Steric control of redox events in organo-uranium chemistry: synthesis and characterisation of U(v) oxo and nitrido complexes
Tsoureas, Nikolaos; Kilpatrick, Alexander F. R.; Inman, Christopher J.; Cloke, F. Geoffrey N.; Chem. Sci. 7 (2016) 4624–; doi:10.1039/C6SC00632A

data_1543103
_publ_section_title
;
 Steric control of redox events in organo-uranium chemistry: synthesis and
 characterisation of U(v) oxo and nitrido complexes
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4624
_journal_paper_doi               10.1039/C6SC00632A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C22 H41.50 N0.50 Na0.50 O Si U0.50'
_chemical_formula_sum            'C22 H41.5 N0.5 Na0.5 O Si U0.5'
_chemical_formula_weight         487.65
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.2380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7251(2)
_cell_length_b                   18.7626(3)
_cell_length_c                   11.9516(2)
_cell_measurement_reflns_used    5838
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.4530
_cell_measurement_theta_min      4.1300
_cell_volume                     2394.99(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9704
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.569
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_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.344
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'intense brown'
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1002
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.540
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0359P)^2^+1.8726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4318
_reflns_number_total             4694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00632a2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 1543100--1543105.cif.'
_cod_original_formula_sum        'C22 H41.50 N0.50 Na0.50 O Si U0.50'
_cod_database_code               1543103
_shelx_estimated_absorpt_t_min   0.182
_shelx_estimated_absorpt_t_max   0.747
_shelxl_version_number           2013-3
_shelx_res_checksum              30794