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_4117708
_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
;
 Synthesis of Uranium(VI) Terminal Oxo Complexes: Molecular Geometry
 Driven by the Inverse Trans-Influence
;
_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         'C51 H78 N3 O4 U, F6 Sb, 3.5(C6 H6)'
_chemical_formula_sum            'C72 H99 F6 N3 O4 Sb U'
_chemical_formula_weight         1544.32
_chemical_name_systematic
; 
 ? 
;
_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                 122.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.190(5)
_cell_length_b                   38.864(8)
_cell_length_c                   18.569(4)
_cell_measurement_reflns_used    127
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     14067(7)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_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 9
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 1.70 \% and 310 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       26
_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       -18
_diffrn_reflns_number            52265
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.747
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             6248
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 10717 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.309(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1582
_refine_ls_number_reflns         25447
_refine_ls_number_restraints     440
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+14.8726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                19879
_reflns_number_total             25447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211618v_si_002.cif
_cod_data_source_block           bk1017
_cod_depositor_comments
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The following automatic conversions were performed:
data name '_publ_author_addres' replaced with '_publ_author_address'
as specified in the replacement file
'/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               4117708