Novel Transition Metal Oxalatophosphates with a Two-Dimensional Honeycomb Structure: (H3TREN)[M2(HPO4)(C2O4)2.5].3H2O (M = MnII and FeII, TREN = Tris(2-aminoethyl)amine)
Yau-Chen Jiang; Sue-Lein Wang; Shang-Fan Lee; Kwang-Hwa Lii; Inorganic Chemistry 42 (2003) 6154–6156; doi:10.1021/ic030019d

data_4314303
_publ_section_title
;
 Novel Transition Metal Oxalatophosphates with a Two-Dimensional Honeycomb
 Structure: (H3TREN)[M2(HPO4)(C2O4)2.5].3H2O (M = MnII and FeII, TREN =
 Tris(2-aminoethyl)amine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6154
_journal_page_last               6156
_journal_paper_doi               10.1021/ic030019d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_iupac          '[(H3NCH2CH2)3N][Fe2(HPO4)(C2O4)2.5].3H2O'
_chemical_formula_sum            'C11 H28 Fe2 N4 O17 P'
_chemical_formula_weight         631.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.630(2)
_cell_angle_beta                 84.018(2)
_cell_angle_gamma                67.372(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7776(9)
_cell_length_b                   8.9257(9)
_cell_length_c                   15.8844(16)
_cell_measurement_temperature    294(2)
_cell_volume                     1125.6(2)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Siemens Smart 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0344
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10789
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0000(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.473
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.8312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                3945
_reflns_number_total             4907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030019d_2.cif
_cod_data_source_block           feoxredm
_cod_database_code               4314303