(+)-(2<i>S</i>,3<i>S</i>,4<i>S</i>,5<i>S</i>)-3-[3,5-Bis(trifluoromethyl)benzyloxy]-<i>N</i>-(<i>tert</i>-butoxycarbonyl)-4,5-dimethyl-2-phenylpyrrolidine, (I), and (+)-(2<i>S</i>,3<i>S</i>,4<i>S</i>,5<i>S</i>)-3-[3,5-bis(trifluoromethyl)benzyloxy]-4,5-dimethyl-2-phenylpyrrolidinium <i>p</i>-toluenesulfonate, (II), at 134K
Bats, Jan W.; Heinrich, Timo; Reggelin, Michael; Acta Crystallographica Section C 55 (1999) IUC9900121–; doi:10.1107/S0108270199098613

data_2009068
_publ_section_title
;(+)-(2<i>S</i>,3<i>S</i>,4<i>S</i>,5<i>S</i>)-3-[3,5-Bis(trifluoromethyl)benzyloxy]-<i>N</i>-(<i>tert</i>-butoxycarbonyl)-4,5-dimethyl-2-phenylpyrrolidine,
 (I), and
 (+)-(2<i>S</i>,3<i>S</i>,4<i>S</i>,5<i>S</i>)-3-[3,5-bis(trifluoromethyl)benzyloxy]-4,5-dimethyl-2-phenylpyrrolidinium
 <i>p</i>-toluenesulfonate, (II), at 134K
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900121
_journal_paper_doi               10.1107/S0108270199098613
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C21 H22 F6 N O 1+, C7 H7 O3 S 1-'
_chemical_formula_sum            'C28 H29 F6 N O4 S'
_chemical_formula_weight         589.58
_chemical_name_systematic
;
(+)-(2S,3S,4S,5S)-3-[3,5-bis-(trifluoromethyl)-phenylmethoxy]-4,5-dimethyl-2-
phenyl-pyrrolidinyl p-toluenesulfonate
;
_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                90.00
_cell_angle_beta                 102.162(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8727(18)
_cell_length_b                   8.8917(11)
_cell_length_c                   16.527(2)
_cell_measurement_reflns_used    183
_cell_measurement_temperature    134(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     1418.3(4)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'CIF in SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1996)'
_diffrn_ambient_temperature      134(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  Siemens_SMART
_diffrn_measurement_method       \w
_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  0.068
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22132
_diffrn_reflns_theta_full        29.73
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  540
_diffrn_standards_number         353
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ruler
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.363
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6962
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.05P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                5978
_reflns_number_total             6962
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0178.cif
_cod_data_source_block           II
_cod_original_cell_volume        1418.2(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2009068