Synthesis of Uranium(VI) Terminal Oxo Complexes: Molecular Geometry Driven by the Inverse Trans-Influence
Boris Kosog; Henry S. La Pierre; Frank W. Heinemann; Stephen T. Liddle; Karsten Meyer; Journal of the American Chemical Society 134 (2012) 5284–5289; doi:10.1021/ja211618v

data_4117710
_publ_contact_author
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        Prof. Dr. K. Meyer 
        Department of Chemistry and Pharmacy
        Inorganic Chemistry
        Universit\"at Erlangen-N\"urnberg 
        Egerlandstr. 1 
        D-91058 Erlangen 
        Bundesrepublik Deutschland 
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_publ_contact_author_email       Karsten.Meyer@chemie.uni-erlangen.de
_publ_contact_author_fax         '049 9131 852-7367'
_publ_contact_author_phone       '049 9131 852-7360'
_publ_section_title
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 Synthesis of Uranium(VI) Terminal Oxo Complexes: Molecular Geometry
 Driven by the Inverse Trans-Influence
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5284
_journal_page_last               5289
_journal_paper_doi               10.1021/ja211618v
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C51 H78 N3 O4 U), 2(F6 Sb), 7(C6 H6)'
_chemical_formula_sum            'C144 H198 F12 N6 O8 Sb2 U2'
_chemical_formula_weight         3088.64
_chemical_name_systematic
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 ? 
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_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 123.063(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.159(3)
_cell_length_b                   38.802(5)
_cell_length_c                   18.622(2)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.47
_cell_volume                     14024(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            87985
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    2.756
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             6248
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 14554 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.105(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1568
_refine_ls_number_reflns         30002
_refine_ls_number_restraints     581
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+4.8726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                20439
_reflns_number_total             30002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211618v_si_004.cif
_cod_data_source_block           bk1205
_cod_depositor_comments
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The following automatic conversions were performed:
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

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Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
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_cod_original_sg_symbol_Hall     C-2yc
_cod_database_code               4117710