Two Homometallic Antiferromagnets Based on Oxalato-Bridged Honeycomb Assemblies: (A)2[MII2(C2O4)3] (A = Ammonium Salt Derived from Diethylenetriamine; MII= Fe2+, Co2+)
Zhiming Duan; Yan Zhang; Bin Zhang; Francis L. Pratt; Inorganic Chemistry 48 (2009) 2140–2146; doi:10.1021/ic8021003

data_4301609
_publ_section_title
;
Two Homometallic Antiferromagnets Based on Oxalato-Bridged Honeycomb
Assemblies: (A)2[MII2(C2O4)3] (A = Ammonium Salt Derived from
Diethylenetriamine; MII= Fe2+, Co2+)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2140
_journal_page_last               2146
_journal_paper_doi               10.1021/ic8021003
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C18 H20 Fe2 N6 O14'
_chemical_formula_weight         656.10
_chemical_name_systematic        C6H10N3O,FeC3O6
_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                 95.7670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2224(4)
_cell_length_b                   9.3151(2)
_cell_length_c                   15.1518(4)
_cell_measurement_reflns_used    9345
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2418.48(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Denzo(Otwinowski & Minor 1997)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (Bruker, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       CCD
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21408
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                1706
_reflns_number_total             2784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8021003_si_002.cif
_cod_data_source_block           Fe
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4301609