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_7713011
_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         'C16 H26 Cl2 Hf Si2'
_chemical_formula_sum            'C16 H26 Cl2 Hf Si2'
_chemical_formula_weight         523.94
_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             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                68.257(6)
_cell_angle_beta                 75.092(8)
_cell_angle_gamma                81.994(7)
_cell_formula_units_Z            2
_cell_length_a                   6.7742(7)
_cell_length_b                   12.8385(8)
_cell_length_c                   12.8570(8)
_cell_measurement_reflns_used    7845
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6290
_cell_measurement_theta_min      3.2360
_cell_volume                     1002.46(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_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 0.998
_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    -46.00  52.00   1.00    2.50    --  -18.93  38.00   0.00   98
  2  \w    -11.00  85.00   1.00    2.50    --   20.18  77.00 -30.00   96
  3  \w    -10.00  91.00   1.00    2.50    --   20.18  77.00-150.00  101
  4  \w    -15.00  64.00   1.00    2.50    --   20.18 -99.00  60.00   79
  5  \w    -47.00  52.00   1.00    2.50    --   20.18 -77.00-150.00   99
  6  \w    -10.00  89.00   1.00    2.50    --   20.18  77.00  90.00   99
  7  \w    -52.00  41.00   1.00    2.50    --   20.18 -38.00  90.00   93
;
_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      0.1069797000
_diffrn_orient_matrix_UB_12      -0.0071887000
_diffrn_orient_matrix_UB_13      -0.0200795000
_diffrn_orient_matrix_UB_21      0.0178738000
_diffrn_orient_matrix_UB_22      0.0314165000
_diffrn_orient_matrix_UB_23      0.0316246000
_diffrn_orient_matrix_UB_31      0.0021767000
_diffrn_orient_matrix_UB_32      -0.0500760000
_diffrn_orient_matrix_UB_33      0.0480622000
_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     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3670
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.842
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.581
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.889
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.168
_refine_diff_density_max         7.083
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3670
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0770P)^2^+34.6537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3468
_reflns_number_total             3670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00987d2.cif
_cod_data_source_block           HfCp2Cl2
_cod_original_cell_volume        1002.46(14)
_cod_database_code               7713011
_manchester_internal_diff_code   adpm639
_manchester_internal_coll_client BR
_manchester_internal_coll_user   BR
_manchester_internal_coll_date   06/12/2019
_manchester_internal_process_date 06/12/2019
_manchester_internal_process_user BR
_manchester_internal_solution_date 06/12/2019
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 11/12/2019
_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         'C16 H26 Cl2 Hf Si2'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.590(5)
 0.410(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Si1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7 \\sim C8 \\sim C6:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Si1, C1, C2, C3, C4, C5, C7, C8, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              93567
_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 2.041
_oxdiff_exptl_absorpt_empirical_full_min 0.573