Coplanar binuclear group 4 post-metallocene complexes supported by chelating μ-(σ<sub>2</sub>-aryl) ligands: characterisation and olefin polymerisation catalysis.
Li, Yufang; Liu, Qian; Bao, Junhui; Yiu, Shek-Man; Chan, Michael C. W.; Dalton transactions (Cambridge, England : 2003) 53 (2023) 346–353; doi:10.1039/d3dt03641c

data_7714570
_publ_section_title
;
 Coplanar binuclear group 4 post-metallocene complexes supported by
 chelating &#x3bc;-(&#x3c3;<sub>2</sub>-aryl) ligands: characterisation
 and olefin polymerisation catalysis.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              346
_journal_page_last               353
_journal_paper_doi               10.1039/d3dt03641c
_journal_volume                  53
_journal_year                    2023
_chemical_formula_moiety         'C80 H91 F N2 O4 Zr2, 2[C5H12]'
_chemical_formula_sum            'C90 H115 F N2 O4 Zr2'
_chemical_formula_weight         1490.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                105.9500(10)
_cell_angle_beta                 103.4350(10)
_cell_angle_gamma                102.2070(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4505(4)
_cell_length_b                   17.7306(4)
_cell_length_c                   22.2391(6)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.37
_cell_volume                     4035.4(2)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics
'Bruker Apex3, Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
'Bruker Apex3, Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement
'SHELXL-2016/6 (Sheldrick, 2016), olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47625
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'micro focus'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1007 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.9434.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         16476
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+1.8771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12549
_reflns_number_total             16476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03641c2.cif
_cod_data_source_block           081121a_yufang
_cod_depositor_comments
'Adding full bibliography for 7714567--7714572.cif.'
_cod_database_code               7714570
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 C33-C34 = C33-C35 = C33-C36
 1.54 with sigma of 0.02
 C37-C38 = C37-C39 = C37-C40
 1.54 with sigma of 0.02
 C37A-C38A = C37A-C39A = C37A-C40A
 1.54 with sigma of 0.02
 C34-C35 = C35-C36 = C36-C34
 2.5 with sigma of 0.04
 C38-C39 = C39-C40 = C40-C38
 2.5 with sigma of 0.04
 C38A-C39A = C39A-C40A = C40A-C38A
 2.5 with sigma of 0.04
3. Rigid bond restraints
 C33, C34, C35, C36, C37, C38, C39, C40, C37A, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim
C37A \\sim C38A \\sim C39A \\sim C40A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C39A)
\\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma of 0.03 and sigma for terminal
atoms of 0.06
5. Others
 Fixed Sof: C37(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C37A(0.5) C38A(0.5)
 H38D(0.5) H38E(0.5) H38F(0.5) C39A(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
 C40A(0.5) H40D(0.5) H40E(0.5) H40F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C52(H52A,H52B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C70(H70A,H70B), C77(H77A,H77B),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C17(H17), C19(H19), C20(H20),
 C21(H21), C24(H24), C26(H26), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
6.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C38A(H38D,H38E,H38F), C39A(H39D,H39E,H39F),
 C40A(H40D,H40E,H40F), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 157 electrons were 
found in a volume of 881\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C5H12] per Formula Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98144
_shelx_fab_checksum              11697
_olex2_submission_special_instructions 'No special instructions were received'