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#$Date: 2021-12-13 12:47:14 +0200 (Mon, 13 Dec 2021) $
#$Revision: 271364 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/57/1565705.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_1565705
loop_
_publ_author_name
'Hua, Zi-Yi'
'Chen, Chen'
'Zhou, Fu-Hou'
'Zhang, Hao'
'Zhu, Zhao Qiang'
'Ge, Wei-Wei'
'Chen, Kai'
_publ_section_title
;
 Anion control in the complexation of cucurbit[6]uril with Cu(II) salts
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119183
_journal_paper_doi               10.1016/j.ica.2019.119183
_journal_volume                  499
_journal_year                    2020
_chemical_formula_sum            'C44 H48 Cu2 N32 O16 S8'
_chemical_formula_weight         1664.70
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.9523(12)
_cell_length_b                   14.9523(12)
_cell_length_c                   39.342(6)
_cell_measurement_reflns_used    9119
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.21
_cell_volume                     7617.3(14)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            33184
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.210
_exptl_absorpt_coefficient_mu    0.428
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.726
_exptl_crystal_description       lump
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+25.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2096
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1496
_reflns_number_total             2512
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-499-119183.cif
_cod_data_source_block           1
_cod_original_cell_volume        7617.3(17)
_cod_database_code               1565705
_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_min   0.927
_shelx_estimated_absorpt_t_max   0.963
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'
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
O1 O -0.0020(3) 0.2322(3) 0.07682(11) 0.0810(12) Uani 1 1 d . . . . .
N1 N 0.0837(3) 0.3294(3) 0.03062(12) 0.0634(12) Uani 1 1 d . . . . .
N2 N -0.0873(3) 0.2481(3) 0.03084(12) 0.0630(12) Uani 1 1 d . . . . .
C1 C 0.1860(3) 0.3719(6) 0.0450(2) 0.067(2) Uani 1 2 d S T P . .
H1A H 0.179699 0.359399 0.069307 0.081 Uiso 1 2 calc R U P . .
H1B H 0.223051 0.446100 0.041549 0.081 Uiso 1 2 calc R U P . .
C2 C -0.1908(3) 0.1908(3) 0.0446(2) 0.072(2) Uani 1 2 d S T P . .
H2A H -0.186917 0.186925 0.069105 0.087 Uiso 1 2 calc R U P . .
H2B H -0.227498 0.227493 0.039516 0.087 Uiso 1 2 calc R U P . .
C3 C -0.0016(5) 0.2656(4) 0.04896(16) 0.0644(14) Uani 1 1 d . . . . .
C4 C 0.0598(3) 0.3656(4) 0.00080(15) 0.0610(14) Uani 1 1 d . . . . .
H4A H 0.087235 0.440327 0.001725 0.073 Uiso 1 1 calc R U . . .
Cu1 Cu 0.666667 0.333333 0.07637(7) 0.1091(9) Uani 1 6 d S T P . .
S1 S 0.48284(10) 0.51716(10) 0.06541(7) 0.0885(8) Uani 1 2 d S T P . .
S2 S 0.666667 0.333333 -0.04372(16) 0.1093(18) Uani 1 6 d S T P . .
O1W O 0.666667 0.333333 0.1248(4) 0.173(6) Uani 1 6 d S T P . .
H1WA H 0.697610 0.302390 0.132044 0.260 Uiso 0.3333 2 d R U P . .
H4WB H 0.697610 0.395220 0.132044 0.260 Uiso 0.3333 2 d R U P . .
H4WC H 0.604780 0.302390 0.132044 0.260 Uiso 0.3333 2 d R U P . .
N3 N 0.5888(3) 0.4112(3) 0.0766(3) 0.109(3) Uani 1 2 d S T P . .
N4 N 0.666667 0.333333 0.0274(5) 0.096(5) Uani 1 6 d S T P . .
C7 C 0.5445(4) 0.4555(4) 0.0724(3) 0.081(3) Uani 1 2 d S T P . .
C8 C 0.666667 0.333333 -0.0019(5) 0.068(4) Uani 1 6 d S T P . .
O2W O 0.064370 0.128740 0.097240 0.158 Uani 0.3333 2 d S T P . .
H2WA H 0.040380 0.166090 0.089980 0.190 Uiso 0.1667 1 d R U P . .
H2WB H 0.035130 0.070260 0.086900 0.237 Uiso 0.3333 2 d R U P . .
H2WC H 0.129050 0.159160 0.093630 0.237 Uiso 0.1667 1 d R U P . .
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'
S S 0.1246 0.1234 '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
C3 N1 C4 112.5(5) . .
C3 N1 C1 121.1(6) . .
C4 N1 C1 124.9(5) . .
C3 N2 C2 122.6(6) . .
C3 N2 C4 111.8(5) . 12
C2 N2 C4 125.0(5) . 12
N1 C1 N1 113.8(6) . 20
N1 C1 H1A 108.8 . .
N1 C1 H1A 108.8 20 .
N1 C1 H1B 108.8 . .
N1 C1 H1B 108.8 20 .
H1A C1 H1B 107.7 . .
N2 C2 N2 112.3(6) 22 .
N2 C2 H2A 109.2 22 .
N2 C2 H2A 109.2 . .
N2 C2 H2B 109.2 22 .
N2 C2 H2B 109.2 . .
H2A C2 H2B 107.9 . .
O1 C3 N2 125.7(6) . .
O1 C3 N1 125.7(6) . .
N2 C3 N1 108.5(5) . .
N1 C4 N2 115.4(4) . 12
N1 C4 C4 104.7(5) . 12
N2 C4 C4 102.2(5) 12 12
N1 C4 H4A 111.3 . .
N2 C4 H4A 111.3 12 .
C4 C4 H4A 111.3 12 .
O1W Cu1 N4 180.0 . .
O1W Cu1 N3 89.8(3) . 5_665
N4 Cu1 N3 90.2(3) . 5_665
O1W Cu1 N3 89.8(3) . 3_655
N4 Cu1 N3 90.2(3) . 3_655
N3 Cu1 N3 119.995(5) 5_665 3_655
O1W Cu1 N3 89.8(3) . .
N4 Cu1 N3 90.2(3) . .
N3 Cu1 N3 120.000(5) 5_665 .
N3 Cu1 N3 120.000(5) 3_655 .
Cu1 O1W H1WA 109.5 . .
Cu1 O1W H4WB 109.5 . .
H1WA O1W H4WB 109.5 . .
Cu1 O1W H4WC 109.5 . .
H1WA O1W H4WC 109.5 . .
H4WB O1W H4WC 109.5 . .
C7 N3 Cu1 171.6(10) . .
C8 N4 Cu1 180.0 . .
N3 C7 S1 178.4(11) . .
N4 C8 S2 180.0 . .
H2WA O2W H2WB 110.0 . .
H2WA O2W H2WC 109.5 . .
H2WB O2W H2WC 109.2 . .
H2WA O2W H2WA 97.3 . 20
H2WB O2W H2WA 110.0 . 20
H2WC O2W H2WA 13.3 . 20
H2WA O2W H2WC 13.3 . 20
H2WB O2W H2WC 109.2 . 20
H2WC O2W H2WC 121.0 . 20
H2WA O2W H2WC 109.5 20 20
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C3 1.203(6) .
N1 C3 1.357(7) .
N1 C4 1.411(7) .
N1 C1 1.445(6) .
N2 C3 1.373(7) .
N2 C2 1.448(6) .
N2 C4 1.452(7) 12
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C4 C4 1.549(9) 12
C4 H4A 0.9800 .
Cu1 O1W 1.907(15) .
Cu1 N4 1.928(19) .
Cu1 N3 2.017(9) 5_665
Cu1 N3 2.017(9) 3_655
Cu1 N3 2.017(9) .
S1 C7 1.621(11) .
S2 C8 1.646(18) .
O1W H1WA 0.8500 .
O1W H4WB 0.8500 .
O1W H4WC 0.8500 .
N3 C7 1.158(11) .
N4 C8 1.151(19) .
O2W H2WA 0.8500 .
O2W H2WB 0.8596 .
O2W H2WC 0.8500 .
O2W H2WA 1(10) 20
O2W H2WC 1(10) 20
