4-Coordinated, 14-electron ruthenium(ii) chalcogenolate complexes: synthesis, electronic structure and reactions with PhICl<sub>2</sub> and organic azides.
Ng, Wai-Ming; Guo, Xueying; Cheung, Wai-Man; So, Yat-Ming; Chong, Man-Chun; Sung, Herman H.-Y.; Williams, Ian D.; Lin, Zhenyang; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13315–13325; doi:10.1039/c9dt02457c

data_7700849
_publ_section_title
;
 4-Coordinated, 14-electron ruthenium(ii) chalcogenolate complexes:
 synthesis, electronic structure and reactions with PhICl<sub>2</sub> and
 organic azides.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13315
_journal_page_last               13325
_journal_paper_doi               10.1039/c9dt02457c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C55 H68 N O2 P Ru S3'
_chemical_formula_sum            'C55 H68 N O2 P Ru S3'
_chemical_formula_weight         1003.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-07-24 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.128(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8430(4)
_cell_length_b                   13.9235(2)
_cell_length_c                   18.7630(4)
_cell_measurement_reflns_used    7380
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6350
_cell_measurement_theta_min      4.7530
_cell_volume                     5203.67(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   84.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000  -90.0000 90

  2 omega   47.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000 -180.0000 68

  3 omega   40.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -120.0000 51

  4 omega   38.00  129.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000    0.0000 91

  5 omega   37.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  150.0000 61

  6 omega   40.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   90.0000 48

  7 omega   38.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000   30.0000 77

  8 omega   36.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -15.0000  -90.0000 129

  9 omega   26.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  -60.0000 73

 10 omega  -49.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  150.0000 84

 11 omega  -70.00   -3.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   57.0000  -30.0000 67

 12 omega  -96.00   -2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  125.0000  150.0000 94

 13 omega -115.00  -11.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000    0.0000 104
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0643262000
_diffrn_orient_matrix_UB_12      -0.0384611000
_diffrn_orient_matrix_UB_13      -0.0145422000
_diffrn_orient_matrix_UB_21      0.0207194000
_diffrn_orient_matrix_UB_22      0.1033839000
_diffrn_orient_matrix_UB_23      -0.0125178000
_diffrn_orient_matrix_UB_31      0.0376280000
_diffrn_orient_matrix_UB_32      0.0086759000
_diffrn_orient_matrix_UB_33      0.0837331000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28996
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.874
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9259
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0491
_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/[\s^2^(Fo^2^)+(0.0360P)^2^+5.6200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7118
_reflns_number_total             9259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02457c2.cif
_cod_data_source_block           benson65cult
_cod_depositor_comments
'Adding full bibliography for 7700845--7700851.cif.'
_cod_original_cell_volume        5203.64(18)
_cod_database_code               7700849
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C62A-C61A \\sim C66A-C61A \\sim C66A-C65A \\sim C65A-C64A \\sim C64A-C63A
\\sim C63A-C62A
 with sigma of 0.02
 C52A-C51A \\sim C53A-C52A \\sim C54A-C53A \\sim C55A-C54A \\sim C56A-C55A
\\sim C56A-C51A
 with sigma of 0.02
3. Restrained planarity
 C51A, C52A, C53A, C54A, C55A, C56A
 with sigma of 0.1
4. Others
 Fixed Sof: P1(0.75) C51(0.7) C52(0.7) H52(0.7) C53(0.7) H53(0.7) C54(0.7)
 H54(0.7) C55(0.7) H55(0.7) C56(0.7) H56(0.7) C61(0.7) C62(0.7) H62(0.7)
 C62A(0.3) H62A(0.3) C63(0.7) H63(0.7) C63A(0.3) H63A(0.3) C64(0.7) H64(0.7)
 C64A(0.3) H64A(0.3) C65(0.7) H65(0.7) C65A(0.3) H65A(0.3) C66(0.7) H66(0.7)
 C66A(0.3) H66A(0.3) C61A(0.3) P1A(0.25) C51A(0.3) C52A(0.3) H52A(0.3)
 C53A(0.3) H53A(0.3) C54A(0.3) H54A(0.3) C55A(0.3) H55A(0.3) C56A(0.3) H56A(0.3)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C23(H23), C37(H37), C40(H40), C43(H43)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C13(H13), C15(H15), C33(H33), C35(H35),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C62A(H62A),
 C63(H63), C63A(H63A), C64(H64), C64A(H64A), C65(H65), C65A(H65A), C66(H66),
 C66A(H66A), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C52A(H52A),
 C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              49099
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-15
_olex2_submission_special_instructions 'No special instructions were received'