1,4-Bis(4-pyridylmethyl)piperazin-1-ium perchlorate fumaric acid hemisolvate
Farnum, Gregory A.; LaDuca, Robert L.; Acta Crystallographica Section E 65 (2009) o1817–; doi:10.1107/S1600536809026026

data_2222893
_publ_section_title
;
 1,4-Bis(4-pyridylmethyl)piperazin-1-ium perchlorate fumaric acid
 hemisolvate
;
_journal_coeditor_code           TK2492
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1817
_journal_paper_doi               10.1107/S1600536809026026
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '2C16 H21 N4 +, 2Cl O4 -, C4 H4 O4'
_chemical_formula_moiety         '2(C16 H21 N4 +), 2(Cl O4 -), C4 H4 O4'
_chemical_formula_sum            'C36 H46 Cl2 N8 O12'
_chemical_formula_weight         853.70
_chemical_name_systematic
;
Bis[1,4-bis(4-pyridylmethyl)piperazin-1-ium] bis(perchlorate) fumaric acid
solvate
;
_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                88.691(2)
_cell_angle_beta                 83.785(2)
_cell_angle_gamma                66.749(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7287(9)
_cell_length_b                   9.6415(11)
_cell_length_c                   14.3440(17)
_cell_measurement_reflns_used    14571
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.3
_cell_volume                     976.0(2)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics
;
<i>Crystal Maker</i> (Palmer, 2005)
;
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and <i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       \w-\y
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14571
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.4
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.5777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                3178
_reflns_number_total             3593
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2492.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C16 H21 N4 +, Cl O4 -, 0.5(C4 H4 O4)'
_cod_original_formula_iupac      'C16 H21 N4 +, Cl O4 -, 0.5C4 H4 O4'
_cod_original_formula_sum        'C18 H23 Cl N4 O6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     426.85
_cod_database_code               2222893
_cod_database_fobs_code          2222893