(3a<i>S</i>,7a<i>S</i>)-1-{2-Oxo-1,3-bis[(<i>S</i>)-1-phenylethyl]perhydro-1,3,2λ^5^-benzodiazaphosphol-2-yl}-1-phenylmethanol: a mixture of diastereoisomers in a disordered crystal
Moreno, Gloria E.; Quintero, Leticia; Bernès, Sylvain; Anaya de Parrodi, Cecilia; Acta Crystallographica Section C 60 (2004) o411–o414; doi:10.1107/S0108270104008492

data_2014068
_publ_section_title
;(3a<i>S</i>,7a<i>S</i>)-1-{2-Oxo-1,3-bis[(<i>S</i>)-1-phenylethyl]perhydro-1,3,2\l^5^-benzodiazaphosphol-2-yl}-1-phenylmethanol:
 a mixture of diastereoisomers in a disordered crystal
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o411
_journal_page_last               o414
_journal_paper_doi               10.1107/S0108270104008492
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C29 H35 N2 O2 P'
_chemical_formula_moiety         'C29 H35 N2 O2 P'
_chemical_formula_sum            'C29 H35 N2 O2 P'
_chemical_formula_weight         474.56
_chemical_melting_point          467
_chemical_name_systematic
;
(3aS,7aS)-1-{2-Oxo-1,3-bis[(S)-1-phenylethyl]perhydro-1,3,2\l^5^-
benzodiazaphosphol-2-yl]-1-phenylmethanol:
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   'See text'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                90.00
_cell_angle_beta                 95.373(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6413(11)
_cell_length_b                   17.3888(11)
_cell_length_c                   15.8778(11)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    300.0(10)
_cell_measurement_theta_max      13.01
_cell_measurement_theta_min      4.68
_cell_volume                     2650.2(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1998)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1998)'
_computing_publication_material  'SHELXTL-Plus (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15139
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '\y scans (XSCANS; Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.210
_refine_ls_abs_structure_details 'Flack (1983), 446 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         7715
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.0908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                5554
_reflns_number_total             7715
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1717.cif
_cod_data_source_block           I
_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 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2014068
_cod_database_fobs_code          2014068