Facile formation of a homoleptic Ce(iv) amide via aerobic oxidation
Hitchcock, Peter B.; Lappert, Michael F.; Protchenko, Andrey V.; Chemical Communications  (2006) 3546–3548; doi:10.1039/b607429d

data_7111506
_publ_section_title
;
 Facile formation of a homoleptic Ce(iv) amide via aerobic oxidation
;
_journal_issue                   33
_journal_name_full               'Chemical Communications'
_journal_page_first              3546
_journal_page_last               3548
_journal_paper_doi               10.1039/b607429d
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H74 Ce N3 O, C7 H8'
_chemical_formula_sum            'C47 H82 Ce N3 O'
_chemical_formula_weight         845.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-09-22T17:02:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.189(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3004(2)
_cell_length_b                   23.4770(4)
_cell_length_c                   19.3077(3)
_cell_measurement_reflns_used    25568
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4580.29(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.945024E-1
_diffrn_orient_matrix_UB_12      0.16173E-2
_diffrn_orient_matrix_UB_13      0.250334E-1
_diffrn_orient_matrix_UB_21      0.292703E-1
_diffrn_orient_matrix_UB_22      -0.15057E-2
_diffrn_orient_matrix_UB_23      -0.464117E-1
_diffrn_orient_matrix_UB_31      -0.25569E-2
_diffrn_orient_matrix_UB_32      0.425375E-1
_diffrn_orient_matrix_UB_33      -0.25946E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39309
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.8216
_exptl_absorpt_correction_T_min  0.7678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+3.2837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.063
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                6438
_reflns_number_total             8044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b607429dsup1.cif
_cod_data_source_block           (1)-sep2804
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7111506