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_7713012
_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         'C25 H53 Cl Hf Si6'
_chemical_formula_sum            'C25 H53 Cl Hf Si6'
_chemical_formula_weight         736.15
_chemical_name_systematic        '[Hf(Cp')2(Cl){Si(SiMe3)3}]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-17
_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                90
_cell_angle_beta                 106.407(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6504(3)
_cell_length_b                   15.5103(3)
_cell_length_c                   19.0960(5)
_cell_measurement_reflns_used    10263
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8060
_cell_measurement_theta_min      3.1070
_cell_volume                     3594.28(16)
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.880
_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    -19.00  25.00   1.00    2.00    --  -18.77 -99.00   0.00   44
  2  \w     -2.00  89.00   1.00    2.00    --   20.02  57.00   0.00   91
  3  \w    -51.00  51.00   1.00    2.00    --   20.02 -77.00 120.00  102
  4  \w    -49.00  42.00   1.00    2.00    --   20.02 -57.00-150.00   91
;
_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      -0.0578711000
_diffrn_orient_matrix_UB_12      0.0020411000
_diffrn_orient_matrix_UB_13      -0.0159981000
_diffrn_orient_matrix_UB_21      0.0080893000
_diffrn_orient_matrix_UB_22      0.0003973000
_diffrn_orient_matrix_UB_23      -0.0352556000
_diffrn_orient_matrix_UB_31      -0.0024750000
_diffrn_orient_matrix_UB_32      -0.0456657000
_diffrn_orient_matrix_UB_33      -0.0010329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.073
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.752
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 'Recrystallised from pentane at -25 oC'
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7137
_reflns_number_total             8467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00987d2.cif
_cod_data_source_block           2
_cod_original_cell_volume        3594.28(15)
_cod_database_code               7713012
_manchester_internal_diff_code   adpm643
_manchester_internal_coll_client BR
_manchester_internal_coll_user   BR
_manchester_internal_coll_date   17/12/2019
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_process_date 17/12/2019
_manchester_internal_process_user BR
_manchester_internal_solution_date 17/12/2019
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 17/12/2019
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 10/01/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 10/01/2020
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.175
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              97157
_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR3.257
_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 2.665
_oxdiff_exptl_absorpt_empirical_full_min 0.526