#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:54:22 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262602 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/65/7706560.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_7706560
loop_
_publ_author_name
'Yang, Lin'
'Wang, Lihong'
'Lv, Xingpu'
'Chen, Jing-Huo'
'Wang, Yang'
'Yang, Guang'
_publ_section_title
;
 Complexation of triangular silver(I) or copper(I) nitropyrazolates with
 dibenzothiophenes having potential use in adsorptive desulfurization.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2915
_journal_page_last               2927
_journal_paper_doi               10.1039/d0dt04037a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '0.5(C42 H60 Cu6 N18 O12)'
_chemical_formula_sum            'C21 H30 Cu3 N9 O6'
_chemical_formula_weight         695.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-08 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.671(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6486(15)
_cell_length_b                   17.7157(10)
_cell_length_c                   12.7565(7)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    298.15(10)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.48
_cell_volume                     5570.0(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            69497
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.558
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0846 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.8542. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         9813
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0519
_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)+(0.0506P)²+17.8403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7444
_reflns_number_total             9813
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04037a2.cif
_cod_data_source_block           cu3(denpz)3
_cod_depositor_comments
'Adding full bibliography for 7706555--7706561.cif.'
_cod_database_code               7706560
_shelx_shelxl_version_number     2017/1
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C27B = C26-C27A
 1.5 with sigma of 0.005
 C27B-C28B = C27A-C28A
 1.52 with sigma of 0.005
 C7B-C6A = C7A-C6B
 1.52 with sigma of 0.005
 C5-C6B = C6A-C5
 1.5 with sigma of 0.005
 C7B-C6B = C7A-C6A
 1.52 with sigma of 0.005
 C23-C22A = C23-C22B
 1.52 with sigma of 0.005
 C31-C30A = C31-C30B
 1.5 with sigma of 0.005
 C29A-C30A = C29B-C30B
 1.52 with sigma of 0.005
 C41-C42A = C41-C42B
 1.52 with sigma of 0.005
 C5-C6A \\sim C5-C6B
 with sigma of 0.005
 C7B-C6A \\sim C7A-C6B
 with sigma of 0.005
 N8B-C11 \\sim N8A-C11
 with sigma of 0.02
 O3B-N8B \\sim O3A-N8A
 with sigma of 0.02
 O4B-N8B \\sim O4A-N8A
 with sigma of 0.02
3. Rigid bond restraints
 N7, O1, O2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N7 \\sim O1 \\sim O2: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C27A) \\sim Ueq, Uanis(C27B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6B) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22B) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42A) \\sim Ueq, Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O8) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O4B) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N8B) \\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(O3A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7B) = Uanis(C7A)
Uanis(C28A) = Uanis(C28B)
Uanis(C27A) = Uanis(C27B)
Uanis(C6A) = Uanis(C6B)
Uanis(C22B) = Uanis(C22A)
Uanis(C30A) = Uanis(C30B)
Uanis(C29B) = Uanis(C29A)
Uanis(C42A) = Uanis(C42B)
Uanis(N8B) = Uanis(N8A)
Uanis(O4B) = Uanis(O4A)
Uanis(O3A) = Uanis(O3B)
5. Others
 Fixed Sof: C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) C7A(0.5)
 H7AA(0.5) H7AB(0.5) H7AC(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) N8A(0.5)
 N8B(0.5) O3A(0.5) O3B(0.5) O4A(0.5) O4B(0.5) C22A(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5) H23C(0.7) H23D(0.7)
 H23A(0.3) H23B(0.3) C27A(0.5) H27A(0.5) H27B(0.5) C27B(0.5) H27C(0.5)
 H27D(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C28B(0.5) H28D(0.5)
 H28E(0.5) H28F(0.5) C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C29B(0.5)
 H29D(0.5) H29E(0.5) H29F(0.5) C30A(0.5) H30A(0.5) H30B(0.5) C30B(0.5)
 H30C(0.5) H30D(0.5) H41C(0.6) H41D(0.6) H41A(0.4) H41B(0.4) C42A(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C42B(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C9(H9A,H9B), C13(H13A,H13B),
 C16(H16A,H16B), C20(H20A,H20B), C23(H23C,H23D), C23(H23A,H23B), C27A(H27A,
 H27B), C27B(H27C,H27D), C30A(H30A,H30B), C30B(H30C,H30D), C34(H34A,H34B),
 C37(H37A,H37B), C41(H41C,H41D), C41(H41A,H41B)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C8(H8A,H8B,H8C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22A(H22A,H22B,
 H22C), C22B(H22D,H22E,H22F), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F),
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C42A(H42A,H42B,H42C), C42B(H42D,H42E,H42F)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3074(4) 0.7364(6) -0.2159(8) 0.124(3) Uani 1 1 d . . . . .
H1A H 0.319853 0.780225 -0.252751 0.186 Uiso 1 1 calc GR . . . .
H1B H 0.316682 0.740893 -0.142907 0.186 Uiso 1 1 calc GR . . . .
H1C H 0.268743 0.732202 -0.223853 0.186 Uiso 1 1 calc GR . . . .
C2 C 0.3339(3) 0.6671(4) -0.2603(6) 0.083(2) Uani 1 1 d . . . . .
H2A H 0.320223 0.622699 -0.224888 0.100 Uiso 1 1 calc R . . . .
H2B H 0.324677 0.662795 -0.334142 0.100 Uiso 1 1 calc R . . . .
C3 C 0.3945(3) 0.6702(4) -0.2475(5) 0.0647(17) Uani 1 1 d . . . . .
C4 C 0.4349(3) 0.7036(4) -0.3068(5) 0.0775(19) Uani 1 1 d . U . . .
C5 C 0.4858(3) 0.6890(5) -0.2606(6) 0.091(2) Uani 1 1 d D U . . .
C6A C 0.5434(5) 0.7172(14) -0.2694(18) 0.122(5) Uani 0.5 1 d D U P A 1
H6AA H 0.564732 0.704251 -0.207632 0.147 Uiso 0.5 1 calc R . P A 1
H6AB H 0.544394 0.771385 -0.279728 0.147 Uiso 0.5 1 calc R . P A 1
C6B C 0.5353(6) 0.7359(10) -0.284(2) 0.122(5) Uani 0.5 1 d D U P A 2
H6BA H 0.548251 0.765650 -0.225117 0.147 Uiso 0.5 1 calc R . P A 2
H6BB H 0.531604 0.766672 -0.346678 0.147 Uiso 0.5 1 calc R . P A 2
C7A C 0.5632(10) 0.6756(13) -0.3651(14) 0.115(5) Uani 0.5 1 d D . P A 1
H7AA H 0.541847 0.690257 -0.425111 0.172 Uiso 0.5 1 calc GR . P A 1
H7AB H 0.559777 0.622220 -0.354173 0.172 Uiso 0.5 1 calc GR . P A 1
H7AC H 0.600569 0.687991 -0.376660 0.172 Uiso 0.5 1 calc GR . P A 1
C7B C 0.5667(10) 0.6637(12) -0.3007(15) 0.115(5) Uani 0.5 1 d D . P A 2
H7BA H 0.557007 0.642453 -0.367554 0.172 Uiso 0.5 1 calc GR . P A 2
H7BB H 0.558196 0.628398 -0.246217 0.172 Uiso 0.5 1 calc GR . P A 2
H7BC H 0.604897 0.674387 -0.298839 0.172 Uiso 0.5 1 calc GR . P A 2
C8 C 0.6530(4) 0.7120(6) -0.0363(9) 0.142(4) Uani 1 1 d . . . . .
H8A H 0.669271 0.728508 -0.100367 0.213 Uiso 1 1 calc GR . . . .
H8B H 0.673653 0.730825 0.022290 0.213 Uiso 1 1 calc GR . . . .
H8C H 0.616514 0.730851 -0.032992 0.213 Uiso 1 1 calc GR . . . .
C9 C 0.6521(3) 0.6272(5) -0.0332(7) 0.094(3) Uani 1 1 d . . . . .
H9A H 0.636719 0.608566 -0.098492 0.113 Uiso 1 1 calc R . . . .
H9B H 0.689161 0.608930 -0.027932 0.113 Uiso 1 1 calc R . . . .
C10 C 0.6204(2) 0.5957(4) 0.0560(6) 0.0649(17) Uani 1 1 d . . . . .
C11 C 0.6330(3) 0.5754(4) 0.1579(7) 0.077(2) Uani 1 1 d D . . . .
C12 C 0.5858(2) 0.5505(4) 0.2057(5) 0.0628(16) Uani 1 1 d . . . . .
C13 C 0.5733(3) 0.5223(4) 0.3137(5) 0.085(2) Uani 1 1 d . . . . .
H13A H 0.540848 0.491336 0.310144 0.102 Uiso 1 1 calc R . . . .
H13B H 0.602918 0.490606 0.338066 0.102 Uiso 1 1 calc R . . . .
C14 C 0.5647(5) 0.5841(6) 0.3912(6) 0.127(4) Uani 1 1 d . . . . .
H14A H 0.539267 0.619956 0.363007 0.191 Uiso 1 1 calc GR . . . .
H14B H 0.598661 0.608926 0.405575 0.191 Uiso 1 1 calc GR . . . .
H14C H 0.550840 0.563276 0.454957 0.191 Uiso 1 1 calc GR . . . .
C15 C 0.4006(5) 0.6064(5) 0.4196(6) 0.119(4) Uani 1 1 d . . . . .
H15A H 0.420052 0.643606 0.380177 0.179 Uiso 1 1 calc GR . . . .
H15B H 0.420034 0.595865 0.483650 0.179 Uiso 1 1 calc GR . . . .
H15C H 0.365158 0.625234 0.435529 0.179 Uiso 1 1 calc GR . . . .
C16 C 0.3954(3) 0.5345(4) 0.3555(5) 0.0713(19) Uani 1 1 d . . . . .
H16A H 0.431302 0.513878 0.343908 0.086 Uiso 1 1 calc R . . . .
H16B H 0.375002 0.497609 0.395100 0.086 Uiso 1 1 calc R . . . .
C17 C 0.3682(2) 0.5465(3) 0.2530(4) 0.0504(13) Uani 1 1 d . . . . .
C18 C 0.3142(2) 0.5574(3) 0.2245(5) 0.0566(15) Uani 1 1 d . . . . .
C19 C 0.3114(2) 0.5678(3) 0.1168(5) 0.0514(14) Uani 1 1 d . . . . .
C20 C 0.2659(2) 0.5781(4) 0.0421(6) 0.0703(18) Uani 1 1 d . . . . .
H20A H 0.236653 0.544290 0.060873 0.084 Uiso 1 1 calc R . . . .
H20B H 0.277823 0.564440 -0.027537 0.084 Uiso 1 1 calc R . . . .
C21 C 0.2441(3) 0.6598(5) 0.0396(7) 0.101(3) Uani 1 1 d . . . . .
H21A H 0.269724 0.691912 0.005194 0.151 Uiso 1 1 calc GR . . . .
H21B H 0.238878 0.677303 0.110038 0.151 Uiso 1 1 calc GR . . . .
H21C H 0.210111 0.661079 0.002124 0.151 Uiso 1 1 calc GR . . . .
Cu1 Cu 0.39169(3) 0.59786(4) -0.04414(5) 0.05175(19) Uani 1 1 d . . . . .
Cu2 Cu 0.52111(3) 0.61074(5) -0.06727(5) 0.0613(2) Uani 1 1 d . . . . .
Cu3 Cu 0.47152(3) 0.54962(4) 0.14612(5) 0.04611(18) Uani 1 1 d . . . . .
N1 N 0.4198(2) 0.6365(3) -0.1675(3) 0.0565(12) Uani 1 1 d . . . . .
N2 N 0.4750(2) 0.6461(3) -0.1738(4) 0.0719(16) Uani 1 1 d . . . . .
N3 N 0.56760(17) 0.5851(3) 0.0431(4) 0.0517(11) Uani 1 1 d . . . . .
N4 N 0.54609(18) 0.5574(3) 0.1350(3) 0.0517(11) Uani 1 1 d . . . . .
N5 N 0.39731(17) 0.5519(2) 0.1660(3) 0.0454(10) Uani 1 1 d . . . . .
N6 N 0.36281(17) 0.5653(2) 0.0816(3) 0.0458(10) Uani 1 1 d . . . . .
N7 N 0.4260(4) 0.7483(4) -0.4019(6) 0.1013(19) Uani 1 1 d . U . . .
N8A N 0.6855(6) 0.5907(12) 0.2065(14) 0.104(4) Uani 0.5 1 d D U P B 1
N8B N 0.6861(6) 0.5657(12) 0.2094(14) 0.104(4) Uani 0.5 1 d D U P B 2
N9 N 0.2694(2) 0.5582(4) 0.2961(5) 0.0784(17) Uani 1 1 d . . . . .
O1 O 0.3804(3) 0.7553(3) -0.4342(4) 0.1095(17) Uani 1 1 d . U . . .
O2 O 0.4647(3) 0.7744(5) -0.4412(5) 0.143(2) Uani 1 1 d . U . . .
O3A O 0.7241(7) 0.5989(11) 0.1385(13) 0.122(4) Uani 0.5 1 d D U P B 1
O3B O 0.7203(7) 0.6184(11) 0.1809(14) 0.122(4) Uani 0.5 1 d D U P B 2
O4A O 0.6885(8) 0.5749(9) 0.2996(14) 0.127(4) Uani 0.5 1 d D U P B 1
O4B O 0.6883(8) 0.5339(9) 0.2948(14) 0.127(4) Uani 0.5 1 d D U P B 2
O5 O 0.2782(2) 0.5396(4) 0.3868(5) 0.122(2) Uani 1 1 d . . . . .
O6 O 0.2253(2) 0.5764(4) 0.2630(5) 0.1050(19) Uani 1 1 d . . . . .
C22A C 0.1302(10) 0.3970(14) -0.8959(19) 0.119(6) Uani 0.5 1 d D U P C 1
H22A H 0.164575 0.371498 -0.896646 0.178 Uiso 0.5 1 calc GR . P C 1
H22B H 0.123653 0.420309 -0.962809 0.178 Uiso 0.5 1 calc GR . P C 1
H22C H 0.101950 0.361178 -0.882055 0.178 Uiso 0.5 1 calc GR . P C 1
C22B C 0.1053(9) 0.3975(14) -0.882(2) 0.119(6) Uani 0.5 1 d D U P C 2
H22D H 0.132119 0.360647 -0.900303 0.178 Uiso 0.5 1 calc GR . P C 2
H22E H 0.091419 0.421124 -0.944406 0.178 Uiso 0.5 1 calc GR . P C 2
H22F H 0.076178 0.373187 -0.845740 0.178 Uiso 0.5 1 calc GR . P C 2
C23 C 0.1309(3) 0.4568(5) -0.8112(6) 0.100(3) Uani 1 1 d D . . . .
H23C H 0.163925 0.475556 -0.842671 0.120 Uiso 0.7 1 calc R . P C 2
H23D H 0.106143 0.498904 -0.803277 0.120 Uiso 0.7 1 calc R . P C 2
H23A H 0.157863 0.494733 -0.827825 0.120 Uiso 0.3 1 calc R . P C 1
H23B H 0.095780 0.481385 -0.809111 0.120 Uiso 0.3 1 calc R . P C 1
C24 C 0.1438(3) 0.4232(4) -0.7056(5) 0.0610(16) Uani 1 1 d . . . . .
C25 C 0.1901(2) 0.3920(4) -0.6604(5) 0.0669(18) Uani 1 1 d . . . . .
C26 C 0.1794(2) 0.3761(4) -0.5554(5) 0.0648(17) Uani 1 1 d D . . . .
C27A C 0.2189(10) 0.3451(16) -0.4757(17) 0.105(5) Uani 0.5 1 d D U P D 1
H27A H 0.223854 0.383344 -0.421948 0.126 Uiso 0.5 1 calc R . P D 1
H27B H 0.253476 0.339100 -0.510082 0.126 Uiso 0.5 1 calc R . P D 1
C27B C 0.2120(11) 0.3602(16) -0.4570(14) 0.105(5) Uani 0.5 1 d D U P D 2
H27C H 0.192937 0.374507 -0.393930 0.126 Uiso 0.5 1 calc R . P D 2
H27D H 0.247538 0.383667 -0.457818 0.126 Uiso 0.5 1 calc R . P D 2
C28A C 0.206(2) 0.2716(18) -0.421(2) 0.133(8) Uani 0.5 1 d D . P D 1
H28A H 0.198847 0.233220 -0.472223 0.199 Uiso 0.5 1 calc GR . P D 1
H28B H 0.175219 0.278109 -0.377195 0.199 Uiso 0.5 1 calc GR . P D 1
H28C H 0.236920 0.256705 -0.378477 0.199 Uiso 0.5 1 calc GR . P D 1
C28B C 0.215(2) 0.2755(15) -0.472(2) 0.133(8) Uani 0.5 1 d D . P D 2
H28D H 0.227572 0.264295 -0.540693 0.199 Uiso 0.5 1 calc GR . P D 2
H28E H 0.179050 0.254312 -0.463553 0.199 Uiso 0.5 1 calc GR . P D 2
H28F H 0.238848 0.254097 -0.420324 0.199 Uiso 0.5 1 calc GR . P D 2
C29A C 0.1265(13) 0.332(2) -0.1409(19) 0.131(8) Uani 0.5 1 d D . P E 1
H29A H 0.117009 0.383770 -0.156432 0.196 Uiso 0.5 1 calc GR . P E 1
H29B H 0.165273 0.326979 -0.141676 0.196 Uiso 0.5 1 calc GR . P E 1
H29C H 0.113318 0.319199 -0.072788 0.196 Uiso 0.5 1 calc GR . P E 1
C29B C 0.1433(12) 0.338(2) -0.202(2) 0.131(8) Uani 0.5 1 d D . P F 2
H29D H 0.157586 0.330935 -0.271308 0.196 Uiso 0.5 1 calc GR . P F 2
H29E H 0.171402 0.329598 -0.151052 0.196 Uiso 0.5 1 calc GR . P F 2
H29F H 0.130395 0.389349 -0.196020 0.196 Uiso 0.5 1 calc GR . P F 2
C30A C 0.1012(5) 0.2807(18) -0.2225(13) 0.071(4) Uani 0.5 1 d D . P E 1
H30A H 0.120139 0.284232 -0.288600 0.085 Uiso 0.5 1 calc R . P E 1
H30B H 0.101612 0.228616 -0.199034 0.085 Uiso 0.5 1 calc R . P E 1
C30B C 0.0969(5) 0.2840(17) -0.1846(14) 0.071(4) Uani 0.5 1 d D . P F 2
H30C H 0.106324 0.235279 -0.214035 0.085 Uiso 0.5 1 calc R . P F 2
H30D H 0.092142 0.277355 -0.109840 0.085 Uiso 0.5 1 calc R . P F 2
C31 C 0.0442(2) 0.3100(3) -0.2327(4) 0.0581(15) Uani 1 1 d D . . . .
C32 C -0.0060(3) 0.2977(3) -0.1870(4) 0.0559(15) Uani 1 1 d . . . . .
C33 C -0.0458(2) 0.3323(3) -0.2504(4) 0.0464(13) Uani 1 1 d . . . . .
C34 C -0.1056(2) 0.3331(4) -0.2459(5) 0.0638(17) Uani 1 1 d . . . . .
H34A H -0.119327 0.375100 -0.287236 0.077 Uiso 1 1 calc R . . . .
H34B H -0.116623 0.340801 -0.173964 0.077 Uiso 1 1 calc R . . . .
C35 C -0.1307(3) 0.2598(4) -0.2871(6) 0.085(2) Uani 1 1 d . . . . .
H35A H -0.116240 0.248458 -0.354858 0.128 Uiso 1 1 calc GR . . . .
H35B H -0.169378 0.265498 -0.292799 0.128 Uiso 1 1 calc GR . . . .
H35C H -0.122315 0.219332 -0.239545 0.128 Uiso 1 1 calc GR . . . .
C36 C -0.1951(3) 0.3461(4) -0.5439(6) 0.078(2) Uani 1 1 d . . . . .
H36A H -0.209357 0.333394 -0.611919 0.117 Uiso 1 1 calc GR . . . .
H36B H -0.223064 0.341020 -0.492693 0.117 Uiso 1 1 calc GR . . . .
H36C H -0.165586 0.312781 -0.526483 0.117 Uiso 1 1 calc GR . . . .
C37 C -0.1748(2) 0.4269(3) -0.5447(5) 0.0565(15) Uani 1 1 d . . . . .
H37A H -0.204368 0.459796 -0.565759 0.068 Uiso 1 1 calc R . . . .
H37B H -0.163875 0.440828 -0.473955 0.068 Uiso 1 1 calc R . . . .
C38 C -0.1279(2) 0.4396(3) -0.6164(4) 0.0450(12) Uani 1 1 d . . . . .
C39 C -0.1264(2) 0.4533(3) -0.7241(4) 0.0483(13) Uani 1 1 d . . . . .
C40 C -0.0714(2) 0.4608(3) -0.7494(4) 0.0475(13) Uani 1 1 d . . . . .
C41 C -0.0438(3) 0.4753(4) -0.8514(4) 0.0673(18) Uani 1 1 d D . . . .
H41C H -0.005390 0.483012 -0.838216 0.081 Uiso 0.6 1 calc R . P G 2
H41D H -0.058303 0.521302 -0.882115 0.081 Uiso 0.6 1 calc R . P G 2
H41A H -0.009933 0.501561 -0.837775 0.081 Uiso 0.4 1 calc R . P H 1
H41B H -0.066581 0.508030 -0.894183 0.081 Uiso 0.4 1 calc R . P H 1
C42A C -0.0322(11) 0.4032(12) -0.912(2) 0.094(6) Uani 0.5 1 d D U P I 1
H42A H -0.008415 0.371538 -0.871349 0.141 Uiso 0.5 1 calc GR . P I 1
H42B H -0.015256 0.415704 -0.977171 0.141 Uiso 0.5 1 calc GR . P I 1
H42C H -0.065609 0.377007 -0.925875 0.141 Uiso 0.5 1 calc GR . P I 1
C42B C -0.0512(11) 0.4109(14) -0.929(2) 0.094(6) Uani 0.5 1 d D U P I 2
H42D H -0.037612 0.365021 -0.898480 0.141 Uiso 0.5 1 calc GR . P I 2
H42E H -0.031515 0.421916 -0.991727 0.141 Uiso 0.5 1 calc GR . P I 2
H42F H -0.089001 0.405166 -0.945857 0.141 Uiso 0.5 1 calc GR . P I 2
Cu4 Cu 0.03213(3) 0.44407(4) -0.64115(5) 0.04731(18) Uani 1 1 d . . . . .
Cu5 Cu 0.08181(3) 0.37708(4) -0.42790(5) 0.05157(19) Uani 1 1 d . . . . .
Cu6 Cu -0.04768(3) 0.40606(4) -0.45251(5) 0.04546(18) Uani 1 1 d . . . . .
N10 N 0.10596(18) 0.4248(3) -0.6317(3) 0.0495(11) Uani 1 1 d . . . . .
N11 N 0.12758(17) 0.3950(3) -0.5402(3) 0.0491(11) Uani 1 1 d . . . . .
N12 N 0.03572(18) 0.3513(3) -0.3184(3) 0.0496(11) Uani 1 1 d . . . . .
N13 N -0.01978(17) 0.3645(2) -0.3291(3) 0.0448(10) Uani 1 1 d . . . . .
N14 N -0.07764(17) 0.4386(2) -0.5800(3) 0.0414(10) Uani 1 1 d . . . . .
N15 N -0.04223(17) 0.4511(2) -0.6623(3) 0.0435(10) Uani 1 1 d . . . . .
N16 N 0.2395(3) 0.3783(4) -0.7133(6) 0.0933(19) Uani 1 1 d . U . . .
N17 N -0.0166(3) 0.2553(3) -0.0948(4) 0.0774(17) Uani 1 1 d . . . . .
N18 N -0.1703(2) 0.4565(3) -0.7960(5) 0.0702(15) Uani 1 1 d . . . . .
O7 O 0.2440(3) 0.4004(4) -0.8031(5) 0.121(2) Uani 1 1 d . U . . .
O8 O 0.2763(3) 0.3480(5) -0.6648(6) 0.149(3) Uani 1 1 d . U . . .
O9 O 0.0222(3) 0.2281(5) -0.0479(5) 0.143(3) Uani 1 1 d . U . . .
O10 O -0.0622(2) 0.2480(3) -0.0642(4) 0.0923(16) Uani 1 1 d . . . . .
O11 O -0.2150(2) 0.4388(4) -0.7644(5) 0.108(2) Uani 1 1 d . . . . .
O12 O -0.1621(2) 0.4759(4) -0.8854(4) 0.108(2) 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'
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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C1 111.5(7) . . ?
C4 C3 C2 132.5(6) . . ?
N1 C3 C2 121.6(6) . . ?
N1 C3 C4 105.9(6) . . ?
C3 C4 C5 109.6(6) . . ?
C3 C4 N7 125.4(7) . . ?
C5 C4 N7 125.0(7) . . ?
C4 C5 C6A 138.1(13) . . ?
C4 C5 C6B 122.4(11) . . ?
N2 C5 C4 105.0(6) . . ?
N2 C5 C6A 115.8(12) . . ?
N2 C5 C6B 129.1(13) . . ?
C5 C6A C7A 102.2(13) . . ?
C5 C6B C7B 88.8(13) . . ?
C10 C9 C8 113.6(7) . . ?
C11 C10 C9 134.4(7) . . ?
N3 C10 C9 118.7(7) . . ?
N3 C10 C11 106.8(6) . . ?
C10 C11 C12 108.4(6) . . ?
C10 C11 N8A 122.8(10) . . ?
C10 C11 N8B 130.0(10) . . ?
C12 C11 N8A 128.1(10) . . ?
C12 C11 N8B 120.8(10) . . ?
C11 C12 C13 133.6(6) . . ?
N4 C12 C11 106.6(6) . . ?
N4 C12 C13 119.7(6) . . ?
C14 C13 C12 113.3(7) . . ?
C17 C16 C15 113.0(6) . . ?
C18 C17 C16 132.5(5) . . ?
N5 C17 C16 120.2(5) . . ?
N5 C17 C18 107.2(5) . . ?
C17 C18 N9 125.1(6) . . ?
C19 C18 C17 108.3(5) . . ?
C19 C18 N9 126.6(6) . . ?
C18 C19 C20 133.3(5) . . ?
N6 C19 C18 106.7(5) . . ?
N6 C19 C20 119.9(5) . . ?
C19 C20 C21 113.1(6) . . ?
N6 Cu1 N1 176.5(2) . . ?
N2 Cu2 Cu3 96.41(19) . 3_665 ?
N3 Cu2 Cu3 89.07(15) . 3_665 ?
N3 Cu2 N2 174.5(2) . . ?
N4 Cu3 Cu2 88.93(15) . 3_665 ?
N5 Cu3 Cu2 97.46(14) . 3_665 ?
N5 Cu3 N4 173.4(2) . . ?
C3 N1 Cu1 129.6(5) . . ?
C3 N1 N2 110.8(5) . . ?
N2 N1 Cu1 118.3(3) . . ?
C5 N2 Cu2 130.6(5) . . ?
C5 N2 N1 108.5(5) . . ?
N1 N2 Cu2 120.6(3) . . ?
C10 N3 Cu2 130.9(5) . . ?
C10 N3 N4 109.4(5) . . ?
N4 N3 Cu2 119.3(3) . . ?
C12 N4 Cu3 131.7(4) . . ?
C12 N4 N3 108.7(5) . . ?
N3 N4 Cu3 118.9(3) . . ?
C17 N5 Cu3 131.0(4) . . ?
C17 N5 N6 109.1(4) . . ?
N6 N5 Cu3 119.8(3) . . ?
C19 N6 Cu1 130.4(4) . . ?
C19 N6 N5 108.5(4) . . ?
N5 N6 Cu1 119.2(3) . . ?
O1 N7 C4 118.2(8) . . ?
O2 N7 C4 116.8(8) . . ?
O2 N7 O1 125.0(8) . . ?
O3A N8A C11 113.0(15) . . ?
O4A N8A C11 114.6(15) . . ?
O4A N8A O3A 129.4(18) . . ?
O3B N8B C11 111.4(15) . . ?
O4B N8B C11 118.8(16) . . ?
O4B N8B O3B 123.4(17) . . ?
O5 N9 C18 117.9(6) . . ?
O6 N9 C18 118.3(7) . . ?
O6 N9 O5 123.8(6) . . ?
C24 C23 C22A 111.3(15) . . ?
C24 C23 C22B 109.9(14) . . ?
C25 C24 C23 133.9(6) . . ?
N10 C24 C23 118.9(6) . . ?
N10 C24 C25 107.1(5) . . ?
C24 C25 C26 108.3(5) . . ?
C24 C25 N16 125.3(7) . . ?
C26 C25 N16 126.4(7) . . ?
C25 C26 C27A 126.5(13) . . ?
C25 C26 C27B 136.9(14) . . ?
N11 C26 C25 106.3(5) . . ?
N11 C26 C27A 127.2(13) . . ?
N11 C26 C27B 115.2(12) . . ?
C26 C27A C28A 120(3) . . ?
C26 C27B C28B 96(2) . . ?
C31 C30A C29A 103.2(18) . . ?
C31 C30B C29B 113(2) . . ?
C32 C31 C30A 138.2(10) . . ?
C32 C31 C30B 123.4(9) . . ?
N12 C31 C30A 113.5(9) . . ?
N12 C31 C30B 129.1(9) . . ?
N12 C31 C32 107.4(5) . . ?
C31 C32 C33 108.0(5) . . ?
C31 C32 N17 127.0(6) . . ?
C33 C32 N17 125.0(6) . . ?
C32 C33 C34 132.3(5) . . ?
N13 C33 C32 106.5(5) . . ?
N13 C33 C34 121.1(5) . . ?
C33 C34 C35 112.3(5) . . ?
C38 C37 C36 113.8(5) . . ?
C39 C38 C37 131.0(5) . . ?
N14 C38 C37 120.7(5) . . ?
N14 C38 C39 108.2(5) . . ?
C38 C39 C40 106.2(4) . . ?
C38 C39 N18 128.1(5) . . ?
C40 C39 N18 125.6(5) . . ?
C39 C40 C41 131.8(5) . . ?
N15 C40 C39 108.1(5) . . ?
N15 C40 C41 120.1(5) . . ?
C40 C41 C42A 112.8(15) . . ?
C40 C41 C42B 112.7(15) . . ?
N10 Cu4 Cu6 90.93(15) . 3_564 ?
N15 Cu4 Cu6 97.07(14) . 3_564 ?
N15 Cu4 N10 171.8(2) . . ?
N11 Cu5 N12 175.6(2) . . ?
N13 Cu6 Cu4 88.19(14) . 3_564 ?
N13 Cu6 N14 174.61(19) . . ?
N14 Cu6 Cu4 97.10(13) . 3_564 ?
C24 N10 Cu4 130.7(4) . . ?
C24 N10 N11 108.8(5) . . ?
N11 N10 Cu4 119.6(3) . . ?
C26 N11 Cu5 131.1(4) . . ?
C26 N11 N10 109.4(4) . . ?
N10 N11 Cu5 118.9(3) . . ?
C31 N12 Cu5 131.2(4) . . ?
C31 N12 N13 108.5(4) . . ?
N13 N12 Cu5 119.4(3) . . ?
C33 N13 Cu6 129.3(4) . . ?
C33 N13 N12 109.7(4) . . ?
N12 N13 Cu6 120.1(3) . . ?
C38 N14 Cu6 132.1(4) . . ?
C38 N14 N15 109.1(4) . . ?
N15 N14 Cu6 117.4(3) . . ?
C40 N15 Cu4 131.0(4) . . ?
C40 N15 N14 108.3(4) . . ?
N14 N15 Cu4 120.5(3) . . ?
O7 N16 C25 118.7(7) . . ?
O8 N16 C25 118.2(7) . . ?
O8 N16 O7 123.1(7) . . ?
O9 N17 C32 117.6(6) . . ?
O10 N17 C32 120.5(6) . . ?
O10 N17 O9 121.9(6) . . ?
O11 N18 C39 117.7(6) . . ?
O12 N18 C39 119.1(6) . . ?
O12 N18 O11 123.2(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.504(11) . ?
C2 C3 1.499(10) . ?
C3 C4 1.391(10) . ?
C3 N1 1.332(7) . ?
C4 C5 1.404(10) . ?
C4 N7 1.462(9) . ?
C5 C6A 1.509(4) . ?
C5 C6B 1.508(4) . ?
C5 N2 1.372(8) . ?
C6A C7A 1.511(5) . ?
C6B C7B 1.511(5) . ?
C8 C9 1.503(12) . ?
C9 C10 1.495(10) . ?
C10 C11 1.381(10) . ?
C10 N3 1.324(7) . ?
C11 C12 1.392(10) . ?
C11 N8A 1.453(14) . ?
C11 N8B 1.467(14) . ?
C12 C13 1.501(10) . ?
C12 N4 1.329(7) . ?
C13 C14 1.492(11) . ?
C15 C16 1.519(10) . ?
C16 C17 1.478(8) . ?
C17 C18 1.388(8) . ?
C17 N5 1.333(6) . ?
C18 C19 1.387(8) . ?
C18 N9 1.442(7) . ?
C19 C20 1.474(8) . ?
C19 N6 1.351(7) . ?
C20 C21 1.544(10) . ?
Cu1 N1 1.858(4) . ?
Cu1 N6 1.855(4) . ?
Cu2 Cu3 3.0199(11) 3_665 ?
Cu2 N2 1.870(5) . ?
Cu2 N3 1.861(5) . ?
Cu3 N4 1.850(5) . ?
Cu3 N5 1.850(4) . ?
N1 N2 1.374(7) . ?
N3 N4 1.383(6) . ?
N5 N6 1.384(6) . ?
N7 O1 1.199(9) . ?
N7 O2 1.177(9) . ?
N8A O3A 1.303(16) . ?
N8A O4A 1.222(15) . ?
N8B O3B 1.312(16) . ?
N8B O4B 1.227(14) . ?
N9 O5 1.220(8) . ?
N9 O6 1.205(8) . ?
C22A C23 1.513(5) . ?
C22B C23 1.517(5) . ?
C23 C24 1.504(10) . ?
C24 C25 1.388(9) . ?
C24 N10 1.334(7) . ?
C25 C26 1.397(9) . ?
C25 N16 1.419(9) . ?
C26 C27A 1.503(5) . ?
C26 C27B 1.509(5) . ?
C26 N11 1.337(7) . ?
C27A C28A 1.512(5) . ?
C27B C28B 1.514(5) . ?
C29A C30A 1.515(5) . ?
C29B C30B 1.516(5) . ?
C30A C31 1.503(5) . ?
C30B C31 1.503(5) . ?
C31 C32 1.392(8) . ?
C31 N12 1.330(7) . ?
C32 C33 1.404(8) . ?
C32 N17 1.423(7) . ?
C33 C34 1.477(8) . ?
C33 N13 1.327(6) . ?
C34 C35 1.529(9) . ?
C36 C37 1.515(9) . ?
C37 C38 1.499(7) . ?
C38 C39 1.396(7) . ?
C38 N14 1.318(6) . ?
C39 C40 1.403(7) . ?
C39 N18 1.412(7) . ?
C40 C41 1.497(7) . ?
C40 N15 1.328(6) . ?
C41 C42A 1.522(5) . ?
C41 C42B 1.520(5) . ?
Cu4 Cu6 2.9349(10) 3_564 ?
Cu4 N10 1.854(4) . ?
Cu4 N15 1.854(4) . ?
Cu5 N11 1.861(4) . ?
Cu5 N12 1.867(4) . ?
Cu6 N13 1.862(4) . ?
Cu6 N14 1.869(4) . ?
N10 N11 1.383(6) . ?
N12 N13 1.393(6) . ?
N14 N15 1.391(5) . ?
N16 O7 1.217(8) . ?
N16 O8 1.216(9) . ?
N17 O9 1.222(8) . ?
N17 O10 1.201(7) . ?
N18 O11 1.219(7) . ?
N18 O12 1.211(7) . ?
