Hydridosilylamido complexes of Ta and Mo isolobal with Berry's zirconocenes: syntheses, β-Si-H agostic interactions, catalytic hydrosilylation, and insight into mechanism.
McLeod, Nicolas A.; Kuzmina, Lyudmila G.; Korobkov, Ilia; Howard, Judith A. K.; Nikonov, Georgii I.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2554–2561; doi:10.1039/c5dt04548g

data_7037684
_publ_section_title
;
 Hydridosilylamido complexes of Ta and Mo isolobal with Berry's
 zirconocenes: syntheses, \b-Si-H agostic interactions, catalytic
 hydrosilylation, and insight into mechanism.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2554
_journal_page_last               2561
_journal_paper_doi               10.1039/c5dt04548g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C30 H50 Cl Mo N3 Si'
_chemical_formula_sum            'C30 H50 Cl Mo N3 Si'
_chemical_formula_weight         612.21
_chemical_name_systematic
;
 ? 
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-17 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                71.491(3)
_cell_angle_beta                 86.247(5)
_cell_angle_gamma                69.622(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1926(8)
_cell_length_b                   10.7193(9)
_cell_length_c                   16.7763(17)
_cell_measurement_reflns_used    3641
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      29.185
_cell_measurement_theta_min      2.433
_cell_volume                     1627.2(3)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.1066
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14571
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.28
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.8456
_exptl_absorpt_correction_T_min  0.5638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brownish-red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.242
_refine_diff_density_min         -2.595
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         8098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0822P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                5446
_reflns_number_total             8098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04548g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7037684--7037685.cif.'
_cod_original_cell_volume        1627.3(2)
_cod_database_code               7037684
_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.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C7A(H7A), C8A(H8A)
2.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F),
 C12A(H12D,H12E,H12F), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C3A(H3A), C4A(H4A), C5A(H5A)
;
_olex2_submission_special_instructions 'No special instructions were received'