Bis[(<i>N</i>,<i>N</i>-3-oxapentamethylenethiocarbamoylthioacetato)triphenyltin] hydrate and bis(dicyclohexylammonium) bis(3-oxapentamethylenethiocarbamoylthioacetate)
Ng, Seik Weng; Hook, James M.; Acta Crystallographica Section C 55 (1999) 312–316; doi:10.1107/S0108270198013092

data_2008297
_publ_section_title
;Bis[(<i>N</i>,<i>N</i>-3-oxapentamethylenethiocarbamoylthioacetato)triphenyltin]
 hydrate and bis(dicyclohexylammonium)
 bis(3-oxapentamethylenethiocarbamoylthioacetate)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              312
_journal_page_last               316
_journal_paper_doi               10.1107/S0108270198013092
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'C12 H24 N+ , C7 H10 N O3 S2-'
_chemical_formula_sum            'C19 H34 N2 O3 S2'
_chemical_formula_weight         402.60
_chemical_name_systematic
;
 Bis(dicyclohexylammonium) bis(3-oxapentamethylenethiocarbomylthioacetate)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.7710(10)
_cell_length_b                   9.1734(6)
_cell_length_c                   22.756(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     4335.9(5)
_computing_cell_refinement       'CELDIM (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD-4/PC (Kretschmar, 1994)'
_computing_data_reduction        'XCAD4 (Harms, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w scans'
_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  0.058
_diffrn_reflns_av_sigmaI/netI    0.057
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3805
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.188
_refine_ls_extinction_coef       0.0051(5)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment
;
H atoms riding, with U(H) = 1.5U~eq~(C).  Ammonium H atoms were located and
refined.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.107
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                2255
_reflns_number_total             3803
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1237.cif
_cod_data_source_block           nsw7xm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.6161P] 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^)+(0.0577P)^2^+0.6161P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2017-04-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H68 N4 O6 S4'
_cod_original_formula_weight         805.20
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               2008297
_cod_database_fobs_code          2008297