Ionothermal Synthesis of Metal Oxalatophosphonates with a Three-Dimensional Framework Structure: Na2M3(C2O4)3(CH3PO3H)2(M = FeIIand MnII)
Tsao, Chun-Po; Sheu, Chyi-Yang; Nguyen, Ninh; Lii, Kwang-Hwa; Inorganic Chemistry 45 (2006) 6361–6364; doi:10.1021/ic0603959

data_4332450
_publ_section_title
;
 Ionothermal Synthesis of Metal Oxalatophosphonates with a
 Three-Dimensional Framework Structure:&#x00A0; Na2M3(C2O4)3(CH3PO3H)2(M =
 FeIIand MnII)
;
_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6361
_journal_page_last               6364
_journal_paper_doi               10.1021/ic0603959
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         Na2Fe3(C2O4)3(CH3PO3H)2
_chemical_formula_sum            'C8 H8 Fe3 Na2 O18 P2'
_chemical_formula_weight         667.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.9260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.80630(10)
_cell_length_b                   10.3867(3)
_cell_length_c                   14.8094(4)
_cell_measurement_temperature    293(2)
_cell_volume                     886.61(4)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scan'
_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    0.0538
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31247
_diffrn_reflns_theta_full        46.03
_diffrn_reflns_theta_max         46.03
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.030
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.0038(6)
_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   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                5193
_reflns_number_total             7179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0603959sup1.cif
_cod_data_source_block           05sp08
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4332450