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

data_7120780
_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            'C56 H121 Ce O17 Si3'
_chemical_formula_weight         1290.91
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.368(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6416(9)
_cell_length_b                   22.8253(13)
_cell_length_c                   18.8236(10)
_cell_measurement_reflns_used    9145
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.697
_cell_volume                     7144.0(7)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0642
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            166796
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.159
_diffrn_reflns_theta_min         1.403
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7250
_exptl_absorpt_correction_T_min  0.6560
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.264
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         19243
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+8.4412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15684
_reflns_number_total             19243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06499c2.cif
_cod_data_source_block           1a_jfr102a_0m
_cod_database_code               7120780
_shelx_estimated_absorpt_t_min   0.778
_shelx_estimated_absorpt_t_max   0.828
_shelxl_version_number           2013-3
_shelx_res_checksum              31352