# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#                                CCDC 
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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
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#  as required by the journal to which it was submitted. 
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data_Mn12XN2K
_database_code_depnum_ccdc_archive 'CCDC 916380'
#TrackingRef 'mn12_xn_2K.cif'
_audit_creation_date             12-11-07
_audit_creation_method           SHELXL-97
_oxford_structure_analysis_title 'Mn12 in I-4'
_exptl_crystal_recrystallisation_method 
;
KMnO4 + Mn(OAc)2.4H2O in AcOH
Crystals formed in sealed vessel at RT.
;
_refine_special_details          
;
The non-H atom structure was solved and refined from X-ray data. H atoms in
methyl groups were placed in calculated positions. This structural model
was allowed to refine against the neutron data. H atoms attached to coordinated
and lattice water molecules, as well as the acidic H atom belonging to the
acetic acid, were found in a difference map calculated from the neutron data.
The model was again refined against the X-ray data with H atoms restrained.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Checkcif output (with comments):
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.909
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 74
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 140
915_ALERT_3_C Low Friedel Pair Coverage ...................... 83 Perc.
The X-ray data to which these alerts refer were measured on the XIPHOS
ultra-low temperature X-ray diffractometer. There are constraints on the
reflections that can be observed due to the geometry of the instrument
and the shroud that encases the crystal in order that ultra-low temperature
can be achieved.
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 .......... ?
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action.
042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
We choose to report the moietyformula string in this way as it is more
chemically meaningful.
125_ALERT_4_C No '_symmetry_space_group_name_Hall' Given ..... ?
No action.
220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.4 Ratio
220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.1 Ratio
241_ALERT_2_C Check High Ueq as Compared to Neighbors for O10
244_ALERT_4_G Low 'Solvent' Ueq as Compared to Neighbors of C9
No action. We are quite sure of the identity of the atoms in question.
975_ALERT_2_C Positive Residual Density at 0.90A from O12 . 0.78 eA-3
976_ALERT_2_C Negative Residual Density at 0.58A from O13 . -0.46 eA-3
976_ALERT_2_C Negative Residual Density at 0.62A from O13 . -0.42 eA-3
H atoms were located from a Fourier difference map calculated from neutron data.
Neutron data are particularly sensitive to H atoms and we are confident that the
correct positions have been obtained in this manner rather than those suggested
by the X-ray dataset.
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 24
007_ALERT_5_G Note: Number of Unrefined D-H Atoms ............ 6
Distance and angle restraints are applied to fix H atom positions according
to the neutron dataset.
005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ?
No action.
033_ALERT_4_G Flack x Parameter Value Deviates from Zero ..... 0.546
Flack 0.546(19)
A Flack parameter of approximately 0.5 indicates a racemic twin.
063_ALERT_4_G Crystal Size Likely too Large for Beam Size .... 1.00 mm
083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 8.61
No action.
152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ... 2 Units
Volume Reported 3595.64(8) Calculated 3595.64(10)
One is calculated by Shelxl, the other by Platon. It is possible
that one program takes the correlation of the errors in the a and b
axes into account, while the other doesn't. In fact neither is correct
because neither program has access to the full correlation matrix
used in cell refinement. The volume calculated by SAINT, which
does take these correlations into account, is 3595.67(13) Ang**3.
301_ALERT_3_G Note: Main Residue Disorder ................... 17 Perc.
302_ALERT_4_G Note: Anion/Solvent Disorder ................... 67 Perc.
Yes, this is described in detail in the accompanying article.
811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms .... !
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 92
952_ALERT_5_G Reported and Calculated Lmax Values Differ by .. 2
No action.
;
_chemical_formula_moiety         '[Mn12O12(O2CCH3)16(H2O)4].2CH3CH2OH.4H2O'
_chemical_compound_source        AF18
_chemical_formula_sum            'C36 H72 Mn12 O56'
_chemical_formula_weight         2060.22
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'
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           Tetragonal
_symmetry_space_group_name_H-M   I-4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
_cell_length_a                   17.1875(2)
_cell_length_b                   17.1875(2)
_cell_length_c                   12.1717(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3595.64(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    2(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2072
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3771
_exptl_absorpt_correction_T_max  0.4512
_exptl_absorpt_process_details   
;
SADABS 2008/1 was used for absorption correction.
;
_exptl_special_details           
;
Two experiments were performed in order to obtain the data presented here:
a 2 K X-ray study and a 2 K neutron study. Due to the different characteristics
of each experiment it was necessary to use two different crystals.
A black crystal (size 0.1 x 0.1 x 1.0 mm) was mounted on a graphite rod and
placed inside the cryostat of the XIPHOS diffractometer at Durham University
and cooled to 2 K. The system has a minimum operating temperature of 1.9 K,
achieved using a modified two-stage closed-cycle refrigerator enhanced with
an additional Joule-Thompson stage. Data were integrated using SAINT and
empirical absorption corrections using equivalent reflections were performed
with the program SADABS. Neutron data were collected using the Very-Intense
Vertical-Axis Laue Diffractometer at Institut Laue-Langevin, Grenoble. The
instrument has a minimum operating temperature of 1.5 K, achieved using a
standard ILL orange cryostat. A black crystal (size 0.2 x 0.2 x 1.0 mm)
was mounted on a vanadium rod perpendicular to the incident beam. The sample
used for the neutron study was isotopically normal. Data were integrated using
ARGONNE BOXES and normalised using LAUENORM; both are ILL in-house packages.
The information fields provided in this CIF primarily relate to the X-ray
determination since the main refinement was performed using these data, while
the neutron were used only for obtaining hydrogen atom positions.
;
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker APEXII area detector'
_diffrn_measurement_device       'XIPHOS four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_measurement_specimen_support '0.5mm graphite fibre'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'Bruker TXS with Helios Optics'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_ambient_temperature      2(2)
_diffrn_reflns_number            24483
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         30.70
_reflns_number_total             4861
_reflns_number_gt                4586
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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^)+(0.0480P)^2^+8.6125P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   other
_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   0.546(19)
_refine_ls_number_reflns         4861
_refine_ls_number_parameters     231
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.005
_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 0.08349(2) -0.01726(2) -0.07862(5) 0.01043(10) Uani 1 1 d . . .
Mn2 Mn 0.24179(2) -0.04679(2) -0.07988(5) 0.01353(11) Uani 1 1 d . . .
Mn3 Mn 0.19825(2) 0.14083(2) -0.01408(5) 0.01432(12) Uani 1 1 d . . .
O1 O 0.07043(11) -0.01443(11) 0.0764(2) 0.0114(4) Uani 1 1 d . . .
O2 O 0.10469(11) 0.14815(11) 0.0667(2) 0.0132(5) Uani 1 1 d . A .
O3 O 0.17494(11) 0.03985(11) -0.0669(2) 0.0122(4) Uani 1 1 d . A .
O4 O 0.08602(11) -0.01936(11) -0.2360(2) 0.0140(5) Uani 1 1 d D . .
O5 O 0.21296(12) -0.04562(12) -0.2580(2) 0.0169(5) Uani 1 1 d D A .
C1 C 0.14585(17) -0.03497(16) -0.2947(3) 0.0158(7) Uani 1 1 d D A .
C2 C 0.1304(2) -0.04269(19) -0.4153(3) 0.0244(8) Uani 1 1 d D . .
H2A H 0.1780 -0.0305 -0.4563 0.037 Uiso 1 1 calc R A .
H2B H 0.0891 -0.0065 -0.4367 0.037 Uiso 1 1 calc R . .
H2C H 0.1142 -0.0961 -0.4317 0.037 Uiso 1 1 calc R . .
O61 O 0.2770(3) -0.0646(3) 0.0857(5) 0.0186(7) Uiso 0.50 1 d PD A 1
O71 O 0.2010(3) -0.1581(3) 0.1558(5) 0.0197(8) Uiso 0.50 1 d PD A 1
C31 C 0.2439(4) -0.0987(4) 0.1651(6) 0.0246(11) Uiso 0.50 1 d PD A 1
C41 C 0.2640(7) -0.0712(6) 0.2789(7) 0.054(3) Uiso 0.50 1 d PD A 1
H41A H 0.2239 -0.0349 0.3047 0.081 Uiso 0.50 1 calc PR A 1
H41B H 0.3145 -0.0447 0.2776 0.081 Uiso 0.50 1 calc PR A 1
H41C H 0.2666 -0.1159 0.3287 0.081 Uiso 0.50 1 calc PR A 1
O62 O 0.2568(3) -0.0438(3) 0.1035(4) 0.0186(7) Uiso 0.50 1 d PD A 2
O72 O 0.1872(3) -0.1439(3) 0.1597(5) 0.0197(8) Uiso 0.50 1 d PD A 2
C32 C 0.2293(4) -0.0876(4) 0.1769(6) 0.0246(11) Uiso 0.50 1 d PD A 2
C42 C 0.2307(7) -0.0597(6) 0.2937(7) 0.052(3) Uiso 0.50 1 d PD A 2
H42A H 0.1855 -0.0262 0.3072 0.078 Uiso 0.50 1 calc PR A 2
H42B H 0.2786 -0.0300 0.3067 0.078 Uiso 0.50 1 calc PR A 2
H42C H 0.2290 -0.1044 0.3435 0.078 Uiso 0.50 1 calc PR A 2
O8 O 0.33465(12) 0.01528(12) -0.1013(2) 0.0189(6) Uani 1 1 d D A .
O9 O 0.29829(13) 0.14006(13) -0.0926(3) 0.0277(7) Uani 1 1 d D A .
C5 C 0.34690(16) 0.08703(16) -0.1106(3) 0.0170(7) Uani 1 1 d D . .
C6 C 0.42677(17) 0.11049(18) -0.1481(4) 0.0225(8) Uani 1 1 d D A .
H6A H 0.4587 0.0639 -0.1591 0.034 Uiso 0.50 1 calc PR . .
H6B H 0.4510 0.1437 -0.0923 0.034 Uiso 0.50 1 calc PR . .
H6C H 0.4228 0.1392 -0.2174 0.034 Uiso 0.50 1 calc PR . .
H6D H 0.4296 0.1673 -0.1534 0.034 Uiso 0.50 1 calc PR . .
H6E H 0.4373 0.0875 -0.2203 0.034 Uiso 0.50 1 calc PR . .
H6F H 0.4655 0.0920 -0.0951 0.034 Uiso 0.50 1 calc PR . .
O10 O 0.30849(14) -0.13511(13) -0.1104(3) 0.0326(8) Uani 1 1 d D A .
O11 O 0.24511(14) -0.23394(13) -0.0330(3) 0.0293(7) Uani 1 1 d D A .
C7 C 0.30174(15) -0.20534(15) -0.0831(3) 0.0160(7) Uani 1 1 d D . .
C8 C 0.36842(17) -0.25784(17) -0.1112(3) 0.0182(7) Uani 1 1 d D A .
H8A H 0.3767 -0.2950 -0.0512 0.027 Uiso 1 1 calc R . .
H8B H 0.4156 -0.2267 -0.1218 0.027 Uiso 1 1 calc R . .
H8C H 0.3566 -0.2862 -0.1790 0.027 Uiso 1 1 calc R . .
O12 O 0.26265(18) 0.10254(17) 0.1283(3) 0.0357(8) Uani 1 1 d . A .
H12A H 0.3038 0.0774 0.1438 0.054 Uiso 0.50 1 d PR B 1
H12B H 0.2617 0.0533 0.1343 0.054 Uiso 0.50 1 d PR B 2
H12C H 0.2459 0.1261 0.1850 0.054 Uiso 1 1 d R . .
O13 O 0.21514(17) 0.18769(18) 0.3057(3) 0.0383(8) Uani 1 1 d . . .
H13A H 0.2440 0.2188 0.3415 0.057 Uiso 1 1 d R . .
H13B H 0.1703 0.2086 0.3039 0.057 Uiso 1 1 d R . .
O14 O 0.4155(6) 0.0761(5) 0.1269(10) 0.079(3) Uiso 0.50 1 d PD C -1
O15 O 0.4379(6) -0.0502(5) 0.0897(11) 0.076(3) Uiso 0.50 1 d PD C -1
H15 H 0.3908 -0.0645 0.0949 0.115 Uiso 0.50 1 d PR C -1
C9 C 0.4591(6) 0.0187(5) 0.1090(14) 0.069(4) Uiso 0.50 1 d PD C -1
C10 C 0.5453(7) 0.0304(11) 0.124(2) 0.112(8) Uiso 0.50 1 d PD C -1
H10A H 0.5597 0.0826 0.0986 0.169 Uiso 0.50 1 calc PR C -1
H10B H 0.5737 -0.0086 0.0811 0.169 Uiso 0.50 1 calc PR C -1
H10C H 0.5586 0.0250 0.2019 0.169 Uiso 0.50 1 calc PR C -1
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 0.00957(17) 0.01019(17) 0.0116(3) 0.00020(16) 0.00041(16) 0.00031(13)
Mn2 0.00972(17) 0.01068(18) 0.0202(3) 0.00276(18) 0.00207(18) 0.00065(13)
Mn3 0.01023(18) 0.01116(18) 0.0216(3) -0.00318(18) 0.00293(17) -0.00040(14)
O1 0.0099(8) 0.0140(8) 0.0103(13) 0.0013(9) 0.0009(8) -0.0005(6)
O2 0.0116(8) 0.0113(8) 0.0167(15) -0.0003(9) 0.0029(9) -0.0002(7)
O3 0.0112(8) 0.0115(8) 0.0138(14) -0.0019(8) 0.0008(8) -0.0007(7)
O4 0.0149(9) 0.0143(9) 0.0128(15) -0.0008(8) -0.0003(8) -0.0001(7)
O5 0.0152(9) 0.0146(9) 0.0209(17) 0.0007(9) 0.0053(9) 0.0000(7)
C1 0.0218(13) 0.0109(11) 0.015(2) -0.0010(11) 0.0037(12) -0.0009(10)
C2 0.0282(16) 0.0227(14) 0.022(2) -0.0017(15) 0.0084(15) -0.0041(12)
O8 0.0128(9) 0.0124(9) 0.0316(19) 0.0048(9) 0.0020(9) -0.0005(7)
O9 0.0175(10) 0.0165(10) 0.049(2) -0.0046(11) 0.0117(11) -0.0026(8)
C5 0.0133(12) 0.0148(12) 0.023(2) 0.0014(12) 0.0037(12) -0.0014(10)
C6 0.0134(12) 0.0179(13) 0.036(3) 0.0066(14) 0.0067(13) 0.0017(10)
O10 0.0172(10) 0.0168(10) 0.064(3) 0.0123(12) 0.0161(12) 0.0057(8)
O11 0.0204(10) 0.0161(10) 0.052(2) 0.0082(11) 0.0162(12) 0.0056(8)
C7 0.0124(11) 0.0140(11) 0.022(2) -0.0015(12) 0.0005(13) 0.0018(9)
C8 0.0167(13) 0.0155(12) 0.023(2) -0.0013(12) 0.0029(12) 0.0064(10)
O12 0.0423(16) 0.0302(13) 0.035(2) -0.0122(13) -0.0173(14) 0.0166(12)
O13 0.0268(13) 0.0412(16) 0.047(2) -0.0110(15) -0.0066(13) -0.0011(11)
_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 O3 1.8585(19) . ?
Mn1 O2 1.875(2) 3 ?
Mn1 O1 1.901(3) . ?
Mn1 O1 1.9153(19) 3 ?
Mn1 O4 1.917(3) . ?
Mn1 O1 1.9186(19) 4 ?
Mn1 Mn2 2.7677(6) . ?
Mn1 Mn1 2.8209(9) 4 ?
Mn1 Mn1 2.8209(9) 3 ?
Mn1 Mn1 2.9307(8) 2 ?
Mn2 O3 1.8875(19) . ?
Mn2 O2 1.899(2) 3 ?
Mn2 O8 1.937(2) . ?
Mn2 O10 1.938(2) . ?
Mn2 O61 2.127(6) . ?
Mn2 O5 2.224(3) . ?
Mn2 O62 2.247(5) . ?
Mn3 O2 1.889(2) . ?
Mn3 O3 1.894(2) . ?
Mn3 O9 1.967(2) . ?
Mn3 O11 1.979(2) 4 ?
Mn3 O71 2.126(6) 4 ?
Mn3 O72 2.156(6) 4 ?
Mn3 O12 2.159(3) . ?
O1 Mn1 1.9153(19) 4 ?
O1 Mn1 1.9186(19) 3 ?
O2 Mn1 1.875(2) 4 ?
O2 Mn2 1.899(2) 4 ?
O4 C1 1.280(4) . ?
O5 C1 1.250(4) . ?
C1 C2 1.497(5) . ?
O61 C31 1.264(6) . ?
O71 C31 1.266(6) . ?
O71 Mn3 2.126(6) 3 ?
C31 C41 1.504(7) . ?
O62 C32 1.261(6) . ?
O72 C32 1.225(6) . ?
O72 Mn3 2.156(6) 3 ?
C32 C42 1.502(7) . ?
O8 C5 1.256(3) . ?
O9 C5 1.256(3) . ?
C5 C6 1.502(4) . ?
O10 C7 1.258(3) . ?
O11 C7 1.249(4) . ?
O11 Mn3 1.979(2) 3 ?
C7 C8 1.498(3) . ?
O14 C9 1.258(7) . ?
O15 C9 1.260(7) . ?
C9 C10 1.506(8) . ?
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
O3 Mn1 O2 85.18(9) . 3 ?
O3 Mn1 O1 90.59(10) . . ?
O2 Mn1 O1 90.77(10) 3 . ?
O3 Mn1 O1 173.74(11) . 3 ?
O2 Mn1 O1 97.90(8) 3 3 ?
O1 Mn1 O1 83.95(11) . 3 ?
O3 Mn1 O4 93.87(10) . . ?
O2 Mn1 O4 92.82(10) 3 . ?
O1 Mn1 O4 174.50(9) . . ?
O1 Mn1 O4 91.43(10) 3 . ?
O3 Mn1 O1 96.15(8) . 4 ?
O2 Mn1 O1 174.47(12) 3 4 ?
O1 Mn1 O1 83.86(11) . 4 ?
O1 Mn1 O1 80.27(9) 3 4 ?
O4 Mn1 O1 92.45(10) . 4 ?
O3 Mn1 Mn2 42.77(6) . . ?
O2 Mn1 Mn2 43.17(6) 3 . ?
O1 Mn1 Mn2 97.26(6) . . ?
O1 Mn1 Mn2 140.94(6) 3 . ?
O4 Mn1 Mn2 88.21(6) . . ?
O1 Mn1 Mn2 138.79(6) 4 . ?
O3 Mn1 Mn1 87.99(7) . 4 ?
O2 Mn1 Mn1 132.73(9) 3 4 ?
O1 Mn1 Mn1 42.54(6) . 4 ?
O1 Mn1 Mn1 85.92(7) 3 4 ?
O4 Mn1 Mn1 134.34(6) . 4 ?
O1 Mn1 Mn1 42.16(8) 4 4 ?
Mn2 Mn1 Mn1 120.86(3) . 4 ?
O3 Mn1 Mn1 132.86(9) . 3 ?
O2 Mn1 Mn1 89.30(7) 3 3 ?
O1 Mn1 Mn1 42.64(6) . 3 ?
O1 Mn1 Mn1 42.15(8) 3 3 ?
O4 Mn1 Mn1 133.20(7) . 3 ?
O1 Mn1 Mn1 85.86(7) 4 3 ?
Mn2 Mn1 Mn1 122.23(3) . 3 ?
Mn1 Mn1 Mn1 62.59(2) 4 3 ?
O3 Mn1 Mn1 136.15(6) . 2 ?
O2 Mn1 Mn1 137.98(6) 3 2 ?
O1 Mn1 Mn1 83.06(6) . 2 ?
O1 Mn1 Mn1 40.19(6) 3 2 ?
O4 Mn1 Mn1 91.49(6) . 2 ?
O1 Mn1 Mn1 40.10(6) 4 2 ?
Mn2 Mn1 Mn1 178.84(3) . 2 ?
Mn1 Mn1 Mn1 58.704(11) 4 2 ?
Mn1 Mn1 Mn1 58.703(11) 3 2 ?
O3 Mn2 O2 83.71(9) . 3 ?
O3 Mn2 O8 94.49(9) . . ?
O2 Mn2 O8 176.50(11) 3 . ?
O3 Mn2 O10 173.71(14) . . ?
O2 Mn2 O10 96.15(9) 3 . ?
O8 Mn2 O10 85.31(10) . . ?
O3 Mn2 O61 101.98(16) . . ?
O2 Mn2 O61 94.89(14) 3 . ?
O8 Mn2 O61 88.42(14) . . ?
O10 Mn2 O61 84.31(17) . . ?
O3 Mn2 O5 86.49(9) . . ?
O2 Mn2 O5 84.18(10) 3 . ?
O8 Mn2 O5 92.72(10) . . ?
O10 Mn2 O5 87.24(12) . . ?
O61 Mn2 O5 171.35(15) . . ?
O3 Mn2 O62 88.22(15) . . ?
O2 Mn2 O62 91.44(14) 3 . ?
O8 Mn2 O62 91.50(15) . . ?
O10 Mn2 O62 98.07(17) . . ?
O61 Mn2 O62 13.90(15) . . ?
O5 Mn2 O62 173.47(14) . . ?
O3 Mn2 Mn1 41.97(6) . . ?
O2 Mn2 Mn1 42.48(6) 3 . ?
O8 Mn2 Mn1 135.20(6) . . ?
O10 Mn2 Mn1 136.56(8) . . ?
O61 Mn2 Mn1 107.50(13) . . ?
O5 Mn2 Mn1 77.57(6) . . ?
O62 Mn2 Mn1 95.93(13) . . ?
O2 Mn3 O3 93.30(9) . . ?
O2 Mn3 O9 175.82(10) . . ?
O3 Mn3 O9 90.80(9) . . ?
O2 Mn3 O11 93.03(10) . 4 ?
O3 Mn3 O11 173.65(10) . 4 ?
O9 Mn3 O11 82.87(10) . 4 ?
O2 Mn3 O71 96.51(16) . 4 ?
O3 Mn3 O71 95.81(17) . 4 ?
O9 Mn3 O71 83.87(17) . 4 ?
O11 Mn3 O71 84.01(18) 4 4 ?
O2 Mn3 O72 91.93(16) . 4 ?
O3 Mn3 O72 88.17(16) . 4 ?
O9 Mn3 O72 89.00(17) . 4 ?
O11 Mn3 O72 92.16(17) 4 4 ?
O71 Mn3 O72 9.2(2) 4 4 ?
O2 Mn3 O12 92.24(12) . . ?
O3 Mn3 O12 95.84(10) . . ?
O9 Mn3 O12 86.53(14) . . ?
O11 Mn3 O12 83.37(13) 4 . ?
O71 Mn3 O12 164.99(17) 4 . ?
O72 Mn3 O12 174.03(17) 4 . ?
Mn1 O1 Mn1 95.32(11) . 4 ?
Mn1 O1 Mn1 95.21(11) . 3 ?
Mn1 O1 Mn1 99.71(9) 4 3 ?
Mn1 O2 Mn3 133.10(12) 4 . ?
Mn1 O2 Mn2 94.35(9) 4 4 ?
Mn3 O2 Mn2 123.14(11) . 4 ?
Mn1 O3 Mn2 95.26(9) . . ?
Mn1 O3 Mn3 133.55(11) . . ?
Mn2 O3 Mn3 128.51(11) . . ?
C1 O4 Mn1 125.4(2) . . ?
C1 O5 Mn2 123.7(2) . . ?
O5 C1 O4 124.9(3) . . ?
O5 C1 C2 120.0(3) . . ?
O4 C1 C2 115.0(3) . . ?
C31 O61 Mn2 131.6(4) . . ?
C31 O71 Mn3 128.2(5) . 3 ?
O61 C31 O71 124.6(6) . . ?
O61 C31 C41 117.1(6) . . ?
O71 C31 C41 118.0(7) . . ?
C32 O62 Mn2 130.3(4) . . ?
C32 O72 Mn3 134.5(5) . 3 ?
O72 C32 O62 124.8(7) . . ?
O72 C32 C42 115.1(7) . . ?
O62 C32 C42 118.3(6) . . ?
C5 O8 Mn2 133.70(19) . . ?
C5 O9 Mn3 132.2(2) . . ?
O9 C5 O8 125.8(3) . . ?
O9 C5 C6 117.8(3) . . ?
O8 C5 C6 116.4(2) . . ?
C7 O10 Mn2 130.3(2) . . ?
C7 O11 Mn3 136.46(19) . 3 ?
O11 C7 O10 125.4(3) . . ?
O11 C7 C8 118.1(3) . . ?
O10 C7 C8 116.5(3) . . ?
O14 C9 O15 126.7(9) . . ?
O14 C9 C10 117.4(9) . . ?
O15 C9 C10 115.6(10) . . ?
_diffrn_measured_fraction_theta_max 0.909
_diffrn_reflns_theta_full        30.70
_diffrn_measured_fraction_theta_full 0.909
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.109


data_Mn12_H2O
_database_code_depnum_ccdc_archive 'CCDC 916381'
#TrackingRef '2.cif'
_audit_creation_date             12-08-23
_audit_creation_method           CRYSTALS_ver_14.40
_oxford_structure_analysis_title 'Mn12_H2O in I-4'
_exptl_crystal_recrystallisation_method 
;
Crystals of Mn12-acetate were heated to 130 C under an N2 atmosphere
for two hours.
;
_exptl_special_details           
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details          
;
The data were cut at 0.84 Ang. in XPREP.
All non-H atoms except for C31/C32 and C41/C42 were refined with adps. Half
occupied atoms C31/C32 and C41/C42 were refined isotropically. H atoms were
added to C atoms in calculated positions. H atoms attached to O12 and O13
were found in a difference map. All H atoms were allowed to ride on their
parent atoms.
This structure is comprised of the {Mn12} cluster present in Mn12-acetate,
but with the removal of the lattice solvent acetic acid.
Checkcif output (with comments):
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) ..... 11
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.595 127
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 10
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ... 17
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still 91 Perc.
951_ALERT_5_G Reported and Calculated Kmax Values Differ by .. 6
The data are not fully complete due to the quality of single crystal samples
available. However all data that were collected (93% of reflections) are
consistent with the structural model.
601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 159 A**3
No action.
152_ALERT_1_C The Supplied and Calc. Volume s.u. Differ by ... 6 Units
Volume Reported 3576.0(14) Calculated 3576(2)
One is calculated by Shelxl, the other by Platon. It is possible
that one program takes the correlation of the errors in the a and b
axes into account, while the other doesn't. In fact neither is correct
because neither program has access to the full correlation matrix
used in cell refinement. The volume calculated by DENZO, which
does take these correlations into account, is 3575.996(1401) Ang**3.
042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
We prefer to report the moiety formula as given as it is more chemically
meaningful.
125_ALERT_4_C No '_symmetry_space_group_name_Hall' Given ..... ?
No action.
737_ALERT_1_C D...A Calc 2.645(5), Rep 2.644(14) ...... 2.80 su-Ra
O12 -O6 1.555 3.565 # 53
737_ALERT_1_C D...A Calc 2.671(5), Rep 2.672(14) ...... 2.80 su-Ra
O12 -O13 1.555 8.565 # 53
737_ALERT_1_C D...A Calc 2.999(5), Rep 2.999(14) ...... 2.80 su-Ra
O13 -O5 1.555 3.565 # 53
737_ALERT_1_C D...A Calc 2.782(5), Rep 2.782(14) ...... 2.80 su-Ra
O13 -O7 1.555 1.555 # 53
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif can be badly in error.
758_ALERT_4_C D-H..A Calc 177.00, Rep 176.57(17) ...... Senseless su
O13 -H132 -O7 1.555 1.555 1.555 # 117
No action
915_ALERT_3_C Low Friedel Pair Coverage ...................... 61 Perc.
033_ALERT_4_G Flack x Parameter Value Deviates from Zero ..... 0.47
Flack 0.47(3)
A Flack Parameter in the region of 0.50 indicates an inversion twin. The small
ESD is evidence of the accuracy of this value. The low Friedel pair coverage
does not concern us as we are not especially interested in the absolute
configuration of the structure. In any case, it appears to be consistent with
the analogous structures of Mn12-acetate and Mn12-acetate (fully desolvated).
No action taken.
341_ALERT_3_A Low Bond Precision on C-C Bonds ............... 8.00 Ang
230_ALERT_2_B Hirshfeld Test Diff for C5 -- C6 .. 7.50 su
242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C31
007_ALERT_5_G Note: Number of Unrefined D-H Atoms ............ 4
We are sure of the identity of these atoms due to the materials used to
synthesize these crystals. No action.
301_ALERT_3_G Note: Main Residue Disorder ................... 9 Perc.
No action.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 68
C31 -O6 -C32 1.555 1.555 1.555 14.40 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 71
C31 -O7 -C32 1.555 1.555 1.555 13.90 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 117
H413 -H421 -C42 1.555 1.555 1.555 30.00 Deg.
790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2
H2 O
No action.
808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found !
929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked !
The following is specified under _refine_ls_weighting_details:
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
3.34 -2.65 0.900
This was chosen over the Sheldrick scheme because it gave a more linear
normal probability plot.
005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ?
The following is specified under _iucr_refine_instruction_details_constraints:
#
# Punched on 23/08/12 at 11:49:43
#
#LIST 12
BLOCK SCALE X'S, MN(1,U'S) UNTIL O(7)
CONT ENANTIO
CONT C(31,U[ISO]) UNTIL C(42)
CONT O(8,U'S) UNTIL O(13)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE O ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
RIDE O ( 13,X'S) H ( 131,X'S) H ( 132,X'S)
END
;
#end of refcif
_cell_length_a                   17.235(4)
_cell_length_b                   17.235(4)
_cell_length_c                   12.038(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3576.0(14)
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z            2
# Given Formula = C32 H64 Mn12 O52
# Dc = 1.80 Fooo = 1944.00 Mu = 21.44 M = 484.99
# Found Formula = C32 H64 Mn12 O52
# Dc = 1.80 FOOO = 1944.00 Mu = 21.44 M = 484.99
_chemical_formula_sum            'C32 H64 Mn12 O52'
_chemical_formula_moiety         '[Mn12O12(OAc)16(H2O)4].4H2O'
_chemical_compound_source        AF37A
_chemical_formula_weight         1939.96
_cell_measurement_reflns_used    1253
_cell_measurement_theta_min      1.000
_cell_measurement_theta_max      25.028
_cell_measurement_temperature    100
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.300
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    2.144
# Sheldrick geometric approximatio 0.81 0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_T_max  1.044
# For a Kappa CCD, set Tmin to 1.0 and
# Tmax to the ratio of max:min frame scales in scale_all.log
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?
_diffrn_ambient_temperature      100
_diffrn_reflns_number            2469
_reflns_number_total             2466
_diffrn_reflns_av_R_equivalents  0.019
# Number of reflections without Friedels Law is 2466
# Number of reflections with Friedels Law is 1627
# Theoretical number of reflections is about 1581
_diffrn_reflns_theta_min         2.363
_diffrn_reflns_theta_max         25.034
_diffrn_measured_fraction_theta_max 0.926
_diffrn_reflns_theta_full        25.034
_diffrn_measured_fraction_theta_full 0.926
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -20
_reflns_limit_h_max              20
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              14
_oxford_diffrn_Wilson_B_factor   1.70
_oxford_diffrn_Wilson_scale      1.83
_atom_sites_solution_primary     'charge flipping' #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   'difmap and calculated'
_refine_diff_density_min         -0.29
_refine_diff_density_max         0.40
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         2385
_refine_ls_number_restraints     0
_refine_ls_number_parameters     216
_oxford_refine_ls_R_factor_ref   0.0445
_refine_ls_wR_factor_ref         0.0332
_refine_ls_goodness_of_fit_ref   1.1297
_refine_ls_shift/su_max          0.0003172
_refine_ls_shift/su_mean         0.0000409
# The values computed with all filters except I/sigma
_oxford_reflns_number_all        2436
_refine_ls_R_factor_all          0.0458
_refine_ls_wR_factor_all         0.0372
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                2351
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_gt          0.0329
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_abs_structure_details 'Flack (1983), 839 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration ad
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
3.34 -2.65 0.900
;
# Insert your own references if required - in alphabetical order
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.41579(5) 0.48543(5) 0.07883(7) 0.0254 1.0000 Uani . . . . . .
Mn2 Mn 0.25738(5) 0.45727(5) 0.07989(7) 0.0271 1.0000 Uani . . . . . .
Mn3 Mn 0.29813(5) 0.63692(5) -0.00364(7) 0.0269 1.0000 Uani . . . . . .
O1 O 0.4290(2) 0.4888(2) -0.0770(3) 0.0231 1.0000 Uani . . . . . .
O2 O 0.3253(2) 0.5446(2) 0.0703(3) 0.0275 1.0000 Uani . . . . . .
O3 O 0.4001(2) 0.6503(2) -0.0623(3) 0.0268 1.0000 Uani . . . . . .
O4 O 0.4123(2) 0.4842(2) 0.2382(3) 0.0302 1.0000 Uani . . . . . .
O5 O 0.2868(2) 0.4518(2) 0.2610(3) 0.0318 1.0000 Uani . . . . . .
C1 C 0.3532(3) 0.4661(3) 0.2972(4) 0.0288 1.0000 Uani . . . . . .
C2 C 0.3679(3) 0.4616(3) 0.4204(5) 0.0327 1.0000 Uani . . . . . .
O6 O 0.2350(2) 0.4614(2) -0.0989(3) 0.0340 1.0000 Uani . . . . . .
O7 O 0.2623(2) 0.5815(2) -0.1555(3) 0.0341 1.0000 Uani . . . . . .
C31 C 0.2422(10) 0.5134(9) -0.1719(12) 0.020(4) 0.5000 Uiso . . . . . .
C32 C 0.2592(11) 0.5065(10) -0.1757(14) 0.030(5) 0.5000 Uiso . . . . . .
C41 C 0.2405(10) 0.4837(9) -0.2914(12) 0.046(4) 0.5000 Uiso . . . . . .
C42 C 0.2735(9) 0.4803(8) -0.2914(11) 0.036(3) 0.5000 Uiso . . . . . .
O8 O 0.3669(2) 0.8090(2) -0.0932(3) 0.0311 1.0000 Uani . . . . . .
O9 O 0.2620(2) 0.7317(2) -0.0775(3) 0.0333 1.0000 Uani . . . . . .
C5 C 0.2948(4) 0.7964(3) -0.0961(4) 0.0315 1.0000 Uani . . . . . .
C6 C 0.2425(3) 0.8644(3) -0.1186(5) 0.0305 1.0000 Uani . . . . . .
O10 O 0.1647(2) 0.5158(2) 0.1148(3) 0.0311 1.0000 Uani . . . . . .
O11 O 0.1910(2) 0.6357(2) 0.0540(3) 0.0336 1.0000 Uani . . . . . .
C7 C 0.1468(3) 0.5856(3) 0.0971(4) 0.0274 1.0000 Uani . . . . . .
C8 C 0.0678(4) 0.6100(4) 0.1300(5) 0.0409 1.0000 Uani . . . . . .
O12 O 0.3218(2) 0.7083(2) 0.1404(3) 0.0312 1.0000 Uani . . . . . .
O13 O 0.2874(2) 0.6836(2) -0.3308(3) 0.0382 1.0000 Uani . . . . . .
H21 H 0.4061 0.4996 0.4424 0.0496 1.0000 Uiso R . . . . .
H22 H 0.3211 0.4699 0.4598 0.0502 1.0000 Uiso R . . . . .
H23 H 0.3876 0.4113 0.4381 0.0503 1.0000 Uiso R . . . . .
H411 H 0.2216 0.4312 -0.2920 0.0669 0.5000 Uiso R . . . . .
H412 H 0.2066 0.5158 -0.3355 0.0672 0.5000 Uiso R . . . . .
H413 H 0.2924 0.4853 -0.3210 0.0670 0.5000 Uiso R . . . . .
H421 H 0.3272 0.4667 -0.2995 0.0529 0.5000 Uiso R . . . . .
H422 H 0.2606 0.5211 -0.3422 0.0530 0.5000 Uiso R . . . . .
H423 H 0.2421 0.4356 -0.3073 0.0529 0.5000 Uiso R . . . . .
H61 H 0.2159 0.8766 -0.0511 0.0469 1.0000 Uiso R . . . . .
H62 H 0.2738 0.9076 -0.1405 0.0470 1.0000 Uiso R . . . . .
H63 H 0.2074 0.8507 -0.1763 0.0476 1.0000 Uiso R . . . . .
H81 H 0.0643 0.6099 0.2086 0.0622 1.0000 Uiso R . . . . .
H82 H 0.0574 0.6615 0.1039 0.0620 1.0000 Uiso R . . . . .
H83 H 0.0300 0.5748 0.1006 0.0621 1.0000 Uiso R . . . . .
H121 H 0.3613 0.7341 0.1307 0.0468 1.0000 Uiso R . . . . .
H122 H 0.2864 0.7391 0.1524 0.0468 1.0000 Uiso R . . . . .
H131 H 0.3267 0.7095 -0.3183 0.0579 1.0000 Uiso R . . . . .
H132 H 0.2817 0.6544 -0.2781 0.0579 1.0000 Uiso R . . . . .
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 0.0273(4) 0.0265(4) 0.0224(4) -0.0006(4) 0.0003(4) 0.0005(3)
Mn2 0.0283(5) 0.0282(5) 0.0246(4) 0.0000(4) 0.0011(4) -0.0008(4)
Mn3 0.0267(4) 0.0277(5) 0.0263(4) 0.0007(4) 0.0013(4) 0.0015(4)
O1 0.021(2) 0.026(2) 0.0224(18) -0.0014(18) -0.0014(17) -0.0058(15)
O2 0.029(2) 0.034(2) 0.0200(17) -0.0020(16) 0.0002(16) -0.0002(17)
O3 0.029(2) 0.030(2) 0.0217(18) -0.0010(15) -0.0030(15) -0.0029(18)
O4 0.033(2) 0.033(2) 0.0249(19) -0.0011(16) -0.0002(17) 0.002(2)
O5 0.034(2) 0.036(2) 0.0255(19) 0.0006(17) 0.0016(16) -0.0022(19)
C1 0.031(3) 0.027(3) 0.028(3) 0.000(2) 0.004(2) 0.004(3)
C2 0.034(3) 0.037(3) 0.026(3) -0.003(3) 0.003(3) 0.004(3)
O6 0.042(3) 0.035(2) 0.025(2) -0.0007(17) -0.0005(17) -0.0043(19)
O7 0.040(2) 0.038(3) 0.025(2) 0.0006(17) -0.0013(17) 0.001(2)
O8 0.033(2) 0.030(2) 0.030(2) 0.0013(17) -0.0002(18) -0.0016(17)
O9 0.033(2) 0.032(2) 0.034(2) 0.0009(19) -0.0011(19) 0.0017(18)
C5 0.042(4) 0.032(3) 0.020(3) -0.008(2) 0.003(2) -0.012(3)
C6 0.028(3) 0.030(3) 0.034(3) 0.004(2) -0.003(2) 0.009(3)
O10 0.028(2) 0.032(2) 0.033(2) -0.0024(16) 0.0005(16) 0.0069(18)
O11 0.033(2) 0.029(2) 0.039(2) 0.0048(16) 0.0015(17) 0.0017(19)
C7 0.025(3) 0.030(3) 0.027(3) -0.009(2) 0.001(2) 0.004(2)
C8 0.032(3) 0.039(4) 0.052(4) -0.002(3) -0.003(3) -0.001(3)
O12 0.030(2) 0.033(2) 0.031(2) -0.0054(16) 0.0039(17) 0.0003(18)
O13 0.040(3) 0.041(2) 0.034(2) 0.0077(19) -0.0037(18) -0.002(2)
_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.8034(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O1 3_565 1.940(4) yes
Mn1 . O1 5_655 1.911(4) yes
Mn1 . O3 5_655 1.871(4) yes
Mn1 . O1 . 1.890(4) yes
Mn1 . O2 . 1.866(4) yes
Mn1 . O4 . 1.919(4) yes
Mn2 . O8 5_655 1.939(4) yes
Mn2 . O3 5_655 1.883(4) yes
Mn2 . O2 . 1.910(4) yes
Mn2 . O5 . 2.240(4) yes
Mn2 . O6 . 2.188(4) yes
Mn2 . O10 . 1.936(4) yes
Mn3 . O2 . 1.882(4) yes
Mn3 . O3 . 1.908(4) yes
Mn3 . O7 . 2.153(4) yes
Mn3 . O9 . 1.961(4) yes
Mn3 . O11 . 1.972(4) yes
Mn3 . O12 . 2.165(4) yes
O4 . C1 . 1.282(6) yes
O5 . C1 . 1.248(7) yes
C1 . C2 . 1.507(8) yes
C2 . H21 . 0.965 no
C2 . H22 . 0.946 no
C2 . H23 . 0.955 no
O6 . C31 . 1.262(15) yes
O6 . C32 . 1.278(17) yes
O7 . C31 . 1.239(15) yes
O7 . C32 . 1.315(18) yes
C31 . C41 . 1.53(2) yes
C32 . C42 . 1.49(2) yes
C41 . H411 . 0.960 no
C41 . H412 . 0.965 no
C41 . H413 . 0.963 no
C42 . H421 . 0.960 no
C42 . H422 . 0.959 no
C42 . H423 . 0.961 no
O8 . C5 . 1.262(7) yes
O9 . C5 . 1.270(6) yes
C5 . C6 . 1.503(8) yes
C6 . H61 . 0.956 no
C6 . H62 . 0.956 no
C6 . H63 . 0.951 no
O10 . C7 . 1.259(7) yes
O11 . C7 . 1.263(7) yes
C7 . C8 . 1.479(8) yes
C8 . H81 . 0.948 no
C8 . H82 . 0.958 no
C8 . H83 . 0.958 no
O12 . H121 . 0.822 no
O12 . H122 . 0.823 no
O13 . H131 . 0.825 no
O13 . H132 . 0.816 no
H413 . H421 . 0.729 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 3_565 Mn1 . O1 5_655 80.15(17) yes
O1 3_565 Mn1 . O3 5_655 172.72(15) yes
O1 5_655 Mn1 . O3 5_655 97.01(15) yes
O1 3_565 Mn1 . O1 . 83.52(17) yes
O1 5_655 Mn1 . O1 . 84.32(17) yes
O3 5_655 Mn1 . O1 . 89.54(15) yes
O1 3_565 Mn1 . O2 . 97.26(15) yes
O1 5_655 Mn1 . O2 . 175.41(16) yes
O3 5_655 Mn1 . O2 . 85.11(16) yes
O1 . Mn1 . O2 . 91.64(16) yes
O1 3_565 Mn1 . O4 . 92.28(16) yes
O1 5_655 Mn1 . O4 . 91.86(17) yes
O3 5_655 Mn1 . O4 . 94.52(16) yes
O1 . Mn1 . O4 . 174.75(17) yes
O2 . Mn1 . O4 . 92.02(16) yes
O8 5_655 Mn2 . O3 5_655 94.99(17) yes
O8 5_655 Mn2 . O2 . 177.96(16) yes
O3 5_655 Mn2 . O2 . 83.56(16) yes
O8 5_655 Mn2 . O5 . 91.14(15) yes
O3 5_655 Mn2 . O5 . 84.03(15) yes
O2 . Mn2 . O5 . 87.30(15) yes
O8 5_655 Mn2 . O6 . 90.18(16) yes
O3 5_655 Mn2 . O6 . 93.16(15) yes
O2 . Mn2 . O6 . 91.32(15) yes
O5 . Mn2 . O6 . 177.00(16) yes
O8 5_655 Mn2 . O10 . 85.10(17) yes
O3 5_655 Mn2 . O10 . 173.89(15) yes
O2 . Mn2 . O10 . 96.19(17) yes
O5 . Mn2 . O10 . 89.85(14) yes
O6 . Mn2 . O10 . 92.95(16) yes
O2 . Mn3 . O3 . 92.76(16) yes
O2 . Mn3 . O7 . 95.60(15) yes
O3 . Mn3 . O7 . 90.19(15) yes
O2 . Mn3 . O9 . 175.86(16) yes
O3 . Mn3 . O9 . 91.35(16) yes
O7 . Mn3 . O9 . 83.92(16) yes
O2 . Mn3 . O11 . 93.29(16) yes
O3 . Mn3 . O11 . 173.54(17) yes
O7 . Mn3 . O11 . 91.48(16) yes
O9 . Mn3 . O11 . 82.62(17) yes
O2 . Mn3 . O12 . 93.14(15) yes
O3 . Mn3 . O12 . 93.09(15) yes
O7 . Mn3 . O12 . 170.51(15) yes
O9 . Mn3 . O12 . 87.11(16) yes
O11 . Mn3 . O12 . 84.31(16) yes
Mn1 5_655 O1 . Mn1 3_565 99.83(17) yes
Mn1 5_655 O1 . Mn1 . 94.73(17) yes
Mn1 3_565 O1 . Mn1 . 95.70(16) yes
Mn2 . O2 . Mn3 . 122.84(19) yes
Mn2 . O2 . Mn1 . 94.50(17) yes
Mn3 . O2 . Mn1 . 134.1(2) yes
Mn3 . O3 . Mn2 3_565 128.7(2) yes
Mn3 . O3 . Mn1 3_565 133.6(2) yes
Mn2 3_565 O3 . Mn1 3_565 95.22(17) yes
Mn1 . O4 . C1 . 125.5(4) yes
Mn2 . O5 . C1 . 122.6(3) yes
O4 . C1 . O5 . 125.7(5) yes
O4 . C1 . C2 . 115.1(5) yes
O5 . C1 . C2 . 119.2(5) yes
C1 . C2 . H21 . 110.6 no
C1 . C2 . H22 . 110.0 no
H21 . C2 . H22 . 109.9 no
C1 . C2 . H23 . 109.1 no
H21 . C2 . H23 . 108.2 no
H22 . C2 . H23 . 109.1 no
Mn2 . O6 . C31 . 133.7(7) yes
Mn2 . O6 . C32 . 132.3(8) yes
C31 . O6 . C32 . 14.4(12) yes
Mn3 . O7 . C31 . 129.4(7) yes
Mn3 . O7 . C32 . 127.2(8) yes
C31 . O7 . C32 . 13.9(12) yes
O6 . C31 . O7 . 126.2(12) yes
O6 . C31 . C41 . 114.5(12) yes
O7 . C31 . C41 . 118.2(12) yes
O7 . C32 . O6 . 118.6(13) yes
O7 . C32 . C42 . 117.7(13) yes
O6 . C32 . C42 . 123.1(14) yes
C31 . C41 . H411 . 109.3 no
C31 . C41 . H412 . 109.8 no
H411 . C41 . H412 . 109.3 no
C31 . C41 . H413 . 108.7 no
H411 . C41 . H413 . 109.8 no
H412 . C41 . H413 . 110.0 no
C32 . C42 . H421 . 109.3 no
C32 . C42 . H422 . 109.7 no
H421 . C42 . H422 . 109.7 no
C32 . C42 . H423 . 109.8 no
H421 . C42 . H423 . 109.1 no
H422 . C42 . H423 . 109.3 no
Mn2 3_565 O8 . C5 . 133.8(4) yes
Mn3 . O9 . C5 . 132.1(4) yes
O9 . C5 . O8 . 125.7(5) yes
O9 . C5 . C6 . 116.8(5) yes
O8 . C5 . C6 . 117.5(5) yes
C5 . C6 . H61 . 107.7 no
C5 . C6 . H62 . 108.6 no
H61 . C6 . H62 . 109.5 no
C5 . C6 . H63 . 108.6 no
H61 . C6 . H63 . 111.7 no
H62 . C6 . H63 . 110.6 no
Mn2 . O10 . C7 . 131.5(4) yes
Mn3 . O11 . C7 . 135.8(4) yes
O11 . C7 . O10 . 125.1(5) yes
O11 . C7 . C8 . 118.1(5) yes
O10 . C7 . C8 . 116.9(5) yes
C7 . C8 . H81 . 109.0 no
C7 . C8 . H82 . 110.4 no
H81 . C8 . H82 . 108.5 no
C7 . C8 . H83 . 110.3 no
H81 . C8 . H83 . 108.8 no
H82 . C8 . H83 . 109.7 no
Mn3 . O12 . H121 . 110.5 no
Mn3 . O12 . H122 . 111.6 no
H121 . O12 . H122 . 106.9 no
H131 . O13 . H132 . 106.9 no
C41 . H413 . H421 . 128.4 no
H413 . H421 . C42 . 30.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H63 . O12 8_564 151.74(16) 0.951 2.481 3.349(14) yes
O12 . H121 . O6 3_565 163.77(17) 0.822 1.844 2.644(14) yes
O12 . H121 . C32 3_565 143.5(4) 0.822 2.563 3.261(14) yes
O12 . H122 . O13 8_565 173.48(18) 0.823 1.853 2.672(14) yes
O13 . H131 . O5 3_565 148.42(14) 0.825 2.265 2.999(14) yes
O13 . H132 . O7 . 176.57(17) 0.816 1.967 2.782(14) yes
_iucr_refine_instruction_details_constraints 
;
#
# Punched on 23/08/12 at 11:49:43
#
#LIST 12
BLOCK SCALE X'S, MN(1,U'S) UNTIL O(7)
CONT ENANTIO
CONT C(31,U[ISO]) UNTIL C(42)
CONT O(8,U'S) UNTIL O(13)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE O ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
RIDE O ( 13,X'S) H ( 131,X'S) H ( 132,X'S)
END
;
_iucr_refine_instruction_details_restraints 
;
#
# Punched on 23/08/12 at 11:49:43
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;


data_AF37A
_database_code_depnum_ccdc_archive 'CCDC 916382'
#TrackingRef '3.cif'
_audit_creation_date             12-04-25
_audit_creation_method           CRYSTALS_ver_14.40
_oxford_structure_analysis_title 'AF37A in I-4'
_exptl_crystal_recrystallisation_method 
;
Crystals of Mn12-acetate were heated to 130 C under an N2 atmosphere
for two hours.
;
_exptl_special_details           
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details          
;
The data were cut at 0.84 Ang. in XPREP.
All non-H atoms except for C41/C42 were refined with adps. Half occupied atoms
C41/C42 were refined isotropically. H atoms were added to C atoms geometrically.
H atoms attached to O12 were found in a difference map. All H atoms were
allowed to ride on their parent atoms.
This structure is comprised of the main {Mn12} cluster present in Mn12-acetate,
but with the removal of the lattice solvent water and acetic acid.
Checkcif output (with comments):
420_ALERT_2_B D-H Without Acceptor O12 - H121 ... ?
No action. H121 was found in a difference map and so its position is not
in doubt.
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
We prefer to report the moiety formula as given as it is more chemically
meaningful.
125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
301_ALERT_3_G Main Residue Disorder ......................... 4.00 Perc.
432_ALERT_2_C Short Inter X...Y Contact C1 .. C6 .. 3.19 Ang.
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 17.80 Deg.
C41 -C3 -C42 1.555 1.555 1.555
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1
C32 H56 Mn12 O48
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C5
No action.
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 10
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 2
909_ALERT_3_G Percentage of Observed Data at Theta(Max) still 92 Perc.
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ... 3
_diffrn_reflns_theta_min 1.794
_diffrn_reflns_theta_max 25.019
_diffrn_measured_fraction_theta_max 1.000
No action.
033_ALERT_2_G Flack Parameter Value Deviates 2 * su from zero. 0.50
Flack=0.497(17)
A Flack Parameter of 0.50 indicates an inversion twin. The small ESD is
evidence of the accuracy of this value. No action taken.
005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ?
The following is specified under _iucr_refine_instruction_details_constraints:
#
# Punched on 09/05/12 at 18:04:57
#
#LIST 12
BLOCK SCALE X'S, MN(1,U'S) UNTIL C(3)
CONT C(41,U[ISO]) UNTIL C(42)
CONT O(8,U'S) UNTIL O(12)
CONT ENANTIO
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE O ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
END
007_ALERT_5_G Note: Number of Unrefined D-H Atoms ............ 2
No action. We are sure of the identity of these atoms.
152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ... 2 Units
Volume Reported 3067.4(4) Calculated 3067.4(6)
One is calculated by Crystals, the other by Platon. It is possible
that one program takes the correlation of the errors in the a and b
axes into account, while the other doesn't. In fact neither is correct
because neither program has access to the full correlation matrix
used in cell refinement.
432_ALERT_2_G Short Inter X...Y Contact C1 .. C6 .. 3.19 Ang.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 73
C41 -C3 -C42 1.555 1.555 1.555 17.80 Deg.
795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C5
No action.
808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found !
929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked !
The following is specified under _refine_ls_weighting_details:
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
5.55 6.99 2.44
This was chosen over the Sheldrick scheme since it gave a more linear normal
probability plot.
;
#end of refcif
_cell_length_a                   16.0506(12)
_cell_length_b                   16.0506(12)
_cell_length_c                   11.9067(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3067.4(4)
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z            2
# Given Formula = C32 H56 Mn12 O48
# Dc = 2.02 Fooo = 1864.00 Mu = 24.91 M = 466.98
# Found Formula = C32 H56 Mn12 O48
# Dc = 2.02 FOOO = 1864.00 Mu = 24.91 M = 466.98
_chemical_formula_sum            'C32 H56 Mn12 O48'
_chemical_formula_moiety         '[Mn12O12(O2CCH3)16(H2O)4]'
_chemical_compound_source        AF37A
_chemical_formula_weight         1867.90
_cell_measurement_reflns_used    1692
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27
_cell_measurement_temperature    100
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.300
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1864
_exptl_absorpt_coefficient_mu    2.491
# Sheldrick geometric approximatio 0.78 0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_T_max  1.31
# For a Kappa CCD, set Tmin to 1.0 and
# Tmax to the ratio of max:min frame scales in scale_all.log
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?
_diffrn_ambient_temperature      100
_diffrn_reflns_number            2694
_reflns_number_total             2694
_diffrn_reflns_av_R_equivalents  0.010
# Number of reflections without Friedels Law is 2694
# Number of reflections with Friedels Law is 1419
# Theoretical number of reflections is about 1354
_diffrn_reflns_theta_min         1.794
_diffrn_reflns_theta_max         25.019
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.019
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -18
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              14
_oxford_diffrn_Wilson_B_factor   1.61
_oxford_diffrn_Wilson_scale      47.83
_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   difmap
_refine_diff_density_min         -0.07
_refine_diff_density_max         0.06
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     0
_refine_ls_number_parameters     208
_oxford_refine_ls_R_factor_ref   0.0234
_refine_ls_wR_factor_ref         0.0457
_refine_ls_goodness_of_fit_ref   0.9668
_refine_ls_shift/su_max          0.0010638
_refine_ls_shift/su_mean         0.0000730
# The values computed with all filters except I/sigma
_oxford_reflns_number_all        2680
_refine_ls_R_factor_all          0.0234
_refine_ls_wR_factor_all         0.0459
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                2605
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_gt          0.0450
_refine_ls_abs_structure_Flack   0.497(17)
_refine_ls_abs_structure_details 'Flack (1983), 1275 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration ad
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
5.55 6.99 2.44
;
# Insert your own references if required - in alphabetical order
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn -0.90969(3) -0.51693(3) -0.32956(4) 0.0210 1.0000 Uani . . . . . .
Mn2 Mn -0.73975(3) -0.55150(3) -0.32485(4) 0.0234 1.0000 Uani . . . . . .
Mn3 Mn -0.86145(3) -0.72008(3) -0.26762(4) 0.0239 1.0000 Uani . . . . . .
O1 O -0.98649(12) -0.42436(12) -0.32881(18) 0.0198 1.0000 Uani . . . . . .
O2 O -0.95607(13) -0.69081(12) -0.17916(18) 0.0214 1.0000 Uani . . . . . .
O3 O -0.84160(13) -0.60944(13) -0.30722(17) 0.0227 1.0000 Uani . . . . . .
O4 O -0.90459(15) -0.52819(14) -0.49012(17) 0.0251 1.0000 Uani . . . . . .
O5 O -0.77126(14) -0.57289(15) -0.50443(19) 0.0273 1.0000 Uani . . . . . .
C1 C -0.8429(2) -0.5630(2) -0.5421(3) 0.0265 1.0000 Uani . . . . . .
C2 C -0.8630(2) -0.5929(2) -0.6591(3) 0.0350 1.0000 Uani . . . . . .
O6 O -1.05110(15) -0.78746(14) -0.35383(19) 0.0304 1.0000 Uani . . . . . .
O7 O -0.92639(15) -0.74860(15) -0.4183(2) 0.0319 1.0000 Uani . . . . . .
C3 C -0.9989(2) -0.7740(2) -0.4317(3) 0.0314 1.0000 Uani . . . . . .
C41 C -1.0264(5) -0.8047(7) -0.5484(7) 0.037(2) 0.5000 Uiso . . . . . .
C42 C -1.0288(5) -0.7754(7) -0.5518(7) 0.037(2) 0.5000 Uiso . . . . . .
O8 O -0.67089(14) -0.65110(13) -0.3364(2) 0.0277 1.0000 Uani . . . . . .
O9 O -0.76238(14) -0.75680(14) -0.3513(2) 0.0287 1.0000 Uani . . . . . .
C5 C -0.6902(2) -0.7254(2) -0.3607(3) 0.0278 1.0000 Uani . . . . . .
C6 C -0.6205(2) -0.7805(2) -0.3992(3) 0.0337 1.0000 Uani . . . . . .
O10 O -0.98869(13) -0.85992(13) -0.1398(2) 0.0271 1.0000 Uani . . . . . .
O11 O -0.86471(14) -0.83600(14) -0.2204(2) 0.0295 1.0000 Uani . . . . . .
C7 C -0.9165(2) -0.88191(19) -0.1698(3) 0.0258 1.0000 Uani . . . . . .
C8 C -0.8912(2) -0.9702(2) -0.1469(3) 0.0294 1.0000 Uani . . . . . .
O12 O -0.76953(16) -0.70732(16) -0.1215(2) 0.0391 1.0000 Uani . . . . . .
H21 H -0.8120 -0.6054 -0.6998 0.0517 1.0000 Uiso R . . . . .
H22 H -0.8939 -0.5508 -0.6998 0.0518 1.0000 Uiso R . . . . .
H23 H -0.8972 -0.6435 -0.6515 0.0524 1.0000 Uiso R . . . . .
H411 H -1.0046 -0.8596 -0.5611 0.0488 0.5000 Uiso R . . . . .
H412 H -1.0031 -0.7662 -0.6013 0.0494 0.5000 Uiso R . . . . .
H413 H -1.0863 -0.8048 -0.5511 0.0493 0.5000 Uiso R . . . . .
H421 H -0.9880 -0.8072 -0.5944 0.0527 0.5000 Uiso R . . . . .
H422 H -1.0826 -0.8015 -0.5531 0.0532 0.5000 Uiso R . . . . .
H423 H -1.0324 -0.7184 -0.5760 0.0528 0.5000 Uiso R . . . . .
H61 H -0.5786 -0.7823 -0.3420 0.0512 1.0000 Uiso R . . . . .
H62 H -0.5982 -0.7583 -0.4666 0.0516 1.0000 Uiso R . . . . .
H63 H -0.6401 -0.8361 -0.4134 0.0503 1.0000 Uiso R . . . . .
H81 H -0.9187 -1.0044 -0.2027 0.0434 1.0000 Uiso R . . . . .
H82 H -0.8330 -0.9746 -0.1566 0.0438 1.0000 Uiso R . . . . .
H83 H -0.9065 -0.9855 -0.0713 0.0439 1.0000 Uiso R . . . . .
H121 H -0.7484 -0.7469 -0.0873 0.0592 1.0000 Uiso R . . . . .
H122 H -0.7452 -0.6610 -0.1096 0.0595 1.0000 Uiso R . . . . .
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 0.0223(2) 0.0209(2) 0.0197(2) -0.00016(19) 0.00118(19) -0.00036(18)
Mn2 0.0227(2) 0.0221(2) 0.0253(2) -0.0003(2) 0.0023(2) -0.00023(19)
Mn3 0.0246(2) 0.0213(2) 0.0257(2) 0.0010(2) 0.0043(2) 0.00037(19)
O1 0.0210(11) 0.0190(10) 0.0193(10) 0.0002(9) 0.0006(10) 0.0008(8)
O2 0.0218(10) 0.0205(10) 0.0220(10) 0.0012(10) -0.0005(10) 0.0022(9)
O3 0.0216(11) 0.0199(11) 0.0266(12) -0.0001(9) 0.0021(9) 0.0002(9)
O4 0.0307(13) 0.0278(12) 0.0168(11) -0.0002(9) 0.0005(9) -0.0009(10)
O5 0.0286(13) 0.0305(13) 0.0228(12) 0.0010(10) 0.0056(10) -0.0014(10)
C1 0.0346(19) 0.0215(16) 0.0233(16) 0.0007(13) 0.0042(14) -0.0042(14)
C2 0.040(2) 0.039(2) 0.0253(18) -0.0092(16) 0.0011(16) -0.0012(15)
O6 0.0310(12) 0.0332(13) 0.0271(13) -0.0028(10) 0.0016(10) -0.0011(10)
O7 0.0320(13) 0.0355(14) 0.0281(12) -0.0019(11) -0.0021(10) -0.0019(11)
C3 0.035(2) 0.0294(18) 0.0299(19) -0.0027(15) 0.0002(16) 0.0043(15)
O8 0.0256(11) 0.0241(11) 0.0333(13) -0.0003(10) 0.0029(11) 0.0004(9)
O9 0.0271(12) 0.0262(12) 0.0328(14) -0.0006(10) 0.0037(10) -0.0002(9)
C5 0.0281(18) 0.0318(18) 0.0234(17) 0.0021(14) 0.0017(14) 0.0028(14)
C6 0.0336(19) 0.0307(19) 0.037(2) -0.0027(16) 0.0081(16) 0.0010(15)
O10 0.0231(12) 0.0230(11) 0.0353(13) 0.0042(10) 0.0027(10) 0.0010(9)
O11 0.0309(12) 0.0247(12) 0.0329(13) 0.0039(10) 0.0048(11) 0.0009(10)
C7 0.0313(17) 0.0269(16) 0.0192(14) -0.0032(14) -0.0020(15) -0.0043(13)
C8 0.0270(17) 0.0248(17) 0.036(2) 0.0049(14) -0.0011(15) 0.0012(14)
O12 0.0416(15) 0.0381(14) 0.0376(15) 0.0052(12) -0.0047(12) 0.0014(12)
_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.15057(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O1 5_345 1.915(2) yes
Mn1 . O1 4_434 1.901(2) yes
Mn1 . O2 8_354 1.889(2) yes
Mn1 . O1 . 1.931(2) yes
Mn1 . O3 . 1.863(2) yes
Mn1 . O4 . 1.922(2) yes
Mn2 . O6 8_354 2.172(2) yes
Mn2 . O10 8_354 1.937(2) yes
Mn2 . O2 8_354 1.895(2) yes
Mn2 . O3 . 1.892(2) yes
Mn2 . O5 . 2.224(2) yes
Mn2 . O8 . 1.948(2) yes
Mn3 . O2 . 1.907(2) yes
Mn3 . O3 . 1.865(2) yes
Mn3 . O7 . 2.125(2) yes
Mn3 . O9 . 1.967(2) yes
Mn3 . O11 . 1.944(2) yes
Mn3 . O12 . 2.290(3) yes
O4 . C1 . 1.294(4) yes
O5 . C1 . 1.245(4) yes
C1 . C2 . 1.508(5) yes
C2 . H21 . 0.973 no
C2 . H22 . 0.968 no
C2 . H23 . 0.985 no
O6 . C3 . 1.268(4) yes
O7 . C3 . 1.243(4) yes
C3 . C41 . 1.540(9) yes
C3 . C42 . 1.509(9) yes
C41 . H411 . 0.961 no
C41 . H412 . 0.958 no
C41 . H413 . 0.961 no
C42 . H421 . 0.973 no
C42 . H422 . 0.960 no
C42 . H423 . 0.960 no
O8 . C5 . 1.266(4) yes
O9 . C5 . 1.269(4) yes
C5 . C6 . 1.498(4) yes
C6 . H61 . 0.958 no
C6 . H62 . 0.948 no
C6 . H63 . 0.962 no
O10 . C7 . 1.263(4) yes
O11 . C7 . 1.264(4) yes
C7 . C8 . 1.498(4) yes
C8 . H81 . 0.969 no
C8 . H82 . 0.944 no
C8 . H83 . 0.965 no
O12 . H121 . 0.827 no
O12 . H122 . 0.851 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 5_345 Mn1 . O1 4_434 84.36(10) yes
O1 5_345 Mn1 . O2 8_354 176.18(9) yes
O1 4_434 Mn1 . O2 8_354 92.08(9) yes
O1 5_345 Mn1 . O1 . 79.81(9) yes
O1 4_434 Mn1 . O1 . 83.92(9) yes
O2 8_354 Mn1 . O1 . 98.46(8) yes
O1 5_345 Mn1 . O3 . 96.75(9) yes
O1 4_434 Mn1 . O3 . 87.36(9) yes
O2 8_354 Mn1 . O3 . 84.45(9) yes
O1 . Mn1 . O3 . 170.90(9) yes
O1 5_345 Mn1 . O4 . 89.74(10) yes
O1 4_434 Mn1 . O4 . 174.02(10) yes
O2 8_354 Mn1 . O4 . 93.84(10) yes
O1 . Mn1 . O4 . 95.98(10) yes
O3 . Mn1 . O4 . 92.41(9) yes
O6 8_354 Mn2 . O10 8_354 92.60(10) yes
O6 8_354 Mn2 . O2 8_354 95.23(9) yes
O10 8_354 Mn2 . O2 8_354 94.05(9) yes
O6 8_354 Mn2 . O3 . 93.81(9) yes
O10 8_354 Mn2 . O3 . 173.31(10) yes
O2 8_354 Mn2 . O3 . 83.48(9) yes
O6 8_354 Mn2 . O5 . 171.12(9) yes
O10 8_354 Mn2 . O5 . 93.39(9) yes
O2 8_354 Mn2 . O5 . 90.88(9) yes
O3 . Mn2 . O5 . 80.47(9) yes
O6 8_354 Mn2 . O8 . 87.56(10) yes
O10 8_354 Mn2 . O8 . 86.74(9) yes
O2 8_354 Mn2 . O8 . 177.06(10) yes
O3 . Mn2 . O8 . 95.43(9) yes
O5 . Mn2 . O8 . 86.25(10) yes
O2 . Mn3 . O3 . 92.36(9) yes
O2 . Mn3 . O7 . 97.40(9) yes
O3 . Mn3 . O7 . 94.32(9) yes
O2 . Mn3 . O9 . 175.91(10) yes
O3 . Mn3 . O9 . 91.10(10) yes
O7 . Mn3 . O9 . 84.51(10) yes
O2 . Mn3 . O11 . 93.14(9) yes
O3 . Mn3 . O11 . 171.49(10) yes
O7 . Mn3 . O11 . 91.41(10) yes
O9 . Mn3 . O11 . 83.18(10) yes
O2 . Mn3 . O12 . 94.10(10) yes
O3 . Mn3 . O12 . 89.82(9) yes
O7 . Mn3 . O12 . 167.59(10) yes
O9 . Mn3 . O12 . 83.72(10) yes
O11 . Mn3 . O12 . 83.30(10) yes
Mn1 . O1 . Mn1 5_345 100.19(9) yes
Mn1 . O1 . Mn1 8_354 94.68(9) yes
Mn1 5_345 O1 . Mn1 8_354 95.20(9) yes
Mn3 . O2 . Mn2 4_434 120.85(11) yes
Mn3 . O2 . Mn1 4_434 130.74(12) yes
Mn2 4_434 O2 . Mn1 4_434 94.75(9) yes
Mn2 . O3 . Mn3 . 130.06(12) yes
Mn2 . O3 . Mn1 . 95.69(9) yes
Mn3 . O3 . Mn1 . 134.03(12) yes
Mn1 . O4 . C1 . 123.3(2) yes
Mn2 . O5 . C1 . 122.5(2) yes
O4 . C1 . O5 . 126.1(3) yes
O4 . C1 . C2 . 114.6(3) yes
O5 . C1 . C2 . 119.3(3) yes
C1 . C2 . H21 . 110.3 no
C1 . C2 . H22 . 110.5 no
H21 . C2 . H22 . 109.0 no
C1 . C2 . H23 . 107.3 no
H21 . C2 . H23 . 110.1 no
H22 . C2 . H23 . 109.7 no
Mn2 4_434 O6 . C3 . 133.1(2) yes
Mn3 . O7 . C3 . 129.6(2) yes
O6 . C3 . O7 . 125.5(3) yes
O6 . C3 . C41 . 114.5(4) yes
O7 . C3 . C41 . 119.3(4) yes
O6 . C3 . C42 . 118.7(4) yes
O7 . C3 . C42 . 115.1(4) yes
C41 . C3 . C42 . 17.8(5) yes
C3 . C41 . H411 . 109.3 no
C3 . C41 . H412 . 105.9 no
H411 . C41 . H412 . 110.2 no
C3 . C41 . H413 . 108.5 no
H411 . C41 . H413 . 111.0 no
H412 . C41 . H413 . 111.7 no
C3 . C42 . H421 . 106.8 no
C3 . C42 . H422 . 107.9 no
H421 . C42 . H422 . 111.5 no
C3 . C42 . H423 . 106.8 no
H421 . C42 . H423 . 112.6 no
H422 . C42 . H423 . 110.9 no
Mn2 . O8 . C5 . 130.6(2) yes
Mn3 . O9 . C5 . 131.6(2) yes
O9 . C5 . O8 . 125.3(3) yes
O9 . C5 . C6 . 118.3(3) yes
O8 . C5 . C6 . 116.3(3) yes
C5 . C6 . H61 . 108.9 no
C5 . C6 . H62 . 108.5 no
H61 . C6 . H62 . 110.4 no
C5 . C6 . H63 . 110.9 no
H61 . C6 . H63 . 109.2 no
H62 . C6 . H63 . 108.9 no
Mn2 4_434 O10 . C7 . 130.3(2) yes
Mn3 . O11 . C7 . 135.5(2) yes
O11 . C7 . O10 . 125.1(3) yes
O11 . C7 . C8 . 117.4(3) yes
O10 . C7 . C8 . 117.5(3) yes
C7 . C8 . H81 . 106.7 no
C7 . C8 . H82 . 108.5 no
H81 . C8 . H82 . 109.0 no
C7 . C8 . H83 . 110.0 no
H81 . C8 . H83 . 112.2 no
H82 . C8 . H83 . 110.3 no
Mn3 . O12 . H121 . 124.7 no
Mn3 . O12 . H122 . 120.0 no
H121 . O12 . H122 . 113.6 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C8 . H82 . O5 6_335 122.29(9) 0.944 2.581 3.186(7) yes
O12 . H122 . O6 8_354 154.58(10) 0.851 1.891 2.685(7) yes
_iucr_refine_instruction_details_constraints 
;
#
# Punched on 09/05/12 at 18:04:57
#
#LIST 12
BLOCK SCALE X'S, MN(1,U'S) UNTIL C(3)
CONT C(41,U[ISO]) UNTIL C(42)
CONT O(8,U'S) UNTIL O(12)
CONT ENANTIO
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE O ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
END
;
_iucr_refine_instruction_details_restraints 
;
#
# Punched on 09/05/12 at 18:04:57
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;