Structure-directing weak phosphoryl <i>X</i>H···O=P (<i>X</i> = C, N) hydrogen bonds in cyclic oxazaphospholidines and oxazaphosphinanes
van der Lee, A.; Rolland, M.; Marat, X.; Virieux, D.; Volle, J.-N.; Pirat, J.-L.; Acta Crystallographica Section B 64 (2008) 196–205; doi:10.1107/S0108768107061770

data_2104078
_publ_section_title
;
 Structure-directing weak phosphoryl
 <i>X</i>H&#x00B7;&#x00B7;&#x00B7;O=P (<i>X</i> = C, N) hydrogen bonds
 in cyclic oxazaphospholidines and oxazaphosphinanes
;
_journal_coeditor_code           GP5020
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              196
_journal_page_last               205
_journal_paper_doi               10.1107/S0108768107061770
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         'C22 H22 N1 O3 P1'
_chemical_formula_sum            'C22 H22 N O3 P'
_chemical_formula_weight         379.40
_chemical_name_systematic
;
(2R,3S,5S)-3,5-diphenyl-2-(4-methoxyphenyl)-
[1,4,2]-oxazaphosphorinane2-oxide
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 109.717(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0104(3)
_cell_length_b                   8.10560(10)
_cell_length_c                   12.5372(3)
_cell_measurement_reflns_used    5384
_cell_measurement_temperature    175
_cell_measurement_theta_max      32.1481
_cell_measurement_theta_min      3.0417
_cell_volume                     957.63(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      175
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12688
_diffrn_reflns_theta_full        29.318
_diffrn_reflns_theta_max         32.217
_diffrn_reflns_theta_min         3.315
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count '25 frames'
_diffrn_standards_number         '4 frames'
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_correction_T_min  0.9515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent pale white'
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details 'Flack (1983), 2104 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.18(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000432
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 18.4 -27.6 15.3 -5.81
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0510
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                3438
_reflns_number_total             5435
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            gp5020.cif
_cod_data_source_block           VII
_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 1 21 1 '
_cod_original_formula_sum        'C22 H22 N1 O3 P1'
_cod_database_code               2104078