Diethyl 5,6-dihydro-2<i>H</i>-1,3-dithiolo[4,5-<i>b</i>][1,4]dithiin-2-ylphosphonate, C~9~H~15~O~3~PS~4~
Kelkar, Shripad V.; Kilburn, Jeremy D.; Webster, Michael; Acta Crystallographica Section C 50 (1994) 724–726; doi:10.1107/S0108270193011941

data_2009693
_publ_section_title
;Diethyl
 5,6-dihydro-2<i>H</i>-1,3-dithiolo[4,5-<i>b</i>][1,4]dithiin-2-ylphosphonate,
 C~9~H~15~O~3~PS~4~
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              724
_journal_page_last               726
_journal_paper_doi               10.1107/S0108270193011941
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C9 H15 O3 P1 S4'
_chemical_formula_sum            'C9 H15 O3 P S4'
_chemical_formula_weight         330.43
_chemical_name_systematic
;
2-Diethoxyphosphoryl-5,6-dihydro-1,3-dithiolo[4,5-b][1,4]dithiin
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.197(6)
_cell_length_b                   9.141(2)
_cell_length_c                   19.5400(10)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     2855.2(12)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 software'
_computing_molecular_graphics    'ORTEPII  (Johnson, 1976)'
_computing_structure_refinement  'SHELX76  (Sheldrick, 1976)'
_computing_structure_solution    'SHELXS86  (Sheldrick, 1985)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device
;                                 Enraf-Nonius FAST area
                                  detector
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14911
_diffrn_reflns_theta_max         30.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.74
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       'air-stable blocks'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.27
_refine_ls_goodness_of_fit_obs   0.31
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0265
_refine_ls_shift/esd_max         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0015F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0367
_reflns_number_observed          3607
_reflns_number_total             7339
_reflns_observed_criterion       F>3\s(F)
_cod_data_source_file            ha1077.cif
_cod_data_source_block           NUM_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F) + 0.0015F^2^]' 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^(F) +
0.0015F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2855.2(1.2)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_original_formula_sum        'C9 H15 O3 P1 S4'
_cod_database_code               2009693