Addition of Si‒H and B‒H Bonds and Redox Reactivity Involving Low-Coordinate Nitrido‒Vanadium Complexes
Thompson, Rick; Tran, Ba L.; Ghosh, Soumya; Chen, Chun-Hsing; Pink, Maren; Gao, Xinfeng; Carroll, Patrick J.; Baik, Mu-Hyun; Mindiola, Daniel J.; Inorganic Chemistry  (2015) 150302094058008–; doi:10.1021/acs.inorgchem.5b00302

data_4342597
_publ_section_title
;
 Addition of Si--H and B--H Bonds and Redox Reactivity Involving
 Low-Coordinate Nitrido--Vanadium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              150302094058008
_journal_paper_doi               10.1021/acs.inorgchem.5b00302
_journal_year                    2015
_chemical_formula_moiety         'C46 H64 Al N4 V'
_chemical_formula_sum            'C46 H64 Al N4 V'
_chemical_formula_weight         750.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.3460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0890(6)
_cell_length_b                   17.6638(7)
_cell_length_c                   19.2166(8)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.00
_cell_measurement_theta_min      2.27
_cell_volume                     4370.7(3)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXTL (Bruker, 2012)'
_computing_structure_solution    'SHELXTL (Bruker, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31832
_diffrn_reflns_theta_full        16.01
_diffrn_reflns_theta_max         16.01
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.9951
_exptl_absorpt_correction_T_min  0.9830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G Sheldrick; 2012'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         10546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0966P)^2^+1.2358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                8177
_reflns_number_total             10546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00302_si_005.cif
_cod_data_source_block           s14006
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4342597