# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Euan Brechin'
'George Christou'
'Muralee Murugesu'
'S. Parsons'
'Richard T. W. Scott'
'Wolfgang Wernsdorfer'

_publ_contact_author_name        'Dr Euan Brechin'
_publ_contact_author_address     
;
School of Chemistry
University of Edinburgh
West Mains Raod
Edinburgh
EH9 3JJ
UNITED KINGDOM
;

_publ_contact_author_email       EBRECHIN@STAFFMAIL.ED.AC.UK

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Synthesis, Structure and Magnetic Properties of a
Trinuclear [MnIIIMnII2] Single-Molecule Magnet
;

data_mnekb7
_database_code_depnum_ccdc_archive 'CCDC 263449'

_audit_creation_method           SHELXL-97
_chemical_compound_source        'Euan Brechin. Reaction EKB7'
_exptl_crystal_recrystallization_method 'Et2O diffusion into MeCN solution.'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Mn3(chtH)2(bipy)4](ClO4)3.Et2O.2MeCN'
_chemical_formula_sum            'C60 H68 Cl3 Mn3 N10 O19'
_chemical_formula_weight         1504.41

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'
Cl Cl 0.1484 0.1585 '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           monoclinic
_symmetry_space_group_name_H-M   'I 2/m'
_symmetry_int_tables_number      12
_symmetry_space_group_name_Hall  '-I 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   11.919(2)
_cell_length_b                   22.044(4)
_cell_length_c                   13.385(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.863(4)
_cell_angle_gamma                90.00
_cell_volume                     3491.6(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4869
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1548
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   Multiscan
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_process_details   'Sadabs v 2004/1'

_exptl_special_details           
;
Data collection strategy optimised with COSMO.
Oxford cryosystems LT device.
;

_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 + phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14880
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         27.04
_reflns_number_total             3915
_reflns_number_gt                3429
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'XCIF, ENCIFER, PLATON'

_refine_special_details          
;
The Mn3 complex resides on a 2/m special position.

Ligand 1 is cht3- (cyclohexan-triol); there is 1/2 of this in the
asymmetric unit.

Ligand 2 is a bipy is a general position.

Disorder:
#3: ClO4-
The Cl sits on or close to the 2-fold at 0 y 1/2.
One O (O13) sits near the two fold, the other three O's are
therefore disordered. A model with the Cl and O13 on the 2-fold
gave high Uiso's for the O-atoms, and in the final model the anion was
treated as a rigid, variable-metric tetrahedron, which was allowed to
refine away from the two-fold axis. The group was refined anisotropically;
some of the resulting adps are quite elongated, and there may be further
unmodelled disorder here.

#4 ClO4-
This resides on the 2-fols at 1/2 y 1/2, but as y~0.1, it is also quite
close to the -1 at 1/2 0 1/2. Like ClO4#3 this group was modelled as a
variable-metric rigid tetrahedron. The Cl-O distances in #3 and 4 were
restrained to be similar.
The group is close to MeCN group 'U', and so it can not have a chemical
occupancy of 1. Moreover, refinement of such a model yielded high
displacement parameters [e.g. that for Cl4 was 0.1]. Reducing the
chemical occupancy to 0.5 cured the problem, and also reduced
the R-factor.

Solvent: S, T, U
A region of density in the lattice voids was modelled as a mixture
of Et2O (S) and MeCN (T & U). Restraints were applied to the
distances and angles, and common U[iso]'s were refined for the the
atoms comprising each molecule. There are still a number of
difference peaks in the region of the solvent, and the model presented
should be regarded as approximate.

The disorder in the ClO4- and solvent regions reduce the
precision of the structure determination, and keep the R-factor high.
Squeeze modelling of the whole region reduced R1 to 5.5%. This
latter model is not presented here because the modelling of the
solvent region establishes the charge of the complex.

Checkcif Output:

432_ALERT_2_A Short Inter X...Y Contact N1T .. C1S .. 2.61 Ang.
432_ALERT_2_A Short Inter X...Y Contact O34 .. C3U .. 2.13 Ang.
411_ALERT_2_B Short Inter H...H Contact H21B .. H3U3 .. 1.91 Ang.
430_ALERT_2_B Short Inter D...A Contact O31 .. N1T .. 2.77 Ang.
432_ALERT_2_B Short Inter X...Y Contact O23 .. C112 .. 2.88 Ang.
432_ALERT_2_B Short Inter X...Y Contact C1S .. O44 .. 2.81 Ang.
432_ALERT_2_B Short Inter X...Y Contact C1S .. O44 .. 2.81 Ang.
432_ALERT_2_B Short Inter X...Y Contact O24 .. C3U .. 2.76 Ang.
432_ALERT_2_B Short Inter X...Y Contact O34 .. C2U .. 2.73 Ang.
432_ALERT_2_B Short Inter X...Y Contact O44 .. C3U .. 2.84 Ang.
432_ALERT_2_B Short Inter X...Y Contact O44 .. C2S .. 2.89 Ang.
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C1S
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O3S
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C5S
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . N1T
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C2T
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C3T
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . H12#
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . N1U
301_ALERT_3_C Main Residue Disorder ......................... 6.00 Perc.
302_ALERT_4_C Anion/Solvent Disorder ......................... 36.00 Perc.
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O14
341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9

All the above atoms have partial occupancies. See above notes on disorder.

761_ALERT_1_A CIF Contains no X-H Bonds ...................... ?
762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?

The H-atoms were all placed in calculated positions.

773_ALERT_2_A Suspect C-C Bond in CIF: C2U -C3U .. 1.97 Ang.
773_ALERT_2_A Suspect C-C Bond in CIF: C3U -C3U .. 1.92 Ang.
773_ALERT_2_A Suspect C-C Bond in CIF: C3U -C2U .. 1.97 Ang.

MeCN #U is disordered about a special position; that in the asymmetric unit
has normal bond distances.

242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for Cl4
242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for Cl3

These are central Cl-atoms in disordered perchlorate anions - this feature
is quite normal.

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?

063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.69 mm
084_ALERT_2_C High R2 Value .................................. 0.26

128_ALERT_4_C Non-standard setting of Space group C2/m .... I2/m

The alternative setting has a beta angle of 127.83 deg.

165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 10
241_ALERT_2_C Check High U(eq) as Compared to Neighbors for O31
242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Mn1
243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for N1U
243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for C2U
244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C2T
244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C3T

All except Mn1 here are part weight and disordered. See above. Central metal
atoms frequently have relatively low U's in complexes.

720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 16
742_ALERT_1_C Angle Calc 90.00(1), Rep 90.00 ...... Missing su
O31 -MN1 -MN2 1.555 1.555 1.555
764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.18 Ratio
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.50 Deg.
O24 -CL4 -O34 2.656 1.555 1.555
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 35.90 Deg.
O34 -CL4 -O24 2.656 1.555 1.555
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 10.00 Deg.
O14 -CL4 -O14 1.555 1.555 2.656
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 15.70 Deg.
CL4 -CL4 -O44 2.656 1.555 2.656
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 16.90 Deg.
CL4 -O14 -CL4 1.555 1.555 2.656
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 15.70 Deg.
CL4 -O24 -CL4 2.656 1.555 1.555
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 17.10 Deg.
CL4 -O34 -CL4 2.656 1.555 1.555
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 4.60 Deg.
CL4 -O44 -CL4 1.555 1.555 2.656
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.20 Deg.
C2S -O3S -C4S 1.555 1.555 6.565
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.20 Deg.
C2S -O3S -C4S 6.565 1.555 1.555
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.10 Deg.
C2U -C2U -C3U 6.565 1.555 6.565
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 29.00 Deg.
C2U -C3U -C2U 1.555 1.555 6.565
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.10 Deg.
C3U -C3U -C2U 6.565 1.555 6.565
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
C4 H10 O
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
C2 H3 N
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C22
796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O13

Noted, but no action taken.

911_ALERT_3_C Missing FCF Refl. Between TH(Min) & STH/L=0.6 .. 5
912_ALERT_3_C Missing FCF Reflections Above STH/L=0.6 ........ 18

#===============================================================================
Resolution & Completeness Statistics (Cumulative)
#===============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#-------------------------------------------------------------------------------
20.82 0.500 1.000 1898 1898 0
23.01 0.550 1.000 2515 2514 1
25.24 0.600 0.998 3256 3251 5
#----------------------------------------------------------- ACTA Min. Res. ----
27.51 0.650 0.994 3938 3915 23

Final shelx res file:
#TITL mnekb7 in I2/m solved shelxs
CELL 0.71073 11.9191 22.0443 13.3848 90.000 96.863 90.000
ZERR 2.00 0.0021 0.0037 0.0023 0.000 0.004 0.000
LATT 2
SYMM -X, Y, -Z
SFAC C H N O CL MN
UNIT 120 136 20 38 6 6
TEMP -123
L.S. 4
FMAP 2
PLAN 10

HTAB
ACTA
DFIX 1.52 0.01 C1S C2S C4S C5S
DFIX 1.45 0.01 O3S C2S O3S C4S
DFIX 2.41 0.02 C1S O3S O3S C5S
DFIX 2.36 0.02 C2S C4S
DFIX 1.20 0.01 N1T C2T N1U C2U
DFIX 1.40 0.01 C2T C3T C2U C3U
DFIX 2.60 0.02 N1T C3T N1U C3U

EADP C1S > C5S
EADP N1T > C3T
EADP N1U > C3U

WGHT 0.126100 19.429701
FVAR 0.22432
MN1 6 0.000000 0.000000 0.000000 10.25000 0.02846 0.03379 =
0.05424 0.00000 0.00663 0.00000
MN2 6 0.000000 0.142606 0.000000 10.50000 0.04562 0.03347 =
0.03302 0.00000 -0.00601 0.00000
C11 1 -0.172444 0.057759 0.104400 11.00000 0.03909 0.04042 =
0.07549 0.00183 0.01962 0.00439
AFIX 13
H11 2 -0.224917 0.093312 0.097829 11.00000 -1.20000
AFIX 0
O11 4 -0.094661 0.064178 0.033793 11.00000 0.03724 0.03776 =
0.04561 0.00208 0.00760 0.00225
C21 1 -0.109739 0.057053 0.212500 11.00000 0.07353 0.04717 =
0.05770 -0.00583 0.03548 -0.00191
AFIX 23
H21A 2 -0.060408 0.093218 0.222304 11.00000 -1.20000
H21B 2 -0.165738 0.059385 0.261356 11.00000 -1.20000
AFIX 0
C31 1 -0.038089 0.000000 0.233321 10.50000 0.08863 0.04399 =
0.04296 0.00000 0.02611 0.00000
AFIX 13
H31 2 -0.006235 -0.000001 0.305911 10.50000 -1.20000
AFIX 0
O31 4 0.054325 0.000000 0.173140 10.50000 0.05600 0.07446 =
0.07645 0.00000 0.01231 0.00000
AFIX 3
H31 2 0.101698 -0.036224 0.190724 10.50000 -1.20000
AFIX 0
C61 1 -0.241928 0.000000 0.082620 10.50000 0.03421 0.05846 =
0.11981 0.00000 0.02401 0.00000
AFIX 23
H61A 2 -0.274517 0.000001 0.011030 10.50000 -1.20000
H61B 2 -0.305337 0.000000 0.124121 10.50000 -1.20000
AFIX 0
N12 3 -0.094077 0.207134 0.092657 11.00000 0.04895 0.03663 =
0.03573 0.00334 0.00278 -0.00581
C22 1 -0.195419 0.230689 0.062371 11.00000 0.04620 0.05252 =
0.04130 0.00539 0.00653 -0.00160
AFIX 43
H22 2 -0.238655 0.213308 0.005263 11.00000 -1.20000
AFIX 0
C32 1 -0.241149 0.279070 0.109518 11.00000 0.04936 0.06134 =
0.05426 0.00594 0.01454 0.00186
AFIX 43
H32 2 -0.314363 0.294049 0.086267 11.00000 -1.20000
AFIX 0
C42 1 -0.177104 0.304953 0.191466 11.00000 0.06310 0.06536 =
0.05948 -0.00168 0.02093 0.00296
AFIX 43
H42 2 -0.204612 0.339159 0.224210 11.00000 -1.20000
AFIX 0
C52 1 -0.072169 0.280427 0.225396 11.00000 0.05428 0.05950 =
0.04860 -0.00607 0.01295 -0.00835
AFIX 43
H52 2 -0.026946 0.297323 0.281829 11.00000 -1.20000
AFIX 0
C62 1 -0.034587 0.230461 0.174856 11.00000 0.05184 0.04592 =
0.03126 0.00314 0.00978 -0.00625
C72 1 0.074810 0.201461 0.208964 11.00000 0.05365 0.04577 =
0.03303 0.00328 0.00159 -0.00839
C82 1 0.135280 0.210108 0.303615 11.00000 0.07889 0.06526 =
0.03427 -0.00454 -0.00284 -0.00845
AFIX 43
H82 2 0.106630 0.236334 0.350868 11.00000 -1.20000
AFIX 0
C92 1 0.236241 0.180706 0.328493 11.00000 0.07605 0.07729 =
0.03868 -0.00237 -0.01837 -0.00383
AFIX 43
H92 2 0.277817 0.186437 0.392895 11.00000 -1.20000
AFIX 0
C102 1 0.275933 0.143567 0.260619 11.00000 0.06798 0.05869 =
0.05823 0.00396 -0.01799 0.00499
AFIX 43
H102 2 0.346141 0.123306 0.276527 11.00000 -1.20000
AFIX 0
C112 1 0.213155 0.135233 0.167234 11.00000 0.06079 0.04890 =
0.05421 -0.00552 -0.01726 0.00287
AFIX 43
H112 2 0.241081 0.108667 0.120070 11.00000 -1.20000
AFIX 0
N122 3 0.113714 0.163769 0.141603 11.00000 0.05565 0.04006 =
0.03767 -0.00097 -0.00460 -0.00157
AFIX 9
PART -1
CL3 5 0.009802 0.349689 0.504935 10.50000 0.03345 0.04967 =
0.04378 0.00878 0.00932 -0.00185
O13 4 -0.015222 0.287146 0.513725 10.50000 0.08264 0.05921 =
0.06175 0.00694 -0.00731 -0.03050
O23 4 0.086838 0.357467 0.432975 10.50000 0.05824 0.07159 =
0.05962 -0.00312 0.03120 -0.01199
O33 4 0.058769 0.372148 0.599530 10.50000 0.10603 0.06247 =
0.05346 -0.00251 0.01897 -0.02128
O43 4 -0.091183 0.382004 0.473530 10.50000 0.03778 0.10310 =
0.16802 0.05464 0.01620 0.02753
PART 1 10.25
AFIX 9
CL4 5 0.482877 0.107728 0.496661 10.25000 0.04491
O14 4 0.490717 0.169725 0.494831 10.25000 0.04477
O24 4 0.549335 0.081480 0.576764 10.25000 0.10119
O34 4 0.516563 0.087032 0.407484 10.25000 0.09198
O44 4 0.371147 0.092331 0.500639 10.25000 0.10052
AFIX 0
PART 2
C1S 1 -0.276964 0.500000 -0.075898 10.25000 0.11550
AFIX 3
H1SA 2 -0.211994 0.523660 -0.087078 10.25000 -1.50000
H1SB 2 -0.253044 0.464200 -0.038418 10.25000 -1.50000
H1SC 2 -0.317374 0.488550 -0.139458 10.25000 -1.50000
AFIX 0
C2S 1 -0.348714 0.536322 -0.009695 10.25000 0.11550
AFIX 3
H2SA 2 -0.373044 0.572324 -0.046425 10.25000 -1.20000
H2SB 2 -0.309094 0.548124 0.054015 10.25000 -1.20000
AFIX 0
O3S 4 -0.449236 0.500000 0.001226 10.25000 0.11550
C4S 1 -0.407366 0.437284 0.000516 10.25000 0.11550
AFIX 3
H4SA 2 -0.357796 0.431533 0.061776 10.25000 -1.20000
H4SB 2 -0.364356 0.430854 -0.054784 10.25000 -1.20000
AFIX 0
C5S 1 -0.500000 0.391629 0.000000 10.25000 0.11550
AFIX 3
H5SA 2 -0.468850 0.351429 0.002580 10.25000 -1.50000
H5SB 2 -0.542330 0.397499 0.055910 10.25000 -1.50000
H5SC 2 -0.548950 0.396799 -0.061760 10.25000 -1.50000
AFIX 0

PART 1
N1T 3 -0.216573 0.500000 -0.257237 10.25000 0.06089
C2T 1 -0.121337 0.500000 -0.275491 10.25000 0.06089
C3T 1 -0.011576 0.500000 -0.302131 10.25000 0.06089
AFIX 3
H3T1 2 -0.000113 0.463951 -0.342543 10.25000 -1.50000
H3T2 2 0.042219 0.500000 -0.240747 10.25000 -1.50000
H3T3 2 0.000460 0.536543 -0.341166 10.25000 -1.50000
AFIX 0
PART 2
N1U 3 -0.053453 0.500000 -0.322946 10.25000 0.11871
C2U 1 0.020075 0.522660 -0.265216 10.25000 0.11871
C3U 1 0.109955 0.543549 -0.197560 10.25000 0.11871
AFIX 3
H3U1 2 0.129149 0.513316 -0.144590 10.25000 -1.50000
H3U2 2 0.085501 0.581123 -0.167543 10.25000 -1.50000
H3U3 2 0.176476 0.551762 -0.231941 10.25000 -1.50000
PART 0
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM mnekb7 in I2/m solved shelxs
REM R1 = 0.0953 for 3429 Fo > 4sig(Fo) and 0.1043 for all 3915 data
REM 240 parameters refined using 13 restraints

END

WGHT 0.1261 19.4697
REM Highest difference peak 1.442, deepest hole -0.806, 1-sigma level 0.152
Q1 1 0.5000 0.1397 0.5000 10.50000 0.05 1.44
Q2 1 -0.4200 0.4153 -0.0019 11.00000 0.05 1.32
Q3 1 0.0578 0.0000 0.2536 10.50000 0.05 1.30
Q4 1 -0.2826 0.5000 -0.1710 10.50000 0.05 1.25
Q5 1 0.0000 0.1063 0.0000 10.50000 0.05 1.04
Q6 1 0.5696 0.0562 0.5214 11.00000 0.05 0.78
Q7 1 0.0000 0.1817 0.0000 10.50000 0.05 0.67
Q8 1 0.0000 0.0397 0.0000 10.50000 0.05 0.62
Q9 1 0.2066 0.5448 -0.1003 11.00000 0.05 0.55
Q10 1 -0.4599 0.5304 0.0012 11.00000 0.05 0.54

;

_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^)+(0.1261P)^2^+19.4297P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3915
_refine_ls_number_parameters     240
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0953
_refine_ls_wR_factor_ref         0.2653
_refine_ls_wR_factor_gt          0.2579
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.003
_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 0.0000 0.0000 0.0000 0.0387(4) Uani 1 4 d S . .
Mn2 Mn 0.0000 0.14261(5) 0.0000 0.0382(3) Uani 1 2 d S . .
C11 C -0.1724(4) 0.0578(2) 0.1044(5) 0.0506(13) Uani 1 1 d . . .
H11 H -0.2249 0.0933 0.0978 0.061 Uiso 1 1 calc R . .
O11 O -0.0947(3) 0.06418(15) 0.0338(3) 0.0400(8) Uani 1 1 d . . .
C21 C -0.1097(6) 0.0571(3) 0.2125(5) 0.0572(15) Uani 1 1 d . . .
H21A H -0.0604 0.0932 0.2223 0.069 Uiso 1 1 calc R . .
H21B H -0.1657 0.0594 0.2614 0.069 Uiso 1 1 calc R . .
C31 C -0.0381(9) 0.0000 0.2333(6) 0.057(2) Uani 1 2 d S . .
H31 H -0.0062 0.0000 0.3059 0.068 Uiso 1 2 calc SR . .
O31 O 0.0543(5) 0.0000 0.1731(5) 0.0686(17) Uani 1 2 d S . .
H31' H 0.1017 -0.0362 0.1907 0.082 Uiso 0.50 1 d PR . .
C61 C -0.2419(7) 0.0000 0.0826(10) 0.070(3) Uani 1 2 d S . .
H61A H -0.2745 0.0000 0.0110 0.084 Uiso 1 2 calc SR . .
H61B H -0.3053 0.0000 0.1241 0.084 Uiso 1 2 calc SR . .
N12 N -0.0941(4) 0.20713(19) 0.0927(3) 0.0406(9) Uani 1 1 d . . .
C22 C -0.1954(5) 0.2307(3) 0.0624(4) 0.0466(12) Uani 1 1 d . . .
H22 H -0.2387 0.2133 0.0053 0.056 Uiso 1 1 calc R . .
C32 C -0.2411(5) 0.2791(3) 0.1095(5) 0.0543(14) Uani 1 1 d . . .
H32 H -0.3144 0.2940 0.0863 0.065 Uiso 1 1 calc R . .
C42 C -0.1771(6) 0.3050(3) 0.1915(5) 0.0615(16) Uani 1 1 d . . .
H42 H -0.2046 0.3392 0.2242 0.074 Uiso 1 1 calc R . .
C52 C -0.0722(5) 0.2804(3) 0.2254(5) 0.0536(14) Uani 1 1 d . . .
H52 H -0.0269 0.2973 0.2818 0.064 Uiso 1 1 calc R . .
C62 C -0.0346(5) 0.2305(2) 0.1749(4) 0.0426(11) Uani 1 1 d . . .
C72 C 0.0748(5) 0.2015(2) 0.2090(4) 0.0444(12) Uani 1 1 d . . .
C82 C 0.1353(6) 0.2101(3) 0.3036(4) 0.0602(16) Uani 1 1 d . . .
H82 H 0.1066 0.2363 0.3509 0.072 Uiso 1 1 calc R . .
C92 C 0.2362(6) 0.1807(3) 0.3285(5) 0.0660(18) Uani 1 1 d . . .
H92 H 0.2778 0.1864 0.3929 0.079 Uiso 1 1 calc R . .
C102 C 0.2759(6) 0.1436(3) 0.2606(5) 0.0637(17) Uani 1 1 d . . .
H102 H 0.3461 0.1233 0.2765 0.076 Uiso 1 1 calc R . .
C112 C 0.2132(5) 0.1352(3) 0.1672(5) 0.0566(15) Uani 1 1 d . . .
H112 H 0.2411 0.1087 0.1201 0.068 Uiso 1 1 calc R . .
N122 N 0.1137(4) 0.1638(2) 0.1416(3) 0.0453(10) Uani 1 1 d . . .
Cl3 Cl 0.0098(5) 0.34969(10) 0.5049(5) 0.0419(8) Uani 0.50 1 d PG A -1
O13 O -0.0152(10) 0.2871(2) 0.5137(8) 0.069(4) Uani 0.50 1 d PG A -1
O23 O 0.0868(6) 0.3575(3) 0.4330(5) 0.061(2) Uani 0.50 1 d PG A -1
O33 O 0.0588(9) 0.3721(4) 0.5995(5) 0.073(3) Uani 0.50 1 d PG A -1
O43 O -0.0912(6) 0.3820(4) 0.4735(8) 0.103(5) Uani 0.50 1 d PG A -1
Cl4 Cl 0.4829(5) 0.10773(18) 0.4967(5) 0.0449(11) Uiso 0.25 1 d PG . 1
O14 O 0.4907(15) 0.1697(4) 0.4948(15) 0.045(3) Uiso 0.25 1 d PG . 1
O24 O 0.5493(15) 0.0815(8) 0.5768(12) 0.101(8) Uiso 0.25 1 d PG . 1
O34 O 0.5166(17) 0.0870(8) 0.4075(11) 0.092(7) Uiso 0.25 1 d PG . 1
O44 O 0.3711(10) 0.0923(8) 0.5006(16) 0.101(7) Uiso 0.25 1 d PG . 1
C1S C -0.277(2) 0.5000 -0.076(2) 0.116(4) Uiso 0.50 2 d SPD . 2
H1SA H -0.2120 0.5237 -0.0871 0.173 Uiso 0.25 1 d PR . 2
H1SB H -0.2530 0.4642 -0.0384 0.173 Uiso 0.25 1 d PR . 2
H1SC H -0.3174 0.4886 -0.1395 0.173 Uiso 0.25 1 d PR . 2
C2S C -0.349(2) 0.5363(9) -0.010(3) 0.116(4) Uiso 0.25 1 d PD . 2
H2SA H -0.3730 0.5723 -0.0464 0.139 Uiso 0.25 1 d PR . 2
H2SB H -0.3091 0.5481 0.0540 0.139 Uiso 0.25 1 d PR . 2
O3S O -0.4492(14) 0.5000 0.0012(17) 0.116(4) Uiso 0.50 2 d SPD . 2
C4S C -0.4074(16) 0.4373(4) 0.001(4) 0.116(4) Uiso 0.25 1 d PD . 2
H4SA H -0.3578 0.4315 0.0618 0.139 Uiso 0.25 1 d PR . 2
H4SB H -0.3644 0.4309 -0.0548 0.139 Uiso 0.25 1 d PR . 2
C5S C -0.5000 0.3916(8) 0.0000 0.116(4) Uiso 0.50 2 d SPD . 2
H5SA H -0.4689 0.3514 0.0026 0.173 Uiso 0.25 1 d PR . 2
H5SB H -0.5423 0.3975 0.0559 0.173 Uiso 0.25 1 d PR . 2
H5SC H -0.5490 0.3968 -0.0618 0.173 Uiso 0.25 1 d PR . 2
N1T N -0.2166(11) 0.5000 -0.2572(12) 0.061(2) Uiso 0.50 2 d SPD B 1
C2T C -0.1213(11) 0.5000 -0.2755(14) 0.061(2) Uiso 0.50 2 d SPD B 1
C3T C -0.0116(13) 0.5000 -0.3021(16) 0.061(2) Uiso 0.50 2 d SPD B 1
H3T1 H -0.0001 0.4640 -0.3425 0.091 Uiso 0.25 1 d PR B 1
H3T2 H 0.0422 0.5000 -0.2407 0.091 Uiso 0.50 2 d SPR B 1
H3T3 H 0.0005 0.5365 -0.3412 0.091 Uiso 0.25 1 d PR B 1
N1U N -0.053(3) 0.5000 -0.323(2) 0.119(7) Uiso 0.50 2 d SPD . 2
C2U C 0.020(3) 0.5227(19) -0.265(3) 0.119(7) Uiso 0.25 1 d PD . 2
C3U C 0.110(3) 0.544(2) -0.198(3) 0.119(7) Uiso 0.25 1 d PD . 2
H3U1 H 0.1291 0.5133 -0.1446 0.178 Uiso 0.25 1 d PR . 2
H3U2 H 0.0855 0.5811 -0.1675 0.178 Uiso 0.25 1 d PR . 2
H3U3 H 0.1765 0.5518 -0.2319 0.178 Uiso 0.25 1 d PR . 2

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 0.0285(7) 0.0338(8) 0.0542(9) 0.000 0.0066(6) 0.000
Mn2 0.0456(6) 0.0335(6) 0.0330(5) 0.000 -0.0060(4) 0.000
C11 0.039(3) 0.040(3) 0.075(4) 0.002(3) 0.020(3) 0.004(2)
O11 0.0372(17) 0.0378(18) 0.0456(19) 0.0021(14) 0.0076(14) 0.0023(14)
C21 0.074(4) 0.047(3) 0.058(3) -0.006(3) 0.035(3) -0.002(3)
C31 0.089(6) 0.044(4) 0.043(4) 0.000 0.026(4) 0.000
O31 0.056(4) 0.074(4) 0.076(4) 0.000 0.012(3) 0.000
C61 0.034(4) 0.058(5) 0.120(9) 0.000 0.024(5) 0.000
N12 0.049(2) 0.037(2) 0.036(2) 0.0033(16) 0.0028(17) -0.0058(18)
C22 0.046(3) 0.053(3) 0.041(3) 0.005(2) 0.007(2) -0.002(2)
C32 0.049(3) 0.061(4) 0.054(3) 0.006(3) 0.015(3) 0.002(3)
C42 0.063(4) 0.065(4) 0.059(4) -0.002(3) 0.021(3) 0.003(3)
C52 0.054(3) 0.059(3) 0.049(3) -0.006(3) 0.013(2) -0.008(3)
C62 0.052(3) 0.046(3) 0.031(2) 0.003(2) 0.010(2) -0.006(2)
C72 0.054(3) 0.046(3) 0.033(2) 0.003(2) 0.002(2) -0.008(2)
C82 0.079(4) 0.065(4) 0.034(3) -0.005(3) -0.003(3) -0.008(3)
C92 0.076(4) 0.077(4) 0.039(3) -0.002(3) -0.018(3) -0.004(4)
C102 0.068(4) 0.059(4) 0.058(4) 0.004(3) -0.018(3) 0.005(3)
C112 0.061(3) 0.049(3) 0.054(3) -0.006(3) -0.017(3) 0.003(3)
N122 0.056(3) 0.040(2) 0.038(2) -0.0010(18) -0.0046(19) -0.0016(19)
Cl3 0.0334(19) 0.0497(10) 0.0438(13) 0.009(2) 0.0093(13) -0.0018(17)
O13 0.083(9) 0.059(4) 0.062(8) 0.007(5) -0.007(6) -0.030(6)
O23 0.058(5) 0.072(6) 0.060(5) -0.003(4) 0.031(4) -0.012(4)
O33 0.106(8) 0.062(6) 0.053(5) -0.003(4) 0.019(5) -0.021(6)
O43 0.038(5) 0.103(9) 0.168(14) 0.055(9) 0.016(6) 0.028(5)

_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 O11 1.898(3) 6 ?
Mn1 O11 1.898(3) 2 ?
Mn1 O11 1.898(3) 5 ?
Mn1 O11 1.898(3) . ?
Mn1 O31 2.330(7) . ?
Mn1 O31 2.331(7) 5 ?
Mn1 Mn2 3.1436(11) . ?
Mn1 Mn2 3.1437(11) 5 ?
Mn2 O11 2.142(3) 2 ?
Mn2 O11 2.142(3) . ?
Mn2 N122 2.243(4) . ?
Mn2 N122 2.243(4) 2 ?
Mn2 N12 2.270(4) 2 ?
Mn2 N12 2.270(4) . ?
C11 O11 1.408(6) . ?
C11 C61 1.528(7) . ?
C11 C21 1.547(9) . ?
C21 C31 1.527(8) . ?
C31 O31 1.440(10) . ?
C31 C21 1.527(8) 6 ?
C61 C11 1.528(7) 6 ?
N12 C22 1.333(7) . ?
N12 C62 1.338(6) . ?
C22 C32 1.384(8) . ?
C32 C42 1.382(9) . ?
C42 C52 1.388(9) . ?
C52 C62 1.394(8) . ?
C62 C72 1.475(8) . ?
C72 N122 1.348(7) . ?
C72 C82 1.394(7) . ?
C82 C92 1.372(10) . ?
C92 C102 1.350(10) . ?
C102 C112 1.390(8) . ?
C112 N122 1.349(7) . ?
Cl3 O23 1.418(4) . ?
Cl3 O43 1.418(4) . ?
Cl3 O13 1.418(4) . ?
Cl3 O33 1.419(4) . ?
Cl4 Cl4 0.407(11) 2_656 ?
Cl4 O24 1.165(18) 2_656 ?
Cl4 O34 1.361(18) 2_656 ?
Cl4 O14 1.370(9) . ?
Cl4 O44 1.381(9) . ?
Cl4 O34 1.382(9) . ?
Cl4 O24 1.382(9) . ?
Cl4 O14 1.404(12) 2_656 ?
Cl4 O44 1.769(17) 2_656 ?
O14 O14 0.25(4) 2_656 ?
O14 Cl4 1.404(10) 2_656 ?
O24 O34 0.85(4) 2_656 ?
O24 Cl4 1.165(15) 2_656 ?
O24 O44 1.50(4) 2_656 ?
O34 O24 0.85(4) 2_656 ?
O34 Cl4 1.361(16) 2_656 ?
O34 O44 1.71(4) 2_656 ?
O44 O24 1.50(3) 2_656 ?
O44 O34 1.71(3) 2_656 ?
O44 Cl4 1.769(14) 2_656 ?
C1S C2S 1.529(10) 6_565 ?
C1S C2S 1.529(10) . ?
C2S C4S 0.93(3) 6_565 ?
C2S O3S 1.463(10) . ?
C2S C2S 1.60(4) 6_565 ?
O3S O3S 1.21(3) 5_465 ?
O3S C2S 1.463(10) 6_565 ?
O3S C4S 1.470(10) 6_565 ?
O3S C4S 1.470(10) . ?
C4S C2S 0.93(3) 6_565 ?
C4S C5S 1.493(10) . ?
C5S C4S 1.493(10) 2_455 ?
N1T C2T 1.189(9) . ?
C2T C3T 1.396(9) . ?
N1U C2U 1.205(9) 6_565 ?
N1U C2U 1.205(9) . ?
C2U C2U 1.00(8) 6_565 ?
C2U C3U 1.396(9) . ?
C2U C3U 1.97(5) 6_565 ?
C3U C3U 1.92(10) 6_565 ?
C3U C2U 1.97(5) 6_565 ?

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
O11 Mn1 O11 180.0 6 2 ?
O11 Mn1 O11 83.6(2) 6 5 ?
O11 Mn1 O11 96.4(2) 2 5 ?
O11 Mn1 O11 96.4(2) 6 . ?
O11 Mn1 O11 83.6(2) 2 . ?
O11 Mn1 O11 180.0 5 . ?
O11 Mn1 O31 82.27(15) 6 . ?
O11 Mn1 O31 97.73(15) 2 . ?
O11 Mn1 O31 97.73(15) 5 . ?
O11 Mn1 O31 82.27(15) . . ?
O11 Mn1 O31 97.73(15) 6 5 ?
O11 Mn1 O31 82.27(15) 2 5 ?
O11 Mn1 O31 82.27(15) 5 5 ?
O11 Mn1 O31 97.73(15) . 5 ?
O31 Mn1 O31 180.0 . 5 ?
O11 Mn1 Mn2 138.21(10) 6 . ?
O11 Mn1 Mn2 41.79(10) 2 . ?
O11 Mn1 Mn2 138.21(10) 5 . ?
O11 Mn1 Mn2 41.80(10) . . ?
O31 Mn1 Mn2 90.0 . . ?
O31 Mn1 Mn2 90.0 5 . ?
O11 Mn1 Mn2 41.79(10) 6 5 ?
O11 Mn1 Mn2 138.21(10) 2 5 ?
O11 Mn1 Mn2 41.79(10) 5 5 ?
O11 Mn1 Mn2 138.21(10) . 5 ?
O31 Mn1 Mn2 90.0 . 5 ?
O31 Mn1 Mn2 90.0 5 5 ?
Mn2 Mn1 Mn2 180.0 . 5 ?
O11 Mn2 O11 72.37(18) 2 . ?
O11 Mn2 N122 93.78(15) 2 . ?
O11 Mn2 N122 105.65(15) . . ?
O11 Mn2 N122 105.65(15) 2 2 ?
O11 Mn2 N122 93.78(15) . 2 ?
N122 Mn2 N122 156.0(2) . 2 ?
O11 Mn2 N12 94.78(14) 2 2 ?
O11 Mn2 N12 158.17(14) . 2 ?
N122 Mn2 N12 92.48(16) . 2 ?
N122 Mn2 N12 72.30(16) 2 2 ?
O11 Mn2 N12 158.17(14) 2 . ?
O11 Mn2 N12 94.78(14) . . ?
N122 Mn2 N12 72.31(16) . . ?
N122 Mn2 N12 92.48(16) 2 . ?
N12 Mn2 N12 102.4(2) 2 . ?
O11 Mn2 Mn1 36.19(9) 2 . ?
O11 Mn2 Mn1 36.19(9) . . ?
N122 Mn2 Mn1 102.00(12) . . ?
N122 Mn2 Mn1 102.00(12) 2 . ?
N12 Mn2 Mn1 128.81(10) 2 . ?
N12 Mn2 Mn1 128.81(10) . . ?
O11 C11 C61 109.9(6) . . ?
O11 C11 C21 110.2(4) . . ?
C61 C11 C21 111.1(6) . . ?
C11 O11 Mn1 122.9(3) . . ?
C11 O11 Mn2 128.9(3) . . ?
Mn1 O11 Mn2 102.02(15) . . ?
C31 C21 C11 112.1(5) . . ?
O31 C31 C21 110.3(4) . 6 ?
O31 C31 C21 110.3(4) . . ?
C21 C31 C21 110.9(8) 6 . ?
C31 O31 Mn1 114.6(5) . . ?
C11 C61 C11 112.9(7) . 6 ?
C22 N12 C62 118.2(5) . . ?
C22 N12 Mn2 124.5(4) . . ?
C62 N12 Mn2 116.2(4) . . ?
N12 C22 C32 123.6(5) . . ?
C42 C32 C22 118.0(6) . . ?
C32 C42 C52 119.3(6) . . ?
C42 C52 C62 118.6(6) . . ?
N12 C62 C52 122.2(5) . . ?
N12 C62 C72 116.7(5) . . ?
C52 C62 C72 121.0(5) . . ?
N122 C72 C82 120.7(5) . . ?
N122 C72 C62 115.0(4) . . ?
C82 C72 C62 124.3(5) . . ?
C92 C82 C72 119.9(6) . . ?
C102 C92 C82 119.4(5) . . ?
C92 C102 C112 119.4(6) . . ?
N122 C112 C102 121.9(6) . . ?
C72 N122 C112 118.6(5) . . ?
C72 N122 Mn2 118.1(4) . . ?
C112 N122 Mn2 122.8(4) . . ?
O23 Cl3 O43 109.5 . . ?
O23 Cl3 O13 109.5 . . ?
O43 Cl3 O13 109.5 . . ?
O23 Cl3 O33 109.5 . . ?
O43 Cl3 O33 109.5 . . ?
O13 Cl3 O33 109.5 . . ?
Cl4 Cl4 O24 114(2) 2_656 2_656 ?
Cl4 Cl4 O34 84(2) 2_656 2_656 ?
O24 Cl4 O34 126.3(7) 2_656 2_656 ?
Cl4 Cl4 O14 86.3(7) 2_656 . ?
O24 Cl4 O14 119.8(6) 2_656 . ?
O34 Cl4 O14 111.0(4) 2_656 . ?
Cl4 Cl4 O44 159.6(15) 2_656 . ?
O24 Cl4 O44 71.9(17) 2_656 . ?
O34 Cl4 O44 77.1(17) 2_656 . ?
O14 Cl4 O44 108.3 . . ?
Cl4 Cl4 O34 79(2) 2_656 . ?
O24 Cl4 O34 37.6(17) 2_656 . ?
O34 Cl4 O34 137.3(8) 2_656 . ?
O14 Cl4 O34 106.6 . . ?
O44 Cl4 O34 109.5 . . ?
Cl4 Cl4 O24 50.4(17) 2_656 . ?
O24 Cl4 O24 123.2(8) 2_656 . ?
O34 Cl4 O24 35.9(17) 2_656 . ?
O14 Cl4 O24 113.4 . . ?
O44 Cl4 O24 109.5 . . ?
O34 Cl4 O24 109.5 . . ?
Cl4 Cl4 O14 76.9(8) 2_656 2_656 ?
O24 Cl4 O14 126.9(15) 2_656 2_656 ?
O34 Cl4 O14 105.9(16) 2_656 2_656 ?
O14 Cl4 O14 10.1(15) . 2_656 ?
O44 Cl4 O14 116.3(15) . 2_656 ?
O34 Cl4 O14 107.8(17) . 2_656 ?
O24 Cl4 O14 104.0(16) . 2_656 ?
Cl4 Cl4 O44 15.8(13) 2_656 2_656 ?
O24 Cl4 O44 98.4(10) 2_656 2_656 ?
O34 Cl4 O44 91.3(8) 2_656 2_656 ?
O14 Cl4 O44 97.05(17) . 2_656 ?
O44 Cl4 O44 154.5(3) . 2_656 ?
O34 Cl4 O44 64.4(17) . 2_656 ?
O24 Cl4 O44 55.4(16) . 2_656 ?
O14 Cl4 O44 88.5(14) 2_656 2_656 ?
O14 O14 Cl4 92.8(5) 2_656 . ?
O14 O14 Cl4 77.1(7) 2_656 2_656 ?
Cl4 O14 Cl4 16.8(4) . 2_656 ?
O34 O24 Cl4 85.2(17) 2_656 2_656 ?
O34 O24 Cl4 70.7(16) 2_656 . ?
Cl4 O24 Cl4 15.6(6) 2_656 . ?
O34 O24 O44 146(2) 2_656 2_656 ?
Cl4 O24 O44 60.8(15) 2_656 2_656 ?
Cl4 O24 O44 75.5(14) . 2_656 ?
O24 O34 Cl4 73.4(16) 2_656 2_656 ?
O24 O34 Cl4 57.2(15) 2_656 . ?
Cl4 O34 Cl4 17.1(5) 2_656 . ?
O24 O34 O44 120(3) 2_656 2_656 ?
Cl4 O34 O44 52.0(13) 2_656 2_656 ?
Cl4 O34 O44 68.9(13) . 2_656 ?
Cl4 O44 O24 47.4(9) . 2_656 ?
Cl4 O44 O34 50.9(10) . 2_656 ?
O24 O44 O34 88.9(13) 2_656 2_656 ?
Cl4 O44 Cl4 4.6(3) . 2_656 ?
O24 O44 Cl4 49.1(8) 2_656 2_656 ?
O34 O44 Cl4 46.8(9) 2_656 2_656 ?
C2S C1S C2S 63.1(17) 6_565 . ?
C4S C2S O3S 71.9(11) 6_565 . ?
C4S C2S C1S 153(6) 6_565 . ?
O3S C2S C1S 107.0(12) . . ?
C4S C2S C2S 128.6(11) 6_565 6_565 ?
O3S C2S C2S 56.8(9) . 6_565 ?
C1S C2S C2S 58.4(8) . 6_565 ?
O3S O3S C2S 145.9(14) 5_465 . ?
O3S O3S C2S 145.9(14) 5_465 6_565 ?
C2S O3S C2S 66.4(18) . 6_565 ?
O3S O3S C4S 109.9(7) 5_465 6_565 ?
C2S O3S C4S 37.1(13) . 6_565 ?
C2S O3S C4S 103.4(11) 6_565 6_565 ?
O3S O3S C4S 109.9(7) 5_465 . ?
C2S O3S C4S 103.4(11) . . ?
C2S O3S C4S 37.1(13) 6_565 . ?
C4S O3S C4S 140.2(15) 6_565 . ?
C2S C4S O3S 71.0(10) 6_565 . ?
C2S C4S C5S 171(6) 6_565 . ?
O3S C4S C5S 112.5(14) . . ?
C4S C5S C4S 95.3(18) . 2_455 ?
N1T C2T C3T 177(2) . . ?
C2U N1U C2U 49(4) 6_565 . ?
C2U C2U N1U 66(2) 6_565 . ?
C2U C2U C3U 109(3) 6_565 . ?
N1U C2U C3U 175(5) . . ?
C2U C2U C3U 42.1(14) 6_565 6_565 ?
N1U C2U C3U 108(3) . 6_565 ?
C3U C2U C3U 67(4) . 6_565 ?
C2U C3U C3U 71(3) . 6_565 ?
C2U C3U C2U 29(2) . 6_565 ?
C3U C3U C2U 42.1(14) 6_565 6_565 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.04
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.152