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

data_7120779
_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            'C46 H101 Ce Cl O14.5 Si3'
_chemical_formula_weight         1146.10
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 107.3820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8822(13)
_cell_length_b                   14.2617(8)
_cell_length_c                   38.922(2)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.153
_cell_volume                     13181.2(12)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            87507
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.138
_diffrn_reflns_theta_min         1.666
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadbas
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 8452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1481
_refine_ls_number_reflns         24728
_refine_ls_number_restraints     1574
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.728
_reflns_Friedel_fraction_full    0.741
_reflns_Friedel_fraction_max     0.713
_reflns_number_gt                22689
_reflns_number_total             24728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06499c2.cif
_cod_data_source_block           3_Multijfr109_0m
_cod_original_cell_volume        13181.1(12)
_cod_original_formula_sum        'C46 H101 Ce Cl O14.50 Si3'
_cod_database_code               7120779
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              2819