Electronic structure comparisons of isostructural early d- and f-block metal(iii) bis(cyclopentadienyl) silanide complexes.
Gransbury, Gemma K.; Réant, Benjamin L L; Wooles, Ashley J.; Emerson-King, Jack; Chilton, Nicholas F.; Liddle, Stephen T.; Mills, David P.; Chemical science 14 (2023) 621–634; doi:10.1039/d2sc04526e

data_1568049
_publ_section_title
;
 Electronic structure comparisons of isostructural early d- and f-block
 metal(iii) bis(cyclopentadienyl) silanide complexes.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              621
_journal_page_last               634
_journal_paper_doi               10.1039/d2sc04526e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C31 H69 Si8 Ti'
_chemical_formula_sum            'C31 H69 Si8 Ti'
_chemical_formula_weight         714.48
_chemical_name_systematic        '[Ti(Cp'')2{Si(SiMe3)3}]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.213(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2297(2)
_cell_length_b                   23.3116(4)
_cell_length_c                   18.6778(4)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9980
_cell_measurement_theta_min      1.7390
_cell_volume                     4369.08(15)
_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 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -38.00  33.00   1.00    5.00    --   -7.30  38.00 -60.00   71
  2  \w    -80.00  20.00   1.00    5.00    --   -7.30 -57.00  90.00  100
  3  \w    -66.00  -7.00   1.00    5.00    --   -7.30 -57.00 -30.00   59
  4  \w    -54.00  72.00   1.00    5.00    --   -7.50  19.00-120.00  126
  5  \w    -84.00 -12.00   1.00    5.00    --   -7.50   0.00  60.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0109236000
_diffrn_orient_matrix_UB_12      0.0296374000
_diffrn_orient_matrix_UB_13      -0.0073557000
_diffrn_orient_matrix_UB_21      -0.0636935000
_diffrn_orient_matrix_UB_22      -0.0021583000
_diffrn_orient_matrix_UB_23      0.0095053000
_diffrn_orient_matrix_UB_31      0.0287613000
_diffrn_orient_matrix_UB_32      0.0064703000
_diffrn_orient_matrix_UB_33      0.0367963000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26334
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         1.747
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.565
_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 blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(2)
_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     383
_refine_ls_number_reflns         8020
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                7530
_reflns_number_total             8020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04526e2.cif
_cod_data_source_block           3-Ti
_cod_depositor_comments
'Adding full bibliography for 1568047--1568055.cif.'
_cod_original_cell_volume        4369.09(17)
_cod_database_code               1568049
_manchester_internal_diff_code   rdpm242
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   15/10/2020
_manchester_internal_process_date 15/10/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 16/10/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 16/10/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 16/10/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 16/10/2020
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ti1 Si8 C31 H69'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(2)
 0.10(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C16(H16), C21(H21), C26(H26), C27(H27)
3.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),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              41883
_shelx_hkl_checksum              70000
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.789