Ruthenium chalcogenonitrosyl and bridged nitrido complexes containing chelating sulfur and oxygen ligands.
Ng, Ho-Yuen; Cheung, Wai-Man; Kwan Huang, Enrique; Wong, Kang-Long; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18459–18468; doi:10.1039/c5dt02513c

data_7036645
_publ_section_title
;
 Ruthenium chalcogenonitrosyl and bridged nitrido complexes containing
 chelating sulfur and oxygen ligands.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18459
_journal_page_last               18468
_journal_paper_doi               10.1039/c5dt02513c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'(C64 H144 N5 P8 Ru2 S8), 0.25(C6 H12), 0.25(C4 H8 O)'
_chemical_formula_sum            'C66.5 H149.5 N5 O0.25 P8 Ru2 S8'
_chemical_formula_weight         1729.79
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-02 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.8792(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.7799(4)
_cell_length_b                   15.6193(3)
_cell_length_c                   27.8342(5)
_cell_measurement_reflns_used    11131
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      75.3240
_cell_measurement_theta_min      4.4300
_cell_volume                     9654.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   33.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000    0.0000 53

  2 omega  -34.00   14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  120.0000 48

  3 omega  -36.00   34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  -60.0000 70

  4 omega -115.00   -3.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -19.0000  120.0000 112

  5 omega   33.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   60.0000 53

  6 omega  140.00  174.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  111.0000 -180.0000 34

  7 omega   85.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000 -180.0000 91

  8 omega  106.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  111.0000  120.0000 72

  9 omega   33.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -120.0000 56

 10 omega -115.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000  -30.0000 104

 11 omega    1.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8203  -99.0000 -150.0000 82

 12 omega   80.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000   30.0000 45
;
_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      -0.0438651000
_diffrn_orient_matrix_UB_12      -0.0436233000
_diffrn_orient_matrix_UB_13      0.0272442000
_diffrn_orient_matrix_UB_21      -0.0531740000
_diffrn_orient_matrix_UB_22      0.0472541000
_diffrn_orient_matrix_UB_23      -0.0334428000
_diffrn_orient_matrix_UB_31      -0.0080188000
_diffrn_orient_matrix_UB_32      -0.0747609000
_diffrn_orient_matrix_UB_33      -0.0369067000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22023
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         5.05
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3686
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.060
_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     417
_refine_ls_number_reflns         8584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.2214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                7670
_reflns_number_total             8584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02513c1.cif
_cod_data_source_block           wai135cult
_cod_depositor_comments
'Adding full bibliography for 7036640--7036645.cif.'
_cod_original_cell_volume        9654.5(3)
_cod_original_formula_sum        'C66.50 H149.50 N5 O0.25 P8 Ru2 S8'
_cod_database_code               7036645
_chemical_oxdiff_formula         'Ru2 N S8 P8 N4 Bu16 OC4H8'
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C)
;
_olex2_date_sample_data_collection 1389321155.0
_olex2_submission_special_instructions 'No special instructions were received'