Synthesis and derivatisation of ceric tris(tert-butoxy)siloxides
Friedrich, Jochen; Maichle-moessmer, Caecilia; Anwander, Reiner; Chem. Commun.  (2017) –; doi:10.1039/C7CC06499C

data_7120774
_publ_section_title
;
 Synthesis and derivatisation of ceric tris(tert-butoxy)siloxides
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06499C
_journal_year                    2017
_chemical_formula_sum            'C72 H162 Ce2 O24 Si6'
_chemical_formula_weight         1860.79
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.351(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0279(10)
_cell_length_b                   14.1706(5)
_cell_length_c                   27.3540(10)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.769
_cell_volume                     10006.1(6)
_computing_cell_refinement       'APEX2 v2014.1-1 (Bruker AXS)'
_computing_data_collection       'COSMO v1.61'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            92996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.501
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.8630
_exptl_absorpt_correction_T_min  0.8000
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       needle
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         11012
_refine_ls_number_restraints     724
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+79.5989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8372
_reflns_number_total             11012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06499c2.cif
_cod_data_source_block           1_mo_jfr102b_07
_cod_database_code               7120774
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              85483