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#$Date: 2022-08-06 14:38:00 +0300 (Sat, 06 Aug 2022) $
#$Revision: 277091 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/71/1567163.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_1567163
loop_
_publ_author_name
'Zafar, Mohammad'
'Ahmad, Asif'
'Saha, Suvam'
'Ramalakshmi, Rongala'
'Roisnel, Thierry'
'Ghosh, Sundargopal'
_publ_section_title
;
 Cooperative B--H bond activation: dual site borane activation by redox
 active κ2-N,S-chelated complexes
;
_journal_issue                   29
_journal_name_full               'Chemical Science'
_journal_page_first              8567
_journal_page_last               8575
_journal_paper_doi               10.1039/D2SC00907B
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C32 H34 B2 N2 Ru S4, C H2 Cl2'
_chemical_formula_sum            'C33 H36 B2 Cl2 N2 Ru S4'
_chemical_formula_weight         782.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-27 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                91.746(5)
_cell_angle_beta                 95.358(6)
_cell_angle_gamma                91.618(5)
_cell_formula_units_Z            1
_cell_length_a                   8.1421(16)
_cell_length_b                   9.0380(16)
_cell_length_c                   11.991(2)
_cell_measurement_reflns_used    9670
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      3.17
_cell_volume                     877.7(3)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31617
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.874
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.785
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.043(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0425P)²+2.0647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3049
_reflns_number_total             3426
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc00907b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1567161--1567164.cif.'
_cod_database_code               1567163
_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   0.881
_shelx_estimated_absorpt_t_max   0.958
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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
Ru1 Ru 0.500000 0.000000 0.000000 0.03569(19) Uani 1 2 d S . P . .
B1 B 0.4737(5) 0.1396(4) 0.1475(4) 0.0336(8) Uani 1 1 d . . . . .
C1 C 0.3709(4) 0.2849(4) 0.1538(3) 0.0341(8) Uani 1 1 d . . . . .
C2 C 0.1984(5) 0.2820(4) 0.1525(3) 0.0396(8) Uani 1 1 d . . . . .
C3 C 0.1144(5) 0.4140(5) 0.1472(4) 0.0477(10) Uani 1 1 d . . . . .
H3 H 0.000069 0.410459 0.146390 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1947(5) 0.5497(4) 0.1433(4) 0.0452(9) Uani 1 1 d . . . . .
C5 C 0.3644(5) 0.5527(4) 0.1466(3) 0.0423(9) Uani 1 1 d . . . . .
H5 H 0.420931 0.643373 0.144869 0.051 Uiso 1 1 calc R U . . .
C6 C 0.4534(4) 0.4236(4) 0.1525(3) 0.0351(8) Uani 1 1 d . . . . .
C7 C 0.6392(5) 0.4380(5) 0.1590(4) 0.0488(10) Uani 1 1 d . . . . .
H7A H 0.672261 0.540849 0.158798 0.073 Uiso 1 1 calc R U . . .
H7B H 0.677765 0.386969 0.095517 0.073 Uiso 1 1 calc R U . . .
H7C H 0.685895 0.395497 0.226700 0.073 Uiso 1 1 calc R U . . .
C8 C 0.0986(6) 0.1388(5) 0.1569(5) 0.0623(13) Uani 1 1 d . . . . .
H8A H -0.012266 0.160555 0.171607 0.093 Uiso 1 1 calc R U . . .
H8B H 0.147801 0.079844 0.215592 0.093 Uiso 1 1 calc R U . . .
H8C H 0.096930 0.085245 0.086458 0.093 Uiso 1 1 calc R U . . .
C9 C 0.0993(7) 0.6907(5) 0.1358(5) 0.0700(15) Uani 1 1 d . . . . .
H9A H 0.065977 0.717536 0.208182 0.105 Uiso 1 1 calc R U . . .
H9B H 0.003363 0.675412 0.083339 0.105 Uiso 1 1 calc R U . . .
H9C H 0.168099 0.768827 0.110957 0.105 Uiso 1 1 calc R U . . .
C10 C 0.5876(5) 0.1436(5) 0.3644(3) 0.0435(9) Uani 1 1 d . . . . .
C11 C 0.4966(6) 0.2557(5) 0.4081(4) 0.0542(11) Uani 1 1 d . . . . .
H11 H 0.420248 0.306004 0.362066 0.065 Uiso 1 1 calc R U . . .
C12 C 0.5224(7) 0.2908(6) 0.5217(4) 0.0677(14) Uani 1 1 d . . . . .
H12 H 0.463935 0.366823 0.551762 0.081 Uiso 1 1 calc R U . . .
C13 C 0.6337(8) 0.2147(7) 0.5916(4) 0.0764(16) Uani 1 1 d . . . . .
H13 H 0.647717 0.239372 0.667792 0.092 Uiso 1 1 calc R U . . .
C14 C 0.7231(7) 0.1036(7) 0.5492(4) 0.0732(15) Uani 1 1 d . . . . .
H14 H 0.797965 0.052482 0.595766 0.088 Uiso 1 1 calc R U . . .
C15 C 0.6995(5) 0.0691(6) 0.4354(4) 0.0537(11) Uani 1 1 d . . . . .
C16 C 0.6787(5) -0.0264(4) 0.2391(3) 0.0405(9) Uani 1 1 d . . . . .
S1 S 0.69006(12) -0.12118(10) 0.11846(9) 0.0424(3) Uani 1 1 d . . . . .
S2 S 0.79454(15) -0.06798(15) 0.36199(10) 0.0591(3) Uani 1 1 d . . . . .
N1 N 0.5789(4) 0.0878(3) 0.2519(3) 0.0366(7) Uani 1 1 d . . . . .
C17 C 0.049(4) 0.454(3) 0.5671(14) 0.193(10) Uani 0.5 1 d D U P . .
H18A H 0.155153 0.493403 0.600327 0.231 Uiso 0.5 1 calc R U P A .
H18B H -0.024507 0.417821 0.619976 0.231 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.0413(7) 0.3675(6) 0.4396(4) 0.247(2) Uani 1 1 d D U . A -1
H2 H 0.386(4) 0.022(4) 0.103(3) 0.030(9) Uiso 1 1 d . . . . .
H1 H 0.573(5) 0.149(4) 0.064(3) 0.032(9) Uiso 1 1 d . . . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 '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
B1 Ru1 B1 180.0(2) 2_655 . ?
B1 Ru1 S1 95.86(11) 2_655 . ?
B1 Ru1 S1 84.14(11) . . ?
B1 Ru1 S1 84.14(11) 2_655 2_655 ?
B1 Ru1 S1 95.86(11) . 2_655 ?
S1 Ru1 S1 180.0 . 2_655 ?
B1 Ru1 H2 142.3(13) 2_655 . ?
B1 Ru1 H2 37.7(13) . . ?
S1 Ru1 H2 89.5(13) . . ?
S1 Ru1 H2 90.5(13) 2_655 . ?
B1 Ru1 H1 141.9(13) 2_655 . ?
B1 Ru1 H1 38.1(13) . . ?
S1 Ru1 H1 85.6(13) . . ?
S1 Ru1 H1 94.4(13) 2_655 . ?
H2 Ru1 H1 75.6(18) . . ?
N1 B1 C1 120.5(3) . . ?
N1 B1 Ru1 112.2(2) . . ?
C1 B1 Ru1 127.2(3) . . ?
N1 B1 H2 107.3(16) . . ?
C1 B1 H2 113.8(16) . . ?
Ru1 B1 H2 48.1(16) . . ?
N1 B1 H1 107.3(16) . . ?
C1 B1 H1 109.7(16) . . ?
Ru1 B1 H1 47.3(16) . . ?
H2 B1 H1 95(2) . . ?
C2 C1 C6 117.9(3) . . ?
C2 C1 B1 122.8(3) . . ?
C6 C1 B1 119.1(3) . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 C8 118.2(4) . . ?
C1 C2 C8 122.0(4) . . ?
C4 C3 C2 122.4(4) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C3 C4 C5 117.9(4) . . ?
C3 C4 C9 121.0(4) . . ?
C5 C4 C9 121.2(4) . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 C7 117.9(3) . . ?
C1 C6 C7 121.7(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C10 C11 119.6(4) . . ?
C15 C10 N1 112.5(4) . . ?
C11 C10 N1 127.9(4) . . ?
C12 C11 C10 118.4(5) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C11 C12 C13 121.3(5) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 118.5(5) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C10 121.7(5) . . ?
C14 C15 S2 127.4(4) . . ?
C10 C15 S2 111.0(3) . . ?
N1 C16 S1 124.3(3) . . ?
N1 C16 S2 113.0(3) . . ?
S1 C16 S2 122.7(2) . . ?
C16 S1 Ru1 101.11(13) . . ?
C16 S2 C15 90.8(2) . . ?
C16 N1 C10 112.7(3) . . ?
C16 N1 B1 118.1(3) . . ?
C10 N1 B1 129.3(3) . . ?
Cl1 C17 C17 58.4(9) . 2_566 ?
Cl1 C17 H18A 117.9 . . ?
C17 C17 H18A 117.9 2_566 . ?
Cl1 C17 H18B 117.9 . . ?
C17 C17 H18B 117.9 2_566 . ?
H18A C17 H18B 115.1 . . ?
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
Ru1 B1 2.172(4) 2_655 ?
Ru1 B1 2.172(4) . ?
Ru1 S1 2.3221(10) . ?
Ru1 S1 2.3221(10) 2_655 ?
Ru1 H2 1.62(4) . ?
Ru1 H1 1.60(4) . ?
B1 N1 1.542(5) . ?
B1 C1 1.580(5) . ?
B1 H2 1.33(4) . ?
B1 H1 1.35(4) . ?
C1 C2 1.403(5) . ?
C1 C6 1.407(5) . ?
C2 C3 1.391(5) . ?
C2 C8 1.514(6) . ?
C3 C4 1.378(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(6) . ?
C4 C9 1.511(5) . ?
C5 C6 1.391(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.510(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C15 1.389(6) . ?
C10 C11 1.390(6) . ?
C10 N1 1.421(5) . ?
C11 C12 1.384(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(7) . ?
C14 H14 0.9300 . ?
C15 S2 1.739(5) . ?
C16 N1 1.345(5) . ?
C16 S1 1.670(4) . ?
C16 S2 1.731(4) . ?
C17 Cl1 1.692(16) . ?
C17 C17 1.95(5) 2_566 ?
C17 H18A 0.9700 . ?
C17 H18B 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 B1 C1 C2 -107.4(4) . . . . ?
Ru1 B1 C1 C2 76.6(5) . . . . ?
N1 B1 C1 C6 77.5(5) . . . . ?
Ru1 B1 C1 C6 -98.6(4) . . . . ?
C6 C1 C2 C3 1.5(6) . . . . ?
B1 C1 C2 C3 -173.7(4) . . . . ?
C6 C1 C2 C8 -178.3(4) . . . . ?
B1 C1 C2 C8 6.5(6) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C8 C2 C3 C4 179.8(4) . . . . ?
C2 C3 C4 C5 -1.1(6) . . . . ?
C2 C3 C4 C9 179.0(4) . . . . ?
C3 C4 C5 C6 0.7(6) . . . . ?
C9 C4 C5 C6 -179.4(4) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C4 C5 C6 C7 -178.3(4) . . . . ?
C2 C1 C6 C5 -1.9(6) . . . . ?
B1 C1 C6 C5 173.5(4) . . . . ?
C2 C1 C6 C7 177.2(4) . . . . ?
B1 C1 C6 C7 -7.4(5) . . . . ?
C15 C10 C11 C12 0.7(7) . . . . ?
N1 C10 C11 C12 178.6(4) . . . . ?
C10 C11 C12 C13 -1.2(8) . . . . ?
C11 C12 C13 C14 0.9(9) . . . . ?
C12 C13 C14 C15 -0.1(9) . . . . ?
C13 C14 C15 C10 -0.4(8) . . . . ?
C13 C14 C15 S2 -178.9(4) . . . . ?
C11 C10 C15 C14 0.1(7) . . . . ?
N1 C10 C15 C14 -178.1(4) . . . . ?
C11 C10 C15 S2 178.8(3) . . . . ?
N1 C10 C15 S2 0.6(5) . . . . ?
N1 C16 S1 Ru1 0.3(4) . . . . ?
S2 C16 S1 Ru1 179.5(2) . . . . ?
N1 C16 S2 C15 2.2(3) . . . . ?
S1 C16 S2 C15 -177.1(3) . . . . ?
C14 C15 S2 C16 177.1(5) . . . . ?
C10 C15 S2 C16 -1.6(4) . . . . ?
S1 C16 N1 C10 177.0(3) . . . . ?
S2 C16 N1 C10 -2.3(4) . . . . ?
S1 C16 N1 B1 -3.0(5) . . . . ?
S2 C16 N1 B1 177.8(3) . . . . ?
C15 C10 N1 C16 1.1(5) . . . . ?
C11 C10 N1 C16 -176.9(4) . . . . ?
C15 C10 N1 B1 -179.0(4) . . . . ?
C11 C10 N1 B1 3.0(7) . . . . ?
C1 B1 N1 C16 -172.4(3) . . . . ?
Ru1 B1 N1 C16 4.2(4) . . . . ?
C1 B1 N1 C10 7.6(6) . . . . ?
Ru1 B1 N1 C10 -175.8(3) . . . . ?
