Oxygen-bridged hybrid metallocene-nonmetallocene polymetallic catalysts of group 4 metals for bimodal activity in olefin polymerization: synthesis, characterization, and theoretical investigation.
Mandal, Swadhin K.; Gurubasavaraj, Prabhuodeyara M.; Roesky, Herbert W.; Schwab, Gerald; Stalke, Dietmar; Oswald, Rainer B.; Dolle, Volker; Inorganic chemistry 46 (2007) 10158–10167; doi:10.1021/ic7011765

data_4339414
_publ_contact_author             'Prof. Dr. Herbert Roesky'
_publ_section_title
;
 Oxygen-bridged hybrid metallocene-nonmetallocene polymetallic catalysts
 of group 4 metals for bimodal activity in olefin polymerization:
 synthesis, characterization, and theoretical investigation.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10158
_journal_page_last               10167
_journal_paper_doi               10.1021/ic7011765
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C46 H78 Hf N2 O2 Zr2'
_chemical_formula_weight         1052.03
_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                 111.0510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8318(8)
_cell_length_b                   18.7743(10)
_cell_length_c                   17.7562(9)
_cell_measurement_reflns_used    39701
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.46
_cell_volume                     4614.4(4)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.0-2'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0122
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            76389
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    2.724
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0312P)^2^+10.4730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                8882
_reflns_number_total             9408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011765-file001.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4339414