#------------------------------------------------------------------------------
#$Date: 2017-06-05 03:09:04 +0300 (Mon, 05 Jun 2017) $
#$Revision: 197396 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/57/4345752.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_4345752
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_moiety
'3(C13 H19.67 B0.67 Cu2 N8 S2 W0.67), B F4 [+ solvent]'
_chemical_formula_sum            'C39 H59 B3 Cu6 F4 N24 S6 W2'
_chemical_formula_weight         1913.83
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-01-06 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.4912(3)
_cell_length_b                   11.4912(3)
_cell_length_c                   93.945(6)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.60
_cell_volume                     10743.2(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_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  0.0679
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       124
_diffrn_reflns_limit_l_min       -124
_diffrn_reflns_number            41259
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.293
_diffrn_reflns_theta_min         2.223
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.175
_exptl_absorpt_correction_T_max  0.460
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Sheldrick, G.M. SADABS (Program for Scaling and Correction of Area Detector
 Data), version 2008/1; University of Göttingen: Göttingen, Germany, 2008.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             5580
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.277
_refine_diff_density_min         -3.045
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0304
_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)+(0.0417P)²+106.0301P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2363
_reflns_number_total             2980
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00261_si_002.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 4345750--4345757.cif.'
_cod_original_cell_volume        10743.2(9)
_cod_database_code               4345752
_publcif_datablock.id            {249d1377-0271-4a0e-b198-ff5a0ce0d74d}
_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   0.424
_shelx_estimated_absorpt_t_max   0.511
_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 0.6667 0.3333 0.96369(2) 0.01540(9) Uani 1 3 d S T P . .
Cu1 Cu 0.70243(6) 0.49318(5) 0.94203(2) 0.02507(13) Uani 1 1 d . . . . .
S1 S 0.86832(11) 0.49009(11) 0.95341(2) 0.0229(2) Uani 1 1 d . . . . .
B1 B 0.6667 0.3333 0.99954(7) 0.0200(15) Uani 1 3 d DS T P . .
H1B1 H 0.6667 0.3333 1.0117(2) 0.024 Uiso 1 3 d DS U P . .
N1 N 0.7222(4) 0.6062(4) 0.92625(4) 0.0303(9) Uani 1 1 d . U . . .
N2 N 0.6253(5) 0.6312(5) 0.92243(5) 0.0482(12) Uani 1 1 d . U . . .
N3 N 0.7861(3) 0.3237(3) 0.99394(3) 0.0177(7) Uani 1 1 d . . . . .
N4 N 0.7954(3) 0.3021(4) 0.97963(3) 0.0197(7) Uani 1 1 d . . . . .
C1 C 0.8186(6) 0.6667 0.9167 0.054(2) Uani 1 2 d S TU P . .
C2 C 0.9710(11) 0.7131(13) 0.92069(11) 0.049(3) Uani 0.5 1 d . U P A -1
H2A H 0.9752 0.6317 0.9228 0.059 Uiso 0.5 1 calc R U P A -1
H2B H 1.0254 0.7534 0.9121 0.059 Uiso 0.5 1 calc R U P A -1
C3 C 1.0399(14) 0.8104(16) 0.93291(15) 0.078(5) Uani 0.5 1 d . U P A -1
H3A H 1.1312 0.8274 0.9339 0.117 Uiso 0.5 1 calc R U P A -1
H3B H 0.9909 0.7716 0.9417 0.117 Uiso 0.5 1 calc R U P A -1
H3C H 1.0417 0.8942 0.9310 0.117 Uiso 0.5 1 calc R U P A -1
C4 C 0.9009(5) 0.3347(5) 1.01691(4) 0.0294(10) Uani 1 1 d . . . . .
H4A H 0.9095 0.4205 1.0195 0.044 Uiso 1 1 calc R U . . .
H4B H 0.9814 0.3334 1.0198 0.044 Uiso 1 1 calc R U . . .
H4C H 0.8236 0.2630 1.0217 0.044 Uiso 1 1 calc R U . . .
C5 C 0.8828(4) 0.3153(4) 1.00129(4) 0.0205(8) Uani 1 1 d . . . . .
C6 C 0.9550(4) 0.2872(4) 0.99167(4) 0.0252(9) Uani 1 1 d . . . . .
H6 H 1.0285 0.2753 0.9937 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8995(4) 0.2796(5) 0.97837(4) 0.0248(9) Uani 1 1 d . . . . .
C8 C 0.9484(6) 0.2502(7) 0.96489(5) 0.0461(14) Uani 1 1 d . . . . .
H8A H 0.8735 0.1776 0.9599 0.069 Uiso 1 1 calc R U . . .
H8B H 1.0146 0.2240 0.9671 0.069 Uiso 1 1 calc R U . . .
H8C H 0.9891 0.3298 0.9589 0.069 Uiso 1 1 calc R U . . .
F1 F 0.0000 0.0000 1.0000 0.0537(13) Uani 1 6 d S TU P . .
B2 B 0.0000 0.0000 0.9863 0.0537(13) Uani 0.1667 1 d S U P B -1
F2 F -0.113(2) -0.009(2) 0.9812(2) 0.0537(13) Uani 0.1667 1 d . U P B -1
F3 F 0.1016 0.1248 0.9813 0.0537(13) Uani 0.1667 1 d . U P B -1
F4 F 0.0088 -0.1160 0.9814 0.0537(13) Uani 0.1667 1 d . U 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'
F F 0.0171 0.0103 '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'
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 80.76(12) 3_665 2_655
N4 W1 N4 80.76(12) 3_665 .
N4 W1 N4 80.76(12) 2_655 .
N4 W1 S1 163.01(9) 3_665 .
N4 W1 S1 87.34(10) 2_655 .
N4 W1 S1 85.41(10) . .
N4 W1 S1 85.41(9) 3_665 3_665
N4 W1 S1 163.01(9) 2_655 3_665
N4 W1 S1 87.34(9) . 3_665
S1 W1 S1 103.85(3) . 3_665
N4 W1 S1 87.34(9) 3_665 2_655
N4 W1 S1 85.41(9) 2_655 2_655
N4 W1 S1 163.01(8) . 2_655
S1 W1 S1 103.85(3) . 2_655
S1 W1 S1 103.85(3) 3_665 2_655
N4 W1 Cu1 137.56(9) 3_665 3_665
N4 W1 Cu1 139.67(10) 2_655 3_665
N4 W1 Cu1 92.22(8) . 3_665
S1 W1 Cu1 52.41(3) . 3_665
S1 W1 Cu1 52.33(3) 3_665 3_665
S1 W1 Cu1 104.73(3) 2_655 3_665
N4 W1 Cu1 92.22(8) 3_665 2_655
N4 W1 Cu1 137.56(9) 2_655 2_655
N4 W1 Cu1 139.68(9) . 2_655
S1 W1 Cu1 104.73(3) . 2_655
S1 W1 Cu1 52.42(3) 3_665 2_655
S1 W1 Cu1 52.33(3) 2_655 2_655
Cu1 W1 Cu1 66.64(2) 3_665 2_655
N4 W1 Cu1 139.67(9) 3_665 .
N4 W1 Cu1 92.22(8) 2_655 .
N4 W1 Cu1 137.56(10) . .
S1 W1 Cu1 52.33(3) . .
S1 W1 Cu1 104.73(3) 3_665 .
S1 W1 Cu1 52.41(3) 2_655 .
Cu1 W1 Cu1 66.64(2) 3_665 .
Cu1 W1 Cu1 66.64(2) 2_655 .
N1 Cu1 S1 125.36(13) . .
N1 Cu1 S1 121.80(13) . 2_655
S1 Cu1 S1 111.88(6) . 2_655
N1 Cu1 W1 178.15(13) . .
S1 Cu1 W1 56.47(3) . .
S1 Cu1 W1 56.44(3) 2_655 .
N1 Cu1 Cu1 124.08(12) . 3_665
S1 Cu1 Cu1 49.02(3) . 3_665
S1 Cu1 Cu1 99.86(3) 2_655 3_665
W1 Cu1 Cu1 56.678(10) . 3_665
N1 Cu1 Cu1 121.93(13) . 2_655
S1 Cu1 Cu1 99.94(4) . 2_655
S1 Cu1 Cu1 48.92(4) 2_655 2_655
W1 Cu1 Cu1 56.678(10) . 2_655
Cu1 Cu1 Cu1 60.001(1) 3_665 2_655
Cu1 S1 Cu1 82.06(5) . 3_665
Cu1 S1 W1 71.20(3) . .
Cu1 S1 W1 71.14(3) 3_665 .
N3 B1 N3 108.7(3) . 3_665
N3 B1 N3 108.7(3) . 2_655
N3 B1 N3 108.7(3) 3_665 2_655
N3 B1 H1B1 110.2(3) . .
N3 B1 H1B1 110.2(3) 3_665 .
N3 B1 H1B1 110.2(3) 2_655 .
C1 N1 N2 105.9(4) . .
C1 N1 Cu1 132.1(4) . .
N2 N1 Cu1 121.9(3) . .
N2 N2 N1 109.1(2) 11_566 .
C5 N3 N4 110.1(3) . .
C5 N3 B1 129.1(4) . .
N4 N3 B1 120.2(4) . .
C7 N4 N3 106.0(3) . .
C7 N4 W1 133.4(3) . .
N3 N4 W1 120.1(2) . .
N1 C1 N1 109.9(6) 11_566 .
N1 C1 C2 124.2(5) 11_566 .
N1 C1 C2 120.2(5) . .
C3 C2 C1 120.3(10) . .
C3 C2 H2A 107.2 . .
C1 C2 H2A 107.2 . .
C3 C2 H2B 107.2 . .
C1 C2 H2B 107.2 . .
H2A C2 H2B 106.9 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 H4A 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C5 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N3 C5 C6 107.3(3) . .
N3 C5 C4 123.5(4) . .
C6 C5 C4 129.2(4) . .
C5 C6 C7 107.2(4) . .
C5 C6 H6 126.4 . .
C7 C6 H6 126.4 . .
N4 C7 C6 109.4(4) . .
N4 C7 C8 126.1(4) . .
C6 C7 C8 124.5(4) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
F1 B2 F2 111.0(9) . .
F1 B2 F3 109.4 . .
F2 B2 F3 103.8(10) . .
F1 B2 F4 108.282(1) . .
F2 B2 F4 109.0(9) . .
F3 B2 F4 115.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N4 2.256(3) 3_665
W1 N4 2.256(3) 2_655
W1 N4 2.256(3) .
W1 S1 2.3183(11) .
W1 S1 2.3183(10) 3_665
W1 S1 2.3183(10) 2_655
W1 Cu1 2.6323(5) 3_665
W1 Cu1 2.6323(5) 2_655
W1 Cu1 2.6325(5) .
Cu1 N1 1.908(4) .
Cu1 S1 2.2012(12) .
Cu1 S1 2.2045(12) 2_655
Cu1 Cu1 2.8919(9) 3_665
Cu1 Cu1 2.8919(10) 2_655
S1 Cu1 2.2043(12) 3_665
B1 N3 1.524(4) .
B1 N3 1.524(4) 3_665
B1 N3 1.524(4) 2_655
B1 H1B1 1.15(2) .
N1 C1 1.323(6) .
N1 N2 1.331(6) .
N2 N2 1.293(8) 11_566
N3 C5 1.352(5) .
N3 N4 1.381(4) .
N4 C7 1.350(5) .
C1 N1 1.323(5) 11_566
C1 C2 1.601(13) .
C2 C3 1.519(18) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 H3C 0.9700 .
C4 C5 1.484(5) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 H4C 0.9700 .
C5 C6 1.370(6) .
C6 C7 1.386(6) .
C6 H6 0.9400 .
C7 C8 1.491(6) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
F1 B2 1.28709(12) .
B2 F2 1.34(2) .
B2 F3 1.40220(10) .
B2 F4 1.46070(10) .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{249d1377-0271-4a0e-b198-ff5a0ce0d74d} y y y
