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_1568133
_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         'C40 H60 Ir4 U, C6 H14'
_chemical_formula_sum            'C46 H74 Ir4 U'
_chemical_formula_weight         1633.88
_chemical_melting_point          499
_chemical_name_systematic        U{(\m-H)3IrCp*}4
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 107.318(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8239(6)
_cell_length_b                   21.1789(6)
_cell_length_c                   17.2427(8)
_cell_measurement_reflns_used    16005
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.6730
_cell_measurement_theta_min      3.1950
_cell_volume                     5168.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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 0.997
_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    -19.00  45.00   0.50    2.50    --    2.33  77.00 -30.00  128
  2  \w    -20.00  15.00   0.50    2.50    --    2.33  77.00 -90.00   70
  3  \w     -8.00  38.00   0.50    2.50    --    2.33  77.00  90.00   92
  4  \w    -11.00  16.00   0.50    2.50    --    2.33 -99.00 -60.00   54
  5  \w    -12.00  35.00   0.50    2.50    --    2.33 -99.00-120.00   94
  6  \w    -12.00  25.00   0.50    2.50    --    2.33 -99.00  30.00   74
  7  \w    -11.00  36.00   0.50    2.50    --    2.33 -99.00  60.00   94
  8  \w    -25.00   0.00   0.50    2.50    --    2.33 -93.00  97.00   50
  9  \w    -27.00  -2.00   0.50    2.50    --   -2.02 -93.00  97.00   50
 10  \w    -26.00  -1.00   0.50    2.50    --   -2.02  93.00-150.00   50
;
_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      -0.0209561000
_diffrn_orient_matrix_UB_12      -0.0275919000
_diffrn_orient_matrix_UB_13      0.0104054000
_diffrn_orient_matrix_UB_21      -0.0453108000
_diffrn_orient_matrix_UB_22      0.0140593000
_diffrn_orient_matrix_UB_23      -0.0151920000
_diffrn_orient_matrix_UB_31      -0.0044380000
_diffrn_orient_matrix_UB_32      -0.0128049000
_diffrn_orient_matrix_UB_33      -0.0389425000
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31322
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.135
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.411
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_description       Rod
_exptl_crystal_F_000             3000
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.361
_refine_diff_density_min         -2.043
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.389
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5280
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0376
_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^)+269.2035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5003
_reflns_number_total             5280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04903a2.cif
_cod_data_source_block           czy_ii_020_b
_cod_depositor_comments
'Adding full bibliography for 1568133--1568135.cif.'
_cod_database_code               1568133
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'U Ir4 C46 H74'
_shelx_estimated_absorpt_t_max   0.413
_shelx_estimated_absorpt_t_min   0.108
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C5) = Uanis(C24)
Uanis(C3) = Uanis(C23)
Uanis(C2) = Uanis(C22)
Uanis(C8) = Uanis(C26)
Uanis(C7) = Uanis(C25)
Uanis(C13) = Uanis(C18)
Uanis(C9) = Uanis(C19)
Uanis(C10) = Uanis(C15)
3. Others
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C26)=Sof(C22)=Sof(C23)=Sof(C24)=
 Sof(C25)=1-FVAR(1)
 Sof(C2)=Sof(C5)=Sof(C7)=Sof(C3)=Sof(C8)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C1(H1A,H1B)
4.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C00C(H00A,H00B,H00C), C00L(H00D,H00E,H00F), C00X(H00G,
 H00H,H00I), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C),
  C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              77808
_shelx_hkl_checksum              35286
_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 4.487
_oxdiff_exptl_absorpt_empirical_full_min 0.722