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_7102497
_publ_section_title
;
 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         '4(C12 H27 O3 S Si), C7 H8, 4(C5 H14 N)'
_chemical_formula_sum            'C75 H172 N4 O12 S4 Si4'
_chemical_formula_weight         1562.77
_chemical_name_common
'3-methyl-n-butylammonium tri-tert-butoxysilanethiolate'
_chemical_name_systematic
;
3-methyl-n-butylammonium tri-tert-butoxysilanethiolate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.709(4)
_cell_length_b                   15.326(3)
_cell_length_c                   30.588(6)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     10171(3)
_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 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'KM4 Oxford Diffraction'
_diffrn_measurement_method       '\w--2\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    0.8906
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21140
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        1.67
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         21140
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1982
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                9864
_reflns_number_total             21140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313576d.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7102497