({-})-Menthyl (<i>S</i>~P~,<i>R</i>~S~)-(2-<i>p</i>-tolylsulfinylethyl)phenylphosphinate
Osiński, Piotr W.; Saadi, Jakub; Ricken, Stefan; Schürmann, Markus; Preut, Hans; Pietrusiewicz, Michal; Eilbracht, Peter; Acta Crystallographica Section E 62 (2006) o1248–o1249; doi:10.1107/S1600536806007458

data_2208548
_publ_section_title
;
 ({-})-Menthyl
 (<i>S</i>~P~,<i>R</i>~S~)-(2-<i>p</i>-tolylsulfinylethyl)phenylphosphinate
;
_journal_coeditor_code           CI2010
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1248
_journal_page_last               o1249
_journal_paper_doi               10.1107/S1600536806007458
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C25 H35 O3 P S'
_chemical_formula_moiety         'C25 H35 O3 P S'
_chemical_formula_sum            'C25 H35 O3 P S'
_chemical_formula_weight         446.56
_chemical_name_systematic
;
(-)-Menthyl (S~P~,R~S~)-(2-p-tolylsulfinylethyl)phenylphosphinate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6199(11)
_cell_length_b                   16.824(3)
_cell_length_c                   26.870(5)
_cell_measurement_reflns_used    10129
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      3.03
_cell_volume                     2540.5(8)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO and SCALEPACK '
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
'SHELXL97, PARST95 (Nardelli, 1995), PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w
_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  0.042
_diffrn_reflns_av_sigmaI/netI    0.2266
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10129
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.096
_refine_diff_density_min         -0.089
_refine_ls_abs_structure_details 'Flack (1983); 1472 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = [exp{5.20(sin\q/\l)^2^}]/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                1555
_reflns_number_total             4029
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2010.cif
_cod_data_source_block           I
_cod_original_cell_volume        2540.6(9)
_cod_database_code               2208548
_cod_database_fobs_code          2208548