Application of Wallach's Rule in a Comparison of the X-ray Crystal Structures of the Racemate and the (<i>S</i>) Enantiomer of (1-Hydroxy-3-phenyl-2-propenyl) Dimethylphosphonate
Blazis, Vincent J.; Koeller, Kevin J.; Rath, Nigam P.; Spilling, Christopher D.; Acta Crystallographica Section B 53 (1997) 838–842; doi:10.1107/S0108768197005703

data_2101912
_publ_section_title
;
 Application of Wallach's Rule in a Comparison of the X-ray Crystal
 Structures of the Racemate and the (<i>S</i>) Enantiomer of
 (1-Hydroxy-3-phenyl-2-propenyl) Dimethylphosphonate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              838
_journal_page_last               842
_journal_paper_doi               10.1107/S0108768197005703
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C11 H15 O4 P'
_chemical_formula_weight         242.20
_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                 107.0370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.17370(10)
_cell_length_b                   13.91270(10)
_cell_length_c                   8.73360(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.0
_cell_volume                     1181.94(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL (Sheldrick, 1995)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1995)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens CCD'
_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  0.045
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17306
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'see text'
_diffrn_standards_number         'see text'
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plates
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.04
_refine_ls_goodness_of_fit_obs   1.06
_refine_ls_hydrogen_treatment    'riding model, see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_restrained_S_obs      1.06
_refine_ls_R_factor_all          0.043
_refine_ls_R_factor_obs          0.033
_refine_ls_shift/esd_max         0.00
_refine_ls_shift/esd_mean        0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.2884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.097
_refine_ls_wR_factor_obs         0.089
_reflns_number_observed          2398
_reflns_number_total             2855
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk1251.cif
_cod_data_source_block           cds9396
_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^)+(0.0533P)^2^+0.2884P] 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^)+(0.0533P)^2^+0.2884P] 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               2101912