Bis[8-ethyl-5-oxo-2-(piperazin-4-ium-1-yl)-5,8-dihydropyrido[2,3-<i>d</i>]pyrimidine-6-carboxylic acid] 2,5-dicarboxybenzene-1,4-dicarboxylate octahydrate
Zhang, Guang-Ju; He, Jiang-Hong; Yan, Shi-Wei; Ye, Zhong-Li; Xin, Guang-Hua; Acta Crystallographica Section E 67 (2011) o1011–o1012; doi:10.1107/S1600536811011068

data_2229636
_publ_section_title
;
 Bis[8-ethyl-5-oxo-2-(piperazin-4-ium-1-yl)-5,8-dihydropyrido[2,3-<i>d</i>]pyrimidine-6-carboxylic
 acid] 2,5-dicarboxybenzene-1,4-dicarboxylate octahydrate
;
_journal_coeditor_code           FF2005
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1011
_journal_page_last               o1012
_journal_paper_doi               10.1107/S1600536811011068
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '2C14 H18 N5 O3 +, C10 H4 O8 -, 8H2 O'
_chemical_formula_moiety         '2(C14 H18 N5 O3 +), C10 H4 O8 -, 8(H2 O)'
_chemical_formula_sum            'C38 H56 N10 O22'
_chemical_formula_weight         1004.92
_chemical_name_systematic
;
Bis[8-ethyl-5-oxo-2-(piperazin-4-ium-1-yl)-5,8-dihydropyrido[2,3-
<i>d</i>]pyrimidine-6-carboxylic acid] 
2,5-dicarboxybenzene-1,4-dicarboxylate octahydrate
;
_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                83.010(2)
_cell_angle_beta                 76.737(2)
_cell_angle_gamma                73.831(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8336(16)
_cell_length_b                   11.103(2)
_cell_length_c                   12.445(2)
_cell_measurement_reflns_used    10252
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.45
_cell_volume                     1138.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10252
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.9395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0458
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                3550
_reflns_number_total             5071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ff2005.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_cell_volume        1138.9(4)
_cod_original_formula_moiety     'C14 H18 N5 O3 +, 0.5(C10 H4 O8 -), 4(H2 O)'
_cod_original_formula_iupac      'C14 H18 N5 O3 +, 0.5C10 H4 O8 -, 4H2 O'
_cod_original_formula_sum        'C19 H28 N5 O11'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     502.46
_cod_database_code               2229636
_cod_database_fobs_code          2229636