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

data_7120778
_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            'C44 H94 Ce Cl O13 Si2'
_chemical_formula_weight         1062.94
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 115.236(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.545(3)
_cell_length_b                   9.2664(15)
_cell_length_c                   20.324(3)
_cell_measurement_reflns_used    953
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.89
_cell_measurement_theta_min      2.582
_cell_volume                     2818.5(8)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0673
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.106
_diffrn_reflns_theta_min         1.361
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.7720
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       plate
_exptl_crystal_F_000             1130
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6192
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+3.0533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5016
_reflns_number_total             6192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06499c2.cif
_cod_data_source_block           6_firstmo_jfr129a_0m
_cod_database_code               7120778
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2013-3
_shelx_res_checksum              25485