Self-Assembled Cationic Heterochiral Honeycomb-Layered Metal Complexes with the in Situ Generated Pyrimidine-2-carboxylato Bisdidentate Ligand. Hydrothermal Synthesis, Crystal Structures, Magnetic Properties, and Theoretical Study of [M2(μ-pymca)3]OH.H2O (M = FeII, CoII)
Antonio Rodríguez-Diéguez; Joan Cano; Raikko Kivekäs; Abderrahmane Debdoubi; Enrique Colacio; Inorganic Chemistry 46 (2007) 2503–2510; doi:10.1021/ic061908e

data_4307418
_publ_contact_author
;
     Prof. Enrique Colacio
     Departamento de Qu\'imica Inorg\'anica
     Facultad de Ciencias
     Universidad de Granada
     E-18071 Granada
     Spain
;
_publ_contact_author_email       ecolacio@ugr.es
_publ_contact_author_fax         '+34 958 248526'
_publ_contact_author_phone       '+34 958 243236'
_publ_section_title
;
Self-Assembled Cationic Heterochiral Honeycomb-Layered Metal Complexes with
the in Situ Generated Pyrimidine-2-carboxylato Bisdidentate Ligand.
Hydrothermal Synthesis, Crystal Structures, Magnetic Properties, and
Theoretical Study of [M2(\m-pymca)3]OH.H2O (M = FeII, CoII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2503
_journal_page_last               2510
_journal_paper_doi               10.1021/ic061908e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C15 H9 Co2 N6 O6, OH, H2 O'
_chemical_formula_sum            'C15 H12 Co2 N6 O8'
_chemical_formula_weight         522.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           157
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2'
_symmetry_space_group_name_H-M   'P 3 1 m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   9.548(5)
_cell_length_b                   9.548(5)
_cell_length_c                   6.077(5)
_cell_measurement_reflns_used    523
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.175
_cell_measurement_theta_min      2.463
_cell_volume                     479.8(5)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  '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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2586
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.788
_exptl_absorpt_correction_T_max  0.9483
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   'empirical (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         579
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0704
_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^)+(0.1306P)^2^+0.3982P] where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2005
_reflns_number_gt                498
_reflns_number_total             579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061908esi20061005_061615_1.cif
_cod_data_source_block           compound_1
_cod_database_code               4307418