6-Oxo-6-phenyl-6-phospha-3,9-dithiabicyclo[9.4.0]pentadeca-1(11),12,14-triene
Kivekäs, R.; Muñoz, J. A.; Escriche, L.; Casabó, J.; Sillanpää, R.; Acta Crystallographica Section C 53 (1997) 126–128; doi:10.1107/S0108270196012140

data_2005839
_publ_contact_author
;
Dr Reijo Sillanpaa
Department of Chemistry
University of Turku
FIN-20014 Turku
Finland
;
_publ_section_title
6-Oxo-6-phenyl-6-phospha-3,9-dithiabicyclo[9.4.0]pentadeca-1(11),12,14-triene
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              126
_journal_page_last               128
_journal_paper_doi               10.1107/S0108270196012140
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C18 H21 O P S2'
_chemical_formula_structural     'C18 H21 O P S2'
_chemical_formula_sum            'C18 H21 O P S2'
_chemical_formula_weight         348.44
_chemical_name_systematic
;
 6-Oxo-6-phenyl-6-phospha-3,9-dithiabicyclo[9,4,0]pentadeca-1(11),12,14-triene
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.31(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.644(2)
_cell_length_b                   13.624(2)
_cell_length_c                   22.617(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      13.2
_cell_volume                     1731.6(7)
_computing_cell_refinement       'MSC/AFC Control Program Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1995)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3622
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type
'empirical via \y scans (North, Phillips & Matthews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.579
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+1.1268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1620
_refine_ls_wR_factor_obs         0.0872
_reflns_number_observed          1960
_reflns_number_total             3544
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1413.cif
_cod_data_source_block           omj2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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^)+1.1268P] 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^)+1.1268P] 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               2005839