({-})-(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_2007543
_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         'C23 H24 N3 O1 S1 1+, Cl1 1-'
_chemical_formula_sum            'C23 H24 Cl N3 O S'
_chemical_formula_weight         425.96
_chemical_name_systematic
;
(-)-(2S)-1,7-Dimethyl-5-phenyl-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                   6.3344(2)
_cell_length_b                   13.5131(7)
_cell_length_c                   25.693(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      10.92
_cell_volume                     2199.3(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  .051
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3007
_diffrn_reflns_theta_max         69.06
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.570
_exptl_absorpt_correction_T_max  .902
_exptl_absorpt_correction_T_min  .555
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XEMP; Siemens, 1989)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      1.281
_exptl_crystal_density_method    'flotation in n-heptane/CCl~4~          '
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          .46
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .04
_refine_diff_density_max         .25
_refine_diff_density_min         -.21
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -.01(3)
_refine_ls_extinction_coef       .0059(6)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         2761
_refine_ls_R_factor_all          .057
_refine_ls_R_factor_gt           .048
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.7366P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .137
_refine_ls_wR_factor_ref         .137
_reflns_number_gt                1864
_reflns_number_total             2204
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            na1340.cif
_cod_data_source_block           na1340b
_cod_depositor_comments
;
 Marking atoms 'C15A', 'C16A', 'S17A', 'C18A', 'C19A' and 'C15B', 'C16B',
 'S17B', 'C18B', 'C19B' as belonging to disorder groups '1' and '2' with the
 occupancies of '0.573(7)' and '0.427(7)' 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        2199.2(2)
_cod_original_formula_sum        'C23 H24 Cl1 N3 O1 S1'
_cod_database_code               2007543