A New Tripodal Ligand System with Steric and Electronic Modularity for Uranium Coordination Chemistry
Suzanne C. Bart; Frank W. Heinemann; Christian Anthon; Christina Hauser; Karsten Meyer; Inorganic Chemistry 48 (2009) 9419–9426; doi:10.1021/ic9012697

data_4303312
_publ_contact_author
;                                                                               
        Prof. Dr. K. Meyer       
        Department of Chemistry and Pharmacy
        Inorganic Chemistry
        Universit\"at Erlangen-N\"urnberg                   
        Egerlandstr. 1                                     
        D-91058 Erlangen                               
        Bundesrepublik Deutschland                             
;
_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
;
A New Tripodal Ligand System with Steric and Electronic Modularity for
Uranium Coordination Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9419
_journal_page_last               9426
_journal_paper_doi               10.1021/ic9012697
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C54 H75 O3 U, 0.75(C5 H12), 0.25(C7 H8)'
_chemical_formula_sum            'C59.5 H86 O3 U'
_chemical_formula_weight         1087.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 132.596(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.768(5)
_cell_length_b                   11.3426(6)
_cell_length_c                   30.362(4)
_cell_measurement_reflns_used    245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     10589(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \w-rotations with 1.40 \% and 196 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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            110665
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    3.108
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         11678
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+29.5032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                9554
_reflns_number_total             11678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012697_si_001_4.cif
_cod_data_source_block           sd0730
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_formula_sum        'C59.50 H86 O3 U'
_cod_database_code               4303312