Isocyanide adducts of tri- and tetravalent uranium metallocenes supported by tetra(isopropyl)cyclopentadienyl ligands.
Boreen, Michael A.; Groß, Oliver A; Hohloch, Stephan; Arnold, John; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11971–11977; doi:10.1039/d0dt02005b

data_7705222
_publ_section_title
;
 Isocyanide adducts of tri- and tetravalent uranium metallocenes supported
 by tetra(isopropyl)cyclopentadienyl ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11971
_journal_page_last               11977
_journal_paper_doi               10.1039/d0dt02005b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C39 H67 I N U'
_chemical_formula_sum            'C39 H67 I N U'
_chemical_formula_weight         914.86
_chemical_name_systematic
Bis(1,2,3,4-tetrakis(iso-propyl)cyclopentadienyl)-(tert-butyl-isocyano)-iodo-uranium(iii)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-28 deposited with the CCDC.	2020-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                100.465(5)
_cell_angle_beta                 96.791(5)
_cell_angle_gamma                110.915(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3988(9)
_cell_length_b                   11.2181(11)
_cell_length_c                   18.702(2)
_cell_measurement_reflns_used    8074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.30
_cell_volume                     1963.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    SHELXT-2014
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20926
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.003
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.943
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.3401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       Plate
_exptl_crystal_F_000             906
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.628
_refine_diff_density_min         -2.862
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7025
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5777
_reflns_number_total             7025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02005b2.cif
_cod_data_source_block           mab_iii_194_0ma
_cod_depositor_comments
'Adding full bibliography for 7705221--7705223.cif.'
_cod_original_cell_volume        1963.8(4)
_cod_database_code               7705222
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.360
_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. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C21) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3.a Ternary CH refined with riding coordinates:
 C26(H26), C15(H15), C29(H29), C12(H12), C9(H9), C23(H23), C6(H6), C32(H32)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C28(H28A,H28B,
 H28C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C30(H30A,
 H30B,H30C), C38(H38A,H38B,H38C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C),
 C39(H39A,H39B,H39C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C37(H37A,H37B,
 H37C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C34(H34A,
 H34B,H34C)
;
_shelx_res_checksum              36828
_olex2_submission_special_instructions 'No special instructions were received'