(4<i>S</i>,6<i>S</i>,11<i>R</i>)-(+)-<i>trans</i>-4,6-Dimethyl-2-(1-phenylethylamino)-2-thio-1,3,2λ^5^-dioxaphosphorinane
Hommer, Herbert; Domínguez, Zaira; Gordillo, Bárbara; Acta Crystallographica Section C 54 (1998) 832–834; doi:10.1107/S0108270197020179

data_2007297
_publ_section_title
(4<i>S</i>,6<i>S</i>,11<i>R</i>)-(+)-<i>trans</i>-4,6-Dimethyl-2-(1-phenylethylamino)-2-thio-1,3,2\l^5^-dioxaphosphorinane
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              832
_journal_page_last               834
_journal_paper_doi               10.1107/S0108270197020179
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C13 H20 N O2 P S'
_chemical_formula_sum            'C13 H20 N O2 P S'
_chemical_formula_weight         285.33
_chemical_melting_point          361.1(10)
_chemical_name_common
;
(2R,4S,6S)-(+)-2-N-benzylmethyl-amino-2-thio-4,6-
dimethyl-1,3,2-dioxaphosphorinane
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.9210(10)
_cell_length_b                   9.9210(10)
_cell_length_c                   26.880(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      11
_cell_volume                     2291.2(5)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD-4'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.042
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1626
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        +-2.4
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       equidimensional
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.04(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.137
_refine_ls_goodness_of_fit_obs   1.262
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.262
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_obs          .037
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.0649P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.112
_refine_ls_wR_factor_obs         .106
_reflns_number_observed          1208
_reflns_number_total             1592
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bk1328.cif
_cod_data_source_block           bk1328
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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:

'_chemical_melting_point' value '87-89\%C' was changed to '361.1(10)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '87-89\%C' was changed to '361.1(10)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Trigonal' changed to
'trigonal' 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^)+(0.0558P)^2^+0.0649P] 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^)+(0.0558P)^2^+0.0649P] 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_Hall     'P 31 2" '
_cod_original_sg_symbol_H-M      'P 31  2 1'
_cod_database_code               2007297