Synthesis and structure of trans-2,5-dimethylpiperazine-1,4-diium dihydrogen diphosphate
Mrad, Houda; Elboulali, Adel; Baptiste, Benoît; Akriche, Samah; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 1202–1205; doi:10.1107/S2056989024010132

data_1572951
_publ_section_title
;
 Synthesis and structure of trans-2,5-dimethylpiperazine-1,4-diium
 dihydrogen diphosphate
;
_journal_coeditor_code           HB8111
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1202
_journal_page_last               1205
_journal_paper_doi               10.1107/S2056989024010132
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C6 H16 N2 2+, H2 O7 P2 2-'
_chemical_formula_moiety         'C6 H16 N2 2+, H2 O7 P2 2-'
_chemical_formula_structural     'P2 O7 H2, C6 H16 N2'
_chemical_formula_sum            'C6 H18 N2 O7 P2'
_chemical_formula_weight         292.16
_chemical_name_systematic
;
<i>trans</i>-2,5-Dimethylpiperazine-1,4-diium
dihydrogen diphosphate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.422(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2557(5)
_cell_length_b                   8.3978(5)
_cell_length_c                   13.7681(7)
_cell_measurement_reflns_used    2302
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.8280
_cell_measurement_theta_min      3.9640
_cell_volume                     1185.42(11)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 2012)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0318
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Xcalibur diffractometer with Sapphire3 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9376
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.136
_diffrn_reflns_theta_min         3.447
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       Needle
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0380P)^2^+1.0885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                1738
_reflns_number_total             2255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8111.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1572951.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1572951
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.962
_shelx_hkl_checksum              24238
_shelx_res_checksum              28259
_shelxl_version_number           .2013