Synthesis and Structure of Bifunctional Zirconocene/Borane Complexes and Their Activation for Ethylene Polymerization
Rojas, Rene S.; Peoples, Brian C.; Cabrera, Alan R.; Valderrama, Mauricio; Fröhlich, Roland; Kehr, Gerald; Erker, Gerhard; Wiegand, Thomas; Eckert, Hellmut; Organometallics 30 (2011) 6372–; doi:10.1021/om200536z

data_4065045
_publ_section_title
;
 Synthesis and Structure of Bifunctional Zirconocene/Borane Complexes and
 Their Activation for Ethylene Polymerization
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6372
_journal_paper_doi               10.1021/om200536z
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C62 H38 B2 Cl2 F25 N3 Zr'
_chemical_formula_weight         1483.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.600(1)
_cell_angle_beta                 97.856(1)
_cell_angle_gamma                107.270(1)
_cell_formula_units_Z            2
_cell_length_a                   11.3834(2)
_cell_length_b                   15.7024(3)
_cell_length_c                   19.0552(4)
_cell_measurement_reflns_used    7478
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      4.08
_cell_volume                     3099.12(11)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15499
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.8940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         10663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0804
_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^)+(0.0672P)^2^+11.6494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                8704
_reflns_number_total             10663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200536z_si_002.cif
_cod_data_source_block           erk5609
_cod_original_cell_volume        3099.12(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065045