Syntheses and crystal structures of three salts of 1-(4-nitro-phenyl)-piperazine.
Prasad, Holehundi J Shankara; Devaraju, ?; Yathirajan, Hemmige S.; Akkurt, Mehmet; Foro, Sabine; Balerao, Rishik; Butcher, Ray J.; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 423–427; doi:10.1107/S205698902300302X

data_2022736
_publ_section_title
;
 Syntheses and crystal structures of three salts of
 1-(4-nitro-phenyl)-piperazine.
;
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              423
_journal_page_last               427
_journal_paper_doi               10.1107/S205698902300302X
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C10 H14 N3 O2 +, C7 H4 I O2 - , 0.5H2 O'
_chemical_formula_moiety         '2(C10 H14 N3 O2 +), 2(C7 H4 I O2 -), H2 O'
_chemical_formula_sum            'C34 H38 I2 N6 O9'
_chemical_formula_weight         928.50
_chemical_name_systematic
;
4-(4-Nitrophenyl)piperazin-1-ium 2-iodobenzoate hemihydrate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                104.967(8)
_cell_angle_beta                 94.707(7)
_cell_angle_gamma                107.430(8)
_cell_formula_units_Z            1
_cell_length_a                   7.3949(6)
_cell_length_b                   9.3440(8)
_cell_length_c                   14.4980(10)
_cell_measurement_reflns_used    2991
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.95
_cell_volume                     909.44(14)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015a)
;
_computing_structure_solution
;
<i>SHELXL2018</i> (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6275
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.015
_diffrn_reflns_theta_min         2.953
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisRed; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       prism
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3904
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0514P)^2^+0.5457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                2443
_reflns_number_total             3904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8051sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2022734--2022736.cif.'
_cod_original_cell_volume        909.44(13)
_cod_database_code               2022736
_cod_database_fobs_code          2022736
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.673
_shelx_hkl_checksum              86732
_shelx_res_checksum              76167