# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

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

data_lb1a
_database_code_depnum_ccdc_archive 'CCDC 1033558'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Sep 17 11:18:06 2014'
;
_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H50 N2 O3, C2 H3 N'
_chemical_formula_sum            'C70 H53 N3 O3'
_chemical_formula_weight         984.15
_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 0.0181 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'

_symmetry_space_group_name_H-M_alt 'P -1'
_cell_length_a                   12.9850(3)
_cell_length_b                   13.0948(3)
_cell_length_c                   16.3926(4)
_cell_angle_alpha                93.7823(19)
_cell_angle_beta                 103.688(2)
_cell_angle_gamma                100.746(2)
_cell_volume                     2642.92(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.7210
_cell_measurement_theta_min      4.1770
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1036
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.889
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17131
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.459
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   15.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -38.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega    9.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -99.0000  120.0000 75

#__ type_ start__ end____ width___ exp.time_
  3 omega   23.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867 -125.0000   60.0000 70

#__ type_ start__ end____ width___ exp.time_
  4 omega   29.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -45.0000   60.0000 65

#__ type_ start__ end____ width___ exp.time_
  5 omega   51.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -94.0000  120.0000 57

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -30.0000    0.0000 38

#__ type_ start__ end____ width___ exp.time_
  7 omega  117.00  169.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698   30.0000  -60.0000 52

#__ type_ start__ end____ width___ exp.time_
  8 omega  107.00  133.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   84.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -94.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
 10 omega   66.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -94.0000 -120.0000 42

#__ type_ start__ end____ width___ exp.time_
 11 omega   36.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -94.0000 -180.0000 72

#__ type_ start__ end____ width___ exp.time_
 12 omega   33.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -77.0000 -180.0000 37

#__ type_ start__ end____ width___ exp.time_
 13 omega    9.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -99.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
 14 omega    7.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -99.0000  -30.0000 34

#__ type_ start__ end____ width___ exp.time_
 15 omega   19.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -77.0000 -150.0000 52

#__ type_ start__ end____ width___ exp.time_
 16 omega   34.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -30.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
 17 omega   29.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -45.0000 -150.0000 69

#__ type_ start__ end____ width___ exp.time_
 18 omega   28.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -30.0000  -30.0000 37

#__ type_ start__ end____ width___ exp.time_
 19 omega   59.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867   57.0000   90.0000 57

#__ type_ start__ end____ width___ exp.time_
 20 omega   10.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867   57.0000   90.0000 34

#__ type_ start__ end____ width___ exp.time_
 21 omega  -29.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -38.0000  150.0000 65

#__ type_ start__ end____ width___ exp.time_
 22 omega   26.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698 -111.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
 23 omega   25.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4698  -94.0000   60.0000 68

#__ type_ start__ end____ width___ exp.time_
 24 omega  -45.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -57.0000 -150.0000 111

#__ type_ start__ end____ width___ exp.time_
 25 omega  -43.00   -5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -38.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
 26 omega -105.00  -75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.2867 -125.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
 27 omega -125.00  -95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.2867  -99.0000 -120.0000 30

#__ type_ start__ end____ width___ exp.time_
 28 omega  -71.00  -24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.2867  -77.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
 29 omega  -50.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2867  -77.0000 -180.0000 78

#__ type_ start__ end____ width___ exp.time_
 30 omega  -98.00  -73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.2867 -125.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1070538000
_diffrn_orient_matrix_UB_12      -0.0157684000
_diffrn_orient_matrix_UB_13      -0.0690368000
_diffrn_orient_matrix_UB_21      0.0407917000
_diffrn_orient_matrix_UB_22      0.1049954000
_diffrn_orient_matrix_UB_23      -0.0308402000
_diffrn_orient_matrix_UB_31      0.0496342000
_diffrn_orient_matrix_UB_32      -0.0570955000
_diffrn_orient_matrix_UB_33      -0.0613587000
_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                7162
_reflns_number_total             8468
_reflns_odcompleteness_completeness 90.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         8468
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0530
_refine_ls_restrained_S_all      1.051
_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)+(0.0734P)²+0.7715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1534
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C33(H33), C35(H35), C36(H36), C39(H39), C40(H40), C42(H42), C46(H46),
 C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C58(H58),
  C59(H59), C60(H60), C61(H61), C64(H64), C65(H65), C66(H66), C67(H67)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C44(H44A,H44B,H44C), C70(H70A,H70B,H70C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 1.1268(2) 0.60293(13) 0.24285(11) 0.1068(7) Uani 1 1 d . . . . .
O2 O 0.9763(2) 0.51469(17) 0.26654(14) 0.1120(7) Uani 1 1 d . . . . .
O3 O 0.88582(10) 0.20395(10) 0.02392(9) 0.0554(3) Uani 1 1 d . . . . .
N1 N 1.32687(14) 1.18773(14) 0.23598(13) 0.0630(5) Uani 1 1 d . . . . .
N2 N 0.73445(14) 0.73900(14) 0.38413(11) 0.0603(4) Uani 1 1 d . . . . .
C1 C 1.0403(2) 0.52492(17) 0.22451(14) 0.0693(6) Uani 1 1 d . . . . .
C2 C 1.03476(17) 0.45577(15) 0.14711(12) 0.0537(5) Uani 1 1 d . . . . .
C3 C 1.10711(16) 0.48455(14) 0.10011(13) 0.0551(5) Uani 1 1 d . . . . .
H3 H 1.1571 0.5477 0.1166 0.066 Uiso 1 1 calc R . . . .
C4 C 1.10821(15) 0.42133(14) 0.02734(12) 0.0493(4) Uani 1 1 d . . . . .
C5 C 1.18458(16) 0.44931(16) -0.01991(14) 0.0588(5) Uani 1 1 d . . . . .
H5 H 1.2359 0.5114 -0.0025 0.071 Uiso 1 1 calc R . . . .
C6 C 1.18583(17) 0.38832(17) -0.09034(14) 0.0596(5) Uani 1 1 d . . . . .
C7 C 1.10738(17) 0.29425(17) -0.11560(14) 0.0610(5) Uani 1 1 d . . . . .
H7 H 1.1072 0.2518 -0.1634 0.073 Uiso 1 1 calc R . . . .
C8 C 1.03198(16) 0.26381(15) -0.07204(13) 0.0555(5) Uani 1 1 d . . . . .
H8 H 0.9813 0.2014 -0.0905 0.067 Uiso 1 1 calc R . . . .
C9 C 1.03016(14) 0.32629(14) 0.00101(12) 0.0473(4) Uani 1 1 d . . . . .
C10 C 0.95472(14) 0.29948(14) 0.04983(12) 0.0474(4) Uani 1 1 d . . . . .
C11 C 0.78346(16) 0.18778(16) 0.04698(13) 0.0557(5) Uani 1 1 d . . . . .
C12 C 0.80296(18) 0.23161(18) 0.13752(14) 0.0653(5) Uani 1 1 d . . . . .
H12 H 0.7593 0.2006 0.1704 0.078 Uiso 1 1 calc R . . . .
C13 C 0.88188(18) 0.31431(17) 0.17120(14) 0.0628(5) Uani 1 1 d . . . . .
H13 H 0.8901 0.3434 0.2263 0.075 Uiso 1 1 calc R . . . .
C14 C 0.95540(16) 0.35955(15) 0.12243(12) 0.0512(4) Uani 1 1 d . . . . .
C15 C 0.74047(16) 0.06902(16) 0.03435(13) 0.0568(5) Uani 1 1 d . . . . .
C16 C 0.79225(19) 0.00008(17) 0.00084(14) 0.0657(6) Uani 1 1 d . . . . .
H16 H 0.8551 0.0252 -0.0157 0.079 Uiso 1 1 calc R . . . .
C17 C 0.7506(2) -0.10671(18) -0.00810(16) 0.0775(7) Uani 1 1 d . . . . .
H17 H 0.7858 -0.1529 -0.0306 0.093 Uiso 1 1 calc R . . . .
C18 C 0.6578(2) -0.14494(19) 0.01590(17) 0.0776(7) Uani 1 1 d . . . . .
H18 H 0.6308 -0.2167 0.0100 0.093 Uiso 1 1 calc R . . . .
C19 C 0.60516(19) -0.07730(19) 0.04858(17) 0.0734(6) Uani 1 1 d . . . . .
H19 H 0.5420 -0.1031 0.0646 0.088 Uiso 1 1 calc R . . . .
C20 C 0.64595(18) 0.02944(18) 0.05780(16) 0.0674(6) Uani 1 1 d . . . . .
H20 H 0.6098 0.0751 0.0799 0.081 Uiso 1 1 calc R . . . .
C21 C 0.70484(17) 0.23971(16) -0.01307(16) 0.0634(5) Uani 1 1 d . . . . .
C22 C 0.7010(2) 0.2315(2) -0.09803(17) 0.0830(7) Uani 1 1 d . . . . .
H22 H 0.7475 0.1963 -0.1182 0.100 Uiso 1 1 calc R . . . .
C23 C 0.6272(3) 0.2758(3) -0.1540(2) 0.1095(11) Uani 1 1 d . . . . .
H23 H 0.6247 0.2704 -0.2113 0.131 Uiso 1 1 calc R . . . .
C24 C 0.5587(3) 0.3271(3) -0.1239(3) 0.1096(12) Uani 1 1 d . . . . .
H24 H 0.5094 0.3564 -0.1610 0.132 Uiso 1 1 calc R . . . .
C25 C 0.5621(2) 0.3356(2) -0.0406(3) 0.0969(10) Uani 1 1 d . . . . .
H25 H 0.5153 0.3706 -0.0206 0.116 Uiso 1 1 calc R . . . .
C26 C 0.63497(19) 0.29233(18) 0.0150(2) 0.0757(7) Uani 1 1 d . . . . .
H26 H 0.6369 0.2988 0.0722 0.091 Uiso 1 1 calc R . . . .
C27 C 1.2667(2) 0.4195(2) -0.14150(18) 0.0852(8) Uani 1 1 d . . . . .
H27A H 1.2325 0.4476 -0.1910 0.128 Uiso 1 1 calc GR . . . .
H27B H 1.2924 0.3592 -0.1581 0.128 Uiso 1 1 calc GR . . . .
H27C H 1.3266 0.4715 -0.1080 0.128 Uiso 1 1 calc GR . . . .
C28 C 1.1421(5) 0.6735(2) 0.3182(2) 0.184(3) Uani 1 1 d . . . . .
H28A H 1.0822 0.6515 0.3434 0.221 Uiso 1 1 calc R . . . .
H28B H 1.2078 0.6666 0.3583 0.221 Uiso 1 1 calc R . . . .
C29 C 1.1488(3) 0.77371(18) 0.30765(16) 0.0853(8) Uani 1 1 d . . . . .
H29A H 1.0817 0.7809 0.2694 0.102 Uiso 1 1 calc R . . . .
H29B H 1.2065 0.7948 0.2801 0.102 Uiso 1 1 calc R . . . .
C30 C 1.16968(18) 0.84969(15) 0.38740(12) 0.0565(5) Uani 1 1 d . . . . .
H30A H 1.2462 0.8819 0.4045 0.068 Uiso 1 1 calc R . . . .
H30B H 1.1531 0.8101 0.4323 0.068 Uiso 1 1 calc R . . . .
C31 C 1.10465(14) 0.93650(13) 0.37851(11) 0.0457(4) Uani 1 1 d . . . . .
C32 C 0.98249(14) 0.89696(13) 0.34733(11) 0.0465(4) Uani 1 1 d . . . . .
C33 C 0.91555(15) 0.82915(14) 0.38270(11) 0.0490(4) Uani 1 1 d . . . . .
H33 H 0.9443 0.7987 0.4303 0.059 Uiso 1 1 calc R . . . .
C34 C 0.80417(15) 0.80678(14) 0.34621(12) 0.0506(4) Uani 1 1 d . . . . .
C35 C 0.76144(15) 0.85169(15) 0.27471(12) 0.0538(5) Uani 1 1 d . . . . .
H35 H 0.6872 0.8352 0.2502 0.065 Uiso 1 1 calc R . . . .
C36 C 0.82859(15) 0.92091(15) 0.23969(12) 0.0519(4) Uani 1 1 d . . . . .
H36 H 0.7997 0.9521 0.1926 0.062 Uiso 1 1 calc R . . . .
C37 C 0.93961(14) 0.94310(13) 0.27587(11) 0.0464(4) Uani 1 1 d . . . . .
C38 C 1.02953(15) 1.01129(14) 0.25342(11) 0.0475(4) Uani 1 1 d . . . . .
C39 C 1.03091(17) 1.07618(16) 0.18964(13) 0.0571(5) Uani 1 1 d . . . . .
H39 H 0.9669 1.0807 0.1514 0.068 Uiso 1 1 calc R . . . .
C40 C 1.12952(17) 1.13407(17) 0.18413(14) 0.0605(5) Uani 1 1 d . . . . .
H40 H 1.1315 1.1773 0.1415 0.073 Uiso 1 1 calc R . . . .
C41 C 1.22492(16) 1.12835(16) 0.24120(14) 0.0563(5) Uani 1 1 d . . . . .
C42 C 1.22359(15) 1.06501(14) 0.30617(13) 0.0520(4) Uani 1 1 d . . . . .
H42 H 1.2875 1.0624 0.3454 0.062 Uiso 1 1 calc R . . . .
C43 C 1.12590(14) 1.00629(13) 0.31142(11) 0.0467(4) Uani 1 1 d . . . . .
C44 C 1.13160(17) 1.00348(16) 0.46473(12) 0.0590(5) Uani 1 1 d . . . . .
H44A H 1.1162 0.9595 0.5068 0.089 Uiso 1 1 calc GR . . . .
H44B H 1.0884 1.0558 0.4608 0.089 Uiso 1 1 calc GR . . . .
H44C H 1.2070 1.0368 0.4803 0.089 Uiso 1 1 calc GR . . . .
C45 C 1.42029(17) 1.14660(18) 0.24526(15) 0.0632(5) Uani 1 1 d . . . . .
C46 C 1.4286(2) 1.0432(2) 0.23381(18) 0.0780(7) Uani 1 1 d . . . . .
H46 H 1.3674 0.9894 0.2177 0.094 Uiso 1 1 calc R . . . .
C47 C 1.5312(2) 1.0230(2) 0.2472(2) 0.0934(9) Uani 1 1 d . . . . .
H47 H 1.5391 0.9542 0.2391 0.112 Uiso 1 1 calc R . . . .
C48 C 1.6234(2) 1.1025(3) 0.2726(2) 0.0983(9) Uani 1 1 d . . . . .
H48 H 1.6916 1.0860 0.2836 0.118 Uiso 1 1 calc R . . . .
C49 C 1.6145(2) 1.2052(3) 0.28138(19) 0.0866(8) Uani 1 1 d . . . . .
H49 H 1.6763 1.2584 0.2972 0.104 Uiso 1 1 calc R . . . .
C50 C 1.51163(18) 1.22892(19) 0.26628(15) 0.0657(6) Uani 1 1 d . . . . .
C51 C 1.47251(18) 1.32474(19) 0.26989(14) 0.0651(6) Uani 1 1 d . . . . .
C52 C 1.5234(2) 1.4298(2) 0.28856(16) 0.0787(7) Uani 1 1 d . . . . .
H52 H 1.5984 1.4499 0.2995 0.094 Uiso 1 1 calc R . . . .
C53 C 1.4612(3) 1.5034(2) 0.29051(18) 0.0893(8) Uani 1 1 d . . . . .
H53 H 1.4948 1.5737 0.3045 0.107 Uiso 1 1 calc R . . . .
C54 C 1.3492(3) 1.4749(2) 0.27205(18) 0.0862(8) Uani 1 1 d . . . . .
H54 H 1.3090 1.5266 0.2729 0.103 Uiso 1 1 calc R . . . .
C55 C 1.2959(2) 1.37122(19) 0.25247(17) 0.0745(6) Uani 1 1 d . . . . .
H55 H 1.2208 1.3521 0.2402 0.089 Uiso 1 1 calc R . . . .
C56 C 1.35923(18) 1.29709(17) 0.25193(14) 0.0612(5) Uani 1 1 d . . . . .
C57 C 0.65348(17) 0.76788(19) 0.41839(13) 0.0664(6) Uani 1 1 d . . . . .
C58 C 0.60819(19) 0.8551(2) 0.40881(17) 0.0794(7) Uani 1 1 d . . . . .
H58 H 0.6304 0.9057 0.3758 0.095 Uiso 1 1 calc R . . . .
C59 C 0.5283(2) 0.8643(3) 0.4503(2) 0.1095(12) Uani 1 1 d . . . . .
H59 H 0.4955 0.9217 0.4438 0.131 Uiso 1 1 calc R . . . .
C60 C 0.4958(3) 0.7907(4) 0.5011(3) 0.1358(18) Uani 1 1 d . . . . .
H60 H 0.4426 0.7996 0.5287 0.163 Uiso 1 1 calc R . . . .
C61 C 0.5417(3) 0.7051(4) 0.5106(2) 0.1158(14) Uani 1 1 d . . . . .
H61 H 0.5201 0.6558 0.5448 0.139 Uiso 1 1 calc R . . . .
C62 C 0.6214(2) 0.6918(2) 0.46883(15) 0.0824(8) Uani 1 1 d . . . . .
C63 C 0.6848(2) 0.6131(2) 0.46477(15) 0.0823(8) Uani 1 1 d . . . . .
C64 C 0.6873(3) 0.5180(3) 0.4983(2) 0.1157(13) Uani 1 1 d . . . . .
H64 H 0.6424 0.4955 0.5330 0.139 Uiso 1 1 calc R . . . .
C65 C 0.7565(4) 0.4580(3) 0.4797(3) 0.1303(16) Uani 1 1 d . . . . .
H65 H 0.7578 0.3943 0.5014 0.156 Uiso 1 1 calc R . . . .
C66 C 0.8247(3) 0.4915(2) 0.4285(2) 0.1072(11) Uani 1 1 d . . . . .
H66 H 0.8714 0.4497 0.4171 0.129 Uiso 1 1 calc R . . . .
C67 C 0.8250(2) 0.58482(19) 0.39436(18) 0.0801(7) Uani 1 1 d . . . . .
H67 H 0.8708 0.6068 0.3602 0.096 Uiso 1 1 calc R . . . .
C68 C 0.75417(19) 0.64468(18) 0.41313(14) 0.0669(6) Uani 1 1 d . . . . .
N3 N 0.9014(3) 0.2275(4) 0.4089(3) 0.1648(17) Uani 1 1 d . . . . .
C69 C 0.9787(3) 0.2531(3) 0.3908(2) 0.0975(9) Uani 1 1 d . . . . .
C70 C 1.0776(3) 0.2863(3) 0.3683(2) 0.1019(9) Uani 1 1 d . . . . .
H70A H 1.0687 0.2624 0.3099 0.153 Uiso 1 1 calc GR . . . .
H70B H 1.1333 0.2576 0.4029 0.153 Uiso 1 1 calc GR . . . .
H70C H 1.0977 0.3613 0.3768 0.153 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 C1 1.329(3) . ?
O1 C28 1.444(3) . ?
O2 C1 1.194(3) . ?
O3 C10 1.371(2) . ?
O3 C11 1.448(2) . ?
N1 C41 1.429(2) . ?
N1 C45 1.397(3) . ?
N1 C56 1.403(3) . ?
N2 C34 1.426(2) . ?
N2 C57 1.401(3) . ?
N2 C68 1.398(3) . ?
C1 C2 1.489(3) . ?
C2 C3 1.366(3) . ?
C2 C14 1.437(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.411(3) . ?
C4 C5 1.408(3) . ?
C4 C9 1.419(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.365(3) . ?
C6 C7 1.411(3) . ?
C6 C27 1.508(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.360(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.413(3) . ?
C9 C10 1.415(3) . ?
C10 C14 1.380(3) . ?
C11 C12 1.501(3) . ?
C11 C15 1.534(3) . ?
C11 C21 1.531(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.329(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.454(3) . ?
C15 C16 1.380(3) . ?
C15 C20 1.391(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.387(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.371(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.370(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.384(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.378(4) . ?
C21 C26 1.378(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.400(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.369(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.353(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.380(4) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.324(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.527(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.532(3) . ?
C31 C32 1.523(2) . ?
C31 C43 1.518(3) . ?
C31 C44 1.542(2) . ?
C32 C33 1.378(2) . ?
C32 C37 1.399(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.395(3) . ?
C34 C35 1.390(3) . ?
C35 H35 0.9300 . ?
C35 C36 1.386(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.390(3) . ?
C37 C38 1.468(2) . ?
C38 C39 1.391(3) . ?
C38 C43 1.396(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.387(3) . ?
C40 H40 0.9300 . ?
C40 C41 1.382(3) . ?
C41 C42 1.394(3) . ?
C42 H42 0.9300 . ?
C42 C43 1.380(2) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.383(3) . ?
C45 C50 1.403(3) . ?
C46 H46 0.9300 . ?
C46 C47 1.376(4) . ?
C47 H47 0.9300 . ?
C47 C48 1.390(4) . ?
C48 H48 0.9300 . ?
C48 C49 1.372(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.397(3) . ?
C50 C51 1.442(3) . ?
C51 C52 1.391(3) . ?
C51 C56 1.401(3) . ?
C52 H52 0.9300 . ?
C52 C53 1.371(4) . ?
C53 H53 0.9300 . ?
C53 C54 1.387(4) . ?
C54 H54 0.9300 . ?
C54 C55 1.382(4) . ?
C55 H55 0.9300 . ?
C55 C56 1.385(3) . ?
C57 C58 1.380(4) . ?
C57 C62 1.402(3) . ?
C58 H58 0.9300 . ?
C58 C59 1.387(3) . ?
C59 H59 0.9300 . ?
C59 C60 1.386(6) . ?
C60 H60 0.9300 . ?
C60 C61 1.365(6) . ?
C61 H61 0.9300 . ?
C61 C62 1.400(4) . ?
C62 C63 1.441(4) . ?
C63 C64 1.397(5) . ?
C63 C68 1.403(3) . ?
C64 H64 0.9300 . ?
C64 C65 1.371(6) . ?
C65 H65 0.9300 . ?
C65 C66 1.391(5) . ?
C66 H66 0.9300 . ?
C66 C67 1.377(4) . ?
C67 H67 0.9300 . ?
C67 C68 1.388(4) . ?
N3 C69 1.112(4) . ?
C69 C70 1.419(4) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?

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
C1 O1 C28 116.7(3) . . ?
C10 O3 C11 117.61(14) . . ?
C45 N1 C41 123.32(18) . . ?
C45 N1 C56 107.78(17) . . ?
C56 N1 C41 125.13(17) . . ?
C57 N2 C34 125.04(18) . . ?
C68 N2 C34 124.76(18) . . ?
C68 N2 C57 108.18(18) . . ?
O1 C1 C2 111.9(2) . . ?
O2 C1 O1 122.2(2) . . ?
O2 C1 C2 125.9(2) . . ?
C3 C2 C1 119.01(19) . . ?
C3 C2 C14 120.29(17) . . ?
C14 C2 C1 120.70(19) . . ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 121.93(17) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C9 119.03(17) . . ?
C5 C4 C3 122.10(17) . . ?
C5 C4 C9 118.87(17) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 C4 122.24(18) . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C7 118.02(19) . . ?
C5 C6 C27 122.0(2) . . ?
C7 C6 C27 120.0(2) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 C6 121.93(18) . . ?
C8 C7 H7 119.0 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.46(18) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C4 118.47(17) . . ?
C8 C9 C10 123.68(16) . . ?
C10 C9 C4 117.84(16) . . ?
O3 C10 C9 114.87(15) . . ?
O3 C10 C14 121.60(17) . . ?
C14 C10 C9 123.30(17) . . ?
O3 C11 C12 108.95(16) . . ?
O3 C11 C15 105.84(16) . . ?
O3 C11 C21 108.95(16) . . ?
C12 C11 C15 111.39(17) . . ?
C12 C11 C21 112.08(18) . . ?
C21 C11 C15 109.42(17) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.75(19) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.36(19) . . ?
C14 C13 H13 119.8 . . ?
C2 C14 C13 125.82(17) . . ?
C10 C14 C2 117.57(17) . . ?
C10 C14 C13 116.34(17) . . ?
C16 C15 C11 122.43(18) . . ?
C16 C15 C20 118.9(2) . . ?
C20 C15 C11 118.71(19) . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0(2) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.7(2) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 119.9(2) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C15 C20 H20 119.7 . . ?
C19 C20 C15 120.6(2) . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C11 119.6(2) . . ?
C26 C21 C11 121.8(2) . . ?
C26 C21 C22 118.6(3) . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(3) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.5(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.2(3) . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 121.0(3) . . ?
C21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C6 C27 H27A 109.5 . . ?
C6 C27 H27B 109.5 . . ?
C6 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 H28A 108.3 . . ?
O1 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 O1 116.0(3) . . ?
C29 C28 H28A 108.3 . . ?
C29 C28 H28B 108.3 . . ?
C28 C29 H29A 108.2 . . ?
C28 C29 H29B 108.2 . . ?
C28 C29 C30 116.5(2) . . ?
H29A C29 H29B 107.3 . . ?
C30 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
C29 C30 H30A 108.5 . . ?
C29 C30 H30B 108.5 . . ?
C29 C30 C31 115.10(18) . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 H30A 108.5 . . ?
C31 C30 H30B 108.5 . . ?
C30 C31 C44 108.67(16) . . ?
C32 C31 C30 114.19(15) . . ?
C32 C31 C44 109.60(14) . . ?
C43 C31 C30 113.64(15) . . ?
C43 C31 C32 100.92(15) . . ?
C43 C31 C44 109.57(15) . . ?
C33 C32 C31 128.19(17) . . ?
C33 C32 C37 120.63(17) . . ?
C37 C32 C31 111.11(15) . . ?
C32 C33 H33 120.4 . . ?
C32 C33 C34 119.11(18) . . ?
C34 C33 H33 120.4 . . ?
C33 C34 N2 119.20(18) . . ?
C35 C34 N2 120.41(17) . . ?
C35 C34 C33 120.38(17) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.54(18) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 120.4 . . ?
C35 C36 C37 119.13(19) . . ?
C37 C36 H36 120.4 . . ?
C32 C37 C38 108.18(16) . . ?
C36 C37 C32 120.19(17) . . ?
C36 C37 C38 131.64(18) . . ?
C39 C38 C37 131.35(18) . . ?
C39 C38 C43 120.20(17) . . ?
C43 C38 C37 108.42(16) . . ?
C38 C39 H39 120.6 . . ?
C40 C39 C38 118.8(2) . . ?
C40 C39 H39 120.6 . . ?
C39 C40 H40 119.6 . . ?
C41 C40 C39 120.9(2) . . ?
C41 C40 H40 119.6 . . ?
C40 C41 N1 121.22(19) . . ?
C40 C41 C42 120.46(18) . . ?
C42 C41 N1 118.32(19) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 C41 118.96(19) . . ?
C43 C42 H42 120.5 . . ?
C38 C43 C31 111.26(15) . . ?
C42 C43 C31 127.97(18) . . ?
C42 C43 C38 120.67(18) . . ?
C31 C44 H44A 109.5 . . ?
C31 C44 H44B 109.5 . . ?
C31 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N1 C45 C50 109.2(2) . . ?
C46 C45 N1 128.6(2) . . ?
C46 C45 C50 122.1(2) . . ?
C45 C46 H46 121.4 . . ?
C47 C46 C45 117.3(3) . . ?
C47 C46 H46 121.4 . . ?
C46 C47 H47 119.1 . . ?
C46 C47 C48 121.9(3) . . ?
C48 C47 H47 119.1 . . ?
C47 C48 H48 119.7 . . ?
C49 C48 C47 120.5(3) . . ?
C49 C48 H48 119.7 . . ?
C48 C49 H49 120.4 . . ?
C48 C49 C50 119.2(3) . . ?
C50 C49 H49 120.4 . . ?
C45 C50 C51 106.88(19) . . ?
C49 C50 C45 118.9(2) . . ?
C49 C50 C51 134.2(2) . . ?
C52 C51 C50 133.6(2) . . ?
C52 C51 C56 119.2(2) . . ?
C56 C51 C50 107.2(2) . . ?
C51 C52 H52 120.5 . . ?
C53 C52 C51 118.9(2) . . ?
C53 C52 H52 120.5 . . ?
C52 C53 H53 119.4 . . ?
C52 C53 C54 121.1(3) . . ?
C54 C53 H53 119.4 . . ?
C53 C54 H54 119.3 . . ?
C55 C54 C53 121.4(3) . . ?
C55 C54 H54 119.3 . . ?
C54 C55 H55 121.4 . . ?
C54 C55 C56 117.2(2) . . ?
C56 C55 H55 121.4 . . ?
C51 C56 N1 108.9(2) . . ?
C55 C56 N1 129.0(2) . . ?
C55 C56 C51 122.1(2) . . ?
N2 C57 C62 108.9(2) . . ?
C58 C57 N2 129.4(2) . . ?
C58 C57 C62 121.7(2) . . ?
C57 C58 H58 121.3 . . ?
C57 C58 C59 117.4(3) . . ?
C59 C58 H58 121.3 . . ?
C58 C59 H59 119.0 . . ?
C60 C59 C58 122.0(4) . . ?
C60 C59 H59 119.0 . . ?
C59 C60 H60 120.0 . . ?
C61 C60 C59 120.1(3) . . ?
C61 C60 H60 120.0 . . ?
C60 C61 H61 120.1 . . ?
C60 C61 C62 119.8(3) . . ?
C62 C61 H61 120.1 . . ?
C57 C62 C63 106.9(2) . . ?
C61 C62 C57 119.0(3) . . ?
C61 C62 C63 134.1(3) . . ?
C64 C63 C62 133.9(3) . . ?
C64 C63 C68 118.7(3) . . ?
C68 C63 C62 107.4(2) . . ?
C63 C64 H64 120.3 . . ?
C65 C64 C63 119.4(3) . . ?
C65 C64 H64 120.3 . . ?
C64 C65 H65 119.6 . . ?
C64 C65 C66 120.7(4) . . ?
C66 C65 H65 119.6 . . ?
C65 C66 H66 119.1 . . ?
C67 C66 C65 121.8(4) . . ?
C67 C66 H66 119.1 . . ?
C66 C67 H67 121.4 . . ?
C66 C67 C68 117.2(3) . . ?
C68 C67 H67 121.4 . . ?
N2 C68 C63 108.6(2) . . ?
C67 C68 N2 129.0(2) . . ?
C67 C68 C63 122.3(3) . . ?
N3 C69 C70 179.6(5) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?

_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_lb1alpha
_database_code_depnum_ccdc_archive 'CCDC 1033559'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Sep 16 07:40:17 2014'
;
_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        
'3-(2,7-di(9H-carbazol-9-yl)-9-methyl-9H-fluoren-9-yl)propyl 8-methyl-2,2-diphenyl-2H-benzo[h]chromene-5-carboxylate'
_chemical_formula_moiety         'C68 H50 N2 O3'
_chemical_formula_sum            'C68 H50 N2 O3'
_chemical_formula_weight         943.10
_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 0.0181 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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.2538(6)
_cell_length_b                   21.2051(4)
_cell_length_c                   25.4117(13)
_cell_angle_alpha                90.0
_cell_angle_beta                 134.348(9)
_cell_angle_gamma                90.0
_cell_volume                     5107.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8333
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.4070
_cell_measurement_theta_min      4.2400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22894
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         65.081
_diffrn_reflns_theta_min         3.701
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   10.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
  2 omega  -14.00   62.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 76

#__ type_ start__ end____ width___ exp.time_
  3 omega  -69.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  125.0000  -90.0000 66

#__ type_ start__ end____ width___ exp.time_
  4 omega  -95.00  -62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  125.0000 -180.0000 33

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  125.0000 -180.0000 47

#__ type_ start__ end____ width___ exp.time_
  6 omega  116.00  141.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega  106.00  141.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000  150.0000 35

#__ type_ start__ end____ width___ exp.time_
  8 omega  104.00  140.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000  -30.0000 36

#__ type_ start__ end____ width___ exp.time_
  9 omega   22.00  140.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000   38.0000   90.0000 118

#__ type_ start__ end____ width___ exp.time_
 10 omega  103.00  178.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
 11 omega   34.00   99.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  150.0000 65

#__ type_ start__ end____ width___ exp.time_
 12 omega   31.00   89.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -25.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
 13 omega   39.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -50.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 14 omega   39.00  133.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000  -60.0000 94

#__ type_ start__ end____ width___ exp.time_
 15 omega   97.00  173.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   63.0000   60.0000 76

#__ type_ start__ end____ width___ exp.time_
 16 omega   43.00  100.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -50.0000 -150.0000 57

#__ type_ start__ end____ width___ exp.time_
 17 omega  110.00  178.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000    0.0000 68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0827251000
_diffrn_orient_matrix_UB_12      0.0617964000
_diffrn_orient_matrix_UB_13      0.0382217000
_diffrn_orient_matrix_UB_21      -0.0594302000
_diffrn_orient_matrix_UB_22      0.0053638000
_diffrn_orient_matrix_UB_23      0.0345964000
_diffrn_orient_matrix_UB_31      0.1266515000
_diffrn_orient_matrix_UB_32      -0.0378147000
_diffrn_orient_matrix_UB_33      0.0672816000
_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                6718
_reflns_number_total             8706
_reflns_odcompleteness_completeness 99.95
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8706
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0961
_refine_ls_restrained_S_all      1.115
_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)+(0.1500P)²+4.7026P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2824
_refine_ls_wR_factor_ref         0.3022
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C57) = Uanis(C68) = Uanis(C63) = Uanis(C67) = Uanis(C62) = Uanis(C65) =
Uanis(C64) = Uanis(C59) = Uanis(C58) = Uanis(C66) = Uanis(C61) = Uanis(C60)
3.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C33(H33), C35(H35), C36(H36), C39(H39), C40(H40), C42(H42), C46(H46),
 C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C58(H58),
  C59(H59), C60(H60), C61(H61), C67(H67), C66(H66), C65(H65), C64(H64)
3.c Fitted hexagon refined as free rotating group:
 C57(C58,C59,C60,C61,C62), C68(C67,C66,C65,C64,C63)
3.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C44(H44A,H44B,H44C)
;
_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 -0.2694(3) 0.44000(15) 0.26997(15) 0.0751(8) Uani 1 1 d . . . . .
O2 O -0.3422(3) 0.36048(18) 0.29265(16) 0.0955(11) Uani 1 1 d . . . . .
O3 O 0.1243(3) 0.31599(12) 0.56773(13) 0.0576(6) Uani 1 1 d . . . . .
N1 N -0.4387(4) 0.70353(19) 0.05716(19) 0.0734(9) Uani 1 1 d . . . . .
N2 N -0.8790(5) 0.5480(2) 0.2126(3) 0.0899(12) Uani 1 1 d . . . . .
C1 C -0.2515(4) 0.3971(2) 0.3145(2) 0.0596(9) Uani 1 1 d . . . . .
C2 C -0.1104(4) 0.40237(17) 0.39150(19) 0.0529(8) Uani 1 1 d . . . . .
C3 C -0.0309(4) 0.45479(18) 0.41244(19) 0.0557(8) Uani 1 1 d . . . . .
H3 H -0.0650 0.4861 0.3778 0.067 Uiso 1 1 calc R . . . .
C4 C 0.1025(4) 0.46326(17) 0.48545(19) 0.0524(8) Uani 1 1 d . . . . .
C5 C 0.1831(4) 0.51823(18) 0.5072(2) 0.0592(9) Uani 1 1 d . . . . .
H5 H 0.1481 0.5499 0.4727 0.071 Uiso 1 1 calc R . . . .
C6 C 0.3118(4) 0.52625(19) 0.5776(2) 0.0611(9) Uani 1 1 d . . . . .
C7 C 0.3634(4) 0.4773(2) 0.6285(2) 0.0635(9) Uani 1 1 d . . . . .
H7 H 0.4518 0.4817 0.6762 0.076 Uiso 1 1 calc R . . . .
C8 C 0.2878(4) 0.4236(2) 0.6103(2) 0.0612(9) Uani 1 1 d . . . . .
H8 H 0.3247 0.3924 0.6455 0.073 Uiso 1 1 calc R . . . .
C9 C 0.1539(3) 0.41530(17) 0.53813(18) 0.0506(8) Uani 1 1 d . . . . .
C10 C 0.0670(4) 0.36205(16) 0.51520(18) 0.0500(8) Uani 1 1 d . . . . .
C11 C -0.0621(4) 0.35339(17) 0.44383(18) 0.0512(8) Uani 1 1 d . . . . .
C12 C -0.1322(4) 0.29360(18) 0.4278(2) 0.0605(9) Uani 1 1 d . . . . .
H12 H -0.2056 0.2806 0.3793 0.073 Uiso 1 1 calc R . . . .
C13 C -0.0914(4) 0.25751(18) 0.4825(2) 0.0625(9) Uani 1 1 d . . . . .
H13 H -0.1352 0.2188 0.4720 0.075 Uiso 1 1 calc R . . . .
C14 C 0.0245(4) 0.27828(16) 0.5612(2) 0.0554(8) Uani 1 1 d . . . . .
C15 C -0.0290(4) 0.31694(17) 0.5881(2) 0.0622(9) Uani 1 1 d . . . . .
C16 C -0.1654(6) 0.3100(2) 0.5566(3) 0.0822(13) Uani 1 1 d . . . . .
H16 H -0.2287 0.2847 0.5153 0.099 Uiso 1 1 calc R . . . .
C17 C -0.2084(8) 0.3409(3) 0.5865(5) 0.117(2) Uani 1 1 d . . . . .
H17 H -0.2994 0.3353 0.5662 0.140 Uiso 1 1 calc R . . . .
C18 C -0.1140(10) 0.3800(3) 0.6467(5) 0.124(3) Uani 1 1 d . . . . .
H18 H -0.1424 0.4014 0.6665 0.149 Uiso 1 1 calc R . . . .
C19 C 0.0191(9) 0.3874(3) 0.6771(4) 0.1084(19) Uani 1 1 d . . . . .
H19 H 0.0812 0.4140 0.7174 0.130 Uiso 1 1 calc R . . . .
C20 C 0.0638(6) 0.3560(2) 0.6488(3) 0.0788(12) Uani 1 1 d . . . . .
H20 H 0.1558 0.3611 0.6703 0.095 Uiso 1 1 calc R . . . .
C21 C 0.1082(4) 0.22159(17) 0.6117(2) 0.0612(9) Uani 1 1 d . . . . .
C22 C 0.2146(6) 0.1963(2) 0.6213(4) 0.1010(17) Uani 1 1 d . . . . .
H22 H 0.2378 0.2140 0.5974 0.121 Uiso 1 1 calc R . . . .
C23 C 0.2887(7) 0.1443(3) 0.6667(5) 0.133(3) Uani 1 1 d . . . . .
H23 H 0.3633 0.1283 0.6742 0.159 Uiso 1 1 calc R . . . .
C24 C 0.2541(7) 0.1165(3) 0.7001(3) 0.115(2) Uani 1 1 d . . . . .
H24 H 0.3034 0.0813 0.7298 0.138 Uiso 1 1 calc R . . . .
C25 C 0.1490(9) 0.1402(3) 0.6901(4) 0.123(2) Uani 1 1 d . . . . .
H25 H 0.1232 0.1209 0.7121 0.148 Uiso 1 1 calc R . . . .
C26 C 0.0773(7) 0.1933(2) 0.6470(3) 0.0962(16) Uani 1 1 d . . . . .
H26 H 0.0063 0.2100 0.6422 0.115 Uiso 1 1 calc R . . . .
C27 C 0.3947(5) 0.5868(2) 0.6014(3) 0.0807(12) Uani 1 1 d . . . . .
H27A H 0.4045 0.5963 0.5682 0.121 Uiso 1 1 calc GR . . . .
H27B H 0.4865 0.5818 0.6503 0.121 Uiso 1 1 calc GR . . . .
H27C H 0.3458 0.6206 0.6008 0.121 Uiso 1 1 calc GR . . . .
C28 C -0.4074(4) 0.4442(2) 0.1957(2) 0.0683(10) Uani 1 1 d . . . . .
H28A H -0.4614 0.4067 0.1844 0.082 Uiso 1 1 calc R . . . .
H28B H -0.3974 0.4464 0.1614 0.082 Uiso 1 1 calc R . . . .
C29 C -0.4832(4) 0.5006(2) 0.1870(2) 0.0739(12) Uani 1 1 d . . . . .
H29A H -0.4281 0.5379 0.1992 0.089 Uiso 1 1 calc R . . . .
H29B H -0.4938 0.4981 0.2210 0.089 Uiso 1 1 calc R . . . .
C30 C -0.6280(4) 0.50661(17) 0.10898(18) 0.0560(8) Uani 1 1 d . . . . .
H30A H -0.6874 0.4729 0.1006 0.067 Uiso 1 1 calc R . . . .
H30B H -0.6179 0.5005 0.0750 0.067 Uiso 1 1 calc R . . . .
C31 C -0.7041(4) 0.56993(17) 0.09065(18) 0.0528(8) Uani 1 1 d . . . . .
C32 C -0.7191(4) 0.58563(17) 0.14341(19) 0.0537(8) Uani 1 1 d . . . . .
C33 C -0.7944(4) 0.55465(18) 0.1542(2) 0.0623(9) Uani 1 1 d . . . . .
H33 H -0.8441 0.5181 0.1280 0.075 Uiso 1 1 calc R . . . .
C34 C -0.7953(4) 0.5787(2) 0.2048(2) 0.0687(10) Uani 1 1 d . . . . .
C35 C -0.7205(5) 0.6327(2) 0.2444(3) 0.0735(11) Uani 1 1 d . . . . .
H35 H -0.7217 0.6480 0.2782 0.088 Uiso 1 1 calc R . . . .
C36 C -0.6439(4) 0.6641(2) 0.2341(2) 0.0674(10) Uani 1 1 d . . . . .
H36 H -0.5926 0.7001 0.2613 0.081 Uiso 1 1 calc R . . . .
C37 C -0.6448(4) 0.64129(17) 0.18278(19) 0.0555(8) Uani 1 1 d . . . . .
C38 C -0.5800(4) 0.66570(18) 0.15844(19) 0.0562(8) Uani 1 1 d . . . . .
C39 C -0.5006(4) 0.7192(2) 0.1777(2) 0.0689(10) Uani 1 1 d . . . . .
H39 H -0.4780 0.7466 0.2133 0.083 Uiso 1 1 calc R . . . .
C40 C -0.4550(5) 0.7315(2) 0.1437(2) 0.0726(11) Uani 1 1 d . . . . .
H40 H -0.4032 0.7678 0.1557 0.087 Uiso 1 1 calc R . . . .
C41 C -0.4860(4) 0.6901(2) 0.0917(2) 0.0644(10) Uani 1 1 d . . . . .
C42 C -0.5651(4) 0.63603(19) 0.0722(2) 0.0602(9) Uani 1 1 d . . . . .
H42 H -0.5843 0.6080 0.0380 0.072 Uiso 1 1 calc R . . . .
C43 C -0.6147(4) 0.62466(17) 0.10427(18) 0.0531(8) Uani 1 1 d . . . . .
C44 C -0.8483(4) 0.56792(19) 0.0103(2) 0.0659(10) Uani 1 1 d . . . . .
H44A H -0.8345 0.5639 -0.0219 0.099 Uiso 1 1 calc GR . . . .
H44B H -0.8990 0.6061 -0.0009 0.099 Uiso 1 1 calc GR . . . .
H44C H -0.9014 0.5325 0.0037 0.099 Uiso 1 1 calc GR . . . .
C45 C -0.3036(5) 0.7237(2) 0.0926(3) 0.0784(12) Uani 1 1 d . . . . .
C46 C -0.1811(6) 0.7244(3) 0.1673(3) 0.0973(17) Uani 1 1 d . . . . .
H46 H -0.1819 0.7134 0.2024 0.117 Uiso 1 1 calc R . . . .
C47 C -0.0590(7) 0.7420(4) 0.1870(4) 0.122(2) Uani 1 1 d . . . . .
H47 H 0.0247 0.7422 0.2366 0.146 Uiso 1 1 calc R . . . .
C48 C -0.0558(8) 0.7594(4) 0.1360(4) 0.135(3) Uani 1 1 d . . . . .
H48 H 0.0288 0.7721 0.1517 0.162 Uiso 1 1 calc R . . . .
C49 C -0.1741(8) 0.7581(4) 0.0636(4) 0.121(2) Uani 1 1 d . . . . .
H49 H -0.1711 0.7699 0.0294 0.145 Uiso 1 1 calc R . . . .
C50 C -0.3011(6) 0.7390(3) 0.0400(3) 0.0881(14) Uani 1 1 d . . . . .
C51 C -0.4418(6) 0.7266(2) -0.0315(3) 0.0795(12) Uani 1 1 d . . . . .
C52 C -0.5030(7) 0.7308(3) -0.1034(3) 0.0955(16) Uani 1 1 d . . . . .
H52 H -0.4513 0.7461 -0.1129 0.115 Uiso 1 1 calc R . . . .
C53 C -0.6396(7) 0.7122(3) -0.1600(3) 0.0957(17) Uani 1 1 d . . . . .
H53 H -0.6807 0.7146 -0.2081 0.115 Uiso 1 1 calc R . . . .
C54 C -0.7173(6) 0.6900(2) -0.1465(3) 0.0905(15) Uani 1 1 d . . . . .
H54 H -0.8100 0.6773 -0.1860 0.109 Uiso 1 1 calc R . . . .
C55 C -0.6611(5) 0.6858(2) -0.0756(2) 0.0793(12) Uani 1 1 d . . . . .
H55 H -0.7147 0.6714 -0.0669 0.095 Uiso 1 1 calc R . . . .
C56 C -0.5225(5) 0.7041(2) -0.0187(2) 0.0704(11) Uani 1 1 d . . . . .
C57 C -1.0227(5) 0.5453(2) 0.1614(3) 0.1510(12) Uani 1 1 d . . . . .
C58 C -1.1166(6) 0.5789(2) 0.0959(3) 0.1510(12) Uani 1 1 d G . . . .
H58 H -1.0828 0.6056 0.0820 0.181 Uiso 1 1 calc R . . . .
C59 C -1.2611(6) 0.5728(2) 0.0512(3) 0.1510(12) Uani 1 1 d G . . . .
H59 H -1.3239 0.5953 0.0073 0.181 Uiso 1 1 calc R . . . .
C60 C -1.3116(5) 0.5330(2) 0.0719(3) 0.1510(12) Uani 1 1 d G . . . .
H60 H -1.4083 0.5289 0.0419 0.181 Uiso 1 1 calc R . . . .
C61 C -1.2177(6) 0.4994(2) 0.1374(3) 0.1510(12) Uani 1 1 d G . . . .
H61 H -1.2515 0.4727 0.1513 0.181 Uiso 1 1 calc R . . . .
C62 C -1.0732(6) 0.5055(2) 0.1822(3) 0.1510(12) Uani 1 1 d G . . . .
C68 C -0.8373(7) 0.5100(2) 0.2679(3) 0.1510(12) Uani 1 1 d . . . . .
C67 C -0.7012(6) 0.4984(2) 0.3354(4) 0.1510(12) Uani 1 1 d G . . . .
H67 H -0.6244 0.5165 0.3464 0.181 Uiso 1 1 calc R . . . .
C66 C -0.6800(5) 0.4597(2) 0.3866(3) 0.1510(12) Uani 1 1 d G . . . .
H66 H -0.5889 0.4519 0.4318 0.181 Uiso 1 1 calc R . . . .
C65 C -0.7948(6) 0.4326(2) 0.3703(3) 0.1510(12) Uani 1 1 d G . . . .
H65 H -0.7805 0.4068 0.4045 0.181 Uiso 1 1 calc R . . . .
C64 C -0.9308(6) 0.4443(2) 0.3027(4) 0.1510(12) Uani 1 1 d G . . . .
H64 H -1.0076 0.4262 0.2918 0.181 Uiso 1 1 calc R . . . .
C63 C -0.9521(5) 0.4830(3) 0.2515(3) 0.1510(12) Uani 1 1 d G . . . .


_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 C1 1.338(5) . ?
O1 C28 1.446(4) . ?
O2 C1 1.194(5) . ?
O3 C10 1.377(4) . ?
O3 C14 1.452(4) . ?
N1 C41 1.419(5) . ?
N1 C45 1.395(6) . ?
N1 C56 1.399(5) . ?
N2 C34 1.414(5) . ?
N2 C57 1.363(6) . ?
N2 C68 1.358(6) . ?
C1 C2 1.490(5) . ?
C2 C3 1.359(5) . ?
C2 C11 1.437(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.419(5) . ?
C4 C5 1.407(5) . ?
C4 C9 1.420(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.369(6) . ?
C6 C7 1.407(6) . ?
C6 C27 1.514(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.366(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.412(5) . ?
C9 C10 1.416(5) . ?
C10 C11 1.383(5) . ?
C11 C12 1.452(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.326(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.504(5) . ?
C14 C15 1.523(5) . ?
C14 C21 1.526(5) . ?
C15 C16 1.381(6) . ?
C15 C20 1.388(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.389(8) . ?
C17 H17 0.9300 . ?
C17 C18 1.386(10) . ?
C18 H18 0.9300 . ?
C18 C19 1.353(10) . ?
C19 H19 0.9300 . ?
C19 C20 1.380(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.361(6) . ?
C21 C26 1.360(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.389(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.350(10) . ?
C24 H24 0.9300 . ?
C24 C25 1.327(10) . ?
C25 H25 0.9300 . ?
C25 C26 1.383(7) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.476(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.520(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.543(5) . ?
C31 C32 1.523(5) . ?
C31 C43 1.516(5) . ?
C31 C44 1.538(5) . ?
C32 C33 1.373(5) . ?
C32 C37 1.409(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.392(6) . ?
C34 C35 1.382(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.383(6) . ?
C36 H36 0.9300 . ?
C36 C37 1.383(5) . ?
C37 C38 1.460(5) . ?
C38 C39 1.384(5) . ?
C38 C43 1.407(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.383(6) . ?
C40 H40 0.9300 . ?
C40 C41 1.387(6) . ?
C41 C42 1.391(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.380(5) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.389(7) . ?
C45 C50 1.399(6) . ?
C46 H46 0.9300 . ?
C46 C47 1.368(8) . ?
C47 H47 0.9300 . ?
C47 C48 1.377(9) . ?
C48 H48 0.9300 . ?
C48 C49 1.346(9) . ?
C49 H49 0.9300 . ?
C49 C50 1.396(8) . ?
C50 C51 1.452(7) . ?
C51 C52 1.390(7) . ?
C51 C56 1.401(6) . ?
C52 H52 0.9300 . ?
C52 C53 1.364(8) . ?
C53 H53 0.9300 . ?
C53 C54 1.375(8) . ?
C54 H54 0.9300 . ?
C54 C55 1.391(7) . ?
C55 H55 0.9300 . ?
C55 C56 1.380(7) . ?
C57 C58 1.3900 . ?
C57 C62 1.3900 . ?
C58 H58 0.9300 . ?
C58 C59 1.3900 . ?
C59 H59 0.9300 . ?
C59 C60 1.3900 . ?
C60 H60 0.9300 . ?
C60 C61 1.3900 . ?
C61 H61 0.9300 . ?
C61 C62 1.3900 . ?
C62 C63 1.399(7) . ?
C68 C67 1.3900 . ?
C68 C63 1.3900 . ?
C67 H67 0.9300 . ?
C67 C66 1.3900 . ?
C66 H66 0.9300 . ?
C66 C65 1.3900 . ?
C65 H65 0.9300 . ?
C65 C64 1.3900 . ?
C64 H64 0.9300 . ?
C64 C63 1.3900 . ?

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
C1 O1 C28 117.5(3) . . ?
C10 O3 C14 116.0(3) . . ?
C45 N1 C41 125.7(4) . . ?
C45 N1 C56 108.1(4) . . ?
C56 N1 C41 125.9(4) . . ?
C57 N2 C34 126.6(5) . . ?
C68 N2 C34 128.7(5) . . ?
C68 N2 C57 104.4(4) . . ?
O1 C1 C2 112.2(3) . . ?
O2 C1 O1 121.6(4) . . ?
O2 C1 C2 126.2(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 C11 120.4(3) . . ?
C11 C2 C1 120.0(3) . . ?
C2 C3 H3 118.9 . . ?
C2 C3 C4 122.1(3) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C9 118.7(3) . . ?
C5 C4 C3 121.9(3) . . ?
C5 C4 C9 119.4(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C7 118.1(4) . . ?
C5 C6 C27 121.4(4) . . ?
C7 C6 C27 120.5(4) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 C6 122.2(4) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 C4 118.3(3) . . ?
C8 C9 C10 123.8(3) . . ?
C10 C9 C4 117.9(3) . . ?
O3 C10 C9 115.4(3) . . ?
O3 C10 C11 121.1(3) . . ?
C11 C10 C9 123.4(3) . . ?
C2 C11 C12 126.0(3) . . ?
C10 C11 C2 117.4(3) . . ?
C10 C11 C12 116.5(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 120.9(4) . . ?
C14 C13 H13 119.5 . . ?
O3 C14 C13 108.4(3) . . ?
O3 C14 C15 109.0(3) . . ?
O3 C14 C21 105.6(3) . . ?
C13 C14 C15 113.0(3) . . ?
C13 C14 C21 110.7(3) . . ?
C15 C14 C21 109.9(3) . . ?
C16 C15 C14 121.0(4) . . ?
C16 C15 C20 119.4(4) . . ?
C20 C15 C14 119.4(4) . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.3(6) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.1(6) . . ?
C18 C17 H17 120.4 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(6) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.7(6) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 H20 120.1 . . ?
C19 C20 C15 119.8(6) . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C14 121.0(4) . . ?
C22 C21 C26 117.3(4) . . ?
C26 C21 C14 121.6(4) . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.3(6) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 119.5 . . ?
C24 C23 C22 121.0(6) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 120.4 . . ?
C25 C24 C23 119.1(5) . . ?
C25 C24 H24 120.4 . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.5(7) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 121.6(6) . . ?
C21 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C6 C27 H27A 109.5 . . ?
C6 C27 H27B 109.5 . . ?
C6 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 H28A 109.5 . . ?
O1 C28 H28B 109.5 . . ?
O1 C28 C29 110.7(3) . . ?
H28A C28 H28B 108.1 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C28 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
C28 C29 C30 111.7(3) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C29 C30 H30A 108.4 . . ?
C29 C30 H30B 108.4 . . ?
C29 C30 C31 115.4(3) . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 H30A 108.4 . . ?
C31 C30 H30B 108.4 . . ?
C32 C31 C30 112.6(3) . . ?
C32 C31 C44 111.6(3) . . ?
C43 C31 C30 110.8(3) . . ?
C43 C31 C32 101.2(3) . . ?
C43 C31 C44 111.9(3) . . ?
C44 C31 C30 108.7(3) . . ?
C33 C32 C31 129.1(3) . . ?
C33 C32 C37 120.2(3) . . ?
C37 C32 C31 110.6(3) . . ?
C32 C33 H33 120.5 . . ?
C32 C33 C34 119.1(4) . . ?
C34 C33 H33 120.5 . . ?
C33 C34 N2 118.4(4) . . ?
C35 C34 N2 120.9(4) . . ?
C35 C34 C33 120.7(4) . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.6(4) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 120.5 . . ?
C37 C36 C35 119.0(4) . . ?
C37 C36 H36 120.5 . . ?
C32 C37 C38 108.8(3) . . ?
C36 C37 C32 120.3(4) . . ?
C36 C37 C38 131.0(3) . . ?
C39 C38 C37 131.9(3) . . ?
C39 C38 C43 120.1(3) . . ?
C43 C38 C37 108.0(3) . . ?
C38 C39 H39 120.3 . . ?
C40 C39 C38 119.3(4) . . ?
C40 C39 H39 120.3 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.5(4) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 N1 119.8(4) . . ?
C40 C41 C42 120.7(4) . . ?
C42 C41 N1 119.5(4) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 C41 119.0(3) . . ?
C43 C42 H42 120.5 . . ?
C38 C43 C31 111.5(3) . . ?
C42 C43 C31 128.2(3) . . ?
C42 C43 C38 120.3(3) . . ?
C31 C44 H44A 109.5 . . ?
C31 C44 H44B 109.5 . . ?
C31 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N1 C45 C50 109.3(4) . . ?
C46 C45 N1 129.3(4) . . ?
C46 C45 C50 121.1(4) . . ?
C45 C46 H46 121.4 . . ?
C47 C46 C45 117.3(5) . . ?
C47 C46 H46 121.4 . . ?
C46 C47 H47 118.9 . . ?
C46 C47 C48 122.3(6) . . ?
C48 C47 H47 118.9 . . ?
C47 C48 H48 119.7 . . ?
C49 C48 C47 120.6(6) . . ?
C49 C48 H48 119.7 . . ?
C48 C49 H49 120.1 . . ?
C48 C49 C50 119.7(6) . . ?
C50 C49 H49 120.1 . . ?
C45 C50 C51 106.6(4) . . ?
C49 C50 C45 118.9(5) . . ?
C49 C50 C51 134.3(5) . . ?
C52 C51 C50 133.8(5) . . ?
C52 C51 C56 119.2(5) . . ?
C56 C51 C50 107.0(4) . . ?
C51 C52 H52 120.3 . . ?
C53 C52 C51 119.5(5) . . ?
C53 C52 H52 120.3 . . ?
C52 C53 H53 119.7 . . ?
C52 C53 C54 120.7(5) . . ?
C54 C53 H53 119.7 . . ?
C53 C54 H54 119.0 . . ?
C53 C54 C55 121.9(5) . . ?
C55 C54 H54 119.0 . . ?
C54 C55 H55 121.5 . . ?
C56 C55 C54 117.0(5) . . ?
C56 C55 H55 121.5 . . ?
N1 C56 C51 108.9(4) . . ?
C55 C56 N1 129.4(4) . . ?
C55 C56 C51 121.8(4) . . ?
N2 C57 C58 127.2(4) . . ?
N2 C57 C62 112.7(4) . . ?
C58 C57 C62 120.0 . . ?
C57 C58 H58 120.0 . . ?
C59 C58 C57 120.0 . . ?
C59 C58 H58 120.0 . . ?
C58 C59 H59 120.0 . . ?
C60 C59 C58 120.0 . . ?
C60 C59 H59 120.0 . . ?
C59 C60 H60 120.0 . . ?
C59 C60 C61 120.0 . . ?
C61 C60 H60 120.0 . . ?
C60 C61 H61 120.0 . . ?
C62 C61 C60 120.0 . . ?
C62 C61 H61 120.0 . . ?
C57 C62 C63 104.6(4) . . ?
C61 C62 C57 120.0 . . ?
C61 C62 C63 135.3(4) . . ?
N2 C68 C67 128.4(4) . . ?
N2 C68 C63 111.5(4) . . ?
C67 C68 C63 120.0 . . ?
C68 C67 H67 120.0 . . ?
C66 C67 C68 120.0 . . ?
C66 C67 H67 120.0 . . ?
C67 C66 H66 120.0 . . ?
C65 C66 C67 120.0 . . ?
C65 C66 H66 120.0 . . ?
C66 C65 H65 120.0 . . ?
C66 C65 C64 120.0 . . ?
C64 C65 H65 120.0 . . ?
C65 C64 H64 120.0 . . ?
C63 C64 C65 120.0 . . ?
C63 C64 H64 120.0 . . ?
C68 C63 C62 106.7(4) . . ?
C64 C63 C62 133.2(4) . . ?
C64 C63 C68 120.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'


