#------------------------------------------------------------------------------
#$Date: 2019-11-22 17:58:56 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231207 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/29/1552956.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_1552956
loop_
_publ_author_name
'Ponce, Aldo'
'Brostoff, Lynn B.'
'Gibbons, Sarah K.'
'Zavalij, Peter'
'Viragh, Carol'
'Hooper, Joseph'
'Alnemrat, Sufian'
'Gaskell, Karen J.'
'Eichhorn, Bryan'
_publ_section_title
;
 Elucidation of the Fe(III) Gallate Structure in Historical Iron Gall Ink.
;
_journal_issue                   10
_journal_name_full               'Analytical chemistry'
_journal_page_first              5152
_journal_page_last               5158
_journal_paper_doi               10.1021/acs.analchem.6b00088
_journal_volume                  88
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C7 H3 Fe O5, 3.2(H2 O)'
_chemical_formula_sum            'C7 H9.37 Fe O8.18'
_chemical_formula_weight         280.29
_chemical_name_common            'Iron gallate hydrate'
_chemical_name_systematic        'Iron gallate tri-hydrate'
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.7445(16)
_cell_length_b                   8.7445(16)
_cell_length_c                   10.935(2)
_cell_measurement_reflns_used    2322
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.7
_cell_volume                     724.1(2)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0603155
_diffrn_orient_matrix_UB_12      -0.0084796
_diffrn_orient_matrix_UB_13      -0.0794817
_diffrn_orient_matrix_UB_21      -0.0575698
_diffrn_orient_matrix_UB_22      -0.1316162
_diffrn_orient_matrix_UB_23      0.0029853
_diffrn_orient_matrix_UB_31      -0.1024368
_diffrn_orient_matrix_UB_32      -0.0061978
_diffrn_orient_matrix_UB_33      0.0451258
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12499
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.968
_diffrn_reflns_theta_min         2.690
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1415
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0100P)²+0.9520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1262
_reflns_number_total             1415
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ac6b00088_si_002.cif
_cod_data_source_block           2352
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Trigonal' was changed to
'trigonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        724.2(3)
_cod_database_code               1552956
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.977
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.95363(8) 1.0000 0.3333 0.01675(15) Uani 1 2 d S T P . .
O1 O 0.8890(3) 0.8890(3) 0.5000 0.0198(7) Uani 1 2 d S T P . .
C1 C 0.7344(6) 0.7344(6) 0.5000 0.0224(11) Uani 1 2 d S T P . .
C2 C 0.6301(5) 0.6845(5) 0.3956(3) 0.0276(8) Uani 1 1 d . . . . .
O2 O 0.6949(4) 0.8030(4) 0.3020(3) 0.0346(7) Uani 1 1 d . . . . .
H2 H 0.645(15) 0.769(16) 0.247(10) 0.06(4) Uiso 0.5 1 d . . P . .
C3 C 0.4718(6) 0.5253(5) 0.3946(4) 0.0314(10) Uani 1 1 d . . . . .
H3 H 0.400(9) 0.488(9) 0.329(6) 0.08(2) Uiso 1 1 d . . . . .
C4 C 0.4211(6) 0.4211(6) 0.5000 0.0297(13) Uani 1 2 d S T P . .
C5 C 0.2517(6) 0.2517(6) 0.5000 0.0249(12) Uani 1 2 d S T P . .
O5 O 0.2001(3) 0.1678(3) 0.3999(2) 0.0298(7) Uani 1 1 d . . . . .
O1W O 0.5372(12) 0.6994(16) 0.0950(9) 0.062(3) Uiso 0.50(2) 1 d . U . A 1
O2W O 0.434(3) 0.846(2) 0.2362(15) 0.093(6) Uiso 0.308(12) 1 d . U . B 1
O3W O 0.451(4) 0.731(4) 0.141(2) 0.072(6) Uiso 0.175(13) 1 d . U . C 2
O4W O 0.539(4) 0.790(6) 0.099(3) 0.069(6) Uiso 0.177(18) 1 d . U . D 3
O5W O 0.468(5) 0.676(5) 0.005(3) 0.078(6) Uiso 0.142(10) 1 d . U . E 4
O6W O 0.550(5) 0.499(5) -0.058(4) 0.108(12) Uiso 0.19(2) 1 d . U . F -4
O7W O 0.569(11) 0.577(11) 0.121(8) 0.076(9) Uiso 0.070(14) 1 d . U . G 5
O8W O 0.639(19) 0.639(19) 0.0000 0.080(8) Uiso 0.049(15) 2 d S U . H 3
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
O1 Fe1 O1 175.45(9) . 3_674
O1 Fe1 O5 87.97(11) . 1_665
O1 Fe1 O5 95.20(8) 3_674 1_665
O1 Fe1 O5 95.20(8) . 5_665
O1 Fe1 O5 87.97(10) 3_674 5_665
O5 Fe1 O5 91.67(16) 1_665 5_665
O1 Fe1 O2 97.14(8) . 5_675
O1 Fe1 O2 79.75(11) 3_674 5_675
O5 Fe1 O2 87.94(13) 1_665 5_675
O5 Fe1 O2 167.63(10) 5_665 5_675
O1 Fe1 O2 79.75(11) . .
O1 Fe1 O2 97.14(8) 3_674 .
O5 Fe1 O2 167.62(10) 1_665 .
O5 Fe1 O2 87.94(13) 5_665 .
O2 Fe1 O2 95.1(2) 5_675 .
C1 O1 Fe1 112.47(8) . 2_765
C1 O1 Fe1 112.47(8) . .
Fe1 O1 Fe1 135.06(16) 2_765 .
O1 C1 C2 119.0(2) . .
O1 C1 C2 119.0(2) . 4_556
C2 C1 C2 122.0(5) . 4_556
O2 C2 C1 114.9(3) . .
O2 C2 C3 125.8(4) . .
C1 C2 C3 119.3(4) . .
C2 O2 Fe1 112.0(2) . .
C2 O2 H2 112(10) . .
Fe1 O2 H2 132(9) . .
C2 C3 C4 118.7(4) . .
C2 C3 H3 122(4) . .
C4 C3 H3 119(4) . .
C3 C4 C3 122.0(5) . 4_556
C3 C4 C5 119.0(3) . .
C3 C4 C5 119.0(3) 4_556 .
O5 C5 O5 124.3(5) . 4_556
O5 C5 C4 117.8(2) . .
O5 C5 C4 117.8(2) 4_556 .
C5 O5 Fe1 131.7(3) . 1_445
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0085(12) .
Fe1 O1 2.0086(12) 3_674
Fe1 O5 2.041(3) 1_665
Fe1 O5 2.041(3) 5_665
Fe1 O2 2.075(3) 5_675
Fe1 O2 2.075(3) .
O1 C1 1.353(6) .
O1 Fe1 2.0085(12) 2_765
C1 C2 1.388(4) .
C1 C2 1.388(4) 4_556
C2 O2 1.361(5) .
C2 C3 1.388(5) .
O2 H2 0.71(11) .
C3 C4 1.396(4) .
C3 H3 0.90(6) .
C4 C3 1.397(4) 4_556
C4 C5 1.482(7) .
C5 O5 1.269(4) .
C5 O5 1.269(4) 4_556
O5 Fe1 2.041(3) 1_445
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O2 H2 O1W 0.71(11) 1.86(11) 2.569(10) 173(13)
O2 H2 O3W 0.71(11) 1.94(11) 2.59(2) 151(13)
O2 H2 O4W 0.71(11) 1.92(11) 2.58(3) 153(14)
O2 H2 O7W 0.71(11) 2.01(14) 2.62(9) 144(13)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Fe1 O1 C1 C2 171.1(2) 2_765 .
Fe1 O1 C1 C2 -8.9(2) . .
Fe1 O1 C1 C2 -8.9(2) 2_765 4_556
Fe1 O1 C1 C2 171.1(2) . 4_556
O1 C1 C2 O2 -1.6(4) . .
C2 C1 C2 O2 178.4(4) 4_556 .
O1 C1 C2 C3 179.5(3) . .
C2 C1 C2 C3 -0.5(3) 4_556 .
C1 C2 O2 Fe1 11.0(4) . .
C3 C2 O2 Fe1 -170.2(4) . .
O2 C2 C3 C4 -177.8(4) . .
C1 C2 C3 C4 1.0(6) . .
C2 C3 C4 C3 -0.5(3) . 4_556
C2 C3 C4 C5 179.5(3) . .
C3 C4 C5 O5 32.0(3) . .
C3 C4 C5 O5 -148.0(3) 4_556 .
C3 C4 C5 O5 -148.0(3) . 4_556
C3 C4 C5 O5 32.0(3) 4_556 4_556
O5 C5 O5 Fe1 29.10(19) 4_556 1_445
C4 C5 O5 Fe1 -150.90(19) . 1_445
