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#$Date: 2022-06-27 11:55:13 +0300 (Mon, 27 Jun 2022) $
#$Revision: 276280 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/55/8105528.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_8105528
loop_
_publ_author_name
'Wei, Xiao'
'Aiqin, Dong'
'Guang-Ming, Bao'
'Xiong-Xin, Peng'
'Ting-Ting, Sun'
'Chun-Yan, Hu'
'Hou-Qun, Yuan'
_publ_section_title
;
 Crystal structure of poly[dodekais(μ2-2,6-difluorobenzoato-κ2
 O:O&#x2032;)-bis((\m3-hexamethylenetetramine-\k3
 N:N′:N′′)hexacopper(II)], C48H30N4O12F12Cu3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              25
_journal_page_last               27
_journal_paper_doi               10.1515/ncrs-2018-0069
_journal_volume                  234
_journal_year                    2018
_chemical_formula_sum            'C48 H30 Cu3 F12 N4 O12'
_chemical_formula_weight         1273.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 110.665(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9112(5)
_cell_length_b                   28.1127(6)
_cell_length_c                   14.2324(5)
_cell_measurement_reflns_used    5129
_cell_measurement_temperature    173(10)
_cell_measurement_theta_max      27.3240
_cell_measurement_theta_min      3.7190
_cell_volume                     4833.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27059
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       Block
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         10405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0489
_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)+(0.0358P)²+2.7543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7283
_reflns_number_total             10405
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0069_suppl.cif
_cod_data_source_block           5411
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8105528
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Cu1 Cu 0.94722(4) 0.27774(2) 0.19889(3) 0.01874(11) Uani 1 1 d . . . . .
Cu2 Cu 0.83750(3) 0.21729(2) 0.05955(3) 0.01827(11) Uani 1 1 d . . . . .
O1 O 0.9699(2) 0.20854(9) 0.0237(2) 0.0301(6) Uani 1 1 d . . . . .
C1 C 1.0556(3) 0.23172(12) 0.0729(3) 0.0202(8) Uani 1 1 d . . . . .
O2 O 1.0651(2) 0.25941(8) 0.14419(19) 0.0250(6) Uani 1 1 d . . . . .
C2 C 1.1551(3) 0.22618(12) 0.0418(3) 0.0219(8) Uani 1 1 d . . . . .
C3 C 1.1911(3) 0.18307(14) 0.0186(3) 0.0333(10) Uani 1 1 d . . . . .
F1 F 1.1326(2) 0.14376(8) 0.0240(2) 0.0531(8) Uani 1 1 d . . . . .
C4 C 1.2825(4) 0.17730(16) -0.0079(4) 0.0464(12) Uani 1 1 d . . . . .
H1 H 1.304524 0.147256 -0.020755 0.056 Uiso 1 1 calc R U . . .
C5 C 1.3409(4) 0.21749(18) -0.0149(4) 0.0534(14) Uani 1 1 d . . . . .
H2 H 1.402430 0.214659 -0.034087 0.064 Uiso 1 1 calc R U . . .
C6 C 1.3089(4) 0.26156(16) 0.0062(4) 0.0491(13) Uani 1 1 d . . . . .
H3 H 1.347726 0.288695 0.001002 0.059 Uiso 1 1 calc R U . . .
C7 C 1.2185(4) 0.26473(14) 0.0352(3) 0.0373(11) Uani 1 1 d . . . . .
F2 F 1.1879(2) 0.30870(8) 0.0541(2) 0.0636(9) Uani 1 1 d . . . . .
O3 O 0.9879(2) 0.22272(9) 0.2878(2) 0.0325(7) Uani 1 1 d . . . . .
C8 C 0.9536(3) 0.18162(13) 0.2578(3) 0.0229(8) Uani 1 1 d . . . . .
O4 O 0.8946(2) 0.17082(8) 0.17000(19) 0.0290(6) Uani 1 1 d . . . . .
C9 C 0.9854(3) 0.14263(13) 0.3354(3) 0.0257(9) Uani 1 1 d . . . . .
C10 C 1.0243(3) 0.15065(13) 0.4381(3) 0.0284(9) Uani 1 1 d . . . . .
F3 F 1.0359(2) 0.19562(8) 0.47232(17) 0.0418(6) Uani 1 1 d . . . . .
C11 C 1.0511(4) 0.11529(16) 0.5087(4) 0.0531(14) Uani 1 1 d . . . . .
H4 H 1.076331 0.122714 0.576712 0.064 Uiso 1 1 calc R U . . .
C12 C 1.0404(6) 0.06916(19) 0.4781(4) 0.087(2) Uani 1 1 d . . . . .
H5 H 1.059937 0.044857 0.525418 0.104 Uiso 1 1 calc R U . . .
C13 C 1.0008(6) 0.05827(17) 0.3773(4) 0.085(2) Uani 1 1 d . . . . .
H6 H 0.990828 0.026754 0.356194 0.102 Uiso 1 1 calc R U . . .
C14 C 0.9760(5) 0.09465(15) 0.3084(3) 0.0517(14) Uani 1 1 d . . . . .
F4 F 0.9428(3) 0.08212(9) 0.2109(2) 0.0716(10) Uani 1 1 d . . . . .
O5 O 0.8026(2) 0.27557(9) -0.0258(2) 0.0335(7) Uani 1 1 d . . . . .
C15 C 0.8339(3) 0.31664(13) 0.0070(3) 0.0237(8) Uani 1 1 d . . . . .
O6 O 0.8940(2) 0.32632(8) 0.0960(2) 0.0305(6) Uani 1 1 d . . . . .
C16 C 0.8002(3) 0.35767(14) -0.0641(3) 0.0313(9) Uani 1 1 d . . . . .
C17 C 0.7602(3) 0.35284(15) -0.1684(3) 0.0355(10) Uani 1 1 d . . . . .
F5 F 0.7502(2) 0.30925(9) -0.20839(18) 0.0508(7) Uani 1 1 d . . . . .
C18 C 0.7307(5) 0.39014(18) -0.2341(4) 0.0604(15) Uani 1 1 d . . . . .
H7 H 0.705758 0.384812 -0.302982 0.072 Uiso 1 1 calc R U . . .
C19 C 0.7384(6) 0.4351(2) -0.1974(4) 0.090(2) Uani 1 1 d . . . . .
H8 H 0.733610 0.460872 -0.239623 0.108 Uiso 1 1 calc R U . A 1
C20A C 0.7542(9) 0.4431(4) -0.0907(8) 0.050(3) Uiso 0.5 1 d . . P B 1
H9A H 0.731687 0.470275 -0.065862 0.060 Uiso 0.5 1 calc R U P B 1
C20B C 0.7988(9) 0.4428(4) -0.1008(8) 0.048(3) Uiso 0.5 1 d . . P B 2
H9B H 0.833648 0.471846 -0.079109 0.058 Uiso 0.5 1 calc R U P B 2
C21 C 0.8073(5) 0.40451(16) -0.0322(4) 0.0707(18) Uani 1 1 d . . . . .
F6A F 0.8148(5) 0.41333(18) 0.0713(4) 0.0471(14) Uiso 0.5 1 d . . P B 1
F6B F 0.8679(5) 0.41503(18) 0.0632(4) 0.0460(14) Uiso 0.5 1 d . . P B 2
O7 O 0.7163(2) 0.23194(9) 0.10723(19) 0.0267(6) Uani 1 1 d . . . . .
C22 C 0.7263(3) 0.25756(12) 0.1819(3) 0.0222(8) Uani 1 1 d . . . . .
O8 O 0.8099(2) 0.28187(9) 0.2301(2) 0.0341(7) Uani 1 1 d . . . . .
C23 C 0.6297(3) 0.25879(13) 0.2170(3) 0.0257(9) Uani 1 1 d . . . . .
C24 C 0.5947(3) 0.29936(14) 0.2514(3) 0.0313(9) Uani 1 1 d . . . . .
F7 F 0.6480(2) 0.34066(8) 0.2494(2) 0.0497(7) Uani 1 1 d . . . . .
C25 C 0.5076(4) 0.30069(16) 0.2856(3) 0.0424(11) Uani 1 1 d . . . . .
H10 H 0.486186 0.329125 0.306759 0.051 Uiso 1 1 calc R U . . .
C26 C 0.4527(4) 0.25878(16) 0.2879(3) 0.0444(12) Uani 1 1 d . . . . .
H11 H 0.394310 0.258768 0.311843 0.053 Uiso 1 1 calc R U . . .
C27 C 0.4838(4) 0.21722(16) 0.2550(4) 0.0498(13) Uani 1 1 d . . . . .
H12 H 0.446858 0.188936 0.256127 0.060 Uiso 1 1 calc R U . . .
C28 C 0.5706(4) 0.21815(14) 0.2203(4) 0.0409(11) Uani 1 1 d . . . . .
F8 F 0.6002(3) 0.17640(9) 0.1902(3) 0.0760(11) Uani 1 1 d . . . . .
N1 N 0.7281(2) 0.16800(9) -0.0511(2) 0.0144(6) Uani 1 1 d . . . . .
C29 C 0.7870(3) 0.14397(11) -0.1111(3) 0.0176(7) Uani 1 1 d . . . . .
H19 H 0.820956 0.167842 -0.140110 0.021 Uiso 1 1 calc R U . . .
H20 H 0.845422 0.124085 -0.067129 0.021 Uiso 1 1 calc R U . . .
N2 N 0.7124(2) 0.11478(9) -0.1913(2) 0.0164(6) Uani 1 1 d . . . . .
C30 C 0.6250(3) 0.14523(12) -0.2572(3) 0.0190(8) Uani 1 1 d . . . . .
H21 H 0.575040 0.126122 -0.310851 0.023 Uiso 1 1 calc R U . . .
H22 H 0.657863 0.169067 -0.287316 0.023 Uiso 1 1 calc R U . . .
N3 N 0.5607(2) 0.16949(9) -0.2016(2) 0.0139(6) Uani 1 1 d . . . . .
C31 C 0.5117(3) 0.13256(11) -0.1567(3) 0.0163(7) Uani 1 1 d . . . . .
H23 H 0.460356 0.113585 -0.209709 0.020 Uiso 1 1 calc R U . . .
H24 H 0.470519 0.147643 -0.119545 0.020 Uiso 1 1 calc R U . . .
N4 N 0.5977(2) 0.10110(9) -0.0883(2) 0.0147(6) Uani 1 1 d . . . . .
C32 C 0.6767(3) 0.13076(11) -0.0079(3) 0.0167(7) Uani 1 1 d . . . . .
H25 H 0.637798 0.145702 0.031442 0.020 Uiso 1 1 calc R U . . .
H26 H 0.734123 0.110577 0.036530 0.020 Uiso 1 1 calc R U . . .
C33 C 0.6605(3) 0.07901(11) -0.1473(3) 0.0185(8) Uani 1 1 d . . . . .
H27 H 0.717277 0.058282 -0.103687 0.022 Uiso 1 1 calc R U . . .
H28 H 0.610506 0.059678 -0.200504 0.022 Uiso 1 1 calc R U . . .
C34 C 0.6396(3) 0.19779(11) -0.1200(2) 0.0152(7) Uani 1 1 d . . . . .
H29 H 0.599930 0.213633 -0.082427 0.018 Uiso 1 1 calc R U . . .
H30 H 0.672539 0.222072 -0.149017 0.018 Uiso 1 1 calc R U . . .
Cu3 Cu 0.52604(3) 0.04192(2) -0.02942(3) 0.01926(11) Uani 1 1 d . . . . .
O9 O 0.3697(2) 0.06138(8) -0.0691(2) 0.0262(6) Uani 1 1 d . . . . .
C35 C 0.3034(3) 0.03038(12) -0.0613(3) 0.0218(8) Uani 1 1 d . . . . .
O10 O 0.3271(2) -0.01021(8) -0.0226(2) 0.0273(6) Uani 1 1 d . . . . .
C36 C 0.1821(3) 0.04197(12) -0.1025(3) 0.0217(8) Uani 1 1 d . . . . .
C37 C 0.1171(3) 0.04125(13) -0.0426(3) 0.0282(9) Uani 1 1 d . . . . .
F9 F 0.1685(2) 0.03229(9) 0.05662(19) 0.0441(6) Uani 1 1 d . . . . .
C38 C 0.0053(3) 0.05003(14) -0.0790(4) 0.0374(11) Uani 1 1 d . . . . .
H13 H -0.035105 0.049576 -0.036340 0.045 Uiso 1 1 calc R U . . .
C39 C -0.0459(4) 0.05952(14) -0.1797(4) 0.0425(12) Uani 1 1 d . . . . .
H14 H -0.121771 0.065108 -0.205495 0.051 Uiso 1 1 calc R U . . .
C40 C 0.0144(3) 0.06082(14) -0.2429(4) 0.0395(11) Uani 1 1 d . . . . .
H15 H -0.019939 0.067351 -0.310974 0.047 Uiso 1 1 calc R U . . .
C41 C 0.1266(3) 0.05222(13) -0.2029(3) 0.0297(9) Uani 1 1 d . . . . .
F10 F 0.1851(2) 0.05218(9) -0.26494(18) 0.0491(7) Uani 1 1 d . . . . .
O11 O 0.5520(2) 0.06365(9) 0.1073(2) 0.0306(6) Uani 1 1 d . . . . .
C42 C 0.5496(3) 0.03463(13) 0.1736(3) 0.0264(9) Uani 1 1 d . . . . .
O12 O 0.5173(2) -0.00798(9) 0.1589(2) 0.0293(6) Uani 1 1 d . . . . .
C43 C 0.5901(4) 0.05191(14) 0.2806(3) 0.0341(10) Uani 1 1 d . . . . .
C44 C 0.5435(5) 0.03883(17) 0.3500(4) 0.0623(16) Uani 1 1 d . . . . .
F11A F 0.4341(5) 0.0167(2) 0.3072(5) 0.0561(17) Uiso 0.5 1 d . . P C 1
F11B F 0.4741(5) 0.00145(19) 0.3319(4) 0.0415(14) Uiso 0.5 1 d . . P C 2
C45 C 0.5785(6) 0.0550(2) 0.4477(4) 0.079(2) Uani 1 1 d . . . . .
H16 H 0.542325 0.045810 0.490870 0.095 Uiso 1 1 calc R U . . .
C46 C 0.6678(6) 0.08476(19) 0.4795(4) 0.078(2) Uani 1 1 d . . . . .
H17 H 0.693570 0.095932 0.545271 0.093 Uiso 1 1 calc R U . . .
C47 C 0.7191(5) 0.0981(2) 0.4148(4) 0.0771(19) Uani 1 1 d . . . . .
H18 H 0.780123 0.118190 0.436028 0.093 Uiso 1 1 calc R U . . .
C48 C 0.6796(5) 0.08140(17) 0.3175(4) 0.0545(14) Uani 1 1 d . . . . .
F12 F 0.7341(3) 0.09399(12) 0.2564(2) 0.0808(10) 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'
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'
F F 0.0171 0.0103 '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'
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
O6 Cu1 O3 171.88(11) . .
O6 Cu1 O8 91.22(12) . .
O3 Cu1 O8 87.62(12) . .
O6 Cu1 O2 90.18(11) . .
O3 Cu1 O2 88.88(11) . .
O8 Cu1 O2 164.88(10) . .
O6 Cu1 N3 89.40(10) . 4_666
O3 Cu1 N3 98.67(10) . 4_666
O8 Cu1 N3 105.13(10) . 4_666
O2 Cu1 N3 89.94(10) . 4_666
O6 Cu1 Cu2 86.12(8) . .
O3 Cu1 Cu2 85.78(8) . .
O8 Cu1 Cu2 85.40(8) . .
O2 Cu1 Cu2 79.68(7) . .
N3 Cu1 Cu2 168.66(7) 4_666 .
O7 Cu2 O1 172.87(11) . .
O7 Cu2 O4 89.03(11) . .
O1 Cu2 O4 90.52(11) . .
O7 Cu2 O5 90.11(11) . .
O1 Cu2 O5 88.56(12) . .
O4 Cu2 O5 165.61(11) . .
O7 Cu2 N1 89.47(10) . .
O1 Cu2 N1 97.64(10) . .
O4 Cu2 N1 96.80(10) . .
O5 Cu2 N1 97.56(10) . .
O7 Cu2 Cu1 83.44(8) . .
O1 Cu2 Cu1 89.45(7) . .
O4 Cu2 Cu1 82.88(7) . .
O5 Cu2 Cu1 82.74(8) . .
N1 Cu2 Cu1 172.91(7) . .
C1 O1 Cu2 117.7(2) . .
O2 C1 O1 125.9(3) . .
O2 C1 C2 117.0(3) . .
O1 C1 C2 117.1(3) . .
C1 O2 Cu1 127.2(2) . .
C3 C2 C7 114.6(3) . .
C3 C2 C1 123.7(3) . .
C7 C2 C1 121.7(3) . .
F1 C3 C4 118.0(4) . .
F1 C3 C2 117.5(3) . .
C4 C3 C2 124.5(4) . .
C3 C4 C5 118.0(4) . .
C6 C5 C4 120.5(4) . .
C7 C6 C5 118.6(4) . .
F2 C7 C6 117.3(4) . .
F2 C7 C2 118.8(3) . .
C6 C7 C2 123.9(4) . .
C8 O3 Cu1 121.8(2) . .
O4 C8 O3 125.5(3) . .
O4 C8 C9 117.9(3) . .
O3 C8 C9 116.6(3) . .
C8 O4 Cu2 124.0(2) . .
C10 C9 C14 114.3(4) . .
C10 C9 C8 123.9(3) . .
C14 C9 C8 121.8(4) . .
F3 C10 C11 116.8(4) . .
F3 C10 C9 119.2(3) . .
C11 C10 C9 124.0(4) . .
C12 C11 C10 119.2(5) . .
C11 C12 C13 120.3(5) . .
C14 C13 C12 119.0(5) . .
F4 C14 C13 116.8(4) . .
F4 C14 C9 120.1(4) . .
C13 C14 C9 123.1(4) . .
C15 O5 Cu2 123.6(2) . .
O5 C15 O6 125.1(3) . .
O5 C15 C16 118.6(3) . .
O6 C15 C16 116.3(3) . .
C15 O6 Cu1 122.3(2) . .
C21 C16 C17 113.5(4) . .
C21 C16 C15 122.8(4) . .
C17 C16 C15 123.7(4) . .
F5 C17 C18 116.8(4) . .
F5 C17 C16 119.0(4) . .
C18 C17 C16 124.2(4) . .
C19 C18 C17 119.1(5) . .
C20B C19 C18 119.0(7) . .
C18 C19 C20A 120.2(6) . .
C21 C20A C19 110.8(8) . .
C19 C20B C21 117.0(9) . .
F6B C21 C16 119.3(4) . .
C16 C21 C20A 125.7(6) . .
F6B C21 C20B 113.7(6) . .
C16 C21 C20B 120.8(6) . .
C16 C21 F6A 117.7(4) . .
C20A C21 F6A 108.2(6) . .
C22 O7 Cu2 124.1(2) . .
O7 C22 O8 125.9(3) . .
O7 C22 C23 116.6(3) . .
O8 C22 C23 117.4(3) . .
C22 O8 Cu1 120.7(2) . .
C24 C23 C28 114.7(3) . .
C24 C23 C22 123.5(3) . .
C28 C23 C22 121.7(3) . .
F7 C24 C25 117.9(3) . .
F7 C24 C23 118.0(3) . .
C25 C24 C23 124.0(4) . .
C24 C25 C26 118.4(4) . .
C27 C26 C25 120.3(4) . .
C26 C27 C28 118.7(4) . .
F8 C28 C27 117.1(4) . .
F8 C28 C23 119.1(3) . .
C27 C28 C23 123.8(4) . .
C34 N1 C32 108.7(3) . .
C34 N1 C29 107.9(3) . .
C32 N1 C29 108.1(2) . .
C34 N1 Cu2 105.66(18) . .
C32 N1 Cu2 114.6(2) . .
C29 N1 Cu2 111.6(2) . .
N2 C29 N1 112.0(3) . .
C29 N2 C30 108.6(2) . .
C29 N2 C33 109.0(3) . .
C30 N2 C33 108.0(3) . .
N2 C30 N3 112.0(3) . .
C31 N3 C34 108.7(3) . .
C31 N3 C30 108.1(2) . .
C34 N3 C30 107.6(3) . .
C31 N3 Cu1 117.5(2) . 4_565
C34 N3 Cu1 105.02(18) . 4_565
C30 N3 Cu1 109.44(19) . 4_565
N3 C31 N4 111.6(3) . .
C31 N4 C32 108.7(2) . .
C31 N4 C33 108.0(3) . .
C32 N4 C33 107.7(3) . .
C31 N4 Cu3 112.47(19) . .
C32 N4 Cu3 113.28(19) . .
C33 N4 Cu3 106.47(18) . .
N1 C32 N4 111.2(3) . .
N2 C33 N4 112.1(2) . .
N3 C34 N1 112.0(2) . .
O11 Cu3 O9 89.85(11) . .
O11 Cu3 O12 167.11(10) . 3_655
O9 Cu3 O12 86.69(11) . 3_655
O11 Cu3 O10 87.89(11) . 3_655
O9 Cu3 O10 167.71(9) . 3_655
O12 Cu3 O10 92.86(11) 3_655 3_655
O11 Cu3 N4 101.24(10) . .
O9 Cu3 N4 101.88(10) . .
O12 Cu3 N4 91.63(10) 3_655 .
O10 Cu3 N4 90.41(10) 3_655 .
O11 Cu3 Cu3 86.41(8) . 3_655
O9 Cu3 Cu3 89.37(7) . 3_655
O12 Cu3 Cu3 81.15(7) 3_655 3_655
O10 Cu3 Cu3 78.44(7) 3_655 3_655
N4 Cu3 Cu3 166.31(7) . 3_655
C35 O9 Cu3 116.3(2) . .
O9 C35 O10 127.0(3) . .
O9 C35 C36 117.7(3) . .
O10 C35 C36 115.3(3) . .
C35 O10 Cu3 128.5(2) . 3_655
C41 C36 C37 115.5(3) . .
C41 C36 C35 122.5(3) . .
C37 C36 C35 121.9(3) . .
F9 C37 C38 119.3(4) . .
F9 C37 C36 117.5(3) . .
C38 C37 C36 123.2(4) . .
C37 C38 C39 118.9(4) . .
C38 C39 C40 120.6(4) . .
C41 C40 C39 118.5(4) . .
F10 C41 C40 118.6(4) . .
F10 C41 C36 118.0(3) . .
C40 C41 C36 123.4(4) . .
C42 O11 Cu3 120.3(2) . .
O11 C42 O12 125.9(4) . .
O11 C42 C43 117.3(3) . .
O12 C42 C43 116.7(4) . .
C42 O12 Cu3 125.6(3) . 3_655
C48 C43 C44 114.3(4) . .
C48 C43 C42 121.9(4) . .
C44 C43 C42 123.8(4) . .
F11B C44 C43 120.1(4) . .
F11B C44 C45 114.2(5) . .
C43 C44 C45 124.4(5) . .
C43 C44 F11A 114.7(5) . .
C45 C44 F11A 119.0(5) . .
C46 C45 C44 118.3(5) . .
C47 C46 C45 119.9(5) . .
C46 C47 C48 119.4(5) . .
F12 C48 C43 118.4(4) . .
F12 C48 C47 117.9(5) . .
C43 C48 C47 123.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O6 1.942(3) .
Cu1 O3 1.949(2) .
Cu1 O8 1.977(3) .
Cu1 O2 2.006(2) .
Cu1 N3 2.211(3) 4_666
Cu1 Cu2 2.6164(6) .
Cu2 O7 1.956(2) .
Cu2 O1 1.964(2) .
Cu2 O4 1.976(3) .
Cu2 O5 1.995(3) .
Cu2 N1 2.196(3) .
O1 C1 1.263(4) .
C1 O2 1.250(4) .
C1 C2 1.506(5) .
C2 C3 1.379(5) .
C2 C7 1.381(5) .
C3 F1 1.355(4) .
C3 C4 1.369(5) .
C4 C5 1.382(6) .
C5 C6 1.372(6) .
C6 C7 1.372(5) .
C7 F2 1.353(4) .
O3 C8 1.257(4) .
C8 O4 1.250(4) .
C8 C9 1.507(5) .
C9 C10 1.387(5) .
C9 C14 1.396(5) .
C10 F3 1.344(4) .
C10 C11 1.368(5) .
C11 C12 1.360(7) .
C12 C13 1.376(7) .
C13 C14 1.375(6) .
C14 F4 1.346(5) .
O5 C15 1.258(4) .
C15 O6 1.259(4) .
C15 C16 1.495(5) .
C16 C21 1.385(6) .
C16 C17 1.396(6) .
C17 F5 1.338(5) .
C17 C18 1.366(6) .
C18 C19 1.357(7) .
C19 C20B 1.338(12) .
C19 C20A 1.477(12) .
C20A C21 1.392(11) .
C20B C21 1.431(11) .
C21 F6B 1.339(7) .
C21 F6A 1.463(7) .
O7 C22 1.252(4) .
C22 O8 1.257(4) .
C22 C23 1.499(5) .
C23 C24 1.378(5) .
C23 C28 1.384(5) .
C24 F7 1.354(4) .
C24 C25 1.375(5) .
C25 C26 1.382(6) .
C26 C27 1.370(6) .
C27 C28 1.375(6) .
C28 F8 1.350(4) .
N1 C34 1.476(4) .
N1 C32 1.484(4) .
N1 C29 1.491(4) .
C29 N2 1.458(4) .
N2 C30 1.462(4) .
N2 C33 1.467(4) .
C30 N3 1.498(4) .
N3 C31 1.474(4) .
N3 C34 1.477(4) .
C31 N4 1.483(4) .
N4 C32 1.490(4) .
N4 C33 1.493(4) .
N4 Cu3 2.207(3) .
Cu3 O11 1.952(3) .
Cu3 O9 1.972(2) .
Cu3 O12 1.973(3) 3_655
Cu3 O10 1.987(2) 3_655
Cu3 Cu3 2.6659(8) 3_655
O9 C35 1.253(4) .
C35 O10 1.257(4) .
C35 C36 1.501(5) .
C36 C41 1.384(5) .
C36 C37 1.392(5) .
C37 F9 1.355(5) .
C37 C38 1.373(5) .
C38 C39 1.376(6) .
C39 C40 1.383(6) .
C40 C41 1.378(5) .
C41 F10 1.349(4) .
O11 C42 1.256(4) .
C42 O12 1.262(4) .
C42 C43 1.506(5) .
C43 C48 1.368(6) .
C43 C44 1.375(6) .
C44 F11B 1.346(7) .
C44 C45 1.379(7) .
C44 F11A 1.464(8) .
C45 C46 1.366(8) .
C46 C47 1.363(7) .
C47 C48 1.378(7) .
C48 F12 1.345(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
Cu2 O1 C1 O2 1.3(5) . . . .
Cu2 O1 C1 C2 -177.6(2) . . . .
O1 C1 O2 Cu1 -2.7(5) . . . .
C2 C1 O2 Cu1 176.2(2) . . . .
O2 C1 C2 C3 137.4(4) . . . .
O1 C1 C2 C3 -43.6(5) . . . .
O2 C1 C2 C7 -42.1(5) . . . .
O1 C1 C2 C7 136.9(4) . . . .
C7 C2 C3 F1 179.8(4) . . . .
C1 C2 C3 F1 0.2(6) . . . .
C7 C2 C3 C4 0.8(7) . . . .
C1 C2 C3 C4 -178.7(4) . . . .
F1 C3 C4 C5 179.0(4) . . . .
C2 C3 C4 C5 -2.1(8) . . . .
C3 C4 C5 C6 1.3(8) . . . .
C4 C5 C6 C7 0.6(8) . . . .
C5 C6 C7 F2 -179.0(5) . . . .
C5 C6 C7 C2 -1.9(8) . . . .
C3 C2 C7 F2 178.3(4) . . . .
C1 C2 C7 F2 -2.2(6) . . . .
C3 C2 C7 C6 1.2(7) . . . .
C1 C2 C7 C6 -179.2(4) . . . .
Cu1 O3 C8 O4 2.6(5) . . . .
Cu1 O3 C8 C9 -176.5(2) . . . .
O3 C8 O4 Cu2 -2.6(5) . . . .
C9 C8 O4 Cu2 176.5(2) . . . .
O4 C8 C9 C10 -162.3(4) . . . .
O3 C8 C9 C10 16.8(5) . . . .
O4 C8 C9 C14 16.6(6) . . . .
O3 C8 C9 C14 -164.3(4) . . . .
C14 C9 C10 F3 -179.7(4) . . . .
C8 C9 C10 F3 -0.7(6) . . . .
C14 C9 C10 C11 -0.4(6) . . . .
C8 C9 C10 C11 178.6(4) . . . .
F3 C10 C11 C12 179.7(5) . . . .
C9 C10 C11 C12 0.4(8) . . . .
C10 C11 C12 C13 -1.4(10) . . . .
C11 C12 C13 C14 2.3(11) . . . .
C12 C13 C14 F4 176.8(6) . . . .
C12 C13 C14 C9 -2.4(10) . . . .
C10 C9 C14 F4 -177.8(4) . . . .
C8 C9 C14 F4 3.2(7) . . . .
C10 C9 C14 C13 1.3(8) . . . .
C8 C9 C14 C13 -177.6(5) . . . .
Cu2 O5 C15 O6 2.6(5) . . . .
Cu2 O5 C15 C16 -178.6(3) . . . .
O5 C15 O6 Cu1 -0.7(5) . . . .
C16 C15 O6 Cu1 -179.5(2) . . . .
O5 C15 C16 C21 164.3(5) . . . .
O6 C15 C16 C21 -16.8(6) . . . .
O5 C15 C16 C17 -16.6(6) . . . .
O6 C15 C16 C17 162.3(4) . . . .
C21 C16 C17 F5 179.6(4) . . . .
C15 C16 C17 F5 0.4(6) . . . .
C21 C16 C17 C18 0.2(7) . . . .
C15 C16 C17 C18 -178.9(4) . . . .
F5 C17 C18 C19 179.5(5) . . . .
C16 C17 C18 C19 -1.1(8) . . . .
C17 C18 C19 C20B 16.3(11) . . . .
C17 C18 C19 C20A -13.3(11) . . . .
C18 C19 C20A C21 26.8(12) . . . .
C18 C19 C20B C21 -29.1(13) . . . .
C17 C16 C21 F6B -164.2(5) . . . .
C15 C16 C21 F6B 14.9(9) . . . .
C17 C16 C21 C20A 17.3(10) . . . .
C15 C16 C21 C20A -163.6(7) . . . .
C17 C16 C21 C20B -13.6(9) . . . .
C15 C16 C21 C20B 165.5(7) . . . .
C17 C16 C21 F6A 161.6(5) . . . .
C15 C16 C21 F6A -19.3(8) . . . .
C19 C20A C21 C16 -29.8(12) . . . .
C19 C20A C21 F6A -176.7(7) . . . .
C19 C20B C21 F6B -179.3(8) . . . .
C19 C20B C21 C16 28.6(13) . . . .
Cu2 O7 C22 O8 8.7(5) . . . .
Cu2 O7 C22 C23 -170.8(2) . . . .
O7 C22 O8 Cu1 -5.7(5) . . . .
C23 C22 O8 Cu1 173.8(2) . . . .
O7 C22 C23 C24 -141.2(4) . . . .
O8 C22 C23 C24 39.3(5) . . . .
O7 C22 C23 C28 41.0(5) . . . .
O8 C22 C23 C28 -138.5(4) . . . .
C28 C23 C24 F7 -179.3(4) . . . .
C22 C23 C24 F7 2.7(6) . . . .
C28 C23 C24 C25 -0.7(7) . . . .
C22 C23 C24 C25 -178.6(4) . . . .
F7 C24 C25 C26 180.0(4) . . . .
C23 C24 C25 C26 1.3(7) . . . .
C24 C25 C26 C27 -1.1(7) . . . .
C25 C26 C27 C28 0.3(8) . . . .
C26 C27 C28 F8 178.9(5) . . . .
C26 C27 C28 C23 0.4(8) . . . .
C24 C23 C28 F8 -178.6(4) . . . .
C22 C23 C28 F8 -0.6(7) . . . .
C24 C23 C28 C27 -0.2(7) . . . .
C22 C23 C28 C27 177.8(4) . . . .
C34 N1 C29 N2 -58.7(3) . . . .
C32 N1 C29 N2 58.7(3) . . . .
Cu2 N1 C29 N2 -174.3(2) . . . .
N1 C29 N2 C30 59.1(3) . . . .
N1 C29 N2 C33 -58.4(3) . . . .
C29 N2 C30 N3 -59.0(3) . . . .
C33 N2 C30 N3 59.2(3) . . . .
N2 C30 N3 C31 -58.9(3) . . . .
N2 C30 N3 C34 58.3(3) . . . .
N2 C30 N3 Cu1 172.0(2) . . . 4_565
C34 N3 C31 N4 -58.4(3) . . . .
C30 N3 C31 N4 58.2(3) . . . .
Cu1 N3 C31 N4 -177.40(19) 4_565 . . .
N3 C31 N4 C32 58.4(3) . . . .
N3 C31 N4 C33 -58.2(3) . . . .
N3 C31 N4 Cu3 -175.36(19) . . . .
C34 N1 C32 N4 57.9(3) . . . .
C29 N1 C32 N4 -59.0(3) . . . .
Cu2 N1 C32 N4 175.88(19) . . . .
C31 N4 C32 N1 -58.0(3) . . . .
C33 N4 C32 N1 58.8(3) . . . .
Cu3 N4 C32 N1 176.23(19) . . . .
C29 N2 C33 N4 58.5(3) . . . .
C30 N2 C33 N4 -59.3(3) . . . .
C31 N4 C33 N2 58.8(3) . . . .
C32 N4 C33 N2 -58.4(3) . . . .
Cu3 N4 C33 N2 179.8(2) . . . .
C31 N3 C34 N1 58.6(3) . . . .
C30 N3 C34 N1 -58.3(3) . . . .
Cu1 N3 C34 N1 -174.9(2) 4_565 . . .
C32 N1 C34 N3 -58.4(3) . . . .
C29 N1 C34 N3 58.6(3) . . . .
Cu2 N1 C34 N3 178.1(2) . . . .
Cu3 O9 C35 O10 7.0(5) . . . .
Cu3 O9 C35 C36 -172.7(2) . . . .
O9 C35 O10 Cu3 -5.5(6) . . . 3_655
C36 C35 O10 Cu3 174.2(2) . . . 3_655
O9 C35 C36 C41 60.7(5) . . . .
O10 C35 C36 C41 -119.0(4) . . . .
O9 C35 C36 C37 -121.8(4) . . . .
O10 C35 C36 C37 58.4(5) . . . .
C41 C36 C37 F9 -178.7(3) . . . .
C35 C36 C37 F9 3.7(5) . . . .
C41 C36 C37 C38 0.0(5) . . . .
C35 C36 C37 C38 -177.6(3) . . . .
F9 C37 C38 C39 179.4(4) . . . .
C36 C37 C38 C39 0.7(6) . . . .
C37 C38 C39 C40 -0.9(6) . . . .
C38 C39 C40 C41 0.3(6) . . . .
C39 C40 C41 F10 178.2(3) . . . .
C39 C40 C41 C36 0.5(6) . . . .
C37 C36 C41 F10 -178.3(3) . . . .
C35 C36 C41 F10 -0.8(5) . . . .
C37 C36 C41 C40 -0.6(6) . . . .
C35 C36 C41 C40 177.0(4) . . . .
Cu3 O11 C42 O12 -10.0(5) . . . .
Cu3 O11 C42 C43 169.4(3) . . . .
O11 C42 O12 Cu3 5.6(5) . . . 3_655
C43 C42 O12 Cu3 -173.7(2) . . . 3_655
O11 C42 C43 C48 -38.6(6) . . . .
O12 C42 C43 C48 140.7(4) . . . .
O11 C42 C43 C44 143.1(5) . . . .
O12 C42 C43 C44 -37.5(6) . . . .
C48 C43 C44 F11B -163.5(6) . . . .
C42 C43 C44 F11B 14.8(9) . . . .
C48 C43 C44 C45 2.7(9) . . . .
C42 C43 C44 C45 -178.9(5) . . . .
C48 C43 C44 F11A 166.6(5) . . . .
C42 C43 C44 F11A -15.1(7) . . . .
F11B C44 C45 C46 164.7(6) . . . .
C43 C44 C45 C46 -2.2(10) . . . .
F11A C44 C45 C46 -165.4(6) . . . .
C44 C45 C46 C47 0.6(10) . . . .
C45 C46 C47 C48 0.3(10) . . . .
C44 C43 C48 F12 176.5(5) . . . .
C42 C43 C48 F12 -1.9(7) . . . .
C44 C43 C48 C47 -1.7(8) . . . .
C42 C43 C48 C47 179.9(5) . . . .
C46 C47 C48 F12 -178.0(6) . . . .
C46 C47 C48 C43 0.3(10) . . . .
