#------------------------------------------------------------------------------
#$Date: 2023-07-26 01:51:16 +0300 (Wed, 26 Jul 2023) $
#$Revision: 285337 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/35/7713560.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7713560
loop_
_publ_author_name
'P. Ferreira, Millena'
'Bezerra Castro, Caio'
'de Araújo Neto, João Honorato'
'he, sheng'
'Gonçalves Guimarães Júnior, Walber'
'Esmieu, Charlene'
'Castellano, Eduardo'
'de Moura, André Farias'
'Truzzi, Daniela Ramos'
'Nascimento, Otaciro'
'Simonneau, Antoine'
'Netto, Caterina Gruenwaldt Cunha Marques'
_publ_section_title
;
 Biomimetic catalysis of nitrite reductase enzyme using copper complexes
 in chemical and electrochemical reduction of nitrite
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01091K
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C31 H33 Cu N5 O2, 2(H2 O), 2(Cl O4)'
_chemical_formula_sum            'C31 H37 Cl2 Cu N5 O12'
_chemical_formula_weight         806.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-04
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0835(5)
_cell_length_b                   9.0835(5)
_cell_length_c                   42.651(4)
_cell_measurement_reflns_used    6999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6190
_cell_measurement_theta_min      2.6560
_cell_volume                     3519.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.25 117.00   0.75   50.00    --   27.63  54.00 -90.00  109
  2  ω     12.75 117.00   0.75   50.00    --   27.63  54.00  30.00  139
  3  ω    -69.00  47.25   0.75   50.00    --   27.63  54.00 120.00  155
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0775242000
_diffrn_orient_matrix_UB_12      -0.0083112000
_diffrn_orient_matrix_UB_13      0.0012524000
_diffrn_orient_matrix_UB_21      0.0100823000
_diffrn_orient_matrix_UB_22      0.0606119000
_diffrn_orient_matrix_UB_23      -0.0102561000
_diffrn_orient_matrix_UB_31      0.0003456000
_diffrn_orient_matrix_UB_32      0.0484205000
_diffrn_orient_matrix_UB_33      0.0130159000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            17810
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81338
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1789 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0425P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.776
_reflns_Friedel_fraction_max     0.775
_reflns_number_gt                5164
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01091k2.cif
_cod_data_source_block           complex8
_cod_original_cell_volume        3519.2(5)
_cod_database_code               7713560
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu1 P3 C55 H44 O5 F8 '
_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.
;
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.85 with sigma of 0.02
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 H2B-H1SA
 2.2 with sigma of 0.002
 H2A-H2B
 1.34 with sigma of 0.04
 H1A-H1B
 1.34 with sigma of 0.04
 Cu01-H2A \\sim Cu01-H2B
 with sigma of 0.02
 Cu01-H1A \\sim Cu01-H1B
 with sigma of 0.02
3.a Free rotating group:
 O2S(H2SA,H2SB), O1S(H1SA,H1SB)
3.b Ternary CH refined with riding coordinates:
 C22(H22)
3.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C23(H23A,H23B), C26(H26A,H26B)
3.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C31(H31), C8(H8), C12(H12), C5(H5), C18(H18), C30(H30),
 C15(H15), C19(H19), C1(H1), C4(H4), C28(H28), C13(H13), C21(H21), C17(H17),
 C2(H2), C3(H3), C20(H20), C29(H29)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.190
_oxdiff_exptl_absorpt_empirical_full_min 0.842
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu01 Cu 0.46053(6) 0.14322(6) 0.48330(2) 0.03469(15) Uani 1 1 d D . . . .
O2 O 0.4530(4) 0.3377(4) 0.46088(10) 0.0455(9) Uani 1 1 d D . . . .
H2A H 0.375(4) 0.386(5) 0.4599(16) 0.068 Uiso 1 1 d D U . . .
H2B H 0.514(4) 0.402(4) 0.4640(15) 0.068 Uiso 1 1 d D U . . .
N2 N 0.3971(4) 0.2327(4) 0.52263(9) 0.0346(9) Uani 1 1 d . . . . .
N4 N 0.4402(4) -0.0648(4) 0.50281(9) 0.0332(9) Uani 1 1 d . . . . .
O2S O 0.2111(5) 0.5203(5) 0.46246(13) 0.0643(11) Uani 1 1 d G . . . .
H2SA H 0.130949 0.518386 0.452191 0.096 Uiso 1 1 d G U . . .
H2SB H 0.184697 0.513246 0.481527 0.096 Uiso 1 1 d G U . . .
N3 N 0.2929(4) 0.1781(4) 0.54196(9) 0.0311(8) Uani 1 1 d . . . . .
N5 N 0.5085(4) 0.0320(4) 0.44544(10) 0.0384(9) Uani 1 1 d . . . . .
N1 N 0.4598(4) 0.3471(4) 0.53553(10) 0.0375(9) Uani 1 1 d . . . . .
O1 O 0.7096(4) 0.2020(4) 0.49196(12) 0.0639(12) Uani 1 1 d D . . . .
H1A H 0.748(5) 0.267(6) 0.5031(17) 0.096 Uiso 1 1 d D U . . .
H1B H 0.786(4) 0.151(6) 0.4880(19) 0.096 Uiso 1 1 d D U . . .
C11 C -0.0096(5) 0.1006(6) 0.56550(14) 0.0443(12) Uani 1 1 d . . . . .
H11 H -0.021648 0.178796 0.551656 0.053 Uiso 1 1 calc R U . . .
C10 C 0.1091(5) 0.0026(5) 0.56133(12) 0.0368(11) Uani 1 1 d . . . . .
O1S O 0.6669(6) 0.5421(5) 0.47570(14) 0.0833(15) Uani 1 1 d G . . . .
H1SA H 0.731586 0.508141 0.463265 0.125 Uiso 1 1 d DG U . . .
H1SB H 0.702791 0.528426 0.493864 0.125 Uiso 1 1 d G U . . .
C7 C 0.3966(5) 0.3679(5) 0.56398(12) 0.0331(10) Uani 1 1 d . . . . .
C14 C 0.0203(7) -0.1330(8) 0.60551(16) 0.0644(18) Uani 1 1 d . . . . .
H14 H 0.028984 -0.213010 0.618996 0.077 Uiso 1 1 calc R U . . .
C6 C 0.4462(5) 0.4852(5) 0.58554(11) 0.0365(11) Uani 1 1 d . . . . .
C31 C 0.5809(6) 0.0872(7) 0.42026(13) 0.0497(14) Uani 1 1 d . . . . .
H31 H 0.599671 0.187744 0.419095 0.060 Uiso 1 1 calc R U . . .
C8 C 0.2917(5) 0.2594(5) 0.56819(12) 0.0365(11) Uani 1 1 d . . . . .
H8 H 0.232290 0.245656 0.585704 0.044 Uiso 1 1 calc R U . . .
C12 C -0.1077(6) 0.0826(7) 0.58968(15) 0.0561(16) Uani 1 1 d . . . . .
H12 H -0.184351 0.149310 0.592349 0.067 Uiso 1 1 calc R U . . .
C22 C 0.3410(5) -0.0845(5) 0.53136(12) 0.0335(10) Uani 1 1 d . . . . .
H22 H 0.293525 -0.181063 0.529636 0.040 Uiso 1 1 calc R U . . .
C24 C 0.5977(6) -0.0535(7) 0.54659(14) 0.0533(14) Uani 1 1 d . . . . .
H24A H 0.615435 0.051846 0.546812 0.064 Uiso 1 1 calc R U . . .
H24B H 0.674290 -0.102238 0.558567 0.064 Uiso 1 1 calc R U . . .
C5 C 0.3513(6) 0.5465(6) 0.60711(13) 0.0465(13) Uani 1 1 d . . . . .
H5 H 0.253297 0.516935 0.607905 0.056 Uiso 1 1 calc R U . . .
C18 C -0.0247(6) -0.0832(7) 0.46640(16) 0.0573(16) Uani 1 1 d . . . . .
H18 H -0.078048 -0.166610 0.460871 0.069 Uiso 1 1 calc R U . . .
C30 C 0.6272(7) -0.0045(7) 0.39622(14) 0.0534(15) Uani 1 1 d . . . . .
H30 H 0.677084 0.033818 0.379015 0.064 Uiso 1 1 calc R U . . .
C25 C 0.5917(6) -0.1104(6) 0.51411(14) 0.0473(13) Uani 1 1 d . . . . .
H25A H 0.602577 -0.216610 0.513739 0.057 Uiso 1 1 calc R U . . .
H25B H 0.668237 -0.066617 0.501266 0.057 Uiso 1 1 calc R U . . .
C15 C 0.1216(7) -0.1162(6) 0.58142(14) 0.0510(14) Uani 1 1 d . . . . .
H15 H 0.197130 -0.184262 0.578805 0.061 Uiso 1 1 calc R U . . .
C27 C 0.4797(6) -0.1130(6) 0.44689(13) 0.0405(12) Uani 1 1 d . . . . .
C19 C -0.0182(7) 0.0308(8) 0.44635(16) 0.0623(17) Uani 1 1 d . . . . .
H19 H -0.064740 0.025002 0.426970 0.075 Uiso 1 1 calc R U . . .
C1 C 0.5906(6) 0.5338(6) 0.58410(14) 0.0472(13) Uani 1 1 d . . . . .
H1 H 0.654417 0.493822 0.569333 0.057 Uiso 1 1 calc R U . . .
C4 C 0.4039(8) 0.6532(6) 0.62770(14) 0.0582(16) Uani 1 1 d . . . . .
H4 H 0.341051 0.693073 0.642658 0.070 Uiso 1 1 calc R U . . .
C23 C 0.4462(6) -0.0896(6) 0.55952(13) 0.0450(13) Uani 1 1 d . . . . .
H23A H 0.417241 -0.017965 0.575216 0.054 Uiso 1 1 calc R U . . .
H23B H 0.445785 -0.186660 0.569001 0.054 Uiso 1 1 calc R U . . .
C28 C 0.5247(7) -0.2078(7) 0.42354(14) 0.0543(15) Uani 1 1 d . . . . .
H28 H 0.505056 -0.308026 0.425019 0.065 Uiso 1 1 calc R U . . .
C9 C 0.2162(5) 0.0349(5) 0.53417(11) 0.0312(10) Uani 1 1 d . . . . .
C16 C 0.1283(5) 0.0454(5) 0.50344(12) 0.0337(10) Uani 1 1 d . . . . .
C13 C -0.0928(7) -0.0341(8) 0.60994(15) 0.0629(18) Uani 1 1 d . . . . .
H13 H -0.158408 -0.046184 0.626483 0.076 Uiso 1 1 calc R U . . .
C21 C 0.1287(5) 0.1640(5) 0.48355(14) 0.0431(11) Uani 1 1 d . . . . .
H21 H 0.176696 0.250235 0.489374 0.052 Uiso 1 1 calc R U . . .
C17 C 0.0460(6) -0.0790(6) 0.49505(14) 0.0462(13) Uani 1 1 d . . . . .
H17 H 0.039071 -0.158423 0.508725 0.055 Uiso 1 1 calc R U . . .
C26 C 0.3967(6) -0.1594(5) 0.47570(12) 0.0421(12) Uani 1 1 d . . . . .
H26A H 0.291704 -0.150361 0.472005 0.051 Uiso 1 1 calc R U . . .
H26B H 0.418146 -0.261621 0.480419 0.051 Uiso 1 1 calc R U . . .
C2 C 0.6407(7) 0.6416(6) 0.60448(16) 0.0573(16) Uani 1 1 d . . . . .
H2 H 0.737699 0.674144 0.603408 0.069 Uiso 1 1 calc R U . . .
C3 C 0.5461(8) 0.6998(7) 0.62622(15) 0.0618(17) Uani 1 1 d . . . . .
H3 H 0.579283 0.771635 0.640060 0.074 Uiso 1 1 calc R U . . .
C20 C 0.0576(7) 0.1560(8) 0.45461(15) 0.0605(17) Uani 1 1 d . . . . .
H20 H 0.061360 0.235476 0.440883 0.073 Uiso 1 1 calc R U . . .
C29 C 0.5985(7) -0.1528(7) 0.39816(15) 0.0613(16) Uani 1 1 d . . . . .
H29 H 0.629273 -0.215667 0.382246 0.074 Uiso 1 1 calc R U . . .
Cl1C Cl 0.97221(16) 0.53007(14) 0.53755(4) 0.0528(4) Uani 1 1 d . . . . .
O4C O 0.8745(5) 0.6503(5) 0.53360(16) 0.0911(17) Uani 1 1 d . . . . .
O3C O 0.9819(6) 0.4890(7) 0.56970(13) 0.0912(15) Uani 1 1 d . . . . .
O1C O 1.1165(5) 0.5700(6) 0.52680(15) 0.0881(16) Uani 1 1 d . . . . .
O2C O 0.9200(8) 0.4089(6) 0.51971(17) 0.113(2) Uani 1 1 d . . . . .
Cl2C Cl 0.86492(18) 0.47323(18) 0.40013(4) 0.0614(4) Uani 1 1 d . . . . .
O8C O 0.8572(9) 0.5633(8) 0.37361(16) 0.129(3) Uani 1 1 d . . . . .
O5C O 0.9496(11) 0.5318(12) 0.4232(2) 0.175(4) Uani 1 1 d . . . . .
O6C O 0.9166(13) 0.3366(9) 0.3903(2) 0.185(5) Uani 1 1 d . . . . .
O7C O 0.7271(10) 0.4494(12) 0.4110(2) 0.184(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 6 29 0.0900
-1 -3 59 0.0509
-1 -13 -11 0.0693
1 4 -57 0.0588
1 12 21 0.0570
-11 -2 -25 0.0977
6 -8 -40 0.0729
12 2 21 0.0454
6 6 43 0.0599
-2 8 46 0.0761
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 Cu01 N4 171.55(16) . . ?
O2 Cu01 O1 84.72(16) . . ?
N2 Cu01 O2 91.88(16) . . ?
N2 Cu01 N4 90.48(16) . . ?
N2 Cu01 N5 172.65(17) . . ?
N2 Cu01 O1 93.12(16) . . ?
N4 Cu01 O1 103.27(16) . . ?
N5 Cu01 O2 93.94(17) . . ?
N5 Cu01 N4 83.13(17) . . ?
N5 Cu01 O1 91.87(17) . . ?
Cu01 O2 H2A 121(3) . . ?
Cu01 O2 H2B 122(4) . . ?
H2A O2 H2B 102(5) . . ?
N3 N2 Cu01 125.4(3) . . ?
N1 N2 Cu01 124.4(3) . . ?
N1 N2 N3 109.9(4) . . ?
C22 N4 Cu01 118.7(3) . . ?
C25 N4 Cu01 107.2(3) . . ?
C25 N4 C22 104.5(4) . . ?
C26 N4 Cu01 103.7(3) . . ?
C26 N4 C22 113.2(4) . . ?
C26 N4 C25 109.2(4) . . ?
H2SA O2S H2SB 104.5 . . ?
N2 N3 C9 120.4(4) . . ?
C8 N3 N2 108.2(3) . . ?
C8 N3 C9 130.8(4) . . ?
C31 N5 Cu01 124.9(4) . . ?
C27 N5 Cu01 115.2(3) . . ?
C27 N5 C31 119.6(5) . . ?
N2 N1 C7 107.7(4) . . ?
Cu01 O1 H1A 130(3) . . ?
Cu01 O1 H1B 129(3) . . ?
H1A O1 H1B 99(5) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C12 C11 C10 121.1(5) . . ?
C11 C10 C9 117.2(4) . . ?
C15 C10 C11 118.5(5) . . ?
C15 C10 C9 124.3(5) . . ?
H1SA O1S H1SB 104.5 . . ?
N1 C7 C6 121.9(4) . . ?
N1 C7 C8 108.0(4) . . ?
C8 C7 C6 130.0(5) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.6(6) . . ?
C5 C6 C7 121.0(4) . . ?
C5 C6 C1 119.6(5) . . ?
C1 C6 C7 119.4(5) . . ?
N5 C31 H31 119.6 . . ?
N5 C31 C30 120.7(5) . . ?
C30 C31 H31 119.6 . . ?
N3 C8 C7 106.2(4) . . ?
N3 C8 H8 126.9 . . ?
C7 C8 H8 126.9 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(6) . . ?
C13 C12 H12 120.0 . . ?
N4 C22 H22 107.8 . . ?
N4 C22 C23 105.1(4) . . ?
N4 C22 C9 113.9(4) . . ?
C23 C22 H22 107.8 . . ?
C23 C22 C9 114.2(4) . . ?
C9 C22 H22 107.8 . . ?
H24A C24 H24B 109.1 . . ?
C25 C24 H24A 111.1 . . ?
C25 C24 H24B 111.1 . . ?
C25 C24 C23 103.4(5) . . ?
C23 C24 H24A 111.1 . . ?
C23 C24 H24B 111.1 . . ?
C6 C5 H5 120.4 . . ?
C6 C5 C4 119.1(5) . . ?
C4 C5 H5 120.4 . . ?
C19 C18 H18 119.3 . . ?
C19 C18 C17 121.4(6) . . ?
C17 C18 H18 119.3 . . ?
C31 C30 H30 120.4 . . ?
C29 C30 C31 119.1(6) . . ?
C29 C30 H30 120.4 . . ?
N4 C25 H25A 111.0 . . ?
N4 C25 H25B 111.0 . . ?
C24 C25 N4 103.6(4) . . ?
C24 C25 H25A 111.0 . . ?
C24 C25 H25B 111.0 . . ?
H25A C25 H25B 109.0 . . ?
C10 C15 C14 119.4(6) . . ?
C10 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
N5 C27 C28 121.4(5) . . ?
N5 C27 C26 114.2(4) . . ?
C28 C27 C26 124.4(5) . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.7(6) . . ?
C20 C19 H19 120.1 . . ?
C6 C1 H1 119.7 . . ?
C6 C1 C2 120.6(6) . . ?
C2 C1 H1 119.7 . . ?
C5 C4 H4 119.5 . . ?
C3 C4 C5 120.9(6) . . ?
C3 C4 H4 119.5 . . ?
C22 C23 H23A 110.6 . . ?
C22 C23 H23B 110.6 . . ?
C24 C23 C22 105.9(4) . . ?
C24 C23 H23A 110.6 . . ?
C24 C23 H23B 110.6 . . ?
H23A C23 H23B 108.7 . . ?
C27 C28 H28 120.4 . . ?
C29 C28 C27 119.3(6) . . ?
C29 C28 H28 120.4 . . ?
N3 C9 C10 106.8(4) . . ?
N3 C9 C22 106.1(3) . . ?
N3 C9 C16 111.9(4) . . ?
C10 C9 C22 112.4(4) . . ?
C16 C9 C10 109.0(4) . . ?
C16 C9 C22 110.6(4) . . ?
C21 C16 C9 125.1(4) . . ?
C21 C16 C17 118.5(5) . . ?
C17 C16 C9 116.4(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 C14 119.4(6) . . ?
C12 C13 H13 120.3 . . ?
C16 C21 H21 119.8 . . ?
C16 C21 C20 120.3(5) . . ?
C20 C21 H21 119.8 . . ?
C18 C17 C16 119.8(5) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
N4 C26 C27 109.8(4) . . ?
N4 C26 H26A 109.7 . . ?
N4 C26 H26B 109.7 . . ?
C27 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.4(6) . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 120.4(6) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C19 C20 C21 120.1(6) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C30 C29 H29 120.1 . . ?
C28 C29 C30 119.9(5) . . ?
C28 C29 H29 120.1 . . ?
O4C Cl1C O3C 110.8(4) . . ?
O4C Cl1C O1C 109.8(3) . . ?
O4C Cl1C O2C 109.0(4) . . ?
O3C Cl1C O1C 108.5(3) . . ?
O2C Cl1C O3C 109.5(4) . . ?
O2C Cl1C O1C 109.3(4) . . ?
O5C Cl2C O8C 112.7(6) . . ?
O5C Cl2C O6C 112.1(6) . . ?
O6C Cl2C O8C 107.2(5) . . ?
O7C Cl2C O8C 108.9(6) . . ?
O7C Cl2C O5C 109.9(7) . . ?
O7C Cl2C O6C 105.8(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu01 O2 2.010(4) . ?
Cu01 N2 1.951(4) . ?
Cu01 N4 2.073(4) . ?
Cu01 N5 1.954(4) . ?
Cu01 O1 2.354(4) . ?
O2 H2A 0.84(2) . ?
O2 H2B 0.81(2) . ?
N2 N3 1.350(5) . ?
N2 N1 1.306(5) . ?
N4 C22 1.525(6) . ?
N4 C25 1.516(6) . ?
N4 C26 1.494(6) . ?
O2S H2SA 0.8497 . ?
O2S H2SB 0.8505 . ?
N3 C8 1.341(6) . ?
N3 C9 1.512(5) . ?
N5 C31 1.356(7) . ?
N5 C27 1.345(6) . ?
N1 C7 1.355(6) . ?
O1 H1A 0.84(3) . ?
O1 H1B 0.85(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.410(7) . ?
C11 C12 1.373(8) . ?
C10 C15 1.383(7) . ?
C10 C9 1.541(7) . ?
O1S H1SA 0.8500 . ?
O1S H1SB 0.8497 . ?
C7 C6 1.478(6) . ?
C7 C8 1.382(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(8) . ?
C14 C13 1.378(10) . ?
C6 C5 1.378(7) . ?
C6 C1 1.385(7) . ?
C31 H31 0.9300 . ?
C31 C30 1.387(8) . ?
C8 H8 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.374(10) . ?
C22 H22 0.9800 . ?
C22 C23 1.535(7) . ?
C22 C9 1.574(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.480(8) . ?
C24 C23 1.519(8) . ?
C5 H5 0.9300 . ?
C5 C4 1.392(8) . ?
C18 H18 0.9300 . ?
C18 C19 1.344(9) . ?
C18 C17 1.381(8) . ?
C30 H30 0.9300 . ?
C30 C29 1.375(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C15 H15 0.9300 . ?
C27 C28 1.378(8) . ?
C27 C26 1.502(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.375(9) . ?
C1 H1 0.9300 . ?
C1 C2 1.386(8) . ?
C4 H4 0.9300 . ?
C4 C3 1.361(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C28 H28 0.9300 . ?
C28 C29 1.368(9) . ?
C9 C16 1.538(7) . ?
C16 C21 1.371(7) . ?
C16 C17 1.401(7) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.395(8) . ?
C17 H17 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C2 H2 0.9300 . ?
C2 C3 1.370(10) . ?
C3 H3 0.9300 . ?
C20 H20 0.9300 . ?
C29 H29 0.9300 . ?
Cl1C O4C 1.417(5) . ?
Cl1C O3C 1.424(6) . ?
Cl1C O1C 1.435(5) . ?
Cl1C O2C 1.420(6) . ?
Cl2C O8C 1.398(6) . ?
Cl2C O5C 1.356(8) . ?
Cl2C O6C 1.391(7) . ?
Cl2C O7C 1.352(8) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu01 N2 N3 C8 172.8(3) . . . . ?
Cu01 N2 N3 C9 1.0(6) . . . . ?
Cu01 N2 N1 C7 -173.6(3) . . . . ?
Cu01 N4 C22 C23 -100.9(4) . . . . ?
Cu01 N4 C22 C9 24.7(5) . . . . ?
Cu01 N4 C25 C24 89.0(4) . . . . ?
Cu01 N4 C26 C27 39.1(5) . . . . ?
Cu01 N5 C31 C30 171.4(4) . . . . ?
Cu01 N5 C27 C28 -171.8(4) . . . . ?
Cu01 N5 C27 C26 8.1(6) . . . . ?
N2 N3 C8 C7 1.3(5) . . . . ?
N2 N3 C9 C10 178.2(4) . . . . ?
N2 N3 C9 C22 58.1(5) . . . . ?
N2 N3 C9 C16 -62.6(5) . . . . ?
N2 N1 C7 C6 177.4(4) . . . . ?
N2 N1 C7 C8 0.4(5) . . . . ?
N4 C22 C23 C24 7.0(5) . . . . ?
N4 C22 C9 N3 -69.3(5) . . . . ?
N4 C22 C9 C10 174.3(4) . . . . ?
N4 C22 C9 C16 52.3(5) . . . . ?
N3 N2 N1 C7 0.4(5) . . . . ?
N3 C9 C16 C21 5.8(6) . . . . ?
N3 C9 C16 C17 -176.4(4) . . . . ?
N5 C31 C30 C29 0.2(9) . . . . ?
N5 C27 C28 C29 -0.8(9) . . . . ?
N5 C27 C26 N4 -33.2(6) . . . . ?
N1 N2 N3 C8 -1.1(5) . . . . ?
N1 N2 N3 C9 -172.9(4) . . . . ?
N1 C7 C6 C5 152.7(5) . . . . ?
N1 C7 C6 C1 -27.6(7) . . . . ?
N1 C7 C8 N3 -1.1(5) . . . . ?
C11 C10 C15 C14 -1.9(8) . . . . ?
C11 C10 C9 N3 65.7(5) . . . . ?
C11 C10 C9 C22 -178.3(4) . . . . ?
C11 C10 C9 C16 -55.4(5) . . . . ?
C11 C12 C13 C14 -0.7(9) . . . . ?
C10 C11 C12 C13 -1.3(8) . . . . ?
C10 C9 C16 C21 123.7(5) . . . . ?
C10 C9 C16 C17 -58.5(5) . . . . ?
C7 C6 C5 C4 177.8(5) . . . . ?
C7 C6 C1 C2 -178.7(5) . . . . ?
C6 C7 C8 N3 -177.7(5) . . . . ?
C6 C5 C4 C3 1.6(9) . . . . ?
C6 C1 C2 C3 0.1(9) . . . . ?
C31 N5 C27 C28 1.2(8) . . . . ?
C31 N5 C27 C26 -179.0(5) . . . . ?
C31 C30 C29 C28 0.2(10) . . . . ?
C8 N3 C9 C10 8.5(7) . . . . ?
C8 N3 C9 C22 -111.6(5) . . . . ?
C8 N3 C9 C16 127.7(5) . . . . ?
C8 C7 C6 C5 -31.1(8) . . . . ?
C8 C7 C6 C1 148.7(5) . . . . ?
C12 C11 C10 C15 2.6(8) . . . . ?
C12 C11 C10 C9 -178.1(5) . . . . ?
C22 N4 C25 C24 -37.8(5) . . . . ?
C22 N4 C26 C27 169.1(4) . . . . ?
C22 C9 C16 C21 -112.3(5) . . . . ?
C22 C9 C16 C17 65.5(5) . . . . ?
C5 C6 C1 C2 1.1(8) . . . . ?
C5 C4 C3 C2 -0.4(9) . . . . ?
C18 C19 C20 C21 0.7(10) . . . . ?
C25 N4 C22 C23 18.4(5) . . . . ?
C25 N4 C22 C9 144.1(4) . . . . ?
C25 N4 C26 C27 -74.9(5) . . . . ?
C25 C24 C23 C22 -30.3(6) . . . . ?
C15 C10 C9 N3 -115.0(5) . . . . ?
C15 C10 C9 C22 1.0(7) . . . . ?
C15 C10 C9 C16 123.9(5) . . . . ?
C15 C14 C13 C12 1.3(10) . . . . ?
C27 N5 C31 C30 -0.9(8) . . . . ?
C27 C28 C29 C30 0.1(10) . . . . ?
C19 C18 C17 C16 -0.9(9) . . . . ?
C1 C6 C5 C4 -1.9(8) . . . . ?
C1 C2 C3 C4 -0.5(10) . . . . ?
C23 C22 C9 N3 51.5(5) . . . . ?
C23 C22 C9 C10 -65.0(5) . . . . ?
C23 C22 C9 C16 173.0(4) . . . . ?
C23 C24 C25 N4 42.0(5) . . . . ?
C28 C27 C26 N4 146.7(5) . . . . ?
C9 N3 C8 C7 171.9(4) . . . . ?
C9 C10 C15 C14 178.7(5) . . . . ?
C9 C22 C23 C24 -118.6(5) . . . . ?
C9 C16 C21 C20 173.1(5) . . . . ?
C9 C16 C17 C18 -174.0(5) . . . . ?
C16 C21 C20 C19 2.4(9) . . . . ?
C13 C14 C15 C10 0.1(9) . . . . ?
C21 C16 C17 C18 4.0(8) . . . . ?
C17 C18 C19 C20 -1.5(10) . . . . ?
C17 C16 C21 C20 -4.7(8) . . . . ?
C26 N4 C22 C23 137.1(4) . . . . ?
C26 N4 C22 C9 -97.2(4) . . . . ?
C26 N4 C25 C24 -159.2(4) . . . . ?
C26 C27 C28 C29 179.3(6) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-9.1312 6.4523 29.1554 -0.7250 0.0000 0.6887
-1.2205 -2.5428 58.6766 -0.0000 -0.7682 0.6402
-1.1660 -12.5493 -11.1043 -0.0000 -0.6585 -0.7526
1.3347 3.8591 -57.0087 0.0000 0.8320 -0.5547
0.9358 11.9524 21.3916 0.0000 0.5145 0.8575
-11.4666 -2.2589 -24.6219 -0.9010 0.0000 -0.4338
5.5893 -7.7219 -40.1403 0.4472 -0.0000 -0.8944
11.8699 1.6195 21.2400 0.9333 -0.0000 0.3590
6.2978 6.2933 43.3835 0.4903 -0.0000 0.8716
-2.0823 8.0785 45.6955 -0.1713 0.0000 0.9852
