# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

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

_publ_contact_author_email       EBRECHIN@STAFFMAIL.ED.AC.UK

_publ_section_title              
;
Turning up the spin, turning on single-molecule
magnetism: from S = 1 to S = 7 in a [Mn8] cluster via ligand induced
structural distortion
;
loop_
_publ_author_name
'Euan Brechin'
'George Christou'
'Ross Inglis'
'Constantinos J Milios'
'S. Parsons'
'Spyros Perlepes'
;
A.Prescimone
;
'Alina Vinslava'
'Wolfgang Wernsdorfer'

data_eb6138
_database_code_depnum_ccdc_archive 'CCDC 638207'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Mn8O2(napth-salox)6(N3)6(MeOH)8].10MeOH'
_chemical_formula_sum            'C84 H114 Mn8 N24 O32'
_chemical_formula_weight         2411.51

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.8273(3)
_cell_length_b                   15.3275(3)
_cell_length_c                   15.5166(4)
_cell_angle_alpha                111.6580(10)
_cell_angle_beta                 109.8920(10)
_cell_angle_gamma                102.6120(10)
_cell_volume                     2642.14(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7762
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1242
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_type   Multiscan
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_process_details   'Sadabs scaled by 1.08'

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

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smarp APEX CCD'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61412
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         30.00
_reflns_number_total             14863
_reflns_number_gt                11955
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Mn1-3 look lile Mn+3; Mn4 looks like Mn+2
Ligands: 1-3 napth-salox
4-6: N3-
7-10: ligating MeOH
11-15: MeOH of solvation.

H-atoms located on MeOH were located in difference maps. The hydroxyl
H-atoms attached to O17 - O110 were refined subject to similarity restraints
on the OH distances and COH angles; those attached to the MeOH of solvation
were refined as rotating rigid groups. All Me-groups were also treated as
rotating rigid groups.

H-bonding:

Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and <DHA > 110 deg.

D-H d(D-H) d(H..A) <DHA d(D..A) A

O17-H17 0.732 2.337 151.79 3.002 O12 [ -x, -y, -z+1 ]
O17-H17 0.732 2.443 134.17 3.000 O131 [ -x, -y, -z+1 ]

O18-H18 0.734 2.014 160.62 2.718 O112

O19-H19 0.730 2.062 175.52 2.790 N36 [ -x, -y, -z ]

O110-H110 0.731 1.921 170.19 2.645 O113

O111-H11A 0.840 2.212 166.37 3.035 N36

O112-H11B 0.840 2.092 163.83 2.908 O114
O112-H11B 0.840 2.590 113.42 3.024 N34

O113-H11C 0.840 1.871 172.82 2.706 O114

O114-H114 0.840 1.866 163.37 2.682 O115 [ -x-1, -y-1, -z ]

O115-H115 0.840 2.196 151.04 2.959 O11
O115-H115 0.840 2.494 132.66 3.125 O133

Checkcif output:

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

No action.

220_ALERT_2_B Large Non-Solvent N Ueq(max)/Ueq(min) ... 4.11 Ratio
220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.94 Ratio
222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.55 Ratio

No action: tehe terminal N and methyl groups of the azide and MeOH show
relatively high thermal motion: this is normal.

912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 555
910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 2
911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 0.600 6

The data collection strategy used aimed to achieve a complete data set to
2\q = 54 deg. Some higher angle data were collected in the process and these
have been included in the refinement.

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 0.999 5528 5525 3
23.01 0.550 1.000 7354 7351 3
25.24 0.600 0.999 9567 9559 8
#----------------------------------------------------------- ACTA Min. Res. ---
27.51 0.650 0.997 12141 12107 34
29.84 0.700 0.968 15212 14728 484
30.00 0.704 0.964 15426 14863 563

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

The one given is more chemically meaningful.

061_ALERT_3_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, changes in the volume of the crystal illuminated, etc.

790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
C H4 O
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
C H4 O
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5
C H4 O
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6
C H4 O
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12
796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12
797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N14

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^)+(0.0500P)^2^+2.3262P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom/difmap
_refine_ls_hydrogen_treatment    'riding/refall/rotating group'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14863
_refine_ls_number_parameters     694
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_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 -0.22237(3) -0.15634(3) 0.27465(3) 0.01541(8) Uani 1 1 d . . .
Mn2 Mn 0.04065(3) -0.00130(3) 0.41141(3) 0.01473(8) Uani 1 1 d . . .
Mn3 Mn -0.14139(3) 0.06196(3) 0.28094(3) 0.01521(8) Uani 1 1 d . . .
Mn4 Mn -0.05966(3) -0.15553(3) 0.12183(3) 0.01970(8) Uani 1 1 d . . .
O1 O -0.10783(12) -0.03318(12) 0.32342(12) 0.0158(3) Uani 1 1 d . . .
O11 O -0.33760(13) -0.26587(12) 0.25336(13) 0.0204(3) Uani 1 1 d . . .
C11 C -0.3337(2) -0.34697(17) 0.26464(19) 0.0192(5) Uani 1 1 d . . .
C21 C -0.4374(2) -0.4295(2) 0.2185(2) 0.0283(6) Uani 1 1 d . . .
H21 H -0.5049 -0.4244 0.1819 0.034 Uiso 1 1 calc R . .
C31 C -0.4417(2) -0.5155(2) 0.2260(2) 0.0316(6) Uani 1 1 d . . .
H31 H -0.5124 -0.5692 0.1953 0.038 Uiso 1 1 calc R . .
C41 C -0.3428(2) -0.52734(19) 0.2786(2) 0.0251(5) Uani 1 1 d . . .
C51 C -0.3472(2) -0.6195(2) 0.2805(2) 0.0320(6) Uani 1 1 d . . .
H51 H -0.4178 -0.6735 0.2494 0.038 Uiso 1 1 calc R . .
C61 C -0.2520(2) -0.6326(2) 0.3262(2) 0.0320(6) Uani 1 1 d . . .
H61 H -0.2562 -0.6955 0.3258 0.038 Uiso 1 1 calc R . .
C71 C -0.1480(2) -0.5526(2) 0.3735(2) 0.0316(6) Uani 1 1 d . . .
H71 H -0.0816 -0.5617 0.4052 0.038 Uiso 1 1 calc R . .
C81 C -0.1405(2) -0.4612(2) 0.3750(2) 0.0278(6) Uani 1 1 d . . .
H81 H -0.0690 -0.4075 0.4088 0.033 Uiso 1 1 calc R . .
C91 C -0.2380(2) -0.44588(18) 0.32664(19) 0.0208(5) Uani 1 1 d . . .
C101 C -0.23458(19) -0.35279(17) 0.32140(18) 0.0183(4) Uani 1 1 d . . .
C111 C -0.12967(19) -0.26536(17) 0.38223(18) 0.0180(4) Uani 1 1 d . . .
H111 H -0.0691 -0.2678 0.4326 0.022 Uiso 1 1 calc R . .
N121 N -0.11275(15) -0.18439(14) 0.37268(15) 0.0159(4) Uani 1 1 d . . .
O131 O -0.01091(13) -0.10413(11) 0.44930(12) 0.0162(3) Uani 1 1 d . . .
O12 O 0.18917(13) 0.04125(13) 0.51250(13) 0.0197(3) Uani 1 1 d . . .
C12 C 0.28080(19) 0.09028(18) 0.51112(18) 0.0188(4) Uani 1 1 d . . .
C22 C 0.3790(2) 0.0753(2) 0.5589(2) 0.0262(5) Uani 1 1 d . . .
H22 H 0.3760 0.0306 0.5879 0.031 Uiso 1 1 calc R . .
C32 C 0.4769(2) 0.1239(2) 0.5638(2) 0.0286(6) Uani 1 1 d . . .
H32 H 0.5412 0.1124 0.5958 0.034 Uiso 1 1 calc R . .
C42 C 0.4851(2) 0.19211(19) 0.5216(2) 0.0240(5) Uani 1 1 d . . .
C52 C 0.5869(2) 0.2426(2) 0.5267(2) 0.0297(6) Uani 1 1 d . . .
H52 H 0.6509 0.2303 0.5581 0.036 Uiso 1 1 calc R . .
C62 C 0.5951(2) 0.3086(2) 0.4874(2) 0.0343(6) Uani 1 1 d . . .
H62 H 0.6645 0.3431 0.4927 0.041 Uiso 1 1 calc R . .
C72 C 0.4997(2) 0.3251(2) 0.4390(2) 0.0347(6) Uani 1 1 d . . .
H72 H 0.5051 0.3707 0.4112 0.042 Uiso 1 1 calc R . .
C82 C 0.3992(2) 0.2763(2) 0.4315(2) 0.0299(6) Uani 1 1 d . . .
H82 H 0.3356 0.2878 0.3977 0.036 Uiso 1 1 calc R . .
C92 C 0.3886(2) 0.20870(19) 0.47358(19) 0.0222(5) Uani 1 1 d . . .
C102 C 0.28459(19) 0.15674(18) 0.46880(19) 0.0192(5) Uani 1 1 d . . .
C112 C 0.18855(19) 0.17936(18) 0.42630(19) 0.0197(5) Uani 1 1 d . . .
H112 H 0.2005 0.2386 0.4180 0.024 Uiso 1 1 calc R . .
N122 N 0.08788(16) 0.12398(15) 0.39905(15) 0.0171(4) Uani 1 1 d . . .
O132 O 0.00900(13) 0.16305(12) 0.37037(13) 0.0188(3) Uani 1 1 d . . .
O13 O -0.18572(14) 0.15204(12) 0.23823(13) 0.0208(3) Uani 1 1 d . . .
C13 C -0.24936(19) 0.12507(18) 0.13870(18) 0.0184(4) Uani 1 1 d . . .
C23 C -0.2332(2) 0.20328(19) 0.1098(2) 0.0229(5) Uani 1 1 d . . .
H23 H -0.1798 0.2705 0.1611 0.027 Uiso 1 1 calc R . .
C33 C -0.2932(2) 0.18279(19) 0.0100(2) 0.0240(5) Uani 1 1 d . . .
H33 H -0.2819 0.2363 -0.0072 0.029 Uiso 1 1 calc R . .
C43 C -0.3725(2) 0.08295(19) -0.06935(19) 0.0209(5) Uani 1 1 d . . .
C53 C -0.4290(2) 0.0605(2) -0.1751(2) 0.0259(5) Uani 1 1 d . . .
H53 H -0.4164 0.1138 -0.1925 0.031 Uiso 1 1 calc R . .
C63 C -0.5012(2) -0.0364(2) -0.2521(2) 0.0285(6) Uani 1 1 d . . .
H63 H -0.5375 -0.0509 -0.3228 0.034 Uiso 1 1 calc R . .
C73 C -0.5214(2) -0.1145(2) -0.2255(2) 0.0290(6) Uani 1 1 d . . .
H73 H -0.5717 -0.1821 -0.2789 0.035 Uiso 1 1 calc R . .
C83 C -0.4697(2) -0.09488(19) -0.1240(2) 0.0240(5) Uani 1 1 d . . .
H83 H -0.4859 -0.1488 -0.1080 0.029 Uiso 1 1 calc R . .
C93 C -0.39244(19) 0.00427(18) -0.04236(19) 0.0193(5) Uani 1 1 d . . .
C103 C -0.33207(19) 0.02713(18) 0.06494(18) 0.0178(4) Uani 1 1 d . . .
C113 C -0.36042(19) -0.04963(18) 0.09554(19) 0.0181(4) Uani 1 1 d . . .
H113 H -0.4303 -0.1063 0.0506 0.022 Uiso 1 1 calc R . .
N123 N -0.29454(15) -0.04432(15) 0.18159(15) 0.0173(4) Uani 1 1 d . . .
O133 O -0.33460(13) -0.11818(12) 0.20484(13) 0.0200(3) Uani 1 1 d . . .
N14 N -0.19705(17) -0.23729(15) 0.14116(16) 0.0226(4) Uani 1 1 d . . .
N24 N -0.25750(18) -0.32590(17) 0.08083(18) 0.0282(5) Uani 1 1 d . . .
N34 N -0.3145(2) -0.4105(2) 0.0245(3) 0.0550(8) Uani 1 1 d . . .
N15 N 0.06232(17) -0.10347(16) 0.28400(16) 0.0217(4) Uani 1 1 d . . .
N25 N 0.1307(2) -0.13884(18) 0.30531(18) 0.0310(5) Uani 1 1 d . . .
N35 N 0.1965(3) -0.1717(3) 0.3271(2) 0.0654(10) Uani 1 1 d . . .
N16 N -0.08895(17) -0.01100(16) 0.15260(16) 0.0214(4) Uani 1 1 d . . .
N26 N -0.05303(18) 0.04628(16) 0.12574(17) 0.0242(4) Uani 1 1 d . . .
N36 N -0.0180(2) 0.1037(2) 0.1015(2) 0.0420(6) Uani 1 1 d . . .
O17 O -0.19533(16) 0.10959(14) 0.40770(14) 0.0260(4) Uani 1 1 d D . .
H17 H -0.175(3) 0.0892(18) 0.4429(18) 0.042(5) Uiso 1 1 d D . .
C27 C -0.1749(3) 0.2129(2) 0.4696(2) 0.0377(7) Uani 1 1 d D . .
H27A H -0.1217 0.2572 0.4598 0.057 Uiso 1 1 calc R . .
H27B H -0.1437 0.2303 0.5435 0.057 Uiso 1 1 calc R . .
H27C H -0.2453 0.2227 0.4483 0.057 Uiso 1 1 calc R . .
O18 O -0.17537(17) -0.22303(15) -0.04723(15) 0.0304(4) Uani 1 1 d D . .
H18 H -0.191(2) -0.2776(16) -0.080(2) 0.042(5) Uiso 1 1 d D . .
C28 C -0.2674(3) -0.1991(3) -0.0890(3) 0.0500(9) Uani 1 1 d D . .
H28A H -0.3277 -0.2295 -0.0762 0.075 Uiso 1 1 calc R . .
H28B H -0.2943 -0.2263 -0.1645 0.075 Uiso 1 1 calc R . .
H28C H -0.2443 -0.1247 -0.0552 0.075 Uiso 1 1 calc R . .
O19 O 0.07839(18) -0.08500(16) 0.09728(17) 0.0347(5) Uani 1 1 d D . .
H19 H 0.066(2) -0.088(2) 0.0462(16) 0.042(5) Uiso 1 1 d D . .
C29 C 0.1830(3) -0.0018(3) 0.1742(3) 0.0521(9) Uani 1 1 d D . .
H29A H 0.1712 0.0618 0.1982 0.078 Uiso 1 1 calc R . .
H29B H 0.2339 0.0031 0.1434 0.078 Uiso 1 1 calc R . .
H29C H 0.2158 -0.0134 0.2337 0.078 Uiso 1 1 calc R . .
O110 O -0.02398(18) -0.29202(15) 0.06070(16) 0.0330(4) Uani 1 1 d D . .
H110 H -0.037(3) -0.3331(19) 0.073(2) 0.042(5) Uiso 1 1 d D . .
C210 C 0.0113(3) -0.3221(3) -0.0179(3) 0.0507(9) Uani 1 1 d D . .
H21A H -0.0424 -0.3264 -0.0815 0.076 Uiso 1 1 calc R . .
H21B H 0.0151 -0.3889 -0.0334 0.076 Uiso 1 1 calc R . .
H21C H 0.0853 -0.2715 0.0071 0.076 Uiso 1 1 calc R . .
O111 O 0.1566(3) 0.3066(2) 0.2884(3) 0.0728(8) Uani 1 1 d . . .
H11A H 0.1119 0.2543 0.2305 0.109 Uiso 1 1 calc R . .
C211 C 0.0968(4) 0.3623(4) 0.3255(4) 0.0773(14) Uani 1 1 d . . .
H21D H 0.1468 0.4175 0.3973 0.116 Uiso 1 1 calc R . .
H21E H 0.0341 0.3165 0.3244 0.116 Uiso 1 1 calc R . .
H21F H 0.0682 0.3912 0.2804 0.116 Uiso 1 1 calc R . .
O112 O -0.2793(3) -0.4298(2) -0.1626(2) 0.0653(8) Uani 1 1 d . . .
H11B H -0.2738 -0.4669 -0.1341 0.098 Uiso 1 1 calc R . .
C212 C -0.3139(4) -0.4876(3) -0.2685(3) 0.0769(14) Uani 1 1 d . . .
H21G H -0.3305 -0.4471 -0.3034 0.115 Uiso 1 1 calc R . .
H21H H -0.3812 -0.5487 -0.2989 0.115 Uiso 1 1 calc R . .
H21I H -0.2543 -0.5081 -0.2780 0.115 Uiso 1 1 calc R . .
O113 O -0.0756(2) -0.45636(17) 0.08288(18) 0.0411(5) Uani 1 1 d . . .
H11C H -0.1353 -0.4986 0.0282 0.062 Uiso 1 1 calc R . .
C213 C -0.0858(4) -0.4545(3) 0.1708(3) 0.0614(11) Uani 1 1 d . . .
H21J H -0.0192 -0.4002 0.2349 0.092 Uiso 1 1 calc R . .
H21K H -0.0930 -0.5205 0.1685 0.092 Uiso 1 1 calc R . .
H21L H -0.1523 -0.4416 0.1701 0.092 Uiso 1 1 calc R . .
O114 O -0.2609(2) -0.58630(19) -0.1023(2) 0.0574(7) Uani 1 1 d . . .
H114 H -0.3082 -0.6151 -0.0886 0.086 Uiso 1 1 calc R . .
C214 C -0.2420(3) -0.6618(3) -0.1745(3) 0.0572(10) Uani 1 1 d . . .
H21M H -0.1726 -0.6296 -0.1748 0.086 Uiso 1 1 calc R . .
H21N H -0.3047 -0.6936 -0.2449 0.086 Uiso 1 1 calc R . .
H21O H -0.2355 -0.7141 -0.1535 0.086 Uiso 1 1 calc R . .
O115 O -0.56122(17) -0.30347(17) 0.10004(18) 0.0404(5) Uani 1 1 d . . .
H115 H -0.4970 -0.2710 0.1515 0.061 Uiso 1 1 calc R . .
C215 C -0.5523(3) -0.3483(3) 0.0070(3) 0.0469(8) Uani 1 1 d . . .
H21P H -0.5078 -0.2947 -0.0004 0.070 Uiso 1 1 calc R . .
H21Q H -0.6272 -0.3853 -0.0532 0.070 Uiso 1 1 calc R . .
H21R H -0.5157 -0.3958 0.0100 0.070 Uiso 1 1 calc 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 0.01414(16) 0.01452(16) 0.01690(18) 0.01007(14) 0.00494(14) 0.00377(13)
Mn2 0.01329(16) 0.01513(16) 0.01472(17) 0.00876(14) 0.00467(13) 0.00399(13)
Mn3 0.01461(16) 0.01470(16) 0.01524(17) 0.00941(14) 0.00422(13) 0.00441(13)
Mn4 0.02206(18) 0.01968(18) 0.01792(19) 0.00992(15) 0.00955(15) 0.00724(15)
O1 0.0142(7) 0.0155(7) 0.0161(8) 0.0094(7) 0.0046(6) 0.0040(6)
O11 0.0173(8) 0.0176(8) 0.0253(9) 0.0142(7) 0.0063(7) 0.0041(7)
C11 0.0223(11) 0.0167(11) 0.0191(12) 0.0109(10) 0.0084(10) 0.0065(9)
C21 0.0199(12) 0.0244(13) 0.0348(15) 0.0183(12) 0.0054(11) 0.0038(10)
C31 0.0231(13) 0.0213(13) 0.0415(17) 0.0189(12) 0.0064(12) 0.0010(10)
C41 0.0260(13) 0.0174(11) 0.0264(14) 0.0115(11) 0.0081(11) 0.0044(10)
C51 0.0342(15) 0.0178(12) 0.0371(16) 0.0162(12) 0.0104(13) 0.0034(11)
C61 0.0419(16) 0.0175(12) 0.0382(16) 0.0182(12) 0.0152(13) 0.0111(12)
C71 0.0328(14) 0.0245(13) 0.0370(16) 0.0184(12) 0.0101(12) 0.0141(12)
C81 0.0259(13) 0.0222(13) 0.0313(15) 0.0142(11) 0.0086(11) 0.0080(11)
C91 0.0268(12) 0.0150(11) 0.0184(12) 0.0087(10) 0.0087(10) 0.0062(9)
C101 0.0210(11) 0.0136(10) 0.0174(11) 0.0087(9) 0.0065(9) 0.0039(9)
C111 0.0212(11) 0.0162(11) 0.0173(11) 0.0099(9) 0.0067(9) 0.0089(9)
N121 0.0147(9) 0.0140(9) 0.0141(9) 0.0058(8) 0.0041(7) 0.0033(7)
O131 0.0150(7) 0.0123(7) 0.0140(8) 0.0059(6) 0.0019(6) 0.0014(6)
O12 0.0138(8) 0.0234(9) 0.0219(9) 0.0136(7) 0.0067(7) 0.0050(7)
C12 0.0153(10) 0.0192(11) 0.0160(11) 0.0064(9) 0.0054(9) 0.0035(9)
C22 0.0206(12) 0.0290(13) 0.0306(14) 0.0180(12) 0.0093(11) 0.0102(10)
C32 0.0193(12) 0.0339(14) 0.0323(15) 0.0175(12) 0.0087(11) 0.0128(11)
C42 0.0173(11) 0.0254(13) 0.0230(13) 0.0077(11) 0.0090(10) 0.0052(10)
C52 0.0192(12) 0.0343(15) 0.0291(15) 0.0114(12) 0.0106(11) 0.0073(11)
C62 0.0216(13) 0.0390(16) 0.0376(17) 0.0158(14) 0.0166(12) 0.0039(12)
C72 0.0293(14) 0.0389(16) 0.0402(17) 0.0236(14) 0.0190(13) 0.0083(13)
C82 0.0238(13) 0.0354(15) 0.0361(16) 0.0222(13) 0.0152(12) 0.0107(11)
C92 0.0182(11) 0.0232(12) 0.0210(12) 0.0087(10) 0.0094(10) 0.0039(10)
C102 0.0166(11) 0.0197(11) 0.0195(12) 0.0091(10) 0.0079(9) 0.0056(9)
C112 0.0191(11) 0.0189(11) 0.0192(12) 0.0103(10) 0.0077(9) 0.0042(9)
N122 0.0179(9) 0.0178(9) 0.0163(10) 0.0099(8) 0.0067(8) 0.0070(8)
O132 0.0161(8) 0.0175(8) 0.0221(9) 0.0120(7) 0.0058(7) 0.0060(6)
O13 0.0224(8) 0.0174(8) 0.0188(9) 0.0105(7) 0.0040(7) 0.0072(7)
C13 0.0183(11) 0.0201(11) 0.0191(12) 0.0123(10) 0.0071(9) 0.0091(9)
C23 0.0245(12) 0.0172(11) 0.0240(13) 0.0121(10) 0.0073(10) 0.0059(10)
C33 0.0284(13) 0.0217(12) 0.0263(13) 0.0170(11) 0.0113(11) 0.0098(10)
C43 0.0203(11) 0.0249(12) 0.0226(12) 0.0160(11) 0.0093(10) 0.0103(10)
C53 0.0298(13) 0.0277(13) 0.0254(13) 0.0193(11) 0.0103(11) 0.0129(11)
C63 0.0327(14) 0.0316(14) 0.0204(13) 0.0162(12) 0.0069(11) 0.0137(12)
C73 0.0274(13) 0.0261(13) 0.0225(13) 0.0115(11) 0.0030(11) 0.0058(11)
C83 0.0241(12) 0.0208(12) 0.0251(13) 0.0145(11) 0.0067(10) 0.0071(10)
C93 0.0183(11) 0.0207(11) 0.0211(12) 0.0128(10) 0.0078(9) 0.0093(9)
C103 0.0167(10) 0.0185(11) 0.0191(12) 0.0115(10) 0.0065(9) 0.0072(9)
C113 0.0148(10) 0.0176(11) 0.0207(12) 0.0111(10) 0.0058(9) 0.0047(9)
N123 0.0154(9) 0.0177(9) 0.0213(10) 0.0129(8) 0.0079(8) 0.0057(8)
O133 0.0171(8) 0.0212(8) 0.0263(9) 0.0187(8) 0.0080(7) 0.0061(7)
N14 0.0224(10) 0.0193(10) 0.0205(11) 0.0071(9) 0.0098(9) 0.0036(8)
N24 0.0222(11) 0.0283(12) 0.0255(12) 0.0065(10) 0.0107(10) 0.0076(10)
N34 0.0428(16) 0.0300(15) 0.059(2) -0.0053(14) 0.0269(15) -0.0007(13)
N15 0.0207(10) 0.0253(11) 0.0202(11) 0.0118(9) 0.0087(8) 0.0109(9)
N25 0.0386(13) 0.0337(13) 0.0215(12) 0.0123(10) 0.0122(10) 0.0202(11)
N35 0.076(2) 0.080(2) 0.0437(18) 0.0235(17) 0.0183(17) 0.064(2)
N16 0.0244(10) 0.0215(10) 0.0209(11) 0.0127(9) 0.0115(9) 0.0075(8)
N26 0.0302(11) 0.0262(11) 0.0225(11) 0.0146(9) 0.0144(9) 0.0132(9)
N36 0.0557(17) 0.0452(15) 0.0492(17) 0.0350(14) 0.0349(14) 0.0218(13)
O17 0.0337(10) 0.0314(10) 0.0262(10) 0.0203(8) 0.0164(8) 0.0200(8)
C27 0.0398(17) 0.0369(16) 0.0359(17) 0.0122(14) 0.0199(14) 0.0200(14)
O18 0.0338(11) 0.0289(10) 0.0204(10) 0.0092(8) 0.0072(8) 0.0122(9)
C28 0.049(2) 0.0416(19) 0.0393(19) 0.0171(16) 0.0005(16) 0.0203(16)
O19 0.0391(12) 0.0385(11) 0.0331(12) 0.0204(10) 0.0236(10) 0.0103(9)
C29 0.0343(18) 0.063(2) 0.060(2) 0.032(2) 0.0262(17) 0.0089(17)
O110 0.0448(12) 0.0275(10) 0.0347(11) 0.0162(9) 0.0233(10) 0.0181(9)
C210 0.069(2) 0.055(2) 0.058(2) 0.0318(19) 0.045(2) 0.041(2)
O111 0.0623(19) 0.073(2) 0.068(2) 0.0385(17) 0.0192(16) 0.0130(16)
C211 0.072(3) 0.074(3) 0.109(4) 0.060(3) 0.047(3) 0.033(3)
O112 0.077(2) 0.0501(16) 0.0506(17) 0.0186(14) 0.0225(15) 0.0157(15)
C212 0.095(4) 0.051(2) 0.053(3) 0.006(2) 0.037(3) 0.005(2)
O113 0.0507(14) 0.0343(12) 0.0418(13) 0.0188(10) 0.0244(11) 0.0171(10)
C213 0.082(3) 0.071(3) 0.051(2) 0.034(2) 0.042(2) 0.037(2)
O114 0.0555(16) 0.0502(15) 0.0509(16) 0.0077(13) 0.0324(14) 0.0119(13)
C214 0.055(2) 0.051(2) 0.052(2) 0.0097(18) 0.0280(19) 0.0182(18)
O115 0.0239(10) 0.0357(12) 0.0462(14) 0.0168(10) 0.0054(9) 0.0085(9)
C215 0.0411(18) 0.0435(19) 0.049(2) 0.0209(17) 0.0183(16) 0.0124(15)

_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 O1 1.8625(15) . ?
Mn1 O11 1.8791(16) . ?
Mn1 O133 1.9089(16) . ?
Mn1 N121 1.9986(18) . ?
Mn1 N14 2.177(2) . ?
Mn2 O1 1.8655(15) . ?
Mn2 O12 1.8897(16) . ?
Mn2 O131 1.9536(15) . ?
Mn2 N122 1.9900(19) . ?
Mn2 N15 2.185(2) . ?
Mn2 O131 2.4017(16) 2_556 ?
Mn2 Mn3 3.2282(5) . ?
Mn3 O13 1.8682(16) . ?
Mn3 O1 1.8902(15) . ?
Mn3 O132 1.9217(16) . ?
Mn3 N123 1.9832(19) . ?
Mn3 O17 2.2658(18) . ?
Mn3 N16 2.331(2) . ?
Mn4 O110 2.1965(19) . ?
Mn4 O19 2.203(2) . ?
Mn4 N15 2.203(2) . ?
Mn4 N14 2.212(2) . ?
Mn4 O18 2.2203(19) . ?
Mn4 N16 2.245(2) . ?
O11 C11 1.327(3) . ?
C11 C101 1.397(3) . ?
C11 C21 1.418(3) . ?
C21 C31 1.355(3) . ?
C31 C41 1.423(4) . ?
C41 C51 1.413(3) . ?
C41 C91 1.415(3) . ?
C51 C61 1.364(4) . ?
C61 C71 1.399(4) . ?
C71 C81 1.373(4) . ?
C81 C91 1.421(3) . ?
C91 C101 1.450(3) . ?
C101 C111 1.441(3) . ?
C111 N121 1.284(3) . ?
N121 O131 1.391(2) . ?
O131 Mn2 2.4017(16) 2_556 ?
O12 C12 1.336(3) . ?
C12 C102 1.402(3) . ?
C12 C22 1.422(3) . ?
C22 C32 1.357(4) . ?
C32 C42 1.427(4) . ?
C42 C52 1.411(4) . ?
C42 C92 1.418(3) . ?
C52 C62 1.365(4) . ?
C62 C72 1.406(4) . ?
C72 C82 1.371(4) . ?
C82 C92 1.421(4) . ?
C92 C102 1.447(3) . ?
C102 C112 1.447(3) . ?
C112 N122 1.287(3) . ?
N122 O132 1.378(2) . ?
O13 C13 1.332(3) . ?
C13 C103 1.401(3) . ?
C13 C23 1.427(3) . ?
C23 C33 1.356(3) . ?
C33 C43 1.421(4) . ?
C43 C93 1.418(3) . ?
C43 C53 1.419(3) . ?
C53 C63 1.364(4) . ?
C63 C73 1.407(4) . ?
C73 C83 1.369(4) . ?
C83 C93 1.416(3) . ?
C93 C103 1.445(3) . ?
C103 C113 1.450(3) . ?
C113 N123 1.296(3) . ?
N123 O133 1.372(2) . ?
N14 N24 1.205(3) . ?
N24 N34 1.147(3) . ?
N15 N25 1.200(3) . ?
N25 N35 1.146(3) . ?
N16 N26 1.188(3) . ?
N26 N36 1.154(3) . ?
O17 C27 1.417(3) . ?
O18 C28 1.412(4) . ?
O19 C29 1.428(4) . ?
O110 C210 1.423(4) . ?
O111 C211 1.419(6) . ?
O112 C212 1.385(5) . ?
O113 C213 1.409(4) . ?
O114 C214 1.428(4) . ?
O115 C215 1.414(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O11 167.60(8) . . ?
O1 Mn1 O133 92.61(7) . . ?
O11 Mn1 O133 88.06(7) . . ?
O1 Mn1 N121 88.24(7) . . ?
O11 Mn1 N121 88.54(7) . . ?
O133 Mn1 N121 167.80(8) . . ?
O1 Mn1 N14 93.61(7) . . ?
O11 Mn1 N14 98.61(8) . . ?
O133 Mn1 N14 96.97(8) . . ?
N121 Mn1 N14 95.12(8) . . ?
O1 Mn2 O12 173.68(7) . . ?
O1 Mn2 O131 89.37(6) . . ?
O12 Mn2 O131 90.33(7) . . ?
O1 Mn2 N122 89.76(7) . . ?
O12 Mn2 N122 89.10(7) . . ?
O131 Mn2 N122 166.90(8) . . ?
O1 Mn2 N15 92.93(7) . . ?
O12 Mn2 N15 93.38(7) . . ?
O131 Mn2 N15 95.35(7) . . ?
N122 Mn2 N15 97.74(8) . . ?
O1 Mn2 O131 86.07(6) . 2_556 ?
O12 Mn2 O131 87.64(6) . 2_556 ?
O131 Mn2 O131 82.16(6) . 2_556 ?
N122 Mn2 O131 84.75(7) . 2_556 ?
N15 Mn2 O131 177.32(7) . 2_556 ?
O1 Mn2 Mn3 30.96(5) . . ?
O12 Mn2 Mn3 146.80(5) . . ?
O131 Mn2 Mn3 118.56(5) . . ?
N122 Mn2 Mn3 58.96(5) . . ?
N15 Mn2 Mn3 99.33(5) . . ?
O131 Mn2 Mn3 81.07(4) 2_556 . ?
O13 Mn3 O1 175.47(7) . . ?
O13 Mn3 O132 90.71(7) . . ?
O1 Mn3 O132 93.01(7) . . ?
O13 Mn3 N123 88.78(7) . . ?
O1 Mn3 N123 87.67(7) . . ?
O132 Mn3 N123 176.61(8) . . ?
O13 Mn3 O17 91.32(7) . . ?
O1 Mn3 O17 85.82(7) . . ?
O132 Mn3 O17 94.06(7) . . ?
N123 Mn3 O17 89.31(8) . . ?
O13 Mn3 N16 97.22(7) . . ?
O1 Mn3 N16 85.44(7) . . ?
O132 Mn3 N16 89.33(7) . . ?
N123 Mn3 N16 87.41(8) . . ?
O17 Mn3 N16 170.78(7) . . ?
O13 Mn3 Mn2 153.37(5) . . ?
O1 Mn3 Mn2 30.51(5) . . ?
O132 Mn3 Mn2 62.67(5) . . ?
N123 Mn3 Mn2 117.75(5) . . ?
O17 Mn3 Mn2 91.37(4) . . ?
N16 Mn3 Mn2 82.56(5) . . ?
O110 Mn4 O19 83.34(8) . . ?
O110 Mn4 N15 92.31(8) . . ?
O19 Mn4 N15 88.99(8) . . ?
O110 Mn4 N14 92.40(8) . . ?
O19 Mn4 N14 175.73(8) . . ?
N15 Mn4 N14 91.50(8) . . ?
O110 Mn4 O18 80.79(8) . . ?
O19 Mn4 O18 89.61(8) . . ?
N15 Mn4 O18 173.08(7) . . ?
N14 Mn4 O18 89.40(8) . . ?
O110 Mn4 N16 165.62(8) . . ?
O19 Mn4 N16 85.70(8) . . ?
N15 Mn4 N16 96.79(8) . . ?
N14 Mn4 N16 98.45(8) . . ?
O18 Mn4 N16 89.87(7) . . ?
Mn1 O1 Mn2 121.98(8) . . ?
Mn1 O1 Mn3 119.48(8) . . ?
Mn2 O1 Mn3 118.53(8) . . ?
C11 O11 Mn1 129.55(15) . . ?
O11 C11 C101 123.5(2) . . ?
O11 C11 C21 116.7(2) . . ?
C101 C11 C21 119.7(2) . . ?
C31 C21 C11 120.9(2) . . ?
C21 C31 C41 121.6(2) . . ?
C51 C41 C91 119.7(2) . . ?
C51 C41 C31 121.4(2) . . ?
C91 C41 C31 118.9(2) . . ?
C61 C51 C41 121.3(2) . . ?
C51 C61 C71 119.4(2) . . ?
C81 C71 C61 121.0(2) . . ?
C71 C81 C91 120.9(2) . . ?
C41 C91 C81 117.7(2) . . ?
C41 C91 C101 119.1(2) . . ?
C81 C91 C101 123.2(2) . . ?
C11 C101 C111 121.4(2) . . ?
C11 C101 C91 119.7(2) . . ?
C111 C101 C91 118.8(2) . . ?
N121 C111 C101 124.2(2) . . ?
C111 N121 O131 114.28(18) . . ?
C111 N121 Mn1 127.38(16) . . ?
O131 N121 Mn1 117.77(13) . . ?
N121 O131 Mn2 114.72(12) . . ?
N121 O131 Mn2 108.01(12) . 2_556 ?
Mn2 O131 Mn2 97.84(6) . 2_556 ?
C12 O12 Mn2 125.05(14) . . ?
O12 C12 C102 123.3(2) . . ?
O12 C12 C22 116.8(2) . . ?
C102 C12 C22 119.9(2) . . ?
C32 C22 C12 121.1(2) . . ?
C22 C32 C42 121.3(2) . . ?
C52 C42 C92 119.8(2) . . ?
C52 C42 C32 121.2(2) . . ?
C92 C42 C32 119.0(2) . . ?
C62 C52 C42 121.2(3) . . ?
C52 C62 C72 119.4(3) . . ?
C82 C72 C62 120.8(3) . . ?
C72 C82 C92 121.0(3) . . ?
C42 C92 C82 117.7(2) . . ?
C42 C92 C102 119.5(2) . . ?
C82 C92 C102 122.9(2) . . ?
C12 C102 C112 121.4(2) . . ?
C12 C102 C92 119.3(2) . . ?
C112 C102 C92 119.2(2) . . ?
N122 C112 C102 123.8(2) . . ?
C112 N122 O132 115.55(18) . . ?
C112 N122 Mn2 126.15(16) . . ?
O132 N122 Mn2 117.84(13) . . ?
N122 O132 Mn3 114.15(13) . . ?
C13 O13 Mn3 123.33(15) . . ?
O13 C13 C103 123.4(2) . . ?
O13 C13 C23 116.5(2) . . ?
C103 C13 C23 120.0(2) . . ?
C33 C23 C13 120.8(2) . . ?
C23 C33 C43 121.3(2) . . ?
C93 C43 C53 119.9(2) . . ?
C93 C43 C33 119.1(2) . . ?
C53 C43 C33 121.0(2) . . ?
C63 C53 C43 121.0(2) . . ?
C53 C63 C73 119.2(2) . . ?
C83 C73 C63 121.1(3) . . ?
C73 C83 C93 121.2(2) . . ?
C83 C93 C43 117.5(2) . . ?
C83 C93 C103 122.9(2) . . ?
C43 C93 C103 119.5(2) . . ?
C13 C103 C93 119.0(2) . . ?
C13 C103 C113 121.0(2) . . ?
C93 C103 C113 119.9(2) . . ?
N123 C113 C103 122.8(2) . . ?
C113 N123 O133 116.99(18) . . ?
C113 N123 Mn3 124.88(16) . . ?
O133 N123 Mn3 118.13(13) . . ?
N123 O133 Mn1 113.64(12) . . ?
N24 N14 Mn1 118.82(17) . . ?
N24 N14 Mn4 122.03(17) . . ?
Mn1 N14 Mn4 119.14(9) . . ?
N34 N24 N14 179.1(3) . . ?
N25 N15 Mn2 118.10(17) . . ?
N25 N15 Mn4 122.89(18) . . ?
Mn2 N15 Mn4 118.26(9) . . ?
N35 N25 N15 179.1(3) . . ?
N26 N16 Mn4 122.41(17) . . ?
N26 N16 Mn3 113.47(16) . . ?
Mn4 N16 Mn3 121.54(9) . . ?
N36 N26 N16 178.5(3) . . ?
C27 O17 Mn3 121.85(17) . . ?
C28 O18 Mn4 125.39(19) . . ?
C29 O19 Mn4 127.81(19) . . ?
C210 O110 Mn4 127.25(19) . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.088

# Attachment 'Complex_3_revised.cif'

data_eb6122
_database_code_depnum_ccdc_archive 'CCDC 638208'

_audit_creation_date             07-02-23
_audit_creation_method           CRYSTALS_ver_12.84

_oxford_structure_analysis_title 'new in P-1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   11.698(2)
_cell_length_b                   12.608(3)
_cell_length_c                   17.019(3)
_cell_angle_alpha                76.05(3)
_cell_angle_beta                 82.03(3)
_cell_angle_gamma                75.41(3)
_cell_volume                     2349.4(9)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

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            1

# Given Formula = C66 H114 Mn8 N24 O32
# Dc = 1.55 Fooo = 954.00 Mu = 11.28 M = 1098.61
# Found Formula = C56 H74 Mn8 N24 O22
# Dc = 1.33 FOOO = 954.00 Mu = 11.08 M = 937.39

_chemical_formula_sum            'C66 H114 Mn8 N24 O32'
_chemical_formula_moiety         '[Mn8(O)2(MeSaO)6(N3)6(MeOH)8].10MeOH'
_chemical_formula_weight         2195.3

_cell_measurement_reflns_used    6945
_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          0.12
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_max          0.42

_exptl_crystal_density_diffrn    1.55
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             954
_exptl_absorpt_coefficient_mu    1.128

# Sheldrick geometric approximatio 0.78 0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.88
_diffrn_measurement_device_type  'Bruker SMART'
_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    'SHELXS 86 (Sheldrick, 1986)'
_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            67762
_reflns_number_total             9606
_diffrn_reflns_av_R_equivalents  0.103
# Number of reflections with Friedels Law is 9606
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 9608

_diffrn_reflns_theta_min         1.237
_diffrn_reflns_theta_max         26.372
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        26.372
_diffrn_measured_fraction_theta_full 0.999

_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_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         -0.84
_refine_diff_density_max         2.05

_refine_ls_number_reflns         4959
_refine_ls_number_restraints     18
_refine_ls_number_parameters     496

#_refine_ls_R_factor_ref 0.0698
_refine_ls_wR_factor_ref         0.0574
_refine_ls_goodness_of_fit_ref   1.2266

#_reflns_number_all 9565
_refine_ls_R_factor_all          0.1203
_refine_ls_wR_factor_all         0.0662

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                4959
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_gt          0.0574

_refine_ls_shift/su_max          0.000272

# 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 F
_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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
2.26 -1.83 1.30
;

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.587 0.500 622.7 184.8
_platon_squeeze_details          
;
This equates to ca 10MeOH molecules per formula unit (180 e/cell).
;

_publ_section_exptl_refinement   
;
The hydrogens atoms were placed geometrically.

Disordered solved was treated with the Squeeze procedure (see above).

The thermal parameters of the terminal N atoms of the azides where restrainted
to be similar to those belonging to the other N atoms.
The same procedure has been applied to C(24) and O(14) of an attached methanol
molecule.

Numbering Scheme:
Mn: 1-4
MeSaO: 1* to 8* (where * is 1-3)
MeOH: 1* to 2* (where * is 4-7)
Azides: 1* to 3* (where * is 8-10)

Oxidation State:

The azides have a charge of 1-, MeSaO and O each have a charge of 2- whereas
the methanols are neutral, this adds up to a charge for the ligands of 22-.
There are 8 Mn atoms, so there must be 6Mn(III) and 2Mn(II).

Checkcif output:

602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure !
602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure !

Squeeze procedure used (see above)

420_ALERT_2_B D-H Without Acceptor O14 - H114 ... ?
420_ALERT_2_B D-H Without Acceptor O15 - H115 ... ?
420_ALERT_2_B D-H Without Acceptor O16 - H116 ... ?
420_ALERT_2_B D-H Without Acceptor O17 - H117 ... ?

Atoms placed geometrically

911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 0.600 3
912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 10

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 1.000 4927 4926 1
23.01 0.550 1.000 6550 6549 1
25.24 0.600 1.000 8485 8482 3
#----------------------------------------------------------- ACTA Min. Res. ---
26.37 0.625 0.999 9619 9606 13

061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.75

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of equivalent data. It is possible that the larger than expected
range of transmission is accounted for by crystal decay or absorption by
the mounting fibre.

220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.04 Ratio
220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.61 Ratio
222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.78 Ratio
414_ALERT_2_C Short Intra D-H..H-X H114 .. H283 .. 1.94 Ang.
232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn3 - O14 .. 5.02 su

No action taken here

094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.44
097_ALERT_2_C Maximum (Positive) Residual Density ............ 2.05 e/A**

Noted but after the squeezing procedure using chemical sense there aren't
reasonable peaks into the difference map.

020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.10
213_ALERT_2_C Atom C25 has ADP max/min Ratio ............. 3.40 oblat
341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11

This might be an indication that the quality of the structure is not very high
;

# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

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.

Sheldrick, G.M. (1986). SHELXS86. Program for the solution of
crystal structures. Univ. of G\"ottingen, Federal Republic of Germany.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437.

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn2 Mn 0.06993(9) 0.88333(9) 0.05227(6) 0.0267 1.0000 Uani . . . . . .
Mn3 Mn -0.09498(9) 0.84949(9) 0.22140(6) 0.0259 1.0000 Uani . . . . . .
Mn1 Mn 0.01297(9) 1.07079(9) 0.16453(6) 0.0256 1.0000 Uani . . . . . .
Mn4 Mn 0.23657(10) 0.79727(9) 0.24110(7) 0.0329 1.0000 Uani . . . . . .
N18 N 0.0716(5) 0.7380(5) 0.2706(4) 0.0300 1.0000 Uani . . . . . .
N19 N 0.2387(5) 0.8226(5) 0.1061(4) 0.0391 1.0000 Uani . . . . . .
N28 N 0.0752(5) 0.6376(6) 0.2863(3) 0.0309 1.0000 Uani . . . . . .
N29 N 0.3297(6) 0.8225(7) 0.0639(5) 0.0559 1.0000 Uani . U . . . .
N38 N 0.0752(6) 0.5438(6) 0.3015(4) 0.0492 1.0000 Uani . . . . . .
N39 N 0.4141(7) 0.8228(8) 0.0208(5) 0.0741 1.0000 Uani . U . . . .
N71 N 0.0057(5) 0.7453(5) 0.0944(3) 0.0284 1.0000 Uani . . . . . .
N72 N -0.1133(5) 0.9589(5) 0.2941(3) 0.0288 1.0000 Uani . . . . . .
N73 N 0.1258(5) 1.0837(5) 0.0655(3) 0.0296 1.0000 Uani . . . . . .
N110 N 0.1546(5) 0.9729(5) 0.2461(3) 0.0285 1.0000 Uani . . . . . .
N210 N 0.1632(7) 1.0051(5) 0.3056(4) 0.0489 1.0000 Uani . U . . . .
N310 N 0.1693(9) 1.0376(7) 0.3622(5) 0.0718 1.0000 Uani . U . . . .
O1 O -0.0061(4) 0.9379(4) 0.1433(3) 0.0277 1.0000 Uani . . . . . .
O11 O 0.1260(4) 0.8332(4) -0.0454(3) 0.0339 1.0000 Uani . . . . . .
O12 O -0.1960(4) 0.7760(4) 0.2994(3) 0.0305 1.0000 Uani . . . . . .
O13 O 0.0233(4) 1.2137(4) 0.1728(3) 0.0310 1.0000 Uani . . . . . .
O14 O -0.2602(4) 0.9863(5) 0.1644(3) 0.0456 1.0000 Uani . U . . . .
O15 O 0.3430(5) 0.6251(5) 0.2453(4) 0.0667 1.0000 Uani . . . . . .
O16 O 0.4136(5) 0.8369(5) 0.2254(4) 0.0508 1.0000 Uani . . . . . .
O17 O 0.2694(5) 0.7552(5) 0.3713(3) 0.0500 1.0000 Uani . . . . . .
O71 O -0.0937(4) 0.7550(4) 0.1482(3) 0.0291 1.0000 Uani . . . . . .
O72 O -0.1062(4) 1.0662(4) 0.2539(3) 0.0358 1.0000 Uani . . . . . .
O73 O 0.1100(4) 1.0313(4) 0.0059(3) 0.0307 1.0000 Uani . . . . . .
C11 C 0.1839(6) 0.7251(6) -0.0406(4) 0.0335 1.0000 Uani . . . . . .
C12 C -0.1730(6) 0.7503(6) 0.3776(4) 0.0323 1.0000 Uani . . . . . .
C13 C 0.1320(6) 1.2336(6) 0.1676(4) 0.0311 1.0000 Uani . . . . . .
C21 C 0.2842(8) 0.7016(7) -0.0930(5) 0.0534 1.0000 Uani . . . . . .
C22 C -0.1777(8) 0.6429(7) 0.4234(5) 0.0509 1.0000 Uani . . . . . .
C23 C 0.1499(7) 1.2957(6) 0.2209(5) 0.0373 1.0000 Uani . . . . . .
C24 C -0.3488(10) 1.0497(10) 0.2203(7) 0.0848 1.0000 Uani . U . . . .
C25 C 0.3647(10) 0.5683(8) 0.1808(7) 0.0837 1.0000 Uani . . . . . .
C26 C 0.4389(8) 0.9421(8) 0.1821(6) 0.0568 1.0000 Uani . . . . . .
C27 C 0.1881(9) 0.7361(9) 0.4388(6) 0.0634 1.0000 Uani . . . . . .
C31 C 0.3488(8) 0.5918(7) -0.0900(6) 0.0606 1.0000 Uani . . . . . .
C32 C -0.1597(9) 0.6138(7) 0.5036(5) 0.0598 1.0000 Uani . . . . . .
C33 C 0.2609(7) 1.3182(7) 0.2199(5) 0.0436 1.0000 Uani . . . . . .
C41 C 0.3144(7) 0.5040(7) -0.0360(6) 0.0526 1.0000 Uani . . . . . .
C42 C -0.1330(9) 0.6896(8) 0.5426(5) 0.0587 1.0000 Uani . . . . . .
C43 C 0.3519(7) 1.2829(7) 0.1675(5) 0.0410 1.0000 Uani . . . . . .
C51 C 0.2139(7) 0.5256(7) 0.0148(5) 0.0395 1.0000 Uani . . . . . .
C52 C -0.1309(8) 0.7945(7) 0.4989(4) 0.0430 1.0000 Uani . . . . . .
C53 C 0.3337(6) 1.2232(6) 0.1128(5) 0.0357 1.0000 Uani . . . . . .
C61 C 0.1467(6) 0.6340(6) 0.0146(4) 0.0310 1.0000 Uani . . . . . .
C62 C -0.1469(6) 0.8274(6) 0.4166(4) 0.0303 1.0000 Uani . . . . . .
C63 C 0.2231(6) 1.1999(6) 0.1111(4) 0.0287 1.0000 Uani . . . . . .
C71 C 0.0406(6) 0.6508(6) 0.0714(4) 0.0281 1.0000 Uani . . . . . .
C72 C -0.1349(6) 0.9402(6) 0.3708(4) 0.0324 1.0000 Uani . . . . . .
C73 C 0.2114(6) 1.1366(6) 0.0520(4) 0.0289 1.0000 Uani . . . . . .
C81 C -0.0276(7) 0.5599(6) 0.1049(5) 0.0384 1.0000 Uani . . . . . .
C82 C -0.1473(8) 1.0340(7) 0.4153(5) 0.0482 1.0000 Uani . . . . . .
C83 C 0.2953(6) 1.1316(7) -0.0221(5) 0.0397 1.0000 Uani . . . . . .
H114 H -0.2846 0.9856 0.1220 0.0621 1.0000 Uiso R . . . . .
H115 H 0.3230 0.5815 0.2858 0.1001 1.0000 Uiso R . . . . .
H116 H 0.4716 0.8019 0.2508 0.0749 1.0000 Uiso R . . . . .
H117 H 0.3314 0.7265 0.3933 0.0758 1.0000 Uiso R . . . . .
H121 H 0.3084 0.7607 -0.1295 0.0671 1.0000 Uiso R . . . . .
H122 H -0.1943 0.5913 0.3983 0.0622 1.0000 Uiso R . . . . .
H123 H 0.0875 1.3224 0.2560 0.0431 1.0000 Uiso R . . . . .
H125 H 0.4082 0.4929 0.1988 0.1289 1.0000 Uiso R . . . . .
H126 H 0.5229 0.9372 0.1755 0.0839 1.0000 Uiso R . . . . .
H127 H 0.1346 0.6964 0.4275 0.1131 1.0000 Uiso R . . . . .
H131 H 0.4154 0.5777 -0.1259 0.0730 1.0000 Uiso R . . . . .
H132 H -0.1643 0.5419 0.5328 0.0698 1.0000 Uiso R . . . . .
H133 H 0.2729 1.3565 0.2572 0.0569 1.0000 Uiso R . . . . .
H141 H 0.3588 0.4312 -0.0338 0.0581 1.0000 Uiso R . . . . .
H142 H -0.1198 0.6696 0.5970 0.0709 1.0000 Uiso R . . . . .
H143 H 0.4265 1.2967 0.1683 0.0500 1.0000 Uiso R . . . . .
H151 H 0.1899 0.4662 0.0518 0.0457 1.0000 Uiso R . . . . .
H152 H -0.1184 0.8460 0.5257 0.0539 1.0000 Uiso R . . . . .
H153 H 0.3964 1.1994 0.0762 0.0429 1.0000 Uiso R . . . . .
H181 H 0.0033 0.4981 0.0791 0.0588 1.0000 Uiso R . . . . .
H182 H -0.0713 1.0502 0.4137 0.0752 1.0000 Uiso R . . . . .
H183 H 0.3366 1.1914 -0.0326 0.0603 1.0000 Uiso R . . . . .
H225 H 0.4099 0.6056 0.1361 0.1290 1.0000 Uiso R . . . . .
H226 H 0.4012 0.9984 0.2139 0.0839 1.0000 Uiso R . . . . .
H227 H 0.1440 0.8055 0.4520 0.1131 1.0000 Uiso R . . . . .
H241 H -0.3144 1.0988 0.2416 0.1622 1.0000 Uiso R . . . . .
H242 H -0.4172 1.0942 0.1915 0.1622 1.0000 Uiso R . . . . .
H243 H -0.3754 0.9955 0.2657 0.1622 1.0000 Uiso R . . . . .
H281 H -0.1105 0.5878 0.0965 0.0587 1.0000 Uiso R . . . . .
H282 H -0.2013 1.0994 0.3891 0.0749 1.0000 Uiso R . . . . .
H283 H 0.2518 1.1388 -0.0673 0.0600 1.0000 Uiso R . . . . .
H325 H 0.2900 0.5677 0.1636 0.1289 1.0000 Uiso R . . . . .
H326 H 0.4074 0.9639 0.1296 0.0840 1.0000 Uiso R . . . . .
H327 H 0.2311 0.6903 0.4844 0.1129 1.0000 Uiso R . . . . .
H381 H -0.0202 0.5339 0.1620 0.0590 1.0000 Uiso R . . . . .
H382 H -0.1761 1.0098 0.4703 0.0750 1.0000 Uiso R . . . . .
H383 H 0.3511 1.0610 -0.0129 0.0602 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
Mn2 0.0251(6) 0.0332(6) 0.0265(6) -0.0157(5) 0.0061(5) -0.0108(5)
Mn3 0.0254(6) 0.0311(6) 0.0241(6) -0.0118(5) 0.0041(5) -0.0096(5)
Mn1 0.0262(6) 0.0253(6) 0.0256(6) -0.0107(5) 0.0044(5) -0.0051(5)
Mn4 0.0290(6) 0.0272(6) 0.0459(7) -0.0177(5) -0.0037(5) -0.0028(5)
N18 0.032(3) 0.026(3) 0.034(3) -0.011(3) 0.000(3) -0.008(3)
N19 0.025(3) 0.041(4) 0.060(4) -0.032(3) 0.011(3) -0.010(3)
N28 0.022(3) 0.042(4) 0.029(3) -0.014(3) 0.005(3) -0.005(3)
N29 0.024(3) 0.083(5) 0.079(5) -0.056(4) 0.024(3) -0.024(3)
N38 0.061(5) 0.022(4) 0.067(5) -0.010(3) 0.004(4) -0.019(3)
N39 0.044(4) 0.115(6) 0.084(5) -0.065(5) 0.027(4) -0.031(4)
N71 0.026(3) 0.033(3) 0.030(3) -0.012(3) 0.000(3) -0.008(3)
N72 0.038(3) 0.023(3) 0.028(3) -0.012(3) 0.002(3) -0.010(3)
N73 0.022(3) 0.037(4) 0.032(3) -0.018(3) -0.004(3) -0.001(3)
N110 0.031(3) 0.029(3) 0.028(3) -0.014(3) 0.001(3) -0.006(3)
N210 0.085(5) 0.026(3) 0.039(4) -0.014(3) -0.020(4) -0.004(3)
N310 0.123(6) 0.046(4) 0.051(5) -0.023(4) -0.029(4) -0.004(4)
O1 0.028(3) 0.034(3) 0.026(3) -0.015(2) 0.005(2) -0.010(2)
O11 0.041(3) 0.036(3) 0.030(3) -0.018(2) 0.004(2) -0.011(2)
O12 0.032(3) 0.032(3) 0.027(3) -0.007(2) 0.003(2) -0.009(2)
O13 0.029(3) 0.029(3) 0.040(3) -0.019(2) 0.006(2) -0.009(2)
O14 0.039(3) 0.055(4) 0.047(3) -0.020(3) 0.001(3) -0.012(3)
O15 0.058(4) 0.041(4) 0.112(6) -0.045(4) -0.008(4) -0.004(3)
O16 0.035(3) 0.034(3) 0.082(4) -0.013(3) -0.008(3) -0.005(3)
O17 0.047(3) 0.048(4) 0.055(4) -0.013(3) -0.006(3) -0.009(3)
O71 0.022(2) 0.038(3) 0.032(3) -0.019(2) 0.012(2) -0.012(2)
O72 0.044(3) 0.025(3) 0.034(3) -0.008(2) 0.011(2) -0.006(2)
O73 0.030(3) 0.041(3) 0.028(3) -0.020(2) 0.009(2) -0.016(2)
C11 0.036(4) 0.037(4) 0.035(4) -0.018(3) 0.004(3) -0.017(4)
C12 0.036(4) 0.039(4) 0.021(4) -0.011(3) 0.009(3) -0.011(3)
C13 0.035(4) 0.031(4) 0.026(4) -0.009(3) 0.001(3) -0.004(3)
C21 0.057(5) 0.047(5) 0.061(6) -0.027(5) 0.032(5) -0.026(4)
C22 0.085(7) 0.033(5) 0.042(5) -0.015(4) -0.002(5) -0.021(5)
C23 0.039(4) 0.039(5) 0.038(4) -0.020(4) 0.006(4) -0.011(4)
C24 0.064(6) 0.088(7) 0.088(7) -0.011(6) 0.002(5) -0.003(5)
C25 0.085(8) 0.046(6) 0.137(10) -0.067(7) -0.005(7) -0.003(5)
C26 0.052(6) 0.047(6) 0.068(6) -0.006(5) -0.013(5) -0.009(4)
C27 0.067(6) 0.079(7) 0.053(6) -0.028(5) 0.016(5) -0.029(6)
C31 0.050(5) 0.043(5) 0.091(7) -0.040(5) 0.043(5) -0.015(4)
C32 0.107(8) 0.032(5) 0.041(5) -0.003(4) -0.001(5) -0.022(5)
C33 0.048(5) 0.047(5) 0.045(5) -0.023(4) -0.002(4) -0.016(4)
C41 0.049(5) 0.040(5) 0.070(6) -0.030(5) 0.015(5) -0.004(4)
C42 0.110(8) 0.053(6) 0.020(4) -0.005(4) -0.009(5) -0.032(6)
C43 0.033(4) 0.042(5) 0.057(5) -0.022(4) -0.002(4) -0.017(4)
C51 0.046(5) 0.038(5) 0.042(5) -0.020(4) 0.010(4) -0.017(4)
C52 0.072(6) 0.036(5) 0.025(4) -0.006(3) -0.002(4) -0.021(4)
C53 0.030(4) 0.041(5) 0.040(4) -0.019(4) 0.003(3) -0.008(3)
C61 0.027(4) 0.041(4) 0.031(4) -0.019(3) -0.002(3) -0.010(3)
C62 0.030(4) 0.024(4) 0.036(4) -0.009(3) -0.001(3) -0.004(3)
C63 0.025(4) 0.030(4) 0.030(4) -0.008(3) -0.002(3) -0.003(3)
C71 0.023(4) 0.040(4) 0.027(4) -0.013(3) -0.002(3) -0.012(3)
C72 0.034(4) 0.036(4) 0.029(4) -0.014(3) 0.001(3) -0.009(3)
C73 0.018(3) 0.038(4) 0.031(4) -0.010(3) 0.000(3) -0.005(3)
C81 0.046(5) 0.037(4) 0.037(4) -0.018(4) 0.010(4) -0.015(4)
C82 0.088(7) 0.035(5) 0.029(4) -0.018(4) 0.014(4) -0.026(5)
C83 0.027(4) 0.053(5) 0.045(5) -0.023(4) 0.005(3) -0.012(4)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4358(7)
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
Mn2 . O73 2_575 2.344(5) yes
Mn2 . Mn2 2_575 3.218(3) yes
Mn2 . N19 . 2.173(6) yes
Mn2 . N71 . 2.004(6) yes
Mn2 . O1 . 1.867(4) yes
Mn2 . O11 . 1.894(4) yes
Mn2 . O73 . 1.987(5) yes
Mn3 . N18 . 2.232(6) yes
Mn3 . N72 . 2.020(5) yes
Mn3 . O1 . 1.891(5) yes
Mn3 . O12 . 1.882(5) yes
Mn3 . O14 . 2.384(6) yes
Mn3 . O71 . 1.916(4) yes
Mn1 . O11 2_575 2.638(5) yes
Mn1 . N73 . 1.992(6) yes
Mn1 . N110 . 2.231(6) yes
Mn1 . O1 . 1.868(4) yes
Mn1 . O13 . 1.876(5) yes
Mn1 . O72 . 1.916(5) yes
Mn4 . N18 . 2.194(6) yes
Mn4 . N19 . 2.240(7) yes
Mn4 . N110 . 2.197(6) yes
Mn4 . O15 . 2.203(6) yes
Mn4 . O16 . 2.216(5) yes
Mn4 . O17 . 2.215(6) yes
N18 . N28 . 1.220(8) yes
N19 . N29 . 1.198(8) yes
N28 . N38 . 1.148(8) yes
N29 . N39 . 1.146(9) yes
N71 . O71 . 1.376(7) yes
N71 . C71 . 1.295(8) yes
N72 . O72 . 1.378(7) yes
N72 . C72 . 1.270(8) yes
N73 . O73 . 1.391(7) yes
N73 . C73 . 1.303(9) yes
N110 . N210 . 1.204(8) yes
N210 . N310 . 1.150(9) yes
O11 . C11 . 1.349(9) yes
O12 . C12 . 1.339(8) yes
O13 . C13 . 1.344(8) yes
O14 . C24 . 1.514(11) yes
O14 . H114 . 0.815 no
O15 . C25 . 1.411(10) yes
O15 . H115 . 0.819 no
O16 . C26 . 1.434(10) yes
O16 . H116 . 0.826 no
O17 . C27 . 1.402(10) yes
O17 . H117 . 0.822 no
C11 . C21 . 1.386(10) yes
C11 . C61 . 1.417(10) yes
C12 . C22 . 1.401(11) yes
C12 . C62 . 1.413(10) yes
C13 . C23 . 1.399(9) yes
C13 . C63 . 1.388(9) yes
C21 . C31 . 1.394(12) yes
C21 . H121 . 0.926 no
C22 . C32 . 1.356(12) yes
C22 . H122 . 0.930 no
C23 . C33 . 1.393(10) yes
C23 . H123 . 0.926 no
C24 . H241 . 0.976 no
C24 . H242 . 0.972 no
C24 . H243 . 0.974 no
C25 . H125 . 0.957 no
C25 . H225 . 0.959 no
C25 . H325 . 0.962 no
C26 . H126 . 0.962 no
C26 . H226 . 0.977 no
C26 . H326 . 0.965 no
C27 . H127 . 0.957 no
C27 . H227 . 0.957 no
C27 . H327 . 0.966 no
C31 . C41 . 1.364(12) yes
C31 . H131 . 0.930 no
C32 . C42 . 1.402(12) yes
C32 . H132 . 0.934 no
C33 . C43 . 1.348(10) yes
C33 . H133 . 0.928 no
C41 . C51 . 1.369(10) yes
C41 . H141 . 0.930 no
C42 . C52 . 1.356(11) yes
C42 . H142 . 0.923 no
C43 . C53 . 1.397(10) yes
C43 . H143 . 0.934 no
C51 . C61 . 1.394(10) yes
C51 . H151 . 0.930 no
C52 . C62 . 1.387(10) yes
C52 . H152 . 0.926 no
C53 . C63 . 1.403(9) yes
C53 . H153 . 0.932 no
C61 . C71 . 1.467(9) yes
C62 . C72 . 1.478(10) yes
C63 . C73 . 1.466(9) yes
C71 . C81 . 1.515(10) yes
C72 . C82 . 1.519(9) yes
C73 . C83 . 1.489(9) yes
C81 . H181 . 0.955 no
C81 . H281 . 0.962 no
C81 . H381 . 0.955 no
C82 . H182 . 0.957 no
C82 . H282 . 0.957 no
C82 . H382 . 0.954 no
C83 . H183 . 0.964 no
C83 . H283 . 0.954 no
C83 . H383 . 0.955 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
O73 2_575 Mn2 . Mn2 2_575 37.92(12) yes
O73 2_575 Mn2 . N19 . 173.7(2) yes
Mn2 2_575 Mn2 . N19 . 136.23(18) yes
O73 2_575 Mn2 . N71 . 87.4(2) yes
Mn2 2_575 Mn2 . N71 . 125.33(18) yes
N19 . Mn2 . N71 . 98.3(2) yes
O73 2_575 Mn2 . O1 . 85.00(18) yes
Mn2 2_575 Mn2 . O1 . 85.69(16) yes
N19 . Mn2 . O1 . 92.4(2) yes
N71 . Mn2 . O1 . 89.1(2) yes
O73 2_575 Mn2 . O11 . 87.29(19) yes
Mn2 2_575 Mn2 . O11 . 89.25(17) yes
N19 . Mn2 . O11 . 95.4(2) yes
N71 . Mn2 . O11 . 88.9(2) yes
O1 . Mn2 . O11 . 172.1(2) yes
O73 2_575 Mn2 . O73 . 84.38(18) yes
Mn2 2_575 Mn2 . O73 . 46.45(14) yes
N19 . Mn2 . O73 . 89.8(2) yes
N71 . Mn2 . O73 . 171.7(2) yes
O1 . Mn2 . O73 . 88.92(19) yes
O11 . Mn2 . O73 . 92.0(2) yes
N18 . Mn3 . N72 . 95.1(2) yes
N18 . Mn3 . O1 . 90.5(2) yes
N72 . Mn3 . O1 . 88.8(2) yes
N18 . Mn3 . O12 . 94.6(2) yes
N72 . Mn3 . O12 . 87.3(2) yes
O1 . Mn3 . O12 . 173.8(2) yes
N18 . Mn3 . O14 . 173.1(2) yes
N72 . Mn3 . O14 . 81.4(2) yes
O1 . Mn3 . O14 . 83.5(2) yes
O12 . Mn3 . O14 . 91.2(2) yes
N18 . Mn3 . O71 . 91.1(2) yes
N72 . Mn3 . O71 . 173.8(2) yes
O1 . Mn3 . O71 . 91.57(19) yes
O12 . Mn3 . O71 . 91.8(2) yes
O14 . Mn3 . O71 . 92.5(2) yes
O11 2_575 Mn1 . N73 . 76.3(2) yes
O11 2_575 Mn1 . N110 . 168.25(16) yes
N73 . Mn1 . N110 . 93.5(2) yes
O11 2_575 Mn1 . O1 . 83.66(18) yes
N73 . Mn1 . O1 . 88.0(2) yes
N110 . Mn1 . O1 . 90.2(2) yes
O11 2_575 Mn1 . O13 . 88.95(19) yes
N73 . Mn1 . O13 . 88.7(2) yes
N110 . Mn1 . O13 . 96.8(2) yes
O1 . Mn1 . O13 . 172.4(2) yes
O11 2_575 Mn1 . O72 . 98.73(19) yes
N73 . Mn1 . O72 . 175.0(2) yes
N110 . Mn1 . O72 . 91.5(2) yes
O1 . Mn1 . O72 . 92.2(2) yes
O13 . Mn1 . O72 . 90.6(2) yes
N18 . Mn4 . N19 . 96.2(2) yes
N18 . Mn4 . N110 . 95.9(2) yes
N19 . Mn4 . N110 . 95.7(2) yes
N18 . Mn4 . O15 . 91.6(2) yes
N19 . Mn4 . O15 . 89.1(3) yes
N110 . Mn4 . O15 . 170.6(2) yes
N18 . Mn4 . O16 . 171.8(2) yes
N19 . Mn4 . O16 . 89.6(2) yes
N110 . Mn4 . O16 . 89.3(2) yes
O15 . Mn4 . O16 . 82.7(2) yes
N18 . Mn4 . O17 . 90.9(2) yes
N19 . Mn4 . O17 . 169.3(2) yes
N110 . Mn4 . O17 . 91.5(2) yes
O15 . Mn4 . O17 . 82.6(2) yes
O16 . Mn4 . O17 . 82.6(2) yes
Mn4 . N18 . Mn3 . 119.1(3) yes
Mn4 . N18 . N28 . 120.0(5) yes
Mn3 . N18 . N28 . 115.7(5) yes
Mn4 . N19 . Mn2 . 117.9(3) yes
Mn4 . N19 . N29 . 120.6(6) yes
Mn2 . N19 . N29 . 120.2(6) yes
N18 . N28 . N38 . 178.2(7) yes
N19 . N29 . N39 . 177.1(9) yes
Mn2 . N71 . O71 . 116.5(4) yes
Mn2 . N71 . C71 . 127.3(5) yes
O71 . N71 . C71 . 115.9(5) yes
Mn3 . N72 . O72 . 114.8(4) yes
Mn3 . N72 . C72 . 127.2(5) yes
O72 . N72 . C72 . 118.0(5) yes
Mn1 . N73 . O73 . 116.1(4) yes
Mn1 . N73 . C73 . 125.9(4) yes
O73 . N73 . C73 . 118.0(5) yes
Mn4 . N110 . Mn1 . 119.7(2) yes
Mn4 . N110 . N210 . 118.5(5) yes
Mn1 . N110 . N210 . 118.9(5) yes
N110 . N210 . N310 . 178.6(9) yes
Mn3 . O1 . Mn1 . 118.6(2) yes
Mn3 . O1 . Mn2 . 118.8(2) yes
Mn1 . O1 . Mn2 . 122.4(2) yes
Mn2 . O11 . Mn1 2_575 113.7(2) yes
Mn2 . O11 . C11 . 118.6(4) yes
Mn1 2_575 O11 . C11 . 118.0(4) yes
Mn3 . O12 . C12 . 118.8(4) yes
Mn1 . O13 . C13 . 117.7(4) yes
Mn3 . O14 . C24 . 118.4(5) yes
Mn3 . O14 . H114 . 122.7 no
C24 . O14 . H114 . 115.3 no
Mn4 . O15 . C25 . 125.5(7) yes
Mn4 . O15 . H115 . 111.3 no
C25 . O15 . H115 . 106.5 no
Mn4 . O16 . C26 . 124.6(5) yes
Mn4 . O16 . H116 . 127.1 no
C26 . O16 . H116 . 106.9 no
Mn4 . O17 . C27 . 127.9(5) yes
Mn4 . O17 . H117 . 130.1 no
C27 . O17 . H117 . 99.2 no
N71 . O71 . Mn3 . 113.5(3) yes
N72 . O72 . Mn1 . 113.6(4) yes
Mn2 2_575 O73 . N73 . 111.5(3) yes
Mn2 2_575 O73 . Mn2 . 95.62(18) yes
N73 . O73 . Mn2 . 112.5(4) yes
O11 . C11 . C21 . 118.4(7) yes
O11 . C11 . C61 . 123.5(6) yes
C21 . C11 . C61 . 118.2(7) yes
O12 . C12 . C22 . 118.6(7) yes
O12 . C12 . C62 . 123.1(7) yes
C22 . C12 . C62 . 118.3(7) yes
O13 . C13 . C23 . 116.6(6) yes
O13 . C13 . C63 . 123.7(6) yes
C23 . C13 . C63 . 119.7(7) yes
C11 . C21 . C31 . 121.0(8) yes
C11 . C21 . H121 . 118.6 no
C31 . C21 . H121 . 120.4 no
C12 . C22 . C32 . 121.1(7) yes
C12 . C22 . H122 . 119.1 no
C32 . C22 . H122 . 119.8 no
C13 . C23 . C33 . 119.9(7) yes
C13 . C23 . H123 . 119.6 no
C33 . C23 . H123 . 120.5 no
O14 . C24 . H241 . 112.1 no
O14 . C24 . H242 . 110.1 no
H241 . C24 . H242 . 109.1 no
O14 . C24 . H243 . 108.5 no
H241 . C24 . H243 . 108.5 no
H242 . C24 . H243 . 108.4 no
O15 . C25 . H125 . 109.6 no
O15 . C25 . H225 . 110.2 no
H125 . C25 . H225 . 109.0 no
O15 . C25 . H325 . 108.8 no
H125 . C25 . H325 . 109.6 no
H225 . C25 . H325 . 109.6 no
O16 . C26 . H126 . 110.6 no
O16 . C26 . H226 . 107.9 no
H126 . C26 . H226 . 108.8 no
O16 . C26 . H326 . 110.2 no
H126 . C26 . H326 . 109.9 no
H226 . C26 . H326 . 109.4 no
O17 . C27 . H127 . 109.6 no
O17 . C27 . H227 . 110.7 no
H127 . C27 . H227 . 109.4 no
O17 . C27 . H327 . 108.6 no
H127 . C27 . H327 . 108.7 no
H227 . C27 . H327 . 109.7 no
C21 . C31 . C41 . 120.9(7) yes
C21 . C31 . H131 . 119.6 no
C41 . C31 . H131 . 119.4 no
C22 . C32 . C42 . 120.9(8) yes
C22 . C32 . H132 . 119.3 no
C42 . C32 . H132 . 119.8 no
C23 . C33 . C43 . 121.4(7) yes
C23 . C33 . H133 . 119.3 no
C43 . C33 . H133 . 119.3 no
C31 . C41 . C51 . 118.8(8) yes
C31 . C41 . H141 . 120.3 no
C51 . C41 . H141 . 121.0 no
C32 . C42 . C52 . 118.2(8) yes
C32 . C42 . H142 . 121.0 no
C52 . C42 . H142 . 120.7 no
C33 . C43 . C53 . 119.0(7) yes
C33 . C43 . H143 . 120.8 no
C53 . C43 . H143 . 120.3 no
C41 . C51 . C61 . 122.5(8) yes
C41 . C51 . H151 . 119.2 no
C61 . C51 . H151 . 118.3 no
C42 . C52 . C62 . 122.8(7) yes
C42 . C52 . H152 . 118.1 no
C62 . C52 . H152 . 119.2 no
C43 . C53 . C63 . 121.5(6) yes
C43 . C53 . H153 . 119.1 no
C63 . C53 . H153 . 119.5 no
C11 . C61 . C51 . 118.6(6) yes
C11 . C61 . C71 . 121.9(6) yes
C51 . C61 . C71 . 119.4(7) yes
C12 . C62 . C52 . 118.6(7) yes
C12 . C62 . C72 . 121.0(6) yes
C52 . C62 . C72 . 120.4(6) yes
C53 . C63 . C13 . 118.4(6) yes
C53 . C63 . C73 . 118.1(6) yes
C13 . C63 . C73 . 123.4(6) yes
C61 . C71 . N71 . 119.0(6) yes
C61 . C71 . C81 . 121.9(6) yes
N71 . C71 . C81 . 119.2(6) yes
C62 . C72 . N72 . 120.1(6) yes
C62 . C72 . C82 . 120.1(6) yes
N72 . C72 . C82 . 119.7(7) yes
C63 . C73 . N73 . 118.6(6) yes
C63 . C73 . C83 . 121.2(6) yes
N73 . C73 . C83 . 120.1(6) yes
C71 . C81 . H181 . 110.1 no
C71 . C81 . H281 . 111.2 no
H181 . C81 . H281 . 108.9 no
C71 . C81 . H381 . 109.8 no
H181 . C81 . H381 . 108.5 no
H281 . C81 . H381 . 108.4 no
C72 . C82 . H182 . 109.0 no
C72 . C82 . H282 . 109.2 no
H182 . C82 . H282 . 109.6 no
C72 . C82 . H382 . 108.8 no
H182 . C82 . H382 . 109.7 no
H282 . C82 . H382 . 110.5 no
C73 . C83 . H183 . 110.2 no
C73 . C83 . H283 . 109.1 no
H183 . C83 . H283 . 109.5 no
C73 . C83 . H383 . 108.3 no
H183 . C83 . H383 . 109.5 no
H283 . C83 . H383 . 110.3 no