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_4081958
_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            'C36 H66 Hf N3 P'
_chemical_formula_weight         750.38
_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                103.5740(10)
_cell_angle_beta                 90.3420(10)
_cell_angle_gamma                106.7450(10)
_cell_formula_units_Z            8
_cell_length_a                   17.5453(3)
_cell_length_b                   21.5242(3)
_cell_length_c                   21.8050(3)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.36
_cell_volume                     7641.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            331839
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    2.798
_exptl_absorpt_correction_T_max  0.7868
_exptl_absorpt_correction_T_min  0.6185
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1724
_refine_ls_number_reflns         35096
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+9.9535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                30842
_reflns_number_total             35096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4008339_si_001.cif
_cod_data_source_block           14
_cod_depositor_comments
;

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C144 H264 Hf4 N12 P4'
_cod_original_formula_weight         3001.51
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081958