({-})-(2<i>S</i>)-Tifluadom Hydrochloride and Two of its ({-})-(2<i>S</i>)-2-(Acylaminomethyl)benzodiazepine Hydrochloride Analogues
Peeters, Oswald M.; Meurisse, Rita L.; Blaton, Norbert M.; De Ranter, Camiel J.; Acta Crystallographica Section C 54 (1998) 1133–1137; doi:10.1107/S0108270198003412

data_2007544
_publ_section_title
;
 ({-})-(2<i>S</i>)-Tifluadom Hydrochloride and Two of its
 ({-})-(2<i>S</i>)-2-(Acylaminomethyl)benzodiazepine Hydrochloride
 Analogues
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1133
_journal_page_last               1137
_journal_paper_doi               10.1107/S0108270198003412
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C26 H27 F1 N3 O1 1+, Cl 1-, 0.5C6 H12 O1'
_chemical_formula_sum            'C29 H33 Cl F N3 O1.5'
_chemical_formula_weight         502.04
_chemical_name_systematic
;(-)-(2S)-5-(4-Fluorophenyl)-1,8-dimethyl-2-(p-toluoylaminomethyl)-2,3-dihydro-
1H-1,4-benzodiazepin-4-ium
 Chloride Methyl isobutyl ketone 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                90.00
_cell_angle_beta                 117.471(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9932(3)
_cell_length_b                   19.6670(10)
_cell_length_c                   12.9428(7)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      10.60
_cell_volume                     2708.6(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .020
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5940
_diffrn_reflns_theta_max         67.33
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  .795
_exptl_absorpt_correction_T_min  .572
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XEMP; Siemens, 1989)'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      1.230
_exptl_crystal_density_method    'flotation in n-heptane/CCl~4~           '
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          .58
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .15
_refine_diff_density_max         .18
_refine_diff_density_min         -.22
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .000(10)
_refine_ls_extinction_coef       .0044(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         5115
_refine_ls_R_factor_all          .038
_refine_ls_R_factor_gt           .037
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.3714P]  where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .105
_refine_ls_wR_factor_ref         .105
_reflns_number_gt                4691
_reflns_number_total             4827
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            na1340.cif
_cod_data_source_block           na1340c
_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:

'_exptl_absorpt_correction_type' value '\y scan' was replaced with
the value 'psi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C29 H33 Cl1 F1 N3 O1.5  '
_cod_database_code               2007544