Triamterene–furosemide salt: structural aspects and physicochemical evaluation
Peng, Bo; Wang, Jian-Rong; Mei, Xuefeng; Acta Crystallographica Section B 74 (2018) –; doi:10.1107/S2052520618013185

data_2108324
_publ_section_title
;
 Triamterene--furosemide salt: structural aspects and physicochemical
 evaluation
;
_journal_coeditor_code           AW5014SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520618013185
_journal_volume                  74
_journal_year                    2018
_chemical_formula_moiety         'C12 H10 Cl N2 O5 S, C12 H12 N7'
_chemical_formula_sum            'C24 H22 Cl N9 O5 S'
_chemical_formula_weight         584.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                92.574(16)
_cell_angle_beta                 98.836(17)
_cell_angle_gamma                103.844(16)
_cell_formula_units_Z            2
_cell_length_a                   7.522(5)
_cell_length_b                   8.110(5)
_cell_length_c                   20.892(14)
_cell_measurement_reflns_used    1237
_cell_measurement_temperature    220
_cell_measurement_theta_max      23.351
_cell_measurement_theta_min      2.836
_cell_volume                     1218.3(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      220
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11115
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         1.980
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0630 before and 0.0500 after correction. The Ratio of 
minimum to maximum transmission is 0.8893. The \l/2 correction factor 
is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5465
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3062
_reflns_number_total             5465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5014sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1218.2(14)
_cod_database_code               2108324
_cod_database_fobs_code          2108324
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.031) H2A(0.037) H2B(0.037) H7A(0.041) H7B(0.041) H8(0.037)
 H4A(0.042) H4B(0.042) H9A(0.04) H9B(0.04) H18(0.027) H6(0.031) H14(0.033)
 H5(0.034) H2(0.034) H4(0.038) H3(0.039) H15A(0.037) H15B(0.037) H24(0.068)
 H22(0.082) H23(0.083)
 Fixed X: H1(0.387) H2A(0.78) H2B(0.5884) H7A(-0.0318) H7B(0.0254) H8(0.3727)
 H4A(0.9652) H4B(0.8354) H18(0.1078) H6(0.504) H14(0.1693) H5(0.5267)
 H2(0.1993) H4(0.3779) H3(0.2173) H15A(0.4248) H15B(0.5762) H24(0.5064)
 H22(0.0835) H23(0.2773)
 Fixed Y: H1(0.5965) H2A(0.7479) H2B(0.63) H7A(0.5464) H7B(0.6353) H8(0.5583)
 H4A(1.0524) H4B(1.0355) H18(0.13) H6(1.0539) H14(0.1966) H5(1.0956) H2(0.5741)
 H4(0.8795) H3(0.6195) H15A(0.3653) H15B(0.5286) H24(0.834) H22(0.6134)
 H23(0.8815)
 Fixed Z: H1(0.4119) H2A(0.3588) H2B(0.3421) H7A(0.5536) H7B(0.6212)
 H8(0.1812) H4A(0.5555) H4B(0.6044) H18(0.2958) H6(0.6991) H14(0.081)
 H5(0.8093) H2(0.7012) H4(0.8666) H3(0.8125) H15A(0.0764) H15B(0.1106)
 H24(0.0687) H22(-0.0694) H23(-0.0277)
;
_olex2_submission_special_instructions 'No special instructions were received'