#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:40:16 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252761 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/40/7704003.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_7704003
loop_
_publ_author_name
'Guo, Jia-Ting'
'Chen, Xu-Dong'
_publ_section_title
;
 Templated syntheses of heterometal tungsten-cobalt-sulfur clusters with
 different nuclearities.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5523
_journal_page_last               5530
_journal_paper_doi               10.1039/d0dt00765j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C30 H44 B2 Co N12 S6 W2'
_chemical_formula_sum            'C30 H44 B2 Co N12 S6 W2'
_chemical_formula_weight         1213.38
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-16 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.248(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.154(10)
_cell_length_b                   16.190(14)
_cell_length_c                   12.030(11)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.320
_cell_measurement_theta_min      2.247
_cell_volume                     2115(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16332
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.146
_exptl_absorpt_coefficient_mu    6.150
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0441 before and 0.0358 after correction. The Ratio of minimum to maximum transmission is 0.9309. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       block
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0268P)²+0.9958P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3564
_reflns_number_total             4861
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00765j1.cif
_cod_data_source_block           mo_lan_0m
_cod_depositor_comments
'Adding full bibliography for 7704003--7704007.cif.'
_cod_database_code               7704003
_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_max   0.887
_shelx_estimated_absorpt_t_min   0.749
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1
 1.05 with sigma of 0.002
3.a Riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C1(H1A,H1B,
 H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
W1 W 0.63588(2) 0.52154(2) 0.35878(2) 0.03544(7) Uani 1 1 d . . . . .
Co1 Co 0.500000 0.500000 0.500000 0.0353(2) Uani 1 2 d S T P . .
S1 S 0.69870(11) 0.45425(8) 0.52548(12) 0.0416(3) Uani 1 1 d . . . . .
S2 S 0.56434(12) 0.63226(8) 0.43192(13) 0.0460(3) Uani 1 1 d . . . . .
S3 S 0.45466(11) 0.45468(8) 0.31209(12) 0.0443(3) Uani 1 1 d . . . . .
N4 N 0.8240(3) 0.5767(2) 0.3770(3) 0.0354(9) Uani 1 1 d . . . . .
N3 N 0.8839(3) 0.5767(2) 0.2888(3) 0.0360(9) Uani 1 1 d . . . . .
N6 N 0.6069(3) 0.5768(3) 0.1847(3) 0.0400(10) Uani 1 1 d . . . . .
N5 N 0.6982(4) 0.5763(3) 0.1249(4) 0.0419(10) Uani 1 1 d . . . . .
N2 N 0.7237(4) 0.4234(2) 0.2700(3) 0.0386(10) Uani 1 1 d . . . . .
N1 N 0.8008(4) 0.4440(3) 0.1996(4) 0.0410(10) Uani 1 1 d . . . . .
B1 B 0.8228(6) 0.5345(4) 0.1761(5) 0.0431(15) Uani 1 1 d D . . . .
H1 H 0.885559 0.540153 0.123466 0.052 Uiso 1 1 d DR . . . .
C12 C 0.9935(4) 0.6134(3) 0.3225(5) 0.0441(13) Uani 1 1 d . . . . .
C2 C 0.6564(5) 0.6136(4) 0.0219(4) 0.0494(14) Uani 1 1 d . . . . .
C9 C 0.7214(5) 0.3399(3) 0.2748(5) 0.0433(13) Uani 1 1 d . . . . .
C14 C 0.9004(4) 0.6141(3) 0.4659(5) 0.0440(13) Uani 1 1 d . . . . .
C11 C 1.0807(5) 0.6241(4) 0.2450(5) 0.0574(16) Uani 1 1 d . . . . .
H11A H 1.108095 0.570920 0.225734 0.086 Uiso 1 1 calc GR . . . .
H11B H 1.150378 0.656220 0.283168 0.086 Uiso 1 1 calc GR . . . .
H11C H 1.039236 0.652066 0.176553 0.086 Uiso 1 1 calc GR . . . .
C13 C 1.0058(4) 0.6383(3) 0.4330(5) 0.0465(14) Uani 1 1 d . . . . .
H13 H 1.072545 0.666341 0.477612 0.056 Uiso 1 1 calc R . . . .
C7 C 0.8436(5) 0.3735(4) 0.1613(5) 0.0507(14) Uani 1 1 d . . . . .
C15 C 0.8738(6) 0.6275(4) 0.5810(5) 0.0654(18) Uani 1 1 d . . . . .
H15A H 0.797087 0.656446 0.572579 0.098 Uiso 1 1 calc GR . . . .
H15B H 0.938757 0.659626 0.627475 0.098 Uiso 1 1 calc GR . . . .
H15C H 0.868458 0.575110 0.616910 0.098 Uiso 1 1 calc GR . . . .
C3 C 0.5380(6) 0.6379(4) 0.0160(5) 0.0619(17) Uani 1 1 d . . . . .
H3 H 0.486458 0.665057 -0.044681 0.074 Uiso 1 1 calc R . . . .
C10 C 0.6494(6) 0.2907(4) 0.3404(5) 0.0622(17) Uani 1 1 d . . . . .
H10A H 0.675529 0.304079 0.420058 0.093 Uiso 1 1 calc GR . . . .
H10B H 0.662637 0.232940 0.329678 0.093 Uiso 1 1 calc GR . . . .
H10C H 0.563465 0.303198 0.314082 0.093 Uiso 1 1 calc GR . . . .
C1 C 0.7367(6) 0.6258(4) -0.0608(5) 0.0668(18) Uani 1 1 d . . . . .
H1A H 0.811895 0.652384 -0.022853 0.100 Uiso 1 1 calc GR . . . .
H1B H 0.694573 0.659705 -0.123100 0.100 Uiso 1 1 calc GR . . . .
H1C H 0.755176 0.573160 -0.089622 0.100 Uiso 1 1 calc GR . . . .
C4 C 0.5091(5) 0.6143(4) 0.1173(5) 0.0530(15) Uani 1 1 d . . . . .
C8 C 0.7948(5) 0.3081(3) 0.2068(5) 0.0527(15) Uani 1 1 d . . . . .
H8 H 0.808215 0.252534 0.194433 0.063 Uiso 1 1 calc R . . . .
C5 C 0.3898(5) 0.6289(5) 0.1504(6) 0.076(2) Uani 1 1 d . . . . .
H5A H 0.347171 0.577401 0.150292 0.115 Uiso 1 1 calc GR . . . .
H5B H 0.339996 0.666040 0.096710 0.115 Uiso 1 1 calc GR . . . .
H5C H 0.405395 0.652755 0.225405 0.115 Uiso 1 1 calc GR . . . .
C6 C 0.9326(6) 0.3751(4) 0.0834(6) 0.078(2) Uani 1 1 d . . . . .
H6A H 0.898357 0.407495 0.016883 0.116 Uiso 1 1 calc GR . . . .
H6B H 0.946761 0.319766 0.060846 0.116 Uiso 1 1 calc GR . . . .
H6C H 1.009168 0.399098 0.123207 0.116 Uiso 1 1 calc GR . . . .
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'
Co Co 0.3494 0.9721 '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'
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
_geom_angle_publ_flag
S1 W1 N2 90.04(12) . . ?
S2 W1 S1 95.99(8) . . ?
S2 W1 S3 95.94(7) . . ?
S2 W1 N4 93.03(12) . . ?
S2 W1 N6 93.46(13) . . ?
S2 W1 N2 170.98(11) . . ?
S3 W1 S1 93.91(6) . . ?
S3 W1 N2 90.33(12) . . ?
N4 W1 S1 90.71(11) . . ?
N4 W1 S3 169.43(10) . . ?
N4 W1 N2 80.16(15) . . ?
N6 W1 S1 168.45(11) . . ?
N6 W1 S3 91.71(11) . . ?
N6 W1 N4 82.16(14) . . ?
N6 W1 N2 79.84(16) . . ?
Co1 Co1 W1 0(10) 3_666 3_666 ?
Co1 Co1 S1 0(10) 3_666 3_666 ?
Co1 Co1 S1 0(10) 3_666 . ?
Co1 Co1 S2 0(10) 3_666 3_666 ?
Co1 Co1 S2 0(10) 3_666 . ?
Co1 Co1 S3 0(10) 3_666 . ?
Co1 Co1 S3 0(10) 3_666 3_666 ?
S1 Co1 W1 55.10(5) 3_666 3_666 ?
S1 Co1 W1 124.90(5) . 3_666 ?
S1 Co1 S1 180.0 . 3_666 ?
S1 Co1 S2 91.21(6) . 3_666 ?
S1 Co1 S2 88.79(6) 3_666 3_666 ?
S1 Co1 S2 91.21(6) 3_666 . ?
S1 Co1 S2 88.79(6) . . ?
S1 Co1 S3 89.06(5) 3_666 . ?
S1 Co1 S3 89.06(5) . 3_666 ?
S1 Co1 S3 90.93(5) . . ?
S1 Co1 S3 90.94(5) 3_666 3_666 ?
S2 Co1 W1 127.26(4) . 3_666 ?
S2 Co1 W1 52.74(4) 3_666 3_666 ?
S2 Co1 S2 180.0 . 3_666 ?
S3 Co1 W1 54.78(5) 3_666 3_666 ?
S3 Co1 W1 125.22(5) . 3_666 ?
S3 Co1 S2 88.05(7) . . ?
S3 Co1 S2 91.95(7) . 3_666 ?
S3 Co1 S2 88.05(7) 3_666 3_666 ?
S3 Co1 S2 91.95(7) 3_666 . ?
S3 Co1 S3 180.00(3) . 3_666 ?
W1 S1 Co1 68.26(4) . 3_666 ?
W1 S1 Co1 68.26(4) . . ?
Co1 S1 Co1 0.0 3_666 . ?
W1 S2 Co1 65.69(7) . . ?
W1 S2 Co1 65.69(7) . 3_666 ?
Co1 S2 Co1 0.0 3_666 . ?
W1 S3 Co1 67.75(4) . 3_666 ?
W1 S3 Co1 67.75(4) . . ?
Co1 S3 Co1 0.0 3_666 . ?
N3 N4 W1 122.2(3) . . ?
C14 N4 W1 131.5(3) . . ?
C14 N4 N3 106.3(4) . . ?
N4 N3 B1 119.0(4) . . ?
C12 N3 N4 109.8(4) . . ?
C12 N3 B1 131.1(4) . . ?
N5 N6 W1 121.6(3) . . ?
C4 N6 W1 132.1(4) . . ?
C4 N6 N5 106.4(4) . . ?
N6 N5 B1 120.0(4) . . ?
C2 N5 N6 109.5(4) . . ?
C2 N5 B1 130.4(5) . . ?
N1 N2 W1 121.3(3) . . ?
C9 N2 W1 131.9(3) . . ?
C9 N2 N1 106.8(4) . . ?
N2 N1 B1 119.8(4) . . ?
C7 N1 N2 108.8(4) . . ?
C7 N1 B1 131.4(5) . . ?
N3 B1 N5 109.6(4) . . ?
N1 B1 N3 108.8(4) . . ?
N1 B1 N5 109.2(4) . . ?
N3 C12 C11 122.7(5) . . ?
N3 C12 C13 107.9(4) . . ?
C13 C12 C11 129.4(5) . . ?
N5 C2 C3 107.5(5) . . ?
N5 C2 C1 122.1(5) . . ?
C3 C2 C1 130.4(5) . . ?
N2 C9 C10 125.3(5) . . ?
N2 C9 C8 109.0(5) . . ?
C8 C9 C10 125.6(5) . . ?
N4 C14 C13 108.9(5) . . ?
N4 C14 C15 125.1(5) . . ?
C13 C14 C15 125.9(5) . . ?
C12 C13 C14 107.1(5) . . ?
N1 C7 C8 108.2(5) . . ?
N1 C7 C6 121.9(5) . . ?
C8 C7 C6 129.9(5) . . ?
C2 C3 C4 107.1(5) . . ?
N6 C4 C3 109.6(5) . . ?
N6 C4 C5 124.0(5) . . ?
C3 C4 C5 126.4(5) . . ?
C7 C8 C9 107.1(5) . . ?
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
W1 S1 2.248(2) . ?
W1 S2 2.2239(19) . ?
W1 S3 2.248(2) . ?
W1 N4 2.245(4) . ?
W1 N6 2.231(4) . ?
W1 N2 2.260(4) . ?
Co1 Co1 0.0000 3_666 ?
Co1 S1 2.290(2) . ?
Co1 S1 2.290(2) 3_666 ?
Co1 S2 2.458(2) . ?
Co1 S2 2.458(2) 3_666 ?
Co1 S3 2.320(2) . ?
Co1 S3 2.320(2) 3_666 ?
N4 N3 1.377(5) . ?
N4 C14 1.349(6) . ?
N3 B1 1.533(7) . ?
N3 C12 1.336(6) . ?
N6 N5 1.376(5) . ?
N6 C4 1.346(6) . ?
N5 B1 1.541(7) . ?
N5 C2 1.361(6) . ?
N2 N1 1.378(5) . ?
N2 C9 1.353(6) . ?
N1 B1 1.523(7) . ?
N1 C7 1.357(7) . ?
C12 C11 1.504(7) . ?
C12 C13 1.365(7) . ?
C2 C3 1.364(8) . ?
C2 C1 1.496(8) . ?
C9 C10 1.481(7) . ?
C9 C8 1.382(7) . ?
C14 C13 1.381(7) . ?
C14 C15 1.497(7) . ?
C7 C8 1.362(8) . ?
C7 C6 1.513(7) . ?
C3 C4 1.384(8) . ?
C4 C5 1.493(8) . ?
