Synthesis and characterisation of hydrido molybdenum and tungsten complexes having a hemilabile tridentate Si,Si,O-ligand: observation of stepwise hydrosilylation of a nitrile to form an N-silylimine on the metal centre.
Komuro, Takashi; Begum, Rockshana; Ono, Rikima; Tobita, Hiromi; Dalton transactions (Cambridge, England : 2003) 40 (2011) 2348–2357; doi:10.1039/c0dt01047b

data_7014683
_publ_section_title
;
 Synthesis and characterisation of hydrido molybdenum and tungsten
 complexes having a hemilabile tridentate Si,Si,O-ligand: observation
 of stepwise hydrosilylation of a nitrile to form an N-silylimine on
 the metal centre.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2348
_journal_page_last               2357
_journal_paper_doi               10.1039/c0dt01047b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C37 H45 N O2 Si2 W'
_chemical_formula_sum            'C37 H45 N O2 Si2 W'
_chemical_formula_weight         775.77
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.2959(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5695(7)
_cell_length_b                   8.7738(2)
_cell_length_c                   21.5198(7)
_cell_measurement_reflns_used    20975
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.1
_cell_volume                     3364.49(18)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25937
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_T_max  0.784820
_exptl_absorpt_correction_T_min  0.451600
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan.
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.789
_refine_diff_density_min         -2.521
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+6.9201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                6724
_reflns_number_total             7306
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0DT01047B.TXT
_cod_data_source_block           compound-5b
_cod_original_cell_volume        3364.49(17)
_cod_database_code               7014683