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_1543104
_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         'C72 H126 N Na1 O6 Si4 U2'
_chemical_formula_sum            'C120 H204 N2 Na O6 Si8 U4'
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_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
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_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                98.997(3)
_cell_angle_beta                 99.477(2)
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_cell_length_b                   13.4214(5)
_cell_length_c                   21.7314(6)
_cell_measurement_reflns_used    9152
_cell_measurement_temperature    173(2)
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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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)
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_computing_data_reduction
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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)
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_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'DIRDIFF 2008'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
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_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.982
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_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_k_max       16
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_diffrn_reflns_limit_l_min       -24
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_diffrn_reflns_theta_min         3.593
_diffrn_source                   'sealed X-ray tube'
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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)
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            'dark brown'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1477
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/THF'
_exptl_crystal_size_max          0.150
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     148
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+3.8670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9505
_reflns_number_total             11925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00632a2.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1543100--1543105.cif.

2023-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1485.33
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C60 H102 N Na0.50 O3 Si4 U2'
_cod_database_code               1543104
_shelx_estimated_absorpt_t_min   0.213
_shelx_estimated_absorpt_t_max   0.382
_shelxl_version_number           2013-3
_shelx_res_checksum              91758