New electron-deficient chiral phosphines: (4<i>R</i>,5<i>R</i>)-1,3-bis(trifluoromethanesulfonyl)perhydro-1,3,2-benzodiazaphosphol-2-yl] substituted amines
Konya, Denés; Philouze, Christian; Gimbert, Yves; Greene, Andrew E.; Acta Crystallographica Section C 58 (2002) o108–o111; doi:10.1107/S0108270101018200

data_2012512
_publ_section_title
;New electron-deficient chiral phosphines:
 (4<i>R</i>,5<i>R</i>)-1,3-bis(trifluoromethanesulfonyl)perhydro-1,3,2-benzodiazaphosphol-2-yl]
 substituted amines
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o108
_journal_page_last               o111
_journal_paper_doi               10.1107/S0108270101018200
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C17 H23 F12 N5 O8 P2 S4 , 0.98(C H Cl3)'
_chemical_formula_structural     'C17 H23 F12 N5 O8 P2 S4 , 0.98(C H Cl3)'
_chemical_formula_sum            'C17.98 H23.98 Cl2.95 F12 N5 O8 P2 S4'
_chemical_formula_weight         960.65
_chemical_name_systematic
;
bis[(4R,5R)-1,3-bis(trifluoromethanesulfonyl)perhydro-1,3,2-
benzodiazaphosphol-2-yl]methylamine chloroform solvate
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 90.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.812(4)
_cell_length_b                   13.897(3)
_cell_length_c                   14.728(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      10.0
_cell_volume                     1803.6(12)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1992-1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full .99
_diffrn_measured_fraction_theta_max .94
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .031
_diffrn_reflns_av_sigmaI/netI    .040
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5666
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         30.86
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        6.99
_diffrn_standards_interval_count 120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .681
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'monoclinic prism'
_exptl_crystal_F_000             954.06
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .15
_refine_diff_density_max         .46
_refine_diff_density_min         -.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.878
_refine_ls_goodness_of_fit_ref   1.878
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     486
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .086
_refine_ls_R_factor_gt           .086
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00013|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .051
_refine_ls_wR_factor_ref         .051
_reflns_number_gt                4855
_reflns_number_total             5519
_reflns_threshold_expression     I>0
_cod_data_source_file            na1537.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1803.0(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2012512
_cod_database_fobs_code          2012512