An S = 12 semiquinoid radical-bridged Mn6 wheel complex assembled from an asymmetric redox-active bridging ligand.
Jeon, Ie-Rang; David Harris, T.; Chemical communications (Cambridge, England) 52 (2016) 1006–1008; doi:10.1039/c5cc08482b

data_7118344
_publ_section_title
;
 An S = 12 semiquinoid radical-bridged Mn6 wheel complex assembled from an
 asymmetric redox-active bridging ligand.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1006
_journal_page_last               1008
_journal_paper_doi               10.1039/c5cc08482b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'3(C20 H20 Co2), C108 H60 Mn6 N24 O24, 8(C2 H6 O S)'
_chemical_formula_sum            'C184 H162 Co6 Mn6 N24 O32 S8'
_chemical_formula_weight         4161.07
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-02 deposited with the CCDC.
2015-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.1209(12)
_cell_length_b                   23.1209(12)
_cell_length_c                   27.281(2)
_cell_measurement_reflns_used    1490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.897
_cell_measurement_theta_min      2.737
_cell_volume                     12629.9(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9223
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        50.455
_diffrn_reflns_theta_max         50.455
_diffrn_reflns_theta_min         3.824
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.651
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1197 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.7629.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             6390
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.1767
_refine_ls_R_factor_gt           0.0905
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1152
_reflns_number_total             2910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08482b2.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        12629.7(16)
_cod_database_code               7118344
_chemw03_alert_2_a
;
PROBLEM: The ratio of given/expected molecular weight 
as calculated from the _atom_site* data lies outside 
the range 0.90 <> 1.10
RESPONSE: Residual electron density found in the difference 
Fourier map was removed using the solvent mask protocol 
included in Olex2. This residual electron density likely 
arises from either residual DMSO solvent molecules. 8 DMSO 
solvent molecules are confirmed by elemental analyses and 
are taken into consideration for the molecular formula.  
Therefore, there is a hugh difference in given and expected 
molecular weight.
;
_thetm01_alert_3_a
;
PROBLEM: The value of sine(theta_max)/wavelength is less 
than 0.550
RESPONSE: The crystal diffracted weakly at high resolution 
although this was the best crystal we could obtain. 
;
_plat051_alert_1_a
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0
RESPONSE: see the answer for the chemw03 alert 2A
;
_plat234_alert_4_a
;
PROBLEM: Large Hirshfeld Difference C2     --  C3
RESPONSE: RIGU restraints were applied to atoms in the disordered
ligand. Several of the atoms were still not ideally shaped, however, 
this does not indicate an incorrect atom-type assignment
;
_plat234_alert_4_b
;
PROBLEM: Large Hirshfeld Difference 
RESPONSE: RIGU restraints were applied to atoms in the disordered
ligand. Several of the atoms were still not ideally shaped, however, 
this does not indicate an incorrect atom-type assignment
;
_plat341_alert_3_b
;
PROBLEM: Low Bond Precision on  C-C Bonds
RESPONSE: This alert is generated due to disorder in the structure.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C27-C28 \\sim C24-C28 \\sim C24-C25 \\sim C25-C26 \\sim C26-C27 \\sim C20-C19
\\sim C20-C21 \\sim C21-C22
 \\sim C23-C22 \\sim C19-C23
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C20, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Co2, Co2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Co2(0.9) Co2A(0.1)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C26(H26), C27(H27), C28(H28)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C1(H1), C2(H2), C3(H3),
 C4(H4), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              8355
_shelx_hkl_checksum              55758
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'