A versatile strategy for the formation of hydride-bridged actinide-iridium multimetallics.
Ye, Christopher Z.; Del Rosal, Iker; Boreen, Michael A.; Ouellette, Erik T.; Russo, Dominic R.; Maron, Laurent; Arnold, John; Camp, Clément; Chemical science 14 (2023) 861–868; doi:10.1039/d2sc04903a

data_1568135
_publ_section_title
;
 A versatile strategy for the formation of hydride-bridged
 actinide-iridium multimetallics.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              861
_journal_page_last               868
_journal_paper_doi               10.1039/d2sc04903a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C60 H90 Ir6 U2'
_chemical_formula_sum            'C60 H90 Ir6 U2'
_chemical_formula_weight         2440.57
_chemical_melting_point          600
_chemical_name_systematic        {U[(\m2-H3)IrCp*]2[(\m3-H2)IrCp*]}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
_audit_creation_date             2022-08-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-29 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                93.8150(10)
_cell_angle_beta                 98.6070(10)
_cell_angle_gamma                93.3650(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0833(2)
_cell_length_b                   15.2848(2)
_cell_length_c                   18.5723(3)
_cell_measurement_reflns_used    35113
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.8150
_cell_measurement_theta_min      3.1380
_cell_volume                     3375.78(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_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    -25.00  45.00   0.50    5.00    --   -2.02  77.00  30.00  140
  2  \w    -15.00  75.00   0.50    5.00    --   -2.02  38.00 120.00  180
  3  \w    -71.00  17.00   0.50    5.00    --    2.33 -57.00 150.00  176
  4  \w    -13.00  75.00   0.50    5.00    --    2.33  57.00-150.00  176
  5  \w    -20.00  45.00   0.50    5.00    --    2.33  77.00  60.00  130
  6  \w    -11.00  82.00   0.50    5.00    --    2.33  19.00 -60.00  186
  7  \w    -12.00  31.00   0.50    5.00    --    2.33 -99.00 -90.00   86
  8  \w      2.00  74.00   0.50    5.00    --    2.33  19.00  30.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027853000
_diffrn_orient_matrix_UB_12      0.0062698000
_diffrn_orient_matrix_UB_13      0.0384317000
_diffrn_orient_matrix_UB_21      0.0489788000
_diffrn_orient_matrix_UB_22      -0.0236958000
_diffrn_orient_matrix_UB_23      0.0048622000
_diffrn_orient_matrix_UB_31      0.0336927000
_diffrn_orient_matrix_UB_32      0.0396584000
_diffrn_orient_matrix_UB_33      0.0003048000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69850
_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         26.370
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_recrystallization_method
'Directly crystallized from a mixture of n-hexane solutions containing the starting materials.'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.008
_refine_diff_density_max         2.723
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         13763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+2.4164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12219
_reflns_number_total             13763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04903a2.cif
_cod_data_source_block           czy_i_146
_cod_depositor_comments
'Adding full bibliography for 1568133--1568135.cif.'
_cod_database_code               1568135
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'U Ir3 C30 H54'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C017(H01D,H01E,H01F), C018(H01G,H01H,H01I), C01E(H01,H,
 HA), C01F(H1,HB,HC), C01G(H01J,H01K,H01L), C01H(H2,HD,HE), C01I(H01M,H01N,
 H01O), C01J(H01P,H01Q,H01R), C01L(H3,HF,HG), C01M(H4,HH,HI), C01O(H01S,H01T,
 H01U), C01Q(H5,HJ,HK), C01R(H6,HL,HM), C01T(H01V,H01W,H01X), C01U(H7,HN,HO),
 C01V(H01Y,HP,HQ), C01W(H01Z,HR,HS), C021(H02A,H02B,H02C), C023(H02D,H02E,H02F),
  C024(H02G,H02H,H02I), C025(H02J,H02K,H02L), C029(H02P,H02Q,H02R), C02C(H02S,
 H02T,H02U), C02E(H02M,H02N,H02O), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              30149
_shelx_hkl_checksum              66924
_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 3.064
_oxdiff_exptl_absorpt_empirical_full_min 0.418