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_1568051
_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         'C44 H84 I2 Si8 U2'
_chemical_formula_sum            'C44 H84 I2 Si8 U2'
_chemical_formula_weight         1567.69
_chemical_name_systematic        '[U(C5H3(1,3-SiMe3))2(I)]2'
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-14
_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                73.117(4)
_cell_angle_beta                 83.273(3)
_cell_angle_gamma                78.875(4)
_cell_formula_units_Z            1
_cell_length_a                   10.6833(4)
_cell_length_b                   11.4914(4)
_cell_length_c                   13.2297(5)
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1000
_cell_measurement_theta_min      3.4850
_cell_volume                     1521.72(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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   -100.00  -9.00   1.00    1.00    --  -45.40 -38.00  60.00   91
  2  \w    -86.00 -22.00   1.00    1.00    --  -45.40  76.00   0.00   64
  3  \w    -85.00 -55.00   1.00    1.00    --  -45.40  38.00  30.00   30
  4  \w    -75.00 -50.00   1.00    1.00    --  -45.40  57.00 -60.00   25
  5  \w   -135.00-109.00   1.00    1.00    --  -45.40 -38.00  60.00   26
  6  \w    -42.00  44.00   1.00    1.00    --  -45.40  57.00 -60.00   86
  7  \w   -113.00 -15.00   1.00    1.00    --  -45.40 -57.00-180.00   98
  8  \w    -24.00  41.00   1.00    1.00    --  -45.40  38.00  30.00   65
  9  \w   -147.00 -19.00   1.00    1.00    -- -107.20  76.00 -90.00  128
 10  \w   -148.00 -39.00   1.00    1.00    -- -107.20   0.00 150.00  109
 11  \w   -109.00 -83.00   1.00    1.00    -- -107.20 -57.00  30.00   26
 12  \w   -197.00 -80.00   1.00    1.00    -- -107.20 -38.00 -60.00  117
 13  \w   -109.00 -24.00   1.00    1.00    -- -107.20  57.00 -90.00   85
 14  \w    -55.00 -28.00   1.00    1.00    -- -107.20  76.00-150.00   27
 15  \w   -163.00-131.00   1.00    1.00    -- -107.20 -57.00  30.00   32
 16  \w   -134.00 -84.00   1.00    1.00    -- -107.20  76.00-150.00   50
 17  \w   -196.00 -68.00   1.00    1.00    -- -107.20 -38.00 -30.00  128
 18  \w   -121.00 -89.00   1.00    1.00    -- -107.20  76.00 120.00   32
 19  \w   -117.00 -82.00   1.00    1.00    -- -107.20  76.00-180.00   35
 20  \w    -96.00 -59.00   1.00    1.00    -- -107.20  76.00 -60.00   37
 21  \w   -131.00 -18.00   1.00    1.00    -- -107.20  76.00  30.00  113
 22  \w   -119.00 -94.00   1.00    1.00    -- -107.20  76.00 -30.00   25
 23  \w   -131.00 -99.00   1.00    1.00    -- -107.20  76.00  90.00   32
 24  \w   -140.00 -19.00   1.00    1.00    -- -107.20  76.00 150.00  121
 25  \w   -121.00 -96.00   1.00    1.00    -- -107.20  76.00-120.00   25
;
_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      -0.1020590000
_diffrn_orient_matrix_UB_12      -0.0373442000
_diffrn_orient_matrix_UB_13      0.0901217000
_diffrn_orient_matrix_UB_21      0.1061712000
_diffrn_orient_matrix_UB_22      -0.0672402000
_diffrn_orient_matrix_UB_23      0.0760451000
_diffrn_orient_matrix_UB_31      -0.0014440000
_diffrn_orient_matrix_UB_32      0.1194871000
_diffrn_orient_matrix_UB_33      0.0311007000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15458
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.523
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.072
_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            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method
'Crystallised from concentrated toluene solution at -25oC'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.051
_refine_diff_density_max         6.777
_refine_diff_density_min         -2.703
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0830P)^2^+4.0484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5285
_reflns_number_total             5530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04526e2.cif
_cod_data_source_block           2-U
_cod_depositor_comments
'Adding full bibliography for 1568047--1568055.cif.'
_cod_database_code               1568051
_manchester_internal_diff_code   rdpm227
_manchester_internal_coll_client AW
_manchester_internal_coll_user   AW
_manchester_internal_coll_date   06/08/2020
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_process_date 08/09/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 10/09/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 25/09/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 25/09/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 25/09/2020
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C44H84I2Si8U2
_chemical_oxdiff_usercomment     ' 	BR4.302'
_reflns_odcompleteness_completeness 99.39
_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:
 C21(H21), C22(H22), C11(H11), C5(H5), C16(H16), C6(H6)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C3(H3A,H3B,
 H3C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C2(H2A,H2B,H2C), C9(H9A,H9B,
 H9C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C1(H1A,H1B,
 H1C)
;
_shelx_res_checksum              24062
_shelx_hkl_checksum              39231
_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR4.302
_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 3.063
_oxdiff_exptl_absorpt_empirical_full_min 0.437