#------------------------------------------------------------------------------
#$Date: 2017-06-05 03:09:04 +0300 (Mon, 05 Jun 2017) $
#$Revision: 197396 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/57/4345755.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_4345755
loop_
_publ_author_name
'Chen, Qiu-Fang'
'Zhao, Xin'
'Liu, Quan'
'Jia, Ji-Dong'
'Qiu, Xiao-Ting'
'Song, Ying-Lin'
'Young, David James'
'Zhang, Wen-Hua'
'Lang, Jian-Ping'
_publ_section_title
;
 Tungsten(VI)-Copper(I)-Sulfur Cluster-Supported Metal-Organic Frameworks
 Bridged by in Situ Click-Formed Tetrazolate Ligands.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5669
_journal_page_last               5679
_journal_paper_doi               10.1021/acs.inorgchem.7b00261
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C16 H14 B Cu2 F1.33 N8 S2 W0.67'
_chemical_formula_weight         668.26
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-09-19 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   11.6295(6)
_cell_length_b                   11.6295(6)
_cell_length_c                   93.185(8)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.62
_cell_volume                     10914.4(12)
_computing_cell_refinement       'Bruker D8 Quest'
_computing_data_collection       'Bruker D8 Quest'
_computing_data_reduction        'Bruker D8 Quest'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       123
_diffrn_reflns_limit_l_min       -123
_diffrn_reflns_number            96444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.356
_diffrn_reflns_theta_min         2.203
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.099
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       block
_exptl_crystal_F_000             5802
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3040
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0426P)²+257.2428P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2715
_reflns_number_total             3040
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00261_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4345750--4345757.cif.'
_cod_original_cell_volume        10914.4(14)
_cod_database_code               4345755
_publcif_datablock.id            {6d635718-bda5-42da-a32e-23b672173dce}
_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   0.429
_shelx_estimated_absorpt_t_max   0.630
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
W1 W 0.0000 1.0000 0.13058(2) 0.01809(11) Uani 1 3 d S T P . .
Cu1 Cu 0.03953(8) 0.88045(8) 0.10877(2) 0.02980(18) Uani 1 1 d . . . . .
S1 S 0.20058(14) 1.04905(15) 0.12017(2) 0.0265(3) Uani 1 1 d . . . . .
N3 N 0.0116(4) 0.8831(4) 0.16099(4) 0.0211(8) Uani 1 1 d . . . . .
N4 N 0.0313(5) 0.8738(4) 0.14665(4) 0.0218(8) Uani 1 1 d . . . . .
N1 N 0.0634(6) 0.7940(6) 0.09267(6) 0.0429(14) Uani 1 1 d . . . . .
N2 N -0.0310(9) 0.6733(8) 0.08892(10) 0.106(4) Uani 1 1 d . . . . .
C7 C 0.0014(7) 0.7703(7) 0.18412(6) 0.0361(14) Uani 1 1 d . . . . .
H7A H 0.0711 0.8484 0.1889 0.054 Uiso 1 1 calc R U . . .
H7B H 0.0061 0.6927 0.1870 0.054 Uiso 1 1 calc R U . . .
H7C H -0.0843 0.7589 0.1868 0.054 Uiso 1 1 calc R U . . .
C8 C 0.0190(5) 0.7872(5) 0.16826(6) 0.0241(10) Uani 1 1 d . . . . .
C9 C 0.0457(6) 0.7148(6) 0.15864(6) 0.0275(11) Uani 1 1 d . . . . .
H9 H 0.0568 0.6418 0.1607 0.033 Uiso 1 1 calc R U . . .
C10 C 0.0530(6) 0.7704(6) 0.14533(6) 0.0276(11) Uani 1 1 d . . . . .
C11 C 0.0822(9) 0.7213(7) 0.13182(7) 0.0450(17) Uani 1 1 d . . . . .
H11A H 0.0025 0.6774 0.1260 0.067 Uiso 1 1 calc R U . . .
H11B H 0.1118 0.6590 0.1341 0.067 Uiso 1 1 calc R U . . .
H11C H 0.1513 0.7957 0.1265 0.067 Uiso 1 1 calc R U . . .
B1 B 0.0000 1.0000 0.16666(10) 0.0219(19) Uani 1 3 d S T P . .
C1 C 0.1591(9) 0.8258(9) 0.0833 0.045(2) Uani 1 2 d DS T P . .
C2 C 0.2896(15) 0.9562(15) 0.0833 0.175(7) Uani 1 2 d DS T P A .
C3 C 0.190(4) 0.947(4) 0.0721(5) 0.175(7) Uani 0.25 1 d D U P A 1
C4 C 0.238(3) 1.067(5) 0.0626(5) 0.175(7) Uani 0.25 1 d D U P A 1
C5 C 0.125(3) 1.085(5) 0.0570(5) 0.175(7) Uani 0.25 1 d D U P A 1
C6 C 0.0000 1.0000 0.0649(5) 0.175(7) Uani 0.75 3 d DS TU P A 1
C3A C 0.327(4) 1.057(4) 0.0708(4) 0.175(7) Uani 0.25 1 d D U P A 2
C4A C 0.476(4) 1.165(4) 0.0711(4) 0.175(7) Uani 0.25 1 d D U P A 2
C5A C 0.517(2) 1.256(5) 0.0579(5) 0.175(7) Uani 0.25 1 d D U P A 2
C6A C 0.6667 1.3333 0.0557(4) 0.175(7) Uani 0.75 3 d DS TU P A 2
B2 B 0.338(3) 0.672(3) 0.1538(2) 0.037(3) Uani 0.1667 1 d D . P B -1
F1 F 0.342(4) 0.785(5) 0.1479(7) 0.037(3) Uani 0.1667 1 d D . P B -1
F2 F 0.365(3) 0.697(5) 0.1684(3) 0.037(3) Uani 0.1667 1 d D . P B -1
F3 F 0.212(3) 0.564(4) 0.1510(6) 0.037(3) Uani 0.1667 1 d D . P B -1
F4 F 0.431(4) 0.643(5) 0.1480(7) 0.037(3) Uani 0.1667 1 d D . P B -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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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'
W W -0.8490 6.8722 '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'
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
N4 W1 N4 80.56(16) 2_675 3_465
N4 W1 N4 80.56(16) 2_675 .
N4 W1 N4 80.56(16) 3_465 .
N4 W1 S1 84.92(12) 2_675 .
N4 W1 S1 162.87(11) 3_465 .
N4 W1 S1 88.15(12) . .
N4 W1 S1 88.16(12) 2_675 2_675
N4 W1 S1 84.93(12) 3_465 2_675
N4 W1 S1 162.88(11) . 2_675
S1 W1 S1 103.74(4) . 2_675
N4 W1 S1 162.88(12) 2_675 3_465
N4 W1 S1 88.16(12) 3_465 3_465
N4 W1 S1 84.93(12) . 3_465
S1 W1 S1 103.74(4) . 3_465
S1 W1 S1 103.73(4) 2_675 3_465
N4 W1 Cu1 136.84(12) 2_675 .
N4 W1 Cu1 140.55(12) 3_465 .
N4 W1 Cu1 92.37(11) . .
S1 W1 Cu1 52.15(4) . .
S1 W1 Cu1 104.64(4) 2_675 .
S1 W1 Cu1 52.45(4) 3_465 .
N4 W1 Cu1 140.55(12) 2_675 3_465
N4 W1 Cu1 92.37(11) 3_465 3_465
N4 W1 Cu1 136.84(12) . 3_465
S1 W1 Cu1 104.65(4) . 3_465
S1 W1 Cu1 52.45(4) 2_675 3_465
S1 W1 Cu1 52.15(4) 3_465 3_465
Cu1 W1 Cu1 66.65(3) . 3_465
N4 W1 Cu1 92.37(11) 2_675 2_675
N4 W1 Cu1 136.84(12) 3_465 2_675
N4 W1 Cu1 140.55(12) . 2_675
S1 W1 Cu1 52.46(4) . 2_675
S1 W1 Cu1 52.15(4) 2_675 2_675
S1 W1 Cu1 104.64(4) 3_465 2_675
Cu1 W1 Cu1 66.65(3) . 2_675
Cu1 W1 Cu1 66.65(3) 3_465 2_675
N1 Cu1 S1 124.75(19) . .
N1 Cu1 S1 122.43(19) . 3_465
S1 Cu1 S1 112.09(7) . 3_465
N1 Cu1 W1 178.1(2) . .
S1 Cu1 W1 56.60(4) . .
S1 Cu1 W1 56.50(4) 3_465 .
N1 Cu1 Cu1 121.4(2) . 3_465
S1 Cu1 Cu1 100.07(4) . 3_465
S1 Cu1 Cu1 48.75(5) 3_465 3_465
W1 Cu1 Cu1 56.677(14) . 3_465
N1 Cu1 Cu1 122.86(19) . 2_675
S1 Cu1 Cu1 49.10(5) . 2_675
S1 Cu1 Cu1 99.79(4) 3_465 2_675
W1 Cu1 Cu1 56.677(14) . 2_675
Cu1 Cu1 Cu1 60.0 3_465 2_675
Cu1 S1 Cu1 82.15(6) . 2_675
Cu1 S1 W1 71.24(5) . .
Cu1 S1 W1 71.05(5) 2_675 .
C8 N3 N4 110.1(4) . .
C8 N3 B1 129.5(5) . .
N4 N3 B1 120.1(5) . .
C10 N4 N3 105.8(4) . .
C10 N4 W1 133.1(3) . .
N3 N4 W1 120.6(3) . .
C1 N1 N2 105.1(6) . .
C1 N1 Cu1 134.5(5) . .
N2 N1 Cu1 120.4(4) . .
N2 N2 N1 109.3(4) 16_454 .
C8 C7 H7A 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C8 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N3 C8 C9 108.0(5) . .
N3 C8 C7 123.2(5) . .
C9 C8 C7 128.8(5) . .
C8 C9 C10 106.3(5) . .
C8 C9 H9 126.9 . .
C10 C9 H9 126.9 . .
N4 C10 C9 109.9(5) . .
N4 C10 C11 126.6(5) . .
C9 C10 C11 123.5(5) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N3 B1 N3 108.7(4) 3_465 2_675
N3 B1 N3 108.7(4) 3_465 .
N3 B1 N3 108.7(4) 2_675 .
N1 C1 N1 111.2(9) 16_454 .
N1 C1 C2 124.4(4) 16_454 .
N1 C1 C2 124.4(4) . .
N1 C1 C3 117.0(19) 16_454 16_454
N1 C1 C3 98.8(17) . 16_454
C2 C1 C3 57.5(11) . 16_454
N1 C1 C3 98.8(17) 16_454 .
N1 C1 C3 117.0(19) . .
C2 C1 C3 57.5(11) . .
C3 C1 C3 115(2) 16_454 .
C1 C2 C3 65.7(17) . 16_454
C1 C2 C3 65.7(17) . .
C3 C2 C3 131(3) 16_454 .
C1 C2 C3A 121.1(15) . .
C1 C2 C3A 121.1(15) . 16_454
C3A C2 C3A 118(3) . 16_454
C4 C3 C2 115(3) . .
C4 C3 C1 172(2) . .
C2 C3 C1 56.8(11) . .
C3 C4 C5 112.5(19) . .
C6 C5 C4 111.3(18) . .
C5 C6 C5 97(3) . 3_465
C5 C6 C5 97(3) . 2_675
C5 C6 C5 97(3) 3_465 2_675
C4A C3A C2 112(2) . .
C5A C4A C3A 112(2) . .
C6A C5A C4A 112(2) . .
C5A C6A C5A 118.3(11) 2_775 3_575
C5A C6A C5A 118.3(11) 2_775 .
C5A C6A C5A 118.3(11) 3_575 .
F2 B2 F3 113(3) . .
F2 B2 F4 108(3) . .
F3 B2 F4 107(3) . .
F2 B2 F1 107(3) . .
F3 B2 F1 108(3) . .
F4 B2 F1 114(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N4 2.250(4) 2_675
W1 N4 2.250(4) 3_465
W1 N4 2.250(4) .
W1 S1 2.3187(13) .
W1 S1 2.3188(13) 2_675
W1 S1 2.3188(14) 3_465
W1 Cu1 2.6299(7) .
W1 Cu1 2.6300(7) 3_465
W1 Cu1 2.6300(7) 2_675
Cu1 N1 1.902(5) .
Cu1 S1 2.1931(16) .
Cu1 S1 2.2046(16) 3_465
Cu1 Cu1 2.8898(13) 3_465
Cu1 Cu1 2.8898(13) 2_675
S1 Cu1 2.2049(16) 2_675
N3 C8 1.344(7) .
N3 N4 1.370(6) .
N3 B1 1.526(5) .
N4 C10 1.352(7) .
N1 C1 1.312(8) .
N1 N2 1.325(9) .
N2 N2 1.289(12) 16_454
C7 C8 1.491(7) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 H7C 0.9700 .
C8 C9 1.368(8) .
C9 C10 1.381(7) .
C9 H9 0.9400 .
C10 C11 1.490(8) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 H11C 0.9700 .
B1 N3 1.526(5) 3_465
B1 N3 1.526(6) 2_675
C1 N1 1.312(8) 16_454
C1 C2 1.517(16) .
C1 C3 1.65(3) 16_454
C1 C3 1.65(3) .
C2 C3 1.530(19) 16_454
C2 C3 1.530(19) .
C2 C3A 1.56(2) .
C2 C3A 1.56(2) 16_454
C3 C4 1.50(2) .
C4 C5 1.522(19) .
C5 C6 1.481(19) .
C6 C5 1.481(19) 3_465
C6 C5 1.481(19) 2_675
C3A C4A 1.55(2) .
C4A C5A 1.54(2) .
C5A C6A 1.522(19) .
C6A C5A 1.52(2) 2_775
C6A C5A 1.522(19) 3_575
B2 F2 1.397(12) .
B2 F3 1.397(12) .
B2 F4 1.397(12) .
B2 F1 1.397(12) .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{6d635718-bda5-42da-a32e-23b672173dce} y y y
