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_4089669
_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         'C84 H100 N2 O6 Zr2'
_chemical_formula_sum            'C84 H100 N2 O6 Zr2'
_chemical_formula_weight         1416.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-12-18
_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                 105.5095(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6061(4)
_cell_length_b                   29.2804(13)
_cell_length_c                   17.7516(8)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.22
_cell_measurement_theta_min      2.20
_cell_volume                     4811.2(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2013.10-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.34A (Bruker-AXS, 2007)'
_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_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            139418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.160
_diffrn_reflns_theta_min         1.190
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0665 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.8589.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
 Solvent molecule disorder could not be resolved so squeeze was 
 employed. Data are listed for all voids in the P1 unit cell.
;
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 9431 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         37155
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                25563
_reflns_number_total             37155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500608j_si_002.cif
_cod_data_source_block           mrr35_sq
_cod_database_code               4089669
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.911
_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), C19(H19A,H19B), C20(H20A,H20B), C41(H41A,H41B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C57(H57A,H57B), C64(H64A,H64B),
  C71(H71A,H71B), C78(H78A,H78B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C33(H33), C35(H35), C44(H44), C46(H46),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67), C68(H68),
  C69(H69), C70(H70), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C)
;
_shelx_fab_checksum              84405