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_7713016
_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         'C28 H58 Hf Si6'
_chemical_formula_sum            'C28 H58 Hf Si6'
_chemical_formula_weight         741.77
_chemical_name_systematic        '[Hf(Cp')2(C3H5){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             2021-06-29
_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                 96.875(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3391(3)
_cell_length_b                   32.1430(10)
_cell_length_c                   11.9936(5)
_cell_measurement_reflns_used    8653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0250
_cell_measurement_theta_min      3.6150
_cell_volume                     3574.4(2)
_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    '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 0.998
_diffrn_measured_fraction_theta_max 0.842
_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    -30.00  12.00   0.50    1.00    --  -19.09 -77.00 -30.00   84
  2  \w    -86.00  16.00   0.50    1.00    --  -19.09 -19.00-150.00  204
  3  \w      2.00  49.50   0.50    1.00    --  -19.09  57.00  30.00   95
  4  \w     -7.00  29.00   0.50    1.00    --   20.18  77.00-120.00   72
;
_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      0.0063029000
_diffrn_orient_matrix_UB_12      0.0062171000
_diffrn_orient_matrix_UB_13      -0.0559462000
_diffrn_orient_matrix_UB_21      0.0202909000
_diffrn_orient_matrix_UB_22      -0.0205290000
_diffrn_orient_matrix_UB_23      -0.0131356000
_diffrn_orient_matrix_UB_31      -0.0734678000
_diffrn_orient_matrix_UB_32      -0.0051467000
_diffrn_orient_matrix_UB_33      -0.0158044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15712
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.168
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.135
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.210
_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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 'Crystallised from pentane at -25 oC'
_exptl_crystal_size_max          0.893
_exptl_crystal_size_mid          0.559
_exptl_crystal_size_min          0.416
_refine_diff_density_max         3.682
_refine_diff_density_min         -2.306
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6774
_reflns_number_total             8127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00987d2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'DIFMAP' was changed
to 'difmap' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        3574.5(2)
_cod_database_code               7713016
_manchester_internal_diff_code   adpm671
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   28/06/2021
_manchester_internal_process_date 28/06/2021
_manchester_internal_process_user BR
_manchester_internal_solution_date 28/06/2021
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 28/06/2021
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 29/06/2021
_manchester_internal_validation_user AW
_manchester_internal_archive_date 29/06/2021
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H58HfSi6
_reflns_odcompleteness_completeness 99.72
_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 Ternary CH refined with riding coordinates:
 C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28)
2.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
2.d Idealised Me refined as rotating group:
 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), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              87389
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.101
_oxdiff_exptl_absorpt_empirical_full_min 0.223