# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_dwb1920
_database_code_depnum_ccdc_archive 'CCDC 2056911'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_audit_creation_date             2020-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C120 H96 N6 O16, 3.31(C1 H1 Cl3), 0.24(O)'
_chemical_formula_sum            'C123.31 H99.31 Cl9.94 N6 O16.24'
_chemical_formula_weight         2277.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C124 H100 Cl12 N6 O16'
_chemical_oxdiff_usercomment     'Alfiya Suleymanova SAY-068'
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'
Cl Cl 0.3639 0.7018 '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                   11.3160(7)
_cell_length_b                   15.6983(10)
_cell_length_c                   16.1277(11)
_cell_angle_alpha                73.671(6)
_cell_angle_beta                 86.678(5)
_cell_angle_gamma                81.686(5)
_cell_volume                     2720.0(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3763
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.2740
_cell_measurement_theta_min      4.8270
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.679
_exptl_absorpt_coefficient_mu    2.910
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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 orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0033
-1 0 0 0.0754
-1 -2 -3 0.0559
1 0 0 0.0615
0 1 0 0.0068
0 -1 -2 0.0463
0 1 2 0.0394

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform and petroleum ether'
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.01
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
0.0000 -0.9997 -0.0004 -0.0271 0.0969 0.0226
-1.0001 0.0005 0.0003 -0.1150 -0.0619 0.0434
-0.9994 -1.9989 -3.0001 -0.0186 0.0310 0.3259
1.0001 -0.0005 -0.0003 0.1150 0.0619 -0.0434
-0.0000 0.9997 0.0004 0.0271 -0.0969 -0.0226
0.0005 -0.9997 -2.0001 0.0733 0.0296 0.1808
-0.0005 0.9997 2.0001 -0.0733 -0.0296 -0.1808

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16956
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.500
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  -1.00   1.00   10.00    --    0.00  77.00   0.00   27
  2  ω      3.00  42.00   1.00   10.00    --    0.00  77.00   0.00   39
  3  ω    -20.00  27.00   1.00   10.00    --    0.00 -77.00-150.00   47
  4  ω    -16.00  84.00   1.00   40.00    --   54.00 -77.00  90.00  100
  5  ω     37.00 108.00   1.00   40.00    --   54.00-125.00 -90.00   71
  6  ω     41.00 123.00   1.00   40.00    --   54.00  57.00 -60.00   82
  7  ω    -17.00  98.00   1.00   40.00    --   54.00 -19.00 120.00  115
  8  ω     -2.00  71.00   1.00   40.00    --   54.00 -57.00 -30.00   73
  9  ω     91.00 129.00   1.00   55.00    --  108.00 -25.00  90.00   38
 10  ω     83.00 109.00   1.00   55.00    --  108.00-111.00  60.00   26
 11  ω     43.00 140.00   1.00   55.00    --  108.00 -25.00 -90.00   97
 12  ω     35.00  72.00   1.00   55.00    --  108.00 -25.00  90.00   37
 13  ω     38.00 130.00   1.00   55.00    --  108.00 -50.00-180.00   92
 14  ω     74.00 109.00   1.00   55.00    --  108.00-111.00 150.00   35
 15  ω     36.00  63.00   1.00   55.00    --  108.00-111.00 150.00   27
 16  ω    106.00 151.00   1.00   55.00    --  108.00 111.00-150.00   45
 17  ω     62.00 109.00   1.00   55.00    --  108.00-111.00 -60.00   47
 18  ω     43.00  96.00   1.00   55.00    --  108.00 -91.00   0.00   53
 19  ω     40.00 126.00   1.00   55.00    --  108.00 -63.00  30.00   86
 20  ω    104.00 172.00   1.00   55.00    --  108.00 111.00  90.00   68
 21  ω    116.00 169.00   1.00   55.00    --  108.00  77.00 -30.00   53
 22  ω     37.00  66.00   1.00   55.00    --  108.00-111.00  60.00   29
 23  ω     40.00 104.00   1.00   55.00    --  108.00 -91.00-180.00   64
 24  ω     87.00 178.00   1.00   55.00    --  108.00  37.00 -90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1149958000
_diffrn_orient_matrix_UB_12      0.0271080000
_diffrn_orient_matrix_UB_13      -0.0501545000
_diffrn_orient_matrix_UB_21      0.0618741000
_diffrn_orient_matrix_UB_22      -0.0969676000
_diffrn_orient_matrix_UB_23      0.0336741000
_diffrn_orient_matrix_UB_31      -0.0434034000
_diffrn_orient_matrix_UB_32      -0.0225967000
_diffrn_orient_matrix_UB_33      -0.0791306000
_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                6674
_reflns_number_total             9662
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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         0.374
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         9662
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0568
_refine_ls_restrained_S_all      1.012
_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)+(0.0706P)²+0.3722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1600
_refine_special_details          
;
The asymmetric unit contain half of the molecule.  
The crystal exhibited disorder of both the solvent and some of the 
methoxy groups.  These were modelled as follows:
Methoxy with O1: Methyl (C29) modelled in two positions with occupancies of 
                 0.759:0.241(19), C(Me)-O bond lengths restrained to be equal. 
				 ADP of C29 & C29a constrained to be equal.
Methoxy with O2: Methyl and Oxygen modelled in two positions with occupancies
                 of 0.737:0.263(6), C(Me)-O bond lengths restrained to be
				 equal. ADP of C30 & C30a constrained to be equal.
Methoxy with O3: Methyl and Oxygen modelled in two positions with occupancies
                 of 0.554:0.446(6), C(Me)-O bond lengths restrained to be
				 equal. ADP of pairs C31 & C31a and O3 & O3a constrained 
				 to be equal.
Two disordered chloroforms of crystallisation were visible, there was also 
evidence of small amounts of hydrocarbon solvent being present but a discrete
model for the latter could not be obtained.
Chloroform 1 (Cl1-Cl3, C61): modelled in two positions with refined 
occupancies of 0.691(3) & 0.066(2) implying ~ 0.24 of 0.24 disordered 
hydrocarbon.  Pairs of atoms were constrained to have the same ADP (i,e,
Cl1a & Cl1b, Cl2a & Cl2b, Cl3, Cl3a, C61a & C61b).
For the minor form, the C-Cl bond lengths were restrained to be 1.735 angstroms 
and the Cl-C-Cl distances restrained to be the same.

Chloroform 2 (Cl4-Cl6, C62): modelled in four positions with refined 
occupancies of 0.800(4), 0.045(2), 0.0277(18) & 0.0262(14) implying ~ 0.1
of disordered hydrocarbon.  Equivalent atoms were constrained to have the same
ADP (e.g. Cl4a, Cl4b, Cl4c & Cl4d).  For the minor forms, the C-Cl bond 
lengths were restrained to be 1.735 angstroms and the Cl-C-Cl distances 
restrained to be the same.

In addition, there is a peak of 1.2 electrons per cubic angstroms which is 
presumed to correspond to a partial water site (O9 occupancy 0.120(7)).
This was modelled isotropically without the hydrogens being modelled.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl5D-C62C = Cl6D-C62C = Cl4D-C62C
 1.735 with sigma of 0.01
 Cl5D-Cl6D = Cl6D-Cl4D = Cl5D-Cl4D
 2.9 with sigma of 0.01
 Cl4B-C62B = Cl5B-C62B = Cl6B-C62B
 1.735 with sigma of 0.01
 Cl4B-Cl5B = Cl5B-Cl6B = Cl6B-Cl4B
 2.9 with sigma of 0.01
 Cl5C-C62D = Cl6C-C62D = Cl4C-C62D
 1.735 with sigma of 0.01
 Cl6C-Cl4C = Cl4C-Cl5C = Cl6C-Cl5C
 2.9 with sigma of 0.01
 Cl2B-C61B = Cl1B-C61B = Cl3B-C61B
 1.735 with sigma of 0.01
 Cl5A-C62A = Cl4A-C62A = Cl6A-C62A
 1.735 with sigma of 0.01
 Cl5A-Cl6A = Cl6A-Cl4A = Cl5A-Cl4A
 2.9 with sigma of 0.01
 O1-C29A \\sim O1-C29
 with sigma of 0.01
 O3A-C31A \\sim O3-C31
 with sigma of 0.01
 O2-C30 \\sim O2-C30A
 with sigma of 0.01
 Cl2B-Cl3B \\sim Cl3B-Cl1B \\sim Cl2B-Cl1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl5D) = Uanis(Cl5B)
Uanis(Cl6D) = Uanis(Cl6B)
Uanis(C62C) = Uanis(C62D)
Uanis(Cl4D) = Uanis(Cl4C)
Uanis(Cl4B) = Uanis(Cl4C)
Uanis(C62B) = Uanis(C62D)
Uanis(Cl6C) = Uanis(Cl6B)
Uanis(C29) = Uanis(C29A)
Uanis(O3A) = Uanis(O3)
Uanis(C31) = Uanis(C31A)
Uanis(Cl2A) = Uanis(Cl2B)
Uanis(Cl1A) = Uanis(Cl1B)
Uanis(Cl3B) = Uanis(Cl3A)
Uanis(C61B) = Uanis(C61A)
Uanis(Cl5A) = Uanis(Cl5B)
Uanis(Cl5C) = Uanis(Cl5A)
Uanis(Cl6B) = Uanis(Cl6A)
Uanis(C62A) = Uanis(C62B)
Uanis(Cl4A) = Uanis(Cl4B)
Uanis(C30A) = Uanis(C30)
4. Others
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(O3A)=1-FVAR(2)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(O3)=FVAR(2)
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(3)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(3)
 Sof(C61A)=Sof(H61A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(4)
 Sof(C61B)=Sof(H61B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=FVAR(5)
 Sof(C62B)=Sof(H62B)=Sof(Cl4B)=Sof(Cl5B)=Sof(Cl6B)=FVAR(6)
 Sof(C62D)=Sof(H62D)=Sof(Cl4C)=Sof(Cl5C)=Sof(Cl6C)=FVAR(7)
 Sof(C62C)=Sof(H62C)=Sof(Cl4D)=Sof(Cl5D)=Sof(Cl6D)=FVAR(8)
 Sof(C62A)=Sof(H62A)=Sof(Cl4A)=Sof(Cl5A)=Sof(Cl6A)=FVAR(9)
5.a Ternary CH refined with riding coordinates:
 C61A(H61A), C61B(H61B), C62A(H62A), C62B(H62B), C62C(H62C), C62D(H62D)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C12(H12), C13(H13), C16(H16), C18(H18), C19(H19),
 C21(H21), C24(H24), C27(H27), C28(H28), C34(H34), C35(H35), C37(H37), C40(H40),
  C41(H41), C44(H44), C46(H46), C47(H47), C49(H49), C52(H52), C55(H55), C56(H56)
5.c Idealised Me refined as rotating group:
 C021(H02A,H02B,H02C), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F), C30(H30A,
 H30B,H30C), C30A(H30D,H30E,H30F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F),
 C32(H32A,H32B,H32C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C)
;
_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
C1 C 0.1481(3) 0.5486(2) 1.10877(18) 0.0266(6) Uani 1 1 d . . . . .
C2 C 0.0726(2) 0.5209(2) 1.05518(17) 0.0229(6) Uani 1 1 d . . . . .
C3 C 0.1253(2) 0.4955(2) 0.98319(17) 0.0235(6) Uani 1 1 d . . . . .
C4 C 0.0510(2) 0.47386(19) 0.92775(17) 0.0228(6) Uani 1 1 d . . . . .
C5 C 0.3362(2) 0.4254(2) 1.01524(18) 0.0264(6) Uani 1 1 d . . . . .
C6 C 0.3280(3) 0.3649(2) 1.09561(18) 0.0298(7) Uani 1 1 d . . . . .
H6 H 0.259539 0.369725 1.131839 0.036 Uiso 1 1 calc R . . . .
C7 C 0.4218(3) 0.2971(2) 1.12195(19) 0.0314(7) Uani 1 1 d . . . . .
H7 H 0.417021 0.254950 1.176966 0.038 Uiso 1 1 calc R . . . .
C8 C 0.5240(3) 0.2888(2) 1.06964(18) 0.0289(7) Uani 1 1 d . . . . .
C9 C 0.5329(3) 0.3534(2) 0.99067(18) 0.0273(6) Uani 1 1 d . . . . .
H9 H 0.602973 0.350636 0.955620 0.033 Uiso 1 1 calc R . . . .
C10 C 0.4395(2) 0.4215(2) 0.96347(17) 0.0250(6) Uani 1 1 d . . . . .
C11 C 0.6172(3) 0.2097(2) 1.09273(18) 0.0285(7) Uani 1 1 d . . . . .
C12 C 0.5885(3) 0.1250(2) 1.1329(2) 0.0382(8) Uani 1 1 d . . . . .
H12 H 0.508693 0.118256 1.152553 0.046 Uiso 1 1 calc R . . . .
C13 C 0.6740(3) 0.0491(2) 1.1452(2) 0.0443(9) Uani 1 1 d . . . . .
H13 H 0.651724 -0.008449 1.172364 0.053 Uiso 1 1 calc R . . . .
C14 C 0.7906(3) 0.0575(2) 1.1180(2) 0.0423(8) Uani 1 1 d . . . . .
C15 C 0.8208(3) 0.1428(2) 1.0770(2) 0.0370(8) Uani 1 1 d . . . . .
C16 C 0.7362(3) 0.2172(2) 1.06507(19) 0.0320(7) Uani 1 1 d . . . . .
H16 H 0.758628 0.274663 1.037663 0.038 Uiso 1 1 calc R . . . .
C17 C 0.3013(2) 0.5336(2) 0.88715(17) 0.0242(6) Uani 1 1 d . . . . .
C18 C 0.2539(3) 0.6048(2) 0.82002(19) 0.0286(7) Uani 1 1 d . . . . .
H18 H 0.177007 0.636638 0.825121 0.034 Uiso 1 1 calc R . . . .
C19 C 0.3224(3) 0.6276(2) 0.74552(18) 0.0283(6) Uani 1 1 d . . . . .
H19 H 0.290196 0.674558 0.697933 0.034 Uiso 1 1 calc R . . . .
C20 C 0.4382(3) 0.5838(2) 0.73747(18) 0.0272(6) Uani 1 1 d . . . . .
C021 C 0.1257(4) 0.8934(3) 0.3966(3) 0.0616(12) Uani 1 1 d . . . . .
H02A H 0.126434 0.955564 0.361843 0.092 Uiso 1 1 calc GR . . . .
H02B H 0.203110 0.870495 0.424317 0.092 Uiso 1 1 calc GR . . . .
H02C H 0.062418 0.890922 0.440994 0.092 Uiso 1 1 calc GR . . . .
C21 C 0.4861(3) 0.5157(2) 0.80745(18) 0.0268(6) Uani 1 1 d . . . . .
H21 H 0.565104 0.486560 0.804006 0.032 Uiso 1 1 calc R . . . .
C22 C 0.4175(2) 0.4907(2) 0.88240(17) 0.0248(6) Uani 1 1 d . . . . .
C23 C 0.5092(3) 0.6109(2) 0.65625(18) 0.0270(6) Uani 1 1 d . . . . .
C24 C 0.4568(3) 0.6303(3) 0.5754(2) 0.0415(8) Uani 1 1 d . . . . .
H24 H 0.374483 0.625556 0.572164 0.050 Uiso 1 1 calc R . . . .
C25 C 0.5230(3) 0.6560(3) 0.5006(2) 0.0438(9) Uani 1 1 d . . . . .
C26 C 0.6420(3) 0.6678(2) 0.50327(19) 0.0312(7) Uani 1 1 d . . . . .
C27 C 0.6947(3) 0.6462(2) 0.5821(2) 0.0365(8) Uani 1 1 d . . . . .
H27 H 0.776873 0.651262 0.585111 0.044 Uiso 1 1 calc R . . . .
C28 C 0.6285(3) 0.6167(2) 0.65819(19) 0.0334(7) Uani 1 1 d . . . . .
H28 H 0.667098 0.600463 0.712246 0.040 Uiso 1 1 calc R . . . .
C29 C 0.8510(6) -0.1015(3) 1.1577(8) 0.064(2) Uani 0.759(19) 1 d D . P A 1
H29A H 0.814158 -0.110485 1.215455 0.095 Uiso 0.759(19) 1 calc GR . P A 1
H29B H 0.923264 -0.144744 1.160092 0.095 Uiso 0.759(19) 1 calc GR . P A 1
H29C H 0.794449 -0.110149 1.117895 0.095 Uiso 0.759(19) 1 calc GR . P A 1
C29A C 0.861(2) -0.0908(12) 1.1981(15) 0.064(2) Uani 0.241(19) 1 d D . P A 2
H29D H 0.844689 -0.073555 1.251951 0.095 Uiso 0.241(19) 1 calc GR . P A 2
H29E H 0.932283 -0.135774 1.204928 0.095 Uiso 0.241(19) 1 calc GR . P A 2
H29F H 0.792639 -0.115966 1.184676 0.095 Uiso 0.241(19) 1 calc GR . P A 2
C30 C 0.9690(4) 0.2260(4) 1.0028(4) 0.0543(14) Uani 0.737(6) 1 d D . P B 1
H30A H 0.913495 0.252067 0.955012 0.081 Uiso 0.737(6) 1 calc GR . P B 1
H30B H 1.050316 0.216688 0.979564 0.081 Uiso 0.737(6) 1 calc GR . P B 1
H30C H 0.965842 0.266720 1.039318 0.081 Uiso 0.737(6) 1 calc GR . P B 1
C30A C 0.9876(12) 0.1369(11) 0.9759(7) 0.0543(14) Uani 0.263(6) 1 d D . P B 2
H30D H 0.987396 0.075262 0.973449 0.081 Uiso 0.263(6) 1 calc GR . P B 2
H30E H 1.070102 0.150249 0.971848 0.081 Uiso 0.263(6) 1 calc GR . P B 2
H30F H 0.942088 0.178375 0.927565 0.081 Uiso 0.263(6) 1 calc GR . P B 2
C31 C 0.4326(15) 0.6142(16) 0.396(2) 0.052(4) Uani 0.554(6) 1 d D . P C 1
H31A H 0.399411 0.634200 0.338169 0.078 Uiso 0.554(6) 1 calc GR . P C 1
H31B H 0.374973 0.582994 0.437117 0.078 Uiso 0.554(6) 1 calc GR . P C 1
H31C H 0.506895 0.573489 0.396299 0.078 Uiso 0.554(6) 1 calc GR . P C 1
C31A C 0.397(2) 0.619(2) 0.404(3) 0.052(4) Uani 0.446(6) 1 d D . P C 2
H31D H 0.388236 0.624399 0.342911 0.078 Uiso 0.446(6) 1 calc GR . P C 2
H31E H 0.328149 0.652876 0.425123 0.078 Uiso 0.446(6) 1 calc GR . P C 2
H31F H 0.402635 0.555570 0.437218 0.078 Uiso 0.446(6) 1 calc GR . P C 2
C32 C 0.8161(3) 0.7175(2) 0.4243(2) 0.0414(8) Uani 1 1 d . . . . .
H32A H 0.844277 0.739889 0.364533 0.062 Uiso 1 1 calc GR . . . .
H32B H 0.866865 0.662065 0.452878 0.062 Uiso 1 1 calc GR . . . .
H32C H 0.819726 0.762514 0.455262 0.062 Uiso 1 1 calc GR . . . .
C33 C 0.1894(2) 0.37174(19) 0.86221(18) 0.0241(6) Uani 1 1 d . . . . .
C34 C 0.2299(3) 0.3032(2) 0.93435(18) 0.0285(7) Uani 1 1 d . . . . .
H34 H 0.195578 0.300422 0.990046 0.034 Uiso 1 1 calc R . . . .
C35 C 0.3215(3) 0.2395(2) 0.92237(19) 0.0304(7) Uani 1 1 d . . . . .
H35 H 0.350911 0.192677 0.971071 0.036 Uiso 1 1 calc R . . . .
C36 C 0.3729(3) 0.2413(2) 0.84041(18) 0.0271(6) Uani 1 1 d . . . . .
C37 C 0.3285(3) 0.3098(2) 0.76844(18) 0.0259(6) Uani 1 1 d . . . . .
H37 H 0.361477 0.311798 0.712498 0.031 Uiso 1 1 calc R . . . .
C38 C 0.2363(2) 0.37462(19) 0.77911(17) 0.0240(6) Uani 1 1 d . . . . .
C39 C 0.4686(3) 0.1698(2) 0.83058(19) 0.0290(7) Uani 1 1 d . . . . .
C40 C 0.5449(3) 0.1233(2) 0.8980(2) 0.0349(7) Uani 1 1 d . . . . .
H40 H 0.536029 0.137835 0.951524 0.042 Uiso 1 1 calc R . . . .
C41 C 0.6343(3) 0.0555(2) 0.8877(2) 0.0374(8) Uani 1 1 d . . . . .
H41 H 0.685557 0.024350 0.934387 0.045 Uiso 1 1 calc R . . . .
C42 C 0.6489(3) 0.0332(2) 0.8104(2) 0.0348(7) Uani 1 1 d . . . . .
C43 C 0.5714(3) 0.0790(2) 0.7424(2) 0.0318(7) Uani 1 1 d . . . . .
C44 C 0.4833(3) 0.1465(2) 0.75235(19) 0.0293(7) Uani 1 1 d . . . . .
H44 H 0.432018 0.177380 0.705656 0.035 Uiso 1 1 calc R . . . .
C45 C 0.0870(2) 0.4933(2) 0.76959(17) 0.0238(6) Uani 1 1 d . . . . .
C46 C 0.0138(3) 0.5725(2) 0.73358(18) 0.0271(6) Uani 1 1 d . . . . .
H46 H -0.042688 0.599104 0.767967 0.033 Uiso 1 1 calc R . . . .
C47 C 0.0260(3) 0.6114(2) 0.64601(17) 0.0262(6) Uani 1 1 d . . . . .
H47 H -0.021963 0.666425 0.620289 0.031 Uiso 1 1 calc R . . . .
C48 C 0.1078(3) 0.5719(2) 0.59324(18) 0.0265(6) Uani 1 1 d . . . . .
C49 C 0.1794(3) 0.4924(2) 0.63102(17) 0.0254(6) Uani 1 1 d . . . . .
H49 H 0.234621 0.464994 0.596441 0.031 Uiso 1 1 calc R . . . .
C50 C 0.1706(2) 0.45257(19) 0.71968(17) 0.0232(6) Uani 1 1 d . . . . .
C51 C 0.1121(3) 0.6158(2) 0.49872(18) 0.0285(7) Uani 1 1 d . . . . .
C52 C 0.1097(3) 0.7081(2) 0.46734(19) 0.0352(7) Uani 1 1 d . . . . .
H52 H 0.108725 0.743206 0.506776 0.042 Uiso 1 1 calc R . . . .
C53 C 0.1087(3) 0.7499(2) 0.3784(2) 0.0406(8) Uani 1 1 d . . . . .
C54 C 0.1104(3) 0.6975(2) 0.3209(2) 0.0384(8) Uani 1 1 d . . . . .
C55 C 0.1133(3) 0.6065(2) 0.35174(19) 0.0334(7) Uani 1 1 d . . . . .
H55 H 0.114380 0.571463 0.312205 0.040 Uiso 1 1 calc R . . . .
C56 C 0.1146(3) 0.5647(2) 0.43995(18) 0.0297(7) Uani 1 1 d . . . . .
H56 H 0.117078 0.501468 0.460402 0.036 Uiso 1 1 calc R . . . .
C57 C 0.8287(3) -0.0651(3) 0.8538(3) 0.0570(11) Uani 1 1 d . . . . .
H57A H 0.887149 -0.107129 0.832867 0.085 Uiso 1 1 calc GR . . . .
H57B H 0.796325 -0.096031 0.910126 0.085 Uiso 1 1 calc GR . . . .
H57C H 0.867635 -0.015269 0.859615 0.085 Uiso 1 1 calc GR . . . .
C58 C 0.5100(4) 0.0923(3) 0.5990(2) 0.0528(11) Uani 1 1 d . . . . .
H58A H 0.531819 0.065677 0.551144 0.079 Uiso 1 1 calc GR . . . .
H58B H 0.515174 0.156726 0.579272 0.079 Uiso 1 1 calc GR . . . .
H58C H 0.428179 0.082859 0.618704 0.079 Uiso 1 1 calc GR . . . .
C60 C 0.2152(5) 0.7665(3) 0.1960(3) 0.0721(15) Uani 1 1 d . . . . .
H60A H 0.202182 0.806214 0.137477 0.108 Uiso 1 1 calc GR . . . .
H60B H 0.272286 0.713977 0.193705 0.108 Uiso 1 1 calc GR . . . .
H60C H 0.247026 0.798727 0.231881 0.108 Uiso 1 1 calc GR . . . .
N1 N 0.2097(2) 0.57013(19) 1.15074(16) 0.0348(6) Uani 1 1 d . . . . .
N2 N 0.2498(2) 0.49464(17) 0.96861(14) 0.0254(5) Uani 1 1 d . . . . .
N3 N 0.0979(2) 0.44306(16) 0.85692(14) 0.0244(5) Uani 1 1 d . . . . .
O1 O 0.8819(2) -0.01159(17) 1.1274(2) 0.0591(8) Uani 1 1 d D . . . .
O2 O 0.9376(2) 0.14631(19) 1.05052(18) 0.0562(7) Uani 1 1 d D . . . .
O3 O 0.4569(5) 0.6906(4) 0.4218(3) 0.0410(11) Uani 0.554(6) 1 d D . P C 1
O3A O 0.5046(7) 0.6534(5) 0.4158(4) 0.0410(11) Uani 0.446(6) 1 d D . P C 2
O4 O 0.6964(2) 0.70009(16) 0.42454(13) 0.0385(6) Uani 1 1 d . . . . .
O5 O 0.7335(2) -0.03117(16) 0.79347(15) 0.0457(6) Uani 1 1 d . . . . .
O6 O 0.5904(2) 0.05096(16) 0.66892(15) 0.0437(6) Uani 1 1 d . . . . .
O7 O 0.1041(3) 0.83983(17) 0.34206(16) 0.0561(7) Uani 1 1 d . . . . .
O8 O 0.1039(2) 0.73827(18) 0.23275(14) 0.0515(7) Uani 1 1 d . . . . .
C61A C 0.2054(5) 0.8863(3) 0.6855(3) 0.0428(13) Uani 0.691(3) 1 d . . P D 1
H61A H 0.255139 0.866011 0.738580 0.051 Uiso 0.691(3) 1 calc R . P D 1
Cl1A Cl 0.29295(15) 0.86079(10) 0.60099(9) 0.0550(5) Uani 0.691(3) 1 d . . P D
1
Cl2A Cl 0.08234(14) 0.82821(12) 0.70594(13) 0.0634(5) Uani 0.691(3) 1 d . . P D
1
Cl3A Cl 0.16031(19) 1.00153(11) 0.66607(11) 0.0637(5) Uani 0.691(3) 1 d . . P D
1
C61B C 0.2341(16) 0.9038(12) 0.6913(18) 0.0428(13) Uani 0.066(2) 1 d D . P E 2
H61B H 0.248403 0.894583 0.753959 0.051 Uiso 0.066(2) 1 calc R . P E 2
Cl1B Cl 0.3560(15) 0.8683(10) 0.6335(11) 0.0550(5) Uani 0.066(2) 1 d D . P E 2
Cl2B Cl 0.1207(15) 0.8504(12) 0.6702(15) 0.0634(5) Uani 0.066(2) 1 d D . P E 2
Cl3B Cl 0.1931(19) 1.0143(12) 0.6332(13) 0.0637(5) Uani 0.066(2) 1 d D . P E 2
C62A C 0.7208(4) 0.8718(3) 0.6493(3) 0.0401(10) Uani 0.800(4) 1 d D . P F 1
H62A H 0.714502 0.920271 0.679109 0.048 Uiso 0.800(4) 1 calc R . P F 1
Cl4A Cl 0.80515(15) 0.77574(10) 0.71426(9) 0.0460(5) Uani 0.800(4) 1 d D . P F
1
Cl5A Cl 0.57621(14) 0.85020(11) 0.63680(9) 0.0513(4) Uani 0.800(4) 1 d D . P F
1
Cl6A Cl 0.79189(15) 0.90923(11) 0.54840(10) 0.0657(5) Uani 0.800(4) 1 d D . P F
1
C62B C 0.747(2) 0.8929(18) 0.6196(16) 0.0401(10) Uani 0.045(2) 1 d D . P G 2
H62B H 0.727672 0.940846 0.649896 0.048 Uiso 0.045(2) 1 calc R . P G 2
Cl4B Cl 0.8510(19) 0.8137(15) 0.6835(14) 0.0460(5) Uani 0.045(2) 1 d D . P G 2
Cl5B Cl 0.611(2) 0.855(2) 0.615(2) 0.0513(4) Uani 0.045(2) 1 d D . P G 2
Cl6B Cl 0.802(3) 0.9459(19) 0.5190(15) 0.0657(5) Uani 0.045(2) 1 d D . P G 2
C62C C 0.777(3) 0.878(3) 0.6373(18) 0.0401(10) Uani 0.0277(18) 1 d D . P H 4
H62C H 0.751045 0.930741 0.659890 0.048 Uiso 0.0277(18) 1 calc R . P H 4
Cl4D Cl 0.807(4) 0.788(4) 0.728(2) 0.0460(5) Uani 0.0277(18) 1 d D . P H 4
Cl5D Cl 0.655(3) 0.870(2) 0.580(2) 0.0513(4) Uani 0.0277(18) 1 d D . P H 4
Cl6D Cl 0.902(3) 0.903(2) 0.573(2) 0.0657(5) Uani 0.0277(18) 1 d D . P H 4
C62D C 0.774(2) 0.910(2) 0.6029(18) 0.0401(10) Uani 0.0262(14) 1 d D . P I 3
H62D H 0.755187 0.956939 0.634901 0.048 Uiso 0.0262(14) 1 calc R . P I 3
Cl4C Cl 0.918(2) 0.859(2) 0.634(2) 0.0460(5) Uani 0.0262(14) 1 d D . P I 3
Cl5C Cl 0.667(2) 0.839(2) 0.637(2) 0.0513(4) Uani 0.0262(14) 1 d D . P I 3
Cl6C Cl 0.765(3) 0.969(2) 0.4944(19) 0.0657(5) Uani 0.0262(14) 1 d D . P I 3
O9 O -0.0233(15) 0.7061(11) 0.8792(10) 0.026(6) Uiso 0.120(7) 1 d . . . J 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.439(4) . ?
C1 N1 1.145(4) . ?
C2 C3 1.405(4) . ?
C2 C4 1.405(4) 2_567 ?
C3 C4 1.401(4) . ?
C3 N2 1.413(4) . ?
C4 N3 1.409(3) . ?
C5 C6 1.382(4) . ?
C5 C10 1.401(4) . ?
C5 N2 1.422(4) . ?
C6 C7 1.383(4) . ?
C7 C8 1.404(4) . ?
C8 C9 1.396(4) . ?
C8 C11 1.483(4) . ?
C9 C10 1.383(4) . ?
C10 C22 1.453(4) . ?
C11 C12 1.382(5) . ?
C11 C16 1.405(4) . ?
C12 C13 1.397(5) . ?
C13 C14 1.379(5) . ?
C14 C15 1.398(5) . ?
C14 O1 1.367(4) . ?
C15 C16 1.374(4) . ?
C15 O2 1.370(4) . ?
C17 C18 1.387(4) . ?
C17 C22 1.396(4) . ?
C17 N2 1.415(4) . ?
C18 C19 1.380(4) . ?
C19 C20 1.405(4) . ?
C20 C21 1.391(4) . ?
C20 C23 1.485(4) . ?
C021 O7 1.429(4) . ?
C21 C22 1.389(4) . ?
C23 C24 1.400(4) . ?
C23 C28 1.370(4) . ?
C24 C25 1.374(5) . ?
C25 C26 1.391(5) . ?
C25 O3 1.439(6) . ?
C25 O3A 1.407(7) . ?
C26 C27 1.368(4) . ?
C26 O4 1.373(4) . ?
C27 C28 1.398(4) . ?
C29 O1 1.445(5) . ?
C29A O1 1.469(10) . ?
C30 O2 1.356(5) . ?
C30A O2 1.337(9) . ?
C31 O3 1.437(11) . ?
C31A O3A 1.441(11) . ?
C32 O4 1.420(4) . ?
C33 C34 1.392(4) . ?
C33 C38 1.404(4) . ?
C33 N3 1.398(3) . ?
C34 C35 1.377(4) . ?
C35 C36 1.407(4) . ?
C36 C37 1.402(4) . ?
C36 C39 1.479(4) . ?
C37 C38 1.387(4) . ?
C38 C50 1.459(4) . ?
C39 C40 1.393(4) . ?
C39 C44 1.404(4) . ?
C40 C41 1.397(4) . ?
C41 C42 1.382(4) . ?
C42 C43 1.405(4) . ?
C42 O5 1.363(4) . ?
C43 C44 1.383(4) . ?
C43 O6 1.372(3) . ?
C45 C46 1.386(4) . ?
C45 C50 1.407(4) . ?
C45 N3 1.410(3) . ?
C46 C47 1.380(4) . ?
C47 C48 1.416(4) . ?
C48 C49 1.387(4) . ?
C48 C51 1.487(4) . ?
C49 C50 1.394(4) . ?
C51 C52 1.390(4) . ?
C51 C56 1.401(4) . ?
C52 C53 1.399(4) . ?
C53 C54 1.400(5) . ?
C53 O7 1.362(4) . ?
C54 C55 1.371(5) . ?
C54 O8 1.387(4) . ?
C55 C56 1.389(4) . ?
C57 O5 1.433(4) . ?
C58 O6 1.435(4) . ?
C60 O8 1.436(5) . ?
C61A Cl1A 1.742(5) . ?
C61A Cl2A 1.739(5) . ?
C61A Cl3A 1.751(5) . ?
C61B Cl1B 1.734(10) . ?
C61B Cl2B 1.728(10) . ?
C61B Cl3B 1.734(10) . ?
Cl3B Cl6B 2.35(3) 2_676 ?
C62A Cl4A 1.759(4) . ?
C62A Cl5A 1.753(5) . ?
C62A Cl6A 1.758(4) . ?
C62B Cl4B 1.732(10) . ?
C62B Cl5B 1.733(10) . ?
C62B Cl6B 1.732(10) . ?
C62C Cl4D 1.735(10) . ?
C62C Cl5D 1.734(10) . ?
C62C Cl6D 1.733(10) . ?
C62D Cl4C 1.735(10) . ?
C62D Cl5C 1.734(10) . ?
C62D Cl6C 1.735(10) . ?

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
N1 C1 C2 178.9(3) . . ?
C3 C2 C1 117.8(3) . . ?
C4 C2 C1 119.7(2) 2_567 . ?
C4 C2 C3 122.3(2) 2_567 . ?
C2 C3 N2 119.1(2) . . ?
C4 C3 C2 118.1(3) . . ?
C4 C3 N2 122.8(2) . . ?
C2 C4 N3 118.8(2) 2_567 . ?
C3 C4 C2 119.6(2) . 2_567 ?
C3 C4 N3 121.5(3) . . ?
C6 C5 C10 121.1(3) . . ?
C6 C5 N2 130.2(3) . . ?
C10 C5 N2 108.6(2) . . ?
C5 C6 C7 118.3(3) . . ?
C6 C7 C8 121.8(3) . . ?
C7 C8 C11 121.7(3) . . ?
C9 C8 C7 118.8(3) . . ?
C9 C8 C11 119.4(3) . . ?
C10 C9 C8 120.0(3) . . ?
C5 C10 C22 107.5(2) . . ?
C9 C10 C5 119.9(3) . . ?
C9 C10 C22 132.3(3) . . ?
C12 C11 C8 121.6(3) . . ?
C12 C11 C16 117.6(3) . . ?
C16 C11 C8 120.4(3) . . ?
C11 C12 C13 121.5(3) . . ?
C14 C13 C12 120.2(3) . . ?
C13 C14 C15 118.8(3) . . ?
O1 C14 C13 125.4(3) . . ?
O1 C14 C15 115.8(3) . . ?
C16 C15 C14 120.7(3) . . ?
O2 C15 C14 115.9(3) . . ?
O2 C15 C16 123.5(3) . . ?
C15 C16 C11 121.1(3) . . ?
C18 C17 C22 121.5(3) . . ?
C18 C17 N2 129.4(3) . . ?
C22 C17 N2 109.1(2) . . ?
C19 C18 C17 117.5(3) . . ?
C18 C19 C20 122.4(3) . . ?
C19 C20 C23 120.6(3) . . ?
C21 C20 C19 118.9(3) . . ?
C21 C20 C23 120.5(3) . . ?
C22 C21 C20 119.5(3) . . ?
C17 C22 C10 107.3(2) . . ?
C21 C22 C10 132.6(3) . . ?
C21 C22 C17 120.1(3) . . ?
C24 C23 C20 121.2(3) . . ?
C28 C23 C20 120.9(3) . . ?
C28 C23 C24 117.9(3) . . ?
C25 C24 C23 120.8(3) . . ?
C24 C25 C26 120.8(3) . . ?
C24 C25 O3 116.3(4) . . ?
C24 C25 O3A 131.2(4) . . ?
C26 C25 O3 121.2(4) . . ?
C26 C25 O3A 106.0(4) . . ?
C27 C26 C25 118.5(3) . . ?
C27 C26 O4 125.9(3) . . ?
O4 C26 C25 115.6(3) . . ?
C26 C27 C28 120.5(3) . . ?
C23 C28 C27 121.2(3) . . ?
C34 C33 C38 121.6(3) . . ?
C34 C33 N3 129.0(2) . . ?
N3 C33 C38 109.4(2) . . ?
C35 C34 C33 117.8(3) . . ?
C34 C35 C36 122.2(3) . . ?
C35 C36 C39 120.1(3) . . ?
C37 C36 C35 118.9(3) . . ?
C37 C36 C39 121.0(3) . . ?
C38 C37 C36 119.8(3) . . ?
C33 C38 C50 106.7(2) . . ?
C37 C38 C33 119.6(3) . . ?
C37 C38 C50 133.7(3) . . ?
C40 C39 C36 121.5(3) . . ?
C40 C39 C44 118.4(3) . . ?
C44 C39 C36 120.1(3) . . ?
C39 C40 C41 120.8(3) . . ?
C42 C41 C40 120.6(3) . . ?
C41 C42 C43 119.0(3) . . ?
O5 C42 C41 125.3(3) . . ?
O5 C42 C43 115.7(3) . . ?
C44 C43 C42 120.4(3) . . ?
O6 C43 C42 115.0(3) . . ?
O6 C43 C44 124.6(3) . . ?
C43 C44 C39 120.8(3) . . ?
C46 C45 C50 122.0(3) . . ?
C46 C45 N3 129.2(2) . . ?
C50 C45 N3 108.7(2) . . ?
C47 C46 C45 117.6(3) . . ?
C46 C47 C48 122.1(3) . . ?
C47 C48 C51 119.0(3) . . ?
C49 C48 C47 119.0(3) . . ?
C49 C48 C51 122.1(2) . . ?
C48 C49 C50 120.1(2) . . ?
C45 C50 C38 107.0(2) . . ?
C49 C50 C38 133.8(3) . . ?
C49 C50 C45 119.1(3) . . ?
C52 C51 C48 120.8(3) . . ?
C52 C51 C56 119.1(3) . . ?
C56 C51 C48 120.1(3) . . ?
C51 C52 C53 120.8(3) . . ?
C52 C53 C54 119.1(3) . . ?
O7 C53 C52 124.8(3) . . ?
O7 C53 C54 116.1(3) . . ?
C55 C54 C53 120.2(3) . . ?
C55 C54 O8 119.9(3) . . ?
O8 C54 C53 119.8(3) . . ?
C54 C55 C56 120.9(3) . . ?
C55 C56 C51 119.9(3) . . ?
C3 N2 C5 123.5(2) . . ?
C3 N2 C17 123.2(2) . . ?
C17 N2 C5 107.5(2) . . ?
C4 N3 C45 124.8(2) . . ?
C33 N3 C4 124.5(2) . . ?
C33 N3 C45 108.2(2) . . ?
C14 O1 C29 117.2(4) . . ?
C14 O1 C29A 113.4(10) . . ?
C30 O2 C15 118.2(3) . . ?
C30A O2 C15 127.8(7) . . ?
C31 O3 C25 106.5(14) . . ?
C25 O3A C31A 115.1(17) . . ?
C26 O4 C32 117.6(2) . . ?
C42 O5 C57 116.6(3) . . ?
C43 O6 C58 117.4(2) . . ?
C53 O7 C021 117.6(3) . . ?
C54 O8 C60 112.4(3) . . ?
Cl1A C61A Cl3A 112.1(3) . . ?
Cl2A C61A Cl1A 110.7(3) . . ?
Cl2A C61A Cl3A 110.7(3) . . ?
Cl1B C61B Cl3B 103.6(13) . . ?
Cl2B C61B Cl1B 104.2(13) . . ?
Cl2B C61B Cl3B 103.0(13) . . ?
C61B Cl3B Cl6B 119.8(15) . 2_676 ?
Cl5A C62A Cl4A 110.4(2) . . ?
Cl5A C62A Cl6A 110.9(2) . . ?
Cl6A C62A Cl4A 110.8(2) . . ?
Cl4B C62B Cl5B 113.7(10) . . ?
Cl6B C62B Cl4B 113.5(9) . . ?
Cl6B C62B Cl5B 113.4(9) . . ?
Cl5D C62C Cl4D 113.6(10) . . ?
Cl6D C62C Cl4D 113.5(10) . . ?
Cl6D C62C Cl5D 113.5(10) . . ?
Cl4C C62D Cl6C 113.6(10) . . ?
Cl5C C62D Cl4C 113.1(10) . . ?
Cl5C C62D Cl6C 113.4(10) . . ?

_olex2_date_sample_data_collection 2019-12-16
_olex2_date_sample_submission    2020-01-09
_olex2_exptl_crystal_mounting_method 'oil on 75 micrometre micromount'
_olex2_submission_original_sample_id SAY-068
_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 2.728
_oxdiff_exptl_absorpt_empirical_full_min 0.635
####################################################################### 
# 
# 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_dwb2007
_database_code_depnum_ccdc_archive 'CCDC 2056912'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_audit_creation_date             2020-05-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
adrian.whitwood@york.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H50 N4 O8, 2(C2 H3 N1)'
_chemical_formula_sum            'C68 H56 N6 O8'
_chemical_formula_weight         1085.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C68 H56 N6 O8'
_chemical_oxdiff_usercomment     'Alfiya Suleymanova SAY-070'
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                   8.7095(6)
_cell_length_b                   12.8934(10)
_cell_length_c                   14.2434(10)
_cell_angle_alpha                101.702(6)
_cell_angle_beta                 105.271(6)
_cell_angle_gamma                108.031(7)
_cell_volume                     1394.93(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2592
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      69.9700
_cell_measurement_theta_min      7.1670
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.849
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.76a (Rigaku Oxford Diffraction, 2020)
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 dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             570
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.0203
-1 1 2 0.0991
1 0 0 0.1017
-1 0 0 0.1032
0 -1 0 0.0164
0 0 -1 0.0140
0 0 1 0.0368
0 1 -1 0.0100
2 -1 -2 0.1034
0 1 0 0.0341

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform and acetonitrile'
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.03
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
-0.0005 -0.9991 0.9999 0.0791 -0.1199 0.0323
-0.9991 1.0023 1.9984 -0.1313 -0.0853 0.2331
1.0008 -0.0007 -0.0004 0.1382 0.1254 0.0682
-1.0008 0.0007 0.0004 -0.1382 -0.1254 -0.0682
-0.0009 -0.9999 0.0006 0.0504 -0.0933 -0.0789
-0.0004 -0.0008 -0.9993 -0.0287 0.0266 -0.1112
0.0004 0.0008 0.9993 0.0287 -0.0266 0.1112
0.0005 0.9991 -0.9999 -0.0791 0.1199 -0.0323
1.9999 -1.0031 -1.9988 0.2695 0.2107 -0.1649
0.0009 0.9999 -0.0006 -0.0504 0.0933 0.0789

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8913
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.068
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         3.383
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  20.00   1.00    8.00    --    0.00 -57.00  90.00   33
  2  ω     30.00  69.00   1.00    8.00    --    0.00  57.00-120.00   39
  3  ω    -67.00 -38.00   1.00    8.00    --    0.00 -57.00  90.00   29
  4  ω    -21.00   4.00   1.00    8.00    --    0.00 -77.00  90.00   25
  5  ω    -17.00  13.00   1.00    8.00    --    0.00  57.00-120.00   30
  6  ω     32.00  71.00   1.00   32.00    --   54.00 -99.00  30.00   39
  7  ω    -10.00  72.00   1.00   32.00    --   54.00 -57.00  60.00   82
  8  ω     38.00 104.00   1.00   32.00    --   54.00-125.00 -30.00   66
  9  ω     10.00 121.00   1.00   32.00    --   54.00  19.00 -30.00  111
 10  ω     33.00 126.00   1.00   32.00    --   54.00  37.00  30.00   93
 11  ω    -12.00  66.00   1.00   32.00    --   54.00 -57.00 150.00   78
 12  ω    104.00 163.00   1.00   32.00    --  108.00  77.00 -30.00   59
 13  ω     36.00 107.00   1.00   32.00    --  108.00-111.00-120.00   71
 14  ω     37.00  97.00   1.00   32.00    --  108.00-111.00 -60.00   60
 15  ω     44.00 109.00   1.00   32.00    --  108.00-111.00 150.00   65
 16  ω    133.00 178.00   1.00   32.00    --  108.00  77.00  60.00   45
 17  ω    121.00 148.00   1.00   32.00    --  108.00  63.00-180.00   27
 18  ω     82.00 141.00   1.00   32.00    --  108.00  37.00  90.00   59
 19  ω    104.00 170.00   1.00   32.00    --  108.00  77.00  90.00   66
 20  ω     74.00 107.00   1.00   32.00    --  108.00 -91.00  30.00   33
 21  ω     86.00 115.00   1.00   32.00    --  108.00 178.00 -30.00   29
 22  ω     88.00 177.00   1.00   32.00    --  108.00  50.00  30.00   89
 23  ω    103.00 175.00   1.00   32.00    --  108.00  77.00 120.00   72
 24  ω     41.00 123.00   1.00   32.00    --  108.00 -63.00 -60.00   82
 25  ω     46.00 119.00   1.00   32.00    --  108.00 -50.00  30.00   73
 26  ω    119.00 175.00   1.00   32.00    --  108.00 111.00 -60.00   56
 27  ω     67.00 109.00   1.00   32.00    --  108.00-111.00   0.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1381022000
_diffrn_orient_matrix_UB_12      -0.0505610000
_diffrn_orient_matrix_UB_13      0.0287018000
_diffrn_orient_matrix_UB_21      0.1253317000
_diffrn_orient_matrix_UB_22      0.0931869000
_diffrn_orient_matrix_UB_23      -0.0267565000
_diffrn_orient_matrix_UB_31      0.0682873000
_diffrn_orient_matrix_UB_32      0.0789160000
_diffrn_orient_matrix_UB_33      0.1112082000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3794
_reflns_number_total             4977
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         4977
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0532P)²+0.3585P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1144
_refine_special_details          
;
The acetonitrile of crystallisation was disordered and modelled in 
two positions with refined occupancies of 0.943:0.057(3). The nitrogens
occupied a common site with coordinates and ADP constrained
to be equal. For these acetonitriles, C-C bond lengths were restrained 
to be equal, C-N bond-lengths restrained to be equal and C-C-N distances
restrained to be equal.  ADP of equivalent pairs of carbons in the 
acetonitrile were constrained to be equal, namely C33 & C33A, C34 & C34A.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N3, N3A}
3. Restrained distances
 N3-C33 \\sim N3A-C33A
 with sigma of 0.001
 C34-C33 \\sim C33A-C34A
 with sigma of 0.001
 N3-C34 \\sim N3A-C34A
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(C34A)
Uanis(N3) = Uanis(N3A)
Uanis(C33) = Uanis(C33A)
5. Others
 Sof(C33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(N3A)=1-FVAR(1)
 Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(N3)=FVAR(1)
6.a Riding coordinates:
 C34A(H34D,H34E,H34F)
6.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C)
;
_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
C1 C 0.3869(2) 0.66476(15) 0.24985(13) 0.0206(4) Uani 1 1 d . . . . .
C2 C 0.3391(2) 0.75775(16) 0.27309(14) 0.0227(4) Uani 1 1 d . . . . .
H2 H 0.228(3) 0.7555(18) 0.2348(16) 0.035(6) Uiso 1 1 d . . . . .
C3 C 0.4547(2) 0.85297(16) 0.35390(14) 0.0224(4) Uani 1 1 d . . . . .
H3 H 0.424(2) 0.9190(17) 0.3714(14) 0.021(5) Uiso 1 1 d . . . . .
C4 C 0.6160(2) 0.85790(15) 0.41475(13) 0.0209(4) Uani 1 1 d . . . . .
C5 C 0.6573(2) 0.76201(15) 0.39360(13) 0.0209(4) Uani 1 1 d . . . . .
H5 H 0.768(3) 0.7614(16) 0.4344(14) 0.021(5) Uiso 1 1 d . . . . .
C6 C 0.5440(2) 0.66550(15) 0.31107(13) 0.0205(4) Uani 1 1 d . . . . .
C7 C 0.5556(2) 0.55873(15) 0.26487(13) 0.0197(4) Uani 1 1 d . . . . .
C8 C 0.6853(2) 0.51615(15) 0.28687(14) 0.0213(4) Uani 1 1 d . . . . .
H8 H 0.791(3) 0.5633(16) 0.3490(14) 0.019(5) Uiso 1 1 d . . . . .
C9 C 0.6677(2) 0.41369(15) 0.22160(14) 0.0213(4) Uani 1 1 d . . . . .
C10 C 0.5145(2) 0.35232(16) 0.13623(14) 0.0227(4) Uani 1 1 d . . . . .
H10 H 0.500(3) 0.2786(17) 0.0898(15) 0.026(5) Uiso 1 1 d . . . . .
C11 C 0.3821(2) 0.39203(16) 0.11357(14) 0.0229(4) Uani 1 1 d . . . . .
H11 H 0.283(3) 0.3484(17) 0.0546(16) 0.027(5) Uiso 1 1 d . . . . .
C12 C 0.4056(2) 0.49625(15) 0.17765(13) 0.0203(4) Uani 1 1 d . . . . .
C13 C 0.1506(2) 0.53128(15) 0.08471(13) 0.0200(4) Uani 1 1 d . . . . .
C14 C 0.1340(2) 0.60447(15) 0.02532(13) 0.0206(4) Uani 1 1 d . . . . .
C15 C 0.0160(2) 0.42642(16) 0.05839(14) 0.0214(4) Uani 1 1 d . . . . .
H15 H 0.024(2) 0.3737(16) 0.0985(14) 0.019(5) Uiso 1 1 d . . . . .
C16 C 0.2756(2) 0.71063(16) 0.04430(14) 0.0238(4) Uani 1 1 d . . . . .
C17 C 0.7397(2) 0.96411(15) 0.49865(13) 0.0214(4) Uani 1 1 d . . . . .
C18 C 0.7629(2) 1.07214(16) 0.48597(14) 0.0222(4) Uani 1 1 d . . . . .
H18 H 0.700(2) 1.0776(15) 0.4172(14) 0.019(5) Uiso 1 1 d . . . . .
C19 C 0.8777(2) 1.17142(15) 0.56311(14) 0.0226(4) Uani 1 1 d . . . . .
C20 C 0.9732(2) 1.16534(15) 0.65740(13) 0.0226(4) Uani 1 1 d . . . . .
C21 C 0.9522(2) 1.05886(17) 0.66953(14) 0.0261(4) Uani 1 1 d . . . . .
H21 H 1.016(3) 1.0531(16) 0.7357(15) 0.024(5) Uiso 1 1 d . . . . .
C22 C 0.8370(2) 0.95913(16) 0.59078(14) 0.0249(4) Uani 1 1 d . . . . .
H22 H 0.822(3) 0.8832(18) 0.6015(15) 0.030(6) Uiso 1 1 d . . . . .
C23 C 0.8020(4) 1.2925(2) 0.4704(2) 0.0516(7) Uani 1 1 d . . . . .
H23A H 0.808(4) 1.252(3) 0.409(2) 0.075(10) Uiso 1 1 d . . . . .
H23B H 0.839(4) 1.377(2) 0.482(2) 0.062(8) Uiso 1 1 d . . . . .
H23C H 0.673(4) 1.251(3) 0.464(2) 0.071(9) Uiso 1 1 d . . . . .
C24 C 1.1913(3) 1.2666(2) 0.82198(16) 0.0391(6) Uani 1 1 d . . . . .
H24A H 1.258(3) 1.350(2) 0.8622(16) 0.033(6) Uiso 1 1 d . . . . .
H24B H 1.123(3) 1.228(2) 0.8648(19) 0.053(7) Uiso 1 1 d . . . . .
H24C H 1.270(3) 1.222(2) 0.8034(19) 0.050(7) Uiso 1 1 d . . . . .
C25 C 0.8120(2) 0.37276(15) 0.24111(13) 0.0211(4) Uani 1 1 d . . . . .
C26 C 0.7818(2) 0.25605(16) 0.20649(14) 0.0238(4) Uani 1 1 d . . . . .
H26 H 0.660(3) 0.1978(18) 0.1655(15) 0.029(5) Uiso 1 1 d . . . . .
C27 C 0.9157(2) 0.21751(16) 0.22534(15) 0.0257(4) Uani 1 1 d . . . . .
C28 C 1.0850(2) 0.29726(17) 0.28259(14) 0.0260(4) Uani 1 1 d . . . . .
C29 C 1.1161(2) 0.41212(17) 0.31565(14) 0.0245(4) Uani 1 1 d . . . . .
H29 H 1.230(3) 0.4687(16) 0.3525(14) 0.019(5) Uiso 1 1 d . . . . .
C30 C 0.9812(2) 0.45056(16) 0.29434(14) 0.0238(4) Uani 1 1 d . . . . .
H30 H 1.012(3) 0.5360(18) 0.3167(15) 0.025(5) Uiso 1 1 d . . . . .
C31 C 0.7286(3) 0.02241(18) 0.13633(19) 0.0419(6) Uani 1 1 d . . . . .
H31A H 0.676787 0.045184 0.078151 0.063 Uiso 1 1 calc R U . . .
H31B H 0.658022 0.017038 0.179920 0.063 Uiso 1 1 calc R U . . .
H31C H 0.734505 -0.052342 0.111132 0.063 Uiso 1 1 calc R U . . .
C32 C 1.3764(3) 0.3261(2) 0.3684(2) 0.0419(6) Uani 1 1 d . . . . .
H32A H 1.429(3) 0.389(2) 0.3449(17) 0.041(6) Uiso 1 1 d . . . . .
H32B H 1.375(3) 0.366(2) 0.437(2) 0.050(7) Uiso 1 1 d . . . . .
H32C H 1.438(4) 0.272(2) 0.370(2) 0.062(8) Uiso 1 1 d . . . . .
N1 N 0.30240(18) 0.56129(12) 0.16878(11) 0.0210(3) Uani 1 1 d . . . . .
N2 N 0.3855(2) 0.79431(15) 0.05626(13) 0.0338(4) Uani 1 1 d . . . . .
O1 O 0.91017(17) 1.28037(11) 0.55766(10) 0.0296(3) Uani 1 1 d . . . . .
O2 O 1.07865(17) 1.26867(11) 0.72934(10) 0.0288(3) Uani 1 1 d . . . . .
O3 O 0.89833(17) 0.10595(11) 0.19429(11) 0.0345(4) Uani 1 1 d . . . . .
O4 O 1.20731(17) 0.25055(12) 0.30034(12) 0.0352(4) Uani 1 1 d . . . . .
C33 C 0.8891(3) 1.0615(2) 0.9264(2) 0.0419(6) Uani 0.938(4) 1 d D . P A 1
C33A C 1.105(2) 1.116(2) 1.0269(13) 0.0419(6) Uani 0.062(4) 1 d D . P A 2
C34 C 0.7470(3) 0.9580(2) 0.8554(2) 0.0521(8) Uani 0.938(4) 1 d D . P A 1
H34A H 0.678242 0.977320 0.800302 0.078 Uiso 0.938(4) 1 calc R U P A 1
H34B H 0.674305 0.923154 0.891698 0.078 Uiso 0.938(4) 1 calc R U P A 1
H34C H 0.792439 0.903667 0.826249 0.078 Uiso 0.938(4) 1 calc R U P A 1
C34A C 1.235(3) 1.088(2) 1.091(2) 0.0521(8) Uani 0.062(4) 1 d D . P A 2
H34D H 1.348426 1.132582 1.089936 0.078 Uiso 0.062(4) 1 d R U P A 2
H34E H 1.209836 1.005832 1.063726 0.078 Uiso 0.062(4) 1 d R U P A 2
H34F H 1.236696 1.105572 1.161416 0.078 Uiso 0.062(4) 1 d R U P A 2
N3 N 1.0011(3) 1.14181(19) 0.98245(18) 0.0558(6) Uani 0.938(4) 1 d D . P A 1
N3A N 1.0011(3) 1.14181(19) 0.98245(18) 0.0558(6) Uani 0.062(4) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.393(2) . ?
C1 C6 1.411(2) . ?
C1 N1 1.405(2) . ?
C2 H2 0.96(2) . ?
C2 C3 1.377(3) . ?
C3 H3 0.97(2) . ?
C3 C4 1.418(2) . ?
C4 C5 1.389(3) . ?
C4 C17 1.486(2) . ?
C5 H5 0.99(2) . ?
C5 C6 1.393(2) . ?
C6 C7 1.446(2) . ?
C7 C8 1.394(2) . ?
C7 C12 1.409(2) . ?
C8 H8 1.005(19) . ?
C8 C9 1.391(3) . ?
C9 C10 1.409(2) . ?
C9 C25 1.491(2) . ?
C10 H10 0.99(2) . ?
C10 C11 1.390(2) . ?
C11 H11 0.95(2) . ?
C11 C12 1.384(3) . ?
C12 N1 1.406(2) . ?
C13 C14 1.404(3) . ?
C13 C15 1.387(3) . ?
C13 N1 1.411(2) . ?
C14 C15 1.397(2) 2_565 ?
C14 C16 1.448(3) . ?
C15 H15 0.979(19) . ?
C16 N2 1.144(2) . ?
C17 C18 1.400(3) . ?
C17 C22 1.388(3) . ?
C18 H18 1.017(19) . ?
C18 C19 1.380(3) . ?
C19 C20 1.413(3) . ?
C19 O1 1.367(2) . ?
C20 C21 1.380(3) . ?
C20 O2 1.364(2) . ?
C21 H21 0.99(2) . ?
C21 C22 1.393(3) . ?
C22 H22 0.99(2) . ?
C23 H23A 0.94(3) . ?
C23 H23B 1.00(3) . ?
C23 H23C 1.05(3) . ?
C23 O1 1.418(3) . ?
C24 H24A 1.01(2) . ?
C24 H24B 1.05(3) . ?
C24 H24C 1.07(3) . ?
C24 O2 1.433(2) . ?
C25 C26 1.401(3) . ?
C25 C30 1.393(2) . ?
C26 H26 1.01(2) . ?
C26 C27 1.388(3) . ?
C27 C28 1.409(3) . ?
C27 O3 1.364(2) . ?
C28 C29 1.375(3) . ?
C28 O4 1.371(2) . ?
C29 H29 0.958(19) . ?
C29 C30 1.396(3) . ?
C30 H30 1.01(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 O3 1.427(2) . ?
C32 H32A 0.97(3) . ?
C32 H32B 1.01(3) . ?
C32 H32C 1.01(3) . ?
C32 O4 1.427(3) . ?
C33 C34 1.452(4) . ?
C33 N3 1.135(3) . ?
C33A C34A 1.452(4) . ?
C33A N3A 1.136(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34A H34D 0.9800 . ?
C34A H34E 0.9800 . ?
C34A H34F 0.9799 . ?

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 C1 C6 120.98(16) . . ?
C2 C1 N1 130.29(16) . . ?
N1 C1 C6 108.72(15) . . ?
C1 C2 H2 121.4(13) . . ?
C3 C2 C1 117.81(16) . . ?
C3 C2 H2 120.8(13) . . ?
C2 C3 H3 119.2(11) . . ?
C2 C3 C4 122.51(17) . . ?
C4 C3 H3 118.2(11) . . ?
C3 C4 C17 120.70(16) . . ?
C5 C4 C3 118.74(16) . . ?
C5 C4 C17 120.55(16) . . ?
C4 C5 H5 121.5(11) . . ?
C4 C5 C6 119.77(16) . . ?
C6 C5 H5 118.7(11) . . ?
C1 C6 C7 106.86(15) . . ?
C5 C6 C1 120.06(16) . . ?
C5 C6 C7 132.92(16) . . ?
C8 C7 C6 132.55(16) . . ?
C8 C7 C12 119.68(16) . . ?
C12 C7 C6 107.58(15) . . ?
C7 C8 H8 117.8(11) . . ?
C9 C8 C7 119.88(16) . . ?
C9 C8 H8 122.3(11) . . ?
C8 C9 C10 118.89(16) . . ?
C8 C9 C25 119.74(16) . . ?
C10 C9 C25 121.34(16) . . ?
C9 C10 H10 119.7(12) . . ?
C11 C10 C9 122.29(17) . . ?
C11 C10 H10 118.1(12) . . ?
C10 C11 H11 119.0(12) . . ?
C12 C11 C10 117.66(16) . . ?
C12 C11 H11 123.3(12) . . ?
C11 C12 C7 121.55(16) . . ?
C11 C12 N1 130.01(16) . . ?
N1 C12 C7 108.34(15) . . ?
C14 C13 N1 121.35(16) . . ?
C15 C13 C14 118.95(16) . . ?
C15 C13 N1 119.69(17) . . ?
C13 C14 C16 121.21(16) . . ?
C15 C14 C13 120.97(17) 2_565 . ?
C15 C14 C16 117.69(17) 2_565 . ?
C13 C15 C14 120.08(17) . 2_565 ?
C13 C15 H15 120.9(11) . . ?
C14 C15 H15 119.1(11) 2_565 . ?
N2 C16 C14 177.9(2) . . ?
C18 C17 C4 120.60(16) . . ?
C22 C17 C4 121.16(17) . . ?
C22 C17 C18 118.23(16) . . ?
C17 C18 H18 119.5(11) . . ?
C19 C18 C17 121.20(17) . . ?
C19 C18 H18 119.1(11) . . ?
C18 C19 C20 120.05(17) . . ?
O1 C19 C18 125.45(17) . . ?
O1 C19 C20 114.50(16) . . ?
C21 C20 C19 118.81(16) . . ?
O2 C20 C19 115.14(16) . . ?
O2 C20 C21 126.05(17) . . ?
C20 C21 H21 119.8(12) . . ?
C20 C21 C22 120.64(18) . . ?
C22 C21 H21 119.5(12) . . ?
C17 C22 C21 121.05(18) . . ?
C17 C22 H22 119.5(12) . . ?
C21 C22 H22 119.5(12) . . ?
H23A C23 H23B 113(3) . . ?
H23A C23 H23C 103(2) . . ?
H23B C23 H23C 115(2) . . ?
O1 C23 H23A 111.6(19) . . ?
O1 C23 H23B 105.6(16) . . ?
O1 C23 H23C 108.1(17) . . ?
H24A C24 H24B 107.9(18) . . ?
H24A C24 H24C 114.1(19) . . ?
H24B C24 H24C 110(2) . . ?
O2 C24 H24A 103.6(13) . . ?
O2 C24 H24B 112.1(14) . . ?
O2 C24 H24C 109.1(13) . . ?
C26 C25 C9 121.25(16) . . ?
C30 C25 C9 120.38(16) . . ?
C30 C25 C26 118.36(16) . . ?
C25 C26 H26 120.0(12) . . ?
C27 C26 C25 121.41(17) . . ?
C27 C26 H26 118.5(12) . . ?
C26 C27 C28 119.22(17) . . ?
O3 C27 C26 125.37(17) . . ?
O3 C27 C28 115.40(16) . . ?
C29 C28 C27 119.70(17) . . ?
O4 C28 C27 114.91(17) . . ?
O4 C28 C29 125.38(17) . . ?
C28 C29 H29 121.6(11) . . ?
C28 C29 C30 120.74(18) . . ?
C30 C29 H29 117.6(11) . . ?
C25 C30 C29 120.50(17) . . ?
C25 C30 H30 121.9(11) . . ?
C29 C30 H30 117.6(12) . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O3 C31 H31A 109.5 . . ?
O3 C31 H31B 109.5 . . ?
O3 C31 H31C 109.5 . . ?
H32A C32 H32B 103(2) . . ?
H32A C32 H32C 113(2) . . ?
H32B C32 H32C 115(2) . . ?
O4 C32 H32A 113.4(14) . . ?
O4 C32 H32B 111.7(15) . . ?
O4 C32 H32C 101.1(15) . . ?
C1 N1 C12 108.50(13) . . ?
C1 N1 C13 126.84(14) . . ?
C12 N1 C13 124.24(14) . . ?
C19 O1 C23 116.87(16) . . ?
C20 O2 C24 116.92(16) . . ?
C27 O3 C31 117.11(15) . . ?
C28 O4 C32 116.73(16) . . ?
N3 C33 C34 179.3(3) . . ?
N3A C33A C34A 175.6(18) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33A C34A H34D 109.1 . . ?
C33A C34A H34E 109.0 . . ?
C33A C34A H34F 110.3 . . ?
H34D C34A H34E 109.5 . . ?
H34D C34A H34F 109.5 . . ?
H34E C34A H34F 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
C1 C2 C3 C4 -1.7(3) . . . . ?
C1 C6 C7 C8 174.59(19) . . . . ?
C1 C6 C7 C12 -0.3(2) . . . . ?
C2 C1 C6 C5 -2.7(3) . . . . ?
C2 C1 C6 C7 -178.64(16) . . . . ?
C2 C1 N1 C12 178.55(19) . . . . ?
C2 C1 N1 C13 5.8(3) . . . . ?
C2 C3 C4 C5 -1.6(3) . . . . ?
C2 C3 C4 C17 177.55(17) . . . . ?
C3 C4 C5 C6 2.7(3) . . . . ?
C3 C4 C17 C18 -39.6(3) . . . . ?
C3 C4 C17 C22 141.33(18) . . . . ?
C4 C5 C6 C1 -0.7(3) . . . . ?
C4 C5 C6 C7 173.97(19) . . . . ?
C4 C17 C18 C19 -179.79(16) . . . . ?
C4 C17 C22 C21 -179.64(17) . . . . ?
C5 C4 C17 C18 139.49(18) . . . . ?
C5 C4 C17 C22 -39.6(3) . . . . ?
C5 C6 C7 C8 -0.6(4) . . . . ?
C5 C6 C7 C12 -175.44(19) . . . . ?
C6 C1 C2 C3 3.9(3) . . . . ?
C6 C1 N1 C12 -0.4(2) . . . . ?
C6 C1 N1 C13 -173.12(17) . . . . ?
C6 C7 C8 C9 -173.03(18) . . . . ?
C6 C7 C12 C11 176.69(17) . . . . ?
C6 C7 C12 N1 0.1(2) . . . . ?
C7 C8 C9 C10 -2.6(3) . . . . ?
C7 C8 C9 C25 175.52(17) . . . . ?
C7 C12 N1 C1 0.2(2) . . . . ?
C7 C12 N1 C13 173.17(16) . . . . ?
C8 C7 C12 C11 1.0(3) . . . . ?
C8 C7 C12 N1 -175.61(16) . . . . ?
C8 C9 C10 C11 1.6(3) . . . . ?
C8 C9 C25 C26 154.58(17) . . . . ?
C8 C9 C25 C30 -25.6(3) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C9 C25 C26 C27 -179.39(17) . . . . ?
C9 C25 C30 C29 177.88(17) . . . . ?
C10 C9 C25 C26 -27.3(3) . . . . ?
C10 C9 C25 C30 152.46(18) . . . . ?
C10 C11 C12 C7 -2.0(3) . . . . ?
C10 C11 C12 N1 173.83(18) . . . . ?
C11 C12 N1 C1 -176.05(19) . . . . ?
C11 C12 N1 C13 -3.1(3) . . . . ?
C12 C7 C8 C9 1.4(3) . . . . ?
C14 C13 C15 C14 -0.7(3) . . . 2_565 ?
C14 C13 N1 C1 50.8(2) . . . . ?
C14 C13 N1 C12 -120.83(19) . . . . ?
C15 C13 C14 C15 0.7(3) . . . 2_565 ?
C15 C13 C14 C16 -174.98(16) . . . . ?
C15 C13 N1 C1 -130.56(19) . . . . ?
C15 C13 N1 C12 57.8(2) . . . . ?
C17 C4 C5 C6 -176.38(16) . . . . ?
C17 C18 C19 C20 -0.7(3) . . . . ?
C17 C18 C19 O1 179.45(17) . . . . ?
C18 C17 C22 C21 1.3(3) . . . . ?
C18 C19 C20 C21 1.5(3) . . . . ?
C18 C19 C20 O2 -177.93(16) . . . . ?
C18 C19 O1 C23 8.1(3) . . . . ?
C19 C20 C21 C22 -0.9(3) . . . . ?
C19 C20 O2 C24 -173.53(17) . . . . ?
C20 C19 O1 C23 -171.8(2) . . . . ?
C20 C21 C22 C17 -0.5(3) . . . . ?
C21 C20 O2 C24 7.1(3) . . . . ?
C22 C17 C18 C19 -0.7(3) . . . . ?
C25 C9 C10 C11 -176.48(18) . . . . ?
C25 C26 C27 C28 1.5(3) . . . . ?
C25 C26 C27 O3 -179.73(17) . . . . ?
C26 C25 C30 C29 -2.3(3) . . . . ?
C26 C27 C28 C29 -2.4(3) . . . . ?
C26 C27 C28 O4 177.72(17) . . . . ?
C26 C27 O3 C31 1.0(3) . . . . ?
C27 C28 C29 C30 0.9(3) . . . . ?
C27 C28 O4 C32 -172.48(18) . . . . ?
C28 C27 O3 C31 179.81(18) . . . . ?
C28 C29 C30 C25 1.5(3) . . . . ?
C29 C28 O4 C32 7.6(3) . . . . ?
C30 C25 C26 C27 0.8(3) . . . . ?
N1 C1 C2 C3 -174.98(18) . . . . ?
N1 C1 C6 C5 176.32(16) . . . . ?
N1 C1 C6 C7 0.4(2) . . . . ?
N1 C13 C14 C15 179.35(15) . . . 2_565 ?
N1 C13 C14 C16 3.6(3) . . . . ?
N1 C13 C15 C14 -179.37(15) . . . 2_565 ?
O1 C19 C20 C21 -178.61(16) . . . . ?
O1 C19 C20 O2 2.0(2) . . . . ?
O2 C20 C21 C22 178.42(17) . . . . ?
O3 C27 C28 C29 178.75(17) . . . . ?
O3 C27 C28 O4 -1.2(2) . . . . ?
O4 C28 C29 C30 -179.20(18) . . . . ?

_olex2_date_sample_data_collection 2020-03-13
_olex2_date_sample_submission    2020-03-04
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id SAY-070
_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 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.769

###END
