A self-assembled octanuclear complex bearing the uncommon close-packed {Fe4Mn4(μ4-O)4(μ-O)4} molecular core.
Nesterova, Oksana V.; Chygorin, Eduard N.; Kokozay, Vladimir N.; Omelchenko, Irina V.; Shishkin, Oleg V.; Boča, Roman; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14918–14924; doi:10.1039/c5dt02076j

data_7036016
_publ_section_title
;
 A self-assembled octanuclear complex bearing the uncommon close-packed
 {Fe4Mn4(\m4-O)4(\m-O)4} molecular core.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14918
_journal_page_last               14924
_journal_paper_doi               10.1039/c5dt02076j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C68 H68 Fe4 Mn4 N12 O24, 2(C3 H7 N O)'
_chemical_formula_sum            'C74 H82 Fe4 Mn4 N14 O26'
_chemical_formula_weight         2026.70
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 122.487(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.509(2)
_cell_length_b                   11.1843(17)
_cell_length_c                   27.176(4)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    298
_cell_measurement_theta_max      2.5
_cell_measurement_theta_min      24.5
_cell_volume                     4232.6(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies, 2010
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies, 2010
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies, 2010
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur Sapphire 3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1547
_diffrn_reflns_av_unetI/netI     0.1324
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33532
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  0.6918
_exptl_absorpt_correction_T_min  0.6918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 2010
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                3849
_reflns_number_total             7391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02076j2.cif
_cod_data_source_block           koko412
_cod_depositor_comments          'Adding full bibliography for 7036016.cif.'
_cod_original_cell_volume        4232.6(10)
_cod_database_code               7036016
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1S-C1S
 1.25 with sigma of 0.02
 N1S-C1S
 1.35 with sigma of 0.02
 N1S-C2S = N1S-C3S
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N1S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(O1S) \\sim Ueq: with sigma of
0.06 and sigma for terminal atoms of 0.12
Uanis(C2S) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C32(H32), C1S(H1S)
;
_olex2_submission_special_instructions 'No special instructions were received'