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_4337137
_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_formula_sum            'C27 H55 N9 Ru Si3'
_chemical_formula_weight         691.11
_chemical_name_common
;  
          
[RuH{kappa-Si,N-(SiMe2)(C7H12N3)}3]
  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3703(2)
_cell_length_b                   18.4278(5)
_cell_length_c                   18.8875(5)
_cell_measurement_reflns_used    6588
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      60.25
_cell_measurement_theta_min      4.05
_cell_volume                     3258.20(14)
_computing_cell_refinement       'ILL RAFD9'
_computing_data_collection       'ILL HKLGEN, MAD'
_computing_data_reduction        'ILL Retreat'
_computing_molecular_graphics
;     
 ORTEP for Windows v1.074 (L.J. Farrugia 1997)
 Mercury CSD 2.4.5 (Build RC3), CCDC, Cambridge (2011)
;
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia, J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.,2008,A64,112)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type
'D19 position-sensitive detector diffractometer'
_diffrn_measurement_method       'omega step-scans'
_diffrn_radiation_monochromator  'Cu (311)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL High Flux Reactor'
_diffrn_radiation_type           monochromatic
_diffrn_radiation_wavelength     1.1700
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31238
_diffrn_reflns_theta_full        60.30
_diffrn_reflns_theta_max         60.30
_diffrn_reflns_theta_min         4.94
_diffrn_standards_interval_time  270
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.6563
_exptl_absorpt_correction_T_min  0.4218
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'program D19abscan'
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             310
_exptl_crystal_size_max          5.0
_exptl_crystal_size_mid          2.6
_exptl_crystal_size_min          1.5
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         9863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+22.0901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                9100
_reflns_number_total             9863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4027199_si_002.cif
_cod_data_source_block           3aneutrons
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4337137
_compound_number                 3a