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_1550744
_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         'C80 H124 O Si6, 0.5(C6 H14)'
_chemical_formula_sum            'C83 H131 O Si6'
_chemical_formula_weight         1313.41
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                67.9010(10)
_cell_angle_beta                 70.1540(10)
_cell_angle_gamma                76.3090(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3961(3)
_cell_length_b                   18.2592(5)
_cell_length_c                   19.4141(4)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      31.55
_cell_measurement_theta_min      2.33
_cell_volume                     4106.07(17)
_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      152(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            127205
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.864
_diffrn_reflns_theta_min         1.179
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       block
_exptl_crystal_F_000             1442
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.580
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         33036
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0695P)^2^+1.7219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22410
_reflns_number_total             33036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05591b2.cif
_cod_data_source_block           sh3824
_cod_original_cell_volume        4106.08(17)
_cod_database_code               1550744
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2014/6
_shelx_res_checksum              19607