#------------------------------------------------------------------------------
#$Date: 2017-08-11 04:17:37 +0300 (Fri, 11 Aug 2017) $
#$Revision: 199709 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/05/7120536.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_7120536
loop_
_publ_author_name
'Zhang, Yixin'
'Tong, Peng'
'Yang, Dawei'
'Li, Jianzhe'
'Wang, Baomin'
'Qu, Jingping'
_publ_section_title
;
 Migratory Insertion and Hydrogenation of a Bridging Azide in
 Thiolate-Bridged Dicobalt Reaction Platform
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05092E
_journal_year                    2017
_chemical_formula_sum            'C48 H62 B Co2 N3 S2'
_chemical_formula_weight         873.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-23 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.675(3)
_cell_length_b                   17.641(5)
_cell_length_c                   26.834(7)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.31
_cell_volume                     4580(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25793
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.105
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5153
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0473
_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)+(0.0831P)²+3.8712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3183
_reflns_number_total             4128
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc05092e2.cif
_cod_data_source_block           1_CCDC2
_cod_database_code               7120536
_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.
;
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.920
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, 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
B1 B 0.5972(5) 0.2500 0.5000 0.0426(11) Uani 1 2 d S T P
Co1 Co 0.87317(5) -0.05165(2) 0.69135(2) 0.04076(18) Uani 1 1 d . . .
S1 S 1.03187(13) -0.07177(7) 0.7500 0.0515(3) Uani 1 2 d S T P
S2 S 0.76167(12) 0.01437(7) 0.7500 0.0481(3) Uani 1 2 d S T P
N1 N 0.7782(4) -0.14242(17) 0.70888(10) 0.0637(9) Uani 1 1 d . . .
H1A H 0.7531 -0.1681 0.6832 0.076 Uiso 1 1 calc R U .
N2 N 0.7427(6) -0.1745(3) 0.7500 0.0731(15) Uani 1 2 d S T P
C1 C 0.9328(4) 0.04137(14) 0.64910(9) 0.0712(12) Uani 1 1 d G . .
C2 C 0.8035(3) 0.01568(17) 0.63367(10) 0.0698(12) Uani 1 1 d G . .
C3 C 0.8182(3) -0.05882(17) 0.61721(9) 0.0638(11) Uani 1 1 d G . .
C4 C 0.9567(3) -0.07917(15) 0.62247(9) 0.0649(11) Uani 1 1 d G . .
C5 C 1.0275(3) -0.01725(18) 0.64218(9) 0.0675(11) Uani 1 1 d G . .
C6 C 0.9706(9) 0.1190(3) 0.6687(2) 0.160(4) Uani 1 1 d . . .
H6A H 1.0674 0.1204 0.6764 0.241 Uiso 1 1 calc R U .
H6B H 0.9501 0.1566 0.6439 0.241 Uiso 1 1 calc R U .
H6C H 0.9181 0.1294 0.6983 0.241 Uiso 1 1 calc R U .
C7 C 0.6755(7) 0.0631(5) 0.6307(2) 0.173(4) Uani 1 1 d . . .
H7A H 0.6000 0.0326 0.6191 0.259 Uiso 1 1 calc R U .
H7B H 0.6541 0.0828 0.6632 0.259 Uiso 1 1 calc R U .
H7C H 0.6904 0.1044 0.6081 0.259 Uiso 1 1 calc R U .
C8 C 0.7069(8) -0.1060(4) 0.59474(19) 0.173(4) Uani 1 1 d . . .
H8A H 0.6211 -0.0787 0.5957 0.260 Uiso 1 1 calc R U .
H8B H 0.7301 -0.1175 0.5608 0.260 Uiso 1 1 calc R U .
H8C H 0.6977 -0.1523 0.6133 0.260 Uiso 1 1 calc R U .
C9 C 1.0193(8) -0.1538(3) 0.60710(18) 0.141(3) Uani 1 1 d . . .
H9A H 0.9481 -0.1866 0.5947 0.211 Uiso 1 1 calc R U .
H9B H 1.0866 -0.1453 0.5814 0.211 Uiso 1 1 calc R U .
H9C H 1.0631 -0.1769 0.6354 0.211 Uiso 1 1 calc R U .
C10 C 1.1827(5) -0.0135(5) 0.6493(2) 0.144(3) Uani 1 1 d . . .
H10A H 1.2071 0.0347 0.6635 0.215 Uiso 1 1 calc R U .
H10B H 1.2115 -0.0533 0.6714 0.215 Uiso 1 1 calc R U .
H10C H 1.2277 -0.0194 0.6177 0.215 Uiso 1 1 calc R U .
C11 C 1.0778(8) -0.1725(4) 0.7500 0.089(2) Uani 1 2 d S T P
H11A H 1.0387 -0.1962 0.7210 0.107 Uiso 1 1 d R U .
C12 C 1.2282(10) -0.1855(6) 0.7500 0.166(5) Uani 1 2 d S T P
H12A H 1.2489 -0.2387 0.7500 0.249 Uiso 1 2 d R U P
H12B H 1.2670 -0.1624 0.7208 0.249 Uiso 1 1 d R U .
C13 C 0.5808(6) -0.0139(5) 0.7500 0.087(2) Uani 1 2 d S T P
H13A H 0.5628 -0.0442 0.7790 0.105 Uiso 1 1 d R U .
C14 C 0.4827(7) 0.0526(6) 0.7500 0.123(3) Uani 1 2 d S T P
H14A H 0.3876 0.0370 0.7500 0.184 Uiso 1 2 d R U P
H14B H 0.5010 0.0824 0.7792 0.184 Uiso 1 1 d R U .
C21 C 0.5062(3) 0.23780(17) 0.55050(12) 0.0455(7) Uani 1 1 d . . .
C22 C 0.3814(4) 0.1980(2) 0.55022(15) 0.0613(10) Uani 1 1 d . . .
H22A H 0.3435 0.1836 0.5198 0.074 Uiso 1 1 calc R U .
C23 C 0.3128(5) 0.1792(2) 0.59324(18) 0.0803(13) Uani 1 1 d . . .
H23A H 0.2300 0.1526 0.5913 0.096 Uiso 1 1 calc R U .
C24 C 0.3640(5) 0.1991(2) 0.63890(18) 0.0751(12) Uani 1 1 d . . .
H24A H 0.3172 0.1862 0.6680 0.090 Uiso 1 1 calc R U .
C25 C 0.4844(4) 0.2379(2) 0.64081(14) 0.0689(11) Uani 1 1 d . . .
H25A H 0.5206 0.2521 0.6715 0.083 Uiso 1 1 calc R U .
C26 C 0.5546(4) 0.2569(2) 0.59743(12) 0.0552(8) Uani 1 1 d . . .
H26A H 0.6374 0.2834 0.6000 0.066 Uiso 1 1 calc R U .
C31 C 0.6889(3) 0.17207(19) 0.49817(11) 0.0473(8) Uani 1 1 d . . .
C32 C 0.6338(4) 0.1063(2) 0.47910(14) 0.0580(9) Uani 1 1 d . . .
H32A H 0.5482 0.1087 0.4634 0.070 Uiso 1 1 calc R U .
C33 C 0.6996(5) 0.0366(2) 0.48211(16) 0.0741(12) Uani 1 1 d . . .
H33A H 0.6584 -0.0067 0.4690 0.089 Uiso 1 1 calc R U .
C34 C 0.8269(5) 0.0327(3) 0.50483(17) 0.0807(14) Uani 1 1 d . . .
H34A H 0.8730 -0.0134 0.5070 0.097 Uiso 1 1 calc R U .
C35 C 0.8848(4) 0.0962(3) 0.52399(15) 0.0725(12) Uani 1 1 d . . .
H35A H 0.9709 0.0934 0.5393 0.087 Uiso 1 1 calc R U .
C36 C 0.8183(4) 0.1648(2) 0.52103(13) 0.0599(9) Uani 1 1 d . . .
H36A H 0.8602 0.2075 0.5346 0.072 Uiso 1 1 calc R U .
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'
Co Co 0.3494 0.9721 '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
C21 B1 C21 114.6(4) . 4_556
C21 B1 C31 112.25(16) . 4_556
C21 B1 C31 101.93(15) 4_556 4_556
C21 B1 C31 101.93(15) . .
C21 B1 C31 112.24(16) 4_556 .
C31 B1 C31 114.4(4) 4_556 .
N1 Co1 C3 93.57(11) . .
N1 Co1 C2 120.75(14) . .
C3 Co1 C2 39.47(6) . .
N1 Co1 C4 102.18(12) . .
C3 Co1 C4 39.36(6) . .
C2 Co1 C4 66.03(8) . .
N1 Co1 C1 158.92(12) . .
C3 Co1 C1 66.02(8) . .
C2 Co1 C1 39.34(6) . .
C4 Co1 C1 65.81(8) . .
N1 Co1 C5 138.32(13) . .
C3 Co1 C5 65.89(8) . .
C2 Co1 C5 65.88(8) . .
C4 Co1 C5 39.17(5) . .
C1 Co1 C5 39.16(5) . .
N1 Co1 S1 91.38(10) . .
C3 Co1 S1 148.13(9) . .
C2 Co1 S1 147.86(10) . .
C4 Co1 S1 108.89(9) . .
C1 Co1 S1 108.67(10) . .
C5 Co1 S1 90.00(8) . .
N1 Co1 S2 91.80(10) . .
C3 Co1 S2 125.91(9) . .
C2 Co1 S2 94.05(8) . .
C4 Co1 S2 159.56(8) . .
C1 Co1 S2 96.13(9) . .
C5 Co1 S2 129.81(10) . .
S1 Co1 S2 85.31(4) . .
C11 S1 Co1 108.77(18) . 6_557
C11 S1 Co1 108.77(18) . .
Co1 S1 Co1 89.92(5) 6_557 .
C13 S2 Co1 108.74(18) . 6_557
C13 S2 Co1 108.74(18) . .
Co1 S2 Co1 89.51(5) 6_557 .
N2 N1 Co1 135.2(2) . .
N1 N2 N1 118.1(4) 6_557 .
C2 C1 C5 108.0 . .
C2 C1 C6 127.9(4) . .
C5 C1 C6 124.0(4) . .
C2 C1 Co1 69.86(10) . .
C5 C1 Co1 70.68(10) . .
C6 C1 Co1 126.4(3) . .
C1 C2 C3 108.0 . .
C1 C2 C7 125.2(5) . .
C3 C2 C7 126.5(5) . .
C1 C2 Co1 70.80(10) . .
C3 C2 Co1 70.23(10) . .
C7 C2 Co1 129.2(3) . .
C4 C3 C2 108.0 . .
C4 C3 C8 126.3(4) . .
C2 C3 C8 125.6(4) . .
C4 C3 Co1 70.77(10) . .
C2 C3 Co1 70.30(10) . .
C8 C3 Co1 127.7(2) . .
C5 C4 C3 108.0 . .
C5 C4 C9 126.2(4) . .
C3 C4 C9 125.7(4) . .
C5 C4 Co1 70.73(10) . .
C3 C4 Co1 69.87(10) . .
C9 C4 Co1 127.2(2) . .
C4 C5 C1 108.0 . .
C4 C5 C10 124.7(4) . .
C1 C5 C10 127.0(4) . .
C4 C5 Co1 70.11(10) . .
C1 C5 Co1 70.16(10) . .
C10 C5 Co1 130.0(2) . .
C12 C11 S1 113.0(7) . .
C14 C13 S2 113.1(6) . .
C26 C21 C22 114.8(3) . .
C26 C21 B1 122.8(3) . .
C22 C21 B1 121.9(3) . .
C23 C22 C21 122.3(4) . .
C22 C23 C24 121.1(4) . .
C25 C24 C23 118.4(4) . .
C24 C25 C26 120.8(4) . .
C21 C26 C25 122.6(4) . .
C32 C31 C36 115.6(3) . .
C32 C31 B1 120.7(3) . .
C36 C31 B1 123.3(3) . .
C31 C32 C33 123.3(4) . .
C34 C33 C32 118.7(4) . .
C35 C34 C33 119.8(4) . .
C34 C35 C36 120.8(4) . .
C35 C36 C31 121.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 C21 1.630(4) .
B1 C21 1.630(4) 4_556
B1 C31 1.637(4) 4_556
B1 C31 1.637(4) .
Co1 N1 1.905(3) .
Co1 C3 2.063(3) .
Co1 C2 2.064(3) .
Co1 C4 2.075(3) .
Co1 C1 2.076(3) .
Co1 C5 2.083(3) .
Co1 S1 2.2272(11) .
Co1 S2 2.2353(10) .
S1 C11 1.832(6) .
S1 Co1 2.2272(10) 6_557
S2 C13 1.820(6) .
S2 Co1 2.2353(10) 6_557
N1 N2 1.286(3) .
N2 N1 1.286(3) 6_557
C1 C2 1.3937(19) .
C1 C5 1.3938(18) .
C1 C6 1.513(5) .
C2 C3 1.3938(19) .
C2 C7 1.496(6) .
C3 C4 1.3937(19) .
C3 C8 1.489(5) .
C4 C5 1.3937(19) .
C4 C9 1.506(6) .
C5 C10 1.515(6) .
C11 C12 1.473(11) .
C13 C14 1.509(10) .
C21 C26 1.385(5) .
C21 C22 1.397(5) .
C22 C23 1.372(6) .
C23 C24 1.367(7) .
C24 C25 1.352(6) .
C25 C26 1.389(5) .
C31 C32 1.375(5) .
C31 C36 1.400(5) .
C32 C33 1.387(5) .
C33 C34 1.376(7) .
C34 C35 1.355(7) .
C35 C36 1.372(6) .
