# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_ThioIndigoPMCpCr
_database_code_depnum_ccdc_archive 'CCDC 1561767'
_audit_update_record             
;
2017-07-12 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Sep 09 14:23:34 2016'
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'pentamethylcyclopentadienyl(thioindigo dianion) chromiunm dimer'
_chemical_name_common            no
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C52 H46 O4 S4 Cr2, C6 H14'
_chemical_formula_sum            'C58 H60 Cr2 O4 S4'
_chemical_formula_weight         1053.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.3104(4)
_cell_length_b                   10.9762(4)
_cell_length_c                   12.2084(2)
_cell_angle_alpha                67.979(2)
_cell_angle_beta                 82.612(6)
_cell_angle_gamma                83.122(3)
_cell_volume                     1266.33(7)
_cell_formula_units_Z            1

_cell_measurement_temperature    200(1)
_cell_measurement_reflns_used    14027
_cell_measurement_theta_min      2.7130
_cell_measurement_theta_max      28.2560

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.641
_shelx_estimated_absorpt_T_min   0.831
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_T_min  0.93123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            22567
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.998
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6189
_reflns_number_gt                5495
_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_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX

_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)+(0.0424P)²+0.4107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6189
_refine_ls_number_parameters     409
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0828
_refine_ls_wR_factor_gt          0.0790
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
S1 S 0.86189(4) 0.35177(4) 0.41025(4) 0.03531(9) Uani 1 1 d . U . . .
S2 S 0.70587(4) 0.39734(4) 0.19240(3) 0.03924(10) Uani 1 1 d . U . . .
O1 O 0.58247(10) 0.13262(10) 0.60418(9) 0.0304(2) Uani 1 1 d . U . . .
O2 O 0.52863(9) 0.08810(9) 0.40306(8) 0.02505(19) Uani 1 1 d . U . . .
C1 C 0.71802(13) 0.26895(13) 0.43347(13) 0.0271(3) Uani 1 1 d . U . . .
C2 C 0.66218(13) 0.27390(13) 0.32908(12) 0.0275(3) Uani 1 1 d . U . . .
C3 C 0.87056(14) 0.30569(14) 0.56129(15) 0.0330(3) Uani 1 1 d . U . . .
C4 C 0.76805(14) 0.22875(14) 0.62672(13) 0.0299(3) Uani 1 1 d . U . . .
C5 C 0.61974(16) 0.33313(16) 0.11636(13) 0.0365(3) Uani 1 1 d . U . . .
C6 C 0.55500(14) 0.22313(14) 0.19382(12) 0.0300(3) Uani 1 1 d . U . . .
C7 C 0.68108(13) 0.20592(13) 0.55293(12) 0.0259(3) Uani 1 1 d . U . . .
C8 C 0.58117(13) 0.19161(13) 0.31476(11) 0.0258(3) Uani 1 1 d . U . . .
C9 C 0.75772(16) 0.18428(17) 0.75044(15) 0.0399(3) Uani 1 1 d . U . . .
H9 H 0.6894 0.1309 0.7960 0.048 Uiso 1 1 calc R U . . .
C10 C 0.84823(19) 0.2190(2) 0.80562(17) 0.0496(4) Uani 1 1 d . U . . .
H10 H 0.8408 0.1909 0.8897 0.060 Uiso 1 1 calc R U . . .
C11 C 0.95045(17) 0.29504(19) 0.73903(18) 0.0495(4) Uani 1 1 d . U . . .
H11 H 1.0122 0.3171 0.7787 0.059 Uiso 1 1 calc R U . . .
C12 C 0.96344(16) 0.33837(17) 0.61778(18) 0.0426(4) Uani 1 1 d . U . . .
H12 H 1.0337 0.3893 0.5731 0.051 Uiso 1 1 calc R U . . .
C13 C 0.47943(16) 0.15812(17) 0.14908(14) 0.0375(3) Uani 1 1 d . U . . .
H13 H 0.4348 0.0840 0.2007 0.045 Uiso 1 1 calc R U . . .
C14 C 0.47100(18) 0.2040(2) 0.02797(15) 0.0477(4) Uani 1 1 d . U . . .
H14 H 0.4202 0.1607 -0.0039 0.057 Uiso 1 1 calc R U . . .
C15 C 0.5363(2) 0.3133(2) -0.04808(15) 0.0524(4) Uani 1 1 d . U . . .
H15 H 0.5294 0.3428 -0.1310 0.063 Uiso 1 1 calc R U . . .
C16 C 0.60984(19) 0.37880(19) -0.00592(14) 0.0481(4) Uani 1 1 d . U . . .
H16 H 0.6532 0.4535 -0.0583 0.058 Uiso 1 1 calc R U . . .
Cr Cr 0.42694(2) 0.10677(2) 0.54658(2) 0.02316(7) Uani 1 1 d . U . . .
C21 C 0.3049(4) 0.2927(4) 0.4821(5) 0.0393(8) Uani 0.634(7) 1 d . U P A 1
C22 C 0.2346(13) 0.1905(10) 0.4753(6) 0.0365(9) Uani 0.634(7) 1 d . U P A 1
C23 C 0.2069(8) 0.1017(7) 0.5913(5) 0.0337(8) Uani 0.634(7) 1 d . U P A 1
C24 C 0.2616(5) 0.1445(5) 0.6702(3) 0.0366(7) Uani 0.634(7) 1 d . U P A 1
C25 C 0.3171(4) 0.2642(5) 0.6037(5) 0.0405(8) Uani 0.634(7) 1 d . U P A 1
C26 C 0.3451(4) 0.4116(4) 0.3792(6) 0.0771(16) Uani 0.634(7) 1 d . U P A 1
H26A H 0.2700 0.4773 0.3599 0.116 Uiso 0.634(7) 1 calc R U P A 1
H26B H 0.3758 0.3868 0.3105 0.116 Uiso 0.634(7) 1 calc R U P A 1
H26C H 0.4161 0.4491 0.3994 0.116 Uiso 0.634(7) 1 calc R U P A 1
C27 C 0.1984(5) 0.1783(7) 0.3663(4) 0.0672(15) Uani 0.634(7) 1 d . U P A 1
H27A H 0.2101 0.0855 0.3741 0.101 Uiso 0.634(7) 1 calc R U P A 1
H27B H 0.2546 0.2304 0.2976 0.101 Uiso 0.634(7) 1 calc R U P A 1
H27C H 0.1064 0.2109 0.3550 0.101 Uiso 0.634(7) 1 calc R U P A 1
C28 C 0.1225(5) -0.0114(5) 0.6284(6) 0.0678(15) Uani 0.634(7) 1 d . U P A 1
H28A H 0.0324 0.0174 0.6497 0.102 Uiso 0.634(7) 1 calc R U P A 1
H28B H 0.1563 -0.0833 0.6972 0.102 Uiso 0.634(7) 1 calc R U P A 1
H28C H 0.1237 -0.0424 0.5627 0.102 Uiso 0.634(7) 1 calc R U P A 1
C29 C 0.2495(6) 0.0765(7) 0.8039(3) 0.0813(18) Uani 0.634(7) 1 d . U P A 1
H29A H 0.3233 0.0958 0.8363 0.122 Uiso 0.634(7) 1 calc R U P A 1
H29B H 0.2505 -0.0189 0.8246 0.122 Uiso 0.634(7) 1 calc R U P A 1
H29C H 0.1669 0.1085 0.8372 0.122 Uiso 0.634(7) 1 calc R U P A 1
C30 C 0.3812(5) 0.3446(6) 0.6534(7) 0.088(2) Uani 0.634(7) 1 d . U P A 1
H30A H 0.4765 0.3250 0.6464 0.132 Uiso 0.634(7) 1 calc R U P A 1
H30B H 0.3494 0.3231 0.7371 0.132 Uiso 0.634(7) 1 calc R U P A 1
H30C H 0.3598 0.4384 0.6092 0.132 Uiso 0.634(7) 1 calc R U P A 1
C31 C 0.3265(7) 0.2940(6) 0.5502(9) 0.0380(11) Uani 0.366(7) 1 d . U P A 2
C32 C 0.2869(9) 0.2787(9) 0.4516(6) 0.0402(12) Uani 0.366(7) 1 d . U P A 2
C33 C 0.224(2) 0.1633(16) 0.4905(12) 0.0354(13) Uani 0.366(7) 1 d . U P A 2
C34 C 0.2170(14) 0.1094(13) 0.6143(8) 0.0331(13) Uani 0.366(7) 1 d . U P A 2
C35 C 0.2841(8) 0.1903(9) 0.6513(7) 0.0356(12) Uani 0.366(7) 1 d . U P A 2
C36 C 0.4007(7) 0.4021(7) 0.5536(13) 0.085(3) Uani 0.366(7) 1 d . U P A 2
H36A H 0.3946 0.3997 0.6352 0.127 Uiso 0.366(7) 1 calc R U P A 2
H36B H 0.3630 0.4876 0.5021 0.127 Uiso 0.366(7) 1 calc R U P A 2
H36C H 0.4930 0.3895 0.5258 0.127 Uiso 0.366(7) 1 calc R U P A 2
C37 C 0.3067(10) 0.3750(10) 0.3239(7) 0.086(3) Uani 0.366(7) 1 d . U P A 2
H37A H 0.2321 0.4416 0.3070 0.129 Uiso 0.366(7) 1 calc R U P A 2
H37B H 0.3130 0.3271 0.2698 0.129 Uiso 0.366(7) 1 calc R U P A 2
H37C H 0.3876 0.4184 0.3129 0.129 Uiso 0.366(7) 1 calc R U P A 2
C38 C 0.1639(9) 0.1114(11) 0.4093(10) 0.072(3) Uani 0.366(7) 1 d . U P A 2
H38A H 0.1503 0.0177 0.4512 0.108 Uiso 0.366(7) 1 calc R U P A 2
H38B H 0.2234 0.1224 0.3374 0.108 Uiso 0.366(7) 1 calc R U P A 2
H38C H 0.0795 0.1608 0.3875 0.108 Uiso 0.366(7) 1 calc R U P A 2
C39 C 0.1433(8) -0.0078(7) 0.6879(9) 0.063(2) Uani 0.366(7) 1 d . U P A 2
H39A H 0.0537 0.0217 0.7100 0.094 Uiso 0.366(7) 1 calc R U P A 2
H39B H 0.1874 -0.0578 0.7598 0.094 Uiso 0.366(7) 1 calc R U P A 2
H39C H 0.1404 -0.0640 0.6422 0.094 Uiso 0.366(7) 1 calc R U P A 2
C40 C 0.3013(8) 0.1615(11) 0.7788(6) 0.068(2) Uani 0.366(7) 1 d . U P A 2
H40A H 0.3939 0.1646 0.7875 0.102 Uiso 0.366(7) 1 calc R U P A 2
H40B H 0.2732 0.0736 0.8273 0.102 Uiso 0.366(7) 1 calc R U P A 2
H40C H 0.2480 0.2274 0.8050 0.102 Uiso 0.366(7) 1 calc R U P A 2
C41 C 0.0067(2) 0.4360(2) 0.99040(18) 0.0626(5) Uani 1 1 d . U . B 2
H41A H 0.0542 0.4489 0.9116 0.075 Uiso 1 1 calc R U . B 2
H41B H -0.0820 0.4106 0.9895 0.075 Uiso 1 1 calc R U . B 2
C42 C 0.0774(3) 0.3250(3) 1.0825(2) 0.0775(7) Uani 1 1 d . U . B 2
H42A H 0.1672 0.3491 1.0809 0.093 Uiso 1 1 calc R U . B 2
H42B H 0.0319 0.3150 1.1615 0.093 Uiso 1 1 calc R U . B 2
C43 C 0.0868(3) 0.1947(3) 1.0678(3) 0.0907(8) Uani 1 1 d . U . B 2
H43A H -0.0015 0.1700 1.0681 0.136 Uiso 1 1 calc R U . B 2
H43B H 0.1308 0.1275 1.1333 0.136 Uiso 1 1 calc R U . B 2
H43C H 0.1373 0.2013 0.9923 0.136 Uiso 1 1 calc R U . B 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
S1 C3 1.7309(17) . ?
S1 C1 1.7689(14) . ?
S2 C5 1.7319(17) . ?
S2 C2 1.7551(14) . ?
O1 C7 1.3143(16) . ?
O1 Cr 1.9223(10) . ?
O2 C8 1.3510(16) . ?
O2 Cr 1.9891(9) . ?
O2 Cr 2.0036(9) 2_656 ?
C1 C7 1.384(2) . ?
C1 C2 1.445(2) . ?
C2 C8 1.3713(19) . ?
C3 C4 1.400(2) . ?
C3 C12 1.400(2) . ?
C4 C9 1.396(2) . ?
C4 C7 1.4524(18) . ?
C5 C16 1.399(2) . ?
C5 C6 1.404(2) . ?
C6 C13 1.396(2) . ?
C6 C8 1.4386(19) . ?
C9 C10 1.382(2) . ?
C10 C11 1.396(3) . ?
C11 C12 1.368(3) . ?
C13 C14 1.383(2) . ?
C14 C15 1.398(3) . ?
C15 C16 1.365(3) . ?
Cr O2 2.0036(9) 2_656 ?
Cr C35 2.172(8) . ?
Cr C21 2.192(4) . ?
Cr C31 2.201(6) . ?
Cr C34 2.217(14) . ?
Cr C22 2.223(14) . ?
Cr C33 2.23(2) . ?
Cr C25 2.233(4) . ?
Cr C24 2.235(5) . ?
Cr C32 2.265(8) . ?
C21 C25 1.416(5) . ?
C21 C22 1.438(6) . ?
C21 C26 1.491(5) . ?
C22 C23 1.402(7) . ?
C22 C27 1.485(8) . ?
C23 C24 1.417(4) . ?
C23 C28 1.496(6) . ?
C24 C25 1.404(5) . ?
C24 C29 1.515(5) . ?
C25 C30 1.493(4) . ?
C31 C32 1.391(9) . ?
C31 C35 1.392(8) . ?
C31 C36 1.504(8) . ?
C32 C33 1.383(10) . ?
C32 C37 1.524(9) . ?
C33 C34 1.397(13) . ?
C33 C38 1.538(13) . ?
C34 C35 1.415(9) . ?
C34 C39 1.493(10) . ?
C35 C40 1.497(8) . ?
C41 C41 1.497(5) 2_567 ?
C41 C42 1.500(3) . ?
C42 C43 1.497(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 S1 C1 91.88(7) . . ?
C5 S2 C2 92.23(7) . . ?
C7 O1 Cr 132.79(9) . . ?
C8 O2 Cr 121.96(8) . . ?
C8 O2 Cr 132.12(8) . 2_656 ?
Cr O2 Cr 103.04(4) . 2_656 ?
C7 C1 C2 131.21(12) . . ?
C7 C1 S1 111.80(10) . . ?
C2 C1 S1 116.95(10) . . ?
C8 C2 C1 130.59(13) . . ?
C8 C2 S2 110.61(10) . . ?
C1 C2 S2 118.72(10) . . ?
C4 C3 C12 121.12(15) . . ?
C4 C3 S1 111.40(11) . . ?
C12 C3 S1 127.47(14) . . ?
C9 C4 C3 119.54(14) . . ?
C9 C4 C7 127.20(14) . . ?
C3 C4 C7 113.26(13) . . ?
C16 C5 C6 120.77(16) . . ?
C16 C5 S2 127.70(14) . . ?
C6 C5 S2 111.53(11) . . ?
C13 C6 C5 120.03(14) . . ?
C13 C6 C8 128.55(14) . . ?
C5 C6 C8 111.41(13) . . ?
O1 C7 C1 129.38(12) . . ?
O1 C7 C4 118.99(12) . . ?
C1 C7 C4 111.63(12) . . ?
O2 C8 C2 125.21(12) . . ?
O2 C8 C6 120.62(12) . . ?
C2 C8 C6 114.17(12) . . ?
C10 C9 C4 119.07(17) . . ?
C9 C10 C11 120.65(17) . . ?
C12 C11 C10 121.29(15) . . ?
C11 C12 C3 118.32(17) . . ?
C14 C13 C6 118.57(16) . . ?
C13 C14 C15 120.76(17) . . ?
C16 C15 C14 121.52(16) . . ?
C15 C16 C5 118.34(17) . . ?
O1 Cr O2 91.79(4) . . ?
O1 Cr O2 92.46(4) . 2_656 ?
O2 Cr O2 76.96(4) . 2_656 ?
O1 Cr C35 97.82(19) . . ?
O2 Cr C35 158.4(2) . . ?
O2 Cr C35 121.6(3) 2_656 . ?
O1 Cr C21 110.35(12) . . ?
O2 Cr C21 105.64(15) . . ?
O2 Cr C21 156.78(12) 2_656 . ?
O1 Cr C31 93.1(2) . . ?
O2 Cr C31 123.5(2) . . ?
O2 Cr C31 158.6(2) 2_656 . ?
C35 Cr C31 37.1(2) . . ?
O1 Cr C34 132.5(2) . . ?
O2 Cr C34 135.6(2) . . ?
O2 Cr C34 100.0(3) 2_656 . ?
C35 Cr C34 37.6(3) . . ?
C31 Cr C34 61.7(4) . . ?
O1 Cr C22 148.2(2) . . ?
O2 Cr C22 100.2(2) . . ?
O2 Cr C22 118.9(2) 2_656 . ?
C21 Cr C22 38.0(2) . . ?
O1 Cr C33 154.0(4) . . ?
O2 Cr C33 102.6(4) . . ?
O2 Cr C33 111.7(3) 2_656 . ?
C35 Cr C33 61.9(5) . . ?
C31 Cr C33 60.9(5) . . ?
C34 Cr C33 36.6(4) . . ?
O1 Cr C25 89.62(10) . . ?
O2 Cr C25 139.12(16) . . ?
O2 Cr C25 143.80(16) 2_656 . ?
C21 Cr C25 37.33(14) . . ?
C22 Cr C25 62.1(3) . . ?
O1 Cr C24 104.94(12) . . ?
O2 Cr C24 161.82(12) . . ?
O2 Cr C24 108.78(12) 2_656 . ?
C21 Cr C24 62.17(16) . . ?
C22 Cr C24 61.7(3) . . ?
C25 Cr C24 36.64(14) . . ?
O1 Cr C32 121.5(3) . . ?
O2 Cr C32 97.39(19) . . ?
O2 Cr C32 145.9(3) 2_656 . ?
C35 Cr C32 61.2(3) . . ?
C31 Cr C32 36.3(2) . . ?
C34 Cr C32 60.5(4) . . ?
C33 Cr C32 35.8(3) . . ?
C25 C21 C22 107.3(4) . . ?
C25 C21 C26 127.5(4) . . ?
C22 C21 C26 125.0(5) . . ?
C25 C21 Cr 72.9(2) . . ?
C22 C21 Cr 72.2(6) . . ?
C26 C21 Cr 124.5(3) . . ?
C23 C22 C21 107.7(6) . . ?
C23 C22 C27 125.3(5) . . ?
C21 C22 C27 127.0(5) . . ?
C23 C22 Cr 73.5(6) . . ?
C21 C22 Cr 69.8(5) . . ?
C27 C22 Cr 121.7(9) . . ?
C22 C23 C24 108.4(5) . . ?
C22 C23 C28 126.4(4) . . ?
C24 C23 C28 124.9(5) . . ?
C22 C23 Cr 70.1(6) . . ?
C24 C23 Cr 70.4(3) . . ?
C28 C23 Cr 129.9(6) . . ?
C25 C24 C23 108.2(4) . . ?
C25 C24 C29 127.1(4) . . ?
C23 C24 C29 124.4(4) . . ?
C25 C24 Cr 71.6(2) . . ?
C23 C24 Cr 72.9(4) . . ?
C29 C24 Cr 125.4(3) . . ?
C24 C25 C21 108.2(3) . . ?
C24 C25 C30 125.4(4) . . ?
C21 C25 C30 126.3(5) . . ?
C24 C25 Cr 71.7(3) . . ?
C21 C25 Cr 69.8(2) . . ?
C30 C25 Cr 122.9(3) . . ?
C32 C31 C35 108.5(6) . . ?
C32 C31 C36 128.2(8) . . ?
C35 C31 C36 123.3(8) . . ?
C32 C31 Cr 74.4(5) . . ?
C35 C31 Cr 70.3(4) . . ?
C36 C31 Cr 121.7(5) . . ?
C33 C32 C31 108.0(8) . . ?
C33 C32 C37 126.5(9) . . ?
C31 C32 C37 125.5(8) . . ?
C33 C32 Cr 70.6(11) . . ?
C31 C32 Cr 69.4(4) . . ?
C37 C32 Cr 126.8(6) . . ?
C32 C33 C34 108.7(10) . . ?
C32 C33 C38 124.6(10) . . ?
C34 C33 C38 126.5(8) . . ?
C32 C33 Cr 73.6(9) . . ?
C34 C33 Cr 71.3(10) . . ?
C38 C33 Cr 124.9(15) . . ?
C33 C34 C35 107.1(9) . . ?
C33 C34 C39 123.7(8) . . ?
C35 C34 C39 129.1(8) . . ?
C33 C34 Cr 72.1(11) . . ?
C35 C34 Cr 69.5(6) . . ?
C39 C34 Cr 126.3(10) . . ?
C31 C35 C34 107.5(6) . . ?
C31 C35 C40 129.6(8) . . ?
C34 C35 C40 122.9(8) . . ?
C31 C35 Cr 72.6(4) . . ?
C34 C35 Cr 72.9(7) . . ?
C40 C35 Cr 120.1(5) . . ?
C41 C41 C42 114.2(2) 2_567 . ?
C43 C42 C41 115.0(2) . . ?

_refine_diff_density_max         0.445
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.045

_shelxl_version_number           2013-4


_chemical_compound_source        no
_chemical_properties_physical    ', Air-sensitive'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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_ThioindigoCryptandNa
_database_code_depnum_ccdc_archive 'CCDC 1561770'
_audit_update_record             
;
2017-07-12 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_audit_creation_date             2017-02-28
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'salt of thioindigo radical anions with cryptand[2,2,2] sodium'
_chemical_name_common            no
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H36 N2 Na1 O6, C16 H8 O2 S2'
_chemical_formula_sum            'C34 H44 N2 Na O8 S2'
_chemical_formula_weight         695.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   12.2584(3)
_cell_length_b                   14.4597(3)
_cell_length_c                   19.1968(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.589(2)
_cell_angle_gamma                90
_cell_volume                     3380.21(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    10780
_cell_measurement_theta_min      2.5130
_cell_measurement_theta_max      27.0800

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_F_000             1476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.122
_exptl_absorpt_coefficient_mu    0.225
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_T_min  0.90925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2283
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            29401
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.085
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13553
_reflns_number_gt                10803
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²+1.0991P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13553
_refine_ls_number_parameters     960
_refine_ls_number_restraints     436
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form
_vrf_PLAT111_ThioIndigo-CryptandNa 
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit  
RESPONSE: Inequal Occupancy factors of the disordered groups indicate that 
centre of symmetry is violated
;
_vrf_PLAT112_ThioIndigo-CryptandNa 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        c        100 %Fit  
RESPONSE: Inequal Occupancy factors of the disordered groups indicate that 
symmetry element c is violated
;
_vrf_PLAT113_ThioIndigo-CryptandNa 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      P21/c Check 
RESPONSE: Inequal Occupancy factors of the disordered groups indicate that 
space group P21/c is violated and reduced to P21
;
_vrf_PLAT214_ThioIndigo-CryptandNa 
;
PROBLEM: Atom C34A    (Anion/Solvent) ADP max/min Ratio          5.9 oblate
RESPONSE: atom c34a is element of disordered group
;
# end Validation Reply Form

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
Na1 Na 0.25593(15) 0.72574(17) 0.27784(11) 0.0272(4) Uani 1 1 d . U . . .
N11 N 0.2672(3) 0.7574(4) 0.4377(2) 0.0253(10) Uani 1 1 d . U . . .
N12 N 0.2477(3) 0.6930(4) 0.1359(2) 0.0244(8) Uani 1 1 d . U . . .
O101 O 0.1939(3) 0.8913(3) 0.3252(2) 0.0279(7) Uani 1 1 d . U . . .
O102 O 0.0981(3) 0.8043(3) 0.20295(19) 0.0277(8) Uani 1 1 d . U . . .
O103 O 0.1342(3) 0.6159(3) 0.3578(2) 0.0289(8) Uani 1 1 d . U . . .
O104 O 0.2317(3) 0.5573(3) 0.23989(19) 0.0274(8) Uani 1 1 d . U . . .
O105 O 0.4518(3) 0.7165(3) 0.35799(19) 0.0256(8) Uani 1 1 d . U . . .
O106 O 0.4229(3) 0.7820(3) 0.2213(2) 0.0263(8) Uani 1 1 d . U . . .
C101 C 0.2050(4) 0.8426(5) 0.4476(3) 0.0290(12) Uani 1 1 d . U . . .
H10A H 0.2257 0.8659 0.4958 0.035 Uiso 1 1 calc R U . . .
H10B H 0.1256 0.8277 0.4428 0.035 Uiso 1 1 calc R U . . .
C102 C 0.2244(5) 0.9173(5) 0.3964(3) 0.0324(11) Uani 1 1 d . U . . .
H10C H 0.1821 0.9729 0.4070 0.039 Uiso 1 1 calc R U . . .
H10D H 0.3033 0.9340 0.4026 0.039 Uiso 1 1 calc R U . . .
C103 C 0.0775(4) 0.8860(5) 0.3073(3) 0.0270(12) Uani 1 1 d . U . . .
H10E H 0.0410 0.9390 0.3275 0.032 Uiso 1 1 calc R U . . .
H10F H 0.0487 0.8281 0.3258 0.032 Uiso 1 1 calc R U . . .
C104 C 0.0561(4) 0.8876(5) 0.2291(3) 0.0290(12) Uani 1 1 d . U . . .
H10G H -0.0238 0.8924 0.2144 0.035 Uiso 1 1 calc R U . . .
H10H H 0.0927 0.9418 0.2104 0.035 Uiso 1 1 calc R U . . .
C105 C 0.0956(4) 0.8074(5) 0.1292(3) 0.0295(12) Uani 1 1 d . U . . .
H10I H 0.1434 0.8580 0.1156 0.035 Uiso 1 1 calc R U . . .
H10J H 0.0198 0.8193 0.1073 0.035 Uiso 1 1 calc R U . . .
C106 C 0.1356(4) 0.7158(5) 0.1042(3) 0.0291(12) Uani 1 1 d . U . . .
H10K H 0.0848 0.6664 0.1157 0.035 Uiso 1 1 calc R U . . .
H10L H 0.1344 0.7176 0.0526 0.035 Uiso 1 1 calc R U . . .
C107 C 0.2196(4) 0.6783(5) 0.4700(3) 0.0270(12) Uani 1 1 d . U . . .
H10M H 0.2026 0.6957 0.5174 0.032 Uiso 1 1 calc R U . . .
H10N H 0.2742 0.6275 0.4752 0.032 Uiso 1 1 calc R U . . .
C108 C 0.1165(4) 0.6442(5) 0.4276(3) 0.0291(12) Uani 1 1 d . U . . .
H10O H 0.0871 0.5912 0.4522 0.035 Uiso 1 1 calc R U . . .
H10P H 0.0608 0.6940 0.4244 0.035 Uiso 1 1 calc R U . . .
C109 C 0.1928(5) 0.5320(5) 0.3574(3) 0.0315(12) Uani 1 1 d . U . . .
H10Q H 0.1644 0.4870 0.3897 0.038 Uiso 1 1 calc R U . . .
H10R H 0.2717 0.5426 0.3727 0.038 Uiso 1 1 calc R U . . .
C110 C 0.1777(4) 0.4953(5) 0.2833(3) 0.0331(13) Uani 1 1 d . U . . .
H11A H 0.2099 0.4326 0.2818 0.040 Uiso 1 1 calc R U . . .
H11B H 0.0985 0.4913 0.2662 0.040 Uiso 1 1 calc R U . . .
C111 C 0.2083(4) 0.5313(5) 0.1682(3) 0.0298(12) Uani 1 1 d . U . . .
H11C H 0.1286 0.5373 0.1531 0.036 Uiso 1 1 calc R U . . .
H11D H 0.2299 0.4662 0.1619 0.036 Uiso 1 1 calc R U . . .
C112 C 0.2721(5) 0.5942(5) 0.1249(3) 0.0290(11) Uani 1 1 d . U . . .
H11E H 0.3517 0.5833 0.1375 0.035 Uiso 1 1 calc R U . . .
H11F H 0.2540 0.5789 0.0747 0.035 Uiso 1 1 calc R U . . .
C113 C 0.3828(4) 0.7689(4) 0.4661(3) 0.0239(11) Uani 1 1 d . U . . .
H11G H 0.3908 0.7570 0.5172 0.029 Uiso 1 1 calc R U . . .
H11H H 0.4054 0.8336 0.4588 0.029 Uiso 1 1 calc R U . . .
C114 C 0.4569(4) 0.7052(5) 0.4323(3) 0.0263(12) Uani 1 1 d . U . . .
H11I H 0.5334 0.7158 0.4534 0.032 Uiso 1 1 calc R U . . .
H11J H 0.4373 0.6406 0.4425 0.032 Uiso 1 1 calc R U . . .
C115 C 0.5020(4) 0.8015(5) 0.3386(3) 0.0273(11) Uani 1 1 d . U . . .
H11K H 0.5711 0.8128 0.3695 0.033 Uiso 1 1 calc R U . . .
H11L H 0.4519 0.8543 0.3430 0.033 Uiso 1 1 calc R U . . .
C116 C 0.5249(4) 0.7912(5) 0.2647(3) 0.0267(12) Uani 1 1 d . U . . .
H11M H 0.5650 0.8460 0.2503 0.032 Uiso 1 1 calc R U . . .
H11N H 0.5709 0.7358 0.2600 0.032 Uiso 1 1 calc R U . . .
C117 C 0.4395(4) 0.7518(5) 0.1530(3) 0.0276(13) Uani 1 1 d . U . . .
H11O H 0.4705 0.6885 0.1550 0.033 Uiso 1 1 calc R U . . .
H11P H 0.4916 0.7935 0.1327 0.033 Uiso 1 1 calc R U . . .
C118 C 0.3297(4) 0.7528(5) 0.1083(3) 0.0282(12) Uani 1 1 d . U . . .
H11Q H 0.3015 0.8170 0.1052 0.034 Uiso 1 1 calc R U . . .
H11R H 0.3399 0.7323 0.0603 0.034 Uiso 1 1 calc R U . . .
Na2 Na 0.74192(15) 0.50143(17) 0.22279(11) 0.0265(4) Uani 1 1 d . U . . .
N21 N 0.7501(3) 0.5324(4) 0.3643(2) 0.0244(8) Uani 1 1 d . U . . .
N22 N 0.7305(3) 0.4678(4) 0.0635(2) 0.0235(10) Uani 1 1 d . U . . .
O21 O 0.8989(3) 0.4209(3) 0.29780(18) 0.0265(8) Uani 1 1 d . U . . .
O22 O 0.8036(3) 0.3362(3) 0.1756(2) 0.0315(8) Uani 1 1 d . U . . .
O23 O 0.7665(3) 0.6697(3) 0.26026(18) 0.0253(7) Uani 1 1 d . U . . .
O24 O 0.8634(3) 0.6096(3) 0.1427(2) 0.0289(8) Uani 1 1 d . U . . .
O25 O 0.5756(3) 0.4448(3) 0.27878(19) 0.0273(8) Uani 1 1 d . U . . .
O26 O 0.5454(3) 0.5104(3) 0.14181(19) 0.0275(8) Uani 1 1 d . U . . .
C201 C 0.8611(4) 0.5097(5) 0.3964(3) 0.0280(11) Uani 1 1 d . U . . .
H20A H 0.8615 0.5085 0.4480 0.034 Uiso 1 1 calc R U . . .
H20B H 0.9120 0.5591 0.3849 0.034 Uiso 1 1 calc R U . . .
C202 C 0.9022(4) 0.4185(5) 0.3727(3) 0.0298(12) Uani 1 1 d . U . . .
H20C H 0.9783 0.4077 0.3944 0.036 Uiso 1 1 calc R U . . .
H20D H 0.8553 0.3677 0.3868 0.036 Uiso 1 1 calc R U . . .
C203 C 0.9415(4) 0.3379(5) 0.2709(3) 0.0275(11) Uani 1 1 d . U . . .
H20E H 0.9052 0.2834 0.2893 0.033 Uiso 1 1 calc R U . . .
H20F H 1.0214 0.3334 0.2856 0.033 Uiso 1 1 calc R U . . .
C204 C 0.9202(4) 0.3405(5) 0.1931(3) 0.0296(12) Uani 1 1 d . U . . .
H20G H 0.9496 0.3983 0.1748 0.036 Uiso 1 1 calc R U . . .
H20H H 0.9559 0.2873 0.1724 0.036 Uiso 1 1 calc R U . . .
C205 C 0.7721(5) 0.3090(5) 0.1041(3) 0.0330(11) Uani 1 1 d . U . . .
H20I H 0.6929 0.2934 0.0981 0.040 Uiso 1 1 calc R U . . .
H20J H 0.8134 0.2528 0.0939 0.040 Uiso 1 1 calc R U . . .
C206 C 0.7934(4) 0.3843(5) 0.0522(3) 0.0296(12) Uani 1 1 d . U . . .
H20K H 0.8727 0.3993 0.0574 0.035 Uiso 1 1 calc R U . . .
H20L H 0.7729 0.3614 0.0039 0.035 Uiso 1 1 calc R U . . .
C207 C 0.7274(4) 0.6302(5) 0.3757(3) 0.0255(10) Uani 1 1 d . U . . .
H20M H 0.7472 0.6449 0.4259 0.031 Uiso 1 1 calc R U . . .
H20N H 0.6476 0.6412 0.3644 0.031 Uiso 1 1 calc R U . . .
C208 C 0.7886(4) 0.6947(5) 0.3325(3) 0.0271(11) Uani 1 1 d . U . . .
H20O H 0.7648 0.7593 0.3392 0.033 Uiso 1 1 calc R U . . .
H20P H 0.8684 0.6906 0.3476 0.033 Uiso 1 1 calc R U . . .
C209 C 0.8189(4) 0.7308(5) 0.2171(3) 0.0303(12) Uani 1 1 d . U . . .
H20Q H 0.8981 0.7351 0.2341 0.036 Uiso 1 1 calc R U . . .
H20R H 0.7865 0.7934 0.2189 0.036 Uiso 1 1 calc R U . . .
C210 C 0.8045(5) 0.6960(5) 0.1441(3) 0.0318(13) Uani 1 1 d . U . . .
H21A H 0.7256 0.6862 0.1283 0.038 Uiso 1 1 calc R U . . .
H21B H 0.8337 0.7413 0.1124 0.038 Uiso 1 1 calc R U . . .
C211 C 0.8815(4) 0.5831(5) 0.0741(3) 0.0294(12) Uani 1 1 d . U . . .
H21C H 0.9382 0.5340 0.0771 0.035 Uiso 1 1 calc R U . . .
H21D H 0.9102 0.6368 0.0500 0.035 Uiso 1 1 calc R U . . .
C212 C 0.7788(4) 0.5479(5) 0.0309(3) 0.0264(12) Uani 1 1 d . U . . .
H21E H 0.7239 0.5984 0.0250 0.032 Uiso 1 1 calc R U . . .
H21F H 0.7968 0.5302 -0.0162 0.032 Uiso 1 1 calc R U . . .
C213 C 0.6673(4) 0.4750(5) 0.3925(3) 0.0293(12) Uani 1 1 d . U . . .
H21G H 0.6565 0.4979 0.4399 0.035 Uiso 1 1 calc R U . . .
H21H H 0.6951 0.4108 0.3976 0.035 Uiso 1 1 calc R U . . .
C214 C 0.5588(4) 0.4744(5) 0.3479(3) 0.0295(13) Uani 1 1 d . U . . .
H21I H 0.5076 0.4318 0.3681 0.035 Uiso 1 1 calc R U . . .
H21J H 0.5264 0.5372 0.3461 0.035 Uiso 1 1 calc R U . . .
C215 C 0.4734(4) 0.4349(5) 0.2360(3) 0.0313(14) Uani 1 1 d . U . . .
H21K H 0.4262 0.4893 0.2415 0.038 Uiso 1 1 calc R U . . .
H21L H 0.4346 0.3790 0.2499 0.038 Uiso 1 1 calc R U . . .
C216 C 0.4966(4) 0.4267(5) 0.1613(3) 0.0290(12) Uani 1 1 d . U . . .
H21M H 0.5469 0.3742 0.1563 0.035 Uiso 1 1 calc R U . . .
H21N H 0.4274 0.4153 0.1304 0.035 Uiso 1 1 calc R U . . .
C217 C 0.5399(4) 0.5236(5) 0.0676(3) 0.0299(13) Uani 1 1 d . U . . .
H21O H 0.5614 0.5880 0.0580 0.036 Uiso 1 1 calc R U . . .
H21P H 0.4632 0.5147 0.0463 0.036 Uiso 1 1 calc R U . . .
C218 C 0.6149(4) 0.4566(5) 0.0334(3) 0.0297(13) Uani 1 1 d . U . . .
H21Q H 0.5911 0.3923 0.0406 0.036 Uiso 1 1 calc R U . . .
H21R H 0.6085 0.4684 -0.0177 0.036 Uiso 1 1 calc R U . . .
C301 C 0.7103(4) 0.7870(5) -0.0467(3) 0.0291(11) Uani 1 1 d . U . . .
C302 C 0.7539(4) 0.8607(5) 0.0004(3) 0.0280(11) Uani 1 1 d . U . . .
C305 C 0.5936(4) 0.6658(5) -0.0996(3) 0.0307(11) Uani 1 1 d . U . . .
C306 C 0.6887(5) 0.6615(5) -0.1318(4) 0.0368(12) Uani 1 1 d . U . . .
C307 C 0.7014(5) 0.5915(5) -0.1809(3) 0.0445(14) Uani 1 1 d . U . . .
H307 H 0.7667 0.5887 -0.2031 0.053 Uiso 1 1 calc R U . . .
C308 C 0.6224(5) 0.5289(5) -0.1968(3) 0.0445(15) Uani 1 1 d . U . . .
H308 H 0.6325 0.4810 -0.2293 0.053 Uiso 1 1 calc R U . . .
C309 C 0.5244(5) 0.5335(5) -0.1656(4) 0.0420(16) Uani 1 1 d . U . . .
H309 H 0.4675 0.4901 -0.1785 0.050 Uiso 1 1 calc R U . . .
C310 C 0.5100(5) 0.5999(5) -0.1168(3) 0.0372(14) Uani 1 1 d . U . . .
H310 H 0.4445 0.6017 -0.0947 0.045 Uiso 1 1 calc R U . . .
C311 C 0.7880(4) 0.9770(4) 0.0986(3) 0.0343(12) Uani 1 1 d . U . . .
C312 C 0.8736(5) 0.9730(4) 0.0544(3) 0.0328(12) Uani 1 1 d . U . . .
C313 C 0.9633(5) 1.0338(5) 0.0736(3) 0.0342(13) Uani 1 1 d . U . . .
H313 H 1.0233 1.0357 0.0465 0.041 Uiso 1 1 calc R U . . .
C314 C 0.9631(4) 1.0903(4) 0.1321(3) 0.0307(13) Uani 1 1 d . U . . .
H314 H 1.0227 1.1314 0.1443 0.037 Uiso 1 1 calc R U . . .
C315 C 0.8768(5) 1.0873(5) 0.1730(3) 0.0363(15) Uani 1 1 d . U . . .
H315 H 0.8781 1.1258 0.2132 0.044 Uiso 1 1 calc R U . . .
C316 C 0.7873(5) 1.0275(5) 0.1550(3) 0.0386(14) Uani 1 1 d . U . . .
H316 H 0.7283 1.0239 0.1829 0.046 Uiso 1 1 calc R U . . .
C33A C 0.7534(11) 0.7422(9) -0.0922(8) 0.035(3) Uani 0.505(7) 1 d . U P A 1
O31A O 0.8525(9) 0.7554(7) -0.1093(5) 0.046(3) Uani 0.505(7) 1 d . U P A 1
S31A S 0.5712(3) 0.7460(2) -0.03209(18) 0.0258(10) Uani 0.505(7) 1 d . U P A 1
C33B C 0.6166(11) 0.7464(8) -0.0528(6) 0.030(2) Uani 0.495(7) 1 d . U P A 2
O31B O 0.5414(7) 0.7638(8) -0.0055(6) 0.052(3) Uani 0.495(7) 1 d . U P A 2
S31B S 0.7930(3) 0.7409(3) -0.1138(2) 0.0355(11) Uani 0.495(7) 1 d . U P A 2
C34A C 0.8487(8) 0.9081(7) 0.0000(4) 0.0238(16) Uani 0.619(7) 1 d . U P B 1
O32A O 0.9170(6) 0.8923(7) -0.0492(4) 0.038(2) Uani 0.619(7) 1 d . U P B 1
S32A S 0.6772(2) 0.90005(19) 0.07084(14) 0.0255(8) Uani 0.619(7) 1 d . U P B 1
C34B C 0.7271(10) 0.8978(8) 0.0476(6) 0.034(2) Uani 0.381(7) 1 d . U P B 2
O32B O 0.6343(12) 0.8790(9) 0.0771(7) 0.054(3) Uani 0.381(7) 1 d . U P B 2
S32B S 0.8973(4) 0.9057(4) -0.0211(3) 0.0341(12) Uani 0.381(7) 1 d . U P B 2
C401 C 0.2496(4) 0.3639(5) 0.5001(3) 0.0302(12) Uani 1 1 d D U . . .
C402 C 0.2947(4) 0.4361(4) 0.5437(3) 0.0288(11) Uani 1 1 d . U . . .
C405 C 0.1270(4) 0.2500(4) 0.4417(3) 0.0286(11) Uani 1 1 d D U . . .
C406 C 0.2151(4) 0.2548(4) 0.4035(3) 0.0334(12) Uani 1 1 d D U . . .
C407 C 0.2085(5) 0.1932(5) 0.3421(4) 0.0379(14) Uani 1 1 d . U . . .
H407 H 0.2663 0.1921 0.3131 0.045 Uiso 1 1 calc R U . . .
C408 C 0.1208(5) 0.1390(5) 0.3274(3) 0.0351(14) Uani 1 1 d . U . . .
H408 H 0.1166 0.1004 0.2871 0.042 Uiso 1 1 calc R U . . .
C409 C 0.0349(4) 0.1372(5) 0.3693(3) 0.0343(13) Uani 1 1 d . U . . .
H409 H -0.0259 0.0970 0.3579 0.041 Uiso 1 1 calc R U . . .
C410 C 0.0385(4) 0.1930(5) 0.4262(3) 0.0309(12) Uani 1 1 d . U . . .
H410 H -0.0195 0.1925 0.4550 0.037 Uiso 1 1 calc R U . . .
C411 C 0.3160(5) 0.5577(5) 0.6290(3) 0.0347(12) Uani 1 1 d D U . . .
C412 C 0.4148(4) 0.5602(4) 0.5990(3) 0.0305(12) Uani 1 1 d D U . . .
C413 C 0.4940(5) 0.6239(5) 0.6194(3) 0.0352(13) Uani 1 1 d . U . . .
H413 H 0.5622 0.6228 0.6003 0.042 Uiso 1 1 calc R U . . .
C414 C 0.4738(6) 0.6894(6) 0.6675(4) 0.0452(16) Uani 1 1 d . U . . .
H414 H 0.5274 0.7355 0.6806 0.054 Uiso 1 1 calc R U . . .
C415 C 0.3768(6) 0.6896(6) 0.6973(3) 0.0525(17) Uani 1 1 d . U . . .
H415 H 0.3645 0.7350 0.7313 0.063 Uiso 1 1 calc R U . . .
C416 C 0.2961(5) 0.6225(5) 0.6775(3) 0.0474(15) Uani 1 1 d . U . . .
H416 H 0.2287 0.6224 0.6975 0.057 Uiso 1 1 calc R U . . .
C43A C 0.1541(6) 0.3196(6) 0.4983(4) 0.0320(15) Uani 0.861(5) 1 d D U P C 1
O41A O 0.0811(3) 0.3319(4) 0.5436(3) 0.0310(12) Uani 0.861(5) 1 d . U P C 1
S41A S 0.32273(14) 0.32666(15) 0.42853(10) 0.0324(6) Uani 0.861(5) 1 d D U P C
1
C43B C 0.2798(9) 0.3326(11) 0.4400(8) 0.035(4) Uani 0.139(5) 1 d D U P C 2
O41B O 0.376(2) 0.364(2) 0.4230(16) 0.057(8) Uani 0.139(5) 1 d . U P C 2
S41B S 0.1145(8) 0.3206(9) 0.5154(6) 0.0261(18) Uani 0.139(5) 1 d D U P C 2
C44A C 0.2495(8) 0.4827(7) 0.5910(5) 0.031(2) Uani 0.607(6) 1 d D U P D 1
O42A O 0.1465(7) 0.4648(7) 0.6099(5) 0.059(3) Uani 0.607(6) 1 d . U P D 1
S42A S 0.4282(2) 0.4808(2) 0.53183(16) 0.0279(8) Uani 0.607(6) 1 d . U P D 1
C44B C 0.3894(12) 0.4852(11) 0.5461(9) 0.028(2) Uani 0.393(6) 1 d D U P D 2
O42B O 0.4668(8) 0.4625(8) 0.5109(7) 0.031(2) Uani 0.393(6) 1 d . U P D 2
S42B S 0.2099(4) 0.4828(4) 0.6124(2) 0.0322(12) Uani 0.393(6) 1 d . U P D 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
Na1 O102 2.542(4) . ?
Na1 O104 2.549(5) . ?
Na1 O106 2.557(4) . ?
Na1 O101 2.701(5) . ?
Na1 O105 2.702(4) . ?
Na1 N12 2.755(5) . ?
Na1 O103 2.762(4) . ?
N11 C107 1.454(8) . ?
N11 C113 1.468(6) . ?
N11 C101 1.472(8) . ?
N12 C118 1.470(7) . ?
N12 C106 1.475(7) . ?
N12 C112 1.479(8) . ?
O101 C102 1.425(7) . ?
O101 C103 1.431(6) . ?
O102 C105 1.414(6) . ?
O102 C104 1.425(7) . ?
O103 C109 1.411(8) . ?
O103 C108 1.440(7) . ?
O104 C111 1.424(6) . ?
O104 C110 1.437(7) . ?
O105 C114 1.430(6) . ?
O105 C115 1.442(7) . ?
O106 C117 1.419(6) . ?
O106 C116 1.426(6) . ?
C101 C102 1.498(9) . ?
C103 C104 1.492(7) . ?
C105 C106 1.510(9) . ?
C107 C108 1.505(8) . ?
C109 C110 1.509(8) . ?
C111 C112 1.509(8) . ?
C113 C114 1.492(8) . ?
C115 C116 1.483(7) . ?
C117 C118 1.511(8) . ?
Na2 O23 2.545(5) . ?
Na2 O25 2.547(4) . ?
Na2 O21 2.549(4) . ?
Na2 O22 2.694(5) . ?
Na2 O26 2.716(4) . ?
Na2 N21 2.743(5) . ?
Na2 O24 2.748(4) . ?
N21 C213 1.462(7) . ?
N21 C207 1.464(8) . ?
N21 C201 1.464(7) . ?
N22 C206 1.462(8) . ?
N22 C212 1.473(8) . ?
N22 C218 1.476(6) . ?
O21 C203 1.429(7) . ?
O21 C202 1.433(6) . ?
O22 C204 1.431(6) . ?
O22 C205 1.437(7) . ?
O23 C209 1.415(7) . ?
O23 C208 1.429(6) . ?
O24 C211 1.414(6) . ?
O24 C210 1.444(8) . ?
O25 C215 1.425(7) . ?
O25 C214 1.431(7) . ?
O26 C216 1.419(8) . ?
O26 C217 1.431(6) . ?
C201 C202 1.501(9) . ?
C203 C204 1.488(8) . ?
C205 C206 1.518(9) . ?
C207 C208 1.504(8) . ?
C209 C210 1.479(8) . ?
C211 C212 1.514(8) . ?
C213 C214 1.498(8) . ?
C215 C216 1.498(7) . ?
C217 C218 1.535(8) . ?
C301 C33A 1.251(14) . ?
C301 C33B 1.283(13) . ?
C301 C302 1.460(9) . ?
C301 S31B 1.851(6) . ?
C301 S31A 1.857(6) . ?
C302 C34B 1.134(13) . ?
C302 C34A 1.350(11) . ?
C302 S32A 1.824(6) . ?
C302 S32B 1.962(7) . ?
C305 C306 1.383(7) . ?
C305 C310 1.409(9) . ?
C305 C33B 1.478(10) . ?
C305 S31A 1.783(7) . ?
C306 C307 1.404(9) . ?
C306 C33A 1.559(12) . ?
C306 S31B 1.724(7) . ?
C307 C308 1.335(9) . ?
C308 C309 1.404(8) . ?
C309 C310 1.367(10) . ?
C311 C316 1.306(8) . ?
C311 C312 1.424(8) . ?
C311 C34B 1.630(12) . ?
C311 S32A 1.788(6) . ?
C312 C34A 1.412(10) . ?
C312 C313 1.423(9) . ?
C312 S32B 1.798(8) . ?
C313 C314 1.389(9) . ?
C314 C315 1.388(7) . ?
C315 C316 1.410(9) . ?
C33A O31A 1.309(16) . ?
C33B O31B 1.388(15) . ?
C34A O32A 1.351(12) . ?
C34B O32B 1.355(18) . ?
C401 C43B 1.331(10) . ?
C401 C43A 1.331(9) . ?
C401 C402 1.410(9) . ?
C401 S41A 1.808(5) . ?
C401 S41B 1.825(11) . ?
C402 C44A 1.305(12) . ?
C402 C44B 1.356(15) . ?
C402 S42A 1.797(5) . ?
C402 S42B 1.896(7) . ?
C405 C410 1.367(8) . ?
C405 C406 1.375(7) . ?
C405 C43A 1.490(8) . ?
C405 S41B 1.765(14) . ?
C406 C407 1.473(8) . ?
C406 C43B 1.503(8) . ?
C406 S41A 1.705(6) . ?
C407 C408 1.334(9) . ?
C408 C409 1.397(7) . ?
C409 C410 1.355(9) . ?
C411 C416 1.363(9) . ?
C411 C412 1.399(7) . ?
C411 C44A 1.495(8) . ?
C411 S42B 1.694(8) . ?
C412 C413 1.363(9) . ?
C412 C44B 1.495(8) . ?
C412 S42A 1.749(7) . ?
C413 C414 1.366(10) . ?
C414 C415 1.377(9) . ?
C415 C416 1.407(10) . ?
C43A O41A 1.330(8) . ?
C43B O41B 1.34(3) . ?
C44A O42A 1.377(12) . ?
C44B O42B 1.270(18) . ?

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
O102 Na1 O104 102.05(15) . . ?
O102 Na1 O106 102.27(14) . . ?
O104 Na1 O106 104.80(14) . . ?
O102 Na1 O101 64.48(14) . . ?
O104 Na1 O101 156.18(13) . . ?
O106 Na1 O101 97.51(14) . . ?
O102 Na1 O105 155.93(17) . . ?
O104 Na1 O105 100.51(15) . . ?
O106 Na1 O105 63.58(12) . . ?
O101 Na1 O105 96.78(14) . . ?
O102 Na1 N12 65.07(14) . . ?
O104 Na1 N12 64.10(15) . . ?
O106 Na1 N12 64.89(13) . . ?
O101 Na1 N12 120.37(17) . . ?
O105 Na1 N12 118.93(12) . . ?
O102 Na1 O103 98.43(13) . . ?
O104 Na1 O103 63.71(13) . . ?
O106 Na1 O103 158.18(16) . . ?
O101 Na1 O103 97.56(13) . . ?
O105 Na1 O103 98.99(14) . . ?
N12 Na1 O103 119.33(16) . . ?
C107 N11 C113 110.4(5) . . ?
C107 N11 C101 111.4(4) . . ?
C113 N11 C101 110.5(5) . . ?
C118 N12 C106 111.2(5) . . ?
C118 N12 C112 111.0(4) . . ?
C106 N12 C112 110.6(5) . . ?
C118 N12 Na1 107.8(3) . . ?
C106 N12 Na1 107.3(3) . . ?
C112 N12 Na1 108.8(4) . . ?
C102 O101 C103 113.0(4) . . ?
C102 O101 Na1 120.2(4) . . ?
C103 O101 Na1 100.5(3) . . ?
C105 O102 C104 111.1(4) . . ?
C105 O102 Na1 120.5(3) . . ?
C104 O102 Na1 117.4(3) . . ?
C109 O103 C108 112.4(5) . . ?
C109 O103 Na1 100.5(3) . . ?
C108 O103 Na1 120.2(4) . . ?
C111 O104 C110 109.9(4) . . ?
C111 O104 Na1 122.2(4) . . ?
C110 O104 Na1 118.5(3) . . ?
C114 O105 C115 112.6(4) . . ?
C114 O105 Na1 120.5(2) . . ?
C115 O105 Na1 100.9(3) . . ?
C117 O106 C116 111.1(3) . . ?
C117 O106 Na1 120.0(3) . . ?
C116 O106 Na1 118.2(3) . . ?
N11 C101 C102 113.3(4) . . ?
O101 C102 C101 113.3(6) . . ?
O101 C103 C104 107.3(4) . . ?
O102 C104 C103 108.2(5) . . ?
O102 C105 C106 108.6(5) . . ?
N12 C106 C105 112.7(5) . . ?
N11 C107 C108 112.4(5) . . ?
O103 C108 C107 112.9(4) . . ?
O103 C109 C110 107.5(5) . . ?
O104 C110 C109 108.1(5) . . ?
O104 C111 C112 108.2(5) . . ?
N12 C112 C111 112.1(4) . . ?
N11 C113 C114 112.3(5) . . ?
O105 C114 C113 113.8(5) . . ?
O105 C115 C116 107.1(5) . . ?
O106 C116 C115 108.6(4) . . ?
O106 C117 C118 108.0(4) . . ?
N12 C118 C117 113.1(5) . . ?
O23 Na2 O25 105.23(14) . . ?
O23 Na2 O21 102.69(15) . . ?
O25 Na2 O21 101.76(14) . . ?
O23 Na2 O22 156.08(13) . . ?
O25 Na2 O22 97.23(15) . . ?
O21 Na2 O22 64.03(14) . . ?
O23 Na2 O26 100.64(15) . . ?
O25 Na2 O26 63.67(12) . . ?
O21 Na2 O26 155.20(17) . . ?
O22 Na2 O26 96.59(14) . . ?
O23 Na2 N21 64.82(15) . . ?
O25 Na2 N21 64.84(13) . . ?
O21 Na2 N21 64.88(13) . . ?
O22 Na2 N21 119.85(17) . . ?
O26 Na2 N21 119.22(12) . . ?
O23 Na2 O24 63.88(12) . . ?
O25 Na2 O24 158.52(16) . . ?
O21 Na2 O24 98.82(13) . . ?
O22 Na2 O24 97.22(13) . . ?
O26 Na2 O24 98.91(14) . . ?
N21 Na2 O24 120.01(16) . . ?
C213 N21 C207 109.9(4) . . ?
C213 N21 C201 111.6(5) . . ?
C207 N21 C201 109.7(5) . . ?
C213 N21 Na2 109.1(3) . . ?
C207 N21 Na2 108.6(3) . . ?
C201 N21 Na2 107.9(3) . . ?
C206 N22 C212 110.0(4) . . ?
C206 N22 C218 110.5(5) . . ?
C212 N22 C218 109.5(5) . . ?
C203 O21 C202 111.9(4) . . ?
C203 O21 Na2 117.6(3) . . ?
C202 O21 Na2 120.7(3) . . ?
C204 O22 C205 112.8(4) . . ?
C204 O22 Na2 101.2(3) . . ?
C205 O22 Na2 120.6(4) . . ?
C209 O23 C208 111.2(5) . . ?
C209 O23 Na2 118.6(3) . . ?
C208 O23 Na2 121.3(4) . . ?
C211 O24 C210 112.6(5) . . ?
C211 O24 Na2 121.3(4) . . ?
C210 O24 Na2 100.2(3) . . ?
C215 O25 C214 110.8(4) . . ?
C215 O25 Na2 118.8(3) . . ?
C214 O25 Na2 120.1(3) . . ?
C216 O26 C217 113.8(5) . . ?
C216 O26 Na2 100.5(3) . . ?
C217 O26 Na2 120.9(3) . . ?
N21 C201 C202 113.4(5) . . ?
O21 C202 C201 108.1(5) . . ?
O21 C203 C204 108.2(5) . . ?
O22 C204 C203 106.9(4) . . ?
O22 C205 C206 112.5(5) . . ?
N22 C206 C205 111.2(4) . . ?
N21 C207 C208 113.7(4) . . ?
O23 C208 C207 109.1(5) . . ?
O23 C209 C210 109.2(5) . . ?
O24 C210 C209 107.8(5) . . ?
O24 C211 C212 113.0(4) . . ?
N22 C212 C211 112.4(5) . . ?
N21 C213 C214 113.5(5) . . ?
O25 C214 C213 108.6(4) . . ?
O25 C215 C216 108.0(4) . . ?
O26 C216 C215 108.5(5) . . ?
O26 C217 C218 112.3(5) . . ?
N22 C218 C217 111.0(5) . . ?
C33A C301 C302 131.0(7) . . ?
C33B C301 C302 130.6(7) . . ?
C33B C301 S31B 109.2(6) . . ?
C302 C301 S31B 120.2(4) . . ?
C33A C301 S31A 114.1(7) . . ?
C302 C301 S31A 114.6(4) . . ?
C34B C302 C301 136.2(7) . . ?
C34A C302 C301 128.4(6) . . ?
C34A C302 S32A 111.4(6) . . ?
C301 C302 S32A 120.2(4) . . ?
C34B C302 S32B 111.2(8) . . ?
C301 C302 S32B 112.6(4) . . ?
C306 C305 C310 119.5(6) . . ?
C306 C305 C33B 101.3(7) . . ?
C310 C305 C33B 139.2(7) . . ?
C306 C305 S31A 124.2(5) . . ?
C310 C305 S31A 116.2(4) . . ?
C305 C306 C307 119.8(6) . . ?
C305 C306 C33A 98.9(7) . . ?
C307 C306 C33A 141.1(7) . . ?
C305 C306 S31B 121.6(5) . . ?
C307 C306 S31B 118.6(4) . . ?
C308 C307 C306 120.6(5) . . ?
C307 C308 C309 120.3(6) . . ?
C310 C309 C308 120.6(7) . . ?
C309 C310 C305 119.2(5) . . ?
C316 C311 C312 126.2(5) . . ?
C316 C311 C34B 147.5(7) . . ?
C312 C311 C34B 86.1(6) . . ?
C316 C311 S32A 121.2(4) . . ?
C312 C311 S32A 112.6(4) . . ?
C34A C312 C313 134.2(6) . . ?
C34A C312 C311 110.9(6) . . ?
C313 C312 C311 114.9(5) . . ?
C313 C312 S32B 110.6(4) . . ?
C311 C312 S32B 134.4(4) . . ?
C314 C313 C312 120.0(5) . . ?
C315 C314 C313 120.7(6) . . ?
C314 C315 C316 120.2(6) . . ?
C311 C316 C315 117.9(5) . . ?
C301 C33A O31A 125.3(11) . . ?
C301 C33A C306 119.7(10) . . ?
O31A C33A C306 114.9(10) . . ?
C305 S31A C301 82.9(3) . . ?
C301 C33B O31B 120.8(9) . . ?
C301 C33B C305 121.5(9) . . ?
O31B C33B C305 116.5(9) . . ?
C306 S31B C301 85.8(3) . . ?
C302 C34A O32A 121.5(9) . . ?
C302 C34A C312 116.4(8) . . ?
O32A C34A C312 122.1(8) . . ?
C311 S32A C302 88.6(3) . . ?
C302 C34B O32B 125.0(11) . . ?
C302 C34B C311 131.0(10) . . ?
O32B C34B C311 103.8(9) . . ?
C312 S32B C302 77.2(3) . . ?
C43B C401 C402 129.5(6) . . ?
C43A C401 C402 131.0(5) . . ?
C43A C401 S41A 110.4(5) . . ?
C402 C401 S41A 118.4(4) . . ?
C43B C401 S41B 111.7(7) . . ?
C402 C401 S41B 117.5(5) . . ?
C44A C402 C401 128.7(6) . . ?
C44B C402 C401 133.1(6) . . ?
C44A C402 S42A 111.6(6) . . ?
C401 C402 S42A 119.5(4) . . ?
C44B C402 S42B 109.0(6) . . ?
C401 C402 S42B 117.8(4) . . ?
C410 C405 C406 124.5(4) . . ?
C410 C405 C43A 132.1(5) . . ?
C406 C405 C43A 103.4(4) . . ?
C410 C405 S41B 112.5(5) . . ?
C406 C405 S41B 122.9(4) . . ?
C405 C406 C407 115.0(4) . . ?
C405 C406 C43B 101.2(4) . . ?
C407 C406 C43B 143.5(6) . . ?
C405 C406 S41A 120.7(3) . . ?
C407 C406 S41A 124.3(4) . . ?
C408 C407 C406 119.6(5) . . ?
C407 C408 C409 122.1(7) . . ?
C410 C409 C408 119.7(6) . . ?
C409 C410 C405 119.1(5) . . ?
C416 C411 C412 119.6(6) . . ?
C416 C411 C44A 134.5(6) . . ?
C412 C411 C44A 105.6(6) . . ?
C416 C411 S42B 111.9(4) . . ?
C412 C411 S42B 128.5(5) . . ?
C413 C412 C411 121.5(6) . . ?
C413 C412 C44B 140.5(8) . . ?
C411 C412 C44B 97.9(8) . . ?
C413 C412 S42A 122.1(4) . . ?
C411 C412 S42A 116.4(5) . . ?
C412 C413 C414 118.9(5) . . ?
C413 C414 C415 121.0(7) . . ?
C414 C415 C416 120.0(6) . . ?
C411 C416 C415 118.9(5) . . ?
O41A C43A C401 125.0(6) . . ?
O41A C43A C405 117.2(6) . . ?
C401 C43A C405 117.8(6) . . ?
C406 S41A C401 87.7(3) . . ?
C401 C43B O41B 115.9(15) . . ?
C401 C43B C406 118.3(6) . . ?
O41B C43B C406 124.9(15) . . ?
C405 S41B C401 84.6(5) . . ?
C402 C44A O42A 124.2(8) . . ?
C402 C44A C411 117.5(8) . . ?
O42A C44A C411 118.2(8) . . ?
C412 S42A C402 88.8(3) . . ?
O42B C44B C402 122.4(10) . . ?
O42B C44B C412 116.1(12) . . ?
C402 C44B C412 120.9(11) . . ?
C411 S42B C402 83.5(3) . . ?

_refine_diff_density_max         0.294
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.040

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/o-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    ', Air-sensitive'
_exptl_crystal_preparation       ', Magnetic properties'
