Structural insights into ketanserin salts with aliphatic acids and their physiochemical properties
Kenguva, Gowtham; Rekha Rout, Smruti; Shaikh, Tabrez R.; Baidya, Debjani; Shelke, Nikita; Sanphui, Palash; Dandela, Rambabu; CrystEngComm 26 (2024) 6260–6268; doi:10.1039/D4CE00738G

data_7249469
_publ_section_title
;
 Structural insights into ketanserin salts with aliphatic acids and their
 physiochemical properties
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              6260
_journal_page_last               6268
_journal_paper_doi               10.1039/D4CE00738G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'H2 N O3 S, C22 H23 F N3 O3, 2(H2 O)'
_chemical_formula_sum            'C22 H29 F N4 O8 S'
_chemical_formula_weight         528.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-21 deposited with the CCDC.	2024-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                86.214(11)
_cell_angle_beta                 71.917(10)
_cell_angle_gamma                82.894(12)
_cell_formula_units_Z            2
_cell_length_a                   9.104(3)
_cell_length_b                   10.937(4)
_cell_length_c                   12.774(5)
_cell_measurement_reflns_used    3041
_cell_measurement_temperature    301.00
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.86
_cell_volume                     1199.3(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      301.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0959
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18053
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.367
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6347
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1459 before and 0.0865 after correction.
The Ratio of minimum to maximum transmission is 0.8513.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4199
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1757
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1371P)^2^+0.2536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.2646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2183
_reflns_number_total             4199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00738g2.cif
_cod_data_source_block           kts_sul_0m
_cod_depositor_comments
'Adding full bibliography for 7249468--7249471.cif.'
_cod_original_cell_volume        1199.3(7)
_cod_database_code               7249469
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 S1-O5 \\sim S2-O6
 with sigma of 0.02
 S1-O7 \\sim S2-O9
 with sigma of 0.02
 S1-N4 \\sim S2-N5
 with sigma of 0.02
 O5-O7 \\sim O6-O9
 with sigma of 0.04
 O5-N4 \\sim O6-N5
 with sigma of 0.04
 O7-N4 \\sim O9-N5
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(S2)
4. Rigid body (RIGU) restrains
 S1, S2, O4, O5, O6, O7, O9, N4, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, S2
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
5. Others
 Sof(S2)=Sof(O6)=Sof(O9)=Sof(N5)=Sof(H5A)=Sof(H5B)=1-FVAR(1)
 Sof(S1)=Sof(O4)=Sof(O7)=Sof(N4)=Sof(H4A)=Sof(H4B)=FVAR(1)
6.a Riding coordinates:
 O8(H8A,H8B), O10(H10C,H10D)
6.b Ternary CH refined with riding coordinates:
 N3(H3), C13(H13)
6.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3A), C4(H4), C5(H5), C18(H18), C19(H19), C21(H21),
 C22(H22)
6.e X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B)
;
_shelx_res_checksum              65606
_shelx_hkl_checksum              55319
_olex2_submission_special_instructions 'No special instructions were received'