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_4313863
_publ_contact_author             'Daniel G. Nocera'
_publ_contact_author_email       nocera@mit.edu
_publ_section_title
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 Bis(alkylamido)phenylborane Complexes of Zirconium, Hafnium, and Vanadium
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_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            'C35 H61 B2 N4 O Zr'
_chemical_formula_weight         666.72
_chemical_name_systematic
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Bis(bis(tert-butylamido)phenylborane)-tetrahydrofuran-zirconium n-hexane solvate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.119(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8574(13)
_cell_length_b                   13.3389(16)
_cell_length_c                   26.086(3)
_cell_measurement_temperature    183(2)
_cell_volume                     3777.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10110
_diffrn_reflns_theta_full        19.99
_diffrn_reflns_theta_max         19.99
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_preparation       hexanes
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0027(3)
_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   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         3466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0050P)^2^+12.2837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                3300
_reflns_number_total             3466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0340478rom20030428_120204_1.cif
_cod_data_source_block           compd1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        3777.3(8)
_cod_database_code               4313863