Propane-1,2-diaminium tris(pyridine-2,6-dicarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)zirconate(IV) trihydrate
Pasdar, Hoda; Shakiba, Shahrzad; Aghabozorg, Hossein; Notash, Behrouz; Acta Crystallographica Section E 67 (2011) m587–; doi:10.1107/S1600536811008488

data_2230176
_publ_section_title
;
 Propane-1,2-diaminium
 tris(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)zirconate(IV)
 trihydrate
;
_journal_coeditor_code           XU5157
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m587
_journal_paper_doi               10.1107/S1600536811008488
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C3 H12 N2) [Zr (C7 H3 N O4)3], 3H2 O'
_chemical_formula_moiety         'C3 H12 N2 2+, C21 H9 N3 O12 Zr 2-, 3(H2 O)'
_chemical_formula_sum            'C24 H27 N5 O15 Zr'
_chemical_formula_weight         716.73
_chemical_name_systematic
;
Propane-1,2-diaminium tris(pyridine-2,6-dicarboxylato-
\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)zirconate(IV) trihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.515(2)
_cell_length_b                   19.195(4)
_cell_length_c                   14.149(3)
_cell_measurement_reflns_used    7481
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.12
_cell_volume                     2778.1(10)
_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_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1329
_diffrn_reflns_av_sigmaI/netI    0.1075
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21838
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.766
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         7481
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0863
_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^)+(0.0753P)^2^+3.9962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2055
_reflns_number_gt                5264
_reflns_number_total             7481
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5157.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2230176
_cod_database_fobs_code          2230176