#------------------------------------------------------------------------------
#$Date: 2023-08-08 00:57:23 +0300 (Tue, 08 Aug 2023) $
#$Revision: 285572 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/20/7132007.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_7132007
loop_
_publ_author_name
'Peng, Xinyang'
'Han, Jinxiu'
'Li, Xialiang'
'Liu, Guijun'
'Xu, Yuhan'
'Peng, Yuxin'
'Nie, Shuai'
'Li, Wenzi'
'Li, Xinrui'
'Chen, Zhuo'
'Peng, Haonan'
'Cao, Rui'
'Fang, Yu'
_publ_section_title
;
 Electrocatalytic hydrogen evolution media with a copper porphyrin bearing
 meso-(o-carborane) substituents
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03104G
_journal_year                    2023
_chemical_formula_sum            'C47 H36 Cu F10 N4 Si2'
_chemical_formula_weight         966.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-06-21 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.824(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2143(18)
_cell_length_b                   6.3478(6)
_cell_length_c                   29.627(2)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.368
_cell_measurement_theta_min      3.2915
_cell_volume                     4310.3(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       multi-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47315
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         3.291
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6270
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6270
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0410
_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)+(0.0633P)²+7.7912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4102
_reflns_number_total             4343
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc03104g2.cif
_cod_data_source_block           pxy20230418_0m_a_sq
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7132007
_shelx_shelxl_version_number     2014/7
_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.
;
_exptl_absorpt_special_details   sadabs
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
Cu1 Cu 0.2500 0.2500 0.7500 0.01940(13) Uani 1 2 d S . P A 1
Si1 Si 0.10409(3) 1.21616(10) 0.83195(2) 0.02941(17) Uani 1 1 d . . . A 1
F1 F 0.35252(8) 0.1549(3) 0.94529(6) 0.0502(4) Uani 1 1 d . . . A 1
F2 F 0.44292(10) 0.1563(3) 1.02727(5) 0.0624(5) Uani 1 1 d . . . A 1
F3 F 0.55111(9) 0.2651(3) 1.02685(7) 0.0657(6) Uani 1 1 d . . . A 1
F4 F 0.56753(6) 0.3875(3) 0.94429(7) 0.0603(5) Uani 1 1 d . . . A 1
F5 F 0.47681(6) 0.3955(3) 0.86281(6) 0.0420(4) Uani 1 1 d . . . A 1
N1 N 0.27325(7) 0.4466(3) 0.80586(6) 0.0216(4) Uani 1 1 d . . . A 1
N2 N 0.31883(7) 0.0666(3) 0.78165(6) 0.0217(4) Uani 1 1 d . . . A 1
C1 C 0.24552(9) 0.6274(3) 0.81196(7) 0.0233(4) Uani 1 1 d . . . A 1
C2 C 0.27553(10) 0.7231(4) 0.85734(8) 0.0278(5) Uani 1 1 d . . . A 1
H13 H 0.2649 0.8460 0.8695 0.033 Uiso 1 1 calc R U . A 1
C3 C 0.32190(10) 0.6001(4) 0.87869(8) 0.0285(5) Uani 1 1 d . . . A 1
H1 H 0.3495 0.6224 0.9085 0.034 Uiso 1 1 calc R U . A 1
C4 C 0.32074(9) 0.4276(3) 0.84690(7) 0.0238(4) Uani 1 1 d . . . A 1
C5 C 0.36181(9) 0.2674(3) 0.85563(8) 0.0241(4) Uani 1 1 d . . . A 1
C6 C 0.41165(10) 0.2741(3) 0.90156(8) 0.0280(5) Uani 1 1 d . . . A 1
C7 C 0.40481(12) 0.2156(4) 0.94424(9) 0.0352(5) Uani 1 1 d . . . A 1
C8 C 0.45159(15) 0.2144(4) 0.98642(9) 0.0447(7) Uani 1 1 d . . . A 1
C9 C 0.50581(14) 0.2703(4) 0.98585(10) 0.0452(8) Uani 1 1 d . . . A 1
C10 C 0.51422(11) 0.3301(4) 0.94418(10) 0.0416(6) Uani 1 1 d . . . A 1
C11 C 0.46737(10) 0.3331(4) 0.90257(9) 0.0328(5) Uani 1 1 d . . . A 1
C12 C 0.36080(9) 0.0987(3) 0.82547(7) 0.0229(4) Uani 1 1 d . . . A 1
C13 C 0.40303(9) -0.0691(4) 0.83554(8) 0.0273(5) Uani 1 1 d . . . A 1
H3 H 0.4353 -0.0834 0.8628 0.033 Uiso 1 1 calc R U . A 1
C14 C 0.38698(10) -0.2018(4) 0.79788(8) 0.0271(5) Uani 1 1 d . . . A 1
H2 H 0.4060 -0.3247 0.7942 0.033 Uiso 1 1 calc R U . A 1
C15 C 0.16512(9) 0.6163(3) 0.73537(7) 0.0230(4) Uani 1 1 d . . . A 1
C16 C 0.19462(9) 0.7084(3) 0.77955(8) 0.0243(4) Uani 1 1 d . . . A 1
C17 C 0.16896(10) 0.8908(4) 0.79332(8) 0.0279(5) Uani 1 1 d . . . A 1
C18 C 0.05286(14) 1.3742(5) 0.78391(12) 0.0521(7) Uani 1 1 d . . . A 1
H4 H 0.0321 1.4708 0.7976 0.078 Uiso 1 1 calc R U . A 1
H5 H 0.0256 1.2822 0.7621 0.078 Uiso 1 1 calc R U . A 1
H6 H 0.0743 1.4516 0.7672 0.078 Uiso 1 1 calc R U . A 1
C19 C 0.06273(13) 1.0490(5) 0.86136(11) 0.0473(7) Uani 1 1 d . . . A 1
H7 H 0.0440 1.1369 0.8785 0.071 Uiso 1 1 calc R U . A 1
H8 H 0.0890 0.9541 0.8832 0.071 Uiso 1 1 calc R U . A 1
H9 H 0.0338 0.9697 0.8376 0.071 Uiso 1 1 calc R U . A 1
C20 C 0.15665(16) 1.3846(6) 0.87662(13) 0.0614(9) Uani 1 1 d . . . A 1
H10 H 0.1830 1.2975 0.9005 0.092 Uiso 1 1 calc R U . A 1
H11 H 0.1359 1.4757 0.8914 0.092 Uiso 1 1 calc R U . A 1
H12 H 0.1783 1.4681 0.8612 0.092 Uiso 1 1 calc R U . A 1
C47 C 0.14523(10) 1.0343(4) 0.80617(8) 0.0324(5) Uani 1 1 d . . . A 1
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'
F F 0.0171 0.0103 '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'
Si Si 0.0817 0.0704 '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
N2 Cu1 N2 180.0 7_556 . ?
N2 Cu1 N1 90.33(7) 7_556 7_556 ?
N2 Cu1 N1 89.67(7) . 7_556 ?
N2 Cu1 N1 89.67(7) 7_556 . ?
N2 Cu1 N1 90.33(7) . . ?
N1 Cu1 N1 180.0 7_556 . ?
C47 Si1 C18 109.77(13) . . ?
C47 Si1 C19 106.37(13) . . ?
C18 Si1 C19 109.93(15) . . ?
C47 Si1 C20 108.62(14) . . ?
C18 Si1 C20 111.83(19) . . ?
C19 Si1 C20 110.17(15) . . ?
C1 N1 C4 105.14(17) . . ?
C1 N1 Cu1 127.70(14) . . ?
C4 N1 Cu1 127.15(14) . . ?
C15 N2 C12 105.12(17) 7_556 . ?
C15 N2 Cu1 127.76(14) 7_556 . ?
C12 N2 Cu1 127.12(14) . . ?
N1 C1 C16 125.5(2) . . ?
N1 C1 C2 110.78(19) . . ?
C16 C1 C2 123.8(2) . . ?
C3 C2 C1 106.7(2) . . ?
C3 C2 H13 126.6 . . ?
C1 C2 H13 126.6 . . ?
C2 C3 C4 107.26(19) . . ?
C2 C3 H1 126.4 . . ?
C4 C3 H1 126.4 . . ?
N1 C4 C5 124.81(19) . . ?
N1 C4 C3 110.11(18) . . ?
C5 C4 C3 125.1(2) . . ?
C4 C5 C12 125.6(2) . . ?
C4 C5 C6 117.83(19) . . ?
C12 C5 C6 116.58(19) . . ?
C7 C6 C11 117.1(2) . . ?
C7 C6 C5 121.7(2) . . ?
C11 C6 C5 121.2(2) . . ?
F1 C7 C6 119.7(2) . . ?
F1 C7 C8 118.8(2) . . ?
C6 C7 C8 121.5(3) . . ?
F2 C8 C9 120.8(3) . . ?
F2 C8 C7 119.5(3) . . ?
C9 C8 C7 119.7(3) . . ?
F3 C9 C10 120.3(3) . . ?
F3 C9 C8 119.2(3) . . ?
C10 C9 C8 120.5(2) . . ?
F4 C10 C9 119.8(2) . . ?
F4 C10 C11 120.8(3) . . ?
C9 C10 C11 119.4(3) . . ?
F5 C11 C10 117.9(2) . . ?
F5 C11 C6 120.3(2) . . ?
C10 C11 C6 121.8(3) . . ?
N2 C12 C5 124.96(19) . . ?
N2 C12 C13 110.09(18) . . ?
C5 C12 C13 124.9(2) . . ?
C14 C13 C12 107.13(19) . . ?
C14 C13 H3 126.4 . . ?
C12 C13 H3 126.4 . . ?
C13 C14 C15 106.63(19) . 7_556 ?
C13 C14 H2 126.7 . . ?
C15 C14 H2 126.7 7_556 . ?
N2 C15 C16 125.27(19) 7_556 . ?
N2 C15 C14 111.02(19) 7_556 7_556 ?
C16 C15 C14 123.7(2) . 7_556 ?
C1 C16 C15 124.1(2) . . ?
C1 C16 C17 118.0(2) . . ?
C15 C16 C17 117.7(2) . . ?
C47 C17 C16 175.4(3) . . ?
Si1 C18 H4 109.5 . . ?
Si1 C18 H5 109.5 . . ?
H4 C18 H5 109.5 . . ?
Si1 C18 H6 109.5 . . ?
H4 C18 H6 109.5 . . ?
H5 C18 H6 109.5 . . ?
Si1 C19 H7 109.5 . . ?
Si1 C19 H8 109.5 . . ?
H7 C19 H8 109.5 . . ?
Si1 C19 H9 109.5 . . ?
H7 C19 H9 109.5 . . ?
H8 C19 H9 109.5 . . ?
Si1 C20 H10 109.5 . . ?
Si1 C20 H11 109.5 . . ?
H10 C20 H11 109.5 . . ?
Si1 C20 H12 109.5 . . ?
H10 C20 H12 109.5 . . ?
H11 C20 H12 109.5 . . ?
C17 C47 Si1 169.3(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 2.0010(17) 7_556 ?
Cu1 N2 2.0010(17) . ?
Cu1 N1 2.0031(17) 7_556 ?
Cu1 N1 2.0032(17) . ?
Si1 C47 1.844(2) . ?
Si1 C18 1.852(3) . ?
Si1 C19 1.858(3) . ?
Si1 C20 1.851(3) . ?
F1 C7 1.333(3) . ?
F2 C8 1.345(3) . ?
F3 C9 1.349(3) . ?
F4 C10 1.341(3) . ?
F5 C11 1.330(3) . ?
N1 C1 1.371(3) . ?
N1 C4 1.383(3) . ?
N2 C15 1.371(3) 7_556 ?
N2 C12 1.381(3) . ?
C1 C16 1.393(3) . ?
C1 C2 1.440(3) . ?
C2 C3 1.346(3) . ?
C2 H13 0.9300 . ?
C3 C4 1.439(3) . ?
C3 H1 0.9300 . ?
C4 C5 1.387(3) . ?
C5 C12 1.390(3) . ?
C5 C6 1.500(3) . ?
C6 C7 1.378(4) . ?
C6 C11 1.391(3) . ?
C7 C8 1.390(4) . ?
C8 C9 1.365(5) . ?
C9 C10 1.368(5) . ?
C10 C11 1.380(3) . ?
C12 C13 1.440(3) . ?
C13 C14 1.351(3) . ?
C13 H3 0.9300 . ?
C14 C15 1.433(3) 7_556 ?
C14 H2 0.9300 . ?
C15 N2 1.371(3) 7_556 ?
C15 C16 1.401(3) . ?
C15 C14 1.433(3) 7_556 ?
C16 C17 1.434(3) . ?
C17 C47 1.203(3) . ?
C18 H4 0.9600 . ?
C18 H5 0.9600 . ?
C18 H6 0.9600 . ?
C19 H7 0.9600 . ?
C19 H8 0.9600 . ?
C19 H9 0.9600 . ?
C20 H10 0.9600 . ?
C20 H11 0.9600 . ?
C20 H12 0.9600 . ?
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
C4 N1 C1 C16 -179.2(2) . . . . ?
Cu1 N1 C1 C16 0.3(3) . . . . ?
C4 N1 C1 C2 -0.3(2) . . . . ?
Cu1 N1 C1 C2 179.21(15) . . . . ?
N1 C1 C2 C3 0.4(3) . . . . ?
C16 C1 C2 C3 179.3(2) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 N1 C4 C5 -178.8(2) . . . . ?
Cu1 N1 C4 C5 1.7(3) . . . . ?
C1 N1 C4 C3 0.1(2) . . . . ?
Cu1 N1 C4 C3 -179.39(14) . . . . ?
C2 C3 C4 N1 0.1(3) . . . . ?
C2 C3 C4 C5 179.0(2) . . . . ?
N1 C4 C5 C12 -2.1(4) . . . . ?
C3 C4 C5 C12 179.2(2) . . . . ?
N1 C4 C5 C6 178.3(2) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C4 C5 C6 C7 77.1(3) . . . . ?
C12 C5 C6 C7 -102.5(3) . . . . ?
C4 C5 C6 C11 -105.1(3) . . . . ?
C12 C5 C6 C11 75.3(3) . . . . ?
C11 C6 C7 F1 -179.1(2) . . . . ?
C5 C6 C7 F1 -1.2(4) . . . . ?
C11 C6 C7 C8 -0.4(4) . . . . ?
C5 C6 C7 C8 177.5(2) . . . . ?
F1 C7 C8 F2 -1.3(4) . . . . ?
C6 C7 C8 F2 180.0(2) . . . . ?
F1 C7 C8 C9 178.2(2) . . . . ?
C6 C7 C8 C9 -0.6(4) . . . . ?
F2 C8 C9 F3 0.5(4) . . . . ?
C7 C8 C9 F3 -178.9(2) . . . . ?
F2 C8 C9 C10 -179.7(2) . . . . ?
C7 C8 C9 C10 0.9(4) . . . . ?
F3 C9 C10 F4 -1.2(4) . . . . ?
C8 C9 C10 F4 179.0(2) . . . . ?
F3 C9 C10 C11 179.6(2) . . . . ?
C8 C9 C10 C11 -0.2(4) . . . . ?
F4 C10 C11 F5 -0.3(4) . . . . ?
C9 C10 C11 F5 178.9(2) . . . . ?
F4 C10 C11 C6 179.9(2) . . . . ?
C9 C10 C11 C6 -0.9(4) . . . . ?
C7 C6 C11 F5 -178.6(2) . . . . ?
C5 C6 C11 F5 3.5(3) . . . . ?
C7 C6 C11 C10 1.1(3) . . . . ?
C5 C6 C11 C10 -176.8(2) . . . . ?
C15 N2 C12 C5 -180.0(2) 7_556 . . . ?
Cu1 N2 C12 C5 0.5(3) . . . . ?
C15 N2 C12 C13 -0.5(2) 7_556 . . . ?
Cu1 N2 C12 C13 179.95(14) . . . . ?
C4 C5 C12 N2 0.9(4) . . . . ?
C6 C5 C12 N2 -179.5(2) . . . . ?
C4 C5 C12 C13 -178.5(2) . . . . ?
C6 C5 C12 C13 1.1(3) . . . . ?
N2 C12 C13 C14 0.4(2) . . . . ?
C5 C12 C13 C14 179.8(2) . . . . ?
C12 C13 C14 C15 -0.1(2) . . . 7_556 ?
N1 C1 C16 C15 -1.2(4) . . . . ?
C2 C1 C16 C15 -179.9(2) . . . . ?
N1 C1 C16 C17 175.19(19) . . . . ?
C2 C1 C16 C17 -3.6(3) . . . . ?
N2 C15 C16 C1 1.5(3) 7_556 . . . ?
C14 C15 C16 C1 -179.5(2) 7_556 . . . ?
N2 C15 C16 C17 -174.9(2) 7_556 . . . ?
C14 C15 C16 C17 4.1(3) 7_556 . . . ?
C18 Si1 C47 C17 -126.9(12) . . . . ?
C19 Si1 C47 C17 -8.0(12) . . . . ?
C20 Si1 C47 C17 110.6(12) . . . . ?
