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_7704174
_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         'C41 H44 Hf N2 Si'
_chemical_formula_sum            'C41 H44 Hf N2 Si'
_chemical_formula_weight         771.36
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_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                98.919(4)
_cell_angle_beta                 95.327(4)
_cell_angle_gamma                106.367(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6765(9)
_cell_length_b                   11.0521(10)
_cell_length_c                   15.8719(14)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.24
_cell_volume                     1756.7(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24355
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.956
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0691 before and 0.0424 after correction. The Ratio of minimum to maximum transmission is 0.7945. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.224
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0262P)^2^+1.0782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6993
_reflns_number_total             7673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01031f2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7704173--7704176.cif.'
_cod_database_code               7704174
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.582
_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:
 C21(H21), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C40(H40A,H40B), C31(H31A,H31B), C39(H39A,H39B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C16(H16), C3(H3), C4(H4), C8(H8), C7(H7), C9(H9),
 C30(H30), C14(H14), C29(H29), C33(H33), C26(H26), C37(H37), C27(H27), C28(H28),
  C36(H36), C34(H34), C35(H35), C2(H2)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              73393
_olex2_submission_special_instructions 'No special instructions were received'