#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/41/7204167.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_7204167
loop_
_publ_author_name
'Myriam Riou-Cavellec'
'Catherine Albinet'
'Jean-Marc Grenèche'
'Gérard Férey'
_publ_section_title
;
 Study of the iron/trimesic acid system for the hydrothermal synthesis
 of hybrid materials
;
_journal_issue                   12
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              3166
_journal_page_last               3171
_journal_paper_doi               10.1039/b104495h
_journal_volume                  11
_chemical_formula_sum            'C9 H15 Fe1.5 O12'
_chemical_formula_weight         398.99
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.0040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5592(4)
_cell_length_b                   12.9874(2)
_cell_length_c                   6.60310(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1396.14(4)
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4811
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.644
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_F_000             816
_refine_diff_density_max         0.925
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(3)
_refine_ls_extinction_coef       0.0046(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2884
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_obs          0.0578
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1142P)²+3.9578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1606
_refine_ls_wR_factor_obs         0.1540
_reflns_number_observed          2743
_reflns_number_total             2884
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b104495h.txt
_cod_data_source_block           ca20sa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+3.9578P] 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^)+(0.1142P)^2^+3.9578P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C9 H15 Fe1.50 O12'
_cod_database_code               7204167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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 0.74122(4) 0.76378(6) 0.71388(11) 0.0236(2) Uani 1 d . .
Fe2 Fe 1.0000 0.04879(8) 1.0000 0.0268(3) Uani 1 d S .
O1 O 0.8218(2) 0.8711(3) 0.6536(7) 0.0293(8) Uani 1 d . .
O2 O 1.0859(3) -0.0470(5) 0.9612(8) 0.0520(15) Uani 1 d . .
O3 O 1.0649(2) 0.1954(3) 1.0186(7) 0.0294(8) Uani 1 d . .
O4 O 0.6586(2) 0.6515(4) 0.7521(7) 0.0321(9) Uani 1 d . .
O5 O 0.8436(2) 0.6697(3) 0.8574(7) 0.0293(8) Uani 1 d . .
O6 O 0.9447(3) 0.0457(4) 0.6487(7) 0.0369(9) Uani 1 d . .
O7 O 0.6456(2) 0.8705(3) 0.5923(7) 0.0295(8) Uani 1 d . .
O8 O 0.7644(3) 0.8318(4) 1.0344(7) 0.0340(9) Uani 1 d . .
O9 O 0.7204(2) 0.7019(4) 0.3888(7) 0.0377(10) Uani 1 d . .
O10 O 0.5682(3) 1.3523(4) 0.5608(8) 0.0377(10) Uani 1 d . .
O11 O 0.7846(2) 0.5252(3) 0.9077(8) 0.0341(9) Uani 1 d . .
O12 O 0.7140(2) 1.0136(3) 0.5824(8) 0.0323(9) Uani 1 d . .
C1A C 0.9272(3) 0.4133(4) 0.9628(8) 0.0242(10) Uani 1 d . .
H1A H 0.8790(3) 0.3775(4) 0.9419(8) 0.029 Uiso 1 calc R .
C2A C 1.0000 0.3586(6) 1.0000 0.0234(13) Uani 1 d S .
C3A C 0.9261(3) 0.5201(4) 0.9567(8) 0.0242(10) Uani 1 d . .
C4A C 1.0000 0.5742(6) 1.0000 0.0222(13) Uani 1 d S .
H4A H 1.0000 0.6458(6) 1.0000 0.027 Uiso 1 calc SR .
C5A C 0.8456(3) 0.5772(4) 0.9041(7) 0.0220(9) Uani 1 d . .
C6A C 1.0000 0.2461(7) 1.0000 0.028(2) Uani 1 d S .
C7B C 0.5000 1.1892(6) 0.5000 0.0213(13) Uani 1 d S .
C8B C 0.5728(3) 1.1347(4) 0.5377(8) 0.0228(10) Uani 1 d . .
H8B H 0.6214(3) 1.1705(4) 0.5630(8) 0.027 Uiso 1 calc R .
C9B C 0.5000 1.3041(7) 0.5000 0.029(2) Uani 1 d S .
C10B C 0.5733(3) 1.0275(4) 0.5377(8) 0.0230(10) Uani 1 d . .
C11B C 0.5000 0.9756(6) 0.5000 0.0225(12) Uani 1 d S .
H11B H 0.5000 0.9040(6) 0.5000 0.027 Uiso 1 calc SR .
C12B C 0.6502(3) 0.9668(4) 0.5753(8) 0.0236(9) Uani 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
O5 Fe1 O7 173.9(2) . . ?
O5 Fe1 O1 87.1(2) . . ?
O7 Fe1 O1 89.3(2) . . ?
O5 Fe1 O4 93.1(2) . . ?
O7 Fe1 O4 90.8(2) . . ?
O1 Fe1 O4 176.0(2) . . ?
O5 Fe1 O8 88.9(2) . . ?
O7 Fe1 O8 86.3(2) . . ?
O1 Fe1 O8 91.2(2) . . ?
O4 Fe1 O8 92.9(2) . . ?
O5 Fe1 O9 91.7(2) . . ?
O7 Fe1 O9 93.0(2) . . ?
O1 Fe1 O9 86.3(2) . . ?
O4 Fe1 O9 89.7(2) . . ?
O8 Fe1 O9 177.4(2) . . ?
O2 Fe2 O2 105.0(4) 2_757 . ?
O2 Fe2 O6 84.8(2) 2_757 2_757 ?
O2 Fe2 O6 93.9(2) . 2_757 ?
O2 Fe2 O6 93.9(2) 2_757 . ?
O2 Fe2 O6 84.8(2) . . ?
O6 Fe2 O6 177.9(3) 2_757 . ?
O2 Fe2 O3 98.2(2) 2_757 2_757 ?
O2 Fe2 O3 155.7(2) . 2_757 ?
O6 Fe2 O3 95.2(2) 2_757 2_757 ?
O6 Fe2 O3 86.6(2) . 2_757 ?
O2 Fe2 O3 155.7(2) 2_757 . ?
O2 Fe2 O3 98.2(2) . . ?
O6 Fe2 O3 86.6(2) 2_757 . ?
O6 Fe2 O3 95.2(2) . . ?
O3 Fe2 O3 60.0(2) 2_757 . ?
C6A O3 Fe2 90.9(4) . . ?
C5A O5 Fe1 128.4(3) . . ?
C12B O7 Fe1 128.4(3) . . ?
C3A C1A C2A 120.9(5) . . ?
C3A C1A H1A 119.5(3) . . ?
C2A C1A H1A 119.5(4) . . ?
C1A C2A C1A 119.1(7) . 2_757 ?
C1A C2A C6A 120.5(4) . . ?
C1A C2A C6A 120.5(4) 2_757 . ?
C1A C3A C4A 119.4(5) . . ?
C1A C3A C5A 119.8(5) . . ?
C4A C3A C5A 120.8(5) . . ?
C3A C4A C3A 120.1(7) . 2_757 ?
C3A C4A H4A 119.9(3) . . ?
C3A C4A H4A 119.9(3) 2_757 . ?
O5 C5A O11 125.0(5) . . ?
O5 C5A C3A 117.9(4) . . ?
O11 C5A C3A 117.0(5) . . ?
O3 C6A O3 118.2(7) . 2_757 ?
O3 C6A C2A 120.9(4) . . ?
O3 C6A C2A 120.9(4) 2_757 . ?
C8B C7B C8B 119.3(7) 2_656 . ?
C8B C7B C9B 120.4(3) 2_656 . ?
C8B C7B C9B 120.4(3) . . ?
C10B C8B C7B 120.7(5) . . ?
C10B C8B H8B 119.7(3) . . ?
C7B C8B H8B 119.7(3) . . ?
O10 C9B O10 121.3(8) 2_656 . ?
O10 C9B C7B 119.4(4) 2_656 . ?
O10 C9B C7B 119.4(4) . . ?
C8B C10B C11B 118.7(5) . . ?
C8B C10B C12B 122.0(5) . . ?
C11B C10B C12B 119.3(5) . . ?
C10B C11B C10B 121.9(7) 2_656 . ?
C10B C11B H11B 119.0(4) 2_656 . ?
C10B C11B H11B 119.0(4) . . ?
O7 C12B O12 124.2(5) . . ?
O7 C12B C10B 116.8(4) . . ?
O12 C12B C10B 119.0(5) . . ?
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 O5 2.084(4) . ?
Fe1 O7 2.092(4) . ?
Fe1 O1 2.127(4) . ?
Fe1 O4 2.137(4) . ?
Fe1 O8 2.186(4) . ?
Fe1 O9 2.191(4) . ?
Fe2 O2 2.045(5) 2_757 ?
Fe2 O2 2.045(5) . ?
Fe2 O6 2.154(4) 2_757 ?
Fe2 O6 2.154(4) . ?
Fe2 O3 2.199(4) 2_757 ?
Fe2 O3 2.199(4) . ?
O3 C6A 1.281(6) . ?
O5 C5A 1.238(7) . ?
O7 C12B 1.261(7) . ?
O10 C9B 1.275(6) . ?
O11 C5A 1.273(6) . ?
O12 C12B 1.259(6) . ?
C1A C3A 1.387(8) . ?
C1A C2A 1.401(6) . ?
C1A H1A 0.93 . ?
C2A C1A 1.401(6) 2_757 ?
C2A C6A 1.462(12) . ?
C3A C4A 1.408(6) . ?
C3A C5A 1.517(7) . ?
C4A C3A 1.408(6) 2_757 ?
C4A H4A 0.93 . ?
C6A O3 1.281(6) 2_757 ?
C7B C8B 1.399(6) 2_656 ?
C7B C8B 1.399(6) . ?
C7B C9B 1.493(12) . ?
C8B C10B 1.391(8) . ?
C8B H8B 0.93 . ?
C9B O10 1.275(6) 2_656 ?
C10B C11B 1.390(6) . ?
C10B C12B 1.503(7) . ?
C11B C10B 1.390(6) 2_656 ?
C11B H11B 0.93 . ?
