# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2016

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

data_nr15010
_database_code_depnum_ccdc_archive 'CCDC 1443037'
_audit_update_record             
;
2015-12-17 deposited with the CCDC.
2016-03-01 downloaded from the CCDC.
;
_audit_creation_date             2015-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            SFX-MeOTAD
_chemical_name_systematic        
'2, 2?, 7, 7?-Tetrakis (N, N-di(4-methoxyphenyl)amino) - spiro (fluorene-9, 9?-xanthene)'
_chemical_formula_moiety         'C81 H68 N4 O9'
_chemical_formula_sum            'C81 H68 N4 O9'
_chemical_formula_weight         1241.39
_chemical_melting_point          510
_chemical_oxdiff_formula         'C81 H68 N4 O9'
_chemical_oxdiff_usercomment     '@ 120 K M18'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.5201(3)
_cell_length_b                   16.2972(4)
_cell_length_c                   20.9582(6)
_cell_angle_alpha                68.652(2)
_cell_angle_beta                 80.004(2)
_cell_angle_gamma                71.759(2)
_cell_volume                     3171.31(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16804
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.9140
_cell_measurement_theta_min      4.3360
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_recrystallization_method 'solvent layering'
_exptl_crystal_size_max          0.4036
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.0334
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51866
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.238
_diffrn_reflns_theta_min         3.026
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -90.0000 79

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -30.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
  7 omega   23.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000 -180.0000 75

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 55

#__ type_ start__ end____ width___ exp.time_
  9 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 79

#__ type_ start__ end____ width___ exp.time_
 10 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 79

#__ type_ start__ end____ width___ exp.time_
 11 omega   37.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -180.0000 105

#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 13 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 79

#__ type_ start__ end____ width___ exp.time_
 14 omega   31.00  156.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  150.0000 125

#__ type_ start__ end____ width___ exp.time_
 15 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 59

#__ type_ start__ end____ width___ exp.time_
 16 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 17 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 59

#__ type_ start__ end____ width___ exp.time_
 18 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 79

#__ type_ start__ end____ width___ exp.time_
 19 omega   31.00  156.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000    0.0000 125

#__ type_ start__ end____ width___ exp.time_
 20 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
 21 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
 22 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 59

#__ type_ start__ end____ width___ exp.time_
 23 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
 24 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

#__ type_ start__ end____ width___ exp.time_
 25 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
 26 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

#__ type_ start__ end____ width___ exp.time_
 27 omega   41.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
 28 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
 29 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 55

#__ type_ start__ end____ width___ exp.time_
 30 omega   83.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 31 omega   94.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   30.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0536309000
_diffrn_orient_matrix_UB_12      0.0166879000
_diffrn_orient_matrix_UB_13      -0.0755760000
_diffrn_orient_matrix_UB_21      0.0360026000
_diffrn_orient_matrix_UB_22      -0.1035206000
_diffrn_orient_matrix_UB_23      0.0123085000
_diffrn_orient_matrix_UB_31      -0.1403920000
_diffrn_orient_matrix_UB_32      0.0114529000
_diffrn_orient_matrix_UB_33      -0.0198448000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10913
_reflns_number_total             13172
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00122(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         13172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0877P)²+1.2167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1668
_refine_special_details          
;
The largest residual peak is 0.72 electrons height, 1.39 A from H26.



#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.44 Report
097_ALERT_2_C Large Reported Max.  (Positive) Residual Density       0.72 eA-3


See above.

906_ALERT_3_C Large K value in the Analysis of Variance ......      5.049 Check
#===============================================================================
154_ALERT_1_G The su's on the Cell Angles are Equal ..........    0.00200 Degree
910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          1 Report
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        120 Note

Noted.
#===============================================================================
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.57407(14) 0.23462(10) 0.16642(7) 0.0266(3) Uani 1 1 d . . . . .
O61 O 0.96311(15) -0.11712(11) 0.59270(8) 0.0322(3) Uani 1 1 d . . . . .
O69 O 0.89802(17) 0.79329(11) 0.01609(9) 0.0370(3) Uani 1 1 d . . . . .
O77 O 0.85194(18) -0.18554(11) 0.29034(10) 0.0403(4) Uani 1 1 d . . . . .
O85 O 0.17959(18) 0.67072(12) 0.49484(9) 0.0426(4) Uani 1 1 d . . . . .
O87 O 0.16657(17) 0.37736(12) 0.58693(10) 0.0416(4) Uani 1 1 d . . . . .
O89 O 0.83774(16) 0.49978(11) -0.29729(8) 0.0342(3) Uani 1 1 d . . . . .
O91 O 1.69307(14) -0.01890(11) 0.15812(9) 0.0360(4) Uani 1 1 d . . . . .
O93 O 0.2694(2) 0.91845(14) 0.02446(10) 0.0539(5) Uani 1 1 d . . . . .
N27 N 0.54701(16) 0.16342(12) 0.44814(9) 0.0262(3) Uani 1 1 d . . . . .
N34 N 0.75520(18) 0.51869(12) -0.03208(9) 0.0275(3) Uani 1 1 d . . . . .
N41 N 1.14078(15) 0.07194(11) 0.22805(9) 0.0251(3) Uani 1 1 d . . . . .
N48 N 0.47618(18) 0.62974(11) 0.25514(9) 0.0302(4) Uani 1 1 d . . . . .
C2 C 0.62240(18) 0.30582(13) 0.11967(10) 0.0242(4) Uani 1 1 d . . . . .
C3 C 0.68643(17) 0.35459(13) 0.13932(10) 0.0223(4) Uani 1 1 d . . . . .
C4 C 0.71364(17) 0.32914(12) 0.21415(9) 0.0203(3) Uani 1 1 d . . . . .
C5 C 0.62748(17) 0.26866(12) 0.26103(10) 0.0215(3) Uani 1 1 d . . . . .
C6 C 0.56835(18) 0.22162(13) 0.23550(10) 0.0228(4) Uani 1 1 d . . . . .
C7 C 0.50218(19) 0.15813(14) 0.27870(11) 0.0266(4) Uani 1 1 d . . . . .
H7 H 0.4636 0.1269 0.2601 0.032 Uiso 1 1 calc R . . . .
C8 C 0.49247(19) 0.14043(14) 0.34857(11) 0.0271(4) Uani 1 1 d . . . . .
H8 H 0.4476 0.0968 0.3784 0.033 Uiso 1 1 calc R . . . .
C9 C 0.54898(17) 0.18689(13) 0.37548(10) 0.0225(4) Uani 1 1 d . . . . .
C10 C 0.61556(17) 0.25026(12) 0.33220(10) 0.0220(3) Uani 1 1 d . . . . .
H10 H 0.6534 0.2815 0.3511 0.026 Uiso 1 1 calc R . . . .
C11 C 0.59967(19) 0.32756(14) 0.05163(11) 0.0275(4) Uani 1 1 d . . . . .
H11 H 0.5552 0.2936 0.0391 0.033 Uiso 1 1 calc R . . . .
C12 C 0.6416(2) 0.39847(14) 0.00206(11) 0.0286(4) Uani 1 1 d . . . . .
H12 H 0.6244 0.4140 -0.0445 0.034 Uiso 1 1 calc R . . . .
C13 C 0.71006(18) 0.44837(13) 0.01993(10) 0.0246(4) Uani 1 1 d . . . . .
C14 C 0.73142(18) 0.42519(13) 0.08858(10) 0.0243(4) Uani 1 1 d . . . . .
H14 H 0.7775 0.4579 0.1013 0.029 Uiso 1 1 calc R . . . .
C15 C 0.70010(18) 0.41333(12) 0.23340(9) 0.0220(3) Uani 1 1 d . . . . .
C16 C 0.82228(19) 0.41190(13) 0.25225(10) 0.0235(4) Uani 1 1 d . . . . .
C17 C 0.92325(18) 0.32841(13) 0.24668(10) 0.0231(4) Uani 1 1 d . . . . .
C18 C 0.86288(17) 0.27903(12) 0.22531(9) 0.0218(3) Uani 1 1 d . . . . .
C19 C 0.93327(18) 0.19574(12) 0.21775(9) 0.0220(3) Uani 1 1 d . . . . .
H19 H 0.8902 0.1631 0.2031 0.026 Uiso 1 1 calc R . . . .
C20 C 1.06973(18) 0.15948(12) 0.23198(9) 0.0215(3) Uani 1 1 d . . . . .
C21 C 1.13094(19) 0.21048(14) 0.25205(10) 0.0259(4) Uani 1 1 d . . . . .
H21 H 1.2235 0.1877 0.2603 0.031 Uiso 1 1 calc R . . . .
C22 C 1.0576(2) 0.29414(13) 0.25996(10) 0.0256(4) Uani 1 1 d . . . . .
H22 H 1.0998 0.3275 0.2744 0.031 Uiso 1 1 calc R . . . .
C23 C 0.58643(18) 0.48524(12) 0.23352(10) 0.0231(4) Uani 1 1 d . . . . .
H23 H 0.5047 0.4865 0.2193 0.028 Uiso 1 1 calc R . . . .
C24 C 0.59303(19) 0.55579(13) 0.25471(10) 0.0243(4) Uani 1 1 d . . . . .
C25 C 0.7146(2) 0.55331(14) 0.27442(11) 0.0298(4) Uani 1 1 d . . . . .
H25 H 0.7192 0.6010 0.2891 0.036 Uiso 1 1 calc R . . . .
C26 C 0.83027(19) 0.48167(14) 0.27303(11) 0.0274(4) Uani 1 1 d . . . . .
H26 H 0.9128 0.4810 0.2861 0.033 Uiso 1 1 calc R . . . .
C28 C 0.64954(18) 0.09073(13) 0.48403(10) 0.0229(4) Uani 1 1 d . . . . .
C29 C 0.75006(19) 0.03930(14) 0.44978(10) 0.0255(4) Uani 1 1 d . . . . .
H29 H 0.7468 0.0528 0.4019 0.031 Uiso 1 1 calc R . . . .
C30 C 0.85484(19) -0.03118(14) 0.48432(10) 0.0265(4) Uani 1 1 d . . . . .
H30 H 0.9217 -0.0655 0.4600 0.032 Uiso 1 1 calc R . . . .
C31 C 0.86191(19) -0.05149(13) 0.55418(10) 0.0253(4) Uani 1 1 d . . . . .
C32 C 0.7608(2) -0.00238(14) 0.58917(10) 0.0280(4) Uani 1 1 d . . . . .
H32 H 0.7639 -0.0169 0.6372 0.034 Uiso 1 1 calc R . . . .
C33 C 0.6555(2) 0.06737(14) 0.55526(10) 0.0267(4) Uani 1 1 d . . . . .
H33 H 0.5869 0.0996 0.5802 0.032 Uiso 1 1 calc R . . . .
C35 C 0.79160(19) 0.58817(13) -0.01980(10) 0.0239(4) Uani 1 1 d . . . . .
C36 C 0.71814(19) 0.63008(14) 0.02817(10) 0.0266(4) Uani 1 1 d . . . . .
H36 H 0.6419 0.6117 0.0535 0.032 Uiso 1 1 calc R . . . .
C37 C 0.7560(2) 0.69798(14) 0.03881(11) 0.0291(4) Uani 1 1 d . . . . .
H37 H 0.7066 0.7251 0.0720 0.035 Uiso 1 1 calc R . . . .
C38 C 0.8666(2) 0.72678(14) 0.00091(11) 0.0280(4) Uani 1 1 d . . . . .
C39 C 0.93794(19) 0.68769(14) -0.04785(10) 0.0273(4) Uani 1 1 d . . . . .
H39 H 1.0119 0.7080 -0.0745 0.033 Uiso 1 1 calc R . . . .
C40 C 0.90048(19) 0.61841(14) -0.05749(10) 0.0268(4) Uani 1 1 d . . . . .
H40 H 0.9504 0.5913 -0.0905 0.032 Uiso 1 1 calc R . . . .
C42 C 1.07233(17) 0.00346(12) 0.24437(10) 0.0224(4) Uani 1 1 d . . . . .
C43 C 0.97673(19) -0.00746(13) 0.30004(10) 0.0248(4) Uani 1 1 d . . . . .
H43 H 0.9609 0.0289 0.3287 0.030 Uiso 1 1 calc R . . . .
C44 C 0.9050(2) -0.07090(14) 0.31371(11) 0.0287(4) Uani 1 1 d . . . . .
H44 H 0.8387 -0.0768 0.3509 0.034 Uiso 1 1 calc R . . . .
C45 C 0.9300(2) -0.12653(13) 0.27268(12) 0.0290(4) Uani 1 1 d . . . . .
C46 C 1.0291(2) -0.11904(14) 0.21934(12) 0.0296(4) Uani 1 1 d . . . . .
H46 H 1.0498 -0.1586 0.1929 0.035 Uiso 1 1 calc R . . . .
C47 C 1.09849(18) -0.05300(13) 0.20468(11) 0.0260(4) Uani 1 1 d . . . . .
H47 H 1.1642 -0.0467 0.1672 0.031 Uiso 1 1 calc R . . . .
C49 C 0.40707(19) 0.63801(13) 0.31674(10) 0.0242(4) Uani 1 1 d . . . . .
C50 C 0.3131(2) 0.72107(13) 0.31770(11) 0.0287(4) Uani 1 1 d . . . . .
H50 H 0.2993 0.7722 0.2766 0.034 Uiso 1 1 calc R . . . .
C51 C 0.2406(2) 0.72888(14) 0.37793(12) 0.0325(4) Uani 1 1 d . . . . .
H51 H 0.1776 0.7854 0.3777 0.039 Uiso 1 1 calc R . . . .
C52 C 0.2587(2) 0.65542(14) 0.43858(11) 0.0299(4) Uani 1 1 d . . . . .
C53 C 0.3521(2) 0.57319(14) 0.43878(11) 0.0282(4) Uani 1 1 d . . . . .
H53 H 0.3661 0.5226 0.4802 0.034 Uiso 1 1 calc R . . . .
C54 C 0.4250(2) 0.56505(13) 0.37818(11) 0.0269(4) Uani 1 1 d . . . . .
H54 H 0.4882 0.5085 0.3788 0.032 Uiso 1 1 calc R . . . .
C55 C 0.44784(19) 0.21946(13) 0.48201(10) 0.0240(4) Uani 1 1 d . . . . .
C56 C 0.3146(2) 0.21860(14) 0.48822(11) 0.0279(4) Uani 1 1 d . . . . .
H56 H 0.2901 0.1813 0.4693 0.033 Uiso 1 1 calc R . . . .
C57 C 0.2160(2) 0.27188(15) 0.52187(11) 0.0310(4) Uani 1 1 d . . . . .
H57 H 0.1246 0.2725 0.5246 0.037 Uiso 1 1 calc R . . . .
C58 C 0.2538(2) 0.32393(14) 0.55125(12) 0.0317(4) Uani 1 1 d . . . . .
C59 C 0.3875(2) 0.32438(14) 0.54609(12) 0.0322(4) Uani 1 1 d . . . . .
H59 H 0.4127 0.3597 0.5666 0.039 Uiso 1 1 calc R . . . .
C60 C 0.4836(2) 0.27313(14) 0.51096(11) 0.0292(4) Uani 1 1 d . . . . .
H60 H 0.5743 0.2746 0.5066 0.035 Uiso 1 1 calc R . . . .
C62 C 1.0530(2) -0.17862(15) 0.56107(12) 0.0328(4) Uani 1 1 d . . . . .
H62A H 1.1050 -0.1452 0.5226 0.049 Uiso 1 1 calc GR . . . .
H62B H 1.0020 -0.2066 0.5441 0.049 Uiso 1 1 calc GR . . . .
H62C H 1.1139 -0.2265 0.5947 0.049 Uiso 1 1 calc GR . . . .
C63 C 0.77666(18) 0.51534(13) -0.10035(10) 0.0234(4) Uani 1 1 d . . . . .
C64 C 0.8739(2) 0.44357(14) -0.11642(11) 0.0286(4) Uani 1 1 d . . . . .
H64 H 0.9284 0.3968 -0.0819 0.034 Uiso 1 1 calc R . . . .
C65 C 0.8910(2) 0.44030(14) -0.18238(11) 0.0296(4) Uani 1 1 d . . . . .
H65 H 0.9569 0.3910 -0.1929 0.035 Uiso 1 1 calc R . . . .
C66 C 0.81223(18) 0.50884(14) -0.23365(10) 0.0245(4) Uani 1 1 d . . . . .
C67 C 0.71684(18) 0.58148(13) -0.21832(10) 0.0246(4) Uani 1 1 d . . . . .
H67 H 0.6632 0.6287 -0.2530 0.030 Uiso 1 1 calc R . . . .
C68 C 0.70062(18) 0.58443(13) -0.15180(10) 0.0255(4) Uani 1 1 d . . . . .
H68 H 0.6364 0.6345 -0.1415 0.031 Uiso 1 1 calc R . . . .
C70 C 0.9999(3) 0.83102(18) -0.02767(14) 0.0422(5) Uani 1 1 d . . . . .
H70A H 0.9746 0.8563 -0.0753 0.063 Uiso 1 1 calc GR . . . .
H70B H 1.0849 0.7829 -0.0240 0.063 Uiso 1 1 calc GR . . . .
H70C H 1.0104 0.8798 -0.0139 0.063 Uiso 1 1 calc GR . . . .
C71 C 1.28093(17) 0.05034(13) 0.20915(10) 0.0224(4) Uani 1 1 d . . . . .
C72 C 1.36740(18) -0.03062(13) 0.24831(10) 0.0243(4) Uani 1 1 d . . . . .
H72 H 1.3322 -0.0717 0.2872 0.029 Uiso 1 1 calc R . . . .
C73 C 1.50465(19) -0.05127(13) 0.23047(10) 0.0256(4) Uani 1 1 d . . . . .
H73 H 1.5628 -0.1061 0.2574 0.031 Uiso 1 1 calc R . . . .
C74 C 1.55689(18) 0.00786(14) 0.17354(11) 0.0260(4) Uani 1 1 d . . . . .
C75 C 1.47192(19) 0.08774(14) 0.13366(10) 0.0263(4) Uani 1 1 d . . . . .
H75 H 1.5075 0.1278 0.0942 0.032 Uiso 1 1 calc R . . . .
C76 C 1.33434(18) 0.10909(13) 0.15147(10) 0.0243(4) Uani 1 1 d . . . . .
H76 H 1.2766 0.1639 0.1242 0.029 Uiso 1 1 calc R . . . .
C78 C 0.8702(3) -0.2394(2) 0.24728(18) 0.0558(7) Uani 1 1 d . . . . .
H78A H 0.8568 -0.1991 0.1997 0.084 Uiso 1 1 calc GR . . . .
H78B H 0.8051 -0.2757 0.2623 0.084 Uiso 1 1 calc GR . . . .
H78C H 0.9614 -0.2806 0.2502 0.084 Uiso 1 1 calc GR . . . .
C79 C 0.4361(2) 0.70022(13) 0.19198(10) 0.0257(4) Uani 1 1 d . . . . .
C80 C 0.4844(2) 0.77668(14) 0.16807(11) 0.0295(4) Uani 1 1 d . . . . .
H80 H 0.5536 0.7784 0.1909 0.035 Uiso 1 1 calc R . . . .
C81 C 0.4336(2) 0.85094(15) 0.11139(12) 0.0336(4) Uani 1 1 d . . . . .
H81 H 0.4670 0.9033 0.0957 0.040 Uiso 1 1 calc R . . . .
C82 C 0.3335(2) 0.84751(16) 0.07803(11) 0.0360(5) Uani 1 1 d . . . . .
C83 C 0.2879(3) 0.76955(18) 0.09994(14) 0.0435(6) Uani 1 1 d . . . . .
H83 H 0.2220 0.7664 0.0758 0.052 Uiso 1 1 calc R . . . .
C84 C 0.3386(2) 0.69656(16) 0.15698(13) 0.0372(5) Uani 1 1 d . . . . .
H84 H 0.3065 0.6437 0.1722 0.045 Uiso 1 1 calc R . . . .
C86 C 0.1973(3) 0.59733(18) 0.55804(13) 0.0478(6) Uani 1 1 d . . . . .
H86A H 0.1787 0.5446 0.5533 0.072 Uiso 1 1 calc GR . . . .
H86B H 0.1355 0.6164 0.5940 0.072 Uiso 1 1 calc GR . . . .
H86C H 0.2899 0.5803 0.5705 0.072 Uiso 1 1 calc GR . . . .
C88 C 0.0274(3) 0.3822(2) 0.59069(16) 0.0494(6) Uani 1 1 d . . . . .
H88A H -0.0050 0.4102 0.5444 0.074 Uiso 1 1 calc GR . . . .
H88B H -0.0238 0.4193 0.6192 0.074 Uiso 1 1 calc GR . . . .
H88C H 0.0156 0.3203 0.6110 0.074 Uiso 1 1 calc GR . . . .
C90 C 0.7587(3) 0.57028(19) -0.35052(12) 0.0406(5) Uani 1 1 d . . . . .
H90A H 0.7835 0.5559 -0.3933 0.061 Uiso 1 1 calc GR . . . .
H90B H 0.7749 0.6290 -0.3573 0.061 Uiso 1 1 calc GR . . . .
H90C H 0.6634 0.5742 -0.3374 0.061 Uiso 1 1 calc GR . . . .
C92 C 1.7608(2) 0.05109(17) 0.13469(13) 0.0376(5) Uani 1 1 d . . . . .
H92A H 1.7204 0.0990 0.0936 0.056 Uiso 1 1 calc GR . . . .
H92B H 1.8558 0.0248 0.1235 0.056 Uiso 1 1 calc GR . . . .
H92C H 1.7527 0.0776 0.1708 0.056 Uiso 1 1 calc GR . . . .
C94 C 0.3079(4) 1.00113(19) 0.00312(15) 0.0602(8) Uani 1 1 d . . . . .
H94A H 0.2535 1.0470 -0.0342 0.090 Uiso 1 1 calc GR . . . .
H94B H 0.4029 0.9896 -0.0130 0.090 Uiso 1 1 calc GR . . . .
H94C H 0.2937 1.0237 0.0419 0.090 Uiso 1 1 calc GR . . . .


_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
O1 C2 1.391(2) . ?
O1 C6 1.378(2) . ?
O61 C31 1.373(2) . ?
O61 C62 1.418(3) . ?
O69 C38 1.377(3) . ?
O69 C70 1.425(3) . ?
O77 C45 1.366(3) . ?
O77 C78 1.426(3) . ?
O85 C52 1.374(3) . ?
O85 C86 1.419(3) . ?
O87 C58 1.376(3) . ?
O87 C88 1.431(3) . ?
O89 C66 1.367(2) . ?
O89 C90 1.431(3) . ?
O91 C74 1.378(2) . ?
O91 C92 1.425(3) . ?
O93 C82 1.372(3) . ?
O93 C94 1.421(4) . ?
N27 C9 1.427(3) . ?
N27 C28 1.402(2) . ?
N27 C55 1.430(2) . ?
N34 C13 1.407(3) . ?
N34 C35 1.419(3) . ?
N34 C63 1.428(3) . ?
N41 C20 1.413(2) . ?
N41 C42 1.421(2) . ?
N41 C71 1.424(2) . ?
N48 C24 1.428(2) . ?
N48 C49 1.398(3) . ?
N48 C79 1.426(3) . ?
C2 C3 1.387(3) . ?
C2 C11 1.383(3) . ?
C3 C4 1.524(2) . ?
C3 C14 1.398(3) . ?
C4 C5 1.518(2) . ?
C4 C15 1.525(2) . ?
C4 C18 1.540(2) . ?
C5 C6 1.405(3) . ?
C5 C10 1.401(3) . ?
C6 C7 1.387(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.398(3) . ?
C9 C10 1.389(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.377(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.415(3) . ?
C13 C14 1.388(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(3) . ?
C15 C23 1.388(3) . ?
C16 C17 1.470(3) . ?
C16 C26 1.387(3) . ?
C17 C18 1.390(3) . ?
C17 C22 1.385(3) . ?
C18 C19 1.379(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.410(3) . ?
C20 C21 1.402(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.394(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.399(3) . ?
C24 C25 1.396(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.403(3) . ?
C26 H26 0.9500 . ?
C28 C29 1.398(3) . ?
C28 C33 1.407(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.392(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.389(3) . ?
C31 C32 1.391(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.386(3) . ?
C33 H33 0.9500 . ?
C35 C36 1.405(3) . ?
C35 C40 1.391(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.386(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.398(3) . ?
C38 C39 1.386(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.394(3) . ?
C40 H40 0.9500 . ?
C42 C43 1.399(3) . ?
C42 C47 1.390(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.385(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.404(3) . ?
C45 C46 1.388(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.399(3) . ?
C47 H47 0.9500 . ?
C49 C50 1.409(3) . ?
C49 C54 1.392(3) . ?
C50 H50 0.9500 . ?
C50 C51 1.383(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.385(3) . ?
C52 C53 1.391(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.393(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.389(3) . ?
C55 C60 1.395(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.398(3) . ?
C57 H57 0.9500 . ?
C57 C58 1.390(3) . ?
C58 C59 1.394(3) . ?
C59 H59 0.9500 . ?
C59 C60 1.386(3) . ?
C60 H60 0.9500 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.395(3) . ?
C63 C68 1.386(3) . ?
C64 H64 0.9500 . ?
C64 C65 1.381(3) . ?
C65 H65 0.9500 . ?
C65 C66 1.394(3) . ?
C66 C67 1.390(3) . ?
C67 H67 0.9500 . ?
C67 C68 1.391(3) . ?
C68 H68 0.9500 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.400(3) . ?
C71 C76 1.397(3) . ?
C72 H72 0.9500 . ?
C72 C73 1.392(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.386(3) . ?
C74 C75 1.390(3) . ?
C75 H75 0.9500 . ?
C75 C76 1.395(3) . ?
C76 H76 0.9500 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 C80 1.384(3) . ?
C79 C84 1.387(3) . ?
C80 H80 0.9500 . ?
C80 C81 1.389(3) . ?
C81 H81 0.9500 . ?
C81 C82 1.387(4) . ?
C82 C83 1.391(4) . ?
C83 H83 0.9500 . ?
C83 C84 1.385(3) . ?
C84 H84 0.9500 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 O1 C2 118.87(15) . . ?
C31 O61 C62 116.41(16) . . ?
C38 O69 C70 116.39(18) . . ?
C45 O77 C78 116.2(2) . . ?
C52 O85 C86 117.11(18) . . ?
C58 O87 C88 116.9(2) . . ?
C66 O89 C90 116.51(17) . . ?
C74 O91 C92 116.58(17) . . ?
C82 O93 C94 116.9(2) . . ?
C9 N27 C55 119.39(16) . . ?
C28 N27 C9 119.20(16) . . ?
C28 N27 C55 121.17(16) . . ?
C13 N34 C35 123.84(17) . . ?
C13 N34 C63 117.96(17) . . ?
C35 N34 C63 117.97(16) . . ?
C20 N41 C42 119.74(15) . . ?
C20 N41 C71 121.10(15) . . ?
C42 N41 C71 119.15(15) . . ?
C49 N48 C24 121.12(16) . . ?
C49 N48 C79 119.44(16) . . ?
C79 N48 C24 119.24(17) . . ?
C3 C2 O1 122.79(18) . . ?
C11 C2 O1 115.97(17) . . ?
C11 C2 C3 121.21(18) . . ?
C2 C3 C4 120.98(17) . . ?
C2 C3 C14 118.65(18) . . ?
C14 C3 C4 120.30(17) . . ?
C3 C4 C15 111.94(15) . . ?
C3 C4 C18 110.33(14) . . ?
C5 C4 C3 110.52(15) . . ?
C5 C4 C15 113.25(15) . . ?
C5 C4 C18 109.65(14) . . ?
C15 C4 C18 100.75(14) . . ?
C6 C5 C4 121.03(17) . . ?
C10 C5 C4 121.15(16) . . ?
C10 C5 C6 117.50(17) . . ?
O1 C6 C5 122.23(17) . . ?
O1 C6 C7 116.01(17) . . ?
C7 C6 C5 121.75(18) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.88(18) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.71(18) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 N27 119.33(17) . . ?
C10 C9 N27 120.10(17) . . ?
C10 C9 C8 120.39(18) . . ?
C5 C10 H10 119.6 . . ?
C9 C10 C5 120.76(17) . . ?
C9 C10 H10 119.6 . . ?
C2 C11 H11 120.1 . . ?
C12 C11 C2 119.85(19) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.54(19) . . ?
C13 C12 H12 119.7 . . ?
N34 C13 C12 119.26(18) . . ?
C14 C13 N34 122.33(18) . . ?
C14 C13 C12 118.41(18) . . ?
C3 C14 H14 119.4 . . ?
C13 C14 C3 121.30(18) . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C4 111.18(15) . . ?
C23 C15 C4 127.98(17) . . ?
C23 C15 C16 120.84(18) . . ?
C15 C16 C17 108.35(17) . . ?
C26 C16 C15 120.09(17) . . ?
C26 C16 C17 131.54(18) . . ?
C18 C17 C16 108.89(16) . . ?
C22 C17 C16 131.55(18) . . ?
C22 C17 C18 119.54(17) . . ?
C17 C18 C4 110.82(16) . . ?
C19 C18 C4 127.60(17) . . ?
C19 C18 C17 121.57(17) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.46(17) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 N41 119.89(16) . . ?
C21 C20 N41 121.33(16) . . ?
C21 C20 C19 118.75(17) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 C20 120.83(17) . . ?
C22 C21 H21 119.6 . . ?
C17 C22 C21 119.81(17) . . ?
C17 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C15 C23 H23 120.2 . . ?
C15 C23 C24 119.59(18) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 N48 119.77(18) . . ?
C25 C24 N48 120.92(18) . . ?
C25 C24 C23 119.31(18) . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.20(19) . . ?
C26 C25 H25 119.4 . . ?
C16 C26 C25 118.95(18) . . ?
C16 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
N27 C28 C33 121.44(18) . . ?
C29 C28 N27 120.74(17) . . ?
C29 C28 C33 117.82(17) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 C28 121.40(18) . . ?
C30 C29 H29 119.3 . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.16(18) . . ?
C31 C30 H30 119.9 . . ?
O61 C31 C30 125.00(18) . . ?
O61 C31 C32 116.01(18) . . ?
C30 C31 C32 118.99(18) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 C31 121.17(19) . . ?
C33 C32 H32 119.4 . . ?
C28 C33 H33 119.8 . . ?
C32 C33 C28 120.41(18) . . ?
C32 C33 H33 119.8 . . ?
C36 C35 N34 121.95(17) . . ?
C40 C35 N34 119.71(18) . . ?
C40 C35 C36 118.32(18) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 C35 120.56(18) . . ?
C37 C36 H36 119.7 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.24(19) . . ?
C38 C37 H37 119.9 . . ?
O69 C38 C37 115.97(19) . . ?
O69 C38 C39 124.21(19) . . ?
C39 C38 C37 119.82(19) . . ?
C38 C39 H39 120.2 . . ?
C38 C39 C40 119.58(18) . . ?
C40 C39 H39 120.2 . . ?
C35 C40 C39 121.46(19) . . ?
C35 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C43 C42 N41 120.57(17) . . ?
C47 C42 N41 120.37(18) . . ?
C47 C42 C43 119.06(17) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 C42 120.53(18) . . ?
C44 C43 H43 119.7 . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.12(19) . . ?
C45 C44 H44 119.9 . . ?
O77 C45 C44 114.96(19) . . ?
O77 C45 C46 125.4(2) . . ?
C46 C45 C44 119.63(18) . . ?
C45 C46 H46 120.1 . . ?
C45 C46 C47 119.81(19) . . ?
C47 C46 H46 120.1 . . ?
C42 C47 C46 120.73(19) . . ?
C42 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?
N48 C49 C50 120.20(18) . . ?
C54 C49 N48 121.90(17) . . ?
C54 C49 C50 117.87(19) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 C49 120.62(19) . . ?
C51 C50 H50 119.7 . . ?
C50 C51 H51 119.6 . . ?
C50 C51 C52 120.86(19) . . ?
C52 C51 H51 119.6 . . ?
O85 C52 C51 115.69(18) . . ?
O85 C52 C53 124.97(19) . . ?
C51 C52 C53 119.3(2) . . ?
C52 C53 H53 120.0 . . ?
C52 C53 C54 119.94(19) . . ?
C54 C53 H53 120.0 . . ?
C49 C54 C53 121.37(18) . . ?
C49 C54 H54 119.3 . . ?
C53 C54 H54 119.3 . . ?
C56 C55 N27 119.87(18) . . ?
C56 C55 C60 119.23(18) . . ?
C60 C55 N27 120.87(17) . . ?
C55 C56 H56 119.5 . . ?
C55 C56 C57 120.97(19) . . ?
C57 C56 H56 119.5 . . ?
C56 C57 H57 120.5 . . ?
C58 C57 C56 118.97(19) . . ?
C58 C57 H57 120.5 . . ?
O87 C58 C57 124.3(2) . . ?
O87 C58 C59 115.2(2) . . ?
C57 C58 C59 120.50(19) . . ?
C58 C59 H59 120.1 . . ?
C60 C59 C58 119.9(2) . . ?
C60 C59 H59 120.1 . . ?
C55 C60 H60 119.8 . . ?
C59 C60 C55 120.43(18) . . ?
C59 C60 H60 119.8 . . ?
O61 C62 H62A 109.5 . . ?
O61 C62 H62B 109.5 . . ?
O61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 N34 120.99(17) . . ?
C68 C63 N34 119.86(17) . . ?
C68 C63 C64 119.16(18) . . ?
C63 C64 H64 119.9 . . ?
C65 C64 C63 120.17(18) . . ?
C65 C64 H64 119.9 . . ?
C64 C65 H65 119.7 . . ?
C64 C65 C66 120.50(18) . . ?
C66 C65 H65 119.7 . . ?
O89 C66 C65 116.00(18) . . ?
O89 C66 C67 124.34(18) . . ?
C67 C66 C65 119.65(18) . . ?
C66 C67 H67 120.3 . . ?
C66 C67 C68 119.47(18) . . ?
C68 C67 H67 120.3 . . ?
C63 C68 C67 121.01(18) . . ?
C63 C68 H68 119.5 . . ?
C67 C68 H68 119.5 . . ?
O69 C70 H70A 109.5 . . ?
O69 C70 H70B 109.5 . . ?
O69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 N41 120.22(17) . . ?
C76 C71 N41 120.81(17) . . ?
C76 C71 C72 118.97(17) . . ?
C71 C72 H72 119.8 . . ?
C73 C72 C71 120.32(18) . . ?
C73 C72 H72 119.8 . . ?
C72 C73 H73 119.9 . . ?
C74 C73 C72 120.29(18) . . ?
C74 C73 H73 119.9 . . ?
O91 C74 C73 116.72(18) . . ?
O91 C74 C75 123.29(19) . . ?
C73 C74 C75 119.95(17) . . ?
C74 C75 H75 120.0 . . ?
C74 C75 C76 120.05(18) . . ?
C76 C75 H75 120.0 . . ?
C71 C76 H76 119.8 . . ?
C75 C76 C71 120.41(17) . . ?
C75 C76 H76 119.8 . . ?
O77 C78 H78A 109.5 . . ?
O77 C78 H78B 109.5 . . ?
O77 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C80 C79 N48 120.73(19) . . ?
C80 C79 C84 119.14(19) . . ?
C84 C79 N48 119.88(19) . . ?
C79 C80 H80 119.4 . . ?
C79 C80 C81 121.3(2) . . ?
C81 C80 H80 119.4 . . ?
C80 C81 H81 120.5 . . ?
C82 C81 C80 119.0(2) . . ?
C82 C81 H81 120.5 . . ?
O93 C82 C81 124.5(2) . . ?
O93 C82 C83 115.2(2) . . ?
C81 C82 C83 120.2(2) . . ?
C82 C83 H83 120.0 . . ?
C84 C83 C82 120.0(2) . . ?
C84 C83 H83 120.0 . . ?
C79 C84 H84 119.8 . . ?
C83 C84 C79 120.3(2) . . ?
C83 C84 H84 119.8 . . ?
O85 C86 H86A 109.5 . . ?
O85 C86 H86B 109.5 . . ?
O85 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
O87 C88 H88A 109.5 . . ?
O87 C88 H88B 109.5 . . ?
O87 C88 H88C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
O89 C90 H90A 109.5 . . ?
O89 C90 H90B 109.5 . . ?
O89 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
O91 C92 H92A 109.5 . . ?
O91 C92 H92B 109.5 . . ?
O91 C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O93 C94 H94A 109.5 . . ?
O93 C94 H94B 109.5 . . ?
O93 C94 H94C 109.5 . . ?
H94A C94 H94B 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 3.1(3) . . . . ?
O1 C2 C3 C14 -179.90(16) . . . . ?
O1 C2 C11 C12 178.62(17) . . . . ?
O1 C6 C7 C8 179.59(17) . . . . ?
O61 C31 C32 C33 178.11(18) . . . . ?
O69 C38 C39 C40 177.69(18) . . . . ?
O77 C45 C46 C47 177.3(2) . . . . ?
O85 C52 C53 C54 178.7(2) . . . . ?
O87 C58 C59 C60 -179.8(2) . . . . ?
O89 C66 C67 C68 -179.07(18) . . . . ?
O91 C74 C75 C76 178.21(19) . . . . ?
O93 C82 C83 C84 -175.1(2) . . . . ?
N27 C9 C10 C5 174.91(16) . . . . ?
N27 C28 C29 C30 177.94(18) . . . . ?
N27 C28 C33 C32 -177.38(18) . . . . ?
N27 C55 C56 C57 179.18(18) . . . . ?
N27 C55 C60 C59 -177.39(19) . . . . ?
N34 C13 C14 C3 -179.54(17) . . . . ?
N34 C35 C36 C37 -179.77(18) . . . . ?
N34 C35 C40 C39 178.80(17) . . . . ?
N34 C63 C64 C65 178.41(19) . . . . ?
N34 C63 C68 C67 -178.14(17) . . . . ?
N41 C20 C21 C22 -175.89(18) . . . . ?
N41 C42 C43 C44 176.56(17) . . . . ?
N41 C42 C47 C46 -178.38(18) . . . . ?
N41 C71 C72 C73 -179.13(18) . . . . ?
N41 C71 C76 C75 179.48(18) . . . . ?
N48 C24 C25 C26 -178.93(19) . . . . ?
N48 C49 C50 C51 177.6(2) . . . . ?
N48 C49 C54 C53 -177.72(19) . . . . ?
N48 C79 C80 C81 -171.80(19) . . . . ?
N48 C79 C84 C83 172.6(2) . . . . ?
C2 O1 C6 C5 -9.6(2) . . . . ?
C2 O1 C6 C7 171.30(16) . . . . ?
C2 C3 C4 C5 -17.1(2) . . . . ?
C2 C3 C4 C15 -144.33(17) . . . . ?
C2 C3 C4 C18 104.35(19) . . . . ?
C2 C3 C14 C13 1.7(3) . . . . ?
C2 C11 C12 C13 1.2(3) . . . . ?
C3 C2 C11 C12 0.3(3) . . . . ?
C3 C4 C5 C6 18.7(2) . . . . ?
C3 C4 C5 C10 -167.96(16) . . . . ?
C3 C4 C15 C16 -116.97(17) . . . . ?
C3 C4 C15 C23 62.8(2) . . . . ?
C3 C4 C18 C17 117.79(17) . . . . ?
C3 C4 C18 C19 -63.6(2) . . . . ?
C4 C3 C14 C13 178.74(16) . . . . ?
C4 C5 C6 O1 -6.5(3) . . . . ?
C4 C5 C6 C7 172.55(17) . . . . ?
C4 C5 C10 C9 -172.74(16) . . . . ?
C4 C15 C16 C17 0.2(2) . . . . ?
C4 C15 C16 C26 -178.59(17) . . . . ?
C4 C15 C23 C24 178.32(17) . . . . ?
C4 C18 C19 C20 -178.45(17) . . . . ?
C5 C4 C15 C16 117.27(17) . . . . ?
C5 C4 C15 C23 -63.0(2) . . . . ?
C5 C4 C18 C17 -120.26(17) . . . . ?
C5 C4 C18 C19 58.3(2) . . . . ?
C5 C6 C7 C8 0.5(3) . . . . ?
C6 O1 C2 C3 11.4(3) . . . . ?
C6 O1 C2 C11 -166.85(16) . . . . ?
C6 C5 C10 C9 0.8(3) . . . . ?
C6 C7 C8 C9 0.3(3) . . . . ?
C7 C8 C9 N27 -175.49(17) . . . . ?
C7 C8 C9 C10 -0.4(3) . . . . ?
C8 C9 C10 C5 -0.1(3) . . . . ?
C9 N27 C28 C29 -2.4(3) . . . . ?
C9 N27 C28 C33 177.20(17) . . . . ?
C9 N27 C55 C56 71.3(2) . . . . ?
C9 N27 C55 C60 -110.8(2) . . . . ?
C10 C5 C6 O1 179.96(16) . . . . ?
C10 C5 C6 C7 -1.0(3) . . . . ?
C11 C2 C3 C4 -178.79(17) . . . . ?
C11 C2 C3 C14 -1.7(3) . . . . ?
C11 C12 C13 N34 178.13(18) . . . . ?
C11 C12 C13 C14 -1.2(3) . . . . ?
C12 C13 C14 C3 -0.2(3) . . . . ?
C13 N34 C35 C36 -40.4(3) . . . . ?
C13 N34 C35 C40 141.66(19) . . . . ?
C13 N34 C63 C64 -63.4(2) . . . . ?
C13 N34 C63 C68 116.9(2) . . . . ?
C14 C3 C4 C5 165.92(16) . . . . ?
C14 C3 C4 C15 38.7(2) . . . . ?
C14 C3 C4 C18 -72.6(2) . . . . ?
C15 C4 C5 C6 145.25(16) . . . . ?
C15 C4 C5 C10 -41.4(2) . . . . ?
C15 C4 C18 C17 -0.62(19) . . . . ?
C15 C4 C18 C19 177.98(18) . . . . ?
C15 C16 C17 C18 -0.6(2) . . . . ?
C15 C16 C17 C22 -179.1(2) . . . . ?
C15 C16 C26 C25 -0.3(3) . . . . ?
C15 C23 C24 N48 -179.78(17) . . . . ?
C15 C23 C24 C25 1.0(3) . . . . ?
C16 C15 C23 C24 -1.9(3) . . . . ?
C16 C17 C18 C4 0.7(2) . . . . ?
C16 C17 C18 C19 -177.95(17) . . . . ?
C16 C17 C22 C21 178.22(19) . . . . ?
C17 C16 C26 C25 -178.7(2) . . . . ?
C17 C18 C19 C20 0.0(3) . . . . ?
C18 C4 C5 C6 -103.09(19) . . . . ?
C18 C4 C5 C10 70.2(2) . . . . ?
C18 C4 C15 C16 0.27(19) . . . . ?
C18 C4 C15 C23 -179.98(18) . . . . ?
C18 C17 C22 C21 -0.2(3) . . . . ?
C18 C19 C20 N41 176.53(17) . . . . ?
C18 C19 C20 C21 -1.4(3) . . . . ?
C19 C20 C21 C22 2.0(3) . . . . ?
C20 N41 C42 C43 -40.7(3) . . . . ?
C20 N41 C42 C47 138.56(19) . . . . ?
C20 N41 C71 C72 131.6(2) . . . . ?
C20 N41 C71 C76 -48.6(3) . . . . ?
C20 C21 C22 C17 -1.2(3) . . . . ?
C22 C17 C18 C4 179.53(17) . . . . ?
C22 C17 C18 C19 0.8(3) . . . . ?
C23 C15 C16 C17 -179.62(17) . . . . ?
C23 C15 C16 C26 1.6(3) . . . . ?
C23 C24 C25 C26 0.3(3) . . . . ?
C24 N48 C49 C50 164.85(19) . . . . ?
C24 N48 C49 C54 -17.1(3) . . . . ?
C24 N48 C79 C80 -89.4(2) . . . . ?
C24 N48 C79 C84 96.5(2) . . . . ?
C24 C25 C26 C16 -0.6(3) . . . . ?
C26 C16 C17 C18 178.0(2) . . . . ?
C26 C16 C17 C22 -0.6(4) . . . . ?
C28 N27 C9 C8 85.5(2) . . . . ?
C28 N27 C9 C10 -89.6(2) . . . . ?
C28 N27 C55 C56 -114.5(2) . . . . ?
C28 N27 C55 C60 63.5(3) . . . . ?
C28 C29 C30 C31 -0.4(3) . . . . ?
C29 C28 C33 C32 2.2(3) . . . . ?
C29 C30 C31 O61 -177.51(19) . . . . ?
C29 C30 C31 C32 2.0(3) . . . . ?
C30 C31 C32 C33 -1.4(3) . . . . ?
C31 C32 C33 C28 -0.7(3) . . . . ?
C33 C28 C29 C30 -1.7(3) . . . . ?
C35 N34 C13 C12 162.44(18) . . . . ?
C35 N34 C13 C14 -18.2(3) . . . . ?
C35 N34 C63 C64 111.3(2) . . . . ?
C35 N34 C63 C68 -68.4(2) . . . . ?
C35 C36 C37 C38 1.2(3) . . . . ?
C36 C35 C40 C39 0.8(3) . . . . ?
C36 C37 C38 O69 -178.77(18) . . . . ?
C36 C37 C38 C39 0.5(3) . . . . ?
C37 C38 C39 C40 -1.5(3) . . . . ?
C38 C39 C40 C35 0.9(3) . . . . ?
C40 C35 C36 C37 -1.8(3) . . . . ?
C42 N41 C20 C19 -31.8(3) . . . . ?
C42 N41 C20 C21 146.13(19) . . . . ?
C42 N41 C71 C72 -47.3(3) . . . . ?
C42 N41 C71 C76 132.6(2) . . . . ?
C42 C43 C44 C45 1.6(3) . . . . ?
C43 C42 C47 C46 0.9(3) . . . . ?
C43 C44 C45 O77 -179.07(19) . . . . ?
C43 C44 C45 C46 1.5(3) . . . . ?
C44 C45 C46 C47 -3.2(3) . . . . ?
C45 C46 C47 C42 2.1(3) . . . . ?
C47 C42 C43 C44 -2.7(3) . . . . ?
C49 N48 C24 C23 107.6(2) . . . . ?
C49 N48 C24 C25 -73.2(3) . . . . ?
C49 N48 C79 C80 85.5(3) . . . . ?
C49 N48 C79 C84 -88.7(3) . . . . ?
C49 C50 C51 C52 0.0(3) . . . . ?
C50 C49 C54 C53 0.4(3) . . . . ?
C50 C51 C52 O85 -178.9(2) . . . . ?
C50 C51 C52 C53 0.7(3) . . . . ?
C51 C52 C53 C54 -0.8(3) . . . . ?
C52 C53 C54 C49 0.3(3) . . . . ?
C54 C49 C50 C51 -0.5(3) . . . . ?
C55 N27 C9 C8 -100.2(2) . . . . ?
C55 N27 C9 C10 84.8(2) . . . . ?
C55 N27 C28 C29 -176.66(17) . . . . ?
C55 N27 C28 C33 2.9(3) . . . . ?
C55 C56 C57 C58 -2.1(3) . . . . ?
C56 C55 C60 C59 0.6(3) . . . . ?
C56 C57 C58 O87 -178.5(2) . . . . ?
C56 C57 C58 C59 1.2(3) . . . . ?
C57 C58 C59 C60 0.5(3) . . . . ?
C58 C59 C60 C55 -1.4(3) . . . . ?
C60 C55 C56 C57 1.2(3) . . . . ?
C62 O61 C31 C30 -11.7(3) . . . . ?
C62 O61 C31 C32 168.78(18) . . . . ?
C63 N34 C13 C12 -23.2(3) . . . . ?
C63 N34 C13 C14 156.09(18) . . . . ?
C63 N34 C35 C36 145.26(18) . . . . ?
C63 N34 C35 C40 -32.7(3) . . . . ?
C63 C64 C65 C66 0.5(3) . . . . ?
C64 C63 C68 C67 2.2(3) . . . . ?
C64 C65 C66 O89 179.44(19) . . . . ?
C64 C65 C66 C67 0.7(3) . . . . ?
C65 C66 C67 C68 -0.5(3) . . . . ?
C66 C67 C68 C63 -1.0(3) . . . . ?
C68 C63 C64 C65 -1.9(3) . . . . ?
C70 O69 C38 C37 -172.65(19) . . . . ?
C70 O69 C38 C39 8.1(3) . . . . ?
C71 N41 C20 C19 149.39(18) . . . . ?
C71 N41 C20 C21 -32.7(3) . . . . ?
C71 N41 C42 C43 138.14(19) . . . . ?
C71 N41 C42 C47 -42.6(3) . . . . ?
C71 C72 C73 C74 -0.4(3) . . . . ?
C72 C71 C76 C75 -0.7(3) . . . . ?
C72 C73 C74 O91 -178.03(18) . . . . ?
C72 C73 C74 C75 -0.6(3) . . . . ?
C73 C74 C75 C76 0.9(3) . . . . ?
C74 C75 C76 C71 -0.3(3) . . . . ?
C76 C71 C72 C73 1.0(3) . . . . ?
C78 O77 C45 C44 176.8(2) . . . . ?
C78 O77 C45 C46 -3.8(3) . . . . ?
C79 N48 C24 C23 -77.6(2) . . . . ?
C79 N48 C24 C25 101.6(2) . . . . ?
C79 N48 C49 C50 -9.9(3) . . . . ?
C79 N48 C49 C54 168.15(19) . . . . ?
C79 C80 C81 C82 -0.6(3) . . . . ?
C80 C79 C84 C83 -1.7(4) . . . . ?
C80 C81 C82 O93 175.6(2) . . . . ?
C80 C81 C82 C83 -2.0(4) . . . . ?
C81 C82 C83 C84 2.7(4) . . . . ?
C82 C83 C84 C79 -0.8(4) . . . . ?
C84 C79 C80 C81 2.4(3) . . . . ?
C86 O85 C52 C51 -179.0(2) . . . . ?
C86 O85 C52 C53 1.5(4) . . . . ?
C88 O87 C58 C57 -3.1(3) . . . . ?
C88 O87 C58 C59 177.2(2) . . . . ?
C90 O89 C66 C65 -179.26(19) . . . . ?
C90 O89 C66 C67 -0.6(3) . . . . ?
C92 O91 C74 C73 -141.2(2) . . . . ?
C92 O91 C74 C75 41.5(3) . . . . ?
C94 O93 C82 C81 -1.1(4) . . . . ?
C94 O93 C82 C83 176.5(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 10 4 0.0262 0.3033 10.1804 4.1826 -0.1299 -0.9915 -0.0090
7 3 5 0.1623 6.6082 3.0457 5.3956 -0.0025 -0.0110 -0.9999
0 -10 -4 0.0508 -0.3033 -10.1804 -4.1826 0.1299 0.9915 0.0090
0 0 -1 0.0167 -0.0000 -0.0000 -1.0000 0.0756 -0.0123 0.0198
0 0 1 0.0167 0.0000 0.0000 1.0000 -0.0756 0.0123 -0.0198
0 5 2 0.0295 0.0000 5.0001 2.0001 -0.0677 -0.4930 0.0176
-2 5 0 0.0877 -1.9999 5.0001 0.0002 -0.0238 -0.5896 0.3380
-5 -2 -4 0.2180 -4.9999 -1.9999 -3.9997 0.0008 -0.0222 0.7584
-1 2 5 0.0740 -0.9999 2.0001 5.0002 -0.3981 -0.1815 0.0641
0 -4 -5 0.0402 -0.0001 -4.0001 -5.0001 0.3111 0.3525 0.0534

_olex2_date_sample_data_collection 2015-08-20
_olex2_date_sample_submission    2015-08-14
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id M18
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nr15009
_database_code_depnum_ccdc_archive 'CCDC 1443040'
_audit_update_record             
;
2015-12-17 deposited with the CCDC.
2016-03-01 downloaded from the CCDC.
;
_audit_creation_date             2015-07-03
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            SFX-TCz
_chemical_name_systematic        
'2, 2?, 7, 7?-Tetrakis (N, N- carbazolo) - spiro (fluorene-9, 9?-xanthene) '
_chemical_formula_moiety         'C73 H44 N4 O'
_chemical_formula_sum            'C73 H44 N4 O'
_chemical_formula_weight         993.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   9.5612(2)
_cell_length_b                   23.4614(4)
_cell_length_c                   46.6024(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10453.8(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5105
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      20.632
_cell_measurement_theta_min      2.303
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.986
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.744552
_exptl_absorpt_correction_T_min  0.630574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0707 before and 0.0651 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0767 before and 0.0684 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 86121 reflections, Rint = 0.0866
 (32024 with I > 3sig(I), Rint = 0.0489)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.102
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13284
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        20.828
_diffrn_reflns_theta_max         20.828
_diffrn_reflns_theta_min         1.736
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker SMART APEXII diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9165
_reflns_number_total             13284
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.904
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         13284
_refine_ls_number_restraints     969
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0916
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1155P)²+32.7285P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2673
_refine_special_details          
;
The measured diffraction pattern is that of a non-merohedral.  The two domains are related by twin law [-1 0 0 / -0.103 1 0 / 0 0 -1] and 

refined twin scale factor 0.423(3).  The two domains overlap for most of the diffraction pattern and it is only really possible to 

distinguish single reflections at higher resolution.  However, observed diffraction ceases at resolutions higher than 1 A (using Mo 

radiation and 30 second/frame exposures) so the data set was cut at this resolution during integration.  Thus the majority of measured 

reflections are composite reflections of both twin domains and so separation of the two domains was not trivial.  This is reflected in 

the high refinement residuals.  Furthermore, approximately one quarter of the molecule was modelled as disordered over two sites 

(discussed below) which brings further problems.

Although the structure solved easily by direct methods it was obvious from the isotropic displacement parameters, residual electron 

density peaks and occupancy refinement that approximately one-quarter of the molecule was disordered over two sites.  This was modelled 

using geometric similarity restraints to keep both disorder components (containing N66 and N66A) the same as the componenet containing 

N27.  Global displacement ellipsoid restraints (the RIGU card in SHELXL) were applied.  Despite this, some ellipsoids (noteably C78A and 

N66A) are rather elongated.  The largest residual peak is 1.90 electrons located 1.50 A from H72.  There is no chemically reasonable 

model for this.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      20.83 Degree

See above.  Data set cut at 1 A.

097_ALERT_2_A Large Reported Max.  (Positive) Residual Density       1.90 eA-3

See above.  The largest residual peak is 1.90 electrons located 1.50 A from H72.

213_ALERT_2_A Atom C78A            has ADP max/min Ratio .....        7.1 prolat

See above for a discussion of disorder in the molecule.  

#===============================================================================
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......      0.955 Note
088_ALERT_3_B Poor Data / Parameter Ratio ....................       6.68 Note

Consequnce of data set truncation.

094_ALERT_2_B Ratio of Maximum / Minimum Residual Density ....       4.06 Report

Discussed above

220_ALERT_2_B Large Non-Solvent  C     Ueq(max)/Ueq(min) Range       10.0 Ratio
222_ALERT_3_B Large Non-Solvent  H     Uiso(max)/Uiso(min) ...        8.9 Ratio
340_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0114 Ang.

Consequence of disorder and data set truncation.  

#===============================================================================
084_ALERT_3_C High wR2 Value (i.e. > 0.25) ...................       0.27 Report
213_ALERT_2_C Atom C69             has ADP max/min Ratio .....        3.5 prolat
213_ALERT_2_C Atom N66A            has ADP max/min Ratio .....        3.9 prolat
213_ALERT_2_C Atom C67A            has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C68A            has ADP max/min Ratio .....        3.4 prolat
213_ALERT_2_C Atom C73A            has ADP max/min Ratio .....        3.1 prolat
220_ALERT_2_C Large Non-Solvent  N     Ueq(max)/Ueq(min) Range        4.8 Ratio
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.2 Note


Consequence of disorder and data set truncation.  


#===============================================================================
;


# start Validation Reply Form
_vrf_DIFMX01_nr15009             
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*2.00
RESPONSE: Please see the _refine_special_details section of the CIF.
;



_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.577(3) 0.423(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C78A) \\sim Ueq, Uanis(N66A) \\sim Ueq: with sigma of 0.3 and sigma for
terminal atoms of 0.4
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39} sigma for
1-2: 0.02, 1-3: 0.02
as
{N66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78}
{N27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39} sigma for
1-2: 0.02, 1-3: 0.02
as
{N66A, C67A, C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A, C76A, C77A, C78A}
6. Others
 Sof(N66A)=Sof(C67A)=Sof(C68A)=Sof(C69A)=Sof(C70A)=Sof(C71A)=Sof(H71A)=
 Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=Sof(C74A)=Sof(H74A)=Sof(C75A)=
 Sof(H75A)=Sof(C76A)=Sof(H76A)=Sof(C77A)=Sof(H77A)=Sof(C78A)=Sof(H78A)=1-FVAR(1)
 Sof(N66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=Sof(C71)=Sof(H71)=Sof(C72)=
 Sof(H72)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=
 Sof(H76)=Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C14(H14), C19(H19),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C71A(H71A),
 C72A(H72A), C73A(H73A), C74A(H74A), C75A(H75A), C76A(H76A), C77A(H77A),
 C78A(H78A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
O1 O 0.2314(5) 0.48951(19) 0.37837(11) 0.0236(13) Uani 1 1 d . U . . .
N27 N 0.5316(6) 0.6912(2) 0.36880(14) 0.0266(17) Uani 1 1 d D U . . .
C28 C 0.5370(8) 0.7356(3) 0.38831(18) 0.030(2) Uani 1 1 d D U . . .
C29 C 0.6096(8) 0.7816(3) 0.37620(19) 0.032(2) Uani 1 1 d D U . . .
C30 C 0.6511(8) 0.7642(3) 0.34752(19) 0.031(2) Uani 1 1 d D U . . .
C31 C 0.6009(8) 0.7079(3) 0.34383(18) 0.027(2) Uani 1 1 d D U . . .
C32 C 0.6224(8) 0.6776(3) 0.31884(18) 0.034(2) Uani 1 1 d D U . . .
H32 H 0.5885 0.6398 0.3168 0.041 Uiso 1 1 calc R . . . .
C33 C 0.6949(9) 0.7042(4) 0.2968(2) 0.043(2) Uani 1 1 d D U . . .
H33 H 0.7104 0.6845 0.2793 0.051 Uiso 1 1 calc R . . . .
C34 C 0.7453(9) 0.7595(4) 0.3001(2) 0.045(3) Uani 1 1 d D U . . .
H34 H 0.7959 0.7767 0.2849 0.054 Uiso 1 1 calc R . . . .
C35 C 0.7233(8) 0.7900(4) 0.3251(2) 0.041(2) Uani 1 1 d D U . . .
H35 H 0.7569 0.8280 0.3270 0.050 Uiso 1 1 calc R . . . .
C36 C 0.4825(9) 0.7376(3) 0.41598(19) 0.040(2) Uani 1 1 d D U . . .
H36 H 0.4316 0.7065 0.4238 0.048 Uiso 1 1 calc R . . . .
C37 C 0.5062(10) 0.7876(3) 0.4318(2) 0.049(3) Uani 1 1 d D U . . .
H37 H 0.4727 0.7901 0.4509 0.059 Uiso 1 1 calc R . . . .
C38 C 0.5765(9) 0.8327(3) 0.4202(2) 0.048(3) Uani 1 1 d D U . . .
H38 H 0.5897 0.8661 0.4314 0.057 Uiso 1 1 calc R . . . .
C39 C 0.6292(9) 0.8311(3) 0.3925(2) 0.041(2) Uani 1 1 d D U . . .
H39 H 0.6775 0.8629 0.3847 0.049 Uiso 1 1 calc R . . . .
N40 N 0.4515(7) 0.2722(2) 0.36531(14) 0.0281(17) Uani 1 1 d . U . . .
N53 N 0.7044(6) 0.4747(2) 0.27121(14) 0.0257(16) Uani 1 1 d . U . . .
N66 N 0.691(2) 0.4778(5) 0.4772(3) 0.020(4) Uani 0.502(6) 1 d D U P A 1
C67 C 0.6189(16) 0.4335(5) 0.4905(3) 0.025(4) Uani 0.502(6) 1 d D U P A 1
C68 C 0.6214(16) 0.4425(6) 0.5205(3) 0.028(4) Uani 0.502(6) 1 d D U P A 1
C69 C 0.7130(19) 0.4915(5) 0.5260(3) 0.016(4) Uani 0.502(6) 1 d D U P A 1
C70 C 0.7515(16) 0.5116(5) 0.4988(3) 0.017(4) Uani 0.502(6) 1 d D U P A 1
C71 C 0.8316(16) 0.5603(6) 0.4955(3) 0.030(4) Uani 0.502(6) 1 d D U P A 1
H71 H 0.8613 0.5727 0.4770 0.036 Uiso 0.502(6) 1 calc R . P A 1
C72 C 0.8666(16) 0.5901(7) 0.5199(3) 0.037(5) Uani 0.502(6) 1 d D U P A 1
H72 H 0.9217 0.6237 0.5183 0.044 Uiso 0.502(6) 1 calc R . P A 1
C73 C 0.823(2) 0.5722(7) 0.5467(4) 0.041(5) Uani 0.502(6) 1 d D U P A 1
H73 H 0.8434 0.5952 0.5630 0.050 Uiso 0.502(6) 1 calc R . P A 1
C74 C 0.7509(17) 0.5214(6) 0.5505(3) 0.028(4) Uani 0.502(6) 1 d D U P A 1
H74 H 0.7282 0.5077 0.5691 0.033 Uiso 0.502(6) 1 calc R . P A 1
C75 C 0.5477(15) 0.3875(5) 0.4786(3) 0.031(4) Uani 0.502(6) 1 d D U P A 1
H75 H 0.5475 0.3813 0.4584 0.037 Uiso 0.502(6) 1 calc R . P A 1
C76 C 0.4753(18) 0.3502(6) 0.4974(3) 0.037(5) Uani 0.502(6) 1 d D U P A 1
H76 H 0.4260 0.3184 0.4899 0.044 Uiso 0.502(6) 1 calc R . P A 1
C77 C 0.4763(18) 0.3598(7) 0.5258(4) 0.047(5) Uani 0.502(6) 1 d D U P A 1
H77 H 0.4255 0.3346 0.5379 0.056 Uiso 0.502(6) 1 calc R . P A 1
C78 C 0.5474(17) 0.4045(6) 0.5383(3) 0.039(4) Uani 0.502(6) 1 d D U P A 1
H78 H 0.5465 0.4096 0.5585 0.047 Uiso 0.502(6) 1 calc R . P A 1
C2 C 0.2970(8) 0.4368(3) 0.37560(16) 0.0191(19) Uani 1 1 d . U . . .
C3 C 0.4397(8) 0.4297(3) 0.37360(16) 0.0182(18) Uani 1 1 d . U . . .
C4 C 0.5391(7) 0.4801(3) 0.37397(16) 0.0184(17) Uani 1 1 d . U . . .
C5 C 0.4576(8) 0.5360(3) 0.37397(16) 0.0174(18) Uani 1 1 d . U . . .
C6 C 0.3152(8) 0.5380(3) 0.37689(16) 0.0199(19) Uani 1 1 d . U . . .
C7 C 0.2418(8) 0.5887(3) 0.37819(16) 0.024(2) Uani 1 1 d . U . . .
H7 H 0.1432 0.5886 0.3806 0.029 Uiso 1 1 calc R . . . .
C8 C 0.3136(8) 0.6395(3) 0.37590(17) 0.027(2) Uani 1 1 d . U . . .
H8 H 0.2647 0.6747 0.3766 0.033 Uiso 1 1 calc R . . . .
C9 C 0.4567(8) 0.6388(3) 0.37256(17) 0.024(2) Uani 1 1 d . U . . .
C10 C 0.5286(8) 0.5879(3) 0.37205(16) 0.0215(19) Uani 1 1 d . U . . .
H10 H 0.6276 0.5881 0.3704 0.026 Uiso 1 1 calc R . . . .
C11 C 0.2032(8) 0.3912(3) 0.37442(16) 0.024(2) Uani 1 1 d . U . . .
H11 H 0.1054 0.3976 0.3758 0.029 Uiso 1 1 calc R . . . .
C12 C 0.2552(9) 0.3367(3) 0.37118(16) 0.026(2) Uani 1 1 d . U . . .
H12 H 0.1931 0.3051 0.3703 0.031 Uiso 1 1 calc R . . . .
C13 C 0.3980(8) 0.3282(3) 0.36929(16) 0.023(2) Uani 1 1 d . U . . .
C14 C 0.4880(8) 0.3742(3) 0.37053(16) 0.022(2) Uani 1 1 d . U . . .
H14 H 0.5859 0.3676 0.3693 0.026 Uiso 1 1 calc R . . . .
C15 C 0.6409(8) 0.4800(3) 0.40004(17) 0.0209(18) Uani 1 1 d . U . . .
C16 C 0.7800(8) 0.4854(3) 0.39090(17) 0.0203(18) Uani 1 1 d . U . . .
C17 C 0.7820(8) 0.4844(3) 0.35928(17) 0.0201(18) Uani 1 1 d . U . . .
C18 C 0.6445(8) 0.4792(3) 0.34930(17) 0.0208(18) Uani 1 1 d . U . . .
C19 C 0.6170(8) 0.4756(3) 0.32012(17) 0.0223(19) Uani 1 1 d . U . . .
H19 H 0.5241 0.4708 0.3133 0.027 Uiso 1 1 calc R . . . .
C20 C 0.7296(9) 0.4790(3) 0.30114(17) 0.0223(19) Uani 1 1 d . U . . .
C21 C 0.8637(9) 0.4856(3) 0.31092(18) 0.026(2) Uani 1 1 d . U . . .
H21 H 0.9385 0.4880 0.2976 0.031 Uiso 1 1 calc R . . . .
C22 C 0.8919(9) 0.4888(3) 0.34014(18) 0.026(2) Uani 1 1 d . U . . .
H22 H 0.9849 0.4938 0.3468 0.031 Uiso 1 1 calc R . . . .
C23 C 0.6088(9) 0.4787(3) 0.42877(18) 0.027(2) Uani 1 1 d . U . . .
H23 H 0.5146 0.4755 0.4351 0.032 Uiso 1 1 calc R . . . .
C24 C 0.7179(9) 0.4822(3) 0.44837(18) 0.033(2) Uani 1 1 d . U . . .
C25 C 0.8558(9) 0.4887(3) 0.43941(18) 0.030(2) Uani 1 1 d . U . . .
H25 H 0.9286 0.4922 0.4532 0.036 Uiso 1 1 calc R . . . .
C26 C 0.8865(8) 0.4902(3) 0.41060(18) 0.0249(19) Uani 1 1 d . U . . .
H26 H 0.9804 0.4945 0.4043 0.030 Uiso 1 1 calc R . . . .
C41 C 0.4325(8) 0.2404(3) 0.34003(19) 0.027(2) Uani 1 1 d . U . . .
C42 C 0.4957(8) 0.1868(3) 0.34384(19) 0.029(2) Uani 1 1 d . U . . .
C43 C 0.5522(8) 0.1858(3) 0.3723(2) 0.032(2) Uani 1 1 d . U . . .
C44 C 0.5227(8) 0.2389(3) 0.38486(19) 0.029(2) Uani 1 1 d . U . . .
C45 C 0.5615(9) 0.2521(4) 0.4128(2) 0.038(2) Uani 1 1 d . U . . .
H45 H 0.5414 0.2884 0.4208 0.046 Uiso 1 1 calc R . . . .
C46 C 0.6306(9) 0.2104(4) 0.4285(2) 0.049(3) Uani 1 1 d . U . . .
H46 H 0.6588 0.2183 0.4476 0.059 Uiso 1 1 calc R . . . .
C47 C 0.6597(9) 0.1566(4) 0.4164(2) 0.050(3) Uani 1 1 d . U . . .
H47 H 0.7072 0.1286 0.4275 0.060 Uiso 1 1 calc R . . . .
C48 C 0.6194(9) 0.1441(4) 0.3886(2) 0.042(2) Uani 1 1 d . U . . .
H48 H 0.6374 0.1076 0.3807 0.051 Uiso 1 1 calc R . . . .
C49 C 0.3653(9) 0.2556(3) 0.31484(19) 0.037(2) Uani 1 1 d . U . . .
H49 H 0.3229 0.2920 0.3126 0.044 Uiso 1 1 calc R . . . .
C50 C 0.3625(9) 0.2153(4) 0.2929(2) 0.041(2) Uani 1 1 d . U . . .
H50 H 0.3160 0.2242 0.2755 0.050 Uiso 1 1 calc R . . . .
C51 C 0.4257(10) 0.1628(4) 0.2960(2) 0.046(2) Uani 1 1 d . U . . .
H51 H 0.4240 0.1367 0.2804 0.055 Uiso 1 1 calc R . . . .
C52 C 0.4907(9) 0.1476(4) 0.3209(2) 0.042(2) Uani 1 1 d . U . . .
H52 H 0.5321 0.1110 0.3229 0.051 Uiso 1 1 calc R . . . .
C54 C 0.7617(8) 0.5105(3) 0.25010(17) 0.0250(19) Uani 1 1 d . U . . .
C55 C 0.7359(8) 0.4876(3) 0.22287(17) 0.0238(19) Uani 1 1 d . U . . .
C56 C 0.6644(8) 0.4342(3) 0.22737(18) 0.027(2) Uani 1 1 d . U . . .
C57 C 0.6431(8) 0.4276(3) 0.25707(18) 0.0238(19) Uani 1 1 d . U . . .
C58 C 0.5755(8) 0.3806(3) 0.26843(19) 0.033(2) Uani 1 1 d . U . . .
H58 H 0.5614 0.3765 0.2885 0.040 Uiso 1 1 calc R . . . .
C59 C 0.5291(9) 0.3396(3) 0.2491(2) 0.041(2) Uani 1 1 d . U . . .
H59 H 0.4801 0.3073 0.2562 0.050 Uiso 1 1 calc R . . . .
C60 C 0.5522(9) 0.3442(4) 0.2197(2) 0.041(2) Uani 1 1 d . U . . .
H60 H 0.5218 0.3147 0.2072 0.050 Uiso 1 1 calc R . . . .
C61 C 0.6184(9) 0.3911(3) 0.20873(19) 0.036(2) Uani 1 1 d . U . . .
H61 H 0.6331 0.3945 0.1886 0.044 Uiso 1 1 calc R . . . .
C62 C 0.8288(8) 0.5625(3) 0.25361(18) 0.030(2) Uani 1 1 d . U . . .
H62 H 0.8466 0.5778 0.2721 0.036 Uiso 1 1 calc R . . . .
C63 C 0.8686(9) 0.5911(3) 0.22902(19) 0.035(2) Uani 1 1 d . U . . .
H63 H 0.9175 0.6262 0.2307 0.043 Uiso 1 1 calc R . . . .
C64 C 0.8391(9) 0.5700(3) 0.20196(18) 0.034(2) Uani 1 1 d . U . . .
H64 H 0.8652 0.5914 0.1855 0.041 Uiso 1 1 calc R . . . .
C65 C 0.7728(8) 0.5188(3) 0.19855(18) 0.031(2) Uani 1 1 d . U . . .
H65 H 0.7523 0.5046 0.1799 0.037 Uiso 1 1 calc R . . . .
N66A N 0.688(4) 0.4834(9) 0.4803(4) 0.096(8) Uani 0.498(6) 1 d D U P A 2
C67A C 0.729(3) 0.4369(10) 0.4974(5) 0.123(9) Uani 0.498(6) 1 d D U P A 2
C68A C 0.750(3) 0.4568(11) 0.5255(5) 0.145(10) Uani 0.498(6) 1 d D U P A 2
C69A C 0.719(4) 0.5175(11) 0.5261(4) 0.141(10) Uani 0.498(6) 1 d D U P A 2
C70A C 0.686(3) 0.5329(10) 0.4981(5) 0.126(10) Uani 0.498(6) 1 d D U P A 2
C71A C 0.652(3) 0.5878(10) 0.4891(5) 0.132(9) Uani 0.498(6) 1 d D U P A 2
H71A H 0.6239 0.5965 0.4701 0.158 Uiso 0.498(6) 1 calc R . P A 2
C72A C 0.663(4) 0.6297(11) 0.5112(6) 0.181(13) Uani 0.498(6) 1 d D U P A 2
H72A H 0.6442 0.6685 0.5069 0.217 Uiso 0.498(6) 1 calc R . P A 2
C73A C 0.701(4) 0.6149(13) 0.5382(6) 0.183(13) Uani 0.498(6) 1 d D U P A 2
H73A H 0.6987 0.6438 0.5524 0.219 Uiso 0.498(6) 1 calc R . P A 2
C74A C 0.744(5) 0.5609(14) 0.5466(5) 0.183(15) Uani 0.498(6) 1 d D U P A 2
H74A H 0.7856 0.5536 0.5647 0.219 Uiso 0.498(6) 1 calc R . P A 2
C75A C 0.740(3) 0.3803(11) 0.4889(5) 0.143(10) Uani 0.498(6) 1 d D U P A 2
H75A H 0.7184 0.3681 0.4700 0.172 Uiso 0.498(6) 1 calc R . P A 2
C76A C 0.789(3) 0.3403(12) 0.5116(6) 0.181(12) Uani 0.498(6) 1 d D U P A 2
H76A H 0.8001 0.3008 0.5078 0.217 Uiso 0.498(6) 1 calc R . P A 2
C77A C 0.816(4) 0.3609(13) 0.5366(6) 0.193(15) Uani 0.498(6) 1 d D U P A 2
H77A H 0.8540 0.3349 0.5502 0.231 Uiso 0.498(6) 1 calc R . P A 2
C78A C 0.797(3) 0.4163(13) 0.5462(5) 0.162(11) Uani 0.498(6) 1 d D U P A 2
H78A H 0.8144 0.4267 0.5656 0.194 Uiso 0.498(6) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.393(8) . ?
O1 C6 1.393(8) . ?
N27 C28 1.384(9) . ?
N27 C31 1.395(9) . ?
N27 C9 1.433(9) . ?
C28 C29 1.402(10) . ?
C28 C36 1.391(11) . ?
C29 C30 1.453(11) . ?
C29 C39 1.399(10) . ?
C30 C31 1.415(10) . ?
C30 C35 1.389(11) . ?
C31 C32 1.380(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.387(11) . ?
C33 H33 0.9500 . ?
C33 C34 1.392(11) . ?
C34 H34 0.9500 . ?
C34 C35 1.384(11) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C36 C37 1.404(10) . ?
C37 H37 0.9500 . ?
C37 C38 1.365(11) . ?
C38 H38 0.9500 . ?
C38 C39 1.386(11) . ?
C39 H39 0.9500 . ?
N40 C13 1.423(9) . ?
N40 C41 1.406(10) . ?
N40 C44 1.379(10) . ?
N53 C20 1.419(10) . ?
N53 C54 1.405(9) . ?
N53 C57 1.412(9) . ?
N66 C67 1.393(18) . ?
N66 C70 1.409(17) . ?
N66 C24 1.371(16) . ?
C67 C68 1.413(17) . ?
C67 C75 1.393(16) . ?
C68 C69 1.468(17) . ?
C68 C78 1.409(16) . ?
C69 C70 1.402(17) . ?
C69 C74 1.387(16) . ?
C70 C71 1.385(16) . ?
C71 H71 0.9500 . ?
C71 C72 1.378(17) . ?
C72 H72 0.9500 . ?
C72 C73 1.382(19) . ?
C73 H73 0.9500 . ?
C73 C74 1.39(2) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
C75 C76 1.419(17) . ?
C76 H76 0.9500 . ?
C76 C77 1.344(18) . ?
C77 H77 0.9500 . ?
C77 C78 1.379(18) . ?
C78 H78 0.9500 . ?
C2 C3 1.378(10) . ?
C2 C11 1.397(10) . ?
C3 C4 1.516(10) . ?
C3 C14 1.391(9) . ?
C4 C5 1.526(9) . ?
C4 C15 1.556(10) . ?
C4 C18 1.529(11) . ?
C5 C6 1.369(10) . ?
C5 C10 1.397(9) . ?
C6 C7 1.382(10) . ?
C7 H7 0.9500 . ?
C7 C8 1.379(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(10) . ?
C9 C10 1.378(10) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.381(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(10) . ?
C13 C14 1.380(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.402(10) . ?
C15 C23 1.374(10) . ?
C16 C17 1.474(10) . ?
C16 C26 1.376(10) . ?
C17 C18 1.400(10) . ?
C17 C22 1.382(10) . ?
C18 C19 1.388(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.397(10) . ?
C20 C21 1.369(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.390(10) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.389(11) . ?
C24 C25 1.392(11) . ?
C24 N66A 1.52(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.375(10) . ?
C26 H26 0.9500 . ?
C41 C42 1.406(10) . ?
C41 C49 1.385(11) . ?
C42 C43 1.431(11) . ?
C42 C52 1.410(11) . ?
C43 C44 1.406(11) . ?
C43 C48 1.395(11) . ?
C44 C45 1.387(11) . ?
C45 H45 0.9500 . ?
C45 C46 1.390(11) . ?
C46 H46 0.9500 . ?
C46 C47 1.410(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.384(12) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C49 C50 1.391(11) . ?
C50 H50 0.9500 . ?
C50 C51 1.380(12) . ?
C51 H51 0.9500 . ?
C51 C52 1.366(12) . ?
C52 H52 0.9500 . ?
C54 C55 1.400(10) . ?
C54 C62 1.389(10) . ?
C55 C56 1.443(10) . ?
C55 C65 1.393(11) . ?
C56 C57 1.408(11) . ?
C56 C61 1.404(11) . ?
C57 C58 1.384(10) . ?
C58 H58 0.9500 . ?
C58 C59 1.391(11) . ?
C59 H59 0.9500 . ?
C59 C60 1.391(12) . ?
C60 H60 0.9500 . ?
C60 C61 1.368(11) . ?
C61 H61 0.9500 . ?
C62 H62 0.9500 . ?
C62 C63 1.381(11) . ?
C63 H63 0.9500 . ?
C63 C64 1.384(11) . ?
C64 H64 0.9500 . ?
C64 C65 1.367(11) . ?
C65 H65 0.9500 . ?
N66A C67A 1.41(2) . ?
N66A C70A 1.426(19) . ?
C67A C68A 1.40(2) . ?
C67A C75A 1.39(2) . ?
C68A C69A 1.46(2) . ?
C68A C78A 1.43(2) . ?
C69A C70A 1.39(2) . ?
C69A C74A 1.42(2) . ?
C70A C71A 1.39(2) . ?
C71A H71A 0.9500 . ?
C71A C72A 1.43(2) . ?
C72A H72A 0.9500 . ?
C72A C73A 1.35(2) . ?
C73A H73A 0.9500 . ?
C73A C74A 1.39(3) . ?
C74A H74A 0.9500 . ?
C75A H75A 0.9500 . ?
C75A C76A 1.49(2) . ?
C76A H76A 0.9500 . ?
C76A C77A 1.29(2) . ?
C77A H77A 0.9500 . ?
C77A C78A 1.39(2) . ?
C78A H78A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 C6 117.5(6) . . ?
C28 N27 C31 108.6(6) . . ?
C28 N27 C9 125.7(7) . . ?
C31 N27 C9 125.5(6) . . ?
N27 C28 C29 109.5(7) . . ?
N27 C28 C36 128.3(7) . . ?
C36 C28 C29 122.2(7) . . ?
C28 C29 C30 106.9(7) . . ?
C39 C29 C28 119.2(8) . . ?
C39 C29 C30 134.0(8) . . ?
C31 C30 C29 106.3(7) . . ?
C35 C30 C29 134.8(8) . . ?
C35 C30 C31 119.0(8) . . ?
N27 C31 C30 108.8(7) . . ?
C32 C31 N27 129.0(7) . . ?
C32 C31 C30 122.2(7) . . ?
C31 C32 H32 121.1 . . ?
C31 C32 C33 117.8(8) . . ?
C33 C32 H32 121.1 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.7(9) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 119.2 . . ?
C35 C34 C33 121.5(8) . . ?
C35 C34 H34 119.2 . . ?
C30 C35 H35 120.6 . . ?
C34 C35 C30 118.8(8) . . ?
C34 C35 H35 120.6 . . ?
C28 C36 H36 121.5 . . ?
C28 C36 C37 117.0(8) . . ?
C37 C36 H36 121.5 . . ?
C36 C37 H37 119.4 . . ?
C38 C37 C36 121.3(9) . . ?
C38 C37 H37 119.4 . . ?
C37 C38 H38 119.1 . . ?
C37 C38 C39 121.8(8) . . ?
C39 C38 H38 119.1 . . ?
C29 C39 H39 120.7 . . ?
C38 C39 C29 118.6(8) . . ?
C38 C39 H39 120.7 . . ?
C41 N40 C13 123.5(6) . . ?
C44 N40 C13 127.9(7) . . ?
C44 N40 C41 108.5(6) . . ?
C54 N53 C20 125.3(6) . . ?
C54 N53 C57 107.6(7) . . ?
C57 N53 C20 125.8(6) . . ?
C67 N66 C70 107.7(12) . . ?
C24 N66 C67 125.9(11) . . ?
C24 N66 C70 125.6(14) . . ?
N66 C67 C68 108.8(11) . . ?
C75 C67 N66 129.9(13) . . ?
C75 C67 C68 121.3(12) . . ?
C67 C68 C69 107.5(10) . . ?
C78 C68 C67 118.7(12) . . ?
C78 C68 C69 133.7(13) . . ?
C70 C69 C68 105.2(10) . . ?
C74 C69 C68 134.2(13) . . ?
C74 C69 C70 120.3(12) . . ?
C69 C70 N66 110.5(12) . . ?
C71 C70 N66 127.7(12) . . ?
C71 C70 C69 121.7(12) . . ?
C70 C71 H71 121.3 . . ?
C72 C71 C70 117.3(13) . . ?
C72 C71 H71 121.3 . . ?
C71 C72 H72 119.3 . . ?
C71 C72 C73 121.4(14) . . ?
C73 C72 H72 119.3 . . ?
C72 C73 H73 119.2 . . ?
C72 C73 C74 121.7(14) . . ?
C74 C73 H73 119.2 . . ?
C69 C74 C73 117.4(14) . . ?
C69 C74 H74 121.3 . . ?
C73 C74 H74 121.3 . . ?
C67 C75 H75 121.0 . . ?
C67 C75 C76 118.0(13) . . ?
C76 C75 H75 121.0 . . ?
C75 C76 H76 119.9 . . ?
C77 C76 C75 120.2(14) . . ?
C77 C76 H76 119.9 . . ?
C76 C77 H77 118.4 . . ?
C76 C77 C78 123.2(14) . . ?
C78 C77 H77 118.4 . . ?
C68 C78 H78 120.7 . . ?
C77 C78 C68 118.6(14) . . ?
C77 C78 H78 120.7 . . ?
O1 C2 C11 113.3(7) . . ?
C3 C2 O1 124.0(6) . . ?
C3 C2 C11 122.7(7) . . ?
C2 C3 C4 121.8(6) . . ?
C2 C3 C14 116.7(7) . . ?
C14 C3 C4 121.5(7) . . ?
C3 C4 C5 110.5(6) . . ?
C3 C4 C15 113.6(6) . . ?
C3 C4 C18 113.2(6) . . ?
C5 C4 C15 108.7(6) . . ?
C5 C4 C18 110.4(6) . . ?
C18 C4 C15 100.1(6) . . ?
C6 C5 C4 122.5(6) . . ?
C6 C5 C10 117.3(7) . . ?
C10 C5 C4 120.1(7) . . ?
C5 C6 O1 123.3(6) . . ?
C5 C6 C7 122.6(7) . . ?
C7 C6 O1 114.1(7) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.2(7) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.6(7) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 N27 120.0(7) . . ?
C8 C9 C10 120.4(7) . . ?
C10 C9 N27 119.5(7) . . ?
C5 C10 H10 119.6 . . ?
C9 C10 C5 120.8(7) . . ?
C9 C10 H10 119.6 . . ?
C2 C11 H11 120.6 . . ?
C12 C11 C2 118.9(7) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.7(7) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 N40 119.7(7) . . ?
C14 C13 N40 120.2(7) . . ?
C14 C13 C12 120.0(7) . . ?
C3 C14 H14 119.0 . . ?
C13 C14 C3 122.0(7) . . ?
C13 C14 H14 119.0 . . ?
C16 C15 C4 110.8(7) . . ?
C23 C15 C4 128.4(7) . . ?
C23 C15 C16 120.6(7) . . ?
C15 C16 C17 108.4(7) . . ?
C26 C16 C15 120.5(8) . . ?
C26 C16 C17 131.2(8) . . ?
C18 C17 C16 108.7(7) . . ?
C22 C17 C16 130.9(8) . . ?
C22 C17 C18 120.4(8) . . ?
C17 C18 C4 111.6(7) . . ?
C19 C18 C4 127.8(7) . . ?
C19 C18 C17 120.6(7) . . ?
C18 C19 H19 121.0 . . ?
C18 C19 C20 118.1(8) . . ?
C20 C19 H19 121.0 . . ?
C19 C20 N53 119.1(7) . . ?
C21 C20 N53 119.7(7) . . ?
C21 C20 C19 121.2(8) . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 120.9(8) . . ?
C22 C21 H21 119.5 . . ?
C17 C22 C21 118.7(8) . . ?
C17 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C15 C23 H23 120.9 . . ?
C15 C23 C24 118.1(8) . . ?
C24 C23 H23 120.9 . . ?
N66 C24 C23 119.9(12) . . ?
N66 C24 C25 118.7(12) . . ?
C23 C24 C25 121.4(8) . . ?
C23 C24 N66A 120.2(15) . . ?
C25 C24 N66A 118.3(15) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.9(8) . . ?
C26 C25 H25 120.1 . . ?
C16 C26 H26 120.3 . . ?
C25 C26 C16 119.5(8) . . ?
C25 C26 H26 120.3 . . ?
N40 C41 C42 108.2(7) . . ?
C49 C41 N40 129.4(7) . . ?
C49 C41 C42 122.4(8) . . ?
C41 C42 C43 107.1(7) . . ?
C41 C42 C52 118.2(8) . . ?
C52 C42 C43 134.6(8) . . ?
C44 C43 C42 107.2(7) . . ?
C48 C43 C42 133.7(8) . . ?
C48 C43 C44 119.1(9) . . ?
N40 C44 C43 109.0(8) . . ?
N40 C44 C45 128.7(7) . . ?
C45 C44 C43 122.3(8) . . ?
C44 C45 H45 121.1 . . ?
C44 C45 C46 117.7(9) . . ?
C46 C45 H45 121.1 . . ?
C45 C46 H46 119.5 . . ?
C45 C46 C47 120.9(10) . . ?
C47 C46 H46 119.5 . . ?
C46 C47 H47 119.8 . . ?
C48 C47 C46 120.5(9) . . ?
C48 C47 H47 119.8 . . ?
C43 C48 H48 120.3 . . ?
C47 C48 C43 119.4(9) . . ?
C47 C48 H48 120.3 . . ?
C41 C49 H49 121.4 . . ?
C41 C49 C50 117.2(8) . . ?
C50 C49 H49 121.4 . . ?
C49 C50 H50 119.3 . . ?
C51 C50 C49 121.5(9) . . ?
C51 C50 H50 119.3 . . ?
C50 C51 H51 119.3 . . ?
C52 C51 C50 121.4(9) . . ?
C52 C51 H51 119.3 . . ?
C42 C52 H52 120.4 . . ?
C51 C52 C42 119.3(8) . . ?
C51 C52 H52 120.4 . . ?
C55 C54 N53 109.7(7) . . ?
C62 C54 N53 128.6(8) . . ?
C62 C54 C55 121.7(7) . . ?
C54 C55 C56 106.5(7) . . ?
C65 C55 C54 119.5(7) . . ?
C65 C55 C56 133.9(8) . . ?
C57 C56 C55 107.9(7) . . ?
C61 C56 C55 133.2(8) . . ?
C61 C56 C57 118.9(8) . . ?
C56 C57 N53 108.2(7) . . ?
C58 C57 N53 129.7(8) . . ?
C58 C57 C56 122.1(7) . . ?
C57 C58 H58 121.5 . . ?
C57 C58 C59 116.9(8) . . ?
C59 C58 H58 121.5 . . ?
C58 C59 H59 118.9 . . ?
C60 C59 C58 122.2(8) . . ?
C60 C59 H59 118.9 . . ?
C59 C60 H60 119.8 . . ?
C61 C60 C59 120.3(8) . . ?
C61 C60 H60 119.8 . . ?
C56 C61 H61 120.3 . . ?
C60 C61 C56 119.5(9) . . ?
C60 C61 H61 120.3 . . ?
C54 C62 H62 121.4 . . ?
C63 C62 C54 117.2(8) . . ?
C63 C62 H62 121.4 . . ?
C62 C63 H63 119.1 . . ?
C62 C63 C64 121.7(8) . . ?
C64 C63 H63 119.1 . . ?
C63 C64 H64 119.5 . . ?
C65 C64 C63 121.0(8) . . ?
C65 C64 H64 119.5 . . ?
C55 C65 H65 120.5 . . ?
C64 C65 C55 118.9(8) . . ?
C64 C65 H65 120.5 . . ?
C67A N66A C24 119(2) . . ?
C67A N66A C70A 107.7(14) . . ?
C70A N66A C24 126.0(16) . . ?
C68A C67A N66A 108.2(15) . . ?
C75A C67A N66A 126.9(18) . . ?
C75A C67A C68A 124.8(17) . . ?
C67A C68A C69A 108.1(15) . . ?
C67A C68A C78A 117.1(17) . . ?
C78A C68A C69A 134.8(19) . . ?
C70A C69A C68A 106.5(14) . . ?
C70A C69A C74A 119.0(18) . . ?
C74A C69A C68A 133(2) . . ?
C69A C70A N66A 109.4(15) . . ?
C69A C70A C71A 125.0(17) . . ?
C71A C70A N66A 125.6(18) . . ?
C70A C71A H71A 123.1 . . ?
C70A C71A C72A 113.8(19) . . ?
C72A C71A H71A 123.1 . . ?
C71A C72A H72A 119.5 . . ?
C73A C72A C71A 121(2) . . ?
C73A C72A H72A 119.5 . . ?
C72A C73A H73A 117.5 . . ?
C72A C73A C74A 125(2) . . ?
C74A C73A H73A 117.5 . . ?
C69A C74A H74A 122.6 . . ?
C73A C74A C69A 115(2) . . ?
C73A C74A H74A 122.6 . . ?
C67A C75A H75A 122.5 . . ?
C67A C75A C76A 115.1(19) . . ?
C76A C75A H75A 122.5 . . ?
C75A C76A H76A 121.0 . . ?
C77A C76A C75A 118(2) . . ?
C77A C76A H76A 121.0 . . ?
C76A C77A H77A 116.0 . . ?
C76A C77A C78A 128(2) . . ?
C78A C77A H77A 116.0 . . ?
C68A C78A H78A 121.7 . . ?
C77A C78A C68A 117(2) . . ?
C77A C78A H78A 121.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 -0.6(11) . . . . ?
O1 C2 C3 C14 -179.2(6) . . . . ?
O1 C2 C11 C12 178.9(6) . . . . ?
O1 C6 C7 C8 -177.7(7) . . . . ?
N27 C28 C29 C30 0.0(9) . . . . ?
N27 C28 C29 C39 -179.2(7) . . . . ?
N27 C28 C36 C37 178.1(8) . . . . ?
N27 C31 C32 C33 179.8(7) . . . . ?
N27 C9 C10 C5 -176.2(7) . . . . ?
C28 N27 C31 C30 -0.1(8) . . . . ?
C28 N27 C31 C32 179.6(8) . . . . ?
C28 N27 C9 C8 61.3(10) . . . . ?
C28 N27 C9 C10 -120.4(8) . . . . ?
C28 C29 C30 C31 -0.1(8) . . . . ?
C28 C29 C30 C35 179.6(9) . . . . ?
C28 C29 C39 C38 0.4(12) . . . . ?
C28 C36 C37 C38 1.6(13) . . . . ?
C29 C28 C36 C37 -1.5(12) . . . . ?
C29 C30 C31 N27 0.1(8) . . . . ?
C29 C30 C31 C32 -179.6(7) . . . . ?
C29 C30 C35 C34 179.5(8) . . . . ?
C30 C29 C39 C38 -178.5(8) . . . . ?
C30 C31 C32 C33 -0.5(12) . . . . ?
C31 N27 C28 C29 0.1(9) . . . . ?
C31 N27 C28 C36 -179.5(8) . . . . ?
C31 N27 C9 C8 -112.7(8) . . . . ?
C31 N27 C9 C10 65.6(10) . . . . ?
C31 C30 C35 C34 -0.9(12) . . . . ?
C31 C32 C33 C34 0.7(12) . . . . ?
C32 C33 C34 C35 -1.0(13) . . . . ?
C33 C34 C35 C30 1.1(13) . . . . ?
C35 C30 C31 N27 -179.6(7) . . . . ?
C35 C30 C31 C32 0.6(12) . . . . ?
C36 C28 C29 C30 179.7(7) . . . . ?
C36 C28 C29 C39 0.5(12) . . . . ?
C36 C37 C38 C39 -0.8(14) . . . . ?
C37 C38 C39 C29 -0.2(13) . . . . ?
C39 C29 C30 C31 178.9(9) . . . . ?
C39 C29 C30 C35 -1.5(16) . . . . ?
N40 C13 C14 C3 178.2(7) . . . . ?
N40 C41 C42 C43 1.0(9) . . . . ?
N40 C41 C42 C52 -179.5(7) . . . . ?
N40 C41 C49 C50 179.8(8) . . . . ?
N40 C44 C45 C46 178.6(8) . . . . ?
N53 C20 C21 C22 -178.6(6) . . . . ?
N53 C54 C55 C56 -2.4(8) . . . . ?
N53 C54 C55 C65 174.4(7) . . . . ?
N53 C54 C62 C63 -176.2(7) . . . . ?
N53 C57 C58 C59 -177.9(7) . . . . ?
N66 C67 C68 C69 -6(2) . . . . ?
N66 C67 C68 C78 176.3(16) . . . . ?
N66 C67 C75 C76 -176.1(18) . . . . ?
N66 C70 C71 C72 172.8(17) . . . . ?
N66 C24 C25 C26 176.6(8) . . . . ?
C67 N66 C70 C69 -3(2) . . . . ?
C67 N66 C70 C71 -179.5(17) . . . . ?
C67 N66 C24 C23 54(2) . . . . ?
C67 N66 C24 C25 -124.6(19) . . . . ?
C67 C68 C69 C70 4.3(18) . . . . ?
C67 C68 C69 C74 176.7(18) . . . . ?
C67 C68 C78 C77 1(2) . . . . ?
C67 C75 C76 C77 0(2) . . . . ?
C68 C67 C75 C76 1(2) . . . . ?
C68 C69 C70 N66 -0.7(19) . . . . ?
C68 C69 C70 C71 175.9(15) . . . . ?
C68 C69 C74 C73 -169.4(19) . . . . ?
C69 C68 C78 C77 -176.0(18) . . . . ?
C69 C70 C71 C72 -3(2) . . . . ?
C70 N66 C67 C68 6(2) . . . . ?
C70 N66 C67 C75 -176.6(17) . . . . ?
C70 N66 C24 C23 -137.9(17) . . . . ?
C70 N66 C24 C25 44(2) . . . . ?
C70 C69 C74 C73 2(2) . . . . ?
C70 C71 C72 C73 0(2) . . . . ?
C71 C72 C73 C74 5(3) . . . . ?
C72 C73 C74 C69 -5(3) . . . . ?
C74 C69 C70 N66 -174.4(16) . . . . ?
C74 C69 C70 C71 2(2) . . . . ?
C75 C67 C68 C69 175.9(15) . . . . ?
C75 C67 C68 C78 -1(2) . . . . ?
C75 C76 C77 C78 -1(3) . . . . ?
C76 C77 C78 C68 1(3) . . . . ?
C78 C68 C69 C70 -179.0(17) . . . . ?
C78 C68 C69 C74 -7(3) . . . . ?
C2 O1 C6 C5 -2.5(10) . . . . ?
C2 O1 C6 C7 176.5(6) . . . . ?
C2 C3 C4 C5 -5.2(9) . . . . ?
C2 C3 C4 C15 117.2(8) . . . . ?
C2 C3 C4 C18 -129.6(7) . . . . ?
C2 C3 C14 C13 0.5(10) . . . . ?
C2 C11 C12 C13 0.3(11) . . . . ?
C3 C2 C11 C12 0.1(11) . . . . ?
C3 C4 C5 C6 7.5(10) . . . . ?
C3 C4 C5 C10 -175.0(6) . . . . ?
C3 C4 C15 C16 127.4(7) . . . . ?
C3 C4 C15 C23 -56.7(9) . . . . ?
C3 C4 C18 C17 -127.1(7) . . . . ?
C3 C4 C18 C19 54.7(9) . . . . ?
C4 C3 C14 C13 -178.0(7) . . . . ?
C4 C5 C6 O1 -4.0(11) . . . . ?
C4 C5 C6 C7 177.0(7) . . . . ?
C4 C5 C10 C9 -178.8(7) . . . . ?
C4 C15 C16 C17 -4.8(8) . . . . ?
C4 C15 C16 C26 175.5(6) . . . . ?
C4 C15 C23 C24 -176.4(7) . . . . ?
C4 C18 C19 C20 176.1(6) . . . . ?
C5 C4 C15 C16 -109.3(7) . . . . ?
C5 C4 C15 C23 66.7(9) . . . . ?
C5 C4 C18 C17 108.5(7) . . . . ?
C5 C4 C18 C19 -69.7(9) . . . . ?
C5 C6 C7 C8 1.3(11) . . . . ?
C6 O1 C2 C3 4.9(10) . . . . ?
C6 O1 C2 C11 -173.8(6) . . . . ?
C6 C5 C10 C9 -1.2(11) . . . . ?
C6 C7 C8 C9 -0.4(11) . . . . ?
C7 C8 C9 N27 177.0(7) . . . . ?
C7 C8 C9 C10 -1.3(12) . . . . ?
C8 C9 C10 C5 2.1(11) . . . . ?
C9 N27 C28 C29 -174.7(7) . . . . ?
C9 N27 C28 C36 5.6(13) . . . . ?
C9 N27 C31 C30 174.7(7) . . . . ?
C9 N27 C31 C32 -5.5(13) . . . . ?
C10 C5 C6 O1 178.5(6) . . . . ?
C10 C5 C6 C7 -0.5(11) . . . . ?
C11 C2 C3 C4 178.0(7) . . . . ?
C11 C2 C3 C14 -0.5(11) . . . . ?
C11 C12 C13 N40 -178.6(7) . . . . ?
C11 C12 C13 C14 -0.2(11) . . . . ?
C12 C13 C14 C3 -0.2(11) . . . . ?
C13 N40 C41 C42 -178.5(7) . . . . ?
C13 N40 C41 C49 1.5(13) . . . . ?
C13 N40 C44 C43 178.1(7) . . . . ?
C13 N40 C44 C45 -1.3(13) . . . . ?
C14 C3 C4 C5 173.2(6) . . . . ?
C14 C3 C4 C15 -64.4(9) . . . . ?
C14 C3 C4 C18 48.9(9) . . . . ?
C15 C4 C5 C6 -117.7(8) . . . . ?
C15 C4 C5 C10 59.7(8) . . . . ?
C15 C4 C18 C17 -5.9(7) . . . . ?
C15 C4 C18 C19 175.9(6) . . . . ?
C15 C16 C17 C18 0.8(8) . . . . ?
C15 C16 C17 C22 179.4(7) . . . . ?
C15 C16 C26 C25 1.0(10) . . . . ?
C15 C23 C24 N66 -176.3(8) . . . . ?
C15 C23 C24 C25 2.1(11) . . . . ?
C15 C23 C24 N66A 177.5(11) . . . . ?
C16 C15 C23 C24 -0.8(10) . . . . ?
C16 C17 C18 C4 3.6(8) . . . . ?
C16 C17 C18 C19 -178.1(6) . . . . ?
C16 C17 C22 C21 179.0(7) . . . . ?
C17 C16 C26 C25 -178.6(7) . . . . ?
C17 C18 C19 C20 -1.9(10) . . . . ?
C18 C4 C5 C6 133.4(7) . . . . ?
C18 C4 C5 C10 -49.1(9) . . . . ?
C18 C4 C15 C16 6.4(7) . . . . ?
C18 C4 C15 C23 -177.7(7) . . . . ?
C18 C17 C22 C21 -2.5(10) . . . . ?
C18 C19 C20 N53 179.2(6) . . . . ?
C18 C19 C20 C21 0.3(10) . . . . ?
C19 C20 C21 C22 0.3(11) . . . . ?
C20 N53 C54 C55 169.0(7) . . . . ?
C20 N53 C54 C62 -14.2(12) . . . . ?
C20 N53 C57 C56 -167.1(7) . . . . ?
C20 N53 C57 C58 11.1(13) . . . . ?
C20 C21 C22 C17 0.8(10) . . . . ?
C22 C17 C18 C4 -175.2(6) . . . . ?
C22 C17 C18 C19 3.1(10) . . . . ?
C23 C15 C16 C17 179.0(6) . . . . ?
C23 C15 C16 C26 -0.8(10) . . . . ?
C23 C24 C25 C26 -1.9(12) . . . . ?
C23 C24 N66A C67A 113(3) . . . . ?
C23 C24 N66A C70A -100(3) . . . . ?
C24 N66 C67 C68 175.9(17) . . . . ?
C24 N66 C67 C75 -7(3) . . . . ?
C24 N66 C70 C69 -173.2(16) . . . . ?
C24 N66 C70 C71 10(3) . . . . ?
C24 C25 C26 C16 0.3(11) . . . . ?
C24 N66A C67A C68A 153(2) . . . . ?
C24 N66A C67A C75A -30(5) . . . . ?
C24 N66A C70A C69A -153(3) . . . . ?
C24 N66A C70A C71A 29(6) . . . . ?
C25 C24 N66A C67A -72(3) . . . . ?
C25 C24 N66A C70A 75(3) . . . . ?
C26 C16 C17 C18 -179.5(7) . . . . ?
C26 C16 C17 C22 -0.9(13) . . . . ?
C41 N40 C13 C12 67.9(10) . . . . ?
C41 N40 C13 C14 -110.4(9) . . . . ?
C41 N40 C44 C43 0.9(9) . . . . ?
C41 N40 C44 C45 -178.4(8) . . . . ?
C41 C42 C43 C44 -0.5(9) . . . . ?
C41 C42 C43 C48 176.3(9) . . . . ?
C41 C42 C52 C51 0.3(12) . . . . ?
C41 C49 C50 C51 -0.9(13) . . . . ?
C42 C41 C49 C50 -0.1(12) . . . . ?
C42 C43 C44 N40 -0.3(9) . . . . ?
C42 C43 C44 C45 179.1(7) . . . . ?
C42 C43 C48 C47 -178.5(8) . . . . ?
C43 C42 C52 C51 179.6(9) . . . . ?
C43 C44 C45 C46 -0.6(12) . . . . ?
C44 N40 C13 C12 -108.9(9) . . . . ?
C44 N40 C13 C14 72.8(10) . . . . ?
C44 N40 C41 C42 -1.2(9) . . . . ?
C44 N40 C41 C49 178.9(8) . . . . ?
C44 C43 C48 C47 -2.1(12) . . . . ?
C44 C45 C46 C47 -0.2(13) . . . . ?
C45 C46 C47 C48 -0.1(14) . . . . ?
C46 C47 C48 C43 1.3(13) . . . . ?
C48 C43 C44 N40 -177.6(7) . . . . ?
C48 C43 C44 C45 1.8(12) . . . . ?
C49 C41 C42 C43 -179.0(7) . . . . ?
C49 C41 C42 C52 0.4(12) . . . . ?
C49 C50 C51 C52 1.7(14) . . . . ?
C50 C51 C52 C42 -1.3(13) . . . . ?
C52 C42 C43 C44 -179.8(9) . . . . ?
C52 C42 C43 C48 -3.1(16) . . . . ?
C54 N53 C20 C19 134.3(7) . . . . ?
C54 N53 C20 C21 -46.7(10) . . . . ?
C54 N53 C57 C56 0.8(8) . . . . ?
C54 N53 C57 C58 179.0(8) . . . . ?
C54 C55 C56 C57 2.8(8) . . . . ?
C54 C55 C56 C61 -176.2(8) . . . . ?
C54 C55 C65 C64 2.8(11) . . . . ?
C54 C62 C63 C64 2.1(12) . . . . ?
C55 C54 C62 C63 0.3(11) . . . . ?
C55 C56 C57 N53 -2.2(8) . . . . ?
C55 C56 C57 C58 179.4(7) . . . . ?
C55 C56 C61 C60 179.9(8) . . . . ?
C56 C55 C65 C64 178.4(8) . . . . ?
C56 C57 C58 C59 0.1(12) . . . . ?
C57 N53 C20 C19 -59.9(10) . . . . ?
C57 N53 C20 C21 119.0(8) . . . . ?
C57 N53 C54 C55 1.1(8) . . . . ?
C57 N53 C54 C62 177.9(8) . . . . ?
C57 C56 C61 C60 1.0(12) . . . . ?
C57 C58 C59 C60 1.7(12) . . . . ?
C58 C59 C60 C61 -2.2(13) . . . . ?
C59 C60 C61 C56 0.7(13) . . . . ?
C61 C56 C57 N53 177.0(7) . . . . ?
C61 C56 C57 C58 -1.4(11) . . . . ?
C62 C54 C55 C56 -179.5(7) . . . . ?
C62 C54 C55 C65 -2.7(11) . . . . ?
C62 C63 C64 C65 -2.1(13) . . . . ?
C63 C64 C65 C55 -0.4(12) . . . . ?
C65 C55 C56 C57 -173.2(8) . . . . ?
C65 C55 C56 C61 7.7(15) . . . . ?
N66A C24 C25 C26 -177.3(11) . . . . ?
N66A C67A C68A C69A 1(4) . . . . ?
N66A C67A C68A C78A -178(3) . . . . ?
N66A C67A C75A C76A 179(3) . . . . ?
N66A C70A C71A C72A -178(3) . . . . ?
C67A N66A C70A C69A -3(4) . . . . ?
C67A N66A C70A C71A 179(3) . . . . ?
C67A C68A C69A C70A -2(4) . . . . ?
C67A C68A C69A C74A -168(4) . . . . ?
C67A C68A C78A C77A -1(5) . . . . ?
C67A C75A C76A C77A 0(5) . . . . ?
C68A C67A C75A C76A -5(5) . . . . ?
C68A C69A C70A N66A 3(4) . . . . ?
C68A C69A C70A C71A -179(3) . . . . ?
C68A C69A C74A C73A 178(4) . . . . ?
C69A C68A C78A C77A -179(4) . . . . ?
C69A C70A C71A C72A 4(5) . . . . ?
C70A N66A C67A C68A 1(4) . . . . ?
C70A N66A C67A C75A 178(3) . . . . ?
C70A C69A C74A C73A 14(6) . . . . ?
C70A C71A C72A C73A -1(5) . . . . ?
C71A C72A C73A C74A 6(6) . . . . ?
C72A C73A C74A C69A -12(7) . . . . ?
C74A C69A C70A N66A 171(3) . . . . ?
C74A C69A C70A C71A -11(6) . . . . ?
C75A C67A C68A C69A -176(3) . . . . ?
C75A C67A C68A C78A 5(5) . . . . ?
C75A C76A C77A C78A 5(6) . . . . ?
C76A C77A C78A C68A -4(6) . . . . ?
C78A C68A C69A C70A 176(3) . . . . ?
C78A C68A C69A C74A 10(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-07-30
_olex2_date_sample_submission    2015-07-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id M14col2TOL
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.577(3)
2 0.423(3)

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

data_nr15008
_database_code_depnum_ccdc_archive 'CCDC 1443041'
_audit_update_record             
;
2015-12-17 deposited with the CCDC.
2016-03-01 downloaded from the CCDC.
;
_audit_creation_date             2015-08-27
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_chemical_name_common            SFX-TPTZ
_chemical_name_systematic        
'2, 2?, 7, 7?-Tetrakis (N- phenothiazylo) - spiro (fluorene-9, 9?-xanthene)  '
_chemical_formula_moiety         'C73 H44 N4 O S4, 0.5 C6 H14'
_chemical_formula_sum            'C76 H51 N4 O S4'
_chemical_formula_weight         1164.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C73 H44 N4 O S4'
_chemical_oxdiff_usercomment     '@ 120 K M12o6'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   35.5400(14)
_cell_length_b                   9.8814(2)
_cell_length_c                   36.3474(14)
_cell_angle_alpha                90
_cell_angle_beta                 119.018(5)
_cell_angle_gamma                90
_cell_volume                     11162.3(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12366
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      76.0870
_cell_measurement_theta_min      4.6810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.5430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0794 after correction.
The Ratio of minimum to maximum transmission is 0.5697.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.4098
_exptl_crystal_size_mid          0.0933
_exptl_crystal_size_min          0.0445
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            118201
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.119
_diffrn_reflns_theta_min         3.723
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -116.00  -23.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega -109.00  -78.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686 -144.0000  -95.0000 31

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00   21.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -180.0000 69

#__ type_ start__ end____ width___ exp.time_
  4 omega  -48.00   27.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega   -7.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000   90.0000 36

#__ type_ start__ end____ width___ exp.time_
  6 omega   61.00   95.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000  -60.0000 34

#__ type_ start__ end____ width___ exp.time_
  7 omega   39.00   81.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000   90.0000 42

#__ type_ start__ end____ width___ exp.time_
  8 omega   62.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 47

#__ type_ start__ end____ width___ exp.time_
  9 omega   36.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 29

#__ type_ start__ end____ width___ exp.time_
 10 omega   32.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  -60.0000 56

#__ type_ start__ end____ width___ exp.time_
 11 omega   93.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -90.0000 85

#__ type_ start__ end____ width___ exp.time_
 12 omega   90.00  172.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
 13 omega  116.00  160.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
 14 omega   92.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 15 omega   32.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 74

#__ type_ start__ end____ width___ exp.time_
 16 omega   96.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 17 omega   39.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 18 omega   39.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 40

#__ type_ start__ end____ width___ exp.time_
 19 omega   59.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 20 omega  125.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -150.0000 49

#__ type_ start__ end____ width___ exp.time_
 21 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 55

#__ type_ start__ end____ width___ exp.time_
 22 omega   40.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 23 omega   48.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 24 omega   31.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 50

#__ type_ start__ end____ width___ exp.time_
 25 omega   52.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 54

#__ type_ start__ end____ width___ exp.time_
 26 omega   66.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000   30.0000 73

#__ type_ start__ end____ width___ exp.time_
 27 omega   64.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 43

#__ type_ start__ end____ width___ exp.time_
 28 omega  111.00  154.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  -60.0000 43

#__ type_ start__ end____ width___ exp.time_
 29 omega   31.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
 30 omega   98.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   60.0000 44

#__ type_ start__ end____ width___ exp.time_
 31 omega   68.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 40

#__ type_ start__ end____ width___ exp.time_
 32 omega   39.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 44

#__ type_ start__ end____ width___ exp.time_
 33 omega   75.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   31.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0310468000
_diffrn_orient_matrix_UB_12      0.0163687000
_diffrn_orient_matrix_UB_13      -0.0180068000
_diffrn_orient_matrix_UB_21      0.0385753000
_diffrn_orient_matrix_UB_22      -0.0035569000
_diffrn_orient_matrix_UB_23      0.0449163000
_diffrn_orient_matrix_UB_31      0.0023946000
_diffrn_orient_matrix_UB_32      -0.1549819000
_diffrn_orient_matrix_UB_33      -0.0029248000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9915
_reflns_number_total             11573
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.617
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         11573
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0698
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0988P)²+16.3516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.1953
_refine_special_details          
;
The diffraction pattern was twinned.  This was handled in SHELXL using twin law [-1 0 0 / 0 -1 0 / 1 0 1] and refined twin scale factor 

0.2623(12).  S58 to C64 was modelled as disordered over two sites with displacement ellipsoid and geometric similarity restraints.  The 

SQUEEZE routine of PLATON was used to handle disordered solvent.  This corresponds to half a hexane molecule per asymmetric unit, which 

could not be modelled with discrete atoms.  The peaks corresponding to this molecule appear around a crystallographic symmetry element, 

modelling was not straightfoward and a better refinement was achieved with the use of SQUEEZE.  This missing solvent was included in the 

chemical formula; checkCIF alerts are thus triggered, and should be ignored.




#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
097_ALERT_2_B Large Reported Max.  (Positive) Residual Density       1.62 eA-3

Squeeze was used, but this peak was too close to an existing atom to be masked
by squeeze.  

#===============================================================================
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.09 Report
220_ALERT_2_C Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        3.3 Ratio
230_ALERT_2_C Hirshfeld Test Diff for    C53    --  C54     ..        6.7 su
230_ALERT_2_C Hirshfeld Test Diff for    C67    --  C68     ..        5.3 su
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         S1 Check
340_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0066 Ang.

Some disorder, which was modelled.  

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         14 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         14 Report
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.0514 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check

Consequence of squeeze

083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large.      16.34 Why ?
175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          1 Report
301_ALERT_3_G Main Residue  Disorder ............ Percentage =          9 Note
605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of .        105 A**3
793_ALERT_4_G The Model has Chirality at C22     (Centro SPGR)          S Verify
795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence ..        C59 Note
797_ALERT_4_G N-Atom in CIF Coordinate List out of Sequence ..        N41 Note
802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          ! Info
860_ALERT_3_G Number of Least-Squares Restraints .............        105 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed ..          ! Info
910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          3 Report
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        100 Note
#===============================================================================



;


_vrf_DIFMX01_nr15008             
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: Please see the _refine_special_details section of the CIF
;



_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.7376(12) 0.2624(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 S58A, C59A, C60A, C61A, C62A, C63A, C64A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S58, C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{S58, C59, C60, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.02
as
{S58A, C59A, C60A, C61A, C62A, C63A, C64A}
5. Others
 Sof(S58A)=Sof(C59A)=Sof(C60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=
 Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=1-FVAR(1)
 Sof(S58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=
 Sof(H63)=Sof(C64)=Sof(H64)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C61(H61), C62(H62), C63(H63), C64(H64), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C24(H24), C25(H25),
  C26(H26), C28(H28), C33(H33), C35(H35), C36(H36), C37(H37), C39(H39),
 C40(H40), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
  C54(H54), C65(H65), C66(H66), C67(H67), C68(H68), C75(H75), C76(H76),
 C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C61A(H61A),
 C62A(H62A), C63A(H63A), C64A(H64A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.08098(4) 0.78766(18) 0.22359(4) 0.0724(4) Uani 1 1 d . . . . .
S44 S 0.55919(4) 0.78801(13) 0.58319(4) 0.0614(3) Uani 1 1 d . . . . .
S58 S 0.41747(16) 0.6892(9) 0.23409(17) 0.0599(13) Uani 0.513(14) 1 d D U P A 1
C59 C 0.4420(3) 0.6439(14) 0.2872(3) 0.047(2) Uani 0.513(14) 1 d D U P A 1
C60 C 0.4218(4) 0.6782(18) 0.3110(4) 0.038(3) Uani 0.513(14) 1 d D U P A 1
C61 C 0.4429(4) 0.6492(14) 0.3543(4) 0.045(3) Uani 0.513(14) 1 d D U P A 1
H61 H 0.4291 0.6684 0.3705 0.054 Uiso 0.513(14) 1 calc R . P A 1
C62 C 0.4835(3) 0.5930(12) 0.3734(3) 0.057(3) Uani 0.513(14) 1 d D U P A 1
H62 H 0.4981 0.5783 0.4029 0.069 Uiso 0.513(14) 1 calc R . P A 1
C63 C 0.5032(3) 0.5576(15) 0.3500(3) 0.072(4) Uani 0.513(14) 1 d D U P A 1
H63 H 0.5302 0.5124 0.3630 0.087 Uiso 0.513(14) 1 calc R . P A 1
C64 C 0.4836(3) 0.5884(16) 0.3074(3) 0.070(4) Uani 0.513(14) 1 d D U P A 1
H64 H 0.4983 0.5720 0.2919 0.084 Uiso 0.513(14) 1 calc R . P A 1
S72 S 0.27386(4) 0.91974(12) 0.55879(4) 0.0535(3) Uani 1 1 d . . . . .
O19 O 0.31900(9) 0.4443(2) 0.40536(9) 0.0376(5) Uani 1 1 d . . . . .
N4 N 0.17012(10) 0.7086(3) 0.28857(10) 0.0382(6) Uani 1 1 d . . . . .
N41 N 0.47238(10) 0.6982(3) 0.51708(10) 0.0393(7) Uani 1 1 d . . . . .
N55 N 0.37902(10) 0.7331(3) 0.28861(10) 0.0349(6) Uani 1 1 d . . . . .
N69 N 0.29303(11) 1.0218(3) 0.49251(10) 0.0366(6) Uani 1 1 d . . . . .
C2 C 0.12788(15) 0.8099(4) 0.21906(13) 0.0496(10) Uani 1 1 d . . . . .
C3 C 0.16730(14) 0.7644(3) 0.25118(12) 0.0400(8) Uani 1 1 d . . . . .
C5 C 0.14518(13) 0.7644(4) 0.30561(13) 0.0440(8) Uani 1 1 d . . . . .
C6 C 0.10347(16) 0.8095(6) 0.27839(18) 0.0633(13) Uani 1 1 d . . . . .
C7 C 0.0788(2) 0.8676(8) 0.2945(2) 0.0838(19) Uani 1 1 d . . . . .
H7 H 0.0510 0.9021 0.2759 0.101 Uiso 1 1 calc R . . . .
C8 C 0.0948(2) 0.8758(8) 0.3381(2) 0.089(2) Uani 1 1 d . . . . .
H8 H 0.0776 0.9138 0.3490 0.107 Uiso 1 1 calc R . . . .
C9 C 0.13563(19) 0.8281(6) 0.36511(18) 0.0648(13) Uani 1 1 d . . . . .
H9 H 0.1464 0.8313 0.3947 0.078 Uiso 1 1 calc R . . . .
C10 C 0.16100(15) 0.7754(4) 0.34904(14) 0.0470(9) Uani 1 1 d . . . . .
H10 H 0.1895 0.7465 0.3678 0.056 Uiso 1 1 calc R . . . .
C11 C 0.12411(19) 0.8637(4) 0.18236(14) 0.0587(13) Uani 1 1 d . . . . .
H11 H 0.0970 0.8966 0.1613 0.070 Uiso 1 1 calc R . . . .
C12 C 0.1587(2) 0.8699(4) 0.17600(14) 0.0594(13) Uani 1 1 d . . . . .
H12 H 0.1557 0.9042 0.1503 0.071 Uiso 1 1 calc R . . . .
C13 C 0.19810(18) 0.8262(4) 0.20700(14) 0.0521(11) Uani 1 1 d . . . . .
H13 H 0.2224 0.8314 0.2028 0.063 Uiso 1 1 calc R . . . .
C14 C 0.20260(15) 0.7740(4) 0.24465(13) 0.0444(9) Uani 1 1 d . . . . .
H14 H 0.2301 0.7449 0.2660 0.053 Uiso 1 1 calc R . . . .
C15 C 0.20925(12) 0.6429(3) 0.31786(11) 0.0338(7) Uani 1 1 d . . . . .
C16 C 0.20941(12) 0.5040(3) 0.32319(12) 0.0349(7) Uani 1 1 d . . . . .
H16 H 0.1842 0.4525 0.3066 0.042 Uiso 1 1 calc R . . . .
C17 C 0.24666(13) 0.4403(3) 0.35298(12) 0.0370(8) Uani 1 1 d . . . . .
H17 H 0.2470 0.3452 0.3571 0.044 Uiso 1 1 calc R . . . .
C18 C 0.28341(12) 0.5167(3) 0.37676(11) 0.0320(7) Uani 1 1 d . . . . .
C20 C 0.35601(11) 0.5139(3) 0.43132(11) 0.0322(7) Uani 1 1 d . . . . .
C21 C 0.36031(11) 0.6524(3) 0.42890(11) 0.0303(6) Uani 1 1 d . . . . .
C22 C 0.32501(11) 0.7393(3) 0.39541(11) 0.0297(6) Uani 1 1 d . . . . .
C23 C 0.28416(11) 0.6559(3) 0.37153(11) 0.0299(6) Uani 1 1 d . . . . .
C24 C 0.24626(11) 0.7170(3) 0.34199(11) 0.0326(7) Uani 1 1 d . . . . .
H24 H 0.2457 0.8122 0.3382 0.039 Uiso 1 1 calc R . . . .
C25 C 0.38960(13) 0.4350(3) 0.46088(13) 0.0384(8) Uani 1 1 d . . . . .
H25 H 0.3859 0.3402 0.4620 0.046 Uiso 1 1 calc R . . . .
C26 C 0.42819(13) 0.4945(4) 0.48845(13) 0.0399(8) Uani 1 1 d . . . . .
H26 H 0.4514 0.4409 0.5083 0.048 Uiso 1 1 calc R . . . .
C27 C 0.43289(12) 0.6340(4) 0.48699(12) 0.0359(7) Uani 1 1 d . . . . .
C28 C 0.39891(11) 0.7109(3) 0.45788(11) 0.0320(7) Uani 1 1 d . . . . .
H28 H 0.4021 0.8063 0.4577 0.038 Uiso 1 1 calc R . . . .
C29 C 0.31767(10) 0.8692(3) 0.41380(10) 0.0267(6) Uani 1 1 d . . . . .
C30 C 0.32557(10) 0.9833(3) 0.39574(10) 0.0277(6) Uani 1 1 d . . . . .
C31 C 0.33905(11) 0.9377(3) 0.36529(10) 0.0285(6) Uani 1 1 d . . . . .
C32 C 0.33906(10) 0.7970(3) 0.36495(10) 0.0286(6) Uani 1 1 d . . . . .
C33 C 0.35164(12) 0.7270(3) 0.33952(11) 0.0320(7) Uani 1 1 d . . . . .
H33 H 0.3516 0.6308 0.3392 0.038 Uiso 1 1 calc R . . . .
C34 C 0.36430(11) 0.7991(3) 0.31461(11) 0.0317(7) Uani 1 1 d . . . . .
C35 C 0.36346(12) 0.9401(3) 0.31445(11) 0.0331(7) Uani 1 1 d . . . . .
H35 H 0.3716 0.9886 0.2969 0.040 Uiso 1 1 calc R . . . .
C36 C 0.35080(12) 1.0104(3) 0.33973(11) 0.0316(7) Uani 1 1 d . . . . .
H36 H 0.3502 1.1066 0.3395 0.038 Uiso 1 1 calc R . . . .
C37 C 0.30671(11) 0.8821(3) 0.44547(11) 0.0293(6) Uani 1 1 d . . . . .
H37 H 0.3014 0.8044 0.4577 0.035 Uiso 1 1 calc R . . . .
C38 C 0.30366(11) 1.0119(3) 0.45900(11) 0.0315(7) Uani 1 1 d . . . . .
C39 C 0.31047(12) 1.1265(3) 0.44037(11) 0.0323(7) Uani 1 1 d . . . . .
H39 H 0.3075 1.2142 0.4494 0.039 Uiso 1 1 calc R . . . .
C40 C 0.32161(11) 1.1126(3) 0.40869(11) 0.0306(6) Uani 1 1 d . . . . .
H40 H 0.3264 1.1902 0.3961 0.037 Uiso 1 1 calc R . . . .
C42 C 0.49634(12) 0.7694(3) 0.50136(13) 0.0391(8) Uani 1 1 d . . . . .
C43 C 0.53612(13) 0.8250(4) 0.52927(14) 0.0465(9) Uani 1 1 d . . . . .
C45 C 0.51161(17) 0.7936(5) 0.58748(14) 0.0558(11) Uani 1 1 d . . . . .
C46 C 0.47328(16) 0.7441(4) 0.55420(13) 0.0482(10) Uani 1 1 d . . . . .
C47 C 0.43669(19) 0.7451(5) 0.55901(16) 0.0584(12) Uani 1 1 d . . . . .
H47 H 0.4103 0.7104 0.5372 0.070 Uiso 1 1 calc R . . . .
C48 C 0.4385(3) 0.7961(6) 0.59523(19) 0.0774(17) Uani 1 1 d . . . . .
H48 H 0.4133 0.7967 0.5981 0.093 Uiso 1 1 calc R . . . .
C49 C 0.4768(3) 0.8465(7) 0.62742(18) 0.083(2) Uani 1 1 d . . . . .
H49 H 0.4779 0.8817 0.6522 0.100 Uiso 1 1 calc R . . . .
C50 C 0.5131(2) 0.8452(6) 0.62318(16) 0.0710(16) Uani 1 1 d . . . . .
H50 H 0.5394 0.8801 0.6450 0.085 Uiso 1 1 calc R . . . .
C51 C 0.48239(13) 0.7846(4) 0.45828(13) 0.0423(8) Uani 1 1 d . . . . .
H51 H 0.4562 0.7434 0.4384 0.051 Uiso 1 1 calc R . . . .
C52 C 0.50608(15) 0.8587(4) 0.44420(16) 0.0491(9) Uani 1 1 d . . . . .
H52 H 0.4960 0.8674 0.4149 0.059 Uiso 1 1 calc R . . . .
C53 C 0.54388(15) 0.9193(4) 0.47216(18) 0.0528(11) Uani 1 1 d . . . . .
H53 H 0.5594 0.9731 0.4624 0.063 Uiso 1 1 calc R . . . .
C54 C 0.55899(14) 0.9014(4) 0.51437(18) 0.0555(12) Uani 1 1 d . . . . .
H54 H 0.5855 0.9416 0.5339 0.067 Uiso 1 1 calc R . . . .
C56 C 0.34841(12) 0.6821(3) 0.24874(12) 0.0347(7) Uani 1 1 d . . . . .
C57 C 0.36025(16) 0.6624(5) 0.21791(14) 0.0512(10) Uani 1 1 d . . . . .
C65 C 0.30666(13) 0.6499(4) 0.23898(12) 0.0378(7) Uani 1 1 d . . . . .
H65 H 0.2977 0.6626 0.2594 0.045 Uiso 1 1 calc R . . . .
C66 C 0.27775(14) 0.5990(4) 0.19948(13) 0.0410(8) Uani 1 1 d . . . . .
H66 H 0.2491 0.5782 0.1931 0.049 Uiso 1 1 calc R . . . .
C67 C 0.29034(14) 0.5785(4) 0.16950(12) 0.0406(8) Uani 1 1 d . . . . .
H67 H 0.2706 0.5434 0.1426 0.049 Uiso 1 1 calc R . . . .
C68 C 0.33154(18) 0.6094(5) 0.17904(15) 0.0570(11) Uani 1 1 d . . . . .
H68 H 0.3406 0.5944 0.1587 0.068 Uiso 1 1 calc R . . . .
C70 C 0.24950(13) 1.0372(3) 0.48206(12) 0.0375(8) Uani 1 1 d . . . . .
C71 C 0.23668(14) 0.9962(4) 0.51132(13) 0.0422(8) Uani 1 1 d . . . . .
C73 C 0.31997(15) 1.0141(4) 0.56814(13) 0.0450(9) Uani 1 1 d . . . . .
C74 C 0.32627(13) 1.0474(4) 0.53404(12) 0.0388(8) Uani 1 1 d . . . . .
C75 C 0.36563(14) 1.1054(4) 0.54303(13) 0.0447(9) Uani 1 1 d . . . . .
H75 H 0.3710 1.1279 0.5206 0.054 Uiso 1 1 calc R . . . .
C76 C 0.39697(16) 1.1307(5) 0.58398(14) 0.0520(10) Uani 1 1 d . . . . .
H76 H 0.4237 1.1689 0.5893 0.062 Uiso 1 1 calc R . . . .
C77 C 0.38975(17) 1.1008(5) 0.61738(14) 0.0552(11) Uani 1 1 d . . . . .
H77 H 0.4111 1.1196 0.6455 0.066 Uiso 1 1 calc R . . . .
C78 C 0.35082(18) 1.0431(5) 0.60908(14) 0.0552(11) Uani 1 1 d . . . . .
H78 H 0.3453 1.0234 0.6316 0.066 Uiso 1 1 calc R . . . .
C79 C 0.21887(14) 1.0914(4) 0.44411(13) 0.0439(8) Uani 1 1 d . . . . .
H79 H 0.2272 1.1215 0.4243 0.053 Uiso 1 1 calc R . . . .
C80 C 0.17660(16) 1.1023(5) 0.43474(15) 0.0534(10) Uani 1 1 d . . . . .
H80 H 0.1559 1.1386 0.4084 0.064 Uiso 1 1 calc R . . . .
C81 C 0.16384(16) 1.0602(5) 0.46376(17) 0.0551(11) Uani 1 1 d . . . . .
H81 H 0.1345 1.0665 0.4571 0.066 Uiso 1 1 calc R . . . .
C82 C 0.19393(16) 1.0098(5) 0.50188(16) 0.0524(10) Uani 1 1 d . . . . .
H82 H 0.1856 0.9838 0.5221 0.063 Uiso 1 1 calc R . . . .
S58A S 0.40632(17) 0.7444(6) 0.22228(17) 0.0467(11) Uani 0.487(14) 1 d D U P A
2
C59A C 0.4388(3) 0.6996(11) 0.2751(3) 0.043(2) Uani 0.487(14) 1 d D U P A 2
C60A C 0.4223(4) 0.700(2) 0.3029(4) 0.044(3) Uani 0.487(14) 1 d D U P A 2
C61A C 0.4488(3) 0.6701(15) 0.3457(4) 0.041(3) Uani 0.487(14) 1 d D U P A 2
H61A H 0.4375 0.6736 0.3646 0.049 Uiso 0.487(14) 1 calc R . P A 2
C62A C 0.4920(3) 0.6354(12) 0.3605(4) 0.053(3) Uani 0.487(14) 1 d D U P A 2
H62A H 0.5100 0.6124 0.3893 0.063 Uiso 0.487(14) 1 calc R . P A 2
C63A C 0.5082(3) 0.6350(11) 0.3326(3) 0.053(3) Uani 0.487(14) 1 d D U P A 2
H63A H 0.5377 0.6152 0.3427 0.064 Uiso 0.487(14) 1 calc R . P A 2
C64A C 0.4822(3) 0.6629(12) 0.2904(3) 0.052(3) Uani 0.487(14) 1 d D U P A 2
H64A H 0.4936 0.6574 0.2716 0.063 Uiso 0.487(14) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C2 1.767(5) . ?
S1 C6 1.763(6) . ?
S44 C43 1.757(5) . ?
S44 C45 1.773(6) . ?
S58 C59 1.748(10) . ?
S58 C57 1.841(6) . ?
C59 C60 1.404(10) . ?
C59 C64 1.406(12) . ?
C60 C61 1.407(12) . ?
C60 N55 1.438(10) . ?
C61 H61 0.9500 . ?
C61 C62 1.379(12) . ?
C62 H62 0.9500 . ?
C62 C63 1.384(14) . ?
C63 H63 0.9500 . ?
C63 C64 1.387(14) . ?
C64 H64 0.9500 . ?
S72 C71 1.755(4) . ?
S72 C73 1.769(5) . ?
O19 C18 1.385(4) . ?
O19 C20 1.374(5) . ?
N4 C3 1.425(5) . ?
N4 C5 1.416(5) . ?
N4 C15 1.433(5) . ?
N41 C27 1.442(5) . ?
N41 C42 1.421(5) . ?
N41 C46 1.409(5) . ?
N55 C34 1.439(4) . ?
N55 C56 1.417(5) . ?
N55 C60A 1.403(11) . ?
N69 C38 1.443(5) . ?
N69 C70 1.411(5) . ?
N69 C74 1.417(5) . ?
C2 C3 1.393(6) . ?
C2 C11 1.380(7) . ?
C3 C14 1.389(6) . ?
C5 C6 1.397(6) . ?
C5 C10 1.400(6) . ?
C6 C7 1.392(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.402(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(7) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.358(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.397(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(5) . ?
C15 C24 1.384(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.390(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(5) . ?
C18 C23 1.390(4) . ?
C20 C21 1.385(4) . ?
C20 C25 1.394(5) . ?
C21 C22 1.521(5) . ?
C21 C28 1.387(5) . ?
C22 C23 1.523(5) . ?
C22 C29 1.527(4) . ?
C22 C32 1.529(4) . ?
C23 C24 1.389(5) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.377(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.392(5) . ?
C27 C28 1.384(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.400(4) . ?
C29 C37 1.388(5) . ?
C30 C31 1.474(4) . ?
C30 C40 1.392(4) . ?
C31 C32 1.390(4) . ?
C31 C36 1.390(5) . ?
C32 C33 1.391(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.388(5) . ?
C34 C35 1.393(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.390(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.397(5) . ?
C38 C39 1.399(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.394(5) . ?
C40 H40 0.9500 . ?
C42 C43 1.393(6) . ?
C42 C51 1.403(6) . ?
C43 C54 1.396(7) . ?
C45 C46 1.400(7) . ?
C45 C50 1.370(7) . ?
C46 C47 1.394(7) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(7) . ?
C48 H48 0.9500 . ?
C48 C49 1.388(11) . ?
C49 H49 0.9500 . ?
C49 C50 1.373(11) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C51 C52 1.387(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.368(7) . ?
C53 H53 0.9500 . ?
C53 C54 1.369(8) . ?
C54 H54 0.9500 . ?
C56 C57 1.389(5) . ?
C56 C65 1.385(6) . ?
C57 C68 1.383(6) . ?
C57 S58A 1.763(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.392(6) . ?
C66 H66 0.9500 . ?
C66 C67 1.379(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.365(7) . ?
C68 H68 0.9500 . ?
C70 C71 1.405(5) . ?
C70 C79 1.385(6) . ?
C71 C82 1.392(7) . ?
C73 C74 1.402(6) . ?
C73 C78 1.384(6) . ?
C74 C75 1.396(6) . ?
C75 H75 0.9500 . ?
C75 C76 1.382(6) . ?
C76 H76 0.9500 . ?
C76 C77 1.389(7) . ?
C77 H77 0.9500 . ?
C77 C78 1.388(8) . ?
C78 H78 0.9500 . ?
C79 H79 0.9500 . ?
C79 C80 1.374(6) . ?
C80 H80 0.9500 . ?
C80 C81 1.398(7) . ?
C81 H81 0.9500 . ?
C81 C82 1.369(8) . ?
C82 H82 0.9500 . ?
S58A C59A 1.751(10) . ?
C59A C60A 1.393(12) . ?
C59A C64A 1.407(11) . ?
C60A C61A 1.405(12) . ?
C61A H61A 0.9500 . ?
C61A C62A 1.400(11) . ?
C62A H62A 0.9500 . ?
C62A C63A 1.388(15) . ?
C63A H63A 0.9500 . ?
C63A C64A 1.382(14) . ?
C64A H64A 0.9500 . ?

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
C6 S1 C2 99.1(2) . . ?
C43 S44 C45 98.2(2) . . ?
C59 S58 C57 101.4(4) . . ?
C60 C59 S58 119.2(7) . . ?
C60 C59 C64 119.7(9) . . ?
C64 C59 S58 120.7(7) . . ?
C59 C60 C61 119.1(8) . . ?
C59 C60 N55 117.3(8) . . ?
C61 C60 N55 123.5(8) . . ?
C60 C61 H61 119.9 . . ?
C62 C61 C60 120.2(10) . . ?
C62 C61 H61 119.9 . . ?
C61 C62 H62 119.6 . . ?
C61 C62 C63 120.8(10) . . ?
C63 C62 H62 119.6 . . ?
C62 C63 H63 120.0 . . ?
C62 C63 C64 120.0(8) . . ?
C64 C63 H63 120.0 . . ?
C59 C64 H64 120.0 . . ?
C63 C64 C59 120.0(8) . . ?
C63 C64 H64 120.0 . . ?
C71 S72 C73 98.5(2) . . ?
C20 O19 C18 118.6(2) . . ?
C3 N4 C15 118.6(3) . . ?
C5 N4 C3 119.8(3) . . ?
C5 N4 C15 116.1(3) . . ?
C42 N41 C27 117.7(3) . . ?
C46 N41 C27 115.5(3) . . ?
C46 N41 C42 119.1(3) . . ?
C60 N55 C34 114.9(5) . . ?
C56 N55 C60 121.4(6) . . ?
C56 N55 C34 119.3(3) . . ?
C60A N55 C34 123.1(6) . . ?
C60A N55 C56 117.1(7) . . ?
C70 N69 C38 118.8(3) . . ?
C70 N69 C74 120.4(3) . . ?
C74 N69 C38 119.1(3) . . ?
C3 C2 S1 119.5(4) . . ?
C11 C2 S1 119.0(4) . . ?
C11 C2 C3 121.4(5) . . ?
C2 C3 N4 120.1(4) . . ?
C14 C3 N4 122.6(4) . . ?
C14 C3 C2 117.4(4) . . ?
C6 C5 N4 119.3(4) . . ?
C6 C5 C10 118.8(4) . . ?
C10 C5 N4 122.0(4) . . ?
C5 C6 S1 120.3(4) . . ?
C7 C6 S1 119.6(4) . . ?
C7 C6 C5 120.1(5) . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.5(6) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.5(5) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0(5) . . ?
C10 C9 H9 120.0 . . ?
C5 C10 H10 119.5 . . ?
C9 C10 C5 121.0(4) . . ?
C9 C10 H10 119.5 . . ?
C2 C11 H11 119.7 . . ?
C12 C11 C2 120.7(5) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.4(5) . . ?
C14 C13 H13 119.8 . . ?
C3 C14 C13 120.6(4) . . ?
C3 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 N4 119.3(3) . . ?
C24 C15 N4 120.8(3) . . ?
C24 C15 C16 119.8(3) . . ?
C15 C16 H16 120.2 . . ?
C15 C16 C17 119.7(3) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 120.3 . . ?
C18 C17 C16 119.5(3) . . ?
C18 C17 H17 120.3 . . ?
O19 C18 C17 115.3(3) . . ?
O19 C18 C23 122.9(3) . . ?
C17 C18 C23 121.8(3) . . ?
O19 C20 C21 123.3(3) . . ?
O19 C20 C25 115.2(3) . . ?
C21 C20 C25 121.5(3) . . ?
C20 C21 C22 122.4(3) . . ?
C20 C21 C28 117.6(3) . . ?
C28 C21 C22 120.0(3) . . ?
C21 C22 C23 109.8(3) . . ?
C21 C22 C29 112.0(3) . . ?
C21 C22 C32 111.0(3) . . ?
C23 C22 C29 112.8(3) . . ?
C23 C22 C32 110.2(3) . . ?
C29 C22 C32 100.9(2) . . ?
C18 C23 C22 122.3(3) . . ?
C24 C23 C18 117.4(3) . . ?
C24 C23 C22 120.3(3) . . ?
C15 C24 C23 121.8(3) . . ?
C15 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C20 C25 H25 120.0 . . ?
C26 C25 C20 120.0(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.3 . . ?
C25 C26 C27 119.4(3) . . ?
C27 C26 H26 120.3 . . ?
C26 C27 N41 119.8(3) . . ?
C28 C27 N41 120.3(3) . . ?
C28 C27 C26 119.8(4) . . ?
C21 C28 H28 119.1 . . ?
C27 C28 C21 121.7(3) . . ?
C27 C28 H28 119.1 . . ?
C30 C29 C22 110.9(3) . . ?
C37 C29 C22 128.1(3) . . ?
C37 C29 C30 121.0(3) . . ?
C29 C30 C31 108.5(3) . . ?
C40 C30 C29 120.3(3) . . ?
C40 C30 C31 131.1(3) . . ?
C32 C31 C30 108.3(3) . . ?
C36 C31 C30 131.0(3) . . ?
C36 C31 C32 120.7(3) . . ?
C31 C32 C22 111.4(3) . . ?
C31 C32 C33 120.3(3) . . ?
C33 C32 C22 128.2(3) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 C32 119.2(3) . . ?
C34 C33 H33 120.4 . . ?
C33 C34 N55 122.1(3) . . ?
C33 C34 C35 120.2(3) . . ?
C35 C34 N55 117.7(3) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.7(3) . . ?
C36 C35 H35 119.6 . . ?
C31 C36 C35 118.8(3) . . ?
C31 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
C29 C37 H37 120.7 . . ?
C29 C37 C38 118.5(3) . . ?
C38 C37 H37 120.7 . . ?
C37 C38 N69 117.1(3) . . ?
C37 C38 C39 120.8(3) . . ?
C39 C38 N69 122.1(3) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.3(3) . . ?
C40 C39 H39 119.8 . . ?
C30 C40 C39 119.1(3) . . ?
C30 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C43 C42 N41 119.8(4) . . ?
C43 C42 C51 117.1(4) . . ?
C51 C42 N41 123.1(3) . . ?
C42 C43 S44 119.3(3) . . ?
C42 C43 C54 120.5(4) . . ?
C54 C43 S44 120.0(3) . . ?
C46 C45 S44 118.9(4) . . ?
C50 C45 S44 119.6(5) . . ?
C50 C45 C46 121.5(6) . . ?
C45 C46 N41 120.0(4) . . ?
C47 C46 N41 122.2(4) . . ?
C47 C46 C45 117.7(4) . . ?
C46 C47 H47 119.8 . . ?
C48 C47 C46 120.5(6) . . ?
C48 C47 H47 119.8 . . ?
C47 C48 H48 119.8 . . ?
C47 C48 C49 120.5(6) . . ?
C49 C48 H48 119.8 . . ?
C48 C49 H49 120.2 . . ?
C50 C49 C48 119.6(5) . . ?
C50 C49 H49 120.2 . . ?
C45 C50 C49 120.1(6) . . ?
C45 C50 H50 119.9 . . ?
C49 C50 H50 119.9 . . ?
C42 C51 H51 119.4 . . ?
C52 C51 C42 121.3(4) . . ?
C52 C51 H51 119.4 . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.7(5) . . ?
C53 C52 H52 119.7 . . ?
C52 C53 H53 120.5 . . ?
C52 C53 C54 119.1(4) . . ?
C54 C53 H53 120.5 . . ?
C43 C54 H54 119.4 . . ?
C53 C54 C43 121.3(4) . . ?
C53 C54 H54 119.4 . . ?
C57 C56 N55 119.5(4) . . ?
C65 C56 N55 122.6(3) . . ?
C65 C56 C57 117.9(4) . . ?
C56 C57 S58 116.2(3) . . ?
C56 C57 S58A 119.6(3) . . ?
C68 C57 S58 122.3(4) . . ?
C68 C57 C56 121.0(4) . . ?
C68 C57 S58A 117.3(4) . . ?
C56 C65 H65 119.7 . . ?
C56 C65 C66 120.7(4) . . ?
C66 C65 H65 119.7 . . ?
C65 C66 H66 119.7 . . ?
C67 C66 C65 120.5(4) . . ?
C67 C66 H66 119.7 . . ?
C66 C67 H67 120.5 . . ?
C68 C67 C66 119.1(4) . . ?
C68 C67 H67 120.5 . . ?
C57 C68 H68 119.6 . . ?
C67 C68 C57 120.9(4) . . ?
C67 C68 H68 119.6 . . ?
C71 C70 N69 118.8(4) . . ?
C79 C70 N69 122.6(3) . . ?
C79 C70 C71 118.6(4) . . ?
C70 C71 S72 120.2(3) . . ?
C82 C71 S72 119.7(3) . . ?
C82 C71 C70 120.1(4) . . ?
C74 C73 S72 119.0(3) . . ?
C78 C73 S72 119.5(3) . . ?
C78 C73 C74 121.3(4) . . ?
C73 C74 N69 119.4(4) . . ?
C75 C74 N69 123.1(3) . . ?
C75 C74 C73 117.5(4) . . ?
C74 C75 H75 119.4 . . ?
C76 C75 C74 121.3(4) . . ?
C76 C75 H75 119.4 . . ?
C75 C76 H76 119.7 . . ?
C75 C76 C77 120.6(4) . . ?
C77 C76 H76 119.7 . . ?
C76 C77 H77 120.5 . . ?
C78 C77 C76 119.0(4) . . ?
C78 C77 H77 120.5 . . ?
C73 C78 C77 120.3(4) . . ?
C73 C78 H78 119.8 . . ?
C77 C78 H78 119.8 . . ?
C70 C79 H79 119.6 . . ?
C80 C79 C70 120.9(4) . . ?
C80 C79 H79 119.6 . . ?
C79 C80 H80 119.8 . . ?
C79 C80 C81 120.4(5) . . ?
C81 C80 H80 119.8 . . ?
C80 C81 H81 120.3 . . ?
C82 C81 C80 119.4(4) . . ?
C82 C81 H81 120.3 . . ?
C71 C82 H82 119.7 . . ?
C81 C82 C71 120.5(4) . . ?
C81 C82 H82 119.7 . . ?
C59A S58A C57 94.2(4) . . ?
C60A C59A S58A 120.6(7) . . ?
C60A C59A C64A 118.7(9) . . ?
C64A C59A S58A 120.8(7) . . ?
N55 C60A C61A 119.0(8) . . ?
C59A C60A N55 120.3(9) . . ?
C59A C60A C61A 120.7(9) . . ?
C60A C61A H61A 120.0 . . ?
C62A C61A C60A 119.9(10) . . ?
C62A C61A H61A 120.0 . . ?
C61A C62A H62A 120.5 . . ?
C63A C62A C61A 119.0(9) . . ?
C63A C62A H62A 120.5 . . ?
C62A C63A H63A 119.3 . . ?
C64A C63A C62A 121.3(8) . . ?
C64A C63A H63A 119.3 . . ?
C59A C64A H64A 119.8 . . ?
C63A C64A C59A 120.3(8) . . ?
C63A C64A H64A 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C2 C3 N4 -4.2(5) . . . . ?
S1 C2 C3 C14 174.8(3) . . . . ?
S1 C2 C11 C12 -173.4(3) . . . . ?
S1 C6 C7 C8 174.7(6) . . . . ?
S44 C43 C54 C53 172.8(3) . . . . ?
S44 C45 C46 N41 -3.7(5) . . . . ?
S44 C45 C46 C47 177.7(3) . . . . ?
S44 C45 C50 C49 -178.1(4) . . . . ?
S58 C59 C60 C61 -176.1(11) . . . . ?
S58 C59 C60 N55 8.2(19) . . . . ?
S58 C59 C64 C63 177.6(11) . . . . ?
S58 C57 C68 C67 173.6(5) . . . . ?
C59 S58 C57 C56 30.3(6) . . . . ?
C59 S58 C57 C68 -141.8(5) . . . . ?
C59 C60 C61 C62 3(2) . . . . ?
C59 C60 N55 C34 -164.3(11) . . . . ?
C59 C60 N55 C56 39.4(17) . . . . ?
C60 C59 C64 C63 5(2) . . . . ?
C60 C61 C62 C63 -3(2) . . . . ?
C60 N55 C34 C33 -75.1(9) . . . . ?
C60 N55 C34 C35 104.3(9) . . . . ?
C60 N55 C56 C57 -47.2(9) . . . . ?
C60 N55 C56 C65 132.5(8) . . . . ?
C61 C60 N55 C34 20.2(18) . . . . ?
C61 C60 N55 C56 -136.1(12) . . . . ?
C61 C62 C63 C64 5(2) . . . . ?
C62 C63 C64 C59 -6(2) . . . . ?
C64 C59 C60 C61 -4(2) . . . . ?
C64 C59 C60 N55 -179.3(12) . . . . ?
S72 C71 C82 C81 -175.3(4) . . . . ?
S72 C73 C74 N69 8.7(5) . . . . ?
S72 C73 C74 C75 -171.4(3) . . . . ?
S72 C73 C78 C77 171.4(4) . . . . ?
O19 C18 C23 C22 3.2(5) . . . . ?
O19 C18 C23 C24 -179.6(3) . . . . ?
O19 C20 C21 C22 -3.5(5) . . . . ?
O19 C20 C21 C28 177.9(3) . . . . ?
O19 C20 C25 C26 179.9(3) . . . . ?
N4 C3 C14 C13 178.2(3) . . . . ?
N4 C5 C6 S1 3.9(7) . . . . ?
N4 C5 C6 C7 -178.4(6) . . . . ?
N4 C5 C10 C9 -178.7(4) . . . . ?
N4 C15 C16 C17 -176.9(3) . . . . ?
N4 C15 C24 C23 177.9(3) . . . . ?
N41 C27 C28 C21 -179.1(3) . . . . ?
N41 C42 C43 S44 8.1(5) . . . . ?
N41 C42 C43 C54 -176.6(3) . . . . ?
N41 C42 C51 C52 177.8(3) . . . . ?
N41 C46 C47 C48 -177.3(4) . . . . ?
N55 C60 C61 C62 178.1(14) . . . . ?
N55 C34 C35 C36 -178.1(3) . . . . ?
N55 C56 C57 S58 6.0(6) . . . . ?
N55 C56 C57 C68 178.3(4) . . . . ?
N55 C56 C57 S58A -18.5(6) . . . . ?
N55 C56 C65 C66 -179.5(3) . . . . ?
N55 C60A C61A C62A 179.4(14) . . . . ?
N69 C38 C39 C40 178.6(3) . . . . ?
N69 C70 C71 S72 -3.1(5) . . . . ?
N69 C70 C71 C82 -179.8(4) . . . . ?
N69 C70 C79 C80 178.7(4) . . . . ?
N69 C74 C75 C76 179.0(4) . . . . ?
C2 S1 C6 C5 -34.8(5) . . . . ?
C2 S1 C6 C7 147.5(6) . . . . ?
C2 C3 C14 C13 -0.7(5) . . . . ?
C2 C11 C12 C13 -2.1(6) . . . . ?
C3 N4 C5 C6 37.4(6) . . . . ?
C3 N4 C5 C10 -142.8(4) . . . . ?
C3 N4 C15 C16 -111.2(4) . . . . ?
C3 N4 C15 C24 71.4(4) . . . . ?
C3 C2 C11 C12 2.0(6) . . . . ?
C5 N4 C3 C2 -37.4(5) . . . . ?
C5 N4 C3 C14 143.7(4) . . . . ?
C5 N4 C15 C16 95.1(4) . . . . ?
C5 N4 C15 C24 -82.2(4) . . . . ?
C5 C6 C7 C8 -3.0(11) . . . . ?
C6 S1 C2 C3 34.8(4) . . . . ?
C6 S1 C2 C11 -149.7(4) . . . . ?
C6 C5 C10 C9 1.1(7) . . . . ?
C6 C7 C8 C9 1.3(13) . . . . ?
C7 C8 C9 C10 1.5(11) . . . . ?
C8 C9 C10 C5 -2.7(9) . . . . ?
C10 C5 C6 S1 -175.9(4) . . . . ?
C10 C5 C6 C7 1.8(8) . . . . ?
C11 C2 C3 N4 -179.5(3) . . . . ?
C11 C2 C3 C14 -0.6(5) . . . . ?
C11 C12 C13 C14 0.8(6) . . . . ?
C12 C13 C14 C3 0.6(6) . . . . ?
C15 N4 C3 C2 170.0(3) . . . . ?
C15 N4 C3 C14 -8.9(5) . . . . ?
C15 N4 C5 C6 -169.3(4) . . . . ?
C15 N4 C5 C10 10.5(5) . . . . ?
C15 C16 C17 C18 -0.6(5) . . . . ?
C16 C15 C24 C23 0.5(5) . . . . ?
C16 C17 C18 O19 -179.5(3) . . . . ?
C16 C17 C18 C23 -0.3(5) . . . . ?
C17 C18 C23 C22 -176.0(3) . . . . ?
C17 C18 C23 C24 1.2(5) . . . . ?
C18 O19 C20 C21 -3.5(5) . . . . ?
C18 O19 C20 C25 176.4(3) . . . . ?
C18 C23 C24 C15 -1.4(5) . . . . ?
C20 O19 C18 C17 -177.1(3) . . . . ?
C20 O19 C18 C23 3.6(5) . . . . ?
C20 C21 C22 C23 9.1(4) . . . . ?
C20 C21 C22 C29 135.1(3) . . . . ?
C20 C21 C22 C32 -113.0(3) . . . . ?
C20 C21 C28 C27 3.1(5) . . . . ?
C20 C25 C26 C27 1.3(6) . . . . ?
C21 C20 C25 C26 -0.2(5) . . . . ?
C21 C22 C23 C18 -8.9(4) . . . . ?
C21 C22 C23 C24 173.9(3) . . . . ?
C21 C22 C29 C30 119.1(3) . . . . ?
C21 C22 C29 C37 -57.9(4) . . . . ?
C21 C22 C32 C31 -119.7(3) . . . . ?
C21 C22 C32 C33 59.1(4) . . . . ?
C22 C21 C28 C27 -175.5(3) . . . . ?
C22 C23 C24 C15 175.9(3) . . . . ?
C22 C29 C30 C31 -0.8(4) . . . . ?
C22 C29 C30 C40 -178.7(3) . . . . ?
C22 C29 C37 C38 176.8(3) . . . . ?
C22 C32 C33 C34 -178.5(3) . . . . ?
C23 C22 C29 C30 -116.5(3) . . . . ?
C23 C22 C29 C37 66.5(4) . . . . ?
C23 C22 C32 C31 118.5(3) . . . . ?
C23 C22 C32 C33 -62.8(4) . . . . ?
C24 C15 C16 C17 0.5(5) . . . . ?
C25 C20 C21 C22 176.6(3) . . . . ?
C25 C20 C21 C28 -1.9(5) . . . . ?
C25 C26 C27 N41 176.9(3) . . . . ?
C25 C26 C27 C28 -0.2(6) . . . . ?
C26 C27 C28 C21 -2.1(5) . . . . ?
C27 N41 C42 C43 -175.6(3) . . . . ?
C27 N41 C42 C51 2.9(5) . . . . ?
C27 N41 C46 C45 172.6(3) . . . . ?
C27 N41 C46 C47 -8.8(5) . . . . ?
C28 C21 C22 C23 -172.4(3) . . . . ?
C28 C21 C22 C29 -46.4(4) . . . . ?
C28 C21 C22 C32 65.5(4) . . . . ?
C29 C22 C23 C18 -134.5(3) . . . . ?
C29 C22 C23 C24 48.3(4) . . . . ?
C29 C22 C32 C31 -0.9(4) . . . . ?
C29 C22 C32 C33 177.9(3) . . . . ?
C29 C30 C31 C32 0.2(4) . . . . ?
C29 C30 C31 C36 -179.3(3) . . . . ?
C29 C30 C40 C39 1.2(5) . . . . ?
C29 C37 C38 N69 -178.8(3) . . . . ?
C29 C37 C38 C39 1.5(5) . . . . ?
C30 C29 C37 C38 0.1(5) . . . . ?
C30 C31 C32 C22 0.5(4) . . . . ?
C30 C31 C32 C33 -178.4(3) . . . . ?
C30 C31 C36 C35 178.2(3) . . . . ?
C31 C30 C40 C39 -176.1(3) . . . . ?
C31 C32 C33 C34 0.2(5) . . . . ?
C32 C22 C23 C18 113.6(3) . . . . ?
C32 C22 C23 C24 -63.5(4) . . . . ?
C32 C22 C29 C30 1.1(4) . . . . ?
C32 C22 C29 C37 -176.0(3) . . . . ?
C32 C31 C36 C35 -1.4(5) . . . . ?
C32 C33 C34 N55 177.9(3) . . . . ?
C32 C33 C34 C35 -1.4(5) . . . . ?
C33 C34 C35 C36 1.3(6) . . . . ?
C34 N55 C56 C57 157.5(4) . . . . ?
C34 N55 C56 C65 -22.8(5) . . . . ?
C34 N55 C60A C59A -148.5(12) . . . . ?
C34 N55 C60A C61A 30(2) . . . . ?
C34 C35 C36 C31 0.1(5) . . . . ?
C36 C31 C32 C22 -179.9(3) . . . . ?
C36 C31 C32 C33 1.2(5) . . . . ?
C37 C29 C30 C31 176.4(3) . . . . ?
C37 C29 C30 C40 -1.5(5) . . . . ?
C37 C38 C39 C40 -1.8(6) . . . . ?
C38 N69 C70 C71 156.0(3) . . . . ?
C38 N69 C70 C79 -24.1(5) . . . . ?
C38 N69 C74 C73 -159.2(3) . . . . ?
C38 N69 C74 C75 21.0(5) . . . . ?
C38 C39 C40 C30 0.4(5) . . . . ?
C40 C30 C31 C32 177.8(4) . . . . ?
C40 C30 C31 C36 -1.8(6) . . . . ?
C42 N41 C27 C26 119.7(4) . . . . ?
C42 N41 C27 C28 -63.3(4) . . . . ?
C42 N41 C46 C45 -38.7(5) . . . . ?
C42 N41 C46 C47 139.9(4) . . . . ?
C42 C43 C54 C53 -2.5(6) . . . . ?
C42 C51 C52 C53 -0.1(6) . . . . ?
C43 S44 C45 C46 37.0(4) . . . . ?
C43 S44 C45 C50 -143.4(4) . . . . ?
C43 C42 C51 C52 -3.7(5) . . . . ?
C45 S44 C43 C42 -39.3(3) . . . . ?
C45 S44 C43 C54 145.4(3) . . . . ?
C45 C46 C47 C48 1.3(7) . . . . ?
C46 N41 C27 C26 -91.2(4) . . . . ?
C46 N41 C27 C28 85.9(4) . . . . ?
C46 N41 C42 C43 36.4(5) . . . . ?
C46 N41 C42 C51 -145.1(4) . . . . ?
C46 C45 C50 C49 1.5(8) . . . . ?
C46 C47 C48 C49 -0.3(8) . . . . ?
C47 C48 C49 C50 -0.2(9) . . . . ?
C48 C49 C50 C45 -0.4(9) . . . . ?
C50 C45 C46 N41 176.8(4) . . . . ?
C50 C45 C46 C47 -1.9(7) . . . . ?
C51 C42 C43 S44 -170.4(3) . . . . ?
C51 C42 C43 C54 4.9(5) . . . . ?
C51 C52 C53 C54 2.6(6) . . . . ?
C52 C53 C54 C43 -1.4(6) . . . . ?
C56 N55 C34 C33 81.7(4) . . . . ?
C56 N55 C34 C35 -98.9(4) . . . . ?
C56 N55 C60A C59A 40(2) . . . . ?
C56 N55 C60A C61A -141.3(13) . . . . ?
C56 C57 C68 C67 1.8(7) . . . . ?
C56 C57 S58A C59A 47.3(6) . . . . ?
C56 C65 C66 C67 0.6(5) . . . . ?
C57 S58 C59 C60 -37.6(12) . . . . ?
C57 S58 C59 C64 150.0(10) . . . . ?
C57 C56 C65 C66 0.2(5) . . . . ?
C57 S58A C59A C60A -38.7(13) . . . . ?
C57 S58A C59A C64A 141.5(8) . . . . ?
C65 C56 C57 S58 -173.7(4) . . . . ?
C65 C56 C57 C68 -1.4(6) . . . . ?
C65 C56 C57 S58A 161.8(4) . . . . ?
C65 C66 C67 C68 -0.3(6) . . . . ?
C66 C67 C68 C57 -0.9(7) . . . . ?
C68 C57 S58A C59A -148.9(5) . . . . ?
C70 N69 C38 C37 -93.5(4) . . . . ?
C70 N69 C38 C39 86.2(4) . . . . ?
C70 N69 C74 C73 35.7(5) . . . . ?
C70 N69 C74 C75 -144.2(4) . . . . ?
C70 C71 C82 C81 1.4(6) . . . . ?
C70 C79 C80 C81 0.8(7) . . . . ?
C71 S72 C73 C74 -38.7(4) . . . . ?
C71 S72 C73 C78 146.9(4) . . . . ?
C71 C70 C79 C80 -1.4(6) . . . . ?
C73 S72 C71 C70 36.1(3) . . . . ?
C73 S72 C71 C82 -147.2(3) . . . . ?
C73 C74 C75 C76 -0.9(6) . . . . ?
C74 N69 C38 C37 101.2(4) . . . . ?
C74 N69 C38 C39 -79.2(4) . . . . ?
C74 N69 C70 C71 -38.8(5) . . . . ?
C74 N69 C70 C79 141.1(4) . . . . ?
C74 C73 C78 C77 -2.9(7) . . . . ?
C74 C75 C76 C77 -1.0(7) . . . . ?
C75 C76 C77 C78 1.0(7) . . . . ?
C76 C77 C78 C73 0.9(7) . . . . ?
C78 C73 C74 N69 -177.0(4) . . . . ?
C78 C73 C74 C75 2.9(6) . . . . ?
C79 C70 C71 S72 177.0(3) . . . . ?
C79 C70 C71 C82 0.3(5) . . . . ?
C79 C80 C81 C82 0.9(7) . . . . ?
C80 C81 C82 C71 -2.1(7) . . . . ?
S58A C57 C68 C67 -161.8(5) . . . . ?
S58A C59A C60A N55 1(2) . . . . ?
S58A C59A C60A C61A -177.0(12) . . . . ?
S58A C59A C64A C63A 176.4(8) . . . . ?
C59A C60A C61A C62A -2(2) . . . . ?
C60A N55 C34 C33 -89.4(11) . . . . ?
C60A N55 C34 C35 90.0(11) . . . . ?
C60A N55 C56 C57 -30.9(10) . . . . ?
C60A N55 C56 C65 148.8(9) . . . . ?
C60A C59A C64A C63A -3.4(17) . . . . ?
C60A C61A C62A C63A 2.0(19) . . . . ?
C61A C62A C63A C64A -2.6(17) . . . . ?
C62A C63A C64A C59A 3.3(16) . . . . ?
C64A C59A C60A N55 -178.7(13) . . . . ?
C64A C59A C60A C61A 3(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3 1 -22 0.0393 2.5353 0.5043 -21.6962 0.4776 -0.8785 -0.0086
23 0 -11 0.0181 23.0035 0.0002 -11.4898 0.9211 0.3713 0.0887
2 -5 -12 0.1599 2.0083 -4.9996 -12.0004 0.1966 -0.4438 0.8148
-23 0 11 0.0264 -23.0035 -0.0002 11.4898 -0.9211 -0.3713 -0.0887
0 0 -21 0.0525 0.0029 -0.0012 -20.5016 0.3692 -0.9207 0.0602
-2 5 12 0.1599 -2.0083 4.9996 12.0004 -0.1966 0.4438 -0.8148
1 0 1 0.0229 1.0000 0.0001 0.5005 0.0220 0.0611 0.0009
-1 3 -19 0.0700 -1.0014 2.9983 -18.5016 0.3511 -0.8803 -0.4130
-1 0 1 0.0297 -1.0002 0.0000 0.9996 -0.0491 0.0063 -0.0053

_olex2_date_sample_data_collection 2015-06-11
_olex2_date_sample_submission    2015-06-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id M12o6
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7376(12)
2 0.2624(12)

