({-})-(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_2007542
_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         'C22 H21 F1 N3 O1 S1 1+, Cl1 1-'
_chemical_formula_sum            'C22 H21 Cl F N3 O S'
_chemical_formula_weight         429.93
_chemical_name_systematic
;
(-)-(2S)-5-(2-Fluorophenyl)-1-methyl-2-(3-thenoylaminomethyl)-2,3-dihydro-
1H-1,4-benzodiazepin-4-ium Chloride
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4494(6)
_cell_length_b                   15.0000(10)
_cell_length_c                   21.3340(10)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      11.02
_cell_volume                     2063.9(3)
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .069
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2691
_diffrn_reflns_theta_max         67.96
_diffrn_standards_decay_%        6.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  .755
_exptl_absorpt_correction_T_min  .330
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XEMP; Siemens, 1989)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      1.382
_exptl_crystal_density_method    'flotation in n-heptane/CCl~4~          '
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          .44
_exptl_crystal_size_mid          .34
_exptl_crystal_size_min          .10
_refine_diff_density_max         .23
_refine_diff_density_min         -.28
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .02(2)
_refine_ls_extinction_coef       .0050(7)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2463
_refine_ls_R_factor_all          .046
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.2960P]  where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .123
_refine_ls_wR_factor_ref         .123
_reflns_number_gt                1925
_reflns_number_total             1995
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            na1340.cif
_cod_data_source_block           na1340a
_cod_depositor_comments
;
 Marking atoms 'F2'', 'H6'' and 'H2'', 'F6'' as belonging to disorder groups
 '1' and '2' with the occupancies of '0.919(6)' and '0.081(6)' respectively
 after consulting the original publication.

 Antanas Vaitkus,
 2017-09-05

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_cell_volume        2064.0(3)
_cod_original_formula_sum        'C22 H21 Cl1 F1 N3 O1 S1'
_cod_database_code               2007542