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_7705223
_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         'C44 H76 I N2 U, C24 B F20'
_chemical_formula_sum            'C68 H76 B F20 I N2 U'
_chemical_formula_weight         1677.04
_chemical_name_systematic
'Bis(1,2,3,4-tetrakis(iso-propyl)cyclopentadienyl)-bis(tert-butyl-isocyano)-iodo-uranium(iv) tetrakis(pentafluorophenyl)borate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 111.882(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2004(4)
_cell_length_b                   19.9489(3)
_cell_length_c                   19.6155(4)
_cell_measurement_reflns_used    35610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3760
_cell_measurement_theta_min      2.9470
_cell_volume                     6608.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -55.00  66.00   0.50    1.00    --  -17.33  72.00  79.00  242
  2  \w    -66.00  44.00   0.50    1.00    --   17.64 -72.00 -49.00  220
  3  \w     40.00  66.00   0.50    1.00    --   17.64  72.00  79.00   52
  4  \w   -108.00 -44.00   0.50    1.00    --  -17.33 179.00-180.00  128
  5  \w    -93.00 -44.00   0.50    1.00    --  -17.33-179.00  90.00   98
  6  \w    -43.00  23.00   0.50    1.00    --  -17.33 -77.00  60.00  132
  7  \w    -23.00  46.00   0.50    1.00    --   17.64  38.00 120.00  138
  8  \w    -45.00 -20.00   0.50    1.00    --   17.64 -77.00-180.00   50
  9  \w    -19.00   7.00   0.50    1.00    --   17.64 -77.00-180.00   52
 10  \w     56.00  82.00   0.50    1.00    --   17.64 179.00 120.00   52
 11  \w     59.00 100.00   0.50    1.00    --   17.64  38.00 120.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78798
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.801
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         13508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0288P)^2^+8.8803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11517
_reflns_number_total             13508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02005b2.cif
_cod_data_source_block           mab_iii_187
_cod_depositor_comments
'Adding full bibliography for 7705221--7705223.cif.'
_cod_database_code               7705223
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.496
_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 Ternary CH refined with riding coordinates:
 C23(H23), C12(H12), C32(H32), C26(H26), C6(H6), C29(H29), C9(H9), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C31(H31A,H31B,H31C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C24(H24A,
 H24B,H24C), C27(H27A,H27B,H27C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C),
 C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C42(H42A,H42B,
 H42C), C7(H7A,H7B,H7C), C33(H33A,H33B,H33C), C14(H14A,H14B,H14C), C44(H44A,
 H44B,H44C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              68822
_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
;