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_7713015
_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         'C31 H69 Cl Si8 Th'
_chemical_formula_sum            'C31 H69 Cl Si8 Th'
_chemical_formula_weight         934.07
_chemical_name_systematic        '[Th(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             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                90
_cell_angle_beta                 144.858(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9729(11)
_cell_length_b                   35.7285(5)
_cell_length_c                   11.2395(6)
_cell_measurement_reflns_used    35771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1820
_cell_measurement_theta_min      2.4310
_cell_volume                     4616.7(14)
_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_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_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     84.00 133.00   1.00    1.00    --   44.80  40.00-180.00   49
  2  \w     12.00  39.00   1.00    1.00    --   44.80  10.00   0.00   27
  3  \w    -44.00 125.00   1.00    1.00    --   44.80  30.00-120.00  169
  4  \w    -43.00   0.00   1.00    1.00    --   44.80  10.00   0.00   43
  5  \w    -42.00  17.00   1.00    1.00    --   44.80  40.00-180.00   59
  6  \w     90.00 116.00   1.00    1.00    --   44.80  20.00   0.00   26
  7  \w    -27.00 115.00   1.00    1.00    --   44.80  20.00 150.00  142
  8  \w     70.00 134.00   1.00    1.00    --   44.80  10.00   0.00   64
  9  \w    137.00 196.00   1.00    1.00    --  108.20  57.00 133.58   59
 10  \w    123.00 156.00   1.00    1.00    --  108.20  20.00 -90.00   33
 11  \w     19.00 132.00   1.00    1.00    --  108.20  57.00 133.58  113
 12  \w     19.00 196.00   1.00    1.00    --  108.20  50.00-120.00  177
 13  \w    163.00 189.00   1.00    1.00    --  108.20  58.00 115.88   26
 14  \w     26.00  98.00   1.00    1.00    --  108.20  20.00 -90.00   72
 15  \w     21.00 156.00   1.00    1.00    --  108.20  30.00-180.00  135
 16  \w    130.00 157.00   1.00    1.00    --  108.20  56.00 126.46   27
 17  \w     19.00 146.00   1.00    1.00    --  108.20  40.00 -60.00  127
 18  \w     69.00 197.00   1.00    1.00    --  108.20  50.00-180.00  128
 19  \w     66.00 170.00   1.00    1.00    --  108.20   0.00 -60.00  104
 20  \w     19.00  38.00   1.00    1.00    --  108.20  56.00 126.46   19
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1307177000
_diffrn_orient_matrix_UB_12      0.0148888000
_diffrn_orient_matrix_UB_13      -0.1188723000
_diffrn_orient_matrix_UB_21      -0.1356786000
_diffrn_orient_matrix_UB_22      -0.0354185000
_diffrn_orient_matrix_UB_23      -0.0594920000
_diffrn_orient_matrix_UB_31      -0.1457592000
_diffrn_orient_matrix_UB_32      0.0195771000
_diffrn_orient_matrix_UB_33      -0.0171950000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43727
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.219
_diffrn_reflns_theta_min         2.473
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.069
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.357
_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    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 'Recrystallised from pentane at 5 oC'
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.173
_refine_diff_density_max         5.455
_refine_diff_density_min         -3.443
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+14.4850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9392
_reflns_number_total             9459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00987d2.cif
_cod_data_source_block           4
_cod_original_cell_volume        4616.6(9)
_cod_database_code               7713015
_manchester_internal_diff_code   ldpm137
_manchester_internal_coll_client BR/GW
_manchester_internal_coll_user   BR/GW
_manchester_internal_coll_date   08/11/2019
_manchester_internal_process_date 08/11/2019
_manchester_internal_process_user BR
_manchester_internal_solution_date 08/11/2019
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 08/11/2019
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 08/11/2019
_manchester_internal_validation_user AW
_manchester_internal_archive_date 08/11/2019
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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), C20(H20), C25(H25), C26(H26), C31(H31)
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), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              35462
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 1s
_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 7.493
_oxdiff_exptl_absorpt_empirical_full_min 0.502