#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314121.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_4314121
loop_
_publ_author_name
'Myriam Riou-Cavellec'
'Cédric Lesaint'
'Marc Noguès'
'Jean-Marc Grenèche'
'Gérard Férey'
_publ_section_title
;
 Synthesis, Structure, and Mössbauer Study of [Fe(H2O)2(C9O6H4)].H2O: A
 Two-Dimensional Iron(II) Trimellitate (MIL-67)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5669
_journal_page_last               5674
_journal_paper_doi               10.1021/ic020715y
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C9 H10 Fe O9'
_chemical_formula_weight         318.02
_chemical_name_common            MIL-67
_chemical_name_systematic
;
  ?
;
_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
_cell_angle_alpha                78.7580(10)
_cell_angle_beta                 89.542(2)
_cell_angle_gamma                65.1970(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9671(2)
_cell_length_b                   7.3089(3)
_cell_length_c                   12.5097(3)
_cell_measurement_temperature    293(2)
_cell_volume                     565.21(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3913
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.377
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             324
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0000(36)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.952
_refine_ls_goodness_of_fit_obs   0.974
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_restrained_S_obs      0.974
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_obs          0.0370
_refine_ls_shift/esd_max         -0.421
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0712P)²+0.2821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1045
_refine_ls_wR_factor_obs         0.0976
_reflns_number_observed          2335
_reflns_number_total             2773
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020715y.cif
_cod_data_source_block           cl039sa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.2821P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.2821P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4314121
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.0000 0.01817(14) Uani 1 d S .
Fe2 Fe -0.5000 1.0000 0.0000 0.01968(14) Uani 1 d S .
O1 O -0.2052(3) 0.4224(2) 0.10331(13) 0.0245(3) Uani 1 d . .
O2 O -0.5322(3) 0.7836(3) 0.12770(15) 0.0323(4) Uani 1 d . .
O3 O 0.2045(2) 0.4196(3) 0.14457(12) 0.0256(3) Uani 1 d . .
O4 O -0.1534(3) 0.8266(3) 0.02324(15) 0.0252(3) Uani 1 d . .
O5 O -0.4897(3) 1.1907(3) 0.09939(14) 0.0293(4) Uani 1 d . .
O6 O 0.2271(3) 0.2847(4) 0.5590(2) 0.0459(5) Uani 1 d . .
O7 O 0.5298(4) 0.2074(4) 0.6561(2) 0.0547(6) Uani 1 d . .
O8 O -0.0081(3) 0.0839(3) 0.1558(2) 0.0410(5) Uani 1 d . .
C1 C 0.5145(3) 0.2833(3) 0.2677(2) 0.0204(4) Uani 1 d . .
C2 C 0.4003(3) 0.2998(3) 0.1624(2) 0.0195(4) Uani 1 d . .
C3 C 0.4153(4) 0.2876(3) 0.3642(2) 0.0224(4) Uani 1 d . .
H3 H 0.2731(4) 0.3119(3) 0.3629(2) 0.027 Uiso 1 calc R .
C4 C 0.7289(3) 0.2500(3) 0.2702(2) 0.0210(4) Uani 1 d . .
C5 C 0.8376(4) 0.2236(4) 0.3691(2) 0.0313(5) Uani 1 d . .
H5 H 0.9787(4) 0.2031(4) 0.3707(2) 0.038 Uiso 1 calc R .
C6 C 0.5269(4) 0.2559(4) 0.4636(2) 0.0266(5) Uani 1 d . .
C7 C -0.1550(3) 0.2500(3) 0.1679(2) 0.0230(4) Uani 1 d . .
C8 C 0.7364(4) 0.2276(4) 0.4651(2) 0.0317(5) Uani 1 d . .
H8 H 0.8094(4) 0.2112(4) 0.5308(2) 0.038 Uiso 1 calc R .
C9 C 0.4287(4) 0.2473(4) 0.5695(2) 0.0328(5) Uani 1 d . .
OW O -0.0228(4) -0.2726(3) 0.2614(2) 0.0488(6) Uani 1 d . .
H2AW H -0.5450(56) 0.8045(55) 0.1838(31) 0.043(10) Uiso 1 d . .
H2BW H -0.4454(72) 0.6621(73) 0.1282(35) 0.068(13) Uiso 1 d . .
H4AW H -0.1004(55) 0.8789(55) -0.0330(30) 0.045(9) Uiso 1 d . .
H4BW H -0.1099(60) 0.8451(61) 0.0838(33) 0.055(11) Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
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
O1 Fe1 O1 180.0 2_565 . ?
O1 Fe1 O3 93.76(6) 2_565 . ?
O1 Fe1 O3 86.24(6) . . ?
O1 Fe1 O3 86.25(6) 2_565 2_565 ?
O1 Fe1 O3 93.75(6) . 2_565 ?
O3 Fe1 O3 180.0 . 2_565 ?
O1 Fe1 O4 89.11(6) 2_565 . ?
O1 Fe1 O4 90.89(6) . . ?
O3 Fe1 O4 88.97(6) . . ?
O3 Fe1 O4 91.03(6) 2_565 . ?
O1 Fe1 O4 90.89(6) 2_565 2_565 ?
O1 Fe1 O4 89.11(6) . 2_565 ?
O3 Fe1 O4 91.03(6) . 2_565 ?
O3 Fe1 O4 88.97(6) 2_565 2_565 ?
O4 Fe1 O4 180.000(1) . 2_565 ?
O5 Fe2 O5 180.0 2_475 . ?
O5 Fe2 O2 94.81(8) 2_475 2_475 ?
O5 Fe2 O2 85.19(8) . 2_475 ?
O5 Fe2 O2 85.19(8) 2_475 . ?
O5 Fe2 O2 94.81(8) . . ?
O2 Fe2 O2 180.0 2_475 . ?
O5 Fe2 O4 90.78(6) 2_475 2_475 ?
O5 Fe2 O4 89.22(6) . 2_475 ?
O2 Fe2 O4 90.12(7) 2_475 2_475 ?
O2 Fe2 O4 89.88(7) . 2_475 ?
O5 Fe2 O4 89.22(6) 2_475 . ?
O5 Fe2 O4 90.78(6) . . ?
O2 Fe2 O4 89.88(7) 2_475 . ?
O2 Fe2 O4 90.12(7) . . ?
O4 Fe2 O4 180.0 2_475 . ?
C7 O1 Fe1 124.93(14) . . ?
Fe2 O2 H2AW 119.7(28) . . ?
Fe2 O2 H2BW 113.1(30) . . ?
H2AW O2 H2BW 111.8(39) . . ?
C2 O3 Fe1 128.60(14) . . ?
Fe2 O4 Fe1 120.01(8) . . ?
Fe2 O4 H4AW 107.2(22) . . ?
Fe1 O4 H4AW 96.1(23) . . ?
Fe2 O4 H4BW 108.0(25) . . ?
Fe1 O4 H4BW 114.6(26) . . ?
H4AW O4 H4BW 109.8(34) . . ?
C2 O5 Fe2 141.2(2) 1_465 . ?
C3 C1 C4 119.3(2) . . ?
C3 C1 C2 120.7(2) . . ?
C4 C1 C2 119.9(2) . . ?
O5 C2 O3 125.6(2) 1_645 . ?
O5 C2 C1 115.9(2) 1_645 . ?
O3 C2 C1 118.5(2) . . ?
C1 C3 C6 120.6(2) . . ?
C1 C3 H3 119.68(13) . . ?
C6 C3 H3 119.68(13) . . ?
C5 C4 C1 119.8(2) . . ?
C5 C4 C7 118.0(2) . 1_655 ?
C1 C4 C7 122.2(2) . 1_655 ?
C8 C5 C4 120.3(2) . . ?
C8 C5 H5 119.86(14) . . ?
C4 C5 H5 119.86(14) . . ?
C8 C6 C3 119.7(2) . . ?
C8 C6 C9 118.3(2) . . ?
C3 C6 C9 122.0(2) . . ?
O8 C7 O1 124.5(2) . . ?
O8 C7 C4 118.5(2) . 1_455 ?
O1 C7 C4 116.9(2) . 1_455 ?
C6 C8 C5 120.3(2) . . ?
C6 C8 H8 119.87(14) . . ?
C5 C8 H8 119.87(14) . . ?
O7 C9 O6 124.7(2) . . ?
O7 C9 C6 121.7(3) . . ?
O6 C9 C6 113.6(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
Fe1 O1 2.098(2) 2_565 ?
Fe1 O1 2.098(2) . ?
Fe1 O3 2.138(2) . ?
Fe1 O3 2.138(2) 2_565 ?
Fe1 O4 2.247(2) . ?
Fe1 O4 2.247(2) 2_565 ?
Fe2 O5 2.062(2) 2_475 ?
Fe2 O5 2.062(2) . ?
Fe2 O2 2.100(2) 2_475 ?
Fe2 O2 2.100(2) . ?
Fe2 O4 2.196(2) 2_475 ?
Fe2 O4 2.196(2) . ?
O1 C7 1.265(3) . ?
O2 H2AW 0.74(4) . ?
O2 H2BW 0.84(5) . ?
O3 C2 1.266(3) . ?
O4 H4AW 0.89(4) . ?
O4 H4BW 0.87(4) . ?
O5 C2 1.252(3) 1_465 ?
O6 C9 1.315(4) . ?
O7 C9 1.213(3) . ?
O8 C7 1.253(3) . ?
C1 C3 1.385(3) . ?
C1 C4 1.409(3) . ?
C1 C2 1.503(3) . ?
C2 O5 1.252(3) 1_645 ?
C3 C6 1.398(3) . ?
C3 H3 0.93 . ?
C4 C5 1.393(3) . ?
C4 C7 1.508(3) 1_655 ?
C5 C8 1.387(4) . ?
C5 H5 0.93 . ?
C6 C8 1.385(4) . ?
C6 C9 1.489(3) . ?
C7 C4 1.508(3) 1_455 ?
C8 H8 0.93 . ?
