# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_lb592
_database_code_depnum_ccdc_archive 'CCDC 1022213'
_audit_update_record             
;
2014-09-01 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C70 H40 Mn3 N10 O8), 2(C4 H8 O)'
_chemical_formula_sum            'C148 H96 Mn6 N20 O18'
_chemical_formula_weight         2772.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Mn Mn 0.2237 0.8587
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   27.159(4)
_cell_length_b                   13.925(2)
_cell_length_c                   41.043(5)
_cell_angle_alpha                90
_cell_angle_beta                 112.375(8)
_cell_angle_gamma                90
_cell_volume                     14353(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9750
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      26.82

_exptl_crystal_description       'thick losange plate'
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             5672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.730
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI US'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            136525
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         2.608
_diffrn_reflns_theta_max         27.189
_diffrn_reflns_theta_full        27.100
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             24403
_reflns_number_gt                20832
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
 All non-hydrogens were refined anisotropically. One of the naphtyl
 groups was refined disordered over two positions of the external
 ring, with relative occupancies of 0.53:0.47. The rest of napthyl
 groups also showed some thermal disorder but splitting them did not
 converge. All were refined with displacement parameters restraints,
 as well as the lattice THF molecules. Hydrogens were placed on their
 carrier atom geometrically and refined with a riding model. At the end
 of the refinement there remained a space in the cell with only weak
 electron density peaks that could not be modeled as lattice solvent
 molecules. This was analyzed and taken into account with PLATON/SQUEEZE
 that recovered a total of ca. 86 electrons per cell over mostly 2
 large voids of 725 cubic angstroms and 4 voids of 165 cubic angstroms.
 at the most these figures would agree with two diffuse lattice THF
 molecules per cell, e.g. at the most half a THF molecule per formula
 unit.
;

_vrf_PLAT015_lb592               
;
PROBLEM: No _shelx_hkl_file record in SHELXL20xy CIF
RESPONSE: The hkl format after using SQUEEZE gave errors with validation
software and the corresponding appended hkl section in the cif was 
removed. The fcf file has been submitted together with the cif to the
CCDC. 
;

_vrf_PLAT027_lb592               
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      27.10 Deg.
RESPONSE: Crystals systematically showed significant diffraction only up
to ca. 0.8-0.85 ansgtrom, even using synchrotron radiation. The present 
data were cut at 0.85 angstrom, as then Rint>25% and I/s(I)<2. This 
results in rather low thetafull and thetamax values. 
;

_vrf_THETM01_lb592               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
            Calculated sin(theta_max)/wavelength =    0.5897
RESPONSE: Crystals systematically showed significant diffraction only up
to ca. 0.8-0.85 ansgtrom, even using synchrotron radiation. The present 
data were cut at 0.85 angstrom, as then Rint>25% and I/s(I)<2. This 
results in rather low thetafull and thetamax values.
;

_vrf_PLAT411_lb592               
;
PROBLEM: Short Inter H...H Contact 
RESPONSE: These short H H contacts all involve at least one hydrogens
from a disordered naphtyl or lattice THF molecule. These hydrogens, 
placed geometrically on their carrier atom, may have ill-defined
positions due the disorder of their carrier, resulting in some of
these short H H contacts.
;

_vrf_PLAT045_lb592               
;
PROBLEM: Calculated and Reported Z Differ by ............       2.00 Ratio
RESPONSE: Although very similar, there are two crystallographically
distinct [Mn3] moieties in the asymmetric unit, so that the correct Z
should be 4 and not 8.
;

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 0.000 0.500 0.000 725.1 31.2
2 0.028 0.596 0.225 22.7 2.0
3 -0.028 0.404 0.775 22.2 1.9
4 0.150 0.225 0.373 164.9 7.1
5 0.350 0.725 0.127 164.8 7.2
6 0.500 0.000 0.500 725.1 31.1
7 0.472 0.096 0.275 22.3 1.9
8 0.528 0.904 0.725 22.5 1.9
9 0.650 0.275 0.873 164.9 7.1
10 0.850 0.775 0.627 164.7 7.2
_platon_squeeze_details          
;
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0953P)²+85.2245P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         24403
_refine_ls_number_parameters     1784
_refine_ls_number_restraints     433
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.1132
_refine_ls_wR_factor_ref         0.2829
_refine_ls_wR_factor_gt          0.2767
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.100
_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_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
Mn1 Mn 0.40903(4) 0.76872(7) 0.86664(2) 0.0406(2) Uani 1 1 d . . . . .
Mn2 Mn 0.29204(4) 0.69953(8) 0.78872(3) 0.0458(3) Uani 1 1 d . . . . .
Mn3 Mn 0.15087(4) 0.65357(7) 0.74866(3) 0.0413(3) Uani 1 1 d . . . . .
O1 O 0.39120(17) 0.6505(4) 0.89631(12) 0.0532(12) Uani 1 1 d . . . . .
O2 O 0.32629(18) 0.6820(4) 0.84695(12) 0.0529(12) Uani 1 1 d . . . . .
O3 O 0.37145(18) 0.8988(3) 0.85000(12) 0.0501(12) Uani 1 1 d . . . . .
O4 O 0.30754(18) 0.8526(4) 0.79963(11) 0.0476(11) Uani 1 1 d . . . . .
O5 O 0.2673(2) 0.5509(4) 0.78410(15) 0.0687(16) Uani 1 1 d . . . . .
O6 O 0.17998(19) 0.5177(4) 0.76795(14) 0.0629(15) Uani 1 1 d . . . . .
O7 O 0.21518(17) 0.7273(3) 0.79506(11) 0.0431(10) Uani 1 1 d . . . . .
O8 O 0.13826(18) 0.7977(4) 0.76925(15) 0.0593(13) Uani 1 1 d . . . . .
N1 N 0.4576(2) 0.8464(4) 0.95106(13) 0.0413(12) Uani 1 1 d . . . . .
H1B H 0.4267 0.8524 0.9532 0.050 Uiso 1 1 calc R U . . .
N2 N 0.4633(2) 0.8239(4) 0.92079(14) 0.0437(13) Uani 1 1 d . . . . .
N3 N 0.4937(2) 0.7681(4) 0.87083(15) 0.0496(14) Uani 1 1 d . . . . .
N4 N 0.4107(2) 0.7076(5) 0.81764(16) 0.0567(16) Uani 1 1 d . . . . .
N5 N 0.3735(2) 0.6640(5) 0.78903(16) 0.0615(18) Uani 1 1 d . . . . .
N6 N 0.2508(2) 0.7307(5) 0.73063(14) 0.0511(15) Uani 1 1 d . . . . .
N7 N 0.2015(2) 0.6910(5) 0.72044(14) 0.0506(14) Uani 1 1 d . . . . .
N8 N 0.1017(2) 0.6411(4) 0.69062(14) 0.0477(14) Uani 1 1 d . . . . .
N9 N 0.0648(2) 0.6245(4) 0.74102(15) 0.0475(14) Uani 1 1 d . . . . .
N10 N 0.0354(2) 0.6233(4) 0.76075(16) 0.0510(14) Uani 1 1 d . . . . .
H10A H 0.0486 0.6317 0.7837 0.061 Uiso 1 1 calc R U . . .
C1 C 0.5616(3) 0.8914(6) 1.04100(19) 0.0565(19) Uani 1 1 d . . . . .
H1A H 0.5925 0.8806 1.0359 0.068 Uiso 1 1 calc R U . . .
C2 C 0.5662(3) 0.9140(6) 1.07440(19) 0.060(2) Uani 1 1 d . . . . .
H2A H 0.6007 0.9190 1.0924 0.073 Uiso 1 1 calc R U . . .
C3 C 0.5216(3) 0.9302(5) 1.08304(17) 0.056(2) Uani 1 1 d . . . . .
C4 C 0.5247(4) 0.9557(6) 1.1179(2) 0.068(2) Uani 1 1 d . . . . .
H4A H 0.5586 0.9618 1.1365 0.082 Uiso 1 1 calc R U . . .
C5 C 0.4804(4) 0.9709(7) 1.1244(2) 0.082(3) Uani 1 1 d . . . . .
H5A H 0.4834 0.9865 1.1476 0.098 Uiso 1 1 calc R U . . .
C6 C 0.4296(4) 0.9640(8) 1.0972(2) 0.076(3) Uani 1 1 d . . . . .
H6A H 0.3985 0.9747 1.1021 0.092 Uiso 1 1 calc R U . . .
C7 C 0.4254(3) 0.9419(7) 1.0641(2) 0.067(2) Uani 1 1 d . . . . .
H7A H 0.3910 0.9387 1.0458 0.080 Uiso 1 1 calc R U . . .
C8 C 0.4696(3) 0.9241(5) 1.05617(17) 0.0545(19) Uani 1 1 d . . . . .
C9 C 0.4661(3) 0.8999(5) 1.02165(17) 0.0486(17) Uani 1 1 d . . . . .
H9A H 0.4318 0.8944 1.0034 0.058 Uiso 1 1 calc R U . . .
C10 C 0.5098(3) 0.8843(5) 1.01376(17) 0.0447(16) Uani 1 1 d . . . . .
C11 C 0.5059(3) 0.8589(4) 0.97818(17) 0.0437(16) Uani 1 1 d . . . . .
C12 C 0.5437(3) 0.8442(5) 0.96407(18) 0.0482(17) Uani 1 1 d . . . . .
H12A H 0.5812 0.8482 0.9760 0.058 Uiso 1 1 calc R U . . .
C13 C 0.5159(3) 0.8223(5) 0.92877(18) 0.0458(16) Uani 1 1 d . . . . .
C14 C 0.5336(3) 0.7982(6) 0.9003(2) 0.0547(18) Uani 1 1 d . . . . .
C15 C 0.5860(3) 0.8021(8) 0.9021(3) 0.078(3) Uani 1 1 d . . . . .
H15A H 0.6142 0.8209 0.9232 0.094 Uiso 1 1 calc R U . . .
C16 C 0.5962(3) 0.7786(9) 0.8731(3) 0.094(4) Uani 1 1 d . . . . .
H16A H 0.6315 0.7815 0.8738 0.112 Uiso 1 1 calc R U . . .
C17 C 0.5551(3) 0.7503(8) 0.8424(3) 0.082(3) Uani 1 1 d . . . . .
H17A H 0.5616 0.7367 0.8217 0.099 Uiso 1 1 calc R U . . .
C18 C 0.5042(3) 0.7424(6) 0.8426(2) 0.0582(19) Uani 1 1 d . . . . .
C19 C 0.4575(3) 0.7026(6) 0.8138(2) 0.060(2) Uani 1 1 d . . . . .
C20 C 0.4525(3) 0.6601(8) 0.7827(2) 0.072(3) Uani 1 1 d . . . . .
H20A H 0.4794 0.6492 0.7736 0.087 Uiso 1 1 calc R U . . .
C21 C 0.3987(3) 0.6366(7) 0.7674(2) 0.064(2) Uani 1 1 d . . . . .
C22 C 0.3718(3) 0.5930(7) 0.7321(2) 0.070(3) Uani 1 1 d . . . . .
C23 C 0.3244(4) 0.5527(9) 0.7223(3) 0.098(4) Uani 1 1 d . . . . .
H23A H 0.3072 0.5485 0.7386 0.118 Uiso 1 1 calc R U . . .
C24 C 0.2977(4) 0.5139(10) 0.6862(3) 0.094(4) Uani 1 1 d . . . . .
C25 C 0.2460(5) 0.4852(10) 0.6740(3) 0.106(3) Uani 1 1 d . U . . .
H25A H 0.2268 0.4864 0.6890 0.127 Uiso 1 1 calc R U . . .
C26 C 0.2219(5) 0.4545(10) 0.6398(3) 0.110(3) Uani 1 1 d . U . . .
H26A H 0.1856 0.4357 0.6314 0.133 Uiso 1 1 calc R U . . .
C27 C 0.2497(5) 0.4498(10) 0.6163(3) 0.105(3) Uani 1 1 d . U . . .
H27A H 0.2331 0.4229 0.5934 0.126 Uiso 1 1 calc R U . . .
C28 C 0.2998(4) 0.4842(9) 0.6271(3) 0.097(3) Uani 1 1 d . . . . .
H28A H 0.3181 0.4866 0.6114 0.116 Uiso 1 1 calc R U . . .
C29 C 0.3257(3) 0.5179(8) 0.6638(3) 0.079(3) Uani 1 1 d . . . . .
C30 C 0.3748(4) 0.5573(8) 0.6744(3) 0.084(3) Uani 1 1 d . . . . .
H30A H 0.3936 0.5584 0.6591 0.101 Uiso 1 1 calc R U . . .
C31 C 0.3968(4) 0.5953(7) 0.7073(2) 0.070(2) Uani 1 1 d . . . . .
H31A H 0.4308 0.6249 0.7141 0.084 Uiso 1 1 calc R U . . .
C32 C 0.3454(3) 0.6313(5) 0.8741(2) 0.0526(18) Uani 1 1 d . . . . .
C33 C 0.3168(4) 0.5446(7) 0.8816(3) 0.085(3) Uani 1 1 d . . . . .
C34 C 0.3336(3) 0.9155(5) 0.82092(17) 0.0467(16) Uani 1 1 d . . . . .
C35 C 0.3196(4) 1.0204(6) 0.8111(2) 0.072(2) Uani 1 1 d . . . . .
C36 C 0.2293(3) 0.4948(7) 0.7785(3) 0.082(3) Uani 1 1 d . U . . .
C37 C 0.2402(5) 0.3855(8) 0.7848(4) 0.117(4) Uani 1 1 d . U . . .
C38 C 0.1850(3) 0.7967(5) 0.79358(18) 0.0482(16) Uani 1 1 d . . . . .
C39 C 0.2027(3) 0.8782(7) 0.8199(3) 0.080(3) Uani 1 1 d . . . . .
C41 C 0.3245(3) 0.7996(6) 0.67353(18) 0.0554(18) Uani 1 1 d . . . . .
H41A H 0.3007 0.7731 0.6520 0.067 Uiso 1 1 calc R U . . .
C42 C 0.3714(3) 0.8366(6) 0.67529(19) 0.060(2) Uani 1 1 d . . . . .
H42A H 0.3789 0.8393 0.6545 0.072 Uiso 1 1 calc R U . . .
C43 C 0.4094(3) 0.8712(6) 0.70706(18) 0.0540(18) Uani 1 1 d . . . . .
C44 C 0.4618(3) 0.9005(7) 0.7108(2) 0.071(3) Uani 1 1 d . . . . .
H44A H 0.4721 0.8964 0.6912 0.085 Uiso 1 1 calc R U . . .
C45 C 0.4970(4) 0.9342(7) 0.7422(2) 0.071(2) Uani 1 1 d . . . . .
H45A H 0.5316 0.9534 0.7443 0.085 Uiso 1 1 calc R U . . .
C46 C 0.4828(3) 0.9407(7) 0.7714(2) 0.074(3) Uani 1 1 d . . . . .
H46A H 0.5074 0.9651 0.7932 0.089 Uiso 1 1 calc R U . . .
C47 C 0.4332(3) 0.9118(7) 0.7685(2) 0.073(3) Uani 1 1 d . . . . .
H47A H 0.4236 0.9170 0.7884 0.087 Uiso 1 1 calc R U . . .
C48 C 0.3955(3) 0.8743(6) 0.73667(17) 0.0511(17) Uani 1 1 d . . . . .
C49 C 0.3459(3) 0.8401(7) 0.73398(18) 0.062(2) Uani 1 1 d . . . . .
H49A H 0.3364 0.8446 0.7539 0.075 Uiso 1 1 calc R U . . .
C50 C 0.3100(3) 0.7997(6) 0.70333(18) 0.0514(17) Uani 1 1 d . . . . .
C51 C 0.2607(3) 0.7562(6) 0.70139(18) 0.0566(19) Uani 1 1 d . . . . .
C52 C 0.2162(3) 0.7300(6) 0.67146(18) 0.058(2) Uani 1 1 d . . . . .
H52A H 0.2118 0.7369 0.6475 0.070 Uiso 1 1 calc R U . . .
C53 C 0.1801(3) 0.6924(6) 0.68421(18) 0.0537(18) Uani 1 1 d . . . . .
C54 C 0.1250(3) 0.6566(6) 0.66793(18) 0.0526(18) Uani 1 1 d . . . . .
C55 C 0.0978(3) 0.6422(7) 0.6321(2) 0.071(2) Uani 1 1 d . . . . .
H55A H 0.1145 0.6538 0.6159 0.085 Uiso 1 1 calc R U . . .
C56 C 0.0455(3) 0.6102(9) 0.6206(2) 0.086(3) Uani 1 1 d . . . . .
H56A H 0.0265 0.5976 0.5963 0.103 Uiso 1 1 calc R U . . .
C57 C 0.0205(3) 0.5963(7) 0.6443(2) 0.070(2) Uani 1 1 d . . . . .
H57A H -0.0155 0.5758 0.6365 0.084 Uiso 1 1 calc R U . . .
C58 C 0.0501(3) 0.6136(5) 0.67947(19) 0.0508(17) Uani 1 1 d . . . . .
C59 C 0.0299(2) 0.6082(5) 0.70782(19) 0.0508(17) Uani 1 1 d . . . . .
C60 C -0.0214(3) 0.5984(6) 0.7073(2) 0.060(2) Uani 1 1 d . . . . .
H60A H -0.0531 0.5873 0.6873 0.072 Uiso 1 1 calc R U . . .
C61 C -0.0169(3) 0.6078(6) 0.7416(2) 0.0551(18) Uani 1 1 d . . . . .
C62 C -0.0573(3) 0.6047(7) 0.7578(2) 0.066(2) Uani 1 1 d . . . . .
C63 C -0.0464(3) 0.6146(6) 0.7916(2) 0.063(2) Uani 1 1 d . . . . .
H63A H -0.0105 0.6271 0.8066 0.076 Uiso 1 1 calc R U . . .
C64 C -0.0837(4) 0.6079(8) 0.8071(3) 0.082(3) Uani 1 1 d . . . . .
C65 C -0.0740(4) 0.6139(8) 0.8420(3) 0.090(3) Uani 1 1 d . . . . .
H65A H -0.0382 0.6236 0.8577 0.109 Uiso 1 1 calc R U . . .
C66 C -0.1124(6) 0.6070(10) 0.8563(4) 0.114(4) Uani 1 1 d . . . . .
H66A H -0.1036 0.6118 0.8809 0.137 Uiso 1 1 calc R U . . .
C67 C -0.1637(6) 0.5929(12) 0.8334(4) 0.132(4) Uani 1 1 d . U . . .
H67A H -0.1905 0.5843 0.8427 0.158 Uiso 1 1 calc R U . . .
C68 C -0.1776(6) 0.5906(13) 0.7986(4) 0.140(3) Uani 1 1 d . U . . .
H68A H -0.2141 0.5881 0.7834 0.167 Uiso 1 1 calc R U . . .
C69 C -0.1374(6) 0.5920(13) 0.7844(4) 0.132(3) Uani 1 1 d . U . . .
C70 C -0.1498(6) 0.5945(13) 0.7477(4) 0.137(3) Uani 1 1 d . U . . .
H70A H -0.1859 0.5968 0.7319 0.165 Uiso 1 1 calc R U . . .
C71 C -0.1102(5) 0.5938(12) 0.7350(4) 0.130(4) Uani 1 1 d . U . . .
H71A H -0.1187 0.5859 0.7104 0.157 Uiso 1 1 calc R U . . .
Mn4 Mn 0.07571(4) 0.82908(9) 0.84710(3) 0.0516(3) Uani 1 1 d . . . . .
Mn5 Mn 0.18666(4) 0.79198(9) 0.92996(3) 0.0565(3) Uani 1 1 d . . . . .
Mn6 Mn 0.32676(4) 0.71737(9) 0.97564(3) 0.0508(3) Uani 1 1 d . . . . .
O9 O 0.09120(19) 0.6813(4) 0.82992(13) 0.0580(13) Uani 1 1 d . . . . .
O10 O 0.15474(19) 0.7502(4) 0.87283(13) 0.0577(13) Uani 1 1 d . . . . .
O11 O 0.11158(19) 0.9634(4) 0.85513(15) 0.0648(15) Uani 1 1 d . . . . .
O12 O 0.1748(2) 0.9368(4) 0.90818(15) 0.0698(16) Uani 1 1 d . . . . .
O13 O 0.20166(18) 0.6403(4) 0.94138(14) 0.0616(14) Uani 1 1 d . . . . .
O14 O 0.28637(18) 0.5890(4) 0.96033(14) 0.0633(15) Uani 1 1 d . . . . .
O15 O 0.26840(17) 0.8013(4) 0.92614(13) 0.0550(13) Uani 1 1 d . . . . .
O16 O 0.35331(17) 0.8365(4) 0.95101(12) 0.0513(12) Uani 1 1 d . . . . .
N11 N 0.0384(2) 0.8581(4) 0.75921(15) 0.0526(15) Uani 1 1 d . . . . .
H11C H 0.0704 0.8508 0.7589 0.063 Uiso 1 1 calc R U . . .
N12 N 0.0282(2) 0.8542(4) 0.78845(16) 0.0512(15) Uani 1 1 d . . . . .
N13 N -0.0105(2) 0.8439(5) 0.83775(16) 0.0542(15) Uani 1 1 d . . . . .
N14 N 0.0674(2) 0.8066(5) 0.89745(16) 0.0566(16) Uani 1 1 d . . . . .
N15 N 0.1023(2) 0.7759(5) 0.92986(16) 0.0575(16) Uani 1 1 d . . . . .
N16 N 0.2291(2) 0.8339(5) 0.98615(18) 0.0612(17) Uani 1 1 d . . . . .
N17 N 0.2769(2) 0.7856(5) 1.00025(17) 0.0586(16) Uani 1 1 d . . . . .
N18 N 0.3729(2) 0.7211(5) 1.03406(16) 0.0570(17) Uani 1 1 d . . . . .
N19 N 0.4098(2) 0.6574(5) 0.98769(16) 0.0561(16) Uani 1 1 d . . . . .
N20 N 0.4391(2) 0.6324(4) 0.96918(16) 0.0535(16) Uani 1 1 d . . . . .
H20B H 0.4259 0.6249 0.9462 0.064 Uiso 1 1 calc R U . . .
C81 C 0.0420(3) 0.8592(6) 0.6890(2) 0.064(2) Uani 1 1 d . . . . .
H81A H 0.0718 0.8345 0.7081 0.077 Uiso 1 1 calc R U . . .
C82 C 0.0457(3) 0.8692(7) 0.6570(2) 0.073(3) Uani 1 1 d . . . . .
H82A H 0.0754 0.8425 0.6534 0.088 Uiso 1 1 calc R U . . .
C83 C 0.0061(3) 0.9187(9) 0.6290(3) 0.084(3) Uani 1 1 d . . . . .
C84 C 0.0099(4) 0.9405(10) 0.5961(3) 0.103(4) Uani 1 1 d . . . . .
H84A H 0.0400 0.9187 0.5918 0.124 Uiso 1 1 calc R U . . .
C85 C -0.0285(4) 0.9916(11) 0.5706(3) 0.109(4) Uani 1 1 d . . . . .
H85A H -0.0245 1.0075 0.5492 0.131 Uiso 1 1 calc R U . . .
C86 C -0.0734(4) 1.0202(10) 0.5765(3) 0.096(4) Uani 1 1 d . . . . .
H86A H -0.1010 1.0531 0.5583 0.116 Uiso 1 1 calc R U . . .
C87 C -0.0796(4) 1.0023(9) 0.6081(3) 0.088(3) Uani 1 1 d . . . . .
H87A H -0.1104 1.0242 0.6116 0.106 Uiso 1 1 calc R U . . .
C88 C -0.0392(3) 0.9509(7) 0.6352(2) 0.070(2) Uani 1 1 d . . . . .
C89 C -0.0431(3) 0.9331(7) 0.6677(2) 0.071(2) Uani 1 1 d . . . . .
H89A H -0.0737 0.9553 0.6713 0.085 Uiso 1 1 calc R U . . .
C90 C -0.0035(3) 0.8835(6) 0.6951(2) 0.063(2) Uani 1 1 d . . . . .
C91 C -0.0063(3) 0.8746(6) 0.7297(2) 0.0552(19) Uani 1 1 d . . . . .
C92 C -0.0474(3) 0.8806(6) 0.7421(2) 0.0570(19) Uani 1 1 d . . . . .
H92A H -0.0840 0.8913 0.7283 0.068 Uiso 1 1 calc R U . . .
C93 C -0.0251(3) 0.8680(5) 0.7782(2) 0.0537(18) Uani 1 1 d . . . . .
C94 C -0.0462(3) 0.8671(6) 0.8054(2) 0.0558(19) Uani 1 1 d . . . . .
C95 C -0.0996(3) 0.8831(7) 0.8005(2) 0.070(2) Uani 1 1 d . . . . .
H95A H -0.1253 0.8990 0.7779 0.084 Uiso 1 1 calc R U . . .
C96 C -0.1140(3) 0.8751(8) 0.8293(3) 0.083(3) Uani 1 1 d . . . . .
H96A H -0.1501 0.8855 0.8262 0.100 Uiso 1 1 calc R U . . .
C97 C -0.0779(3) 0.8528(8) 0.8616(2) 0.078(3) Uani 1 1 d . . . . .
H97A H -0.0879 0.8490 0.8814 0.094 Uiso 1 1 calc R U . . .
C98 C -0.0248(3) 0.8354(6) 0.8653(2) 0.061(2) Uani 1 1 d . . . . .
C99 C 0.0190(3) 0.8090(6) 0.8983(2) 0.0585(19) Uani 1 1 d . . . . .
C100 C 0.0205(3) 0.7794(7) 0.9305(2) 0.071(2) Uani 1 1 d . . . . .
H10B H -0.0087 0.7742 0.9378 0.085 Uiso 1 1 calc R U . . .
C101 C 0.0736(3) 0.7587(6) 0.9503(2) 0.060(2) Uani 1 1 d . . . . .
C102 C 0.0968(3) 0.7238(7) 0.9867(2) 0.069(2) Uani 1 1 d . . . . .
C103 C 0.1439(3) 0.6811(7) 1.0004(2) 0.071(2) Uani 1 1 d . . . . .
H10C H 0.1639 0.6727 0.9860 0.085 Uiso 1 1 calc R U . . .
C104 C 0.1661(3) 0.6469(7) 1.0361(2) 0.072(2) Uani 1 1 d . . . . .
C105 C 0.2164(5) 0.6126(10) 1.0509(3) 0.107(3) Uani 1 1 d . U . . .
H10D H 0.2382 0.6090 1.0375 0.129 Uiso 1 1 calc R U . . .
C106 C 0.2358(5) 0.5828(10) 1.0856(3) 0.110(3) Uani 1 1 d . U . . .
H10E H 0.2712 0.5591 1.0960 0.132 Uiso 1 1 calc R U . . .
C107 C 0.2040(5) 0.5869(10) 1.1060(3) 0.106(3) Uani 1 1 d . U . . .
H10F H 0.2171 0.5623 1.1293 0.127 Uiso 1 1 calc R U . . .
C108 C 0.1566(4) 0.6246(8) 1.0927(3) 0.085(3) Uani 1 1 d . . . . .
H10G H 0.1360 0.6300 1.1068 0.102 Uiso 1 1 calc R U . . .
C109 C 0.1349(3) 0.6586(7) 1.0563(2) 0.071(2) Uani 1 1 d . . . . .
C110 C 0.0862(4) 0.7037(10) 1.0422(3) 0.104(4) Uani 1 1 d . . . . .
H11A H 0.0652 0.7123 1.0559 0.125 Uiso 1 1 calc R U . . .
C111 C 0.0687(4) 0.7351(9) 1.0089(3) 0.091(3) Uani 1 1 d . U . . .
H11B H 0.0353 0.7670 0.9998 0.109 Uiso 1 1 calc R U . . .
C112 C 0.1390(3) 0.6811(7) 0.8521(2) 0.059(2) Uani 1 1 d . . . . .
C113 C 0.1771(4) 0.6016(8) 0.8530(3) 0.084(3) Uani 1 1 d . . . . .
C114 C 0.1502(3) 0.9887(6) 0.8819(2) 0.069(2) Uani 1 1 d . . . . .
C115 C 0.1714(5) 1.0933(8) 0.8824(3) 0.112(4) Uani 1 1 d . U . . .
C116 C 0.2360(3) 0.5767(6) 0.9512(2) 0.058(2) Uani 1 1 d . . . . .
C117 C 0.2191(4) 0.4731(7) 0.9533(3) 0.094(4) Uani 1 1 d . U . . .
C118 C 0.3069(3) 0.8562(6) 0.92884(18) 0.0503(17) Uani 1 1 d . . . . .
C119 C 0.3000(3) 0.9457(6) 0.9064(2) 0.062(2) Uani 1 1 d . . . . .
C121 C 0.1499(4) 0.9893(9) 0.9763(3) 0.104(3) Uani 1 1 d . U . . .
H121 H 0.1566 0.9689 0.9563 0.125 Uiso 1 1 calc R U . A 1
C122 C 0.1187(6) 1.0684(16) 0.9729(6) 0.103(3) Uani 0.532(8) 1 d . U P B 1
C123 C 0.1017(7) 1.1356(16) 0.9452(5) 0.098(3) Uani 0.532(8) 1 d . U P B 1
H12E H 0.1119 1.1239 0.9259 0.118 Uiso 0.532(8) 1 calc R U P B 1
C124 C 0.0704(7) 1.2198(18) 0.9433(5) 0.096(4) Uani 0.532(8) 1 d . U P B 1
H12B H 0.0635 1.2667 0.9253 0.115 Uiso 0.532(8) 1 calc R U P B 1
C125 C 0.0507(8) 1.2271(18) 0.9706(5) 0.101(4) Uani 0.532(8) 1 d . U P B 1
H12C H 0.0254 1.2755 0.9693 0.121 Uiso 0.532(8) 1 calc R U P B 1
C126 C 0.0677(8) 1.1642(19) 0.9994(6) 0.107(3) Uani 0.532(8) 1 d . U P B 1
H12F H 0.0548 1.1744 1.0176 0.129 Uiso 0.532(8) 1 calc R U P B 1
C127 C 0.1033(9) 1.086(2) 1.0030(6) 0.106(3) Uani 0.532(8) 1 d . U P B 1
C222 C 0.0958(10) 1.0291(15) 0.9695(7) 0.108(3) Uani 0.468(8) 1 d . U P B 2
H222 H 0.0761 1.0548 0.9468 0.129 Uiso 0.468(8) 1 calc R U P B 2
C223 C 0.0728(10) 1.0306(14) 0.9943(6) 0.110(3) Uani 0.468(8) 1 d . U P B 2
C224 C 0.0201(10) 1.073(2) 0.9865(7) 0.113(4) Uani 0.468(8) 1 d . U P B 2
H22E H -0.0001 1.1023 0.9646 0.136 Uiso 0.468(8) 1 calc R U P B 2
C225 C 0.0035(11) 1.066(2) 1.0122(7) 0.115(4) Uani 0.468(8) 1 d . U P B 2
H22A H -0.0317 1.0856 1.0082 0.138 Uiso 0.468(8) 1 calc R U P B 2
C226 C 0.0327(11) 1.032(2) 1.0431(7) 0.118(5) Uani 0.468(8) 1 d . U P B 2
H22B H 0.0173 1.0348 1.0604 0.141 Uiso 0.468(8) 1 calc R U P B 2
C227 C 0.0783(11) 0.998(2) 1.0531(7) 0.115(4) Uani 0.468(8) 1 d . U P B 2
H227 H 0.0933 0.9660 1.0751 0.138 Uiso 0.468(8) 1 calc R U P B 2
C128 C 0.1100(5) 1.0073(11) 1.0296(3) 0.118(3) Uani 1 1 d . U . . .
H128 H 0.0871 0.9989 1.0420 0.142 Uiso 0.532(8) 1 calc R U P B 1
C129 C 0.1548(5) 0.9464(10) 1.0343(3) 0.106(3) Uani 1 1 d . U . . .
H12D H 0.1720 0.9133 1.0559 0.127 Uiso 1 1 calc R U . . .
C130 C 0.1727(4) 0.9361(8) 1.0074(2) 0.080(3) Uani 1 1 d . . . . .
C131 C 0.2194(3) 0.8741(7) 1.0132(2) 0.069(2) Uani 1 1 d . . . . .
C132 C 0.2600(3) 0.8508(7) 1.0450(2) 0.069(2) Uani 1 1 d . . . . .
H13A H 0.2629 0.8680 1.0681 0.083 Uiso 1 1 calc R U . . .
C133 C 0.2957(3) 0.7960(6) 1.0354(2) 0.063(2) Uani 1 1 d . . . . .
C134 C 0.3483(3) 0.7544(6) 1.0549(2) 0.060(2) Uani 1 1 d . . . . .
C135 C 0.3733(4) 0.7527(8) 1.0908(2) 0.076(3) Uani 1 1 d . . . . .
H13B H 0.3557 0.7745 1.1055 0.091 Uiso 1 1 calc R U . . .
C136 C 0.4252(4) 0.7184(8) 1.1052(2) 0.081(3) Uani 1 1 d . . . . .
H13C H 0.4433 0.7166 1.1301 0.098 Uiso 1 1 calc R U . . .
C137 C 0.4507(4) 0.6871(7) 1.0841(2) 0.078(3) Uani 1 1 d . . . . .
H13D H 0.4864 0.6649 1.0940 0.094 Uiso 1 1 calc R U . . .
C138 C 0.4230(3) 0.6887(6) 1.0479(2) 0.060(2) Uani 1 1 d . . . . .
C139 C 0.4445(3) 0.6590(5) 1.0220(2) 0.056(2) Uani 1 1 d . . . . .
C140 C 0.4953(3) 0.6361(5) 1.0240(2) 0.060(2) Uani 1 1 d . . . . .
H14A H 0.5266 0.6323 1.0448 0.072 Uiso 1 1 calc R U . . .
C141 C 0.4917(3) 0.6198(5) 0.9897(2) 0.055(2) Uani 1 1 d . . . . .
C142 C 0.5313(3) 0.5963(5) 0.9753(2) 0.061(2) Uani 1 1 d . . . . .
C143 C 0.5189(3) 0.5816(6) 0.9401(2) 0.064(2) Uani 1 1 d . . . . .
H14B H 0.4826 0.5860 0.9246 0.077 Uiso 1 1 calc R U . . .
C144 C 0.5565(4) 0.5606(7) 0.9254(3) 0.078(3) Uani 1 1 d . . . . .
C145 C 0.5455(4) 0.5478(8) 0.8900(3) 0.094(3) Uani 1 1 d . . . . .
H14C H 0.5091 0.5512 0.8745 0.112 Uiso 1 1 calc R U . . .
C146 C 0.5813(6) 0.5310(12) 0.8752(4) 0.133(4) Uani 1 1 d . U . . .
H14D H 0.5714 0.5282 0.8504 0.160 Uiso 1 1 calc R U . . .
C147 C 0.6357(6) 0.5173(13) 0.8994(5) 0.144(4) Uani 1 1 d . U . . .
H14E H 0.6625 0.5010 0.8908 0.173 Uiso 1 1 calc R U . . .
C148 C 0.6484(5) 0.5281(12) 0.9350(4) 0.143(5) Uani 1 1 d . U . . .
H14F H 0.6845 0.5197 0.9504 0.171 Uiso 1 1 calc R U . . .
C149 C 0.6114(4) 0.5505(9) 0.9496(4) 0.105(4) Uani 1 1 d . . . . .
C150 C 0.6232(4) 0.5630(8) 0.9852(3) 0.096(4) Uani 1 1 d . . . . .
H15B H 0.6590 0.5548 1.0012 0.115 Uiso 1 1 calc R U . . .
C151 C 0.5854(3) 0.5865(6) 0.9982(3) 0.074(3) Uani 1 1 d . . . . .
H15C H 0.5955 0.5965 1.0228 0.089 Uiso 1 1 calc R U . . .
O1S O 0.3995(6) 0.4530(11) 0.8361(5) 0.222(5) Uani 1 1 d . U . . .
C1S C 0.4101(10) 0.3966(17) 0.8118(8) 0.227(6) Uani 1 1 d . U . . .
H1SA H 0.4424 0.4222 0.8093 0.272 Uiso 1 1 calc R U . . .
H1SB H 0.3802 0.4043 0.7888 0.272 Uiso 1 1 calc R U . . .
C2S C 0.4182(10) 0.2918(16) 0.8194(8) 0.237(6) Uani 1 1 d . U . . .
H2SA H 0.4560 0.2723 0.8271 0.284 Uiso 1 1 calc R U . . .
H2SB H 0.3957 0.2514 0.7994 0.284 Uiso 1 1 calc R U . . .
C3S C 0.3967(9) 0.2935(16) 0.8524(7) 0.226(6) Uani 1 1 d . U . . .
H3SA H 0.3576 0.2848 0.8434 0.272 Uiso 1 1 calc R U . . .
H3SB H 0.4137 0.2417 0.8695 0.272 Uiso 1 1 calc R U . . .
C4S C 0.4124(8) 0.3934(14) 0.8701(7) 0.211(6) Uani 1 1 d . U . . .
H4SA H 0.3902 0.4123 0.8834 0.253 Uiso 1 1 calc R U . . .
H4SB H 0.4506 0.3968 0.8856 0.253 Uiso 1 1 calc R U . . .
O2S O 0.3187(5) 0.1190(9) 0.9802(4) 0.188(4) Uani 1 1 d . U . . .
C5S C 0.2974(8) 0.2008(14) 0.9725(7) 0.193(5) Uani 1 1 d . U . . .
H5SA H 0.2678 0.2012 0.9491 0.231 Uiso 1 1 calc R U . . .
H5SB H 0.3236 0.2511 0.9733 0.231 Uiso 1 1 calc R U . . .
C6S C 0.2756(8) 0.2125(13) 1.0051(6) 0.193(5) Uani 1 1 d . U . . .
H6SA H 0.2993 0.2554 1.0237 0.231 Uiso 1 1 calc R U . . .
H6SB H 0.2390 0.2392 0.9962 0.231 Uiso 1 1 calc R U . . .
C7S C 0.2763(8) 0.1159(13) 1.0186(6) 0.187(5) Uani 1 1 d . U . . .
H7SA H 0.2409 0.0969 1.0181 0.224 Uiso 1 1 calc R U . . .
H7SB H 0.3031 0.1095 1.0429 0.224 Uiso 1 1 calc R U . . .
C8S C 0.2927(7) 0.0541(13) 0.9910(6) 0.180(5) Uani 1 1 d . U . . .
H8SA H 0.3159 -0.0007 1.0027 0.216 Uiso 1 1 calc R U . . .
H8SB H 0.2609 0.0302 0.9713 0.216 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 2.064(5) . ?
Mn1 N4 2.200(6) . ?
Mn1 O1 2.209(5) . ?
Mn1 N3 2.239(6) . ?
Mn1 N2 2.282(5) . ?
Mn1 O2 2.404(5) . ?
Mn2 O5 2.162(6) . ?
Mn2 O4 2.185(5) . ?
Mn2 O2 2.224(5) . ?
Mn2 O7 2.233(4) . ?
Mn2 N6 2.257(6) . ?
Mn2 N5 2.263(6) . ?
Mn3 O6 2.087(5) . ?
Mn3 N7 2.171(6) . ?
Mn3 N8 2.251(5) . ?
Mn3 O8 2.253(5) . ?
Mn3 N9 2.274(6) . ?
Mn3 O7 2.280(4) . ?
Mn3 C38 2.632(7) . ?
O1 C32 1.259(8) . ?
O2 C32 1.252(9) . ?
O3 C34 1.266(8) . ?
O4 C34 1.249(8) . ?
O5 C36 1.245(11) . ?
O6 C36 1.281(10) . ?
O7 C38 1.254(8) . ?
O8 C38 1.281(8) . ?
N1 N2 1.347(8) . ?
N1 C11 1.372(8) . ?
N1 H1B 0.8800 . ?
N2 C13 1.338(8) . ?
N3 C18 1.345(9) . ?
N3 C14 1.348(9) . ?
N4 C19 1.341(9) . ?
N4 N5 1.365(8) . ?
N5 C21 1.367(10) . ?
N6 N7 1.360(8) . ?
N6 C51 1.372(9) . ?
N7 C53 1.375(9) . ?
N8 C54 1.328(9) . ?
N8 C58 1.352(8) . ?
N9 N10 1.336(8) . ?
N9 C59 1.350(8) . ?
N10 C61 1.354(8) . ?
N10 H10A 0.8800 . ?
C1 C2 1.365(11) . ?
C1 C10 1.429(9) . ?
C1 H1A 0.9500 . ?
C2 C3 1.402(12) . ?
C2 H2A 0.9500 . ?
C3 C8 1.427(10) . ?
C3 C4 1.446(11) . ?
C4 C5 1.346(14) . ?
C4 H4A 0.9500 . ?
C5 C6 1.410(13) . ?
C5 H5A 0.9500 . ?
C6 C7 1.358(11) . ?
C6 H6A 0.9500 . ?
C7 C8 1.380(12) . ?
C7 H7A 0.9500 . ?
C8 C9 1.424(10) . ?
C9 C10 1.362(10) . ?
C9 H9A 0.9500 . ?
C10 C11 1.467(10) . ?
C11 C12 1.371(10) . ?
C12 C13 1.389(9) . ?
C12 H12A 0.9500 . ?
C13 C14 1.460(10) . ?
C14 C15 1.400(11) . ?
C15 C16 1.360(13) . ?
C15 H15A 0.9500 . ?
C16 C17 1.382(13) . ?
C16 H16A 0.9500 . ?
C17 C18 1.390(11) . ?
C17 H17A 0.9500 . ?
C18 C19 1.471(10) . ?
C19 C20 1.368(11) . ?
C20 C21 1.392(11) . ?
C20 H20A 0.9500 . ?
C21 C22 1.481(11) . ?
C22 C23 1.320(13) . ?
C22 C31 1.421(12) . ?
C23 C24 1.483(13) . ?
C23 H23A 0.9500 . ?
C24 C25 1.358(14) . ?
C24 C29 1.398(13) . ?
C25 C26 1.370(15) . ?
C25 H25A 0.9500 . ?
C26 C27 1.437(16) . ?
C26 H26A 0.9500 . ?
C27 C28 1.348(15) . ?
C27 H27A 0.9500 . ?
C28 C29 1.476(14) . ?
C28 H28A 0.9500 . ?
C29 C30 1.351(14) . ?
C30 C31 1.358(12) . ?
C30 H30A 0.9500 . ?
C31 H31A 0.9500 . ?
C32 C33 1.530(11) . ?
C34 C35 1.525(11) . ?
C36 C37 1.552(14) . ?
C38 C39 1.514(10) . ?
C41 C42 1.350(10) . ?
C41 C50 1.420(10) . ?
C41 H41A 0.9500 . ?
C42 C43 1.405(10) . ?
C42 H42A 0.9500 . ?
C43 C48 1.405(10) . ?
C43 C44 1.429(10) . ?
C44 C45 1.364(11) . ?
C44 H44A 0.9500 . ?
C45 C46 1.394(11) . ?
C45 H45A 0.9500 . ?
C46 C47 1.367(11) . ?
C46 H46A 0.9500 . ?
C47 C48 1.417(10) . ?
C47 H47A 0.9500 . ?
C48 C49 1.393(10) . ?
C49 C50 1.384(10) . ?
C49 H49A 0.9500 . ?
C50 C51 1.445(10) . ?
C51 C52 1.404(10) . ?
C52 C53 1.377(11) . ?
C52 H52A 0.9500 . ?
C53 C54 1.474(10) . ?
C54 C55 1.385(10) . ?
C55 C56 1.389(12) . ?
C55 H55A 0.9500 . ?
C56 C57 1.394(13) . ?
C56 H56A 0.9500 . ?
C57 C58 1.380(10) . ?
C57 H57A 0.9500 . ?
C58 C59 1.465(11) . ?
C59 C60 1.394(10) . ?
C60 C61 1.372(11) . ?
C60 H60A 0.9500 . ?
C61 C62 1.481(11) . ?
C62 C63 1.315(12) . ?
C62 C71 1.393(15) . ?
C63 C64 1.388(12) . ?
C63 H63A 0.9500 . ?
C64 C65 1.358(14) . ?
C64 C69 1.415(17) . ?
C65 C66 1.380(15) . ?
C65 H65A 0.9500 . ?
C66 C67 1.365(18) . ?
C66 H66A 0.9500 . ?
C67 C68 1.330(19) . ?
C67 H67A 0.9500 . ?
C68 C69 1.420(18) . ?
C68 H68A 0.9500 . ?
C69 C70 1.413(19) . ?
C70 C71 1.364(17) . ?
C70 H70A 0.9500 . ?
C71 H71A 0.9500 . ?
Mn4 O11 2.077(6) . ?
Mn4 N14 2.184(6) . ?
Mn4 N13 2.233(6) . ?
Mn4 O9 2.266(6) . ?
Mn4 O10 2.281(5) . ?
Mn4 N12 2.284(6) . ?
Mn5 O13 2.168(6) . ?
Mn5 O12 2.180(6) . ?
Mn5 N16 2.228(7) . ?
Mn5 O10 2.245(5) . ?
Mn5 O15 2.288(5) . ?
Mn5 N15 2.300(6) . ?
Mn6 O14 2.066(5) . ?
Mn6 N17 2.190(7) . ?
Mn6 O16 2.202(5) . ?
Mn6 N18 2.244(6) . ?
Mn6 N19 2.276(6) . ?
Mn6 O15 2.357(4) . ?
Mn6 C118 2.632(7) . ?
O9 C112 1.271(8) . ?
O10 C112 1.246(10) . ?
O11 C114 1.247(9) . ?
O12 C114 1.257(9) . ?
O13 C116 1.238(9) . ?
O14 C116 1.285(8) . ?
O15 C118 1.265(8) . ?
O16 C118 1.272(7) . ?
N11 N12 1.332(8) . ?
N11 C91 1.371(8) . ?
N11 H11C 0.8800 . ?
N12 C93 1.358(8) . ?
N13 C98 1.334(10) . ?
N13 C94 1.352(9) . ?
N14 C99 1.331(9) . ?
N14 N15 1.374(8) . ?
N15 C101 1.365(10) . ?
N16 C131 1.357(11) . ?
N16 N17 1.379(9) . ?
N17 C133 1.344(10) . ?
N18 C138 1.335(10) . ?
N18 C134 1.352(10) . ?
N19 N20 1.339(9) . ?
N19 C139 1.364(9) . ?
N20 C141 1.365(8) . ?
N20 H20B 0.8800 . ?
C81 C82 1.365(12) . ?
C81 C90 1.390(11) . ?
C81 H81A 0.9500 . ?
C82 C83 1.419(12) . ?
C82 H82A 0.9500 . ?
C83 C88 1.421(12) . ?
C83 C84 1.426(14) . ?
C84 C85 1.363(15) . ?
C84 H84A 0.9500 . ?
C85 C86 1.391(14) . ?
C85 H85A 0.9500 . ?
C86 C87 1.394(14) . ?
C86 H86A 0.9500 . ?
C87 C88 1.423(12) . ?
C87 H87A 0.9500 . ?
C88 C89 1.398(13) . ?
C89 C90 1.407(11) . ?
C89 H89A 0.9500 . ?
C90 C91 1.456(11) . ?
C91 C92 1.396(11) . ?
C92 C93 1.381(11) . ?
C92 H92A 0.9500 . ?
C93 C94 1.436(11) . ?
C94 C95 1.404(10) . ?
C95 C96 1.382(13) . ?
C95 H95A 0.9500 . ?
C96 C97 1.354(12) . ?
C96 H96A 0.9500 . ?
C97 C98 1.412(11) . ?
C97 H97A 0.9500 . ?
C98 C99 1.468(10) . ?
C99 C100 1.369(12) . ?
C100 C101 1.390(11) . ?
C100 H10B 0.9500 . ?
C101 C102 1.468(12) . ?
C102 C103 1.326(12) . ?
C102 C111 1.403(13) . ?
C103 C104 1.437(12) . ?
C103 H10C 0.9500 . ?
C104 C105 1.356(13) . ?
C104 C109 1.402(12) . ?
C105 C106 1.381(15) . ?
C105 H10D 0.9500 . ?
C106 C107 1.415(16) . ?
C106 H10E 0.9500 . ?
C107 C108 1.301(14) . ?
C107 H10F 0.9500 . ?
C108 C109 1.461(13) . ?
C108 H10G 0.9500 . ?
C109 C110 1.377(13) . ?
C110 C111 1.338(14) . ?
C110 H11A 0.9500 . ?
C111 H11B 0.9500 . ?
C112 C113 1.507(12) . ?
C114 C115 1.564(14) . ?
C116 C117 1.525(12) . ?
C118 C119 1.520(10) . ?
C121 C122 1.36(3) . ?
C121 C130 1.401(14) . ?
C121 C222 1.49(3) . ?
C121 H121 0.9500 . ?
C122 C123 1.41(3) . ?
C122 C127 1.47(3) . ?
C123 C124 1.43(3) . ?
C123 H12E 0.9500 . ?
C124 C125 1.42(3) . ?
C124 H12B 0.9500 . ?
C125 C126 1.40(3) . ?
C125 H12C 0.9500 . ?
C126 C127 1.43(3) . ?
C126 H12F 0.9500 . ?
C127 C128 1.50(3) . ?
C222 C223 1.38(3) . ?
C222 H222 0.9500 . ?
C223 C224 1.46(3) . ?
C224 C225 1.30(3) . ?
C224 C225 2.03(4) 3_577 ?
C224 H22E 0.9500 . ?
C225 C226 1.30(3) . ?
C225 C224 2.03(4) 3_577 ?
C225 H22A 0.9500 . ?
C226 C227 1.24(3) . ?
C226 H22B 0.9500 . ?
C227 C128 1.52(3) . ?
C227 H227 0.9500 . ?
C128 C129 1.433(16) . ?
C128 H128 0.9500 . ?
C129 C130 1.371(14) . ?
C129 H12D 0.9500 . ?
C130 C131 1.477(13) . ?
C131 C132 1.389(12) . ?
C132 C133 1.402(13) . ?
C132 H13A 0.9500 . ?
C133 C134 1.465(11) . ?
C134 C135 1.369(11) . ?
C135 C136 1.388(13) . ?
C135 H13B 0.9500 . ?
C136 C137 1.371(14) . ?
C136 H13C 0.9500 . ?
C137 C138 1.385(11) . ?
C137 H13D 0.9500 . ?
C138 C139 1.455(12) . ?
C139 C140 1.389(11) . ?
C140 C141 1.390(12) . ?
C140 H14A 0.9500 . ?
C141 C142 1.448(12) . ?
C142 C143 1.372(12) . ?
C142 C151 1.418(10) . ?
C143 C144 1.398(13) . ?
C143 H14B 0.9500 . ?
C144 C145 1.380(15) . ?
C144 C149 1.450(13) . ?
C145 C146 1.349(16) . ?
C145 H14C 0.9500 . ?
C146 C147 1.445(19) . ?
C146 H14D 0.9500 . ?
C147 C148 1.37(2) . ?
C147 H14E 0.9500 . ?
C148 C149 1.389(17) . ?
C148 H14F 0.9500 . ?
C149 C150 1.382(16) . ?
C150 C151 1.365(15) . ?
C150 H15B 0.9500 . ?
C151 H15C 0.9500 . ?
O1S C1S 1.38(3) . ?
O1S C4S 1.54(3) . ?
C1S C2S 1.49(3) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.67(3) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S C4S 1.55(3) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
O2S C5S 1.26(2) . ?
O2S C8S 1.323(19) . ?
C5S C6S 1.67(3) . ?
C5S H5SA 0.9900 . ?
C5S H5SB 0.9900 . ?
C6S C7S 1.45(2) . ?
C6S H6SA 0.9900 . ?
C6S H6SB 0.9900 . ?
C7S C8S 1.61(3) . ?
C7S H7SA 0.9900 . ?
C7S H7SB 0.9900 . ?
C8S H8SA 0.9900 . ?
C8S H8SB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 N4 102.5(2) . . ?
O3 Mn1 O1 130.7(2) . . ?
N4 Mn1 O1 107.5(2) . . ?
O3 Mn1 N3 113.1(2) . . ?
N4 Mn1 N3 72.0(2) . . ?
O1 Mn1 N3 112.9(2) . . ?
O3 Mn1 N2 94.7(2) . . ?
N4 Mn1 N2 142.2(2) . . ?
O1 Mn1 N2 84.84(18) . . ?
N3 Mn1 N2 70.3(2) . . ?
O3 Mn1 O2 92.79(18) . . ?
N4 Mn1 O2 80.8(2) . . ?
O1 Mn1 O2 55.78(16) . . ?
N3 Mn1 O2 145.6(2) . . ?
N2 Mn1 O2 132.16(19) . . ?
O5 Mn2 O4 168.7(2) . . ?
O5 Mn2 O2 88.7(2) . . ?
O4 Mn2 O2 85.29(18) . . ?
O5 Mn2 O7 84.4(2) . . ?
O4 Mn2 O7 85.59(17) . . ?
O2 Mn2 O7 85.46(17) . . ?
O5 Mn2 N6 94.5(2) . . ?
O4 Mn2 N6 90.5(2) . . ?
O2 Mn2 N6 173.1(2) . . ?
O7 Mn2 N6 88.85(18) . . ?
O5 Mn2 N5 93.5(2) . . ?
O4 Mn2 N5 95.8(2) . . ?
O2 Mn2 N5 87.8(2) . . ?
O7 Mn2 N5 173.0(2) . . ?
N6 Mn2 N5 98.0(2) . . ?
O6 Mn3 N7 101.2(2) . . ?
O6 Mn3 N8 108.5(2) . . ?
N7 Mn3 N8 72.3(2) . . ?
O6 Mn3 O8 139.0(2) . . ?
N7 Mn3 O8 101.8(2) . . ?
N8 Mn3 O8 110.6(2) . . ?
O6 Mn3 N9 96.4(2) . . ?
N7 Mn3 N9 142.7(2) . . ?
N8 Mn3 N9 71.1(2) . . ?
O8 Mn3 N9 85.1(2) . . ?
O6 Mn3 O7 91.84(18) . . ?
N7 Mn3 O7 84.16(18) . . ?
N8 Mn3 O7 151.2(2) . . ?
O8 Mn3 O7 57.55(17) . . ?
N9 Mn3 O7 128.00(19) . . ?
O6 Mn3 C38 116.1(2) . . ?
N7 Mn3 C38 93.8(2) . . ?
N8 Mn3 C38 135.1(2) . . ?
O8 Mn3 C38 29.1(2) . . ?
N9 Mn3 C38 107.5(2) . . ?
O7 Mn3 C38 28.45(18) . . ?
C32 O1 Mn1 97.0(4) . . ?
C32 O2 Mn2 151.7(5) . . ?
C32 O2 Mn1 88.0(4) . . ?
Mn2 O2 Mn1 105.1(2) . . ?
C34 O3 Mn1 126.5(5) . . ?
C34 O4 Mn2 147.2(4) . . ?
C36 O5 Mn2 145.6(5) . . ?
C36 O6 Mn3 123.4(6) . . ?
C38 O7 Mn2 138.7(4) . . ?
C38 O7 Mn3 91.6(4) . . ?
Mn2 O7 Mn3 106.12(18) . . ?
C38 O8 Mn3 92.1(4) . . ?
N2 N1 C11 111.5(5) . . ?
N2 N1 H1B 124.3 . . ?
C11 N1 H1B 124.3 . . ?
C13 N2 N1 105.4(5) . . ?
C13 N2 Mn1 117.8(4) . . ?
N1 N2 Mn1 135.9(4) . . ?
C18 N3 C14 119.7(6) . . ?
C18 N3 Mn1 118.9(4) . . ?
C14 N3 Mn1 121.3(5) . . ?
C19 N4 N5 107.5(6) . . ?
C19 N4 Mn1 118.4(5) . . ?
N5 N4 Mn1 133.9(5) . . ?
N4 N5 C21 107.2(6) . . ?
N4 N5 Mn2 108.0(4) . . ?
C21 N5 Mn2 142.0(5) . . ?
N7 N6 C51 109.5(5) . . ?
N7 N6 Mn2 106.3(4) . . ?
C51 N6 Mn2 142.2(4) . . ?
N6 N7 C53 106.7(6) . . ?
N6 N7 Mn3 133.1(4) . . ?
C53 N7 Mn3 119.2(4) . . ?
C54 N8 C58 121.2(6) . . ?
C54 N8 Mn3 118.7(4) . . ?
C58 N8 Mn3 120.1(5) . . ?
N10 N9 C59 104.9(5) . . ?
N10 N9 Mn3 137.7(4) . . ?
C59 N9 Mn3 117.3(5) . . ?
N9 N10 C61 112.8(6) . . ?
N9 N10 H10A 123.6 . . ?
C61 N10 H10A 123.6 . . ?
C2 C1 C10 119.2(8) . . ?
C2 C1 H1A 120.4 . . ?
C10 C1 H1A 120.4 . . ?
C1 C2 C3 122.2(7) . . ?
C1 C2 H2A 118.9 . . ?
C3 C2 H2A 118.9 . . ?
C2 C3 C8 119.4(7) . . ?
C2 C3 C4 124.0(7) . . ?
C8 C3 C4 116.6(8) . . ?
C5 C4 C3 121.1(8) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 120.8(8) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C7 C6 C5 119.5(9) . . ?
C7 C6 H6A 120.2 . . ?
C5 C6 H6A 120.2 . . ?
C6 C7 C8 121.8(8) . . ?
C6 C7 H7A 119.1 . . ?
C8 C7 H7A 119.1 . . ?
C7 C8 C9 122.8(7) . . ?
C7 C8 C3 120.2(7) . . ?
C9 C8 C3 117.0(7) . . ?
C10 C9 C8 122.7(6) . . ?
C10 C9 H9A 118.6 . . ?
C8 C9 H9A 118.6 . . ?
C9 C10 C1 119.4(7) . . ?
C9 C10 C11 122.5(6) . . ?
C1 C10 C11 118.1(7) . . ?
C12 C11 N1 106.1(6) . . ?
C12 C11 C10 132.5(6) . . ?
N1 C11 C10 121.5(6) . . ?
C11 C12 C13 106.1(6) . . ?
C11 C12 H12A 127.0 . . ?
C13 C12 H12A 126.9 . . ?
N2 C13 C12 110.9(6) . . ?
N2 C13 C14 116.9(6) . . ?
C12 C13 C14 132.2(6) . . ?
N3 C14 C15 120.8(7) . . ?
N3 C14 C13 113.1(6) . . ?
C15 C14 C13 126.0(7) . . ?
C16 C15 C14 119.1(8) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
C15 C16 C17 120.2(8) . . ?
C15 C16 H16A 119.9 . . ?
C17 C16 H16A 119.9 . . ?
C16 C17 C18 118.6(8) . . ?
C16 C17 H17A 120.7 . . ?
C18 C17 H17A 120.7 . . ?
N3 C18 C17 121.4(7) . . ?
N3 C18 C19 113.0(6) . . ?
C17 C18 C19 125.6(7) . . ?
N4 C19 C20 111.7(7) . . ?
N4 C19 C18 117.0(7) . . ?
C20 C19 C18 131.4(7) . . ?
C19 C20 C21 103.8(7) . . ?
C19 C20 H20A 128.1 . . ?
C21 C20 H20A 128.1 . . ?
N5 C21 C20 109.8(7) . . ?
N5 C21 C22 124.6(7) . . ?
C20 C21 C22 125.5(7) . . ?
C23 C22 C31 118.0(8) . . ?
C23 C22 C21 122.2(9) . . ?
C31 C22 C21 119.9(8) . . ?
C22 C23 C24 120.5(10) . . ?
C22 C23 H23A 119.7 . . ?
C24 C23 H23A 119.7 . . ?
C25 C24 C29 120.9(10) . . ?
C25 C24 C23 121.2(9) . . ?
C29 C24 C23 117.4(9) . . ?
C24 C25 C26 119.6(12) . . ?
C24 C25 H25A 120.2 . . ?
C26 C25 H25A 120.2 . . ?
C25 C26 C27 122.2(12) . . ?
C25 C26 H26A 118.9 . . ?
C27 C26 H26A 118.9 . . ?
C28 C27 C26 119.1(11) . . ?
C28 C27 H27A 120.5 . . ?
C26 C27 H27A 120.5 . . ?
C27 C28 C29 118.5(11) . . ?
C27 C28 H28A 120.7 . . ?
C29 C28 H28A 120.7 . . ?
C30 C29 C24 121.4(9) . . ?
C30 C29 C28 119.1(10) . . ?
C24 C29 C28 119.4(9) . . ?
C29 C30 C31 119.1(10) . . ?
C29 C30 H30A 120.5 . . ?
C31 C30 H30A 120.5 . . ?
C30 C31 C22 123.5(10) . . ?
C30 C31 H31A 118.2 . . ?
C22 C31 H31A 118.2 . . ?
O2 C32 O1 119.1(7) . . ?
O2 C32 C33 123.6(7) . . ?
O1 C32 C33 117.3(7) . . ?
O4 C34 O3 124.9(7) . . ?
O4 C34 C35 118.0(6) . . ?
O3 C34 C35 117.1(6) . . ?
O5 C36 O6 126.4(8) . . ?
O5 C36 C37 119.5(8) . . ?
O6 C36 C37 114.1(9) . . ?
O7 C38 O8 118.8(6) . . ?
O7 C38 C39 121.2(6) . . ?
O8 C38 C39 120.0(7) . . ?
O7 C38 Mn3 60.0(3) . . ?
O8 C38 Mn3 58.8(4) . . ?
C39 C38 Mn3 177.7(6) . . ?
C42 C41 C50 121.2(7) . . ?
C42 C41 H41A 119.4 . . ?
C50 C41 H41A 119.4 . . ?
C41 C42 C43 121.7(6) . . ?
C41 C42 H42A 119.1 . . ?
C43 C42 H42A 119.1 . . ?
C48 C43 C42 117.9(6) . . ?
C48 C43 C44 118.9(6) . . ?
C42 C43 C44 123.2(7) . . ?
C45 C44 C43 120.7(7) . . ?
C45 C44 H44A 119.6 . . ?
C43 C44 H44A 119.6 . . ?
C44 C45 C46 120.7(8) . . ?
C44 C45 H45A 119.6 . . ?
C46 C45 H45A 119.6 . . ?
C47 C46 C45 119.4(7) . . ?
C47 C46 H46A 120.3 . . ?
C45 C46 H46A 120.3 . . ?
C46 C47 C48 122.2(7) . . ?
C46 C47 H47A 118.9 . . ?
C48 C47 H47A 118.9 . . ?
C49 C48 C43 119.5(6) . . ?
C49 C48 C47 122.5(7) . . ?
C43 C48 C47 118.0(7) . . ?
C50 C49 C48 122.4(7) . . ?
C50 C49 H49A 118.8 . . ?
C48 C49 H49A 118.8 . . ?
C49 C50 C41 116.9(7) . . ?
C49 C50 C51 122.5(6) . . ?
C41 C50 C51 120.5(6) . . ?
N6 C51 C52 108.0(6) . . ?
N6 C51 C50 123.1(6) . . ?
C52 C51 C50 128.9(7) . . ?
C53 C52 C51 105.4(6) . . ?
C53 C52 H52A 127.3 . . ?
C51 C52 H52A 127.3 . . ?
N7 C53 C52 110.3(6) . . ?
N7 C53 C54 115.0(6) . . ?
C52 C53 C54 134.6(7) . . ?
N8 C54 C55 121.1(7) . . ?
N8 C54 C53 114.2(6) . . ?
C55 C54 C53 124.7(7) . . ?
C54 C55 C56 118.1(8) . . ?
C54 C55 H55A 121.0 . . ?
C56 C55 H55A 121.0 . . ?
C55 C56 C57 120.9(7) . . ?
C55 C56 H56A 119.6 . . ?
C57 C56 H56A 119.6 . . ?
C58 C57 C56 117.4(7) . . ?
C58 C57 H57A 121.3 . . ?
C56 C57 H57A 121.3 . . ?
N8 C58 C57 121.3(7) . . ?
N8 C58 C59 113.5(6) . . ?
C57 C58 C59 125.2(7) . . ?
N9 C59 C60 110.2(7) . . ?
N9 C59 C58 117.5(6) . . ?
C60 C59 C58 131.9(6) . . ?
C61 C60 C59 106.1(6) . . ?
C61 C60 H60A 127.0 . . ?
C59 C60 H60A 127.0 . . ?
N10 C61 C60 105.9(7) . . ?
N10 C61 C62 122.5(7) . . ?
C60 C61 C62 131.6(7) . . ?
C63 C62 C71 118.7(9) . . ?
C63 C62 C61 124.3(7) . . ?
C71 C62 C61 116.9(9) . . ?
C62 C63 C64 124.5(9) . . ?
C62 C63 H63A 117.7 . . ?
C64 C63 H63A 117.7 . . ?
C65 C64 C63 126.6(10) . . ?
C65 C64 C69 116.1(10) . . ?
C63 C64 C69 117.4(11) . . ?
C64 C65 C66 124.7(12) . . ?
C64 C65 H65A 117.6 . . ?
C66 C65 H65A 117.6 . . ?
C67 C66 C65 117.1(13) . . ?
C67 C66 H66A 121.4 . . ?
C65 C66 H66A 121.4 . . ?
C68 C67 C66 122.7(14) . . ?
C68 C67 H67A 118.7 . . ?
C66 C67 H67A 118.7 . . ?
C67 C68 C69 119.4(15) . . ?
C67 C68 H68A 120.3 . . ?
C69 C68 H68A 120.3 . . ?
C70 C69 C64 117.6(12) . . ?
C70 C69 C68 121.9(14) . . ?
C64 C69 C68 119.6(14) . . ?
C71 C70 C69 120.4(14) . . ?
C71 C70 H70A 119.8 . . ?
C69 C70 H70A 119.8 . . ?
C70 C71 C62 120.3(14) . . ?
C70 C71 H71A 119.9 . . ?
C62 C71 H71A 119.9 . . ?
O11 Mn4 N14 100.9(2) . . ?
O11 Mn4 N13 110.0(2) . . ?
N14 Mn4 N13 72.4(2) . . ?
O11 Mn4 O9 137.4(2) . . ?
N14 Mn4 O9 105.2(2) . . ?
N13 Mn4 O9 109.7(2) . . ?
O11 Mn4 O10 93.4(2) . . ?
N14 Mn4 O10 84.9(2) . . ?
N13 Mn4 O10 149.8(2) . . ?
O9 Mn4 O10 56.86(19) . . ?
O11 Mn4 N12 94.1(2) . . ?
N14 Mn4 N12 143.0(2) . . ?
N13 Mn4 N12 70.7(2) . . ?
O9 Mn4 N12 84.8(2) . . ?
O10 Mn4 N12 128.0(2) . . ?
O13 Mn5 O12 167.5(2) . . ?
O13 Mn5 N16 92.9(2) . . ?
O12 Mn5 N16 96.8(2) . . ?
O13 Mn5 O10 86.5(2) . . ?
O12 Mn5 O10 82.7(2) . . ?
N16 Mn5 O10 172.2(2) . . ?
O13 Mn5 O15 87.87(19) . . ?
O12 Mn5 O15 85.1(2) . . ?
N16 Mn5 O15 85.5(2) . . ?
O10 Mn5 O15 86.68(18) . . ?
O13 Mn5 N15 90.6(2) . . ?
O12 Mn5 N15 95.6(2) . . ?
N16 Mn5 N15 98.6(2) . . ?
O10 Mn5 N15 89.1(2) . . ?
O15 Mn5 N15 175.6(2) . . ?
O14 Mn6 N17 99.5(2) . . ?
O14 Mn6 O16 137.8(2) . . ?
N17 Mn6 O16 104.6(2) . . ?
O14 Mn6 N18 111.2(2) . . ?
N17 Mn6 N18 71.9(2) . . ?
O16 Mn6 N18 109.0(2) . . ?
O14 Mn6 N19 96.7(2) . . ?
N17 Mn6 N19 142.6(2) . . ?
O16 Mn6 N19 84.6(2) . . ?
N18 Mn6 N19 70.8(2) . . ?
O14 Mn6 O15 93.54(18) . . ?
N17 Mn6 O15 81.5(2) . . ?
O16 Mn6 O15 57.37(16) . . ?
N18 Mn6 O15 146.0(2) . . ?
N19 Mn6 O15 130.9(2) . . ?
O14 Mn6 C118 118.4(2) . . ?
N17 Mn6 C118 91.6(2) . . ?
O16 Mn6 C118 28.80(18) . . ?
N18 Mn6 C118 129.7(2) . . ?
N19 Mn6 C118 109.8(2) . . ?
O15 Mn6 C118 28.70(18) . . ?
C112 O9 Mn4 92.2(5) . . ?
C112 O10 Mn5 143.8(5) . . ?
C112 O10 Mn4 92.2(4) . . ?
Mn5 O10 Mn4 106.2(2) . . ?
C114 O11 Mn4 125.5(6) . . ?
C114 O12 Mn5 146.1(6) . . ?
C116 O13 Mn5 145.5(5) . . ?
C116 O14 Mn6 126.0(5) . . ?
C118 O15 Mn5 145.0(5) . . ?
C118 O15 Mn6 87.8(4) . . ?
Mn5 O15 Mn6 105.33(19) . . ?
C118 O16 Mn6 94.7(4) . . ?
N12 N11 C91 112.6(6) . . ?
N12 N11 H11C 123.7 . . ?
C91 N11 H11C 123.7 . . ?
N11 N12 C93 106.2(6) . . ?
N11 N12 Mn4 136.7(4) . . ?
C93 N12 Mn4 117.1(5) . . ?
C98 N13 C94 121.5(6) . . ?
C98 N13 Mn4 118.1(5) . . ?
C94 N13 Mn4 120.3(5) . . ?
C99 N14 N15 107.9(6) . . ?
C99 N14 Mn4 118.7(5) . . ?
N15 N14 Mn4 132.8(5) . . ?
C101 N15 N14 107.7(6) . . ?
C101 N15 Mn5 144.8(5) . . ?
N14 N15 Mn5 106.9(4) . . ?
C131 N16 N17 107.6(6) . . ?
C131 N16 Mn5 140.4(5) . . ?
N17 N16 Mn5 109.9(5) . . ?
C133 N17 N16 108.0(7) . . ?
C133 N17 Mn6 119.7(5) . . ?
N16 N17 Mn6 131.8(5) . . ?
C138 N18 C134 121.0(7) . . ?
C138 N18 Mn6 120.8(6) . . ?
C134 N18 Mn6 118.2(5) . . ?
N20 N19 C139 105.3(6) . . ?
N20 N19 Mn6 136.6(4) . . ?
C139 N19 Mn6 117.1(5) . . ?
N19 N20 C141 113.0(7) . . ?
N19 N20 H20B 123.5 . . ?
C141 N20 H20B 123.5 . . ?
C82 C81 C90 122.9(7) . . ?
C82 C81 H81A 118.5 . . ?
C90 C81 H81A 118.5 . . ?
C81 C82 C83 121.3(8) . . ?
C81 C82 H82A 119.4 . . ?
C83 C82 H82A 119.4 . . ?
C82 C83 C88 116.7(9) . . ?
C82 C83 C84 124.4(9) . . ?
C88 C83 C84 118.9(9) . . ?
C85 C84 C83 121.9(10) . . ?
C85 C84 H84A 119.0 . . ?
C83 C84 H84A 119.0 . . ?
C84 C85 C86 118.7(12) . . ?
C84 C85 H85A 120.6 . . ?
C86 C85 H85A 120.6 . . ?
C85 C86 C87 122.5(10) . . ?
C85 C86 H86A 118.8 . . ?
C87 C86 H86A 118.8 . . ?
C86 C87 C88 119.1(9) . . ?
C86 C87 H87A 120.4 . . ?
C88 C87 H87A 120.4 . . ?
C89 C88 C83 120.1(8) . . ?
C89 C88 C87 121.1(9) . . ?
C83 C88 C87 118.8(9) . . ?
C88 C89 C90 122.4(8) . . ?
C88 C89 H89A 118.8 . . ?
C90 C89 H89A 118.8 . . ?
C81 C90 C89 116.0(8) . . ?
C81 C90 C91 122.2(7) . . ?
C89 C90 C91 120.9(7) . . ?
N11 C91 C92 104.4(7) . . ?
N11 C91 C90 121.3(7) . . ?
C92 C91 C90 134.3(6) . . ?
C93 C92 C91 107.4(6) . . ?
C93 C92 H92A 126.3 . . ?
C91 C92 H92A 126.3 . . ?
N12 C93 C92 109.3(7) . . ?
N12 C93 C94 116.9(6) . . ?
C92 C93 C94 133.8(7) . . ?
N13 C94 C95 119.7(8) . . ?
N13 C94 C93 114.6(6) . . ?
C95 C94 C93 125.7(7) . . ?
C96 C95 C94 118.5(8) . . ?
C96 C95 H95A 120.8 . . ?
C94 C95 H95A 120.8 . . ?
C97 C96 C95 121.5(7) . . ?
C97 C96 H96A 119.3 . . ?
C95 C96 H96A 119.3 . . ?
C96 C97 C98 118.3(8) . . ?
C96 C97 H97A 120.9 . . ?
C98 C97 H97A 120.9 . . ?
N13 C98 C97 120.6(7) . . ?
N13 C98 C99 114.2(7) . . ?
C97 C98 C99 125.2(8) . . ?
N14 C99 C100 110.5(7) . . ?
N14 C99 C98 116.4(7) . . ?
C100 C99 C98 133.0(7) . . ?
C99 C100 C101 105.6(7) . . ?
C99 C100 H10B 127.2 . . ?
C101 C100 H10B 127.2 . . ?
N15 C101 C100 108.2(7) . . ?
N15 C101 C102 124.1(7) . . ?
C100 C101 C102 127.7(8) . . ?
C103 C102 C111 116.8(9) . . ?
C103 C102 C101 123.4(8) . . ?
C111 C102 C101 119.7(8) . . ?
C102 C103 C104 122.8(8) . . ?
C102 C103 H10C 118.6 . . ?
C104 C103 H10C 118.6 . . ?
C105 C104 C109 120.6(9) . . ?
C105 C104 C103 122.2(9) . . ?
C109 C104 C103 116.9(8) . . ?
C104 C105 C106 119.5(11) . . ?
C104 C105 H10D 120.3 . . ?
C106 C105 H10D 120.3 . . ?
C105 C106 C107 121.2(11) . . ?
C105 C106 H10E 119.4 . . ?
C107 C106 H10E 119.4 . . ?
C108 C107 C106 119.9(10) . . ?
C108 C107 H10F 120.0 . . ?
C106 C107 H10F 120.0 . . ?
C107 C108 C109 120.6(10) . . ?
C107 C108 H10G 119.7 . . ?
C109 C108 H10G 119.7 . . ?
C110 C109 C104 120.2(9) . . ?
C110 C109 C108 121.9(9) . . ?
C104 C109 C108 117.9(9) . . ?
C111 C110 C109 119.4(10) . . ?
C111 C110 H11A 120.3 . . ?
C109 C110 H11A 120.3 . . ?
C110 C111 C102 123.8(10) . . ?
C110 C111 H11B 118.1 . . ?
C102 C111 H11B 118.1 . . ?
O10 C112 O9 118.7(7) . . ?
O10 C112 C113 119.8(7) . . ?
O9 C112 C113 121.5(8) . . ?
O11 C114 O12 126.0(8) . . ?
O11 C114 C115 117.2(8) . . ?
O12 C114 C115 116.8(8) . . ?
O13 C116 O14 125.8(7) . . ?
O13 C116 C117 119.3(7) . . ?
O14 C116 C117 114.9(7) . . ?
O15 C118 O16 119.6(6) . . ?
O15 C118 C119 122.4(6) . . ?
O16 C118 C119 118.0(6) . . ?
O15 C118 Mn6 63.5(3) . . ?
O16 C118 Mn6 56.5(3) . . ?
C119 C118 Mn6 171.6(5) . . ?
C122 C121 C130 124.2(14) . . ?
C130 C121 C222 115.4(14) . . ?
C122 C121 H121 117.9 . . ?
C130 C121 H121 117.9 . . ?
C121 C122 C123 128.3(19) . . ?
C121 C122 C127 114(2) . . ?
C123 C122 C127 117(2) . . ?
C122 C123 C124 126.5(19) . . ?
C122 C123 H12E 116.8 . . ?
C124 C123 H12E 116.8 . . ?
C125 C124 C123 114(2) . . ?
C125 C124 H12B 122.9 . . ?
C123 C124 H12B 122.9 . . ?
C126 C125 C124 121(2) . . ?
C126 C125 H12C 119.3 . . ?
C124 C125 H12C 119.3 . . ?
C125 C126 C127 124(2) . . ?
C125 C126 H12F 118.0 . . ?
C127 C126 H12F 118.0 . . ?
C126 C127 C122 116(2) . . ?
C126 C127 C128 121.5(19) . . ?
C122 C127 C128 120(2) . . ?
C223 C222 C121 124(2) . . ?
C223 C222 H222 118.1 . . ?
C121 C222 H222 118.1 . . ?
C222 C223 C224 122(2) . . ?
C225 C224 C223 114(2) . . ?
C225 C224 C225 72(2) . 3_577 ?
C223 C224 C225 84.8(16) . 3_577 ?
C225 C224 H22E 123.0 . . ?
C223 C224 H22E 123.0 . . ?
C225 C224 H22E 111.1 3_577 . ?
C226 C225 C224 123(3) . . ?
C226 C225 C224 74(2) . 3_577 ?
C224 C225 C224 108(2) . 3_577 ?
C226 C225 H22A 118.4 . . ?
C224 C225 H22A 118.4 . . ?
C224 C225 H22A 88.6 3_577 . ?
C227 C226 C225 128(3) . . ?
C227 C226 H22B 115.9 . . ?
C225 C226 H22B 115.9 . . ?
C226 C227 C128 120(2) . . ?
C226 C227 H227 120.2 . . ?
C128 C227 H227 120.2 . . ?
C129 C128 C127 113.0(13) . . ?
C129 C128 C227 121.3(15) . . ?
C129 C128 H128 123.5 . . ?
C127 C128 H128 123.5 . . ?
C130 C129 C128 119.8(11) . . ?
C130 C129 H12D 120.1 . . ?
C128 C129 H12D 120.1 . . ?
C129 C130 C121 120.6(10) . . ?
C129 C130 C131 118.6(9) . . ?
C121 C130 C131 120.7(9) . . ?
N16 C131 C132 109.9(8) . . ?
N16 C131 C130 122.2(8) . . ?
C132 C131 C130 127.9(9) . . ?
C131 C132 C133 104.4(8) . . ?
C131 C132 H13A 127.8 . . ?
C133 C132 H13A 127.8 . . ?
N17 C133 C132 109.9(7) . . ?
N17 C133 C134 115.7(8) . . ?
C132 C133 C134 134.2(8) . . ?
N18 C134 C135 120.8(8) . . ?
N18 C134 C133 114.0(7) . . ?
C135 C134 C133 125.1(9) . . ?
C134 C135 C136 118.2(9) . . ?
C134 C135 H13B 120.9 . . ?
C136 C135 H13B 120.9 . . ?
C137 C136 C135 120.9(8) . . ?
C137 C136 H13C 119.5 . . ?
C135 C136 H13C 119.5 . . ?
C136 C137 C138 118.3(9) . . ?
C136 C137 H13D 120.9 . . ?
C138 C137 H13D 120.9 . . ?
N18 C138 C137 120.8(9) . . ?
N18 C138 C139 114.3(6) . . ?
C137 C138 C139 125.0(8) . . ?
N19 C139 C140 109.7(8) . . ?
N19 C139 C138 116.6(6) . . ?
C140 C139 C138 133.6(7) . . ?
C139 C140 C141 107.0(6) . . ?
C139 C140 H14A 126.5 . . ?
C141 C140 H14A 126.5 . . ?
N20 C141 C140 105.0(7) . . ?
N20 C141 C142 122.8(7) . . ?
C140 C141 C142 132.2(6) . . ?
C143 C142 C151 117.4(9) . . ?
C143 C142 C141 122.9(7) . . ?
C151 C142 C141 119.7(8) . . ?
C142 C143 C144 124.0(8) . . ?
C142 C143 H14B 118.0 . . ?
C144 C143 H14B 118.0 . . ?
C145 C144 C143 125.4(9) . . ?
C145 C144 C149 117.6(11) . . ?
C143 C144 C149 117.0(10) . . ?
C146 C145 C144 126.3(12) . . ?
C146 C145 H14C 116.8 . . ?
C144 C145 H14C 116.8 . . ?
C145 C146 C147 115.9(14) . . ?
C145 C146 H14D 122.0 . . ?
C147 C146 H14D 122.0 . . ?
C148 C147 C146 119.5(14) . . ?
C148 C147 H14E 120.2 . . ?
C146 C147 H14E 120.2 . . ?
C147 C148 C149 123.7(13) . . ?
C147 C148 H14F 118.2 . . ?
C149 C148 H14F 118.2 . . ?
C150 C149 C148 124.8(11) . . ?
C150 C149 C144 118.5(10) . . ?
C148 C149 C144 116.7(13) . . ?
C151 C150 C149 122.5(9) . . ?
C151 C150 H15B 118.8 . . ?
C149 C150 H15B 118.8 . . ?
C150 C151 C142 120.5(10) . . ?
C150 C151 H15C 119.7 . . ?
C142 C151 H15C 119.7 . . ?
C1S O1S C4S 107.9(16) . . ?
O1S C1S C2S 117(2) . . ?
O1S C1S H1SA 107.9 . . ?
C2S C1S H1SA 107.9 . . ?
O1S C1S H1SB 107.9 . . ?
C2S C1S H1SB 107.9 . . ?
H1SA C1S H1SB 107.2 . . ?
C1S C2S C3S 95(2) . . ?
C1S C2S H2SA 112.8 . . ?
C3S C2S H2SA 112.8 . . ?
C1S C2S H2SB 112.8 . . ?
C3S C2S H2SB 112.8 . . ?
H2SA C2S H2SB 110.2 . . ?
C4S C3S C2S 106(2) . . ?
C4S C3S H3SA 110.6 . . ?
C2S C3S H3SA 110.6 . . ?
C4S C3S H3SB 110.6 . . ?
C2S C3S H3SB 110.6 . . ?
H3SA C3S H3SB 108.7 . . ?
O1S C4S C3S 97.6(19) . . ?
O1S C4S H4SA 112.2 . . ?
C3S C4S H4SA 112.2 . . ?
O1S C4S H4SB 112.2 . . ?
C3S C4S H4SB 112.2 . . ?
H4SA C4S H4SB 109.8 . . ?
C5S O2S C8S 116.6(18) . . ?
O2S C5S C6S 98.9(18) . . ?
O2S C5S H5SA 112.0 . . ?
C6S C5S H5SA 112.0 . . ?
O2S C5S H5SB 112.0 . . ?
C6S C5S H5SB 112.0 . . ?
H5SA C5S H5SB 109.7 . . ?
C7S C6S C5S 105.0(18) . . ?
C7S C6S H6SA 110.7 . . ?
C5S C6S H6SA 110.7 . . ?
C7S C6S H6SB 110.7 . . ?
C5S C6S H6SB 110.7 . . ?
H6SA C6S H6SB 108.8 . . ?
C6S C7S C8S 101.2(19) . . ?
C6S C7S H7SA 111.5 . . ?
C8S C7S H7SA 111.5 . . ?
C6S C7S H7SB 111.5 . . ?
C8S C7S H7SB 111.5 . . ?
H7SA C7S H7SB 109.3 . . ?
O2S C8S C7S 101.3(16) . . ?
O2S C8S H8SA 111.5 . . ?
C7S C8S H8SA 111.5 . . ?
O2S C8S H8SB 111.5 . . ?
C7S C8S H8SB 111.5 . . ?
H8SA C8S H8SB 109.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B O16 0.88 1.97 2.834(7) 166.0 .
N10 H10A O9 0.88 1.93 2.781(8) 161.1 .
N11 H11C O8 0.88 1.88 2.716(7) 158.6 .
N20 H20B O1 0.88 1.93 2.782(8) 161.9 .

_refine_diff_density_max         1.508
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.100

_shelxl_version_number           2013-2



####################################################################### 
# 
# 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_lb622
_database_code_depnum_ccdc_archive 'CCDC 1022214'
_audit_update_record             
;
2014-09-01 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H21 N5, C16 H36 N, C2 H3 O2, H2 O'
_chemical_formula_sum            'C49 H62 N6 O3'
_chemical_formula_weight         783.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.623(3)
_cell_length_b                   16.641(4)
_cell_length_c                   18.326(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.777(3)
_cell_angle_gamma                90
_cell_volume                     4365.6(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7622
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      31.65

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.089
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI US'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32623
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.813
_diffrn_reflns_theta_max         30.209
_diffrn_reflns_theta_full        30.200
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             9930
_reflns_number_gt                7580
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0605P)²+0.9732P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9930
_refine_ls_number_parameters     540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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_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
N1 N 0.84634(8) 0.11704(7) 0.15007(6) 0.0249(2) Uani 1 1 d . . . . .
N2 N 0.77155(8) 0.15293(7) 0.10733(6) 0.0247(2) Uani 1 1 d . . . . .
H2 H 0.7127(13) 0.1545(10) 0.1261(10) 0.037 Uiso 1 1 d . U . . .
N3 N 0.63332(8) 0.22113(7) 0.00722(6) 0.0251(2) Uani 1 1 d . . . . .
N4 N 0.46761(9) 0.22159(8) 0.05290(7) 0.0270(3) Uani 1 1 d . . . . .
H4 H 0.5155(13) 0.1944(11) 0.0861(10) 0.040 Uiso 1 1 d . U . . .
N5 N 0.38256(9) 0.23042(7) 0.06925(7) 0.0277(3) Uani 1 1 d . . . . .
C1 C 1.06180(11) 0.05325(9) 0.09188(8) 0.0310(3) Uani 1 1 d . . . . .
H1A H 1.0448 0.0643 0.0400 0.037 Uiso 1 1 calc R U . . .
C2 C 1.14148(11) 0.01104(10) 0.11896(9) 0.0332(3) Uani 1 1 d . . . . .
H2A H 1.1790 -0.0069 0.0855 0.040 Uiso 1 1 calc R U . . .
C3 C 1.16945(10) -0.00658(9) 0.19600(8) 0.0288(3) Uani 1 1 d . . . . .
C4 C 1.24827(11) -0.05481(10) 0.22483(9) 0.0345(3) Uani 1 1 d . . . . .
H4A H 1.2865 -0.0740 0.1924 0.041 Uiso 1 1 calc R U . . .
C5 C 1.26987(11) -0.07405(10) 0.29911(9) 0.0363(4) Uani 1 1 d . . . . .
H5A H 1.3221 -0.1075 0.3176 0.044 Uiso 1 1 calc R U . . .
C6 C 1.21508(11) -0.04447(10) 0.34814(9) 0.0351(3) Uani 1 1 d . . . . .
H6A H 1.2309 -0.0578 0.3996 0.042 Uiso 1 1 calc R U . . .
C7 C 1.13955(11) 0.00315(9) 0.32229(8) 0.0301(3) Uani 1 1 d . . . . .
H7A H 1.1038 0.0233 0.3561 0.036 Uiso 1 1 calc R U . . .
C8 C 1.11363(10) 0.02311(9) 0.24528(8) 0.0261(3) Uani 1 1 d . . . . .
C9 C 1.03203(10) 0.06721(8) 0.21577(7) 0.0248(3) Uani 1 1 d . . . . .
H9A H 0.9955 0.0880 0.2487 0.030 Uiso 1 1 calc R U . . .
C10 C 1.00398(10) 0.08092(8) 0.14021(8) 0.0255(3) Uani 1 1 d . . . . .
C11 C 0.91328(10) 0.11851(8) 0.10986(7) 0.0244(3) Uani 1 1 d . . . . .
C12 C 0.88001(10) 0.15535(9) 0.04023(8) 0.0267(3) Uani 1 1 d . . . . .
H12A H 0.9132 0.1636 0.0014 0.032 Uiso 1 1 calc R U . . .
C13 C 0.78897(10) 0.17677(8) 0.04061(7) 0.0251(3) Uani 1 1 d . . . . .
C14 C 0.71595(10) 0.21758(9) -0.01313(7) 0.0255(3) Uani 1 1 d . . . . .
C15 C 0.73163(11) 0.25141(9) -0.07929(8) 0.0298(3) Uani 1 1 d . . . . .
H15A H 0.7910 0.2476 -0.0925 0.036 Uiso 1 1 calc R U . . .
C16 C 0.65779(11) 0.29079(10) -0.12519(8) 0.0332(3) Uani 1 1 d . . . . .
H16A H 0.6661 0.3145 -0.1705 0.040 Uiso 1 1 calc R U . . .
C17 C 0.57224(11) 0.29517(9) -0.10446(8) 0.0301(3) Uani 1 1 d . . . . .
H17A H 0.5212 0.3222 -0.1350 0.036 Uiso 1 1 calc R U . . .
C18 C 0.56237(10) 0.25895(8) -0.03763(7) 0.0253(3) Uani 1 1 d . . . . .
C19 C 0.47484(10) 0.26029(8) -0.01094(7) 0.0257(3) Uani 1 1 d . . . . .
C20 C 0.38972(10) 0.29636(9) -0.03808(8) 0.0261(3) Uani 1 1 d . . . . .
H20A H 0.3722 0.3279 -0.0819 0.031 Uiso 1 1 calc R U . . .
C21 C 0.33459(10) 0.27588(8) 0.01388(8) 0.0253(3) Uani 1 1 d . . . . .
C22 C 0.23618(10) 0.29618(9) 0.01161(8) 0.0258(3) Uani 1 1 d . . . . .
C23 C 0.18905(10) 0.34899(9) -0.04045(8) 0.0262(3) Uani 1 1 d . . . . .
H23A H 0.2205 0.3719 -0.0759 0.031 Uiso 1 1 calc R U . . .
C24 C 0.09483(10) 0.36999(9) -0.04244(8) 0.0273(3) Uani 1 1 d . . . . .
C25 C 0.04576(11) 0.42473(10) -0.09557(9) 0.0334(3) Uani 1 1 d . . . . .
H25A H 0.0762 0.4481 -0.1315 0.040 Uiso 1 1 calc R U . . .
C26 C -0.04511(12) 0.44420(10) -0.09553(10) 0.0388(4) Uani 1 1 d . . . . .
H26A H -0.0773 0.4809 -0.1315 0.047 Uiso 1 1 calc R U . . .
C27 C -0.09126(12) 0.41035(11) -0.04262(9) 0.0383(4) Uani 1 1 d . . . . .
H27A H -0.1541 0.4249 -0.0428 0.046 Uiso 1 1 calc R U . . .
C28 C -0.04642(11) 0.35688(10) 0.00888(9) 0.0345(3) Uani 1 1 d . . . . .
H28A H -0.0785 0.3342 0.0441 0.041 Uiso 1 1 calc R U . . .
C29 C 0.04755(10) 0.33485(9) 0.01036(8) 0.0292(3) Uani 1 1 d . . . . .
C30 C 0.09662(11) 0.27846(9) 0.06193(8) 0.0312(3) Uani 1 1 d . . . . .
H30A H 0.0653 0.2532 0.0964 0.037 Uiso 1 1 calc R U . . .
C31 C 0.18776(11) 0.25975(9) 0.06321(8) 0.0290(3) Uani 1 1 d . . . . .
H31A H 0.2192 0.2222 0.0987 0.035 Uiso 1 1 calc R U . . .
O1 O 0.60518(7) 0.15025(6) 0.16185(6) 0.0322(2) Uani 1 1 d . . . . .
O2 O 0.64342(8) 0.05812(7) 0.25092(6) 0.0396(3) Uani 1 1 d . . . . .
C32 C 0.58687(11) 0.09256(10) 0.19952(8) 0.0313(3) Uani 1 1 d . . . . .
C33 C 0.48780(12) 0.05806(11) 0.18143(9) 0.0393(4) Uani 1 1 d . . . . .
H33A H 0.4450 0.0981 0.1539 0.059 Uiso 1 1 calc R U . . .
H33B H 0.4680 0.0444 0.2279 0.059 Uiso 1 1 calc R U . . .
H33C H 0.4869 0.0096 0.1509 0.059 Uiso 1 1 calc R U . . .
N6 N 0.67550(9) 0.36575(8) 0.27732(7) 0.0311(3) Uani 1 1 d . . . . .
C34 C 0.59981(12) 0.30912(9) 0.29234(9) 0.0348(4) Uani 1 1 d . . . . .
H34A H 0.5810 0.2734 0.2487 0.042 Uiso 1 1 calc R U . . .
H34B H 0.6265 0.2749 0.3356 0.042 Uiso 1 1 calc R U . . .
C35 C 0.51306(13) 0.35056(10) 0.30785(11) 0.0409(4) Uani 1 1 d . . . . .
H35A H 0.4810 0.3791 0.2624 0.049 Uiso 1 1 calc R U . . .
H35B H 0.5319 0.3910 0.3477 0.049 Uiso 1 1 calc R U . . .
C36 C 0.44548(12) 0.29096(10) 0.33158(9) 0.0365(4) Uani 1 1 d . . . . .
H36A H 0.4797 0.2586 0.3738 0.044 Uiso 1 1 calc R U . . .
H36B H 0.3961 0.3213 0.3495 0.044 Uiso 1 1 calc R U . . .
C37 C 0.39981(15) 0.23471(14) 0.26998(12) 0.0578(5) Uani 1 1 d . . . . .
H37A H 0.3556 0.1997 0.2884 0.087 Uiso 1 1 calc R U . . .
H37B H 0.4478 0.2018 0.2541 0.087 Uiso 1 1 calc R U . . .
H37C H 0.3664 0.2662 0.2276 0.087 Uiso 1 1 calc R U . . .
C38 C 0.63967(12) 0.41964(9) 0.21048(8) 0.0318(3) Uani 1 1 d . . . . .
H38A H 0.5948 0.4583 0.2246 0.038 Uiso 1 1 calc R U . . .
H38B H 0.6931 0.4511 0.2002 0.038 Uiso 1 1 calc R U . . .
C39 C 0.59230(12) 0.37867(9) 0.13848(9) 0.0341(3) Uani 1 1 d . . . . .
H39A H 0.5305 0.3578 0.1434 0.041 Uiso 1 1 calc R U . . .
H39B H 0.6307 0.3329 0.1278 0.041 Uiso 1 1 calc R U . . .
C40 C 0.58055(13) 0.43999(10) 0.07475(9) 0.0386(4) Uani 1 1 d . . . . .
H40A H 0.5325 0.4201 0.0325 0.046 Uiso 1 1 calc R U . . .
H40B H 0.5577 0.4912 0.0919 0.046 Uiso 1 1 calc R U . . .
C41 C 0.67000(14) 0.45579(12) 0.04759(10) 0.0491(5) Uani 1 1 d . . . . .
H41A H 0.6583 0.4959 0.0076 0.074 Uiso 1 1 calc R U . . .
H41B H 0.6917 0.4057 0.0286 0.074 Uiso 1 1 calc R U . . .
H41C H 0.7179 0.4759 0.0890 0.074 Uiso 1 1 calc R U . . .
C42 C 0.75497(11) 0.31283(9) 0.26332(9) 0.0330(3) Uani 1 1 d . . . . .
H42A H 0.7334 0.2834 0.2160 0.040 Uiso 1 1 calc R U . . .
H42B H 0.7691 0.2725 0.3038 0.040 Uiso 1 1 calc R U . . .
C43 C 0.84476(12) 0.35699(10) 0.25888(11) 0.0397(4) Uani 1 1 d . . . . .
H43A H 0.8303 0.4029 0.2241 0.048 Uiso 1 1 calc R U . . .
H43B H 0.8735 0.3784 0.3087 0.048 Uiso 1 1 calc R U . . .
C44 C 0.91288(12) 0.30142(10) 0.23231(10) 0.0378(4) Uani 1 1 d . . . . .
H44A H 0.8861 0.2840 0.1807 0.045 Uiso 1 1 calc R U . . .
H44B H 0.9222 0.2529 0.2643 0.045 Uiso 1 1 calc R U . . .
C45 C 1.00670(13) 0.34128(11) 0.23412(11) 0.0441(4) Uani 1 1 d . . . . .
H45A H 1.0493 0.3026 0.2182 0.066 Uiso 1 1 calc R U . . .
H45B H 1.0331 0.3594 0.2849 0.066 Uiso 1 1 calc R U . . .
H45C H 0.9983 0.3876 0.2003 0.066 Uiso 1 1 calc R U . . .
C46 C 0.70808(12) 0.42329(9) 0.34168(8) 0.0336(3) Uani 1 1 d . . . . .
H46A H 0.7589 0.4570 0.3298 0.040 Uiso 1 1 calc R U . . .
H46B H 0.6556 0.4595 0.3457 0.040 Uiso 1 1 calc R U . . .
C47 C 0.74290(14) 0.38411(10) 0.41689(9) 0.0414(4) Uani 1 1 d . . . . .
H47A H 0.7934 0.3456 0.4133 0.050 Uiso 1 1 calc R U . . .
H47B H 0.6913 0.3538 0.4317 0.050 Uiso 1 1 calc R U . . .
C48 C 0.77969(13) 0.44745(11) 0.47611(9) 0.0413(4) Uani 1 1 d . . . . .
H48A H 0.7336 0.4917 0.4720 0.050 Uiso 1 1 calc R U . . .
H48B H 0.7853 0.4229 0.5260 0.050 Uiso 1 1 calc R U . . .
C49 C 0.87333(15) 0.48213(13) 0.46983(11) 0.0522(5) Uani 1 1 d . . . . .
H49A H 0.8928 0.5220 0.5093 0.078 Uiso 1 1 calc R U . . .
H49B H 0.8681 0.5080 0.4211 0.078 Uiso 1 1 calc R U . . .
H49C H 0.9198 0.4390 0.4750 0.078 Uiso 1 1 calc R U . . .
O1W O 0.81821(9) 0.11564(7) 0.30241(6) 0.0352(3) Uani 1 1 d . . . . .
H1W H 0.8380(15) 0.1178(12) 0.2623(13) 0.053 Uiso 1 1 d . U . . .
H2W H 0.7562(16) 0.1002(13) 0.2888(12) 0.053 Uiso 1 1 d . U . . .


_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
N1 C11 1.3402(18) . ?
N1 N2 1.3478(16) . ?
N2 C13 1.3581(17) . ?
N2 H2 0.990(18) . ?
N3 C14 1.3365(19) . ?
N3 C18 1.3416(18) . ?
N4 N5 1.3455(17) . ?
N4 C19 1.3582(18) . ?
N4 H4 0.94(2) . ?
N5 C21 1.3429(18) . ?
C1 C2 1.364(2) . ?
C1 C10 1.420(2) . ?
C1 H1A 0.9500 . ?
C2 C3 1.418(2) . ?
C2 H2A 0.9500 . ?
C3 C4 1.415(2) . ?
C3 C8 1.424(2) . ?
C4 C5 1.371(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.409(2) . ?
C5 H5A 0.9500 . ?
C6 C7 1.363(2) . ?
C6 H6A 0.9500 . ?
C7 C8 1.424(2) . ?
C7 H7A 0.9500 . ?
C8 C9 1.411(2) . ?
C9 C10 1.3805(19) . ?
C9 H9A 0.9500 . ?
C10 C11 1.469(2) . ?
C11 C12 1.4098(19) . ?
C12 C13 1.380(2) . ?
C12 H12A 0.9500 . ?
C13 C14 1.4636(19) . ?
C14 C15 1.3976(19) . ?
C15 C16 1.390(2) . ?
C15 H15A 0.9500 . ?
C16 C17 1.382(2) . ?
C16 H16A 0.9500 . ?
C17 C18 1.399(2) . ?
C17 H17A 0.9500 . ?
C18 C19 1.461(2) . ?
C19 C20 1.380(2) . ?
C20 C21 1.4093(19) . ?
C20 H20A 0.9500 . ?
C21 C22 1.471(2) . ?
C22 C23 1.374(2) . ?
C22 C31 1.427(2) . ?
C23 C24 1.415(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.417(2) . ?
C24 C29 1.425(2) . ?
C25 C26 1.368(2) . ?
C25 H25A 0.9500 . ?
C26 C27 1.407(2) . ?
C26 H26A 0.9500 . ?
C27 C28 1.364(2) . ?
C27 H27A 0.9500 . ?
C28 C29 1.417(2) . ?
C28 H28A 0.9500 . ?
C29 C30 1.418(2) . ?
C30 C31 1.364(2) . ?
C30 H30A 0.9500 . ?
C31 H31A 0.9500 . ?
O1 C32 1.2431(19) . ?
O2 C32 1.2576(18) . ?
C32 C33 1.531(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N6 C46 1.518(2) . ?
N6 C34 1.521(2) . ?
N6 C42 1.5209(19) . ?
N6 C38 1.5222(19) . ?
C34 C35 1.521(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.525(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.513(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.521(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.534(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.514(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.521(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.511(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.518(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.516(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.530(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.512(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
O1W H1W 0.84(2) . ?
O1W H2W 0.93(2) . ?

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
C11 N1 N2 105.63(11) . . ?
N1 N2 C13 111.94(12) . . ?
N1 N2 H2 118.0(10) . . ?
C13 N2 H2 129.9(10) . . ?
C14 N3 C18 118.68(12) . . ?
N5 N4 C19 112.21(12) . . ?
N5 N4 H4 120.5(11) . . ?
C19 N4 H4 127.2(11) . . ?
C21 N5 N4 104.91(11) . . ?
C2 C1 C10 120.87(14) . . ?
C2 C1 H1A 119.6 . . ?
C10 C1 H1A 119.6 . . ?
C1 C2 C3 121.34(14) . . ?
C1 C2 H2A 119.3 . . ?
C3 C2 H2A 119.3 . . ?
C4 C3 C2 122.44(14) . . ?
C4 C3 C8 119.26(14) . . ?
C2 C3 C8 118.26(13) . . ?
C5 C4 C3 120.54(15) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 120.38(15) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C7 C6 C5 120.48(14) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C6 C7 C8 120.86(14) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
C9 C8 C3 119.13(13) . . ?
C9 C8 C7 122.31(13) . . ?
C3 C8 C7 118.47(13) . . ?
C10 C9 C8 121.68(13) . . ?
C10 C9 H9A 119.2 . . ?
C8 C9 H9A 119.2 . . ?
C9 C10 C1 118.63(13) . . ?
C9 C10 C11 120.69(13) . . ?
C1 C10 C11 120.56(13) . . ?
N1 C11 C12 110.48(13) . . ?
N1 C11 C10 119.23(12) . . ?
C12 C11 C10 130.22(13) . . ?
C13 C12 C11 105.23(12) . . ?
C13 C12 H12A 127.4 . . ?
C11 C12 H12A 127.4 . . ?
N2 C13 C12 106.72(12) . . ?
N2 C13 C14 119.75(12) . . ?
C12 C13 C14 133.53(12) . . ?
N3 C14 C15 122.82(13) . . ?
N3 C14 C13 114.19(12) . . ?
C15 C14 C13 122.98(13) . . ?
C16 C15 C14 118.05(14) . . ?
C16 C15 H15A 121.0 . . ?
C14 C15 H15A 121.0 . . ?
C17 C16 C15 119.58(13) . . ?
C17 C16 H16A 120.2 . . ?
C15 C16 H16A 120.2 . . ?
C16 C17 C18 118.63(14) . . ?
C16 C17 H17A 120.7 . . ?
C18 C17 H17A 120.7 . . ?
N3 C18 C17 122.24(13) . . ?
N3 C18 C19 115.02(12) . . ?
C17 C18 C19 122.74(13) . . ?
N4 C19 C20 107.08(13) . . ?
N4 C19 C18 120.58(13) . . ?
C20 C19 C18 132.33(13) . . ?
C19 C20 C21 104.44(12) . . ?
C19 C20 H20A 127.8 . . ?
C21 C20 H20A 127.8 . . ?
N5 C21 C20 111.36(13) . . ?
N5 C21 C22 120.53(12) . . ?
C20 C21 C22 128.08(13) . . ?
C23 C22 C31 119.03(13) . . ?
C23 C22 C21 121.04(13) . . ?
C31 C22 C21 119.92(13) . . ?
C22 C23 C24 121.57(13) . . ?
C22 C23 H23A 119.2 . . ?
C24 C23 H23A 119.2 . . ?
C23 C24 C25 122.03(13) . . ?
C23 C24 C29 119.10(14) . . ?
C25 C24 C29 118.87(14) . . ?
C26 C25 C24 120.50(15) . . ?
C26 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?
C25 C26 C27 120.54(16) . . ?
C25 C26 H26A 119.7 . . ?
C27 C26 H26A 119.7 . . ?
C28 C27 C26 120.51(15) . . ?
C28 C27 H27A 119.7 . . ?
C26 C27 H27A 119.7 . . ?
C27 C28 C29 120.62(15) . . ?
C27 C28 H28A 119.7 . . ?
C29 C28 H28A 119.7 . . ?
C28 C29 C30 122.72(14) . . ?
C28 C29 C24 118.95(14) . . ?
C30 C29 C24 118.32(14) . . ?
C31 C30 C29 121.47(14) . . ?
C31 C30 H30A 119.3 . . ?
C29 C30 H30A 119.3 . . ?
C30 C31 C22 120.45(14) . . ?
C30 C31 H31A 119.8 . . ?
C22 C31 H31A 119.8 . . ?
O1 C32 O2 125.78(15) . . ?
O1 C32 C33 118.10(14) . . ?
O2 C32 C33 116.10(14) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C46 N6 C34 112.00(11) . . ?
C46 N6 C42 111.51(13) . . ?
C34 N6 C42 106.32(11) . . ?
C46 N6 C38 104.80(11) . . ?
C34 N6 C38 111.53(13) . . ?
C42 N6 C38 110.78(11) . . ?
C35 C34 N6 114.74(13) . . ?
C35 C34 H34A 108.6 . . ?
N6 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
N6 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C34 C35 C36 111.86(13) . . ?
C34 C35 H35A 109.2 . . ?
C36 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C36 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C37 C36 C35 113.75(14) . . ?
C37 C36 H36A 108.8 . . ?
C35 C36 H36A 108.8 . . ?
C37 C36 H36B 108.8 . . ?
C35 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 N6 117.07(12) . . ?
C39 C38 H38A 108.0 . . ?
N6 C38 H38A 108.0 . . ?
C39 C38 H38B 108.0 . . ?
N6 C38 H38B 108.0 . . ?
H38A C38 H38B 107.3 . . ?
C38 C39 C40 108.84(13) . . ?
C38 C39 H39A 109.9 . . ?
C40 C39 H39A 109.9 . . ?
C38 C39 H39B 109.9 . . ?
C40 C39 H39B 109.9 . . ?
H39A C39 H39B 108.3 . . ?
C41 C40 C39 113.31(15) . . ?
C41 C40 H40A 108.9 . . ?
C39 C40 H40A 108.9 . . ?
C41 C40 H40B 108.9 . . ?
C39 C40 H40B 108.9 . . ?
H40A C40 H40B 107.7 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N6 C42 C43 115.27(13) . . ?
N6 C42 H42A 108.5 . . ?
C43 C42 H42A 108.5 . . ?
N6 C42 H42B 108.5 . . ?
C43 C42 H42B 108.5 . . ?
H42A C42 H42B 107.5 . . ?
C44 C43 C42 110.77(14) . . ?
C44 C43 H43A 109.5 . . ?
C42 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
C43 C44 C45 112.20(14) . . ?
C43 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 N6 115.41(13) . . ?
C47 C46 H46A 108.4 . . ?
N6 C46 H46A 108.4 . . ?
C47 C46 H46B 108.4 . . ?
N6 C46 H46B 108.4 . . ?
H46A C46 H46B 107.5 . . ?
C46 C47 C48 110.68(13) . . ?
C46 C47 H47A 109.5 . . ?
C48 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C48 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C49 C48 C47 113.70(15) . . ?
C49 C48 H48A 108.8 . . ?
C47 C48 H48A 108.8 . . ?
C49 C48 H48B 108.8 . . ?
C47 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
H1W O1W H2W 105.4(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O1 0.990(18) 1.824(18) 2.8127(16) 176.2(16) .
N4 H4 O1 0.94(2) 1.86(2) 2.7934(17) 171.8(17) .
O1W H2W O2 0.93(2) 1.80(2) 2.7120(18) 169.6(19) .
O1W H1W N1 0.84(2) 2.08(2) 2.9038(17) 163(2) .

_refine_diff_density_max         0.355
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.045

_shelxl_version_number           2014-3

