Pyridylamido hafnium complexes with a silylene bridge: synthesis and olefin polymerization.
Kulyabin, Pavel S.; Uborsky, Dmitry V.; Voskoboynikov, Alexander Z.; Canich, Jo Ann M.; Hagadorn, John R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6693–6702; doi:10.1039/d0dt01031f

data_7704175
_publ_section_title
;
 Pyridylamido hafnium complexes with a silylene bridge: synthesis and
 olefin polymerization.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6693
_journal_page_last               6702
_journal_paper_doi               10.1039/d0dt01031f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H46 Hf N2 Si'
_chemical_formula_sum            'C43 H46 Hf N2 Si'
_chemical_formula_weight         797.40
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-28 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.015(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.805(3)
_cell_length_b                   11.0536(19)
_cell_length_c                   19.590(3)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      2.18
_cell_volume                     3659.5(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.003
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0826 before and 0.0491 after correction. The Ratio of minimum to maximum transmission is 0.8077. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+4.2930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6986
_reflns_number_total             7973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01031f2.cif
_cod_data_source_block           pk1286
_cod_depositor_comments
'Adding full bibliography for 7704173--7704176.cif.'
_cod_original_cell_volume        3659.5(11)
_cod_database_code               7704175
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.653
_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 Ternary CH refined with riding coordinates:
 C25(H25), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C4(H4), C14(H14), C2(H2), C40(H40), C9(H9), C20(H20),
 C18(H18), C19(H19), C39(H39), C38(H38), C10(H10), C37(H37), C11(H11), C8(H8),
 C41(H41), C34(H34), C30(H30), C33(H33), C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              5543
_olex2_submission_special_instructions 'No special instructions were received'