Group-4 Transition-Metal Boryl Complexes: Syntheses, Structures, Boron-Metal Bonding Properties, and Application as a Polymerization Catalyst
Tomomi Terabayashi; Takashi Kajiwara; Makoto Yamashita; Kyoko Nozaki; Journal of the American Chemical Society 131 (2009) 14162–14163; doi:10.1021/ja905950g

data_4105114
_publ_section_title
;
 Group-4 Transition-Metal Boryl Complexes: Syntheses, Structures,
 Boron-Metal Bonding Properties, and Application as a Polymerization
 Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14162
_journal_page_last               14163
_journal_paper_doi               10.1021/ja905950g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C50 H65 B Hf N2'
_chemical_formula_weight         883.34
_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
_cell_angle_beta                 104.7340(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.700(3)
_cell_length_b                   12.582(2)
_cell_length_c                   19.211(4)
_cell_measurement_reflns_used    13655
_cell_measurement_temperature    121.1500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1533
_cell_volume                     4371.4(13)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      121(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27275
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  0.4443
_exptl_absorpt_correction_T_min  0.3773
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       Block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.534
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+7.8122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                6654
_reflns_number_total             7419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905950g_si_002_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4105114