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_7700851
_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         'C48 H62 Cl O P Ru S2'
_chemical_formula_sum            'C48 H62 Cl O P Ru S2'
_chemical_formula_weight         886.58
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.473(3)
_cell_angle_beta                 82.579(3)
_cell_angle_gamma                72.678(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6919(3)
_cell_length_b                   14.1709(4)
_cell_length_c                   17.7259(6)
_cell_measurement_reflns_used    8624
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      75.5810
_cell_measurement_theta_min      4.5140
_cell_volume                     2270.91(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     36.00 121.00   1.00    4.00    --  110.57-125.00 150.00   85
  2  \w    -70.00  32.00   1.00    2.00    --  -40.57  57.00 -30.00  102
  3  \w    -70.00  33.00   1.00    2.00    --  -40.57  57.00-150.00  103
  4  \w    -74.00  38.00   1.00    2.00    --  -40.57  77.00  60.00  112
  5  \w     36.00 108.00   1.00    4.00    --  110.57 -94.00 -30.00   72
  6  \w     37.00 137.00   1.00    4.00    --  110.57 -45.00 -60.00  100
  7  \w     80.00 178.00   1.00    4.00    --  110.57  30.00-120.00   98
  8  \w    101.00 173.00   1.00    4.00    --  110.57 125.00 -90.00   72
  9  \w     80.00 178.00   1.00    4.00    --  110.57  30.00 -30.00   98
 10  \w     41.00 106.00   1.00    4.00    --  110.57 -45.00-180.00   65
 11  \w     28.00 108.00   1.00    4.00    --  110.57 -94.00-150.00   80
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1497230000
_diffrn_orient_matrix_UB_12      0.0162928000
_diffrn_orient_matrix_UB_13      -0.0280377000
_diffrn_orient_matrix_UB_21      -0.0005798000
_diffrn_orient_matrix_UB_22      -0.0420296000
_diffrn_orient_matrix_UB_23      -0.0736411000
_diffrn_orient_matrix_UB_31      -0.0739004000
_diffrn_orient_matrix_UB_32      0.1064156000
_diffrn_orient_matrix_UB_33      -0.0412595000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12355
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.993
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'micro-focus 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    4.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0350P)^2^+0.7090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7469
_reflns_number_total             7932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02457c2.cif
_cod_data_source_block           ng46cult
_cod_depositor_comments
'Adding full bibliography for 7700845--7700851.cif.'
_cod_database_code               7700851
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.61
_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, All O(H) groups
2. Restrained distances
 C32A-C30A = C31A-C30A
 1.52 with sigma of 0.02
 C32-C30 = C31-C30
 1.52 with sigma of 0.02
3. Others
 Fixed Sof: C30(0.7) H30(0.7) C30A(0.3) H30A(0.3) C31(0.55) H31A(0.55)
 H31B(0.55) H31C(0.55) C31A(0.45) H31D(0.45) H31E(0.45) H31F(0.45) C32(0.55)
 H32A(0.55) H32B(0.55) H32C(0.55) C32A(0.45) H32D(0.45) H32E(0.45) H32F(0.45)
4.a Riding coordinates:
 O1(H1)
4.b Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C27(H27), C30(H30), C30A(H30A), C33(H33)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C23(H23), C25(H25), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F), C32(H32A,H32B,H32C),
 C32A(H32D,H32E,H32F), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              53904
_olex2_date_sample_data_collection 2017-04-10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.423
_oxdiff_exptl_absorpt_empirical_full_min 0.830