Syntheses and crystal structures of 4-(4-methoxyphenyl)piperazin-1-ium 4-methylbenzoate monohydrate and bis[4-(4-methoxyphenyl)piperazin-1-ium] benzene-1,2-dicarboxylate
Shankara Prasad, Holehundi J.; Devaraju; Vinaya; Yathirajan, Hemmige S.; Parkin, Sean R.; Glidewell, Christopher; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022008337

data_2244152
_publ_section_title
;
 Syntheses and crystal structures of 4-(4-methoxyphenyl)piperazin-1-ium
 4-methylbenzoate monohydrate and bis[4-(4-methoxyphenyl)piperazin-1-ium]
 benzene-1,2-dicarboxylate
;
_journal_coeditor_code           ZL5034
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022008337
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C11 H17 N2 O +, C8 H7 O2 -, H2 O'
_chemical_formula_moiety         'C11 H17 N2 O +, C8 H7 O2 -, H2 O'
_chemical_formula_sum            'C19 H26 N2 O4'
_chemical_formula_weight         346.42
_chemical_name_systematic
;
4-(4-Methoxyphenyl)piperazin-1-ium 4-methylbenzoate monohydrate
;
_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     dual
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                86.695(2)
_cell_angle_beta                 83.654(2)
_cell_angle_gamma                82.182(3)
_cell_formula_units_Z            4
_cell_length_a                   7.4141(5)
_cell_length_b                   12.3595(11)
_cell_length_c                   19.9917(17)
_cell_measurement_reflns_used    8258
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.535
_cell_measurement_theta_min      1.917
_cell_volume                     1802.1(3)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
<i>SHELXL2014</i> (Sheldrick, 2015b) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54020
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         1.917
_diffrn_source                   microsource
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.3838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                5772
_reflns_number_total             8288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5034sup1.cif
_cod_data_source_block           I
_cod_database_code               2244152
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.993
_shelx_hkl_checksum              79165
_shelx_res_checksum              97417
_shelxl_version_number           2.014
_cod_database_fobs_code 2244152