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_4089668
_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         'C80 H88 Cl4 N2 O6 Zr2, 3(C7 H8), C6 H6'
_chemical_formula_sum            'C107 H118 Cl4 N2 O6 Zr2'
_chemical_formula_weight         1852.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9447(8)
_cell_length_b                   19.0668(10)
_cell_length_c                   29.5530(17)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      24.35
_cell_measurement_theta_min      2.33
_cell_volume                     9548.0(9)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.1157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            152911
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         1.608
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0690 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.9005.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       triangular
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 5869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.026(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         26017
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+9.4320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.2082
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                16063
_reflns_number_total             26017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500608j_si_002.cif
_cod_data_source_block           mrr33
_cod_database_code               4089668
_shelxl_version_number           2013-4
_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. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C37A \\sim C38A \\sim C39A \\sim C40A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) = Uanis(C37A)
3. Same fragment restrains
{C37, C38, C39, C40}
as
{C37A, C38A, C39A, C40A}
{C101, C102, C103, C104, C105, C106, C107}
as
{C201, C202, C203, C204, C205, C206, C207}
{C101, C102, C103, C104, C105, C106, C107}
as
{C401, C402, C403, C404, C405, C406, C407}
4. Others
 Sof(C37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
5.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), C53(H53A,H53B), C60(H60A,H60B),
  C67(H67A,H67B), C74(H74A,H74B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C33(H33), C35(H35), C44(H44), C46(H46),
 C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
 C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C201(H201), C202(H202), C203(H203),
 C204(H204), C205(H205), C301(H301), C302(H302), C303(H303), C304(H304),
 C305(H305), C306(H306), C401(H401), C402(H402), C403(H403), C404(H404),
 C405(H405)
5.c Idealised Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F)
5.d 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), C38A(H38D,H38E,H38F), C39A(H39D,H39E,H39F),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C107(H10A,H10B,H10C), C207(H20C,H20D,
 H20E), C407(H40G,H40H,H40I)
;
_shelx_res_checksum              91672
_shelx_hkl_checksum              19367