# Electronic Supplementary Material (ESI) for RSC Advances.
# 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).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Please retain this information to preserve the provenance of 
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data_srs33mqz_sq_s
_database_code_depnum_ccdc_archive 'CCDC 1457935'
_audit_update_record             
;
2016-03-04 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;
_audit_creation_date             2013-11-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C48 H34 N6 O2'
_chemical_formula_sum            'C48 H34 N6 O2'
_chemical_formula_weight         726.81
_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           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.711(5)
_cell_length_b                   8.983(2)
_cell_length_c                   26.520(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4695.7(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.639
_cell_measurement_theta_min      2.607
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 5 sets of ω and φ scans each set at different φ and/or
 ω angles and each scan (15 s exposure) covering -0.300° degrees.
 The crystal to detector distance was 4.956 cm.
;
_diffrn_reflns_av_R_equivalents  0.1417
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45741
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.539
_diffrn_reflns_theta_min         1.536
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_current           37.0
_diffrn_source_power             1.739
_diffrn_source_target            Mo
_diffrn_source_voltage           47.0
_reflns_number_gt                2052
_reflns_number_total             3087
_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       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0596
_refine_ls_restrained_S_all      1.080
_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)+(0.0974P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1868
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-H1 \\sim N2-H2
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C19(H19),
 C20(H20), C22(H22), C23(H23)
;
_atom_sites_solution_hydrogens   mixed
_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 0.74584(11) 0.6500(3) -0.00937(9) 0.0466(7) Uani 1 1 d . . . . .
N1 N 0.79190(15) 0.4419(4) 0.02503(12) 0.0494(9) Uani 1 1 d D . . . .
H1 H 0.7896(18) 0.346(4) 0.0319(14) 0.060(13) Uiso 1 1 d D . . . .
N2 N 0.69196(15) 0.4292(4) -0.01985(12) 0.0480(8) Uani 1 1 d D . . . .
H2 H 0.6984(19) 0.331(4) -0.0173(14) 0.067(13) Uiso 1 1 d D . . . .
N3 N 0.34035(15) 0.9279(3) 0.16822(11) 0.0502(8) Uani 1 1 d . . . . .
C1 C 0.74336(17) 0.5126(4) -0.00218(14) 0.0430(9) Uani 1 1 d . . . . .
C2 C 0.63743(16) 0.4998(4) -0.04825(15) 0.0480(10) Uani 1 1 d . . . . .
H2A H 0.6105 0.4217 -0.0654 0.058 Uiso 1 1 calc R U . . .
H2B H 0.6575 0.5643 -0.0746 0.058 Uiso 1 1 calc R U . . .
C3 C 0.59056(16) 0.5925(4) -0.01589(14) 0.0398(9) Uani 1 1 d . . . . .
C4 C 0.55223(16) 0.7053(4) -0.03775(14) 0.0443(9) Uani 1 1 d . . . . .
H4 H 0.5559 0.7238 -0.0729 0.053 Uiso 1 1 calc R U . . .
C5 C 0.50880(17) 0.7910(4) -0.00866(14) 0.0456(10) Uani 1 1 d . . . . .
H5 H 0.4834 0.8685 -0.0241 0.055 Uiso 1 1 calc R U . . .
C6 C 0.50179(16) 0.7654(4) 0.04255(15) 0.0413(9) Uani 1 1 d . . . . .
C7 C 0.53952(18) 0.6525(4) 0.06445(14) 0.0499(10) Uani 1 1 d . . . . .
H7 H 0.5350 0.6323 0.0995 0.060 Uiso 1 1 calc R U . . .
C8 C 0.58409(17) 0.5684(4) 0.03516(15) 0.0480(10) Uani 1 1 d . . . . .
H8 H 0.6105 0.4929 0.0508 0.058 Uiso 1 1 calc R U . . .
C9 C 0.45428(18) 0.8497(4) 0.07212(14) 0.0466(10) Uani 1 1 d . . . . .
C10 C 0.41189(18) 0.9149(4) 0.09650(14) 0.0481(10) Uani 1 1 d . . . . .
C11 C 0.35639(17) 0.9870(4) 0.12291(14) 0.0455(10) Uani 1 1 d . . . . .
C12 C 0.32127(18) 1.1026(4) 0.10116(14) 0.0490(10) Uani 1 1 d . . . . .
H12 H 0.3348 1.1414 0.0694 0.059 Uiso 1 1 calc R U . . .
C13 C 0.26626(19) 1.1613(5) 0.12613(15) 0.0534(10) Uani 1 1 d . . . . .
H13 H 0.2417 1.2421 0.1119 0.064 Uiso 1 1 calc R U . . .
C14 C 0.2472(2) 1.1022(5) 0.17161(15) 0.0544(11) Uani 1 1 d . . . . .
H14 H 0.2086 1.1394 0.1890 0.065 Uiso 1 1 calc R U . . .
C15 C 0.28517(19) 0.9877(5) 0.19164(14) 0.0510(10) Uani 1 1 d . . . . .
C16 C 0.2657(2) 0.9183(5) 0.23806(15) 0.0565(11) Uani 1 1 d . . . . .
C17 C 0.2455(2) 0.8566(5) 0.27538(16) 0.0595(11) Uani 1 1 d . . . . .
C18 C 0.2232(2) 0.7755(4) 0.31959(14) 0.0519(10) Uani 1 1 d . . . . .
C19 C 0.1569(2) 0.7931(5) 0.33891(15) 0.0582(11) Uani 1 1 d . . . . .
H19 H 0.1262 0.8600 0.3231 0.070 Uiso 1 1 calc R U . . .
C20 C 0.13682(19) 0.7132(4) 0.38055(14) 0.0525(10) Uani 1 1 d . . . . .
H20 H 0.0922 0.7264 0.3934 0.063 Uiso 1 1 calc R U . . .
C21 C 0.18046(17) 0.6135(4) 0.40431(13) 0.0426(9) Uani 1 1 d . . . . .
C22 C 0.24551(19) 0.5985(4) 0.38518(14) 0.0541(10) Uani 1 1 d . . . . .
H22 H 0.2765 0.5322 0.4010 0.065 Uiso 1 1 calc R U . . .
C23 C 0.2660(2) 0.6787(5) 0.34340(14) 0.0567(11) Uani 1 1 d . . . . .
H23 H 0.3108 0.6662 0.3309 0.068 Uiso 1 1 calc R U . . .
C24 C 0.15611(16) 0.5257(4) 0.44905(15) 0.0494(10) Uani 1 1 d . . . . .
H24A H 0.1349 0.5952 0.4734 0.059 Uiso 1 1 calc R U . . .
H24B H 0.1205 0.4557 0.4376 0.059 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.250(4) . ?
N1 H1 0.88(3) . ?
N1 C1 1.356(5) . ?
N1 C24 1.445(4) 3_655 ?
N2 H2 0.89(3) . ?
N2 C1 1.344(4) . ?
N2 C2 1.458(4) . ?
N3 C11 1.351(4) . ?
N3 C15 1.363(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.511(5) . ?
C3 C4 1.391(5) . ?
C3 C8 1.377(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(5) . ?
C6 C7 1.385(5) . ?
C6 C9 1.437(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.395(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.208(5) . ?
C10 C11 1.452(5) . ?
C11 C12 1.375(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.375(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.370(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(5) . ?
C15 C16 1.432(5) . ?
C16 C17 1.203(5) . ?
C17 C18 1.448(6) . ?
C18 C19 1.412(5) . ?
C18 C23 1.366(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.375(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.393(5) . ?
C21 C22 1.386(5) . ?
C21 C24 1.503(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(5) . ?
C23 H23 0.9500 . ?
C24 N1 1.446(4) 3_655 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 H1 122(2) . . ?
C1 N1 C24 120.6(3) . 3_655 ?
C24 N1 H1 117(2) 3_655 . ?
C1 N2 H2 115(3) . . ?
C1 N2 C2 119.6(3) . . ?
C2 N2 H2 125(3) . . ?
C11 N3 C15 116.0(3) . . ?
O1 C1 N1 121.1(3) . . ?
O1 C1 N2 121.8(3) . . ?
N2 C1 N1 117.2(3) . . ?
N2 C2 H2A 108.9 . . ?
N2 C2 H2B 108.9 . . ?
N2 C2 C3 113.4(3) . . ?
H2A C2 H2B 107.7 . . ?
C3 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C4 C3 C2 119.8(3) . . ?
C8 C3 C2 121.9(3) . . ?
C8 C3 C4 118.3(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C7 118.6(3) . . ?
C5 C6 C9 120.9(3) . . ?
C7 C6 C9 120.5(4) . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.1(4) . . ?
C8 C7 H7 120.0 . . ?
C3 C8 C7 121.4(3) . . ?
C3 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C6 176.6(4) . . ?
C9 C10 C11 174.8(4) . . ?
N3 C11 C10 115.5(3) . . ?
N3 C11 C12 123.5(3) . . ?
C12 C11 C10 120.9(3) . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C13 119.0(4) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 120.7 . . ?
C13 C14 C15 118.6(4) . . ?
C15 C14 H14 120.7 . . ?
N3 C15 C14 123.5(4) . . ?
N3 C15 C16 115.7(4) . . ?
C14 C15 C16 120.7(4) . . ?
C17 C16 C15 175.5(4) . . ?
C16 C17 C18 177.0(5) . . ?
C19 C18 C17 121.2(4) . . ?
C23 C18 C17 120.5(4) . . ?
C23 C18 C19 118.3(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0(4) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.4(3) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C24 119.8(3) . . ?
C22 C21 C20 117.9(3) . . ?
C22 C21 C24 122.2(3) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.9(4) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 121.5(4) . . ?
C18 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
N1 C24 C21 115.0(3) 3_655 . ?
N1 C24 H24A 108.5 3_655 . ?
N1 C24 H24B 108.5 3_655 . ?
C21 C24 H24A 108.5 . . ?
C21 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.88(3) 2.19(4) 2.874(4) 134(3) 8_755
N2 H2 O1 0.89(3) 1.97(3) 2.806(4) 154(4) 8_755

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C3 C4 157.5(3) . . . . ?
N2 C2 C3 C8 -22.8(4) . . . . ?
N3 C11 C12 C13 -0.8(6) . . . . ?
C1 N2 C2 C3 -72.5(4) . . . . ?
C2 N2 C1 O1 0.1(5) . . . . ?
C2 N2 C1 N1 178.5(3) . . . . ?
C2 C3 C4 C5 179.8(3) . . . . ?
C2 C3 C8 C7 -178.5(3) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C4 C3 C8 C7 1.1(5) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C4 C5 C6 C9 -177.0(3) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
C6 C7 C8 C3 -1.6(5) . . . . ?
C8 C3 C4 C5 0.1(5) . . . . ?
C9 C6 C7 C8 178.2(3) . . . . ?
C10 C11 C12 C13 175.8(3) . . . . ?
C11 N3 C15 C14 -0.5(5) . . . . ?
C11 N3 C15 C16 176.1(3) . . . . ?
C11 C12 C13 C14 -0.9(6) . . . . ?
C12 C13 C14 C15 1.7(6) . . . . ?
C13 C14 C15 N3 -1.1(6) . . . . ?
C13 C14 C15 C16 -177.5(4) . . . . ?
C15 N3 C11 C10 -175.3(3) . . . . ?
C15 N3 C11 C12 1.5(5) . . . . ?
C17 C18 C19 C20 179.2(4) . . . . ?
C17 C18 C23 C22 -179.0(4) . . . . ?
C18 C19 C20 C21 -0.4(6) . . . . ?
C19 C18 C23 C22 0.4(6) . . . . ?
C19 C20 C21 C22 1.0(5) . . . . ?
C19 C20 C21 C24 -178.6(3) . . . . ?
C20 C21 C22 C23 -0.9(5) . . . . ?
C20 C21 C24 N1 -171.7(3) . . . 3_655 ?
C21 C22 C23 C18 0.2(6) . . . . ?
C22 C21 C24 N1 8.7(5) . . . 3_655 ?
C23 C18 C19 C20 -0.3(6) . . . . ?
C24 N1 C1 O1 6.6(5) 3_655 . . . ?
C24 N1 C1 N2 -171.8(3) 3_655 . . . ?
C24 C21 C22 C23 178.7(3) . . . . ?

_vrf_PLAT023_srs33mqz_sq_s       
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.54 Deg.  
RESPONSE: Weakly diffracting needle crystal. No diffraction observed 
above a 2-theta value of ca. 45 degrees, and the data were truncated
there.
;
_vrf_PLAT027_srs33mqz_sq_s       
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      22.50 Deg.  
RESPONSE: Weakly diffracting needle crystal. No diffraction observed 
above a 2-theta value of ca. 45 degrees, and the data were truncated
there.
;
_vrf_THETM01_srs33mqz_sq_s       
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Weakly diffracting needle crystal. No diffraction observed 
above a 2-theta value of ca. 45 degrees, and the data were truncated
there.
;
####################################################################### 
# 
# 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_yx031_3m
_database_code_depnum_ccdc_archive 'CCDC 1463771'
_audit_update_record             
;
2016-03-10 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H56 N8 O2, C H2 Cl2'
_chemical_formula_sum            'C61 H58 Cl2 N8 O2'
_chemical_formula_weight         1006.05


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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'

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

_cell_length_a                   9.6662(4)
_cell_length_b                   18.8900(8)
_cell_length_c                   14.4567(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4640(10)
_cell_angle_gamma                90.00
_cell_volume                     2638.85(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3774
_cell_measurement_theta_min      2.505
_cell_measurement_theta_max      20.845

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1060
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28637
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         23.26
_reflns_number_total             3930
_reflns_number_gt                2476
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'

_refine_special_details          
; 
Heavy disorder of methylene chloride solvent and t-butyl groups 
Ten C-C same-distance restraints used for modeling t-butyl disorder 
  
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1545P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3930
_refine_ls_number_parameters     379
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0750
_refine_ls_wR_factor_ref         0.2410
_refine_ls_wR_factor_gt          0.2161
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0057(6) 0.7500 0.3967(5) 0.0611(15) Uani 1 2 d S . .
C2 C 1.0338(6) 0.6884(3) 0.2452(3) 0.0868(15) Uani 1 1 d . . .
H2A H 1.0849 0.6454 0.2266 0.104 Uiso 1 1 calc R . .
H2B H 0.9405 0.6864 0.2156 0.104 Uiso 1 1 calc R . .
C3 C 1.2609(7) 0.7500 0.2197(4) 0.0784(19) Uani 1 2 d SD . .
C4 C 1.3180(8) 0.7500 0.3193(4) 0.105(3) Uani 1 2 d SD . .
H4A H 1.2850 0.7921 0.3515 0.157 Uiso 0.50 1 calc PR . .
H4B H 1.4194 0.7504 0.3190 0.157 Uiso 1 2 calc SR . .
H4C H 1.2864 0.7074 0.3512 0.157 Uiso 0.50 1 calc PR . .
C5 C 1.3117(6) 0.6840(4) 0.1704(5) 0.145(3) Uani 1 1 d D . .
H5A H 1.2976 0.6424 0.2096 0.218 Uiso 1 1 calc R . .
H5B H 1.4104 0.6890 0.1580 0.218 Uiso 1 1 calc R . .
H5C H 1.2597 0.6781 0.1118 0.218 Uiso 1 1 calc R . .
C6 C 0.9997(4) 0.6223(2) 0.3956(3) 0.0736(13) Uani 1 1 d . . .
H6A H 1.0237 0.6293 0.4619 0.088 Uiso 1 1 calc R . .
H6B H 1.0637 0.5864 0.3711 0.088 Uiso 1 1 calc R . .
C7 C 0.8546(4) 0.5945(2) 0.3870(3) 0.0574(11) Uani 1 1 d . . .
C8 C 0.8253(5) 0.5259(2) 0.4148(3) 0.0681(12) Uani 1 1 d . . .
H8 H 0.8983 0.4969 0.4383 0.082 Uiso 1 1 calc R . .
C9 C 0.6943(5) 0.4993(2) 0.4091(3) 0.0676(12) Uani 1 1 d . . .
H9 H 0.6768 0.4528 0.4311 0.081 Uiso 1 1 calc R . .
C10 C 0.5869(4) 0.5390(2) 0.3719(3) 0.0562(10) Uani 1 1 d . . .
C11 C 0.6147(5) 0.6062(2) 0.3439(3) 0.0752(13) Uani 1 1 d . . .
H11 H 0.5418 0.6346 0.3187 0.090 Uiso 1 1 calc R . .
C12 C 0.7458(5) 0.6337(2) 0.3514(3) 0.0734(13) Uani 1 1 d . . .
H12 H 0.7618 0.6809 0.3315 0.088 Uiso 1 1 calc R . .
C13 C 0.4496(5) 0.5100(2) 0.3603(3) 0.0623(11) Uani 1 1 d . . .
C14 C 0.3355(5) 0.4858(2) 0.3458(3) 0.0610(11) Uani 1 1 d . . .
C15 C 0.2063(4) 0.4528(2) 0.3236(3) 0.0579(11) Uani 1 1 d . . .
C16 C 0.1668(5) 0.3898(2) 0.3644(3) 0.0701(12) Uani 1 1 d . . .
H16 H 0.2240 0.3683 0.4109 0.084 Uiso 1 1 calc R . .
C17 C 0.0441(6) 0.3589(2) 0.3368(4) 0.0827(14) Uani 1 1 d . . .
H17 H 0.0146 0.3160 0.3641 0.099 Uiso 1 1 calc R . .
C18 C -0.0344(5) 0.3910(2) 0.2696(3) 0.0781(13) Uani 1 1 d . . .
H18 H -0.1181 0.3697 0.2477 0.094 Uiso 1 1 calc R . .
C19 C 0.0091(4) 0.4558(2) 0.2328(3) 0.0607(11) Uani 1 1 d . . .
C20 C -0.0776(5) 0.4918(2) 0.1654(3) 0.0608(11) Uani 1 1 d . . .
C21 C -0.1559(4) 0.5174(2) 0.1106(3) 0.0587(11) Uani 1 1 d . . .
C22 C -0.2579(4) 0.5455(2) 0.0450(3) 0.0552(10) Uani 1 1 d . . .
C23 C -0.2878(5) 0.5101(2) -0.0363(3) 0.0643(12) Uani 1 1 d . . .
H23 H -0.2372 0.4688 -0.0517 0.077 Uiso 1 1 calc R . .
C24 C -0.3917(5) 0.5347(2) -0.0955(3) 0.0651(12) Uani 1 1 d . . .
H24 H -0.4130 0.5093 -0.1507 0.078 Uiso 1 1 calc R . .
C25 C -0.4646(4) 0.5949(2) -0.0763(2) 0.0534(10) Uani 1 1 d . . .
C26 C -0.4312(5) 0.6316(2) 0.0033(3) 0.0730(13) Uani 1 1 d . . .
H26 H -0.4787 0.6742 0.0167 0.088 Uiso 1 1 calc R . .
C27 C -0.3292(5) 0.6072(2) 0.0640(3) 0.0731(13) Uani 1 1 d . . .
H27 H -0.3078 0.6329 0.1190 0.088 Uiso 1 1 calc R . .
C28 C -0.5807(4) 0.6216(2) -0.1400(3) 0.0626(11) Uani 1 1 d . . .
H28A H -0.5990 0.5860 -0.1890 0.075 Uiso 1 1 calc R . .
H28B H -0.6659 0.6264 -0.1039 0.075 Uiso 1 1 calc R . .
C29 C -0.5950(5) 0.7500 -0.1444(4) 0.0530(14) Uani 1 2 d S . .
C30 C -0.4430(4) 0.68920(19) -0.2516(3) 0.0543(10) Uani 1 1 d . . .
H30A H -0.3517 0.6880 -0.2190 0.065 Uiso 1 1 calc R . .
H30B H -0.4514 0.6458 -0.2897 0.065 Uiso 1 1 calc R . .
C31 C -0.5563(5) 0.7500 -0.3885(3) 0.0563(14) Uani 1 2 d SD . .
C32 C -0.6960(7) 0.7154(4) -0.3638(6) 0.068(2) Uani 0.50 1 d PD A -2
H32A H -0.7409 0.7439 -0.3166 0.102 Uiso 0.50 1 calc PR A -2
H32B H -0.6792 0.6675 -0.3399 0.102 Uiso 0.50 1 calc PR A -2
H32C H -0.7560 0.7129 -0.4193 0.102 Uiso 0.50 1 calc PR A -2
C33 C -0.4917(10) 0.7008(4) -0.4625(5) 0.063(2) Uani 0.50 1 d PD A -2
H33A H -0.5595 0.6925 -0.5129 0.094 Uiso 0.50 1 calc PR A -2
H33B H -0.4657 0.6555 -0.4339 0.094 Uiso 0.50 1 calc PR A -2
H33C H -0.4093 0.7235 -0.4872 0.094 Uiso 0.50 1 calc PR A -2
C34 C -0.5819(11) 0.8219(3) -0.4299(6) 0.066(2) Uani 0.50 1 d PD A -2
H34A H -0.6248 0.8166 -0.4917 0.099 Uiso 0.50 1 calc PR A -2
H34B H -0.4937 0.8471 -0.4348 0.099 Uiso 0.50 1 calc PR A -2
H34C H -0.6437 0.8488 -0.3904 0.099 Uiso 0.50 1 calc PR A -2
N1 N 1.0205(4) 0.68857(17) 0.3469(2) 0.0699(10) Uani 1 1 d . . .
N2 N 1.1051(5) 0.7500 0.2130(4) 0.0747(15) Uani 1 2 d S . .
N3 N 0.1275(3) 0.48724(16) 0.2590(2) 0.0549(9) Uani 1 1 d . . .
N4 N -0.5513(3) 0.68882(16) -0.1831(2) 0.0541(8) Uani 1 1 d . . .
N5 N -0.4489(4) 0.7500 -0.3114(3) 0.0497(11) Uani 1 2 d S . .
O1 O 0.9830(4) 0.7500 0.4810(3) 0.0650(11) Uani 1 2 d S . .
O2 O -0.6783(4) 0.7500 -0.0795(3) 0.0726(12) Uani 1 2 d S . .
C1S C 1.0165(7) 0.7500 0.9724(6) 0.095(2) Uani 1 2 d S . .
H1SA H 1.0974 0.7656 0.9411 0.113 Uiso 0.50 1 d PR . .
H1SB H 1.0159 0.7718 1.0323 0.113 Uiso 0.50 1 d PR . .
Cl1 Cl 1.0186(3) 0.65637(16) 0.9837(2) 0.1126(10) Uani 0.50 1 d P . .
Cl2 Cl 0.8700(8) 0.7737(4) 0.9086(8) 0.131(3) Uani 0.25 1 d P . .
Cl3 Cl 0.876(2) 0.7854(11) 0.9847(17) 0.105(6) Uiso 0.07 1 d P . .
Cl4 Cl 0.957(3) 0.7698(13) 0.8646(14) 0.111(8) Uiso 0.07 1 d P . .
Cl5 Cl 0.904(2) 0.8147(10) 0.9054(12) 0.105(6) Uiso 0.10 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.244(7) . ?
C1 N1 1.375(5) . ?
C1 N1 1.375(5) 4_575 ?
C2 N2 1.436(5) . ?
C2 N1 1.479(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N2 1.506(8) . ?
C3 C5 1.524(5) . ?
C3 C5 1.524(5) 4_575 ?
C3 C4 1.529(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N1 1.452(5) . ?
C6 C7 1.499(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C12 1.376(6) . ?
C7 C8 1.387(5) . ?
C8 C9 1.364(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.361(6) . ?
C10 C13 1.442(7) . ?
C11 C12 1.372(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.207(6) . ?
C14 C15 1.424(6) . ?
C15 N3 1.357(5) . ?
C15 C16 1.385(6) . ?
C16 C17 1.372(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.360(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.404(6) . ?
C18 H18 0.9500 . ?
C19 N3 1.336(5) . ?
C19 C20 1.439(6) . ?
C20 C21 1.185(5) . ?
C21 C22 1.451(6) . ?
C22 C23 1.376(5) . ?
C22 C27 1.385(6) . ?
C23 C24 1.383(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.369(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(5) . ?
C25 C28 1.520(5) . ?
C26 C27 1.382(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 N4 1.445(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O2 1.253(6) . ?
C29 N4 1.356(4) 4_575 ?
C29 N4 1.356(4) . ?
C30 N5 1.438(4) . ?
C30 N4 1.458(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C34 1.502(6) . ?
C31 C34 1.502(6) 4_575 ?
C31 N5 1.504(7) . ?
C31 C32 1.550(6) 4_575 ?
C31 C32 1.550(6) . ?
C31 C33 1.559(6) 4_575 ?
C31 C33 1.559(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
N2 C2 1.436(5) 4_575 ?
N5 C30 1.438(4) 4_575 ?
C1S Cl3 1.53(2) . ?
C1S Cl3 1.53(2) 4_575 ?
C1S Cl4 1.69(2) 4_575 ?
C1S Cl4 1.69(2) . ?
C1S Cl2 1.729(9) . ?
C1S Cl2 1.729(9) 4_575 ?
C1S Cl1 1.776(3) 4_575 ?
C1S Cl1 1.776(3) . ?
C1S Cl5 1.887(19) . ?
C1S Cl5 1.887(19) 4_575 ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
Cl1 Cl5 1.657(19) 4_575 ?
Cl1 Cl3 1.77(2) 4_575 ?
Cl1 Cl2 2.216(8) 4_575 ?
Cl1 Cl4 2.28(2) 4_575 ?
Cl2 Cl5 0.844(17) . ?
Cl2 Cl2 0.894(15) 4_575 ?
Cl2 Cl4 1.07(2) . ?
Cl2 Cl3 1.12(2) . ?
Cl2 Cl4 1.35(2) 4_575 ?
Cl2 Cl3 1.57(2) 4_575 ?
Cl2 Cl5 1.70(2) 4_575 ?
Cl2 Cl1 2.216(8) 4_575 ?
Cl3 Cl5 1.31(3) . ?
Cl3 Cl3 1.34(4) 4_575 ?
Cl3 Cl2 1.57(2) 4_575 ?
Cl3 Cl1 1.77(2) 4_575 ?
Cl3 Cl4 1.95(3) . ?
Cl3 Cl4 2.19(3) 4_575 ?
Cl3 Cl5 2.23(3) 4_575 ?
Cl3 H1SB 1.5260 . ?
Cl4 Cl4 0.75(5) 4_575 ?
Cl4 Cl5 1.16(3) . ?
Cl4 Cl2 1.35(2) 4_575 ?
Cl4 Cl5 1.78(3) 4_575 ?
Cl4 Cl3 2.19(3) 4_575 ?
Cl4 Cl1 2.28(2) 4_575 ?
Cl4 H1SA 1.7285 . ?
Cl5 Cl1 1.657(19) 4_575 ?
Cl5 Cl2 1.70(2) 4_575 ?
Cl5 Cl4 1.78(3) 4_575 ?
Cl5 Cl3 2.23(3) 4_575 ?
Cl5 Cl5 2.44(4) 4_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 122.4(3) . . ?
O1 C1 N1 122.4(3) . 4_575 ?
N1 C1 N1 115.1(5) . 4_575 ?
N2 C2 N1 112.0(4) . . ?
N2 C2 H2A 109.2 . . ?
N1 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
N1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 C5 107.7(4) . . ?
N2 C3 C5 107.7(4) . 4_575 ?
C5 C3 C5 109.8(7) . 4_575 ?
N2 C3 C4 113.4(5) . . ?
C5 C3 C4 109.1(4) . . ?
C5 C3 C4 109.1(4) 4_575 . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 113.7(4) . . ?
N1 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 . . ?
N1 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C12 C7 C8 116.8(4) . . ?
C12 C7 C6 123.1(4) . . ?
C8 C7 C6 120.0(4) . . ?
C9 C8 C7 121.6(4) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 120.7(4) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 118.1(4) . . ?
C11 C10 C13 120.5(4) . . ?
C9 C10 C13 121.4(4) . . ?
C10 C11 C12 121.3(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C7 121.4(4) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
C14 C13 C10 176.7(4) . . ?
C13 C14 C15 175.1(4) . . ?
N3 C15 C16 123.3(4) . . ?
N3 C15 C14 114.8(4) . . ?
C16 C15 C14 122.0(4) . . ?
C17 C16 C15 119.1(4) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C18 C17 C16 118.8(4) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 119.4(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
N3 C19 C18 122.9(4) . . ?
N3 C19 C20 117.5(3) . . ?
C18 C19 C20 119.6(4) . . ?
C21 C20 C19 175.1(4) . . ?
C20 C21 C22 176.4(4) . . ?
C23 C22 C27 118.9(4) . . ?
C23 C22 C21 120.3(4) . . ?
C27 C22 C21 120.8(4) . . ?
C22 C23 C24 119.9(4) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 121.6(4) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 118.5(4) . . ?
C24 C25 C28 122.0(4) . . ?
C26 C25 C28 119.5(4) . . ?
C25 C26 C27 120.7(4) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C26 C27 C22 120.4(4) . . ?
C26 C27 H27 119.8 . . ?
C22 C27 H27 119.8 . . ?
N4 C28 C25 113.7(3) . . ?
N4 C28 H28A 108.8 . . ?
C25 C28 H28A 108.8 . . ?
N4 C28 H28B 108.8 . . ?
C25 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
O2 C29 N4 121.5(2) . 4_575 ?
O2 C29 N4 121.5(2) . . ?
N4 C29 N4 116.9(5) 4_575 . ?
N5 C30 N4 113.2(3) . . ?
N5 C30 H30A 108.9 . . ?
N4 C30 H30A 108.9 . . ?
N5 C30 H30B 108.9 . . ?
N4 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C34 C31 C34 129.4(7) . 4_575 ?
C34 C31 N5 113.5(4) . . ?
C34 C31 N5 113.5(4) 4_575 . ?
C34 C31 C32 64.9(5) . 4_575 ?
C34 C31 C32 109.7(6) 4_575 4_575 ?
N5 C31 C32 114.7(4) . 4_575 ?
C34 C31 C32 109.7(6) . . ?
C34 C31 C32 64.9(5) 4_575 . ?
N5 C31 C32 114.7(4) . . ?
C32 C31 C32 49.9(6) 4_575 . ?
C34 C31 C33 109.3(6) 4_575 4_575 ?
N5 C31 C33 103.1(4) . 4_575 ?
C32 C31 C33 105.8(5) 4_575 4_575 ?
C32 C31 C33 140.9(6) . 4_575 ?
C34 C31 C33 109.3(6) . . ?
N5 C31 C33 103.1(4) . . ?
C32 C31 C33 140.9(6) 4_575 . ?
C32 C31 C33 105.8(5) . . ?
C33 C31 C33 73.2(8) 4_575 . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C6 117.2(4) . . ?
C1 N1 C2 122.4(4) . . ?
C6 N1 C2 119.7(4) . . ?
C2 N2 C2 108.3(5) 4_575 . ?
C2 N2 C3 117.8(3) 4_575 . ?
C2 N2 C3 117.8(3) . . ?
C19 N3 C15 116.4(3) . . ?
C29 N4 C28 120.2(3) . . ?
C29 N4 C30 120.8(3) . . ?
C28 N4 C30 116.7(3) . . ?
C30 N5 C30 106.0(4) 4_575 . ?
C30 N5 C31 117.5(2) 4_575 . ?
C30 N5 C31 117.5(2) . . ?

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
N1 C6 C7 C12 -11.4(6) . . . . ?
N1 C6 C7 C8 168.0(4) . . . . ?
C12 C7 C8 C9 -1.5(6) . . . . ?
C6 C7 C8 C9 179.1(4) . . . . ?
C7 C8 C9 C10 2.6(7) . . . . ?
C8 C9 C10 C11 -2.2(6) . . . . ?
C8 C9 C10 C13 176.2(4) . . . . ?
C9 C10 C11 C12 0.7(6) . . . . ?
C13 C10 C11 C12 -177.7(4) . . . . ?
C10 C11 C12 C7 0.3(7) . . . . ?
C8 C7 C12 C11 0.1(6) . . . . ?
C6 C7 C12 C11 179.4(4) . . . . ?
N3 C15 C16 C17 2.1(6) . . . . ?
C14 C15 C16 C17 -176.8(4) . . . . ?
C15 C16 C17 C18 0.5(7) . . . . ?
C16 C17 C18 C19 -2.3(7) . . . . ?
C17 C18 C19 N3 1.9(7) . . . . ?
C17 C18 C19 C20 -176.5(4) . . . . ?
C27 C22 C23 C24 -2.8(6) . . . . ?
C21 C22 C23 C24 175.7(4) . . . . ?
C22 C23 C24 C25 1.5(6) . . . . ?
C23 C24 C25 C26 0.9(6) . . . . ?
C23 C24 C25 C28 -178.9(4) . . . . ?
C24 C25 C26 C27 -1.9(6) . . . . ?
C28 C25 C26 C27 177.8(4) . . . . ?
C25 C26 C27 C22 0.6(7) . . . . ?
C23 C22 C27 C26 1.7(6) . . . . ?
C21 C22 C27 C26 -176.7(4) . . . . ?
C24 C25 C28 N4 -114.4(4) . . . . ?
C26 C25 C28 N4 65.9(5) . . . . ?
O1 C1 N1 C6 3.8(7) . . . . ?
N1 C1 N1 C6 -177.3(3) 4_575 . . . ?
O1 C1 N1 C2 173.8(5) . . . . ?
N1 C1 N1 C2 -7.3(8) 4_575 . . . ?
C7 C6 N1 C1 93.2(5) . . . . ?
C7 C6 N1 C2 -77.1(5) . . . . ?
N2 C2 N1 C1 32.8(7) . . . . ?
N2 C2 N1 C6 -157.4(4) . . . . ?
N1 C2 N2 C2 -55.7(7) . . . 4_575 ?
N1 C2 N2 C3 81.2(5) . . . . ?
C5 C3 N2 C2 -172.8(5) . . . 4_575 ?
C5 C3 N2 C2 -54.4(6) 4_575 . . 4_575 ?
C4 C3 N2 C2 66.4(4) . . . 4_575 ?
C5 C3 N2 C2 54.4(6) . . . . ?
C5 C3 N2 C2 172.8(5) 4_575 . . . ?
C4 C3 N2 C2 -66.4(4) . . . . ?
C18 C19 N3 C15 0.5(6) . . . . ?
C20 C19 N3 C15 179.0(3) . . . . ?
C16 C15 N3 C19 -2.5(5) . . . . ?
C14 C15 N3 C19 176.4(3) . . . . ?
O2 C29 N4 C28 -10.8(6) . . . . ?
N4 C29 N4 C28 173.3(3) 4_575 . . . ?
O2 C29 N4 C30 -173.2(4) . . . . ?
N4 C29 N4 C30 10.8(7) 4_575 . . . ?
C25 C28 N4 C29 -94.6(5) . . . . ?
C25 C28 N4 C30 68.5(4) . . . . ?
N5 C30 N4 C29 -35.5(5) . . . . ?
N5 C30 N4 C28 161.5(3) . . . . ?
N4 C30 N5 C30 55.9(5) . . . 4_575 ?
N4 C30 N5 C31 -77.8(4) . . . . ?
C34 C31 N5 C30 35.4(7) . . . 4_575 ?
C34 C31 N5 C30 -163.8(5) 4_575 . . 4_575 ?
C32 C31 N5 C30 -36.5(5) 4_575 . . 4_575 ?
C32 C31 N5 C30 -91.9(4) . . . 4_575 ?
C33 C31 N5 C30 78.1(5) 4_575 . . 4_575 ?
C33 C31 N5 C30 153.5(5) . . . 4_575 ?
C34 C31 N5 C30 163.8(5) . . . . ?
C34 C31 N5 C30 -35.4(7) 4_575 . . . ?
C32 C31 N5 C30 91.9(4) 4_575 . . . ?
C32 C31 N5 C30 36.5(5) . . . . ?
C33 C31 N5 C30 -153.5(5) 4_575 . . . ?
C33 C31 N5 C30 -78.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.063
