data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Andrea Cornia'
'Daniele Bonacchi'
'Andrea Caneschi'
'Guillaume Chastanet'
'Antonio C. Febretti'
'Dante Gatteschi'
'Mirko Pacchioni'
'Roberta Sessoli'
'Laura Zobbi'

_publ_contact_author_name        'Dr Andrea Cornia'
_publ_contact_author_address     
;
Department of Chemistry
INSTM and University of Modena and Reggio Emilia
via G. Campi 183
Modena
41100
ITALY
;

_publ_contact_author_email       ACORNIA@UNIMORE.IT

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Site-specific ligation of
anthracene-1,8-dicarboxylates to Mn12 core: a route to the controlled
functionalisation of Single-Molecule Magnets
;

data_mn12adc
_database_code_depnum_ccdc_archive 'CCDC 246075'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C156 H112 Mn12 O52 S4,8(C H2 Cl2)'
_chemical_formula_sum            'C164 H128 Cl16 Mn12 O52 S4'
_chemical_formula_weight         4285.38

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'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 '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 41/amd'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_Int_Tables_number      141

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'-y+1/4, -x+1/4, -z+3/4'
'y+1/4, x+3/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-y+3/4, -x+3/4, -z+5/4'
'y+3/4, x+5/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'y-1/4, x-1/4, z-3/4'
'-y-1/4, -x-3/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/4, x+1/4, z-1/4'
'-y+1/4, -x-1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   26.2604(12)
_cell_length_b                   26.2604(12)
_cell_length_c                   27.4733(13)
_cell_angle_alpha                90.0000(18)
_cell_angle_beta                 90.0000(17)
_cell_angle_gamma                90.0000(17)
_cell_volume                     18945.8(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.30
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.70
_exptl_crystal_density_meas      1.52(4)
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    
;
flotation in aqueous NaBr, at room temperature;
the reported value was obtained from the experimental
room-temperature result 1.40(4) g/mL and the unit cell volume
at room temperature, 20569(6) Ang.3'
;
_exptl_crystal_F_000             8656
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
crystal removed from the mother liquid, immediately mounted
on a quartz fiber using vacuum grease and flash-cooled in the
nitrogen stream
;

_diffrn_ambient_temperature      100(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 AXS SMART 2000'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            68467
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         23.67
_reflns_number_total             3758
_reflns_number_gt                3047
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART CCD Software'
_computing_cell_refinement       'Bruker SMART CCD Software'
_computing_data_reduction        'Bruker SMART CCD Software'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
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.
The crystal, although apparently well-developed, are exceedingly weak X-ray
diffractors and the investigation required the use of large crystals.
The diffraction pattern exhibits clear 4/mmm symmetry and systematic
absences consistent with space-group I41/amd (hhl, 2h + l <> 4n;
hk0, h and k <> 2n). The same results were obtained on different crystals
from the same batch and from different preparations, as well as using
a Siemens P4/RA diffractometer equipped with a point-detector.
The Mn12 clusters, which have no intrinsic mirror symmetry, develop around
D2d-symmetry sites and are consequently heavily disordered.
The L2- ligands were thus refined with half occupancy.
All non-hydrogen atoms were treated anisotropically, with the exception
of those belonging to the PhCH2SCOCH3 moiety and to the dichloromethane
solvent molecule. All the hydrogen atoms were added in idealized positions,
with the exception of those belonging to the coordinated H2O molecules, which
were neglected.
Restraints were applied to the geometry and atomic displacement parameters
of the L2- ligand. In particular, the heavily-disordered CH2SC(O)CH3 moiety
was constrained to have the same geometry found in a crystallographically-
characterized thioacetyl derivative, ethanedithiol diacetate, at 183 K
(H. Fleischer and D. Schollmeyer, Acta Cryst., 2001, E57, o330).
Residual electron density peaks on mirror planes suggest additional disorder
due to a small fraction of L2- ligand displaying bridging Mode II.
No improvement in structure refinement was obtained by assuming
a different space-group and/or twinning effects.
;

_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^)+(0.1792P)^2^+197.7636P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3758
_refine_ls_number_parameters     351
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.1136
_refine_ls_wR_factor_ref         0.3464
_refine_ls_wR_factor_gt          0.3157
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.002
_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 0.5000 0.08911(6) 0.08523(7) 0.0487(6) Uani 1 2 d S . .
Mn2 Mn 0.5000 0.19451(6) 0.08967(6) 0.0430(6) Uani 1 2 d S . .
Mn3 Mn 0.38867(5) 0.13867(5) 0.1250 0.0774(9) Uani 1 2 d S . .
O1 O 0.5000 0.0679(3) 0.1622(3) 0.057(2) Uani 1 2 d S . .
O2 O 0.6398(3) 0.2500 0.2433(3) 0.060(2) Uani 1 2 d S . .
O3 O 0.5561(3) 0.2500 0.2298(3) 0.055(2) Uani 1 2 d S . .
O4 O 0.5000 0.2028(2) 0.1583(2) 0.0381(16) Uani 1 2 d S . .
O5 O 0.4487(2) 0.0376(2) 0.0728(2) 0.0553(15) Uani 1 1 d . . .
O6 O 0.45219(17) 0.14219(18) 0.0936(2) 0.0440(13) Uani 1 1 d . . .
O7 O 0.3739(6) 0.0797(6) 0.0809(6) 0.057(4) Uani 0.50 1 d P . .
O8 O 0.6197(6) 0.0662(6) 0.1084(6) 0.061(4) Uani 0.50 1 d P . .
O9 O 0.5691(5) 0.1037(5) 0.1933(5) 0.058(3) Uani 0.50 1 d P . .
O10 O 0.4038(6) 0.0925(5) 0.1788(6) 0.069(4) Uani 0.50 1 d P . .
C1 C 0.4020(4) 0.0370(4) 0.0778(4) 0.069(3) Uani 1 1 d . . .
C2 C 0.3742(4) -0.0096(4) 0.0645(5) 0.080(3) Uani 1 1 d . . .
C3 C 0.3991(4) -0.0506(3) 0.0448(4) 0.070(3) Uani 1 1 d . . .
H3 H 0.4350 -0.0495 0.0401 0.083 Uiso 1 1 calc R . .
C4 C 0.3717(4) -0.0935(4) 0.0317(5) 0.088(3) Uani 1 1 d . . .
H4 H 0.3887 -0.1214 0.0169 0.105 Uiso 1 1 calc R . .
C5 C 0.3214(5) -0.0960(5) 0.0396(7) 0.127(6) Uani 1 1 d . . .
H5 H 0.3037 -0.1268 0.0331 0.152 Uiso 1 1 calc R . .
C6 C 0.2944(5) -0.0539(6) 0.0575(8) 0.158(9) Uani 1 1 d . . .
H6 H 0.2584 -0.0548 0.0608 0.189 Uiso 1 1 calc R . .
C7 C 0.3217(5) -0.0112(5) 0.0701(7) 0.132(6) Uani 1 1 d . . .
H7 H 0.3044 0.0176 0.0828 0.158 Uiso 1 1 calc R . .
C8 C 0.5941(5) 0.2500 0.2575(5) 0.059(3) Uani 1 2 d S . .
C9 C 0.5279(7) 0.0825(7) 0.1986(6) 0.066(5) Uani 0.50 1 d PD . .
C10 C 0.5041(8) 0.0717(6) 0.2477(6) 0.081(6) Uani 0.50 1 d PD . .
C11 C 0.4834(7) 0.0278(7) 0.2575(9) 0.100(11) Uani 0.50 1 d PD . .
H11 H 0.4770 0.0043 0.2320 0.120 Uiso 0.50 1 calc PR . .
C12 C 0.4703(8) 0.0150(11) 0.3062(10) 0.120(11) Uani 0.50 1 d PD . .
H12 H 0.4553 -0.0174 0.3120 0.144 Uiso 0.50 1 calc PR . .
C13 C 0.4781(6) 0.0462(9) 0.3450(9) 0.114(11) Uani 0.50 1 d PD . .
H13 H 0.4689 0.0363 0.3770 0.136 Uiso 0.50 1 calc PR . .
C14 C 0.5000 0.0932(7) 0.3357(7) 0.095(5) Uani 1 2 d SD . .
C15 C 0.5144(5) 0.1084(7) 0.2867(7) 0.076(6) Uani 0.50 1 d PD . .
C16 C 0.5166(9) 0.1242(7) 0.3738(11) 0.14(2) Uani 0.50 1 d PD . .
C17 C 0.5412(12) 0.1709(11) 0.3673(9) 0.122(10) Uani 0.50 1 d PD . .
C18 C 0.5509(9) 0.1871(9) 0.3176(8) 0.093(7) Uani 0.50 1 d PD . .
C19 C 0.5361(8) 0.1554(6) 0.2807(10) 0.089(7) Uani 0.50 1 d PD . .
H19 H 0.5413 0.1668 0.2483 0.107 Uiso 0.50 1 calc PR . .
C20 C 0.5572(16) 0.2058(12) 0.4019(14) 0.206(15) Uani 0.50 1 d PDU . .
H20 H 0.5487 0.1978 0.4346 0.247 Uiso 0.50 1 calc PR . .
C21 C 0.5834(14) 0.2500 0.3954(9) 0.182(11) Uani 1 2 d SDU . .
H21 H 0.5937 0.2715 0.4214 0.219 Uiso 0.50 1 calc PR . .
C22 C 0.5937(12) 0.2606(8) 0.3457(9) 0.165(13) Uani 0.50 1 d PDU . .
H22 H 0.6109 0.2917 0.3390 0.198 Uiso 0.50 1 calc PR . .
C23 C 0.5822(9) 0.2325(8) 0.3083(8) 0.095(9) Uani 0.50 1 d PD . .
C24 C 0.5000 0.1069(7) 0.4252(10) 0.171(11) Uiso 1 2 d SD . .
C25 C 0.5375(9) 0.0815(14) 0.4518(13) 0.35(3) Uiso 0.50 1 d PDU . .
H25 H 0.5706 0.0762 0.4386 0.416 Uiso 0.50 1 calc PR . .
C26 C 0.5251(13) 0.0642(14) 0.4981(13) 0.31(2) Uiso 0.50 1 d PDU . .
H26 H 0.5504 0.0468 0.5165 0.366 Uiso 0.50 1 calc PR . .
C27 C 0.4770(13) 0.0713(10) 0.5185(12) 0.30(2) Uiso 0.50 1 d PDU . .
C28 C 0.4398(12) 0.0966(16) 0.4918(12) 0.31(3) Uiso 0.50 1 d PDU . .
H28 H 0.4068 0.1018 0.5051 0.375 Uiso 0.50 1 calc PR . .
C29 C 0.4517(7) 0.1142(15) 0.4453(12) 0.29(3) Uiso 0.50 1 d PDU . .
H29 H 0.4265 0.1315 0.4270 0.350 Uiso 0.50 1 calc PR . .
C30 C 0.4668(16) 0.0520(14) 0.5692(13) 0.32(3) Uiso 0.50 1 d PGDU . .
H30A H 0.4829 0.0757 0.5927 0.482 Uiso 0.50 1 calc PR . .
H30B H 0.4836 0.0185 0.5729 0.482 Uiso 0.50 1 calc PR . .
S1 S 0.4006(17) 0.0451(19) 0.5854(17) 0.71(4) Uiso 0.50 1 d PGD . .
C31 C 0.396(2) 0.089(2) 0.634(2) 0.71(4) Uiso 0.50 1 d PG . .
C32 C 0.344(2) 0.091(3) 0.657(3) 0.71(4) Uiso 0.50 1 d PG . .
H32A H 0.3216 0.0673 0.6400 1.072 Uiso 0.50 1 calc PR . .
H32B H 0.3307 0.1259 0.6535 1.072 Uiso 0.50 1 calc PR . .
H32C H 0.3465 0.0822 0.6912 1.072 Uiso 0.50 1 calc PR . .
O11 O 0.432(3) 0.114(3) 0.648(3) 0.71(4) Uiso 0.50 1 d PG . .
Cl1 Cl 0.2007(6) 0.3378(10) 0.0622(6) 0.437(12) Uani 1 1 d . . .
Cl2 Cl 0.1806(11) 0.4500(11) 0.0466(8) 0.59(2) Uani 1 1 d . . .
C33A C 0.223(2) 0.405(2) 0.058(2) 0.20(2) Uiso 0.50 1 d P . .
H33A H 0.2395 0.4134 0.0895 0.297 Uiso 0.50 1 calc PR . .
H33B H 0.2492 0.4066 0.0327 0.297 Uiso 0.50 1 calc PR . .
C33B C 0.1626(17) 0.3897(16) 0.0780(15) 0.151(13) Uiso 0.50 1 d P . .
H33C H 0.1648 0.3950 0.1136 0.227 Uiso 0.50 1 calc PR . .
H33D H 0.1267 0.3816 0.0701 0.227 Uiso 0.50 1 calc PR . .

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 0.0334(9) 0.0354(9) 0.0773(13) -0.0091(8) 0.000 0.000
Mn2 0.0292(9) 0.0328(9) 0.0670(12) -0.0047(7) 0.000 0.000
Mn3 0.0458(8) 0.0458(8) 0.141(2) -0.0361(9) 0.0361(9) -0.0172(8)
O1 0.048(4) 0.038(4) 0.085(6) -0.004(4) 0.000 0.000
O2 0.056(5) 0.042(4) 0.083(6) 0.000 -0.022(4) 0.000
O3 0.051(5) 0.039(4) 0.075(5) 0.000 0.002(4) 0.000
O4 0.031(3) 0.023(3) 0.060(4) -0.001(3) 0.000 0.000
O5 0.044(3) 0.040(3) 0.082(4) -0.015(3) 0.001(3) -0.005(2)
O6 0.025(2) 0.037(3) 0.070(3) -0.004(2) 0.003(2) -0.0032(19)
O7 0.049(7) 0.055(9) 0.067(9) -0.021(7) 0.021(7) -0.010(6)
O8 0.050(8) 0.048(8) 0.086(11) -0.014(8) -0.026(8) 0.020(6)
O9 0.039(8) 0.063(8) 0.072(8) 0.001(6) -0.005(6) -0.008(7)
O10 0.056(9) 0.054(8) 0.098(11) 0.014(7) 0.013(8) 0.018(7)
C1 0.052(5) 0.060(6) 0.096(7) -0.031(5) 0.021(5) -0.015(5)
C2 0.048(5) 0.059(6) 0.134(9) -0.035(6) 0.016(6) -0.014(4)
C3 0.062(6) 0.050(5) 0.097(7) -0.021(5) -0.008(5) -0.008(4)
C4 0.079(7) 0.050(5) 0.134(10) -0.037(6) -0.006(7) -0.010(5)
C5 0.090(9) 0.079(8) 0.212(17) -0.051(10) 0.021(10) -0.047(7)
C6 0.070(8) 0.115(11) 0.29(2) -0.104(14) 0.047(11) -0.048(8)
C7 0.073(8) 0.093(9) 0.229(17) -0.092(11) 0.041(9) -0.033(7)
C8 0.053(8) 0.047(6) 0.076(8) 0.000 -0.008(6) 0.000
C9 0.056(11) 0.042(9) 0.098(15) 0.006(9) -0.018(10) -0.009(9)
C10 0.096(15) 0.056(9) 0.092(11) 0.015(8) -0.03(3) -0.01(2)
C11 0.13(3) 0.066(12) 0.101(15) 0.022(11) -0.007(14) -0.028(13)
C12 0.087(17) 0.093(19) 0.18(3) 0.06(2) -0.015(18) 0.007(14)
C13 0.15(3) 0.112(19) 0.080(15) 0.016(14) -0.011(14) -0.055(18)
C14 0.090(12) 0.100(13) 0.097(13) -0.007(11) 0.000 0.000
C15 0.050(15) 0.069(11) 0.107(14) 0.013(11) 0.001(9) -0.005(8)
C16 0.19(6) 0.12(2) 0.12(2) 0.045(18) 0.01(2) 0.00(2)
C17 0.15(3) 0.10(2) 0.11(2) -0.006(18) 0.028(19) -0.02(2)
C18 0.091(17) 0.093(18) 0.095(17) -0.002(14) -0.038(14) 0.004(13)
C19 0.072(14) 0.073(14) 0.123(19) 0.004(13) 0.011(13) -0.005(11)
C20 0.33(4) 0.14(2) 0.15(2) -0.02(2) 0.06(3) 0.01(2)
C21 0.34(3) 0.076(13) 0.131(16) 0.000 0.068(19) 0.000
C22 0.34(4) 0.05(2) 0.106(16) 0.006(12) 0.04(2) -0.041(18)
C23 0.113(18) 0.10(2) 0.074(13) -0.009(11) 0.004(12) 0.019(14)
Cl1 0.327(16) 0.64(3) 0.342(17) -0.202(19) -0.062(13) 0.20(2)
Cl2 0.63(4) 0.63(4) 0.50(3) 0.28(3) -0.10(3) -0.27(3)

_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 O6 1.890(5) 19_655 ?
Mn1 O6 1.890(5) . ?
Mn1 O5 1.939(5) . ?
Mn1 O5 1.939(5) 19_655 ?
Mn1 O1 2.188(9) . ?
Mn1 O2 2.228(9) 13_554 ?
Mn1 Mn2 2.770(2) . ?
Mn2 O6 1.864(5) . ?
Mn2 O6 1.864(5) 19_655 ?
Mn2 O4 1.898(7) . ?
Mn2 O3 1.909(9) 13_554 ?
Mn2 O4 1.914(4) 13_554 ?
Mn2 O4 1.914(4) 6_545 ?
Mn2 Mn2 2.831(3) 13_554 ?
Mn2 Mn2 2.831(3) 6_545 ?
Mn2 Mn2 2.915(3) 2_655 ?
Mn3 O6 1.880(5) . ?
Mn3 O6 1.880(5) 6_545 ?
Mn3 O10 1.953(15) . ?
Mn3 O10 1.953(15) 6_545 ?
Mn3 O8 1.970(14) 32_565 ?
Mn3 O8 1.970(14) 19_655 ?
Mn3 O7 2.004(14) . ?
Mn3 O7 2.004(14) 6_545 ?
Mn3 O9 2.364(14) 19_655 ?
Mn3 O9 2.364(14) 32_565 ?
O1 C9 1.296(19) 19_655 ?
O1 C9 1.296(19) . ?
O2 C8 1.261(15) . ?
O2 Mn1 2.228(9) 13_554 ?
O3 C8 1.256(14) . ?
O3 Mn2 1.909(9) 13_554 ?
O4 Mn2 1.914(4) 6_545 ?
O4 Mn2 1.914(4) 13_554 ?
O5 C1 1.236(10) . ?
O7 O8 0.853(16) 19_655 ?
O7 C1 1.346(18) . ?
O8 O7 0.853(16) 19_655 ?
O8 C1 1.271(17) 19_655 ?
O8 Mn3 1.970(14) 19_655 ?
O9 O10 0.865(16) 19_655 ?
O9 C9 1.23(2) . ?
O9 Mn3 2.364(14) 19_655 ?
O10 O9 0.865(16) 19_655 ?
O10 C9 1.89(2) 19_655 ?
C1 O8 1.271(17) 19_655 ?
C1 C2 1.471(13) . ?
C2 C3 1.370(13) . ?
C2 C7 1.388(16) . ?
C3 C4 1.386(13) . ?
C4 C5 1.341(17) . ?
C5 C6 1.402(19) . ?
C6 C7 1.375(16) . ?
C8 C23 1.50(3) . ?
C9 C10 1.512(10) . ?
C10 C11 1.30(2) . ?
C10 C15 1.47(2) . ?
C11 C12 1.42(3) . ?
C12 C13 1.36(3) . ?
C13 C14 1.38(3) . ?
C14 C16 1.40(2) . ?
C14 C15 1.45(2) . ?
C15 C19 1.369(19) . ?
C16 C17 1.40(2) . ?
C16 C24 1.55(4) . ?
C17 C20 1.38(3) . ?
C17 C18 1.45(2) . ?
C18 C19 1.370(19) . ?
C18 C23 1.47(2) . ?
C20 C21 1.36(3) . ?
C21 C22 1.42(3) . ?
C22 C23 1.30(2) . ?
C24 C25 1.396(10) . ?
C24 C29 1.396(10) . ?
C25 C26 1.390(10) . ?
C26 C27 1.395(10) . ?
C27 C28 1.390(10) . ?
C27 C30 1.508(10) . ?
C28 C29 1.393(10) . ?
C30 S1 1.8053 . ?
S1 C31 1.7719 . ?
C31 O11 1.2079 . ?
C31 C32 1.4944 . ?
Cl1 C33B 1.75(4) . ?
Cl1 C33A 1.86(6) . ?
Cl2 C33A 1.65(6) . ?
Cl2 C33B 1.86(4) . ?

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
O6 Mn1 O6 83.3(3) 19_655 . ?
O6 Mn1 O5 175.8(3) 19_655 . ?
O6 Mn1 O5 94.3(2) . . ?
O6 Mn1 O5 94.3(2) 19_655 19_655 ?
O6 Mn1 O5 175.8(3) . 19_655 ?
O5 Mn1 O5 87.9(3) . 19_655 ?
O6 Mn1 O1 94.0(2) 19_655 . ?
O6 Mn1 O1 94.0(2) . . ?
O5 Mn1 O1 89.6(2) . . ?
O5 Mn1 O1 89.6(2) 19_655 . ?
O6 Mn1 O2 86.3(2) 19_655 13_554 ?
O6 Mn1 O2 86.3(2) . 13_554 ?
O5 Mn1 O2 90.1(2) . 13_554 ?
O5 Mn1 O2 90.1(2) 19_655 13_554 ?
O1 Mn1 O2 179.6(3) . 13_554 ?
O6 Mn2 O6 84.7(3) . 19_655 ?
O6 Mn2 O4 91.5(2) . . ?
O6 Mn2 O4 91.5(2) 19_655 . ?
O6 Mn2 O3 93.0(2) . 13_554 ?
O6 Mn2 O3 93.0(2) 19_655 13_554 ?
O4 Mn2 O3 173.9(3) . 13_554 ?
O6 Mn2 O4 174.6(3) . 13_554 ?
O6 Mn2 O4 97.1(2) 19_655 13_554 ?
O4 Mn2 O4 83.3(3) . 13_554 ?
O3 Mn2 O4 92.0(3) 13_554 13_554 ?
O6 Mn2 O4 97.1(2) . 6_545 ?
O6 Mn2 O4 174.6(3) 19_655 6_545 ?
O4 Mn2 O4 83.3(3) . 6_545 ?
O3 Mn2 O4 92.0(3) 13_554 6_545 ?
O4 Mn2 O4 80.7(3) 13_554 6_545 ?
Mn1 Mn2 Mn2 122.98(7) . 13_554 ?
Mn1 Mn2 Mn2 122.98(7) . 6_545 ?
Mn2 Mn2 Mn2 61.96(7) 13_554 6_545 ?
Mn1 Mn2 Mn2 177.48(5) . 2_655 ?
Mn2 Mn2 Mn2 59.02(3) 13_554 2_655 ?
Mn2 Mn2 Mn2 59.02(3) 6_545 2_655 ?
O6 Mn3 O6 97.1(3) . 6_545 ?
O6 Mn3 O10 101.4(5) . . ?
O6 Mn3 O10 101.1(5) 6_545 . ?
O6 Mn3 O10 101.1(5) . 6_545 ?
O6 Mn3 O10 101.4(5) 6_545 6_545 ?
O10 Mn3 O10 145.7(11) . 6_545 ?
O6 Mn3 O8 165.7(5) . 32_565 ?
O6 Mn3 O8 92.3(4) 6_545 32_565 ?
O10 Mn3 O8 87.3(7) . 32_565 ?
O10 Mn3 O8 66.3(7) 6_545 32_565 ?
O6 Mn3 O8 92.3(4) . 19_655 ?
O6 Mn3 O8 165.7(5) 6_545 19_655 ?
O10 Mn3 O8 66.3(7) . 19_655 ?
O10 Mn3 O8 87.3(7) 6_545 19_655 ?
O8 Mn3 O8 80.7(8) 32_565 19_655 ?
O6 Mn3 O7 86.1(4) . . ?
O6 Mn3 O7 166.5(5) 6_545 . ?
O10 Mn3 O7 91.1(7) . . ?
O10 Mn3 O7 65.1(7) 6_545 . ?
O8 Mn3 O7 82.3(5) 32_565 . ?
O8 Mn3 O7 24.8(5) 19_655 . ?
O6 Mn3 O7 166.5(5) . 6_545 ?
O6 Mn3 O7 86.1(4) 6_545 6_545 ?
O10 Mn3 O7 65.1(7) . 6_545 ?
O10 Mn3 O7 91.1(7) 6_545 6_545 ?
O8 Mn3 O7 24.8(5) 32_565 6_545 ?
O8 Mn3 O7 82.3(5) 19_655 6_545 ?
O7 Mn3 O7 93.8(8) . 6_545 ?
O6 Mn3 O9 88.1(4) . 19_655 ?
O6 Mn3 O9 87.6(4) 6_545 19_655 ?
O10 Mn3 O9 20.4(5) . 19_655 ?
O10 Mn3 O9 166.1(8) 6_545 19_655 ?
O8 Mn3 O9 103.1(6) 32_565 19_655 ?
O8 Mn3 O9 82.0(7) 19_655 19_655 ?
O7 Mn3 O9 105.7(6) . 19_655 ?
O7 Mn3 O9 78.9(6) 6_545 19_655 ?
O6 Mn3 O9 87.6(4) . 32_565 ?
O6 Mn3 O9 88.1(4) 6_545 32_565 ?
O10 Mn3 O9 166.1(8) . 32_565 ?
O10 Mn3 O9 20.4(5) 6_545 32_565 ?
O8 Mn3 O9 82.0(7) 32_565 32_565 ?
O8 Mn3 O9 103.1(6) 19_655 32_565 ?
O7 Mn3 O9 78.9(6) . 32_565 ?
O7 Mn3 O9 105.7(6) 6_545 32_565 ?
O9 Mn3 O9 173.5(7) 19_655 32_565 ?
C9 O1 Mn1 132.1(8) . . ?
C8 O2 Mn1 122.3(8) . 13_554 ?
C8 O3 Mn2 127.7(8) . 13_554 ?
Mn2 O4 Mn2 95.9(3) . 6_545 ?
Mn2 O4 Mn2 95.9(3) . 13_554 ?
Mn2 O4 Mn2 99.2(3) 6_545 13_554 ?
C1 O5 Mn1 132.7(6) . . ?
Mn2 O6 Mn3 131.3(3) . . ?
Mn2 O6 Mn1 95.1(2) . . ?
Mn3 O6 Mn1 127.5(3) . . ?
C1 O7 Mn3 125.1(11) . . ?
C1 O8 Mn3 133.3(10) 19_655 19_655 ?
C9 O9 Mn3 133.2(12) . 19_655 ?
C9 O10 Mn3 119.8(9) 19_655 . ?
O5 C1 O8 120.7(10) . 19_655 ?
O5 C1 O7 122.8(10) . . ?
O5 C1 C2 118.3(8) . . ?
O7 C1 C2 116.0(10) . . ?
C3 C2 C7 119.7(9) . . ?
C3 C2 C1 121.0(8) . . ?
C7 C2 C1 119.3(9) . . ?
C2 C3 C4 119.5(10) . . ?
C5 C4 C3 120.7(10) . . ?
C4 C5 C6 121.0(10) . . ?
C7 C6 C5 117.9(12) . . ?
C6 C7 C2 120.9(12) . . ?
O3 C8 O2 124.8(12) . . ?
O3 C8 C23 113.3(13) . . ?
O2 C8 C23 119.0(13) . . ?
O9 C9 O1 122.7(15) . . ?
O9 C9 C10 123.8(17) . . ?
O1 C9 C10 113.5(14) . . ?
C11 C10 C15 120.3(18) . . ?
C11 C10 C9 121.5(17) . . ?
C15 C10 C9 117.0(16) . . ?
C10 C11 C12 120(2) . . ?
C13 C12 C11 124(3) . . ?
C12 C13 C14 117(2) . . ?
C13 C14 C16 121(2) . . ?
C13 C14 C15 121.5(19) . . ?
C16 C14 C15 116.9(17) . . ?
C19 C15 C14 117.9(18) . . ?
C19 C15 C10 125.4(19) . . ?
C14 C15 C10 116.7(16) . . ?
C17 C16 C14 124(3) . . ?
C17 C16 C24 120.3(17) . . ?
C14 C16 C24 115.1(15) . . ?
C20 C17 C16 129(3) . . ?
C20 C17 C18 113(3) . . ?
C16 C17 C18 117(2) . . ?
C19 C18 C17 118(2) . . ?
C19 C18 C23 122(2) . . ?
C17 C18 C23 120(2) . . ?
C15 C19 C18 125(3) . . ?
C21 C20 C17 129(4) . . ?
C20 C21 C22 113(3) . . ?
C23 C22 C21 127(2) . . ?
C22 C23 C18 117(2) . . ?
C22 C23 C8 121(2) . . ?
C18 C23 C8 121.8(18) . . ?
C25 C24 C29 120(2) . . ?
C25 C24 C16 114.7(15) . . ?
C29 C24 C16 125.3(17) . . ?
C26 C25 C24 118(2) . . ?
C25 C26 C27 122(2) . . ?
C28 C27 C26 119(2) . . ?
C28 C27 C30 121.5(14) . . ?
C26 C27 C30 119.2(14) . . ?
C27 C28 C29 119(2) . . ?
C28 C29 C24 121(2) . . ?
C27 C30 S1 115.7(13) . . ?
C31 S1 C30 100.7 . . ?
O11 C31 C32 124.0 . . ?
O11 C31 S1 122.4 . . ?
C32 C31 S1 113.6 . . ?
C33B Cl1 C33A 57(2) . . ?
C33A Cl2 C33B 58(2) . . ?
Cl2 C33A Cl1 119(4) . . ?
Cl1 C33B Cl2 114(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.67
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.150