Nature of si-h interactions in a series of ruthenium silazane complexes using multinuclear solid-state NMR and neutron diffraction.
Smart, Katharine A.; Grellier, Mary; Coppel, Yannick; Vendier, Laure; Mason, Sax A.; Capelli, Silvia C.; Albinati, Alberto; Montiel-Palma, Virginia; Muñoz-Hernández, Miguel A; Sabo-Etienne, Sylviane; Inorganic chemistry 53 (2014) 1156–1165; doi:10.1021/ic4027199

data_4337135
_publ_section_title
;
 Nature of si-h interactions in a series of ruthenium silazane complexes
 using multinuclear solid-state NMR and neutron diffraction.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1156
_journal_page_last               1165
_journal_paper_doi               10.1021/ic4027199
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H27 Cl3 N9 Ru Si3'
_chemical_formula_sum            'C24 H28 Cl3 N9 Ru Si3'
_chemical_formula_weight         734.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.921(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7355(6)
_cell_length_b                   9.5108(6)
_cell_length_c                   33.6476(17)
_cell_measurement_reflns_used    4722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.3652
_cell_measurement_theta_min      3.9462
_cell_measurement_wavelength     1.5418
_cell_volume                     3115.1(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0724212
_diffrn_orient_matrix_UB_12      0.0141872
_diffrn_orient_matrix_UB_13      0.0402472
_diffrn_orient_matrix_UB_21      0.1205694
_diffrn_orient_matrix_UB_22      0.0893448
_diffrn_orient_matrix_UB_23      0.0158225
_diffrn_orient_matrix_UB_31      -0.0720605
_diffrn_orient_matrix_UB_32      0.1345742
_diffrn_orient_matrix_UB_33      -0.01505
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            19076
_diffrn_reflns_theta_full        61.39
_diffrn_reflns_theta_max         61.39
_diffrn_reflns_theta_min         4.71
_exptl_absorpt_coefficient_mu    7.815
_exptl_absorpt_correction_T_max  0.9125
_exptl_absorpt_correction_T_min  0.6991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+16.8731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                4031
_reflns_number_total             4735
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4027199_si_002.cif
_cod_data_source_block           3c(CSO080911Ge)
_cod_database_code               4337135