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_7041558
_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_formula_moiety         'C17 H23 Br4 Co N O12 P3 Ru'
_chemical_formula_sum            'C17 H23 Br4 Co N O12 P3 Ru'
_chemical_formula_weight         1005.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-29
_audit_creation_method
;
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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.071(3)
_cell_length_b                   14.2382(17)
_cell_length_c                   17.677(2)
_cell_measurement_reflns_used    29419
_cell_measurement_temperature    98
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.0
_cell_volume                     6058.4(13)
_computing_cell_refinement
;
CrystalClear-SM Auto 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Auto 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Auto 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      98
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
scan:
    Number of images: 246
               Slice: -68.0000 - 55.0000
         Image width: 0.5000
            Exp time: 35.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 90.0000
                 XTD: 35.0000
              2theta: -35.0000
scan:
    Number of images: 222
               Slice: -67.0000 - 44.0000
         Image width: 0.5000
            Exp time: 35.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 270.0000
                 XTD: 35.0000
              2theta: -35.0000
scan:
    Number of images: 122
               Slice: -81.0000 - -20.0000
         Image width: 0.5000
            Exp time: 35.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 90.0000
                 XTD: 35.0000
              2theta: -35.0000
scan:
    Number of images: 60
               Slice: -115.0000 - -85.0000
         Image width: 0.5000
            Exp time: 35.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 35.0000
              2theta: -35.0000
scan:
    Number of images: 56
               Slice: -61.0000 - -33.0000
         Image width: 0.5000
            Exp time: 35.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 180.0000
                 XTD: 35.0000
              2theta: -35.0000
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.030540
_diffrn_orient_matrix_UB_12      -0.022213
_diffrn_orient_matrix_UB_13      -0.059872
_diffrn_orient_matrix_UB_21      0.045726
_diffrn_orient_matrix_UB_22      -0.031441
_diffrn_orient_matrix_UB_23      -0.012618
_diffrn_orient_matrix_UB_31      -0.016451
_diffrn_orient_matrix_UB_32      -0.032665
_diffrn_orient_matrix_UB_33      0.020439
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.433
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.536
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_description       plank
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.199(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0200P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                11355
_reflns_number_total             12832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04717c2.cif
_cod_data_source_block           LRuNOBr4cat
_cod_depositor_comments
'Adding full bibliography for 7041555--7041559.cif.'
_cod_original_cell_volume        6058.5(13)
_cod_database_code               7041558
_shelx_estimated_absorpt_t_max   0.484
_shelx_estimated_absorpt_t_min   0.245
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.801(6) 0.199(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17)
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C31(H31), C17(H17), C15(H15), C32(H32), C16(H16),
 C34(H34), C30(H30), C33(H33)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C7(H7A,
 H7B,H7C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'