Bis(alkylamido)phenylborane Complexes of Zirconium, Hafnium, and Vanadium
David R. Manke; Daniel G. Nocera; Inorganic Chemistry 42 (2003) 4431–4436; doi:10.1021/ic0340478

data_4313867
_publ_contact_author             'Daniel G. Nocera'
_publ_contact_author_email       nocera@mit.edu
_publ_section_title
;
 Bis(alkylamido)phenylborane Complexes of Zirconium, Hafnium, and Vanadium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4431
_journal_page_last               4436
_journal_paper_doi               10.1021/ic0340478
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C28 H46 B2 N4 V'
_chemical_formula_weight         511.26
_chemical_name_systematic        Bis(bis(tert-butylamido)phenylborane)-vanadium
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.297(7)
_cell_length_b                   8.976(4)
_cell_length_c                   20.237(9)
_cell_measurement_temperature    183(2)
_cell_volume                     3142(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4017
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.7911
_exptl_absorpt_correction_T_min  0.5906
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0003(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                942
_reflns_number_total             1457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0340478rom20030428_120204_5.cif
_cod_data_source_block           compd5
_cod_depositor_comments
;

2021-05-16
Formula fixed to be consistent with given Z
                 miguel
;
_cod_original_formula_sum            'C28 H46 B2 N4 V2'
_cod_original_formula_weight         562.19
_cod_database_code               4313867