Synthesis and crystal structure of double-three ring (D3R)-type cage siloxanes modified with dimethylsilanol groups.
Sato, Naoto; Tochigi, Kazuma; Kuroda, Yoshiyuki; Wada, Hiroaki; Shimojima, Atsushi; Kuroda, Kazuyuki; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1969–1975; doi:10.1039/c8dt04244f

data_7048300
_publ_section_title
;
 Synthesis and crystal structure of double-three ring (D3R)-type cage
 siloxanes modified with dimethylsilanol groups.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1969
_journal_page_last               1975
_journal_paper_doi               10.1039/c8dt04244f
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H50 O22 Si12'
_chemical_formula_sum            'C16 H50 O22 Si12'
_chemical_formula_weight         931.58
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-10-24 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.452(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.2739(5)
_cell_length_b                   10.8748(3)
_cell_length_c                   23.2168(7)
_cell_measurement_reflns_used    27796
_cell_measurement_temperature    123
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      3.81
_cell_volume                     4361.1(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35301
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.808
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.30
_refine_ls_abs_structure_details
;
 Flack x determined using 1804 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7872
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0610P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                5085
_reflns_number_total             7872
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8dt04244f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7048300--7048301.cif.'
_cod_database_code               7048300
_shelxl_version_number           2014/6
_shelx_res_checksum              11976