# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       f.j.white@sms.ed.ac.uk
_publ_contact_author_name        'Fraser J. White'
_publ_author_name                'Euan Brechin'

data_eb9009
_database_code_depnum_ccdc_archive 'CCDC 806066'
#TrackingRef '- revised CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_compound_source        'Ross Inglis'
_exptl_crystal_recrystallization_method 
'Diffusion of Et2O into Acetone solution'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H67 Mn9 N6 O29'
_chemical_formula_sum            'C58 H69 Mn9 N6 O28.50'
_chemical_formula_weight         1800.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I 2 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, z, x'
'z, x, y'
'x, -y, -z'
'y, -z, -x'
'z, -x, -y'
'-y, z, -x'
'-z, x, -y'
'-z, -x, y'
'-x, -y, z'
'-y, -z, x'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, z+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, -z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   25.729(4)
_cell_length_b                   25.729(4)
_cell_length_c                   25.729(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17032(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2918
_cell_measurement_theta_min      2.239
_cell_measurement_theta_max      19.809

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7296
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26150
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_min       1
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5844
_reflns_number_gt                4776
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    Shelxs
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_refine_special_details          
;

#==========================================================================
The Following Model and Quality ALERTS were generated - (Acta-Mode) <<<
#==========================================================================
Format: alert-number_ALERT_alert-type_alert-level text

601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 1995.00 A**3
420_ALERT_2_B D-H Without Acceptor O1E - H1E1 ... ?
420_ALERT_2_B D-H Without Acceptor O1E - H1E2 ... ?

There was diffuse solvent which was difficult to model and so the solvent
region was treated using the Spek/van der Sluis method.
Approximately 704 electrons were removed from the unit cell. The most likely
candidate for the solvents are MeCN or NEt3

770_ALERT_2_A Suspect C-H Bond in CIF: C2E -- H1E2 .. 1.49 Ang.
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.49
220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.23 Ratio
301_ALERT_3_G Note Main Residue Disorder .................... 1.00 Perc.
041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 34.50 Deg.
O1E -C2E -H1E2 1.555 1.555 1.555
764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.16 Ratio

There is a complicated disorder situation with one of the ligands. It has been
modelled as 66% H2O 33% MeO. This, when multiplied up by the 3-fold axis,
give 2 H2O and one MeO per molecule. This composition has been dictated by the
available materials in preparation steps and to produce a charge neutral
complex. Also present is a solvent water molecule without its hydrogens
which is disordered over the three fold with a total occupancy of 50%
with respect to the main cluster. Some residual density remains but anttempts
to model it results in unreasonable chemistry or structure. The peak height
is ~0.78 eA-3 which compared to the heaviest element, Mn, is not large.

230_ALERT_2_C Hirshfeld Test Diff for C4B -- C5B .. 5.08 su
232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn2 -- N22B .. 5.04 su
341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 8

No action taken

910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1

The data collection strategy used was intended to collect fully complete data
to 2TH= 53deg. Please refer to the completeness statistics below

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 0.999 1618 1616 2
23.01 0.550 0.999 2143 2141 2
25.24 0.600 0.999 2763 2761 2
#----------------------------------------------------------- ACTA Min. Res. ---
26.37 0.625 0.999 3125 3123 2

083_ALERT_2_G SHELXL Second Parameter in WGHT unusually Large. 7.04
125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
731_ALERT_1_C Bond Calc 1.880(3), Rep 1.8797(9) ...... 3.33 su-Ra
MN3 -O333 1.555 1.555
731_ALERT_1_C Bond Calc 1.880(3), Rep 1.8798(9) ...... 3.33 su-Ra
O333 -MN3 1.555 6.566
731_ALERT_1_C Bond Calc 1.880(3), Rep 1.8798(10) ...... 3.00 su-Ra
O333 -MN3 1.555 11.665

No action taken

952_ALERT_1_C Reported and Calculated Lmax Values Differ by .. 14
953_ALERT_1_C Reported and Actual Hmax Values in FCF Differ by 10
954_ALERT_1_C Reported and Actual Kmax Values in FCF Differ by 10
955_ALERT_1_C Reported and Actual Lmax Values in FCF Differ by 14

As far as I can tell this is a matter of interpretation.
The hkl file has been checked and agrees with the Hmax, Kmax and Lmax
values reported in the cif. Shelx appears to be outputting different
values to the FCF file, which I presume is due to the equivalence of
H, K and L in the cubic crystal system.

720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 11
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O123
850_ALERT_4_G Check Flack Parameter Exact Value 0.00 and su .. 0.03

No action taken.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+7.0372P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_number_reflns         5844
_refine_ls_number_parameters     309
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1312
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.19823(3) 0.69527(3) 0.22157(3) 0.02471(18) Uani 1 1 d . . .
Mn2 Mn 0.13501(3) 0.73177(3) 0.32326(3) 0.02785(19) Uani 1 1 d . . .
Mn3 Mn 0.24651(3) 0.67297(3) 0.34215(3) 0.02472(18) Uani 1 1 d . B .
O333 O 0.30933(13) 0.69067(13) 0.30933(13) 0.0235(13) Uani 1 3 d S . .
C2A C 0.1789(2) 0.7524(2) 0.1202(2) 0.0378(14) Uani 1 1 d . . .
C1A C 0.1488(3) 0.7894(3) 0.0858(3) 0.061(2) Uani 1 1 d . . .
H1A1 H 0.1401 0.8208 0.1056 0.091 Uiso 1 1 calc R . .
H1A2 H 0.1168 0.7726 0.0739 0.091 Uiso 1 1 calc R . .
H1A3 H 0.1701 0.7990 0.0557 0.091 Uiso 1 1 calc R . .
O22A O 0.16455(14) 0.74581(15) 0.16597(15) 0.0338(9) Uani 1 1 d . . .
O21A O 0.21648(15) 0.72999(16) 0.09878(15) 0.0373(9) Uani 1 1 d . . .
O1B O 0.07747(14) 0.72756(17) 0.36656(15) 0.0370(9) Uani 1 1 d . . .
C1B C 0.0496(2) 0.6856(2) 0.3773(2) 0.0336(13) Uani 1 1 d . . .
C2B C 0.0477(2) 0.6406(2) 0.3445(2) 0.0353(13) Uani 1 1 d . . .
C6B C 0.0191(2) 0.6866(3) 0.4220(2) 0.0412(15) Uani 1 1 d . . .
H6B H 0.0197 0.7162 0.4441 0.049 Uiso 1 1 calc R . .
C5B C -0.0121(2) 0.6443(3) 0.4344(2) 0.055(2) Uani 1 1 d . . .
H5B H -0.0333 0.6458 0.4646 0.066 Uiso 1 1 calc R . .
C4B C -0.0131(3) 0.6013(3) 0.4047(3) 0.0508(18) Uani 1 1 d . . .
H4B H -0.0337 0.5724 0.4150 0.061 Uiso 1 1 calc R . .
C3B C 0.0148(2) 0.5988(3) 0.3606(3) 0.0484(17) Uani 1 1 d . . .
H3B H 0.0127 0.5685 0.3396 0.058 Uiso 1 1 calc R . .
C21B C 0.0750(2) 0.6375(2) 0.2938(2) 0.0323(12) Uani 1 1 d . . .
N22B N 0.11019(16) 0.67111(19) 0.28250(18) 0.0319(10) Uani 1 1 d . . .
C24B C 0.0620(3) 0.5966(3) 0.2558(3) 0.0508(17) Uani 1 1 d . . .
H24A H 0.0842 0.6002 0.2251 0.076 Uiso 1 1 calc R . .
H24B H 0.0254 0.6000 0.2455 0.076 Uiso 1 1 calc R . .
H24C H 0.0676 0.5624 0.2716 0.076 Uiso 1 1 calc R . .
O23B O 0.13161(14) 0.66727(15) 0.23508(14) 0.0326(9) Uani 1 1 d . . .
O1C O 0.18106(13) 0.66606(14) 0.37441(12) 0.0276(8) Uani 1 1 d . . .
C1C C 0.1792(2) 0.6616(2) 0.4269(2) 0.0297(12) Uani 1 1 d . . .
C2C C 0.2095(2) 0.6921(2) 0.4605(2) 0.0304(12) Uani 1 1 d . . .
C6C C 0.1454(2) 0.6242(2) 0.4479(2) 0.0344(13) Uani 1 1 d . . .
H6C H 0.1230 0.6046 0.4260 0.041 Uiso 1 1 calc R . .
C5C C 0.1456(2) 0.6164(2) 0.5012(3) 0.0444(15) Uani 1 1 d . . .
H5C H 0.1243 0.5898 0.5155 0.053 Uiso 1 1 calc R . .
C4C C 0.1760(3) 0.6461(3) 0.5342(2) 0.0453(16) Uani 1 1 d . . .
H4C H 0.1752 0.6405 0.5707 0.054 Uiso 1 1 calc R . .
C3C C 0.2073(2) 0.6838(2) 0.5131(2) 0.0357(13) Uani 1 1 d . . .
H3C H 0.2280 0.7046 0.5355 0.043 Uiso 1 1 calc R . .
C21C C 0.2414(2) 0.7344(2) 0.43966(19) 0.0295(12) Uani 1 1 d . . .
C24C C 0.2523(3) 0.7825(2) 0.4712(2) 0.0459(16) Uani 1 1 d . . .
H24D H 0.2746 0.8060 0.4511 0.069 Uiso 1 1 calc R . .
H24E H 0.2699 0.7728 0.5035 0.069 Uiso 1 1 calc R . .
H24F H 0.2195 0.8001 0.4793 0.069 Uiso 1 1 calc R . .
N22C N 0.26062(17) 0.72969(17) 0.39300(17) 0.0277(10) Uani 1 1 d . . .
O23C O 0.28492(13) 0.77198(14) 0.37186(14) 0.0289(8) Uani 1 1 d . . .
O123 O 0.20032(13) 0.73210(14) 0.28663(13) 0.0241(7) Uani 1 1 d . . .
O1D O 0.21213(14) 0.64156(14) 0.16930(14) 0.0291(8) Uani 1 1 d . . .
C2D C 0.1752(2) 0.6114(2) 0.1422(3) 0.0460(16) Uani 1 1 d . . .
H2D1 H 0.1505 0.5963 0.1670 0.069 Uiso 1 1 calc R . .
H2D2 H 0.1930 0.5835 0.1233 0.069 Uiso 1 1 calc R . .
H2D3 H 0.1564 0.6335 0.1175 0.069 Uiso 1 1 calc R . .
O1E O 0.28120(19) 0.61223(17) 0.38699(18) 0.0519(12) Uani 1 1 d D . .
H1E1 H 0.2578 0.5970 0.4047 0.078 Uiso 1 1 d R A 1
H1E2 H 0.2955 0.5905 0.3666 0.078 Uiso 1 1 d R A 1
C2E C 0.3204(7) 0.6009(10) 0.4180(8) 0.068(7) Uiso 0.33 1 d PD B 2
H2E1 H 0.3166 0.5653 0.4309 0.103 Uiso 0.33 1 calc PR B 2
H2E2 H 0.3207 0.6252 0.4474 0.103 Uiso 0.33 1 calc PR B 2
H2E3 H 0.3531 0.6040 0.3987 0.103 Uiso 0.33 1 calc PR B 2
O1S O 0.3635(6) 0.6141(7) 0.3912(7) 0.016(4) Uiso 0.17 1 d P C 3

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0230(4) 0.0281(4) 0.0230(4) -0.0025(3) 0.0001(3) -0.0028(3)
Mn2 0.0224(4) 0.0305(4) 0.0307(4) -0.0030(4) 0.0043(3) -0.0017(3)
Mn3 0.0243(4) 0.0262(4) 0.0236(4) -0.0026(3) 0.0032(3) -0.0016(3)
O333 0.0235(13) 0.0235(13) 0.0235(13) 0.0002(14) -0.0002(14) 0.0002(14)
C2A 0.033(3) 0.046(4) 0.034(3) 0.000(3) -0.004(3) 0.005(3)
C1A 0.070(5) 0.067(5) 0.045(4) 0.009(4) -0.005(4) 0.027(4)
O22A 0.033(2) 0.037(2) 0.031(2) -0.0006(17) -0.0045(17) 0.0031(17)
O21A 0.038(2) 0.044(2) 0.030(2) 0.0013(19) -0.0016(17) 0.0039(19)
O1B 0.0262(19) 0.049(3) 0.035(2) -0.004(2) 0.0085(17) -0.0059(18)
C1B 0.025(3) 0.047(4) 0.029(3) 0.005(3) -0.004(2) 0.000(3)
C2B 0.026(3) 0.046(3) 0.034(3) 0.011(3) 0.000(2) -0.009(3)
C6B 0.026(3) 0.057(4) 0.041(3) 0.005(3) -0.003(3) 0.004(3)
C5B 0.025(3) 0.109(6) 0.031(3) 0.019(4) 0.001(3) -0.010(4)
C4B 0.046(4) 0.070(5) 0.036(4) 0.014(3) 0.004(3) -0.029(4)
C3B 0.045(4) 0.052(4) 0.048(4) 0.007(3) -0.013(3) -0.015(3)
C21B 0.028(3) 0.034(3) 0.035(3) 0.003(2) -0.009(2) -0.004(2)
N22B 0.020(2) 0.039(3) 0.037(3) 0.005(2) 0.0054(19) -0.002(2)
C24B 0.048(4) 0.058(4) 0.046(4) -0.007(3) 0.007(3) -0.025(3)
O23B 0.0281(19) 0.043(2) 0.0269(19) -0.0065(17) -0.0013(16) -0.0106(17)
O1C 0.0245(18) 0.039(2) 0.0194(17) 0.0021(15) 0.0016(14) -0.0066(16)
C1C 0.024(3) 0.034(3) 0.031(3) 0.000(2) 0.005(2) 0.002(2)
C2C 0.029(3) 0.033(3) 0.029(3) -0.002(2) 0.009(2) -0.001(2)
C6C 0.035(3) 0.042(3) 0.027(3) -0.002(2) 0.007(2) -0.007(3)
C5C 0.040(3) 0.043(3) 0.050(4) 0.012(3) 0.019(3) -0.001(3)
C4C 0.048(4) 0.064(4) 0.024(3) 0.011(3) 0.005(3) 0.014(3)
C3C 0.043(3) 0.038(3) 0.026(3) -0.002(2) 0.005(2) 0.002(3)
C21C 0.041(3) 0.026(3) 0.021(3) -0.004(2) -0.001(2) 0.002(2)
C24C 0.070(5) 0.037(4) 0.031(3) -0.009(3) 0.011(3) -0.007(3)
N22C 0.029(2) 0.027(2) 0.027(2) 0.0019(19) 0.0024(19) -0.0036(19)
O23C 0.0309(19) 0.0270(19) 0.029(2) -0.0045(16) 0.0079(15) -0.0004(16)
O123 0.0218(17) 0.0262(18) 0.0242(18) -0.0028(14) 0.0007(14) -0.0015(15)
O1D 0.0281(19) 0.0287(19) 0.031(2) -0.0045(16) -0.0037(16) -0.0084(15)
C2D 0.036(3) 0.046(4) 0.056(4) -0.022(3) 0.000(3) -0.011(3)
O1E 0.060(3) 0.042(3) 0.053(3) 0.008(2) 0.003(2) 0.015(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O23B 1.891(4) . ?
Mn1 O123 1.924(3) . ?
Mn1 O123 1.931(4) 11_665 ?
Mn1 O1D 1.961(4) . ?
Mn1 O22A 2.118(4) . ?
Mn1 O23C 2.495(4) 11_665 ?
Mn1 Mn2 2.9036(12) 11_665 ?
Mn1 Mn2 3.2209(12) . ?
Mn2 O1B 1.856(4) . ?
Mn2 O1D 1.918(4) 6_566 ?
Mn2 O123 1.927(3) . ?
Mn2 N22B 1.986(5) . ?
Mn2 O21A 2.126(4) 6_566 ?
Mn2 O1C 2.448(4) . ?
Mn2 Mn1 2.9034(12) 6_566 ?
Mn3 O333 1.8797(9) . ?
Mn3 O1C 1.886(3) . ?
Mn3 O23C 1.930(3) 11_665 ?
Mn3 N22C 1.993(5) . ?
Mn3 O1E 2.138(4) . ?
Mn3 O123 2.402(3) . ?
O333 Mn3 1.8798(9) 6_566 ?
O333 Mn3 1.8798(10) 11_665 ?
C2A O22A 1.246(7) . ?
C2A O21A 1.252(7) . ?
C2A C1A 1.514(9) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C1A H1A3 0.9800 . ?
O21A Mn2 2.126(4) 11_665 ?
O1B C1B 1.325(7) . ?
C1B C6B 1.393(8) . ?
C1B C2B 1.432(9) . ?
C2B C3B 1.431(8) . ?
C2B C21B 1.484(8) . ?
C6B C5B 1.388(9) . ?
C6B H6B 0.9500 . ?
C5B C4B 1.345(10) . ?
C5B H5B 0.9500 . ?
C4B C3B 1.344(9) . ?
C4B H4B 0.9500 . ?
C3B H3B 0.9500 . ?
C21B N22B 1.286(7) . ?
C21B C24B 1.474(8) . ?
N22B O23B 1.343(6) . ?
C24B H24A 0.9800 . ?
C24B H24B 0.9800 . ?
C24B H24C 0.9800 . ?
O1C C1C 1.356(6) . ?
C1C C2C 1.404(8) . ?
C1C C6C 1.404(8) . ?
C2C C3C 1.371(8) . ?
C2C C21C 1.465(8) . ?
C6C C5C 1.386(9) . ?
C6C H6C 0.9500 . ?
C5C C4C 1.385(9) . ?
C5C H5C 0.9500 . ?
C4C C3C 1.373(9) . ?
C4C H4C 0.9500 . ?
C3C H3C 0.9500 . ?
C21C N22C 1.304(7) . ?
C21C C24C 1.507(8) . ?
C24C H24D 0.9800 . ?
C24C H24E 0.9800 . ?
C24C H24F 0.9800 . ?
N22C O23C 1.368(5) . ?
O23C Mn3 1.930(3) 6_566 ?
O23C Mn1 2.495(4) 6_566 ?
O123 Mn1 1.931(4) 6_566 ?
O1D C2D 1.411(7) . ?
O1D Mn2 1.919(4) 11_665 ?
C2D H2D1 0.9800 . ?
C2D H2D2 0.9800 . ?
C2D H2D3 0.9800 . ?
O1E C2E 1.319(10) . ?
O1E H1E1 0.8499 . ?
O1E H1E2 0.8498 . ?
C2E H1E2 1.4939 . ?
C2E H2E1 0.9800 . ?
C2E H2E2 0.9800 . ?
C2E H2E3 0.9800 . ?
O1S O1S 0.93(3) 6_566 ?
O1S O1S 0.93(3) 11_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O23B Mn1 O123 93.04(15) . . ?
O23B Mn1 O123 170.09(16) . 11_665 ?
O123 Mn1 O123 95.83(19) . 11_665 ?
O23B Mn1 O1D 91.31(15) . . ?
O123 Mn1 O1D 159.79(15) . . ?
O123 Mn1 O1D 78.85(14) 11_665 . ?
O23B Mn1 O22A 89.26(16) . . ?
O123 Mn1 O22A 107.25(15) . . ?
O123 Mn1 O22A 92.32(15) 11_665 . ?
O1D Mn1 O22A 92.53(15) . . ?
O23B Mn1 O23C 83.96(15) . 11_665 ?
O123 Mn1 O23C 76.35(13) . 11_665 ?
O123 Mn1 O23C 93.82(13) 11_665 11_665 ?
O1D Mn1 O23C 84.50(13) . 11_665 ?
O22A Mn1 O23C 172.53(14) . 11_665 ?
O23B Mn1 Mn2 129.83(11) . 11_665 ?
O123 Mn1 Mn2 136.95(10) . 11_665 ?
O123 Mn1 Mn2 41.13(10) 11_665 11_665 ?
O1D Mn1 Mn2 41.00(10) . 11_665 ?
O22A Mn1 Mn2 80.60(11) . 11_665 ?
O23C Mn1 Mn2 101.35(9) 11_665 11_665 ?
O23B Mn1 Mn2 60.27(11) . . ?
O123 Mn1 Mn2 33.26(10) . . ?
O123 Mn1 Mn2 128.93(10) 11_665 . ?
O1D Mn1 Mn2 148.71(11) . . ?
O22A Mn1 Mn2 99.38(11) . . ?
O23C Mn1 Mn2 80.00(8) 11_665 . ?
Mn2 Mn1 Mn2 169.81(3) 11_665 . ?
O1B Mn2 O1D 97.33(17) . 6_566 ?
O1B Mn2 O123 171.73(17) . . ?
O1D Mn2 O123 80.01(15) 6_566 . ?
O1B Mn2 N22B 90.83(18) . . ?
O1D Mn2 N22B 171.23(17) 6_566 . ?
O123 Mn2 N22B 91.47(16) . . ?
O1B Mn2 O21A 94.22(17) . 6_566 ?
O1D Mn2 O21A 91.98(16) 6_566 6_566 ?
O123 Mn2 O21A 93.69(15) . 6_566 ?
N22B Mn2 O21A 90.62(18) . 6_566 ?
O1B Mn2 O1C 91.32(15) . . ?
O1D Mn2 O1C 92.49(14) 6_566 . ?
O123 Mn2 O1C 81.02(13) . . ?
N22B Mn2 O1C 84.08(16) . . ?
O21A Mn2 O1C 172.38(14) 6_566 . ?
O1B Mn2 Mn1 138.30(13) . 6_566 ?
O1D Mn2 Mn1 42.11(11) 6_566 6_566 ?
O123 Mn2 Mn1 41.23(10) . 6_566 ?
N22B Mn2 Mn1 130.35(13) . 6_566 ?
O21A Mn2 Mn1 80.91(11) 6_566 6_566 ?
O1C Mn2 Mn1 98.36(9) . 6_566 ?
O1B Mn2 Mn1 150.86(13) . . ?
O1D Mn2 Mn1 111.74(11) 6_566 . ?
O123 Mn2 Mn1 33.22(10) . . ?
N22B Mn2 Mn1 60.28(12) . . ?
O21A Mn2 Mn1 83.13(11) 6_566 . ?
O1C Mn2 Mn1 89.48(8) . . ?
Mn1 Mn2 Mn1 70.13(3) 6_566 . ?
O333 Mn3 O1C 171.29(18) . . ?
O333 Mn3 O23C 90.79(12) . 11_665 ?
O1C Mn3 O23C 93.41(15) . 11_665 ?
O333 Mn3 N22C 87.76(13) . . ?
O1C Mn3 N22C 86.72(17) . . ?
O23C Mn3 N22C 169.48(17) 11_665 . ?
O333 Mn3 O1E 93.5(2) . . ?
O1C Mn3 O1E 93.81(17) . . ?
O23C Mn3 O1E 94.46(17) 11_665 . ?
N22C Mn3 O1E 96.03(18) . . ?
O333 Mn3 O123 90.27(19) . . ?
O1C Mn3 O123 83.09(13) . . ?
O23C Mn3 O123 78.63(14) 11_665 . ?
N22C Mn3 O123 90.95(15) . . ?
O1E Mn3 O123 172.20(16) . . ?
Mn3 O333 Mn3 119.06(6) . 6_566 ?
Mn3 O333 Mn3 119.07(6) . 11_665 ?
Mn3 O333 Mn3 119.07(6) 6_566 11_665 ?
O22A C2A O21A 125.6(6) . . ?
O22A C2A C1A 119.1(5) . . ?
O21A C2A C1A 115.3(5) . . ?
C2A C1A H1A1 109.5 . . ?
C2A C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
C2A C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
C2A O22A Mn1 126.9(4) . . ?
C2A O21A Mn2 125.9(4) . 11_665 ?
C1B O1B Mn2 127.1(4) . . ?
O1B C1B C6B 117.4(5) . . ?
O1B C1B C2B 123.7(5) . . ?
C6B C1B C2B 118.9(5) . . ?
C3B C2B C1B 117.2(5) . . ?
C3B C2B C21B 119.5(6) . . ?
C1B C2B C21B 123.1(5) . . ?
C5B C6B C1B 120.0(6) . . ?
C5B C6B H6B 120.0 . . ?
C1B C6B H6B 120.0 . . ?
C4B C5B C6B 121.7(6) . . ?
C4B C5B H5B 119.2 . . ?
C6B C5B H5B 119.2 . . ?
C3B C4B C5B 120.6(6) . . ?
C3B C4B H4B 119.7 . . ?
C5B C4B H4B 119.7 . . ?
C4B C3B C2B 121.6(7) . . ?
C4B C3B H3B 119.2 . . ?
C2B C3B H3B 119.2 . . ?
N22B C21B C24B 119.4(5) . . ?
N22B C21B C2B 119.6(5) . . ?
C24B C21B C2B 121.0(5) . . ?
C21B N22B O23B 116.4(5) . . ?
C21B N22B Mn2 129.5(4) . . ?
O23B N22B Mn2 113.9(3) . . ?
C21B C24B H24A 109.5 . . ?
C21B C24B H24B 109.5 . . ?
H24A C24B H24B 109.5 . . ?
C21B C24B H24C 109.5 . . ?
H24A C24B H24C 109.5 . . ?
H24B C24B H24C 109.5 . . ?
N22B O23B Mn1 120.7(3) . . ?
C1C O1C Mn3 118.6(3) . . ?
C1C O1C Mn2 125.2(3) . . ?
Mn3 O1C Mn2 97.50(14) . . ?
O1C C1C C2C 123.1(5) . . ?
O1C C1C C6C 117.6(5) . . ?
C2C C1C C6C 119.3(5) . . ?
C3C C2C C1C 119.9(5) . . ?
C3C C2C C21C 120.0(5) . . ?
C1C C2C C21C 120.1(5) . . ?
C5C C6C C1C 118.5(6) . . ?
C5C C6C H6C 120.7 . . ?
C1C C6C H6C 120.7 . . ?
C4C C5C C6C 122.0(6) . . ?
C4C C5C H5C 119.0 . . ?
C6C C5C H5C 119.0 . . ?
C3C C4C C5C 118.6(6) . . ?
C3C C4C H4C 120.7 . . ?
C5C C4C H4C 120.7 . . ?
C2C C3C C4C 121.6(6) . . ?
C2C C3C H3C 119.2 . . ?
C4C C3C H3C 119.2 . . ?
N22C C21C C2C 118.8(5) . . ?
N22C C21C C24C 120.0(5) . . ?
C2C C21C C24C 121.2(5) . . ?
C21C C24C H24D 109.5 . . ?
C21C C24C H24E 109.5 . . ?
H24D C24C H24E 109.5 . . ?
C21C C24C H24F 109.5 . . ?
H24D C24C H24F 109.5 . . ?
H24E C24C H24F 109.5 . . ?
C21C N22C O23C 117.8(4) . . ?
C21C N22C Mn3 127.1(4) . . ?
O23C N22C Mn3 113.9(3) . . ?
N22C O23C Mn3 113.0(3) . 6_566 ?
N22C O23C Mn1 102.8(3) . 6_566 ?
Mn3 O23C Mn1 99.24(14) 6_566 6_566 ?
Mn1 O123 Mn2 113.52(16) . . ?
Mn1 O123 Mn1 132.44(18) . 6_566 ?
Mn2 O123 Mn1 97.64(16) . 6_566 ?
Mn1 O123 Mn3 102.67(15) . . ?
Mn2 O123 Mn3 97.92(14) . . ?
Mn1 O123 Mn3 107.73(14) 6_566 . ?
C2D O1D Mn2 122.6(4) . 11_665 ?
C2D O1D Mn1 127.1(3) . . ?
Mn2 O1D Mn1 96.89(15) 11_665 . ?
O1D C2D H2D1 109.5 . . ?
O1D C2D H2D2 109.5 . . ?
H2D1 C2D H2D2 109.5 . . ?
O1D C2D H2D3 109.5 . . ?
H2D1 C2D H2D3 109.5 . . ?
H2D2 C2D H2D3 109.5 . . ?
C2E O1E Mn3 143.8(12) . . ?
C2E O1E H1E1 96.6 . . ?
Mn3 O1E H1E1 109.3 . . ?
C2E O1E H1E2 84.1 . . ?
Mn3 O1E H1E2 109.2 . . ?
H1E1 O1E H1E2 109.5 . . ?
O1E C2E H1E2 34.5 . . ?
O1E C2E H2E1 109.5 . . ?
H1E2 C2E H2E1 95.1 . . ?
O1E C2E H2E2 109.5 . . ?
H1E2 C2E H2E2 143.2 . . ?
H2E1 C2E H2E2 109.5 . . ?
O1E C2E H2E3 109.5 . . ?
H1E2 C2E H2E3 86.3 . . ?
H2E1 C2E H2E3 109.5 . . ?
H2E2 C2E H2E3 109.5 . . ?
O1S O1S O1S 60.000(6) 6_566 11_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.092