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_4303311
_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 H78 O3, C2 H3 N'
_chemical_formula_sum            'C56 H81 N O3'
_chemical_formula_weight         816.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.168(5)
_cell_angle_beta                 104.788(4)
_cell_angle_gamma                111.500(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7954(4)
_cell_length_b                   14.2154(9)
_cell_length_c                   17.2602(15)
_cell_measurement_reflns_used    152
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     2567.7(3)
_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      150(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 2.00 \% and 180 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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55238
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.9675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                7119
_reflns_number_total             10486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012697_si_001_3.cif
_cod_data_source_block           ch0701
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4303311