# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_coden_Cambridge         1350

_publ_requested_journal          CrystEngComm
loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
'Giannis Papaefstathiou'
;
? # Address for author 1
;
;
? # Footnote for author 1
;
'Euan Brechin'
;
? # Address 2
;
;
? # Footnote 2
;
'Anna Collins' '' ''
'Ross Inglis' '' ''
'Athanasios D. Katsenis' '' ''
'Constantinos Milios' '' ''
'Fraser White' '' ''

_publ_contact_author_name        'Giannis Papaefstathiou'
_publ_contact_author_address     
;
Department of Chemistry
Laboratory of Inorganic Chemistry
National and Kapodistrian Universit
Panepistimiopolis
Zografou
15771
GREECE
;

_publ_contact_author_email       GSPAPAEF@CHEM.UOA.GR

_publ_section_title              
;Assembling molecular triangles into discrete and
infinite architectures
;

_publ_contact_author_phone       '+44 131 650 4806'

_publ_contact_letter             
;
;

# Attachment '(2).cif'

data_EB8039
_database_code_depnum_ccdc_archive 'CCDC 696166'

_audit_creation_date             08-03-10
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title 'eb8039 in P-3c1'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H30 Cl1 Mn3 N6 O11, 4(C H4 O)'
_chemical_compound_source        CMs8
_exptl_crystal_recrystallization_method 
;
Slow evaporation of MeOH/CH~2~Cl~2~ solution.
;

_cell_length_a                   15.6887(3)
_cell_length_b                   15.6887(3)
_cell_length_c                   22.2702(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4747.1(2)

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P -3 c 1 '
_symmetry_space_group_name_Hall  '-P 3 2"c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y,x-y,z
y,-x+y,-z
-x+y,-x,z
x-y,x,-z
-x+y,y,z+1/2
x-y,-y,-z+1/2
x,x-y,z+1/2
-x,-x+y,-z+1/2
-y,-x,z+1/2
y,x,-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'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 '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'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 '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            4

# Given Formula = C42 H42 Cl1.00 Mn3 N6 O14
# Dc = 1.48 Fooo = 1944.00 Mu = 9.12 M = 351.69
# Found Formula = C39 H30 Cl1 Mn3 N6 O11
# Dc = 1.34 FOOO = 1944.00 Mu = 9.00 M = 319.65

_chemical_formula_sum            'C42 H42 Cl1 Mn3 N6 O14'
_chemical_formula_weight         1055.07

_cell_measurement_reflns_used    4984
_cell_measurement_theta_min      2
_cell_measurement_theta_max      26
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_min          0.19
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.48
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    0.912

# Sheldrick geometric approximatio 0.81 0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.84
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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      150
_diffrn_reflns_number            21939
_reflns_number_total             4188
_diffrn_reflns_av_R_equivalents  0.075
# Number of reflections with Friedels Law is 4188
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 4386

_diffrn_reflns_theta_min         2.365
_diffrn_reflns_theta_max         29.443
_diffrn_measured_fraction_theta_max 0.951

_diffrn_reflns_theta_full        28.266
_diffrn_measured_fraction_theta_full 0.996

_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       29
_reflns_limit_h_min              -18
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              29

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.95
_refine_diff_density_max         0.99

# 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>-10.0\s(I)
_refine_ls_number_reflns         4173
_refine_ls_number_restraints     0
_refine_ls_number_parameters     181
_oxford_refine_ls_R_factor_ref   0.1095
_refine_ls_wR_factor_ref         0.1807
_refine_ls_goodness_of_fit_ref   0.7718
_refine_ls_shift/su_max          0.000525

# The values computed from all data
_oxford_reflns_number_all        4173
_refine_ls_R_factor_all          0.1095
_refine_ls_wR_factor_all         0.1807

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                2569
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_gt          0.1370

# 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 .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed

# WARNING. The IUCr will not accept Unit Weights
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method= Quasi-Unit weights
W = 1.0 or 1./2F
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Siemens Industrial Automation, Inc (1993).
SMART: Area-Detector Software Package; Madison, WI.

Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Mn1 Mn 0.65454(5) 0.44607(5) 0.46730(3) 0.0242 1.0000 Uani . . . . . . .
O2 O 0.6667 0.3333 0.4809(2) 0.0235 1.0000 Uani S T . . . . .
O3 O 0.5152(3) 0.3702(3) 0.46918(17) 0.0331 1.0000 Uani . . . . . . .
N4 N 0.4715(3) 0.2713(3) 0.45941(19) 0.0285 1.0000 Uani . . . . . . .
C5 C 0.3788(4) 0.2281(5) 0.4488(3) 0.0423 1.0000 Uani . . . . . . .
C6 C 0.3174(4) 0.1251(5) 0.4370(3) 0.0486 1.0000 Uani . . . . . . .
C7 C 0.3544(4) 0.0608(4) 0.4335(3) 0.0368 1.0000 Uani . . . . . . .
O8 O 0.4482(3) 0.0894(3) 0.44114(17) 0.0343 1.0000 Uani . . . . . . .
C9 C 0.2897(5) -0.0385(5) 0.4193(3) 0.0530 1.0000 Uani . . . . . . .
C10 C 0.1915(6) -0.0716(6) 0.4106(5) 0.0802 1.0000 Uani . . . . . . .
C11 C 0.1539(6) -0.0091(7) 0.4154(6) 0.1086 1.0000 Uani . . . . . . .
C12 C 0.2162(6) 0.0877(6) 0.4271(6) 0.0970 1.0000 Uani . . . . . . .
N13 N 0.6548(3) 0.4895(3) 0.56485(19) 0.0291 1.0000 Uani . . . . . . .
C14 C 0.7025(4) 0.4817(4) 0.6117(2) 0.0348 1.0000 Uani . . . . . . .
C15 C 0.6865(5) 0.5019(4) 0.6702(3) 0.0383 1.0000 Uani . . . . . . .
C16 C 0.6197(4) 0.5333(4) 0.6816(2) 0.0326 1.0000 Uani . . . . . . .
C17 C 0.5706(4) 0.5419(4) 0.6316(2) 0.0365 1.0000 Uani . . . . . . .
C18 C 0.5896(4) 0.5194(4) 0.5761(2) 0.0360 1.0000 Uani . . . . . . .
C19 C 0.6019(4) 0.5547(4) 0.7433(2) 0.0370 1.0000 Uani . . . . . . .
Cl20 Cl 0.6667 0.3333 0.33521(9) 0.0331 1.0000 Uani S T . . . . .
O21 O 0.6407(3) 0.4033(3) 0.35753(17) 0.0461 1.0000 Uani . . . . . . .
O22 O 0.6667 0.3333 0.2710(3) 0.0543 1.0000 Uani S T . . . . .
H51 H 0.3493 0.2681 0.4495 0.0481 1.0000 Uiso R . . . . . .
H91 H 0.3130 -0.0840 0.4160 0.0543 1.0000 Uiso R . . . . . .
H101 H 0.1500 -0.1391 0.4008 0.0859 1.0000 Uiso R . . . . . .
H111 H 0.0877 -0.0322 0.4078 0.1362 1.0000 Uiso R . . . . . .
H121 H 0.1920 0.1306 0.4296 0.1190 1.0000 Uiso R . . . . . .
H141 H 0.7487 0.4606 0.6042 0.0376 1.0000 Uiso R . . . . . .
H151 H 0.7218 0.4947 0.7007 0.0450 1.0000 Uiso R . . . . . .
H171 H 0.5244 0.5607 0.6364 0.0463 1.0000 Uiso R . . . . . .
H181 H 0.5562 0.5251 0.5431 0.0441 1.0000 Uiso R . . . . . .
H191 H 0.6265 0.5346 0.7749 0.0454 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 0.0251(4) 0.0241(4) 0.0244(3) 0.0007(3) 0.0008(3) 0.0130(3)
O2 0.0241(18) 0.0241(18) 0.022(3) 0.0000 0.0000 0.0120(9)
O3 0.0240(18) 0.0290(19) 0.046(2) -0.0046(17) 0.0010(16) 0.0132(15)
N4 0.029(2) 0.024(2) 0.030(2) 0.0033(17) 0.0044(17) 0.0112(18)
C5 0.030(3) 0.037(3) 0.061(4) 0.005(3) 0.001(3) 0.017(3)
C6 0.025(3) 0.033(3) 0.077(5) 0.008(3) -0.006(3) 0.007(2)
C7 0.031(3) 0.036(3) 0.037(3) 0.006(2) 0.000(2) 0.013(2)
O8 0.0303(19) 0.030(2) 0.039(2) -0.0061(16) -0.0047(16) 0.0126(16)
C9 0.041(4) 0.033(3) 0.076(5) 0.000(3) -0.011(3) 0.012(3)
C10 0.037(4) 0.035(4) 0.151(9) -0.004(5) -0.022(5) 0.004(3)
C11 0.039(4) 0.049(5) 0.229(14) -0.010(7) -0.028(6) 0.015(4)
C12 0.032(4) 0.047(5) 0.210(12) -0.001(6) -0.011(6) 0.019(4)
N13 0.029(2) 0.027(2) 0.033(2) -0.0014(18) 0.0019(18) 0.0144(18)
C14 0.035(3) 0.040(3) 0.032(3) -0.003(2) 0.002(2) 0.022(3)
C15 0.045(3) 0.045(3) 0.037(3) 0.003(2) -0.005(2) 0.031(3)
C16 0.035(3) 0.038(3) 0.026(2) -0.001(2) -0.002(2) 0.019(2)
C17 0.041(3) 0.048(3) 0.034(3) -0.005(2) -0.003(2) 0.033(3)
C18 0.046(3) 0.043(3) 0.028(2) -0.006(2) -0.008(2) 0.029(3)
C19 0.047(3) 0.050(3) 0.024(2) 0.002(2) 0.002(2) 0.032(3)
Cl20 0.0390(7) 0.0390(7) 0.0212(9) 0.0000 0.0000 0.0195(4)
O21 0.063(3) 0.054(3) 0.0322(19) 0.0035(19) 0.0007(19) 0.037(2)
O22 0.068(3) 0.068(3) 0.026(3) 0.0000 0.0000 0.0341(17)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2095(2)
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 . N4 5_665 1.988(4) yes
Mn1 . O8 5_665 1.866(4) yes
Mn1 . Mn1 5_665 3.2407(13) yes
Mn1 . O2 . 1.8955(11) yes
Mn1 . O3 . 1.896(4) yes
Mn1 . N13 . 2.276(4) yes
Mn1 . O21 . 2.515(4) yes
O3 . N4 . 1.364(5) yes
N4 . C5 . 1.283(7) yes
C5 . C6 . 1.433(8) yes
C5 . H51 . 0.947 no
C6 . C7 . 1.395(9) yes
C6 . C12 . 1.408(9) yes
C7 . O8 . 1.317(7) yes
C7 . C9 . 1.406(8) yes
C9 . C10 . 1.372(10) yes
C9 . H91 . 0.953 no
C10 . C11 . 1.378(12) yes
C10 . H101 . 0.951 no
C11 . C12 . 1.358(12) yes
C11 . H111 . 0.928 no
C12 . H121 . 0.924 no
N13 . C14 . 1.324(7) yes
N13 . C18 . 1.346(7) yes
C14 . C15 . 1.392(7) yes
C14 . H141 . 0.951 no
C15 . C16 . 1.385(8) yes
C15 . H151 . 0.919 no
C16 . C17 . 1.398(7) yes
C16 . C19 . 1.475(7) yes
C17 . C18 . 1.358(7) yes
C17 . H171 . 0.915 no
C18 . H181 . 0.932 no
C19 . C19 12_556 1.317(11) yes
C19 . H191 . 0.930 no
Cl20 . O21 3_655 1.438(4) yes
Cl20 . O21 5_665 1.438(4) yes
Cl20 . O21 . 1.438(4) yes
Cl20 . O22 . 1.429(7) yes
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
N4 5_665 Mn1 . O8 5_665 89.77(18) yes
N4 5_665 Mn1 . Mn1 5_665 59.53(13) yes
O8 5_665 Mn1 . Mn1 5_665 146.04(13) yes
N4 5_665 Mn1 . O2 . 90.22(13) yes
O8 5_665 Mn1 . O2 . 171.0(2) yes
Mn1 5_665 Mn1 . O2 . 31.26(4) yes
N4 5_665 Mn1 . O3 . 175.91(18) yes
O8 5_665 Mn1 . O3 . 87.62(17) yes
Mn1 5_665 Mn1 . O3 . 122.10(11) yes
O2 . Mn1 . O3 . 91.87(12) yes
N4 5_665 Mn1 . N13 . 93.41(17) yes
O8 5_665 Mn1 . N13 . 90.93(16) yes
Mn1 5_665 Mn1 . N13 . 104.07(11) yes
O2 . Mn1 . N13 . 98.1(2) yes
O3 . Mn1 . N13 . 89.77(16) yes
N4 5_665 Mn1 . O21 . 90.32(16) yes
O8 5_665 Mn1 . O21 . 84.28(15) yes
Mn1 5_665 Mn1 . O21 . 81.95(10) yes
O2 . Mn1 . O21 . 86.71(19) yes
O3 . Mn1 . O21 . 86.30(16) yes
N13 . Mn1 . O21 . 173.93(15) yes
Mn1 3_655 O2 . Mn1 . 117.48(9) yes
Mn1 3_655 O2 . Mn1 5_665 117.48(9) yes
Mn1 . O2 . Mn1 5_665 117.48(9) yes
Mn1 . O3 . N4 . 118.5(3) yes
O3 . N4 . Mn1 3_655 117.9(3) yes
O3 . N4 . C5 . 115.0(4) yes
Mn1 3_655 N4 . C5 . 127.0(4) yes
N4 . C5 . C6 . 125.1(6) yes
N4 . C5 . H51 . 116.6 no
C6 . C5 . H51 . 118.3 no
C5 . C6 . C7 . 122.6(5) yes
C5 . C6 . C12 . 118.7(6) yes
C7 . C6 . C12 . 118.8(6) yes
C6 . C7 . O8 . 123.0(5) yes
C6 . C7 . C9 . 118.8(6) yes
O8 . C7 . C9 . 118.2(6) yes
C7 . O8 . Mn1 3_655 131.6(4) yes
C7 . C9 . C10 . 120.2(7) yes
C7 . C9 . H91 . 120.8 no
C10 . C9 . H91 . 119.0 no
C9 . C10 . C11 . 121.3(7) yes
C9 . C10 . H101 . 117.9 no
C11 . C10 . H101 . 120.8 no
C10 . C11 . C12 . 119.1(8) yes
C10 . C11 . H111 . 120.0 no
C12 . C11 . H111 . 120.8 no
C6 . C12 . C11 . 121.8(8) yes
C6 . C12 . H121 . 118.5 no
C11 . C12 . H121 . 119.8 no
Mn1 . N13 . C14 . 129.9(4) yes
Mn1 . N13 . C18 . 113.2(3) yes
C14 . N13 . C18 . 116.6(5) yes
N13 . C14 . C15 . 122.8(5) yes
N13 . C14 . H141 . 117.2 no
C15 . C14 . H141 . 120.0 no
C14 . C15 . C16 . 120.4(5) yes
C14 . C15 . H151 . 118.4 no
C16 . C15 . H151 . 121.2 no
C15 . C16 . C17 . 116.1(5) yes
C15 . C16 . C19 . 121.0(5) yes
C17 . C16 . C19 . 122.9(5) yes
C16 . C17 . C18 . 119.7(5) yes
C16 . C17 . H171 . 120.1 no
C18 . C17 . H171 . 120.1 no
C17 . C18 . N13 . 124.3(5) yes
C17 . C18 . H181 . 119.0 no
N13 . C18 . H181 . 116.7 no
C16 . C19 . C19 12_556 124.4(7) yes
C16 . C19 . H191 . 118.0 no
C19 12_556 C19 . H191 . 117.6 no
O21 3_655 Cl20 . O21 5_665 108.70(17) yes
O21 3_655 Cl20 . O21 . 108.70(17) yes
O21 5_665 Cl20 . O21 . 108.70(17) yes
O21 3_655 Cl20 . O22 . 110.23(17) yes
O21 5_665 Cl20 . O22 . 110.23(17) yes
O21 . Cl20 . O22 . 110.23(17) yes
Mn1 . O21 . Cl20 . 121.3(2) yes
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
C18 . H181 . O3 2_666 129 0.93 2.42 3.094(11) yes

# Attachment '(3).cif'

data_EB8139
_database_code_depnum_ccdc_archive 'CCDC 696167'

_audit_creation_date             08-07-17
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title 'eb7139 in P2(1)/n'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H94 Mn6 N10 O20'
_exptl_crystal_recrystallization_method 
;

;

_publ_section_figure_captions    
# Captions to figures - Start each caption on a new line after a blank line
;
Fig. 1.
The title compound with displacement ellipsoids drawn at the 50%
probability level. H atoms are shown as spheres of
arbitary radius.

;

_publ_section_exptl_refinement   
# Some potentially useful phrases are donated by Bill Clegg:
;

The 4,4'-bpe ligands are disordered over two positions. These
groups have been modelled using partial occupancy of multiple atomic
sites, with the occupancy fixed at 0.5 due to symmetry. The
positions of these atomic sites were refined, and these atoms
were refined isotropically. Disordered groups were numbered from
C101-112 with equivalent atoms C201-C212. The disordered nitrogen atoms
were numbered N40 and N41.

All other non-H atoms were refined anisotropically.
Thermal similarity restraints were applied to one of the Et-sao
ligands.

In the absence of significant anomalous scattering, Friedel pairs were
merged.

The H atoms were all located in a difference map, but those
attached to carbon atoms were repositioned geometrically.
The H atoms were initially refined with soft restraints on the
bond lengths and angles to regularise their geometry
(C---H in the range 0.93--0.98\%A) and
U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom),
after which the positions were refined with riding constraints.

Checkcif alerts
912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1027
919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 1

The data collection strategy used aimed to achieve a complete data set to
2\q = 53 deg. Some higher angle data were collected in the process, and
some of these have been included in the refinement.
Reflections were required to fall in the range:
0.01 >(sin(\q/\l))^2^ > 0.42.
The lower limit excludes reflections that may be prroly measured in the
vicinity of the beamstop, and the high angle limit excludes some of the
weak data above 2\q = 53 deg.

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 1.000 4969 4969 0
23.01 0.550 1.000 6595 6595 0
25.24 0.600 1.000 8575 8575 0
#----------------------------------------------------------- ACTA Min. Res. ---
27.51 0.650 1.000 10893 10889 4
29.84 0.700 0.942 13597 12804 793
30.02 0.704 0.926 13836 12809 1027

220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.67 Ratio
222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.11 Ratio

041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
The value of Z has been chacked and is 2, with each molecule located on an
inversion centre. The difference may arise between calculated and reported
values due to the use of Parts in refining the disordered 4,4'-bpe ligands.
The difference between calculated and reported formula strings arises
solely from the difference in calculated and reported Z.

061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.85

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay, changes in the volume of the crystal illuminated, etc.

301_ALERT_3_C Main Residue Disorder ......................... 15.00 Perc.
720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 20

See above for comment on disorder and labelling.

341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9
410_ALERT_2_C Short Intra H...H Contact H141 .. H172 .. 1.95 Ang.

No action.

860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 54
The following thermal similarity restraints were applied.

U(IJ)'S 0.0, 0.010000 = C(29) TO C(34)
U(IJ)'S 0.0, 0.010000 = C(33) TO C(34)
U(IJ)'S 0.0, 0.010000 = C(32) TO C(33)
U(IJ)'S 0.0, 0.010000 = C(29) TO C(30)
U(IJ)'S 0.0, 0.010000 = C(30) TO C(31)
U(IJ)'S 0.0, 0.010000 = C(10) TO C(11)
U(IJ)'S 0.0, 0.010000 = C(11) TO C(12)
U(IJ)'S 0.0, 0.010000 = C(13) TO C(14)
U(IJ)'S 0.0, 0.010000 = C(14) TO C(15)

;

_cell_length_a                   13.4841(4)
_cell_length_b                   18.4592(5)
_cell_length_c                   19.6489(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.358(2)
_cell_angle_gamma                90
_cell_volume                     4738.0(2)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

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'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 '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'
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'

_cell_formula_units_Z            2

# Given Formula = C96 H94 Mn6 N10 O20
# Dc = 1.43 Fooo = 2100.00 Mu = 8.50 M = 1018.71
# Found Formula = C96 H94 Mn6 N10 O20
# Dc = 1.43 FOOO = 2100.00 Mu = 8.50 M = 1018.71

_chemical_formula_sum            'C96 H94 Mn6 N10 O20'
_chemical_compound_source        ?
_chemical_formula_weight         2037.43

_cell_measurement_reflns_used    8667
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    0.850

# Sheldrick geometric approximatio 0.82 0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_T_max  0.84
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  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       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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      150
_diffrn_reflns_number            70341
_reflns_number_total             12809
_diffrn_reflns_av_R_equivalents  0.059
# Number of reflections with Friedels Law is 12809
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 10804

_diffrn_reflns_theta_min         1.537
_diffrn_reflns_theta_max         30.018
_diffrn_measured_fraction_theta_max 0.926

_diffrn_reflns_theta_full        28.217
_diffrn_measured_fraction_theta_full 0.998

_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -18
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   1.80
_oxford_diffrn_Wilson_scale      31.96

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.98
_refine_diff_density_max         1.88

# 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>-10.0\s(I)
_refine_ls_number_reflns         10756
_refine_ls_number_restraints     54
_refine_ls_number_parameters     583
_oxford_refine_ls_R_factor_ref   0.1119
_refine_ls_wR_factor_ref         0.1737
_refine_ls_goodness_of_fit_ref   0.9928
_refine_ls_shift/su_max          0.002588

# The values computed from all data
_oxford_reflns_number_all        10756
_refine_ls_R_factor_all          0.1119
_refine_ls_wR_factor_all         0.1737

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                7818
_refine_ls_R_factor_gt           0.0717
_refine_ls_wR_factor_gt          0.1528

# 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 .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.00P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Siemens Industrial Automation, Inc (1993).
SMART: Area-Detector Software Package; Madison, WI.

Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Mn1 Mn 0.55564(5) 0.20127(3) 0.86523(3) 0.0238 1.0000 Uani . . . . . . .
Mn2 Mn 0.63569(6) 0.27940(4) 0.73965(3) 0.0277 1.0000 Uani . . . . . . .
Mn3 Mn 0.71706(5) 0.33436(3) 0.89616(3) 0.0257 1.0000 Uani . . . . . . .
O2 O 0.6504(2) 0.26020(15) 0.83448(14) 0.0237 1.0000 Uani . . . . . . .
O4 O 0.7913(3) 0.36275(19) 0.83000(17) 0.0383 1.0000 Uani . . . . . . .
O7 O 0.5191(3) 0.21716(17) 0.71496(16) 0.0369 1.0000 Uani . . . . . . .
O12 O 0.4598(2) 0.14180(17) 0.89247(16) 0.0322 1.0000 Uani . . . . . . .
O17 O 0.5549(3) 0.37960(16) 0.72851(16) 0.0346 1.0000 Uani . . . . . . .
O19 O 0.5841(3) 0.41036(16) 0.84203(17) 0.0369 1.0000 Uani . . . . . . .
O26 O 0.6536(3) 0.2649(2) 0.65006(18) 0.0489 1.0000 Uani . . . . . . .
O31 O 0.7762(3) 0.40758(17) 0.95736(17) 0.0394 1.0000 Uani . . . . . . .
O36 O 0.6026(2) 0.23706(16) 0.95929(15) 0.0294 1.0000 Uani . . . . . . .
O49 O 0.4456(2) 0.30008(17) 0.84784(17) 0.0348 1.0000 Uani . . . . . . .
N1 N 0.4997(3) 0.17231(19) 0.76573(19) 0.0293 1.0000 Uani . . . . . . .
N2 N 0.7659(3) 0.3342(2) 0.7632(2) 0.0337 1.0000 Uani . . . . . . .
N3 N 0.6339(3) 0.30824(19) 0.96279(19) 0.0278 1.0000 Uani . . . . . . .
N4 N 0.8381(3) 0.2519(2) 0.9489(2) 0.0389 1.0000 Uani . . . . . . .
N5 N 0.6664(3) 0.1040(2) 0.8827(2) 0.0344 1.0000 Uani . . . . . . .
C1 C 0.4254(3) 0.0795(2) 0.8621(3) 0.0297 1.0000 Uani . . . . . . .
C2 C 0.4021(4) 0.0243(3) 0.9046(3) 0.0420 1.0000 Uani . . . . . . .
C3 C 0.3623(4) -0.0407(3) 0.8757(3) 0.0504 1.0000 Uani . . . . . . .
C4 C 0.3429(4) -0.0529(3) 0.8051(3) 0.0469 1.0000 Uani . . . . . . .
C5 C 0.3639(4) 0.0003(3) 0.7618(3) 0.0408 1.0000 Uani . . . . . . .
C6 C 0.4073(3) 0.0672(2) 0.7885(3) 0.0310 1.0000 Uani . . . . . . .
C7 C 0.4348(4) 0.1197(2) 0.7407(2) 0.0289 1.0000 Uani . . . . . . .
C8 C 0.3925(4) 0.1132(3) 0.6621(3) 0.0454 1.0000 Uani . . . . . . .
C9 C 0.4702(5) 0.0806(3) 0.6255(3) 0.0551 1.0000 Uani . . . . . . .
C10 C 0.7261(5) 0.2854(3) 0.6193(3) 0.0471 1.0000 Uani . U . . . . .
C11 C 0.7142(6) 0.2620(3) 0.5494(3) 0.0612 1.0000 Uani . U . . . . .
C12 C 0.7829(6) 0.2848(4) 0.5124(4) 0.0697 1.0000 Uani . U . . . . .
C13 C 0.8629(6) 0.3276(4) 0.5412(4) 0.0726 1.0000 Uani . U . . . . .
C14 C 0.8778(5) 0.3493(3) 0.6106(4) 0.0615 1.0000 Uani . U . . . . .
C15 C 0.8095(5) 0.3292(3) 0.6517(3) 0.0458 1.0000 Uani . U . . . . .
C16 C 0.8274(4) 0.3536(3) 0.7242(3) 0.0368 1.0000 Uani . . . . . . .
C17 C 0.9173(4) 0.4012(3) 0.7575(3) 0.0464 1.0000 Uani . . . . . . .
C18 C 1.0061(5) 0.3563(4) 0.8003(4) 0.0674 1.0000 Uani . . . . . . .
C19 C 0.7269(4) 0.4483(2) 0.9936(2) 0.0381 1.0000 Uani . . . . . . .
C20 C 0.7599(5) 0.5206(3) 1.0067(3) 0.0548 1.0000 Uani . . . . . . .
C21 C 0.7151(7) 0.5657(3) 1.0456(4) 0.0774 1.0000 Uani . . . . . . .
C22 C 0.6363(6) 0.5419(4) 1.0720(4) 0.0816 1.0000 Uani . . . . . . .
C23 C 0.6035(5) 0.4711(3) 1.0618(3) 0.0570 1.0000 Uani . . . . . . .
C24 C 0.6469(4) 0.4231(3) 1.0213(3) 0.0383 1.0000 Uani . . . . . . .
C25 C 0.6098(4) 0.3479(2) 1.0109(2) 0.0319 1.0000 Uani . . . . . . .
C26 C 0.5450(4) 0.3145(3) 1.0551(3) 0.0455 1.0000 Uani . . . . . . .
C27 C 0.6126(6) 0.2740(4) 1.1180(3) 0.0630 1.0000 Uani . . . . . . .
C28 C 0.5541(4) 0.4241(2) 0.7769(3) 0.0316 1.0000 Uani . . . . . . .
C29 C 0.5183(5) 0.4995(3) 0.7577(3) 0.0487 1.0000 Uani . U . . . . .
C30 C 0.5687(6) 0.5579(3) 0.7969(4) 0.0660 1.0000 Uani . U . . . . .
C31 C 0.5364(7) 0.6281(4) 0.7773(4) 0.0842 1.0000 Uani . U . . . . .
C32 C 0.4510(8) 0.6382(4) 0.7221(5) 0.0937 1.0000 Uani . U . . . . .
C33 C 0.3978(7) 0.5806(4) 0.6846(4) 0.0881 1.0000 Uani . U . . . . .
C34 C 0.4358(5) 0.5113(4) 0.7007(3) 0.0632 1.0000 Uani . U . . . . .
C35 C 0.3571(4) 0.3093(3) 0.7900(3) 0.0428 1.0000 Uani . . . . . . .
C36 C 0.2710(4) 0.2673(3) 0.8035(3) 0.0483 1.0000 Uani . . . . . . .
C101 C 0.8788(10) 0.2420(7) 1.0105(7) 0.043(3) 0.5000 Uiso . . . 1 1 . .
C102 C 0.9509(9) 0.1862(6) 1.0387(6) 0.043(3) 0.5000 Uiso . . . 1 1 . .
C103 C 0.9871(8) 0.1432(5) 0.9899(6) 0.031(2) 0.5000 Uiso . . . 1 1 . .
C104 C 0.9475(8) 0.1559(6) 0.9212(6) 0.037(3) 0.5000 Uiso . . . 1 1 . .
C105 C 0.8775(10) 0.2082(7) 0.9002(7) 0.032(3) 0.5000 Uiso . . . 1 1 . .
C106 C 1.0632(8) 0.0843(6) 1.0128(6) 0.039(2) 0.5000 Uiso . . . 1 1 . .
C107 C 0.8915(7) -0.0629(5) 0.9242(5) 0.033(2) 0.5000 Uiso . . . 1 1 . .
C108 C 0.8132(7) -0.0069(5) 0.9089(6) 0.0256(19) 0.5000 Uiso . . . 1 1 . .
C109 C 0.7692(11) 0.0214(8) 0.9601(8) 0.048(4) 0.5000 Uiso . . . 1 1 . .
C110 C 0.6895(12) 0.0755(8) 0.9422(8) 0.043(4) 0.5000 Uiso . . . 1 1 . .
C111 C 0.7071(12) 0.0728(8) 0.8293(8) 0.034(4) 0.5000 Uiso . . . 1 1 . .
C112 C 0.7775(8) 0.0203(5) 0.8413(6) 0.030(2) 0.5000 Uiso . . . 1 1 . .
C201 C 0.8547(9) 0.2382(6) 1.0237(6) 0.033(3) 0.5000 Uiso . . . 1 2 . .
C202 C 0.9216(8) 0.1902(6) 1.0594(6) 0.037(2) 0.5000 Uiso . . . 1 2 . .
C203 C 0.9745(8) 0.1477(5) 1.0213(6) 0.032(2) 0.5000 Uiso . . . 1 2 . .
C204 C 0.9543(9) 0.1591(6) 0.9500(7) 0.036(2) 0.5000 Uiso . . . 1 2 . .
C205 C 0.8835(12) 0.2135(8) 0.9190(8) 0.044(4) 0.5000 Uiso . . . 1 2 . .
C206 C 1.0486(8) 0.0949(5) 1.0595(5) 0.036(2) 0.5000 Uiso . . . 1 2 . .
C207 C 0.8894(8) -0.0586(5) 0.9697(5) 0.033(2) 0.5000 Uiso . . . 1 2 . .
C208 C 0.8136(7) -0.0038(5) 0.9390(6) 0.027(2) 0.5000 Uiso . . . 1 2 . .
C209 C 0.7646(9) 0.0325(6) 0.9808(7) 0.038(3) 0.5000 Uiso . . . 1 2 . .
C210 C 0.7020(12) 0.0868(9) 0.9547(8) 0.043(4) 0.5000 Uiso . . . 1 2 . .
C211 C 0.7104(14) 0.0689(10) 0.8454(9) 0.049(5) 0.5000 Uiso . . . 1 2 . .
C212 C 0.7867(9) 0.0130(6) 0.8692(7) 0.036(2) 0.5000 Uiso . . . 1 2 . .
H21 H 0.4139 0.0319 0.9528 0.0510 1.0000 Uiso R . . . . . .
H31 H 0.3478 -0.0766 0.9046 0.0630 1.0000 Uiso R . . . . . .
H41 H 0.3159 -0.0970 0.7864 0.0557 1.0000 Uiso R . . . . . .
H51 H 0.3496 -0.0076 0.7138 0.0468 1.0000 Uiso R . . . . . .
H82 H 0.3756 0.1621 0.6434 0.0508 1.0000 Uiso R . . . . . .
H81 H 0.3300 0.0845 0.6523 0.0508 1.0000 Uiso R . . . . . .
H91 H 0.4405 0.0803 0.5757 0.0799 1.0000 Uiso R . . . . . .
H92 H 0.5324 0.1089 0.6360 0.0798 1.0000 Uiso R . . . . . .
H93 H 0.4857 0.0313 0.6419 0.0800 1.0000 Uiso R . . . . . .
H111 H 0.6608 0.2313 0.5287 0.0761 1.0000 Uiso R . . . . . .
H121 H 0.7731 0.2703 0.4651 0.0881 1.0000 Uiso R . . . . . .
H131 H 0.9082 0.3417 0.5145 0.0960 1.0000 Uiso R . . . . . .
H141 H 0.9344 0.3780 0.6316 0.0811 1.0000 Uiso R . . . . . .
H171 H 0.8976 0.4362 0.7876 0.0569 1.0000 Uiso R . . . . . .
H172 H 0.9395 0.4260 0.7208 0.0570 1.0000 Uiso R . . . . . .
H182 H 1.0596 0.3877 0.8255 0.1019 1.0000 Uiso R . . . . . .
H181 H 0.9818 0.3275 0.8333 0.1019 1.0000 Uiso R . . . . . .
H183 H 1.0316 0.3250 0.7694 0.1021 1.0000 Uiso R . . . . . .
H201 H 0.8123 0.5373 0.9888 0.0620 1.0000 Uiso R . . . . . .
H211 H 0.7383 0.6129 1.0540 0.0859 1.0000 Uiso R . . . . . .
H221 H 0.6051 0.5729 1.0971 0.0940 1.0000 Uiso R . . . . . .
H231 H 0.5524 0.4550 1.0809 0.0669 1.0000 Uiso R . . . . . .
H262 H 0.5071 0.3515 1.0717 0.0551 1.0000 Uiso R . . . . . .
H261 H 0.4961 0.2813 1.0265 0.0547 1.0000 Uiso R . . . . . .
H271 H 0.5721 0.2543 1.1475 0.0959 1.0000 Uiso R . . . . . .
H273 H 0.6628 0.3067 1.1451 0.0961 1.0000 Uiso R . . . . . .
H272 H 0.6479 0.2351 1.1008 0.0958 1.0000 Uiso R . . . . . .
H301 H 0.6244 0.5506 0.8360 0.0808 1.0000 Uiso R . . . . . .
H311 H 0.5720 0.6672 0.8013 0.1029 1.0000 Uiso R . . . . . .
H321 H 0.4284 0.6858 0.7087 0.1121 1.0000 Uiso R . . . . . .
H331 H 0.3377 0.5875 0.6489 0.1050 1.0000 Uiso R . . . . . .
H341 H 0.4064 0.4719 0.6732 0.0776 1.0000 Uiso R . . . . . .
H351 H 0.3390 0.3601 0.7853 0.0487 1.0000 Uiso R . . . . . .
H352 H 0.3715 0.2913 0.7464 0.0489 1.0000 Uiso R . . . . . .
H361 H 0.2131 0.2704 0.7629 0.0688 1.0000 Uiso R . . . . . .
H362 H 0.2537 0.2866 0.8439 0.0690 1.0000 Uiso R . . . . . .
H363 H 0.2909 0.2185 0.8124 0.0687 1.0000 Uiso R . . . . . .
H1021 H 0.9733 0.1787 1.0872 0.0510 0.5000 Uiso R . . 1 1 . .
H1041 H 0.9696 0.1291 0.8881 0.0440 0.5000 Uiso R . . 1 1 . .
H1051 H 0.8532 0.2162 0.8527 0.0388 0.5000 Uiso R . . 1 1 . .
H1061 H 1.0817 0.0595 0.9766 0.0471 0.5000 Uiso R . . 1 1 . .
H1071 H 0.9102 -0.0847 0.8866 0.0399 0.5000 Uiso R . . 1 1 . .
H1091 H 0.7915 0.0059 1.0062 0.0563 0.5000 Uiso R . . 1 1 . .
H1101 H 0.6544 0.0894 0.9749 0.0479 0.5000 Uiso R . . 1 1 . .
H1111 H 0.6827 0.0893 0.7835 0.0419 0.5000 Uiso R . . 1 1 . .
H1121 H 0.8030 0.0022 0.8048 0.0360 0.5000 Uiso R . . 1 1 . .
H2011 H 0.8163 0.2639 1.0483 0.0389 0.5000 Uiso R . . 1 2 . .
H2021 H 0.9335 0.1854 1.1077 0.0441 0.5000 Uiso R . . 1 2 . .
H2041 H 0.9870 0.1322 0.9222 0.0431 0.5000 Uiso R . . 1 2 . .
H2061 H 1.0518 0.0868 1.1065 0.0430 0.5000 Uiso R . . 1 2 . .
H2071 H 0.8943 -0.0699 1.0167 0.0400 0.5000 Uiso R . . 1 2 . .
H2091 H 0.7740 0.0196 1.0279 0.0470 0.5000 Uiso R . . 1 2 . .
H2101 H 0.6811 0.1168 0.9864 0.0541 0.5000 Uiso R . . 1 2 . .
H2111 H 0.6935 0.0795 0.7977 0.0568 0.5000 Uiso R . . 1 2 . .
H2121 H 0.8166 -0.0105 0.8375 0.0422 0.5000 Uiso R . . 1 2 . .
H1011 H 0.8604 0.2730 1.0423 0.0500 0.5000 Uiso R . . 1 1 . .
H2051 H 0.8716 0.2193 0.8710 0.0518 0.5000 Uiso R . . 1 2 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0294(4) 0.0185(3) 0.0230(3) 0.0006(2) 0.0059(3) 0.0011(3)
Mn2 0.0381(4) 0.0229(3) 0.0235(3) 0.0009(3) 0.0102(3) 0.0015(3)
Mn3 0.0286(3) 0.0217(3) 0.0260(3) -0.0017(3) 0.0054(3) 0.0009(3)
O2 0.0272(16) 0.0202(14) 0.0240(15) -0.0005(11) 0.0070(12) 0.0003(12)
O4 0.0378(19) 0.0417(19) 0.0369(19) -0.0033(15) 0.0123(15) -0.0114(16)
O7 0.052(2) 0.0316(17) 0.0243(16) 0.0036(13) 0.0045(15) -0.0099(16)
O12 0.0359(18) 0.0300(16) 0.0316(17) -0.0016(13) 0.0102(14) -0.0040(14)
O17 0.048(2) 0.0241(16) 0.0302(17) 0.0050(13) 0.0070(15) 0.0040(15)
O19 0.052(2) 0.0227(15) 0.0346(18) 0.0012(13) 0.0076(16) 0.0095(15)
O26 0.061(3) 0.060(2) 0.0308(19) -0.0084(17) 0.0208(18) -0.006(2)
O31 0.048(2) 0.0319(18) 0.0372(19) -0.0121(15) 0.0092(16) -0.0111(16)
O36 0.0397(18) 0.0240(15) 0.0249(15) -0.0009(12) 0.0085(13) -0.0034(14)
O49 0.0292(17) 0.0338(17) 0.0392(19) 0.0008(14) 0.0041(14) 0.0072(14)
N1 0.045(2) 0.0196(17) 0.0277(19) 0.0063(14) 0.0167(17) 0.0083(16)
N2 0.043(2) 0.0275(19) 0.031(2) 0.0007(16) 0.0107(18) 0.0112(18)
N3 0.0285(19) 0.0214(17) 0.0299(19) 0.0042(15) 0.0002(16) 0.0028(15)
N4 0.032(2) 0.032(2) 0.045(2) -0.0026(19) -0.0053(19) 0.0054(18)
N5 0.034(2) 0.0253(19) 0.044(2) 0.0003(17) 0.0097(18) 0.0041(17)
C1 0.024(2) 0.025(2) 0.042(3) 0.0011(19) 0.009(2) -0.0001(18)
C2 0.047(3) 0.037(3) 0.046(3) 0.007(2) 0.017(3) -0.001(2)
C3 0.059(4) 0.031(3) 0.069(4) 0.009(3) 0.029(3) -0.009(3)
C4 0.048(3) 0.028(3) 0.067(4) -0.006(2) 0.018(3) -0.011(2)
C5 0.036(3) 0.033(3) 0.052(3) -0.007(2) 0.008(2) -0.005(2)
C6 0.026(2) 0.024(2) 0.040(3) -0.0009(19) 0.003(2) 0.0009(18)
C7 0.033(2) 0.021(2) 0.031(2) -0.0015(17) 0.0045(19) 0.0036(18)
C8 0.056(3) 0.036(3) 0.038(3) 0.001(2) 0.000(3) -0.007(3)
C9 0.072(4) 0.059(4) 0.032(3) -0.008(3) 0.009(3) -0.010(3)
C10 0.071(4) 0.039(3) 0.039(3) 0.011(2) 0.028(3) 0.020(3)
C11 0.098(4) 0.051(3) 0.044(3) 0.002(2) 0.036(3) 0.018(3)
C12 0.111(5) 0.061(4) 0.052(4) 0.005(3) 0.048(4) 0.031(4)
C13 0.106(5) 0.059(4) 0.077(4) 0.020(3) 0.070(4) 0.019(4)
C14 0.079(4) 0.048(3) 0.075(4) 0.020(3) 0.052(3) 0.018(3)
C15 0.063(3) 0.033(2) 0.054(3) 0.016(2) 0.038(3) 0.021(3)
C16 0.040(3) 0.029(2) 0.046(3) 0.009(2) 0.019(2) 0.012(2)
C17 0.036(3) 0.042(3) 0.067(4) 0.016(3) 0.024(3) 0.003(2)
C18 0.047(4) 0.067(4) 0.091(5) 0.033(4) 0.023(4) 0.008(3)
C19 0.052(3) 0.022(2) 0.031(2) -0.0053(19) -0.008(2) 0.008(2)
C20 0.074(4) 0.031(3) 0.052(4) -0.004(2) 0.003(3) -0.003(3)
C21 0.093(6) 0.033(3) 0.089(5) -0.024(3) -0.010(5) 0.009(4)
C22 0.078(5) 0.063(4) 0.095(6) -0.049(4) 0.002(4) 0.024(4)
C23 0.055(4) 0.056(4) 0.057(4) -0.024(3) 0.010(3) 0.013(3)
C24 0.041(3) 0.035(3) 0.033(3) -0.010(2) -0.003(2) 0.012(2)
C25 0.033(3) 0.033(2) 0.024(2) -0.0025(18) -0.0039(19) 0.011(2)
C26 0.052(3) 0.054(3) 0.035(3) -0.008(2) 0.019(2) 0.000(3)
C27 0.090(5) 0.064(4) 0.039(3) 0.008(3) 0.022(3) -0.007(4)
C28 0.030(2) 0.029(2) 0.037(3) 0.0087(19) 0.012(2) 0.0055(19)
C29 0.074(4) 0.035(3) 0.049(3) 0.015(2) 0.036(3) 0.021(3)
C30 0.105(5) 0.034(3) 0.071(4) 0.002(3) 0.044(4) 0.008(3)
C31 0.137(6) 0.039(3) 0.088(5) -0.004(3) 0.048(5) 0.014(4)
C32 0.141(7) 0.054(4) 0.094(6) 0.024(4) 0.043(5) 0.048(5)
C33 0.116(5) 0.066(4) 0.087(5) 0.034(4) 0.034(4) 0.047(4)
C34 0.073(4) 0.056(3) 0.068(4) 0.026(3) 0.033(3) 0.028(3)
C35 0.040(3) 0.043(3) 0.043(3) 0.004(2) 0.003(2) 0.011(2)
C36 0.037(3) 0.047(3) 0.057(4) 0.004(3) 0.005(3) 0.007(3)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.21926(16)
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 . Mn2 . 3.2641(9) yes
Mn1 . Mn3 . 3.2383(9) yes
Mn1 . O2 . 1.887(3) yes
Mn1 . O12 . 1.872(3) yes
Mn1 . O36 . 1.917(3) yes
Mn1 . O49 . 2.323(3) yes
Mn1 . N1 . 1.986(4) yes
Mn1 . N5 . 2.307(4) yes
Mn2 . Mn3 . 3.1649(9) yes
Mn2 . O2 . 1.858(3) yes
Mn2 . O7 . 1.910(3) yes
Mn2 . O17 . 2.130(3) yes
Mn2 . O26 . 1.855(3) yes
Mn2 . N2 . 1.979(4) yes
Mn3 . O2 . 1.900(3) yes
Mn3 . O4 . 1.900(3) yes
Mn3 . O19 . 2.317(3) yes
Mn3 . O31 . 1.853(3) yes
Mn3 . N3 . 1.983(4) yes
Mn3 . N4 . 2.283(4) yes
O4 . N2 . 1.376(5) yes
O7 . N1 . 1.371(4) yes
O12 . C1 . 1.326(5) yes
O17 . C28 . 1.258(5) yes
O19 . C28 . 1.268(5) yes
O26 . C10 . 1.325(6) yes
O31 . C19 . 1.323(6) yes
O36 . N3 . 1.376(4) yes
O49 . C35 . 1.439(6) yes
N1 . C7 . 1.317(6) yes
N2 . C16 . 1.311(6) yes
N3 . C25 . 1.299(6) yes
N4 . C101 . 1.213(13) yes
N4 . C105 . 1.449(14) yes
N4 . C201 . 1.454(12) yes
N4 . C205 . 1.183(15) yes
N5 . C110 . 1.249(16) yes
N5 . C111 . 1.420(16) yes
N5 . C210 . 1.413(16) yes
N5 . C211 . 1.233(18) yes
C1 . C2 . 1.403(6) yes
C1 . C6 . 1.423(6) yes
C2 . C3 . 1.378(7) yes
C2 . H21 . 0.930 no
C3 . C4 . 1.365(8) yes
C3 . H31 . 0.924 no
C4 . C5 . 1.375(7) yes
C4 . H41 . 0.929 no
C5 . C6 . 1.411(6) yes
C5 . H51 . 0.925 no
C6 . C7 . 1.461(6) yes
C7 . C8 . 1.511(6) yes
C8 . C9 . 1.533(8) yes
C8 . H82 . 0.981 no
C8 . H81 . 0.973 no
C9 . H91 . 0.961 no
C9 . H92 . 0.966 no
C9 . H93 . 0.971 no
C10 . C11 . 1.410(7) yes
C10 . C15 . 1.404(8) yes
C11 . C12 . 1.378(9) yes
C11 . H111 . 0.928 no
C12 . C13 . 1.344(10) yes
C12 . H121 . 0.945 no
C13 . C14 . 1.388(9) yes
C13 . H131 . 0.935 no
C14 . C15 . 1.416(7) yes
C14 . H141 . 0.936 no
C15 . C16 . 1.457(7) yes
C16 . C17 . 1.508(7) yes
C17 . C18 . 1.526(7) yes
C17 . H171 . 0.958 no
C17 . H172 . 0.963 no
C18 . H182 . 0.962 no
C18 . H181 . 0.955 no
C18 . H183 . 0.962 no
C19 . C20 . 1.409(7) yes
C19 . C24 . 1.403(7) yes
C20 . C21 . 1.368(9) yes
C20 . H201 . 0.918 no
C21 . C22 . 1.365(10) yes
C21 . H211 . 0.926 no
C22 . C23 . 1.378(9) yes
C22 . H221 . 0.923 no
C23 . C24 . 1.412(7) yes
C23 . H231 . 0.913 no
C24 . C25 . 1.473(7) yes
C25 . C26 . 1.509(7) yes
C26 . C27 . 1.536(8) yes
C26 . H262 . 0.956 no
C26 . H261 . 0.972 no
C27 . H271 . 0.962 no
C27 . H273 . 0.963 no
C27 . H272 . 0.968 no
C28 . C29 . 1.491(6) yes
C29 . C30 . 1.400(9) yes
C29 . C34 . 1.386(8) yes
C30 . C31 . 1.392(9) yes
C30 . H301 . 0.942 no
C31 . C32 . 1.384(11) yes
C31 . H311 . 0.929 no
C32 . C33 . 1.388(11) yes
C32 . H321 . 0.945 no
C33 . C34 . 1.385(8) yes
C33 . H331 . 0.941 no
C34 . H341 . 0.933 no
C35 . C36 . 1.474(7) yes
C35 . H351 . 0.969 no
C35 . H352 . 0.983 no
C36 . H361 . 0.969 no
C36 . H362 . 0.951 no
C36 . H363 . 0.943 no
C101 . C102 . 1.429(17) yes
C101 . H1011 . 0.925 no
C102 . C103 . 1.421(15) yes
C102 . H1021 . 0.937 no
C103 . C104 . 1.345(15) yes
C103 . C106 . 1.485(14) yes
C104 . C105 . 1.341(17) yes
C104 . H1041 . 0.924 no
C105 . H1051 . 0.921 no
C106 . C107 2_757 1.300(14) yes
C106 . H1061 . 0.930 no
C107 . C108 . 1.454(13) yes
C107 . H1071 . 0.928 no
C108 . C109 . 1.390(16) yes
C108 . C112 . 1.391(14) yes
C109 . C110 . 1.45(2) yes
C109 . H1091 . 0.927 no
C110 . H1101 . 0.924 no
C111 . C112 . 1.336(18) yes
C111 . H1111 . 0.929 no
C112 . H1121 . 0.931 no
C201 . C202 . 1.333(15) yes
C201 . H2011 . 0.921 no
C202 . C203 . 1.397(15) yes
C202 . H2021 . 0.926 no
C203 . C204 . 1.375(15) yes
C203 . C206 . 1.463(13) yes
C204 . C205 . 1.416(19) yes
C204 . H2041 . 0.926 no
C205 . H2051 . 0.923 no
C206 . C207 2_757 1.310(13) yes
C206 . H2061 . 0.926 no
C207 . C208 . 1.458(13) yes
C207 . H2071 . 0.932 no
C208 . C209 . 1.352(16) yes
C208 . C212 . 1.363(15) yes
C209 . C210 . 1.329(19) yes
C209 . H2091 . 0.934 no
C210 . H2101 . 0.928 no
C211 . C212 . 1.45(2) yes
C211 . H2111 . 0.929 no
C212 . H2121 . 0.929 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
Mn2 . Mn1 . Mn3 . 58.25(2) yes
Mn2 . Mn1 . O2 . 29.13(9) yes
Mn3 . Mn1 . O2 . 31.36(8) yes
Mn2 . Mn1 . O12 . 148.91(10) yes
Mn3 . Mn1 . O12 . 150.54(10) yes
O2 . Mn1 . O12 . 178.00(13) yes
Mn2 . Mn1 . O36 . 118.97(9) yes
Mn3 . Mn1 . O36 . 60.75(9) yes
O2 . Mn1 . O36 . 91.25(13) yes
O12 . Mn1 . O36 . 90.75(13) yes
Mn2 . Mn1 . O49 . 82.00(8) yes
Mn3 . Mn1 . O49 . 78.87(8) yes
O2 . Mn1 . O49 . 87.63(12) yes
O12 . Mn1 . O49 . 92.38(13) yes
O36 . Mn1 . O49 . 85.28(12) yes
Mn2 . Mn1 . N1 . 59.40(11) yes
Mn3 . Mn1 . N1 . 117.54(11) yes
O2 . Mn1 . N1 . 87.82(14) yes
O12 . Mn1 . N1 . 90.18(15) yes
O36 . Mn1 . N1 . 174.87(14) yes
Mn2 . Mn1 . N5 . 97.64(11) yes
Mn3 . Mn1 . N5 . 100.52(10) yes
O2 . Mn1 . N5 . 91.81(13) yes
O12 . Mn1 . N5 . 88.18(14) yes
O36 . Mn1 . N5 . 94.47(14) yes
O49 . Mn1 . N1 . 89.64(13) yes
O49 . Mn1 . N5 . 179.38(13) yes
N1 . Mn1 . N5 . 90.60(15) yes
Mn1 . Mn2 . Mn3 . 60.47(2) yes
Mn1 . Mn2 . O2 . 29.63(9) yes
Mn3 . Mn2 . O2 . 33.06(9) yes
Mn1 . Mn2 . O7 . 61.36(9) yes
Mn3 . Mn2 . O7 . 120.32(10) yes
O2 . Mn2 . O7 . 90.93(13) yes
Mn1 . Mn2 . O17 . 101.81(9) yes
Mn3 . Mn2 . O17 . 82.34(9) yes
O2 . Mn2 . O17 . 101.14(12) yes
O7 . Mn2 . O17 . 97.39(14) yes
Mn1 . Mn2 . O26 . 143.02(13) yes
Mn3 . Mn2 . O26 . 150.83(13) yes
O2 . Mn2 . O26 . 156.55(16) yes
O7 . Mn2 . O26 . 87.97(16) yes
O17 . Mn2 . O26 . 102.24(15) yes
Mn1 . Mn2 . N2 . 119.29(11) yes
Mn3 . Mn2 . N2 . 62.28(11) yes
O2 . Mn2 . N2 . 89.71(14) yes
O7 . Mn2 . N2 . 173.38(15) yes
O17 . Mn2 . N2 . 88.95(14) yes
O26 . Mn2 . N2 . 88.82(17) yes
Mn2 . Mn3 . Mn1 . 61.28(2) yes
Mn2 . Mn3 . O2 . 32.24(8) yes
Mn1 . Mn3 . O2 . 31.13(9) yes
Mn2 . Mn3 . O4 . 62.50(10) yes
Mn1 . Mn3 . O4 . 121.62(10) yes
O2 . Mn3 . O4 . 90.49(13) yes
Mn2 . Mn3 . O19 . 72.88(8) yes
Mn1 . Mn3 . O19 . 88.03(9) yes
O2 . Mn3 . O19 . 87.33(12) yes
O4 . Mn3 . O19 . 89.87(14) yes
Mn2 . Mn3 . O31 . 148.66(11) yes
Mn1 . Mn3 . O31 . 146.76(11) yes
O2 . Mn3 . O31 . 177.28(15) yes
O4 . Mn3 . O31 . 91.59(15) yes
O19 . Mn3 . O31 . 90.91(14) yes
Mn2 . Mn3 . N3 . 116.55(11) yes
Mn1 . Mn3 . N3 . 58.37(11) yes
O2 . Mn3 . N3 . 89.44(14) yes
O4 . Mn3 . N3 . 177.04(15) yes
O19 . Mn3 . N3 . 87.17(13) yes
Mn2 . Mn3 . N4 . 105.28(11) yes
Mn1 . Mn3 . N4 . 87.19(11) yes
O2 . Mn3 . N4 . 88.92(13) yes
O4 . Mn3 . N4 . 93.19(16) yes
O19 . Mn3 . N4 . 175.18(14) yes
O31 . Mn3 . N3 . 88.40(15) yes
O31 . Mn3 . N4 . 92.72(15) yes
N3 . Mn3 . N4 . 89.77(15) yes
Mn3 . O2 . Mn1 . 117.51(14) yes
Mn3 . O2 . Mn2 . 114.70(14) yes
Mn1 . O2 . Mn2 . 121.24(15) yes
Mn3 . O4 . N2 . 119.8(3) yes
Mn2 . O7 . N1 . 118.2(3) yes
Mn1 . O12 . C1 . 124.7(3) yes
Mn2 . O17 . C28 . 126.1(3) yes
Mn3 . O19 . C28 . 126.9(3) yes
Mn2 . O26 . C10 . 132.5(4) yes
Mn3 . O31 . C19 . 124.8(3) yes
Mn1 . O36 . N3 . 113.6(2) yes
Mn1 . O49 . C35 . 125.7(3) yes
O7 . N1 . Mn1 . 117.3(3) yes
O7 . N1 . C7 . 113.7(4) yes
Mn1 . N1 . C7 . 128.4(3) yes
O4 . N2 . Mn2 . 114.6(3) yes
O4 . N2 . C16 . 114.1(4) yes
Mn2 . N2 . C16 . 131.0(4) yes
O36 . N3 . Mn3 . 114.6(3) yes
O36 . N3 . C25 . 116.5(4) yes
Mn3 . N3 . C25 . 128.9(3) yes
Mn3 . N4 . C101 . 130.5(7) yes
Mn3 . N4 . C105 . 114.2(6) yes
C101 . N4 . C105 . 115.1(9) yes
Mn3 . N4 . C201 . 119.2(5) yes
Mn3 . N4 . C205 . 125.0(8) yes
C201 . N4 . C205 . 115.4(9) yes
Mn1 . N5 . C110 . 117.9(8) yes
Mn1 . N5 . C111 . 124.1(7) yes
C110 . N5 . C111 . 118.0(10) yes
Mn1 . N5 . C210 . 111.7(7) yes
Mn1 . N5 . C211 . 135.2(8) yes
C210 . N5 . C211 . 112.5(11) yes
O12 . C1 . C2 . 117.8(4) yes
O12 . C1 . C6 . 123.3(4) yes
C2 . C1 . C6 . 118.9(4) yes
C1 . C2 . C3 . 120.6(5) yes
C1 . C2 . H21 . 119.3 no
C3 . C2 . H21 . 120.1 no
C2 . C3 . C4 . 121.3(5) yes
C2 . C3 . H31 . 119.3 no
C4 . C3 . H31 . 119.4 no
C3 . C4 . C5 . 119.7(5) yes
C3 . C4 . H41 . 120.2 no
C5 . C4 . H41 . 120.1 no
C4 . C5 . C6 . 121.7(5) yes
C4 . C5 . H51 . 119.6 no
C6 . C5 . H51 . 118.7 no
C1 . C6 . C5 . 117.9(4) yes
C1 . C6 . C7 . 122.7(4) yes
C5 . C6 . C7 . 119.3(4) yes
C6 . C7 . N1 . 120.0(4) yes
C6 . C7 . C8 . 120.8(4) yes
N1 . C7 . C8 . 119.2(4) yes
C7 . C8 . C9 . 112.4(4) yes
C7 . C8 . H82 . 107.6 no
C9 . C8 . H82 . 107.9 no
C7 . C8 . H81 . 109.6 no
C9 . C8 . H81 . 110.7 no
H82 . C8 . H81 . 108.5 no
C8 . C9 . H91 . 108.7 no
C8 . C9 . H92 . 110.3 no
H91 . C9 . H92 . 110.0 no
C8 . C9 . H93 . 109.2 no
H91 . C9 . H93 . 109.4 no
H92 . C9 . H93 . 109.3 no
O26 . C10 . C11 . 116.0(6) yes
O26 . C10 . C15 . 123.8(5) yes
C11 . C10 . C15 . 120.2(5) yes
C10 . C11 . C12 . 119.4(7) yes
C10 . C11 . H111 . 120.2 no
C12 . C11 . H111 . 120.4 no
C11 . C12 . C13 . 122.2(6) yes
C11 . C12 . H121 . 119.0 no
C13 . C12 . H121 . 118.8 no
C12 . C13 . C14 . 119.2(6) yes
C12 . C13 . H131 . 119.7 no
C14 . C13 . H131 . 121.1 no
C13 . C14 . C15 . 121.9(7) yes
C13 . C14 . H141 . 119.9 no
C15 . C14 . H141 . 118.2 no
C14 . C15 . C10 . 117.0(6) yes
C14 . C15 . C16 . 120.2(6) yes
C10 . C15 . C16 . 122.8(5) yes
C15 . C16 . N2 . 120.8(5) yes
C15 . C16 . C17 . 121.6(5) yes
N2 . C16 . C17 . 117.6(5) yes
C16 . C17 . C18 . 111.1(5) yes
C16 . C17 . H171 . 110.2 no
C18 . C17 . H171 . 109.0 no
C16 . C17 . H172 . 108.6 no
C18 . C17 . H172 . 108.9 no
H171 . C17 . H172 . 109.0 no
C17 . C18 . H182 . 110.0 no
C17 . C18 . H181 . 108.7 no
H182 . C18 . H181 . 109.1 no
C17 . C18 . H183 . 109.4 no
H182 . C18 . H183 . 110.2 no
H181 . C18 . H183 . 109.4 no
O31 . C19 . C20 . 117.3(5) yes
O31 . C19 . C24 . 123.9(4) yes
C20 . C19 . C24 . 118.7(5) yes
C19 . C20 . C21 . 121.1(7) yes
C19 . C20 . H201 . 119.2 no
C21 . C20 . H201 . 119.8 no
C20 . C21 . C22 . 120.6(6) yes
C20 . C21 . H211 . 119.7 no
C22 . C21 . H211 . 119.7 no
C21 . C22 . C23 . 120.2(6) yes
C21 . C22 . H221 . 120.3 no
C23 . C22 . H221 . 119.6 no
C22 . C23 . C24 . 120.9(7) yes
C22 . C23 . H231 . 119.8 no
C24 . C23 . H231 . 119.2 no
C23 . C24 . C19 . 118.5(5) yes
C23 . C24 . C25 . 119.8(5) yes
C19 . C24 . C25 . 121.7(4) yes
C24 . C25 . N3 . 119.7(4) yes
C24 . C25 . C26 . 122.0(4) yes
N3 . C25 . C26 . 118.3(4) yes
C25 . C26 . C27 . 110.4(5) yes
C25 . C26 . H262 . 109.9 no
C27 . C26 . H262 . 109.5 no
C25 . C26 . H261 . 109.3 no
C27 . C26 . H261 . 109.9 no
H262 . C26 . H261 . 107.7 no
C26 . C27 . H271 . 110.9 no
C26 . C27 . H273 . 109.6 no
H271 . C27 . H273 . 109.3 no
C26 . C27 . H272 . 109.0 no
H271 . C27 . H272 . 109.4 no
H273 . C27 . H272 . 108.6 no
O19 . C28 . O17 . 124.9(4) yes
O19 . C28 . C29 . 116.4(4) yes
O17 . C28 . C29 . 118.7(4) yes
C28 . C29 . C30 . 119.8(6) yes
C28 . C29 . C34 . 119.7(6) yes
C30 . C29 . C34 . 120.5(6) yes
C29 . C30 . C31 . 119.3(7) yes
C29 . C30 . H301 . 121.3 no
C31 . C30 . H301 . 119.4 no
C30 . C31 . C32 . 119.0(8) yes
C30 . C31 . H311 . 119.7 no
C32 . C31 . H311 . 121.3 no
C31 . C32 . C33 . 122.2(7) yes
C31 . C32 . H321 . 119.4 no
C33 . C32 . H321 . 118.4 no
C32 . C33 . C34 . 118.3(8) yes
C32 . C33 . H331 . 121.9 no
C34 . C33 . H331 . 119.9 no
C29 . C34 . C33 . 120.4(7) yes
C29 . C34 . H341 . 119.1 no
C33 . C34 . H341 . 120.5 no
O49 . C35 . C36 . 109.4(4) yes
O49 . C35 . H351 . 109.2 no
C36 . C35 . H351 . 109.6 no
O49 . C35 . H352 . 110.1 no
C36 . C35 . H352 . 108.3 no
H351 . C35 . H352 . 110.1 no
C35 . C36 . H361 . 109.2 no
C35 . C36 . H362 . 108.6 no
H361 . C36 . H362 . 110.6 no
C35 . C36 . H363 . 109.5 no
H361 . C36 . H363 . 110.2 no
H362 . C36 . H363 . 108.7 no
N4 . C101 . C102 . 126.3(12) yes
N4 . C101 . H1011 . 116.8 no
C102 . C101 . H1011 . 117.0 no
C101 . C102 . C103 . 117.1(11) yes
C101 . C102 . H1021 . 121.2 no
C103 . C102 . H1021 . 121.7 no
C102 . C103 . C104 . 117.5(10) yes
C102 . C103 . C106 . 122.2(10) yes
C104 . C103 . C106 . 120.3(10) yes
C103 . C104 . C105 . 120.6(12) yes
C103 . C104 . H1041 . 119.7 no
C105 . C104 . H1041 . 119.7 no
N4 . C105 . C104 . 122.9(12) yes
N4 . C105 . H1051 . 118.8 no
C104 . C105 . H1051 . 118.3 no
C103 . C106 . C107 2_757 129.5(11) yes
C103 . C106 . H1061 . 115.2 no
C107 2_757 C106 . H1061 . 115.3 no
C106 2_757 C107 . C108 . 123.9(10) yes
C106 2_757 C107 . H1071 . 118.1 no
C108 . C107 . H1071 . 118.0 no
C107 . C108 . C109 . 122.5(12) yes
C107 . C108 . C112 . 121.0(9) yes
C109 . C108 . C112 . 116.5(10) yes
C108 . C109 . C110 . 120.6(13) yes
C108 . C109 . H1091 . 119.8 no
C110 . C109 . H1091 . 119.6 no
C109 . C110 . N5 . 121.1(14) yes
C109 . C110 . H1101 . 120.0 no
N5 . C110 . H1101 . 118.9 no
N5 . C111 . C112 . 123.4(13) yes
N5 . C111 . H1111 . 118.2 no
C112 . C111 . H1111 . 118.3 no
C108 . C112 . C111 . 119.6(11) yes
C108 . C112 . H1121 . 120.0 no
C111 . C112 . H1121 . 120.4 no
N4 . C201 . C202 . 124.3(10) yes
N4 . C201 . H2011 . 118.3 no
C202 . C201 . H2011 . 117.4 no
C201 . C202 . C203 . 117.3(11) yes
C201 . C202 . H2021 . 121.7 no
C203 . C202 . H2021 . 120.9 no
C202 . C203 . C204 . 117.6(10) yes
C202 . C203 . C206 . 118.2(9) yes
C204 . C203 . C206 . 124.2(11) yes
C203 . C204 . C205 . 119.2(11) yes
C203 . C204 . H2041 . 121.0 no
C205 . C204 . H2041 . 119.7 no
C204 . C205 . N4 . 126.1(13) yes
C204 . C205 . H2051 . 116.7 no
N4 . C205 . H2051 . 117.3 no
C203 . C206 . C207 2_757 123.0(10) yes
C203 . C206 . H2061 . 118.5 no
C207 2_757 C206 . H2061 . 118.6 no
C206 2_757 C207 . C208 . 129.2(10) yes
C206 2_757 C207 . H2071 . 115.0 no
C208 . C207 . H2071 . 115.8 no
C207 . C208 . C209 . 119.3(10) yes
C207 . C208 . C212 . 123.9(11) yes
C209 . C208 . C212 . 116.8(10) yes
C208 . C209 . C210 . 119.9(13) yes
C208 . C209 . H2091 . 120.7 no
C210 . C209 . H2091 . 119.4 no
N5 . C210 . C209 . 125.5(14) yes
N5 . C210 . H2101 . 117.0 no
C209 . C210 . H2101 . 117.5 no
N5 . C211 . C212 . 126.1(14) yes
N5 . C211 . H2111 . 117.0 no
C212 . C211 . H2111 . 116.9 no
C211 . C212 . C208 . 118.4(11) yes
C211 . C212 . H2121 . 120.4 no
C208 . C212 . H2121 . 121.1 no


# Attachment '_1_.cif'

data_eb9028
_database_code_depnum_ccdc_archive 'CCDC 765867'
#TrackingRef '_1_.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_compound_source        'Ross Inglis'
_exptl_crystal_recrystallization_method 
'Diffusion of n-hexane into MeOH solution'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C81 H66 Cl3 Mn3 N6 O10), Cl O4, OH, 2MeOH'
_chemical_formula_sum            'C164 H141 Cl7 Mn6 N12 O27'
_chemical_formula_weight         3289.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  -R3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   21.4412(13)
_cell_length_b                   21.4412(13)
_cell_length_c                   28.5829(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     11379.8(12)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5614
_cell_measurement_theta_min      2.3065
_cell_measurement_theta_max      30.2605
_exptl_crystal_description       cube
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5082
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7323
_exptl_absorpt_correction_T_max  0.8580
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22940
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         30.51
_reflns_number_total             7686
_reflns_number_gt                5838
_reflns_threshold_expression     >2sigma(I)

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

PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.92 Ratio
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.64
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.79 Ratio
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.69 Ratio
PLAT302_ALERT_4_G Note Anion/Solvent Disorder .................... 33.00 Perc.

There is disorder in the MeO group. Modelling the q-peaks produces unreasonable
geometry. The ligand was assigned as MeO on the basis of the strongest q-peaks
in this region and the possibilities given the reaction mixture.

ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.732 0.858
Tmin(prime) and Tmax expected: 0.851 0.854
RR(prime) = 0.857
Please check that your absorption correction is appropriate.
PLAT061_ALERT_4_C Tmax/Tmin Range Test RR' too Large ............. 0.85

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc. The crystal was a rather irregular shape, being
a fragment of a larger block; this precluded integration methods for
correcting for absorption.

CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 3
From the CIF: _chemical_formula_weight 3288.67
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 162.00 1945.78
H 1.01 132.00 133.06
N 14.01 12.00 168.08
O 16.00 25.02 400.29
Cl 35.45 7.00 248.17
Mn 54.94 6.00 329.63
Calculated formula weight 3225.02
PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ?
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 3288.67
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C164 H140 Cl7 Mn6 N12 O27
Atom count from _chemical_formula_moiety:C162 H135 Cl7 Mn6 N12 O27
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C164 H140 Cl7 Mn6 N12 O27
Atom count from the _atom_site data: C162 H132 Cl7 Mn6 N12 O25.02
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
symmetry error - see SYMMG tests
From the CIF: _cell_formula_units_Z 3
From the CIF: _chemical_formula_sum C164 H140 Cl7 Mn6 N12 O27
TEST: Compare cell contents of formula and atom_site data

atom Z*formula cif sites diff
C 492.00 486.00 6.00
H 420.00 396.00 24.00
Cl 21.00 21.00 0.00
Mn 18.00 18.00 0.00
N 36.00 36.00 0.00
O 81.00 75.06 5.94

Platon squeeze was used to treat disordered MeOH solvent. All properties have
been calculated including the MeOH molecules of which there are 2 per formula
unit.
Note that there is an O6 molecule in calculated formulae. This is disordered
OH- which is required to balance charge.

PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
O6
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 20.33
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 13

No action taken

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1077P)^2^+20.3300P] 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         7686
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1929
_refine_ls_wR_factor_gt          0.1771
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.68210(2) 0.42741(2) 0.050797(15) 0.02371(13) Uani 1 1 d . . .
O111 O 0.6667 0.3333 0.06033(11) 0.0226(6) Uani 1 3 d S . .
O1A O 0.82331(10) 0.30571(10) 0.03712(7) 0.0278(4) Uani 1 1 d . . .
C1A C 0.88924(13) 0.34362(14) 0.05493(10) 0.0246(5) Uani 1 1 d . . .
O2A O 0.78460(9) 0.46824(9) 0.04877(7) 0.0266(4) Uani 1 1 d . . .
C2A C 0.91892(13) 0.41536(14) 0.07039(9) 0.0240(5) Uani 1 1 d . . .
C3A C 0.98969(15) 0.44981(16) 0.08873(11) 0.0310(6) Uani 1 1 d . . .
H3AA H 1.0105 0.4981 0.0995 0.037 Uiso 1 1 calc R . .
C4A C 1.02913(16) 0.41534(17) 0.09138(12) 0.0364(7) Uani 1 1 d . . .
H4AA H 1.0763 0.4393 0.1042 0.044 Uiso 1 1 calc R . .
C5A C 0.99935(15) 0.34517(16) 0.07514(11) 0.0334(6) Uani 1 1 d . . .
H5AA H 1.0267 0.3215 0.0763 0.040 Uiso 1 1 calc R . .
C6A C 0.93062(14) 0.30964(15) 0.05736(11) 0.0298(6) Uani 1 1 d . . .
H6AA H 0.9109 0.2615 0.0466 0.036 Uiso 1 1 calc R . .
C21A C 0.88111(13) 0.45604(13) 0.06694(9) 0.0227(5) Uani 1 1 d . . .
N22A N 0.81308(11) 0.42425(11) 0.05603(8) 0.0230(4) Uani 1 1 d . . .
C23A C 0.92134(13) 0.53438(13) 0.07875(10) 0.0248(5) Uani 1 1 d . . .
C24A C 0.91293(16) 0.55500(16) 0.12310(11) 0.0322(6) Uani 1 1 d . . .
H24A H 0.8790 0.5202 0.1441 0.039 Uiso 1 1 calc R . .
C25A C 0.95369(18) 0.62613(17) 0.13710(12) 0.0398(7) Uani 1 1 d . . .
H25A H 0.9475 0.6400 0.1675 0.048 Uiso 1 1 calc R . .
C26A C 1.00314(17) 0.67674(17) 0.10702(13) 0.0413(7) Uani 1 1 d . . .
H26A H 1.0312 0.7254 0.1168 0.050 Uiso 1 1 calc R . .
C27A C 1.01219(18) 0.65702(17) 0.06258(13) 0.0417(7) Uani 1 1 d . . .
H27A H 1.0464 0.6921 0.0419 0.050 Uiso 1 1 calc R . .
C28A C 0.97100(16) 0.58555(15) 0.04825(11) 0.0326(6) Uani 1 1 d . . .
H28A H 0.9769 0.5719 0.0177 0.039 Uiso 1 1 calc R . .
N1B N 0.69178(12) 0.46177(12) 0.12997(8) 0.0271(5) Uani 1 1 d . . .
C2B C 0.74503(16) 0.52775(16) 0.14048(11) 0.0332(6) Uani 1 1 d . . .
H2BA H 0.7736 0.5584 0.1158 0.040 Uiso 1 1 calc R . .
C3B C 0.76040(17) 0.55332(16) 0.18599(11) 0.0352(6) Uani 1 1 d . . .
H3BA H 0.7990 0.6006 0.1919 0.042 Uiso 1 1 calc R . .
C4B C 0.71951(16) 0.50993(15) 0.22311(11) 0.0315(6) Uani 1 1 d . . .
C5B C 0.66392(16) 0.44113(15) 0.21147(11) 0.0321(6) Uani 1 1 d . . .
H5BA H 0.6346 0.4090 0.2353 0.039 Uiso 1 1 calc R . .
C6B C 0.65159(15) 0.41995(15) 0.16520(11) 0.0309(6) Uani 1 1 d . . .
H6BA H 0.6127 0.3734 0.1580 0.037 Uiso 1 1 calc R . .
C7B C 0.73385(17) 0.53358(16) 0.27218(11) 0.0340(6) Uani 1 1 d . . .
H7BA H 0.7167 0.4979 0.2960 0.041 Uiso 1 1 calc R . .
C8B C 0.76978(16) 0.60261(16) 0.28485(11) 0.0331(6) Uani 1 1 d . . .
H8BA H 0.7842 0.6367 0.2602 0.040 Uiso 1 1 calc R . .
C9B C 0.78995(15) 0.63266(16) 0.33243(10) 0.0300(6) Uani 1 1 d . . .
Cl1B Cl 0.86783(6) 0.74102(6) 0.47255(3) 0.0554(3) Uani 1 1 d . . .
C10B C 0.82249(15) 0.70691(15) 0.33704(11) 0.0308(6) Uani 1 1 d . . .
H10A H 0.8281 0.7353 0.3101 0.037 Uiso 1 1 calc R . .
C11B C 0.84689(15) 0.74060(16) 0.37989(11) 0.0324(6) Uani 1 1 d . . .
H11B H 0.8695 0.7915 0.3825 0.039 Uiso 1 1 calc R . .
C12B C 0.83768(16) 0.69861(18) 0.41873(11) 0.0346(6) Uani 1 1 d . . .
C13B C 0.80551(17) 0.62480(19) 0.41560(11) 0.0372(7) Uani 1 1 d . . .
H13A H 0.7996 0.5968 0.4428 0.045 Uiso 1 1 calc R . .
C14B C 0.78172(16) 0.59153(16) 0.37236(11) 0.0345(6) Uani 1 1 d . . .
H14A H 0.7598 0.5407 0.3699 0.041 Uiso 1 1 calc R . .
Cl1S Cl 0.6667 0.3333 0.3333 0.0461(5) Uani 1 6 d S . .
O1S O 0.7346(2) 0.3895(2) 0.30885(19) 0.0433(11) Uani 0.50 1 d P . .
O2S O 0.6667 0.3333 0.2895(3) 0.060(3) Uani 0.50 3 d SP . .
O1C O 0.66506(18) 0.40954(18) -0.02946(11) 0.0630(8) Uiso 1 1 d . . .
C2C C 0.6198(4) 0.4342(4) -0.0563(2) 0.0889(17) Uiso 1 1 d . . .
H2CA H 0.6187 0.4222 -0.0895 0.133 Uiso 1 1 calc R . .
H2CB H 0.6410 0.4864 -0.0529 0.133 Uiso 1 1 calc R . .
H2CC H 0.5706 0.4098 -0.0439 0.133 Uiso 1 1 calc R . .
O1T O 0.650(3) 0.360(2) -0.1724(11) 0.093(8) Uiso 0.17 1 d P A -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 0.01611(19) 0.01520(18) 0.0403(2) 0.00134(15) 0.00033(15) 0.00816(14)
O111 0.0162(8) 0.0162(8) 0.0355(16) 0.000 0.000 0.0081(4)
O1A 0.0189(8) 0.0221(9) 0.0426(11) -0.0056(8) -0.0002(7) 0.0106(7)
C1A 0.0155(10) 0.0238(11) 0.0338(13) 0.0011(10) 0.0025(9) 0.0094(9)
O2A 0.0189(8) 0.0165(8) 0.0456(11) 0.0034(7) 0.0003(8) 0.0096(7)
C2A 0.0187(11) 0.0225(11) 0.0327(13) -0.0008(10) -0.0002(9) 0.0117(9)
C3A 0.0219(12) 0.0273(13) 0.0437(16) -0.0048(11) -0.0061(11) 0.0122(10)
C4A 0.0241(13) 0.0370(15) 0.0515(18) -0.0056(13) -0.0103(12) 0.0178(12)
C5A 0.0250(13) 0.0353(15) 0.0477(17) 0.0022(12) 0.0005(12) 0.0210(12)
C6A 0.0212(12) 0.0247(12) 0.0448(16) -0.0002(11) 0.0026(11) 0.0125(10)
C21A 0.0183(10) 0.0189(11) 0.0291(12) -0.0013(9) 0.0007(9) 0.0080(9)
N22A 0.0191(9) 0.0177(9) 0.0334(11) 0.0027(8) 0.0018(8) 0.0101(8)
C23A 0.0181(11) 0.0200(11) 0.0354(13) 0.0004(10) -0.0010(10) 0.0089(9)
C24A 0.0302(14) 0.0269(13) 0.0360(14) -0.0025(11) -0.0002(11) 0.0117(11)
C25A 0.0357(16) 0.0334(15) 0.0463(18) -0.0116(13) -0.0043(13) 0.0142(13)
C26A 0.0316(15) 0.0253(14) 0.060(2) -0.0104(13) -0.0075(14) 0.0089(12)
C27A 0.0353(16) 0.0242(14) 0.054(2) 0.0032(13) 0.0058(14) 0.0063(12)
C28A 0.0275(13) 0.0247(13) 0.0405(15) 0.0010(11) 0.0019(11) 0.0092(11)
N1B 0.0233(10) 0.0229(10) 0.0364(12) -0.0011(9) -0.0009(9) 0.0126(9)
C2B 0.0287(13) 0.0274(13) 0.0384(15) 0.0003(11) -0.0007(11) 0.0103(11)
C3B 0.0317(14) 0.0260(13) 0.0391(16) -0.0025(11) 0.0011(12) 0.0077(12)
C4B 0.0287(13) 0.0285(13) 0.0397(15) 0.0004(11) 0.0031(11) 0.0160(11)
C5B 0.0303(13) 0.0246(13) 0.0412(16) 0.0055(11) 0.0058(12) 0.0135(11)
C6B 0.0261(13) 0.0226(12) 0.0454(16) 0.0010(11) 0.0019(11) 0.0132(10)
C7B 0.0353(15) 0.0309(14) 0.0375(15) 0.0041(12) 0.0030(12) 0.0177(12)
C8B 0.0294(14) 0.0301(14) 0.0402(15) 0.0055(12) 0.0027(12) 0.0153(12)
C9B 0.0254(12) 0.0302(13) 0.0358(14) 0.0006(11) 0.0016(11) 0.0148(11)
Cl1B 0.0607(6) 0.0673(6) 0.0392(4) -0.0093(4) -0.0129(4) 0.0328(5)
C10B 0.0261(13) 0.0284(13) 0.0366(14) 0.0056(11) 0.0042(11) 0.0126(11)
C11B 0.0274(13) 0.0322(14) 0.0364(15) 0.0008(11) 0.0024(11) 0.0141(11)
C12B 0.0262(13) 0.0426(16) 0.0360(15) -0.0046(12) -0.0031(11) 0.0179(12)
C13B 0.0338(15) 0.0473(18) 0.0389(16) 0.0116(13) 0.0032(12) 0.0265(14)
C14B 0.0323(14) 0.0277(13) 0.0454(17) 0.0049(12) 0.0031(12) 0.0162(12)
Cl1S 0.0271(5) 0.0271(5) 0.0843(16) 0.000 0.000 0.0135(3)
O1S 0.025(2) 0.029(2) 0.065(3) -0.001(2) 0.000(2) 0.0059(18)
O2S 0.081(4) 0.081(4) 0.019(4) 0.000 0.000 0.040(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1A 1.8587(18) 2_655 ?
Mn1 O111 1.8935(6) . ?
Mn1 O2A 1.9174(18) . ?
Mn1 N22A 2.005(2) 2_655 ?
Mn1 O1C 2.324(3) . ?
Mn1 N1B 2.357(2) . ?
O111 Mn1 1.8936(6) 3_665 ?
O111 Mn1 1.8936(6) 2_655 ?
O1A C1A 1.330(3) . ?
O1A Mn1 1.8587(18) 3_665 ?
C1A C6A 1.403(4) . ?
C1A C2A 1.410(4) . ?
O2A N22A 1.372(3) . ?
C2A C3A 1.415(4) . ?
C2A C21A 1.461(3) . ?
C3A C4A 1.376(4) . ?
C3A H3AA 0.9500 . ?
C4A C5A 1.388(4) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.374(4) . ?
C5A H5AA 0.9500 . ?
C6A H6AA 0.9500 . ?
C21A N22A 1.302(3) . ?
C21A C23A 1.494(3) . ?
N22A Mn1 2.005(2) 3_665 ?
C23A C24A 1.384(4) . ?
C23A C28A 1.389(4) . ?
C24A C25A 1.385(4) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.375(5) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.383(5) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.394(4) . ?
C27A H27A 0.9500 . ?
C28A H28A 0.9500 . ?
N1B C2B 1.334(4) . ?
N1B C6B 1.337(4) . ?
C2B C3B 1.386(4) . ?
C2B H2BA 0.9500 . ?
C3B C4B 1.394(4) . ?
C3B H3BA 0.9500 . ?
C4B C5B 1.396(4) . ?
C4B C7B 1.471(4) . ?
C5B C6B 1.380(4) . ?
C5B H5BA 0.9500 . ?
C6B H6BA 0.9500 . ?
C7B C8B 1.332(4) . ?
C7B H7BA 0.9500 . ?
C8B C9B 1.474(4) . ?
C8B H8BA 0.9500 . ?
C9B C10B 1.389(4) . ?
C9B C14B 1.398(4) . ?
Cl1B C12B 1.739(3) . ?
C10B C11B 1.385(4) . ?
C10B H10A 0.9500 . ?
C11B C12B 1.380(4) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.377(5) . ?
C13B C14B 1.390(5) . ?
C13B H13A 0.9500 . ?
C14B H14A 0.9500 . ?
Cl1S O2S 1.252(8) . ?
Cl1S O2S 1.252(8) 16_655 ?
Cl1S O1S 1.520(5) 3_665 ?
Cl1S O1S 1.519(5) 17 ?
Cl1S O1S 1.519(5) . ?
Cl1S O1S 1.519(5) 16_655 ?
Cl1S O1S 1.520(5) 2_655 ?
Cl1S O1S 1.519(5) 18_545 ?
O1S O2S 1.458(5) . ?
O2S O1S 1.458(5) 3_665 ?
O2S O1S 1.458(5) 2_655 ?
O1C C2C 1.525(7) . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?

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
O1A Mn1 O111 175.81(11) 2_655 . ?
O1A Mn1 O2A 89.19(8) 2_655 . ?
O111 Mn1 O2A 92.32(5) . . ?
O1A Mn1 N22A 89.10(8) 2_655 2_655 ?
O111 Mn1 N22A 89.59(6) . 2_655 ?
O2A Mn1 N22A 176.57(9) . 2_655 ?
O1A Mn1 O1C 83.84(10) 2_655 . ?
O111 Mn1 O1C 92.12(13) . . ?
O2A Mn1 O1C 95.46(10) . . ?
N22A Mn1 O1C 87.31(11) 2_655 . ?
O1A Mn1 N1B 86.11(9) 2_655 . ?
O111 Mn1 N1B 97.81(11) . . ?
O2A Mn1 N1B 89.12(9) . . ?
N22A Mn1 N1B 87.80(9) 2_655 . ?
O1C Mn1 N1B 168.89(10) . . ?
Mn1 O111 Mn1 117.96(5) 3_665 . ?
Mn1 O111 Mn1 117.96(5) 3_665 2_655 ?
Mn1 O111 Mn1 117.96(5) . 2_655 ?
C1A O1A Mn1 126.13(16) . 3_665 ?
O1A C1A C6A 117.1(2) . . ?
O1A C1A C2A 123.3(2) . . ?
C6A C1A C2A 119.6(2) . . ?
N22A O2A Mn1 118.97(14) . . ?
C1A C2A C3A 117.9(2) . . ?
C1A C2A C21A 123.2(2) . . ?
C3A C2A C21A 118.9(2) . . ?
C4A C3A C2A 121.8(3) . . ?
C4A C3A H3AA 119.1 . . ?
C2A C3A H3AA 119.1 . . ?
C3A C4A C5A 119.4(3) . . ?
C3A C4A H4AA 120.3 . . ?
C5A C4A H4AA 120.3 . . ?
C6A C5A C4A 120.6(3) . . ?
C6A C5A H5AA 119.7 . . ?
C4A C5A H5AA 119.7 . . ?
C5A C6A C1A 120.8(3) . . ?
C5A C6A H6AA 119.6 . . ?
C1A C6A H6AA 119.6 . . ?
N22A C21A C2A 121.0(2) . . ?
N22A C21A C23A 120.6(2) . . ?
C2A C21A C23A 118.4(2) . . ?
C21A N22A O2A 116.3(2) . . ?
C21A N22A Mn1 126.75(17) . 3_665 ?
O2A N22A Mn1 116.88(14) . 3_665 ?
C24A C23A C28A 119.6(3) . . ?
C24A C23A C21A 118.2(2) . . ?
C28A C23A C21A 122.0(2) . . ?
C23A C24A C25A 120.4(3) . . ?
C23A C24A H24A 119.8 . . ?
C25A C24A H24A 119.8 . . ?
C26A C25A C24A 120.1(3) . . ?
C26A C25A H25A 119.9 . . ?
C24A C25A H25A 119.9 . . ?
C25A C26A C27A 120.3(3) . . ?
C25A C26A H26A 119.9 . . ?
C27A C26A H26A 119.9 . . ?
C26A C27A C28A 119.8(3) . . ?
C26A C27A H27A 120.1 . . ?
C28A C27A H27A 120.1 . . ?
C23A C28A C27A 119.9(3) . . ?
C23A C28A H28A 120.1 . . ?
C27A C28A H28A 120.1 . . ?
C2B N1B C6B 117.7(3) . . ?
C2B N1B Mn1 116.28(19) . . ?
C6B N1B Mn1 125.95(19) . . ?
N1B C2B C3B 122.6(3) . . ?
N1B C2B H2BA 118.7 . . ?
C3B C2B H2BA 118.7 . . ?
C2B C3B C4B 120.3(3) . . ?
C2B C3B H3BA 119.9 . . ?
C4B C3B H3BA 119.9 . . ?
C3B C4B C5B 116.3(3) . . ?
C3B C4B C7B 122.8(3) . . ?
C5B C4B C7B 120.8(3) . . ?
C6B C5B C4B 119.9(3) . . ?
C6B C5B H5BA 120.1 . . ?
C4B C5B H5BA 120.1 . . ?
N1B C6B C5B 123.2(3) . . ?
N1B C6B H6BA 118.4 . . ?
C5B C6B H6BA 118.4 . . ?
C8B C7B C4B 123.2(3) . . ?
C8B C7B H7BA 118.4 . . ?
C4B C7B H7BA 118.4 . . ?
C7B C8B C9B 128.1(3) . . ?
C7B C8B H8BA 116.0 . . ?
C9B C8B H8BA 116.0 . . ?
C10B C9B C14B 118.6(3) . . ?
C10B C9B C8B 117.3(3) . . ?
C14B C9B C8B 124.1(3) . . ?
C11B C10B C9B 121.6(3) . . ?
C11B C10B H10A 119.2 . . ?
C9B C10B H10A 119.2 . . ?
C12B C11B C10B 118.5(3) . . ?
C12B C11B H11B 120.7 . . ?
C10B C11B H11B 120.7 . . ?
C11B C12B C13B 121.6(3) . . ?
C11B C12B Cl1B 118.4(3) . . ?
C13B C12B Cl1B 120.0(3) . . ?
C12B C13B C14B 119.5(3) . . ?
C12B C13B H13A 120.3 . . ?
C14B C13B H13A 120.3 . . ?
C13B C14B C9B 120.3(3) . . ?
C13B C14B H14A 119.9 . . ?
C9B C14B H14A 119.9 . . ?
O2S Cl1S O2S 179.999(2) . 16_655 ?
O2S Cl1S O1S 62.6(2) . 3_665 ?
O2S Cl1S O1S 117.4(2) 16_655 3_665 ?
O2S Cl1S O1S 117.4(2) . 17 ?
O2S Cl1S O1S 62.6(2) 16_655 17 ?
O1S Cl1S O1S 79.5(2) 3_665 17 ?
O2S Cl1S O1S 62.6(2) . . ?
O2S Cl1S O1S 117.4(2) 16_655 . ?
O1S Cl1S O1S 100.5(2) 3_665 . ?
O1S Cl1S O1S 79.5(3) 17 . ?
O2S Cl1S O1S 117.4(2) . 16_655 ?
O2S Cl1S O1S 62.6(2) 16_655 16_655 ?
O1S Cl1S O1S 79.5(3) 3_665 16_655 ?
O1S Cl1S O1S 100.5(3) 17 16_655 ?
O1S Cl1S O1S 179.999(2) . 16_655 ?
O2S Cl1S O1S 62.6(2) . 2_655 ?
O2S Cl1S O1S 117.4(2) 16_655 2_655 ?
O1S Cl1S O1S 100.5(3) 3_665 2_655 ?
O1S Cl1S O1S 179.996(1) 17 2_655 ?
O1S Cl1S O1S 100.5(2) . 2_655 ?
O1S Cl1S O1S 79.5(3) 16_655 2_655 ?
O2S Cl1S O1S 117.4(2) . 18_545 ?
O2S Cl1S O1S 62.6(2) 16_655 18_545 ?
O1S Cl1S O1S 179.996(2) 3_665 18_545 ?
O1S Cl1S O1S 100.5(3) 17 18_545 ?
O1S Cl1S O1S 79.5(3) . 18_545 ?
O1S Cl1S O1S 100.5(2) 16_655 18_545 ?
O1S Cl1S O1S 79.5(3) 2_655 18_545 ?
O2S O1S Cl1S 49.7(3) . . ?
Cl1S O2S O1S 67.7(3) . 3_665 ?
Cl1S O2S O1S 67.7(3) . . ?
O1S O2S O1S 106.5(4) 3_665 . ?
Cl1S O2S O1S 67.7(3) . 2_655 ?
O1S O2S O1S 106.5(4) 3_665 2_655 ?
O1S O2S O1S 106.5(4) . 2_655 ?
C2C O1C Mn1 121.0(3) . . ?
O1C C2C H2CA 109.5 . . ?
O1C C2C H2CB 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
O1C C2C H2CC 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.814
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.098

# Attachment '_2_.cif'

data_eb9047
_database_code_depnum_ccdc_archive 'CCDC 765868'
#TrackingRef '_2_.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_compound_source        'Ross Inglis'
_exptl_crystal_recrystallization_method 'Slow evaporation of MeOH solution'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C87 H81 Mn3 N6 O10), N O3, OH'
_chemical_formula_sum            'C174 H163 Mn6 N13 O24'
_chemical_formula_weight         3149.81

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   21.4257(4)
_cell_length_b                   21.4257(4)
_cell_length_c                   28.5757(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     11360.5(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8183
_cell_measurement_theta_min      2.6175
_cell_measurement_theta_max      26.3455
_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4920
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7656
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Sphere (omega scans)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41157
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.39
_reflns_number_total             5184
_reflns_number_gt                4519
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    'Shelxs Sheldrick'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_refine_special_details          
;
220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.25 Ratio
222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.34 Ratio
432_ALERT_2_A Short Inter X...Y Contact C3C .. O1S .. 2.64 Ang.
242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C2C
432_ALERT_2_B Short Inter X...Y Contact C3C .. O1S .. 2.72 Ang.
432_ALERT_2_B Short Inter X...Y Contact C3C .. O1S .. 2.79 Ang.
220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.62 Ratio
230_ALERT_2_C Hirshfeld Test Diff for C2C -- C3C .. 5.40 su
232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 -- O1C .. 7.99 su
083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 31.85
301_ALERT_3_G Note Main Residue Disorder .................... 5.00 Perc.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 32

THere is a disordered EtO ligand in this structure. It has been modelled in two
parts with restraints on 1,2 distances and thermal similarity.

911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 2
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 4

The data collection strategy used was to collect fully complete data to
2TH= 53deg. Some higher angle data were collected in the process and these
have been included in the refinement. Please refer to the completeness
statistics below
#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 0.999 2662 2660 2
23.01 0.550 0.999 3534 3532 2
25.24 0.600 1.000 4579 4577 2
#----------------------------------------------------------- ACTA Min. Res. ---
26.39 0.625 0.999 5190 5184 6

041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ?
042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?

They do not really differ. An extra 0.02 oxygen atoms is being calculated by
platon due to rounding errors.

061_ALERT_4_C Tmax/Tmin Range Test RR' too Large ............. 0.88

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc. The crystal was a rather irregular shape, being
a fragment of a larger block; this precluded integration methods for
correcting for absorption.

790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
H O1.02
720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 12
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?

No action taken

302_ALERT_4_G Note Anion/Solvent Disorder .................... 31.00 Perc.

This is due to the OH- and NO3- being disordered over the three fold axis

764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.20 Ratio
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 33.40 Deg.
C2C' -O1C -C2C 1.555 1.555 1.555
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 36.20 Deg.
O1S -O1S -O1S 17.554 1.555 3.665
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 36.20 Deg.
O1S -O1S -O1S 18.544 1.555 2.655
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 31.80 Deg.
O1S -O1S -O1S 3.665 1.555 16.654
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 31.80 Deg.
O1S -O1S -O1S 2.655 1.555 16.654
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 31.80 Deg.
O1S -O1S -H1S 3.665 1.555 1.555
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 31.80 Deg.
O1S -O1S -H1S 2.655 1.555 1.555
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg.
O1S -O1S -H1S 16.654 1.555 1.555

These are the result of disorder. No further action taken
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+31.8479P] 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         5184
_refine_ls_number_parameters     354
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1385
_refine_ls_wR_factor_gt          0.1325
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.68138(2) 0.42710(2) 0.056300(15) 0.02600(14) Uani 1 1 d . . .
O111 O 0.6667 0.3333 0.06592(12) 0.0258(7) Uani 1 3 d S . .
O1A O 0.69393(10) 0.51690(9) 0.04173(7) 0.0284(4) Uani 1 1 d . . .
C1A C 0.65462(14) 0.54483(14) 0.05691(9) 0.0254(5) Uani 1 1 d . . .
C2A C 0.58191(14) 0.50305(14) 0.07067(9) 0.0249(5) Uani 1 1 d . . .
O2A O 0.53140(9) 0.31526(9) 0.05382(7) 0.0286(4) Uani 1 1 d . . .
C3A C 0.54574(15) 0.53928(15) 0.08539(10) 0.0300(6) Uani 1 1 d . . .
H3A H 0.4968 0.5118 0.0949 0.036 Uiso 1 1 calc R . .
C4A C 0.57925(16) 0.61326(15) 0.08637(11) 0.0340(6) Uani 1 1 d . . .
H4A H 0.5537 0.6364 0.0965 0.041 Uiso 1 1 calc R . .
C5A C 0.65100(16) 0.65398(15) 0.07247(10) 0.0324(6) Uani 1 1 d . . .
H5A H 0.6745 0.7051 0.0730 0.039 Uiso 1 1 calc R . .
C6A C 0.68784(15) 0.62025(14) 0.05796(10) 0.0294(6) Uani 1 1 d . . .
H6A H 0.7367 0.6485 0.0485 0.035 Uiso 1 1 calc R . .
C21A C 0.54224(13) 0.42418(14) 0.06895(9) 0.0239(5) Uani 1 1 d . . .
N22A N 0.57482(11) 0.38812(11) 0.05980(8) 0.0242(5) Uani 1 1 d . . .
C23A C 0.46381(14) 0.38512(13) 0.08043(9) 0.0247(5) Uani 1 1 d . . .
C24A C 0.44295(15) 0.35605(15) 0.12485(10) 0.0321(6) Uani 1 1 d . . .
H24A H 0.4780 0.3579 0.1461 0.038 Uiso 1 1 calc R . .
C25A C 0.37138(17) 0.32429(17) 0.13860(11) 0.0393(7) Uani 1 1 d . . .
H25A H 0.3574 0.3045 0.1691 0.047 Uiso 1 1 calc R . .
C26A C 0.32063(16) 0.32158(17) 0.10778(12) 0.0396(7) Uani 1 1 d . . .
H26A H 0.2717 0.3001 0.1172 0.047 Uiso 1 1 calc R . .
C27A C 0.34034(16) 0.34970(17) 0.06345(12) 0.0404(7) Uani 1 1 d . . .
H27A H 0.3049 0.3471 0.0423 0.048 Uiso 1 1 calc R . .
C28A C 0.41210(15) 0.38196(16) 0.04953(10) 0.0326(6) Uani 1 1 d . . .
H28A H 0.4258 0.4018 0.0190 0.039 Uiso 1 1 calc R . .
N1B N 0.69009(12) 0.46096(12) 0.13460(8) 0.0303(5) Uani 1 1 d . . .
C2B C 0.74363(16) 0.52776(15) 0.14527(11) 0.0344(6) Uani 1 1 d . . .
H2B H 0.7710 0.5588 0.1204 0.041 Uiso 1 1 calc R . .
C3B C 0.76068(17) 0.55319(16) 0.19020(11) 0.0378(7) Uani 1 1 d . . .
H3B H 0.7991 0.6008 0.1957 0.045 Uiso 1 1 calc R . .
C4B C 0.72186(16) 0.50947(16) 0.22790(11) 0.0343(6) Uani 1 1 d . . .
C5B C 0.66654(16) 0.44022(16) 0.21671(11) 0.0355(6) Uani 1 1 d . . .
H5B H 0.6388 0.4076 0.2409 0.043 Uiso 1 1 calc R . .
C6B C 0.65226(15) 0.41934(15) 0.17069(11) 0.0327(6) Uani 1 1 d . . .
H6B H 0.6132 0.3725 0.1641 0.039 Uiso 1 1 calc R . .
C7B C 0.73769(17) 0.53368(17) 0.27681(11) 0.0368(7) Uani 1 1 d . . .
H7B H 0.7221 0.4983 0.3008 0.044 Uiso 1 1 calc R . .
C8B C 0.77303(16) 0.60312(16) 0.28907(10) 0.0340(6) Uani 1 1 d . . .
H8B H 0.7865 0.6368 0.2641 0.041 Uiso 1 1 calc R . .
C9B C 0.79358(15) 0.63396(16) 0.33597(10) 0.0316(6) Uani 1 1 d . . .
C10B C 0.82702(15) 0.70822(16) 0.34063(10) 0.0324(6) Uani 1 1 d . . .
H10B H 0.8336 0.7369 0.3137 0.039 Uiso 1 1 calc R . .
C11B C 0.85090(15) 0.74129(16) 0.38355(11) 0.0349(6) Uani 1 1 d . . .
H11B H 0.8748 0.7924 0.3856 0.042 Uiso 1 1 calc R . .
C12B C 0.84037(16) 0.70076(18) 0.42386(11) 0.0371(7) Uani 1 1 d . . .
C13B C 0.80636(17) 0.62608(18) 0.41930(11) 0.0377(7) Uani 1 1 d . . .
H13B H 0.7987 0.5974 0.4464 0.045 Uiso 1 1 calc R . .
C14B C 0.78362(17) 0.59302(17) 0.37653(11) 0.0372(7) Uani 1 1 d . . .
H14B H 0.7610 0.5420 0.3744 0.045 Uiso 1 1 calc R . .
C15B C 0.8653(2) 0.7371(2) 0.47052(12) 0.0551(9) Uani 1 1 d . . .
H15A H 0.8235 0.7233 0.4908 0.083 Uiso 1 1 calc R . .
H15B H 0.8915 0.7895 0.4662 0.083 Uiso 1 1 calc R . .
H15C H 0.8973 0.7222 0.4850 0.083 Uiso 1 1 calc R . .
O1C O 0.66344(17) 0.40751(16) -0.02510(10) 0.0673(8) Uani 1 1 d DU . .
C2C C 0.6186(5) 0.4281(5) -0.0512(3) 0.058(2) Uani 0.613(13) 1 d PDU A 1
H2C1 H 0.6456 0.4747 -0.0679 0.070 Uiso 0.613(13) 1 calc PR A 1
H2C2 H 0.5779 0.4254 -0.0331 0.070 Uiso 0.613(13) 1 calc PR A 1
C3C C 0.5971(7) 0.3573(5) -0.0838(4) 0.125(5) Uani 0.613(13) 1 d PDU A 1
H3C1 H 0.5633 0.3536 -0.1082 0.187 Uiso 0.613(13) 1 calc PR A 1
H3C2 H 0.5744 0.3138 -0.0643 0.187 Uiso 0.613(13) 1 calc PR A 1
H3C3 H 0.6407 0.3620 -0.0983 0.187 Uiso 0.613(13) 1 calc PR A 1
C2C' C 0.6331(9) 0.4061(10) -0.0662(4) 0.113(5) Uani 0.387(13) 1 d PDU A 2
H2C3 H 0.5884 0.3598 -0.0722 0.136 Uiso 0.387(13) 1 calc PR A 2
H2C4 H 0.6668 0.4186 -0.0929 0.136 Uiso 0.387(13) 1 calc PR A 2
C3C' C 0.6193(10) 0.4645(11) -0.0534(8) 0.120(6) Uani 0.387(13) 1 d PDU A 2
H3C4 H 0.5928 0.4718 -0.0787 0.180 Uiso 0.387(13) 1 calc PR A 2
H3C5 H 0.6653 0.5090 -0.0484 0.180 Uiso 0.387(13) 1 calc PR A 2
H3C6 H 0.5907 0.4516 -0.0246 0.180 Uiso 0.387(13) 1 calc PR A 2
N1S N 0.6667 0.3333 0.3333 0.069(2) Uani 1 6 d S . .
O2S O 0.6781(5) 0.3938(4) 0.3483(3) 0.095(2) Uani 0.50 1 d P . .
O1S O 0.6410(14) 0.3507(15) -0.1722(7) 0.061(5) Uiso 0.17 1 d P . .
H1S H 0.6667 0.3333 -0.1667 0.092 Uiso 1 6 d S . .

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 0.0163(2) 0.0153(2) 0.0468(3) 0.00056(16) 0.00043(16) 0.00826(16)
O111 0.0169(9) 0.0169(9) 0.0435(19) 0.000 0.000 0.0085(5)
O1A 0.0220(9) 0.0205(9) 0.0446(11) 0.0038(8) 0.0052(8) 0.0120(8)
C1A 0.0261(13) 0.0230(13) 0.0307(13) 0.0024(10) -0.0014(10) 0.0150(11)
C2A 0.0243(13) 0.0217(13) 0.0297(13) 0.0005(10) -0.0005(10) 0.0123(11)
O2A 0.0187(9) 0.0155(8) 0.0508(12) -0.0017(8) -0.0027(8) 0.0080(7)
C3A 0.0258(14) 0.0266(14) 0.0393(15) 0.0010(11) 0.0055(11) 0.0144(11)
C4A 0.0357(16) 0.0270(14) 0.0453(17) -0.0015(12) 0.0043(13) 0.0201(13)
C5A 0.0352(15) 0.0202(13) 0.0421(16) -0.0005(11) -0.0035(12) 0.0140(12)
C6A 0.0251(13) 0.0215(13) 0.0405(16) 0.0041(11) 0.0000(11) 0.0109(11)
C21A 0.0208(12) 0.0234(13) 0.0286(13) 0.0012(10) -0.0006(10) 0.0120(11)
N22A 0.0205(10) 0.0158(10) 0.0354(12) 0.0017(8) -0.0004(9) 0.0085(9)
C23A 0.0204(12) 0.0209(12) 0.0348(14) -0.0016(10) 0.0009(10) 0.0118(10)
C24A 0.0292(14) 0.0326(15) 0.0358(15) 0.0019(12) 0.0006(11) 0.0166(12)
C25A 0.0357(16) 0.0383(17) 0.0428(17) 0.0049(13) 0.0101(13) 0.0177(14)
C26A 0.0240(14) 0.0354(16) 0.059(2) 0.0006(14) 0.0096(13) 0.0143(13)
C27A 0.0253(15) 0.0409(17) 0.056(2) -0.0016(14) -0.0044(13) 0.0173(13)
C28A 0.0269(14) 0.0372(16) 0.0354(15) 0.0028(12) 0.0005(11) 0.0173(13)
N1B 0.0260(12) 0.0256(12) 0.0424(13) -0.0010(10) -0.0003(10) 0.0152(10)
C2B 0.0293(15) 0.0268(14) 0.0420(16) 0.0006(12) 0.0015(12) 0.0101(12)
C3B 0.0327(15) 0.0285(15) 0.0437(17) -0.0030(12) 0.0000(13) 0.0088(13)
C4B 0.0318(15) 0.0331(15) 0.0424(16) 0.0009(12) 0.0040(12) 0.0195(13)
C5B 0.0350(16) 0.0305(15) 0.0448(17) 0.0045(12) 0.0082(13) 0.0192(13)
C6B 0.0255(14) 0.0237(14) 0.0490(17) -0.0001(12) 0.0029(12) 0.0124(12)
C7B 0.0371(16) 0.0356(16) 0.0391(16) 0.0035(13) 0.0060(13) 0.0192(14)
C8B 0.0310(15) 0.0372(16) 0.0362(16) 0.0035(12) 0.0030(12) 0.0188(13)
C9B 0.0254(14) 0.0346(15) 0.0380(15) 0.0033(12) 0.0034(11) 0.0173(12)
C10B 0.0261(14) 0.0337(15) 0.0359(15) 0.0053(12) 0.0054(11) 0.0139(12)
C11B 0.0243(14) 0.0334(15) 0.0446(17) 0.0002(12) 0.0014(12) 0.0126(12)
C12B 0.0272(15) 0.0515(19) 0.0373(16) -0.0023(13) -0.0031(12) 0.0231(14)
C13B 0.0377(16) 0.0480(18) 0.0360(16) 0.0112(13) 0.0037(12) 0.0277(15)
C14B 0.0351(16) 0.0364(16) 0.0451(17) 0.0057(13) 0.0040(13) 0.0216(14)
C15B 0.055(2) 0.068(3) 0.0444(19) -0.0053(17) -0.0106(16) 0.032(2)
O1C 0.0734(19) 0.0649(18) 0.0620(17) -0.0047(14) -0.0039(14) 0.0332(16)
C2C 0.069(4) 0.065(5) 0.042(3) -0.008(3) -0.004(3) 0.035(4)
C3C 0.156(10) 0.091(7) 0.089(7) -0.006(5) -0.024(7) 0.033(7)
C2C' 0.090(8) 0.098(8) 0.073(7) -0.033(7) 0.000(6) -0.011(7)
C3C' 0.064(9) 0.136(14) 0.130(13) 0.004(12) 0.003(9) 0.027(10)
N1S 0.045(3) 0.045(3) 0.117(8) 0.000 0.000 0.0224(14)
O2S 0.104(6) 0.058(4) 0.124(7) 0.013(4) 0.005(6) 0.041(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1A 1.8520(18) . ?
Mn1 O111 1.8916(6) . ?
Mn1 O2A 1.9143(18) 3_665 ?
Mn1 N22A 2.003(2) . ?
Mn1 N1B 2.331(2) . ?
Mn1 O1C 2.361(3) . ?
O111 Mn1 1.8916(6) 3_665 ?
O111 Mn1 1.8916(6) 2_655 ?
O1A C1A 1.326(3) . ?
C1A C6A 1.403(4) . ?
C1A C2A 1.410(4) . ?
C2A C3A 1.408(4) . ?
C2A C21A 1.464(4) . ?
O2A N22A 1.371(3) . ?
O2A Mn1 1.9144(18) 2_655 ?
C3A C4A 1.375(4) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.393(4) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.374(4) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C21A N22A 1.301(3) . ?
C21A C23A 1.492(3) . ?
C23A C24A 1.386(4) . ?
C23A C28A 1.392(4) . ?
C24A C25A 1.388(4) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.378(5) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.375(5) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.392(4) . ?
C27A H27A 0.9500 . ?
C28A H28A 0.9500 . ?
N1B C6B 1.339(4) . ?
N1B C2B 1.347(4) . ?
C2B C3B 1.371(4) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.397(4) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.396(4) . ?
C4B C7B 1.470(4) . ?
C5B C6B 1.374(4) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C7B C8B 1.335(4) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.461(4) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.387(4) . ?
C9B C14B 1.404(4) . ?
C10B C11B 1.380(4) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.391(4) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.394(5) . ?
C12B C15B 1.501(5) . ?
C13B C14B 1.374(4) . ?
C13B H13B 0.9500 . ?
C14B H14B 0.9500 . ?
C15B H15A 0.9800 . ?
C15B H15B 0.9800 . ?
C15B H15C 0.9800 . ?
O1C C2C' 1.335(9) . ?
O1C C2C 1.449(7) . ?
C2C C3C 1.638(8) . ?
C2C H2C1 0.9900 . ?
C2C H2C2 0.9900 . ?
C3C H3C1 0.9800 . ?
C3C H3C2 0.9800 . ?
C3C H3C3 0.9800 . ?
C2C' C3C' 1.469(10) . ?
C2C' H2C3 0.9900 . ?
C2C' H2C4 0.9900 . ?
C3C' H3C4 0.9800 . ?
C3C' H3C5 0.9800 . ?
C3C' H3C6 0.9800 . ?
N1S O2S 1.267(7) 18_545 ?
N1S O2S 1.267(7) . ?
N1S O2S 1.267(7) 3_665 ?
N1S O2S 1.267(7) 2_655 ?
N1S O2S 1.267(7) 17 ?
N1S O2S 1.267(7) 16_655 ?
O2S O2S 1.468(11) 18_545 ?
O2S O2S 1.468(11) 17 ?
O1S O1S 0.863(17) 17_554 ?
O1S O1S 0.863(17) 18_544 ?
O1S O1S 1.39(2) 3_665 ?
O1S O1S 1.39(2) 2_655 ?
O1S O1S 1.64(3) 16_654 ?
O1S H1S 0.819(13) . ?

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
O1A Mn1 O111 175.27(12) . . ?
O1A Mn1 O2A 88.40(8) . 3_665 ?
O111 Mn1 O2A 92.41(5) . 3_665 ?
O1A Mn1 N22A 89.29(8) . . ?
O111 Mn1 N22A 90.00(6) . . ?
O2A Mn1 N22A 177.35(8) 3_665 . ?
O1A Mn1 N1B 86.85(8) . . ?
O111 Mn1 N1B 97.81(12) . . ?
O2A Mn1 N1B 89.78(8) 3_665 . ?
N22A Mn1 N1B 88.80(9) . . ?
O1A Mn1 O1C 83.65(10) . . ?
O111 Mn1 O1C 91.63(12) . . ?
O2A Mn1 O1C 95.34(10) 3_665 . ?
N22A Mn1 O1C 85.69(10) . . ?
N1B Mn1 O1C 169.07(9) . . ?
Mn1 O111 Mn1 117.92(5) 3_665 . ?
Mn1 O111 Mn1 117.92(5) 3_665 2_655 ?
Mn1 O111 Mn1 117.93(5) . 2_655 ?
C1A O1A Mn1 126.86(17) . . ?
O1A C1A C6A 117.1(2) . . ?
O1A C1A C2A 123.6(2) . . ?
C6A C1A C2A 119.2(2) . . ?
C3A C2A C1A 118.1(2) . . ?
C3A C2A C21A 119.0(2) . . ?
C1A C2A C21A 122.9(2) . . ?
N22A O2A Mn1 119.36(14) . 2_655 ?
C4A C3A C2A 121.8(3) . . ?
C4A C3A H3A 119.1 . . ?
C2A C3A H3A 119.1 . . ?
C3A C4A C5A 119.5(3) . . ?
C3A C4A H4A 120.2 . . ?
C5A C4A H4A 120.2 . . ?
C6A C5A C4A 120.1(3) . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C6A C1A 121.2(3) . . ?
C5A C6A H6A 119.4 . . ?
C1A C6A H6A 119.4 . . ?
N22A C21A C2A 121.2(2) . . ?
N22A C21A C23A 120.0(2) . . ?
C2A C21A C23A 118.8(2) . . ?
C21A N22A O2A 116.2(2) . . ?
C21A N22A Mn1 126.92(18) . . ?
O2A N22A Mn1 116.84(14) . . ?
C24A C23A C28A 119.3(2) . . ?
C24A C23A C21A 118.2(2) . . ?
C28A C23A C21A 122.3(2) . . ?
C23A C24A C25A 120.6(3) . . ?
C23A C24A H24A 119.7 . . ?
C25A C24A H24A 119.7 . . ?
C26A C25A C24A 119.7(3) . . ?
C26A C25A H25A 120.2 . . ?
C24A C25A H25A 120.2 . . ?
C27A C26A C25A 120.5(3) . . ?
C27A C26A H26A 119.8 . . ?
C25A C26A H26A 119.8 . . ?
C26A C27A C28A 120.1(3) . . ?
C26A C27A H27A 119.9 . . ?
C28A C27A H27A 119.9 . . ?
C23A C28A C27A 119.8(3) . . ?
C23A C28A H28A 120.1 . . ?
C27A C28A H28A 120.1 . . ?
C6B N1B C2B 116.3(3) . . ?
C6B N1B Mn1 127.19(19) . . ?
C2B N1B Mn1 116.16(19) . . ?
N1B C2B C3B 123.4(3) . . ?
N1B C2B H2B 118.3 . . ?
C3B C2B H2B 118.3 . . ?
C2B C3B C4B 120.3(3) . . ?
C2B C3B H3B 119.8 . . ?
C4B C3B H3B 119.8 . . ?
C5B C4B C3B 116.1(3) . . ?
C5B C4B C7B 121.1(3) . . ?
C3B C4B C7B 122.8(3) . . ?
C6B C5B C4B 119.9(3) . . ?
C6B C5B H5B 120.1 . . ?
C4B C5B H5B 120.1 . . ?
N1B C6B C5B 123.9(3) . . ?
N1B C6B H6B 118.0 . . ?
C5B C6B H6B 118.0 . . ?
C8B C7B C4B 123.0(3) . . ?
C8B C7B H7B 118.5 . . ?
C4B C7B H7B 118.5 . . ?
C7B C8B C9B 128.3(3) . . ?
C7B C8B H8B 115.9 . . ?
C9B C8B H8B 115.9 . . ?
C10B C9B C14B 117.9(3) . . ?
C10B C9B C8B 118.2(3) . . ?
C14B C9B C8B 123.9(3) . . ?
C11B C10B C9B 121.4(3) . . ?
C11B C10B H10B 119.3 . . ?
C9B C10B H10B 119.3 . . ?
C10B C11B C12B 120.8(3) . . ?
C10B C11B H11B 119.6 . . ?
C12B C11B H11B 119.6 . . ?
C11B C12B C13B 117.9(3) . . ?
C11B C12B C15B 120.5(3) . . ?
C13B C12B C15B 121.6(3) . . ?
C14B C13B C12B 121.5(3) . . ?
C14B C13B H13B 119.3 . . ?
C12B C13B H13B 119.3 . . ?
C13B C14B C9B 120.5(3) . . ?
C13B C14B H14B 119.7 . . ?
C9B C14B H14B 119.7 . . ?
C12B C15B H15A 109.5 . . ?
C12B C15B H15B 109.5 . . ?
H15A C15B H15B 109.5 . . ?
C12B C15B H15C 109.5 . . ?
H15A C15B H15C 109.5 . . ?
H15B C15B H15C 109.5 . . ?
C2C' O1C C2C 33.4(8) . . ?
C2C' O1C Mn1 154.8(9) . . ?
C2C O1C Mn1 121.8(4) . . ?
O1C C2C C3C 86.1(6) . . ?
O1C C2C H2C1 114.3 . . ?
C3C C2C H2C1 114.3 . . ?
O1C C2C H2C2 114.3 . . ?
C3C C2C H2C2 114.3 . . ?
H2C1 C2C H2C2 111.4 . . ?
C2C C3C H3C1 109.5 . . ?
C2C C3C H3C2 109.5 . . ?
H3C1 C3C H3C2 109.5 . . ?
C2C C3C H3C3 109.5 . . ?
H3C1 C3C H3C3 109.5 . . ?
H3C2 C3C H3C3 109.5 . . ?
O1C C2C' C3C' 93.7(13) . . ?
O1C C2C' H2C3 113.0 . . ?
C3C' C2C' H2C3 113.0 . . ?
O1C C2C' H2C4 113.0 . . ?
C3C' C2C' H2C4 113.0 . . ?
H2C3 C2C' H2C4 110.4 . . ?
C2C' C3C' H3C4 109.5 . . ?
C2C' C3C' H3C5 109.5 . . ?
H3C4 C3C' H3C5 109.5 . . ?
C2C' C3C' H3C6 109.5 . . ?
H3C4 C3C' H3C6 109.5 . . ?
H3C5 C3C' H3C6 109.5 . . ?
O2S N1S O2S 70.8(4) 18_545 . ?
O2S N1S O2S 179.991(4) 18_545 3_665 ?
O2S N1S O2S 109.2(4) . 3_665 ?
O2S N1S O2S 70.8(4) 18_545 2_655 ?
O2S N1S O2S 109.2(4) . 2_655 ?
O2S N1S O2S 109.2(4) 3_665 2_655 ?
O2S N1S O2S 109.2(4) 18_545 17 ?
O2S N1S O2S 70.8(4) . 17 ?
O2S N1S O2S 70.8(4) 3_665 17 ?
O2S N1S O2S 179.995(2) 2_655 17 ?
O2S N1S O2S 109.2(4) 18_545 16_655 ?
O2S N1S O2S 179.993(1) . 16_655 ?
O2S N1S O2S 70.8(4) 3_665 16_655 ?
O2S N1S O2S 70.8(4) 2_655 16_655 ?
O2S N1S O2S 109.2(4) 17 16_655 ?
N1S O2S O2S 54.58(19) . 18_545 ?
N1S O2S O2S 54.59(19) . 17 ?
O2S O2S O2S 89.4(8) 18_545 17 ?
O1S O1S O1S 108(3) 17_554 18_544 ?
O1S O1S O1S 36.2(13) 17_554 3_665 ?
O1S O1S O1S 89.997(6) 18_544 3_665 ?
O1S O1S O1S 89.996(6) 17_554 2_655 ?
O1S O1S O1S 36.2(13) 18_544 2_655 ?
O1S O1S O1S 60.001(3) 3_665 2_655 ?
O1S O1S O1S 58.2(4) 17_554 16_654 ?
O1S O1S O1S 58.2(4) 18_544 16_654 ?
O1S O1S O1S 31.8(4) 3_665 16_654 ?
O1S O1S O1S 31.8(4) 2_655 16_654 ?
O1S O1S H1S 58.2(4) 17_554 . ?
O1S O1S H1S 58.2(4) 18_544 . ?
O1S O1S H1S 31.8(4) 3_665 . ?
O1S O1S H1S 31.8(4) 2_655 . ?
O1S O1S H1S 0.0(14) 16_654 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.071

# Attachment '_3_.cif'

data_eb9021
_database_code_depnum_ccdc_archive 'CCDC 765869'
#TrackingRef '_3_.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_compound_source        'Ross Inglis'
_exptl_crystal_recrystallization_method 'Diffusion of Et2O into MeOH solution'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C48 H46 Mn3 N7 O8), 4(C4 H10 O), C2 H8 O2, 4(C H4 O), 4(Cl O4)'
_chemical_formula_sum            'C214 H248 Cl4 Mn12 N28 O58'
_chemical_formula_weight         4941.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.8361(10)
_cell_length_b                   15.6707(6)
_cell_length_c                   30.6046(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.593(2)
_cell_angle_gamma                90.00
_cell_volume                     12325.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7562
_cell_measurement_theta_min      2.2965
_cell_measurement_theta_max      25.9925
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5120
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7252
_exptl_absorpt_correction_T_max  0.8796
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44430
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         23.26
_reflns_number_total             8852
_reflns_number_gt                7602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    'Shelxs Sheldrick'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_refine_special_details          
;
#==========================================================================
The Following Model and Quality ALERTS were generated - (Acta-Mode) <<<
#==========================================================================
Format: alert-number_ALERT_alert-type_alert-level text

601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 348.00 A**3

Squeeze was used to remove some unidentifiable solvent

023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.26 Deg.
213_ALERT_2_B Atom C3E has ADP max/min Ratio ............. 4.20 prola
220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.89 Ratio
241_ALERT_2_B Check High Ueq as Compared to Neighbors for C3E
242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C4E
413_ALERT_2_B Short Inter XH3 .. XHn H8D .. H2R3 .. 1.96 Ang.
420_ALERT_2_B D-H Without Acceptor O1S - H1S ... ?
213_ALERT_2_C Atom C2E has ADP max/min Ratio ............. 3.30 prola
222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.10 Ratio
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C2E
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C8D
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C12E
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1E
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N10D
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N10E
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C7E
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 154

There is significant absorption with this dataset. Restraints have been
applied to try and produce more appropriate ADP's. For most ADP's are
quite reasonable.

341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 12
083_ALERT_2_G SHELXL Second Parameter in WGHT unusually Large. 177.35

Again, absorption is significant and higer angle data were very weak and
therefore a cutoff was applied.

360_ALERT_2_C Short C(sp3)-C(sp3) Bond C1T - C2T ... 1.42 Ang.
360_ALERT_2_C Short C(sp3)-C(sp3) Bond C4T - C5T ... 1.42 Ang.

This is a solvent Et2O molecule. It's geometry is slightly poor.

410_ALERT_2_C Short Intra H...H Contact H3A .. H23B .. 1.95 Ang.
410_ALERT_2_C Short Intra H...H Contact H3C .. H23F .. 1.98 Ang.

As there are intramolecular, I checked for the possibility of deprotonation.
These H must be there for charge balance.

910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 5
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.556 4

The data collection strategy used was to collect fully complete data to
2TH= 53deg. Upon refinement a cutoff at 0.9 was considered appropriate.
Please refer to the completeness statistics below

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 0.999 6453 6444 9
23.01 0.550 0.999 8599 8590 9
23.26 0.556 0.999 8861 8852 9
#----------------------------------------------------------- ACTA Min. Res. ---

062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.18
125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1U

This is a ClO4 molecule which has some rotational motion.

302_ALERT_4_G Note Anion/Solvent Disorder .................... 7.00 Perc.

One of the MeOH molecules is 0.5 occupancy.

720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 19
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?

No action taken
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+177.3497P] 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         8852
_refine_ls_number_parameters     656
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0877
_refine_ls_wR_factor_ref         0.2261
_refine_ls_wR_factor_gt          0.2198
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_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 0.16147(4) 0.82071(6) 0.14787(3) 0.0235(3) Uani 1 1 d . . .
Mn2 Mn 0.11325(4) 0.63699(6) 0.10365(4) 0.0246(3) Uani 1 1 d . . .
Mn3 Mn 0.03982(4) 0.80879(6) 0.07648(4) 0.0253(3) Uani 1 1 d . . .
O123 O 0.10423(17) 0.7544(3) 0.10835(15) 0.0268(10) Uani 1 1 d . . .
O1A O -0.02339(18) 0.8620(3) 0.04227(17) 0.0335(11) Uani 1 1 d . . .
C1A C -0.0695(3) 0.8285(4) 0.0215(2) 0.0314(15) Uani 1 1 d U . .
O2A O 0.04533(18) 0.6289(3) 0.05706(17) 0.0337(11) Uani 1 1 d . . .
C2A C -0.0781(3) 0.7418(5) 0.0069(3) 0.0373(16) Uani 1 1 d U . .
C3A C -0.1300(3) 0.7172(6) -0.0195(3) 0.052(2) Uani 1 1 d U . .
H3A H -0.1366 0.6603 -0.0310 0.063 Uiso 1 1 calc R . .
C4A C -0.1705(3) 0.7711(6) -0.0290(4) 0.061(2) Uani 1 1 d U . .
H4A H -0.2048 0.7523 -0.0473 0.073 Uiso 1 1 calc R . .
C5A C -0.1619(3) 0.8545(5) -0.0121(3) 0.052(2) Uani 1 1 d U . .
H5A H -0.1904 0.8921 -0.0177 0.063 Uiso 1 1 calc R . .
C6A C -0.1123(3) 0.8818(5) 0.0127(3) 0.0401(17) Uani 1 1 d U . .
H6A H -0.1067 0.9387 0.0243 0.048 Uiso 1 1 calc R . .
C21A C -0.0361(3) 0.6777(4) 0.0187(2) 0.0270(15) Uani 1 1 d . . .
N22A N 0.0098(2) 0.6963(3) 0.04782(19) 0.0266(13) Uani 1 1 d . . .
C23A C -0.0479(3) 0.5883(5) -0.0001(3) 0.0416(19) Uani 1 1 d . . .
H23A H -0.0181 0.5663 -0.0068 0.050 Uiso 1 1 calc R . .
H23B H -0.0787 0.5892 -0.0302 0.050 Uiso 1 1 calc R . .
C24A C -0.0584(4) 0.5278(6) 0.0344(4) 0.058(2) Uani 1 1 d . . .
H24A H -0.0649 0.4702 0.0208 0.088 Uiso 1 1 calc R . .
H24B H -0.0890 0.5476 0.0400 0.088 Uiso 1 1 calc R . .
H24C H -0.0281 0.5267 0.0644 0.088 Uiso 1 1 calc R . .
O1B O 0.11109(19) 0.5196(3) 0.11154(18) 0.0373(12) Uani 1 1 d . . .
C1B C 0.1464(3) 0.4667(4) 0.1393(2) 0.0324(15) Uani 1 1 d U . .
O2B O 0.20178(17) 0.7204(3) 0.17233(16) 0.0279(10) Uani 1 1 d . . .
C2B C 0.1940(3) 0.4891(4) 0.1743(2) 0.0304(15) Uani 1 1 d U . .
C3B C 0.2269(3) 0.4235(5) 0.2004(3) 0.0417(17) Uani 1 1 d U . .
H3B H 0.2598 0.4386 0.2238 0.050 Uiso 1 1 calc R . .
C4B C 0.2138(4) 0.3387(5) 0.1938(3) 0.051(2) Uani 1 1 d U . .
H4B H 0.2370 0.2959 0.2121 0.061 Uiso 1 1 calc R . .
C5B C 0.1662(4) 0.3176(5) 0.1602(3) 0.053(2) Uani 1 1 d U . .
H5B H 0.1561 0.2594 0.1557 0.064 Uiso 1 1 calc R . .
C6B C 0.1330(3) 0.3787(5) 0.1331(3) 0.0447(18) Uani 1 1 d U . .
H6B H 0.1004 0.3621 0.1097 0.054 Uiso 1 1 calc R . .
C21B C 0.2105(3) 0.5795(4) 0.1848(2) 0.0296(16) Uani 1 1 d . . .
N22B N 0.1804(2) 0.6397(3) 0.15977(19) 0.0279(13) Uani 1 1 d . . .
C23B C 0.2613(3) 0.6000(4) 0.2236(3) 0.0340(17) Uani 1 1 d . . .
H23C H 0.2684 0.5584 0.2497 0.041 Uiso 1 1 calc R . .
H23D H 0.2597 0.6576 0.2361 0.041 Uiso 1 1 calc R . .
C24B C 0.3054(3) 0.5966(6) 0.2049(3) 0.057(2) Uani 1 1 d . . .
H24D H 0.3386 0.6102 0.2306 0.085 Uiso 1 1 calc R . .
H24E H 0.2985 0.6382 0.1793 0.085 Uiso 1 1 calc R . .
H24F H 0.3072 0.5392 0.1929 0.085 Uiso 1 1 calc R . .
O1C O 0.21552(17) 0.8872(3) 0.18792(16) 0.0283(10) Uani 1 1 d . . .
C1C C 0.2301(3) 0.9624(4) 0.1765(2) 0.0289(14) Uani 1 1 d U . .
O2C O 0.06845(17) 0.9174(3) 0.10259(16) 0.0296(11) Uani 1 1 d . . .
C2C C 0.1944(3) 1.0226(4) 0.1470(2) 0.0290(14) Uani 1 1 d U . .
C3C C 0.2148(3) 1.1007(5) 0.1402(3) 0.0393(16) Uani 1 1 d U . .
H3C H 0.1918 1.1419 0.1202 0.047 Uiso 1 1 calc R . .
C4C C 0.2663(3) 1.1203(5) 0.1611(3) 0.0467(18) Uani 1 1 d U . .
H4C H 0.2783 1.1750 0.1565 0.056 Uiso 1 1 calc R . .
C5C C 0.3009(3) 1.0608(5) 0.1887(3) 0.0441(17) Uani 1 1 d U . .
H5C H 0.3370 1.0735 0.2025 0.053 Uiso 1 1 calc R . .
C6C C 0.2826(3) 0.9818(5) 0.1963(3) 0.0380(16) Uani 1 1 d U . .
H6C H 0.3066 0.9407 0.2154 0.046 Uiso 1 1 calc R . .
C21C C 0.1382(3) 1.0060(4) 0.1246(2) 0.0271(15) Uani 1 1 d . . .
N22C N 0.1216(2) 0.9271(3) 0.12165(19) 0.0265(13) Uani 1 1 d . . .
C23C C 0.0998(3) 1.0771(4) 0.1083(3) 0.0410(19) Uani 1 1 d . . .
H23E H 0.0688 1.0576 0.0810 0.049 Uiso 1 1 calc R . .
H23F H 0.1155 1.1254 0.0976 0.049 Uiso 1 1 calc R . .
C24C C 0.0834(4) 1.1065(6) 0.1471(3) 0.057(2) Uani 1 1 d . . .
H24G H 0.0583 1.1532 0.1354 0.086 Uiso 1 1 calc R . .
H24H H 0.1140 1.1267 0.1739 0.086 Uiso 1 1 calc R . .
H24I H 0.0673 1.0589 0.1573 0.086 Uiso 1 1 calc R . .
N1D N 0.0026(2) 0.7977(3) 0.1338(2) 0.0291(13) Uani 1 1 d . . .
C2D C -0.0079(3) 0.7285(5) 0.1534(3) 0.046(2) Uani 1 1 d . . .
H2D H 0.0041 0.6752 0.1468 0.056 Uiso 1 1 calc R . .
C3D C -0.0349(4) 0.7285(5) 0.1826(3) 0.048(2) Uani 1 1 d . . .
H3D H -0.0409 0.6764 0.1956 0.058 Uiso 1 1 calc R . .
C4D C -0.0535(3) 0.8052(4) 0.1931(2) 0.0299(16) Uani 1 1 d . . .
C5D C -0.0435(3) 0.8757(5) 0.1727(3) 0.0400(19) Uani 1 1 d . . .
H5D H -0.0557 0.9297 0.1783 0.048 Uiso 1 1 calc R . .
C6D C -0.0154(3) 0.8705(5) 0.1433(3) 0.0418(19) Uani 1 1 d . . .
H6D H -0.0091 0.9215 0.1295 0.050 Uiso 1 1 calc R . .
C7D C -0.0815(3) 0.8091(4) 0.2255(2) 0.0287(15) Uani 1 1 d . . .
C8D C -0.0991(4) 0.7372(5) 0.2405(3) 0.055(2) Uani 1 1 d . . .
H8D H -0.0946 0.6828 0.2290 0.066 Uiso 1 1 calc R . .
C9D C -0.1231(4) 0.7433(5) 0.2721(3) 0.050(2) Uani 1 1 d . . .
H9D H -0.1352 0.6923 0.2811 0.060 Uiso 1 1 calc R . .
N10D N -0.1304(2) 0.8165(3) 0.2908(2) 0.0283(13) Uani 1 1 d . . .
C11D C -0.1150(3) 0.8857(5) 0.2752(3) 0.045(2) Uani 1 1 d . . .
H11D H -0.1210 0.9393 0.2867 0.054 Uiso 1 1 calc R . .
C12D C -0.0909(3) 0.8855(5) 0.2434(3) 0.047(2) Uani 1 1 d . . .
H12D H -0.0807 0.9378 0.2338 0.056 Uiso 1 1 calc R . .
N1E N 0.1545(2) 0.6326(4) 0.0540(2) 0.0291(13) Uani 1 1 d . . .
C2E C 0.1952(4) 0.5848(9) 0.0607(4) 0.096(5) Uani 1 1 d . . .
H2E H 0.2062 0.5473 0.0872 0.116 Uiso 1 1 calc R . .
C3E C 0.2235(4) 0.5848(9) 0.0321(4) 0.106(6) Uani 1 1 d . . .
H3E H 0.2531 0.5491 0.0393 0.127 Uiso 1 1 calc R . .
C5E C 0.1636(3) 0.6824(6) -0.0151(3) 0.049(2) Uani 1 1 d . . .
H5E H 0.1499 0.7181 -0.0422 0.059 Uiso 1 1 calc R . .
C4E C 0.2079(3) 0.6376(4) -0.0071(2) 0.0286(15) Uani 1 1 d . . .
C6E C 0.1384(3) 0.6769(6) 0.0153(3) 0.049(2) Uani 1 1 d . . .
H6E H 0.1068 0.7078 0.0075 0.058 Uiso 1 1 calc R . .
C7E C 0.2381(3) 0.6435(4) -0.0381(2) 0.0277(15) Uani 1 1 d . . .
C8E C 0.2866(3) 0.6082(5) -0.0249(3) 0.0421(19) Uani 1 1 d . . .
H8E H 0.3012 0.5765 0.0036 0.051 Uiso 1 1 calc R . .
C9E C 0.3140(3) 0.6195(5) -0.0538(3) 0.0400(19) Uani 1 1 d . . .
H9E H 0.3474 0.5940 -0.0444 0.048 Uiso 1 1 calc R . .
N10E N 0.2966(2) 0.6636(4) -0.0937(2) 0.0306(13) Uani 1 1 d . . .
C11E C 0.2500(4) 0.6959(6) -0.1059(3) 0.063(3) Uani 1 1 d . . .
H11E H 0.2359 0.7261 -0.1350 0.075 Uiso 1 1 calc R . .
C12E C 0.2206(4) 0.6891(7) -0.0799(3) 0.067(3) Uani 1 1 d . . .
H12E H 0.1875 0.7160 -0.0904 0.081 Uiso 1 1 calc R . .
O1F O 0.05749(19) 0.8360(3) 0.00895(17) 0.0353(12) Uani 1 1 d . . .
C2F C 0.0467(4) 0.9242(5) -0.0097(3) 0.052(2) Uani 1 1 d . . .
H2F1 H 0.0553 0.9293 -0.0378 0.077 Uiso 1 1 calc R . .
H2F2 H 0.0679 0.9643 0.0146 0.077 Uiso 1 1 calc R . .
H2F3 H 0.0098 0.9371 -0.0182 0.077 Uiso 1 1 calc R . .
O1S O 0.0303(3) 0.7595(5) -0.0750(3) 0.087(2) Uiso 1 1 d . . .
H1S H 0.0055 0.7858 -0.0720 0.131 Uiso 1 1 d R . .
C2S C 0.0131(5) 0.6831(9) -0.0979(5) 0.101(4) Uiso 1 1 d . . .
H2S1 H 0.0373 0.6622 -0.1118 0.151 Uiso 1 1 d R . .
H2S2 H -0.0215 0.6908 -0.1229 0.151 Uiso 1 1 d R . .
H2S3 H 0.0109 0.6415 -0.0748 0.151 Uiso 1 1 d R . .
C1T C -0.3106(6) 0.8833(9) -0.0615(5) 0.110(4) Uiso 1 1 d U . .
H1T1 H -0.3377 0.9240 -0.0623 0.165 Uiso 1 1 calc R . .
H1T2 H -0.2898 0.9075 -0.0780 0.165 Uiso 1 1 calc R . .
H1T3 H -0.2880 0.8715 -0.0285 0.165 Uiso 1 1 calc R . .
C2T C -0.3343(5) 0.8059(8) -0.0840(5) 0.089(3) Uiso 1 1 d U . .
H2T1 H -0.3559 0.7826 -0.0676 0.106 Uiso 1 1 calc R . .
H2T2 H -0.3576 0.8185 -0.1171 0.106 Uiso 1 1 calc R . .
O3T O -0.2990(3) 0.7456(5) -0.0842(3) 0.081(2) Uiso 1 1 d U . .
C4T C -0.3164(4) 0.6651(7) -0.1029(4) 0.076(3) Uiso 1 1 d U . .
H4T1 H -0.3393 0.6724 -0.1366 0.091 Uiso 1 1 calc R . .
H4T2 H -0.3381 0.6420 -0.0865 0.091 Uiso 1 1 calc R . .
C5T C -0.2784(5) 0.6029(8) -0.1003(5) 0.095(4) Uiso 1 1 d U . .
H5T1 H -0.2957 0.5492 -0.1140 0.142 Uiso 1 1 calc R . .
H5T2 H -0.2555 0.5937 -0.0671 0.142 Uiso 1 1 calc R . .
H5T3 H -0.2577 0.6228 -0.1179 0.142 Uiso 1 1 calc R . .
Cl1U Cl -0.10466(10) 1.10143(16) 0.12220(9) 0.0611(6) Uani 1 1 d U . .
O1U O -0.1032(3) 1.0690(5) 0.1653(3) 0.080(2) Uiso 1 1 d U . .
O2U O -0.1114(5) 1.1875(8) 0.1180(4) 0.143(4) Uiso 1 1 d U . .
O3U O -0.1314(5) 1.0517(8) 0.0838(4) 0.143(4) Uiso 1 1 d U . .
O4U O -0.0511(4) 1.0941(6) 0.1250(3) 0.104(3) Uiso 1 1 d U . .
O1R O 0.0626(6) 0.5086(11) 0.1979(6) 0.088(5) Uiso 0.50 1 d P . .
H1R H 0.0457 0.4645 0.1855 0.132 Uiso 0.50 1 d PR . .
C2R C 0.0472(8) 0.5348(13) 0.2287(7) 0.066(5) Uiso 0.50 1 d P . .
H2R1 H 0.0689 0.5136 0.2603 0.099 Uiso 0.50 1 d PR . .
H2R2 H 0.0111 0.5165 0.2206 0.099 Uiso 0.50 1 d PR . .
H2R3 H 0.0487 0.5972 0.2284 0.099 Uiso 0.50 1 d 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 0.0310(6) 0.0185(5) 0.0293(6) 0.0008(4) 0.0208(5) 0.0009(4)
Mn2 0.0320(6) 0.0197(5) 0.0315(6) 0.0007(4) 0.0226(5) 0.0018(4)
Mn3 0.0304(6) 0.0215(5) 0.0328(6) 0.0001(4) 0.0220(5) 0.0027(4)
O123 0.033(3) 0.021(2) 0.033(3) -0.004(2) 0.020(2) 0.0007(19)
O1A 0.032(3) 0.036(3) 0.041(3) 0.004(2) 0.024(2) 0.003(2)
C1A 0.039(4) 0.024(3) 0.036(4) 0.002(3) 0.019(3) 0.006(3)
O2A 0.038(3) 0.024(3) 0.044(3) -0.005(2) 0.021(2) 0.006(2)
C2A 0.036(3) 0.032(3) 0.043(4) -0.001(3) 0.014(3) 0.002(3)
C3A 0.037(4) 0.044(4) 0.069(5) -0.002(4) 0.013(4) 0.005(3)
C4A 0.036(4) 0.046(4) 0.086(5) 0.003(4) 0.008(4) 0.002(3)
C5A 0.039(4) 0.043(4) 0.075(5) 0.002(4) 0.020(4) 0.011(3)
C6A 0.037(3) 0.036(4) 0.050(4) 0.001(3) 0.020(3) 0.006(3)
C21A 0.030(4) 0.027(4) 0.028(4) -0.006(3) 0.016(3) 0.002(3)
N22A 0.035(3) 0.021(3) 0.032(3) 0.004(2) 0.023(3) 0.008(2)
C23A 0.037(4) 0.037(4) 0.049(5) -0.011(4) 0.015(4) 0.005(3)
C24A 0.054(5) 0.044(5) 0.083(7) -0.009(5) 0.033(5) -0.005(4)
O1B 0.045(3) 0.022(3) 0.046(3) 0.003(2) 0.019(2) -0.001(2)
C1B 0.052(4) 0.022(3) 0.032(3) 0.005(3) 0.024(3) 0.008(3)
O2B 0.031(2) 0.015(2) 0.041(3) 0.007(2) 0.019(2) 0.0001(19)
C2B 0.049(4) 0.020(3) 0.030(3) 0.001(3) 0.024(3) 0.006(3)
C3B 0.060(4) 0.028(3) 0.039(4) 0.003(3) 0.020(3) 0.007(3)
C4B 0.079(5) 0.020(3) 0.049(4) 0.003(3) 0.020(4) 0.013(3)
C5B 0.081(5) 0.022(4) 0.053(4) 0.002(3) 0.022(4) 0.003(4)
C6B 0.066(4) 0.023(3) 0.048(4) 0.001(3) 0.025(4) 0.003(3)
C21B 0.044(4) 0.028(4) 0.028(4) 0.008(3) 0.026(3) 0.004(3)
N22B 0.034(3) 0.028(3) 0.030(3) -0.001(3) 0.021(3) 0.007(3)
C23B 0.050(4) 0.021(4) 0.037(4) 0.010(3) 0.023(4) 0.003(3)
C24B 0.039(5) 0.069(6) 0.062(6) 0.018(5) 0.019(4) 0.009(4)
O1C 0.034(3) 0.023(2) 0.033(3) 0.000(2) 0.018(2) -0.003(2)
C1C 0.040(3) 0.027(3) 0.032(3) -0.004(3) 0.027(3) -0.001(3)
O2C 0.033(3) 0.022(2) 0.040(3) -0.001(2) 0.021(2) 0.000(2)
C2C 0.038(3) 0.025(3) 0.035(3) 0.000(3) 0.027(3) 0.003(3)
C3C 0.047(4) 0.026(3) 0.051(4) 0.004(3) 0.025(3) 0.002(3)
C4C 0.052(4) 0.032(4) 0.064(5) 0.000(3) 0.031(4) -0.007(3)
C5C 0.044(4) 0.037(4) 0.062(4) -0.003(3) 0.033(3) -0.008(3)
C6C 0.040(4) 0.032(4) 0.051(4) -0.003(3) 0.027(3) -0.004(3)
C21C 0.043(4) 0.017(3) 0.029(4) 0.000(3) 0.023(3) 0.002(3)
N22C 0.030(3) 0.025(3) 0.032(3) -0.004(2) 0.021(3) -0.001(2)
C23C 0.046(4) 0.016(4) 0.058(5) 0.001(3) 0.017(4) 0.005(3)
C24C 0.059(5) 0.041(5) 0.082(7) -0.006(5) 0.038(5) 0.020(4)
N1D 0.035(3) 0.027(3) 0.032(3) -0.003(3) 0.021(3) 0.004(2)
C2D 0.077(6) 0.025(4) 0.058(5) 0.006(4) 0.050(5) 0.016(4)
C3D 0.084(6) 0.026(4) 0.064(6) 0.004(4) 0.062(5) 0.006(4)
C4D 0.031(4) 0.035(4) 0.027(4) -0.005(3) 0.015(3) -0.003(3)
C5D 0.059(5) 0.026(4) 0.057(5) -0.003(4) 0.046(4) -0.001(3)
C6D 0.060(5) 0.028(4) 0.056(5) -0.002(4) 0.043(4) -0.003(4)
C7D 0.031(4) 0.028(4) 0.032(4) -0.003(3) 0.018(3) 0.002(3)
C8D 0.093(7) 0.032(4) 0.073(6) -0.009(4) 0.070(6) -0.006(4)
C9D 0.085(6) 0.026(4) 0.067(6) -0.008(4) 0.060(5) -0.011(4)
N10D 0.035(3) 0.025(3) 0.033(3) -0.005(3) 0.022(3) -0.004(2)
C11D 0.077(6) 0.023(4) 0.064(5) 0.006(4) 0.058(5) 0.008(4)
C12D 0.079(6) 0.024(4) 0.063(5) 0.010(4) 0.055(5) 0.006(4)
N1E 0.035(3) 0.030(3) 0.030(3) 0.002(3) 0.023(3) 0.009(3)
C2E 0.099(8) 0.148(11) 0.079(7) 0.082(8) 0.074(7) 0.091(8)
C3E 0.093(8) 0.175(13) 0.089(8) 0.094(9) 0.081(7) 0.102(9)
C5E 0.045(5) 0.072(6) 0.041(5) 0.020(4) 0.030(4) 0.023(4)
C4E 0.036(4) 0.022(3) 0.038(4) -0.002(3) 0.025(3) 0.005(3)
C6E 0.035(4) 0.077(6) 0.045(5) 0.016(5) 0.029(4) 0.024(4)
C7E 0.035(4) 0.026(4) 0.031(4) 0.005(3) 0.022(3) 0.002(3)
C8E 0.039(4) 0.058(5) 0.037(4) 0.013(4) 0.023(4) 0.010(4)
C9E 0.035(4) 0.058(5) 0.036(4) 0.006(4) 0.024(3) 0.004(4)
N10E 0.040(3) 0.026(3) 0.036(3) -0.001(3) 0.025(3) 0.000(3)
C11E 0.062(6) 0.079(7) 0.066(6) 0.047(5) 0.046(5) 0.043(5)
C12E 0.066(6) 0.094(8) 0.070(6) 0.052(6) 0.057(5) 0.052(6)
O1F 0.042(3) 0.033(3) 0.041(3) 0.012(2) 0.028(2) 0.010(2)
C2F 0.063(5) 0.046(5) 0.046(5) 0.009(4) 0.021(4) 0.001(4)
Cl1U 0.0705(15) 0.0640(15) 0.0578(14) 0.0157(12) 0.0347(12) 0.0135(12)

_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 O1C 1.853(4) . ?
Mn1 O123 1.898(4) . ?
Mn1 O2B 1.909(4) . ?
Mn1 N22C 1.992(6) . ?
Mn1 N10D 2.352(5) 2 ?
Mn1 N10E 2.377(6) 7_565 ?
Mn2 O1B 1.859(5) . ?
Mn2 O123 1.870(4) . ?
Mn2 O2A 1.885(5) . ?
Mn2 N22B 1.995(6) . ?
Mn2 N1E 2.230(5) . ?
Mn3 O1A 1.863(5) . ?
Mn3 O123 1.884(4) . ?
Mn3 O2C 1.918(4) . ?
Mn3 N22A 2.003(6) . ?
Mn3 O1F 2.340(5) . ?
Mn3 N1D 2.361(5) . ?
O1A C1A 1.304(8) . ?
C1A C6A 1.393(10) . ?
C1A C2A 1.421(10) . ?
O2A N22A 1.401(7) . ?
C2A C3A 1.411(11) . ?
C2A C21A 1.477(10) . ?
C3A C4A 1.348(12) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.392(12) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.365(11) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C21A N22A 1.279(9) . ?
C21A C23A 1.502(10) . ?
C23A C24A 1.527(12) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
O1B C1B 1.316(8) . ?
C1B C2B 1.392(10) . ?
C1B C6B 1.422(10) . ?
O2B N22B 1.388(7) . ?
C2B C3B 1.403(10) . ?
C2B C21B 1.486(10) . ?
C3B C4B 1.372(11) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.369(12) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.369(11) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C21B N22B 1.299(9) . ?
C21B C23B 1.490(10) . ?
C23B C24B 1.543(11) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
O1C C1C 1.336(8) . ?
C1C C6C 1.385(10) . ?
C1C C2C 1.416(10) . ?
O2C N22C 1.376(7) . ?
C2C C3C 1.398(10) . ?
C2C C21C 1.471(10) . ?
C3C C4C 1.360(11) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.373(11) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.391(10) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
C21C N22C 1.310(8) . ?
C21C C23C 1.491(9) . ?
C23C C24C 1.500(11) . ?
C23C H23E 0.9900 . ?
C23C H23F 0.9900 . ?
C24C H24G 0.9800 . ?
C24C H24H 0.9800 . ?
C24C H24I 0.9800 . ?
N1D C6D 1.323(9) . ?
N1D C2D 1.326(9) . ?
C2D C3D 1.371(10) . ?
C2D H2D 0.9500 . ?
C3D C4D 1.394(10) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.351(10) . ?
C4D C7D 1.480(9) . ?
C5D C6D 1.403(10) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
C7D C8D 1.376(10) . ?
C7D C12D 1.381(10) . ?
C8D C9D 1.371(11) . ?
C8D H8D 0.9500 . ?
C9D N10D 1.332(9) . ?
C9D H9D 0.9500 . ?
N10D C11D 1.320(9) . ?
N10D Mn1 2.352(5) 2 ?
C11D C12D 1.379(10) . ?
C11D H11D 0.9500 . ?
C12D H12D 0.9500 . ?
N1E C6E 1.296(9) . ?
N1E C2E 1.307(10) . ?
C2E C3E 1.384(12) . ?
C2E H2E 0.9500 . ?
C3E C4E 1.384(11) . ?
C3E H3E 0.9500 . ?
C5E C4E 1.359(10) . ?
C5E C6E 1.366(11) . ?
C5E H5E 0.9500 . ?
C4E C7E 1.491(9) . ?
C6E H6E 0.9500 . ?
C7E C8E 1.368(10) . ?
C7E C12E 1.381(10) . ?
C8E C9E 1.382(10) . ?
C8E H8E 0.9500 . ?
C9E N10E 1.324(9) . ?
C9E H9E 0.9500 . ?
N10E C11E 1.306(10) . ?
N10E Mn1 2.377(6) 7_565 ?
C11E C12E 1.347(11) . ?
C11E H11E 0.9500 . ?
C12E H12E 0.9500 . ?
O1F C2F 1.481(9) . ?
C2F H2F1 0.9800 . ?
C2F H2F2 0.9800 . ?
C2F H2F3 0.9800 . ?
O1S C2S 1.378(14) . ?
O1S H1S 0.8400 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C1T C2T 1.427(17) . ?
C1T H1T1 0.9800 . ?
C1T H1T2 0.9800 . ?
C1T H1T3 0.9800 . ?
C2T O3T 1.363(13) . ?
C2T H2T1 0.9900 . ?
C2T H2T2 0.9900 . ?
O3T C4T 1.392(13) . ?
C4T C5T 1.418(15) . ?
C4T H4T1 0.9900 . ?
C4T H4T2 0.9900 . ?
C5T H5T1 0.9800 . ?
C5T H5T2 0.9800 . ?
C5T H5T3 0.9800 . ?
Cl1U O2U 1.362(12) . ?
Cl1U O3U 1.369(12) . ?
Cl1U O1U 1.399(8) . ?
Cl1U O4U 1.466(9) . ?
O1R C2R 1.25(2) . ?
O1R H1R 0.8400 . ?
C2R H2R1 0.9800 . ?
C2R H2R2 0.9800 . ?
C2R H2R3 0.9800 . ?

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
O1C Mn1 O123 177.39(19) . . ?
O1C Mn1 O2B 89.86(19) . . ?
O123 Mn1 O2B 91.28(19) . . ?
O1C Mn1 N22C 88.9(2) . . ?
O123 Mn1 N22C 90.0(2) . . ?
O2B Mn1 N22C 177.7(2) . . ?
O1C Mn1 N10D 86.7(2) . 2 ?
O123 Mn1 N10D 90.99(19) . 2 ?
O2B Mn1 N10D 90.28(19) . 2 ?
N22C Mn1 N10D 91.5(2) . 2 ?
O1C Mn1 N10E 84.9(2) . 7_565 ?
O123 Mn1 N10E 97.42(19) . 7_565 ?
O2B Mn1 N10E 89.2(2) . 7_565 ?
N22C Mn1 N10E 88.8(2) . 7_565 ?
N10D Mn1 N10E 171.6(2) 2 7_565 ?
O1B Mn2 O123 162.1(2) . . ?
O1B Mn2 O2A 87.6(2) . . ?
O123 Mn2 O2A 89.94(19) . . ?
O1B Mn2 N22B 88.6(2) . . ?
O123 Mn2 N22B 91.2(2) . . ?
O2A Mn2 N22B 171.4(2) . . ?
O1B Mn2 N1E 96.2(2) . . ?
O123 Mn2 N1E 101.7(2) . . ?
O2A Mn2 N1E 96.4(2) . . ?
N22B Mn2 N1E 91.7(2) . . ?
O1A Mn3 O123 177.3(2) . . ?
O1A Mn3 O2C 89.4(2) . . ?
O123 Mn3 O2C 91.45(19) . . ?
O1A Mn3 N22A 90.1(2) . . ?
O123 Mn3 N22A 89.0(2) . . ?
O2C Mn3 N22A 178.8(2) . . ?
O1A Mn3 O1F 84.02(18) . . ?
O123 Mn3 O1F 93.36(18) . . ?
O2C Mn3 O1F 90.68(19) . . ?
N22A Mn3 O1F 88.1(2) . . ?
O1A Mn3 N1D 82.0(2) . . ?
O123 Mn3 N1D 100.59(19) . . ?
O2C Mn3 N1D 89.20(19) . . ?
N22A Mn3 N1D 91.8(2) . . ?
O1F Mn3 N1D 166.06(18) . . ?
Mn2 O123 Mn3 122.3(2) . . ?
Mn2 O123 Mn1 118.9(2) . . ?
Mn3 O123 Mn1 118.8(2) . . ?
C1A O1A Mn3 129.4(4) . . ?
O1A C1A C6A 117.5(6) . . ?
O1A C1A C2A 123.6(6) . . ?
C6A C1A C2A 118.9(7) . . ?
N22A O2A Mn2 121.9(4) . . ?
C3A C2A C1A 116.9(7) . . ?
C3A C2A C21A 119.6(7) . . ?
C1A C2A C21A 123.5(6) . . ?
C4A C3A C2A 122.7(8) . . ?
C4A C3A H3A 118.7 . . ?
C2A C3A H3A 118.7 . . ?
C3A C4A C5A 119.9(8) . . ?
C3A C4A H4A 120.1 . . ?
C5A C4A H4A 120.1 . . ?
C6A C5A C4A 119.6(8) . . ?
C6A C5A H5A 120.2 . . ?
C4A C5A H5A 120.2 . . ?
C5A C6A C1A 121.8(7) . . ?
C5A C6A H6A 119.1 . . ?
C1A C6A H6A 119.1 . . ?
N22A C21A C2A 120.0(6) . . ?
N22A C21A C23A 119.5(6) . . ?
C2A C21A C23A 120.3(6) . . ?
C21A N22A O2A 114.1(5) . . ?
C21A N22A Mn3 130.1(5) . . ?
O2A N22A Mn3 115.6(4) . . ?
C21A C23A C24A 112.8(7) . . ?
C21A C23A H23A 109.0 . . ?
C24A C23A H23A 109.0 . . ?
C21A C23A H23B 109.0 . . ?
C24A C23A H23B 109.0 . . ?
H23A C23A H23B 107.8 . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C1B O1B Mn2 130.8(5) . . ?
O1B C1B C2B 126.3(6) . . ?
O1B C1B C6B 115.6(7) . . ?
C2B C1B C6B 118.1(7) . . ?
N22B O2B Mn1 121.1(4) . . ?
C1B C2B C3B 118.3(6) . . ?
C1B C2B C21B 122.0(6) . . ?
C3B C2B C21B 119.7(7) . . ?
C4B C3B C2B 123.2(8) . . ?
C4B C3B H3B 118.4 . . ?
C2B C3B H3B 118.4 . . ?
C5B C4B C3B 118.0(8) . . ?
C5B C4B H4B 121.0 . . ?
C3B C4B H4B 121.0 . . ?
C6B C5B C4B 121.4(8) . . ?
C6B C5B H5B 119.3 . . ?
C4B C5B H5B 119.3 . . ?
C5B C6B C1B 121.0(8) . . ?
C5B C6B H6B 119.5 . . ?
C1B C6B H6B 119.5 . . ?
N22B C21B C2B 119.3(6) . . ?
N22B C21B C23B 120.8(6) . . ?
C2B C21B C23B 119.8(6) . . ?
C21B N22B O2B 112.9(5) . . ?
C21B N22B Mn2 132.1(5) . . ?
O2B N22B Mn2 114.7(4) . . ?
C21B C23B C24B 110.1(6) . . ?
C21B C23B H23C 109.6 . . ?
C24B C23B H23C 109.6 . . ?
C21B C23B H23D 109.6 . . ?
C24B C23B H23D 109.6 . . ?
H23C C23B H23D 108.1 . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C1C O1C Mn1 125.1(4) . . ?
O1C C1C C6C 117.1(6) . . ?
O1C C1C C2C 123.0(6) . . ?
C6C C1C C2C 119.8(6) . . ?
N22C O2C Mn3 118.8(3) . . ?
C3C C2C C1C 116.9(6) . . ?
C3C C2C C21C 120.4(6) . . ?
C1C C2C C21C 122.7(6) . . ?
C4C C3C C2C 122.9(7) . . ?
C4C C3C H3C 118.5 . . ?
C2C C3C H3C 118.5 . . ?
C3C C4C C5C 119.8(7) . . ?
C3C C4C H4C 120.1 . . ?
C5C C4C H4C 120.1 . . ?
C4C C5C C6C 119.5(7) . . ?
C4C C5C H5C 120.2 . . ?
C6C C5C H5C 120.2 . . ?
C1C C6C C5C 121.0(7) . . ?
C1C C6C H6C 119.5 . . ?
C5C C6C H6C 119.5 . . ?
N22C C21C C2C 118.8(6) . . ?
N22C C21C C23C 119.6(6) . . ?
C2C C21C C23C 121.4(6) . . ?
C21C N22C O2C 115.2(5) . . ?
C21C N22C Mn1 129.5(5) . . ?
O2C N22C Mn1 114.8(4) . . ?
C21C C23C C24C 111.2(7) . . ?
C21C C23C H23E 109.4 . . ?
C24C C23C H23E 109.4 . . ?
C21C C23C H23F 109.4 . . ?
C24C C23C H23F 109.4 . . ?
H23E C23C H23F 108.0 . . ?
C23C C24C H24G 109.5 . . ?
C23C C24C H24H 109.5 . . ?
H24G C24C H24H 109.5 . . ?
C23C C24C H24I 109.5 . . ?
H24G C24C H24I 109.5 . . ?
H24H C24C H24I 109.5 . . ?
C6D N1D C2D 115.9(6) . . ?
C6D N1D Mn3 114.3(5) . . ?
C2D N1D Mn3 129.3(5) . . ?
N1D C2D C3D 124.6(7) . . ?
N1D C2D H2D 117.7 . . ?
C3D C2D H2D 117.7 . . ?
C2D C3D C4D 119.7(7) . . ?
C2D C3D H3D 120.2 . . ?
C4D C3D H3D 120.2 . . ?
C5D C4D C3D 116.0(6) . . ?
C5D C4D C7D 122.1(6) . . ?
C3D C4D C7D 121.9(6) . . ?
C4D C5D C6D 120.9(7) . . ?
C4D C5D H5D 119.6 . . ?
C6D C5D H5D 119.6 . . ?
N1D C6D C5D 122.9(7) . . ?
N1D C6D H6D 118.5 . . ?
C5D C6D H6D 118.5 . . ?
C8D C7D C12D 115.5(6) . . ?
C8D C7D C4D 122.4(6) . . ?
C12D C7D C4D 122.0(6) . . ?
C9D C8D C7D 120.6(7) . . ?
C9D C8D H8D 119.7 . . ?
C7D C8D H8D 119.7 . . ?
N10D C9D C8D 123.9(7) . . ?
N10D C9D H9D 118.0 . . ?
C8D C9D H9D 118.0 . . ?
C11D N10D C9D 115.4(6) . . ?
C11D N10D Mn1 122.3(5) . 2 ?
C9D N10D Mn1 122.1(5) . 2 ?
N10D C11D C12D 124.4(7) . . ?
N10D C11D H11D 117.8 . . ?
C12D C11D H11D 117.8 . . ?
C11D C12D C7D 120.0(7) . . ?
C11D C12D H12D 120.0 . . ?
C7D C12D H12D 120.0 . . ?
C6E N1E C2E 115.2(6) . . ?
C6E N1E Mn2 121.2(5) . . ?
C2E N1E Mn2 123.6(5) . . ?
N1E C2E C3E 124.8(8) . . ?
N1E C2E H2E 117.6 . . ?
C3E C2E H2E 117.6 . . ?
C4E C3E C2E 119.0(8) . . ?
C4E C3E H3E 120.5 . . ?
C2E C3E H3E 120.5 . . ?
C4E C5E C6E 120.9(7) . . ?
C4E C5E H5E 119.6 . . ?
C6E C5E H5E 119.6 . . ?
C5E C4E C3E 115.1(7) . . ?
C5E C4E C7E 123.3(6) . . ?
C3E C4E C7E 121.6(6) . . ?
N1E C6E C5E 124.7(7) . . ?
N1E C6E H6E 117.7 . . ?
C5E C6E H6E 117.7 . . ?
C8E C7E C12E 116.0(6) . . ?
C8E C7E C4E 121.4(6) . . ?
C12E C7E C4E 122.5(6) . . ?
C7E C8E C9E 118.9(7) . . ?
C7E C8E H8E 120.5 . . ?
C9E C8E H8E 120.5 . . ?
N10E C9E C8E 124.2(7) . . ?
N10E C9E H9E 117.9 . . ?
C8E C9E H9E 117.9 . . ?
C11E N10E C9E 115.8(6) . . ?
C11E N10E Mn1 117.5(5) . 7_565 ?
C9E N10E Mn1 126.5(5) . 7_565 ?
N10E C11E C12E 124.3(8) . . ?
N10E C11E H11E 117.8 . . ?
C12E C11E H11E 117.8 . . ?
C11E C12E C7E 120.7(7) . . ?
C11E C12E H12E 119.7 . . ?
C7E C12E H12E 119.7 . . ?
C2F O1F Mn3 115.4(4) . . ?
O1F C2F H2F1 109.5 . . ?
O1F C2F H2F2 109.5 . . ?
H2F1 C2F H2F2 109.5 . . ?
O1F C2F H2F3 109.5 . . ?
H2F1 C2F H2F3 109.5 . . ?
H2F2 C2F H2F3 109.5 . . ?
C2S O1S H1S 110.1 . . ?
O1S C2S H2S1 110.3 . . ?
O1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O1S C2S H2S3 108.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C2T C1T H1T1 109.5 . . ?
C2T C1T H1T2 109.5 . . ?
H1T1 C1T H1T2 109.5 . . ?
C2T C1T H1T3 109.5 . . ?
H1T1 C1T H1T3 109.5 . . ?
H1T2 C1T H1T3 109.5 . . ?
O3T C2T C1T 113.1(11) . . ?
O3T C2T H2T1 109.0 . . ?
C1T C2T H2T1 109.0 . . ?
O3T C2T H2T2 109.0 . . ?
C1T C2T H2T2 109.0 . . ?
H2T1 C2T H2T2 107.8 . . ?
C2T O3T C4T 119.5(9) . . ?
O3T C4T C5T 117.8(10) . . ?
O3T C4T H4T1 107.9 . . ?
C5T C4T H4T1 107.9 . . ?
O3T C4T H4T2 107.9 . . ?
C5T C4T H4T2 107.9 . . ?
H4T1 C4T H4T2 107.2 . . ?
C4T C5T H5T1 109.5 . . ?
C4T C5T H5T2 109.5 . . ?
H5T1 C5T H5T2 109.5 . . ?
C4T C5T H5T3 109.5 . . ?
H5T1 C5T H5T3 109.5 . . ?
H5T2 C5T H5T3 109.5 . . ?
O2U Cl1U O3U 118.3(7) . . ?
O2U Cl1U O1U 113.7(6) . . ?
O3U Cl1U O1U 114.3(6) . . ?
O2U Cl1U O4U 100.5(7) . . ?
O3U Cl1U O4U 102.2(6) . . ?
O1U Cl1U O4U 104.9(5) . . ?
C2R O1R H1R 108.4 . . ?
O1R C2R H2R1 111.9 . . ?
O1R C2R H2R2 109.3 . . ?
H2R1 C2R H2R2 109.5 . . ?
O1R C2R H2R3 107.1 . . ?
H2R1 C2R H2R3 109.5 . . ?
H2R2 C2R H2R3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.495
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.114