# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_s6125r
_database_code_depnum_ccdc_archive 'CCDC 2281755'
loop_
_audit_author_name
_audit_author_address
'Inigo J. Vitorica-Yrezabal'
;The University of Manchester
United Kingdom
;
_audit_update_record             
;
2023-07-15 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2022-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        H2NAib4-L-AlaNHtBu
_chemical_formula_moiety         'C23 H44 N6 O5, H2 O'
_chemical_formula_sum            'C23 H46 N6 O6'
_chemical_formula_weight         502.66
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   11.6820(2)
_cell_length_b                   16.3850(3)
_cell_length_c                   15.2184(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.063(2)
_cell_angle_gamma                90
_cell_volume                     2837.57(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19451
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      75.7350
_cell_measurement_theta_min      3.0120
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.927
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72133
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.438
_diffrn_reflns_theta_min         2.981
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  42.00   1.00    3.00    --  -44.36   0.00 150.00   29
  2  ω   -129.00   7.00   1.00    3.00    --  -44.36   0.00 150.00  136
  3  ω    -73.00  -1.00   1.00    3.00    --  -44.36  38.00 -30.00   72
  4  ω    -70.00  18.00   1.00    3.00    --  -46.44  57.00-180.00   88
  5  ω    -87.00  26.00   1.00    3.00    --  -46.44  76.00  30.00  113
  6  ω   -145.00-119.00   1.00   10.00    -- -107.20  76.00-120.00   26
  7  ω   -174.00 -70.00   1.00   10.00    -- -107.20   0.00  30.00  104
  8  ω   -148.00 -19.00   1.00   10.00    -- -107.20  76.00   0.00  129
  9  ω    -83.00 -19.00   1.00   10.00    -- -107.20  76.00  60.00   64
 10  ω   -140.00 -86.00   1.00   10.00    -- -107.20  76.00  60.00   54
 11  ω   -196.00 -77.00   1.00   10.00    -- -107.20 -38.00 150.00  119
 12  ω   -110.00 -42.00   1.00   10.00    -- -107.20  76.00-180.00   68
 13  ω   -188.00 -69.00   1.00   10.00    -- -107.20 -38.00-180.00  119
 14  ω   -141.00 -24.00   1.00   10.00    -- -107.20  76.00 120.00  117
 15  ω   -112.00 -18.00   1.00   10.00    -- -107.20  76.00-120.00   94
 16  ω   -144.00-117.00   1.00   10.00    -- -107.20  76.00-180.00   27
 17  ω    -83.00 -24.00   1.00    4.00    --    5.00 -76.00  90.00   59
 18  ω    -19.00  38.00   1.00    4.00    --    5.00 -76.00  90.00   57
 19  ω   -131.00 -80.00   1.00    4.00    --  -43.99 -76.00  60.00   51
 20  ω    -29.00  -4.00   1.00    4.00    --  -43.99 -76.00  60.00   25
 21  ω   -134.00 -89.00   1.00    4.00    --  -46.21 -76.00   0.00   45
 22  ω    -87.00 -54.00   1.00    4.00    --  -46.21 -76.00-150.00   33
 23  ω    -60.00  -7.00   1.00    4.00    --  -46.21 -76.00   0.00   53
 24  ω   -134.00-108.00   1.00    4.00    --  -46.21 -76.00-150.00   26
 25  ω    -37.00  -8.00   1.00    4.00    --  -46.21 -76.00-150.00   29
 26  ω    -52.00 -22.00   1.00    4.00    --  -62.00 -76.00 -56.17   30
 27  ω    -68.00 -26.00   1.00    4.00    --  -66.00 -76.00 157.85   42
 28  ω    -55.00 -26.00   1.00    4.00    --  -66.00 -76.00  99.69   29
 29  ω    -63.00 -30.00   1.00    4.00    --  -70.00 -76.00  23.59   33
 30  ω    -56.00 -31.00   1.00    4.00    --  -70.00 -74.00-163.77   25
 31  ω    -60.00 -34.00   1.00    4.00    --  -74.00 -76.00  64.11   26
 32  ω    -60.00 -34.00   1.00    4.00    --  -74.00 -76.00  10.08   26
 33  ω    -62.00 -37.00   1.00    4.00    --  -74.00 -70.00 -84.48   25
 34  ω    -62.00 -34.00   1.00    4.00    --  -74.00 -76.00-104.75   28
 35  ω   -111.00 -43.00   1.00   10.00    --  -82.00 -75.00 111.19   68
 36  ω    -78.00 -47.00   1.00   10.00    --  -86.00 -75.00  -2.49   31
 37  ω    -79.00 -54.00   1.00   10.00    --  -90.00 -73.00-173.20   25
 38  ω   -133.00-107.00   1.00   10.00    --  -90.00 -76.00 141.67   26
 39  ω   -145.00 -99.00   1.00   10.00    --  -90.00 -71.00  87.92   46
 40  ω    -86.00 -53.00   1.00   10.00    --  -90.00 -71.00  87.92   33
 41  ω    -94.00 -50.00   1.00   10.00    --  -90.00 -76.00 141.67   44
 42  ω   -166.00 -54.00   1.00   10.00    --  -94.00 -76.00-116.48  112
 43  ω    -88.00 -54.00   1.00   10.00    --  -94.00 -76.00  52.90   34
 44  ω   -167.00 -94.00   1.00   10.00    --  -94.00 -76.00  52.90   73
 45  ω    -81.00 -54.00   1.00   10.00    --  -94.00 -76.00 -86.49   27
 46  ω   -131.00 -87.00   1.00   10.00    --  -94.00 -76.00 -86.49   44
 47  ω    -80.00 -55.00   1.00   10.00    --  -94.00 -74.00 -43.09   25
 48  ω   -138.00-111.00   1.00   10.00    --  -94.00 -74.00 -43.09   27
 49  ω   -156.00-122.00   1.00   10.00    --  -98.00 -70.00 120.16   34
 50  ω   -122.00 -59.00   1.00   10.00    --  -98.00 -76.00  79.24   63
 51  ω   -157.00 -65.00   1.00   10.00    --  -98.00 -71.00  -2.68   92
 52  ω   -104.00 -59.00   1.00   10.00    --  -98.00 -74.00 -65.19   45
 53  ω   -182.00-156.00   1.00   10.00    --  -98.00 -76.00  79.24   26
 54  ω   -164.00 -60.00   1.00   10.00    --  -98.00 -73.00 -17.07  104
 55  ω   -155.00 -64.00   1.00   10.00    --  -98.00 -69.00   4.29   91
 56  ω    -97.00 -60.00   1.00   10.00    --  -98.00 -73.00  40.75   37
 57  ω   -113.00 -62.00   1.00   10.00    --  -98.00 -73.00-135.88   51
 58  ω   -170.00-103.00   1.00   10.00    --  -98.00 -73.00  40.75   67
 59  ω   -167.00 -60.00   1.00   10.00    --  -98.00 -74.00 -48.87  107
 60  ω   -117.00 -61.00   1.00   10.00    --  -98.00 -70.00 120.16   56
 61  ω   -146.00-109.00   1.00   10.00    --  -98.00 -74.00 -65.19   37
 62  ω    -89.00 -64.00   1.00   10.00    -- -102.00 -74.00 -92.23   25
 63  ω   -191.00-123.00   1.00   10.00    -- -102.00 -74.00 -92.23   68
 64  ω    -93.00 -62.00   1.00   10.00    -- -102.00 -76.00-177.92   31
 65  ω   -189.00-161.00   1.00   10.00    -- -102.00 -76.00-177.92   28
 66  ω   -119.00 -69.00   1.00   10.00    -- -107.20 -74.00 155.91   50
 67  ω   -137.00 -71.00   1.00   10.00    -- -107.20  76.00 -60.00   66
 68  ω   -195.00-169.00   1.00   10.00    -- -107.20 -74.00 155.91   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0356702000
_diffrn_orient_matrix_UB_12      -0.0071230000
_diffrn_orient_matrix_UB_13      -0.0911954000
_diffrn_orient_matrix_UB_21      -0.0280960000
_diffrn_orient_matrix_UB_22      -0.0919616000
_diffrn_orient_matrix_UB_23      -0.0027985000
_diffrn_orient_matrix_UB_31      -0.1275145000
_diffrn_orient_matrix_UB_32      0.0181907000
_diffrn_orient_matrix_UB_33      -0.0497791000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                9824
_reflns_number_total             11450
_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 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 
;
 Flack x determined using 4102 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.060
_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)+(0.0497P)²+0.2530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0972
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Riding coordinates:
 N3(H3), N6(H6), N9(H9), N12(H12), N23(H23), N27(H27A,H27B), N1(H1A,H1B),
 N37(H37), N40(H40), N43(H43), N49(H49), N52(H52), O69(H69A,H69B), O70(H70A,
 H70B)
1.b Ternary CH refined with riding coordinates:
 C10(H10), C41(H41)
1.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C),
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C)
;
_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
O1 O 0.21585(15) 0.48476(12) 0.28815(12) 0.0272(4) Uani 1 1 d . . . . .
O17 O -0.15462(16) 0.45822(13) 0.36949(13) 0.0340(5) Uani 1 1 d . . . . .
O19 O 0.15274(17) 0.56638(14) 0.59344(12) 0.0353(5) Uani 1 1 d . . . . .
O29 O 0.41686(18) 0.63513(13) 0.34705(13) 0.0339(4) Uani 1 1 d . . . . .
O32 O 0.29485(16) 0.38583(12) 0.49403(12) 0.0279(4) Uani 1 1 d . . . . .
N3 N 0.40830(19) 0.45370(14) 0.30887(14) 0.0254(5) Uani 1 1 d . . . . .
H3 H 0.474860 0.464046 0.293175 0.031 Uiso 1 1 d R U . . .
N6 N 0.37602(19) 0.50816(13) 0.47495(14) 0.0227(4) Uani 1 1 d . . . . .
H6 H 0.417349 0.535925 0.443460 0.027 Uiso 1 1 d R U . . .
N9 N 0.14058(18) 0.53624(14) 0.44763(13) 0.0229(4) Uani 1 1 d . . . . .
H9 H 0.179217 0.523549 0.406152 0.028 Uiso 1 1 d R U . . .
N12 N 0.01651(19) 0.39218(14) 0.42536(15) 0.0287(5) Uani 1 1 d . . . . .
H12 H 0.091656 0.398990 0.449921 0.034 Uiso 1 1 d R U . . .
N23 N 0.4349(2) 0.59302(16) 0.20978(15) 0.0307(5) Uani 1 1 d . . . . .
H23 H 0.479029 0.592338 0.169952 0.037 Uiso 1 1 d R U . . .
N27 N 0.6487(3) 0.66697(18) 0.2252(2) 0.0467(7) Uani 1 1 d . . . . .
H27A H 0.658832 0.614500 0.217187 0.056 Uiso 1 1 d R U . . .
H27B H 0.603792 0.687750 0.175947 0.056 Uiso 1 1 d R U . . .
C2 C 0.3113(2) 0.49376(17) 0.26755(16) 0.0252(6) Uani 1 1 d . . . . .
C4 C 0.4072(2) 0.39321(17) 0.37937(17) 0.0250(5) Uani 1 1 d . . . . .
C5 C 0.3522(2) 0.42896(16) 0.45406(17) 0.0237(5) Uani 1 1 d . . . . .
C7 C 0.3361(2) 0.55006(17) 0.54793(16) 0.0250(5) Uani 1 1 d . . . . .
C8 C 0.2013(2) 0.54951(17) 0.53132(16) 0.0250(5) Uani 1 1 d . . . . .
C10 C 0.0134(2) 0.54177(17) 0.42147(17) 0.0249(5) Uani 1 1 d . . . . .
H10 H -0.013560 0.566968 0.473137 0.030 Uiso 1 1 calc R U . . .
C11 C -0.0483(2) 0.45933(17) 0.40245(16) 0.0251(5) Uani 1 1 d . . . . .
C13 C -0.0276(3) 0.30724(18) 0.4128(2) 0.0323(6) Uani 1 1 d . . . . .
C14 C -0.1217(3) 0.2931(2) 0.4662(3) 0.0483(9) Uani 1 1 d . . . . .
H14A H -0.149851 0.236689 0.457673 0.072 Uiso 1 1 calc R U . . .
H14B H -0.187489 0.330610 0.444765 0.072 Uiso 1 1 calc R U . . .
H14C H -0.088345 0.302997 0.530364 0.072 Uiso 1 1 calc R U . . .
C15 C -0.0765(3) 0.2910(2) 0.3135(2) 0.0502(9) Uani 1 1 d . . . . .
H15A H -0.017312 0.305115 0.279551 0.075 Uiso 1 1 calc R U . . .
H15B H -0.147004 0.324196 0.292141 0.075 Uiso 1 1 calc R U . . .
H15C H -0.096721 0.233050 0.304663 0.075 Uiso 1 1 calc R U . . .
C16 C 0.0764(3) 0.2519(2) 0.4491(3) 0.0488(9) Uani 1 1 d . . . . .
H16A H 0.051024 0.194833 0.442097 0.073 Uiso 1 1 calc R U . . .
H16B H 0.107897 0.263795 0.513093 0.073 Uiso 1 1 calc R U . . .
H16C H 0.137516 0.261431 0.415464 0.073 Uiso 1 1 calc R U . . .
C18 C -0.0220(2) 0.59924(18) 0.34173(18) 0.0316(6) Uani 1 1 d . . . . .
H18A H 0.011792 0.580097 0.292075 0.047 Uiso 1 1 calc R U . . .
H18B H 0.007171 0.654238 0.359642 0.047 Uiso 1 1 calc R U . . .
H18C H -0.107866 0.600511 0.322001 0.047 Uiso 1 1 calc R U . . .
C20 C 0.3732(3) 0.63918(18) 0.54669(19) 0.0317(6) Uani 1 1 d . . . . .
H20A H 0.336222 0.663575 0.488391 0.048 Uiso 1 1 calc R U . . .
H20B H 0.458867 0.642335 0.555764 0.048 Uiso 1 1 calc R U . . .
H20C H 0.348452 0.668901 0.595115 0.048 Uiso 1 1 calc R U . . .
C21 C 0.3901(2) 0.51229(19) 0.63914(18) 0.0309(6) Uani 1 1 d . . . . .
H21A H 0.362526 0.541752 0.686487 0.046 Uiso 1 1 calc R U . . .
H21B H 0.475889 0.515899 0.650498 0.046 Uiso 1 1 calc R U . . .
H21C H 0.366567 0.454877 0.639225 0.046 Uiso 1 1 calc R U . . .
C22 C 0.3221(2) 0.54988(19) 0.18887(18) 0.0299(6) Uani 1 1 d . . . . .
C24 C 0.4732(2) 0.63347(18) 0.28729(19) 0.0302(6) Uani 1 1 d . . . . .
C25 C 0.5910(3) 0.67837(19) 0.3004(2) 0.0351(7) Uani 1 1 d . . . . .
C26 C 0.5663(3) 0.7689(2) 0.3089(3) 0.0557(10) Uani 1 1 d . . . . .
H26A H 0.640487 0.799261 0.320263 0.084 Uiso 1 1 calc R U . . .
H26B H 0.527852 0.777345 0.359097 0.084 Uiso 1 1 calc R U . . .
H26C H 0.514798 0.788278 0.252793 0.084 Uiso 1 1 calc R U . . .
C28 C 0.6696(3) 0.6464(3) 0.3872(2) 0.0517(9) Uani 1 1 d . . . . .
H28A H 0.687309 0.588650 0.379738 0.078 Uiso 1 1 calc R U . . .
H28B H 0.629195 0.652116 0.436741 0.078 Uiso 1 1 calc R U . . .
H28C H 0.742958 0.677684 0.401126 0.078 Uiso 1 1 calc R U . . .
C30 C 0.2219(3) 0.6112(2) 0.1703(2) 0.0366(7) Uani 1 1 d . . . . .
H30A H 0.146710 0.582097 0.155024 0.055 Uiso 1 1 calc R U . . .
H30B H 0.229260 0.646330 0.119697 0.055 Uiso 1 1 calc R U . . .
H30C H 0.225018 0.644782 0.224057 0.055 Uiso 1 1 calc R U . . .
C31 C 0.3198(3) 0.4961(2) 0.10628(18) 0.0373(7) Uani 1 1 d . . . . .
H31A H 0.387912 0.459508 0.118514 0.056 Uiso 1 1 calc R U . . .
H31B H 0.322546 0.530652 0.054239 0.056 Uiso 1 1 calc R U . . .
H31C H 0.247416 0.463687 0.093203 0.056 Uiso 1 1 calc R U . . .
C33 C 0.3403(3) 0.31682(19) 0.3398(2) 0.0347(7) Uani 1 1 d . . . . .
H33A H 0.341257 0.276935 0.387922 0.052 Uiso 1 1 calc R U . . .
H33B H 0.377772 0.293144 0.294217 0.052 Uiso 1 1 calc R U . . .
H33C H 0.258814 0.331321 0.311739 0.052 Uiso 1 1 calc R U . . .
C34 C 0.5345(2) 0.37145(18) 0.42262(19) 0.0309(6) Uani 1 1 d . . . . .
H34A H 0.577477 0.421015 0.446440 0.046 Uiso 1 1 calc R U . . .
H34B H 0.571397 0.346735 0.377255 0.046 Uiso 1 1 calc R U . . .
H34C H 0.536494 0.332625 0.471928 0.046 Uiso 1 1 calc R U . . .
O35 O 0.78288(17) 0.62469(12) 0.97372(12) 0.0292(4) Uani 1 1 d . . . . .
O58 O 0.88397(17) 0.36628(12) 0.85007(13) 0.0328(4) Uani 1 1 d . . . . .
O61 O 0.71521(16) 0.52432(13) 0.77281(12) 0.0309(4) Uani 1 1 d . . . . .
O64 O 0.33884(17) 0.55081(14) 0.88177(14) 0.0366(5) Uani 1 1 d . . . . .
O66 O 0.61566(17) 0.47265(14) 1.06771(12) 0.0365(5) Uani 1 1 d . . . . .
N1 N 1.1394(2) 0.31945(19) 0.76137(19) 0.0473(7) Uani 1 1 d . . . . .
H1A H 1.182434 0.281468 0.743603 0.057 Uiso 1 1 d R U . . .
H1B H 1.164854 0.367908 0.749733 0.057 Uiso 1 1 d R U . . .
N37 N 0.86615(19) 0.50057(14) 0.97069(14) 0.0255(5) Uani 1 1 d . . . . .
H37 H 0.913280 0.470074 0.946869 0.031 Uiso 1 1 d R U . . .
N40 N 0.63242(19) 0.46823(14) 0.92319(14) 0.0252(5) Uani 1 1 d . . . . .
H40 H 0.682316 0.465945 0.887737 0.030 Uiso 1 1 d R U . . .
N43 N 0.5129(2) 0.61699(14) 0.90252(15) 0.0289(5) Uani 1 1 d . . . . .
H43 H 0.589688 0.610857 0.913008 0.035 Uiso 1 1 d R U . . .
N49 N 0.9116(2) 0.54418(15) 0.80330(14) 0.0278(5) Uani 1 1 d . . . . .
H49 H 0.979105 0.529327 0.791770 0.033 Uiso 1 1 d R U . . .
N52 N 0.9295(2) 0.39586(16) 0.71779(15) 0.0313(5) Uani 1 1 d . . . . .
H52 H 0.978501 0.388225 0.682256 0.038 Uiso 1 1 d R U . . .
C36 C 0.8454(2) 0.57834(16) 0.94195(17) 0.0251(5) Uani 1 1 d . . . . .
C38 C 0.8121(2) 0.46531(17) 1.04084(16) 0.0259(5) Uani 1 1 d . . . . .
C39 C 0.6773(2) 0.47047(18) 1.01171(17) 0.0271(6) Uani 1 1 d . . . . .
C41 C 0.5079(2) 0.46933(17) 0.88005(17) 0.0272(5) Uani 1 1 d . . . . .
H41 H 0.503644 0.463344 0.813992 0.033 Uiso 1 1 calc R U . . .
C42 C 0.4467(2) 0.54981(18) 0.89032(17) 0.0276(6) Uani 1 1 d . . . . .
C44 C 0.4664(3) 0.70051(18) 0.8998(2) 0.0335(6) Uani 1 1 d . . . . .
C45 C 0.3862(4) 0.7177(2) 0.8082(2) 0.0521(9) Uani 1 1 d . . . . .
H45A H 0.361777 0.775065 0.805220 0.078 Uiso 1 1 calc R U . . .
H45B H 0.316732 0.682563 0.799639 0.078 Uiso 1 1 calc R U . . .
H45C H 0.428484 0.706662 0.760701 0.078 Uiso 1 1 calc R U . . .
C46 C 0.5725(3) 0.7572(2) 0.9134(2) 0.0402(7) Uani 1 1 d . . . . .
H46A H 0.617183 0.745761 0.867557 0.060 Uiso 1 1 calc R U . . .
H46B H 0.622762 0.748299 0.973564 0.060 Uiso 1 1 calc R U . . .
H46C H 0.545692 0.814061 0.908001 0.060 Uiso 1 1 calc R U . . .
C47 C 0.4023(3) 0.7129(2) 0.9758(2) 0.0447(8) Uani 1 1 d . . . . .
H47A H 0.377366 0.769980 0.976521 0.067 Uiso 1 1 calc R U . . .
H47B H 0.455241 0.699487 1.033700 0.067 Uiso 1 1 calc R U . . .
H47C H 0.333233 0.677281 0.966022 0.067 Uiso 1 1 calc R U . . .
C48 C 0.9107(3) 0.60781(18) 0.87036(19) 0.0293(6) Uani 1 1 d . . . . .
C50 C 0.8120(2) 0.50746(18) 0.75844(17) 0.0278(6) Uani 1 1 d . . . . .
C51 C 0.8249(2) 0.44538(19) 0.68551(18) 0.0311(6) Uani 1 1 d . . . . .
C53 C 0.9537(2) 0.36150(17) 0.80000(18) 0.0286(6) Uani 1 1 d . . . . .
C54 C 1.0706(3) 0.31807(19) 0.8311(2) 0.0335(6) Uani 1 1 d . . . . .
C55 C 1.1361(3) 0.3598(2) 0.9177(2) 0.0371(7) Uani 1 1 d . . . . .
H55A H 1.153730 0.416338 0.904455 0.056 Uiso 1 1 calc R U . . .
H55B H 1.209610 0.330548 0.942094 0.056 Uiso 1 1 calc R U . . .
H55C H 1.087018 0.359223 0.962078 0.056 Uiso 1 1 calc R U . . .
C57 C 1.0455(3) 0.2302(2) 0.8514(3) 0.0483(8) Uani 1 1 d . . . . .
H57A H 0.993769 0.228816 0.893799 0.072 Uiso 1 1 calc R U . . .
H57B H 1.119503 0.202432 0.878042 0.072 Uiso 1 1 calc R U . . .
H57C H 1.007147 0.202632 0.795306 0.072 Uiso 1 1 calc R U . . .
C59 C 0.7162(3) 0.3907(2) 0.6624(2) 0.0404(7) Uani 1 1 d . . . . .
H59A H 0.646476 0.424340 0.639354 0.061 Uiso 1 1 calc R U . . .
H59B H 0.706984 0.361808 0.716772 0.061 Uiso 1 1 calc R U . . .
H59C H 0.725393 0.351029 0.616360 0.061 Uiso 1 1 calc R U . . .
C60 C 0.8400(3) 0.4935(2) 0.60311(19) 0.0391(7) Uani 1 1 d . . . . .
H60A H 0.843228 0.455690 0.553859 0.059 Uiso 1 1 calc R U . . .
H60B H 0.913065 0.525067 0.618432 0.059 Uiso 1 1 calc R U . . .
H60C H 0.773324 0.530754 0.584089 0.059 Uiso 1 1 calc R U . . .
C62 C 1.0384(3) 0.6249(2) 0.9183(2) 0.0371(7) Uani 1 1 d . . . . .
H62A H 1.040463 0.666965 0.964436 0.056 Uiso 1 1 calc R U . . .
H62B H 1.082067 0.643924 0.874315 0.056 Uiso 1 1 calc R U . . .
H62C H 1.074497 0.574714 0.946985 0.056 Uiso 1 1 calc R U . . .
C63 C 0.8521(3) 0.6845(2) 0.8249(2) 0.0403(7) Uani 1 1 d . . . . .
H63A H 0.771571 0.671721 0.792697 0.060 Uiso 1 1 calc R U . . .
H63B H 0.896531 0.705020 0.782100 0.060 Uiso 1 1 calc R U . . .
H63C H 0.850301 0.726271 0.870722 0.060 Uiso 1 1 calc R U . . .
C65 C 0.4408(3) 0.39736(19) 0.90553(19) 0.0347(6) Uani 1 1 d . . . . .
H65A H 0.433853 0.403321 0.968177 0.052 Uiso 1 1 calc R U . . .
H65B H 0.483008 0.346767 0.899248 0.052 Uiso 1 1 calc R U . . .
H65C H 0.362245 0.395419 0.865649 0.052 Uiso 1 1 calc R U . . .
C67 C 0.8577(3) 0.50794(19) 1.13051(18) 0.0323(6) Uani 1 1 d . . . . .
H67A H 0.827652 0.563960 1.127002 0.048 Uiso 1 1 calc R U . . .
H67B H 0.943818 0.508981 1.144160 0.048 Uiso 1 1 calc R U . . .
H67C H 0.831153 0.478390 1.178241 0.048 Uiso 1 1 calc R U . . .
C68 C 0.8450(3) 0.37494(18) 1.04979(19) 0.0326(6) Uani 1 1 d . . . . .
H68A H 0.805860 0.349075 1.093177 0.049 Uiso 1 1 calc R U . . .
H68B H 0.930294 0.369518 1.070994 0.049 Uiso 1 1 calc R U . . .
H68C H 0.819776 0.348260 0.990953 0.049 Uiso 1 1 calc R U . . .
O69 O 0.13883(18) 0.51282(15) 0.75961(14) 0.0440(6) Uani 1 1 d . . . . .
H69A H 0.197364 0.535729 0.797052 0.066 Uiso 1 1 d R U . . .
H69B H 0.138884 0.535259 0.707792 0.066 Uiso 1 1 d R U . . .
O70 O 0.62707(18) 0.44954(17) 0.24968(14) 0.0496(7) Uani 1 1 d . . . . .
H70A H 0.637971 0.454816 0.195289 0.074 Uiso 1 1 d R U . . .
H70B H 0.697571 0.448966 0.284029 0.074 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.233(3) . ?
O17 C11 1.230(3) . ?
O19 C8 1.238(3) . ?
O29 C24 1.238(3) . ?
O32 C5 1.226(3) . ?
N3 H3 0.8799 . ?
N3 C2 1.337(3) . ?
N3 C4 1.463(3) . ?
N6 H6 0.8799 . ?
N6 C5 1.350(3) . ?
N6 C7 1.469(3) . ?
N9 H9 0.8799 . ?
N9 C8 1.328(3) . ?
N9 C10 1.451(3) . ?
N12 H12 0.8801 . ?
N12 C11 1.337(4) . ?
N12 C13 1.481(4) . ?
N23 H23 0.8800 . ?
N23 C22 1.465(4) . ?
N23 C24 1.339(4) . ?
N27 H27A 0.8801 . ?
N27 H27B 0.8804 . ?
N27 C25 1.465(4) . ?
C2 C22 1.537(4) . ?
C4 C5 1.542(3) . ?
C4 C33 1.526(4) . ?
C4 C34 1.527(4) . ?
C7 C8 1.537(4) . ?
C7 C20 1.525(4) . ?
C7 C21 1.520(4) . ?
C10 H10 1.0000 . ?
C10 C11 1.528(4) . ?
C10 C18 1.518(4) . ?
C13 C14 1.526(4) . ?
C13 C15 1.513(5) . ?
C13 C16 1.516(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C30 1.521(4) . ?
C22 C31 1.530(4) . ?
C24 C25 1.533(4) . ?
C25 C26 1.522(5) . ?
C25 C28 1.521(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O35 C36 1.226(3) . ?
O58 C53 1.238(3) . ?
O61 C50 1.231(3) . ?
O64 C42 1.237(3) . ?
O66 C39 1.234(3) . ?
N1 H1A 0.8804 . ?
N1 H1B 0.8800 . ?
N1 C54 1.469(4) . ?
N37 H37 0.8801 . ?
N37 C36 1.351(3) . ?
N37 C38 1.475(3) . ?
N40 H40 0.8800 . ?
N40 C39 1.331(3) . ?
N40 C41 1.454(3) . ?
N43 H43 0.8803 . ?
N43 C42 1.334(4) . ?
N43 C44 1.470(4) . ?
N49 H49 0.8800 . ?
N49 C48 1.461(4) . ?
N49 C50 1.350(4) . ?
N52 H52 0.8803 . ?
N52 C51 1.457(4) . ?
N52 C53 1.342(4) . ?
C36 C48 1.543(4) . ?
C38 C39 1.539(4) . ?
C38 C67 1.518(4) . ?
C38 C68 1.528(4) . ?
C41 H41 1.0000 . ?
C41 C42 1.525(4) . ?
C41 C65 1.514(4) . ?
C44 C45 1.520(4) . ?
C44 C46 1.525(4) . ?
C44 C47 1.527(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C62 1.531(4) . ?
C48 C63 1.521(4) . ?
C50 C51 1.538(4) . ?
C51 C59 1.529(4) . ?
C51 C60 1.525(4) . ?
C53 C54 1.517(4) . ?
C54 C55 1.527(4) . ?
C54 C57 1.514(5) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
O69 H69A 0.8700 . ?
O69 H69B 0.8702 . ?
O70 H70A 0.8698 . ?
O70 H70B 0.8701 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N3 H3 119.0 . . ?
C2 N3 C4 122.0(2) . . ?
C4 N3 H3 119.0 . . ?
C5 N6 H6 118.5 . . ?
C5 N6 C7 122.9(2) . . ?
C7 N6 H6 118.5 . . ?
C8 N9 H9 118.5 . . ?
C8 N9 C10 123.0(2) . . ?
C10 N9 H9 118.5 . . ?
C11 N12 H12 117.3 . . ?
C11 N12 C13 125.4(2) . . ?
C13 N12 H12 117.3 . . ?
C22 N23 H23 118.8 . . ?
C24 N23 H23 118.8 . . ?
C24 N23 C22 122.4(2) . . ?
H27A N27 H27B 109.4 . . ?
C25 N27 H27A 109.5 . . ?
C25 N27 H27B 109.0 . . ?
O1 C2 N3 122.7(2) . . ?
O1 C2 C22 120.5(2) . . ?
N3 C2 C22 116.7(2) . . ?
N3 C4 C5 111.0(2) . . ?
N3 C4 C33 110.8(2) . . ?
N3 C4 C34 107.7(2) . . ?
C33 C4 C5 110.0(2) . . ?
C33 C4 C34 109.9(2) . . ?
C34 C4 C5 107.4(2) . . ?
O32 C5 N6 122.9(2) . . ?
O32 C5 C4 120.8(2) . . ?
N6 C5 C4 116.2(2) . . ?
N6 C7 C8 111.2(2) . . ?
N6 C7 C20 107.3(2) . . ?
N6 C7 C21 111.3(2) . . ?
C20 C7 C8 106.7(2) . . ?
C21 C7 C8 110.2(2) . . ?
C21 C7 C20 109.9(2) . . ?
O19 C8 N9 122.1(2) . . ?
O19 C8 C7 120.1(2) . . ?
N9 C8 C7 117.6(2) . . ?
N9 C10 H10 107.2 . . ?
N9 C10 C11 114.0(2) . . ?
N9 C10 C18 109.6(2) . . ?
C11 C10 H10 107.2 . . ?
C18 C10 H10 107.2 . . ?
C18 C10 C11 111.4(2) . . ?
O17 C11 N12 123.7(3) . . ?
O17 C11 C10 118.7(2) . . ?
N12 C11 C10 117.6(2) . . ?
N12 C13 C14 110.2(2) . . ?
N12 C13 C15 109.6(3) . . ?
N12 C13 C16 106.7(2) . . ?
C15 C13 C14 110.5(3) . . ?
C15 C13 C16 110.4(3) . . ?
C16 C13 C14 109.3(3) . . ?
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 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 C20 H20A 109.5 . . ?
C7 C20 H20B 109.5 . . ?
C7 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 C21 H21A 109.5 . . ?
C7 C21 H21B 109.5 . . ?
C7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N23 C22 C2 110.3(2) . . ?
N23 C22 C30 109.8(3) . . ?
N23 C22 C31 107.7(2) . . ?
C30 C22 C2 110.2(2) . . ?
C30 C22 C31 111.0(2) . . ?
C31 C22 C2 107.8(2) . . ?
O29 C24 N23 122.0(3) . . ?
O29 C24 C25 120.3(3) . . ?
N23 C24 C25 117.7(2) . . ?
N27 C25 C24 113.2(2) . . ?
N27 C25 C26 108.6(3) . . ?
N27 C25 C28 109.9(3) . . ?
C26 C25 C24 107.3(3) . . ?
C26 C25 C28 110.6(3) . . ?
C28 C25 C24 107.2(3) . . ?
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 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C22 C31 H31A 109.5 . . ?
C22 C31 H31B 109.5 . . ?
C22 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C4 C33 H33A 109.5 . . ?
C4 C33 H33B 109.5 . . ?
C4 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C4 C34 H34A 109.5 . . ?
C4 C34 H34B 109.5 . . ?
C4 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
H1A N1 H1B 109.4 . . ?
C54 N1 H1A 130.9 . . ?
C54 N1 H1B 115.1 . . ?
C36 N37 H37 119.0 . . ?
C36 N37 C38 121.9(2) . . ?
C38 N37 H37 119.0 . . ?
C39 N40 H40 117.2 . . ?
C39 N40 C41 125.6(2) . . ?
C41 N40 H40 117.2 . . ?
C42 N43 H43 117.8 . . ?
C42 N43 C44 124.4(2) . . ?
C44 N43 H43 117.8 . . ?
C48 N49 H49 119.0 . . ?
C50 N49 H49 119.0 . . ?
C50 N49 C48 122.0(2) . . ?
C51 N52 H52 119.0 . . ?
C53 N52 H52 118.9 . . ?
C53 N52 C51 122.1(2) . . ?
O35 C36 N37 122.4(2) . . ?
O35 C36 C48 121.2(2) . . ?
N37 C36 C48 116.3(2) . . ?
N37 C38 C39 110.3(2) . . ?
N37 C38 C67 110.5(2) . . ?
N37 C38 C68 107.7(2) . . ?
C67 C38 C39 111.2(2) . . ?
C67 C38 C68 109.6(2) . . ?
C68 C38 C39 107.4(2) . . ?
O66 C39 N40 122.8(2) . . ?
O66 C39 C38 121.4(2) . . ?
N40 C39 C38 115.7(2) . . ?
N40 C41 H41 105.7 . . ?
N40 C41 C42 114.1(2) . . ?
N40 C41 C65 113.4(2) . . ?
C42 C41 H41 105.7 . . ?
C65 C41 H41 105.7 . . ?
C65 C41 C42 111.4(2) . . ?
O64 C42 N43 123.3(3) . . ?
O64 C42 C41 119.4(3) . . ?
N43 C42 C41 117.2(2) . . ?
N43 C44 C45 110.3(3) . . ?
N43 C44 C46 106.3(2) . . ?
N43 C44 C47 110.1(2) . . ?
C45 C44 C46 109.0(3) . . ?
C45 C44 C47 111.3(3) . . ?
C46 C44 C47 109.8(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N49 C48 C36 110.7(2) . . ?
N49 C48 C62 107.7(2) . . ?
N49 C48 C63 110.2(2) . . ?
C62 C48 C36 107.7(2) . . ?
C63 C48 C36 109.6(2) . . ?
C63 C48 C62 110.9(3) . . ?
O61 C50 N49 122.1(3) . . ?
O61 C50 C51 121.4(2) . . ?
N49 C50 C51 116.5(2) . . ?
N52 C51 C50 109.7(2) . . ?
N52 C51 C59 110.0(3) . . ?
N52 C51 C60 108.8(2) . . ?
C59 C51 C50 110.0(2) . . ?
C60 C51 C50 107.4(2) . . ?
C60 C51 C59 111.0(2) . . ?
O58 C53 N52 121.2(3) . . ?
O58 C53 C54 120.6(2) . . ?
N52 C53 C54 118.2(2) . . ?
N1 C54 C53 111.6(2) . . ?
N1 C54 C55 111.6(3) . . ?
N1 C54 C57 108.9(3) . . ?
C53 C54 C55 107.4(2) . . ?
C57 C54 C53 107.9(3) . . ?
C57 C54 C55 109.4(3) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C51 C59 H59A 109.5 . . ?
C51 C59 H59B 109.5 . . ?
C51 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C51 C60 H60A 109.5 . . ?
C51 C60 H60B 109.5 . . ?
C51 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C48 C62 H62A 109.5 . . ?
C48 C62 H62B 109.5 . . ?
C48 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C48 C63 H63A 109.5 . . ?
C48 C63 H63B 109.5 . . ?
C48 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C41 C65 H65A 109.5 . . ?
C41 C65 H65B 109.5 . . ?
C41 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C38 C67 H67A 109.5 . . ?
C38 C67 H67B 109.5 . . ?
C38 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C38 C68 H68A 109.5 . . ?
C38 C68 H68B 109.5 . . ?
C38 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
H69A O69 H69B 104.5 . . ?
H70A O70 H70B 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C22 N23 143.1(3) . . . . ?
O1 C2 C22 C30 21.7(4) . . . . ?
O1 C2 C22 C31 -99.5(3) . . . . ?
O29 C24 C25 N27 177.3(3) . . . . ?
O29 C24 C25 C26 -62.9(4) . . . . ?
O29 C24 C25 C28 55.9(4) . . . . ?
N3 C2 C22 N23 -39.5(3) . . . . ?
N3 C2 C22 C30 -160.9(2) . . . . ?
N3 C2 C22 C31 77.9(3) . . . . ?
N3 C4 C5 O32 146.4(2) . . . . ?
N3 C4 C5 N6 -36.7(3) . . . . ?
N6 C7 C8 O19 164.9(2) . . . . ?
N6 C7 C8 N9 -19.8(3) . . . . ?
N9 C10 C11 O17 -171.4(2) . . . . ?
N9 C10 C11 N12 10.6(3) . . . . ?
N23 C24 C25 N27 -2.6(4) . . . . ?
N23 C24 C25 C26 117.2(3) . . . . ?
N23 C24 C25 C28 -124.0(3) . . . . ?
C2 N3 C4 C5 -52.8(3) . . . . ?
C2 N3 C4 C33 69.7(3) . . . . ?
C2 N3 C4 C34 -170.0(2) . . . . ?
C4 N3 C2 O1 2.7(4) . . . . ?
C4 N3 C2 C22 -174.6(2) . . . . ?
C5 N6 C7 C8 -60.1(3) . . . . ?
C5 N6 C7 C20 -176.5(2) . . . . ?
C5 N6 C7 C21 63.2(3) . . . . ?
C7 N6 C5 O32 0.4(4) . . . . ?
C7 N6 C5 C4 -176.4(2) . . . . ?
C8 N9 C10 C11 -107.6(3) . . . . ?
C8 N9 C10 C18 126.7(3) . . . . ?
C10 N9 C8 O19 1.2(4) . . . . ?
C10 N9 C8 C7 -174.0(2) . . . . ?
C11 N12 C13 C14 -61.0(4) . . . . ?
C11 N12 C13 C15 60.8(3) . . . . ?
C11 N12 C13 C16 -179.6(3) . . . . ?
C13 N12 C11 O17 1.7(4) . . . . ?
C13 N12 C11 C10 179.6(2) . . . . ?
C18 C10 C11 O17 -46.7(3) . . . . ?
C18 C10 C11 N12 135.3(2) . . . . ?
C20 C7 C8 O19 -78.3(3) . . . . ?
C20 C7 C8 N9 97.0(3) . . . . ?
C21 C7 C8 O19 41.0(4) . . . . ?
C21 C7 C8 N9 -143.7(2) . . . . ?
C22 N23 C24 O29 1.8(4) . . . . ?
C22 N23 C24 C25 -178.3(3) . . . . ?
C24 N23 C22 C2 -50.3(4) . . . . ?
C24 N23 C22 C30 71.3(3) . . . . ?
C24 N23 C22 C31 -167.7(3) . . . . ?
C33 C4 C5 O32 23.5(4) . . . . ?
C33 C4 C5 N6 -159.6(2) . . . . ?
C34 C4 C5 O32 -96.1(3) . . . . ?
C34 C4 C5 N6 80.8(3) . . . . ?
O35 C36 C48 N49 -142.4(3) . . . . ?
O35 C36 C48 C62 100.1(3) . . . . ?
O35 C36 C48 C63 -20.6(4) . . . . ?
O58 C53 C54 N1 179.9(3) . . . . ?
O58 C53 C54 C55 -57.6(4) . . . . ?
O58 C53 C54 C57 60.3(4) . . . . ?
O61 C50 C51 N52 -140.9(3) . . . . ?
O61 C50 C51 C59 -19.9(4) . . . . ?
O61 C50 C51 C60 101.0(3) . . . . ?
N37 C36 C48 N49 41.1(3) . . . . ?
N37 C36 C48 C62 -76.4(3) . . . . ?
N37 C36 C48 C63 162.9(3) . . . . ?
N37 C38 C39 O66 -154.0(3) . . . . ?
N37 C38 C39 N40 29.3(3) . . . . ?
N40 C41 C42 O64 -158.1(2) . . . . ?
N40 C41 C42 N43 26.1(3) . . . . ?
N49 C50 C51 N52 41.2(3) . . . . ?
N49 C50 C51 C59 162.3(3) . . . . ?
N49 C50 C51 C60 -76.8(3) . . . . ?
N52 C53 C54 N1 -1.5(4) . . . . ?
N52 C53 C54 C55 121.1(3) . . . . ?
N52 C53 C54 C57 -121.1(3) . . . . ?
C36 N37 C38 C39 57.6(3) . . . . ?
C36 N37 C38 C67 -65.7(3) . . . . ?
C36 N37 C38 C68 174.6(2) . . . . ?
C38 N37 C36 O35 1.7(4) . . . . ?
C38 N37 C36 C48 178.2(2) . . . . ?
C39 N40 C41 C42 68.0(3) . . . . ?
C39 N40 C41 C65 -61.1(4) . . . . ?
C41 N40 C39 O66 1.0(5) . . . . ?
C41 N40 C39 C38 177.7(2) . . . . ?
C42 N43 C44 C45 -59.9(4) . . . . ?
C42 N43 C44 C46 -177.9(3) . . . . ?
C42 N43 C44 C47 63.3(4) . . . . ?
C44 N43 C42 O64 -5.4(4) . . . . ?
C44 N43 C42 C41 170.2(2) . . . . ?
C48 N49 C50 O61 -1.5(4) . . . . ?
C48 N49 C50 C51 176.3(2) . . . . ?
C50 N49 C48 C36 53.0(3) . . . . ?
C50 N49 C48 C62 170.6(2) . . . . ?
C50 N49 C48 C63 -68.4(3) . . . . ?
C51 N52 C53 O58 4.6(4) . . . . ?
C51 N52 C53 C54 -174.0(3) . . . . ?
C53 N52 C51 C50 47.4(4) . . . . ?
C53 N52 C51 C59 -73.6(3) . . . . ?
C53 N52 C51 C60 164.6(3) . . . . ?
C65 C41 C42 O64 -28.0(3) . . . . ?
C65 C41 C42 N43 156.2(2) . . . . ?
C67 C38 C39 O66 -31.0(4) . . . . ?
C67 C38 C39 N40 152.2(3) . . . . ?
C68 C38 C39 O66 88.9(3) . . . . ?
C68 C38 C39 N40 -87.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.516
_oxdiff_exptl_absorpt_empirical_full_min 0.568
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
