Oxidation in Nonclassical Organolanthanide Chemistry: Synthesis, Characterization, and X-ray Crystal Structures of Cerium(III) and -(IV) Amides
Peter B. Hitchcock; Alexander G. Hulkes; Michael F. Lappert; Inorganic Chemistry 43 (2004) 1031–1038; doi:10.1021/ic035100v

data_4310564
_publ_section_title
;
 Oxidation in Nonclassical Organolanthanide Chemistry: Synthesis,
 Characterization, and X-ray Crystal Structures of Cerium(III) and -(IV)
 Amides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1031
_journal_page_last               1038
_journal_paper_doi               10.1021/ic035100v
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H32 Br3 Ce O4'
_chemical_formula_structural     'C16 H32 Br3 Ce O4'
_chemical_formula_sum            'C16 H32 Br3 Ce O4'
_chemical_formula_weight         668.27
_chemical_name_common            '[CeBr3(thf)4]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-11-22T17:01:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.009(5)
_cell_angle_beta                 87.290(3)
_cell_angle_gamma                74.835(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2536(7)
_cell_length_b                   9.4157(5)
_cell_length_c                   15.5935(14)
_cell_measurement_reflns_used    7976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1148.17(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9106
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    7.217
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.749
_refine_diff_density_min         -2.446
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+4.2907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                4224
_reflns_number_total             5428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035100vsi20030917_111540_4.cif
_cod_data_source_block           nov2400
_cod_original_cell_volume        1148.17(15)
_cod_database_code               4310564