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_2012511
_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         'C10 H16 F6 N3 O4 P S2'
_chemical_formula_structural     'C10 H16 F6 N3 O4 P S2'
_chemical_formula_sum            'C10 H16 F6 N3 O4 P S2'
_chemical_formula_weight         451.34
_chemical_name_systematic
;
[(4RS,5RS)-1,3-bis(trifluoromethanesulfonyl)perhydro-1,3,2-benzodiaza-
phosphol-2-yl]dimethylamine
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                97.40(4)
_cell_angle_beta                 104.03(4)
_cell_angle_gamma                60.58(4)
_cell_formula_units_Z            2
_cell_length_a                   8.972(2)
_cell_length_b                   9.116(6)
_cell_length_c                   12.990(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      10.0
_cell_volume                     897.8(9)
_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 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_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  .022
_diffrn_reflns_av_sigmaI/netI    .030
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5444
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        10.83
_diffrn_standards_interval_count 120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .467
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             460.00
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .18
_refine_diff_density_max         .53
_refine_diff_density_min         -.39
_refine_ls_extinction_method     none
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_refine_ls_number_constraints    0
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3076
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .049
_refine_ls_R_factor_gt           .049
_refine_ls_shift/su_max          .008
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .070
_refine_ls_wR_factor_ref         .070
_reflns_number_gt                3076
_reflns_number_total             5227
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            na1537.cif
_cod_data_source_block           IIIb
_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_sg_symbol_Hall     -P1
_cod_database_code               2012511