Synthesis and Characterization of Fluorinated Metal Arsenates with a Layer Structure: (C4H12N2)1.5[M3F5(HAsO4)2(AsO4)] (M = Fe, Ga)
Shi-Hao Luo; Yau-Chen Jiang; Sue-Lein Wang; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 40 (2001) 5381–5384; doi:10.1021/ic010150q

data_4320346
_publ_contact_author
;
Kwang-Hwa Lii,
Department of Chemistry,
National Central University,
Chungli, Taiwan 320
;
_publ_contact_author_email       liikh@cc.ncu.edu.tw
_publ_section_title
;
 Synthesis and Characterization of Fluorinated Metal Arsenates with a
 Layer Structure: (C4H12N2)1.5[M3F5(HAsO4)2(AsO4)] (M = Fe, Ga)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5381
_journal_page_last               5384
_journal_paper_doi               10.1021/ic010150q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         (C4H12N2)1.5[Fe3F5(HAsO4)2(AsO4)]
_chemical_formula_sum            'C6 H20 As3 F5 Fe3 N3 O12'
_chemical_formula_weight         813.56
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.188(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3944(10)
_cell_length_b                   21.992(3)
_cell_length_c                   10.8466(12)
_cell_measurement_temperature    295(2)
_cell_volume                     1990.7(4)
_computing_molecular_graphics    ATOMS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12579
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    7.217
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_pink
_exptl_crystal_density_diffrn    2.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00003(7)
_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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0299P)^2^+4.7726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                4132
_reflns_number_total             4745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010150q_1.cif
_cod_data_source_block           fm
_cod_database_code               4320346