5-Hydroxy-1-phosphabicyclo[3.3.1]nonane <i>P</i>-sulfide
Ziemer, Burkhard; Krauss, Babett; Acta Crystallographica Section C 55 (1999) IUC9900143–; doi:10.1107/S0108270199098534

data_2009169
_publ_section_title
;
 5-Hydroxy-1-phosphabicyclo[3.3.1]nonane <i>P</i>-sulfide
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900143
_journal_paper_doi               10.1107/S0108270199098534
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C8 H15 O P S'
_chemical_formula_weight         190.26
_chemical_melting_point          515.0(10)
_chemical_name_systematic
;
 5-Hydroxy-1-phosphabicyclo[3.3.1]nonansulfide
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9099(13)
_cell_length_b                   14.9099(13)
_cell_length_c                   8.548(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      13.5
_cell_volume                     1900.3(5)
_computing_cell_refinement       'STADI4-1.07 (Stoe, 1997)'
_computing_data_collection       'STADI4-1.07 (Stoe, 1997)'
_computing_data_reduction        'XRED-1.08 (Stoe, 1997)'
_computing_molecular_graphics    'XSTEP-2.04 (Stoe, 1997)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method
'2\q/\w scan, ratio = 1.0, width (\w) = 1.1-1.25\%'
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5888
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          1.02
_exptl_crystal_size_mid          0.91
_exptl_crystal_size_min          0.76
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.185
_refine_ls_extinction_coef       0.0341(14)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.021
_refine_ls_R_factor_obs          .020
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.1149P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.055
_refine_ls_wR_factor_obs         .054
_reflns_number_observed          2710
_reflns_number_total             2767
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            qa0182.cif
_cod_data_source_block           QA0182
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 'Tetragonal' changed to 'tetragonal'
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^)+(0.0301P)^2^+0.1149P] 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^)+(0.0301P)^2^+0.1149P] 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        1900.4(4)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C8 H15 O1 P1 S1'
_cod_database_code               2009169