Synthetic Optimization and Scale-Up of Imino‒Amido Hafnium and Zirconium Olefin Polymerization Catalysts
Zhang, Chunming; Pan, Heqi; Klosin, Jerzy; Tu, Siyu; Jaganathan, Arvind; Fontaine, Philip P.; Organic Process Research & Development 19 (2015) 1383–; doi:10.1021/acs.oprd.5b00047

data_1519691
_publ_section_title
;
 Synthetic Optimization and Scale-Up of Imino--Amido Hafnium and Zirconium
 Olefin Polymerization Catalysts
;
_journal_issue                   10
_journal_name_full               'Organic Process Research &amp; Development'
_journal_page_first              1383
_journal_paper_doi               10.1021/acs.oprd.5b00047
_journal_volume                  19
_journal_year                    2015
_chemical_formula_sum            'C28 H52 N2 Zr'
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                80.898(3)
_cell_angle_beta                 88.203(3)
_cell_angle_gamma                89.242(3)
_cell_formula_units_Z            4
_cell_length_a                   9.7837(5)
_cell_length_b                   17.3161(10)
_cell_length_c                   17.4313(10)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.37
_cell_volume                     2914.4(3)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_laue_measured_fraction_full 0.990
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_diffrn_reflns_point_group_measured_fraction_full 0.990
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_diffrn_reflns_theta_full        25.242
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_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.164
_refine_diff_density_max         2.568
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+23.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10869
_reflns_number_total             12279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op5b00047_si_002.cif
_cod_data_source_block           Complex_15
_cod_depositor_comments          'Adding full bibliography for 1519691.cif.'
_cod_database_code               1519691
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              89014
_shelx_hkl_checksum              3300