Elucidation of the Fe(III) Gallate Structure in Historical Iron Gall Ink.
Ponce, Aldo; Brostoff, Lynn B.; Gibbons, Sarah K.; Zavalij, Peter; Viragh, Carol; Hooper, Joseph; Alnemrat, Sufian; Gaskell, Karen J.; Eichhorn, Bryan; Analytical chemistry 88 (2016) 5152–5158; doi:10.1021/acs.analchem.6b00088

data_1552956
_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       '\f and \w 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/[\s^2^(Fo^2^)+(0.0100P)^2^+0.9520P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              49760
_shelx_hkl_checksum              21622