#------------------------------------------------------------------------------
#$Date: 2023-07-26 04:17:24 +0300 (Wed, 26 Jul 2023) $
#$Revision: 285347 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/71/7247103.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_7247103
loop_
_publ_author_name
'Xia, Liang-hong'
'Wang, Yan-na'
'Yang, Xiao-ming'
'Liang, Lin-na'
'Li, Zhi-min'
'Zhang, Tong-lai'
_publ_section_title
;
 Cupric coordination compounds with multiple anions: a promising strategy
 for the regulation of energetic materials
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              22549
_journal_page_last               22558
_journal_paper_doi               10.1039/D3RA01739G
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         '4(C15 H33 Cl Cu3 N30 O6), 16(Cl O4), 12(H2 O)'
_chemical_formula_sum            'C60 H156 Cl20 Cu12 N120 O100'
_chemical_formula_weight         5630.52
_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   mixed
_audit_creation_date             2023-01-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-03 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   22.1106(10)
_cell_length_b                   14.1198(7)
_cell_length_c                   14.6843(6)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.25
_cell_volume                     4568.8(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  ccd
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            102200
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.004
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_description       block
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.864
_exptl_transmission_factor_min   0.864
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         8041
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      6.192
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0429
_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)+(0.0343P)²+16.4670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6147
_reflns_number_total             8041
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ra01739g2.cif
_cod_data_source_block           1_a
_cod_database_code               7247103
_shelx_shelxl_version_number     2018/3
_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   0.715
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H13,H14} of O24A, {H11,H12} of O24, All N(H,H) groups,
  All O(H) groups
 At 1.5 times of:
  {H5,H6} of O25, {H7,H8} of O22, {H9,H10} of O23
2. Restrained distances
 O25-HX = O25-HY
 0.84 with sigma of 0.02
 N28-H3 = N28-H2
 0.9 with sigma of 0.02
 N20-HT = N20-HU = N10-HL = N10-HM
 0.9 with sigma of 0.02
 HX-HY
 0.02 with sigma of 1.39
 O6A-O7A \\sim O6A-O9A \\sim O6B-O7B \\sim O6B-O9B \\sim O7A-O9A \\sim O7B-O9B
 with sigma of 0.01
 O8-O6A \\sim O8-O6B \\sim O8-O7A \\sim O8-O7B \\sim O8-O9A \\sim O8-O9B
 with sigma of 0.01
3. Rigid bond restraints
 Cl2, O8, O7A, O7B, O9A, O9B, O6A, O6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O24A \\sim O24: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
Cl2 \\sim O8 \\sim O7A \\sim O7B \\sim O9A \\sim O9B \\sim O6A \\sim O6B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O24A) \\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
5. Others
 Sof(O6B)=Sof(O7B)=Sof(O9B)=1-FVAR(1)
 Sof(O6A)=Sof(O7A)=Sof(O9A)=FVAR(1)
 Sof(O24A)=Sof(H13)=Sof(H14)=1-FVAR(2)
 Sof(O24)=Sof(H11)=Sof(H12)=FVAR(2)
6.a Riding coordinates:
 O5(H4), O25(H5,H6), O22(H7,H8), O23(H9,H10), O24(H11,H12), O24A(H13,H14)
6.b Secondary CH2 refined with riding coordinates:
 C3(H,HA), C8(HB,HC), C13(HD,HE)
6.c X=CH2 refined with riding coordinates:
 N1(HF,HG), N2(HH,HI), N8(HJ,HK), N11(HN,HO), N12(HP,HQ), N19(HR,HS), N24(HV,
 HW), N25(HX,HY), N26(HZ,H1)
;
_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 0.7335(2) 0.0364(3) 0.2584(3) 0.0280(11) Uani 1 1 d . . . A 2
C2 C 0.6498(2) -0.0051(3) 0.3032(3) 0.0303(11) Uani 1 1 d . . . A 2
C3 C 0.63029(19) 0.1337(3) 0.4037(3) 0.0224(10) Uani 1 1 d . . . A 2
H H 0.651959 0.132565 0.463886 0.027 Uiso 1 1 calc R U . A 2
HA H 0.590594 0.105740 0.408427 0.027 Uiso 1 1 calc R U . A 2
C4 C 0.62313(18) 0.2330(3) 0.3720(3) 0.0194(9) Uani 1 1 d . . . A 2
C5 C 0.58628(19) 0.3751(3) 0.3475(3) 0.0227(10) Uani 1 1 d . . . A 2
C6 C 0.86692(19) 0.1645(3) 0.3904(3) 0.0205(9) Uani 1 1 d . . . A 2
C7 C 0.92517(18) 0.2820(3) 0.3545(3) 0.0206(9) Uani 1 1 d . . . A 2
C8 C 0.9787(2) 0.3452(3) 0.3515(3) 0.0262(10) Uani 1 1 d . . . A 2
HB H 0.980592 0.387661 0.403610 0.031 Uiso 1 1 calc R U . A 2
HC H 1.015411 0.307223 0.355940 0.031 Uiso 1 1 calc R U . A 2
C9 C 1.02060(18) 0.4190(3) 0.2140(3) 0.0227(10) Uani 1 1 d . . . A 2
C10 C 0.94047(19) 0.4818(3) 0.1539(3) 0.0219(10) Uani 1 1 d . . . A 2
C11 C 0.83185(18) 0.6385(3) 0.2584(3) 0.0204(9) Uani 1 1 d . . . A 2
C12 C 0.73441(18) 0.6494(3) 0.2248(3) 0.0181(9) Uani 1 1 d . . . A 2
C13 C 0.67249(19) 0.6879(3) 0.2061(3) 0.0246(10) Uani 1 1 d . . . A 2
HD H 0.653369 0.694535 0.262837 0.029 Uiso 1 1 calc R U . A 2
HE H 0.674413 0.749966 0.178152 0.029 Uiso 1 1 calc R U . A 2
C14 C 0.60457(19) 0.6427(3) 0.0668(3) 0.0265(10) Uani 1 1 d . . . A 2
C15 C 0.58188(19) 0.5051(3) 0.1071(3) 0.0244(10) Uani 1 1 d . . . A 2
Cl1 Cl 0.75403(5) 0.31110(8) 0.09766(7) 0.0262(3) Uani 1 1 d . . . A 2
Cu1 Cu 0.74448(2) 0.24338(3) 0.31469(3) 0.01971(13) Uani 1 1 d . . . A 2
Cu2 Cu 0.84205(2) 0.42421(4) 0.27856(4) 0.02030(14) Uani 1 1 d . . . A 2
Cu3 Cu 0.68875(2) 0.45878(4) 0.24649(4) 0.02048(14) Uani 1 1 d . . . A 2
N1 N 0.78523(19) 0.0328(3) 0.2151(3) 0.0371(10) Uani 1 1 d . . . A 2
HF H 0.811532 0.077560 0.222692 0.044 Uiso 1 1 calc R U . A 2
HG H 0.791771 -0.014295 0.180123 0.044 Uiso 1 1 calc R U . A 2
N2 N 0.5995(2) -0.0542(3) 0.3177(3) 0.0496(12) Uani 1 1 d . . . A 2
HH H 0.592985 -0.108365 0.292044 0.060 Uiso 1 1 calc R U . A 2
HI H 0.573740 -0.031390 0.352724 0.060 Uiso 1 1 calc R U . A 2
N3 N 0.69233(19) -0.0337(3) 0.2506(3) 0.0340(10) Uani 1 1 d . . . A 2
N4 N 0.72010(16) 0.1075(2) 0.3141(2) 0.0234(8) Uani 1 1 d . . . A 2
N5 N 0.66325(16) 0.0788(2) 0.3410(2) 0.0251(9) Uani 1 1 d . . . A 2
N6 N 0.65937(15) 0.2770(2) 0.3211(2) 0.0207(8) Uani 1 1 d . . . A 2
N7 N 0.63629(15) 0.3679(2) 0.3034(2) 0.0223(8) Uani 1 1 d . . . A 2
N8 N 0.54963(17) 0.4488(3) 0.3491(3) 0.0385(11) Uani 1 1 d . . . A 2
HJ H 0.557156 0.499354 0.319355 0.046 Uiso 1 1 calc R U . A 2
HK H 0.518252 0.446368 0.379997 0.046 Uiso 1 1 calc R U . A 2
N9 N 0.57723(15) 0.2911(2) 0.3904(2) 0.0212(8) Uani 1 1 d . . . A 2
N10 N 0.53269(19) 0.2681(3) 0.4490(3) 0.0331(10) Uani 1 1 d D . . A 2
HL H 0.4970(13) 0.277(4) 0.418(3) 0.040 Uiso 1 1 d D U . B 2
HM H 0.539(2) 0.303(3) 0.500(2) 0.040 Uiso 1 1 d D U . C 2
N11 N 0.90194(16) 0.5274(3) 0.0912(2) 0.0263(9) Uani 1 1 d . . . A 2
HN H 0.864224 0.533341 0.100451 0.032 Uiso 1 1 calc R U . A 2
HO H 0.915360 0.550163 0.042452 0.032 Uiso 1 1 calc R U . A 2
N12 N 1.07801(16) 0.3873(3) 0.2312(3) 0.0343(10) Uani 1 1 d . . . A 2
HP H 1.104630 0.398566 0.193088 0.041 Uiso 1 1 calc R U . A 2
HQ H 1.087967 0.355868 0.280346 0.041 Uiso 1 1 calc R U . A 2
N13 N 0.99960(15) 0.4681(3) 0.1410(2) 0.0245(8) Uani 1 1 d . . . A 2
N14 N 0.92298(15) 0.4447(2) 0.2310(2) 0.0214(8) Uani 1 1 d . . . A 2
N15 N 0.97601(15) 0.4003(2) 0.2683(2) 0.0215(8) Uani 1 1 d . . . A 2
N16 N 0.92495(15) 0.1982(2) 0.3997(2) 0.0198(8) Uani 1 1 d . . . A 2
N17 N 0.87050(15) 0.3003(2) 0.3201(2) 0.0214(8) Uani 1 1 d . . . A 2
N18 N 0.83252(15) 0.2256(2) 0.3413(2) 0.0218(8) Uani 1 1 d . . . A 2
N19 N 0.85091(17) 0.0810(3) 0.4217(3) 0.0286(9) Uani 1 1 d . . . A 2
HR H 0.814300 0.061037 0.410614 0.034 Uiso 1 1 calc R U . A 2
HS H 0.877139 0.046712 0.453166 0.034 Uiso 1 1 calc R U . A 2
N20 N 0.97579(17) 0.1549(3) 0.4450(3) 0.0288(9) Uani 1 1 d D . . A 2
HT H 0.974(2) 0.165(3) 0.5045(15) 0.035 Uiso 1 1 d D U . D 2
HU H 0.971(2) 0.0955(18) 0.426(3) 0.035 Uiso 1 1 d D U . E 2
N21 N 0.56916(17) 0.5696(3) 0.0404(2) 0.0265(9) Uani 1 1 d . . . A 2
N22 N 0.62293(15) 0.5328(2) 0.1746(2) 0.0228(8) Uani 1 1 d . . . A 2
N23 N 0.63721(15) 0.6247(3) 0.1454(2) 0.0236(8) Uani 1 1 d . . . A 2
N24 N 0.60580(18) 0.7267(3) 0.0231(3) 0.0389(11) Uani 1 1 d . . . A 2
HV H 0.582471 0.736179 -0.025840 0.047 Uiso 1 1 calc R U . A 2
HW H 0.629904 0.770738 0.044225 0.047 Uiso 1 1 calc R U . A 2
N25 N 0.55606(19) 0.4208(3) 0.1068(3) 0.0384(10) Uani 1 1 d . . . A 2
HX H 0.565367 0.381615 0.150584 0.046 Uiso 1 1 calc DR U . A 2
HY H 0.529946 0.404969 0.062762 0.046 Uiso 1 1 calc DR U . A 2
N26 N 0.88875(16) 0.6651(3) 0.2779(3) 0.0356(10) Uani 1 1 d . . . A 2
HZ H 0.916764 0.623183 0.287528 0.043 Uiso 1 1 calc R U . A 2
H1 H 0.897753 0.724326 0.280970 0.043 Uiso 1 1 calc R U . A 2
N27 N 0.78550(15) 0.7013(2) 0.2410(2) 0.0186(8) Uani 1 1 d . . . A 2
N28 N 0.79393(17) 0.7986(3) 0.2297(3) 0.0268(9) Uani 1 1 d D . . A 2
H2 H 0.7715(18) 0.826(3) 0.269(3) 0.032 Uiso 1 1 d D U . F 2
H3 H 0.780(2) 0.814(3) 0.1731(17) 0.032 Uiso 1 1 d D U . G 2
N29 N 0.74738(14) 0.5603(2) 0.2306(2) 0.0186(8) Uani 1 1 d . . . A 2
N30 N 0.80978(14) 0.5512(2) 0.2509(2) 0.0194(8) Uani 1 1 d . . . A 2
O1 O 0.75497(17) 0.2300(2) 0.1565(2) 0.0429(9) Uani 1 1 d . . . A 2
O2 O 0.70069(15) 0.3662(3) 0.1125(2) 0.0423(9) Uani 1 1 d . . . A 2
O3 O 0.80680(16) 0.3669(3) 0.1200(2) 0.0468(10) Uani 1 1 d . . . A 2
O4 O 0.75139(15) 0.2803(2) 0.0046(2) 0.0377(8) Uani 1 1 d . . . A 2
O5 O 0.75900(12) 0.38459(19) 0.31065(19) 0.0195(6) Uani 1 1 d . . . A 2
H4 H 0.754680 0.404449 0.364522 0.023 Uiso 1 1 d R U . A 2
O25 O 0.87427(19) 0.4854(3) 0.4270(3) 0.0623(12) Uani 1 1 d D . . A 2
H5 H 0.845352 0.517574 0.446496 0.093 Uiso 1 1 d R U . A 2
H6 H 0.879372 0.439614 0.464776 0.093 Uiso 1 1 d R U . A 2
Cl2 Cl 0.94870(6) 0.35269(10) 0.62948(8) 0.0409(3) Uani 1 1 d . U . . .
Cl3 Cl 0.72104(6) 0.56420(9) 0.47174(8) 0.0386(3) Uani 1 1 d . . . . .
Cl4 Cl 0.50752(5) 0.69552(8) 0.28910(8) 0.0353(3) Uani 1 1 d . . . . .
O6A O 0.9037(3) 0.3367(6) 0.5561(5) 0.097(3) Uani 0.634(8) 1 d D U P H 1
O7A O 0.9780(4) 0.2668(5) 0.6485(7) 0.106(3) Uani 0.634(8) 1 d D U P H 1
O9A O 0.9212(4) 0.3837(6) 0.7025(5) 0.099(3) Uani 0.634(8) 1 d D U P H 1
O6B O 0.9701(6) 0.3525(9) 0.7276(5) 0.081(4) Uani 0.366(8) 1 d D U P H 2
O7B O 0.8920(4) 0.3912(11) 0.6243(11) 0.111(4) Uani 0.366(8) 1 d D U P H 2
O9B O 0.9515(7) 0.2660(6) 0.5996(9) 0.118(5) Uani 0.366(8) 1 d D U P H 2
O8 O 0.9889(3) 0.4162(5) 0.5960(4) 0.145(3) Uani 1 1 d D U . . .
O10 O 0.7345(2) 0.4648(3) 0.4857(3) 0.0649(12) Uani 1 1 d . . . . .
O11 O 0.77277(17) 0.6093(3) 0.4368(3) 0.0553(10) Uani 1 1 d . . . . .
O12 O 0.7078(2) 0.6069(3) 0.5552(3) 0.0654(12) Uani 1 1 d . . . . .
O13 O 0.67093(18) 0.5724(3) 0.4054(3) 0.0660(12) Uani 1 1 d . . . . .
O14 O 0.49692(18) 0.6182(3) 0.2287(3) 0.0512(10) Uani 1 1 d . . . . .
O15 O 0.45095(19) 0.7301(3) 0.3145(3) 0.0619(12) Uani 1 1 d . . . . .
O16 O 0.5452(3) 0.6663(3) 0.3662(3) 0.0911(18) Uani 1 1 d . . . . .
O17 O 0.53693(19) 0.7692(3) 0.2406(3) 0.0672(13) Uani 1 1 d . . . . .
Cl5 Cl 0.76865(7) 0.85844(10) 0.46952(9) 0.0447(3) Uani 1 1 d . . . I 1
O18 O 0.7524(3) 0.9536(3) 0.4872(4) 0.0931(17) Uani 1 1 d . . . I 1
O19 O 0.8255(2) 0.8577(4) 0.4295(4) 0.0999(19) Uani 1 1 d . . . I 1
O20 O 0.7740(3) 0.8081(4) 0.5517(3) 0.0971(19) Uani 1 1 d . . . I 1
O21 O 0.7249(2) 0.8141(3) 0.4074(3) 0.0730(13) Uani 1 1 d . . . I 1
O22 O 0.3702(2) 0.6235(4) 0.4267(3) 0.0837(15) Uani 1 1 d . . . . .
H7 H 0.338188 0.612659 0.453207 0.126 Uiso 1 1 d R U . . .
H8 H 0.359018 0.661559 0.383747 0.126 Uiso 1 1 d R U . . .
O23 O 0.4363(2) 0.4487(4) 0.4272(4) 0.0988(19) Uani 1 1 d . . . . .
H9 H 0.428720 0.507290 0.433452 0.148 Uiso 1 1 d R U . . .
H10 H 0.402460 0.424560 0.407852 0.148 Uiso 1 1 d R U . . .
O24 O 0.8864(3) 0.6705(10) 0.5617(6) 0.092(3) Uani 0.81(2) 1 d . U P J 1
H11 H 0.894007 0.630004 0.522362 0.110 Uiso 0.81(2) 1 d R U P J 1
H12 H 0.875747 0.725094 0.544043 0.110 Uiso 0.81(2) 1 d R U P J 1
O24A O 0.8791(15) 0.614(4) 0.587(2) 0.087(5) Uani 0.19(2) 1 d . U P J 2
H13 H 0.868458 0.668984 0.569621 0.104 Uiso 0.19(2) 1 d R U P J 2
H14 H 0.886718 0.573894 0.547921 0.104 Uiso 0.19(2) 1 d R U P J 2
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_
_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
N3 C1 N1 121.6(4) . . ?
N4 C1 N1 123.4(4) . . ?
N4 C1 N3 114.9(4) . . ?
N3 C2 N2 124.8(4) . . ?
N3 C2 N5 111.7(4) . . ?
N5 C2 N2 123.5(4) . . ?
H C3 HA 108.1 . . ?
C4 C3 H 109.5 . . ?
C4 C3 HA 109.5 . . ?
N5 C3 H 109.5 . . ?
N5 C3 HA 109.5 . . ?
N5 C3 C4 110.7(3) . . ?
N6 C4 C3 125.4(4) . . ?
N6 C4 N9 109.5(4) . . ?
N9 C4 C3 125.1(4) . . ?
N7 C5 N9 108.5(4) . . ?
N8 C5 N7 127.2(4) . . ?
N8 C5 N9 124.3(4) . . ?
N18 C6 N16 108.7(4) . . ?
N18 C6 N19 127.7(4) . . ?
N19 C6 N16 123.5(4) . . ?
N16 C7 C8 124.9(4) . . ?
N17 C7 C8 126.0(4) . . ?
N17 C7 N16 108.9(4) . . ?
C7 C8 HB 109.3 . . ?
C7 C8 HC 109.3 . . ?
HB C8 HC 107.9 . . ?
N15 C8 C7 111.7(3) . . ?
N15 C8 HB 109.3 . . ?
N15 C8 HC 109.3 . . ?
N13 C9 N12 125.8(4) . . ?
N13 C9 N15 110.9(4) . . ?
N15 C9 N12 123.2(4) . . ?
N13 C10 N11 122.0(4) . . ?
N14 C10 N11 123.4(4) . . ?
N14 C10 N13 114.6(4) . . ?
N26 C11 N27 122.9(4) . . ?
N26 C11 N30 128.2(4) . . ?
N30 C11 N27 108.8(3) . . ?
N27 C12 C13 125.6(4) . . ?
N29 C12 C13 124.6(4) . . ?
N29 C12 N27 109.8(4) . . ?
C12 C13 HD 109.8 . . ?
C12 C13 HE 109.8 . . ?
HD C13 HE 108.2 . . ?
N23 C13 C12 109.4(4) . . ?
N23 C13 HD 109.8 . . ?
N23 C13 HE 109.8 . . ?
N21 C14 N23 111.6(4) . . ?
N21 C14 N24 125.1(4) . . ?
N23 C14 N24 123.2(4) . . ?
N22 C15 N21 115.2(4) . . ?
N25 C15 N21 122.8(4) . . ?
N25 C15 N22 122.0(4) . . ?
O1 Cl1 O2 108.1(2) . . ?
O3 Cl1 O1 109.4(2) . . ?
O3 Cl1 O2 109.3(2) . . ?
O3 Cl1 O4 110.9(2) . . ?
O4 Cl1 O1 109.3(2) . . ?
O4 Cl1 O2 109.8(2) . . ?
N4 Cu1 O1 88.13(13) . . ?
N4 Cu1 O5 173.33(13) . . ?
N6 Cu1 N4 88.45(14) . . ?
N6 Cu1 N18 164.36(15) . . ?
N6 Cu1 O1 103.92(14) . . ?
N6 Cu1 O5 85.26(12) . . ?
N18 Cu1 N4 98.09(14) . . ?
N18 Cu1 O1 90.54(14) . . ?
N18 Cu1 O5 88.55(13) . . ?
O5 Cu1 O1 91.21(11) . . ?
N14 Cu2 O5 169.90(13) . . ?
N14 Cu2 O25 93.33(15) . . ?
N17 Cu2 N14 87.94(14) . . ?
N17 Cu2 N30 173.24(14) . . ?
N17 Cu2 O5 87.37(12) . . ?
N17 Cu2 O25 88.54(14) . . ?
N30 Cu2 N14 96.67(14) . . ?
N30 Cu2 O5 88.81(12) . . ?
N30 Cu2 O25 86.26(14) . . ?
O5 Cu2 O25 95.49(13) . . ?
N7 Cu3 N22 97.78(14) . . ?
N7 Cu3 O2 95.85(14) . . ?
N7 Cu3 O5 85.51(13) . . ?
N22 Cu3 O2 88.63(13) . . ?
N22 Cu3 O5 175.62(13) . . ?
N29 Cu3 N7 161.67(15) . . ?
N29 Cu3 N22 90.84(14) . . ?
N29 Cu3 O2 100.52(14) . . ?
N29 Cu3 O5 86.82(12) . . ?
O5 Cu3 O2 88.17(11) . . ?
C1 N1 HF 120.0 . . ?
C1 N1 HG 120.0 . . ?
HF N1 HG 120.0 . . ?
C2 N2 HH 120.0 . . ?
C2 N2 HI 120.0 . . ?
HH N2 HI 120.0 . . ?
C2 N3 C1 103.4(4) . . ?
C1 N4 Cu1 130.5(3) . . ?
C1 N4 N5 101.7(3) . . ?
N5 N4 Cu1 121.5(3) . . ?
C2 N5 C3 129.5(4) . . ?
C2 N5 N4 108.2(4) . . ?
N4 N5 C3 122.2(3) . . ?
C4 N6 Cu1 123.7(3) . . ?
C4 N6 N7 108.3(3) . . ?
N7 N6 Cu1 123.6(2) . . ?
C5 N7 Cu3 134.5(3) . . ?
C5 N7 N6 106.5(3) . . ?
N6 N7 Cu3 117.4(2) . . ?
C5 N8 HJ 120.0 . . ?
C5 N8 HK 120.0 . . ?
HJ N8 HK 120.0 . . ?
C4 N9 C5 107.1(3) . . ?
C4 N9 N10 124.2(4) . . ?
C5 N9 N10 128.5(4) . . ?
N9 N10 HL 107(3) . . ?
N9 N10 HM 109(3) . . ?
HL N10 HM 114(5) . . ?
C10 N11 HN 120.0 . . ?
C10 N11 HO 120.0 . . ?
HN N11 HO 120.0 . . ?
C9 N12 HP 120.0 . . ?
C9 N12 HQ 120.0 . . ?
HP N12 HQ 120.0 . . ?
C9 N13 C10 103.8(3) . . ?
C10 N14 Cu2 133.3(3) . . ?
C10 N14 N15 102.5(3) . . ?
N15 N14 Cu2 122.9(3) . . ?
C9 N15 C8 128.8(4) . . ?
C9 N15 N14 108.1(3) . . ?
N14 N15 C8 123.2(3) . . ?
C6 N16 N20 127.4(4) . . ?
C7 N16 C6 107.2(3) . . ?
C7 N16 N20 125.4(4) . . ?
C7 N17 Cu2 124.7(3) . . ?
C7 N17 N18 108.7(3) . . ?
N18 N17 Cu2 124.4(3) . . ?
C6 N18 Cu1 134.8(3) . . ?
C6 N18 N17 106.5(3) . . ?
N17 N18 Cu1 117.5(2) . . ?
C6 N19 HR 120.0 . . ?
C6 N19 HS 120.0 . . ?
HR N19 HS 120.0 . . ?
N16 N20 HT 107(3) . . ?
N16 N20 HU 101(3) . . ?
HT N20 HU 116(5) . . ?
C14 N21 C15 103.2(4) . . ?
C15 N22 Cu3 130.5(3) . . ?
C15 N22 N23 101.4(3) . . ?
N23 N22 Cu3 117.7(2) . . ?
C14 N23 C13 130.0(4) . . ?
C14 N23 N22 108.6(3) . . ?
N22 N23 C13 120.3(3) . . ?
C14 N24 HV 120.0 . . ?
C14 N24 HW 120.0 . . ?
HV N24 HW 120.0 . . ?
C15 N25 HX 120.0 . . ?
C15 N25 HY 120.0 . . ?
HX N25 HY 120.0 . . ?
C11 N26 HZ 120.0 . . ?
C11 N26 H1 120.0 . . ?
HZ N26 H1 120.0 . . ?
C11 N27 N28 123.8(3) . . ?
C12 N27 C11 106.6(3) . . ?
C12 N27 N28 129.0(3) . . ?
N27 N28 H2 105(3) . . ?
N27 N28 H3 108(3) . . ?
H2 N28 H3 110(4) . . ?
C12 N29 Cu3 125.1(3) . . ?
C12 N29 N30 108.3(3) . . ?
N30 N29 Cu3 124.1(2) . . ?
C11 N30 Cu2 135.0(3) . . ?
C11 N30 N29 106.4(3) . . ?
N29 N30 Cu2 117.8(2) . . ?
Cl1 O1 Cu1 122.1(2) . . ?
Cl1 O2 Cu3 124.37(19) . . ?
Cu1 O5 Cu3 113.80(13) . . ?
Cu1 O5 H4 105.5 . . ?
Cu2 O5 Cu1 115.55(13) . . ?
Cu2 O5 Cu3 115.09(13) . . ?
Cu2 O5 H4 107.5 . . ?
Cu3 O5 H4 96.9 . . ?
Cu2 O25 H5 108.8 . . ?
Cu2 O25 H6 109.4 . . ?
H5 O25 H6 104.4 . . ?
O7A Cl2 O6A 107.3(4) . . ?
O9A Cl2 O6A 108.7(5) . . ?
O9A Cl2 O7A 110.8(4) . . ?
O9A Cl2 O8 114.7(4) . . ?
O7B Cl2 O6B 105.9(6) . . ?
O7B Cl2 O8 109.7(6) . . ?
O9B Cl2 O6B 107.8(6) . . ?
O9B Cl2 O7B 115.1(6) . . ?
O9B Cl2 O8 116.1(6) . . ?
O8 Cl2 O6A 105.3(4) . . ?
O8 Cl2 O7A 109.6(4) . . ?
O8 Cl2 O6B 100.6(5) . . ?
O11 Cl3 O10 108.6(3) . . ?
O12 Cl3 O10 110.2(3) . . ?
O12 Cl3 O11 110.3(3) . . ?
O12 Cl3 O13 110.7(3) . . ?
O13 Cl3 O10 108.5(3) . . ?
O13 Cl3 O11 108.5(3) . . ?
O14 Cl4 O15 109.0(3) . . ?
O14 Cl4 O17 107.7(3) . . ?
O15 Cl4 O17 108.9(3) . . ?
O16 Cl4 O14 109.6(3) . . ?
O16 Cl4 O15 111.3(3) . . ?
O16 Cl4 O17 110.3(3) . . ?
O18 Cl5 O19 109.0(3) . . ?
O20 Cl5 O18 109.2(3) . . ?
O20 Cl5 O19 109.6(4) . . ?
O20 Cl5 O21 109.6(3) . . ?
O21 Cl5 O18 111.4(3) . . ?
O21 Cl5 O19 107.9(3) . . ?
H7 O22 H8 104.5 . . ?
H9 O23 H10 104.5 . . ?
H11 O24 H12 118.7 . . ?
H13 O24A H14 118.7 . . ?
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
C1 N1 1.354(6) . ?
C1 N3 1.344(6) . ?
C1 N4 1.343(6) . ?
C2 N2 1.343(6) . ?
C2 N3 1.328(6) . ?
C2 N5 1.332(6) . ?
C3 H 0.9700 . ?
C3 HA 0.9700 . ?
C3 C4 1.482(6) . ?
C3 N5 1.445(5) . ?
C4 N6 1.298(5) . ?
C4 N9 1.349(5) . ?
C5 N7 1.331(5) . ?
C5 N8 1.321(6) . ?
C5 N9 1.365(5) . ?
C6 N16 1.365(5) . ?
C6 N18 1.324(5) . ?
C6 N19 1.324(5) . ?
C7 C8 1.486(6) . ?
C7 N16 1.357(5) . ?
C7 N17 1.297(5) . ?
C8 HB 0.9700 . ?
C8 HC 0.9700 . ?
C8 N15 1.445(5) . ?
C9 N12 1.350(5) . ?
C9 N13 1.328(6) . ?
C9 N15 1.345(5) . ?
C10 N11 1.363(5) . ?
C10 N13 1.351(5) . ?
C10 N14 1.333(5) . ?
C11 N26 1.322(5) . ?
C11 N27 1.364(5) . ?
C11 N30 1.327(5) . ?
C12 C13 1.478(6) . ?
C12 N27 1.351(5) . ?
C12 N29 1.292(5) . ?
C13 HD 0.9700 . ?
C13 HE 0.9700 . ?
C13 N23 1.443(6) . ?
C14 N21 1.333(6) . ?
C14 N23 1.334(6) . ?
C14 N24 1.351(6) . ?
C15 N21 1.350(6) . ?
C15 N22 1.345(6) . ?
C15 N25 1.321(6) . ?
Cl1 O1 1.434(3) . ?
Cl1 O2 1.445(3) . ?
Cl1 O3 1.424(3) . ?
Cl1 O4 1.430(3) . ?
Cu1 N4 1.993(4) . ?
Cu1 N6 1.951(3) . ?
Cu1 N18 1.970(3) . ?
Cu1 O1 2.360(3) . ?
Cu1 O5 2.021(3) . ?
Cu2 N14 1.995(3) . ?
Cu2 N17 1.940(3) . ?
Cu2 N30 1.960(3) . ?
Cu2 O5 2.012(3) . ?
Cu2 O25 2.398(4) . ?
Cu3 N7 1.962(3) . ?
Cu3 N22 2.018(3) . ?
Cu3 N29 1.959(3) . ?
Cu3 O2 2.395(3) . ?
Cu3 O5 2.039(3) . ?
N1 HF 0.8600 . ?
N1 HG 0.8600 . ?
N2 HH 0.8600 . ?
N2 HI 0.8600 . ?
N4 N5 1.408(5) . ?
N6 N7 1.397(5) . ?
N8 HJ 0.8600 . ?
N8 HK 0.8600 . ?
N9 N10 1.398(5) . ?
N10 HL 0.885(19) . ?
N10 HM 0.89(2) . ?
N11 HN 0.8600 . ?
N11 HO 0.8600 . ?
N12 HP 0.8600 . ?
N12 HQ 0.8600 . ?
N14 N15 1.402(5) . ?
N16 N20 1.399(5) . ?
N17 N18 1.400(5) . ?
N19 HR 0.8600 . ?
N19 HS 0.8600 . ?
N20 HT 0.890(19) . ?
N20 HU 0.886(19) . ?
N22 N23 1.410(5) . ?
N24 HV 0.8600 . ?
N24 HW 0.8600 . ?
N25 HX 0.8600 . ?
N25 HY 0.8600 . ?
N26 HZ 0.8600 . ?
N26 H1 0.8600 . ?
N27 N28 1.398(5) . ?
N28 H2 0.883(19) . ?
N28 H3 0.885(19) . ?
N29 N30 1.393(4) . ?
O5 H4 0.8520 . ?
O25 H5 0.8531 . ?
O25 H6 0.8528 . ?
Cl2 O6A 1.422(6) . ?
Cl2 O7A 1.392(6) . ?
Cl2 O9A 1.349(6) . ?
Cl2 O6B 1.480(8) . ?
Cl2 O7B 1.363(9) . ?
Cl2 O9B 1.303(9) . ?
Cl2 O8 1.382(6) . ?
Cl3 O10 1.446(4) . ?
Cl3 O11 1.440(4) . ?
Cl3 O12 1.418(4) . ?
Cl3 O13 1.418(4) . ?
Cl4 O14 1.414(4) . ?
Cl4 O15 1.421(4) . ?
Cl4 O16 1.411(4) . ?
Cl4 O17 1.445(4) . ?
Cl5 O18 1.420(5) . ?
Cl5 O19 1.431(5) . ?
Cl5 O20 1.397(4) . ?
Cl5 O21 1.419(4) . ?
O22 H7 0.8499 . ?
O22 H8 0.8500 . ?
O23 H9 0.8501 . ?
O23 H10 0.8501 . ?
O24 H11 0.8402 . ?
O24 H12 0.8399 . ?
O24A H13 0.8400 . ?
O24A H14 0.8402 . ?
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
C1 N4 N5 C2 2.3(4) . . . . ?
C1 N4 N5 C3 179.1(4) . . . . ?
C3 C4 N6 Cu1 -25.0(6) . . . . ?
C3 C4 N6 N7 177.9(4) . . . . ?
C3 C4 N9 C5 -178.6(4) . . . . ?
C3 C4 N9 N10 5.9(7) . . . . ?
C4 C3 N5 C2 -130.8(5) . . . . ?
C4 C3 N5 N4 53.2(5) . . . . ?
C4 N6 N7 C5 1.3(5) . . . . ?
C4 N6 N7 Cu3 169.3(3) . . . . ?
C7 C8 N15 C9 -136.9(4) . . . . ?
C7 C8 N15 N14 43.4(5) . . . . ?
C7 N17 N18 C6 1.0(4) . . . . ?
C7 N17 N18 Cu1 170.5(3) . . . . ?
C8 C7 N16 C6 176.6(4) . . . . ?
C8 C7 N16 N20 -4.9(6) . . . . ?
C8 C7 N17 Cu2 -13.2(6) . . . . ?
C8 C7 N17 N18 -176.9(4) . . . . ?
C10 N14 N15 C8 -176.8(4) . . . . ?
C10 N14 N15 C9 3.5(4) . . . . ?
C12 C13 N23 C14 -127.9(4) . . . . ?
C12 C13 N23 N22 65.7(5) . . . . ?
C12 N29 N30 C11 1.3(4) . . . . ?
C12 N29 N30 Cu2 172.8(3) . . . . ?
C13 C12 N27 C11 177.6(4) . . . . ?
C13 C12 N27 N28 -11.4(7) . . . . ?
C13 C12 N29 Cu3 -16.0(6) . . . . ?
C13 C12 N29 N30 -178.7(4) . . . . ?
C15 N22 N23 C13 169.3(4) . . . . ?
C15 N22 N23 C14 0.2(4) . . . . ?
Cu1 N4 N5 C2 157.1(3) . . . . ?
Cu1 N4 N5 C3 -26.1(5) . . . . ?
Cu1 N6 N7 C5 -155.8(3) . . . . ?
Cu1 N6 N7 Cu3 12.2(4) . . . . ?
Cu2 N14 N15 C8 -8.2(5) . . . . ?
Cu2 N14 N15 C9 172.1(3) . . . . ?
Cu2 N17 N18 C6 -162.6(3) . . . . ?
Cu2 N17 N18 Cu1 6.8(4) . . . . ?
Cu3 N22 N23 C13 -42.0(4) . . . . ?
Cu3 N22 N23 C14 148.9(3) . . . . ?
Cu3 N29 N30 C11 -161.5(3) . . . . ?
Cu3 N29 N30 Cu2 10.0(4) . . . . ?
N1 C1 N3 C2 178.9(4) . . . . ?
N1 C1 N4 Cu1 28.5(7) . . . . ?
N1 C1 N4 N5 -180.0(4) . . . . ?
N2 C2 N3 C1 -178.8(5) . . . . ?
N2 C2 N5 C3 1.1(8) . . . . ?
N2 C2 N5 N4 177.6(4) . . . . ?
N3 C1 N4 Cu1 -153.6(3) . . . . ?
N3 C1 N4 N5 -2.0(5) . . . . ?
N3 C2 N5 C3 -178.5(4) . . . . ?
N3 C2 N5 N4 -2.0(5) . . . . ?
N4 C1 N3 C2 0.9(5) . . . . ?
N5 C2 N3 C1 0.7(5) . . . . ?
N5 C3 C4 N6 -26.6(6) . . . . ?
N5 C3 C4 N9 152.2(4) . . . . ?
N6 C4 N9 C5 0.3(5) . . . . ?
N6 C4 N9 N10 -175.1(4) . . . . ?
N7 C5 N9 C4 0.5(5) . . . . ?
N7 C5 N9 N10 175.7(4) . . . . ?
N8 C5 N7 Cu3 15.6(7) . . . . ?
N8 C5 N7 N6 -179.5(4) . . . . ?
N8 C5 N9 C4 178.9(4) . . . . ?
N8 C5 N9 N10 -5.9(7) . . . . ?
N9 C4 N6 Cu1 156.1(3) . . . . ?
N9 C4 N6 N7 -1.0(5) . . . . ?
N9 C5 N7 Cu3 -166.1(3) . . . . ?
N9 C5 N7 N6 -1.1(5) . . . . ?
N11 C10 N13 C9 -177.7(4) . . . . ?
N11 C10 N14 Cu2 8.8(7) . . . . ?
N11 C10 N14 N15 175.6(4) . . . . ?
N12 C9 N13 C10 179.1(4) . . . . ?
N12 C9 N15 C8 -0.5(7) . . . . ?
N12 C9 N15 N14 179.2(4) . . . . ?
N13 C9 N15 C8 176.7(4) . . . . ?
N13 C9 N15 N14 -3.6(5) . . . . ?
N13 C10 N14 Cu2 -169.2(3) . . . . ?
N13 C10 N14 N15 -2.4(5) . . . . ?
N14 C10 N13 C9 0.4(5) . . . . ?
N15 C9 N13 C10 2.0(5) . . . . ?
N16 C6 N18 Cu1 -167.2(3) . . . . ?
N16 C6 N18 N17 -0.5(4) . . . . ?
N16 C7 C8 N15 151.5(4) . . . . ?
N16 C7 N17 Cu2 162.4(3) . . . . ?
N16 C7 N17 N18 -1.2(4) . . . . ?
N17 C7 C8 N15 -33.5(6) . . . . ?
N17 C7 N16 C6 0.9(5) . . . . ?
N17 C7 N16 N20 179.4(4) . . . . ?
N18 C6 N16 C7 -0.2(4) . . . . ?
N18 C6 N16 N20 -178.7(4) . . . . ?
N19 C6 N16 C7 175.9(4) . . . . ?
N19 C6 N16 N20 -2.5(7) . . . . ?
N19 C6 N18 Cu1 16.8(7) . . . . ?
N19 C6 N18 N17 -176.4(4) . . . . ?
N21 C14 N23 C13 -167.7(4) . . . . ?
N21 C14 N23 N22 0.0(5) . . . . ?
N21 C15 N22 Cu3 -143.1(3) . . . . ?
N21 C15 N22 N23 -0.3(5) . . . . ?
N22 C15 N21 C14 0.3(5) . . . . ?
N23 C14 N21 C15 -0.2(5) . . . . ?
N24 C14 N21 C15 -177.0(4) . . . . ?
N24 C14 N23 C13 9.3(7) . . . . ?
N24 C14 N23 N22 176.9(4) . . . . ?
N25 C15 N21 C14 -179.7(4) . . . . ?
N25 C15 N22 Cu3 36.9(6) . . . . ?
N25 C15 N22 N23 179.7(4) . . . . ?
N26 C11 N27 C12 -179.5(4) . . . . ?
N26 C11 N27 N28 8.9(6) . . . . ?
N26 C11 N30 Cu2 10.0(7) . . . . ?
N26 C11 N30 N29 179.3(4) . . . . ?
N27 C11 N30 Cu2 -171.0(3) . . . . ?
N27 C11 N30 N29 -1.7(4) . . . . ?
N27 C12 C13 N23 148.2(4) . . . . ?
N27 C12 N29 Cu3 162.2(3) . . . . ?
N27 C12 N29 N30 -0.5(4) . . . . ?
N29 C12 C13 N23 -33.9(6) . . . . ?
N29 C12 N27 C11 -0.6(4) . . . . ?
N29 C12 N27 N28 170.4(4) . . . . ?
N30 C11 N27 C12 1.4(4) . . . . ?
N30 C11 N27 N28 -170.1(4) . . . . ?
O1 Cl1 O2 Cu3 72.3(3) . . . . ?
O2 Cl1 O1 Cu1 -51.2(3) . . . . ?
O3 Cl1 O1 Cu1 67.7(3) . . . . ?
O3 Cl1 O2 Cu3 -46.7(3) . . . . ?
O4 Cl1 O1 Cu1 -170.7(2) . . . . ?
O4 Cl1 O2 Cu3 -168.5(2) . . . . ?
