Synthesis and characterisation of ruthenium-nitrosyl complexes in oxygen-rich ligand environments.
Krishnan, V. Mahesh; Arman, Hadi D.; Tonzetich, Zachary J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1186–1193; doi:10.1039/c6dt04717c

data_7041556
_publ_section_title
;
 Synthesis and characterisation of ruthenium-nitrosyl complexes in
 oxygen-rich ligand environments.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1186
_journal_page_last               1193
_journal_paper_doi               10.1039/c6dt04717c
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H44 Co N3 O12 P3 Ru, 2(C F3 O3 S)'
_chemical_formula_sum            'C22 H44 Co F6 N3 O18 P3 Ru S2'
_chemical_formula_weight         1069.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-03
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;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.902(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.084(3)
_cell_length_b                   12.6011(17)
_cell_length_c                   16.863(2)
_cell_measurement_reflns_used    7388
_cell_measurement_temperature    298
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      3.1
_cell_volume                     4257.8(10)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
    Number of images: 246
               Slice: -68.0000 - 55.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 0.0000
                 XTD: 35.0086
              2theta: -35.0172
scan:
    Number of images: 238
               Slice: -68.0000 - 51.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 180.0000
                 XTD: 35.0086
              2theta: -35.0172
scan:
    Number of images: 74
               Slice: -71.0000 - -34.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 180.0000
                 XTD: 35.0086
              2theta: -35.0172
scan:
    Number of images: 66
               Slice: -125.0000 - -92.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 90.0000
                 XTD: 35.0086
              2theta: -35.0172
scan:
    Number of images: 64
               Slice: -38.0000 - -6.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 90.0000
                 XTD: 35.0086
              2theta: -35.0172
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724 (2x2 bin mode)'
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_diffrn_orient_matrix_type       d*Trek
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_diffrn_orient_matrix_UB_13      0.016900
_diffrn_orient_matrix_UB_21      -0.073455
_diffrn_orient_matrix_UB_22      0.004285
_diffrn_orient_matrix_UB_23      0.029728
_diffrn_orient_matrix_UB_31      -0.021573
_diffrn_orient_matrix_UB_32      -0.024210
_diffrn_orient_matrix_UB_33      -0.049816
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12678
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.3
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_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6982
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0850P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.867
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                6835
_reflns_number_total             6982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04717c2.cif
_cod_data_source_block           cd1331a
_cod_depositor_comments
'Adding full bibliography for 7041555--7041559.cif.'
_cod_database_code               7041556
_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
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C3(H3), C18(H18), C4(H4), C1(H1), C2(H2), C5(H5)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C),
 C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C),
  C19(H19A,H19B,H19C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              88625
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'