#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179312 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/09/4320986.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320986
loop_
_publ_author_name
'S. Ekambaram'
'Slavi C. Sevov'
_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 H15 As2 F2 Fe2 N2 O10'
_chemical_formula_weight         526.70
_chemical_name_systematic
;
Compound2
;
_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                67.32(3)
_cell_angle_beta                 82.77(3)
_cell_angle_gamma                69.76(3)
_cell_formula_units_Z            1
_cell_length_a                   5.289(1)
_cell_length_b                   7.573(1)
_cell_length_c                   8.888(2)
_cell_measurement_temperature    293(2)
_cell_volume                     308.17(13)
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2154
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    7.762
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   xabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             257
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.422
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0371
_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/[σ²(Fo²)+(0.0801P)²+0.1217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                1028
_reflns_number_total             1076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991367b_2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        308.2(1)
_cod_database_code               4320986
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As As 0.43753(7) 0.03759(5) 0.72407(4) 0.0084(2) Uani 1 1 d . . .
Fe1 Fe 0.0000 0.0000 0.5000 0.0083(3) Uani 1 2 d S . .
Fe2 Fe 0.0000 -0.5000 0.5000 0.0113(3) Uani 1 2 d S . .
F F 0.0561(5) -0.2859(4) 0.5704(3) 0.0197(6) Uani 1 1 d . . .
O1 O 0.4182(6) -0.0824(4) 0.9298(3) 0.0140(6) Uani 1 1 d . . .
H1 H 0.473(6) -0.028(6) 0.977(5) 0.021 Uiso 0.50 1 calc PR . .
O2 O 0.3230(5) -0.0825(4) 0.6388(3) 0.0125(6) Uani 1 1 d . . .
O3 O 0.7668(5) 0.0078(5) 0.6938(4) 0.0182(7) Uani 1 1 d . . .
O4 O 0.2582(6) 0.2808(4) 0.6851(3) 0.0165(6) Uani 1 1 d . . .
O5 O 0.3526(7) -0.4964(6) 0.3328(4) 0.0223(7) Uani 1 1 d . . .
H2 H 0.439(11) -0.426(9) 0.338(6) 0.025(14) Uiso 1 1 d . . .
H3 H 0.453(17) -0.602(13) 0.333(9) 0.07(3) Uiso 1 1 d . . .
N N 0.0354(7) -0.2663(5) 0.0070(4) 0.0167(7) Uani 1 1 d . . .
H0A H 0.177(5) -0.2279(14) -0.0015(5) 0.025 Uiso 1 1 calc R . .
H0B H -0.040(3) -0.2748(6) 0.102(3) 0.025 Uiso 1 1 calc R . .
H0C H -0.081(4) -0.178(3) -0.071(3) 0.025 Uiso 1 1 calc R . .
C C 0.1196(9) -0.4662(7) -0.0082(6) 0.0191(9) Uani 1 1 d . . .
H0D H 0.244(5) -0.558(4) 0.071(3) 0.023 Uiso 1 1 calc R . .
H0E H 0.198(4) -0.4579(7) -0.107(4) 0.023 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 As O2 116.00(15) . . ?
O4 As O3 110.80(16) . . ?
O2 As O3 113.81(14) . . ?
O4 As O1 105.67(15) . . ?
O2 As O1 105.86(14) . . ?
O3 As O1 103.41(15) . . ?
F Fe1 F 180.0 2_556 . ?
F Fe1 O3 90.85(13) 2_556 1_455 ?
F Fe1 O3 89.15(13) . 1_455 ?
F Fe1 O3 89.15(13) 2_556 2_656 ?
F Fe1 O3 90.85(13) . 2_656 ?
O3 Fe1 O3 180.0 1_455 2_656 ?
F Fe1 O2 94.25(12) 2_556 . ?
F Fe1 O2 85.75(12) . . ?
O3 Fe1 O2 88.92(12) 1_455 . ?
O3 Fe1 O2 91.08(12) 2_656 . ?
F Fe1 O2 85.75(12) 2_556 2_556 ?
F Fe1 O2 94.25(12) . 2_556 ?
O3 Fe1 O2 91.08(12) 1_455 2_556 ?
O3 Fe1 O2 88.92(12) 2_656 2_556 ?
O2 Fe1 O2 180.0 . 2_556 ?
O4 Fe2 O4 180.0 1_545 2_556 ?
O4 Fe2 F 88.17(12) 1_545 . ?
O4 Fe2 F 91.83(12) 2_556 . ?
O4 Fe2 F 91.83(12) 1_545 2_546 ?
O4 Fe2 F 88.17(12) 2_556 2_546 ?
F Fe2 F 179.999(1) . 2_546 ?
O4 Fe2 O5 91.21(13) 1_545 2_546 ?
O4 Fe2 O5 88.79(13) 2_556 2_546 ?
F Fe2 O5 88.58(13) . 2_546 ?
F Fe2 O5 91.42(13) 2_546 2_546 ?
O4 Fe2 O5 88.79(13) 1_545 . ?
O4 Fe2 O5 91.21(13) 2_556 . ?
F Fe2 O5 91.42(13) . . ?
F Fe2 O5 88.58(13) 2_546 . ?
O5 Fe2 O5 180.0 2_546 . ?
Fe1 F Fe2 142.68(14) . . ?
As O1 H1 109.5 . . ?
As O2 Fe1 133.63(16) . . ?
As O3 Fe1 131.73(16) . 1_655 ?
As O4 Fe2 133.74(16) . 1_565 ?
Fe2 O5 H2 114(4) . . ?
Fe2 O5 H3 117(6) . . ?
H2 O5 H3 110(6) . . ?
C N H0A 109.5 . . ?
C N H0B 109.5 . . ?
H0A N H0B 109.5 . . ?
C N H0C 109.5 . . ?
H0A N H0C 109.5 . . ?
H0B N H0C 109.5 . . ?
N C C 109.8(5) . 2_545 ?
N C H0D 109.7 . . ?
C C H0D 109.7 2_545 . ?
N C H0E 109.7 . . ?
C C H0E 109.7 2_545 . ?
H0D C H0E 108.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As O4 1.671(3) . ?
As O2 1.672(3) . ?
As O3 1.677(3) . ?
As O1 1.708(3) . ?
Fe1 F 1.930(3) 2_556 ?
Fe1 F 1.930(3) . ?
Fe1 O3 1.996(3) 1_455 ?
Fe1 O3 1.996(3) 2_656 ?
Fe1 O2 2.007(3) . ?
Fe1 O2 2.007(3) 2_556 ?
Fe2 O4 2.054(3) 1_545 ?
Fe2 O4 2.054(3) 2_556 ?
Fe2 F 2.067(3) . ?
Fe2 F 2.067(3) 2_546 ?
Fe2 O5 2.235(3) 2_546 ?
Fe2 O5 2.235(3) . ?
O1 H1 0.8221 . ?
O3 Fe1 1.997(3) 1_655 ?
O4 Fe2 2.054(3) 1_565 ?
O5 H2 0.83(6) . ?
O5 H3 0.79(9) . ?
N C 1.478(5) . ?
N H0A 0.8763 . ?
N H0B 0.8763 . ?
N H0C 0.8763 . ?
C C 1.492(8) 2_545 ?
C H0D 0.9124 . ?
C H0E 0.9124 . ?
