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_7714572
_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 Hf2 N2 O4, 0.5[C4H8O]'
_chemical_formula_sum            'C82 H95 F Hf2 N2 O4.5'
_chemical_formula_weight         1556.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 99.6070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1231(5)
_cell_length_b                   22.0856(6)
_cell_length_c                   18.4615(6)
_cell_measurement_reflns_used    9650
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      74.66
_cell_measurement_theta_min      3.15
_cell_volume                     7285.8(4)
_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      233(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            151777
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.864
_diffrn_reflns_theta_min         3.146
_diffrn_source                   'micro focus'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.581
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1384 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.6949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         14938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+1.3044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13514
_reflns_number_total             14938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03641c2.cif
_cod_data_source_block           110320a_yufang
_cod_depositor_comments
'Adding full bibliography for 7714567--7714572.cif.'
_cod_original_formula_sum        'C82 H95 F Hf2 N2 O4.50'
_cod_database_code               7714572
_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.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C52(H52A,H52B), C59(H59A,H59B), C66(H66A,H66B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B)
2.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), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
2.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), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 80 electrons were 
found in a volume of 806\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[C4H8O] per Formula Unit 
which account for 80 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24184
_shelx_fab_checksum              62173
_olex2_submission_special_instructions 'No special instructions were received'