# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 917757'
_audit_update_record             
;
2015-11-26 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;
_audit_creation_date             2015-11-21
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C104 H124 Co12 N8 Na4 O72), C4 H9 N O, 2(H2 O)'
_chemical_formula_sum            'C56 H75 Co6 N5 Na2 O39'
_chemical_formula_weight         1841.77
_chemical_absolute_configuration .
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'
Na Na 0.0362 0.0249 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.1249(7)
_cell_length_b                   12.1064(5)
_cell_length_c                   17.7333(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.3010(10)
_cell_angle_gamma                90
_cell_volume                     3715.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18461
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.4
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.1461
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19250
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.366
_diffrn_ambient_temperature      293.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                7085
_reflns_number_total             8441
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 
;
 Flack x determined using 2438 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8441
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0740
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0670P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1880
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H19A,H19B} of O19
 At 1.5 times of:
  All C(H,H,H) groups, {H20A,H20B} of O20, {H14A,H14B} of O14, All O(H,H,H)
  groups
2. Restrained distances
 H20A-O4_$1
 2.1 with sigma of 0.02
 O13-H13
 0.82 with sigma of 0.02
3. Restrained planarity
 O17, N3, C27, C28, C29, C30
 with sigma of 0.1
4. Rigid bond restraints
 O15, N1, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O16, N2, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O16, N2, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O17, N3, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Others
 Fixed Sof: O17(0.5) N3(0.5) C27(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
7.a Riding coordinates:
 O19(H19A,H19B), O20(H20A,H20B), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C),
 O18(H18A,H18B)
7.b Rotating group:
 O14(H14A,H14B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C13(H13A), C15(H15)
7.d Idealised Me refined as rotating group:
 C20(H20C,H20D,H20E), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.78998(7) 0.15718(12) 0.68643(8) 0.0256(4) Uani 1 1 d . . . . .
Co2 Co 0.66714(7) 0.34578(9) 0.66121(6) 0.0122(3) Uani 1 1 d . . . . .
Co3 Co 0.80626(7) 0.31383(9) 0.83621(6) 0.0136(3) Uani 1 1 d . . . . .
Na1A Na 0.5997(3) 1.0024(4) 0.9945(3) 0.0493(13) Uani 1 1 d . . . . .
O1 O 0.7483(4) 0.1339(7) 0.5702(4) 0.0324(18) Uani 1 1 d . . . . .
O2 O 0.6454(4) 0.2336(6) 0.5682(4) 0.0282(17) Uani 1 1 d . . . . .
O3 O 0.4396(4) 0.2944(5) 0.3255(4) 0.0223(15) Uani 1 1 d . . . . .
O4 O 0.4066(4) 0.1526(7) 0.2421(4) 0.038(2) Uani 1 1 d D . . . .
O5 O 0.6419(4) -0.0800(6) 0.2278(4) 0.0263(16) Uani 1 1 d . . . . .
O6 O 0.7138(4) -0.1351(7) 0.3474(4) 0.0303(18) Uani 1 1 d . . . . .
O7 O 0.6707(4) 0.4754(6) 0.7382(4) 0.0275(16) Uani 1 1 d . . . . .
O8 O 0.7432(5) 0.4396(6) 0.8622(4) 0.0321(18) Uani 1 1 d . . . . .
O9 O 0.4069(5) 0.6436(9) 0.7115(5) 0.053(3) Uani 1 1 d . . . . .
O10 O 0.3891(4) 0.6976(9) 0.8239(6) 0.051(2) Uani 1 1 d . . . . .
O11 O 0.7137(4) 0.7031(6) 1.0729(4) 0.0242(15) Uani 1 1 d . . . . .
O12 O 0.6192(4) 0.8241(6) 1.0417(4) 0.0298(17) Uani 1 1 d . . . . .
O13 O 0.7284(4) 0.2359(5) 0.7448(3) 0.0162(13) Uani 1 1 d D . . . .
O14 O 0.6219(5) 0.4650(6) 0.5735(4) 0.0358(19) Uani 1 1 d . . . . .
H14A H 0.5761 0.4999 0.5772 0.054 Uiso 1 1 d GR . . . .
H14B H 0.6075 0.4377 0.5207 0.054 Uiso 1 1 d GR . . . .
O15 O 0.7578(6) 0.0043(8) 0.7157(6) 0.054(2) Uani 1 1 d . U . . .
O16 O 0.6032(9) 1.1762(10) 1.0578(9) 0.099(4) Uani 1 1 d . U . . .
O19 O 0.4762(5) 1.0082(7) 0.9026(5) 0.047(2) Uani 1 1 d . . . . .
H19A H 0.4648 0.9529 0.8719 0.056 Uiso 1 1 d R . . . .
H19B H 0.4667 1.0658 0.8761 0.056 Uiso 1 1 d R . . . .
O20 O 0.6628(5) 1.0552(9) 0.9055(5) 0.054(3) Uani 1 1 d . . . . .
H20A H 0.6369 1.0437 0.8570 0.081 Uiso 1 1 d DR . . . .
H20B H 0.7118 1.0668 0.9133 0.081 Uiso 1 1 d R . . . .
N1 N 0.7114(10) -0.1646(11) 0.7067(9) 0.084(4) Uani 1 1 d . U . . .
N2 N 0.6024(15) 1.3506(17) 1.0851(11) 0.127(7) Uani 1 1 d . U . . .
C1 C 0.6415(6) 0.1341(7) 0.4547(5) 0.0181(18) Uani 1 1 d . . . . .
C2 C 0.5703(5) 0.1815(8) 0.4151(5) 0.020(2) Uani 1 1 d . . . . .
H2 H 0.5489 0.2362 0.4409 0.024 Uiso 1 1 calc R . . . .
C3 C 0.5306(5) 0.1500(8) 0.3390(5) 0.0177(18) Uani 1 1 d . . . . .
C4 C 0.5599(5) 0.0682(8) 0.3019(5) 0.020(2) Uani 1 1 d . . . . .
H4 H 0.5314 0.0451 0.2502 0.024 Uiso 1 1 calc R . . . .
C5 C 0.6316(5) 0.0186(8) 0.3400(5) 0.018(2) Uani 1 1 d . . . . .
C6 C 0.6715(5) 0.0510(8) 0.4172(5) 0.0166(19) Uani 1 1 d . . . . .
H6 H 0.7191 0.0165 0.4443 0.020 Uiso 1 1 calc R . . . .
C7 C 0.6827(5) 0.1712(8) 0.5378(5) 0.0183(19) Uani 1 1 d . . . . .
C8 C 0.4535(5) 0.2022(8) 0.2981(5) 0.0168(18) Uani 1 1 d . . . . .
C9 C 0.6650(5) -0.0720(8) 0.3018(5) 0.0188(19) Uani 1 1 d . . . . .
C10 C 0.6407(6) 0.5677(7) 0.8410(5) 0.0184(19) Uani 1 1 d . . . . .
C11 C 0.5649(6) 0.5876(8) 0.7972(5) 0.023(2) Uani 1 1 d . . . . .
H11 H 0.5447 0.5544 0.7467 0.027 Uiso 1 1 calc R . . . .
C12 C 0.5175(5) 0.6562(9) 0.8265(5) 0.022(2) Uani 1 1 d . . . . .
C13 C 0.5464(6) 0.7069(8) 0.8997(5) 0.022(2) Uani 1 1 d . . . . .
H13A H 0.5139 0.7525 0.9198 0.026 Uiso 1 1 calc R . . . .
C14 C 0.6243(5) 0.6901(8) 0.9439(5) 0.0182(19) Uani 1 1 d . . . . .
C15 C 0.6700(5) 0.6178(8) 0.9153(5) 0.0187(19) Uani 1 1 d . . . . .
H15 H 0.7214 0.6025 0.9465 0.022 Uiso 1 1 calc R . . . .
C16 C 0.6885(6) 0.4863(8) 0.8108(5) 0.020(2) Uani 1 1 d . . . . .
C17 C 0.4316(6) 0.6674(11) 0.7846(7) 0.037(3) Uani 1 1 d . . . . .
C18 C 0.6551(5) 0.7405(8) 1.0246(5) 0.019(2) Uani 1 1 d . . . . .
C19 C 0.7525(11) -0.0897(11) 0.6837(11) 0.066(4) Uani 1 1 d . U . . .
C20 C 0.7929(14) -0.1188(16) 0.6239(13) 0.102(6) Uani 1 1 d . U . . .
H20C H 0.8227 -0.0550 0.6152 0.152 Uiso 1 1 calc GR . . . .
H20D H 0.7546 -0.1394 0.5741 0.152 Uiso 1 1 calc GR . . . .
H20E H 0.8280 -0.1811 0.6434 0.152 Uiso 1 1 calc GR . . . .
C21 C 0.707(2) -0.2811(16) 0.6880(19) 0.150(9) Uani 1 1 d . U . . .
H21A H 0.7233 -0.3241 0.7370 0.225 Uiso 1 1 calc GR . . . .
H21B H 0.7402 -0.2978 0.6552 0.225 Uiso 1 1 calc GR . . . .
H21C H 0.6532 -0.3003 0.6592 0.225 Uiso 1 1 calc GR . . . .
C22 C 0.6616(16) -0.133(2) 0.7565(14) 0.126(8) Uani 1 1 d . U . . .
H22A H 0.6333 -0.0653 0.7357 0.189 Uiso 1 1 calc GR . . . .
H22B H 0.6939 -0.1206 0.8109 0.189 Uiso 1 1 calc GR . . . .
H22C H 0.6248 -0.1927 0.7557 0.189 Uiso 1 1 calc GR . . . .
C23 C 0.6132(15) 1.2762(17) 1.0507(16) 0.104(6) Uani 1 1 d . U . . .
C24 C 0.6485(18) 1.330(2) 0.9916(17) 0.145(8) Uani 1 1 d . U . . .
H24A H 0.6935 1.3739 1.0199 0.218 Uiso 1 1 calc GR . . . .
H24B H 0.6101 1.3772 0.9556 0.218 Uiso 1 1 calc GR . . . .
H24C H 0.6648 1.2719 0.9611 0.218 Uiso 1 1 calc GR . . . .
C25 C 0.6066(19) 1.4678(16) 1.0899(17) 0.135(8) Uani 1 1 d . U . . .
H25A H 0.5908 1.4929 1.1353 0.202 Uiso 1 1 calc GR . . . .
H25B H 0.5722 1.4998 1.0413 0.202 Uiso 1 1 calc GR . . . .
H25C H 0.6598 1.4915 1.0962 0.202 Uiso 1 1 calc GR . . . .
C26 C 0.560(2) 1.303(2) 1.1527(15) 0.151(9) Uani 1 1 d . U . . .
H26A H 0.5050 1.3099 1.1382 0.227 Uiso 1 1 d R . . . .
H26B H 0.5831 1.3414 1.2012 0.227 Uiso 1 1 d R . . . .
H26C H 0.5739 1.2258 1.1597 0.227 Uiso 1 1 d R . . . .
O17 O 0.5447(17) 0.652(2) 0.5734(15) 0.092(7) Uani 0.5 1 d . U P A -1
N3 N 0.5034(19) 0.814(3) 0.5321(15) 0.089(7) Uani 0.5 1 d . U P A -1
C27 C 0.5501(19) 0.744(3) 0.5278(18) 0.075(7) Uani 0.5 1 d . U P A -1
C28 C 0.605(2) 0.761(3) 0.481(2) 0.082(8) Uani 0.5 1 d . U P A -1
H28A H 0.6567 0.7744 0.5172 0.123 Uiso 0.5 1 calc GR . P A -1
H28B H 0.5883 0.8253 0.4466 0.123 Uiso 0.5 1 calc GR . P A -1
H28C H 0.6056 0.6955 0.4492 0.123 Uiso 0.5 1 calc GR . P A -1
C29 C 0.489(4) 0.928(3) 0.483(3) 0.093(11) Uani 0.5 1 d . U P A -1
H29A H 0.4508 0.9168 0.4319 0.139 Uiso 0.5 1 calc GR . P A -1
H29B H 0.5380 0.9530 0.4755 0.139 Uiso 0.5 1 calc GR . P A -1
H29C H 0.4707 0.9846 0.5130 0.139 Uiso 0.5 1 calc GR . P A -1
C30 C 0.451(3) 0.800(4) 0.590(3) 0.134(12) Uani 0.5 1 d . U P A -1
H30A H 0.4384 0.7239 0.5922 0.201 Uiso 0.5 1 d R . P A -1
H30B H 0.4048 0.8427 0.5694 0.201 Uiso 0.5 1 d R . P A -1
H30C H 0.4791 0.8263 0.6414 0.201 Uiso 0.5 1 d R . P A -1
O18 O 0.5432(6) 0.4629(8) 0.4083(6) 0.059(3) Uani 1 1 d . . . . .
H18A H 0.5379 0.5362 0.4029 0.088 Uiso 1 1 d R . . . .
H18B H 0.5166 0.4317 0.3674 0.088 Uiso 1 1 d R . . . .
H13 H 0.699(8) 0.204(13) 0.766(9) 0.088 Uiso 1 1 d DR . . . .


_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
Co1 O1 1.992(7) . ?
Co1 O9 2.038(9) 3_545 ?
Co1 O13 1.978(6) . ?
Co1 O15 2.053(10) . ?
Co2 O2 2.081(7) . ?
Co2 O3 2.112(6) 2_656 ?
Co2 O6 2.221(7) 4_656 ?
Co2 O7 2.068(7) . ?
Co2 O13 2.054(7) . ?
Co2 O14 2.102(7) . ?
Co3 O5 2.112(6) 4_656 ?
Co3 O8 2.038(7) . ?
Co3 O10 2.117(9) 3_545 ?
Co3 O11 2.207(6) 4_647 ?
Co3 O12 2.189(7) 4_647 ?
Co3 O13 2.037(6) . ?
Co3 C18 2.518(9) 4_647 ?
Na1A Na1A 3.678(11) 2_657 ?
Na1A O12 2.304(9) . ?
Na1A O16 2.377(14) . ?
Na1A O19 2.345(11) . ?
Na1A O19 2.593(10) 2_657 ?
Na1A O20 2.297(9) . ?
O1 C7 1.242(11) . ?
O2 C7 1.239(11) . ?
O3 Co2 2.112(6) 2_656 ?
O3 C8 1.271(11) . ?
O4 C8 1.252(11) . ?
O5 Co3 2.112(6) 4_646 ?
O5 C9 1.257(11) . ?
O6 Co2 2.221(7) 4_646 ?
O6 C9 1.262(11) . ?
O7 C16 1.239(11) . ?
O8 C16 1.264(12) . ?
O9 Co1 2.038(9) 3_455 ?
O9 C17 1.272(14) . ?
O10 Co3 2.117(9) 3_455 ?
O10 C17 1.237(15) . ?
O11 Co3 2.207(6) 4_657 ?
O11 C18 1.235(11) . ?
O12 Co3 2.189(7) 4_657 ?
O12 C18 1.287(11) . ?
O13 H13 0.83(3) . ?
O14 H14A 0.9506 . ?
O14 H14B 0.9532 . ?
O15 C19 1.262(18) . ?
O16 C23 1.24(2) . ?
O19 Na1A 2.593(10) 2_657 ?
O19 H19A 0.8492 . ?
O19 H19B 0.8294 . ?
O20 H20A 0.8605 . ?
O20 H20B 0.8696 . ?
N1 C19 1.31(2) . ?
N1 C21 1.45(2) . ?
N1 C22 1.49(2) . ?
N2 C23 1.14(3) . ?
N2 C25 1.42(3) . ?
N2 C26 1.70(3) . ?
C1 C2 1.395(13) . ?
C1 C6 1.402(12) . ?
C1 C7 1.509(12) . ?
C2 H2 0.9500 . ?
C2 C3 1.382(12) . ?
C3 C4 1.379(13) . ?
C3 C8 1.509(12) . ?
C4 H4 0.9500 . ?
C4 C5 1.409(13) . ?
C5 C6 1.401(12) . ?
C5 C9 1.507(12) . ?
C6 H6 0.9500 . ?
C10 C11 1.385(14) . ?
C10 C15 1.403(12) . ?
C10 C16 1.510(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.400(14) . ?
C12 C13 1.390(13) . ?
C12 C17 1.519(14) . ?
C13 H13A 0.9500 . ?
C13 C14 1.411(13) . ?
C14 C15 1.400(13) . ?
C14 C18 1.503(12) . ?
C15 H15 0.9500 . ?
C18 Co3 2.518(9) 4_657 ?
C19 C20 1.50(2) . ?
C20 H20C 0.9800 . ?
C20 H20D 0.9800 . ?
C20 H20E 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.53(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9598 . ?
C26 H26B 0.9597 . ?
C26 H26C 0.9599 . ?
O17 C27 1.40(4) . ?
N3 C27 1.22(4) . ?
N3 C29 1.61(5) . ?
N3 C30 1.59(5) . ?
C27 C28 1.48(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9599 . ?
C30 H30B 0.9601 . ?
C30 H30C 0.9600 . ?
O18 H18A 0.8948 . ?
O18 H18B 0.8323 . ?

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 Co1 O9 105.3(3) . 3_545 ?
O1 Co1 O15 94.9(4) . . ?
O9 Co1 O15 103.1(4) 3_545 . ?
O13 Co1 O1 120.6(3) . . ?
O13 Co1 O9 129.5(3) . 3_545 ?
O13 Co1 O15 93.2(3) . . ?
O2 Co2 O3 86.1(3) . 2_656 ?
O2 Co2 O6 88.4(3) . 4_656 ?
O2 Co2 O14 85.5(3) . . ?
O3 Co2 O6 168.6(3) 2_656 4_656 ?
O7 Co2 O2 168.3(3) . . ?
O7 Co2 O3 90.0(3) . 2_656 ?
O7 Co2 O6 97.2(3) . 4_656 ?
O7 Co2 O14 84.0(3) . . ?
O13 Co2 O2 94.8(3) . . ?
O13 Co2 O3 92.6(2) . 2_656 ?
O13 Co2 O6 77.9(3) . 4_656 ?
O13 Co2 O7 96.4(3) . . ?
O13 Co2 O14 170.7(3) . . ?
O14 Co2 O3 96.7(3) . 2_656 ?
O14 Co2 O6 92.9(3) . 4_656 ?
O5 Co3 O10 84.6(3) 4_656 3_545 ?
O5 Co3 O11 163.3(3) 4_656 4_647 ?
O5 Co3 O12 104.8(2) 4_656 4_647 ?
O5 Co3 C18 134.7(3) 4_656 4_647 ?
O8 Co3 O5 92.1(3) . 4_656 ?
O8 Co3 O10 169.5(4) . 3_545 ?
O8 Co3 O11 93.7(3) . 4_647 ?
O8 Co3 O12 87.5(3) . 4_647 ?
O8 Co3 C18 93.0(3) . 4_647 ?
O10 Co3 O11 87.0(3) 3_545 4_647 ?
O10 Co3 O12 83.8(3) 3_545 4_647 ?
O10 Co3 C18 82.4(3) 3_545 4_647 ?
O11 Co3 C18 29.4(3) 4_647 4_647 ?
O12 Co3 O11 59.9(2) 4_647 4_647 ?
O12 Co3 C18 30.7(3) 4_647 4_647 ?
O13 Co3 O5 99.7(2) . 4_656 ?
O13 Co3 O8 102.9(3) . . ?
O13 Co3 O10 87.4(3) . 3_545 ?
O13 Co3 O11 94.3(2) . 4_647 ?
O13 Co3 O12 153.1(2) . 4_647 ?
O13 Co3 C18 122.8(3) . 4_647 ?
O12 Na1A Na1A 91.6(2) . 2_657 ?
O12 Na1A O16 132.7(4) . . ?
O12 Na1A O19 80.0(3) . 2_657 ?
O12 Na1A O19 107.0(3) . . ?
O16 Na1A Na1A 82.2(4) . 2_657 ?
O16 Na1A O19 65.7(4) . 2_657 ?
O19 Na1A Na1A 39.3(2) 2_657 2_657 ?
O19 Na1A Na1A 44.5(2) . 2_657 ?
O19 Na1A O16 100.8(5) . . ?
O19 Na1A O19 83.8(3) . 2_657 ?
O20 Na1A Na1A 137.3(4) . 2_657 ?
O20 Na1A O12 117.1(4) . . ?
O20 Na1A O16 97.5(5) . . ?
O20 Na1A O19 162.3(4) . 2_657 ?
O20 Na1A O19 94.7(4) . . ?
C7 O1 Co1 116.4(6) . . ?
C7 O2 Co2 138.0(6) . . ?
C8 O3 Co2 126.3(6) . 2_656 ?
C9 O5 Co3 123.0(6) . 4_646 ?
C9 O6 Co2 122.0(6) . 4_646 ?
C16 O7 Co2 135.6(7) . . ?
C16 O8 Co3 122.9(6) . . ?
C17 O9 Co1 103.5(8) . 3_455 ?
C17 O10 Co3 146.6(8) . 3_455 ?
C18 O11 Co3 89.4(5) . 4_657 ?
Co3 O12 Na1A 113.3(3) 4_657 . ?
C18 O12 Co3 88.9(5) . 4_657 ?
C18 O12 Na1A 133.2(7) . . ?
Co1 O13 Co2 101.7(3) . . ?
Co1 O13 Co3 105.9(3) . . ?
Co1 O13 H13 123(10) . . ?
Co2 O13 H13 110(10) . . ?
Co3 O13 Co2 111.9(3) . . ?
Co3 O13 H13 104(10) . . ?
Co2 O14 H14A 114.2 . . ?
Co2 O14 H14B 114.9 . . ?
H14A O14 H14B 103.4 . . ?
C19 O15 Co1 133.5(10) . . ?
C23 O16 Na1A 143.4(16) . . ?
Na1A O19 Na1A 96.1(3) . 2_657 ?
Na1A O19 H19A 110.5 2_657 . ?
Na1A O19 H19A 115.0 . . ?
Na1A O19 H19B 114.5 . . ?
Na1A O19 H19B 110.8 2_657 . ?
H19A O19 H19B 109.3 . . ?
Na1A O20 H20A 114.1 . . ?
Na1A O20 H20B 129.0 . . ?
H20A O20 H20B 114.3 . . ?
C19 N1 C21 127.1(17) . . ?
C19 N1 C22 120.5(15) . . ?
C21 N1 C22 112.4(18) . . ?
C23 N2 C25 144(3) . . ?
C23 N2 C26 107(2) . . ?
C25 N2 C26 109(2) . . ?
C2 C1 C6 119.2(8) . . ?
C2 C1 C7 118.9(8) . . ?
C6 C1 C7 121.9(8) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.8(8) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C8 119.5(8) . . ?
C4 C3 C2 120.1(8) . . ?
C4 C3 C8 120.3(8) . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.6(8) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C9 122.1(8) . . ?
C6 C5 C4 118.9(8) . . ?
C6 C5 C9 118.9(8) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.3(8) . . ?
C5 C6 H6 119.9 . . ?
O1 C7 C1 118.1(8) . . ?
O2 C7 O1 126.2(8) . . ?
O2 C7 C1 115.6(8) . . ?
O3 C8 C3 116.4(8) . . ?
O4 C8 O3 124.1(8) . . ?
O4 C8 C3 119.5(8) . . ?
O5 C9 O6 125.1(8) . . ?
O5 C9 C5 118.1(8) . . ?
O6 C9 C5 116.8(8) . . ?
C11 C10 C15 119.1(9) . . ?
C11 C10 C16 119.5(8) . . ?
C15 C10 C16 121.2(9) . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.7(8) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C17 121.6(9) . . ?
C13 C12 C11 120.5(8) . . ?
C13 C12 C17 117.6(9) . . ?
C12 C13 H13A 120.3 . . ?
C12 C13 C14 119.4(9) . . ?
C14 C13 H13A 120.3 . . ?
C13 C14 C18 119.9(8) . . ?
C15 C14 C13 119.4(8) . . ?
C15 C14 C18 120.4(8) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 C10 120.8(9) . . ?
C14 C15 H15 119.6 . . ?
O7 C16 O8 127.5(9) . . ?
O7 C16 C10 116.0(9) . . ?
O8 C16 C10 116.5(8) . . ?
O9 C17 C12 118.5(11) . . ?
O10 C17 O9 123.4(10) . . ?
O10 C17 C12 118.1(10) . . ?
O11 C18 Co3 61.2(5) . 4_657 ?
O11 C18 O12 121.1(8) . . ?
O11 C18 C14 120.8(9) . . ?
O12 C18 Co3 60.3(5) . 4_657 ?
O12 C18 C14 118.2(8) . . ?
C14 C18 Co3 173.2(7) . 4_657 ?
O15 C19 N1 117.3(14) . . ?
O15 C19 C20 122.8(16) . . ?
N1 C19 C20 119.9(15) . . ?
C19 C20 H20C 109.5 . . ?
C19 C20 H20D 109.5 . . ?
C19 C20 H20E 109.5 . . ?
H20C C20 H20D 109.5 . . ?
H20C C20 H20E 109.5 . . ?
H20D C20 H20E 109.5 . . ?
N1 C21 H21A 109.5 . . ?
N1 C21 H21B 109.5 . . ?
N1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O16 C23 C24 126(2) . . ?
N2 C23 O16 132(3) . . ?
N2 C23 C24 102(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 H26A 115.4 . . ?
N2 C26 H26B 107.3 . . ?
N2 C26 H26C 105.6 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.4 . . ?
H26B C26 H26C 109.5 . . ?
C27 N3 C29 125(4) . . ?
C27 N3 C30 121(3) . . ?
C30 N3 C29 114(4) . . ?
O17 C27 C28 128(3) . . ?
N3 C27 O17 111(3) . . ?
N3 C27 C28 122(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 109.6 . . ?
N3 C30 H30B 109.1 . . ?
N3 C30 H30C 109.7 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H18A O18 H18B 110.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C7 O2 10.4(14) . . . . ?
Co1 O1 C7 C1 -166.4(6) . . . . ?
Co1 O9 C17 O10 -4.1(15) 3_455 . . . ?
Co1 O9 C17 C12 174.8(8) 3_455 . . . ?
Co1 O15 C19 N1 -162.8(12) . . . . ?
Co1 O15 C19 C20 19(3) . . . . ?
Co2 O2 C7 O1 22.4(17) . . . . ?
Co2 O2 C7 C1 -160.7(7) . . . . ?
Co2 O3 C8 O4 37.6(13) 2_656 . . . ?
Co2 O3 C8 C3 -140.3(7) 2_656 . . . ?
Co2 O6 C9 O5 59.2(14) 4_646 . . . ?
Co2 O6 C9 C5 -121.6(8) 4_646 . . . ?
Co2 O7 C16 O8 38.5(16) . . . . ?
Co2 O7 C16 C10 -143.6(8) . . . . ?
Co3 O5 C9 O6 -10.0(15) 4_646 . . . ?
Co3 O5 C9 C5 170.8(6) 4_646 . . . ?
Co3 O8 C16 O7 -10.0(15) . . . . ?
Co3 O8 C16 C10 172.2(6) . . . . ?
Co3 O10 C17 O9 -57(2) 3_455 . . . ?
Co3 O10 C17 C12 124.0(13) 3_455 . . . ?
Co3 O11 C18 O12 8.0(10) 4_657 . . . ?
Co3 O11 C18 C14 -172.5(8) 4_657 . . . ?
Co3 O12 C18 O11 -8.1(10) 4_657 . . . ?
Co3 O12 C18 C14 172.4(8) 4_657 . . . ?
Na1A O12 C18 Co3 121.7(8) . . . 4_657 ?
Na1A O12 C18 O11 113.6(10) . . . . ?
Na1A O12 C18 C14 -65.9(12) . . . . ?
Na1A O16 C23 N2 168(3) . . . . ?
Na1A O16 C23 C24 -15(5) . . . . ?
C1 C2 C3 C4 2.1(15) . . . . ?
C1 C2 C3 C8 179.5(9) . . . . ?
C2 C1 C6 C5 2.0(14) . . . . ?
C2 C1 C7 O1 -175.1(9) . . . . ?
C2 C1 C7 O2 7.7(13) . . . . ?
C2 C3 C4 C5 -2.2(15) . . . . ?
C2 C3 C8 O3 20.6(13) . . . . ?
C2 C3 C8 O4 -157.4(10) . . . . ?
C3 C4 C5 C6 2.2(15) . . . . ?
C3 C4 C5 C9 179.2(9) . . . . ?
C4 C3 C8 O3 -162.0(9) . . . . ?
C4 C3 C8 O4 20.0(14) . . . . ?
C4 C5 C6 C1 -2.1(14) . . . . ?
C4 C5 C9 O5 22.2(15) . . . . ?
C4 C5 C9 O6 -157.0(10) . . . . ?
C6 C1 C2 C3 -2.0(14) . . . . ?
C6 C1 C7 O1 6.9(14) . . . . ?
C6 C1 C7 O2 -170.2(9) . . . . ?
C6 C5 C9 O5 -160.8(9) . . . . ?
C6 C5 C9 O6 20.0(14) . . . . ?
C7 C1 C2 C3 180.0(9) . . . . ?
C7 C1 C6 C5 180.0(9) . . . . ?
C8 C3 C4 C5 -179.5(9) . . . . ?
C9 C5 C6 C1 -179.2(9) . . . . ?
C10 C11 C12 C13 1.1(15) . . . . ?
C10 C11 C12 C17 -171.9(10) . . . . ?
C11 C10 C15 C14 -2.2(15) . . . . ?
C11 C10 C16 O7 28.2(13) . . . . ?
C11 C10 C16 O8 -153.8(10) . . . . ?
C11 C12 C13 C14 0.9(15) . . . . ?
C11 C12 C17 O9 -22.1(16) . . . . ?
C11 C12 C17 O10 156.8(11) . . . . ?
C12 C13 C14 C15 -3.5(15) . . . . ?
C12 C13 C14 C18 -177.3(9) . . . . ?
C13 C12 C17 O9 164.7(11) . . . . ?
C13 C12 C17 O10 -16.4(16) . . . . ?
C13 C14 C15 C10 4.2(15) . . . . ?
C13 C14 C18 O11 158.9(10) . . . . ?
C13 C14 C18 O12 -21.6(14) . . . . ?
C15 C10 C11 C12 -0.5(15) . . . . ?
C15 C10 C16 O7 -156.3(9) . . . . ?
C15 C10 C16 O8 21.7(14) . . . . ?
C15 C14 C18 O11 -14.9(14) . . . . ?
C15 C14 C18 O12 164.6(9) . . . . ?
C16 C10 C11 C12 175.1(9) . . . . ?
C16 C10 C15 C14 -177.7(9) . . . . ?
C17 C12 C13 C14 174.2(9) . . . . ?
C18 C14 C15 C10 178.0(9) . . . . ?
C21 N1 C19 O15 -170(2) . . . . ?
C21 N1 C19 C20 8(3) . . . . ?
C22 N1 C19 O15 11(3) . . . . ?
C22 N1 C19 C20 -171(2) . . . . ?
C25 N2 C23 O16 -179(3) . . . . ?
C25 N2 C23 C24 4(6) . . . . ?
C26 N2 C23 O16 -4(5) . . . . ?
C26 N2 C23 C24 179(2) . . . . ?
C29 N3 C27 O17 -176(3) . . . . ?
C29 N3 C27 C28 6(4) . . . . ?
C30 N3 C27 O17 5(3) . . . . ?
C30 N3 C27 C28 -173(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 917758'
_audit_update_record             
;
2016-01-09 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r3563)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C36 H24 Ni6 O32)'
_chemical_formula_sum            'C18 H12 Ni3 O16'
_chemical_formula_weight         660.41
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Ni Ni 0.3393 1.1124 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           44
_space_group_name_H-M_alt        'I m m 2'
_space_group_name_Hall           'I 2 -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z'
'-x, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   9.787(2)
_cell_length_b                   12.157(2)
_cell_length_c                   15.182(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1806.5(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9545
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.352
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCX-mini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2213
_reflns_number_total             2286
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0321P)²+1.2700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0769
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.95(3) 0.05(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 H4_$1-H4
 1.4 with sigma of 0.02
4. Rigid body (RIGU) restrains
 O4, Ni2, O6, Ni1, O5, O1, C6, C1, H1, C2, C3, H3, C4, O2, C5, O3, H5, H4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Riding coordinates:
 O4(H4), O5(H5)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.5000 -0.1470(5) 0.8995(4) 0.0253(13) Uani 1 2 d S TU P . .
H1 H 1.5000 -0.1022 0.9508 0.030 Uiso 1 2 calc RS TU P . .
C2 C 1.3785(4) -0.1794(4) 0.8623(3) 0.0261(9) Uani 1 1 d . U . . .
C3 C 1.3783(4) -0.2432(4) 0.7877(3) 0.0292(10) Uani 1 1 d . U . . .
H3 H 1.2945 -0.2623 0.7601 0.035 Uiso 1 1 calc R U . . .
C4 C 1.5000 -0.2790(5) 0.7533(4) 0.0262(13) Uani 1 2 d S TU P . .
C5 C 1.5000 -0.3522(5) 0.6738(4) 0.0251(13) Uani 1 2 d S TU P . .
C6 C 1.2485(4) -0.1345(4) 0.9025(3) 0.0292(10) Uani 1 1 d . U . . .
Ni1 Ni 1.0000 0.0000 0.86322(6) 0.0251(3) Uani 1 4 d S TU P . .
Ni2 Ni 0.83138(6) 0.0000 1.06020(4) 0.01676(17) Uani 1 2 d S TU P . .
O1 O 1.1511(3) -0.1190(3) 0.8529(2) 0.0369(9) Uani 1 1 d . U . . .
O2 O 1.2553(3) -0.1156(3) 0.9825(2) 0.0374(9) Uani 1 1 d . U . . .
O3 O 1.3865(3) -0.3816(3) 0.6455(2) 0.0343(8) Uani 1 1 d . U . . .
O4 O 0.6460(5) 0.0000 1.1311(3) 0.0469(15) Uani 1 2 d S TU P . .
H4 H 0.6429 -0.0569 1.1680 0.070 Uiso 1 1 d DR U . . .
O5 O 1.0000 0.0000 0.7277(4) 0.051(2) Uani 1 4 d S TU P . .
H5 H 1.0000 -0.0540 0.6822 0.077 Uiso 1 2 d RS TU P . .
O6 O 1.0000 0.0000 0.9909(4) 0.041(2) Uani 1 4 d S TU P . .


_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
C1 H1 0.9500 . ?
C1 C2 1.374(5) 4_855 ?
C1 C2 1.374(5) . ?
C2 C3 1.372(6) . ?
C2 C6 1.514(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(5) . ?
C4 C3 1.371(5) 4_855 ?
C4 C5 1.500(8) . ?
C5 O3 1.244(4) . ?
C5 O3 1.244(4) 4_855 ?
C6 O1 1.229(5) . ?
C6 O2 1.237(5) . ?
Ni1 O1 2.075(3) . ?
Ni1 O1 2.075(3) 3 ?
Ni1 O1 2.075(3) 2_755 ?
Ni1 O1 2.075(3) 4_755 ?
Ni1 O5 2.058(6) . ?
Ni1 O6 1.939(6) . ?
Ni2 O2 2.021(3) 4_755 ?
Ni2 O2 2.021(3) 2_755 ?
Ni2 O3 2.010(3) 7_445 ?
Ni2 O3 2.010(3) 5_455 ?
Ni2 O4 2.110(5) . ?
Ni2 O6 1.957(3) . ?
O2 Ni2 2.021(3) 2_755 ?
O3 Ni2 2.010(3) 5_544 ?
O4 H4 0.8908 . ?
O5 H5 0.9531 . ?
O6 Ni2 1.957(3) 2_755 ?

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
C2 C1 H1 120.1 . . ?
C2 C1 H1 120.1 4_855 . ?
C2 C1 C2 119.8(6) 4_855 . ?
C1 C2 C6 117.3(4) . . ?
C3 C2 C1 120.1(4) . . ?
C3 C2 C6 122.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C3 120.6(6) 4_855 . ?
C3 C4 C5 119.7(3) 4_855 . ?
C3 C4 C5 119.7(3) . . ?
O3 C5 C4 116.7(3) . . ?
O3 C5 C4 116.7(3) 4_855 . ?
O3 C5 O3 126.6(6) . 4_855 ?
O1 C6 C2 117.4(4) . . ?
O1 C6 O2 127.9(4) . . ?
O2 C6 C2 114.7(4) . . ?
O1 Ni1 O1 90.9(2) . 4_755 ?
O1 Ni1 O1 90.9(2) 3 2_755 ?
O1 Ni1 O1 88.4(2) 4_755 2_755 ?
O1 Ni1 O1 88.4(2) . 3 ?
O1 Ni1 O1 171.4(2) . 2_755 ?
O1 Ni1 O1 171.4(2) 4_755 3 ?
O5 Ni1 O1 85.68(10) . 3 ?
O5 Ni1 O1 85.68(10) . 4_755 ?
O5 Ni1 O1 85.68(10) . 2_755 ?
O5 Ni1 O1 85.68(10) . . ?
O6 Ni1 O1 94.32(10) . 3 ?
O6 Ni1 O1 94.32(10) . 2_755 ?
O6 Ni1 O1 94.32(10) . 4_755 ?
O6 Ni1 O1 94.32(10) . . ?
O6 Ni1 O5 180.0 . . ?
O2 Ni2 O2 88.1(2) 4_755 2_755 ?
O2 Ni2 O4 86.40(14) 4_755 . ?
O2 Ni2 O4 86.40(14) 2_755 . ?
O3 Ni2 O2 89.46(16) 5_455 2_755 ?
O3 Ni2 O2 89.46(16) 7_445 4_755 ?
O3 Ni2 O2 170.58(14) 7_445 2_755 ?
O3 Ni2 O2 170.58(14) 5_455 4_755 ?
O3 Ni2 O3 91.5(2) 5_455 7_445 ?
O3 Ni2 O4 84.36(14) 5_455 . ?
O3 Ni2 O4 84.36(14) 7_445 . ?
O6 Ni2 O2 92.30(14) . 4_755 ?
O6 Ni2 O2 92.30(14) . 2_755 ?
O6 Ni2 O3 96.90(14) . 5_455 ?
O6 Ni2 O3 96.90(14) . 7_445 ?
O6 Ni2 O4 178.2(2) . . ?
C6 O1 Ni1 127.8(3) . . ?
C6 O2 Ni2 132.8(3) . 2_755 ?
C5 O3 Ni2 131.9(3) . 5_544 ?
Ni2 O4 H4 110.5 . . ?
Ni1 O5 H5 136.4 . . ?
Ni1 O6 Ni2 122.51(15) . . ?
Ni1 O6 Ni2 122.51(15) . 2_755 ?
Ni2 O6 Ni2 115.0(3) 2_755 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 3.5(8) . . . . ?
C1 C2 C6 O1 147.8(5) . . . . ?
C1 C2 C6 O2 -30.8(7) . . . . ?
C2 C1 C2 C3 -0.7(10) 4_855 . . . ?
C2 C1 C2 C6 -175.8(4) 4_855 . . . ?
C2 C3 C4 C3 -6.3(10) . . . 4_855 ?
C2 C3 C4 C5 177.7(5) . . . . ?
C2 C6 O1 Ni1 -148.7(3) . . . . ?
C2 C6 O2 Ni2 146.4(4) . . . 2_755 ?
C3 C2 C6 O1 -27.2(7) . . . . ?
C3 C2 C6 O2 154.2(5) . . . . ?
C3 C4 C5 O3 -3.7(9) . . . . ?
C3 C4 C5 O3 179.7(6) . . . 4_855 ?
C3 C4 C5 O3 -179.7(6) 4_855 . . . ?
C3 C4 C5 O3 3.7(9) 4_855 . . 4_855 ?
C4 C5 O3 Ni2 -165.5(4) . . . 5_544 ?
C6 C2 C3 C4 178.3(5) . . . . ?
O1 C6 O2 Ni2 -32.0(8) . . . 2_755 ?
O2 C6 O1 Ni1 29.6(8) . . . . ?
O3 C5 O3 Ni2 10.7(11) 4_855 . . 5_544 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.95(3)
2 0.05(3)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 917759'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r3563)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C88 H48 Mn12 O64)'
_chemical_formula_sum            'C22 H12 Mn3 O16'
_chemical_formula_weight         697.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.3370 0.7280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.692(3)
_cell_length_b                   14.424(3)
_cell_length_c                   21.492(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3934.5(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3564
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.98
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1527
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31002
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         2.979
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCX-mini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2709
_reflns_number_total             3564
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0852
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0601P)²+12.1819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1845
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-C6 \\sim C6-O8A
 with sigma of 0.02
 O8A-C6 \\sim O8-C6
 with sigma of 0.001
3. Rigid bond restraints
 C6, O8, O8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Mn1, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C2, C3, C4, C5, C6, O8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C6, C5, C4, C3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O2, C1, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O8(0.5) O8A(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C2(H2), C4(H4)
7.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O6 O 0.3192(4) 0.2654(3) -0.0678(2) 0.0587(14) Uani 1 1 d . . . . .
Mn1 Mn 0.27295(7) 0.37110(6) 0.03244(5) 0.0298(3) Uani 1 1 d . U . . .
Mn2 Mn 0.5000 0.5000 0.0000 0.0265(3) Uani 1 2 d S T P . .
C12 C -0.0748(6) 0.7500 0.0000 0.036(2) Uani 1 2 d S T P . .
O2 O 0.4270(5) 0.4474(5) 0.0843(2) 0.0826(19) Uani 1 1 d . U . . .
C1 C 0.3774(6) 0.4409(5) 0.1329(3) 0.0453(16) Uani 1 1 d . U . . .
C11 C 0.0440(6) 0.7500 0.0000 0.032(2) Uani 1 2 d S T P . .
O5 O 0.4081(4) 0.3813(3) -0.0346(3) 0.0589(15) Uani 1 1 d . U . . .
C9 C 0.2617(7) 0.7500 0.0000 0.034(2) Uani 1 2 d S T P . .
H9 H 0.3366 0.7500 0.0000 0.041 Uiso 1 2 calc RS T P . .
C8 C 0.2086(4) 0.6664(4) -0.0037(3) 0.0318(15) Uani 1 1 d . . . . .
O1 O 0.2811(4) 0.4175(4) 0.1321(2) 0.0597(14) Uani 1 1 d . U . . .
O3 O 0.2192(3) 0.5026(3) 0.0010(2) 0.0461(12) Uani 1 1 d . . . . .
C10 C 0.0997(4) 0.6673(4) -0.0038(3) 0.0329(15) Uani 1 1 d . . . . .
H10 H 0.0623 0.6104 -0.0064 0.039 Uiso 1 1 calc R . . . .
C7 C 0.2693(5) 0.5772(4) -0.0058(3) 0.0380(16) Uani 1 1 d . . . . .
C2 C 0.3801(8) 0.4468(6) 0.2500 0.042(2) Uani 1 2 d S TU P . .
H2 H 0.3063 0.4358 0.2500 0.051 Uiso 1 2 calc RS T P . .
C3 C 0.4319(5) 0.4545(4) 0.1929(3) 0.0408(15) Uani 1 1 d . U . . .
C13 C 0.3995(5) 0.3142(4) -0.0714(3) 0.0405(17) Uani 1 1 d . . . . .
C4 C 0.5384(6) 0.4718(5) 0.1941(4) 0.056(2) Uani 1 1 d . U . . .
H4 H 0.5749 0.4797 0.1558 0.067 Uiso 1 1 calc R . . . .
C14 C 0.4840(8) 0.2943(7) -0.1156(5) 0.097(4) Uani 1 1 d . . . . .
H14A H 0.5283 0.2442 -0.0993 0.146 Uiso 1 1 calc GR . . . .
H14B H 0.5270 0.3501 -0.1216 0.146 Uiso 1 1 calc GR . . . .
H14C H 0.4535 0.2755 -0.1555 0.146 Uiso 1 1 calc GR . . . .
C5 C 0.5948(9) 0.4781(8) 0.2500 0.068(3) Uani 1 2 d S TU P A .
O7 O -0.1194(3) 0.8230(3) 0.0178(2) 0.0463(13) Uani 1 1 d . . . . .
O4 O 0.3671(3) 0.5835(3) -0.0121(3) 0.0575(15) Uani 1 1 d . . . . .
C6 C 0.7174(12) 0.4937(13) 0.2500 0.117(5) Uani 1 2 d DS TU P . .
O8 O 0.7642(14) 0.4678(14) 0.2984(7) 0.135(7) Uani 0.5 1 d D U . A 1
O8A O 0.7549(17) 0.5326(14) 0.2028(8) 0.140(7) Uani 0.5 1 d D U . A 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
O6 Mn1 2.191(5) 3 ?
O6 C13 1.240(7) . ?
Mn1 O6 2.191(5) 3 ?
Mn1 O2 2.506(7) . ?
Mn1 O5 2.245(5) . ?
Mn1 O1 2.246(5) . ?
Mn1 O3 2.126(4) . ?
Mn1 O7 2.092(4) 7 ?
Mn2 O2 2.171(5) 5_665 ?
Mn2 O2 2.171(5) . ?
Mn2 O5 2.201(4) 5_665 ?
Mn2 O5 2.201(4) . ?
Mn2 O4 2.089(4) . ?
Mn2 O4 2.089(4) 5_665 ?
C12 C11 1.509(11) . ?
C12 O7 1.255(5) . ?
C12 O7 1.255(5) 3_565 ?
O2 C1 1.224(8) . ?
C1 O1 1.268(8) . ?
C1 C3 1.476(10) . ?
C11 C10 1.389(7) . ?
C11 C10 1.389(7) 3_565 ?
O5 C13 1.254(8) . ?
C9 H9 0.9500 . ?
C9 C8 1.384(7) . ?
C9 C8 1.384(7) 3_565 ?
C8 C10 1.382(7) . ?
C8 C7 1.500(8) . ?
O3 C7 1.259(7) . ?
C10 H10 0.9500 . ?
C7 O4 1.252(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.397(8) . ?
C2 C3 1.397(8) 6_556 ?
C3 C4 1.375(9) . ?
C13 C14 1.462(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.402(10) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C5 C4 1.402(10) 6_556 ?
C5 C6 1.572(19) . ?
O7 Mn1 2.092(4) 7_565 ?
C6 O8 1.254(11) 6_556 ?
C6 O8 1.254(11) . ?
C6 O8A 1.254(11) . ?
C6 O8A 1.254(11) 6_556 ?

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
C13 O6 Mn1 138.7(5) . 3 ?
O6 Mn1 O2 91.8(2) 3 . ?
O6 Mn1 O5 94.43(19) 3 . ?
O6 Mn1 O1 85.6(2) 3 . ?
O5 Mn1 O2 70.15(18) . . ?
O5 Mn1 O1 123.88(19) . . ?
O1 Mn1 O2 53.78(18) . . ?
O3 Mn1 O6 176.51(18) . 3 ?
O3 Mn1 O2 90.01(19) . . ?
O3 Mn1 O5 88.99(18) . . ?
O3 Mn1 O1 93.0(2) . . ?
O7 Mn1 O6 90.20(18) 7 3 ?
O7 Mn1 O2 159.97(18) 7 . ?
O7 Mn1 O5 129.55(19) 7 . ?
O7 Mn1 O1 106.6(2) 7 . ?
O7 Mn1 O3 87.09(16) 7 . ?
O2 Mn2 O2 180.0 . 5_665 ?
O2 Mn2 O5 77.6(2) . . ?
O2 Mn2 O5 102.4(2) . 5_665 ?
O2 Mn2 O5 77.6(2) 5_665 5_665 ?
O2 Mn2 O5 102.4(2) 5_665 . ?
O5 Mn2 O5 180.0 . 5_665 ?
O4 Mn2 O2 87.7(2) . . ?
O4 Mn2 O2 92.3(2) . 5_665 ?
O4 Mn2 O2 87.7(2) 5_665 5_665 ?
O4 Mn2 O2 92.3(2) 5_665 . ?
O4 Mn2 O5 88.76(18) 5_665 5_665 ?
O4 Mn2 O5 91.23(18) 5_665 . ?
O4 Mn2 O5 88.77(18) . . ?
O4 Mn2 O5 91.24(18) . 5_665 ?
O4 Mn2 O4 180.0(2) . 5_665 ?
O7 C12 C11 116.8(4) 3_565 . ?
O7 C12 C11 116.8(4) . . ?
O7 C12 O7 126.4(7) . 3_565 ?
Mn2 O2 Mn1 96.6(2) . . ?
C1 O2 Mn1 86.8(5) . . ?
C1 O2 Mn2 163.5(6) . . ?
O2 C1 O1 120.3(7) . . ?
O2 C1 C3 119.6(7) . . ?
O1 C1 C3 119.9(7) . . ?
C10 C11 C12 120.6(4) 3_565 . ?
C10 C11 C12 120.6(4) . . ?
C10 C11 C10 118.8(7) . 3_565 ?
Mn2 O5 Mn1 103.8(2) . . ?
C13 O5 Mn1 106.7(4) . . ?
C13 O5 Mn2 149.2(5) . . ?
C8 C9 H9 119.2 . . ?
C8 C9 H9 119.2 3_565 . ?
C8 C9 C8 121.7(8) 3_565 . ?
C9 C8 C7 119.9(5) . . ?
C10 C8 C9 118.6(6) . . ?
C10 C8 C7 121.5(5) . . ?
C1 O1 Mn1 97.9(5) . . ?
C7 O3 Mn1 129.6(4) . . ?
C11 C10 H10 119.4 . . ?
C8 C10 C11 121.2(6) . . ?
C8 C10 H10 119.4 . . ?
O3 C7 C8 118.1(5) . . ?
O4 C7 C8 116.8(5) . . ?
O4 C7 O3 125.1(5) . . ?
C3 C2 H2 118.5 . . ?
C3 C2 H2 118.5 6_556 . ?
C3 C2 C3 123.0(10) 6_556 . ?
C2 C3 C1 122.4(7) . . ?
C4 C3 C1 120.1(7) . . ?
C4 C3 C2 117.4(7) . . ?
O6 C13 O5 118.1(6) . . ?
O6 C13 C14 122.1(7) . . ?
O5 C13 C14 119.8(7) . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 122.0(8) . . ?
C5 C4 H4 119.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C5 C4 118.0(11) 6_556 . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 C6 121.0(5) 6_556 . ?
C12 O7 Mn1 138.1(4) . 7_565 ?
C7 O4 Mn2 138.2(4) . . ?
O8 C6 C5 115.2(12) 6_556 . ?
O8 C6 C5 115.2(12) . . ?
O8 C6 O8 112(2) . 6_556 ?
O8A C6 C5 116.1(14) 6_556 . ?
O8A C6 C5 116.1(14) . . ?
O8A C6 O8A 108(2) . 6_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O6 C13 O5 -104.5(8) 3 . . . ?
Mn1 O6 C13 C14 74.2(11) 3 . . . ?
Mn1 O2 C1 O1 -10.5(7) . . . . ?
Mn1 O2 C1 C3 165.4(6) . . . . ?
Mn1 O5 C13 O6 6.9(8) . . . . ?
Mn1 O5 C13 C14 -171.7(7) . . . . ?
Mn1 O3 C7 C8 -155.8(5) . . . . ?
Mn1 O3 C7 O4 21.5(11) . . . . ?
Mn2 O2 C1 O1 92(2) . . . . ?
Mn2 O2 C1 C3 -92(2) . . . . ?
Mn2 O5 C13 O6 179.2(6) . . . . ?
Mn2 O5 C13 C14 0.6(14) . . . . ?
C12 C11 C10 C8 -179.9(5) . . . . ?
O2 C1 O1 Mn1 11.9(8) . . . . ?
O2 C1 C3 C2 -179.1(7) . . . . ?
O2 C1 C3 C4 -1.8(10) . . . . ?
C1 C3 C4 C5 -175.1(8) . . . . ?
C11 C12 O7 Mn1 -177.6(3) . . . 7_565 ?
C9 C8 C10 C11 -0.3(10) . . . . ?
C9 C8 C7 O3 168.7(6) . . . . ?
C9 C8 C7 O4 -8.8(10) . . . . ?
C8 C9 C8 C10 0.1(5) 3_565 . . . ?
C8 C9 C8 C7 -178.3(7) 3_565 . . . ?
C8 C7 O4 Mn2 163.2(5) . . . . ?
O1 C1 C3 C2 -3.1(10) . . . . ?
O1 C1 C3 C4 174.2(7) . . . . ?
O3 C7 O4 Mn2 -14.2(13) . . . . ?
C10 C11 C10 C8 0.1(5) 3_565 . . . ?
C10 C8 C7 O3 -9.6(10) . . . . ?
C10 C8 C7 O4 172.8(7) . . . . ?
C7 C8 C10 C11 178.1(5) . . . . ?
C2 C3 C4 C5 2.4(12) . . . . ?
C3 C1 O1 Mn1 -164.1(5) . . . . ?
C3 C2 C3 C1 176.4(5) 6_556 . . . ?
C3 C2 C3 C4 -1.0(13) 6_556 . . . ?
C3 C4 C5 C4 -3.8(16) . . . 6_556 ?
C3 C4 C5 C6 177.3(11) . . . . ?
C4 C5 C6 O8 156.9(16) 6_556 . . 6_556 ?
C4 C5 C6 O8 -24(2) . . . 6_556 ?
C4 C5 C6 O8 24(2) 6_556 . . . ?
C4 C5 C6 O8 -156.9(16) . . . . ?
C4 C5 C6 O8A 153.8(16) . . . 6_556 ?
C4 C5 C6 O8A 25(2) . . . . ?
C4 C5 C6 O8A -25(2) 6_556 . . 6_556 ?
C4 C5 C6 O8A -153.8(16) 6_556 . . . ?
O7 C12 C11 C10 -16.1(4) 3_565 . . . ?
O7 C12 C11 C10 163.9(4) . . . . ?
O7 C12 C11 C10 -16.1(4) . . . 3_565 ?
O7 C12 C11 C10 163.9(4) 3_565 . . 3_565 ?
O7 C12 O7 Mn1 2.4(3) 3_565 . . 7_565 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
