Bimetallic Zirconium Amine Bis(phenolate) Polymerization Catalysts: Enhanced Activity and Tacticity Control for Polyolefin Synthesis.
Radlauer, Madalyn R.; Agapie, Theodor; Organometallics 33 (2014) 3247–3250; doi:10.1021/om500608j

data_4089667
_publ_section_title
;
 Bimetallic Zirconium Amine Bis(phenolate) Polymerization Catalysts:
 Enhanced Activity and Tacticity Control for Polyolefin Synthesis.
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3247
_journal_page_last               3250
_journal_paper_doi               10.1021/om500608j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C39 H47 Cl2 N O3 Zr'
_chemical_formula_sum            'C39 H47 Cl2 N O3 Zr'
_chemical_formula_weight         739.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601),
 SHELXL-2013,
 and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 101.11(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.100(2)
_cell_length_b                   21.150(4)
_cell_length_c                   17.180(3)
_cell_measurement_temperature    100
_cell_volume                     3601.1(12)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'BluIce (SSRL, 2001)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013/2 (Sheldrick, 2013)'
_computing_structure_solution    'XT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SSRL BL 12-2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'K-B focussing mirrors'
_diffrn_radiation_monochromator  'liquid nitrogen-cooled double Si(111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.95369
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            58273
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        34.905
_diffrn_reflns_theta_max         33.976
_diffrn_reflns_theta_min         2.073
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0187P)^2^+6.6762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5622
_reflns_number_total             6007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500608j_si_002.cif
_cod_data_source_block           mrr-6-107
_cod_original_cell_volume        3601.1(13)
_cod_database_code               4089667
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B),
 C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C)
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