1-Methylpiperazine-1,4-diium dipicrate
Dutkiewicz, Grzegorz; Samshuddin, S.; Narayana, B.; Yathirajan, H. S.; Kubicki, Maciej; Acta Crystallographica Section E 67 (2011) o390–o391; doi:10.1107/S1600536811001024

data_2229045
_publ_section_title
;
 1-Methylpiperazine-1,4-diium dipicrate
;
_journal_coeditor_code           FL2330
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o390
_journal_page_last               o391
_journal_paper_doi               10.1107/S1600536811001024
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C5 H14 N2 2+, 2C6 H2 N3 O7 -'
_chemical_formula_moiety         'C5 H14 N2 2+, 2(C6 H2 N3 O7 -)'
_chemical_formula_sum            'C17 H18 N8 O14'
_chemical_formula_weight         558.39
_chemical_name_common            '1-methylpiperazine-1,4-diium dipicrate'
_chemical_name_systematic
;
1-methylpiperazine-1,4-diium bis(2,4,6-trinitrophenolate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.798(12)
_cell_angle_beta                 78.130(11)
_cell_angle_gamma                81.558(12)
_cell_formula_units_Z            2
_cell_length_a                   8.2001(12)
_cell_length_b                   10.1780(15)
_cell_length_c                   13.7399(18)
_cell_measurement_reflns_used    12041
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.0422
_cell_measurement_theta_min      3.0164
_cell_volume                     1109.6(3)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics
'Stereochemical Workstation Operation Manual (Siemens, 1989)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21056
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.3607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                3624
_reflns_number_total             4891
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fl2330.cif
_cod_data_source_block           I
_cod_database_code               2229045
_cod_database_fobs_code          2229045