Site-Selective Functionalization of Si6R6 Siliconoids
Heider, Yannic; Poitiers, Nadine Elisabeth; Willmes, Philipp; Leszczynska, Kinga; Huch, Volker; Scheschkewitz, David; Chemical Science  (2019) –; doi:10.1039/C8SC05591B

data_1550745
_publ_section_title
;
 Site-Selective Functionalization of Si6R6 Siliconoids
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05591B
_journal_year                    2019
_chemical_formula_moiety         'C158 H252 B2 Li2 O2 Si12, 2(C6 H6)'
_chemical_formula_sum            'C170 H264 B2 Li2 O2 Si12'
_chemical_formula_weight         2712.38
_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   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-11-06 deposited with the CCDC.    2019-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.856(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.8496(8)
_cell_length_b                   24.9370(10)
_cell_length_c                   20.3519(9)
_cell_measurement_reflns_used    7163
_cell_measurement_temperature    192(2)
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      2.33
_cell_volume                     8925.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      192(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_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       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            96855
_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         29.617
_diffrn_reflns_theta_min         1.158
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.778
_exptl_crystal_size_mid          0.754
_exptl_crystal_size_min          0.306
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.403
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         25096
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.421
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0560P)^2^+5.8666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17999
_reflns_number_total             25096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05591b2.cif
_cod_data_source_block           sh3732
_cod_database_code               1550745
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2014/6
_shelx_res_checksum              19651