# Electronic Supplementary Material (ESI) for Polymer Chemistry.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ltb-38-002_100k_mp_hjs1-ref
_database_code_depnum_ccdc_archive 'CCDC 2005040'
loop_
_audit_author_name
_audit_author_address
'Helena J. Shepherd'
;School of Physical Sciences, University of Kent
United Kingdom
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;
_audit_creation_date             2019-01-10
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H11 N O4'
_chemical_formula_sum            'C11 H11 N O4'
_chemical_formula_weight         221.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H11 N1 O4'
_chemical_oxdiff_usercomment     100k
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                   6.29482(14)
_cell_length_b                   13.8975(3)
_cell_length_c                   11.1692(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.663(2)
_cell_angle_gamma                90
_cell_volume                     977.04(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4862
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.2290
_cell_measurement_theta_min      5.0550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             464
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 3 -7 0.0782
-4 4 -1 0.0811
2 -4 6 0.0263
4 -1 -3 0.0455
1 9 -1 0.0987
1 0 7 0.0061
-1 0 -7 0.0521
-1 -9 0 0.1637

_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0793 3.3405 -6.7330 -0.0402 -0.1107 0.9930
-3.6512 3.6925 -1.2575 0.2974 0.8432 0.4479
1.5929 -4.1426 5.7556 -0.0936 -0.2677 -0.9590
3.5676 -1.3387 -3.4387 -0.3231 -0.9136 0.2468
0.9046 8.6763 -1.1907 -0.8145 0.2871 0.5042
1.0713 0.2248 6.9722 -0.4138 0.1473 -0.8984
-1.0163 0.2479 -6.9988 0.3673 -0.1309 0.9208
-0.8782 -9.0768 -0.0196 0.8835 -0.3740 -0.3717

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6593
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.391
_diffrn_reflns_theta_min         5.080
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  61.00   1.00    1.00    --   42.70 -57.00 -30.00   45
  2  ω     45.00  92.00   1.00    1.00    --   42.70-125.00-150.00   47
  3  ω     36.00 104.00   1.00    4.00    --  105.99 -94.00 -90.00   68
  4  ω     68.00 107.00   1.00    4.00    --  105.99 -94.00-180.00   39
  5  ω     59.00 118.00   1.00    4.00    --  105.99 -30.00-150.00   59
  6  ω     97.00 176.00   1.00    4.00    --  105.99  30.00 -90.00   79
  7  ω    138.00 163.00   1.00    4.00    --  105.99 125.00  60.00   25
  8  ω    108.00 175.00   1.00    4.00    --  105.99 125.00 120.00   67
  9  ω    102.00 129.00   1.00    4.00    --  105.99 125.00 -90.00   27
 10  ω     62.00 162.00   1.00    4.00    --  105.99  15.00-150.00  100
 11  ω     75.00 121.00   1.00    4.00    --  105.99-125.00  90.00   46
 12  ω     44.00 120.00   1.00    4.00    --  105.99 -45.00 -30.00   76
 13  ω     31.00  99.00   1.00    4.00    --  105.99 -94.00 120.00   68
 14  ω     37.00 151.00   1.00    4.00    --  105.99 -15.00 150.00  114
 15  ω    -65.00  26.00   1.00    1.00    --  -42.70  38.00   0.00   91
 16  ω    -80.00  36.00   1.00    1.00    --  -42.70  19.00 -90.00  116
 17  ω    -96.00 -20.00   1.00    1.00    --  -42.70 -38.00 150.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1534113000
_diffrn_orient_matrix_UB_12      -0.0824252000
_diffrn_orient_matrix_UB_13      -0.0331244000
_diffrn_orient_matrix_UB_21      -0.1875605000
_diffrn_orient_matrix_UB_22      0.0592433000
_diffrn_orient_matrix_UB_23      0.0480376000
_diffrn_orient_matrix_UB_31      -0.0345582000
_diffrn_orient_matrix_UB_32      0.0445594000
_diffrn_orient_matrix_UB_33      -0.1249755000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus 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                1807
_reflns_number_total             1934
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1934
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.072
_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)+(0.0610P)²+0.4662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1134
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_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
O12 O 0.88407(16) 0.25659(7) 0.22761(9) 0.0190(3) Uani 1 1 d . . . . .
O3 O 0.99054(17) 0.59970(7) 0.14962(9) 0.0203(3) Uani 1 1 d . . . . .
O2 O 0.91566(19) 0.52479(8) 0.32251(10) 0.0269(3) Uani 1 1 d . . . . .
O1 O 0.41844(18) 0.50526(8) 0.20535(10) 0.0269(3) Uani 1 1 d . . . . .
N1 N 0.67763(18) 0.39010(8) 0.20058(10) 0.0148(3) Uani 1 1 d . . . . .
C3 C 0.7177(2) 0.29938(10) 0.24420(12) 0.0143(3) Uani 1 1 d . . . . .
C1 C 0.9151(2) 0.52826(10) 0.21518(12) 0.0166(3) Uani 1 1 d . . . . .
C7 C 0.5784(2) 0.25399(10) 0.44995(12) 0.0172(3) Uani 1 1 d . . . . .
C4 C 0.5269(2) 0.26523(10) 0.31321(12) 0.0146(3) Uani 1 1 d . . . . .
C2 C 0.8278(2) 0.44876(10) 0.13540(12) 0.0172(3) Uani 1 1 d . . . . .
C11 C 0.3692(2) 0.22235(11) 0.50423(12) 0.0202(3) Uani 1 1 d . . . . .
C5 C 0.3711(2) 0.35119(10) 0.30979(12) 0.0167(3) Uani 1 1 d . . . . .
C9 C 0.3549(2) 0.38064(11) 0.44510(13) 0.0199(3) Uani 1 1 d . . . . .
C6 C 0.4802(2) 0.42640(10) 0.23474(12) 0.0167(3) Uani 1 1 d . . . . .
C10 C 0.2380(2) 0.29729(11) 0.50215(13) 0.0222(3) Uani 1 1 d . . . . .
C8 C 0.5838(2) 0.36015(11) 0.48905(13) 0.0196(3) Uani 1 1 d . . . . .
H4 H 0.472(3) 0.2047(13) 0.2786(15) 0.012(4) Uiso 1 1 d . . . . .
H2A H 0.760(3) 0.4763(13) 0.0671(17) 0.019(4) Uiso 1 1 d . . . . .
H7 H 0.699(3) 0.2132(14) 0.4645(17) 0.021(4) Uiso 1 1 d . . . . .
H8A H 0.688(3) 0.3988(13) 0.4458(16) 0.017(4) Uiso 1 1 d . . . . .
H11 H 0.338(3) 0.1564(16) 0.5253(18) 0.028(5) Uiso 1 1 d . . . . .
H5 H 0.230(3) 0.3383(14) 0.2742(16) 0.021(4) Uiso 1 1 d . . . . .
H2B H 0.944(3) 0.4080(14) 0.1108(17) 0.021(4) Uiso 1 1 d . . . . .
H10 H 0.082(3) 0.2997(15) 0.5233(18) 0.031(5) Uiso 1 1 d . . . . .
H9 H 0.295(3) 0.4440(16) 0.4566(18) 0.030(5) Uiso 1 1 d . . . . .
H8B H 0.596(3) 0.3677(15) 0.574(2) 0.030(5) Uiso 1 1 d . . . . .
H3 H 1.042(4) 0.6449(18) 0.198(2) 0.039(6) Uiso 1 1 d . . . . .


_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
O12 C3 1.2205(17) . ?
O3 C1 1.3251(17) . ?
O3 H3 0.89(3) . ?
O2 C1 1.1997(18) . ?
O1 C6 1.2070(18) . ?
N1 C3 1.3739(18) . ?
N1 C2 1.4504(17) . ?
N1 C6 1.3985(18) . ?
C3 C4 1.5110(18) . ?
C1 C2 1.518(2) . ?
C7 C4 1.5654(18) . ?
C7 C11 1.5210(19) . ?
C7 C8 1.539(2) . ?
C7 H7 0.96(2) . ?
C4 C5 1.5459(19) . ?
C4 H4 0.985(17) . ?
C2 H2A 0.949(19) . ?
C2 H2B 0.97(2) . ?
C11 C10 1.329(2) . ?
C11 H11 0.97(2) . ?
C5 C9 1.5701(19) . ?
C5 C6 1.5100(19) . ?
C5 H5 0.99(2) . ?
C9 C10 1.517(2) . ?
C9 C8 1.543(2) . ?
C9 H9 0.97(2) . ?
C10 H10 1.01(2) . ?
C8 H8A 0.978(19) . ?
C8 H8B 0.96(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O3 H3 108.8(15) . . ?
C3 N1 C2 125.16(11) . . ?
C3 N1 C6 113.22(11) . . ?
C6 N1 C2 121.37(11) . . ?
O12 C3 N1 123.20(12) . . ?
O12 C3 C4 127.80(13) . . ?
N1 C3 C4 109.00(11) . . ?
O3 C1 C2 110.52(12) . . ?
O2 C1 O3 125.82(14) . . ?
O2 C1 C2 123.65(13) . . ?
C4 C7 H7 112.3(11) . . ?
C11 C7 C4 104.31(11) . . ?
C11 C7 C8 100.40(12) . . ?
C11 C7 H7 116.7(12) . . ?
C8 C7 C4 100.66(11) . . ?
C8 C7 H7 120.2(11) . . ?
C3 C4 C7 111.85(11) . . ?
C3 C4 C5 104.62(11) . . ?
C3 C4 H4 110.1(10) . . ?
C7 C4 H4 111.4(10) . . ?
C5 C4 C7 103.02(11) . . ?
C5 C4 H4 115.6(10) . . ?
N1 C2 C1 110.36(11) . . ?
N1 C2 H2A 110.0(11) . . ?
N1 C2 H2B 108.2(11) . . ?
C1 C2 H2A 109.5(11) . . ?
C1 C2 H2B 108.9(11) . . ?
H2A C2 H2B 109.9(16) . . ?
C7 C11 H11 123.4(12) . . ?
C10 C11 C7 107.88(13) . . ?
C10 C11 H11 128.2(13) . . ?
C4 C5 C9 103.06(11) . . ?
C4 C5 H5 116.0(11) . . ?
C9 C5 H5 111.5(11) . . ?
C6 C5 C4 104.85(11) . . ?
C6 C5 C9 112.89(12) . . ?
C6 C5 H5 108.4(11) . . ?
C5 C9 H9 113.3(12) . . ?
C10 C9 C5 104.04(12) . . ?
C10 C9 C8 100.43(12) . . ?
C10 C9 H9 116.5(12) . . ?
C8 C9 C5 100.79(11) . . ?
C8 C9 H9 119.5(12) . . ?
O1 C6 N1 122.53(13) . . ?
O1 C6 C5 129.23(13) . . ?
N1 C6 C5 108.24(11) . . ?
C11 C10 C9 107.55(13) . . ?
C11 C10 H10 128.7(12) . . ?
C9 C10 H10 123.3(12) . . ?
C7 C8 C9 93.96(11) . . ?
C7 C8 H8A 113.5(11) . . ?
C7 C8 H8B 112.8(12) . . ?
C9 C8 H8A 111.7(11) . . ?
C9 C8 H8B 111.1(13) . . ?
H8A C8 H8B 112.5(17) . . ?

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
O12 C3 C4 C7 66.10(18) . . . . ?
O12 C3 C4 C5 176.92(13) . . . . ?
O3 C1 C2 N1 -158.41(11) . . . . ?
O2 C1 C2 N1 22.2(2) . . . . ?
N1 C3 C4 C7 -113.60(12) . . . . ?
N1 C3 C4 C5 -2.78(14) . . . . ?
C3 N1 C2 C1 -104.79(14) . . . . ?
C3 N1 C6 O1 179.56(13) . . . . ?
C3 N1 C6 C5 -0.57(16) . . . . ?
C3 C4 C5 C9 -115.98(11) . . . . ?
C3 C4 C5 C6 2.34(13) . . . . ?
C7 C4 C5 C9 1.08(13) . . . . ?
C7 C4 C5 C6 119.41(11) . . . . ?
C7 C11 C10 C9 0.68(16) . . . . ?
C4 C7 C11 C10 -71.49(14) . . . . ?
C4 C7 C8 C9 57.72(12) . . . . ?
C4 C5 C9 C10 -68.60(13) . . . . ?
C4 C5 C9 C8 35.15(13) . . . . ?
C4 C5 C6 O1 178.65(15) . . . . ?
C4 C5 C6 N1 -1.21(14) . . . . ?
C2 N1 C3 O12 -3.3(2) . . . . ?
C2 N1 C3 C4 176.41(12) . . . . ?
C2 N1 C6 O1 5.1(2) . . . . ?
C2 N1 C6 C5 -175.05(11) . . . . ?
C11 C7 C4 C3 178.47(11) . . . . ?
C11 C7 C4 C5 66.64(13) . . . . ?
C11 C7 C8 C9 -49.15(12) . . . . ?
C5 C9 C10 C11 70.56(15) . . . . ?
C5 C9 C8 C7 -56.94(12) . . . . ?
C9 C5 C6 O1 -69.91(19) . . . . ?
C9 C5 C6 N1 110.24(13) . . . . ?
C6 N1 C3 O12 -177.54(12) . . . . ?
C6 N1 C3 C4 2.18(15) . . . . ?
C6 N1 C2 C1 69.00(16) . . . . ?
C6 C5 C9 C10 178.85(12) . . . . ?
C6 C5 C9 C8 -77.40(14) . . . . ?
C10 C9 C8 C7 49.68(12) . . . . ?
C8 C7 C4 C3 74.73(14) . . . . ?
C8 C7 C4 C5 -37.10(13) . . . . ?
C8 C7 C11 C10 32.45(15) . . . . ?
C8 C9 C10 C11 -33.46(15) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.798
####################################################################### 
# 
# 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_ltb-82_ref
_database_code_depnum_ccdc_archive 'CCDC 2005042'
loop_
_audit_author_name
_audit_author_address
'Helena J. Shepherd'
;School of Physical Sciences, University of Kent
United Kingdom
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;
_audit_creation_date             2020-05-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C39 H42 N4 O4, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C41 H42 N4 O5'
_chemical_formula_weight         670.78
_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'

_cell_length_a                   10.4936(3)
_cell_length_b                   12.3484(3)
_cell_length_c                   16.1383(4)
_cell_angle_alpha                99.335(2)
_cell_angle_beta                 102.497(2)
_cell_angle_gamma                112.561(2)
_cell_volume                     1814.32(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8190
_cell_measurement_theta_min      4.2400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             712
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 0 0 0.0482
5 -6 -3 0.1072
-6 1 0 0.0643
-1 3 9 0.0974
1 -1 -10 0.0327
1 -8 3 0.1561
-1 -1 10 0.0904
-6 5 2 0.0331

_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.123
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.394
_diffrn_reflns_theta_min         4.029
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00 132.00   1.00    4.00    --  105.91 -45.00  30.00   98
  2  ω     78.00 154.00   1.00    4.00    --  105.91  61.00 -90.00   76
  3  ω    125.00 151.00   1.00    4.00    --  105.91  77.00 -30.00   26
  4  ω     95.00 142.00   1.00    1.00    --   66.00  76.00  29.13   47
  5  ω    119.00 149.00   1.00    4.00    --  105.91  77.00  90.00   30
  6  ω    125.00 151.00   1.00    4.00    --  105.91  77.00 150.00   26
  7  ω    111.00 142.00   1.00    1.00    --   66.00  77.00 132.75   31
  8  ω     78.00 114.00   1.00    4.00    --  105.91  61.00 120.00   36
  9  ω     73.00 177.00   1.00    4.00    --  105.91  77.00 120.00  104
 10  ω     79.00 108.00   1.00    4.00    --  105.91  61.00  30.00   29
 11  ω     74.00  99.00   1.00    4.00    --  105.91  77.00   0.00   25
 12  ω     73.00 142.00   1.00    4.00    --  105.91  77.00  30.00   69
 13  ω     78.00 112.00   1.00    4.00    --  105.91  61.00 -60.00   34
 14  ω     78.00 173.00   1.00    4.00    --  105.91  61.00   0.00   95
 15  ω    152.00 178.00   1.00    4.00    --  105.91 125.00-150.00   26
 16  ω    103.00 129.00   1.00    1.00    --   70.00  77.00-168.95   26
 17  ω    101.00 127.00   1.00    4.00    --  105.91 125.00-150.00   26
 18  ω     79.00 175.00   1.00    4.00    --  105.91  61.00-180.00   96
 19  ω     77.00 169.00   1.00    4.00    --  105.91  61.00-150.00   92
 20  ω     74.00 114.00   1.00    4.00    --  105.91  76.00-127.00   40
 21  ω     73.00 164.00   1.00    4.00    --  105.91  77.00 -60.00   91
 22  ω     74.00  99.00   1.00    4.00    --  105.91  77.00-150.00   25
 23  ω     74.00 100.00   1.00    4.00    --  105.91  77.00-180.00   26
 24  ω     73.00  99.00   1.00    4.00    --  105.91  77.00 -90.00   26
 25  ω     73.00  99.00   1.00    4.00    --  105.91  77.00 -30.00   26
 26  ω     73.00 178.00   1.00    4.00    --  105.91  77.00  60.00  105
 27  ω     73.00  98.00   1.00    4.00    --  105.91  77.00  90.00   25
 28  ω     73.00  99.00   1.00    4.00    --  105.91  77.00 150.00   26
 29  ω     36.00  69.00   1.00    1.00    --   66.00  77.00 132.75   33
 30  ω     39.00  67.00   1.00    1.00    --   66.00  76.00  61.66   28
 31  ω     34.00  60.00   1.00    1.00    --   66.00  76.00  29.13   26
 32  ω     38.00  66.00   1.00    1.00    --   70.00  76.00 -18.38   28
 33  ω     31.00  59.00   1.00    1.00    --   62.00  77.00 -53.83   28
 34  ω     41.00  97.00   1.00    1.00    --   74.00  77.00 -79.06   56
 35  ω     37.00  68.00   1.00    1.00    --   70.00  77.00-126.29   31
 36  ω     37.00  63.00   1.00    1.00    --   70.00  77.00-168.95   26
 37  ω     20.00  46.00   1.00    1.00    --   54.00  81.00-174.68   26
 38  ω     16.00  42.00   1.00    1.00    --   50.00  81.00-149.47   26
 39  ω      6.00  31.00   1.00    1.00    --   42.00  88.00-105.05   25
 40  ω     20.00  45.00   1.00    1.00    --   54.00  81.00 -72.32   25
 41  ω     12.00  37.00   1.00    1.00    --   46.00  84.00 -27.53   25
 42  ω     20.00  45.00   1.00    1.00    --   54.00  81.00   8.41   25
 43  ω     21.00  46.00   1.00    1.00    --   54.00  79.00  63.78   25
 44  ω     38.00  71.00   1.00    1.00    --   70.00  76.00  96.72   33
 45  ω     20.00  45.00   1.00    1.00    --   54.00  81.00 121.83   25
 46  ω     -5.00  20.00   1.00    1.00    --   34.00  96.00 134.21   25
 47  ω     64.00 119.00   1.00    4.00    --  105.91-125.00-150.00   55
 48  ω     33.00 103.00   1.00    4.00    --  105.91 -94.00 -30.00   70
 49  ω     23.00  70.00   1.00    1.00    --   42.16-125.00  90.00   47
 50  ω     34.00 103.00   1.00    4.00    --  105.91 -94.00  30.00   69
 51  ω     23.00 102.00   1.00    4.00    --  105.91 -94.00 -90.00   79
 52  ω     30.00  82.00   1.00    4.00    --  105.91 -94.00-150.00   52
 53  ω    -65.00  27.00   1.00    1.00    --  -42.16  57.00-180.00   92
 54  ω    -46.00 -14.00   1.00    1.00    --  -42.16 -57.00  30.00   32
 55  ω   -106.00 -23.00   1.00    1.00    --  -42.16 -38.00-150.00   83
 56  ω   -108.00 -50.00   1.00    1.00    --  -42.16 -57.00  30.00   58
 57  ω   -114.00 -18.00   1.00    1.00    --  -42.16 -38.00 120.00   96
 58  ω    -89.00 -11.00   1.00    1.00    --  -42.16 125.00-120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5955
_reflns_number_total             7133
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0512
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0871P)²+0.3690P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1571
_refine_special_details          
;
 The structure contains a molecule of ethyl acetate, which is 
 disordered about a special position.  As a consequence a number
 of restraints on ADPs and bondlengths were required to ensure
 a stable and chemically sensible model.  Details can be found
 in the _olex2_refinement_description section.
;
_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. Restrained distances
 C2S-C1S
 1.5 with sigma of 0.02
 O3S-C4S
 1.32 with sigma of 0.02
 C5S-C4S
 1.49 with sigma of 0.02
 O3S-C2S
 1.46 with sigma of 0.02
 O6S-C4S
 1.22 with sigma of 0.02
 O6S-C5S
 2.4 with sigma of 0.04
 O3S-C5S
 2.35 with sigma of 0.04
 O3S-O6S
 2.24 with sigma of 0.04
 O3S-C1S
 2.38 with sigma of 0.04
 N2-C20A \\sim N2-C20 \\sim N2-C18 \\sim N1-C2 \\sim N1-C3
 with sigma of 0.02
 C21A-C20A \\sim C21-C20 \\sim C19-C18 \\sim C1-C2 \\sim C4-C3
 with sigma of 0.02
 C5S-C4S \\sim C2S-C1S
 with sigma of 0.02
3. Restrained planarity
 O3S, O6S, C5S, C4S, C2S, C1S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O3S \\sim O6S \\sim C5S \\sim C4S \\sim C2S \\sim C1S: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C20A) = Uanis(C20)
Uanis(C21A) = Uanis(C21)
Uanis(C2S) = Uanis(O3S) = Uanis(C4S) = Uanis(O6S) = Uanis(C5S) = Uanis(C1S)
5. Rigid body (RIGU) restrains
 O3S, O6S, C5S, C4S, C2S, C1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C20)=Sof(H20C)=Sof(H20D)=Sof(C21)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Fixed Sof: O3S(0.5) O6S(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5) C4S(0.5)
 C2S(0.5) H2SA(0.5) H2SB(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5)
7.a Ternary CH refined with riding coordinates:
 C32(H32), C38(H38), C33(H33), C36(H36)
7.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C3(H3A,H3B), C37(H37A,H37B), C2(H2A,H2B),
 C18(H18A,H18B), C20A(H20A,H20B), C20(H20C,H20D), C2S(H2SA,H2SB)
7.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C6(H6), C17(H17), C14(H14), C16(H16), C26(H26), C23(H23),
 C35(H35), C34(H34), C25(H25), C24(H24)
7.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C21A(H21A,H21B,H21C),
 C21(H21D,H21E,H21F), C5S(H5SA,H5SB,H5SC), C1S(H1SA,H1SB,H1SC)
;
_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 0.66643(15) 0.60720(11) 0.52840(8) 0.0576(3) Uani 1 1 d . . . . .
O2 O 0.44052(14) 0.71990(11) 0.17485(7) 0.0612(3) Uani 1 1 d . . . . .
N3 N 0.51802(13) 0.67271(11) 0.30278(7) 0.0424(3) Uani 1 1 d . . . . .
N4 N 0.28989(14) 0.44979(12) 0.15001(8) 0.0488(3) Uani 1 1 d . . . . .
O3 O 0.48625(15) 0.43344(15) 0.12009(9) 0.0758(4) Uani 1 1 d . . . . .
O4 O 0.07250(15) 0.45646(15) 0.14082(9) 0.0748(4) Uani 1 1 d . . . . .
N1 N 0.58959(17) 0.90899(14) 0.70427(9) 0.0595(4) Uani 1 1 d D . . . .
C8 C 0.63951(15) 0.76421(13) 0.46375(9) 0.0430(3) Uani 1 1 d . . . . .
C9 C 0.64482(16) 0.71067(14) 0.53259(10) 0.0446(3) Uani 1 1 d . . . . .
C28 C 0.53574(18) 0.73490(14) 0.24060(9) 0.0464(3) Uani 1 1 d . . . . .
C12 C 0.69258(16) 0.60679(14) 0.38280(9) 0.0448(3) Uani 1 1 d . . . . .
C11 C 0.65421(16) 0.71174(14) 0.37674(9) 0.0429(3) Uani 1 1 d . . . . .
C5 C 0.60941(16) 0.86358(15) 0.62658(10) 0.0479(3) Uani 1 1 d . . . . .
C22 C 0.76007(17) 0.80944(14) 0.34702(10) 0.0479(3) Uani 1 1 d . . . . .
C27 C 0.69050(18) 0.82240(14) 0.26907(10) 0.0491(4) Uani 1 1 d . . . . .
C10 C 0.62985(18) 0.75792(15) 0.61188(10) 0.0492(3) Uani 1 1 d . . . . .
H10 H 0.6335 0.7184 0.6561 0.059 Uiso 1 1 calc R U . . .
C13 C 0.69678(17) 0.56108(14) 0.45544(10) 0.0467(3) Uani 1 1 d . . . . .
C7 C 0.62093(18) 0.87054(15) 0.47955(10) 0.0509(4) Uani 1 1 d . . . . .
H7 H 0.6175 0.9097 0.4351 0.061 Uiso 1 1 calc R U . . .
C6 C 0.60736(19) 0.92045(16) 0.55791(10) 0.0522(4) Uani 1 1 d . . . . .
H6 H 0.5967 0.9925 0.5655 0.063 Uiso 1 1 calc R U . . .
C29 C 0.37933(17) 0.58273(15) 0.30249(10) 0.0476(3) Uani 1 1 d . . . . .
H29A H 0.3062 0.6109 0.2837 0.057 Uiso 1 1 calc R U . . .
H29B H 0.3851 0.5773 0.3624 0.057 Uiso 1 1 calc R U . . .
C31 C 0.37591(19) 0.44473(16) 0.09674(11) 0.0548(4) Uani 1 1 d . . . . .
C17 C 0.7245(2) 0.54905(17) 0.31394(11) 0.0568(4) Uani 1 1 d . . . . .
H17 H 0.7215 0.5763 0.2634 0.068 Uiso 1 1 calc R U . . .
C30 C 0.33020(18) 0.45565(15) 0.24329(10) 0.0509(4) Uani 1 1 d . . . . .
H30A H 0.4079 0.4310 0.2567 0.061 Uiso 1 1 calc R U . . .
H30B H 0.2478 0.3986 0.2559 0.061 Uiso 1 1 calc R U . . .
C14 C 0.7327(2) 0.46513(16) 0.46070(12) 0.0578(4) Uani 1 1 d . . . . .
H14 H 0.7339 0.4371 0.5109 0.069 Uiso 1 1 calc R U . . .
C39 C 0.16370(19) 0.45504(16) 0.10670(11) 0.0540(4) Uani 1 1 d . . . . .
C32 C 0.3057(2) 0.45354(17) 0.00790(11) 0.0579(4) Uani 1 1 d . . . . .
H32 H 0.3677 0.5276 -0.0046 0.070 Uiso 1 1 calc R U . . .
C38 C 0.1635(2) 0.45651(17) 0.01373(11) 0.0578(4) Uani 1 1 d . . . . .
H38 H 0.1591 0.5304 0.0015 0.069 Uiso 1 1 calc R U . . .
C16 C 0.7602(2) 0.45374(18) 0.31752(12) 0.0613(4) Uani 1 1 d . . . . .
H16 H 0.7801 0.4179 0.2697 0.074 Uiso 1 1 calc R U . . .
N2 N 0.8058(3) 0.31591(19) 0.39756(14) 0.0934(7) Uani 1 1 d D . . . .
C26 C 0.7643(2) 0.90726(17) 0.22904(13) 0.0653(5) Uani 1 1 d . . . . .
H26 H 0.7171 0.9156 0.1763 0.078 Uiso 1 1 calc R U . . .
C15 C 0.7669(2) 0.40983(16) 0.39201(13) 0.0601(4) Uani 1 1 d . . . . .
C23 C 0.9067(2) 0.88205(17) 0.38889(14) 0.0641(5) Uani 1 1 d . . . . .
H23 H 0.9538 0.8740 0.4418 0.077 Uiso 1 1 calc R U . . .
C33 C 0.2552(2) 0.33887(19) -0.07077(11) 0.0656(5) Uani 1 1 d . . . . .
H33 H 0.3290 0.3347 -0.0977 0.079 Uiso 1 1 calc R U . . .
C35 C 0.0544(2) 0.23286(19) -0.03326(13) 0.0741(6) Uani 1 1 d . . . . .
H35 H -0.0146 0.1770 -0.0149 0.089 Uiso 1 1 calc R U . . .
C34 C 0.1768(3) 0.23035(19) -0.04025(13) 0.0726(5) Uani 1 1 d . . . . .
H34 H 0.2085 0.1721 -0.0284 0.087 Uiso 1 1 calc R U . . .
C25 C 0.9110(3) 0.97900(18) 0.27068(18) 0.0785(6) Uani 1 1 d . . . . .
H25 H 0.9635 1.0363 0.2453 0.094 Uiso 1 1 calc R U . . .
C3 C 0.5926(2) 1.02897(19) 0.72472(13) 0.0672(5) Uani 1 1 d D . . . .
H3A H 0.5534 1.0367 0.7734 0.081 Uiso 1 1 calc R U . . .
H3B H 0.5298 1.0357 0.6740 0.081 Uiso 1 1 calc R U . . .
C37 C 0.1268(2) 0.3478(2) -0.12979(12) 0.0731(5) Uani 1 1 d . . . . .
H37A H 0.0739 0.2797 -0.1823 0.088 Uiso 1 1 calc R U . . .
H37B H 0.1538 0.4243 -0.1455 0.088 Uiso 1 1 calc R U . . .
C36 C 0.0464(2) 0.3409(2) -0.06003(12) 0.0675(5) Uani 1 1 d . . . . .
H36 H -0.0506 0.3376 -0.0790 0.081 Uiso 1 1 calc R U . . .
C24 C 0.9806(2) 0.96696(19) 0.34924(18) 0.0770(6) Uani 1 1 d . . . . .
H24 H 1.0790 1.0168 0.3760 0.092 Uiso 1 1 calc R U . . .
C2 C 0.5952(3) 0.8495(2) 0.77476(13) 0.0746(6) Uani 1 1 d D . . . .
H2A H 0.5410 0.7621 0.7491 0.089 Uiso 1 1 calc R U . . .
H2B H 0.5471 0.8743 0.8139 0.089 Uiso 1 1 calc R U . . .
C4 C 0.7411(3) 1.1327(2) 0.74879(18) 0.0894(7) Uani 1 1 d D . . . .
H4A H 0.7808 1.1263 0.7009 0.134 Uiso 1 1 calc R U . . .
H4B H 0.8030 1.1293 0.8006 0.134 Uiso 1 1 calc R U . . .
H4C H 0.7342 1.2087 0.7602 0.134 Uiso 1 1 calc R U . . .
C18 C 0.8253(3) 0.2482(2) 0.32341(19) 0.0904(7) Uani 1 1 d D . . . .
H18A H 0.7539 0.2387 0.2699 0.108 Uiso 1 1 calc R U . . .
H18B H 0.8072 0.1674 0.3301 0.108 Uiso 1 1 calc R U . . .
C1 C 0.7446(4) 0.8759(3) 0.82844(17) 0.1061(9) Uani 1 1 d D . . . .
H1A H 0.7950 0.8548 0.7903 0.159 Uiso 1 1 calc R U . . .
H1B H 0.7382 0.8288 0.8705 0.159 Uiso 1 1 calc R U . . .
H1C H 0.7964 0.9611 0.8590 0.159 Uiso 1 1 calc R U . . .
C19 C 0.9713(3) 0.3056(3) 0.3132(3) 0.1142(10) Uani 1 1 d D . . . .
H19A H 0.9718 0.2631 0.2580 0.171 Uiso 1 1 calc R U . . .
H19B H 1.0411 0.3018 0.3607 0.171 Uiso 1 1 calc R U . . .
H19C H 0.9956 0.3892 0.3142 0.171 Uiso 1 1 calc R U . . .
C20A C 0.8913(5) 0.3164(4) 0.4880(4) 0.0715(8) Uani 0.490(3) 1 d D . P A 1
H20A H 0.9708 0.2967 0.4831 0.086 Uiso 0.490(3) 1 calc R U P A 1
H20B H 0.9304 0.3959 0.5296 0.086 Uiso 0.490(3) 1 calc R U P A 1
C21A C 0.7867(6) 0.2226(6) 0.5176(5) 0.1067(14) Uani 0.490(3) 1 d D . P A 1
H21A H 0.7563 0.1435 0.4790 0.160 Uiso 0.490(3) 1 calc R U P A 1
H21B H 0.7038 0.2387 0.5162 0.160 Uiso 0.490(3) 1 calc R U P A 1
H21C H 0.8323 0.2249 0.5767 0.160 Uiso 0.490(3) 1 calc R U P A 1
C20 C 0.7698(4) 0.2491(4) 0.4640(3) 0.0715(8) Uani 0.510(3) 1 d D . P A 2
H20C H 0.7518 0.1649 0.4425 0.086 Uiso 0.510(3) 1 calc R U P A 2
H20D H 0.6836 0.2504 0.4758 0.086 Uiso 0.510(3) 1 calc R U P A 2
C21 C 0.8990(6) 0.3125(6) 0.5476(5) 0.1067(14) Uani 0.510(3) 1 d D . P A 2
H21D H 0.9820 0.3060 0.5360 0.160 Uiso 0.510(3) 1 calc R U P A 2
H21E H 0.8768 0.2747 0.5934 0.160 Uiso 0.510(3) 1 calc R U P A 2
H21F H 0.9195 0.3970 0.5661 0.160 Uiso 0.510(3) 1 calc R U P A 2
O3S O 0.5127(16) -0.0044(15) 0.0051(12) 0.218(2) Uani 0.5 1 d D U P B -1
O6S O 0.2868(9) -0.0522(8) -0.0572(6) 0.218(2) Uani 0.5 1 d D U P B -1
C5S C 0.3615(14) -0.2034(13) -0.0208(13) 0.218(2) Uani 0.5 1 d D U P B -1
H5SA H 0.4546 -0.2043 -0.0052 0.328 Uiso 0.5 1 calc R U P B -1
H5SB H 0.3027 -0.2609 -0.0770 0.328 Uiso 0.5 1 calc R U P B -1
H5SC H 0.3151 -0.2250 0.0231 0.328 Uiso 0.5 1 calc R U P B -1
C4S C 0.3798(14) -0.0833(13) -0.0256(9) 0.218(2) Uani 0.5 1 d D U P B -1
C2S C 0.5405(12) 0.1179(12) -0.0021(9) 0.218(2) Uani 0.5 1 d D U P B -1
H2SA H 0.5135 0.1164 -0.0638 0.262 Uiso 0.5 1 calc R U P B -1
H2SB H 0.4817 0.1464 0.0257 0.262 Uiso 0.5 1 calc R U P B -1
C1S C 0.6922(13) 0.2009(14) 0.0399(12) 0.218(2) Uani 0.5 1 d D U P B -1
H1SA H 0.7503 0.1734 0.0117 0.328 Uiso 0.5 1 calc R U P B -1
H1SB H 0.7186 0.2031 0.1011 0.328 Uiso 0.5 1 calc R U P B -1
H1SC H 0.7083 0.2810 0.0345 0.328 Uiso 0.5 1 calc R U P B -1


_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 C9 1.3746(18) . ?
O1 C13 1.3770(18) . ?
O2 C28 1.2223(19) . ?
N3 C28 1.3612(19) . ?
N3 C11 1.4985(18) . ?
N3 C29 1.452(2) . ?
N4 C31 1.385(2) . ?
N4 C30 1.455(2) . ?
N4 C39 1.388(2) . ?
O3 C31 1.206(2) . ?
O4 C39 1.207(2) . ?
N1 C5 1.380(2) . ?
N1 C3 1.451(2) . ?
N1 C2 1.454(3) . ?
C8 C9 1.384(2) . ?
C8 C11 1.5135(19) . ?
C8 C7 1.391(2) . ?
C9 C10 1.385(2) . ?
C28 C27 1.478(2) . ?
C12 C11 1.509(2) . ?
C12 C13 1.381(2) . ?
C12 C17 1.394(2) . ?
C11 C22 1.520(2) . ?
C5 C10 1.393(2) . ?
C5 C6 1.406(2) . ?
C22 C27 1.378(2) . ?
C22 C23 1.387(2) . ?
C27 C26 1.389(2) . ?
C10 H10 0.9300 . ?
C13 C14 1.383(2) . ?
C7 H7 0.9300 . ?
C7 C6 1.375(2) . ?
C6 H6 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.523(2) . ?
C31 C32 1.505(2) . ?
C17 H17 0.9300 . ?
C17 C16 1.371(2) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C14 H14 0.9300 . ?
C14 C15 1.393(3) . ?
C39 C38 1.503(2) . ?
C32 H32 0.9800 . ?
C32 C38 1.529(3) . ?
C32 C33 1.564(2) . ?
C38 H38 0.9800 . ?
C38 C36 1.560(3) . ?
C16 H16 0.9300 . ?
C16 C15 1.396(3) . ?
N2 C15 1.378(2) . ?
N2 C18 1.445(3) . ?
N2 C20A 1.537(5) . ?
N2 C20 1.482(5) . ?
C26 H26 0.9300 . ?
C26 C25 1.385(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.385(3) . ?
C33 H33 0.9800 . ?
C33 C34 1.503(3) . ?
C33 C37 1.525(3) . ?
C35 H35 0.9300 . ?
C35 C34 1.325(3) . ?
C35 C36 1.494(3) . ?
C34 H34 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.381(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.505(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C36 1.541(3) . ?
C36 H36 0.9800 . ?
C24 H24 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.497(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.480(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C20A C21A 1.485(7) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
C20 H20C 0.9700 . ?
C20 H20D 0.9700 . ?
C20 C21 1.524(7) . ?
C21 H21D 0.9600 . ?
C21 H21E 0.9600 . ?
C21 H21F 0.9600 . ?
O3S C4S 1.281(15) . ?
O3S C2S 1.454(16) . ?
O6S C4S 1.223(12) . ?
C5S H5SA 0.9600 . ?
C5S H5SB 0.9600 . ?
C5S H5SC 0.9600 . ?
C5S C4S 1.438(11) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C2S C1S 1.449(11) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 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
C9 O1 C13 118.30(12) . . ?
C28 N3 C11 113.86(12) . . ?
C28 N3 C29 124.08(12) . . ?
C29 N3 C11 121.92(11) . . ?
C31 N4 C30 123.82(14) . . ?
C31 N4 C39 113.31(13) . . ?
C39 N4 C30 122.80(13) . . ?
C5 N1 C3 120.77(15) . . ?
C5 N1 C2 120.28(15) . . ?
C3 N1 C2 117.76(15) . . ?
C9 C8 C11 122.47(13) . . ?
C9 C8 C7 115.83(13) . . ?
C7 C8 C11 121.70(13) . . ?
O1 C9 C8 123.02(13) . . ?
O1 C9 C10 114.48(13) . . ?
C8 C9 C10 122.49(14) . . ?
O2 C28 N3 125.76(15) . . ?
O2 C28 C27 127.86(14) . . ?
N3 C28 C27 106.39(13) . . ?
C13 C12 C11 122.71(13) . . ?
C13 C12 C17 115.92(14) . . ?
C17 C12 C11 121.36(14) . . ?
N3 C11 C8 110.96(11) . . ?
N3 C11 C12 111.07(12) . . ?
N3 C11 C22 100.00(11) . . ?
C8 C11 C22 111.58(12) . . ?
C12 C11 C8 109.85(12) . . ?
C12 C11 C22 113.08(12) . . ?
N1 C5 C10 121.55(15) . . ?
N1 C5 C6 121.61(15) . . ?
C10 C5 C6 116.83(14) . . ?
C27 C22 C11 110.70(14) . . ?
C27 C22 C23 120.93(16) . . ?
C23 C22 C11 128.35(16) . . ?
C22 C27 C28 109.04(13) . . ?
C22 C27 C26 121.52(17) . . ?
C26 C27 C28 129.44(17) . . ?
C9 C10 C5 121.19(14) . . ?
C9 C10 H10 119.4 . . ?
C5 C10 H10 119.4 . . ?
O1 C13 C12 123.00(14) . . ?
O1 C13 C14 114.61(14) . . ?
C12 C13 C14 122.39(15) . . ?
C8 C7 H7 118.5 . . ?
C6 C7 C8 123.04(15) . . ?
C6 C7 H7 118.5 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.58(15) . . ?
C7 C6 H6 119.7 . . ?
N3 C29 H29A 108.6 . . ?
N3 C29 H29B 108.6 . . ?
N3 C29 C30 114.81(12) . . ?
H29A C29 H29B 107.5 . . ?
C30 C29 H29A 108.6 . . ?
C30 C29 H29B 108.6 . . ?
N4 C31 C32 108.12(15) . . ?
O3 C31 N4 123.92(16) . . ?
O3 C31 C32 127.96(16) . . ?
C12 C17 H17 118.6 . . ?
C16 C17 C12 122.77(16) . . ?
C16 C17 H17 118.6 . . ?
N4 C30 C29 112.58(13) . . ?
N4 C30 H30A 109.1 . . ?
N4 C30 H30B 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C13 C14 H14 119.5 . . ?
C13 C14 C15 121.00(16) . . ?
C15 C14 H14 119.5 . . ?
N4 C39 C38 108.16(14) . . ?
O4 C39 N4 123.54(15) . . ?
O4 C39 C38 128.30(16) . . ?
C31 C32 H32 110.9 . . ?
C31 C32 C38 105.12(13) . . ?
C31 C32 C33 115.25(16) . . ?
C38 C32 H32 110.9 . . ?
C38 C32 C33 103.40(14) . . ?
C33 C32 H32 110.9 . . ?
C39 C38 C32 105.19(14) . . ?
C39 C38 H38 110.7 . . ?
C39 C38 C36 115.98(15) . . ?
C32 C38 H38 110.7 . . ?
C32 C38 C36 103.03(14) . . ?
C36 C38 H38 110.7 . . ?
C17 C16 H16 119.6 . . ?
C17 C16 C15 120.82(16) . . ?
C15 C16 H16 119.6 . . ?
C15 N2 C18 122.1(2) . . ?
C15 N2 C20A 118.7(2) . . ?
C15 N2 C20 118.9(2) . . ?
C18 N2 C20A 114.3(2) . . ?
C18 N2 C20 114.5(2) . . ?
C27 C26 H26 121.3 . . ?
C25 C26 C27 117.4(2) . . ?
C25 C26 H26 121.3 . . ?
C14 C15 C16 117.06(16) . . ?
N2 C15 C14 121.33(18) . . ?
N2 C15 C16 121.61(17) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 C22 117.7(2) . . ?
C24 C23 H23 121.1 . . ?
C32 C33 H33 116.2 . . ?
C34 C33 C32 106.22(14) . . ?
C34 C33 H33 116.2 . . ?
C34 C33 C37 100.27(17) . . ?
C37 C33 C32 99.20(16) . . ?
C37 C33 H33 116.2 . . ?
C34 C35 H35 125.9 . . ?
C34 C35 C36 108.21(19) . . ?
C36 C35 H35 125.9 . . ?
C33 C34 H34 126.3 . . ?
C35 C34 C33 107.5(2) . . ?
C35 C34 H34 126.3 . . ?
C26 C25 H25 119.4 . . ?
C24 C25 C26 121.16(18) . . ?
C24 C25 H25 119.4 . . ?
N1 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
N1 C3 C4 114.24(17) . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C33 C37 H37A 112.9 . . ?
C33 C37 H37B 112.9 . . ?
C33 C37 C36 94.10(15) . . ?
H37A C37 H37B 110.3 . . ?
C36 C37 H37A 112.9 . . ?
C36 C37 H37B 112.9 . . ?
C38 C36 H36 116.2 . . ?
C35 C36 C38 107.05(15) . . ?
C35 C36 C37 100.21(18) . . ?
C35 C36 H36 116.2 . . ?
C37 C36 C38 98.58(15) . . ?
C37 C36 H36 116.2 . . ?
C23 C24 H24 119.4 . . ?
C25 C24 C23 121.3(2) . . ?
C25 C24 H24 119.4 . . ?
N1 C2 H2A 108.5 . . ?
N1 C2 H2B 108.5 . . ?
N1 C2 C1 115.0(2) . . ?
H2A C2 H2B 107.5 . . ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C18 H18A 108.7 . . ?
N2 C18 H18B 108.7 . . ?
N2 C18 C19 114.1(3) . . ?
H18A C18 H18B 107.6 . . ?
C19 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20A H20A 110.5 . . ?
N2 C20A H20B 110.5 . . ?
H20A C20A H20B 108.7 . . ?
C21A C20A N2 106.1(4) . . ?
C21A C20A H20A 110.5 . . ?
C21A C20A H20B 110.5 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
N2 C20 H20C 110.3 . . ?
N2 C20 H20D 110.3 . . ?
N2 C20 C21 107.3(4) . . ?
H20C C20 H20D 108.5 . . ?
C21 C20 H20C 110.3 . . ?
C21 C20 H20D 110.3 . . ?
C20 C21 H21D 109.5 . . ?
C20 C21 H21E 109.5 . . ?
C20 C21 H21F 109.5 . . ?
H21D C21 H21E 109.5 . . ?
H21D C21 H21F 109.5 . . ?
H21E C21 H21F 109.5 . . ?
C4S O3S C2S 115.6(12) . . ?
H5SA C5S H5SB 109.5 . . ?
H5SA C5S H5SC 109.5 . . ?
H5SB C5S H5SC 109.5 . . ?
C4S C5S H5SA 109.5 . . ?
C4S C5S H5SB 109.5 . . ?
C4S C5S H5SC 109.5 . . ?
O3S C4S C5S 112.4(13) . . ?
O6S C4S O3S 119.5(13) . . ?
O6S C4S C5S 128.0(13) . . ?
O3S C2S H2SA 109.5 . . ?
O3S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 108.1 . . ?
C1S C2S O3S 110.8(12) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C9 C10 C5 179.07(14) . . . . ?
O1 C13 C14 C15 -179.58(16) . . . . ?
O2 C28 C27 C22 179.93(15) . . . . ?
O2 C28 C27 C26 0.0(3) . . . . ?
N3 C28 C27 C22 0.15(16) . . . . ?
N3 C28 C27 C26 -179.80(16) . . . . ?
N3 C11 C22 C27 0.80(15) . . . . ?
N3 C11 C22 C23 179.27(16) . . . . ?
N3 C29 C30 N4 -70.06(17) . . . . ?
N4 C31 C32 C38 -3.36(19) . . . . ?
N4 C31 C32 C33 -116.49(16) . . . . ?
N4 C39 C38 C32 -0.87(18) . . . . ?
N4 C39 C38 C36 112.23(17) . . . . ?
O3 C31 C32 C38 175.67(19) . . . . ?
O3 C31 C32 C33 62.5(3) . . . . ?
O4 C39 C38 C32 -179.99(19) . . . . ?
O4 C39 C38 C36 -66.9(3) . . . . ?
N1 C5 C10 C9 177.81(15) . . . . ?
N1 C5 C6 C7 -177.10(16) . . . . ?
C8 C9 C10 C5 -0.4(2) . . . . ?
C8 C11 C22 C27 -116.61(14) . . . . ?
C8 C11 C22 C23 61.9(2) . . . . ?
C8 C7 C6 C5 -1.1(3) . . . . ?
C9 O1 C13 C12 -6.5(2) . . . . ?
C9 O1 C13 C14 173.24(14) . . . . ?
C9 C8 C11 N3 116.31(15) . . . . ?
C9 C8 C11 C12 -6.9(2) . . . . ?
C9 C8 C11 C22 -133.11(15) . . . . ?
C9 C8 C7 C6 -0.5(2) . . . . ?
C28 N3 C11 C8 117.14(14) . . . . ?
C28 N3 C11 C12 -120.37(13) . . . . ?
C28 N3 C11 C22 -0.73(15) . . . . ?
C28 N3 C29 C30 82.66(18) . . . . ?
C28 C27 C26 C25 179.74(16) . . . . ?
C12 C11 C22 C27 118.96(14) . . . . ?
C12 C11 C22 C23 -62.6(2) . . . . ?
C12 C13 C14 C15 0.2(3) . . . . ?
C12 C17 C16 C15 -0.3(3) . . . . ?
C11 N3 C28 O2 -179.38(14) . . . . ?
C11 N3 C28 C27 0.40(16) . . . . ?
C11 N3 C29 C30 -101.95(15) . . . . ?
C11 C8 C9 O1 1.2(2) . . . . ?
C11 C8 C9 C10 -179.30(14) . . . . ?
C11 C8 C7 C6 -179.96(15) . . . . ?
C11 C12 C13 O1 0.0(2) . . . . ?
C11 C12 C13 C14 -179.72(15) . . . . ?
C11 C12 C17 C16 179.81(16) . . . . ?
C11 C22 C27 C28 -0.63(16) . . . . ?
C11 C22 C27 C26 179.33(14) . . . . ?
C11 C22 C23 C24 -178.91(16) . . . . ?
C5 N1 C3 C4 -72.5(2) . . . . ?
C5 N1 C2 C1 77.9(2) . . . . ?
C22 C27 C26 C25 -0.2(2) . . . . ?
C22 C23 C24 C25 -0.1(3) . . . . ?
C27 C22 C23 C24 -0.6(3) . . . . ?
C27 C26 C25 C24 -0.4(3) . . . . ?
C10 C5 C6 C7 1.8(2) . . . . ?
C13 O1 C9 C8 5.9(2) . . . . ?
C13 O1 C9 C10 -173.63(14) . . . . ?
C13 C12 C11 N3 -116.83(15) . . . . ?
C13 C12 C11 C8 6.3(2) . . . . ?
C13 C12 C11 C22 131.68(15) . . . . ?
C13 C12 C17 C16 -0.9(3) . . . . ?
C13 C14 C15 C16 -1.4(3) . . . . ?
C13 C14 C15 N2 178.6(2) . . . . ?
C7 C8 C9 O1 -178.25(14) . . . . ?
C7 C8 C9 C10 1.2(2) . . . . ?
C7 C8 C11 N3 -64.24(18) . . . . ?
C7 C8 C11 C12 172.56(14) . . . . ?
C7 C8 C11 C22 46.33(19) . . . . ?
C6 C5 C10 C9 -1.1(2) . . . . ?
C29 N3 C28 O2 -3.7(2) . . . . ?
C29 N3 C28 C27 176.12(13) . . . . ?
C29 N3 C11 C8 -58.69(17) . . . . ?
C29 N3 C11 C12 63.81(17) . . . . ?
C29 N3 C11 C22 -176.55(12) . . . . ?
C31 N4 C30 C29 104.17(18) . . . . ?
C31 N4 C39 O4 177.83(18) . . . . ?
C31 N4 C39 C38 -1.35(19) . . . . ?
C31 C32 C38 C39 2.51(18) . . . . ?
C31 C32 C38 C36 -119.41(15) . . . . ?
C31 C32 C33 C34 46.3(2) . . . . ?
C31 C32 C33 C37 149.93(16) . . . . ?
C17 C12 C11 N3 62.41(19) . . . . ?
C17 C12 C11 C8 -174.45(14) . . . . ?
C17 C12 C11 C22 -49.1(2) . . . . ?
C17 C12 C13 O1 -179.29(15) . . . . ?
C17 C12 C13 C14 1.0(2) . . . . ?
C17 C16 C15 C14 1.5(3) . . . . ?
C17 C16 C15 N2 -178.5(2) . . . . ?
C30 N4 C31 O3 7.1(3) . . . . ?
C30 N4 C31 C32 -173.86(14) . . . . ?
C30 N4 C39 O4 -5.2(3) . . . . ?
C30 N4 C39 C38 175.58(14) . . . . ?
C39 N4 C31 O3 -176.04(18) . . . . ?
C39 N4 C31 C32 3.03(19) . . . . ?
C39 N4 C30 C29 -72.44(19) . . . . ?
C39 C38 C36 C35 -49.2(2) . . . . ?
C39 C38 C36 C37 -152.68(17) . . . . ?
C32 C38 C36 C35 65.16(18) . . . . ?
C32 C38 C36 C37 -38.35(18) . . . . ?
C32 C33 C34 C35 69.0(2) . . . . ?
C32 C33 C37 C36 -58.87(17) . . . . ?
C38 C32 C33 C34 -67.81(19) . . . . ?
C38 C32 C33 C37 35.80(18) . . . . ?
C26 C25 C24 C23 0.6(3) . . . . ?
C15 N2 C18 C19 84.9(3) . . . . ?
C15 N2 C20A C21A 104.9(4) . . . . ?
C15 N2 C20 C21 -91.3(4) . . . . ?
C23 C22 C27 C28 -179.23(15) . . . . ?
C23 C22 C27 C26 0.7(2) . . . . ?
C33 C32 C38 C39 123.75(15) . . . . ?
C33 C32 C38 C36 1.83(18) . . . . ?
C33 C37 C36 C38 60.07(18) . . . . ?
C33 C37 C36 C35 -49.10(18) . . . . ?
C34 C33 C37 C36 49.60(17) . . . . ?
C34 C35 C36 C38 -70.4(2) . . . . ?
C34 C35 C36 C37 32.0(2) . . . . ?
C3 N1 C5 C10 169.67(16) . . . . ?
C3 N1 C5 C6 -11.5(3) . . . . ?
C3 N1 C2 C1 -89.7(2) . . . . ?
C37 C33 C34 C35 -33.82(19) . . . . ?
C36 C35 C34 C33 0.9(2) . . . . ?
C2 N1 C5 C10 2.4(3) . . . . ?
C2 N1 C5 C6 -178.76(17) . . . . ?
C2 N1 C3 C4 95.1(2) . . . . ?
C18 N2 C15 C14 172.7(2) . . . . ?
C18 N2 C15 C16 -7.3(4) . . . . ?
C18 N2 C20A C21A -99.4(4) . . . . ?
C18 N2 C20 C21 112.1(4) . . . . ?
C20A N2 C15 C14 -33.7(4) . . . . ?
C20A N2 C15 C16 146.3(3) . . . . ?
C20A N2 C18 C19 -69.8(3) . . . . ?
C20A N2 C20 C21 11.5(4) . . . . ?
C20 N2 C15 C14 18.0(4) . . . . ?
C20 N2 C15 C16 -162.0(3) . . . . ?
C20 N2 C18 C19 -119.5(3) . . . . ?
C20 N2 C20A C21A 1.6(4) . . . . ?
C4S O3S C2S C1S 176.2(10) . . . . ?
C2S O3S C4S O6S -0.8(19) . . . . ?
C2S O3S C4S C5S 176.8(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_ltb108-hjs1
_database_code_depnum_ccdc_archive 'CCDC 2005041'
loop_
_audit_author_name
_audit_author_address
'Helena J. Shepherd'
;School of Physical Sciences, University of Kent
United Kingdom
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;
_audit_creation_date             2019-02-01
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H42 N4 O4'
_chemical_formula_sum            'C39 H42 N4 O4'
_chemical_formula_weight         630.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H28 O4 N4'
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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.72214(17)
_cell_length_b                   19.9433(2)
_cell_length_c                   20.9335(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6563.71(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10027
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      72.9670
_cell_measurement_theta_min      4.4130
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 -2 1 0.0529
-1 0 13 0.0702
-10 2 -1 0.0386
1 0 -14 0.0876
10 1 -1 0.0570
1 -13 1 0.0368
-10 0 1 0.0254
0 13 -1 0.0681
-3 -7 -11 0.0653
3 7 11 0.0999

_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.085
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10.0868 -1.7486 0.9738 0.0980 0.1296 0.9867
-1.3913 0.1888 13.4641 0.5925 0.7729 -0.2273
-10.0560 1.7450 -1.4378 -0.1185 -0.1564 -0.9806
0.7371 -0.0753 -13.5570 -0.6001 -0.7830 0.1635
10.1333 0.6187 -1.4841 0.1308 -0.1254 0.9834
0.6455 -12.8715 1.1089 -0.7132 0.6755 0.1873
-10.1464 0.4695 1.3845 -0.0701 0.0679 -0.9952
0.1454 12.8868 -1.2217 0.7215 -0.6836 -0.1103
-3.0000 -7.0000 -11.0000 -0.9605 -0.3019 -0.1438
3.0000 7.0000 11.0000 0.9605 0.3019 0.1438

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23316
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.099
_diffrn_reflns_theta_min         4.157
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     76.00 121.00   1.00   10.00    --  105.91-125.00 150.00   45
  2  ω     72.00 108.00   1.00   10.00    --  105.91-118.00 -81.00   36
  3  ω     33.00 126.00   1.00   10.00    --  105.91 -45.00 -90.00   93
  4  ω     89.00 156.00   1.00   10.00    --  105.91  45.00 -60.00   67
  5  ω     97.00 146.00   1.00   10.00    --  105.91  45.00  60.00   49
  6  ω     95.00 164.00   1.00   10.00    --  105.91 125.00  30.00   69
  7  ω     98.00 145.00   1.00   10.00    --  105.91 125.00-120.00   47
  8  ω    -89.00  -9.00   1.00    2.50    --  -42.16 125.00-150.00   80
  9  ω   -115.00 -55.00   1.00    2.50    --  -42.16 -57.00 -90.00   60
 10  ω   -105.00 -55.00   1.00    2.50    --  -42.16 -57.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0158049000
_diffrn_orient_matrix_UB_12      0.0600573000
_diffrn_orient_matrix_UB_13      0.0447939000
_diffrn_orient_matrix_UB_21      -0.0009858000
_diffrn_orient_matrix_UB_22      -0.0475368000
_diffrn_orient_matrix_UB_23      0.0579663000
_diffrn_orient_matrix_UB_31      0.0966895000
_diffrn_orient_matrix_UB_32      -0.0102879000
_diffrn_orient_matrix_UB_33      -0.0067495000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus 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                5632
_reflns_number_total             6468
_reflns_odcompleteness_completeness 99.94
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+2.1360P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0948
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C38A \\sim N4-C38
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C38) = Uanis(C38A)
Uanis(C39) = Uanis(C39A)
4. Others
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C38A(H38C,H38D)
5.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F)
;
_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
O4 O 0.63415(5) 0.70302(4) 0.47955(4) 0.02200(18) Uani 1 1 d . . . . .
O3 O 0.35353(6) 0.78262(6) 0.67281(5) 0.0397(3) Uani 1 1 d . . . . .
O1 O 0.36760(8) 0.92156(5) 0.51732(5) 0.0390(2) Uani 1 1 d . . . . .
N2 N 0.45697(6) 0.76876(5) 0.59611(5) 0.0204(2) Uani 1 1 d . . . . .
N1 N 0.38033(6) 0.82044(5) 0.46660(5) 0.0229(2) Uani 1 1 d . . . . .
O2 O 0.39620(9) 0.73710(5) 0.39236(5) 0.0469(3) Uani 1 1 d . . . . .
N4 N 0.68760(7) 0.91297(5) 0.38007(5) 0.0246(2) Uani 1 1 d D . . . .
N3 N 0.63250(7) 0.48394(5) 0.56896(6) 0.0285(2) Uani 1 1 d . . . . .
C25 C 0.61476(7) 0.66431(6) 0.53226(5) 0.0182(2) Uani 1 1 d . . . . .
C12 C 0.55197(7) 0.76380(5) 0.59227(5) 0.0178(2) Uani 1 1 d . . . . .
C35 C 0.58412(7) 0.87310(6) 0.53425(6) 0.0196(2) Uani 1 1 d . . . . .
C33 C 0.65292(7) 0.87710(6) 0.43044(6) 0.0202(2) Uani 1 1 d . . . . .
C30 C 0.58733(7) 0.80286(6) 0.53646(5) 0.0179(2) Uani 1 1 d . . . . .
C15 C 0.57644(8) 0.79238(5) 0.65708(6) 0.0209(2) Uani 1 1 d . . . . .
C20 C 0.57750(7) 0.69063(5) 0.58679(5) 0.0177(2) Uani 1 1 d . . . . .
C31 C 0.62483(7) 0.77170(6) 0.48444(6) 0.0189(2) Uani 1 1 d . . . . .
C32 C 0.65701(8) 0.80696(6) 0.43237(6) 0.0211(2) Uani 1 1 d . . . . .
C23 C 0.61508(7) 0.55112(6) 0.57466(6) 0.0212(2) Uani 1 1 d . . . . .
C21 C 0.55926(7) 0.64489(6) 0.63552(6) 0.0207(2) Uani 1 1 d . . . . .
C24 C 0.63433(7) 0.59674(6) 0.52557(6) 0.0206(2) Uani 1 1 d . . . . .
C34 C 0.61561(7) 0.90966(6) 0.48367(6) 0.0204(2) Uani 1 1 d . . . . .
C22 C 0.57701(8) 0.57751(6) 0.63049(6) 0.0223(2) Uani 1 1 d . . . . .
C14 C 0.50444(9) 0.80258(6) 0.69405(6) 0.0265(3) Uani 1 1 d . . . . .
C11 C 0.40248(8) 0.73395(6) 0.55076(6) 0.0231(2) Uani 1 1 d . . . . .
C9 C 0.38788(8) 0.88947(6) 0.47081(6) 0.0252(3) Uani 1 1 d . . . . .
C17 C 0.65689(9) 0.80415(6) 0.68156(6) 0.0264(3) Uani 1 1 d . . . . .
C13 C 0.42820(8) 0.78476(6) 0.65582(6) 0.0270(3) Uani 1 1 d . . . . .
C10 C 0.34013(8) 0.77909(6) 0.51551(6) 0.0250(3) Uani 1 1 d . . . . .
C7 C 0.29852(8) 0.90087(7) 0.34318(6) 0.0274(3) Uani 1 1 d . . . . .
C28 C 0.67019(8) 0.45712(6) 0.51081(7) 0.0282(3) Uani 1 1 d . . . . .
C36 C 0.72561(9) 0.87643(7) 0.32675(6) 0.0277(3) Uani 1 1 d . . . . .
C6 C 0.42175(8) 0.91575(7) 0.40833(7) 0.0283(3) Uani 1 1 d . . . . .
C8 C 0.40324(9) 0.79547(7) 0.40713(6) 0.0293(3) Uani 1 1 d . . . . .
C5 C 0.43392(9) 0.85318(7) 0.36624(7) 0.0309(3) Uani 1 1 d . . . . .
C4 C 0.35368(9) 0.95740(7) 0.37077(7) 0.0296(3) Uani 1 1 d . . . . .
C26 C 0.60669(9) 0.43590(6) 0.61791(7) 0.0311(3) Uani 1 1 d . . . . .
C16 C 0.51054(11) 0.82259(8) 0.75765(7) 0.0370(3) Uani 1 1 d . . . . .
C38 C 0.65582(11) 0.98008(7) 0.36313(7) 0.0252(3) Uani 0.914(3) 1 d D . P A 1
H38A H 0.6189 0.9959 0.3971 0.030 Uiso 0.914(3) 1 calc R . P A 1
H38B H 0.6219 0.9766 0.3245 0.030 Uiso 0.914(3) 1 calc R . P A 1
C19 C 0.66338(10) 0.82578(7) 0.74480(7) 0.0342(3) Uani 1 1 d . . . . .
C3 C 0.37306(9) 0.86655(8) 0.30832(6) 0.0330(3) Uani 1 1 d . . . . .
C37 C 0.66047(11) 0.84695(8) 0.28105(7) 0.0358(3) Uani 1 1 d . . . . .
C29 C 0.60568(10) 0.44792(7) 0.45744(8) 0.0349(3) Uani 1 1 d . . . . .
C18 C 0.59092(11) 0.83437(7) 0.78230(7) 0.0396(4) Uani 1 1 d . . . . .
C2 C 0.39867(10) 0.98035(8) 0.31055(8) 0.0402(4) Uani 1 1 d . . . . .
C1 C 0.41023(10) 0.92673(9) 0.27401(7) 0.0423(4) Uani 1 1 d . . . . .
C27 C 0.67110(12) 0.43014(9) 0.67151(10) 0.0500(4) Uani 1 1 d . . . . .
C39 C 0.72585(11) 1.03134(8) 0.35241(8) 0.0378(4) Uani 0.914(3) 1 d D . P A 1
H39A H 0.7618 1.0168 0.3180 0.057 Uiso 0.914(3) 1 calc GR . P A 1
H39B H 0.7591 1.0358 0.3907 0.057 Uiso 0.914(3) 1 calc GR . P A 1
H39C H 0.7010 1.0739 0.3418 0.057 Uiso 0.914(3) 1 calc GR . P A 1
H28A H 0.7158(10) 0.4861(8) 0.4963(7) 0.028(4) Uiso 1 1 d . . . . .
H21 H 0.5335(9) 0.6612(7) 0.6753(7) 0.020(3) Uiso 1 1 d . . . . .
H22 H 0.5646(10) 0.5487(8) 0.6663(7) 0.027(4) Uiso 1 1 d . . . . .
H34 H 0.6139(9) 0.9581(7) 0.4855(6) 0.018(3) Uiso 1 1 d . . . . .
H32 H 0.6812(10) 0.7814(8) 0.3983(8) 0.028(4) Uiso 1 1 d . . . . .
H7A H 0.2703(10) 0.8724(8) 0.3769(7) 0.027(4) Uiso 1 1 d . . . . .
H24 H 0.6605(9) 0.5843(7) 0.4859(7) 0.023(4) Uiso 1 1 d . . . . .
H36A H 0.7632(10) 0.9083(8) 0.3036(8) 0.031(4) Uiso 1 1 d . . . . .
H35 H 0.5588(9) 0.8967(7) 0.5696(7) 0.021(3) Uiso 1 1 d . . . . .
H11A H 0.4394(10) 0.7099(7) 0.5181(7) 0.024(4) Uiso 1 1 d . . . . .
H28B H 0.6966(11) 0.4127(8) 0.5220(8) 0.035(4) Uiso 1 1 d . . . . .
H17 H 0.7084(11) 0.7953(8) 0.6563(8) 0.030(4) Uiso 1 1 d . . . . .
H4 H 0.3249(11) 0.9918(9) 0.3977(8) 0.038(4) Uiso 1 1 d . . . . .
H36B H 0.7656(10) 0.8385(8) 0.3415(8) 0.033(4) Uiso 1 1 d . . . . .
H10A H 0.2976(11) 0.7503(9) 0.4931(8) 0.036(4) Uiso 1 1 d . . . . .
H26A H 0.5495(11) 0.4478(8) 0.6351(7) 0.031(4) Uiso 1 1 d . . . . .
H7B H 0.2554(10) 0.9173(8) 0.3134(8) 0.031(4) Uiso 1 1 d . . . . .
H6 H 0.4722(11) 0.9419(8) 0.4159(8) 0.034(4) Uiso 1 1 d . . . . .
H29A H 0.5796(11) 0.4933(9) 0.4450(9) 0.043(5) Uiso 1 1 d . . . . .
H26B H 0.5997(11) 0.3923(9) 0.5957(8) 0.036(4) Uiso 1 1 d . . . . .
H16 H 0.4611(12) 0.8261(9) 0.7834(9) 0.045(5) Uiso 1 1 d . . . . .
H10B H 0.3116(10) 0.8084(8) 0.5456(8) 0.031(4) Uiso 1 1 d . . . . .
H19 H 0.7204(12) 0.8327(9) 0.7634(9) 0.042(5) Uiso 1 1 d . . . . .
H11B H 0.3688(10) 0.6996(8) 0.5738(7) 0.027(4) Uiso 1 1 d . . . . .
H5 H 0.4922(12) 0.8458(9) 0.3543(8) 0.038(4) Uiso 1 1 d . . . . .
H3 H 0.3606(11) 0.8260(9) 0.2832(8) 0.038(4) Uiso 1 1 d . . . . .
H29B H 0.5601(13) 0.4173(10) 0.4720(9) 0.050(5) Uiso 1 1 d . . . . .
H37A H 0.6226(11) 0.8139(9) 0.3037(9) 0.042(5) Uiso 1 1 d . . . . .
H37B H 0.6244(12) 0.8840(10) 0.2638(9) 0.048(5) Uiso 1 1 d . . . . .
H2 H 0.4182(12) 1.0271(10) 0.3032(9) 0.052(5) Uiso 1 1 d . . . . .
H1 H 0.4404(14) 0.9231(10) 0.2328(10) 0.057(6) Uiso 1 1 d . . . . .
H37C H 0.6910(14) 0.8248(10) 0.2448(11) 0.059(6) Uiso 1 1 d . . . . .
H18 H 0.5957(13) 0.8488(10) 0.8273(10) 0.054(5) Uiso 1 1 d . . . . .
H29C H 0.6339(12) 0.4293(9) 0.4190(9) 0.048(5) Uiso 1 1 d . . . . .
H27A H 0.6785(14) 0.4762(12) 0.6947(11) 0.067(6) Uiso 1 1 d . . . . .
H27B H 0.7260(17) 0.4175(12) 0.6519(11) 0.075(7) Uiso 1 1 d . . . . .
H27C H 0.6553(15) 0.3944(12) 0.7022(11) 0.069(7) Uiso 1 1 d . . . . .
C38A C 0.6955(11) 0.9854(6) 0.3720(8) 0.0252(3) Uani 0.086(3) 1 d D . P A 2
H38C H 0.7456 0.9946 0.3464 0.030 Uiso 0.086(3) 1 calc R . P A 2
H38D H 0.7040 1.0057 0.4136 0.030 Uiso 0.086(3) 1 calc R . P A 2
C39A C 0.6182(11) 1.0184(8) 0.3399(9) 0.0378(4) Uani 0.086(3) 1 d D . P A 2
H39D H 0.6102 0.9995 0.2982 0.057 Uiso 0.086(3) 1 calc GR . P A 2
H39E H 0.6277 1.0658 0.3363 0.057 Uiso 0.086(3) 1 calc GR . P A 2
H39F H 0.5684 1.0105 0.3654 0.057 Uiso 0.086(3) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C25 1.3807(14) . ?
O4 C31 1.3813(14) . ?
O3 C13 1.2273(16) . ?
O1 C9 1.2078(17) . ?
N2 C12 1.4989(14) . ?
N2 C11 1.4551(16) . ?
N2 C13 1.3671(16) . ?
N1 C9 1.3846(16) . ?
N1 C10 1.4589(16) . ?
N1 C8 1.3883(17) . ?
O2 C8 1.2094(18) . ?
N4 C33 1.3859(15) . ?
N4 C36 1.4607(16) . ?
N4 C38 1.4721(17) . ?
N4 C38A 1.459(13) . ?
N3 C23 1.3727(15) . ?
N3 C28 1.4557(17) . ?
N3 C26 1.4605(17) . ?
C25 C20 1.3863(16) . ?
C25 C24 1.3894(16) . ?
C12 C30 1.5104(15) . ?
C12 C15 1.5210(16) . ?
C12 C20 1.5178(15) . ?
C35 C30 1.4025(16) . ?
C35 C34 1.3776(17) . ?
C35 H35 0.962(15) . ?
C33 C32 1.4009(16) . ?
C33 C34 1.4170(17) . ?
C30 C31 1.3855(16) . ?
C15 C14 1.3862(18) . ?
C15 C17 1.3848(18) . ?
C20 C21 1.3981(16) . ?
C31 C32 1.3924(16) . ?
C32 H32 0.956(16) . ?
C23 C24 1.4055(17) . ?
C23 C22 1.4147(17) . ?
C21 C22 1.3765(17) . ?
C21 H21 0.980(15) . ?
C24 H24 0.959(15) . ?
C34 H34 0.967(15) . ?
C22 H22 0.964(16) . ?
C14 C13 1.4844(19) . ?
C14 C16 1.3932(19) . ?
C11 C10 1.5218(17) . ?
C11 H11A 1.017(15) . ?
C11 H11B 0.990(16) . ?
C9 C6 1.5064(18) . ?
C17 C19 1.3959(19) . ?
C17 H17 0.984(17) . ?
C10 H10A 0.999(18) . ?
C10 H10B 0.970(17) . ?
C7 C4 1.5352(19) . ?
C7 C3 1.5410(18) . ?
C7 H7A 1.010(16) . ?
C7 H7B 0.978(17) . ?
C28 C29 1.520(2) . ?
C28 H28A 0.969(16) . ?
C28 H28B 1.007(17) . ?
C36 C37 1.520(2) . ?
C36 H36A 0.994(17) . ?
C36 H36B 1.032(17) . ?
C6 C5 1.540(2) . ?
C6 C4 1.5664(17) . ?
C6 H6 0.962(17) . ?
C8 C5 1.5133(19) . ?
C5 C3 1.5673(19) . ?
C5 H5 0.961(18) . ?
C4 C2 1.516(2) . ?
C4 H4 0.997(18) . ?
C26 C27 1.516(2) . ?
C26 H26A 0.997(17) . ?
C26 H26B 0.991(18) . ?
C16 C18 1.385(2) . ?
C16 H16 0.948(19) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.519(2) . ?
C19 C18 1.394(2) . ?
C19 H19 0.986(19) . ?
C3 C1 1.516(2) . ?
C3 H3 0.984(18) . ?
C37 H37A 1.007(19) . ?
C37 H37B 1.00(2) . ?
C37 H37C 1.00(2) . ?
C29 H29A 1.027(19) . ?
C29 H29B 0.99(2) . ?
C29 H29C 0.99(2) . ?
C18 H18 0.99(2) . ?
C2 C1 1.327(3) . ?
C2 H2 0.99(2) . ?
C1 H1 0.99(2) . ?
C27 H27A 1.04(2) . ?
C27 H27B 0.99(3) . ?
C27 H27C 0.99(2) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C38A H38C 0.9700 . ?
C38A H38D 0.9700 . ?
C38A C39A 1.536(16) . ?
C39A H39D 0.9600 . ?
C39A H39E 0.9600 . ?
C39A H39F 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
C25 O4 C31 118.14(9) . . ?
C11 N2 C12 121.35(9) . . ?
C13 N2 C12 113.21(10) . . ?
C13 N2 C11 120.86(10) . . ?
C9 N1 C10 123.67(11) . . ?
C9 N1 C8 113.06(11) . . ?
C8 N1 C10 122.61(11) . . ?
C33 N4 C36 119.00(10) . . ?
C33 N4 C38 121.27(11) . . ?
C33 N4 C38A 129.3(7) . . ?
C36 N4 C38 114.10(10) . . ?
C38A N4 C36 111.7(7) . . ?
C23 N3 C28 120.84(11) . . ?
C23 N3 C26 121.59(11) . . ?
C28 N3 C26 117.30(10) . . ?
O4 C25 C20 122.67(10) . . ?
O4 C25 C24 114.38(10) . . ?
C20 C25 C24 122.94(11) . . ?
N2 C12 C30 111.97(9) . . ?
N2 C12 C15 100.34(9) . . ?
N2 C12 C20 109.33(9) . . ?
C30 C12 C15 113.80(9) . . ?
C30 C12 C20 109.88(9) . . ?
C20 C12 C15 111.15(9) . . ?
C30 C35 H35 118.5(9) . . ?
C34 C35 C30 122.75(11) . . ?
C34 C35 H35 118.8(9) . . ?
N4 C33 C32 121.29(11) . . ?
N4 C33 C34 121.65(11) . . ?
C32 C33 C34 116.99(10) . . ?
C35 C30 C12 121.83(10) . . ?
C31 C30 C12 122.22(10) . . ?
C31 C30 C35 115.95(10) . . ?
C14 C15 C12 110.27(11) . . ?
C17 C15 C12 128.66(11) . . ?
C17 C15 C14 120.96(12) . . ?
C25 C20 C12 122.55(10) . . ?
C25 C20 C21 116.13(10) . . ?
C21 C20 C12 121.19(10) . . ?
O4 C31 C30 123.25(10) . . ?
O4 C31 C32 113.84(10) . . ?
C30 C31 C32 122.91(11) . . ?
C33 C32 H32 122.0(9) . . ?
C31 C32 C33 120.69(11) . . ?
C31 C32 H32 117.3(9) . . ?
N3 C23 C24 121.69(11) . . ?
N3 C23 C22 121.29(11) . . ?
C24 C23 C22 117.02(11) . . ?
C20 C21 H21 119.2(8) . . ?
C22 C21 C20 122.65(11) . . ?
C22 C21 H21 118.1(8) . . ?
C25 C24 C23 120.43(11) . . ?
C25 C24 H24 115.6(9) . . ?
C23 C24 H24 123.9(9) . . ?
C35 C34 C33 120.72(11) . . ?
C35 C34 H34 119.2(8) . . ?
C33 C34 H34 120.1(8) . . ?
C23 C22 H22 120.4(9) . . ?
C21 C22 C23 120.81(11) . . ?
C21 C22 H22 118.8(9) . . ?
C15 C14 C13 108.87(11) . . ?
C15 C14 C16 121.28(13) . . ?
C16 C14 C13 129.74(13) . . ?
N2 C11 C10 114.41(10) . . ?
N2 C11 H11A 109.1(8) . . ?
N2 C11 H11B 109.1(9) . . ?
C10 C11 H11A 108.6(8) . . ?
C10 C11 H11B 107.5(9) . . ?
H11A C11 H11B 107.9(12) . . ?
O1 C9 N1 123.75(12) . . ?
O1 C9 C6 127.50(12) . . ?
N1 C9 C6 108.72(11) . . ?
C15 C17 C19 118.04(13) . . ?
C15 C17 H17 121.5(9) . . ?
C19 C17 H17 120.3(9) . . ?
O3 C13 N2 124.99(13) . . ?
O3 C13 C14 128.64(12) . . ?
N2 C13 C14 106.35(10) . . ?
N1 C10 C11 113.31(10) . . ?
N1 C10 H10A 106.6(10) . . ?
N1 C10 H10B 108.4(9) . . ?
C11 C10 H10A 108.6(10) . . ?
C11 C10 H10B 109.9(10) . . ?
H10A C10 H10B 110.0(13) . . ?
C4 C7 C3 94.28(11) . . ?
C4 C7 H7A 113.5(9) . . ?
C4 C7 H7B 112.7(9) . . ?
C3 C7 H7A 114.6(9) . . ?
C3 C7 H7B 112.0(9) . . ?
H7A C7 H7B 109.2(13) . . ?
N3 C28 C29 112.79(11) . . ?
N3 C28 H28A 110.1(9) . . ?
N3 C28 H28B 107.3(10) . . ?
C29 C28 H28A 109.6(9) . . ?
C29 C28 H28B 109.9(10) . . ?
H28A C28 H28B 107.0(13) . . ?
N4 C36 C37 113.46(12) . . ?
N4 C36 H36A 107.3(9) . . ?
N4 C36 H36B 112.7(9) . . ?
C37 C36 H36A 110.0(9) . . ?
C37 C36 H36B 108.4(9) . . ?
H36A C36 H36B 104.7(13) . . ?
C9 C6 C5 105.00(10) . . ?
C9 C6 C4 112.26(11) . . ?
C9 C6 H6 109.6(10) . . ?
C5 C6 C4 103.14(11) . . ?
C5 C6 H6 115.5(10) . . ?
C4 C6 H6 111.1(10) . . ?
N1 C8 C5 108.48(11) . . ?
O2 C8 N1 123.42(13) . . ?
O2 C8 C5 128.07(13) . . ?
C6 C5 C3 103.24(11) . . ?
C6 C5 H5 113.1(10) . . ?
C8 C5 C6 104.66(11) . . ?
C8 C5 C3 111.85(12) . . ?
C8 C5 H5 109.5(10) . . ?
C3 C5 H5 114.0(10) . . ?
C7 C4 C6 100.69(10) . . ?
C7 C4 H4 117.6(10) . . ?
C6 C4 H4 113.0(10) . . ?
C2 C4 C7 99.92(11) . . ?
C2 C4 C6 104.99(11) . . ?
C2 C4 H4 118.3(10) . . ?
N3 C26 C27 112.55(12) . . ?
N3 C26 H26A 110.4(9) . . ?
N3 C26 H26B 106.1(10) . . ?
C27 C26 H26A 110.6(9) . . ?
C27 C26 H26B 110.8(10) . . ?
H26A C26 H26B 106.2(13) . . ?
C14 C16 H16 120.5(11) . . ?
C18 C16 C14 117.86(14) . . ?
C18 C16 H16 121.6(11) . . ?
N4 C38 H38A 108.8 . . ?
N4 C38 H38B 108.8 . . ?
N4 C38 C39 113.67(14) . . ?
H38A C38 H38B 107.7 . . ?
C39 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C17 C19 H19 118.9(11) . . ?
C18 C19 C17 120.80(14) . . ?
C18 C19 H19 120.2(10) . . ?
C7 C3 C5 100.00(10) . . ?
C7 C3 H3 117.8(10) . . ?
C5 C3 H3 113.2(10) . . ?
C1 C3 C7 99.54(12) . . ?
C1 C3 C5 105.42(12) . . ?
C1 C3 H3 118.3(10) . . ?
C36 C37 H37A 110.9(10) . . ?
C36 C37 H37B 108.9(11) . . ?
C36 C37 H37C 108.9(12) . . ?
H37A C37 H37B 108.6(15) . . ?
H37A C37 H37C 110.5(15) . . ?
H37B C37 H37C 109.0(16) . . ?
C28 C29 H29A 110.3(10) . . ?
C28 C29 H29B 109.4(11) . . ?
C28 C29 H29C 110.1(11) . . ?
H29A C29 H29B 109.5(15) . . ?
H29A C29 H29C 107.6(15) . . ?
H29B C29 H29C 110.0(15) . . ?
C16 C18 C19 121.00(13) . . ?
C16 C18 H18 118.3(12) . . ?
C19 C18 H18 120.7(12) . . ?
C4 C2 H2 123.8(12) . . ?
C1 C2 C4 107.45(13) . . ?
C1 C2 H2 128.6(12) . . ?
C3 C1 H1 122.7(12) . . ?
C2 C1 C3 108.19(13) . . ?
C2 C1 H1 129.0(12) . . ?
C26 C27 H27A 110.6(12) . . ?
C26 C27 H27B 107.1(14) . . ?
C26 C27 H27C 111.5(14) . . ?
H27A C27 H27B 108.6(18) . . ?
H27A C27 H27C 111.0(18) . . ?
H27B C27 H27C 107.8(18) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N4 C38A H38C 108.7 . . ?
N4 C38A H38D 108.7 . . ?
N4 C38A C39A 114.1(13) . . ?
H38C C38A H38D 107.6 . . ?
C39A C38A H38C 108.7 . . ?
C39A C38A H38D 108.7 . . ?
C38A C39A H39D 109.5 . . ?
C38A C39A H39E 109.5 . . ?
C38A C39A H39F 109.5 . . ?
H39D C39A H39E 109.5 . . ?
H39D C39A H39F 109.5 . . ?
H39E C39A H39F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 C25 C20 C12 2.23(17) . . . . ?
O4 C25 C20 C21 178.11(10) . . . . ?
O4 C25 C24 C23 -177.66(10) . . . . ?
O4 C31 C32 C33 -179.51(10) . . . . ?
O1 C9 C6 C5 -178.31(13) . . . . ?
O1 C9 C6 C4 -66.97(18) . . . . ?
N2 C12 C30 C35 67.82(13) . . . . ?
N2 C12 C30 C31 -112.18(12) . . . . ?
N2 C12 C15 C14 7.29(12) . . . . ?
N2 C12 C15 C17 -176.71(11) . . . . ?
N2 C12 C20 C25 113.10(11) . . . . ?
N2 C12 C20 C21 -62.57(13) . . . . ?
N2 C11 C10 N1 74.00(14) . . . . ?
N1 C9 C6 C5 -0.28(13) . . . . ?
N1 C9 C6 C4 111.07(12) . . . . ?
N1 C8 C5 C6 -2.77(14) . . . . ?
N1 C8 C5 C3 -113.87(12) . . . . ?
O2 C8 C5 C6 175.17(14) . . . . ?
O2 C8 C5 C3 64.07(19) . . . . ?
N4 C33 C32 C31 177.50(11) . . . . ?
N4 C33 C34 C35 -177.76(11) . . . . ?
N3 C23 C24 C25 178.99(11) . . . . ?
N3 C23 C22 C21 -179.53(12) . . . . ?
C25 O4 C31 C30 -8.23(16) . . . . ?
C25 O4 C31 C32 171.46(10) . . . . ?
C25 C20 C21 C22 0.13(17) . . . . ?
C12 N2 C11 C10 -124.45(11) . . . . ?
C12 N2 C13 O3 -169.44(12) . . . . ?
C12 N2 C13 C14 9.06(13) . . . . ?
C12 C30 C31 O4 -0.95(17) . . . . ?
C12 C30 C31 C32 179.39(11) . . . . ?
C12 C15 C14 C13 -2.59(13) . . . . ?
C12 C15 C14 C16 173.97(12) . . . . ?
C12 C15 C17 C19 -174.84(11) . . . . ?
C12 C20 C21 C22 176.07(11) . . . . ?
C35 C30 C31 O4 179.04(10) . . . . ?
C35 C30 C31 C32 -0.61(17) . . . . ?
C33 N4 C36 C37 77.11(15) . . . . ?
C33 N4 C38 C39 133.26(13) . . . . ?
C33 N4 C38A C39A -88.7(14) . . . . ?
C30 C12 C15 C14 127.04(11) . . . . ?
C30 C12 C15 C17 -56.97(16) . . . . ?
C30 C12 C20 C25 -10.17(15) . . . . ?
C30 C12 C20 C21 174.16(10) . . . . ?
C30 C35 C34 C33 0.39(18) . . . . ?
C30 C31 C32 C33 0.18(18) . . . . ?
C15 C12 C30 C35 -45.10(14) . . . . ?
C15 C12 C30 C31 134.90(11) . . . . ?
C15 C12 C20 C25 -137.04(11) . . . . ?
C15 C12 C20 C21 47.28(14) . . . . ?
C15 C14 C13 O3 174.58(13) . . . . ?
C15 C14 C13 N2 -3.85(14) . . . . ?
C15 C14 C16 C18 2.3(2) . . . . ?
C15 C17 C19 C18 0.8(2) . . . . ?
C20 C25 C24 C23 1.25(18) . . . . ?
C20 C12 C30 C35 -170.47(10) . . . . ?
C20 C12 C30 C31 9.52(15) . . . . ?
C20 C12 C15 C14 -108.27(11) . . . . ?
C20 C12 C15 C17 67.73(15) . . . . ?
C20 C21 C22 C23 -0.11(19) . . . . ?
C31 O4 C25 C20 7.55(16) . . . . ?
C31 O4 C25 C24 -173.55(10) . . . . ?
C32 C33 C34 C35 -0.82(17) . . . . ?
C23 N3 C28 C29 -79.07(15) . . . . ?
C23 N3 C26 C27 -85.77(17) . . . . ?
C24 C25 C20 C12 -176.58(11) . . . . ?
C24 C25 C20 C21 -0.70(17) . . . . ?
C24 C23 C22 C21 0.60(17) . . . . ?
C34 C35 C30 C12 -179.67(11) . . . . ?
C34 C35 C30 C31 0.33(17) . . . . ?
C34 C33 C32 C31 0.55(17) . . . . ?
C22 C23 C24 C25 -1.14(17) . . . . ?
C14 C15 C17 C19 0.79(18) . . . . ?
C14 C16 C18 C19 -0.7(2) . . . . ?
C11 N2 C12 C30 72.63(13) . . . . ?
C11 N2 C12 C15 -166.30(9) . . . . ?
C11 N2 C12 C20 -49.38(13) . . . . ?
C11 N2 C13 O3 -13.14(19) . . . . ?
C11 N2 C13 C14 165.37(10) . . . . ?
C9 N1 C10 C11 -111.71(13) . . . . ?
C9 N1 C8 O2 -175.26(13) . . . . ?
C9 N1 C8 C5 2.80(14) . . . . ?
C9 C6 C5 C8 1.80(13) . . . . ?
C9 C6 C5 C3 118.99(11) . . . . ?
C9 C6 C4 C7 -77.37(13) . . . . ?
C9 C6 C4 C2 179.21(12) . . . . ?
C17 C15 C14 C13 -178.95(11) . . . . ?
C17 C15 C14 C16 -2.38(19) . . . . ?
C17 C19 C18 C16 -0.9(2) . . . . ?
C13 N2 C12 C30 -131.19(10) . . . . ?
C13 N2 C12 C15 -10.12(12) . . . . ?
C13 N2 C12 C20 106.79(11) . . . . ?
C13 N2 C11 C10 81.17(14) . . . . ?
C13 C14 C16 C18 178.04(13) . . . . ?
C10 N1 C9 O1 5.63(19) . . . . ?
C10 N1 C9 C6 -172.49(10) . . . . ?
C10 N1 C8 O2 -4.2(2) . . . . ?
C10 N1 C8 C5 173.82(10) . . . . ?
C7 C4 C2 C1 -33.59(15) . . . . ?
C7 C3 C1 C2 32.90(15) . . . . ?
C28 N3 C23 C24 -1.34(18) . . . . ?
C28 N3 C23 C22 178.81(11) . . . . ?
C28 N3 C26 C27 100.06(16) . . . . ?
C36 N4 C33 C32 2.81(17) . . . . ?
C36 N4 C33 C34 179.62(11) . . . . ?
C36 N4 C38 C39 -73.48(15) . . . . ?
C36 N4 C38A C39A 93.6(13) . . . . ?
C6 C5 C3 C7 -37.02(13) . . . . ?
C6 C5 C3 C1 65.87(13) . . . . ?
C6 C4 C2 C1 70.41(15) . . . . ?
C8 N1 C9 O1 176.55(13) . . . . ?
C8 N1 C9 C6 -1.58(14) . . . . ?
C8 N1 C10 C11 78.22(15) . . . . ?
C8 C5 C3 C7 74.97(14) . . . . ?
C8 C5 C3 C1 177.87(12) . . . . ?
C5 C6 C4 C7 35.13(13) . . . . ?
C5 C6 C4 C2 -68.29(13) . . . . ?
C5 C3 C1 C2 -70.33(15) . . . . ?
C4 C7 C3 C5 57.75(12) . . . . ?
C4 C7 C3 C1 -49.91(12) . . . . ?
C4 C6 C5 C8 -115.92(11) . . . . ?
C4 C6 C5 C3 1.26(13) . . . . ?
C4 C2 C1 C3 0.30(16) . . . . ?
C26 N3 C23 C24 -175.30(12) . . . . ?
C26 N3 C23 C22 4.84(19) . . . . ?
C26 N3 C28 C29 95.14(14) . . . . ?
C16 C14 C13 O3 -1.6(2) . . . . ?
C16 C14 C13 N2 179.97(13) . . . . ?
C38 N4 C33 C32 154.80(12) . . . . ?
C38 N4 C33 C34 -28.39(18) . . . . ?
C38 N4 C36 C37 -76.80(15) . . . . ?
C3 C7 C4 C6 -57.16(12) . . . . ?
C3 C7 C4 C2 50.31(12) . . . . ?
C38A N4 C33 C32 -174.7(9) . . . . ?
C38A N4 C33 C34 2.1(9) . . . . ?
C38A N4 C36 C37 -104.9(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.237
_oxdiff_exptl_absorpt_empirical_full_min 0.891
