#------------------------------------------------------------------------------
#$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/4000193.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_4000193
_journal_name_full 'Chemistry of Materials'
_journal_year    2002
_chemical_formula_sum             'C3 H13 F2 Fe3 N2 O12 P3'
_chemical_formula_weight          567.61
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P-1'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a                    6.431(4)
_cell_length_b                    10.274(5)
_cell_length_c                    10.439(3)
_cell_angle_alpha                 80.56(4)
_cell_angle_beta                  89.53(2)
_cell_angle_gamma                 87.94(4)
_cell_volume                      680.0(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_exptl_crystal_colour             'brownish red'
_exptl_crystal_size_max           0.24
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.772
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              564
_exptl_absorpt_coefficient_mu     3.610
_exptl_absorpt_correction_type    SADABS
_exptl_absorpt_correction_T_min   0.616642
_exptl_absorpt_correction_T_max   1.000000
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        ?
_diffrn_measurement_method        ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             2915
_diffrn_reflns_av_R_equivalents   0.0448
_diffrn_reflns_av_sigmaI/netI     0.0981
_diffrn_reflns_limit_h_min        -4
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          1.98
_diffrn_reflns_theta_max          23.31
_reflns_number_total              1943
_reflns_number_observed           1267
_reflns_observed_criterion        >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1943
_refine_ls_number_parameters      226
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0977
_refine_ls_R_factor_obs           0.0634
_refine_ls_wR_factor_all          0.1809
_refine_ls_wR_factor_obs          0.1573
_refine_ls_goodness_of_fit_all    0.965
_refine_ls_goodness_of_fit_obs    1.072
_refine_ls_restrained_S_all       0.967
_refine_ls_restrained_S_obs       1.075
_refine_ls_shift/esd_max          0.000
_refine_ls_shift/esd_mean         0.000
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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Fe1 Fe 0.5054(2) 0.29765(15) 0.78252(15) 0.0119(5) Uani 1 d . .
Fe2 Fe 0.2496(2) 0.49885(15) 0.50015(15) 0.0154(5) Uani 1 d . .
Fe3 Fe 0.7524(2) 0.4976(2) 1.00189(15) 0.0172(5) Uani 1 d . .
P1 P 0.5117(5) 0.2318(3) 1.0782(3) 0.0189(7) Uani 1 d . .
P2 P 1.0057(4) 0.3850(3) 0.7687(3) 0.0106(7) Uani 1 d . .
P3 P 0.5210(5) 0.2335(3) 0.5083(3) 0.0171(7) Uani 1 d . .
O1 O 0.2011(11) 0.2974(7) 0.7829(7) 0.015(2) Uani 1 d . .
O2 O 0.8178(11) 0.2975(7) 0.7845(7) 0.012(2) Uani 1 d . .
O3 O 0.5212(11) 0.1765(7) 0.9485(7) 0.017(2) Uani 1 d . .
O4 O 0.5238(11) 0.1778(7) 0.6541(7) 0.016(2) Uani 1 d . .
F5 F 0.5037(10) 0.4525(6) 0.8807(6) 0.026(2) Uani 1 d . .
F6 F 0.4986(11) 0.4547(6) 0.6352(6) 0.029(2) Uani 1 d . .
O7 O 0.2853(11) 0.6852(7) 0.5331(7) 0.020(2) Uani 1 d . .
O8 O 0.3185(13) 0.3120(6) 0.4685(7) 0.020(2) Uani 1 d . .
O9 O 0.0019(11) 0.5278(7) 0.3674(6) 0.015(2) Uani 1 d . .
O10 O 0.7036(12) 0.3085(7) 1.0977(7) 0.022(2) Uani 1 d . .
O11 O 0.6916(12) 0.6878(7) 0.9072(7) 0.023(2) Uani 1 d . .
O12 O 0.9997(11) 0.5233(7) 1.1277(6) 0.013(2) Uani 1 d . .
O13 O 0.5345(13) 0.1114(7) 0.4372(7) 0.023(2) Uani 1 d . .
H30 H 0.5334(13) 0.1364(7) 0.3584(7) 0.035 Uiso 1 calc R .
O14 O 0.5101(13) 0.1070(7) 1.1886(8) 0.029(2) Uani 1 d . .
H20 H 0.4077(13) 0.0639(7) 1.1801(8) 0.043 Uiso 1 calc R .
N1 N -0.0191(15) 0.7639(8) 0.7164(9) 0.024(2) Uani 1 d D .
H1 H -0.0537(15) 0.7111(8) 0.6610(9) 0.036 Uiso 1 calc R .
H2 H -0.1072(15) 0.7545(8) 0.7832(9) 0.036 Uiso 1 calc R .
H3 H 0.1097(15) 0.7427(8) 0.7451(9) 0.036 Uiso 1 calc R .
C1 C -0.0290(22) 0.9032(9) 0.6496(11) 0.035(3) Uani 1 d D .
H4 H -0.1689(22) 0.9232(9) 0.6163(11) 0.042 Uiso 1 calc R .
H5 H 0.0642(22) 0.9105(9) 0.5754(11) 0.042 Uiso 1 calc R .
C2 C 0.0258(18) 1.0079(12) 0.7301(12) 0.043(4) Uani 1 d D .
H6 H 0.1606(18) 0.9844(12) 0.7699(12) 0.051 Uiso 1 calc R .
H7 H 0.0381(18) 1.0915(12) 0.6725(12) 0.051 Uiso 1 calc R .
N2 N -0.1286(16) 1.0259(10) 0.8346(9) 0.034(3) Uani 1 d D .
H8 H -0.1473(16) 1.1129(10) 0.8356(9) 0.041 Uiso 1 calc R .
H9 H -0.2512(16) 0.9956(10) 0.8134(9) 0.041 Uiso 1 calc R .
C3 C -0.0730(23) 0.9594(11) 0.9688(11) 0.038(4) Uani 1 d D .
H10 H -0.0081(23) 0.8734(11) 0.9652(11) 0.045 Uiso 1 calc R .
H11 H -0.1984(23) 0.9464(11) 1.0209(11) 0.045 Uiso 1 calc R .
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Fe1 0.0085(9) 0.0141(9) 0.0128(9) -0.0008(6) 0.0014(6) -0.0026(6)
Fe2 0.0133(9) 0.0177(9) 0.0148(9) -0.0012(7) 0.0007(7) -0.0030(7)
Fe3 0.0155(9) 0.0199(9) 0.0163(9) -0.0028(7) 0.0010(7) -0.0031(7)
P1 0.020(2) 0.017(2) 0.020(2) -0.0018(13) 0.0010(13) -0.0026(13)
P2 0.0109(15) 0.012(2) 0.0085(14) -0.0005(11) 0.0012(11) -0.0039(12)
P3 0.019(2) 0.013(2) 0.019(2) -0.0017(12) 0.0029(13) -0.0034(13)
O1 0.006(4) 0.014(4) 0.024(4) -0.001(3) 0.002(3) 0.000(3)
O2 0.008(4) 0.012(4) 0.017(4) -0.003(3) 0.000(3) 0.000(3)
O3 0.019(4) 0.013(4) 0.015(4) 0.007(3) 0.006(3) 0.002(3)
O4 0.018(4) 0.013(4) 0.020(4) -0.010(3) 0.000(3) 0.003(3)
F5 0.030(4) 0.031(4) 0.019(4) -0.011(3) 0.002(3) -0.004(3)
F6 0.037(5) 0.029(4) 0.017(4) 0.006(3) 0.005(3) -0.009(3)
O7 0.013(4) 0.019(4) 0.028(5) 0.000(4) 0.007(4) -0.009(3)
O8 0.035(5) 0.006(4) 0.020(4) 0.001(3) -0.005(4) -0.009(4)
O9 0.020(4) 0.019(4) 0.005(4) 0.000(3) -0.002(3) -0.005(3)
O10 0.025(5) 0.014(4) 0.026(4) 0.004(3) -0.006(4) -0.002(4)
O11 0.017(5) 0.019(4) 0.031(5) -0.002(4) 0.005(4) -0.001(4)
O12 0.021(4) 0.013(4) 0.005(4) -0.005(3) -0.001(3) 0.001(3)
O13 0.034(5) 0.018(4) 0.018(4) -0.004(3) 0.003(4) -0.005(4)
O14 0.036(5) 0.020(4) 0.030(5) -0.001(4) -0.001(4) -0.011(4)
N1 0.022(6) 0.038(6) 0.013(5) -0.006(4) 0.008(4) -0.006(5)
C1 0.042(9) 0.020(7) 0.040(8) 0.006(6) -0.001(7) 0.000(6)
C2 0.028(8) 0.026(8) 0.075(12) -0.011(8) -0.005(8) -0.002(6)
N2 0.029(7) 0.025(6) 0.050(7) -0.010(5) -0.003(6) 0.000(5)
C3 0.044(9) 0.023(7) 0.045(9) -0.004(6) -0.016(7) 0.001(7)
_cod_database_code 4000193