Synthesis and Characterization of Octakis(3-propyl ethanethioate)octasilsesquioxane
Ervithayasuporn, Vuthichai; Tomeechai, Thapakorn; Takeda, Nobuhiro; Unno, Masafumi; Chaiyanurakkul, Arada; Hamkool, Rangsinee; Osotchan, Tanakorn; Organometallics 30 (2011) 4475–; doi:10.1021/om200477a

data_4064986
_publ_section_title
;
 Synthesis and Characterization of Octakis(3-propyl
 ethanethioate)octasilsesquioxane
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4475
_journal_paper_doi               10.1021/om200477a
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C40 H72 O20 S8 Si8'
_chemical_formula_sum            'C40 H72 O20 S8 Si8'
_chemical_formula_weight         1354.18
_chemical_melting_point          491.2(3)
_chemical_name_common            octakis(3-thioacetatepropyl)octasilsesquioxane
_chemical_name_systematic
;octakis(3-propyl ethanethioate)octasilsesquioxane  
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.100(7)
_cell_angle_beta                 97.918(8)
_cell_angle_gamma                96.815(8)
_cell_formula_units_Z            1
_cell_length_a                   8.8878(16)
_cell_length_b                   9.681(2)
_cell_length_c                   18.822(4)
_cell_measurement_reflns_used    2158
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      3.5247
_cell_volume                     1591.7(6)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device
;
RAXIS conversion
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10750
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.8655
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.1637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                4802
_reflns_number_total             5486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200477a_si_002.cif
_cod_data_source_block           octakis(3-thioacetatepropyl)octasilsesquioxane
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '217.8 - 218.3 degree celcius' was
changed to '491.2(3)' - it was converted from degrees Celsius(C) to
Kelvins(K), the average value was taken and precision was
estimated.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1591.7(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064986