Spirapril Hydrochloride Hydrate
Xu, Wei; Wahle, Mark C.; Stowell, Joseph G.; Byrn, Stephen R.; Acta Crystallographica Section C 53 (1997) 1917–1919; doi:10.1107/S0108270197008287

data_2006754
_publ_section_title
;
 Spirapril Hydrochloride Hydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1917
_journal_page_last               1919
_journal_paper_doi               10.1107/S0108270197008287
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C22 H31 N2 O5 S2, Cl1 -, H2 O1'
_chemical_formula_structural     'C22 H31 N2 O5 S2,Cl1,H2 O1'
_chemical_formula_sum            'C22 H33 Cl N2 O6 S2'
_chemical_formula_weight         521.10
_chemical_name_systematic
;
[8S-[7[R*(R*)],8R*]]-7-[2-[[1-(ethoxycarbonyl)-3-
phenylpropyl]-amino]-1-oxopropyl]-1,4-dithia-7-
azaspiro[4.4]nonane-8-carboxylic acid hydrochloride
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_type_scat_source
'International Tables for Crystallography (Vol. C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5075(15)
_cell_length_b                   10.6251(15)
_cell_length_c                   23.407(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      24
_cell_measurement_theta_min      20
_cell_volume                     2613.2(6)
_computing_cell_refinement       CAD-4
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'PROCESS MolEN (Fair, 1990)'
_computing_molecular_graphics    ORTEPII
_computing_publication_material  'CIF VAX MolEN'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR (Altomare et al., 1989) (direct methods)'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       3\q/5\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3482
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0.16
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_Flack   -0.22(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.09
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         3482
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_obs          .040
_refine_ls_shift/esd_max         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.7969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.108
_refine_ls_wR_factor_obs         .092
_reflns_number_observed          2786
_reflns_number_total             3482
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            bk1260.cif
_cod_data_source_block           SPIRAH
_cod_depositor_comments
;
 Updating space group information and adding the symmetry operation list.

 Antanas Vaitkus,
 2018-06-18

 Marking atoms 'C20A', 'H20A', 'H20B', 'H20C' and 'C20B', 'H20D', 'H20E', 'H20F'
 as belonging to disorder groups '1' and '2' with the occupancies of 0.659(8)
 and 0.341(8) accordingly after consulting the original publication.

 Antanas Vaitkus,
 2018-06-18

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.7969P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.7969P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2613.1(6)
_cod_original_formula_sum        'C22 H33 Cl1 N2 O6 S2'
_cod_database_code               2006754