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_7041557
_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         'C21 H29 Co N O12 P3 Ru'
_chemical_formula_sum            'C21 H29 Co N O12 P3 Ru'
_chemical_formula_weight         740.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-12
_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                 97.413(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4496(16)
_cell_length_b                   11.5244(17)
_cell_length_c                   22.855(4)
_cell_measurement_reflns_used    12939
_cell_measurement_temperature    98
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.0
_cell_volume                     2729.3(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 270
               Slice: -125.0000 - 10.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 34.4966
              2theta: -34.6962
scan:
    Number of images: 112
               Slice: -68.0000 - -12.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 180.0000
                 XTD: 34.4966
              2theta: -34.6962
scan:
    Number of images: 108
               Slice: -65.0000 - -11.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 0.0000
                 XTD: 34.4966
              2theta: -34.6962
scan:
    Number of images: 62
               Slice: -65.0000 - -34.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 90.0000
                 XTD: 34.4966
              2theta: -34.6962
;
_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      0.003614
_diffrn_orient_matrix_UB_12      0.067969
_diffrn_orient_matrix_UB_13      0.068412
_diffrn_orient_matrix_UB_21      -0.058051
_diffrn_orient_matrix_UB_22      0.047260
_diffrn_orient_matrix_UB_23      -0.043887
_diffrn_orient_matrix_UB_31      -0.032266
_diffrn_orient_matrix_UB_32      -0.015912
_diffrn_orient_matrix_UB_33      0.025544
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14121
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.965
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.430
_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    1.802
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.788
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0560P)^2^+6.9280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4608
_reflns_number_total             5033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04717c2.cif
_cod_data_source_block           LRuNOnaphcat
_cod_depositor_comments
'Adding full bibliography for 7041555--7041559.cif.'
_cod_original_cell_volume        2729.3(7)
_cod_database_code               7041557
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.787
_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. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C21) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(Co1)
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C8(H8), C11(H11), C20(H20), C21(H21), C12(H12), C10(H10),
 C18(H18), C19(H19), C13(H13)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C1(H1A,
 H1B,H1C), C6(H6A,H6B,H6C)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'