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_7700848
_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
'C44 H47 N O2 P Ru S Se2, 1.5(C H2 Cl2), C F3 O3 S, 0.25(H2 O)'
_chemical_formula_sum            'C46.5 H50.5 Cl3 F3 N O5.25 P Ru S2 Se2'
_chemical_formula_weight         1224.81
_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     iterative
_audit_creation_date             2018-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-13 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                76.926(3)
_cell_angle_beta                 88.118(3)
_cell_angle_gamma                89.849(3)
_cell_formula_units_Z            4
_cell_length_a                   12.4019(5)
_cell_length_b                   20.0163(8)
_cell_length_c                   20.6971(8)
_cell_measurement_reflns_used    7334
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.3810
_cell_measurement_theta_min      4.1200
_cell_volume                     5001.9(3)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_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     36.00 129.00   1.00    7.00    --  110.57 -45.00   0.00   93
  2  \w    -67.00  33.00   1.00    4.00    --  -40.57  57.00 150.00  100
  3  \w    -70.00  33.00   1.00    4.00    --  -40.57  57.00  30.00  103
  4  \w    -73.00  38.00   1.00    4.00    --  -40.57  77.00-120.00  111
  5  \w     69.00 115.00   1.00    7.00    --  110.57-111.00 -60.00   46
  6  \w     52.00 108.00   1.00    7.00    --  110.57 -94.00  30.00   56
  7  \w     56.00 108.00   1.00    7.00    --  110.57 -94.00 120.00   52
  8  \w     34.00 167.00   1.00    7.00    --  110.57 -15.00 150.00  133
  9  \w     82.00 178.00   1.00    7.00    --  110.57  61.00 150.00   96
 10  \w    100.00 178.00   1.00    7.00    --  110.57 111.00 -30.00   78
 11  \w     36.00 122.00   1.00    7.00    --  110.57 -61.00-120.00   86
 12  \w     34.00  59.00   1.00    7.00    --  110.57-111.00 -60.00   25
 13  \w     26.00  51.00   1.00    7.00    --  110.57 -94.00 120.00   25
;
_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      -0.0827452000
_diffrn_orient_matrix_UB_12      -0.0086819000
_diffrn_orient_matrix_UB_13      0.0584987000
_diffrn_orient_matrix_UB_21      0.0235778000
_diffrn_orient_matrix_UB_22      0.0737966000
_diffrn_orient_matrix_UB_23      0.0061457000
_diffrn_orient_matrix_UB_31      -0.0896939000
_diffrn_orient_matrix_UB_32      0.0268691000
_diffrn_orient_matrix_UB_33      -0.0488436000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28086
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.493
_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    7.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79949
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2462
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1182
_refine_ls_number_reflns         17772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12272
_reflns_number_total             17772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02457c2.cif
_cod_data_source_block           ng73cult
_cod_depositor_comments
'Adding full bibliography for 7700845--7700851.cif.'
_cod_original_formula_sum        'C46.50 H50.50 Cl3 F3 N O5.25 P Ru S2 Se2'
_cod_database_code               7700848
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10A,H10B,H10C} of C10, All C(H,H) groups
 At 1.5 times of:
  {H19D,H19E,H19F} of C19A, {H18D,H18E,H18F} of C18A, {H7AA,H7AB,H7AC} of C7A,
   {H10D,H10E,H10F} of C10A, {H17D,H17E,H17F} of C17A, {H18A,H18B,H18C} of C18,
  {H28A,H28B,H28C} of C28, {H29A,H29B,H29C} of C29, {H17A,H17B,H17C} of C17,
  {H27A,H27B,H27C} of C27, {H19A,H19B,H19C} of C19, {H7A,H7B,H7C} of C7, {H29D,
  H29E,H29F} of C29A, {H28D,H28E,H28F} of C28A, {H27D,H27E,H27F} of C27A
2. Others
 Fixed Sof: O1W(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB)
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),
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C13A(H13A), C15A(H15A), C23A(H23A),
 C25A(H25A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
 C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C52A(H52A),
 C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C7A(H7AA,H7AB,H7AC), C10A(H10D,H10E,H10F), C17A(H17D,H17E,H17F),
 C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C27A(H27D,H27E,H27F), C28A(H28D,
 H28E,H28F), C29A(H29D,H29E,H29F)
;
_shelx_res_checksum              54964
_olex2_date_sample_data_collection 2017-10-20
_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.831