Reactions of a cerium(iii) amide with heteroallenes: insertion, silyl-migration and de-insertion.
Yin, Haolin; Carroll, Patrick J.; Schelter, Eric J.; Chemical communications (Cambridge, England) 52 (2016) 9813–9816; doi:10.1039/c6cc03719d

data_7124682
_publ_section_title
;
 Reactions of a cerium(iii) amide with heteroallenes: insertion,
 silyl-migration and de-insertion.
;
_journal_issue                   63
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9813
_journal_page_last               9816
_journal_paper_doi               10.1039/c6cc03719d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C66 H57 Ce F15 N3 O2 P2 S6 Si3'
_chemical_formula_weight         1687.84
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-29 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.799(2)
_cell_angle_beta                 87.413(2)
_cell_angle_gamma                75.372(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5981(6)
_cell_length_b                   14.8764(7)
_cell_length_c                   21.2531(9)
_cell_measurement_reflns_used    9025
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.84
_cell_volume                     4032.2(3)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            97499
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1702
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         18193
_refine_ls_number_restraints     1002
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0468P)^2^+11.1031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                15214
_reflns_number_total             18193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc03719d2.cif
_cod_data_source_block           UP4579
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               7124682