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_7700847
_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         'C62 H75 N4 P Ru S2'
_chemical_formula_sum            'C62 H75 N4 P Ru S2'
_chemical_formula_weight         1072.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2018-07-24 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                96.126(3)
_cell_angle_beta                 93.546(3)
_cell_angle_gamma                100.986(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1803(5)
_cell_length_b                   14.8921(6)
_cell_length_c                   17.3023(7)
_cell_measurement_reflns_used    7185
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.0680
_cell_measurement_theta_min      5.1430
_cell_volume                     2801.9(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   55.00  141.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000    0.0000 86

  2 omega   15.00  117.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5703   37.0000  -60.0000 102

  3 omega   81.00  178.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000  -30.0000 97

  4 omega   54.00  172.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000   90.0000 118

  5 omega   45.00  107.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000   30.0000 62

  6 omega   36.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  -90.0000 62

  7 omega   32.00  115.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  -60.0000 83

  8 omega   32.00  115.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000 -180.0000 83

  9 omega   36.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  150.0000 62

 10 omega  -60.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5703   57.0000 -180.0000 93

 11 omega  -95.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5703  125.0000  -90.0000 92

 12 omega -107.00  -17.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5703  -57.0000   30.0000 90
;
_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      -0.0937787000
_diffrn_orient_matrix_UB_12      -0.0349994000
_diffrn_orient_matrix_UB_13      -0.0709350000
_diffrn_orient_matrix_UB_21      0.0732101000
_diffrn_orient_matrix_UB_22      0.0698240000
_diffrn_orient_matrix_UB_23      -0.0476602000
_diffrn_orient_matrix_UB_31      0.0754246000
_diffrn_orient_matrix_UB_32      -0.0718984000
_diffrn_orient_matrix_UB_33      -0.0278038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15645
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.988
_diffrn_reflns_theta_min         4.223
_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    3.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77763
_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            green
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.100
_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     645
_refine_ls_number_reflns         9872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8463
_reflns_number_total             9872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02457c2.cif
_cod_data_source_block           ng8cult
_cod_depositor_comments
'Adding full bibliography for 7700845--7700851.cif.'
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               7700847
_shelx_shelxl_version_number     2014/7
_cell_oxdiff_angle_alpha         96.126(3)
_cell_oxdiff_angle_beta          93.546(3)
_cell_oxdiff_angle_gamma         100.986(4)
_cell_oxdiff_length_a            11.1803(5)
_cell_oxdiff_length_b            14.8921(6)
_cell_oxdiff_length_c            17.3023(7)
_cell_oxdiff_measurement_reflns_used 7185
_cell_oxdiff_volume              2801.9(2)
_reflns_odcompleteness_completeness 98.68
_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.a Ternary CH refined with riding coordinates:
 C27(H27), C30(H30), C33(H33), C47(H47), C50(H50), C53(H53)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C23(H23), C25(H25), C43(H43), C45(H45), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              27579
_olex2_date_sample_data_collection 2016-01-22
_olex2_submission_special_instructions 'No special instructions were received'