Preparation of New Olefin Polymerization Precatalysts by Facile Derivatization of Imino–Enamido ZrMe3and HfMe3Complexes
Klosin, Jerzy; Fontaine, Philip P.; Figueroa, Ruth; McCann, Scott D.; Mort, Darrek; Organometallics 32 (2013) 6488–; doi:10.1021/om4008339

data_4081957
_publ_section_title
;
 Preparation of New Olefin Polymerization Precatalysts by Facile
 Derivatization of Imino--Enamido ZrMe3and HfMe3Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6488
_journal_paper_doi               10.1021/om4008339
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C52.5 H78.5 Hf N5'
_chemical_formula_weight         958.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.6355(10)
_cell_length_b                   20.2804(9)
_cell_length_c                   39.6424(16)
_cell_measurement_temperature    100(2)
_cell_volume                     19806.0(14)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            102349
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.027
_exptl_absorpt_coefficient_mu    2.145
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             8008
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         22747
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+28.6840P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18713
_reflns_number_total             22747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4008339_si_001.cif
_cod_data_source_block           12
_cod_original_formula_sum        'C52.50 H78.50 Hf N5'
_cod_database_code               4081957
_shelx_estimated_absorpt_t_min   0.650
_shelx_estimated_absorpt_t_max   0.814