#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000264.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_4000264
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm021701t
_journal_year                    2003
_chemical_formula_moiety         (H3DETA)[Fe3(C2O4)2(HPO4)2(PO4)]
_chemical_formula_sum            'C8 H18 Fe3 N3 O20 P3'
_chemical_formula_weight         736.72
_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
_cell_angle_alpha                86.3020(10)
_cell_angle_beta                 68.8800(10)
_cell_angle_gamma                61.8000(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6367(7)
_cell_length_b                   10.1760(7)
_cell_length_c                   12.6164(9)
_cell_measurement_temperature    294(2)
_cell_volume                     1008.66(12)
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Simens Smart CCD'
_diffrn_measurement_method       ?
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10472
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    2.481
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   'Empirical based on symmetry equivalents'
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             740
_exptl_crystal_size_max          '0.15 mm'
_exptl_crystal_size_mid          '0.10 mm'
_exptl_crystal_size_min          '0.06 mm'
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.802
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0395P)²+3.0897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                4053
_reflns_number_total             4719
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4000264
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
Fe1 Fe 0.09655(6) 0.15034(5) 0.33713(4) 0.00966(12) Uani 1 1 d . . .
Fe2 Fe -0.13709(6) -0.07729(6) 0.16702(4) 0.01007(12) Uani 1 1 d . . .
Fe3 Fe -0.26192(6) -0.23158(6) 0.42321(5) 0.01485(13) Uani 1 1 d . . .
P1 P -0.52321(11) 0.02234(10) 0.32227(7) 0.01083(18) Uani 1 1 d . . .
P2 P -0.10860(11) -0.03665(10) 0.41685(7) 0.01075(18) Uani 1 1 d . . .
P3 P -0.00401(11) -0.16191(10) -0.11181(7) 0.01049(18) Uani 1 1 d . . .
O1 O -0.3842(3) 0.0256(3) 0.2148(2) 0.0150(5) Uani 1 1 d . . .
O2 O -0.6596(3) 0.0289(3) 0.2815(2) 0.0139(5) Uani 1 1 d . . .
O3 O -0.5912(3) 0.1565(3) 0.4089(2) 0.0172(5) Uani 1 1 d . . .
O4 O -0.4608(3) -0.1267(3) 0.3726(2) 0.0167(5) Uani 1 1 d . . .
O5 O 0.0419(3) -0.0137(3) 0.3509(2) 0.0133(5) Uani 1 1 d . . .
O6 O -0.0742(3) -0.1509(3) 0.5005(2) 0.0159(5) Uani 1 1 d . . .
O7 O -0.1629(3) -0.0931(3) 0.3366(2) 0.0144(5) Uani 1 1 d . . .
O8 O -0.2609(3) 0.1209(3) 0.4810(2) 0.0176(5) Uani 1 1 d . . .
H8O H -0.3642 0.1348 0.5256 0.050 Uiso 1 1 d . . .
O9 O -0.1143(3) -0.0789(3) 0.0078(2) 0.0184(5) Uani 1 1 d . . .
O10 O 0.1236(3) -0.1077(3) -0.1760(2) 0.0139(5) Uani 1 1 d . . .
O11 O -0.1187(3) -0.1498(3) -0.1738(2) 0.0147(5) Uani 1 1 d . . .
O12 O 0.1110(3) -0.3341(3) -0.1087(2) 0.0189(6) Uani 1 1 d . . .
H12O H 0.0648 -0.4017 -0.1053 0.050 Uiso 1 1 d . . .
O13 O 0.1335(3) -0.6624(3) 0.3269(2) 0.0166(5) Uani 1 1 d . . .
O14 O -0.0135(3) -0.4120(3) 0.3708(2) 0.0199(6) Uani 1 1 d . . .
O15 O -0.1508(3) -0.6755(3) 0.3868(2) 0.0180(5) Uani 1 1 d . . .
O16 O -0.3032(3) -0.4279(3) 0.4410(2) 0.0228(6) Uani 1 1 d . . .
O17 O -0.1269(3) -0.2851(3) 0.1666(2) 0.0178(5) Uani 1 1 d . . .
O18 O 0.0615(4) -0.5288(3) 0.1079(3) 0.0241(6) Uani 1 1 d . . .
O19 O 0.1164(3) -0.2181(3) 0.1291(2) 0.0177(5) Uani 1 1 d . . .
O20 O 0.3079(3) -0.4596(3) 0.1019(3) 0.0249(6) Uani 1 1 d . . .
N1 N -0.5608(4) -0.3433(4) 0.6649(3) 0.0242(7) Uani 1 1 d . . .
N2 N -0.3990(4) -0.7241(4) 0.7756(3) 0.0246(7) Uani 1 1 d . . .
N3 N -0.6021(5) -0.7727(4) 1.0824(3) 0.0313(8) Uani 1 1 d . . .
C1 C -0.0004(5) -0.5397(4) 0.3642(3) 0.0158(7) Uani 1 1 d . . .
C2 C -0.1678(4) -0.5469(4) 0.4020(3) 0.0147(7) Uani 1 1 d . . .
C3 C 0.0208(5) -0.3969(4) 0.1310(3) 0.0159(7) Uani 1 1 d . . .
C4 C 0.1633(5) -0.3573(4) 0.1184(3) 0.0156(7) Uani 1 1 d . . .
C5 C -0.4749(6) -0.4592(5) 0.7309(4) 0.0273(9) Uani 1 1 d . . .
H5A H -0.5429 -0.4292 0.8121 0.033 Uiso 1 1 calc R . .
H5B H -0.3654 -0.4671 0.7174 0.033 Uiso 1 1 calc R . .
C6 C -0.4500(7) -0.6114(5) 0.6951(4) 0.0307(10) Uani 1 1 d . . .
H6A H -0.5550 -0.5981 0.6922 0.037 Uiso 1 1 calc R . .
H6B H -0.3632 -0.6505 0.6188 0.037 Uiso 1 1 calc R . .
C7 C -0.5427(5) -0.7004(5) 0.8844(4) 0.0275(9) Uani 1 1 d . . .
H7A H -0.6259 -0.7149 0.8681 0.033 Uiso 1 1 calc R . .
H7B H -0.5977 -0.5984 0.9214 0.033 Uiso 1 1 calc R . .
C8 C -0.4762(6) -0.8112(6) 0.9631(4) 0.0372(12) Uani 1 1 d . . .
H8A H -0.4452 -0.9110 0.9334 0.045 Uiso 1 1 calc R . .
H8B H -0.3744 -0.8137 0.9634 0.045 Uiso 1 1 calc R . .
