Synthesis and Characterization of Four Ethylenediamine-Templated Iron Arsenates
S. Ekambaram; Slavi C. Sevov; Inorganic Chemistry 39 (2000) 2405–2410; doi:10.1021/ic991367b

data_4320987
_publ_section_title
;
 Synthesis and Characterization of Four Ethylenediamine-Templated Iron
 Arsenates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2405
_journal_page_last               2410
_journal_paper_doi               10.1021/ic991367b
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C2 H16 As6 Fe3 N4 O24'
_chemical_formula_weight         1097.26
_chemical_name_systematic
; 
Compound3
;
_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                 111.110(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.384(3)
_cell_length_b                   8.7850(10)
_cell_length_c                   16.052(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2418.5(6)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDP_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    SHELXTL-V5.0
_computing_publication_material  SHELXTL-V5.0
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       Omega-2Theta
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2199
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    10.036
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   xabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pentagonal bipyramid'
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.793
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       0.00013(8)
_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   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0641P)^2^+90.6422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                1821
_reflns_number_total             2121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991367b_3.cif
_cod_data_source_block           compound3
_cod_database_code               4320987