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_7700846
_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 O4 P Ru S4, 0.25(C6 H14), 0.5(C4 H10 O)'
_chemical_formula_sum            'C65.5 H83.5 N4 O4.5 P Ru S4'
_chemical_formula_weight         1259.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-07-24 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1209(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.57442(18)
_cell_length_b                   42.0951(6)
_cell_length_c                   13.6150(3)
_cell_measurement_reflns_used    15539
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      29.4340
_cell_measurement_theta_min      3.6180
_cell_volume                     6567.1(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -48.00   46.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7012  -37.0000 -120.0000 188

  2 omega  -17.00   85.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7012   77.0000  150.0000 204

  3 omega   -1.00   89.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7012   37.0000   60.0000 180
;
_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      -0.0032719000
_diffrn_orient_matrix_UB_12      0.0123415000
_diffrn_orient_matrix_UB_13      -0.0357235000
_diffrn_orient_matrix_UB_21      0.0089044000
_diffrn_orient_matrix_UB_22      -0.0112408000
_diffrn_orient_matrix_UB_23      -0.0370275000
_diffrn_orient_matrix_UB_31      -0.0611896000
_diffrn_orient_matrix_UB_32      -0.0022796000
_diffrn_orient_matrix_UB_33      -0.0110003000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39783
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.283
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72802
_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    1.274
_exptl_crystal_F_000             2654
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 7662 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(14)
_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     1500
_refine_ls_number_reflns         23188
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+2.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.818
_reflns_Friedel_fraction_max     0.799
_reflns_number_gt                20706
_reflns_number_total             23188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02457c2.cif
_cod_data_source_block           ng17molt
_cod_depositor_comments
'Adding full bibliography for 7700845--7700851.cif.'
_cod_original_cell_volume        6567.0(2)
_cod_original_formula_sum        'C65.50 H83.50 N4 O4.50 P Ru S4'
_cod_database_code               7700846
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6S) \\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(C3S)
\\sim Ueq, Uanis(C2S) \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
4.a Ternary CH refined with riding coordinates:
 C27(H27), C30(H30), C33(H33), C47(H47), C50(H50), C53(H53), C27A(H27A),
 C30A(H30A), C33A(H33A), C47A(H47A), C50A(H50A), C53A(H53A)
4.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C12S(H12B,
 H12C), C14S(H14A,H14B)
4.c 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), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A),
  C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A), C23A(H23A), C25A(H25A),
 C43A(H43A), C45A(H45A), C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A),
 C66A(H66A), C72A(H72A), C73A(H73A), C74A(H74A), C75A(H75A), C76A(H76A),
 C82A(H82A), C83A(H83A), C84A(H84A), C85A(H85A), C86A(H86A)
4.d 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), C7A(H7AA,H7AB,
 H7AC), C17A(H17D,H17E,H17F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F),
 C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C34A(H34D,H34E,H34F), C35A(H35D,
 H35E,H35F), C48A(H48D,H48E,H48F), C49A(H49D,H49E,H49F), C51A(H51D,H51E,H51F),
 C52A(H52D,H52E,H52F), C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C1S(H1SA,
 H1SB,H1SC), C6S(H6SA,H6SB,H6SC), C11S(H11A,H11B,H11C), C15S(H15B,H15C,H15D)
;
_shelx_res_checksum              51365
_olex2_date_sample_data_collection 2016-04-29
_olex2_submission_special_instructions 'No special instructions were received'