Bis(2-amino-6-methylpyridinium) tris(pyridine-2,6-dicarboxylato)zirconate(IV) dihydrate
Pasdar, Hoda; Ebdam, Ali; Aghabozorg, Hossein; Notash, Behrouz; Acta Crystallographica Section E 67 (2011) m294–; doi:10.1107/S1600536811003072

data_2229331
_publ_section_title
;
 Bis(2-amino-6-methylpyridinium)
 tris(pyridine-2,6-dicarboxylato)zirconate(IV) dihydrate
;
_journal_coeditor_code           BT5467
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m294
_journal_paper_doi               10.1107/S1600536811003072
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C6 H9 N2)2 [Zr (C7 H3 N O4)3], 2H2 O'
_chemical_formula_moiety         '2(C6 H9 N2 +), C21 H9 N3 O12 Zr 2-, 2(H2 O)'
_chemical_formula_sum            'C33 H31 N7 O14 Zr'
_chemical_formula_weight         840.87
_chemical_name_systematic
;
Bis(2-amino-6-methylpyridinium) tris(pyridine-2,6-dicarboxylato)zirconate(IV)
dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.719(4)
_cell_length_b                   10.536(2)
_cell_length_c                   18.781(4)
_cell_measurement_reflns_used    4705
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.22
_cell_measurement_theta_min      2.30
_cell_volume                     3511.0(14)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12273
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[shape of crystal determined optically
(X-SHAPE and X-RED32; Stoe& Cie, 2005)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          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^)+(0.0339P)^2^+1.0948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                4284
_reflns_number_total             4705
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5467.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2229331
_cod_database_fobs_code          2229331