8 121.1(7) . . ?
N9 C30 C29 121.1(8) . . ?
N8 C30 C29 117.8(8) . . ?
C44 C48 C47 116.6(8) . . ?
C44 C48 C49 119.3(8) . . ?
C47 C48 C49 124.0(7) . . ?
N23 C95 C96 122.4(8) . . ?
O6 C36 C35 124.0(7) . . ?
O6 C36 C37 114.7(7) . . ?
C35 C36 C37 121.3(8) . . ?
N5 C18 C17 120.9(8) . . ?
N5 C18 C19 118.6(7) . . ?
C17 C18 C19 120.5(8) . . ?
N18 C73 C72 122.8(8) . . ?
C12 C7 C8 120.5(8) . . ?
C12 C7 C6 122.3(7) . . ?
C8 C7 C6 117.2(8) . . ?
C3 C4 C5 118.5(9) . . ?
N19 C77 N20 128.2(7) . . ?
N19 C77 O10 118.4(7) . . ?
N20 C77 O10 113.3(6) . . ?
C61 C60 C59 117.8(10) . . ?
C54 C55 C56 120.8(9) . . ?
N1 C3 C4 123.9(8) . . ?
C71 C70 C74 117.9(8) . . ?
C71 C70 C69 122.7(8) . . ?
C74 C70 C69 119.5(9) . . ?
N24 C89 C90 123.3(8) . . ?
N21 C80 N20 121.1(7) . . ?
N21 C80 C79 120.7(7) . . ?
N20 C80 C79 118.2(7) . . ?
N6 C19 C23 122.8(9) . . ?
N6 C19 C18 117.8(7) . . ?
C23 C19 C18 119.4(8) . . ?
C91 C92 C93 117.2(8) . . ?
C91 C92 C100 124.7(8) . . ?
C93 C92 C100 117.9(9) . . ?
C97 C98 C94 116.5(8) . . ?
C97 C98 C99 124.8(8) . . ?
C94 C98 C99 118.6(8) . . ?
O7 C52 C53 125.4(8) . . ?
O7 C52 C57 113.0(7) . . ?
C53 C52 C57 121.6(8) . . ?
N12 C45 C46 122.4(8) . . ?
C10 C11 O3 123.2(8) . . ?
C10 C11 C12 122.5(9) . . ?
O3 C11 C12 114.3(7) . . ?
C9 C8 C7 120.4(9) . . ?
C34 C35 C36 121.0(8) . . ?
N5 C14 C15 122.9(8) . . ?
C41 C42 C43 117.2(8) . . ?
C41 C42 C50 123.3(9) . . ?
C43 C42 C50 119.5(8) . . ?
N17 C75 C67 124.8(8) . . ?
N17 C75 C74 117.3(7) . . ?
C67 C75 C74 117.9(7) . . ?
C50 C49 C48 121.6(8) . . ?
C46 C47 C48 119.8(7) . . ?
C81 C82 C83 117.7(7) . . ?
C81 C82 C87 124.2(7) . . ?
C83 C82 C87 117.9(8) . . ?
C91 C90 C89 119.1(9) . . ?
C84 C83 C82 122.1(9) . . ?
C83 C84 C85 119.2(9) . . ?
C66 C67 C75 115.1(9) . . ?
C66 C67 C68 125.3(9) . . ?
C75 C67 C68 119.6(9) . . ?
C72 C71 C70 119.9(8) . . ?
C71 C72 C73 119.2(9) . . ?
N11 C39 C40 121.7(9) . . ?
C8 C9 C10 120.1(9) . . ?
C85 C86 O12 125.4(8) . . ?
C85 C86 C87 120.4(9) . . ?
O12 C86 C87 114.2(8) . . ?
N15 C59 N14 121.9(7) . . ?
N15 C59 C60 120.6(8) . . ?
N14 C59 C60 117.5(9) . . ?
C90 C91 C92 119.9(8) . . ?
O11 C87 C86 118.4(8) . . ?
O11 C87 C82 123.3(7) . . ?
C86 C87 C82 118.3(7) . . ?
C25 C24 C23 120.6(9) . . ?
N16 C58 C56 125.5(8) . . ?
C60 C61 N13 125.3(9) . . ?
C99 C100 C92 123.2(9) . . ?
C47 C46 C45 120.2(8) . . ?
C100 C99 C98 120.7(8) . . ?
C28 C29 C30 118.6(9) . . ?
C29 C28 N7 125.1(9) . . ?
C49 C50 C42 120.3(8) . . ?
C55 C54 C53 120.0(9) . . ?
C11 C10 C9 119.3(9) . . ?
C86 C85 C84 122.0(9) . . ?
C19 C23 C22 117.0(10) . . ?
C19 C23 C24 119.3(10) . . ?
C22 C23 C24 123.7(10) . . ?
C96 C97 C98 120.0(8) . . ?
C33 C34 C35 119.9(8) . . ?
C24 C25 C17 123.0(10) . . ?
C40 C41 C42 119.4(9) . . ?
C16 C17 C18 117.4(8) . . ?
C16 C17 C25 125.4(9) . . ?
C18 C17 C25 117.2(10) . . ?
C16 C15 C14 119.5(9) . . ?
N6 C20 C21 120.8(10) . . ?
C69 C68 C67 122.0(9) . . ?
C22 C21 C20 120.1(11) . . ?
N1 C2 N2 127.8(8) . . ?
N1 C2 O1 117.7(8) . . ?
N2 C2 O1 114.6(7) . . ?
C52 C53 C54 121.0(9) . . ?
C97 C96 C95 119.9(8) . . ?
N17 C64 C65 124.8(10) . . ?
C68 C69 C70 120.8(9) . . ?
C15 C16 C17 120.2(9) . . ?
C41 C40 C39 119.6(10) . . ?
C21 C22 C23 120.5(11) . . ?
C65 C66 C67 121.7(10) . . ?
C66 C65 C64 117.4(10) . . ?
C26 O4 C27 119.1(7) . . ?

_refine_diff_density_max         0.354
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.056

_shelxl_version_number           2014-3



