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_4307419
_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 Fe2 N6 O6, OH, H2 O'
_chemical_formula_sum            'C15 H12 Fe2 N6 O8'
_chemical_formula_weight         516.01
_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                   9.6956(8)
_cell_length_b                   9.6956(8)
_cell_length_c                   6.0530(10)
_cell_measurement_reflns_used    1072
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.668
_cell_measurement_theta_min      2.425
_cell_volume                     492.78(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Mercury 1.4.1'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3060
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.624020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, G.M., 2003'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         755
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0744
_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^)+(0.1336P)^2^+0.4661P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                685
_reflns_number_total             755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061908esi20061005_061615_2.cif
_cod_data_source_block           compound_2
_cod_database_code               4307419