Unique anisotropic optical properties of a highly stable metal-organic framework based on trinuclear iron(iii) secondary building units linked by tetracarboxylic linkers with an anthracene core.
Vinogradov, A. V.; Milichko, V. A.; Zaake-Hertling, H; Aleksovska, A.; Gruschinski, S.; Schmorl, S.; Kersting, B.; Zolnhofer, E. M.; Sutter, J.; Meyer, K.; Lönnecke, P; Hey-Hawkins, E; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7244–7249; doi:10.1039/c6dt00390g

data_7038405
_publ_section_title
;
 Unique anisotropic optical properties of a highly stable metal-organic
 framework based on trinuclear iron(iii) secondary building units linked
 by tetracarboxylic linkers with an anthracene core.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7244
_journal_page_last               7249
_journal_paper_doi               10.1039/c6dt00390g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C114 H110 Cl Fe3 N6 O22'
_chemical_formula_weight         2119.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_audit_update_record
;
2015-04-30 deposited with the CCDC.
2016-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                118.491(4)
_cell_angle_beta                 99.961(4)
_cell_angle_gamma                100.101(4)
_cell_formula_units_Z            1
_cell_length_a                   13.3774(7)
_cell_length_b                   17.0481(7)
_cell_length_c                   17.4322(7)
_cell_measurement_reflns_used    13226
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      3.081
_cell_volume                     3285.2(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
 SHELXS-2013
 Program for Crystal Structure Analysis (Release 2013-1)
 G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at,
 Tammanstrasse 4, D-3400 G\"ottingen, Germany.
 G. M. Sheldrick, Acta. Cryst., 2008, A64, 112 - 122 
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55391
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.784
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.98597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       prism
_exptl_crystal_F_000             1107
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
All attempts to locate highly disordered solvent molecules failed. The 
electron density for these highly disordered solvent molecules had been 
removed with the SQUEEZE routine implemented in PLATON.

Based on magnetic measurements the oxidation state of all iron cations 
seems to be +3. From the squeeze electron count we suggest to remove the 
electron density of 6 poorly defined and diffuse oriented DEF 
(Diethylformamide) molecules from the unit cell and one chloride anion 
for charge neutrality reasons ((6 x 56) + (1 x 17) = 353 electrons). 

These values correspond well with the estimated "squeezed" electron density 
of 344 electrons. A volume of 322 A^3^ for one DEF molecule (Approximately 
46 A^3^ for each non-hydrogen atom) is acceptable for extremely loosely 
packed and disordered solvent molecules. 
;
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         13416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+1.1599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9248
_reflns_number_total             13416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00390g1.cif
_cod_data_source_block           x1842sqfin
_cod_depositor_comments          'Adding full bibliography for 7038405.cif.'
_cod_original_cell_volume        3285.1(3)
_cod_database_code               7038405
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              93392
_shelx_fab_checksum              71111