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_1568048
_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 Nd2 Si8'
_chemical_formula_sum            'C44 H84 I2 Nd2 Si8'
_chemical_formula_weight         1380.11
_chemical_name_systematic        '[{Nd(Cp'')2(uI)}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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-15
_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                73.257(3)
_cell_angle_beta                 83.329(2)
_cell_angle_gamma                78.423(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7367(3)
_cell_length_b                   11.5169(3)
_cell_length_c                   13.3589(4)
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      75.9850
_cell_measurement_theta_min      3.4320
_cell_volume                     1546.66(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.949
_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    119.00 163.00   1.00    1.00    --  108.20  19.00  35.00   44
  2  \w     35.00 108.00   1.00    1.00    --  108.20  19.00  35.00   73
  3  \w    -44.00  17.00   1.00    1.00    --   44.60  60.00-150.00   61
  4  \w     18.00  45.00   1.00    1.00    --   44.60  19.00  35.00   27
  5  \w    -44.00  39.00   1.00    1.00    --   44.60  60.00  90.00   83
  6  \w     71.00 106.00   1.00    1.00    --   44.60  60.00-150.00   35
  7  \w    -45.00  68.00   1.00    1.00    --   44.60  60.00 -30.00  113
  8  \w     77.00 113.00   1.00    1.00    --   44.60  60.00 -30.00   36
  9  \w     99.00 133.00   1.00    1.00    --   44.60  60.00  90.00   34
 10  \w     44.00  78.00   1.00    1.00    --   44.60  60.00  90.00   34
 11  \w    -45.00  57.00   1.00    1.00    --   44.60  60.00 -90.00  102
 12  \w     65.00 133.00   1.00    1.00    --   44.60  60.00 -90.00   68
 13  \w     20.00 137.00   1.00    1.00    --  108.20  50.00-180.00  117
 14  \w    126.00 188.00   1.00    1.00    --  108.20  50.00  90.00   62
 15  \w     21.00  73.00   1.00    1.00    --  108.20  50.00  90.00   52
 16  \w    149.00 198.00   1.00    1.00    --  108.20  50.00-180.00   49
 17  \w     22.00 198.00   1.00    1.00    --  108.20  50.00 120.00  176
 18  \w    152.00 179.00   1.00    1.00    --  108.20  50.00-150.00   27
 19  \w    147.00 194.00   1.00    1.00    --  108.20  50.00 150.00   47
 20  \w     75.00 161.00   1.00    1.00    --  108.20  50.00   0.00   86
 21  \w     37.00  71.00   1.00    1.00    --  108.20  50.00   0.00   34
 22  \w     50.00  75.00   1.00    1.00    --  108.20  50.00 150.00   25
 23  \w    120.00 196.00   1.00    1.00    --  108.20  50.00  30.00   76
 24  \w     19.00 198.00   1.00    1.00    --  108.20  50.00 -30.00  179
 25  \w    114.00 198.00   1.00    1.00    --  108.20  50.00 -90.00   84
 26  \w     23.00  91.00   1.00    1.00    --  108.20  50.00 -90.00   68
 27  \w     61.00  87.00   1.00    1.00    --  108.20  50.00  30.00   26
 28  \w     40.00  65.00   1.00    1.00    --  108.20  50.00-150.00   25
;
_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      -0.0790340000
_diffrn_orient_matrix_UB_12      0.1310908000
_diffrn_orient_matrix_UB_13      -0.0225343000
_diffrn_orient_matrix_UB_21      -0.1233670000
_diffrn_orient_matrix_UB_22      -0.0543151000
_diffrn_orient_matrix_UB_23      0.0310940000
_diffrn_orient_matrix_UB_31      0.0083375000
_diffrn_orient_matrix_UB_32      -0.0001383000
_diffrn_orient_matrix_UB_33      0.1143858000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18441
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.219
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.162
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.137
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       needle
_exptl_crystal_F_000             686
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method
'Crystallised from concentrated toluene at -25oC'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.047
_refine_diff_density_max         3.273
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0680P)^2^+0.6420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5784
_reflns_number_total             6153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04526e2.cif
_cod_data_source_block           2-Nd
_cod_depositor_comments
'Adding full bibliography for 1568047--1568055.cif.'
_cod_database_code               1568048
_manchester_internal_diff_code   ldpm177
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   27/11/2020
_manchester_internal_process_date 27/11/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 11/12/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 11/12/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 15/12/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 15/12/2020
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Nd2 I2 Si8 C44'
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.860
_reflns_odcompleteness_completeness 98.00
_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:
 C1(H1), C6(H6), C7(H7), C12(H12), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              95332
_shelx_hkl_checksum              24993
_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_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR4.347
_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 2.085
_oxdiff_exptl_absorpt_empirical_full_min 0.461