Bis(guanidinium) tris(pyridine-2,6-dicarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)zirconate(II) tetrahydrate
Tabatabaee, Masoumeh; Adineh, Mahnaz; Derikvand, Zohreh; Attar Gharamaleki, Jafar; Acta Crystallographica Section E 68 (2012) m462–m463; doi:10.1107/S1600536812011439

data_2234324
_publ_section_title
;
 Bis(guanidinium)
 tris(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)zirconate(II)
 tetrahydrate
;
_journal_coeditor_code           LH5430
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m462
_journal_page_last               m463
_journal_paper_doi               10.1107/S1600536812011439
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C H6 N3)2 [Zr (C7 H3 N O4)3], 4H2 O'
_chemical_formula_moiety         '2(C H6 N3 +), C21 H9 N3 O12 Zr 2-, 4(H2 O)'
_chemical_formula_sum            'C23 H29 N9 O16 Zr'
_chemical_formula_weight         778.77
_chemical_name_systematic
;
Bis(guanidinium) tris(pyridine-2,6-dicarboxylato-
\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)zirconate(II) tetrahydrate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2444(9)
_cell_length_b                   10.8583(5)
_cell_length_c                   16.5268(8)
_cell_measurement_reflns_used    4151
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.3
_cell_volume                     3094.6(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008), DIAMOND (Brandenburg, 1999) and
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32229
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.470
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0562P)^2^+8.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                2884
_reflns_number_total             4116
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5430.cif
_cod_data_source_block           I
_cod_database_code               2234324
_cod_database_fobs_code          2234324