<i>cis</i>-1-Phosphabicyclo[4.3.0]nonane <i>P</i>-sulfide
Krauss, Babett; Ziemer, Burkhard; Acta Crystallographica Section C 55 (1999) IUC9900148–; doi:10.1107/S0108270199098522

data_2009170
_publ_section_title
;
 <i>cis</i>-1-Phosphabicyclo[4.3.0]nonane <i>P</i>-sulfide
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900148
_journal_paper_doi               10.1107/S0108270199098522
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C8 H15 P S'
_chemical_formula_weight         174.23
_chemical_melting_point          330.0(10)
_chemical_name_systematic
;
cis-1-Phosphabicyclo[4.3.0]nonansulfide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 116.71(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.108(3)
_cell_length_b                   11.694(2)
_cell_length_c                   13.410(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     1836.2(7)
_computing_cell_refinement       'IPDS-2.87 (Stoe, 1997)'
_computing_data_collection       'IPDS-2.87 (Stoe, 1997)'
_computing_data_reduction        'IPDS-2.87 (Stoe, 1997)'
_computing_molecular_graphics    'XSTEP-2.04 (Stoe, 1997)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-rotation,\f-incr.=2.1\%,86 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12738
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 'not applicable to area detector'
_diffrn_standards_interval_time  'not applicable to area detector'
_diffrn_standards_number         'not applicable to area detector'
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 All crystal faces were indexed by microscope on the diffractometer and
 thereafter a gaussian integration for absorption correction,
 implemented in XRED (Stoe, 1997), was carried out.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.925
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_restrained_S_obs      1.062
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_obs          .035
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.105
_refine_ls_wR_factor_obs         .079
_reflns_number_observed          2268
_reflns_number_total             3231
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            qa0183.cif
_cod_data_source_block           qa0183
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0355P)^2^] 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^)+(0.0355P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1836.2(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2009170