Ligand template synthesis of an undecametallic iron(III) complex: X-ray structure, magnetism and catecholase activity
Mal, Sunit K.; Mitra, Merry; Biswas, Bhaskar; Kaur, Gurpreet; Bag, Partha P.; Reddy, C. Malla; Choudhury, Angshuman Roy; Aliaga-Alcalde, Nuria; Ghosh, Rajarshi; Inorganica Chimica Acta 425 (2015) 61–66; doi:10.1016/j.ica.2014.09.027

data_1518336
_publ_contact_author_name
;
;
_publ_section_title
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 Ligand template synthesis of an undecametallic iron(III) complex: X-ray
 structure, magnetism and catecholase activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              61
_journal_page_last               66
_journal_paper_doi               10.1016/j.ica.2014.09.027
_journal_volume                  425
_journal_year                    2015
_chemical_formula_moiety         'C75 H45 Fe11 O57, 5.23(O)'
_chemical_formula_sum            'C75 H45 Fe11 O62.23'
_chemical_formula_weight         2556.14
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2013-10-19
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                99.165(5)
_cell_angle_beta                 99.281(5)
_cell_angle_gamma                94.805(5)
_cell_formula_units_Z            2
_cell_length_a                   14.600(3)
_cell_length_b                   14.602(3)
_cell_length_c                   23.236(4)
_cell_measurement_temperature    100.0
_cell_volume                     4795.9(16)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35467
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         0.902
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0576 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8693.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       block
_exptl_crystal_F_000             2557.7
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         16775
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0690
_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^)+(0.0836P)^2^+15.4239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9837
_reflns_number_total             16775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            S_FE_1.cif
_cod_data_source_block           s_fe_1
_cod_original_cell_volume        4795.8(14)
_cod_database_code               1518336
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C31-C30
 1.34 with sigma of 0.02
 C30-C28
 1.44 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C62) = Uanis(C64) = Uanis(C65) = Uanis(C66) = Uanis(C26) = Uanis(C28) = Uanis(C30) = Uanis(C31) = Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C51)
4. Others
 Fixed Sof: O3W(0.77044) O4W(0.73672) O5W(0.77175) O6W(0.75347) O7W(0.19804)
5.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C69(H69), C39(H39), C13(H13), C55(H55), C59(H59), C34(H34),
 C74(H74), C20(H20), C35(H35), C75(H75), C36(H36), C19(H19), C40(H40), C14(H14),
  C10(H10), C9(H9), C23(H23), C60(H60), C61(H61), C70(H70), C15(H15), C8(H8),
 C5(H5), C45(H45), C4(H4), C71(H71), C25(H25), C54(H54), C56(H56), C18(H18),
 C44(H44), C3(H3), C41(H41), C73(H73), C46(H46), C28(H28), C64(H64), C49(H49),
 C50(H50), C65(H65), C66(H66), C51(H51), C31(H31), C30(H30)
;
_shelx_hkl_checksum              26168
_shelx_res_checksum              6635
_shelxl_version_number           2013-4