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_7705221
_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         'C54 H94 N4 U, 2(B C24 F20)'
_chemical_formula_sum            'C102 H94 B2 F40 N4 U'
_chemical_formula_weight         2395.46
_chemical_name_systematic
'Bis(1,2,3,4-tetrakis(iso-propyl)cyclopentadienyl)-tetrakis(tert-butyl-isocyano)-uranium(iv) bis(tetrakis(pentafluorophenyl)borate)'
_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             2020-04-23
_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                105.1690(10)
_cell_angle_beta                 111.9920(10)
_cell_angle_gamma                95.6830(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9587(3)
_cell_length_b                   13.9699(6)
_cell_length_c                   16.9802(4)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.18
_cell_volume                     2890.57(16)
_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 0.989
_diffrn_measured_fraction_theta_max 0.988
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32610
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.367
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.4902
_exptl_absorpt_correction_T_min  0.4300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether/THF (20:1)'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.758
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         10440
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1269P)^2^+5.1210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9421
_reflns_number_total             10440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02005b2.cif
_cod_data_source_block           mab_iv_007_0ma
_cod_depositor_comments
'Adding full bibliography for 7705221--7705223.cif.'
_cod_original_cell_volume        2890.56(16)
_cod_database_code               7705221
_shelx_shelxl_version_number     2014/7
_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
C12 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.1
Uanis(C9) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C6(H6), C15(H15)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C27(H27A,H27B,
 H27C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C20(H20A,
 H20B,H20C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C8(H8A,
 H8B,H8C), C26(H26A,H26B,H26C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              88691
_shelx_fab_checksum              11018
_olex2_submission_special_instructions 'No special instructions were received'