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

data_7120776
_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            'C48 H108 Ce Cl O16 Si4 Zn'
_chemical_formula_weight         1294.64
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.639(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.237(2)
_cell_length_b                   20.065(4)
_cell_length_c                   28.704(5)
_cell_measurement_reflns_used    603
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.020
_cell_volume                     7623(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker COSMO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-13 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Smart APEX II '
_diffrn_measurement_method       omega/phi-scans
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1958
_diffrn_reflns_av_unetI/netI     0.1162
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            81641
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.745
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7590
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       plate
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         15374
_refine_ls_number_restraints     717
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10073
_reflns_number_total             15374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06499c2.cif
_cod_data_source_block           5Cl_jfr190a_0m_sq
_cod_database_code               7120776
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              60977
_shelx_fab_checksum              6699