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_7714571
_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_absolute_configuration uk
_chemical_formula_moiety         'C80 H92 Hf2 N2 O4, 4[C4H8O]'
_chemical_formula_sum            'C96 H124 Hf2 N2 O8'
_chemical_formula_weight         1790.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0624(6)
_cell_length_b                   44.306(2)
_cell_length_c                   15.5799(7)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      74.53
_cell_measurement_theta_min      3.01
_cell_volume                     8326.5(7)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics
'Bruker Apex3, Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material
'Bruker Apex3, Olex2 1.5-dev (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      233.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            127643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.003
_diffrn_reflns_theta_min         3.007
_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    4.972
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1091 before and 0.0706 after correction.
The Ratio of minimum to maximum transmission is 0.7251.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.087(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         16911
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.7708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                16173
_reflns_number_total             16911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03641c2.cif
_cod_data_source_block           111120a_yufang
_cod_depositor_comments
'Adding full bibliography for 7714567--7714572.cif.'
_cod_original_cell_volume        8326.6(7)
_cod_database_code               7714571
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.913(8)
 0.087(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{C53, C53A}
4. Restrained distances
 C33-C34 = C33-C35 = C33-C36
 1.54 with sigma of 0.02
 C33A-C34A = C33A-C35A = C33A-C36A
 1.54 with sigma of 0.02
 C53-C54 = C54-C55 = C55-C56 = C56-C57 = C57-C58 = C58-C53
 1.39 with sigma of 0.02
 C53A-C54A = C54A-C55A = C55A-C56A = C56A-C57A = C57A-C58A = C58A-C53A
 1.39 with sigma of 0.02
 C34A-C35A = C35A-C36A = C36A-C34A
 2.52 with sigma of 0.01
 C34-C35 = C35-C36 = C36-C34
 2.52 with sigma of 0.04
5. Rigid bond restraints
 C33, C34, C35, C36, C33A, C34A, C35A, C36A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C53, C54, C55, C56, C57, C58, C53A, C54A, C55A, C56A, C57A, C58A
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
6. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C33A \\sim C34A \\sim C35A \\sim C36A:
within 2A with sigma of 0.005 and sigma for terminal atoms of 2 within 2A
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C53A \\sim C54A
\\sim C55A \\sim C56A \\sim C57A \\sim C58A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35A) \\sim Ueq,
Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C53A) \\sim Ueq,
Uanis(C54A) \\sim Ueq, Uanis(C55A) \\sim Ueq, Uanis(C56A) \\sim Ueq,
Uanis(C57A) \\sim Ueq, Uanis(C58A) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C53) = Uanis(C53A)
7. Others
 Fixed Sof: C33(0.6) C34(0.6) H34A(0.6) H34B(0.6) H34C(0.6) C35(0.6) H35A(0.6)
 H35B(0.6) H35C(0.6) C36(0.6) H36A(0.6) H36B(0.6) H36C(0.6) C33A(0.4) C34A(0.4)
 H34D(0.4) H34E(0.4) H34F(0.4) C35A(0.4) H35D(0.4) H35E(0.4) H35F(0.4)
 C36A(0.4) H36D(0.4) H36E(0.4) H36F(0.4) H52A(0.5) H52B(0.5) H52C(0.5)
 H52D(0.5) C53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5) H56(0.5)
 C57(0.5) H57(0.5) C58(0.5) H58(0.5) C53A(0.5) C54A(0.5) H54A(0.5) C55A(0.5)
 H55A(0.5) C56A(0.5) H56A(0.5) C57A(0.5) H57A(0.5) C58A(0.5) H58A(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C52(H52A,H52B), C52(H52C,H52D), 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)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), 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), C54A(H54A),
 C55A(H55A), C56A(H56A), C57A(H57A), C58A(H58A), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
8.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), C34A(H34D,H34E,H34F),
 C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F), 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 614 electrons were 
found in a volume of 1978\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[C4H8O] per Formula Unit 
which account for 640 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              632
_shelx_fab_checksum              43841
_olex2_submission_special_instructions 'No special instructions were received'