# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_rottschaefer61
_database_code_depnum_ccdc_archive 'CCDC 1826567'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_audit_creation_date             2017-12-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H80 N4, 2(I), 2(C H4 O)'
_chemical_formula_sum            'C62 H88 I2 N4 O2'
_chemical_formula_weight         1175.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C62 H88 I1 N4 O2'
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'
I I -0.4742 1.8119 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.01776(12)
_cell_length_b                   11.68842(10)
_cell_length_c                   18.61137(19)
_cell_angle_alpha                90
_cell_angle_beta                 97.6225(9)
_cell_angle_gamma                90
_cell_volume                     3022.44(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    68766
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      31.8190
_cell_measurement_theta_min      2.0570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1220
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 0 5 0.1022
3 0 -5 0.1022
2 5 -2 0.1403
-2 -5 2 0.1403
4 0 5 0.1425
-4 0 -5 0.1425
5 -1 -5 0.1202
-1 3 5 0.1689

_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.204
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
-3.0008 0.0006 5.0018 0.1918 0.1142 -0.0530
3.0008 -0.0006 -5.0018 -0.1918 -0.1142 0.0530
2.0005 4.9994 -2.0030 -0.2150 0.1981 0.1443
-2.0005 -4.9994 2.0030 0.2150 -0.1981 -0.1443
3.9987 0.0012 4.9982 -0.1010 0.1113 -0.2577
-3.9987 -0.0012 -4.9982 0.1010 -0.1113 0.2577
5.0006 -1.0004 -5.0025 -0.2546 -0.1638 -0.0348
-1.0008 3.0005 4.9997 0.0453 0.2598 -0.0236

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            171581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.028
_diffrn_reflns_theta_min         1.714
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00   5.00   1.00    1.25    --  -23.50 -77.00   0.00   98
  2  ω      6.00  93.00   1.00    1.25    --   24.78  57.00  60.00   87
  3  ω      6.00  93.00   1.00    1.25    --   24.78  57.00-120.00   87
  4  ω    -20.00  65.00   1.00    1.25    --   24.78 -99.00-150.00   85
  5  ω      6.00  93.00   1.00    1.25    --   24.78  57.00 150.00   87
  6  ω    -44.00  43.00   1.00    1.25    --   24.78 -57.00  90.00   87
  7  ω      6.00  83.00   1.00    1.25    --   24.78-130.00  58.60   77
  8  ω     -4.00  94.00   1.00    1.25    --   24.78  77.00 -60.00   98
  9  ω    -44.00  43.00   1.00    1.25    --   24.78 -57.00   0.00   87
 10  ω    -44.00  43.00   1.00    1.25    --   24.78 -57.00 -90.00   87
 11  ω    -95.00  48.00   1.00    1.25    --  -23.50   0.00-180.00  143
 12  ω    -95.00  48.00   1.00    1.25    --  -23.50   0.00-150.00  143
 13  ω     -4.00  94.00   1.00    1.25    --   24.78  77.00-180.00   98
 14  ω      3.00  95.00   1.00    1.25    --   24.78  38.00 120.00   92
 15  ω      6.00  93.00   1.00    1.25    --   24.78  57.00 130.00   87
 16  ω      6.00  93.00   1.00    1.25    --   24.78  57.00   0.00   87
 17  ω    -20.00  65.00   1.00    1.25    --   24.78 -99.00  90.00   85
 18  ω    -10.00  72.00   1.00    1.25    --   24.78-111.00-111.39   82
 19  ω    -46.00  47.00   1.00    1.25    --   24.78 -38.00 150.00   93
 20  ω    -95.00  48.00   1.00    1.25    --  -23.50   0.00 -90.00  143
 21  ω    -95.00  48.00   1.00    1.25    --  -23.50   0.00 -60.00  143
 22  ω    -95.00  48.00   1.00    1.25    --  -23.50   0.00 -30.00  143
 23  ω    -95.00  48.00   1.00    1.25    --  -23.50   0.00-120.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0418293000
_diffrn_orient_matrix_UB_12      -0.0209447000
_diffrn_orient_matrix_UB_13      0.0132613000
_diffrn_orient_matrix_UB_21      -0.0003972000
_diffrn_orient_matrix_UB_22      0.0488355000
_diffrn_orient_matrix_UB_23      0.0225820000
_diffrn_orient_matrix_UB_31      -0.0292732000
_diffrn_orient_matrix_UB_32      0.0292949000
_diffrn_orient_matrix_UB_33      -0.0281546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8020
_reflns_number_total             8848
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         8848
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0220
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0176P)²+1.7845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0499
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
N1 N 0.26909(7) 0.51231(8) 0.58241(5) 0.01220(18) Uani 1 1 d . . . . .
N2 N 0.38393(7) 0.45233(8) 0.66720(5) 0.01143(17) Uani 1 1 d . . . . .
C1 C 0.35998(8) 0.48017(9) 0.59792(6) 0.01064(19) Uani 1 1 d . . . . .
C2 C 0.22171(9) 0.51530(11) 0.64911(7) 0.0174(2) Uani 1 1 d . . . . .
H2A H 0.166590 0.464423 0.645082 0.021 Uiso 1 1 calc R . . . .
H2B H 0.201017 0.592183 0.659135 0.021 Uiso 1 1 calc R . . . .
C3 C 0.30177(9) 0.47408(11) 0.70809(7) 0.0172(2) Uani 1 1 d . . . . .
H3A H 0.317681 0.532399 0.744804 0.021 Uiso 1 1 calc R . . . .
H3B H 0.282830 0.404757 0.731118 0.021 Uiso 1 1 calc R . . . .
C4 C 0.22155(8) 0.54037(10) 0.51059(6) 0.0137(2) Uani 1 1 d . . . . .
C5 C 0.16590(8) 0.45485(11) 0.47184(7) 0.0169(2) Uani 1 1 d . . . . .
C6 C 0.12590(10) 0.48081(13) 0.40101(7) 0.0231(3) Uani 1 1 d . . . . .
H6 H 0.088855 0.426139 0.373783 0.028 Uiso 1 1 calc R . . . .
C7 C 0.14034(10) 0.58646(14) 0.37049(8) 0.0270(3) Uani 1 1 d . . . . .
H7 H 0.114650 0.601328 0.322738 0.032 Uiso 1 1 calc R . . . .
C8 C 0.19292(10) 0.66990(13) 0.41095(8) 0.0245(3) Uani 1 1 d . . . . .
H8 H 0.201116 0.740962 0.390137 0.029 Uiso 1 1 calc R . . . .
C9 C 0.23396(9) 0.64970(11) 0.48235(7) 0.0174(2) Uani 1 1 d . . . . .
C10 C 0.14598(9) 0.33915(11) 0.50428(8) 0.0198(2) Uani 1 1 d . . . . .
H10 H 0.187622 0.332010 0.550701 0.024 Uiso 1 1 calc R . . . .
C11 C 0.16841(11) 0.23936(13) 0.45622(9) 0.0309(3) Uani 1 1 d . . . . .
H11A H 0.124798 0.240759 0.411868 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.161210 0.168541 0.481073 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.233317 0.246064 0.445532 0.046 Uiso 1 1 calc GR . . . .
C12 C 0.04110(11) 0.33210(14) 0.51944(10) 0.0340(4) Uani 1 1 d . . . . .
H12A H 0.028840 0.392262 0.552119 0.051 Uiso 1 1 calc GR . . . .
H12B H 0.030181 0.259375 0.540893 0.051 Uiso 1 1 calc GR . . . .
H12C H -0.001287 0.340255 0.474796 0.051 Uiso 1 1 calc GR . . . .
C13 C 0.28670(9) 0.74485(11) 0.52639(8) 0.0206(3) Uani 1 1 d . . . . .
H13 H 0.316973 0.711938 0.572244 0.025 Uiso 1 1 calc R . . . .
C14 C 0.36628(11) 0.79695(14) 0.48773(9) 0.0318(3) Uani 1 1 d . . . . .
H14A H 0.407595 0.737212 0.474475 0.048 Uiso 1 1 calc GR . . . .
H14B H 0.403235 0.849922 0.519580 0.048 Uiso 1 1 calc GR . . . .
H14C H 0.337906 0.836363 0.444906 0.048 Uiso 1 1 calc GR . . . .
C15 C 0.21575(11) 0.83706(13) 0.54414(10) 0.0322(3) Uani 1 1 d . . . . .
H15A H 0.185467 0.871147 0.499992 0.048 Uiso 1 1 calc GR . . . .
H15B H 0.249718 0.894802 0.574040 0.048 Uiso 1 1 calc GR . . . .
H15C H 0.167602 0.803007 0.569523 0.048 Uiso 1 1 calc GR . . . .
C16 C 0.46189(8) 0.37518(10) 0.69317(6) 0.0126(2) Uani 1 1 d . . . . .
C17 C 0.45297(9) 0.25905(10) 0.67317(6) 0.0145(2) Uani 1 1 d . . . . .
C18 C 0.52720(10) 0.18535(11) 0.70086(7) 0.0198(2) Uani 1 1 d . . . . .
H18 H 0.522470 0.107810 0.689759 0.024 Uiso 1 1 calc R . . . .
C19 C 0.60782(10) 0.22583(12) 0.74463(7) 0.0221(3) Uani 1 1 d . . . . .
H19 H 0.657363 0.175824 0.761530 0.026 Uiso 1 1 calc R . . . .
C20 C 0.61488(9) 0.34060(12) 0.76330(7) 0.0205(2) Uani 1 1 d . . . . .
H20 H 0.669642 0.366862 0.792295 0.025 Uiso 1 1 calc R . . . .
C21 C 0.54126(9) 0.41754(10) 0.73936(6) 0.0153(2) Uani 1 1 d . . . . .
C22 C 0.36558(9) 0.21058(10) 0.62580(7) 0.0166(2) Uani 1 1 d . . . . .
H22 H 0.331131 0.274435 0.599931 0.020 Uiso 1 1 calc R . . . .
C23 C 0.29695(10) 0.15281(13) 0.67238(8) 0.0261(3) Uani 1 1 d . . . . .
H23A H 0.328404 0.088166 0.696993 0.039 Uiso 1 1 calc GR . . . .
H23B H 0.240196 0.127667 0.641883 0.039 Uiso 1 1 calc GR . . . .
H23C H 0.279315 0.206445 0.707391 0.039 Uiso 1 1 calc GR . . . .
C24 C 0.39224(10) 0.12525(13) 0.56927(8) 0.0249(3) Uani 1 1 d . . . . .
H24A H 0.436845 0.160326 0.541073 0.037 Uiso 1 1 calc GR . . . .
H24B H 0.335233 0.103105 0.537956 0.037 Uiso 1 1 calc GR . . . .
H24C H 0.421341 0.058820 0.593349 0.037 Uiso 1 1 calc GR . . . .
C25 C 0.54718(9) 0.54064(11) 0.76470(7) 0.0183(2) Uani 1 1 d . . . . .
H25 H 0.496980 0.583844 0.734551 0.022 Uiso 1 1 calc R . . . .
C26 C 0.52700(12) 0.54888(13) 0.84365(8) 0.0290(3) Uani 1 1 d . . . . .
H26A H 0.465413 0.515447 0.847804 0.044 Uiso 1 1 calc GR . . . .
H26B H 0.526829 0.627777 0.857964 0.044 Uiso 1 1 calc GR . . . .
H26C H 0.576126 0.508565 0.874526 0.044 Uiso 1 1 calc GR . . . .
C27 C 0.64424(10) 0.59598(12) 0.75665(8) 0.0257(3) Uani 1 1 d . . . . .
H27A H 0.693391 0.563335 0.791463 0.039 Uiso 1 1 calc GR . . . .
H27B H 0.640567 0.676865 0.764826 0.039 Uiso 1 1 calc GR . . . .
H27C H 0.659608 0.582442 0.708621 0.039 Uiso 1 1 calc GR . . . .
C28 C 0.43162(8) 0.48550(9) 0.54644(6) 0.0109(2) Uani 1 1 d . . . . .
C29 C 0.51128(8) 0.55601(10) 0.56650(6) 0.0135(2) Uani 1 1 d . . . . .
H29 H 0.518127 0.593329 0.611016 0.016 Uiso 1 1 calc R . . . .
C30 C 0.58029(8) 0.57048(10) 0.52007(6) 0.0136(2) Uani 1 1 d . . . . .
H30 H 0.633616 0.616903 0.533290 0.016 Uiso 1 1 calc R . . . .
I1 I 0.41279(2) 0.82305(2) 0.72122(2) 0.02068(3) Uani 1 1 d . . . . .
O1 O 0.61400(10) 0.80540(10) 0.62463(8) 0.0405(3) Uani 1 1 d . . . . .
C31 C 0.63576(10) 0.92208(12) 0.62316(8) 0.0250(3) Uani 1 1 d . . . . .
H31A H 0.584478 0.961767 0.594086 0.037 Uiso 1 1 calc GR . . . .
H31B H 0.694561 0.932578 0.602763 0.037 Uiso 1 1 calc GR . . . .
H31C H 0.643176 0.951977 0.671623 0.037 Uiso 1 1 calc GR . . . .
H1 H 0.5686(16) 0.8001(18) 0.6441(12) 0.047(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
N1 C1 1.3230(14) . ?
N1 C2 1.4839(14) . ?
N1 C4 1.4498(15) . ?
N2 C1 1.3291(14) . ?
N2 C3 1.4840(14) . ?
N2 C16 1.4494(14) . ?
C1 C28 1.4784(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.5394(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.4066(17) . ?
C4 C9 1.4015(17) . ?
C5 C6 1.3958(18) . ?
C5 C10 1.5218(18) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.383(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.3965(18) . ?
C9 C13 1.5146(19) . ?
C10 H10 0.9800 . ?
C10 C11 1.5278(19) . ?
C10 C12 1.5355(19) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.5317(19) . ?
C13 C15 1.532(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.4086(16) . ?
C16 C21 1.4030(17) . ?
C17 C18 1.3956(17) . ?
C17 C22 1.5207(17) . ?
C18 H18 0.9300 . ?
C18 C19 1.3859(19) . ?
C19 H19 0.9300 . ?
C19 C20 1.3860(19) . ?
C20 H20 0.9300 . ?
C20 C21 1.3964(17) . ?
C21 C25 1.5130(17) . ?
C22 H22 0.9800 . ?
C22 C23 1.5343(18) . ?
C22 C24 1.5316(18) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.5357(19) . ?
C25 C27 1.5318(19) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.3982(16) . ?
C28 C30 1.3905(16) 3_666 ?
C29 H29 0.9300 . ?
C29 C30 1.3903(15) . ?
C30 H30 0.9300 . ?
O1 C31 1.3986(18) . ?
O1 H1 0.78(2) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 110.43(9) . . ?
C1 N1 C4 125.24(9) . . ?
C4 N1 C2 124.33(9) . . ?
C1 N2 C3 110.02(9) . . ?
C1 N2 C16 123.92(9) . . ?
C16 N2 C3 122.52(9) . . ?
N1 C1 N2 113.15(10) . . ?
N1 C1 C28 124.33(10) . . ?
N2 C1 C28 122.23(10) . . ?
N1 C2 H2A 111.2 . . ?
N1 C2 H2B 111.2 . . ?
N1 C2 C3 102.96(9) . . ?
H2A C2 H2B 109.1 . . ?
C3 C2 H2A 111.2 . . ?
C3 C2 H2B 111.2 . . ?
N2 C3 C2 103.29(9) . . ?
N2 C3 H3A 111.1 . . ?
N2 C3 H3B 111.1 . . ?
C2 C3 H3A 111.1 . . ?
C2 C3 H3B 111.1 . . ?
H3A C3 H3B 109.1 . . ?
C5 C4 N1 117.89(10) . . ?
C9 C4 N1 119.16(11) . . ?
C9 C4 C5 122.94(11) . . ?
C4 C5 C10 123.12(11) . . ?
C6 C5 C4 117.12(12) . . ?
C6 C5 C10 119.74(12) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.25(13) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.10(13) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.3 . . ?
C7 C8 C9 121.42(13) . . ?
C9 C8 H8 119.3 . . ?
C4 C9 C13 122.86(11) . . ?
C8 C9 C4 117.07(12) . . ?
C8 C9 C13 120.05(12) . . ?
C5 C10 H10 107.8 . . ?
C5 C10 C11 112.54(12) . . ?
C5 C10 C12 110.56(11) . . ?
C11 C10 H10 107.8 . . ?
C11 C10 C12 110.06(12) . . ?
C12 C10 H10 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.9 . . ?
C9 C13 C14 111.80(12) . . ?
C9 C13 C15 110.43(11) . . ?
C14 C13 H13 107.9 . . ?
C14 C13 C15 110.84(12) . . ?
C15 C13 H13 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 118.36(10) . . ?
C21 C16 N2 119.10(10) . . ?
C21 C16 C17 122.49(11) . . ?
C16 C17 C22 123.27(11) . . ?
C18 C17 C16 117.49(11) . . ?
C18 C17 C22 119.20(11) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.08(12) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.22(12) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.21(12) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C25 122.20(11) . . ?
C20 C21 C16 117.43(11) . . ?
C20 C21 C25 120.35(11) . . ?
C17 C22 H22 107.9 . . ?
C17 C22 C23 110.71(11) . . ?
C17 C22 C24 112.94(10) . . ?
C23 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C24 C22 C23 109.26(11) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.8 . . ?
C21 C25 C26 110.39(11) . . ?
C21 C25 C27 112.58(11) . . ?
C26 C25 H25 107.8 . . ?
C27 C25 H25 107.8 . . ?
C27 C25 C26 110.23(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 116.03(10) . . ?
C30 C28 C1 123.05(10) 3_666 . ?
C30 C28 C29 120.83(10) 3_666 . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.18(10) . . ?
C30 C29 H29 119.9 . . ?
C28 C30 H30 120.5 3_666 . ?
C29 C30 C28 119.00(10) . 3_666 ?
C29 C30 H30 120.5 . . ?
C31 O1 H1 106.3(16) . . ?
O1 C31 H31A 109.5 . . ?
O1 C31 H31B 109.5 . . ?
O1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
N1 C1 C28 C29 118.61(13) . . . . ?
N1 C1 C28 C30 -58.01(16) . . . 3_666 ?
N1 C2 C3 N2 -0.35(12) . . . . ?
N1 C4 C5 C6 -175.86(10) . . . . ?
N1 C4 C5 C10 5.84(16) . . . . ?
N1 C4 C9 C8 175.19(11) . . . . ?
N1 C4 C9 C13 -6.50(17) . . . . ?
N2 C1 C28 C29 -54.74(15) . . . . ?
N2 C1 C28 C30 128.63(12) . . . 3_666 ?
N2 C16 C17 C18 -177.72(10) . . . . ?
N2 C16 C17 C22 -0.09(16) . . . . ?
N2 C16 C21 C20 179.94(11) . . . . ?
N2 C16 C21 C25 1.64(17) . . . . ?
C1 N1 C2 C3 -1.95(13) . . . . ?
C1 N1 C4 C5 97.38(14) . . . . ?
C1 N1 C4 C9 -81.58(15) . . . . ?
C1 N2 C3 C2 2.55(13) . . . . ?
C1 N2 C16 C17 -66.82(15) . . . . ?
C1 N2 C16 C21 115.71(13) . . . . ?
C1 C28 C29 C30 -177.12(11) . . . . ?
C2 N1 C1 N2 3.87(14) . . . . ?
C2 N1 C1 C28 -170.02(10) . . . . ?
C2 N1 C4 C5 -82.33(14) . . . . ?
C2 N1 C4 C9 98.70(14) . . . . ?
C3 N2 C1 N1 -4.11(14) . . . . ?
C3 N2 C1 C28 169.93(10) . . . . ?
C3 N2 C16 C17 89.80(13) . . . . ?
C3 N2 C16 C21 -87.67(14) . . . . ?
C4 N1 C1 N2 -175.88(10) . . . . ?
C4 N1 C1 C28 10.23(18) . . . . ?
C4 N1 C2 C3 177.80(11) . . . . ?
C4 C5 C6 C7 -0.19(19) . . . . ?
C4 C5 C10 C11 -129.31(13) . . . . ?
C4 C5 C10 C12 107.16(14) . . . . ?
C4 C9 C13 C14 127.21(13) . . . . ?
C4 C9 C13 C15 -108.88(14) . . . . ?
C5 C4 C9 C8 -3.72(18) . . . . ?
C5 C4 C9 C13 174.59(11) . . . . ?
C5 C6 C7 C8 -1.9(2) . . . . ?
C6 C5 C10 C11 52.43(16) . . . . ?
C6 C5 C10 C12 -71.10(16) . . . . ?
C6 C7 C8 C9 1.2(2) . . . . ?
C7 C8 C9 C4 1.5(2) . . . . ?
C7 C8 C9 C13 -176.83(13) . . . . ?
C8 C9 C13 C14 -54.53(16) . . . . ?
C8 C9 C13 C15 69.38(16) . . . . ?
C9 C4 C5 C6 3.07(17) . . . . ?
C9 C4 C5 C10 -175.24(11) . . . . ?
C10 C5 C6 C7 178.18(12) . . . . ?
C16 N2 C1 N1 155.03(10) . . . . ?
C16 N2 C1 C28 -30.93(16) . . . . ?
C16 N2 C3 C2 -156.93(10) . . . . ?
C16 C17 C18 C19 -1.85(18) . . . . ?
C16 C17 C22 C23 -98.91(13) . . . . ?
C16 C17 C22 C24 138.20(12) . . . . ?
C16 C21 C25 C26 103.94(14) . . . . ?
C16 C21 C25 C27 -132.41(12) . . . . ?
C17 C16 C21 C20 2.57(17) . . . . ?
C17 C16 C21 C25 -175.73(11) . . . . ?
C17 C18 C19 C20 1.7(2) . . . . ?
C18 C17 C22 C23 78.68(14) . . . . ?
C18 C17 C22 C24 -44.20(16) . . . . ?
C18 C19 C20 C21 0.7(2) . . . . ?
C19 C20 C21 C16 -2.72(19) . . . . ?
C19 C20 C21 C25 175.62(12) . . . . ?
C20 C21 C25 C26 -74.32(15) . . . . ?
C20 C21 C25 C27 49.33(16) . . . . ?
C21 C16 C17 C18 -0.34(17) . . . . ?
C21 C16 C17 C22 177.30(11) . . . . ?
C22 C17 C18 C19 -179.59(12) . . . . ?
C28 C29 C30 C28 0.41(19) . . . 3_666 ?
C30 C28 C29 C30 -0.42(19) 3_666 . . . ?

_olex2_date_sample_data_collection 2017-12-06
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.223
_oxdiff_exptl_absorpt_empirical_full_min 0.849
####################################################################### 
# 
# 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_rottschaefer54
_database_code_depnum_ccdc_archive 'CCDC 1826569'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_audit_creation_date             2017-11-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H80 N4'
_chemical_formula_sum            'C60 H80 N4'
_chemical_formula_weight         857.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H80 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'

_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                   10.4185(5)
_cell_length_b                   10.5244(5)
_cell_length_c                   25.1966(7)
_cell_angle_alpha                97.968(3)
_cell_angle_beta                 90.283(3)
_cell_angle_gamma                110.092(4)
_cell_volume                     2565.45(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13860
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.3920
_cell_measurement_theta_min      4.5030
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             936
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0187
0 0 1 0.0187
0 -5 -4 0.0521
0 5 4 0.0521
-3 -1 5 0.0556
3 1 -5 0.0556
-5 3 1 0.1049
5 -3 -1 0.1049

_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.037
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
0.0011 -0.0025 -0.9986 0.0446 0.0026 0.0427
-0.0011 0.0025 0.9986 -0.0446 -0.0026 -0.0427
-0.0295 -5.0242 -3.9759 0.1768 -0.7499 0.3938
0.0295 5.0242 3.9759 -0.1768 0.7499 -0.3938
-3.0083 -0.9672 4.9795 0.0796 -0.4128 -0.4314
3.0083 0.9672 -4.9795 -0.0796 0.4128 0.4314
-4.9744 3.0492 0.9584 0.4612 0.0401 -0.6138
4.9744 -3.0492 -0.9584 -0.4612 -0.0401 0.6138

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37630
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_min         3.548
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     21.00  84.00   1.00   10.57    --    0.00  57.00 150.00   63
  2  ω    -91.00 -58.00   1.00   10.57    --    0.00 -77.00-180.00   33
  3  ω     18.00  69.00   1.00   10.57    --    0.00  57.00 -90.00   51
  4  ω    -33.00  13.00   1.00   10.57    --    0.00  57.00 -90.00   46
  5  ω    -16.00  45.00   1.00   10.57    --    0.00  57.00   0.00   61
  6  ω    -47.00  35.00   1.00   10.57    --    0.00 -77.00-180.00   82
  7  ω    -37.00   5.00   1.00   10.57    --    0.00  57.00 150.00   42
  8  ω    -57.00 -20.00   1.00   42.28    --  -59.50 -77.00  60.00   37
  9  ω    -60.00 -20.00   1.00   42.28    --  -59.50 -77.00 -90.00   40
 10  ω   -147.00 -20.00   1.00   42.28    --  -59.50 -77.00   0.00  127
 11  ω   -151.00 -21.00   1.00   42.28    --  -59.50 -77.00 120.00  130
 12  ω   -130.00 -51.00   1.00   42.28    --  -59.50 -77.00 -60.00   79
 13  ω   -112.00 -62.00   1.00   42.28    --  -59.50 -77.00  60.00   50
 14  ω   -121.00 -57.00   1.00   42.28    --  -59.50 -77.00 150.00   64
 15  ω    -47.00 -20.00   1.00   42.28    --  -59.50 -77.00 -60.00   27
 16  ω    -94.00 -11.00   1.00   42.28    --  -59.50 125.00   0.00   83
 17  ω    -89.00  -2.00   1.00   42.28    --  -59.50 125.00 150.00   87
 18  ω    -48.00 -20.00   1.00   42.28    --  -59.50 -77.00-180.00   28
 19  ω   -101.00 -20.00   1.00   42.28    --  -59.50 -77.00  30.00   81
 20  ω    -59.00 -20.00   1.00   42.28    --  -59.50 -77.00  90.00   39
 21  ω   -150.00 -58.00   1.00   42.28    --  -59.50 -77.00-150.00   92
 22  ω    -56.00 -20.00   1.00   42.28    --  -59.50 -77.00 150.00   36
 23  ω    -54.00 -20.00   1.00   42.28    --  -59.50 -77.00-150.00   34
 24  ω   -129.00 -72.00   1.00   42.28    --  -59.50 -77.00 -90.00   57
 25  ω     23.00  68.00   1.00   42.28    --   59.50-125.00 150.00   45
 26  ω    110.00 143.00   1.00   42.28    --   59.50 125.00 120.00   33
 27  ω    108.00 139.00   1.00   42.28    --   59.50 125.00  30.00   31
 28  ω     90.00 122.00   1.00   42.28    --   59.50-125.00 150.00   32
 29  ω     94.00 143.00   1.00   42.28    --   59.50 125.00  60.00   49
 30  ω     82.00 108.00   1.00    5.00    --  119.00  63.00   0.00   26
 31  ω     82.00 110.00   1.00    5.00    --  119.00  63.00-120.00   28
 32  ω     34.00 113.00   1.00    5.00    --  119.00-111.00 -30.00   79
 33  ω     82.00 170.00   1.00    5.00    --  119.00  63.00  90.00   88
 34  ω     81.00 177.00   1.00    5.00    --  119.00  77.00 120.00   96
 35  ω     80.00 178.00   1.00    5.00    --  119.00  77.00 -30.00   98
 36  ω     81.00 126.00   1.00    5.00    --  119.00  66.00  35.68   45
 37  ω     80.00 177.00   1.00    5.00    --  119.00  77.00   0.00   97
 38  ω     80.00 178.00   1.00    5.00    --  119.00  77.00 -60.00   98
 39  ω     33.00 116.00   1.00    5.00    --  119.00-111.00 150.00   83
 40  ω     80.00 107.00   1.00    5.00    --  119.00  77.00  30.00   27
 41  ω    110.00 176.00   1.00    5.00    --  119.00  77.00 150.00   66
 42  ω     82.00 109.00   1.00    5.00    --  119.00  63.00 -60.00   27
 43  ω     81.00 109.00   1.00    5.00    --  119.00  66.00-137.16   28
 44  ω     83.00 111.00   1.00    5.00    --  119.00  56.00-129.64   28
 45  ω     80.00 107.00   1.00    5.00    --  119.00  77.00 150.00   27
 46  ω     82.00 109.00   1.00    5.00    --  119.00  63.00 -30.00   27
 47  ω     83.00 110.00   1.00    5.00    --  119.00  50.00-150.00   27
 48  ω     83.00 109.00   1.00    5.00    --  119.00  63.00 -90.00   26
 49  ω     81.00 107.00   1.00    5.00    --  119.00  77.00 -90.00   26
 50  ω     82.00 109.00   1.00    5.00    --  119.00  63.00  30.00   27
 51  ω     30.00 158.00   1.00    5.00    --  119.00 -77.00 -30.00  128
 52  ω     84.00 111.00   1.00    5.00    --  119.00  63.00-180.00   27
 53  ω     80.00 178.00   1.00    5.00    --  119.00  77.00-180.00   98
 54  ω     83.00 114.00   1.00    5.00    --  119.00  50.00  90.00   31
 55  ω     82.00 109.00   1.00    5.00    --  119.00  63.00 150.00   27
 56  ω     83.00 108.00   1.00    5.00    --  119.00  63.00 120.00   25
 57  ω    117.00 176.00   1.00    5.00    --  119.00  63.00-150.00   59
 58  ω     43.00 157.00   1.00    5.00    --  119.00 -77.00 150.00  114
 59  ω     82.00 109.00   1.00    5.00    --  119.00  59.00 112.11   27
 60  ω     82.00 110.00   1.00    5.00    --  119.00  63.00-150.00   28
 61  ω     64.00 115.00   1.00    5.00    --  119.00-111.00-120.00   51
 62  ω     90.00 115.00   1.00    5.00    --  119.00-111.00  60.00   25
 63  ω     82.00 161.00   1.00    5.00    --  119.00  63.00  60.00   79
 64  ω     80.00 155.00   1.00    5.00    --  119.00  77.00-120.00   75
 65  ω     54.00  81.00   1.00    5.00    --  119.00-111.00  60.00   27
 66  ω    128.00 163.00   1.00    5.00    --  119.00  66.00  35.68   35
 67  ω     82.00 107.00   1.00    5.00    --  119.00  66.00 126.96   25
 68  ω     82.00 109.00   1.00    5.00    --  119.00  60.00 178.42   27
 69  ω     83.00 175.00   1.00    5.00    --  119.00  60.00 -80.22   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1008393000
_diffrn_orient_matrix_UB_12      0.0008290000
_diffrn_orient_matrix_UB_13      -0.0447645000
_diffrn_orient_matrix_UB_21      0.0839591000
_diffrn_orient_matrix_UB_22      0.1510127000
_diffrn_orient_matrix_UB_23      -0.0028516000
_diffrn_orient_matrix_UB_31      0.0874787000
_diffrn_orient_matrix_UB_32      -0.0452060000
_diffrn_orient_matrix_UB_33      -0.0425649000
_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                7686
_reflns_number_total             9804
_reflns_odcompleteness_completeness 97.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9804
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0716
_refine_ls_restrained_S_all      1.068
_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)+(0.1194P)²+1.8830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2208
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C40(H40), C43(H43), C52(H52), C55(H55)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C32(H32A,H32B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C36(H36), C37(H37), C38(H38), C48(H48), C49(H49), C50(H50), C59(H59), C60(H60)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
N1 N 0.1559(2) 0.61566(19) 0.14380(7) 0.0261(4) Uani 1 1 d . . . . .
N2 N 0.0486(2) 0.76176(19) 0.12617(7) 0.0266(4) Uani 1 1 d . . . . .
N3 N 0.6487(2) 0.8460(2) 0.37957(8) 0.0289(4) Uani 1 1 d . . . . .
N4 N 0.4940(2) 0.9282(2) 0.34684(8) 0.0293(4) Uani 1 1 d . . . . .
C1 C 0.0782(2) 0.6457(2) 0.10477(9) 0.0246(5) Uani 1 1 d . . . . .
C2 C 0.1960(3) 0.7287(2) 0.18920(9) 0.0297(5) Uani 1 1 d . . . . .
H2A H 0.288705 0.790417 0.186586 0.036 Uiso 1 1 calc R . . . .
H2B H 0.189412 0.694212 0.223218 0.036 Uiso 1 1 calc R . . . .
C3 C 0.0928(3) 0.7998(2) 0.18342(9) 0.0307(5) Uani 1 1 d . . . . .
H3A H 0.016332 0.767103 0.205789 0.037 Uiso 1 1 calc R . . . .
H3B H 0.135208 0.898191 0.192904 0.037 Uiso 1 1 calc R . . . .
C4 C 0.1303(2) 0.4808(2) 0.15732(9) 0.0262(5) Uani 1 1 d . . . . .
C5 C 0.0021(2) 0.4038(2) 0.17449(9) 0.0288(5) Uani 1 1 d . . . . .
C6 C -0.0100(3) 0.2827(2) 0.19357(10) 0.0312(5) Uani 1 1 d . . . . .
H6 H -0.093329 0.231642 0.205754 0.037 Uiso 1 1 calc R . . . .
C7 C 0.0990(3) 0.2361(2) 0.19490(10) 0.0335(6) Uani 1 1 d . . . . .
H7 H 0.088537 0.154916 0.207983 0.040 Uiso 1 1 calc R . . . .
C8 C 0.2232(3) 0.3105(2) 0.17675(10) 0.0318(5) Uani 1 1 d . . . . .
H8 H 0.295729 0.278156 0.177205 0.038 Uiso 1 1 calc R . . . .
C9 C 0.2414(2) 0.4335(2) 0.15773(9) 0.0284(5) Uani 1 1 d . . . . .
C10 C -0.1231(2) 0.4481(3) 0.17431(10) 0.0308(5) Uani 1 1 d . . . . .
H10 H -0.096345 0.535555 0.160466 0.037 Uiso 1 1 calc R . . . .
C11 C -0.2391(3) 0.3440(3) 0.13657(13) 0.0459(7) Uani 1 1 d . . . . .
H11A H -0.206497 0.332456 0.101290 0.069 Uiso 1 1 calc GR . . . .
H11B H -0.314240 0.376715 0.135005 0.069 Uiso 1 1 calc GR . . . .
H11C H -0.269042 0.257866 0.149805 0.069 Uiso 1 1 calc GR . . . .
C12 C -0.1710(3) 0.4706(3) 0.23080(11) 0.0404(6) Uani 1 1 d . . . . .
H12A H -0.199626 0.385783 0.245065 0.061 Uiso 1 1 calc GR . . . .
H12B H -0.246361 0.503006 0.229510 0.061 Uiso 1 1 calc GR . . . .
H12C H -0.097062 0.537087 0.253384 0.061 Uiso 1 1 calc GR . . . .
C13 C 0.3809(2) 0.5120(2) 0.13859(10) 0.0309(5) Uani 1 1 d . . . . .
H13 H 0.374847 0.593022 0.125269 0.037 Uiso 1 1 calc R . . . .
C14 C 0.4251(3) 0.4271(3) 0.09307(11) 0.0373(6) Uani 1 1 d . . . . .
H14A H 0.512361 0.480919 0.081801 0.056 Uiso 1 1 calc GR . . . .
H14B H 0.358479 0.399666 0.063382 0.056 Uiso 1 1 calc GR . . . .
H14C H 0.432185 0.347306 0.105381 0.056 Uiso 1 1 calc GR . . . .
C15 C 0.4888(3) 0.5602(3) 0.18562(11) 0.0383(6) Uani 1 1 d . . . . .
H15A H 0.496586 0.482214 0.199208 0.057 Uiso 1 1 calc GR . . . .
H15B H 0.461797 0.616062 0.213591 0.057 Uiso 1 1 calc GR . . . .
H15C H 0.575565 0.612676 0.173497 0.057 Uiso 1 1 calc GR . . . .
C16 C 0.0536(2) 0.8727(2) 0.09776(9) 0.0262(5) Uani 1 1 d . . . . .
C17 C 0.1752(2) 0.9467(2) 0.07503(9) 0.0279(5) Uani 1 1 d . . . . .
C18 C 0.1776(3) 1.0624(2) 0.05348(9) 0.0301(5) Uani 1 1 d . . . . .
H18 H 0.255731 1.111141 0.037381 0.036 Uiso 1 1 calc R . . . .
C19 C 0.0672(3) 1.1069(2) 0.05534(10) 0.0316(5) Uani 1 1 d . . . . .
H19 H 0.072553 1.186156 0.041720 0.038 Uiso 1 1 calc R . . . .
C20 C -0.0512(3) 1.0328(2) 0.07758(10) 0.0299(5) Uani 1 1 d . . . . .
H20 H -0.125618 1.062544 0.078538 0.036 Uiso 1 1 calc R . . . .
C21 C -0.0608(2) 0.9145(2) 0.09857(9) 0.0262(5) Uani 1 1 d . . . . .
C22 C 0.3021(2) 0.9053(2) 0.07314(10) 0.0313(5) Uani 1 1 d . . . . .
H22 H 0.286055 0.830325 0.094256 0.038 Uiso 1 1 calc R . . . .
C23 C 0.3251(3) 0.8522(3) 0.01562(11) 0.0389(6) Uani 1 1 d . . . . .
H23A H 0.245214 0.776758 0.000992 0.058 Uiso 1 1 calc GR . . . .
H23B H 0.402527 0.822494 0.015691 0.058 Uiso 1 1 calc GR . . . .
H23C H 0.342168 0.924178 -0.005914 0.058 Uiso 1 1 calc GR . . . .
C24 C 0.4293(3) 1.0238(3) 0.09861(12) 0.0395(6) Uani 1 1 d . . . . .
H24A H 0.451145 1.096412 0.077223 0.059 Uiso 1 1 calc GR . . . .
H24B H 0.505082 0.992127 0.100346 0.059 Uiso 1 1 calc GR . . . .
H24C H 0.411168 1.057057 0.134191 0.059 Uiso 1 1 calc GR . . . .
C25 C -0.1945(2) 0.8335(2) 0.12151(10) 0.0304(5) Uani 1 1 d . . . . .
H25 H -0.186162 0.748386 0.129937 0.036 Uiso 1 1 calc R . . . .
C26 C -0.3158(3) 0.7955(3) 0.08050(11) 0.0377(6) Uani 1 1 d . . . . .
H26A H -0.325790 0.877372 0.071475 0.057 Uiso 1 1 calc GR . . . .
H26B H -0.397934 0.742642 0.095633 0.057 Uiso 1 1 calc GR . . . .
H26C H -0.299658 0.742546 0.048725 0.057 Uiso 1 1 calc GR . . . .
C27 C -0.2217(3) 0.9118(3) 0.17328(11) 0.0419(6) Uani 1 1 d . . . . .
H27A H -0.145757 0.934129 0.198845 0.063 Uiso 1 1 calc GR . . . .
H27B H -0.303478 0.856046 0.187749 0.063 Uiso 1 1 calc GR . . . .
H27C H -0.233048 0.994433 0.165824 0.063 Uiso 1 1 calc GR . . . .
C28 C 0.0387(2) 0.5737(2) 0.05399(9) 0.0253(5) Uani 1 1 d . . . . .
C29 C 0.0972(2) 0.4735(2) 0.03073(9) 0.0268(5) Uani 1 1 d . . . . .
H29 H 0.161385 0.455360 0.051308 0.032 Uiso 1 1 calc R . . . .
C30 C -0.0620(2) 0.5945(2) 0.01966(9) 0.0265(5) Uani 1 1 d . . . . .
H30 H -0.103816 0.656692 0.032761 0.032 Uiso 1 1 calc R . . . .
C31 C 0.5545(2) 0.9119(2) 0.39420(10) 0.0282(5) Uani 1 1 d . . . . .
C32 C 0.6341(3) 0.7993(3) 0.32124(10) 0.0354(6) Uani 1 1 d . . . . .
H32A H 0.577812 0.703309 0.312939 0.042 Uiso 1 1 calc R . . . .
H32B H 0.722624 0.813116 0.306251 0.042 Uiso 1 1 calc R . . . .
C33 C 0.5644(3) 0.8900(3) 0.30028(10) 0.0335(5) Uani 1 1 d . . . . .
H33A H 0.631081 0.970122 0.289012 0.040 Uiso 1 1 calc R . . . .
H33B H 0.499700 0.840052 0.270347 0.040 Uiso 1 1 calc R . . . .
C34 C 0.7832(2) 0.8845(2) 0.40471(9) 0.0274(5) Uani 1 1 d . . . . .
C35 C 0.8787(2) 1.0183(3) 0.40677(9) 0.0304(5) Uani 1 1 d . . . . .
C36 C 1.0119(3) 1.0445(3) 0.42714(10) 0.0331(5) Uani 1 1 d . . . . .
H36 H 1.076193 1.132200 0.428994 0.040 Uiso 1 1 calc R . . . .
C37 C 1.0501(3) 0.9436(3) 0.44452(10) 0.0341(6) Uani 1 1 d . . . . .
H37 H 1.139662 0.962964 0.457290 0.041 Uiso 1 1 calc R . . . .
C38 C 0.9549(3) 0.8134(3) 0.44295(10) 0.0330(5) Uani 1 1 d . . . . .
H38 H 0.981148 0.745964 0.455136 0.040 Uiso 1 1 calc R . . . .
C39 C 0.8202(2) 0.7815(3) 0.42337(9) 0.0299(5) Uani 1 1 d . . . . .
C40 C 0.8430(3) 1.1329(3) 0.38733(10) 0.0337(5) Uani 1 1 d . . . . .
H40 H 0.746570 1.095252 0.374345 0.040 Uiso 1 1 calc R . . . .
C41 C 0.9269(3) 1.1863(3) 0.34069(13) 0.0481(7) Uani 1 1 d . . . . .
H41A H 1.021769 1.227488 0.352557 0.072 Uiso 1 1 calc GR . . . .
H41B H 0.896156 1.253253 0.327812 0.072 Uiso 1 1 calc GR . . . .
H41C H 0.915596 1.111778 0.312271 0.072 Uiso 1 1 calc GR . . . .
C42 C 0.8573(4) 1.2483(3) 0.43394(13) 0.0520(8) Uani 1 1 d . . . . .
H42A H 0.803229 1.211287 0.462595 0.078 Uiso 1 1 calc GR . . . .
H42B H 0.826018 1.315708 0.421790 0.078 Uiso 1 1 calc GR . . . .
H42C H 0.951609 1.290020 0.446594 0.078 Uiso 1 1 calc GR . . . .
C43 C 0.7185(3) 0.6368(3) 0.42114(11) 0.0348(6) Uani 1 1 d . . . . .
H43 H 0.627413 0.638521 0.412304 0.042 Uiso 1 1 calc R . . . .
C44 C 0.7503(3) 0.5391(3) 0.37674(12) 0.0428(6) Uani 1 1 d . . . . .
H44A H 0.745443 0.569218 0.342759 0.064 Uiso 1 1 calc GR . . . .
H44B H 0.684890 0.448591 0.375935 0.064 Uiso 1 1 calc GR . . . .
H44C H 0.840720 0.538273 0.383643 0.064 Uiso 1 1 calc GR . . . .
C45 C 0.7134(3) 0.5841(3) 0.47531(12) 0.0462(7) Uani 1 1 d . . . . .
H45A H 0.798769 0.573102 0.483333 0.069 Uiso 1 1 calc GR . . . .
H45B H 0.640350 0.497640 0.473414 0.069 Uiso 1 1 calc GR . . . .
H45C H 0.697830 0.648788 0.503019 0.069 Uiso 1 1 calc GR . . . .
C46 C 0.3505(2) 0.9046(2) 0.33882(9) 0.0279(5) Uani 1 1 d . . . . .
C47 C 0.2502(3) 0.7790(3) 0.34496(9) 0.0305(5) Uani 1 1 d . . . . .
C48 C 0.1136(3) 0.7621(3) 0.33339(10) 0.0327(5) Uani 1 1 d . . . . .
H48 H 0.045535 0.680229 0.337833 0.039 Uiso 1 1 calc R . . . .
C49 C 0.0768(3) 0.8638(3) 0.31553(10) 0.0345(6) Uani 1 1 d . . . . .
H49 H -0.014888 0.849867 0.307894 0.041 Uiso 1 1 calc R . . . .
C50 C 0.1765(3) 0.9859(3) 0.30907(10) 0.0340(6) Uani 1 1 d . . . . .
H50 H 0.151503 1.053875 0.296713 0.041 Uiso 1 1 calc R . . . .
C51 C 0.3143(3) 1.0090(3) 0.32082(10) 0.0322(5) Uani 1 1 d . . . . .
C52 C 0.2829(3) 0.6609(3) 0.36233(10) 0.0349(6) Uani 1 1 d . . . . .
H52 H 0.382814 0.687344 0.365488 0.042 Uiso 1 1 calc R . . . .
C53 C 0.2284(4) 0.5330(3) 0.32008(14) 0.0514(8) Uani 1 1 d . . . . .
H53A H 0.130503 0.504993 0.315971 0.077 Uiso 1 1 calc GR . . . .
H53B H 0.253272 0.460691 0.331310 0.077 Uiso 1 1 calc GR . . . .
H53C H 0.267152 0.553161 0.286417 0.077 Uiso 1 1 calc GR . . . .
C54 C 0.2291(4) 0.6316(4) 0.41717(13) 0.0542(8) Uani 1 1 d . . . . .
H54A H 0.267081 0.712560 0.443111 0.081 Uiso 1 1 calc GR . . . .
H54B H 0.255188 0.559251 0.427738 0.081 Uiso 1 1 calc GR . . . .
H54C H 0.131094 0.604432 0.415191 0.081 Uiso 1 1 calc GR . . . .
C55 C 0.4228(3) 1.1444(3) 0.31343(13) 0.0438(7) Uani 1 1 d . . . . .
H55 H 0.507581 1.152300 0.332861 0.053 Uiso 1 1 calc R . . . .
C56 C 0.4512(4) 1.1468(4) 0.25345(15) 0.0629(10) Uani 1 1 d . . . . .
H56A H 0.485293 1.074854 0.240629 0.094 Uiso 1 1 calc GR . . . .
H56B H 0.517976 1.233453 0.249065 0.094 Uiso 1 1 calc GR . . . .
H56C H 0.367874 1.133438 0.233354 0.094 Uiso 1 1 calc GR . . . .
C57 C 0.3824(4) 1.2651(3) 0.3355(2) 0.0734(12) Uani 1 1 d . . . . .
H57A H 0.300768 1.260600 0.316306 0.110 Uiso 1 1 calc GR . . . .
H57B H 0.454986 1.348407 0.331485 0.110 Uiso 1 1 calc GR . . . .
H57C H 0.365566 1.263075 0.372894 0.110 Uiso 1 1 calc GR . . . .
C58 C 0.5276(2) 0.9544(2) 0.44523(9) 0.0279(5) Uani 1 1 d . . . . .
C59 C 0.4527(2) 1.0471(2) 0.45745(9) 0.0286(5) Uani 1 1 d . . . . .
H59 H 0.421012 1.078729 0.429217 0.034 Uiso 1 1 calc R . . . .
C60 C 0.5732(2) 0.9105(2) 0.49212(10) 0.0287(5) Uani 1 1 d . . . . .
H60 H 0.622038 0.851031 0.486979 0.034 Uiso 1 1 calc R . . . .


_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
N1 C1 1.406(3) . ?
N1 C2 1.475(3) . ?
N1 C4 1.441(3) . ?
N2 C1 1.398(3) . ?
N2 C3 1.470(3) . ?
N2 C16 1.439(3) . ?
N3 C31 1.407(3) . ?
N3 C32 1.474(3) . ?
N3 C34 1.435(3) . ?
N4 C31 1.405(3) . ?
N4 C33 1.468(3) . ?
N4 C46 1.437(3) . ?
C1 C28 1.376(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.522(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.410(3) . ?
C4 C9 1.408(3) . ?
C5 C6 1.390(3) . ?
C5 C10 1.529(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.384(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.380(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.395(3) . ?
C9 C13 1.523(3) . ?
C10 H10 0.9800 . ?
C10 C11 1.534(3) . ?
C10 C12 1.525(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.526(4) . ?
C13 C15 1.534(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.411(3) . ?
C16 C21 1.404(3) . ?
C17 C18 1.393(3) . ?
C17 C22 1.527(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.381(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.382(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.392(3) . ?
C21 C25 1.526(3) . ?
C22 H22 0.9800 . ?
C22 C23 1.530(4) . ?
C22 C24 1.536(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.533(3) . ?
C25 C27 1.526(4) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.449(3) . ?
C28 C30 1.448(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.349(3) 2_565 ?
C30 H30 0.9300 . ?
C31 C58 1.365(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.526(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.411(3) . ?
C34 C39 1.404(3) . ?
C35 C36 1.398(3) . ?
C35 C40 1.518(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.377(4) . ?
C37 H37 0.9300 . ?
C37 C38 1.383(4) . ?
C38 H38 0.9300 . ?
C38 C39 1.397(3) . ?
C39 C43 1.520(3) . ?
C40 H40 0.9800 . ?
C40 C41 1.522(4) . ?
C40 C42 1.534(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43 0.9800 . ?
C43 C44 1.529(4) . ?
C43 C45 1.538(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.405(3) . ?
C46 C51 1.405(3) . ?
C47 C48 1.397(3) . ?
C47 C52 1.515(4) . ?
C48 H48 0.9300 . ?
C48 C49 1.381(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.379(4) . ?
C50 H50 0.9300 . ?
C50 C51 1.395(4) . ?
C51 C55 1.520(4) . ?
C52 H52 0.9800 . ?
C52 C53 1.529(4) . ?
C52 C54 1.525(4) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55 0.9800 . ?
C55 C56 1.543(5) . ?
C55 C57 1.509(5) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 C59 1.448(3) . ?
C58 C60 1.460(3) . ?
C59 H59 0.9300 . ?
C59 C60 1.347(4) 2_676 ?
C60 H60 0.9300 . ?

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 C2 109.19(18) . . ?
C1 N1 C4 124.31(18) . . ?
C4 N1 C2 115.89(18) . . ?
C1 N2 C3 109.92(18) . . ?
C1 N2 C16 125.16(19) . . ?
C16 N2 C3 115.97(18) . . ?
C31 N3 C32 109.87(19) . . ?
C31 N3 C34 124.4(2) . . ?
C34 N3 C32 116.64(19) . . ?
C31 N4 C33 109.84(19) . . ?
C31 N4 C46 124.0(2) . . ?
C46 N4 C33 117.15(18) . . ?
N2 C1 N1 108.47(18) . . ?
C28 C1 N1 125.8(2) . . ?
C28 C1 N2 125.8(2) . . ?
N1 C2 H2A 111.1 . . ?
N1 C2 H2B 111.1 . . ?
N1 C2 C3 103.37(18) . . ?
H2A C2 H2B 109.1 . . ?
C3 C2 H2A 111.1 . . ?
C3 C2 H2B 111.1 . . ?
N2 C3 C2 103.19(19) . . ?
N2 C3 H3A 111.1 . . ?
N2 C3 H3B 111.1 . . ?
C2 C3 H3A 111.1 . . ?
C2 C3 H3B 111.1 . . ?
H3A C3 H3B 109.1 . . ?
C5 C4 N1 121.3(2) . . ?
C9 C4 N1 117.7(2) . . ?
C9 C4 C5 120.7(2) . . ?
C4 C5 C10 123.4(2) . . ?
C6 C5 C4 118.1(2) . . ?
C6 C5 C10 118.5(2) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 C5 121.7(2) . . ?
C7 C6 H6 119.2 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.8(2) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 120.9(2) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C13 122.5(2) . . ?
C8 C9 C4 118.8(2) . . ?
C8 C9 C13 118.7(2) . . ?
C5 C10 H10 107.7 . . ?
C5 C10 C11 110.7(2) . . ?
C11 C10 H10 107.7 . . ?
C12 C10 C5 111.6(2) . . ?
C12 C10 H10 107.7 . . ?
C12 C10 C11 111.2(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.1 . . ?
C9 C13 C14 112.3(2) . . ?
C9 C13 C15 110.1(2) . . ?
C14 C13 H13 108.1 . . ?
C14 C13 C15 110.0(2) . . ?
C15 C13 H13 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 120.8(2) . . ?
C21 C16 N2 117.8(2) . . ?
C21 C16 C17 121.1(2) . . ?
C16 C17 C22 123.0(2) . . ?
C18 C17 C16 117.7(2) . . ?
C18 C17 C22 119.4(2) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 C17 121.9(2) . . ?
C19 C18 H18 119.0 . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.6(2) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.1(2) . . ?
C21 C20 H20 119.5 . . ?
C16 C21 C25 121.8(2) . . ?
C20 C21 C16 118.6(2) . . ?
C20 C21 C25 119.6(2) . . ?
C17 C22 H22 107.7 . . ?
C17 C22 C23 111.0(2) . . ?
C17 C22 C24 111.3(2) . . ?
C23 C22 H22 107.7 . . ?
C23 C22 C24 111.1(2) . . ?
C24 C22 H22 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.9 . . ?
C21 C25 C26 111.3(2) . . ?
C26 C25 H25 107.9 . . ?
C27 C25 C21 111.6(2) . . ?
C27 C25 H25 107.9 . . ?
C27 C25 C26 110.1(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 C28 C29 122.2(2) . . ?
C1 C28 C30 122.5(2) . . ?
C30 C28 C29 115.3(2) . . ?
C28 C29 H29 118.7 . . ?
C30 C29 C28 122.5(2) 2_565 . ?
C30 C29 H29 118.7 2_565 . ?
C28 C30 H30 118.9 . . ?
C29 C30 C28 122.1(2) 2_565 . ?
C29 C30 H30 118.9 2_565 . ?
N4 C31 N3 107.9(2) . . ?
C58 C31 N3 126.3(2) . . ?
C58 C31 N4 125.8(2) . . ?
N3 C32 H32A 111.2 . . ?
N3 C32 H32B 111.2 . . ?
N3 C32 C33 102.7(2) . . ?
H32A C32 H32B 109.1 . . ?
C33 C32 H32A 111.2 . . ?
C33 C32 H32B 111.2 . . ?
N4 C33 C32 103.29(19) . . ?
N4 C33 H33A 111.1 . . ?
N4 C33 H33B 111.1 . . ?
C32 C33 H33A 111.1 . . ?
C32 C33 H33B 111.1 . . ?
H33A C33 H33B 109.1 . . ?
C35 C34 N3 121.3(2) . . ?
C39 C34 N3 117.5(2) . . ?
C39 C34 C35 121.0(2) . . ?
C34 C35 C40 122.8(2) . . ?
C36 C35 C34 118.0(2) . . ?
C36 C35 C40 119.2(2) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.5(2) . . ?
C37 C36 H36 119.2 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C38 119.9(2) . . ?
C38 C37 H37 120.0 . . ?
C37 C38 H38 119.5 . . ?
C37 C38 C39 121.1(2) . . ?
C39 C38 H38 119.5 . . ?
C34 C39 C43 121.5(2) . . ?
C38 C39 C34 118.5(2) . . ?
C38 C39 C43 120.0(2) . . ?
C35 C40 H40 107.4 . . ?
C35 C40 C41 112.2(2) . . ?
C35 C40 C42 110.5(2) . . ?
C41 C40 H40 107.4 . . ?
C41 C40 C42 111.6(3) . . ?
C42 C40 H40 107.4 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C43 H43 107.7 . . ?
C39 C43 C44 110.8(2) . . ?
C39 C43 C45 112.2(2) . . ?
C44 C43 H43 107.7 . . ?
C44 C43 C45 110.5(2) . . ?
C45 C43 H43 107.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 N4 121.7(2) . . ?
C47 C46 C51 120.9(2) . . ?
C51 C46 N4 117.3(2) . . ?
C46 C47 C52 123.4(2) . . ?
C48 C47 C46 117.9(2) . . ?
C48 C47 C52 118.7(2) . . ?
C47 C48 H48 119.1 . . ?
C49 C48 C47 121.7(2) . . ?
C49 C48 H48 119.1 . . ?
C48 C49 H49 120.1 . . ?
C50 C49 C48 119.7(2) . . ?
C50 C49 H49 120.1 . . ?
C49 C50 H50 119.6 . . ?
C49 C50 C51 120.9(2) . . ?
C51 C50 H50 119.6 . . ?
C46 C51 C55 121.0(2) . . ?
C50 C51 C46 118.8(2) . . ?
C50 C51 C55 120.1(2) . . ?
C47 C52 H52 107.6 . . ?
C47 C52 C53 111.0(2) . . ?
C47 C52 C54 111.6(2) . . ?
C53 C52 H52 107.6 . . ?
C54 C52 H52 107.6 . . ?
C54 C52 C53 111.2(3) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C51 C55 H55 108.2 . . ?
C51 C55 C56 110.1(2) . . ?
C56 C55 H55 108.2 . . ?
C57 C55 C51 112.1(3) . . ?
C57 C55 H55 108.2 . . ?
C57 C55 C56 110.1(3) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C31 C58 C59 123.0(2) . . ?
C31 C58 C60 122.5(2) . . ?
C59 C58 C60 114.5(2) . . ?
C58 C59 H59 118.5 . . ?
C60 C59 C58 122.9(2) 2_676 . ?
C60 C59 H59 118.5 2_676 . ?
C58 C60 H60 118.7 . . ?
C59 C60 C58 122.6(2) 2_676 . ?
C59 C60 H60 118.7 2_676 . ?

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 C1 C28 C29 -13.1(4) . . . . ?
N1 C1 C28 C30 168.1(2) . . . . ?
N1 C2 C3 N2 -23.7(2) . . . . ?
N1 C4 C5 C6 -171.7(2) . . . . ?
N1 C4 C5 C10 7.0(3) . . . . ?
N1 C4 C9 C8 172.5(2) . . . . ?
N1 C4 C9 C13 -7.0(3) . . . . ?
N2 C1 C28 C29 166.4(2) . . . . ?
N2 C1 C28 C30 -12.3(4) . . . . ?
N2 C16 C17 C18 -172.8(2) . . . . ?
N2 C16 C17 C22 7.2(3) . . . . ?
N2 C16 C21 C20 171.5(2) . . . . ?
N2 C16 C21 C25 -8.7(3) . . . . ?
N3 C31 C58 C59 166.1(2) . . . . ?
N3 C31 C58 C60 -13.5(4) . . . . ?
N3 C32 C33 N4 -24.7(2) . . . . ?
N3 C34 C35 C36 -173.8(2) . . . . ?
N3 C34 C35 C40 5.5(4) . . . . ?
N3 C34 C39 C38 173.6(2) . . . . ?
N3 C34 C39 C43 -4.7(3) . . . . ?
N4 C31 C58 C59 -12.9(4) . . . . ?
N4 C31 C58 C60 167.5(2) . . . . ?
N4 C46 C47 C48 -176.4(2) . . . . ?
N4 C46 C47 C52 2.4(4) . . . . ?
N4 C46 C51 C50 175.6(2) . . . . ?
N4 C46 C51 C55 -3.6(3) . . . . ?
C1 N1 C2 C3 20.6(2) . . . . ?
C1 N1 C4 C5 -56.8(3) . . . . ?
C1 N1 C4 C9 129.1(2) . . . . ?
C1 N2 C3 C2 19.8(2) . . . . ?
C1 N2 C16 C17 -57.5(3) . . . . ?
C1 N2 C16 C21 129.4(2) . . . . ?
C1 C28 C29 C30 -177.9(2) . . . 2_565 ?
C1 C28 C30 C29 177.9(2) . . . 2_565 ?
C2 N1 C1 N2 -8.9(2) . . . . ?
C2 N1 C1 C28 170.7(2) . . . . ?
C2 N1 C4 C5 83.9(3) . . . . ?
C2 N1 C4 C9 -90.3(3) . . . . ?
C3 N2 C1 N1 -7.4(2) . . . . ?
C3 N2 C1 C28 173.0(2) . . . . ?
C3 N2 C16 C17 86.3(3) . . . . ?
C3 N2 C16 C21 -86.8(3) . . . . ?
C4 N1 C1 N2 134.0(2) . . . . ?
C4 N1 C1 C28 -46.4(3) . . . . ?
C4 N1 C2 C3 -125.7(2) . . . . ?
C4 C5 C6 C7 -1.3(3) . . . . ?
C4 C5 C10 C11 117.7(3) . . . . ?
C4 C5 C10 C12 -117.9(3) . . . . ?
C4 C9 C13 C14 -122.1(2) . . . . ?
C4 C9 C13 C15 115.1(2) . . . . ?
C5 C4 C9 C8 -1.6(3) . . . . ?
C5 C4 C9 C13 178.9(2) . . . . ?
C5 C6 C7 C8 -0.3(4) . . . . ?
C6 C5 C10 C11 -63.6(3) . . . . ?
C6 C5 C10 C12 60.8(3) . . . . ?
C6 C7 C8 C9 1.0(4) . . . . ?
C7 C8 C9 C4 0.0(4) . . . . ?
C7 C8 C9 C13 179.5(2) . . . . ?
C8 C9 C13 C14 58.4(3) . . . . ?
C8 C9 C13 C15 -64.4(3) . . . . ?
C9 C4 C5 C6 2.3(3) . . . . ?
C9 C4 C5 C10 -179.1(2) . . . . ?
C10 C5 C6 C7 179.9(2) . . . . ?
C16 N2 C1 N1 138.2(2) . . . . ?
C16 N2 C1 C28 -41.4(3) . . . . ?
C16 N2 C3 C2 -129.3(2) . . . . ?
C16 C17 C18 C19 1.8(3) . . . . ?
C16 C17 C22 C23 110.0(3) . . . . ?
C16 C17 C22 C24 -125.6(2) . . . . ?
C16 C21 C25 C26 -125.2(2) . . . . ?
C16 C21 C25 C27 111.4(3) . . . . ?
C17 C16 C21 C20 -1.5(3) . . . . ?
C17 C16 C21 C25 178.2(2) . . . . ?
C17 C18 C19 C20 -2.1(4) . . . . ?
C18 C17 C22 C23 -69.9(3) . . . . ?
C18 C17 C22 C24 54.5(3) . . . . ?
C18 C19 C20 C21 0.5(4) . . . . ?
C19 C20 C21 C16 1.3(3) . . . . ?
C19 C20 C21 C25 -178.5(2) . . . . ?
C20 C21 C25 C26 54.5(3) . . . . ?
C20 C21 C25 C27 -68.9(3) . . . . ?
C21 C16 C17 C18 0.0(3) . . . . ?
C21 C16 C17 C22 -179.9(2) . . . . ?
C22 C17 C18 C19 -178.2(2) . . . . ?
C29 C28 C30 C29 -0.9(4) . . . 2_565 ?
C30 C28 C29 C30 0.9(4) . . . 2_565 ?
C31 N3 C32 C33 21.2(3) . . . . ?
C31 N3 C34 C35 -57.2(3) . . . . ?
C31 N3 C34 C39 127.8(2) . . . . ?
C31 N4 C33 C32 21.0(3) . . . . ?
C31 N4 C46 C47 -55.7(3) . . . . ?
C31 N4 C46 C51 128.7(2) . . . . ?
C31 C58 C59 C60 -179.7(2) . . . 2_676 ?
C31 C58 C60 C59 179.7(2) . . . 2_676 ?
C32 N3 C31 N4 -8.9(3) . . . . ?
C32 N3 C31 C58 172.0(2) . . . . ?
C32 N3 C34 C35 86.3(3) . . . . ?
C32 N3 C34 C39 -88.7(3) . . . . ?
C33 N4 C31 N3 -8.3(3) . . . . ?
C33 N4 C31 C58 170.9(2) . . . . ?
C33 N4 C46 C47 88.0(3) . . . . ?
C33 N4 C46 C51 -87.6(3) . . . . ?
C34 N3 C31 N4 136.7(2) . . . . ?
C34 N3 C31 C58 -42.4(4) . . . . ?
C34 N3 C32 C33 -127.3(2) . . . . ?
C34 C35 C36 C37 0.3(4) . . . . ?
C34 C35 C40 C41 -117.7(3) . . . . ?
C34 C35 C40 C42 117.1(3) . . . . ?
C34 C39 C43 C44 106.2(3) . . . . ?
C34 C39 C43 C45 -129.7(3) . . . . ?
C35 C34 C39 C38 -1.5(4) . . . . ?
C35 C34 C39 C43 -179.7(2) . . . . ?
C35 C36 C37 C38 -1.2(4) . . . . ?
C36 C35 C40 C41 61.6(3) . . . . ?
C36 C35 C40 C42 -63.6(3) . . . . ?
C36 C37 C38 C39 0.7(4) . . . . ?
C37 C38 C39 C34 0.6(4) . . . . ?
C37 C38 C39 C43 178.9(2) . . . . ?
C38 C39 C43 C44 -72.0(3) . . . . ?
C38 C39 C43 C45 52.1(3) . . . . ?
C39 C34 C35 C36 1.0(4) . . . . ?
C39 C34 C35 C40 -179.7(2) . . . . ?
C40 C35 C36 C37 -179.0(2) . . . . ?
C46 N4 C31 N3 137.7(2) . . . . ?
C46 N4 C31 C58 -43.2(4) . . . . ?
C46 N4 C33 C32 -127.5(2) . . . . ?
C46 C47 C48 C49 1.1(4) . . . . ?
C46 C47 C52 C53 -121.4(3) . . . . ?
C46 C47 C52 C54 114.0(3) . . . . ?
C46 C51 C55 C56 101.2(3) . . . . ?
C46 C51 C55 C57 -135.9(3) . . . . ?
C47 C46 C51 C50 0.0(4) . . . . ?
C47 C46 C51 C55 -179.2(2) . . . . ?
C47 C48 C49 C50 -0.4(4) . . . . ?
C48 C47 C52 C53 57.4(3) . . . . ?
C48 C47 C52 C54 -67.2(3) . . . . ?
C48 C49 C50 C51 -0.6(4) . . . . ?
C49 C50 C51 C46 0.8(4) . . . . ?
C49 C50 C51 C55 180.0(2) . . . . ?
C50 C51 C55 C56 -78.0(3) . . . . ?
C50 C51 C55 C57 44.9(4) . . . . ?
C51 C46 C47 C48 -1.0(3) . . . . ?
C51 C46 C47 C52 177.8(2) . . . . ?
C52 C47 C48 C49 -177.7(2) . . . . ?
C59 C58 C60 C59 0.1(4) . . . 2_676 ?
C60 C58 C59 C60 -0.1(4) . . . 2_676 ?

_olex2_date_sample_data_collection 2017-11-15
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.534
_oxdiff_exptl_absorpt_empirical_full_min 0.728
####################################################################### 
# 
# 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_rottschaefer57
_database_code_depnum_ccdc_archive 'CCDC 1826570'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_audit_creation_date             2017-11-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H84 N4, C4 H8 O'
_chemical_formula_sum            'C70 H92 N4 O'
_chemical_formula_weight         1005.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C66 H84 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      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                   9.3970(3)
_cell_length_b                   11.5574(5)
_cell_length_c                   15.1108(6)
_cell_angle_alpha                70.870(4)
_cell_angle_beta                 84.424(3)
_cell_angle_gamma                76.360(3)
_cell_volume                     1506.40(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11350
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9740
_cell_measurement_theta_min      3.0880
_shelx_estimated_absorpt_T_max   0.987
_shelx_estimated_absorpt_T_min   0.844
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (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            'metallic green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0131
0 0 -1 0.0131
1 5 3 0.0917
0 -1 0 0.0752
0 1 0 0.0752
-5 -3 -1 0.1664
5 3 1 0.1664
5 5 1 0.1439
1 0 0 0.1740
-5 3 2 0.1701

_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.026
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
-0.0010 0.0023 0.9997 -0.1017 -0.0194 -0.0302
0.0010 -0.0023 -0.9997 0.1017 0.0194 0.0302
1.0008 5.0042 2.9923 -0.2676 -0.0704 0.6138
-0.0010 -0.9996 0.0017 -0.0003 -0.0305 -0.1412
0.0010 0.9996 -0.0017 0.0003 0.0305 0.1412
-4.9971 -2.9983 -1.0040 -0.0791 0.7514 -0.3842
4.9971 2.9983 1.0040 0.0791 -0.7514 0.3842
4.9990 4.9974 1.0005 0.0797 -0.6904 0.6667
0.9991 -0.0005 0.0019 0.0360 -0.1647 -0.0019
-4.9944 3.0060 1.9847 -0.3825 0.8762 0.3727

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25880
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         3.096
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00  -4.00   1.00    1.00    --  -24.12 -77.00 -90.00   90
  2  ω    -95.00 -65.00   1.00    1.00    --  -24.12 -38.00-180.00   30
  3  ω   -102.00 -34.00   1.00    1.00    --  -24.12 178.00 -90.00   68
  4  ω    -50.00   4.00   1.00    1.00    --  -24.12 -77.00 150.00   54
  5  ω    -68.00  -4.00   1.00    1.00    --  -24.12 -77.00  90.00   64
  6  ω    -42.00 -15.00   1.00    1.00    --  -24.12 -19.00-180.00   27
  7  ω    -82.00 -54.00   1.00    1.00    --  -24.12 -19.00-180.00   28
  8  ω    -35.00  -8.00   1.00    1.00    --  -24.12 -77.00   0.00   27
  9  ω   -101.00   6.00   1.00    1.00    --  -24.12 -19.00  60.00  107
 10  ω    -79.00 -54.00   1.00    1.00    --  -24.12 -77.00 150.00   25
 11  ω    -94.00 -61.00   1.00    1.00    --  -24.12 -77.00   0.00   33
 12  ω    -61.00 -13.00   1.00    1.00    --  -24.12 -38.00-180.00   48
 13  ω   -100.00 -73.00   1.00    1.00    --  -24.12 -19.00 -30.00   27
 14  ω    -55.00  -6.00   1.00    1.00    --  -24.12 -19.00 -30.00   49
 15  ω    -65.00 -18.00   1.00    1.00    --  -24.12 103.00-118.00   47
 16  ω    -73.00 -10.00   1.00    1.00    --  -24.12 -57.00 -30.00   63
 17  ω    -92.00 -56.00   1.00    1.00    --  -24.12-178.00-180.00   36
 18  ω    -98.00 -36.00   1.00    1.00    --  -24.12-178.00  90.00   62
 19  ω   -109.00 -34.00   1.00    1.00    --  -24.12 178.00   0.00   75
 20  ω      3.00  33.00   1.00    1.00    --   24.12  38.00 -90.00   30
 21  ω     20.00  57.00   1.00    1.00    --   24.12  57.00   0.00   37
 22  ω     36.00  63.00   1.00    1.00    --   24.12 -99.00  60.00   27
 23  ω     76.00 101.00   1.00    1.00    --   24.12  19.00  60.00   25
 24  ω     -7.00  43.00   1.00    1.00    --   24.12  19.00  60.00   50
 25  ω     48.00  73.00   1.00    1.00    --   24.12-116.00-128.30   25
 26  ω     86.00 111.00   1.00    1.33    --  111.00  61.00-180.00   25
 27  ω     85.00 112.00   1.00    1.33    --  111.00  61.00-120.00   27
 28  ω     94.00 121.00   1.00    1.33    --  111.00-125.00   0.00   27
 29  ω    115.00 177.00   1.00    1.33    --  111.00  61.00-180.00   62
 30  ω     81.00 112.00   1.00    1.33    --  111.00  77.00 -60.00   31
 31  ω     50.00 137.00   1.00    1.33    --  111.00 -77.00-120.00   87
 32  ω     84.00 110.00   1.00    1.33    --  111.00  66.00-170.20   26
 33  ω     44.00  77.00   1.00    1.33    --  111.00-125.00   0.00   33
 34  ω    134.00 161.00   1.00    1.33    --  111.00  77.00 150.00   27
 35  ω     42.00 113.00   1.00    1.33    --  111.00-125.00-180.00   71
 36  ω     81.00 107.00   1.00    1.33    --  111.00  77.00 150.00   26
 37  ω    113.00 178.00   1.00    1.33    --  111.00  77.00   0.00   65
 38  ω     86.00 113.00   1.00    1.33    --  111.00  61.00 -90.00   27
 39  ω     85.00 111.00   1.00    1.33    --  111.00  60.00  10.47   26
 40  ω     88.00 143.00   1.00    1.33    --  111.00  49.00   2.27   55
 41  ω     86.00 111.00   1.00    1.33    --  111.00  61.00 120.00   25
 42  ω    131.00 158.00   1.00    1.33    --  111.00  77.00  90.00   27
 43  ω     82.00 107.00   1.00    1.33    --  111.00  77.00  90.00   25
 44  ω     85.00 111.00   1.00    1.33    --  111.00  61.00  30.00   26
 45  ω     85.00 111.00   1.00    1.33    --  111.00  61.00 -30.00   26
 46  ω     81.00 108.00   1.00    1.33    --  111.00  77.00   0.00   27
 47  ω     85.00 111.00   1.00    1.33    --  111.00  61.00 150.00   26
 48  ω     81.00 107.00   1.00    1.33    --  111.00  77.00-150.00   26
 49  ω     85.00 112.00   1.00    1.33    --  111.00  61.00   0.00   27
 50  ω    124.00 151.00   1.00    1.33    --  111.00  45.00 -60.00   27
 51  ω     81.00 107.00   1.00    1.33    --  111.00  77.00 120.00   26
 52  ω    116.00 176.00   1.00    1.33    --  111.00  77.00 120.00   60
 53  ω     89.00 115.00   1.00    1.33    --  111.00  45.00 -60.00   26
 54  ω     41.00  94.00   1.00    1.33    --  111.00 -77.00  60.00   53
 55  ω    115.00 140.00   1.00    1.33    --  111.00 -77.00  60.00   25
 56  ω     89.00 116.00   1.00    1.33    --  111.00  45.00 -30.00   27
 57  ω     33.00  98.00   1.00    1.33    --  111.00 -94.00-150.00   65
 58  ω     89.00 121.00   1.00    1.33    --  111.00  45.00  60.00   32
 59  ω    133.00 160.00   1.00    1.33    --  111.00  65.00-128.53   27
 60  ω    132.00 177.00   1.00    1.33    --  111.00  62.00 -22.85   45
 61  ω    122.00 172.00   1.00    1.33    --  111.00  77.00  30.00   50
 62  ω     85.00 111.00   1.00    1.33    --  111.00  61.00  90.00   26
 63  ω     81.00 108.00   1.00    1.33    --  111.00  77.00  30.00   27
 64  ω    114.00 175.00   1.00    1.33    --  111.00  77.00-120.00   61
 65  ω     81.00 108.00   1.00    1.33    --  111.00  77.00-120.00   27
 66  ω     41.00 109.00   1.00    1.33    --  111.00 -94.00  30.00   68
 67  ω     84.00 110.00   1.00    1.33    --  111.00  65.00-128.53   26
 68  ω     85.00 122.00   1.00    1.33    --  111.00  61.00-150.00   37
 69  ω     89.00 143.00   1.00    1.33    --  111.00  45.00 120.00   54
 70  ω    122.00 176.00   1.00    1.33    --  111.00  77.00  60.00   54
 71  ω     89.00 134.00   1.00    1.33    --  111.00  45.00-180.00   45
 72  ω     89.00 116.00   1.00    1.33    --  111.00  45.00-150.00   27
 73  ω    151.00 176.00   1.00    1.33    --  111.00  45.00-150.00   25
 74  ω     92.00 119.00   1.00    1.33    --  111.00  45.00  30.00   27
 75  ω     85.00 143.00   1.00    1.33    --  111.00  61.00 -60.00   58
 76  ω     94.00 119.00   1.00    1.33    --  111.00-125.00-120.00   25
 77  ω     89.00 115.00   1.00    1.33    --  111.00  45.00 -90.00   26
 78  ω     89.00 123.00   1.00    1.33    --  111.00  45.00  90.00   34
 79  ω     81.00 107.00   1.00    1.33    --  111.00  77.00  60.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0362254000
_diffrn_orient_matrix_UB_12      0.0000593000
_diffrn_orient_matrix_UB_13      -0.1016568000
_diffrn_orient_matrix_UB_21      -0.1647963000
_diffrn_orient_matrix_UB_22      0.0306327000
_diffrn_orient_matrix_UB_23      -0.0196330000
_diffrn_orient_matrix_UB_31      -0.0017315000
_diffrn_orient_matrix_UB_32      0.1412455000
_diffrn_orient_matrix_UB_33      -0.0305041000
_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                5051
_reflns_number_total             5928
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.038
_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)+(0.0645P)²+0.5839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1314
_refine_special_details          
'Disordered C4 H8 O near an inversion center was squeezed using the routine of Olex. The sum formular contains the solvent for further calculations. Disorder of C10, C11, C12 over two sites (74:26),SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10B) = Uanis(C10A)
Uanis(C12B) = Uanis(C12A)
Uanis(C11B) = Uanis(C11A)
3. Others
 Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12B)=
 Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12A)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10A(H10A), C10B(H10B), C13(H13), C22(H22), C25(H25)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C32(H32), C33(H33)
4.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C12A(H12A,H12B,H12C), C12B(H12D,
 H12E,H12F), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
N1 N 0.82435(12) 0.28651(10) 0.72773(7) 0.0207(2) Uani 1 1 d . . . . .
N2 N 0.65312(11) 0.46477(10) 0.70828(7) 0.0187(2) Uani 1 1 d . . . . .
C1 C 0.77822(13) 0.39052(11) 0.75777(8) 0.0172(3) Uani 1 1 d . . . . .
C2 C 0.61938(15) 0.40686(15) 0.64199(11) 0.0314(3) Uani 1 1 d . . . . .
H2A H 0.611070 0.466047 0.579068 0.038 Uiso 1 1 calc R . . . .
H2B H 0.528050 0.379017 0.659690 0.038 Uiso 1 1 calc R . . . .
C3 C 0.7442(2) 0.29788(15) 0.64679(12) 0.0400(4) Uani 1 1 d . . . . .
H3A H 0.709336 0.222273 0.655315 0.048 Uiso 1 1 calc R . . . .
H3B H 0.805105 0.314027 0.590333 0.048 Uiso 1 1 calc R . . . .
C4 C 0.96358(15) 0.20019(13) 0.74464(9) 0.0251(3) Uani 1 1 d . . . . .
C5 C 1.09236(16) 0.23884(16) 0.70480(10) 0.0348(4) Uani 1 1 d . . . . .
C6 C 1.22463(18) 0.14986(18) 0.72517(11) 0.0453(5) Uani 1 1 d . . . . .
H6 H 1.311831 0.173190 0.700068 0.054 Uiso 1 1 calc R . . . .
C7 C 1.2281(2) 0.02809(17) 0.78184(12) 0.0459(5) Uani 1 1 d . . . . .
H7 H 1.317282 -0.029141 0.795393 0.055 Uiso 1 1 calc R . . . .
C8 C 1.0997(2) -0.00879(15) 0.81834(12) 0.0434(4) Uani 1 1 d . . . . .
H8 H 1.103094 -0.091485 0.855212 0.052 Uiso 1 1 calc R . . . .
C9 C 0.96407(18) 0.07638(14) 0.80077(10) 0.0322(3) Uani 1 1 d . . . . .
C10A C 1.0950(3) 0.3781(3) 0.6436(2) 0.0302(6) Uani 0.739(3) 1 d . . P A 1
H10A H 0.992833 0.423791 0.633826 0.036 Uiso 0.739(3) 1 calc R . P A 1
C10B C 1.0792(11) 0.3463(9) 0.6282(7) 0.0302(6) Uani 0.261(3) 1 d . . P A 2
H10B H 0.979512 0.396892 0.627940 0.036 Uiso 0.261(3) 1 calc R . P A 2
C11A C 1.1626(3) 0.3796(3) 0.54692(17) 0.0492(7) Uani 0.739(3) 1 d . . P A 1
H11A H 1.264478 0.339019 0.553185 0.074 Uiso 0.739(3) 1 calc GR . P A 1
H11B H 1.152944 0.464777 0.506925 0.074 Uiso 0.739(3) 1 calc GR . P A 1
H11C H 1.112834 0.335871 0.520054 0.074 Uiso 0.739(3) 1 calc GR . P A 1
C11B C 1.1152(9) 0.3269(9) 0.5307(5) 0.0492(7) Uani 0.261(3) 1 d . . P A 2
H11D H 1.212617 0.277181 0.530335 0.074 Uiso 0.261(3) 1 calc GR . P A 2
H11E H 1.108573 0.406997 0.483165 0.074 Uiso 0.261(3) 1 calc GR . P A 2
H11F H 1.046537 0.284654 0.518282 0.074 Uiso 0.261(3) 1 calc GR . P A 2
C12A C 1.1696(3) 0.4485(3) 0.6880(2) 0.0420(6) Uani 0.739(3) 1 d . . P A 1
H12A H 1.123627 0.448154 0.747644 0.063 Uiso 0.739(3) 1 calc GR . P A 1
H12B H 1.160932 0.533473 0.647773 0.063 Uiso 0.739(3) 1 calc GR . P A 1
H12C H 1.271329 0.408179 0.696613 0.063 Uiso 0.739(3) 1 calc GR . P A 1
C12B C 1.1840(9) 0.4127(8) 0.6504(6) 0.0420(6) Uani 0.261(3) 1 d . . P A 2
H12D H 1.155153 0.428621 0.708789 0.063 Uiso 0.261(3) 1 calc GR . P A 2
H12E H 1.182659 0.490799 0.601416 0.063 Uiso 0.261(3) 1 calc GR . P A 2
H12F H 1.281118 0.361087 0.655223 0.063 Uiso 0.261(3) 1 calc GR . P A 2
C13 C 0.8238(2) 0.03600(15) 0.84299(13) 0.0435(4) Uani 1 1 d . . . . .
H13 H 0.742768 0.108672 0.821025 0.052 Uiso 1 1 calc R . . . .
C14 C 0.7972(3) -0.06847(19) 0.80919(17) 0.0750(8) Uani 1 1 d . . . . .
H14A H 0.790477 -0.038971 0.742179 0.112 Uiso 1 1 calc GR . . . .
H14B H 0.707530 -0.091746 0.836732 0.112 Uiso 1 1 calc GR . . . .
H14C H 0.877062 -0.140075 0.827499 0.112 Uiso 1 1 calc GR . . . .
C15 C 0.8224(2) -0.00257(17) 0.95002(13) 0.0462(4) Uani 1 1 d . . . . .
H15A H 0.902020 -0.072714 0.973728 0.069 Uiso 1 1 calc GR . . . .
H15B H 0.731327 -0.025709 0.974505 0.069 Uiso 1 1 calc GR . . . .
H15C H 0.832780 0.066521 0.968982 0.069 Uiso 1 1 calc GR . . . .
C16 C 0.52636(13) 0.52522(12) 0.75162(9) 0.0200(3) Uani 1 1 d . . . . .
C17 C 0.46155(14) 0.45779(13) 0.83469(10) 0.0258(3) Uani 1 1 d . . . . .
C18 C 0.33213(16) 0.51986(15) 0.86731(11) 0.0346(3) Uani 1 1 d . . . . .
H18 H 0.288010 0.477375 0.922290 0.041 Uiso 1 1 calc R . . . .
C19 C 0.26756(16) 0.64275(15) 0.82023(11) 0.0346(3) Uani 1 1 d . . . . .
H19 H 0.179910 0.681393 0.842712 0.041 Uiso 1 1 calc R . . . .
C20 C 0.33355(15) 0.70823(14) 0.73956(10) 0.0280(3) Uani 1 1 d . . . . .
H20 H 0.290435 0.791366 0.708571 0.034 Uiso 1 1 calc R . . . .
C21 C 0.46409(14) 0.65115(13) 0.70402(9) 0.0217(3) Uani 1 1 d . . . . .
C22 C 0.52369(15) 0.32179(14) 0.89132(11) 0.0314(3) Uani 1 1 d . . . . .
H22 H 0.612134 0.291458 0.858227 0.038 Uiso 1 1 calc R . . . .
C23 C 0.41740(19) 0.23712(17) 0.89936(17) 0.0546(5) Uani 1 1 d . . . . .
H23A H 0.328640 0.265714 0.930474 0.082 Uiso 1 1 calc GR . . . .
H23B H 0.461174 0.152539 0.934811 0.082 Uiso 1 1 calc GR . . . .
H23C H 0.395547 0.239838 0.837866 0.082 Uiso 1 1 calc GR . . . .
C24 C 0.5691(2) 0.31345(19) 0.98848(12) 0.0474(5) Uani 1 1 d . . . . .
H24A H 0.640102 0.363621 0.981544 0.071 Uiso 1 1 calc GR . . . .
H24B H 0.610962 0.227718 1.022378 0.071 Uiso 1 1 calc GR . . . .
H24C H 0.484592 0.343795 1.022283 0.071 Uiso 1 1 calc GR . . . .
C25 C 0.53390(15) 0.72636(13) 0.61550(9) 0.0253(3) Uani 1 1 d . . . . .
H25 H 0.629553 0.675155 0.605754 0.030 Uiso 1 1 calc R . . . .
C26 C 0.44138(18) 0.75490(16) 0.52971(11) 0.0377(4) Uani 1 1 d . . . . .
H26A H 0.428982 0.677734 0.523679 0.056 Uiso 1 1 calc GR . . . .
H26B H 0.489978 0.798963 0.474474 0.056 Uiso 1 1 calc GR . . . .
H26C H 0.347209 0.805886 0.537237 0.056 Uiso 1 1 calc GR . . . .
C27 C 0.55918(19) 0.84828(15) 0.62408(12) 0.0379(4) Uani 1 1 d . . . . .
H27A H 0.466527 0.902214 0.630230 0.057 Uiso 1 1 calc GR . . . .
H27B H 0.610484 0.889577 0.569076 0.057 Uiso 1 1 calc GR . . . .
H27C H 0.616397 0.829519 0.678298 0.057 Uiso 1 1 calc GR . . . .
C28 C 0.84117(13) 0.41930(12) 0.82494(8) 0.0177(3) Uani 1 1 d . . . . .
C29 C 0.80257(13) 0.54309(12) 0.83442(9) 0.0197(3) Uani 1 1 d . . . . .
H29 H 0.733931 0.604542 0.794360 0.024 Uiso 1 1 calc R . . . .
C30 C 0.86299(13) 0.57315(12) 0.89988(9) 0.0193(3) Uani 1 1 d . . . . .
H30 H 0.835021 0.654988 0.901923 0.023 Uiso 1 1 calc R . . . .
C31 C 0.96840(12) 0.48425(11) 0.96631(8) 0.0170(3) Uani 1 1 d . . . . .
C32 C 1.00344(13) 0.36021(12) 0.95771(9) 0.0190(3) Uani 1 1 d . . . . .
H32 H 1.068954 0.297933 0.999532 0.023 Uiso 1 1 calc R . . . .
C33 C 0.94581(13) 0.32943(12) 0.89169(9) 0.0194(3) Uani 1 1 d . . . . .
H33 H 0.974645 0.247754 0.889368 0.023 Uiso 1 1 calc R . . . .


_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
N1 C1 1.3830(16) . ?
N1 C3 1.4515(17) . ?
N1 C4 1.4333(16) . ?
N2 C1 1.3972(15) . ?
N2 C2 1.4674(16) . ?
N2 C16 1.4463(15) . ?
C1 C28 1.3862(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.493(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.401(2) . ?
C4 C9 1.403(2) . ?
C5 C6 1.400(2) . ?
C5 C10A 1.576(3) . ?
C5 C10B 1.382(10) . ?
C6 H6 0.9300 . ?
C6 C7 1.382(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.379(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.402(2) . ?
C9 C13 1.514(2) . ?
C10A H10A 0.9800 . ?
C10A C11A 1.532(4) . ?
C10A C12A 1.524(3) . ?
C10B H10B 0.9800 . ?
C10B C11B 1.556(11) . ?
C10B C12B 1.504(10) . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 0.9600 . ?
C11B H11D 0.9600 . ?
C11B H11E 0.9600 . ?
C11B H11F 0.9600 . ?
C12A H12A 0.9600 . ?
C12A H12B 0.9600 . ?
C12A H12C 0.9600 . ?
C12B H12D 0.9600 . ?
C12B H12E 0.9600 . ?
C12B H12F 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.534(2) . ?
C13 C15 1.530(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.4100(18) . ?
C16 C21 1.4043(18) . ?
C17 C18 1.393(2) . ?
C17 C22 1.525(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.381(2) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.3968(18) . ?
C21 C25 1.5203(18) . ?
C22 H22 0.9800 . ?
C22 C23 1.526(2) . ?
C22 C24 1.535(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.5326(19) . ?
C25 C27 1.530(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.4417(18) . ?
C28 C33 1.4448(17) . ?
C29 H29 0.9300 . ?
C29 C30 1.3597(18) . ?
C30 H30 0.9300 . ?
C30 C31 1.4429(17) . ?
C31 C31 1.408(2) 2_767 ?
C31 C32 1.4393(17) . ?
C32 H32 0.9300 . ?
C32 C33 1.3578(17) . ?
C33 H33 0.9300 . ?

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 C3 111.68(11) . . ?
C1 N1 C4 126.47(11) . . ?
C4 N1 C3 117.92(11) . . ?
C1 N2 C2 109.63(10) . . ?
C1 N2 C16 122.98(10) . . ?
C16 N2 C2 114.72(10) . . ?
N1 C1 N2 107.89(10) . . ?
N1 C1 C28 127.63(11) . . ?
C28 C1 N2 124.49(11) . . ?
N2 C2 H2A 110.6 . . ?
N2 C2 H2B 110.6 . . ?
N2 C2 C3 105.58(11) . . ?
H2A C2 H2B 108.8 . . ?
C3 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
N1 C3 C2 103.73(12) . . ?
N1 C3 H3A 111.0 . . ?
N1 C3 H3B 111.0 . . ?
C2 C3 H3A 111.0 . . ?
C2 C3 H3B 111.0 . . ?
H3A C3 H3B 109.0 . . ?
C5 C4 N1 120.67(12) . . ?
C5 C4 C9 122.14(13) . . ?
C9 C4 N1 117.17(13) . . ?
C4 C5 C10A 123.06(15) . . ?
C6 C5 C4 117.57(15) . . ?
C6 C5 C10A 119.29(17) . . ?
C10B C5 C4 117.7(4) . . ?
C10B C5 C6 121.9(4) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.29(17) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.17(15) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.06(16) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C13 121.48(13) . . ?
C8 C9 C4 117.73(16) . . ?
C8 C9 C13 120.77(15) . . ?
C5 C10A H10A 106.9 . . ?
C11A C10A C5 109.4(2) . . ?
C11A C10A H10A 106.9 . . ?
C12A C10A C5 115.2(2) . . ?
C12A C10A H10A 106.9 . . ?
C12A C10A C11A 111.1(2) . . ?
C5 C10B H10B 108.9 . . ?
C5 C10B C11B 116.4(7) . . ?
C5 C10B C12B 102.2(6) . . ?
C11B C10B H10B 108.9 . . ?
C12B C10B H10B 108.9 . . ?
C12B C10B C11B 111.3(7) . . ?
C10A C11A H11A 109.5 . . ?
C10A C11A H11B 109.5 . . ?
C10A C11A H11C 109.5 . . ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C10B C11B H11D 109.5 . . ?
C10B C11B H11E 109.5 . . ?
C10B C11B H11F 109.5 . . ?
H11D C11B H11E 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C10A C12A H12A 109.5 . . ?
C10A C12A H12B 109.5 . . ?
C10A C12A H12C 109.5 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C10B C12B H12D 109.5 . . ?
C10B C12B H12E 109.5 . . ?
C10B C12B H12F 109.5 . . ?
H12D C12B H12E 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C9 C13 H13 107.4 . . ?
C9 C13 C14 111.34(18) . . ?
C9 C13 C15 111.52(13) . . ?
C14 C13 H13 107.4 . . ?
C15 C13 H13 107.4 . . ?
C15 C13 C14 111.45(15) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 121.25(12) . . ?
C21 C16 N2 117.29(11) . . ?
C21 C16 C17 121.30(12) . . ?
C16 C17 C22 124.48(12) . . ?
C18 C17 C16 117.68(13) . . ?
C18 C17 C22 117.84(13) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.79(14) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.85(13) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.87(13) . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C25 122.15(11) . . ?
C20 C21 C16 118.48(12) . . ?
C20 C21 C25 119.37(12) . . ?
C17 C22 H22 107.6 . . ?
C17 C22 C23 112.24(13) . . ?
C17 C22 C24 110.53(14) . . ?
C23 C22 H22 107.6 . . ?
C23 C22 C24 111.04(15) . . ?
C24 C22 H22 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.8 . . ?
C21 C25 C26 111.12(12) . . ?
C21 C25 C27 111.98(12) . . ?
C26 C25 H25 107.8 . . ?
C27 C25 H25 107.8 . . ?
C27 C25 C26 110.09(12) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 C28 C29 121.42(11) . . ?
C1 C28 C33 123.71(11) . . ?
C29 C28 C33 114.85(11) . . ?
C28 C29 H29 118.8 . . ?
C30 C29 C28 122.31(12) . . ?
C30 C29 H29 118.8 . . ?
C29 C30 H30 118.4 . . ?
C29 C30 C31 123.19(12) . . ?
C31 C30 H30 118.4 . . ?
C31 C31 C30 123.12(14) 2_767 . ?
C31 C31 C32 122.86(14) 2_767 . ?
C32 C31 C30 114.03(11) . . ?
C31 C32 H32 118.3 . . ?
C33 C32 C31 123.40(11) . . ?
C33 C32 H32 118.3 . . ?
C28 C33 H33 118.9 . . ?
C32 C33 C28 122.20(12) . . ?
C32 C33 H33 118.9 . . ?

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 C1 C28 C29 165.68(12) . . . . ?
N1 C1 C28 C33 -16.0(2) . . . . ?
N1 C4 C5 C6 179.31(13) . . . . ?
N1 C4 C5 C10A 2.8(2) . . . . ?
N1 C4 C5 C10B -19.6(5) . . . . ?
N1 C4 C9 C8 -179.60(12) . . . . ?
N1 C4 C9 C13 -0.9(2) . . . . ?
N2 C1 C28 C29 -14.60(19) . . . . ?
N2 C1 C28 C33 163.74(11) . . . . ?
N2 C2 C3 N1 10.92(17) . . . . ?
N2 C16 C17 C18 -174.28(13) . . . . ?
N2 C16 C17 C22 5.9(2) . . . . ?
N2 C16 C21 C20 173.91(11) . . . . ?
N2 C16 C21 C25 -5.91(18) . . . . ?
C1 N1 C3 C2 -12.45(17) . . . . ?
C1 N1 C4 C5 -66.61(18) . . . . ?
C1 N1 C4 C9 114.56(15) . . . . ?
C1 N2 C2 C3 -6.35(16) . . . . ?
C1 N2 C16 C17 -49.89(17) . . . . ?
C1 N2 C16 C21 134.70(12) . . . . ?
C1 C28 C29 C30 179.96(12) . . . . ?
C1 C28 C33 C32 -178.80(12) . . . . ?
C2 N2 C1 N1 -1.24(14) . . . . ?
C2 N2 C1 C28 178.99(12) . . . . ?
C2 N2 C16 C17 87.80(15) . . . . ?
C2 N2 C16 C21 -87.60(14) . . . . ?
C3 N1 C1 N2 8.86(15) . . . . ?
C3 N1 C1 C28 -171.38(14) . . . . ?
C3 N1 C4 C5 89.13(17) . . . . ?
C3 N1 C4 C9 -89.70(16) . . . . ?
C4 N1 C1 N2 165.86(12) . . . . ?
C4 N1 C1 C28 -14.4(2) . . . . ?
C4 N1 C3 C2 -171.62(13) . . . . ?
C4 C5 C6 C7 0.5(2) . . . . ?
C4 C5 C10A C11A -122.6(2) . . . . ?
C4 C5 C10A C12A 111.5(2) . . . . ?
C4 C5 C10B C11B -101.8(7) . . . . ?
C4 C5 C10B C12B 136.7(5) . . . . ?
C4 C9 C13 C14 119.83(16) . . . . ?
C4 C9 C13 C15 -115.00(16) . . . . ?
C5 C4 C9 C8 1.6(2) . . . . ?
C5 C4 C9 C13 -179.75(14) . . . . ?
C5 C6 C7 C8 1.1(3) . . . . ?
C6 C5 C10A C11A 60.9(2) . . . . ?
C6 C5 C10A C12A -65.0(3) . . . . ?
C6 C5 C10B C11B 58.5(8) . . . . ?
C6 C5 C10B C12B -63.0(7) . . . . ?
C6 C7 C8 C9 -1.5(2) . . . . ?
C7 C8 C9 C4 0.1(2) . . . . ?
C7 C8 C9 C13 -178.53(15) . . . . ?
C8 C9 C13 C14 -61.5(2) . . . . ?
C8 C9 C13 C15 63.6(2) . . . . ?
C9 C4 C5 C6 -1.9(2) . . . . ?
C9 C4 C5 C10A -178.46(17) . . . . ?
C9 C4 C5 C10B 159.2(4) . . . . ?
C10A C5 C6 C7 177.21(18) . . . . ?
C10B C5 C6 C7 -159.8(4) . . . . ?
C16 N2 C1 N1 138.28(11) . . . . ?
C16 N2 C1 C28 -41.49(18) . . . . ?
C16 N2 C2 C3 -149.52(13) . . . . ?
C16 C17 C18 C19 0.6(2) . . . . ?
C16 C17 C22 C23 -120.12(17) . . . . ?
C16 C17 C22 C24 115.32(15) . . . . ?
C16 C21 C25 C26 110.78(14) . . . . ?
C16 C21 C25 C27 -125.65(14) . . . . ?
C17 C16 C21 C20 -1.49(19) . . . . ?
C17 C16 C21 C25 178.69(12) . . . . ?
C17 C18 C19 C20 -1.5(3) . . . . ?
C18 C17 C22 C23 60.1(2) . . . . ?
C18 C17 C22 C24 -64.50(17) . . . . ?
C18 C19 C20 C21 0.9(2) . . . . ?
C19 C20 C21 C16 0.5(2) . . . . ?
C19 C20 C21 C25 -179.63(13) . . . . ?
C20 C21 C25 C26 -69.04(16) . . . . ?
C20 C21 C25 C27 54.53(17) . . . . ?
C21 C16 C17 C18 0.9(2) . . . . ?
C21 C16 C17 C22 -178.88(13) . . . . ?
C22 C17 C18 C19 -179.58(15) . . . . ?
C28 C29 C30 C31 -1.10(19) . . . . ?
C29 C28 C33 C32 -0.36(17) . . . . ?
C29 C30 C31 C31 179.58(14) . . . 2_767 ?
C29 C30 C31 C32 -0.42(17) . . . . ?
C30 C31 C32 C33 1.56(17) . . . . ?
C31 C31 C32 C33 -178.44(14) 2_767 . . . ?
C31 C32 C33 C28 -1.18(19) . . . . ?
C33 C28 C29 C30 1.48(18) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 178.4 42.9 ?
2 0.479 -0.050 0.907 7.2 0.0 ?
3 0.521 0.050 0.093 7.2 0.0 ?

_olex2_date_sample_data_collection 2017-11-23
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.181
_oxdiff_exptl_absorpt_empirical_full_min 0.878
####################################################################### 
# 
# 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_rottschaefer51
_database_code_depnum_ccdc_archive 'CCDC 1826568'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_audit_creation_date             2017-11-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Br), 3.22(C H4 O), C66 H84 N4'
_chemical_formula_sum            'C69.21 H96.87 Br2 N4 O3.22'
_chemical_formula_weight         1196.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C68 H92 Br N4 O2'
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'
Br Br -0.2901 2.4595 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.3343(2)
_cell_length_b                   17.7848(3)
_cell_length_c                   20.1423(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.674(2)
_cell_angle_gamma                90
_cell_volume                     3327.41(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    33245
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      26.3630
_cell_measurement_theta_min      2.0270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -3 -5 0.0566
0 3 5 0.0566
0 -5 4 0.0541
0 5 -4 0.0541
5 2 4 0.1555
-5 -2 -4 0.1555

_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.108
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
-0.0001 -3.0008 -4.9981 0.1393 0.1595 -0.0279
0.0001 3.0008 4.9981 -0.1393 -0.1595 0.0279
-0.0014 -5.0025 3.9962 0.1612 -0.1629 -0.0856
0.0014 5.0025 -3.9962 -0.1612 0.1629 0.0856
4.9986 1.9983 3.9980 0.0294 -0.2204 0.3651
-4.9986 -1.9983 -3.9980 -0.0294 0.2204 -0.3651

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            192850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         1.531
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  94.00   1.00    8.00    --   24.94  77.00 120.00   98
  2  ω    -46.00  47.00   1.00    8.00    --   24.94 -38.00-180.00   93
  3  ω    -20.00  65.00   1.00    8.00    --   24.94 -99.00 -60.00   85
  4  ω    -47.00  63.00   1.00    8.00    --   24.94 -19.00  60.00  110
  5  ω     -4.00  94.00   1.00    8.00    --   24.94  77.00 -30.00   98
  6  ω     -4.00  94.00   1.00    8.00    --   24.94  77.00-150.00   98
  7  ω      3.00  96.00   1.00    8.00    --   24.94  38.00-180.00   93
  8  ω    -43.00  43.00   1.00    8.00    --   24.94 -57.00   0.00   86
  9  ω      6.00  93.00   1.00    8.00    --   24.94  57.00  90.00   87
 10  ω     -6.00  75.00   1.00    8.00    --   24.94-116.00 150.86   81
 11  ω    -97.00 -35.00   1.00    8.00    --  -23.50-178.00 -60.00   62
 12  ω    -95.00  48.00   1.00    8.00    --  -23.50   0.00-180.00  143
 13  ω    -95.00  48.00   1.00    8.00    --  -23.50   0.00-150.00  143
 14  ω      6.00  93.00   1.00    8.00    --   24.94  57.00 -90.00   87
 15  ω      6.00  93.00   1.00    8.00    --   24.94  57.00  30.00   87
 16  ω     14.00  95.00   1.00    8.00    --   24.94-149.00  57.00   81
 17  ω      5.00  82.00   1.00    8.00    --   24.94-129.00 -65.41   77
 18  ω    -44.00  54.00   1.00    8.00    --   24.94 -77.00  30.00   98
 19  ω    -20.00  65.00   1.00    8.00    --   24.94 -99.00   0.00   85
 20  ω     34.00 100.00   1.00    8.00    --   24.94-178.00 -60.00   66
 21  ω    -95.00  48.00   1.00    8.00    --  -23.50   0.00 -90.00  143
 22  ω    -95.00  48.00   1.00    8.00    --  -23.50   0.00 -60.00  143
 23  ω    -95.00  11.00   1.00    8.00    --  -23.50   0.00 -30.00  106
 24  ω    -95.00  48.00   1.00    8.00    --  -23.50   0.00-120.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0252004000
_diffrn_orient_matrix_UB_12      -0.0368200000
_diffrn_orient_matrix_UB_13      -0.0057554000
_diffrn_orient_matrix_UB_21      -0.0181906000
_diffrn_orient_matrix_UB_22      0.0047823000
_diffrn_orient_matrix_UB_23      -0.0347760000
_diffrn_orient_matrix_UB_31      0.0697476000
_diffrn_orient_matrix_UB_32      0.0145566000
_diffrn_orient_matrix_UB_33      -0.0031640000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7860
_reflns_number_total             9771
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.676
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         9771
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0733
_refine_ls_restrained_S_all      1.173
_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)+(0.0100P)²+7.9834P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1430
_refine_special_details          'Methanol O2/C35 is not fully occupied (0.61)'
_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, All O(H) groups
2. Others
 Sof(O2)=Sof(H2)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C32(H32), C33(H33)
3.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
3.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Br1 Br 0.51221(6) 0.16949(3) 0.17076(2) 0.07193(19) Uani 1 1 d . . . . .
O1 O 0.5475(3) 0.07422(14) 0.30901(14) 0.0478(7) Uani 1 1 d . . . . .
H1 H 0.542527 0.099412 0.274763 0.072 Uiso 1 1 calc GR . . . .
C34 C 0.5840(4) -0.0008(2) 0.2943(2) 0.0526(10) Uani 1 1 d . . . . .
H34A H 0.657356 -0.000752 0.264051 0.079 Uiso 1 1 calc GR . . . .
H34B H 0.500303 -0.026459 0.274087 0.079 Uiso 1 1 calc GR . . . .
H34C H 0.619268 -0.026120 0.334744 0.079 Uiso 1 1 calc GR . . . .
O2 O 0.2249(5) 0.2894(3) 0.1714(2) 0.0503(13) Uani 0.609(6) 1 d . . P . .
H2 H 0.274365 0.255630 0.158028 0.075 Uiso 0.609(6) 1 calc GR . P . .
C35 C 0.1626(8) 0.3317(4) 0.1166(4) 0.064(2) Uani 0.609(6) 1 d . . P . .
H35A H 0.098552 0.300218 0.088596 0.096 Uiso 0.609(6) 1 calc GR . P . .
H35B H 0.237201 0.350316 0.091364 0.096 Uiso 0.609(6) 1 calc GR . P . .
H35C H 0.109851 0.373211 0.132434 0.096 Uiso 0.609(6) 1 calc GR . P . .
N1 N 0.3834(2) 0.32885(11) 0.34196(10) 0.0154(4) Uani 1 1 d . . . . .
N2 N 0.2330(2) 0.23966(11) 0.36545(10) 0.0163(4) Uani 1 1 d . . . . .
C1 C 0.2673(2) 0.31168(13) 0.37280(11) 0.0143(4) Uani 1 1 d . . . . .
C2 C 0.4455(3) 0.26000(14) 0.31490(13) 0.0204(5) Uani 1 1 d . . . . .
H2A H 0.532337 0.244576 0.341877 0.024 Uiso 1 1 calc R . . . .
H2B H 0.467114 0.267366 0.269225 0.024 Uiso 1 1 calc R . . . .
C3 C 0.3247(3) 0.20279(14) 0.31881(14) 0.0216(5) Uani 1 1 d . . . . .
H3A H 0.272133 0.194674 0.275422 0.026 Uiso 1 1 calc R . . . .
H3B H 0.361841 0.155071 0.336358 0.026 Uiso 1 1 calc R . . . .
C4 C 0.4773(2) 0.39332(13) 0.35356(13) 0.0176(5) Uani 1 1 d . . . . .
C5 C 0.5677(3) 0.39682(16) 0.41307(14) 0.0238(5) Uani 1 1 d . . . . .
C6 C 0.6663(3) 0.45647(19) 0.41947(18) 0.0363(7) Uani 1 1 d . . . . .
H6 H 0.726366 0.461436 0.458909 0.044 Uiso 1 1 calc R . . . .
C7 C 0.6769(3) 0.50750(19) 0.36951(19) 0.0406(8) Uani 1 1 d . . . . .
H7 H 0.744970 0.545771 0.374919 0.049 Uiso 1 1 calc R . . . .
C8 C 0.5871(3) 0.50247(16) 0.31113(18) 0.0338(7) Uani 1 1 d . . . . .
H8 H 0.594517 0.537911 0.277690 0.041 Uiso 1 1 calc R . . . .
C9 C 0.4848(3) 0.44484(14) 0.30128(14) 0.0228(5) Uani 1 1 d . . . . .
C10 C 0.5674(3) 0.33997(18) 0.46839(15) 0.0307(6) Uani 1 1 d . . . . .
H10 H 0.493570 0.302332 0.454887 0.037 Uiso 1 1 calc R . . . .
C11 C 0.5289(4) 0.3762(2) 0.53334(17) 0.0468(9) Uani 1 1 d . . . . .
H11A H 0.600559 0.412895 0.548011 0.070 Uiso 1 1 calc GR . . . .
H11B H 0.525324 0.338178 0.566959 0.070 Uiso 1 1 calc GR . . . .
H11C H 0.436639 0.400238 0.525716 0.070 Uiso 1 1 calc GR . . . .
C12 C 0.7130(4) 0.2992(3) 0.4795(2) 0.0544(10) Uani 1 1 d . . . . .
H12A H 0.734522 0.276252 0.438509 0.082 Uiso 1 1 calc GR . . . .
H12B H 0.708280 0.261223 0.513037 0.082 Uiso 1 1 calc GR . . . .
H12C H 0.787022 0.334784 0.493834 0.082 Uiso 1 1 calc GR . . . .
C13 C 0.3911(3) 0.43981(16) 0.23588(14) 0.0272(6) Uani 1 1 d . . . . .
H13 H 0.317194 0.401469 0.240274 0.033 Uiso 1 1 calc R . . . .
C14 C 0.3155(4) 0.51482(19) 0.21793(18) 0.0409(8) Uani 1 1 d . . . . .
H14A H 0.268177 0.532312 0.255226 0.061 Uiso 1 1 calc GR . . . .
H14B H 0.245566 0.507753 0.180173 0.061 Uiso 1 1 calc GR . . . .
H14C H 0.385369 0.551291 0.207153 0.061 Uiso 1 1 calc GR . . . .
C15 C 0.4810(4) 0.4159(2) 0.17977(17) 0.0430(8) Uani 1 1 d . . . . .
H15A H 0.557488 0.451323 0.176505 0.064 Uiso 1 1 calc GR . . . .
H15B H 0.420772 0.414418 0.138290 0.064 Uiso 1 1 calc GR . . . .
H15C H 0.520890 0.366868 0.189387 0.064 Uiso 1 1 calc GR . . . .
C16 C 0.1035(3) 0.20121(13) 0.38094(12) 0.0172(4) Uani 1 1 d . . . . .
C17 C -0.0208(3) 0.20812(14) 0.33663(14) 0.0215(5) Uani 1 1 d . . . . .
C18 C -0.1382(3) 0.16303(15) 0.34869(16) 0.0285(6) Uani 1 1 d . . . . .
H18 H -0.222478 0.165730 0.320037 0.034 Uiso 1 1 calc R . . . .
C19 C -0.1309(3) 0.11460(16) 0.40243(17) 0.0316(7) Uani 1 1 d . . . . .
H19 H -0.210083 0.084953 0.409480 0.038 Uiso 1 1 calc R . . . .
C20 C -0.0072(3) 0.10976(16) 0.44583(16) 0.0304(6) Uani 1 1 d . . . . .
H20 H -0.004767 0.077419 0.482199 0.036 Uiso 1 1 calc R . . . .
C21 C 0.1146(3) 0.15257(14) 0.43611(13) 0.0223(5) Uani 1 1 d . . . . .
C22 C -0.0335(3) 0.26094(15) 0.27690(15) 0.0259(5) Uani 1 1 d . . . . .
H22 H 0.058045 0.287777 0.276291 0.031 Uiso 1 1 calc R . . . .
C23 C -0.1521(3) 0.31910(18) 0.2826(2) 0.0421(8) Uani 1 1 d . . . . .
H23A H -0.243185 0.294022 0.282449 0.063 Uiso 1 1 calc GR . . . .
H23B H -0.154993 0.353142 0.245519 0.063 Uiso 1 1 calc GR . . . .
H23C H -0.132569 0.346689 0.323476 0.063 Uiso 1 1 calc GR . . . .
C24 C -0.0614(5) 0.2171(2) 0.21125(17) 0.0491(10) Uani 1 1 d . . . . .
H24A H 0.012769 0.180149 0.208626 0.074 Uiso 1 1 calc GR . . . .
H24B H -0.061173 0.251229 0.174321 0.074 Uiso 1 1 calc GR . . . .
H24C H -0.153254 0.192554 0.209730 0.074 Uiso 1 1 calc GR . . . .
C25 C 0.2505(3) 0.14475(15) 0.48356(14) 0.0267(6) Uani 1 1 d . . . . .
H25 H 0.315205 0.186061 0.474427 0.032 Uiso 1 1 calc R . . . .
C26 C 0.2197(4) 0.15081(19) 0.55672(15) 0.0379(7) Uani 1 1 d . . . . .
H26A H 0.166244 0.195942 0.562926 0.057 Uiso 1 1 calc GR . . . .
H26B H 0.309054 0.152274 0.584760 0.057 Uiso 1 1 calc GR . . . .
H26C H 0.164672 0.108014 0.568286 0.057 Uiso 1 1 calc GR . . . .
C27 C 0.3291(4) 0.0705(2) 0.47267(17) 0.0411(8) Uani 1 1 d . . . . .
H27A H 0.267741 0.029045 0.481206 0.062 Uiso 1 1 calc GR . . . .
H27B H 0.415681 0.068128 0.502560 0.062 Uiso 1 1 calc GR . . . .
H27C H 0.352911 0.068096 0.427437 0.062 Uiso 1 1 calc GR . . . .
C28 C 0.1884(2) 0.36650(13) 0.40959(11) 0.0141(4) Uani 1 1 d . . . . .
C29 C 0.1413(3) 0.34752(13) 0.47094(12) 0.0174(5) Uani 1 1 d . . . . .
H29 H 0.158569 0.299574 0.488338 0.021 Uiso 1 1 calc R . . . .
C30 C 0.0688(3) 0.39974(13) 0.50610(12) 0.0163(4) Uani 1 1 d . . . . .
H30 H 0.039647 0.386644 0.547395 0.020 Uiso 1 1 calc R . . . .
C31 C 0.0385(2) 0.47196(13) 0.48063(11) 0.0138(4) Uani 1 1 d . . . . .
C32 C 0.0859(3) 0.49005(13) 0.41872(12) 0.0183(5) Uani 1 1 d . . . . .
H32 H 0.067288 0.537632 0.400765 0.022 Uiso 1 1 calc R . . . .
C33 C 0.1599(3) 0.43842(13) 0.38391(12) 0.0178(5) Uani 1 1 d . . . . .
H33 H 0.190956 0.451690 0.343035 0.021 Uiso 1 1 calc R . . . .


_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 H1 0.8200 . ?
O1 C34 1.416(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
O2 H2 0.8200 . ?
O2 C35 1.413(9) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
N1 C1 1.337(3) . ?
N1 C2 1.481(3) . ?
N1 C4 1.448(3) . ?
N2 C1 1.325(3) . ?
N2 C3 1.485(3) . ?
N2 C16 1.449(3) . ?
C1 C28 1.466(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.526(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.398(4) . ?
C4 C9 1.403(4) . ?
C5 C6 1.402(4) . ?
C5 C10 1.505(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.366(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.402(4) . ?
C9 C13 1.510(4) . ?
C10 H10 0.9800 . ?
C10 C11 1.533(4) . ?
C10 C12 1.536(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.536(4) . ?
C13 C15 1.533(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.398(4) . ?
C16 C21 1.404(3) . ?
C17 C18 1.398(4) . ?
C17 C22 1.522(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.380(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.398(4) . ?
C21 C25 1.517(4) . ?
C22 H22 0.9800 . ?
C22 C23 1.527(4) . ?
C22 C24 1.535(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.533(4) . ?
C25 C27 1.536(4) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.394(3) . ?
C28 C33 1.395(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.384(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.401(3) . ?
C31 C31 1.494(4) 3_566 ?
C31 C32 1.401(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.381(3) . ?
C33 H33 0.9300 . ?

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
C34 O1 H1 109.5 . . ?
O1 C34 H34A 109.5 . . ?
O1 C34 H34B 109.5 . . ?
O1 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 O2 H2 109.5 . . ?
O2 C35 H35A 109.5 . . ?
O2 C35 H35B 109.5 . . ?
O2 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C1 N1 C2 110.29(19) . . ?
C1 N1 C4 127.68(19) . . ?
C4 N1 C2 117.51(18) . . ?
C1 N2 C3 110.43(19) . . ?
C1 N2 C16 129.04(19) . . ?
C16 N2 C3 118.25(19) . . ?
N1 C1 C28 123.6(2) . . ?
N2 C1 N1 111.5(2) . . ?
N2 C1 C28 124.8(2) . . ?
N1 C2 H2A 111.3 . . ?
N1 C2 H2B 111.3 . . ?
N1 C2 C3 102.39(18) . . ?
H2A C2 H2B 109.2 . . ?
C3 C2 H2A 111.3 . . ?
C3 C2 H2B 111.3 . . ?
N2 C3 C2 102.32(18) . . ?
N2 C3 H3A 111.3 . . ?
N2 C3 H3B 111.3 . . ?
C2 C3 H3A 111.3 . . ?
C2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C5 C4 N1 118.6(2) . . ?
C5 C4 C9 122.9(2) . . ?
C9 C4 N1 118.1(2) . . ?
C4 C5 C6 116.6(3) . . ?
C4 C5 C10 124.1(2) . . ?
C6 C5 C10 119.3(3) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 C5 122.0(3) . . ?
C7 C6 H6 119.0 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.2(3) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.1(3) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C13 123.3(2) . . ?
C8 C9 C4 117.1(3) . . ?
C8 C9 C13 119.6(3) . . ?
C5 C10 H10 107.8 . . ?
C5 C10 C11 111.5(3) . . ?
C5 C10 C12 111.0(3) . . ?
C11 C10 H10 107.8 . . ?
C11 C10 C12 110.7(3) . . ?
C12 C10 H10 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.3 . . ?
C9 C13 C14 111.5(3) . . ?
C9 C13 C15 110.3(2) . . ?
C14 C13 H13 108.3 . . ?
C15 C13 H13 108.3 . . ?
C15 C13 C14 109.9(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 118.6(2) . . ?
C17 C16 C21 123.5(2) . . ?
C21 C16 N2 117.6(2) . . ?
C16 C17 C18 117.0(3) . . ?
C16 C17 C22 123.7(2) . . ?
C18 C17 C22 119.4(3) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.1(3) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.2(3) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C25 123.2(2) . . ?
C20 C21 C16 116.7(3) . . ?
C20 C21 C25 120.2(2) . . ?
C17 C22 H22 108.1 . . ?
C17 C22 C23 111.0(2) . . ?
C17 C22 C24 111.2(2) . . ?
C23 C22 H22 108.1 . . ?
C23 C22 C24 110.3(3) . . ?
C24 C22 H22 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.8 . . ?
C21 C25 C26 112.0(2) . . ?
C21 C25 C27 111.7(2) . . ?
C26 C25 H25 107.8 . . ?
C26 C25 C27 109.6(3) . . ?
C27 C25 H25 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 120.4(2) . . ?
C29 C28 C33 119.0(2) . . ?
C33 C28 C1 120.6(2) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.3(2) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.4 . . ?
C29 C30 C31 121.2(2) . . ?
C31 C30 H30 119.4 . . ?
C30 C31 C31 120.7(3) . 3_566 ?
C32 C31 C30 117.8(2) . . ?
C32 C31 C31 121.5(3) . 3_566 ?
C31 C32 H32 119.4 . . ?
C33 C32 C31 121.1(2) . . ?
C33 C32 H32 119.4 . . ?
C28 C33 H33 119.7 . . ?
C32 C33 C28 120.5(2) . . ?
C32 C33 H33 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C28 C29 -137.4(2) . . . . ?
N1 C1 C28 C33 42.3(3) . . . . ?
N1 C2 C3 N2 -16.6(3) . . . . ?
N1 C4 C5 C6 174.1(2) . . . . ?
N1 C4 C5 C10 -4.1(4) . . . . ?
N1 C4 C9 C8 -173.5(2) . . . . ?
N1 C4 C9 C13 5.2(3) . . . . ?
N2 C1 C28 C29 43.0(4) . . . . ?
N2 C1 C28 C33 -137.2(3) . . . . ?
N2 C16 C17 C18 172.3(2) . . . . ?
N2 C16 C17 C22 -7.3(3) . . . . ?
N2 C16 C21 C20 -173.1(2) . . . . ?
N2 C16 C21 C25 6.3(3) . . . . ?
C1 N1 C2 C3 14.4(3) . . . . ?
C1 N1 C4 C5 70.5(3) . . . . ?
C1 N1 C4 C9 -116.7(3) . . . . ?
C1 N2 C3 C2 14.8(3) . . . . ?
C1 N2 C16 C17 78.3(3) . . . . ?
C1 N2 C16 C21 -108.4(3) . . . . ?
C1 C28 C29 C30 179.0(2) . . . . ?
C1 C28 C33 C32 -179.8(2) . . . . ?
C2 N1 C1 N2 -5.6(3) . . . . ?
C2 N1 C1 C28 174.8(2) . . . . ?
C2 N1 C4 C5 -83.1(3) . . . . ?
C2 N1 C4 C9 89.7(3) . . . . ?
C3 N2 C1 N1 -6.4(3) . . . . ?
C3 N2 C1 C28 173.2(2) . . . . ?
C3 N2 C16 C17 -82.8(3) . . . . ?
C3 N2 C16 C21 90.5(3) . . . . ?
C4 N1 C1 N2 -160.8(2) . . . . ?
C4 N1 C1 C28 19.6(4) . . . . ?
C4 N1 C2 C3 172.4(2) . . . . ?
C4 C5 C6 C7 -1.8(4) . . . . ?
C4 C5 C10 C11 -118.9(3) . . . . ?
C4 C5 C10 C12 117.2(3) . . . . ?
C4 C9 C13 C14 128.8(3) . . . . ?
C4 C9 C13 C15 -108.8(3) . . . . ?
C5 C4 C9 C8 -1.0(4) . . . . ?
C5 C4 C9 C13 177.7(2) . . . . ?
C5 C6 C7 C8 1.5(5) . . . . ?
C6 C5 C10 C11 63.0(4) . . . . ?
C6 C5 C10 C12 -61.0(4) . . . . ?
C6 C7 C8 C9 -0.8(5) . . . . ?
C7 C8 C9 C4 0.6(4) . . . . ?
C7 C8 C9 C13 -178.3(3) . . . . ?
C8 C9 C13 C14 -52.5(3) . . . . ?
C8 C9 C13 C15 69.9(3) . . . . ?
C9 C4 C5 C6 1.6(4) . . . . ?
C9 C4 C5 C10 -176.6(2) . . . . ?
C10 C5 C6 C7 176.5(3) . . . . ?
C16 N2 C1 N1 -168.6(2) . . . . ?
C16 N2 C1 C28 11.0(4) . . . . ?
C16 N2 C3 C2 179.2(2) . . . . ?
C16 C17 C18 C19 0.6(4) . . . . ?
C16 C17 C22 C23 -118.8(3) . . . . ?
C16 C17 C22 C24 118.0(3) . . . . ?
C16 C21 C25 C26 130.7(3) . . . . ?
C16 C21 C25 C27 -105.9(3) . . . . ?
C17 C16 C21 C20 -0.1(4) . . . . ?
C17 C16 C21 C25 179.3(2) . . . . ?
C17 C18 C19 C20 0.2(4) . . . . ?
C18 C17 C22 C23 61.6(3) . . . . ?
C18 C17 C22 C24 -61.5(3) . . . . ?
C18 C19 C20 C21 -1.1(4) . . . . ?
C19 C20 C21 C16 1.0(4) . . . . ?
C19 C20 C21 C25 -178.5(3) . . . . ?
C20 C21 C25 C26 -49.8(3) . . . . ?
C20 C21 C25 C27 73.5(3) . . . . ?
C21 C16 C17 C18 -0.6(4) . . . . ?
C21 C16 C17 C22 179.8(2) . . . . ?
C22 C17 C18 C19 -179.8(3) . . . . ?
C28 C29 C30 C31 1.3(4) . . . . ?
C29 C28 C33 C32 -0.1(4) . . . . ?
C29 C30 C31 C31 -179.4(3) . . . 3_566 ?
C29 C30 C31 C32 -0.9(4) . . . . ?
C30 C31 C32 C33 0.1(4) . . . . ?
C31 C31 C32 C33 178.5(3) 3_566 . . . ?
C31 C32 C33 C28 0.4(4) . . . . ?
C33 C28 C29 C30 -0.8(4) . . . . ?

_olex2_date_sample_data_collection 2017-11-08
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.896
