Selective Synthesis of cis-trans-cis Cyclic Tetrasiloxanes and the Formation of Their Two-Dimensional Layered Aggregates.
Kinoshita, Shota; Watase, Seiji; Matsukawa, Kimihiro; Kaneko, Yoshiro; Journal of the American Chemical Society 137 (2015) 5061–5065; doi:10.1021/jacs.5b00319

data_4129297
_publ_section_title
;
 Selective Synthesis of cis-trans-cis Cyclic Tetrasiloxanes and the
 Formation of Their Two-Dimensional Layered Aggregates.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5061
_journal_page_last               5065
_journal_paper_doi               10.1021/jacs.5b00319
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C36 H76 N4 O12 Si4'
_chemical_formula_sum            'C36 H76 N4 O12 Si4'
_chemical_formula_weight         869.36
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.0691(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   17.2620(4)
_cell_length_b                   14.7551(4)
_cell_length_c                   10.0083(2)
_cell_measurement_reflns_used    21077
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.00
_cell_volume                     2547.48(10)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            40384
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.003
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.412
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.346
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2940
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0070Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2491
_reflns_number_gt                2940
_reflns_number_total             5810
_reflns_threshold_expression     F^2^>2.7\s(F^2^)
_cod_data_source_file            ja5b00319_si_001.cif
_cod_data_source_block           Boc-CYTS
_cod_original_cell_volume        2547.46(11)
_cod_database_code               4129297