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_7037685
_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_sum            'C31 H53 Mo N3 Si'
_chemical_formula_weight         591.79
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-17 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                108.896(2)
_cell_angle_beta                 90.882(3)
_cell_angle_gamma                110.844(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8122(14)
_cell_length_b                   10.8705(14)
_cell_length_c                   16.219(2)
_cell_measurement_reflns_used    2565
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.45
_cell_volume                     1667.0(4)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11842
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.855
_diffrn_reflns_theta_max         24.855
_diffrn_reflns_theta_min         2.038
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0450P)^2^+0.1350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4283
_reflns_number_total             5716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04548g2.cif
_cod_data_source_block           gn033
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7037684--7037685.cif.
;
_cod_database_code               7037685
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              29263
_shelx_hkl_checksum              51665