Cubane-like structure of a silanethiol–primary amine assembly–a novel, unusual hydrogen bond pattern.
Becker, Barbara; Baranowska, Katarzyna; Chojnacki, Jaroslaw; Wojnowski, Wieslaw; Chemical communications (Cambridge, England)  (2004) 620–621; doi:10.1039/b313576d

data_7102495
_publ_section_title
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 Cubane-like structure of a silanethiol--primary amine assembly--a
 novel, unusual hydrogen bond pattern.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              620
_journal_page_last               621
_journal_paper_doi               10.1039/b313576d
_journal_year                    2004
_chemical_formula_moiety         'C9 H21 O3 S Si, C4 H12 N'
_chemical_formula_sum            'C13 H33 N O3 S Si'
_chemical_formula_weight         311.55
_chemical_melting_point          129.0(10)
_chemical_name_common
'Tert-butylammonium triisopropoxysilanethiolate'
_chemical_name_systematic
;
Tert-butylammonium triisopropoxysilanethiolate
;
_space_group_IT_number           217
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.974(2)
_cell_length_b                   15.974(2)
_cell_length_c                   15.974(2)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      3.12
_cell_volume                     4076.1(9)
_computing_cell_refinement       'KM4 System (Ga\/ldecki, 1996)'
_computing_data_collection       'KM4 System (Ga\/ldecki, 1996)'
_computing_data_reduction        'DATAPROC (Ga\/ldecki, 1996)'
_computing_molecular_graphics    'RESVIEW, (Schwenk, 1998)'
_computing_publication_material  'SHELXL - 97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL - 97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS - 97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KM4 Oxford Diffraction'
_diffrn_measurement_method       '\w--1.4\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            531
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0592
_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^)+(0.1096P)^2^+3.5511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1773
_reflns_number_gt                440
_reflns_number_total             531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313576d.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '128-130' was changed to '129.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               7102495