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_7700850
_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
'C43 H44 N O2 P Ru S Se2, 0.75(C4 H8 O), 0.25(H2 O)'
_chemical_formula_sum            'C46 H50.5 N O3 P Ru S Se2'
_chemical_formula_weight         987.39
_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
_audit_creation_date             2016-09-14
_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                70.854(4)
_cell_angle_beta                 82.761(3)
_cell_angle_gamma                72.261(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9055(3)
_cell_length_b                   14.8954(7)
_cell_length_c                   15.8159(7)
_cell_measurement_reflns_used    4922
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.1940
_cell_measurement_theta_min      4.6720
_cell_volume                     2098.80(16)
_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)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega   29.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -100.0000  -11.0000 82

  2 omega  -49.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   37.0000   90.0000 80

  3 omega  -92.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  125.0000   60.0000 83

  4 omega -115.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  -57.0000  -60.0000 103

  5 omega  -38.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953  -77.0000 -150.0000 112

  6 omega   38.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -125.0000 -120.0000 84

  7 omega   36.00  136.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000   30.0000 100

  8 omega   52.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000  120.0000 32
;
_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      -0.0505361000
_diffrn_orient_matrix_UB_12      0.1000863000
_diffrn_orient_matrix_UB_13      -0.0732314000
_diffrn_orient_matrix_UB_21      -0.0128156000
_diffrn_orient_matrix_UB_22      -0.0544474000
_diffrn_orient_matrix_UB_23      -0.0650017000
_diffrn_orient_matrix_UB_31      -0.1548157000
_diffrn_orient_matrix_UB_32      0.0056621000
_diffrn_orient_matrix_UB_33      0.0324407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11466
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.994
_diffrn_reflns_theta_min         5.044
_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    6.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69226
_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    1.562
_exptl_crystal_description       needle
_exptl_crystal_F_000             1001
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0650P)^2^+0.9250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6762
_reflns_number_total             7294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02457c2.cif
_cod_data_source_block           ng26cult
_cod_depositor_comments
'Adding full bibliography for 7700845--7700851.cif.'
_cod_original_formula_sum        'C46 H50.50 N O3 P Ru S Se2'
_cod_database_code               7700850
_reflns_odcompleteness_completeness 70.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Others
 Fixed Sof: O1S(0.75) C2S(0.75) H2SA(0.75) H2SB(0.75) C3S(0.75) H3SA(0.75)
 H3SB(0.75) C4S(0.75) H4SA(0.75) H4SB(0.75) C5S(0.75) H5SA(0.75) H5SB(0.75)
 O1W(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C13(H13), C15(H15), C23(H23), C25(H25),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              91303
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'