Comparison of group 4 and thorium M(IV) substituted cyclopentadienyl silanide complexes
Réant, Benjamin Luke Leonard; De Alwis Jayasinghe, Dukula Prathapa Bilesha; Wooles, Ashley; Liddle, Stephen; Mills, David P.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00987D

data_7713013
_publ_section_title
;
 Comparison of group 4 and thorium M(IV) substituted cyclopentadienyl
 silanide complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00987D
_journal_year                    2023
_chemical_formula_moiety         'C30 H40 Hf Si2'
_chemical_formula_sum            'C30 H40 Hf Si2'
_chemical_formula_weight         635.29
_chemical_name_systematic        '[Hf(Cp')2(Bn)2]'
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2023-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                86.723(3)
_cell_angle_beta                 74.850(4)
_cell_angle_gamma                63.240(5)
_cell_formula_units_Z            4
_cell_length_a                   12.1816(6)
_cell_length_b                   13.2144(6)
_cell_length_c                   20.7629(8)
_cell_measurement_reflns_used    6702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5290
_cell_measurement_theta_min      2.3500
_cell_volume                     2873.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  41.00   1.00    3.16    --   20.18  77.00-180.00   46
  2  \w     48.00  89.00   1.00    3.16    --   20.18  57.00-180.00   41
  3  \w     -4.00  40.00   1.00    3.16    --   20.18  77.00   0.00   44
  4  \w     -5.00  42.00   1.00    3.16    --   20.18  77.00 -90.00   47
  5  \w    -11.00  25.00   1.00    3.16    --   20.18  77.00 150.00   36
  6  \w    -28.00  88.00   1.00    3.16    --   20.18  19.00   0.00  116
  7  \w    -49.00  41.00   1.00    3.16    --   20.18 -57.00  30.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0389423000
_diffrn_orient_matrix_UB_12      0.0282691000
_diffrn_orient_matrix_UB_13      -0.0066492000
_diffrn_orient_matrix_UB_21      -0.0102077000
_diffrn_orient_matrix_UB_22      0.0091636000
_diffrn_orient_matrix_UB_23      0.0348491000
_diffrn_orient_matrix_UB_31      0.0543252000
_diffrn_orient_matrix_UB_32      -0.0524266000
_diffrn_orient_matrix_UB_33      -0.0003578000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.084
_diffrn_reflns_theta_min         2.037
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.729
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method
'Crystallised from concentrated pentane at -25oC'
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.147
_refine_diff_density_max         2.419
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         13234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.3388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9151
_reflns_number_total             13234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00987d2.cif
_cod_data_source_block           6
_cod_database_code               7713013
_manchester_internal_diff_code   adpm680
_manchester_internal_coll_client GW
_manchester_internal_coll_user   GW
_manchester_internal_coll_date   24/07/2021
_manchester_internal_process_date 24/07/2021
_manchester_internal_process_user BR
_manchester_internal_solution_date 28/07/2021
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 28/07/2021
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 25/01/2023
_manchester_internal_validation_user AW
_manchester_internal_archive_date 25/01/2023
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.469
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C1(H1A,H1B), C8(H8A,H8B), C31(H31A,H31B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49), C50(H50), C51(H51),
  C52(H52), C57(H57), C58(H58), C59(H59), C60(H60)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C)
;
_shelx_res_checksum              98538
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 3.16s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_type   custom
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.594
_oxdiff_exptl_absorpt_empirical_full_min 0.538