# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Audit and citation data items may have been added by the CCDC. 
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data_mo_kz022_0m
_database_code_depnum_ccdc_archive 'CCDC 1563641'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_audit_creation_date             2017-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2014-3
# start Validation Reply Form
_vrf_THETM01_mo_kz022_0m         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Very small crystal did not diffract significantly past d = 1.0.
          Cut-off was required to achieve solution. Other fractions of
          the data including full data were attempted for refinement but
          resulted in very high residuals. Final model clearly provides
          good connectivity map and makes chemical sense.
;
_vrf_PLAT410_mo_kz022_0m         
;
PROBLEM: Short Intra H...H Contact H76B .. H78 . 1.76 Ang.
RESPONSE: Close contact between crown ether Hs due to
          high thermal motion of interlcoked macroycle.
;
_vrf_PLAT234_mo_kz022_0m         
;
PROBLEM: Large Hirshfeld Difference O3 -- C74 .. 0.27 Ang.
RESPONSE:Due to high thermal motion of interlcoked macroycle
          and possible disorder (not modeled) of ethylene linkage.
;
_vrf_PLAT241_mo_kz022_0m         
;
PROBLEM: High ?MainMol? Ueq as Compared to Neighbors of O1 Check
RESPONSE: Due to high thermal motion of interlcoked macroycle
          and possible disorder (not modeled).
;
_vrf_PLAT242_mo_kz022_0m         
;
PROBLEM: Low ?MainMol? Ueq as Compared to Neighbors of C86 Check
RESPONSE: Due to reltive high thermal motion of interlcoked macroycle.
;
_vrf_PLAT340_mo_kz022_0m         
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01617 Ang.
RESPONSE: Due to very weak diffraction and lack of good high angle data.
;
_vrf_PLAT360_mo_kz022_0m         
;
PROBLEM: Short C(sp3)-C(sp3) Bond C71 - C72 .. 1.32 Ang.
RESPONSE: Due to high thermal motion of interlcoked macroycle
          and possible disorder (not modeled) of ethylene chain.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H64 N4, C24 H32 O8, 2(C3 H7 N O)'
_chemical_formula_sum            'C94 H110 N6 O10'
_chemical_formula_weight         1483.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   14.3220(13)
_cell_length_b                   15.9818(16)
_cell_length_c                   20.0611(16)
_cell_angle_alpha                107.703(4)
_cell_angle_beta                 90.106(4)
_cell_angle_gamma                110.238(4)
_cell_volume                     4074.8(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5727
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.887
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0846 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9035.
The λ/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_av_unetI/netI     0.1148
_diffrn_reflns_Laue_measured_fraction_full 0.578
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40316
_diffrn_reflns_point_group_measured_fraction_full 0.578
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         2.795
_diffrn_ambient_temperature      173.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.578
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4295
_reflns_number_total             8510
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         8510
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.2001
_refine_ls_R_factor_gt           0.1040
_refine_ls_restrained_S_all      1.024
_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)+(0.0694P)²+20.5414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2713
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C4S \\sim N2S \\sim C6S \\sim O2S \\sim C5S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O1S \\sim C3S \\sim N1S \\sim C2S \\sim C1S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O2S) \\sim Ueq, Uanis(C6S) \\sim Ueq, Uanis(N2S) \\sim Ueq, Uanis(C5S)
\\sim Ueq, Uanis(C4S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(O1S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(N1S) \\sim Ueq, Uanis(C2S)
\\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C3) = Uanis(C3A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
3. Same fragment restrains
{C4, C3A, C2A, C1A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C4, C3, C2, C1}
4. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B),
 C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B)
5.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC),
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16),
 C18(H18), C19(H19), C21(H21), C22(H22), C29(H29), C30(H30), C32(H32), C34(H34),
  C35(H35), C37(H37), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50),
 C51(H51), C56(H56), C57(H57), C59(H59), C60(H60), C66(H66), C67(H67), C68(H68),
  C69(H69), C78(H78), C79(H79), C80(H80), C81(H81), C3S(H3S), C6S(H6S)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C3A(H3AA,H3AB,H3AC),
 C2A(H2AA,H2AB,H2AC), C1A(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.9093(5) 0.3629(5) 0.7394(3) 0.0317(18) Uani 1 1 d . . . . .
N2 N 0.7428(5) 0.3042(5) 0.7376(3) 0.0334(18) Uani 1 1 d . . . . .
H2 H 0.6787 0.2791 0.7212 0.040 Uiso 1 1 calc R . . . .
N3 N 0.7550(5) 0.1909(5) 0.2482(3) 0.0295(18) Uani 1 1 d . . . . .
H3 H 0.8190 0.2129 0.2642 0.035 Uiso 1 1 calc R . . . .
N4 N 0.5888(4) 0.1392(4) 0.2482(3) 0.0251(17) Uani 1 1 d . . . . .
C4 C 1.3872(7) 0.5504(7) 0.8786(5) 0.050(3) Uani 1 1 d D . . . .
C3 C 1.4124(9) 0.4968(10) 0.8113(8) 0.080(5) Uani 0.811(11) 1 d D . P A 1
H3A H 1.3761 0.5010 0.7717 0.120 Uiso 0.811(11) 1 calc GR . P A 1
H3B H 1.3931 0.4306 0.8084 0.120 Uiso 0.811(11) 1 calc GR . P A 1
H3C H 1.4847 0.5234 0.8093 0.120 Uiso 0.811(11) 1 calc GR . P A 1
C2 C 1.4248(9) 0.6530(8) 0.8921(9) 0.070(5) Uani 0.811(11) 1 d D . P A 1
H2A H 1.4980 0.6767 0.8942 0.105 Uiso 0.811(11) 1 calc GR . P A 1
H2B H 1.4055 0.6840 0.9371 0.105 Uiso 0.811(11) 1 calc GR . P A 1
H2C H 1.3960 0.6664 0.8540 0.105 Uiso 0.811(11) 1 calc GR . P A 1
C1 C 1.4400(9) 0.5340(12) 0.9399(8) 0.085(5) Uani 0.811(11) 1 d D . P A 1
H1A H 1.4254 0.4664 0.9293 0.128 Uiso 0.811(11) 1 calc GR . P A 1
H1B H 1.4149 0.5582 0.9843 0.128 Uiso 0.811(11) 1 calc GR . P A 1
H1C H 1.5126 0.5673 0.9442 0.128 Uiso 0.811(11) 1 calc GR . P A 1
C5 C 1.2730(6) 0.5115(7) 0.8780(5) 0.043(3) Uani 1 1 d . . . . .
C6 C 1.2116(8) 0.5304(7) 0.8359(5) 0.061(3) Uani 1 1 d . . . . .
H6 H 1.2412 0.5688 0.8079 0.074 Uiso 1 1 calc R . . . .
C7 C 1.1078(7) 0.4950(7) 0.8334(5) 0.057(3) Uani 1 1 d . . . . .
H7 H 1.0683 0.5096 0.8038 0.068 Uiso 1 1 calc R . . . .
C8 C 1.0615(6) 0.4395(6) 0.8730(4) 0.031(2) Uani 1 1 d . . . . .
C9 C 1.1220(6) 0.4194(6) 0.9145(4) 0.039(2) Uani 1 1 d . . . . .
H9 H 1.0921 0.3799 0.9417 0.047 Uiso 1 1 calc R . . . .
C10 C 1.2254(7) 0.4554(7) 0.9175(4) 0.045(3) Uani 1 1 d . . . . .
H10 H 1.2647 0.4412 0.9475 0.054 Uiso 1 1 calc R . . . .
C11 C 0.9513(6) 0.4012(6) 0.8703(4) 0.030(2) Uani 1 1 d . . . . .
C12 C 0.8870(6) 0.3702(6) 0.8079(4) 0.031(2) Uani 1 1 d . . . . .
C13 C 0.7827(6) 0.3325(6) 0.8069(4) 0.029(2) Uani 1 1 d . . . . .
C14 C 0.7352(6) 0.3229(6) 0.8671(4) 0.029(2) Uani 1 1 d . . . . .
C15 C 0.8008(6) 0.3540(6) 0.9283(4) 0.033(2) Uani 1 1 d . . . . .
H15 H 0.7741 0.3489 0.9708 0.039 Uiso 1 1 calc R . . . .
C16 C 0.9049(6) 0.3925(6) 0.9293(4) 0.032(2) Uani 1 1 d . . . . .
H16 H 0.9458 0.4138 0.9729 0.038 Uiso 1 1 calc R . . . .
C17 C 0.6251(6) 0.2794(6) 0.8642(4) 0.028(2) Uani 1 1 d . . . . .
C18 C 0.5591(7) 0.2957(7) 0.8237(5) 0.063(3) Uani 1 1 d . . . . .
H18 H 0.5845 0.3402 0.7997 0.076 Uiso 1 1 calc R . . . .
C19 C 0.4570(7) 0.2482(8) 0.8177(5) 0.060(3) Uani 1 1 d . . . . .
H19 H 0.4143 0.2596 0.7881 0.072 Uiso 1 1 calc R . . . .
C20 C 0.4150(6) 0.1855(6) 0.8525(4) 0.032(2) Uani 1 1 d . . . . .
C21 C 0.4808(7) 0.1731(7) 0.8948(4) 0.049(3) Uani 1 1 d . . . . .
H21 H 0.4548 0.1309 0.9207 0.059 Uiso 1 1 calc R . . . .
C22 C 0.5833(7) 0.2192(7) 0.9015(4) 0.041(3) Uani 1 1 d . . . . .
H22 H 0.6256 0.2092 0.9324 0.049 Uiso 1 1 calc R . . . .
C23 C 0.3015(6) 0.1313(6) 0.8412(4) 0.041(2) Uani 1 1 d . . . . .
C24 C 0.2678(6) 0.0835(7) 0.8965(5) 0.054(3) Uani 1 1 d . . . . .
H24A H 0.3036 0.0409 0.8955 0.081 Uiso 1 1 calc R . . . .
H24B H 0.2825 0.1314 0.9432 0.081 Uiso 1 1 calc R . . . .
H24C H 0.1955 0.0474 0.8864 0.081 Uiso 1 1 calc R . . . .
C25 C 0.2459(7) 0.1967(8) 0.8432(6) 0.070(3) Uani 1 1 d . . . . .
H25A H 0.2672 0.2278 0.8076 0.105 Uiso 1 1 calc R . . . .
H25B H 0.1736 0.1604 0.8332 0.105 Uiso 1 1 calc R . . . .
H25C H 0.2607 0.2444 0.8900 0.105 Uiso 1 1 calc R . . . .
C26 C 0.2764(8) 0.0540(8) 0.7692(5) 0.091(4) Uani 1 1 d . . . . .
H26A H 0.3129 0.0120 0.7685 0.137 Uiso 1 1 calc R . . . .
H26B H 0.2042 0.0176 0.7607 0.137 Uiso 1 1 calc R . . . .
H26C H 0.2961 0.0829 0.7323 0.137 Uiso 1 1 calc R . . . .
C27 C 0.8200(6) 0.3221(6) 0.6999(4) 0.029(2) Uani 1 1 d . . . . .
C28 C 0.8087(7) 0.2975(6) 0.6222(4) 0.031(2) Uani 1 1 d . . . . .
C29 C 0.8939(6) 0.3044(6) 0.5868(4) 0.039(2) Uani 1 1 d . . . . .
H29 H 0.9577 0.3264 0.6132 0.046 Uiso 1 1 calc R . . . .
C30 C 0.8865(6) 0.2798(6) 0.5147(4) 0.040(2) Uani 1 1 d . . . . .
H30 H 0.9450 0.2840 0.4916 0.048 Uiso 1 1 calc R . . . .
C31 C 0.7924(6) 0.2484(6) 0.4746(4) 0.029(2) Uani 1 1 d . . . . .
C32 C 0.7811(6) 0.2236(6) 0.4011(4) 0.032(2) Uani 1 1 d . . . . .
H32 H 0.8382 0.2261 0.3766 0.038 Uiso 1 1 calc R . . . .
C33 C 0.6887(6) 0.1955(6) 0.3634(4) 0.028(2) Uani 1 1 d . . . . .
C34 C 0.6044(6) 0.1918(6) 0.3998(4) 0.042(3) Uani 1 1 d . . . . .
H34 H 0.5408 0.1737 0.3742 0.050 Uiso 1 1 calc R . . . .
C35 C 0.6127(6) 0.2136(6) 0.4711(4) 0.037(2) Uani 1 1 d . . . . .
H35 H 0.5544 0.2092 0.4945 0.044 Uiso 1 1 calc R . . . .
C36 C 0.7067(6) 0.2430(5) 0.5110(4) 0.027(2) Uani 1 1 d . . . . .
C37 C 0.7174(6) 0.2666(6) 0.5844(4) 0.034(2) Uani 1 1 d . . . . .
H37 H 0.6596 0.2608 0.6084 0.041 Uiso 1 1 calc R . . . .
C38 C 0.6768(6) 0.1738(6) 0.2864(4) 0.027(2) Uani 1 1 d . . . . .
C39 C 1.2299(7) 0.4423(7) 0.1320(5) 0.060(3) Uani 1 1 d . . . . .
H39A H 1.2171 0.4707 0.1801 0.090 Uiso 1 1 calc R . . . .
H39B H 1.3020 0.4664 0.1288 0.090 Uiso 1 1 calc R . . . .
H39C H 1.1946 0.4585 0.0988 0.090 Uiso 1 1 calc R . . . .
C40 C 1.2527(7) 0.3132(7) 0.1650(5) 0.065(3) Uani 1 1 d . . . . .
H40A H 1.2297 0.2448 0.1543 0.098 Uiso 1 1 calc R . . . .
H40B H 1.3240 0.3377 0.1595 0.098 Uiso 1 1 calc R . . . .
H40C H 1.2426 0.3426 0.2136 0.098 Uiso 1 1 calc R . . . .
C41 C 1.2117(7) 0.2906(7) 0.0397(5) 0.062(3) Uani 1 1 d . . . . .
H41A H 1.1872 0.2220 0.0288 0.092 Uiso 1 1 calc R . . . .
H41B H 1.1763 0.3062 0.0061 0.092 Uiso 1 1 calc R . . . .
H41C H 1.2838 0.3141 0.0361 0.092 Uiso 1 1 calc R . . . .
C42 C 1.1926(6) 0.3362(6) 0.1141(4) 0.035(2) Uani 1 1 d . . . . .
C43 C 1.0801(6) 0.2956(6) 0.1188(4) 0.029(2) Uani 1 1 d . . . . .
C44 C 1.0150(6) 0.3231(6) 0.0874(4) 0.037(2) Uani 1 1 d . . . . .
H44 H 1.0417 0.3701 0.0656 0.045 Uiso 1 1 calc R . . . .
C45 C 0.9121(6) 0.2844(6) 0.0865(4) 0.037(2) Uani 1 1 d . . . . .
H45 H 0.8701 0.3042 0.0631 0.045 Uiso 1 1 calc R . . . .
C46 C 0.8691(6) 0.2172(6) 0.1189(4) 0.029(2) Uani 1 1 d . . . . .
C47 C 0.9338(6) 0.1895(6) 0.1509(4) 0.038(2) Uani 1 1 d . . . . .
H47 H 0.9072 0.1428 0.1730 0.045 Uiso 1 1 calc R . . . .
C48 C 1.0367(6) 0.2286(6) 0.1514(4) 0.037(2) Uani 1 1 d . . . . .
H48 H 1.0788 0.2089 0.1747 0.044 Uiso 1 1 calc R . . . .
C49 C 0.7592(6) 0.1775(5) 0.1190(4) 0.026(2) Uani 1 1 d . . . . .
C50 C 0.6937(6) 0.1484(6) 0.0590(4) 0.030(2) Uani 1 1 d . . . . .
H50 H 0.7203 0.1515 0.0161 0.036 Uiso 1 1 calc R . . . .
C51 C 0.5898(6) 0.1143(6) 0.0588(4) 0.029(2) Uani 1 1 d . . . . .
H51 H 0.5483 0.0972 0.0161 0.035 Uiso 1 1 calc R . . . .
C52 C 0.5444(6) 0.1045(5) 0.1189(4) 0.026(2) Uani 1 1 d . . . . .
C53 C 0.6111(6) 0.1337(6) 0.1803(4) 0.027(2) Uani 1 1 d . . . . .
C54 C 0.7150(6) 0.1671(6) 0.1792(4) 0.027(2) Uani 1 1 d . . . . .
C55 C 0.4336(6) 0.0661(6) 0.1167(4) 0.026(2) Uani 1 1 d . . . . .
C56 C 0.3707(7) 0.0880(6) 0.0797(4) 0.037(2) Uani 1 1 d . . . . .
H56 H 0.3983 0.1307 0.0545 0.044 Uiso 1 1 calc R . . . .
C57 C 0.2678(6) 0.0496(6) 0.0780(4) 0.036(2) Uani 1 1 d . . . . .
H57 H 0.2269 0.0669 0.0515 0.044 Uiso 1 1 calc R . . . .
C58 C 0.2220(6) -0.0132(6) 0.1135(4) 0.027(2) Uani 1 1 d . . . . .
C59 C 0.2861(6) -0.0365(6) 0.1500(4) 0.040(2) Uani 1 1 d . . . . .
H59 H 0.2589 -0.0805 0.1743 0.047 Uiso 1 1 calc R . . . .
C60 C 0.3887(7) 0.0029(7) 0.1519(4) 0.041(3) Uani 1 1 d . . . . .
H60 H 0.4302 -0.0141 0.1782 0.049 Uiso 1 1 calc R . . . .
C61 C 0.1087(6) -0.0529(6) 0.1150(4) 0.035(2) Uani 1 1 d . . . . .
C62 C 0.0851(7) 0.0056(6) 0.1839(4) 0.048(3) Uani 1 1 d . . . . .
H62A H 0.1084 0.0719 0.1863 0.072 Uiso 1 1 calc R . . . .
H62B H 0.0125 -0.0175 0.1859 0.072 Uiso 1 1 calc R . . . .
H62C H 0.1191 0.0000 0.2239 0.072 Uiso 1 1 calc R . . . .
C63 C 0.0731(7) -0.1565(6) 0.1101(5) 0.051(3) Uani 1 1 d . . . . .
H63A H 0.0004 -0.1805 0.1111 0.076 Uiso 1 1 calc R . . . .
H63B H 0.0896 -0.1929 0.0659 0.076 Uiso 1 1 calc R . . . .
H63C H 0.1065 -0.1627 0.1500 0.076 Uiso 1 1 calc R . . . .
C64 C 0.0527(6) -0.0457(7) 0.0523(5) 0.059(3) Uani 1 1 d . . . . .
H64A H 0.0744 0.0204 0.0543 0.089 Uiso 1 1 calc R . . . .
H64B H 0.0678 -0.0829 0.0079 0.089 Uiso 1 1 calc R . . . .
H64C H -0.0196 -0.0699 0.0548 0.089 Uiso 1 1 calc R . . . .
O1 O 1.1211(7) 0.3494(8) 0.6582(8) 0.188(7) Uani 1 1 d . . . . .
O2 O 0.9868(7) 0.1662(6) 0.6519(5) 0.108(3) Uani 1 1 d . . . . .
O3 O 0.7337(8) 0.0944(7) 0.6741(5) 0.115(3) Uani 1 1 d . . . . .
O4 O 0.5467(6) 0.1434(6) 0.6689(6) 0.109(3) Uani 1 1 d . . . . .
O5 O 0.5166(6) 0.2891(6) 0.6565(5) 0.084(2) Uani 1 1 d . . . . .
O6 O 0.6791(10) 0.4613(8) 0.6524(8) 0.169(6) Uani 1 1 d . . . . .
O7 O 0.8925(12) 0.5886(10) 0.6585(7) 0.199(7) Uani 1 1 d . . . . .
O8 O 1.0841(8) 0.5008(7) 0.6648(6) 0.110(3) Uani 1 1 d . . . . .
C65 C 1.1619(14) 0.4867(10) 0.6316(9) 0.100(5) Uani 1 1 d . . . . .
C66 C 1.2247(17) 0.5530(13) 0.6033(10) 0.138(6) Uani 1 1 d . . . . .
H66 H 1.2127 0.6090 0.6072 0.166 Uiso 1 1 calc R . . . .
C67 C 1.3049(18) 0.5369(15) 0.5696(10) 0.160(8) Uani 1 1 d . . . . .
H67 H 1.3441 0.5822 0.5494 0.192 Uiso 1 1 calc R . . . .
C68 C 1.3304(15) 0.4630(16) 0.5637(10) 0.141(7) Uani 1 1 d . . . . .
H68 H 1.3866 0.4552 0.5412 0.169 Uiso 1 1 calc R . . . .
C69 C 1.2684(16) 0.3967(13) 0.5931(13) 0.168(10) Uani 1 1 d . . . . .
H69 H 1.2825 0.3418 0.5902 0.201 Uiso 1 1 calc R . . . .
C70 C 1.1870(13) 0.4099(10) 0.6263(11) 0.131(8) Uani 1 1 d . . . . .
C71 C 1.1437(10) 0.2858(12) 0.6756(9) 0.127(6) Uani 1 1 d . . . . .
H71A H 1.1999 0.3193 0.7141 0.152 Uiso 1 1 calc R . . . .
H71B H 1.1692 0.2512 0.6346 0.152 Uiso 1 1 calc R . . . .
C72 C 1.0735(11) 0.2227(11) 0.6959(11) 0.164(9) Uani 1 1 d . . . . .
H72A H 1.0547 0.2568 0.7407 0.197 Uiso 1 1 calc R . . . .
H72B H 1.1044 0.1809 0.7068 0.197 Uiso 1 1 calc R . . . .
C73 C 0.9080(14) 0.1373(11) 0.6810(9) 0.120(5) Uani 1 1 d . . . . .
H73A H 0.9028 0.1939 0.7160 0.144 Uiso 1 1 calc R . . . .
H73B H 0.9215 0.0994 0.7081 0.144 Uiso 1 1 calc R . . . .
C74 C 0.8140(12) 0.0855(10) 0.6441(10) 0.126(6) Uani 1 1 d . . . . .
H74A H 0.8132 0.1010 0.6000 0.151 Uiso 1 1 calc R . . . .
H74B H 0.8056 0.0181 0.6304 0.151 Uiso 1 1 calc R . . . .
C75 C 0.6430(11) 0.0488(11) 0.6600(9) 0.124(6) Uani 1 1 d . . . . .
H75A H 0.6350 -0.0110 0.6686 0.149 Uiso 1 1 calc R . . . .
H75B H 0.6308 0.0322 0.6082 0.149 Uiso 1 1 calc R . . . .
C76 C 0.5632(11) 0.0672(10) 0.6831(10) 0.151(8) Uani 1 1 d . . . . .
H76A H 0.5687 0.0804 0.7347 0.182 Uiso 1 1 calc R . . . .
H76B H 0.5031 0.0096 0.6621 0.182 Uiso 1 1 calc R . . . .
C77 C 0.4663(10) 0.1235(10) 0.6234(7) 0.068(3) Uani 1 1 d . . . . .
C78 C 0.4011(13) 0.0385(13) 0.5874(7) 0.102(5) Uani 1 1 d . . . . .
H78 H 0.4139 -0.0142 0.5918 0.123 Uiso 1 1 calc R . . . .
C79 C 0.3192(16) 0.0207(11) 0.5457(9) 0.157(8) Uani 1 1 d . . . . .
H79 H 0.2742 -0.0419 0.5224 0.188 Uiso 1 1 calc R . . . .
C80 C 0.3028(15) 0.1001(14) 0.5379(8) 0.168(9) Uani 1 1 d . . . . .
H80 H 0.2467 0.0918 0.5078 0.202 Uiso 1 1 calc R . . . .
C81 C 0.3688(11) 0.1889(10) 0.5743(7) 0.093(4) Uani 1 1 d . . . . .
H81 H 0.3577 0.2419 0.5690 0.112 Uiso 1 1 calc R . . . .
C82 C 0.4491(9) 0.2031(10) 0.6176(6) 0.064(3) Uani 1 1 d . . . . .
C83 C 0.5102(11) 0.3701(10) 0.6445(7) 0.092(4) Uani 1 1 d . . . . .
H83A H 0.4477 0.3790 0.6601 0.111 Uiso 1 1 calc R . . . .
H83B H 0.5095 0.3625 0.5936 0.111 Uiso 1 1 calc R . . . .
C84 C 0.5954(15) 0.4496(11) 0.6836(9) 0.129(6) Uani 1 1 d . . . . .
H84A H 0.5791 0.5072 0.6926 0.155 Uiso 1 1 calc R . . . .
H84B H 0.6085 0.4430 0.7299 0.155 Uiso 1 1 calc R . . . .
C85 C 0.7212(18) 0.5131(13) 0.6270(11) 0.183(10) Uani 1 1 d . . . . .
H85A H 0.7237 0.5748 0.6593 0.219 Uiso 1 1 calc R . . . .
H85B H 0.6763 0.4997 0.5845 0.219 Uiso 1 1 calc R . . . .
C86 C 0.8176(15) 0.5305(13) 0.6050(9) 0.130(6) Uani 1 1 d . . . . .
H86A H 0.8272 0.4698 0.5848 0.156 Uiso 1 1 calc R . . . .
H86B H 0.8222 0.5595 0.5674 0.156 Uiso 1 1 calc R . . . .
C87 C 0.957(2) 0.5628(14) 0.6800(13) 0.189(11) Uani 1 1 d . . . . .
H87A H 0.9204 0.4974 0.6794 0.227 Uiso 1 1 calc R . . . .
H87B H 0.9778 0.6018 0.7301 0.227 Uiso 1 1 calc R . . . .
C88 C 1.0395(17) 0.5630(12) 0.6514(13) 0.198(11) Uani 1 1 d . . . . .
H88A H 1.0896 0.6281 0.6687 0.237 Uiso 1 1 calc R . . . .
H88B H 1.0247 0.5460 0.5997 0.237 Uiso 1 1 calc R . . . .
O1S O 0.9438(7) 0.1700(9) 0.3025(5) 0.145(5) Uani 1 1 d . U . . .
N1S N 1.0302(12) 0.1465(14) 0.3902(8) 0.159(6) Uani 1 1 d . U . . .
C1S C 1.1103(17) 0.1817(19) 0.4403(12) 0.304(16) Uani 1 1 d . U . . .
H1SA H 1.1009 0.1402 0.4690 0.456 Uiso 1 1 calc R . . . .
H1SB H 1.1714 0.1853 0.4175 0.456 Uiso 1 1 calc R . . . .
H1SC H 1.1164 0.2449 0.4704 0.456 Uiso 1 1 calc R . . . .
C2S C 0.9550(18) 0.0641(14) 0.3984(14) 0.244(14) Uani 1 1 d . U . . .
H2SA H 0.9795 0.0482 0.4368 0.366 Uiso 1 1 calc R . . . .
H2SB H 0.8936 0.0768 0.4095 0.366 Uiso 1 1 calc R . . . .
H2SC H 0.9407 0.0111 0.3545 0.366 Uiso 1 1 calc R . . . .
C3S C 1.0164(13) 0.1821(17) 0.3429(10) 0.177(8) Uani 1 1 d . U . . .
H3S H 1.0762 0.2287 0.3379 0.212 Uiso 1 1 calc R . . . .
O2S O 0.3818(15) 0.2866(16) 0.4419(9) 0.254(9) Uani 1 1 d . U . . .
N2S N 0.3963(14) 0.2623(13) 0.3322(7) 0.139(6) Uani 1 1 d . U . . .
C4S C 0.4664(17) 0.3063(15) 0.2875(10) 0.194(9) Uani 1 1 d . U . . .
H4SA H 0.4473 0.2658 0.2382 0.291 Uiso 1 1 calc R . . . .
H4SB H 0.4635 0.3681 0.2922 0.291 Uiso 1 1 calc R . . . .
H4SC H 0.5348 0.3140 0.3028 0.291 Uiso 1 1 calc R . . . .
C5S C 0.3311(17) 0.1729(14) 0.3013(9) 0.260(15) Uani 1 1 d . U . . .
H5SA H 0.3323 0.1551 0.2502 0.389 Uiso 1 1 calc R . . . .
H5SB H 0.3506 0.1299 0.3192 0.389 Uiso 1 1 calc R . . . .
H5SC H 0.2634 0.1689 0.3122 0.389 Uiso 1 1 calc R . . . .
C6S C 0.417(2) 0.311(2) 0.3959(14) 0.193(9) Uani 1 1 d . U . . .
H6S H 0.4653 0.3726 0.4075 0.231 Uiso 1 1 calc R . . . .
C3A C 1.434(4) 0.619(4) 0.9493(17) 0.080(5) Uani 0.189(11) 1 d D . P A 2
H3AA H 1.4577 0.5881 0.9772 0.120 Uiso 0.189(11) 1 calc GR . P A 2
H3AB H 1.3844 0.6432 0.9734 0.120 Uiso 0.189(11) 1 calc GR . P A 2
H3AC H 1.4908 0.6718 0.9440 0.120 Uiso 0.189(11) 1 calc GR . P A 2
C2A C 1.429(4) 0.476(3) 0.855(3) 0.070(5) Uani 0.189(11) 1 d D . P A 2
H2AA H 1.4001 0.4358 0.8065 0.105 Uiso 0.189(11) 1 calc GR . P A 2
H2AB H 1.4140 0.4369 0.8860 0.105 Uiso 0.189(11) 1 calc GR . P A 2
H2AC H 1.5023 0.5042 0.8564 0.105 Uiso 0.189(11) 1 calc GR . P A 2
C1A C 1.419(4) 0.609(4) 0.825(3) 0.085(5) Uani 0.189(11) 1 d D . P A 2
H1AA H 1.4922 0.6347 0.8275 0.128 Uiso 0.189(11) 1 calc GR . P A 2
H1AB H 1.3934 0.6604 0.8371 0.128 Uiso 0.189(11) 1 calc GR . P A 2
H1AC H 1.3906 0.5669 0.7767 0.128 Uiso 0.189(11) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C12 1.391(9) . ?
N1 C27 1.340(9) . ?
N2 C13 1.378(9) . ?
N2 C27 1.339(10) . ?
N3 C38 1.354(9) . ?
N3 C54 1.384(9) . ?
N4 C38 1.318(9) . ?
N4 C53 1.384(9) . ?
C4 C3 1.484(15) . ?
C4 C2 1.472(14) . ?
C4 C1 1.575(15) . ?
C4 C5 1.533(12) . ?
C4 C3A 1.49(2) . ?
C4 C2A 1.48(2) . ?
C4 C1A 1.60(2) . ?
C5 C6 1.384(12) . ?
C5 C10 1.381(12) . ?
C6 C7 1.389(12) . ?
C7 C8 1.372(12) . ?
C8 C9 1.378(11) . ?
C8 C11 1.477(11) . ?
C9 C10 1.384(11) . ?
C11 C12 1.402(10) . ?
C11 C16 1.379(11) . ?
C12 C13 1.402(11) . ?
C13 C14 1.410(11) . ?
C14 C15 1.393(10) . ?
C14 C17 1.479(11) . ?
C15 C16 1.400(11) . ?
C17 C18 1.384(11) . ?
C17 C22 1.374(11) . ?
C18 C19 1.380(12) . ?
C19 C20 1.365(12) . ?
C20 C21 1.372(11) . ?
C20 C23 1.532(12) . ?
C21 C22 1.381(11) . ?
C23 C24 1.520(12) . ?
C23 C25 1.510(12) . ?
C23 C26 1.532(12) . ?
C27 C28 1.482(10) . ?
C28 C29 1.400(11) . ?
C28 C37 1.360(11) . ?
C29 C30 1.373(10) . ?
C30 C31 1.414(10) . ?
C31 C32 1.399(10) . ?
C31 C36 1.420(10) . ?
C32 C33 1.380(10) . ?
C33 C34 1.404(11) . ?
C33 C38 1.474(10) . ?
C34 C35 1.360(10) . ?
C35 C36 1.417(10) . ?
C36 C37 1.398(10) . ?
C39 C42 1.515(12) . ?
C40 C42 1.535(11) . ?
C41 C42 1.521(11) . ?
C42 C43 1.530(11) . ?
C43 C44 1.382(10) . ?
C43 C48 1.388(11) . ?
C44 C45 1.383(11) . ?
C45 C46 1.386(11) . ?
C46 C47 1.387(11) . ?
C46 C49 1.480(11) . ?
C47 C48 1.386(11) . ?
C49 C50 1.378(10) . ?
C49 C54 1.393(10) . ?
C50 C51 1.397(10) . ?
C51 C52 1.397(10) . ?
C52 C53 1.408(10) . ?
C52 C55 1.485(11) . ?
C53 C54 1.399(10) . ?
C55 C56 1.362(10) . ?
C55 C60 1.385(11) . ?
C56 C57 1.383(11) . ?
C57 C58 1.389(11) . ?
C58 C59 1.385(10) . ?
C58 C61 1.527(11) . ?
C59 C60 1.379(11) . ?
C61 C62 1.529(11) . ?
C61 C63 1.526(12) . ?
C61 C64 1.546(11) . ?
O1 C70 1.41(2) . ?
O1 C71 1.303(15) . ?
O2 C72 1.368(14) . ?
O2 C73 1.278(17) . ?
O3 C74 1.330(16) . ?
O3 C75 1.232(14) . ?
O4 C76 1.424(13) . ?
O4 C77 1.351(13) . ?
O5 C82 1.364(13) . ?
O5 C83 1.420(12) . ?
O6 C84 1.335(17) . ?
O6 C85 1.103(17) . ?
O7 C86 1.366(18) . ?
O7 C87 1.250(19) . ?
O8 C65 1.349(18) . ?
O8 C88 1.438(19) . ?
C65 C66 1.40(2) . ?
C65 C70 1.369(19) . ?
C66 C67 1.39(2) . ?
C67 C68 1.33(2) . ?
C68 C69 1.41(2) . ?
C69 C70 1.39(2) . ?
C71 C72 1.321(19) . ?
C73 C74 1.378(18) . ?
C75 C76 1.327(17) . ?
C77 C78 1.328(17) . ?
C77 C82 1.414(15) . ?
C78 C79 1.333(19) . ?
C79 C80 1.421(19) . ?
C80 C81 1.371(18) . ?
C81 C82 1.350(15) . ?
C83 C84 1.428(17) . ?
C85 C86 1.41(2) . ?
C87 C88 1.32(2) . ?
O1S C3S 1.241(17) . ?
N1S C1S 1.359(19) . ?
N1S C2S 1.44(2) . ?
N1S C3S 1.29(2) . ?
O2S C6S 1.15(2) . ?
N2S C4S 1.49(2) . ?
N2S C5S 1.35(2) . ?
N2S C6S 1.25(3) . ?

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
C27 N1 C12 104.6(6) . . ?
C27 N2 C13 107.0(6) . . ?
C38 N3 C54 106.9(6) . . ?
C38 N4 C53 104.6(6) . . ?
C3 C4 C1 107.2(10) . . ?
C3 C4 C5 108.2(8) . . ?
C2 C4 C3 113.6(9) . . ?
C2 C4 C1 106.6(9) . . ?
C2 C4 C5 110.8(9) . . ?
C5 C4 C1 110.3(9) . . ?
C5 C4 C1A 111(2) . . ?
C3A C4 C5 109(2) . . ?
C3A C4 C1A 105.4(17) . . ?
C2A C4 C5 113(2) . . ?
C2A C4 C3A 113.2(18) . . ?
C2A C4 C1A 104.5(17) . . ?
C6 C5 C4 120.7(9) . . ?
C10 C5 C4 123.2(9) . . ?
C10 C5 C6 116.2(8) . . ?
C5 C6 C7 122.0(9) . . ?
C8 C7 C6 121.2(9) . . ?
C7 C8 C9 117.2(9) . . ?
C7 C8 C11 121.5(8) . . ?
C9 C8 C11 121.3(8) . . ?
C8 C9 C10 121.5(9) . . ?
C5 C10 C9 121.9(9) . . ?
C12 C11 C8 122.5(7) . . ?
C16 C11 C8 121.9(7) . . ?
C16 C11 C12 115.6(8) . . ?
N1 C12 C11 129.8(8) . . ?
N1 C12 C13 108.9(7) . . ?
C13 C12 C11 121.1(8) . . ?
N2 C13 C12 106.2(7) . . ?
N2 C13 C14 130.3(8) . . ?
C12 C13 C14 123.4(7) . . ?
C13 C14 C17 122.4(7) . . ?
C15 C14 C13 114.3(7) . . ?
C15 C14 C17 123.3(8) . . ?
C14 C15 C16 122.3(8) . . ?
C11 C16 C15 123.4(7) . . ?
C18 C17 C14 122.6(8) . . ?
C22 C17 C14 120.9(8) . . ?
C22 C17 C18 116.5(8) . . ?
C19 C18 C17 121.1(9) . . ?
C20 C19 C18 122.7(9) . . ?
C19 C20 C21 115.6(8) . . ?
C19 C20 C23 120.5(8) . . ?
C21 C20 C23 123.8(8) . . ?
C20 C21 C22 122.9(9) . . ?
C17 C22 C21 121.0(8) . . ?
C20 C23 C26 107.6(7) . . ?
C24 C23 C20 111.8(7) . . ?
C24 C23 C26 107.7(8) . . ?
C25 C23 C20 110.5(8) . . ?
C25 C23 C24 109.0(8) . . ?
C25 C23 C26 110.3(8) . . ?
N1 C27 C28 122.9(8) . . ?
N2 C27 N1 113.3(6) . . ?
N2 C27 C28 123.8(7) . . ?
C29 C28 C27 119.1(7) . . ?
C37 C28 C27 121.5(8) . . ?
C37 C28 C29 119.4(7) . . ?
C30 C29 C28 121.1(7) . . ?
C29 C30 C31 120.3(8) . . ?
C30 C31 C36 118.2(6) . . ?
C32 C31 C30 122.5(7) . . ?
C32 C31 C36 119.3(7) . . ?
C33 C32 C31 121.3(7) . . ?
C32 C33 C34 119.2(7) . . ?
C32 C33 C38 121.7(7) . . ?
C34 C33 C38 119.0(7) . . ?
C35 C34 C33 120.8(7) . . ?
C34 C35 C36 121.2(8) . . ?
C35 C36 C31 118.2(6) . . ?
C37 C36 C31 119.5(7) . . ?
C37 C36 C35 122.3(8) . . ?
C28 C37 C36 121.5(8) . . ?
N3 C38 C33 123.5(7) . . ?
N4 C38 N3 113.4(6) . . ?
N4 C38 C33 123.1(7) . . ?
C39 C42 C40 108.1(7) . . ?
C39 C42 C41 110.3(8) . . ?
C39 C42 C43 111.2(7) . . ?
C41 C42 C40 107.6(8) . . ?
C41 C42 C43 108.3(7) . . ?
C43 C42 C40 111.2(7) . . ?
C44 C43 C42 119.9(8) . . ?
C44 C43 C48 116.2(8) . . ?
C48 C43 C42 123.8(7) . . ?
C43 C44 C45 122.2(8) . . ?
C44 C45 C46 121.4(8) . . ?
C45 C46 C47 116.9(8) . . ?
C45 C46 C49 121.1(8) . . ?
C47 C46 C49 122.0(8) . . ?
C48 C47 C46 121.2(8) . . ?
C47 C48 C43 122.1(8) . . ?
C50 C49 C46 121.8(7) . . ?
C50 C49 C54 115.5(7) . . ?
C54 C49 C46 122.6(7) . . ?
C49 C50 C51 122.5(7) . . ?
C52 C51 C50 122.5(7) . . ?
C51 C52 C53 115.2(7) . . ?
C51 C52 C55 121.2(7) . . ?
C53 C52 C55 123.6(7) . . ?
N4 C53 C52 128.3(7) . . ?
N4 C53 C54 110.2(6) . . ?
C54 C53 C52 121.4(7) . . ?
N3 C54 C49 132.1(8) . . ?
N3 C54 C53 104.9(7) . . ?
C49 C54 C53 122.8(7) . . ?
C56 C55 C52 123.4(8) . . ?
C56 C55 C60 116.3(8) . . ?
C60 C55 C52 120.3(7) . . ?
C55 C56 C57 121.7(8) . . ?
C56 C57 C58 122.5(8) . . ?
C57 C58 C61 123.3(7) . . ?
C59 C58 C57 115.6(7) . . ?
C59 C58 C61 121.1(8) . . ?
C60 C59 C58 121.4(8) . . ?
C59 C60 C55 122.5(8) . . ?
C58 C61 C62 107.7(7) . . ?
C58 C61 C64 110.7(7) . . ?
C62 C61 C64 109.2(7) . . ?
C63 C61 C58 110.8(7) . . ?
C63 C61 C62 110.5(7) . . ?
C63 C61 C64 108.0(7) . . ?
C71 O1 C70 122.2(13) . . ?
C73 O2 C72 116.8(15) . . ?
C75 O3 C74 134.2(15) . . ?
C77 O4 C76 118.3(12) . . ?
C82 O5 C83 117.9(10) . . ?
C85 O6 C84 132.9(19) . . ?
C87 O7 C86 123.1(19) . . ?
C65 O8 C88 121.3(14) . . ?
O8 C65 C66 121.3(16) . . ?
O8 C65 C70 122.6(19) . . ?
C70 C65 C66 116(2) . . ?
C67 C66 C65 120.2(19) . . ?
C68 C67 C66 125(2) . . ?
C67 C68 C69 115(2) . . ?
C70 C69 C68 121.3(17) . . ?
C65 C70 O1 112(2) . . ?
C65 C70 C69 122.3(19) . . ?
C69 C70 O1 126.2(16) . . ?
O1 C71 C72 119.0(14) . . ?
C71 C72 O2 119.6(16) . . ?
O2 C73 C74 123.6(17) . . ?
O3 C74 C73 119.6(17) . . ?
O3 C75 C76 132.9(17) . . ?
C75 C76 O4 117.0(12) . . ?
O4 C77 C82 115.0(12) . . ?
C78 C77 O4 126.7(13) . . ?
C78 C77 C82 118.2(13) . . ?
C77 C78 C79 125.7(16) . . ?
C78 C79 C80 116.5(16) . . ?
C81 C80 C79 119.2(15) . . ?
C82 C81 C80 121.8(14) . . ?
O5 C82 C77 116.3(11) . . ?
C81 C82 O5 125.1(13) . . ?
C81 C82 C77 118.5(13) . . ?
O5 C83 C84 107.8(11) . . ?
O6 C84 C83 114.8(14) . . ?
O6 C85 C86 130(2) . . ?
O7 C86 C85 113.0(17) . . ?
O7 C87 C88 125(2) . . ?
C87 C88 O8 116.1(18) . . ?
C1S N1S C2S 111(2) . . ?
C3S N1S C1S 127(2) . . ?
C3S N1S C2S 121.9(19) . . ?
O1S C3S N1S 135(2) . . ?
C5S N2S C4S 117.2(16) . . ?
C6S N2S C4S 113(2) . . ?
C6S N2S C5S 129(2) . . ?
O2S C6S N2S 126(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
####################################################################### 
# 
# 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_kz71
_database_code_depnum_ccdc_archive 'CCDC 1563644'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_audit_creation_date             2017-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2014-3
# start Validation Reply Form
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H10 Br4 N4, C16 H32 O8'
_chemical_formula_sum            'C36 H42 Br4 N4 O8'
_chemical_formula_weight         978.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.6346(14)
_cell_length_b                   10.1658(15)
_cell_length_c                   11.2070(17)
_cell_angle_alpha                68.379(2)
_cell_angle_beta                 82.740(2)
_cell_angle_gamma                68.992(2)
_cell_volume                     952.6(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6123
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.391
_shelx_estimated_absorpt_T_min   0.238
_exptl_absorpt_coefficient_mu    4.281
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1009 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.27
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (30 s exposure) covering -0.500° degrees in ω.
 The crystal to detector distance was 6.05 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9812
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.955
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3291
_reflns_number_total             3839
_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       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART V5.631 (?, 2016)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0374
_refine_ls_restrained_S_all      1.032
_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)+(0.0533P)²+0.1474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1042
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C016(H01A,H01B), C017(H01C,H01D), C018(H01E,H01F), C021(H02A,H02B), C022(H02C,
 H02D), C024(H02E,H02F), C025(H02G,H02H), C026(H02I,H02J)
2.b Aromatic/amide H refined with riding coordinates:
 N009(H009), C011(H011), C019(H019), C020(H020), C023(H023)
;
_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
Br01 Br 0.96391(3) 0.18592(3) 0.07963(3) 0.03187(12) Uani 1 1 d . . . . .
Br02 Br 0.24534(3) 0.32712(4) 0.05009(3) 0.04362(13) Uani 1 1 d . . . . .
O6 O 0.9581(2) 0.3536(2) 0.3348(2) 0.0296(4) Uani 1 1 d . . . . .
O7 O 0.8046(2) 0.1453(2) 0.53328(19) 0.0312(5) Uani 1 1 d . . . . .
O005 O 0.8527(2) 0.6782(2) 0.31509(19) 0.0302(4) Uani 1 1 d . . . . .
C006 C 0.7571(3) 0.2376(3) 0.0599(3) 0.0259(6) Uani 1 1 d . . . . .
N007 N 0.4347(2) 0.3908(3) 0.2305(2) 0.0253(5) Uani 1 1 d . . . . .
C008 C 0.6601(3) 0.3072(3) 0.1387(3) 0.0232(5) Uani 1 1 d . . . . .
N009 N 0.6788(2) 0.3551(2) 0.2324(2) 0.0226(5) Uani 1 1 d . . . . .
H009 H 0.7611 0.3551 0.2544 0.027 Uiso 1 1 calc R . . . .
C010 C 0.5054(3) 0.3323(3) 0.1375(3) 0.0235(5) Uani 1 1 d . . . . .
C011 C 0.5463(4) 0.2305(4) -0.0314(3) 0.0358(7) Uani 1 1 d . . . . .
H011 H 0.5090 0.2070 -0.0906 0.043 Uiso 1 1 calc R . . . .
C012 C 0.4508(3) 0.2943(3) 0.0499(3) 0.0289(6) Uani 1 1 d . . . . .
C013 C 0.5418(3) 0.4033(3) 0.2848(3) 0.0235(5) Uani 1 1 d . . . . .
O8 O 0.5298(2) 0.8696(2) 0.29352(19) 0.0332(5) Uani 1 1 d . . . . .
C015 C 0.5195(3) 0.4552(3) 0.3937(3) 0.0226(5) Uani 1 1 d . . . . .
C016 C 0.7129(3) 0.1338(3) 0.6435(3) 0.0333(7) Uani 1 1 d . . . . .
H01A H 0.6719 0.2302 0.6555 0.040 Uiso 1 1 calc R . . . .
H01B H 0.7710 0.0608 0.7191 0.040 Uiso 1 1 calc R . . . .
C017 C 0.7853(4) 0.8311(3) 0.2370(3) 0.0360(7) Uani 1 1 d . . . . .
H01C H 0.7521 0.8365 0.1566 0.043 Uiso 1 1 calc R . . . .
H01D H 0.8572 0.8827 0.2178 0.043 Uiso 1 1 calc R . . . .
C018 C 0.9776(3) 0.6008(3) 0.2546(3) 0.0306(6) Uani 1 1 d . . . . .
H01E H 1.0514 0.6501 0.2360 0.037 Uiso 1 1 calc R . . . .
H01F H 0.9465 0.6048 0.1740 0.037 Uiso 1 1 calc R . . . .
C019 C 0.7001(3) 0.2007(3) -0.0254(3) 0.0314(6) Uani 1 1 d . . . . .
H019 H 0.7639 0.1556 -0.0795 0.038 Uiso 1 1 calc R . . . .
C020 C 0.6229(3) 0.5074(3) 0.4218(3) 0.0248(6) Uani 1 1 d . . . . .
H020 H 0.7050 0.5127 0.3692 0.030 Uiso 1 1 calc R . . . .
C021 C 1.0158(3) 0.2021(3) 0.4217(3) 0.0357(7) Uani 1 1 d . . . . .
H02A H 1.1200 0.1784 0.4383 0.043 Uiso 1 1 calc R . . . .
H02B H 1.0094 0.1346 0.3816 0.043 Uiso 1 1 calc R . . . .
C022 C 1.0448(3) 0.4410(3) 0.3386(3) 0.0296(6) Uani 1 1 d . . . . .
H02C H 1.1452 0.3997 0.3104 0.036 Uiso 1 1 calc R . . . .
H02D H 1.0503 0.4358 0.4262 0.036 Uiso 1 1 calc R . . . .
C023 C 0.3966(3) 0.4490(3) 0.4731(3) 0.0240(6) Uani 1 1 d . . . . .
H023 H 0.3270 0.4150 0.4547 0.029 Uiso 1 1 calc R . . . .
C024 C 0.9339(3) 0.1757(3) 0.5472(3) 0.0336(7) Uani 1 1 d . . . . .
H02E H 0.9979 0.0912 0.6140 0.040 Uiso 1 1 calc R . . . .
H02F H 0.9055 0.2639 0.5718 0.040 Uiso 1 1 calc R . . . .
C025 C 0.6552(4) 0.9058(3) 0.3060(3) 0.0360(7) Uani 1 1 d . . . . .
H02G H 0.6799 0.8721 0.3961 0.043 Uiso 1 1 calc R . . . .
H02H H 0.6322 1.0139 0.2702 0.043 Uiso 1 1 calc R . . . .
C026 C 0.5894(3) 0.0854(3) 0.6250(3) 0.0348(7) Uani 1 1 d . . . . .
H02I H 0.5566 0.1323 0.5361 0.042 Uiso 1 1 calc R . . . .
H02J H 0.6236 -0.0229 0.6470 0.042 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br01 C006 1.889(3) . ?
Br02 C012 1.886(3) . ?
O6 C021 1.431(4) . ?
O6 C022 1.435(3) . ?
O7 C016 1.418(4) . ?
O7 C024 1.426(4) . ?
O005 C017 1.422(4) . ?
O005 C018 1.426(3) . ?
C006 C008 1.390(4) . ?
C006 C019 1.379(4) . ?
N007 C010 1.376(4) . ?
N007 C013 1.327(3) . ?
C008 N009 1.364(3) . ?
C008 C010 1.420(4) . ?
N009 C013 1.371(3) . ?
C010 C012 1.394(4) . ?
C011 C012 1.376(4) . ?
C011 C019 1.407(4) . ?
C013 C015 1.462(4) . ?
O8 C025 1.419(4) . ?
O8 C026 1.424(4) 2_666 ?
C015 C020 1.399(4) . ?
C015 C023 1.394(4) . ?
C016 C026 1.503(4) . ?
C017 C025 1.500(4) . ?
C018 C022 1.489(4) . ?
C020 C023 1.374(4) 2_666 ?
C021 C024 1.506(4) . ?
C023 C020 1.374(4) 2_666 ?
C026 O8 1.424(4) 2_666 ?

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
C021 O6 C022 111.3(2) . . ?
C016 O7 C024 112.8(2) . . ?
C017 O005 C018 112.3(2) . . ?
C008 C006 Br01 119.0(2) . . ?
C019 C006 Br01 121.9(2) . . ?
C019 C006 C008 119.0(3) . . ?
C013 N007 C010 104.7(2) . . ?
C006 C008 C010 120.9(2) . . ?
N009 C008 C006 133.9(3) . . ?
N009 C008 C010 105.1(2) . . ?
C008 N009 C013 107.2(2) . . ?
N007 C010 C008 110.1(2) . . ?
N007 C010 C012 131.1(3) . . ?
C012 C010 C008 118.7(3) . . ?
C012 C011 C019 120.3(3) . . ?
C010 C012 Br02 118.3(2) . . ?
C011 C012 Br02 121.4(2) . . ?
C011 C012 C010 120.3(3) . . ?
N007 C013 N009 112.9(2) . . ?
N007 C013 C015 124.2(2) . . ?
N009 C013 C015 122.9(2) . . ?
C025 O8 C026 112.6(2) . 2_666 ?
C020 C015 C013 120.6(2) . . ?
C023 C015 C013 120.2(2) . . ?
C023 C015 C020 119.1(2) . . ?
O7 C016 C026 108.7(2) . . ?
O005 C017 C025 109.6(2) . . ?
O005 C018 C022 110.8(2) . . ?
C006 C019 C011 120.7(3) . . ?
C023 C020 C015 120.1(3) 2_666 . ?
O6 C021 C024 112.8(2) . . ?
O6 C022 C018 110.8(2) . . ?
C020 C023 C015 120.8(2) 2_666 . ?
O7 C024 C021 109.1(2) . . ?
O8 C025 C017 109.9(3) . . ?
O8 C026 C016 107.7(2) 2_666 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethyl acetate'
####################################################################### 
# 
# 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_gg011
_database_code_depnum_ccdc_archive 'CCDC 1563643'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_audit_creation_date             2017-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2016/4
# start Validation Reply Form
_vrf_PLAT411_gg011               
;
PROBLEM: Short Inter H...H Contact H49B .. H50C . 1.67 Ang.
RESPONSE: Due to disorder in a THF molecule.
;
_vrf_PLAT701_gg011               
;
PROBLEM: Bond Calc 1.06(2), Rep 1.418(6), Dev.. 17.90 Sigma
RESPONSE: Atoms are not actually bonded. Are parts of different disorder models.
;
_vrf_PLAT702_gg011               
;
PROBLEM: Angle Calc 70.2(7), Rep 106.6(5), Dev.. 52.00 Sigma
RESPONSE: Atoms are not actually bonded. Are parts of different disorder models.
;
_vrf_PLAT220_gg011               
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 6.1 Ratio
RESPONSE: Due to high thermal motion of interlocked macrocycle.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H32 O8, C66 H66 N4, 4(C4 H8 O)'
_chemical_formula_sum            'C106 H130 N4 O12'
_chemical_formula_weight         1652.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.0595(2)
_cell_length_b                   12.5637(3)
_cell_length_c                   16.8685(3)
_cell_angle_alpha                74.7825(11)
_cell_angle_beta                 76.6602(12)
_cell_angle_gamma                70.7332(11)
_cell_volume                     2298.72(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.43
_cell_measurement_theta_min      2.75
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.7402
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1057 before and 0.0908 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44412
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         2.749
_diffrn_ambient_temperature      172.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5476
_reflns_number_total             8028
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         8028
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0584
_refine_ls_restrained_S_all      1.138
_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)+(0.0690P)²+1.0855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1570
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-C32 \\sim C35-C32 \\sim C34-C32
 with sigma of 0.02
 C33-C34 \\sim C34-C35
 with sigma of 0.02
 C45-C42 \\sim C44-C42 \\sim C43-C42
 with sigma of 0.02
 C45-C44 \\sim C44-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6A \\sim C53A \\sim C52A \\sim C51A \\sim C50A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Same fragment restrains
{O6A, C53A, C52A, C51A, C50A} sigma for 1-2: 0.02, 1-3: 0.02
{O6, C50, C51, C52, C53} sigma for 1-2: 0.02, 1-3: 0.02
as
{O6, C53, C52, C51, C50}
{C32, C33A, C34A, C35A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C32, C33, C34, C35}
{C42, C45A, C44A, C43A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C42, C45, C44, C43}
5. Others
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(2)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(2)
 Sof(O6A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=1-FVAR(3)
 Sof(O6)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(C50)=Sof(H50A)=Sof(H50B)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C8(H8A,H8B), C12(H12A,H12B), C10(H10A,H10B),
 C1(H1A,H1B), C53(H53A,H53B), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B),
 C48(H48A,H48B), C47(H47A,H47B), C49(H49A,H49B), C46(H46A,H46B), C53A(H53C,
 H53D), C52A(H52C,H52D), C51A(H51C,H51D), C50A(H50C,H50D)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C23(H23), C18(H18), C14(H14), C22(H22), C17(H17), C15(H15), C41(H41),
 C31(H31), C37(H37), C27(H27), C3(H3), C6(H6), C30(H30), C4(H4), C38(H38),
 C40(H40), C28(H28), C5(H5)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C45(H45A,H45B,
 H45C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C33A(H33D,H33E,H33F),
 C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F), C45A(H45D,H45E,H45F), C44A(H44D,
 H44E,H44F), C43A(H43D,H43E,H43F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.39772(15) 1.30679(14) 0.44249(10) 0.0435(4) Uani 1 1 d . . . . .
O3 O 0.52155(14) 1.49730(14) 0.27760(10) 0.0426(4) Uani 1 1 d . . . . .
N1 N 0.99633(15) 1.21920(15) 0.44866(11) 0.0294(4) Uani 1 1 d . . . . .
O2 O 0.64030(14) 1.67221(14) 0.25901(9) 0.0404(4) Uani 1 1 d . . . . .
N2 N 0.93753(15) 1.12887(15) 0.57687(11) 0.0295(4) Uani 1 1 d . . . . .
H2 H 0.891001 1.113302 0.624206 0.035 Uiso 1 1 calc R . . . .
O1 O 0.67387(15) 1.75314(14) 0.37514(9) 0.0418(4) Uani 1 1 d . . . . .
C16 C 0.78841(18) 1.29885(18) 0.50985(13) 0.0272(5) Uani 1 1 d . . . . .
C13 C 0.55991(18) 1.45813(18) 0.50209(13) 0.0260(5) Uani 1 1 d . . . . .
C23 C 1.24338(19) 0.93288(19) 0.55457(14) 0.0330(5) Uani 1 1 d . . . . .
H23 H 1.298190 0.866257 0.580304 0.040 Uiso 1 1 calc R . . . .
C25 C 1.05473(18) 1.06891(18) 0.55518(13) 0.0285(5) Uani 1 1 d . . . . .
C36 C 1.09813(19) 0.91931(19) 0.68690(14) 0.0313(5) Uani 1 1 d . . . . .
C21 C 1.20599(19) 1.08553(18) 0.43081(13) 0.0301(5) Uani 1 1 d . . . . .
C20 C 1.09011(18) 1.12548(18) 0.47386(13) 0.0278(5) Uani 1 1 d . . . . .
C18 C 0.57738(19) 1.35494(19) 0.56031(14) 0.0324(5) Uani 1 1 d . . . . .
H18 H 0.510998 1.337598 0.598183 0.039 Uiso 1 1 calc R . . . .
C2 C 0.6754(2) 1.8235(2) 0.29796(15) 0.0378(6) Uani 1 1 d . . . . .
C24 C 1.13058(19) 0.97239(18) 0.59909(14) 0.0300(5) Uani 1 1 d . . . . .
C14 C 0.66017(19) 1.47938(19) 0.44745(13) 0.0303(5) Uani 1 1 d . . . . .
H14 H 0.651561 1.548991 0.406887 0.036 Uiso 1 1 calc R . . . .
C11 C 0.3928(2) 1.3955(2) 0.37047(14) 0.0401(6) Uani 1 1 d . . . . .
H11A H 0.354510 1.471557 0.386004 0.048 Uiso 1 1 calc R . . . .
H11B H 0.345942 1.386072 0.333046 0.048 Uiso 1 1 calc R . . . .
C26 C 1.25058(19) 1.14498(19) 0.34707(14) 0.0311(5) Uani 1 1 d . . . . .
C19 C 0.90730(19) 1.21692(18) 0.51111(13) 0.0277(5) Uani 1 1 d . . . . .
C22 C 1.2790(2) 0.98699(19) 0.47399(14) 0.0331(5) Uani 1 1 d . . . . .
H22 H 1.357090 0.955197 0.447010 0.040 Uiso 1 1 calc R . . . .
C17 C 0.68884(19) 1.27712(19) 0.56438(14) 0.0329(5) Uani 1 1 d . . . . .
H17 H 0.697696 1.207627 0.605071 0.040 Uiso 1 1 calc R . . . .
C29 C 1.3385(2) 1.2633(2) 0.18915(14) 0.0412(6) Uani 1 1 d . . . . .
C15 C 0.77144(19) 1.40132(19) 0.45119(13) 0.0316(5) Uani 1 1 d . . . . .
H15 H 0.837770 1.418013 0.412872 0.038 Uiso 1 1 calc R . . . .
C9 C 0.6361(2) 1.4969(2) 0.23284(15) 0.0426(6) Uani 1 1 d . . . . .
H9A H 0.655900 1.452122 0.188613 0.051 Uiso 1 1 calc R . . . .
H9B H 0.695886 1.459908 0.270748 0.051 Uiso 1 1 calc R . . . .
C41 C 1.1289(2) 0.8005(2) 0.71431(15) 0.0394(6) Uani 1 1 d . . . . .
H41 H 1.165968 0.752222 0.675033 0.047 Uiso 1 1 calc R . . . .
C31 C 1.3707(2) 1.1361(2) 0.32205(14) 0.0360(6) Uani 1 1 d . . . . .
H31 H 1.425146 1.089502 0.358849 0.043 Uiso 1 1 calc R . . . .
C7 C 0.6575(2) 1.7797(2) 0.23467(14) 0.0364(6) Uani 1 1 d . . . . .
C37 C 1.0420(2) 0.9864(2) 0.74642(15) 0.0406(6) Uani 1 1 d . . . . .
H37 H 1.017638 1.067910 0.729603 0.049 Uiso 1 1 calc R . . . .
C8 C 0.6396(2) 1.6177(2) 0.19483(14) 0.0431(6) Uani 1 1 d . . . . .
H8A H 0.711825 1.617367 0.152583 0.052 Uiso 1 1 calc R . . . .
H8B H 0.569066 1.660345 0.167098 0.052 Uiso 1 1 calc R . . . .
C27 C 1.1749(2) 1.2133(2) 0.29025(15) 0.0417(6) Uani 1 1 d . . . . .
H27 H 1.092169 1.220560 0.304371 0.050 Uiso 1 1 calc R . . . .
C3 C 0.6957(2) 1.9303(2) 0.27875(16) 0.0446(6) Uani 1 1 d . . . . .
H3 H 0.706951 1.960827 0.321246 0.054 Uiso 1 1 calc R . . . .
C12 C 0.2824(2) 1.3050(2) 0.48628(15) 0.0429(6) Uani 1 1 d . . . . .
H12A H 0.236478 1.292129 0.449794 0.051 Uiso 1 1 calc R . . . .
H12B H 0.239696 1.380091 0.502447 0.051 Uiso 1 1 calc R . . . .
C6 C 0.6602(2) 1.8438(2) 0.15444(15) 0.0457(7) Uani 1 1 d . . . . .
H6 H 0.647313 1.815004 0.111641 0.055 Uiso 1 1 calc R . . . .
C30 C 1.4134(2) 1.1931(2) 0.24530(14) 0.0386(6) Uani 1 1 d . . . . .
H30 H 1.496482 1.183928 0.230494 0.046 Uiso 1 1 calc R . . . .
C10 C 0.5186(2) 1.3874(2) 0.32743(15) 0.0404(6) Uani 1 1 d . . . . .
H10A H 0.572541 1.363941 0.369129 0.048 Uiso 1 1 calc R . . . .
H10B H 0.545313 1.329099 0.292089 0.048 Uiso 1 1 calc R . . . .
C1 C 0.7081(2) 1.7887(2) 0.43780(15) 0.0460(7) Uani 1 1 d . . . . .
H1A H 0.648178 1.859820 0.451559 0.055 Uiso 1 1 calc R . . . .
H1B H 0.785660 1.805298 0.416799 0.055 Uiso 1 1 calc R . . . .
C4 C 0.6997(2) 1.9928(2) 0.19763(18) 0.0515(7) Uani 1 1 d . . . . .
H4 H 0.714984 2.065423 0.184713 0.062 Uiso 1 1 calc R . . . .
C39 C 1.0540(2) 0.8180(2) 0.85760(15) 0.0461(7) Uani 1 1 d . . . . .
C38 C 1.0212(2) 0.9364(2) 0.82957(16) 0.0482(7) Uani 1 1 d . . . . .
H38 H 0.983210 0.984649 0.868823 0.058 Uiso 1 1 calc R . . . .
C40 C 1.1065(2) 0.7514(2) 0.79752(16) 0.0470(7) Uani 1 1 d . . . . .
H40 H 1.127486 0.669872 0.814126 0.056 Uiso 1 1 calc R . . . .
C28 C 1.2184(2) 1.2705(2) 0.21369(16) 0.0484(7) Uani 1 1 d . . . . .
H28 H 1.164372 1.316462 0.176488 0.058 Uiso 1 1 calc R . . . .
C5 C 0.6819(2) 1.9508(2) 0.13606(17) 0.0528(7) Uani 1 1 d . . . . .
H5 H 0.684331 1.994524 0.080726 0.063 Uiso 1 1 calc R . . . .
O6 O 0.9998(3) 0.2901(3) 0.68722(19) 0.0680(14) Uani 0.753(10) 1 d D . P A 1
C53 C 1.0162(4) 0.3163(5) 0.7597(3) 0.0592(14) Uani 0.753(10) 1 d D . P A 1
H53A H 1.086403 0.259094 0.782220 0.071 Uiso 0.753(10) 1 calc R . P A 1
H53B H 0.945226 0.317234 0.803232 0.071 Uiso 0.753(10) 1 calc R . P A 1
C52 C 1.0351(5) 0.4344(5) 0.7310(4) 0.0690(16) Uani 0.753(10) 1 d D . P A 1
H52A H 1.118735 0.430393 0.705774 0.083 Uiso 0.753(10) 1 calc R . P A 1
H52B H 1.011203 0.476815 0.777016 0.083 Uiso 0.753(10) 1 calc R . P A 1
C51 C 0.9509(6) 0.4882(4) 0.6660(5) 0.076(2) Uani 0.753(10) 1 d D . P A 1
H51A H 0.867985 0.518571 0.692824 0.091 Uiso 0.753(10) 1 calc R . P A 1
H51B H 0.975440 0.551401 0.624283 0.091 Uiso 0.753(10) 1 calc R . P A 1
C50 C 0.9620(5) 0.3935(5) 0.6279(4) 0.0668(15) Uani 0.753(10) 1 d D . P A 1
H50A H 0.884621 0.399604 0.613698 0.080 Uiso 0.753(10) 1 calc R . P A 1
H50B H 1.021178 0.394370 0.576284 0.080 Uiso 0.753(10) 1 calc R . P A 1
C32 C 1.3850(2) 1.3318(3) 0.10660(17) 0.0633(9) Uani 1 1 d D . . . .
C33 C 1.3377(8) 1.3334(10) 0.0361(4) 0.099(4) Uani 0.538(8) 1 d D . P B 1
H33A H 1.250632 1.361270 0.047133 0.149 Uiso 0.538(8) 1 calc GR . P B 1
H33B H 1.361964 1.255307 0.025238 0.149 Uiso 0.538(8) 1 calc GR . P B 1
H33C H 1.367867 1.384566 -0.012620 0.149 Uiso 0.538(8) 1 calc GR . P B 1
C34 C 1.3417(7) 1.4659(5) 0.1201(4) 0.078(3) Uani 0.538(8) 1 d D . P B 1
H34A H 1.378097 1.470229 0.165061 0.117 Uiso 0.538(8) 1 calc GR . P B 1
H34B H 1.254908 1.491000 0.134752 0.117 Uiso 0.538(8) 1 calc GR . P B 1
H34C H 1.366544 1.516150 0.068552 0.117 Uiso 0.538(8) 1 calc GR . P B 1
C35 C 1.5170(6) 1.3079(8) 0.0911(7) 0.063(3) Uani 0.538(8) 1 d D . P B 1
H35A H 1.554517 1.226864 0.087619 0.094 Uiso 0.538(8) 1 calc GR . P B 1
H35B H 1.542100 1.324133 0.136875 0.094 Uiso 0.538(8) 1 calc GR . P B 1
H35C H 1.540973 1.357074 0.038697 0.094 Uiso 0.538(8) 1 calc GR . P B 1
C42 C 1.0372(2) 0.7648(3) 0.95058(16) 0.0600(8) Uani 1 1 d D . . . .
C45 C 0.9140(4) 0.8114(5) 0.9917(3) 0.077(2) Uani 0.679(7) 1 d D . P C 1
H45A H 0.857642 0.806488 0.960127 0.116 Uiso 0.679(7) 1 calc GR . P C 1
H45B H 0.900341 0.892010 0.993747 0.116 Uiso 0.679(7) 1 calc GR . P C 1
H45C H 0.902407 0.766434 1.048418 0.116 Uiso 0.679(7) 1 calc GR . P C 1
C44 C 1.1332(6) 0.7708(8) 0.9866(5) 0.091(3) Uani 0.679(7) 1 d D . P C 1
H44A H 1.130408 0.851566 0.979527 0.136 Uiso 0.679(7) 1 calc GR . P C 1
H44B H 1.209788 0.729349 0.958394 0.136 Uiso 0.679(7) 1 calc GR . P C 1
H44C H 1.123962 0.735629 1.045958 0.136 Uiso 0.679(7) 1 calc GR . P C 1
C43 C 1.0503(6) 0.6288(4) 0.9628(3) 0.0793(19) Uani 0.679(7) 1 d D . P C 1
H43A H 1.131747 0.588686 0.940774 0.119 Uiso 0.679(7) 1 calc GR . P C 1
H43B H 0.994431 0.619555 0.932887 0.119 Uiso 0.679(7) 1 calc GR . P C 1
H43C H 1.032494 0.595974 1.022157 0.119 Uiso 0.679(7) 1 calc GR . P C 1
O5 O 1.23312(19) 0.87838(19) 0.26186(12) 0.0718(6) Uani 1 1 d . . . . .
C48 C 1.3011(4) 0.8091(5) 0.1399(3) 0.1107(15) Uani 1 1 d . . . . .
H48A H 1.230386 0.821475 0.114621 0.133 Uiso 1 1 calc R . . . .
H48B H 1.368466 0.750438 0.115674 0.133 Uiso 1 1 calc R . . . .
C47 C 1.3321(4) 0.9207(5) 0.1260(2) 0.1057(15) Uani 1 1 d . . . . .
H47A H 1.417802 0.910636 0.104394 0.127 Uiso 1 1 calc R . . . .
H47B H 1.284709 0.982452 0.086676 0.127 Uiso 1 1 calc R . . . .
C49 C 1.2767(4) 0.7734(4) 0.2295(3) 0.1020(13) Uani 1 1 d . . . . .
H49A H 1.349995 0.722712 0.251462 0.122 Uiso 1 1 calc R . . . .
H49B H 1.216050 0.731144 0.245380 0.122 Uiso 1 1 calc R . . . .
C46 C 1.3013(4) 0.9459(4) 0.2089(2) 0.0963(13) Uani 1 1 d . . . . .
H46A H 1.375002 0.931659 0.231331 0.116 Uiso 1 1 calc R . . . .
H46B H 1.256448 1.028210 0.205795 0.116 Uiso 1 1 calc R . . . .
C33A C 1.4877(13) 1.3670(14) 0.1074(10) 0.156(10) Uani 0.462(8) 1 d D . P B 2
H33D H 1.552647 1.298791 0.124209 0.234 Uiso 0.462(8) 1 calc GR . P B 2
H33E H 1.466631 1.418125 0.146847 0.234 Uiso 0.462(8) 1 calc GR . P B 2
H33F H 1.513139 1.407745 0.051557 0.234 Uiso 0.462(8) 1 calc GR . P B 2
C34A C 1.4410(11) 1.2326(8) 0.0484(4) 0.125(5) Uani 0.462(8) 1 d D . P B 2
H34D H 1.378168 1.201476 0.044796 0.187 Uiso 0.462(8) 1 calc GR . P B 2
H34E H 1.504615 1.170326 0.073531 0.187 Uiso 0.462(8) 1 calc GR . P B 2
H34F H 1.473349 1.267477 -0.007564 0.187 Uiso 0.462(8) 1 calc GR . P B 2
C35A C 1.2919(8) 1.4137(9) 0.0607(6) 0.116(6) Uani 0.462(8) 1 d D . P B 2
H35D H 1.240159 1.469011 0.094721 0.173 Uiso 0.462(8) 1 calc GR . P B 2
H35E H 1.244612 1.372041 0.047691 0.173 Uiso 0.462(8) 1 calc GR . P B 2
H35F H 1.328419 1.454768 0.008874 0.173 Uiso 0.462(8) 1 calc GR . P B 2
C45A C 1.1551(11) 0.7003(15) 0.9791(12) 0.122(10) Uani 0.321(7) 1 d D . P C 2
H45D H 1.209798 0.747937 0.957673 0.183 Uiso 0.321(7) 1 calc GR . P C 2
H45E H 1.188404 0.628629 0.958172 0.183 Uiso 0.321(7) 1 calc GR . P C 2
H45F H 1.143918 0.682431 1.040048 0.183 Uiso 0.321(7) 1 calc GR . P C 2
C44A C 0.9430(12) 0.7124(13) 0.9760(7) 0.095(6) Uani 0.321(7) 1 d D . P C 2
H44D H 0.960608 0.649365 0.946773 0.143 Uiso 0.321(7) 1 calc GR . P C 2
H44E H 0.868411 0.769817 0.962505 0.143 Uiso 0.321(7) 1 calc GR . P C 2
H44F H 0.935013 0.681979 1.036126 0.143 Uiso 0.321(7) 1 calc GR . P C 2
C43A C 0.9940(12) 0.8702(8) 1.0060(5) 0.079(4) Uani 0.321(7) 1 d D . P C 2
H43D H 0.917899 0.924006 0.992062 0.118 Uiso 0.321(7) 1 calc GR . P C 2
H43E H 1.054260 0.911458 0.992332 0.118 Uiso 0.321(7) 1 calc GR . P C 2
H43F H 0.984660 0.835983 1.065547 0.118 Uiso 0.321(7) 1 calc GR . P C 2
O6A O 1.006(2) 0.381(2) 0.7922(13) 0.192(9) Uani 0.247(10) 1 d D U P A 2
C53A C 1.025(3) 0.486(2) 0.7446(17) 0.163(12) Uani 0.247(10) 1 d D U P A 2
H53C H 1.110668 0.476420 0.724837 0.196 Uiso 0.247(10) 1 calc R . P A 2
H53D H 0.993303 0.546459 0.778077 0.196 Uiso 0.247(10) 1 calc R . P A 2
C52A C 0.960(2) 0.516(2) 0.6734(12) 0.144(13) Uani 0.247(10) 1 d D U P A 2
H52C H 0.994644 0.565030 0.624544 0.172 Uiso 0.247(10) 1 calc R . P A 2
H52D H 0.874218 0.554830 0.688428 0.172 Uiso 0.247(10) 1 calc R . P A 2
C51A C 0.981(4) 0.394(3) 0.6579(17) 0.197(15) Uani 0.247(10) 1 d D U P A 2
H51C H 0.918868 0.392372 0.628651 0.236 Uiso 0.247(10) 1 calc R . P A 2
H51D H 1.060126 0.365954 0.625327 0.236 Uiso 0.247(10) 1 calc R . P A 2
C50A C 0.971(4) 0.325(3) 0.744(2) 0.237(17) Uani 0.247(10) 1 d D U P A 2
H50C H 0.888551 0.321860 0.765340 0.285 Uiso 0.247(10) 1 calc R . P A 2
H50D H 1.024284 0.245625 0.745836 0.285 Uiso 0.247(10) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C11 1.414(3) . ?
O4 C12 1.421(3) . ?
O6Ab C53A 1.408(15) . ?
C53Ab C52A 1.483(17) . ?
C52Ab C51A 1.553(19) . ?
O6Ab C50A 1.405(15) . ?
C51Ab C50A 1.484(17) . ?
O3 C9 1.413(3) . ?
O3 C10 1.423(3) . ?
N1 C20 1.388(3) . ?
N1 C19 1.321(3) . ?
O2 C7 1.374(3) . ?
O2 C8 1.428(3) . ?
N2 C25 1.379(3) . ?
N2 C19 1.365(3) . ?
O1 C2 1.368(3) . ?
O1 C1 1.435(3) . ?
C16 C19 1.464(3) . ?
C16 C17 1.392(3) . ?
C16 C15 1.389(3) . ?
C13 C13 1.485(4) 2_686 ?
C13 C18 1.392(3) . ?
C13 C14 1.397(3) . ?
C23 C24 1.393(3) . ?
C23 C22 1.390(3) . ?
C25 C20 1.410(3) . ?
C25 C24 1.402(3) . ?
C36 C24 1.476(3) . ?
C36 C41 1.389(3) . ?
C36 C37 1.390(3) . ?
C21 C20 1.412(3) . ?
C21 C26 1.484(3) . ?
C21 C22 1.394(3) . ?
C18 C17 1.381(3) . ?
C2 C7 1.408(3) . ?
C2 C3 1.385(3) . ?
C14 C15 1.380(3) . ?
C11 C10 1.506(3) . ?
C26 C31 1.388(3) . ?
C26 C27 1.394(3) . ?
C29 C30 1.387(3) . ?
C29 C28 1.390(3) . ?
C29 C32 1.524(3) . ?
C9 C8 1.494(4) . ?
C41 C40 1.380(3) . ?
C31 C30 1.379(3) . ?
C7 C6 1.381(3) . ?
C37 C38 1.380(3) . ?
C27 C28 1.382(3) . ?
C3 C4 1.386(4) . ?
C12 C1 1.492(3) 2_686 ?
C6 C5 1.396(4) . ?
C1 C12 1.492(3) 2_686 ?
C4 C5 1.366(4) . ?
C39 C38 1.387(4) . ?
C39 C40 1.388(4) . ?
C39 C42 1.530(3) . ?
C32 C33 1.427(6) . ?
C32 C34 1.653(6) . ?
C32 C35 1.492(7) . ?
C32 C33A 1.449(9) . ?
C32 C34A 1.659(8) . ?
C32 C35A 1.463(8) . ?
C42 C45 1.482(5) . ?
C42 C44 1.456(6) . ?
C42 C43 1.625(6) . ?
C42 C45A 1.503(10) . ?
C42 C44A 1.425(9) . ?
C42 C43A 1.693(8) . ?
O5 C49 1.450(4) . ?
O5 C46 1.385(4) . ?
C48 C47 1.515(6) . ?
C48 C49 1.447(6) . ?
C47 C46 1.453(5) . ?
O6A C53 1.418(6) . ?
O6A C50 1.426(6) . ?
C53A C52 1.512(8) . ?
C52A C51 1.537(8) . ?
C51A C50 1.450(9) . ?

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
C11 O4 C12 111.88(18) . . ?
C50Ab O6Ab C53A 110.7(12) . . ?
O6Ab C53Ab C52A 105.6(11) . . ?
C9 O3 C10 112.21(18) . . ?
C19 N1 C20 105.35(17) . . ?
C7 O2 C8 117.11(17) . . ?
C50Ab C51Ab C52A 101.6(12) . . ?
O6Ab C50Ab C51A 106.3(11) . . ?
C53Ab C52Ab C51A 100.0(11) . . ?
C19 N2 C25 107.11(17) . . ?
C2 O1 C1 116.55(18) . . ?
C17 C16 C19 122.46(19) . . ?
C15 C16 C19 119.93(19) . . ?
C15 C16 C17 117.59(19) . . ?
C18 C13 C13 121.6(2) . 2_686 ?
C18 C13 C14 117.03(19) . . ?
C14 C13 C13 121.4(2) . 2_686 ?
C22 C23 C24 122.7(2) . . ?
N2 C25 C20 105.35(18) . . ?
N2 C25 C24 131.3(2) . . ?
C24 C25 C20 123.33(19) . . ?
C41 C36 C24 121.5(2) . . ?
C41 C36 C37 117.3(2) . . ?
C37 C36 C24 121.1(2) . . ?
C20 C21 C26 123.49(19) . . ?
C22 C21 C20 115.1(2) . . ?
C22 C21 C26 121.4(2) . . ?
N1 C20 C25 109.43(18) . . ?
N1 C20 C21 129.58(19) . . ?
C25 C20 C21 120.98(19) . . ?
C17 C18 C13 121.6(2) . . ?
O1 C2 C7 115.7(2) . . ?
O1 C2 C3 124.9(2) . . ?
C3 C2 C7 119.5(2) . . ?
C23 C24 C25 114.58(19) . . ?
C23 C24 C36 121.63(19) . . ?
C25 C24 C36 123.70(19) . . ?
C15 C14 C13 121.4(2) . . ?
O4 C11 C10 107.59(19) . . ?
C33Ab C32 C29 115.0(6) . . ?
C31 C26 C21 121.1(2) . . ?
C35Ab C32 C29 114.2(4) . . ?
C35Ab C32 C34A 101.1(6) . . ?
C33Ab C32 C34A 102.8(7) . . ?
C33Ab C32 C35A 118.2(7) . . ?
C45Ab C42 C39 110.9(8) . . ?
C44Ab C42 C39 113.2(5) . . ?
C44Ab C42 C45A 119.1(9) . . ?
C45Ab C42 C43A 98.7(7) . . ?
C44Ab C42 C43A 103.7(6) . . ?
C31 C26 C27 116.7(2) . . ?
C27 C26 C21 122.3(2) . . ?
N1 C19 N2 112.73(18) . . ?
N1 C19 C16 123.86(19) . . ?
N2 C19 C16 123.41(18) . . ?
C23 C22 C21 123.3(2) . . ?
C18 C17 C16 121.1(2) . . ?
C30 C29 C28 116.2(2) . . ?
C30 C29 C32 121.7(2) . . ?
C28 C29 C32 122.1(2) . . ?
C14 C15 C16 121.3(2) . . ?
O3 C9 C8 109.8(2) . . ?
C40 C41 C36 121.2(2) . . ?
C30 C31 C26 121.9(2) . . ?
O2 C7 C2 115.5(2) . . ?
O2 C7 C6 124.9(2) . . ?
C6 C7 C2 119.6(2) . . ?
C38 C37 C36 121.0(2) . . ?
O2 C8 C9 108.71(19) . . ?
C28 C27 C26 121.0(2) . . ?
C2 C3 C4 120.1(3) . . ?
O4 C12 C1 110.0(2) . 2_686 ?
C7 C6 C5 120.2(3) . . ?
C31 C30 C29 121.8(2) . . ?
O3 C10 C11 108.29(19) . . ?
O1 C1 C12 109.23(19) . 2_686 ?
C5 C4 C3 120.6(3) . . ?
C38 C39 C40 116.7(2) . . ?
C38 C39 C42 121.0(3) . . ?
C40 C39 C42 122.2(2) . . ?
C37 C38 C39 122.0(2) . . ?
C41 C40 C39 121.7(2) . . ?
C27 C28 C29 122.4(2) . . ?
C4 C5 C6 120.0(2) . . ?
C29 C32 C34 104.6(3) . . ?
C29 C32 C34A 102.0(4) . . ?
C33A C32 C29 115.9(4) . . ?
C33A C32 C34 106.6(5) . . ?
C33A C32 C35 113.5(5) . . ?
C35A C32 C29 113.3(5) . . ?
C35A C32 C34 101.1(4) . . ?
C39 C42 C43 109.3(3) . . ?
C39 C42 C43A 109.4(4) . . ?
C45A C42 C39 111.6(3) . . ?
C45A C42 C43 103.1(4) . . ?
C44A C42 C39 108.9(4) . . ?
C44A C42 C45 117.2(4) . . ?
C44A C42 C43 106.2(4) . . ?
C46 O5 C49 102.5(3) . . ?
C49 C48 C47 104.7(4) . . ?
C46 C47 C48 102.6(3) . . ?
C48 C49 O5 105.9(4) . . ?
O5 C46 C47 111.2(4) . . ?
C53A O6A C50 110.1(4) . . ?
O6A C53A C52 104.6(4) . . ?
C53A C52A C51 99.8(4) . . ?
C50A C51A C52 104.0(4) . . ?
O6A C50A C51 106.7(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
####################################################################### 
# 
# 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_mo_gg025_0m
_database_code_depnum_ccdc_archive 'CCDC 1563642'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_audit_creation_date             2017-07-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2014-3
# start Validation Reply Form
_vrf_PLAT213_mo_gg025_0m         
;
PROBLEM: Atom C10U has ADP max/min Ratio ..... 5.8 prolat
RESPONSE: Due to high thermal motion of a disordered tBu group.
;
_vrf_PLAT411_mo_gg025_0m         
;
PROBLEM: Short Inter H...H Contact H6A .. H95 . 1.68 Ang.
RESPONSE: Due to disordered toluene.
;
_vrf_PLAT214_mo_gg025_0m         
;
PROBLEM: Atom F9B (Anion/Solvent) ADP max/min Ratio 5.9 prolat
RESPONSE: Due to heavily disordered BF4 anion.
;
_vrf_PLAT220_mo_gg025_0m         
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 6.8 Ratio
RESPONSE:Due to high thermal motion of interlocked macrocycle.
;
_vrf_PLAT250_mo_gg025_0m         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.9 Note
RESPONSE: Due to high thermal motion of heavily disordered toluene.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C64 H66 N4, C24 H32 O8, 2(B F4), 3(C7 H8), H2 O'
_chemical_formula_sum            'C109 H124 B2 F8 N4 O9'
_chemical_formula_weight         1807.73
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   14.2079(9)
_cell_length_b                   18.9576(11)
_cell_length_c                   20.1063(13)
_cell_angle_alpha                97.249(3)
_cell_angle_beta                 100.114(3)
_cell_angle_gamma                108.536(3)
_cell_volume                     4957.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.73
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.958
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.8920.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79916
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.475
_diffrn_reflns_theta_min         2.705
_diffrn_ambient_temperature      170.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11452
_reflns_number_total             20185
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1400
_refine_ls_number_reflns         20185
_refine_ls_number_restraints     328
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.1057
_refine_ls_restrained_S_all      1.141
_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)+(0.0622P)²+10.8936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2079
_refine_ls_wR_factor_ref         0.2555
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4
 with sigma of 0.04
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4
 with sigma of 0.02
 C2T-C3T \\sim C2T-C4T \\sim C3T-C4T
 with sigma of 0.04
 C1T-C2T \\sim C1T-C3T \\sim C1T-C4T
 with sigma of 0.02
 C6T-C7T \\sim C6T-C8T \\sim C7T-C8T
 with sigma of 0.04
 C5T-C6T \\sim C5T-C7T \\sim C5T-C8T
 with sigma of 0.02
 C10T-C11T \\sim C10T-C12T \\sim C11T-C12T
 with sigma of 0.04
 C9T-C10T \\sim C9T-C11T \\sim C9T-C12T
 with sigma of 0.02
 C14T-C15T \\sim C14T-C16T \\sim C15T-C16T
 with sigma of 0.04
 C13T-C14T \\sim C13T-C15T \\sim C13T-C16T
 with sigma of 0.02
 C2-C13 \\sim C2-C5
 with sigma of 0.04
 C15-C1F \\sim C15-C1B
 with sigma of 0.04
 B3-F9 \\sim B3-F10 \\sim B3-F11 \\sim B3-F12
 with sigma of 0.02
 F9-F10 \\sim F10-F11 \\sim F11-F12 \\sim F12-F9 \\sim F10-F12 \\sim F9-F11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F12A) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(F12B) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F9B) \\sim Ueq, Uanis(F11A) \\sim Ueq,
Uanis(F10A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F11B)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F10B) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uanis(B1) = Uanis(B1A)
Uanis(F2) = Uanis(F2A)
Uanis(F4) = Uanis(F4A)
Uanis(C1W) = Uanis(C1X) = Uanis(C1Y)
Uanis(C2W) = Uanis(C2X) = Uanis(C2Y)
Uanis(C3W) = Uanis(C3X) = Uanis(C3Y)
Uanis(C4W) = Uanis(C4X) = Uanis(C4Y)
Uanis(C5W) = Uanis(C5X) = Uanis(C5Y)
Uanis(C6W) = Uanis(C6X) = Uanis(C6Y)
Uanis(C7W) = Uanis(C7X) = Uanis(C7Y)
Uanis(C13) = Uanis(C5)
Uanis(C9) = Uanis(C6)
Uanis(C1F) = Uanis(C1C)
Uanis(C1B) = Uanis(C1E)
Uanis(C1A) = Uanis(C1D)
4. Same fragment restrains
{C13T, C14U, C15U, C16U} sigma for 1-2: 0.02, 1-3: 0.02
as
{C13T, C14T, C15T, C16T}
{F1, B1A, F2A, F4A, F3} sigma for 1-2: 0.02, 1-3: 0.02
as
{F1, B1, F2, F4, F3}
{C9T, C10U, C11U, C12U} sigma for 1-2: 0.02, 1-3: 0.02
as
{C9T, C10T, C11T, C12T}
{C1Y, C2Y, C7Y, C6Y, C5Y, C4Y, C3Y} sigma for 1-2: 0.02, 1-3: 0.02
{C1X, C2X, C7X, C6X, C5X, C4X, C3X} sigma for 1-2: 0.02, 1-3: 0.02
as
{C1W, C2W, C7W, C6W, C5W, C4W, C3W}
{B3, F9A, F10A, F11A, F12A} sigma for 1-2: 0.02, 1-3: 0.02
{B3, F9B, F10B, F11B, F12B} sigma for 1-2: 0.02, 1-3: 0.02
as
{B3, F9, F10, F11, F12}
5. Others
 1*[Sof(F9)+Sof(F10)+Sof(F11)+Sof(F12)]+1*[Sof(F9A)+Sof(F10A)+Sof(F11A)+
 Sof(F12A)]+1*[Sof(F9B)+Sof(F10B)+Sof(F11B)+Sof(F12B)]=1 with esd of 0.001
 1*[Sof(C1W)+Sof(H1WA)+Sof(H1WB)+Sof(H1WC)+Sof(C2W)+Sof(C7W)+Sof(H7W)+Sof(C6W)+
 Sof(H6W)+Sof(C5W)+Sof(H5W)+Sof(C4W)+Sof(H4W)+Sof(C3W)+Sof(H3W)]+1*[Sof(C1X)+
 Sof(H1XA)+Sof(H1XB)+Sof(H1XC)+Sof(C2X)+Sof(C7X)+Sof(H7X)+Sof(C6X)+Sof(H6X)+
 Sof(C5X)+Sof(H5X)+Sof(C4X)+Sof(H4X)+Sof(C3X)+Sof(H3X)]+1*[Sof(C1Y)+Sof(H1YA)+
 Sof(H1YB)+Sof(H1YC)+Sof(C2Y)+Sof(C7Y)+Sof(H7Y)+Sof(C6Y)+Sof(H6Y)+Sof(C5Y)+
 Sof(H5Y)+Sof(C4Y)+Sof(H4Y)+Sof(C3Y)+Sof(H3Y)]=1 with esd of 0.001
 Sof(C10U)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11U)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C12U)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C10T)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11T)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12T)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(C14U)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15U)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16U)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(C14T)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15T)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16T)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(4)
 Sof(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=FVAR(5)
 Sof(B1A)=Sof(F2A)=Sof(F4A)=1-FVAR(6)
 Sof(B1)=Sof(F2)=Sof(F4)=FVAR(6)
 Sof(C1W)=Sof(H1WA)=Sof(H1WB)=Sof(H1WC)=Sof(C2W)=Sof(C7W)=Sof(H7W)=Sof(C6W)=
 Sof(H6W)=Sof(C5W)=Sof(H5W)=Sof(C4W)=Sof(H4W)=Sof(C3W)=Sof(H3W)=FVAR(7)
 Sof(C1X)=Sof(H1XA)=Sof(H1XB)=Sof(H1XC)=Sof(C2X)=Sof(C7X)=Sof(H7X)=Sof(C6X)=
 Sof(H6X)=Sof(C5X)=Sof(H5X)=Sof(C4X)=Sof(H4X)=Sof(C3X)=Sof(H3X)=FVAR(8)
 Sof(C1Y)=Sof(H1YA)=Sof(H1YB)=Sof(H1YC)=Sof(C2Y)=Sof(C7Y)=Sof(H7Y)=Sof(C6Y)=
 Sof(H6Y)=Sof(C5Y)=Sof(H5Y)=Sof(C4Y)=Sof(H4Y)=Sof(C3Y)=Sof(H3Y)=FVAR(9)
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) C5(0.5) H5A(0.5)
 C6(0.5) H6A(0.5) C8(0.5) H8A(0.5) C9(0.5) H9(0.5) C13(0.5) H13(0.5) C15(0.5)
 H15G(0.5) H15H(0.5) H15I(0.5) C1A(0.5) C1F(0.5) H1F(0.5) C1E(0.5) H1E(0.5)
 C1D(0.5) H1D(0.5) C1C(0.5) H1C(0.5) C1B(0.5) H1B(0.5)
6.a Free rotating group:
 O1(H1A,H1G)
6.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C51(H51A,H51B), C53(H53A,H53B), C55(H55A,H55B), C58(H58A,
 H58B), C60(H60A,H60B), C63(H63A,H63B), C72(H72A,H72B), C78(H78A,H78B),
 C86(H86A,H86B), C100(H10G,H10H), C108(H10I,H10J)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N5(H5), N6(H6), N8(H8), C11(H11), C19(H19), C20(H20), C24(H24),
 C27(H27), C31(H31), C32(H32), C34(H34), C39(H39), C41(H41), C45(H45), C46(H46),
  C47(H47), C54(H54), C57(H57), C64(H64), C65(H65), C67(H67), C69(H69),
 C73(H73), C75(H75), C76(H76), C77(H77), C83(H83), C84(H84), C103(H103),
 C66(H66), C82(H82), C88(H88), C91(H91), C95(H95), C99(H99), C101(H101),
 C104(H104), C74(H74), C80(H80), C89(H89), C97(H97), C109(H109), C7W(H7W),
 C6W(H6W), C5W(H5W), C4W(H4W), C3W(H3W), C5(H5A), C6(H6A), C8(H8A), C9(H9),
 C13(H13), C1F(H1F), C1E(H1E), C1D(H1D), C1C(H1C), C1B(H1B), C7X(H7X), C6X(H6X),
  C5X(H5X), C4X(H4X), C3X(H3X), C7Y(H7Y), C6Y(H6Y), C5Y(H5Y), C4Y(H4Y), C3Y(H3Y)
6.d Fitted hexagon refined as free rotating group:
 C2W(C7W,C6W,C5W,C4W,C3W), C3(C5,C6,C8,C9,C13), C1A(C1F,C1E,C1D,C1C,C1B)
6.e Idealised Me refined as rotating group:
 C8T(H8TA,H8TB,H8TC), C2T(H2TA,H2TB,H2TC), C3T(H3TA,H3TB,H3TC), C14T(H14A,H14B,
 H14C), C15T(H15A,H15B,H15C), C16T(H16A,H16B,H16C), C4T(H4TA,H4TB,H4TC),
 C6T(H6TA,H6TB,H6TC), C7T(H7TA,H7TB,H7TC), C14(H14G,H14H,H14I), C10T(H10A,H10B,
 H10C), C11T(H11A,H11B,H11C), C12T(H12A,H12B,H12C), C1W(H1WA,H1WB,H1WC),
 C10U(H10D,H10E,H10F), C11U(H11D,H11E,H11F), C12U(H12D,H12E,H12F), C14U(H14D,
 H14E,H14F), C15U(H15D,H15E,H15F), C16U(H16D,H16E,H16F), C2(H2A,H2B,H2C),
 C15(H15G,H15H,H15I), C1X(H1XA,H1XB,H1XC), C1Y(H1YA,H1YB,H1YC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.1224(2) 0.66523(14) 0.35969(14) 0.0289(6) Uani 1 1 d . . . . .
H1 H 0.1464 0.6309 0.3737 0.035 Uiso 1 1 calc R . . . .
N5 N 0.5042(2) 0.95037(17) 0.80965(15) 0.0401(7) Uani 1 1 d . . . . .
H5 H 0.5038 0.9036 0.8075 0.048 Uiso 1 1 calc R . . . .
N6 N 0.0889(2) 0.76915(15) 0.36026(14) 0.0306(6) Uani 1 1 d . . . . .
H6 H 0.0885 0.8149 0.3744 0.037 Uiso 1 1 calc R . . . .
N8 N 0.4841(2) 1.05049(16) 0.77858(15) 0.0369(7) Uani 1 1 d . . . . .
H8 H 0.4690 1.0811 0.7526 0.044 Uiso 1 1 calc R . . . .
C10 C 0.1982(2) 0.76330(18) 0.46799(17) 0.0291(7) Uani 1 1 d . . . . .
C11 C 0.3542(3) 0.86702(19) 0.67235(18) 0.0348(8) Uani 1 1 d . . . . .
H11 H 0.3378 0.8428 0.7095 0.042 Uiso 1 1 calc R . . . .
C12 C 0.3032(3) 0.82935(18) 0.60358(17) 0.0314(7) Uani 1 1 d . . . . .
C16 C 0.1374(2) 0.73233(18) 0.39707(17) 0.0292(7) Uani 1 1 d . . . . .
C17 C 0.3296(3) 0.86695(19) 0.54955(17) 0.0325(7) Uani 1 1 d . . . . .
C18 C 0.0390(3) 0.72379(19) 0.29587(17) 0.0318(7) Uani 1 1 d . . . . .
C19 C 0.1735(3) 0.72414(19) 0.52151(18) 0.0339(8) Uani 1 1 d . . . . .
H19 H 0.1214 0.6756 0.5116 0.041 Uiso 1 1 calc R . . . .
C20 C 0.2742(3) 0.83171(19) 0.48080(17) 0.0332(7) Uani 1 1 d . . . . .
H20 H 0.2904 0.8562 0.4438 0.040 Uiso 1 1 calc R . . . .
C21 C -0.0239(3) 0.7357(2) 0.23964(19) 0.0394(9) Uani 1 1 d . . . . .
C22 C 0.4262(3) 0.9376(2) 0.68542(17) 0.0357(8) Uani 1 1 d . . . . .
C23 C 0.0626(2) 0.65789(18) 0.29491(17) 0.0308(7) Uani 1 1 d . . . . .
C24 C 0.2259(3) 0.75741(19) 0.58793(18) 0.0373(8) Uani 1 1 d . . . . .
H24 H 0.2099 0.7314 0.6242 0.045 Uiso 1 1 calc R . . . .
C25 C 0.5251(3) 1.0704(2) 0.84953(18) 0.0349(8) Uani 1 1 d . . . . .
C27 C 0.4547(3) 0.9736(2) 0.63094(19) 0.0435(9) Uani 1 1 d . . . . .
H27 H 0.5068 1.0221 0.6405 0.052 Uiso 1 1 calc R . . . .
C28 C 0.0278(3) 0.59942(19) 0.23681(18) 0.0344(8) Uani 1 1 d . . . . .
C29 C 0.4716(3) 0.9786(2) 0.75631(18) 0.0368(8) Uani 1 1 d . . . . .
C30 C 0.0549(3) 0.53055(19) 0.23557(18) 0.0337(8) Uani 1 1 d . . . . .
C31 C -0.0172(3) 0.4590(2) 0.2087(2) 0.0424(9) Uani 1 1 d . . . . .
H31 H -0.0854 0.4543 0.1893 0.051 Uiso 1 1 calc R . . . .
C32 C 0.1781(3) 0.4699(2) 0.2637(2) 0.0417(9) Uani 1 1 d . . . . .
H32 H 0.2465 0.4745 0.2824 0.050 Uiso 1 1 calc R . . . .
C34 C 0.6222(3) 1.0754(2) 0.9804(2) 0.0503(10) Uani 1 1 d . . . . .
H34 H 0.6574 1.0794 1.0263 0.060 Uiso 1 1 calc R . . . .
C36 C 0.5389(3) 1.0060(2) 0.86915(18) 0.0400(9) Uani 1 1 d . . . . .
C38 C -0.0500(3) 0.8058(2) 0.2409(2) 0.0439(9) Uani 1 1 d . . . . .
C39 C 0.1539(3) 0.53471(19) 0.26354(19) 0.0378(8) Uani 1 1 d . . . . .
H39 H 0.2053 0.5828 0.2827 0.045 Uiso 1 1 calc R . . . .
C40 C 0.5555(3) 1.1391(2) 0.89504(19) 0.0397(8) Uani 1 1 d . . . . .
C41 C 0.5327(3) 0.8659(2) 0.9274(2) 0.0481(10) Uani 1 1 d . . . . .
H41 H 0.4691 0.8619 0.8998 0.058 Uiso 1 1 calc R . . . .
C42 C 0.1065(3) 0.39876(19) 0.2377(2) 0.0393(8) Uani 1 1 d . . . . .
C43 C 0.5369(3) 1.2069(2) 0.87424(19) 0.0420(9) Uani 1 1 d . . . . .
C45 C 0.4067(3) 0.9382(2) 0.56442(19) 0.0449(9) Uani 1 1 d . . . . .
H45 H 0.4260 0.9623 0.5278 0.054 Uiso 1 1 calc R . . . .
C46 C -0.0333(3) 0.6124(2) 0.1812(2) 0.0494(10) Uani 1 1 d . . . . .
H46 H -0.0595 0.5747 0.1402 0.059 Uiso 1 1 calc R . . . .
C47 C -0.0580(3) 0.6777(2) 0.1826(2) 0.0505(11) Uani 1 1 d . . . . .
H47 H -0.1002 0.6827 0.1426 0.061 Uiso 1 1 calc R . . . .
C50 C 0.5887(3) 1.0062(2) 0.9359(2) 0.0467(10) Uani 1 1 d . . . . .
C52 C 0.6050(4) 0.9367(2) 0.95419(19) 0.0518(11) Uani 1 1 d . . . . .
C54 C -0.0957(3) 0.8289(2) 0.2909(2) 0.0494(10) Uani 1 1 d . . . . .
H54 H -0.1094 0.8004 0.3259 0.059 Uiso 1 1 calc R . . . .
C57 C 0.6103(3) 1.2781(2) 0.8931(2) 0.0527(11) Uani 1 1 d . . . . .
H57 H 0.6748 1.2845 0.9212 0.063 Uiso 1 1 calc R . . . .
C1T C 0.1313(3) 0.3262(2) 0.2424(2) 0.0564(12) Uani 1 1 d D . . . .
C61 C -0.1005(3) 0.9387(2) 0.2410(3) 0.0567(13) Uani 1 1 d . . . . .
C64 C 0.4436(3) 1.2001(2) 0.8331(2) 0.0516(10) Uani 1 1 d . . . . .
H64 H 0.3906 1.1519 0.8198 0.062 Uiso 1 1 calc R . . . .
C65 C -0.1217(3) 0.8942(2) 0.2899(2) 0.0574(12) Uani 1 1 d . . . . .
H65 H -0.1549 0.9083 0.3237 0.069 Uiso 1 1 calc R . . . .
C67 C 0.0074(3) 0.3945(2) 0.2093(2) 0.0450(9) Uani 1 1 d . . . . .
H67 H -0.0439 0.3463 0.1902 0.054 Uiso 1 1 calc R . . . .
C68 C 0.5002(4) 1.3338(2) 0.8306(2) 0.0570(12) Uani 1 1 d . . . . .
C69 C 0.5500(4) 0.8004(3) 0.9397(2) 0.0545(11) Uani 1 1 d . . . . .
H69 H 0.4986 0.7525 0.9197 0.065 Uiso 1 1 calc R . . . .
C73 C 0.5929(4) 1.3409(2) 0.8724(2) 0.0593(12) Uani 1 1 d . . . . .
H73 H 0.6451 1.3894 0.8870 0.071 Uiso 1 1 calc R . . . .
C75 C 0.6066(3) 1.1398(2) 0.9610(2) 0.0479(10) Uani 1 1 d . . . . .
H75 H 0.6318 1.1858 0.9941 0.058 Uiso 1 1 calc R . . . .
C76 C -0.0306(4) 0.8494(2) 0.1912(2) 0.0566(12) Uani 1 1 d . . . . .
H76 H 0.0003 0.8344 0.1563 0.068 Uiso 1 1 calc R . . . .
C77 C -0.0554(4) 0.9147(3) 0.1914(3) 0.0629(13) Uani 1 1 d . . . . .
H77 H -0.0409 0.9434 0.1567 0.075 Uiso 1 1 calc R . . . .
C5T C 0.6617(5) 0.7296(3) 0.9885(2) 0.0793(18) Uani 1 1 d D . . . .
C83 C 0.6950(5) 0.9406(3) 0.9978(3) 0.085(2) Uani 1 1 d . . . . .
H83 H 0.7452 0.9886 1.0193 0.103 Uiso 1 1 calc R . . . .
C84 C 0.4266(4) 1.2626(2) 0.8113(2) 0.0585(12) Uani 1 1 d . . . . .
H84 H 0.3627 1.2561 0.7823 0.070 Uiso 1 1 calc R . . . .
C85 C 0.6414(4) 0.8033(3) 0.9809(2) 0.0650(14) Uani 1 1 d . . . . .
C8T C 0.5648(6) 0.6657(3) 0.9928(4) 0.107(2) Uani 1 1 d D . . . .
H8TA H 0.5394 0.6819 1.0322 0.161 Uiso 1 1 calc GR . . . .
H8TB H 0.5810 0.6200 0.9987 0.161 Uiso 1 1 calc GR . . . .
H8TC H 0.5124 0.6547 0.9503 0.161 Uiso 1 1 calc GR . . . .
C2T C 0.2451(4) 0.3415(3) 0.2495(3) 0.0730(15) Uani 1 1 d D . . . .
H2TA H 0.2665 0.3630 0.2105 0.109 Uiso 1 1 calc GR . . . .
H2TB H 0.2583 0.2939 0.2501 0.109 Uiso 1 1 calc GR . . . .
H2TC H 0.2834 0.3775 0.2925 0.109 Uiso 1 1 calc GR . . . .
C3T C 0.0744(5) 0.2659(3) 0.1772(4) 0.110(3) Uani 1 1 d D . . . .
H3TA H 0.0010 0.2487 0.1752 0.165 Uiso 1 1 calc GR . . . .
H3TB H 0.0983 0.2229 0.1779 0.165 Uiso 1 1 calc GR . . . .
H3TC H 0.0874 0.2877 0.1366 0.165 Uiso 1 1 calc GR . . . .
C103 C 0.7115(5) 0.8748(3) 1.0100(3) 0.092(2) Uani 1 1 d . . . . .
H103 H 0.7738 0.8790 1.0397 0.110 Uiso 1 1 calc R . . . .
C13T C -0.1261(3) 1.0116(2) 0.2415(3) 0.0633(14) Uani 1 1 d D . . . .
C14T C -0.0783(8) 1.0675(5) 0.3041(4) 0.065(3) Uani 0.528(8) 1 d D . P A 1
H14A H -0.1038 1.0474 0.3426 0.097 Uiso 0.528(8) 1 calc GR . P A 1
H14B H -0.0942 1.1135 0.2992 0.097 Uiso 0.528(8) 1 calc GR . P A 1
H14C H -0.0042 1.0798 0.3132 0.097 Uiso 0.528(8) 1 calc GR . P A 1
C15T C -0.2393(5) 0.9909(5) 0.2144(5) 0.047(2) Uani 0.528(8) 1 d D . P A 1
H15A H -0.2600 0.9590 0.1682 0.070 Uiso 0.528(8) 1 calc GR . P A 1
H15B H -0.2554 1.0372 0.2119 0.070 Uiso 0.528(8) 1 calc GR . P A 1
H15C H -0.2761 0.9629 0.2452 0.070 Uiso 0.528(8) 1 calc GR . P A 1
C16T C -0.0841(6) 1.0577(4) 0.1801(4) 0.053(2) Uani 0.528(8) 1 d D . P A 1
H16A H -0.0094 1.0764 0.1909 0.080 Uiso 0.528(8) 1 calc GR . P A 1
H16B H -0.1082 1.1007 0.1785 0.080 Uiso 0.528(8) 1 calc GR . P A 1
H16C H -0.1104 1.0230 0.1353 0.080 Uiso 0.528(8) 1 calc GR . P A 1
C4T C 0.0979(6) 0.2976(3) 0.3046(4) 0.107(3) Uani 1 1 d D . . . .
H4TA H 0.1387 0.3346 0.3466 0.161 Uiso 1 1 calc GR . . . .
H4TB H 0.1079 0.2490 0.3069 0.161 Uiso 1 1 calc GR . . . .
H4TC H 0.0257 0.2906 0.3006 0.161 Uiso 1 1 calc GR . . . .
O2 O 0.1254(2) 0.91919(14) 0.42412(14) 0.0449(6) Uani 1 1 d . . . . .
O3 O 0.2261(2) 0.57782(15) 0.43556(14) 0.0472(7) Uani 1 1 d . . . . .
O4 O -0.0177(2) 0.80230(14) 0.46605(14) 0.0456(6) Uani 1 1 d . . . . .
O7 O -0.0791(2) 0.63337(15) 0.43213(15) 0.0484(7) Uani 1 1 d . . . . .
O9 O 0.0147(2) 0.53578(14) 0.42473(14) 0.0454(6) Uani 1 1 d . . . . .
O13 O 0.3467(2) 0.68499(16) 0.38086(15) 0.0534(7) Uani 1 1 d . . . . .
O14 O 0.2941(2) 0.93064(15) 0.36051(15) 0.0496(7) Uani 1 1 d . . . . .
O15 O 0.2971(2) 0.79822(18) 0.31074(15) 0.0580(8) Uani 1 1 d . . . . .
C44 C -0.0825(3) 0.5122(2) 0.3845(2) 0.0474(10) Uani 1 1 d . . . . .
C48 C 0.0664(3) 0.4817(2) 0.4232(3) 0.0542(11) Uani 1 1 d . . . . .
H48A H 0.0693 0.4641 0.3754 0.065 Uiso 1 1 calc R . . . .
H48B H 0.0297 0.4372 0.4413 0.065 Uiso 1 1 calc R . . . .
C51 C 0.0604(3) 0.9334(2) 0.4664(2) 0.0475(10) Uani 1 1 d . . . . .
H51A H -0.0037 0.9329 0.4371 0.057 Uiso 1 1 calc R . . . .
H51B H 0.0942 0.9842 0.4965 0.057 Uiso 1 1 calc R . . . .
C53 C 0.0368(3) 0.8745(2) 0.5096(2) 0.0490(10) Uani 1 1 d . . . . .
H53A H 0.1009 0.8739 0.5378 0.059 Uiso 1 1 calc R . . . .
H53B H -0.0048 0.8865 0.5410 0.059 Uiso 1 1 calc R . . . .
C55 C 0.1714(3) 0.5206(3) 0.4670(2) 0.0553(11) Uani 1 1 d . . . . .
H55A H 0.1680 0.5433 0.5133 0.066 Uiso 1 1 calc R . . . .
H55B H 0.2065 0.4834 0.4725 0.066 Uiso 1 1 calc R . . . .
C56 C -0.1327(3) 0.5642(2) 0.3891(2) 0.0491(10) Uani 1 1 d . . . . .
C58 C 0.1605(3) 0.9771(2) 0.3862(2) 0.0536(11) Uani 1 1 d . . . . .
H58A H 0.1481 1.0233 0.4051 0.064 Uiso 1 1 calc R . . . .
H58B H 0.1231 0.9598 0.3373 0.064 Uiso 1 1 calc R . . . .
C60 C -0.1374(3) 0.6787(2) 0.4511(3) 0.0548(11) Uani 1 1 d . . . . .
H60A H -0.1919 0.6492 0.4717 0.066 Uiso 1 1 calc R . . . .
H60B H -0.1701 0.6927 0.4095 0.066 Uiso 1 1 calc R . . . .
C62 C 0.2704(3) 0.9104(2) 0.2907(2) 0.0502(10) Uani 1 1 d . . . . .
C63 C -0.0705(3) 0.7484(2) 0.5012(2) 0.0506(10) Uani 1 1 d . . . . .
H63A H -0.1121 0.7696 0.5268 0.061 Uiso 1 1 calc R . . . .
H63B H -0.0211 0.7361 0.5348 0.061 Uiso 1 1 calc R . . . .
C66 C -0.1320(4) 0.4411(2) 0.3432(2) 0.0585(11) Uani 1 1 d . . . . .
H66 H -0.0978 0.4056 0.3403 0.070 Uiso 1 1 calc R . . . .
C71 C 0.2691(3) 0.8391(3) 0.2634(2) 0.0541(11) Uani 1 1 d . . . . .
C72 C 0.4105(3) 0.7375(3) 0.3521(3) 0.0597(12) Uani 1 1 d . . . . .
H72A H 0.4635 0.7183 0.3396 0.072 Uiso 1 1 calc R . . . .
H72B H 0.4451 0.7854 0.3864 0.072 Uiso 1 1 calc R . . . .
C78 C 0.3528(3) 0.7526(3) 0.2897(3) 0.0568(11) Uani 1 1 d . . . . .
H78A H 0.4005 0.7793 0.2630 0.068 Uiso 1 1 calc R . . . .
H78B H 0.3055 0.7042 0.2599 0.068 Uiso 1 1 calc R . . . .
C82 C 0.2442(4) 0.8131(3) 0.1932(3) 0.0682(13) Uani 1 1 d . . . . .
H82 H 0.2421 0.7637 0.1750 0.082 Uiso 1 1 calc R . . . .
C86 C 0.2735(3) 0.9948(2) 0.3915(3) 0.0567(11) Uani 1 1 d . . . . .
H86A H 0.2995 1.0377 0.3683 0.068 Uiso 1 1 calc R . . . .
H86B H 0.3099 1.0104 0.4406 0.068 Uiso 1 1 calc R . . . .
C88 C 0.2509(4) 0.9563(3) 0.2452(3) 0.0676(14) Uani 1 1 d . . . . .
H88 H 0.2535 1.0060 0.2625 0.081 Uiso 1 1 calc R . . . .
C91 C -0.2323(4) 0.5438(3) 0.3519(3) 0.0756(15) Uani 1 1 d . . . . .
H91 H -0.2672 0.5789 0.3548 0.091 Uiso 1 1 calc R . . . .
C95 C 0.2282(4) 0.9304(4) 0.1757(3) 0.0820(18) Uani 1 1 d . . . . .
H95 H 0.2163 0.9629 0.1454 0.098 Uiso 1 1 calc R . . . .
C99 C 0.2221(4) 0.8596(4) 0.1490(3) 0.0801(17) Uani 1 1 d . . . . .
H99 H 0.2030 0.8417 0.1005 0.096 Uiso 1 1 calc R . . . .
C100 C 0.3298(4) 0.6080(4) 0.4640(3) 0.0843(18) Uani 1 1 d . . . . .
H10G H 0.3394 0.6296 0.5132 0.101 Uiso 1 1 calc R . . . .
H10H H 0.3563 0.5655 0.4623 0.101 Uiso 1 1 calc R . . . .
C101 C -0.2813(5) 0.4727(3) 0.3106(3) 0.094(2) Uani 1 1 d . . . . .
H101 H -0.3497 0.4592 0.2854 0.113 Uiso 1 1 calc R . . . .
C104 C -0.2317(5) 0.4217(3) 0.3057(3) 0.0827(17) Uani 1 1 d . . . . .
H104 H -0.2654 0.3731 0.2769 0.099 Uiso 1 1 calc R . . . .
C108 C 0.3895(4) 0.6624(3) 0.4359(3) 0.089(2) Uani 1 1 d . . . . .
H10I H 0.4247 0.7080 0.4728 0.107 Uiso 1 1 calc R . . . .
H10J H 0.4428 0.6441 0.4227 0.107 Uiso 1 1 calc R . . . .
F1 F 0.1897(2) 0.7498(2) 0.75829(16) 0.0875(10) Uani 1 1 d D . . . .
B1 B 0.2692(4) 0.7750(3) 0.8162(3) 0.0562(15) Uani 0.844(5) 1 d D . P B 1
F2 F 0.3543(2) 0.7675(2) 0.7953(2) 0.0756(11) Uani 0.844(5) 1 d D . P B 1
F4 F 0.2473(4) 0.7346(3) 0.8654(2) 0.134(2) Uani 0.844(5) 1 d D . P B 1
F3 F 0.2956(3) 0.85126(19) 0.83920(18) 0.0965(11) Uani 1 1 d D . . . .
C74 C 0.5892(4) 0.7945(3) 0.7610(3) 0.0607(12) Uani 1 1 d . . . . .
H74 H 0.5348 0.7765 0.7830 0.073 Uiso 1 1 calc R . . . .
C80 C 0.6838(4) 0.8401(3) 0.7994(3) 0.0653(13) Uani 1 1 d . . . . .
H80 H 0.6942 0.8539 0.8479 0.078 Uiso 1 1 calc R . . . .
C89 C 0.7620(4) 0.8656(3) 0.7692(4) 0.088(2) Uani 1 1 d . . . . .
H89 H 0.8275 0.8965 0.7964 0.105 Uiso 1 1 calc R . . . .
C90 C 0.5726(5) 0.7747(3) 0.6901(3) 0.0824(18) Uani 1 1 d . . . . .
C97 C 0.7470(8) 0.8466(4) 0.6985(6) 0.114(3) Uani 1 1 d . . . . .
H97 H 0.8024 0.8648 0.6772 0.136 Uiso 1 1 calc R . . . .
C109 C 0.6551(8) 0.8029(4) 0.6598(4) 0.102(3) Uani 1 1 d . . . . .
H109 H 0.6456 0.7908 0.6112 0.122 Uiso 1 1 calc R . . . .
O1 O 0.4029(3) 1.1197(2) 0.68095(17) 0.0697(9) Uani 1 1 d . . . . .
H1A H 0.3974 1.1640 0.6907 0.105 Uiso 1 1 d G . . . .
H1G H 0.3855 1.1038 0.6366 0.105 Uiso 1 1 d G . . . .
C6T C 0.7402(6) 0.7406(4) 1.0536(4) 0.116(3) Uani 1 1 d D . . . .
H6TA H 0.8062 0.7756 1.0504 0.173 Uiso 1 1 calc GR . . . .
H6TB H 0.7463 0.6916 1.0596 0.173 Uiso 1 1 calc GR . . . .
H6TC H 0.7191 0.7617 1.0931 0.173 Uiso 1 1 calc GR . . . .
C7T C 0.6888(8) 0.7019(4) 0.9236(4) 0.140(4) Uani 1 1 d D . . . .
H7TA H 0.6378 0.7013 0.8836 0.210 Uiso 1 1 calc GR . . . .
H7TB H 0.6901 0.6505 0.9233 0.210 Uiso 1 1 calc GR . . . .
H7TC H 0.7561 0.7359 0.9215 0.210 Uiso 1 1 calc GR . . . .
C14 C 0.4732(7) 0.7257(5) 0.6481(5) 0.166(5) Uani 1 1 d . . . . .
H14G H 0.4720 0.6733 0.6391 0.250 Uiso 1 1 calc GR . . . .
H14H H 0.4607 0.7425 0.6043 0.250 Uiso 1 1 calc GR . . . .
H14I H 0.4201 0.7282 0.6726 0.250 Uiso 1 1 calc GR . . . .
C9T C 0.4812(5) 1.4036(3) 0.8077(3) 0.0785(16) Uani 1 1 d D . . . .
C10T C 0.5626(14) 1.4794(6) 0.8421(10) 0.148(12) Uani 0.527(16) 1 d D . P C 1
H10A H 0.5564 1.4931 0.8893 0.221 Uiso 0.527(16) 1 calc GR . P C 1
H10B H 0.5540 1.5183 0.8162 0.221 Uiso 0.527(16) 1 calc GR . P C 1
H10C H 0.6301 1.4759 0.8428 0.221 Uiso 0.527(16) 1 calc GR . P C 1
C11T C 0.3740(12) 1.4021(10) 0.8179(9) 0.151(12) Uani 0.527(16) 1 d D . P C 1
H11A H 0.3218 1.3544 0.7918 0.227 Uiso 0.527(16) 1 calc GR . P C 1
H11B H 0.3595 1.4449 0.8014 0.227 Uiso 0.527(16) 1 calc GR . P C 1
H11C H 0.3736 1.4061 0.8669 0.227 Uiso 0.527(16) 1 calc GR . P C 1
C12T C 0.4709(11) 1.3987(8) 0.7290(5) 0.085(4) Uani 0.527(16) 1 d D . P C 1
H12A H 0.5354 1.3994 0.7175 0.127 Uiso 0.527(16) 1 calc GR . P C 1
H12B H 0.4545 1.4420 0.7155 0.127 Uiso 0.527(16) 1 calc GR . P C 1
H12C H 0.4164 1.3515 0.7042 0.127 Uiso 0.527(16) 1 calc GR . P C 1
C1W C 0.102(4) 0.651(2) 1.008(2) 0.114(7) Uani 0.424(15) 1 d D . P D 1
H1WA H 0.0393 0.6326 0.9722 0.171 Uiso 0.424(15) 1 calc GR . P D 1
H1WB H 0.1468 0.6997 1.0023 0.171 Uiso 0.424(15) 1 calc GR . P D 1
H1WC H 0.0857 0.6566 1.0536 0.171 Uiso 0.424(15) 1 calc GR . P D 1
C2W C 0.1548(18) 0.5953(10) 1.0039(13) 0.098(4) Uani 0.424(15) 1 d D . P D 1
C7W C 0.1333(18) 0.5353(12) 1.0387(13) 0.104(5) Uani 0.424(15) 1 d DG . P D 1
H7W H 0.0892 0.5324 1.0695 0.124 Uiso 0.424(15) 1 calc R . P D 1
C6W C 0.1763(17) 0.4796(10) 1.0285(13) 0.109(7) Uani 0.424(15) 1 d DG . P D 1
H6W H 0.1616 0.4386 1.0522 0.131 Uiso 0.424(15) 1 calc R . P D 1
C5W C 0.2408(16) 0.4839(9) 0.9834(14) 0.108(8) Uani 0.424(15) 1 d DG . P D 1
H5W H 0.2703 0.4458 0.9764 0.130 Uiso 0.424(15) 1 calc R . P D 1
C4W C 0.2623(16) 0.5439(10) 0.9486(10) 0.098(6) Uani 0.424(15) 1 d DG . P D 1
H4W H 0.3065 0.5469 0.9178 0.118 Uiso 0.424(15) 1 calc R . P D 1
C3W C 0.2193(17) 0.5996(8) 0.9588(9) 0.083(4) Uani 0.424(15) 1 d DG . P D 1
H3W H 0.2340 0.6406 0.9351 0.099 Uiso 0.424(15) 1 calc R . P D 1
C10U C 0.3830(14) 1.3826(8) 0.7593(12) 0.19(2) Uani 0.473(16) 1 d D . P C 2
H10D H 0.3280 1.3620 0.7825 0.292 Uiso 0.473(16) 1 calc GR . P C 2
H10E H 0.3787 1.3441 0.7204 0.292 Uiso 0.473(16) 1 calc GR . P C 2
H10F H 0.3763 1.4275 0.7426 0.292 Uiso 0.473(16) 1 calc GR . P C 2
C11U C 0.5767(13) 1.4457(9) 0.7820(10) 0.131(9) Uani 0.473(16) 1 d D . P C 2
H11D H 0.6379 1.4582 0.8189 0.196 Uiso 0.473(16) 1 calc GR . P C 2
H11E H 0.5707 1.4925 0.7690 0.196 Uiso 0.473(16) 1 calc GR . P C 2
H11F H 0.5817 1.4130 0.7420 0.196 Uiso 0.473(16) 1 calc GR . P C 2
C12U C 0.4881(13) 1.4561(8) 0.8747(6) 0.088(5) Uani 0.473(16) 1 d D . P C 2
H12D H 0.4318 1.4319 0.8955 0.131 Uiso 0.473(16) 1 calc GR . P C 2
H12E H 0.4838 1.5043 0.8643 0.131 Uiso 0.473(16) 1 calc GR . P C 2
H12F H 0.5532 1.4657 0.9068 0.131 Uiso 0.473(16) 1 calc GR . P C 2
C14U C -0.1969(9) 1.0100(6) 0.1817(6) 0.073(4) Uani 0.472(8) 1 d D . P A 2
H14D H -0.1679 1.0048 0.1414 0.109 Uiso 0.472(8) 1 calc GR . P A 2
H14E H -0.2117 1.0572 0.1865 0.109 Uiso 0.472(8) 1 calc GR . P A 2
H14F H -0.2600 0.9668 0.1759 0.109 Uiso 0.472(8) 1 calc GR . P A 2
C15U C -0.0275(7) 1.0741(5) 0.2719(7) 0.073(4) Uani 0.472(8) 1 d D . P A 2
H15D H -0.0002 1.0685 0.3184 0.110 Uiso 0.472(8) 1 calc GR . P A 2
H15E H -0.0381 1.1229 0.2741 0.110 Uiso 0.472(8) 1 calc GR . P A 2
H15F H 0.0210 1.0723 0.2431 0.110 Uiso 0.472(8) 1 calc GR . P A 2
C16U C -0.1867(8) 1.0199(5) 0.3058(5) 0.065(3) Uani 0.472(8) 1 d D . P A 2
H16D H -0.2527 0.9785 0.2952 0.097 Uiso 0.472(8) 1 calc GR . P A 2
H16E H -0.1976 1.0687 0.3103 0.097 Uiso 0.472(8) 1 calc GR . P A 2
H16F H -0.1449 1.0174 0.3491 0.097 Uiso 0.472(8) 1 calc GR . P A 2
C2 C 0.023(3) 0.8830(19) 0.9882(14) 0.29(3) Uani 0.5 1 d D . P E -1
H2A H -0.0414 0.8431 0.9868 0.440 Uiso 0.5 1 calc GR . P E -1
H2B H 0.0761 0.8817 1.0262 0.440 Uiso 0.5 1 calc GR . P E -1
H2C H 0.0434 0.8746 0.9446 0.440 Uiso 0.5 1 calc GR . P E -1
C3 C 0.0106(11) 0.9589(8) 0.9992(9) 0.126(7) Uani 0.5 1 d . . P E -1
C5 C -0.0621(12) 0.9715(10) 0.9509(9) 0.264(10) Uani 0.5 1 d DG . P E -1
H5A H -0.1024 0.9325 0.9125 0.316 Uiso 0.5 1 calc R . P E -1
C6 C -0.0759(13) 1.0412(12) 0.9587(10) 0.310(19) Uani 0.5 1 d G . P E -1
H6A H -0.1256 1.0498 0.9256 0.372 Uiso 0.5 1 calc R . P E -1
C8 C -0.0169(14) 1.0984(10) 1.0148(11) 0.144(13) Uani 0.5 1 d G . P E -1
H8A H -0.0263 1.1460 1.0202 0.173 Uiso 0.5 1 calc R . P E -1
C9 C 0.0558(14) 1.0858(9) 1.0632(10) 0.310(19) Uani 0.5 1 d G . P E -1
H9 H 0.0961 1.1248 1.1016 0.372 Uiso 0.5 1 calc R . P E -1
C13 C 0.0696(13) 1.0161(9) 1.0554(9) 0.264(10) Uani 0.5 1 d DG . P E -1
H13 H 0.1193 1.0075 1.0885 0.316 Uiso 0.5 1 calc R . P E -1
C15 C 0.626(2) 0.619(2) 0.5425(14) 0.235(17) Uani 0.5 1 d D . P F -1
H15G H 0.6930 0.6129 0.5520 0.352 Uiso 0.5 1 calc GR . P F -1
H15H H 0.6138 0.6410 0.5855 0.352 Uiso 0.5 1 calc GR . P F -1
H15I H 0.6259 0.6532 0.5097 0.352 Uiso 0.5 1 calc GR . P F -1
C1A C 0.5556(9) 0.5537(6) 0.5166(7) 0.113(6) Uani 0.5 1 d . . P F -1
C1F C 0.5000(11) 0.5055(9) 0.5537(5) 0.097(4) Uani 0.5 1 d DG . P F -1
H1F H 0.5083 0.5216 0.6017 0.117 Uiso 0.5 1 calc R . P F -1
C1E C 0.4324(9) 0.4338(8) 0.5205(8) 0.108(5) Uani 0.5 1 d G . P F -1
H1E H 0.3944 0.4009 0.5458 0.129 Uiso 0.5 1 calc R . P F -1
C1D C 0.4204(9) 0.4102(6) 0.4502(8) 0.113(6) Uani 0.5 1 d G . P F -1
H1D H 0.3742 0.3612 0.4275 0.135 Uiso 0.5 1 calc R . P F -1
C1C C 0.4759(11) 0.4584(8) 0.4131(5) 0.097(4) Uani 0.5 1 d G . P F -1
H1C H 0.4677 0.4423 0.3651 0.117 Uiso 0.5 1 calc R . P F -1
C1B C 0.5436(10) 0.5301(8) 0.4463(7) 0.108(5) Uani 0.5 1 d DG . P F -1
H1B H 0.5816 0.5630 0.4210 0.129 Uiso 0.5 1 calc R . P F -1
B3 B 0.2909(4) 1.1688(3) 0.5419(3) 0.0617(14) Uani 1 1 d D U . . .
F9 F 0.3231(10) 1.2307(5) 0.5126(5) 0.129(5) Uani 0.555(14) 1 d D U P G 1
F10 F 0.1980(6) 1.1293(7) 0.5074(10) 0.163(9) Uani 0.555(14) 1 d D U P G 1
F11 F 0.3488(11) 1.1249(9) 0.5372(8) 0.122(8) Uani 0.555(14) 1 d D U P G 1
F12 F 0.2974(11) 1.1977(7) 0.6090(4) 0.089(4) Uani 0.555(14) 1 d D U P G 1
F9A F 0.2371(15) 1.1558(14) 0.4761(5) 0.085(9) Uani 0.232(13) 1 d D U P G 2
F10A F 0.2163(18) 1.135(2) 0.5732(16) 0.186(19) Uani 0.232(13) 1 d D U P G 2
F11A F 0.3574(11) 1.1320(10) 0.5502(11) 0.045(5) Uani 0.232(13) 1 d D U P G 2
F12A F 0.3313(17) 1.2434(8) 0.566(2) 0.19(2) Uani 0.232(13) 1 d D U P G 2
F9B F 0.2035(15) 1.1549(15) 0.4976(15) 0.18(2) Uani 0.213(13) 1 d D U P G 3
F10B F 0.279(3) 1.0981(9) 0.5573(13) 0.149(15) Uani 0.213(13) 1 d D U P G 3
F11B F 0.3740(11) 1.1827(17) 0.5131(10) 0.115(10) Uani 0.213(13) 1 d D U P G 3
F12B F 0.306(2) 1.2208(10) 0.5973(10) 0.097(12) Uani 0.213(13) 1 d D U P G 3
B1A B 0.2490(13) 0.7744(8) 0.8239(7) 0.0562(15) Uani 0.156(5) 1 d D . P B 2
F2A F 0.3217(14) 0.7418(10) 0.8353(10) 0.0756(11) Uani 0.156(5) 1 d D . P B 2
F4A F 0.1891(17) 0.7636(13) 0.8704(9) 0.134(2) Uani 0.156(5) 1 d D . P B 2
C1X C 0.113(4) 0.664(2) 0.988(3) 0.114(7) Uani 0.370(13) 1 d D . P H 2
H1XA H 0.0391 0.6494 0.9804 0.171 Uiso 0.370(13) 1 calc GR . P H 2
H1XB H 0.1358 0.6847 0.9490 0.171 Uiso 0.370(13) 1 calc GR . P H 2
H1XC H 0.1462 0.7016 1.0305 0.171 Uiso 0.370(13) 1 calc GR . P H 2
C2X C 0.142(2) 0.5954(14) 0.9938(16) 0.098(4) Uani 0.370(13) 1 d D . P H 2
C7X C 0.125(2) 0.5608(16) 1.0502(16) 0.104(5) Uani 0.370(13) 1 d D . P H 2
H7X H 0.0946 0.5798 1.0835 0.124 Uiso 0.370(13) 1 calc R . P H 2
C6X C 0.154(2) 0.4977(15) 1.0558(14) 0.109(7) Uani 0.370(13) 1 d D . P H 2
H6X H 0.1340 0.4683 1.0893 0.131 Uiso 0.370(13) 1 calc R . P H 2
C5X C 0.211(3) 0.4777(16) 1.0128(17) 0.108(8) Uani 0.370(13) 1 d D . P H 2
H5X H 0.2299 0.4342 1.0166 0.130 Uiso 0.370(13) 1 calc R . P H 2
C4X C 0.242(2) 0.5205(13) 0.9644(14) 0.098(6) Uani 0.370(13) 1 d D . P H 2
H4X H 0.2889 0.5111 0.9396 0.118 Uiso 0.370(13) 1 calc R . P H 2
C3X C 0.202(2) 0.5782(12) 0.9523(11) 0.083(4) Uani 0.370(13) 1 d D . P H 2
H3X H 0.2161 0.6046 0.9161 0.099 Uiso 0.370(13) 1 calc R . P H 2
C1Y C 0.287(2) 0.563(2) 0.8998(16) 0.114(7) Uani 0.206(10) 1 d D . P I 3
H1YA H 0.2571 0.5259 0.8564 0.171 Uiso 0.206(10) 1 calc GR . P I 3
H1YB H 0.3565 0.5640 0.9180 0.171 Uiso 0.206(10) 1 calc GR . P I 3
H1YC H 0.2900 0.6133 0.8914 0.171 Uiso 0.206(10) 1 calc GR . P I 3
C2Y C 0.224(3) 0.541(2) 0.9505(17) 0.098(4) Uani 0.206(10) 1 d D . P I 3
C7Y C 0.181(5) 0.593(3) 0.976(3) 0.104(5) Uani 0.206(10) 1 d D . P I 3
H7Y H 0.1900 0.6390 0.9601 0.124 Uiso 0.206(10) 1 calc R . P I 3
C6Y C 0.124(4) 0.575(3) 1.025(3) 0.109(7) Uani 0.206(10) 1 d D . P I 3
H6Y H 0.0807 0.6015 1.0356 0.131 Uiso 0.206(10) 1 calc R . P I 3
C5Y C 0.133(4) 0.517(3) 1.060(2) 0.108(8) Uani 0.206(10) 1 d D . P I 3
H5Y H 0.0989 0.5073 1.0963 0.130 Uiso 0.206(10) 1 calc R . P I 3
C4Y C 0.189(3) 0.4735(19) 1.041(2) 0.098(6) Uani 0.206(10) 1 d D . P I 3
H4Y H 0.1976 0.4361 1.0666 0.118 Uiso 0.206(10) 1 calc R . P I 3
C3Y C 0.235(3) 0.4849(14) 0.9849(16) 0.083(4) Uani 0.206(10) 1 d D . P I 3
H3Y H 0.2718 0.4542 0.9708 0.099 Uiso 0.206(10) 1 calc R . P I 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C16 1.326(4) . ?
N1 C23 1.389(4) . ?
N5 C29 1.334(4) . ?
N5 C36 1.389(4) . ?
N6 C16 1.329(4) . ?
N6 C18 1.388(4) . ?
N8 C25 1.396(4) . ?
N8 C29 1.324(4) . ?
C10 C16 1.469(4) . ?
C10 C19 1.415(5) . ?
C10 C20 1.357(5) . ?
C11 C12 1.420(5) . ?
C11 C22 1.361(5) . ?
C12 C17 1.413(5) . ?
C12 C24 1.408(5) . ?
C17 C20 1.424(5) . ?
C17 C45 1.399(5) . ?
C18 C21 1.402(5) . ?
C18 C23 1.391(4) . ?
C19 C24 1.370(5) . ?
C21 C38 1.487(5) . ?
C21 C47 1.381(5) . ?
C22 C27 1.414(5) . ?
C22 C29 1.460(5) . ?
C23 C28 1.400(5) . ?
C25 C36 1.391(5) . ?
C25 C40 1.386(5) . ?
C27 C45 1.366(5) . ?
C28 C30 1.472(4) . ?
C28 C46 1.389(5) . ?
C30 C31 1.385(5) . ?
C30 C39 1.393(5) . ?
C31 C67 1.374(5) . ?
C32 C39 1.378(5) . ?
C32 C42 1.375(5) . ?
C34 C50 1.381(5) . ?
C34 C75 1.398(6) . ?
C36 C50 1.402(5) . ?
C38 C54 1.386(6) . ?
C38 C76 1.385(6) . ?
C40 C43 1.485(5) . ?
C40 C75 1.393(5) . ?
C41 C52 1.376(6) . ?
C41 C69 1.385(6) . ?
C42 C1T 1.534(5) . ?
C42 C67 1.396(5) . ?
C43 C57 1.375(6) . ?
C43 C64 1.393(6) . ?
C46 C47 1.389(5) . ?
C50 C52 1.485(5) . ?
C52 C83 1.393(6) . ?
C54 C65 1.400(5) . ?
C57 C73 1.389(6) . ?
C1T C2T 1.526(6) . ?
C1T C3T 1.531(7) . ?
C1T C4T 1.516(7) . ?
C61 C65 1.387(7) . ?
C61 C77 1.381(7) . ?
C61 C13T 1.535(5) . ?
C64 C84 1.390(6) . ?
C68 C73 1.390(7) . ?
C68 C84 1.375(6) . ?
C68 C9T 1.540(6) . ?
C69 C85 1.392(6) . ?
C76 C77 1.390(6) . ?
C5T C85 1.535(6) . ?
C5T C8T 1.542(8) . ?
C5T C6T 1.505(7) . ?
C5T C7T 1.504(7) . ?
C83 C103 1.384(7) . ?
C85 C103 1.382(8) . ?
C13T C14T 1.441(8) . ?
C13T C15T 1.509(7) . ?
C13T C16T 1.687(8) . ?
C13T C14U 1.416(9) . ?
C13T C15U 1.484(9) . ?
C13T C16U 1.692(9) . ?
O2 C51 1.424(4) . ?
O2 C58 1.426(5) . ?
O3 C55 1.411(5) . ?
O3 C100 1.382(5) . ?
O4 C53 1.424(5) . ?
O4 C63 1.411(5) . ?
O7 C56 1.377(5) . ?
O7 C60 1.433(5) . ?
O9 C44 1.372(5) . ?
O9 C48 1.439(4) . ?
O13 C72 1.379(5) . ?
O13 C108 1.351(5) . ?
O14 C62 1.359(5) . ?
O14 C86 1.432(5) . ?
O15 C71 1.383(5) . ?
O15 C78 1.419(5) . ?
C44 C56 1.391(6) . ?
C44 C66 1.382(6) . ?
C48 C55 1.491(6) . ?
C51 C53 1.490(6) . ?
C56 C91 1.386(6) . ?
C58 C86 1.513(6) . ?
C60 C63 1.481(6) . ?
C62 C71 1.387(6) . ?
C62 C88 1.392(6) . ?
C66 C104 1.391(7) . ?
C71 C82 1.379(7) . ?
C72 C78 1.487(6) . ?
C82 C99 1.394(7) . ?
C88 C95 1.365(8) . ?
C91 C101 1.381(7) . ?
C95 C99 1.352(8) . ?
C100 C108 1.365(7) . ?
C101 C104 1.369(8) . ?
F1 B1 1.384(6) . ?
F1 B1A 1.369(13) . ?
B1 F2 1.389(7) . ?
B1 F4 1.345(6) . ?
B1 F3 1.367(7) . ?
F3 B1A 1.363(14) . ?
C74 C80 1.371(7) . ?
C74 C90 1.384(7) . ?
C80 C89 1.344(8) . ?
C89 C97 1.383(10) . ?
C90 C109 1.403(10) . ?
C90 C14 1.456(9) . ?
C97 C109 1.338(11) . ?
C9T C10T 1.514(10) . ?
C9T C11T 1.564(11) . ?
C9T C12T 1.553(10) . ?
C9T C10U 1.457(11) . ?
C9T C11U 1.551(11) . ?
C9T C12U 1.538(10) . ?
C1W C2W 1.470(13) . ?
C2W C7W 1.3900 . ?
C2W C3W 1.3900 . ?
C7W C6W 1.3900 . ?
C6W C5W 1.3900 . ?
C5W C4W 1.3900 . ?
C4W C3W 1.3900 . ?
C2 C3 1.50(4) . ?
C3 C5 1.3900 . ?
C3 C13 1.3900 . ?
C5 C6 1.3900 . ?
C6 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C13 1.3900 . ?
C15 C1A 1.30(4) . ?
C1A C1F 1.3900 . ?
C1A C1B 1.3900 . ?
C1F C1E 1.3900 . ?
C1E C1D 1.3900 . ?
C1D C1C 1.3900 . ?
C1C C1B 1.3900 . ?
B3 F9 1.364(8) . ?
B3 F10 1.305(9) . ?
B3 F11 1.350(8) . ?
B3 F12 1.365(8) . ?
B3 F9A 1.356(10) . ?
B3 F10A 1.356(11) . ?
B3 F11A 1.343(10) . ?
B3 F12A 1.331(11) . ?
B3 F9B 1.322(12) . ?
B3 F10B 1.379(12) . ?
B3 F11B 1.371(11) . ?
B3 F12B 1.328(12) . ?
B1A F2A 1.364(13) . ?
B1A F4A 1.363(13) . ?
C1X C2X 1.484(16) . ?
C2X C7X 1.398(15) . ?
C2X C3X 1.372(14) . ?
C7X C6X 1.395(15) . ?
C6X C5X 1.386(16) . ?
C5X C4X 1.385(16) . ?
C4X C3X 1.410(15) . ?
C1Y C2Y 1.485(19) . ?
C2Y C7Y 1.399(17) . ?
C2Y C3Y 1.378(16) . ?
C7Y C6Y 1.394(17) . ?
C6Y C5Y 1.388(17) . ?
C5Y C4Y 1.385(16) . ?
C4Y C3Y 1.406(16) . ?

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
C16 N1 C23 109.1(3) . . ?
C29 N5 C36 109.7(3) . . ?
C16 N6 C18 109.0(3) . . ?
C29 N8 C25 109.8(3) . . ?
C19 C10 C16 120.2(3) . . ?
C20 C10 C16 118.2(3) . . ?
C20 C10 C19 121.6(3) . . ?
C22 C11 C12 120.5(3) . . ?
C17 C12 C11 118.3(3) . . ?
C24 C12 C11 122.3(3) . . ?
C24 C12 C17 119.4(3) . . ?
N1 C16 N6 109.4(3) . . ?
N1 C16 C10 126.6(3) . . ?
N6 C16 C10 123.9(3) . . ?
C12 C17 C20 118.5(3) . . ?
C45 C17 C12 120.0(3) . . ?
C45 C17 C20 121.5(3) . . ?
N6 C18 C21 131.1(3) . . ?
N6 C18 C23 106.2(3) . . ?
C23 C18 C21 122.7(3) . . ?
C24 C19 C10 118.8(3) . . ?
C10 C20 C17 120.3(3) . . ?
C18 C21 C38 122.7(3) . . ?
C47 C21 C18 114.4(3) . . ?
C47 C21 C38 122.9(3) . . ?
C11 C22 C27 120.8(3) . . ?
C11 C22 C29 120.1(3) . . ?
C27 C22 C29 119.0(3) . . ?
N1 C23 C18 106.2(3) . . ?
N1 C23 C28 131.3(3) . . ?
C18 C23 C28 122.4(3) . . ?
C19 C24 C12 121.3(3) . . ?
C36 C25 N8 105.8(3) . . ?
C40 C25 N8 131.3(3) . . ?
C40 C25 C36 122.8(3) . . ?
C45 C27 C22 119.5(3) . . ?
C23 C28 C30 122.2(3) . . ?
C46 C28 C23 114.3(3) . . ?
C46 C28 C30 123.5(3) . . ?
N5 C29 C22 126.6(3) . . ?
N8 C29 N5 108.5(3) . . ?
N8 C29 C22 124.9(3) . . ?
C31 C30 C28 121.7(3) . . ?
C31 C30 C39 117.2(3) . . ?
C39 C30 C28 121.1(3) . . ?
C67 C31 C30 121.7(3) . . ?
C42 C32 C39 122.1(3) . . ?
C50 C34 C75 123.0(4) . . ?
N5 C36 C25 106.1(3) . . ?
N5 C36 C50 131.0(3) . . ?
C25 C36 C50 122.6(3) . . ?
C54 C38 C21 121.4(4) . . ?
C76 C38 C21 120.6(4) . . ?
C76 C38 C54 118.0(4) . . ?
C32 C39 C30 120.8(3) . . ?
C25 C40 C43 122.4(3) . . ?
C25 C40 C75 114.7(3) . . ?
C75 C40 C43 122.9(3) . . ?
C52 C41 C69 121.9(4) . . ?
C32 C42 C1T 122.3(3) . . ?
C32 C42 C67 117.2(3) . . ?
C67 C42 C1T 120.5(3) . . ?
C57 C43 C40 122.3(4) . . ?
C57 C43 C64 117.0(4) . . ?
C64 C43 C40 120.6(3) . . ?
C27 C45 C17 120.9(3) . . ?
C28 C46 C47 123.1(3) . . ?
C21 C47 C46 123.0(3) . . ?
C34 C50 C36 114.4(4) . . ?
C34 C50 C52 124.6(4) . . ?
C36 C50 C52 120.9(3) . . ?
C41 C52 C50 121.3(4) . . ?
C41 C52 C83 117.4(4) . . ?
C83 C52 C50 121.3(4) . . ?
C38 C54 C65 120.2(4) . . ?
C43 C57 C73 122.0(4) . . ?
C2T C1T C42 111.1(3) . . ?
C2T C1T C3T 107.5(4) . . ?
C3T C1T C42 110.3(4) . . ?
C4T C1T C42 107.7(4) . . ?
C4T C1T C2T 110.3(4) . . ?
C4T C1T C3T 109.9(5) . . ?
C65 C61 C13T 121.7(4) . . ?
C77 C61 C65 117.2(4) . . ?
C77 C61 C13T 121.2(5) . . ?
C84 C64 C43 121.2(4) . . ?
C61 C65 C54 121.9(4) . . ?
C31 C67 C42 121.0(3) . . ?
C73 C68 C9T 120.7(4) . . ?
C84 C68 C73 117.5(4) . . ?
C84 C68 C9T 121.8(4) . . ?
C41 C69 C85 121.1(5) . . ?
C57 C73 C68 120.8(4) . . ?
C40 C75 C34 122.4(4) . . ?
C38 C76 C77 121.2(4) . . ?
C61 C77 C76 121.5(5) . . ?
C85 C5T C8T 111.8(5) . . ?
C6T C5T C85 111.3(5) . . ?
C6T C5T C8T 106.5(5) . . ?
C7T C5T C85 107.6(4) . . ?
C7T C5T C8T 105.1(6) . . ?
C7T C5T C6T 114.5(6) . . ?
C103 C83 C52 120.2(5) . . ?
C68 C84 C64 121.5(4) . . ?
C69 C85 C5T 119.8(5) . . ?
C103 C85 C69 116.4(4) . . ?
C103 C85 C5T 123.7(5) . . ?
C85 C103 C83 122.8(5) . . ?
C61 C13T C16T 111.6(4) . . ?
C61 C13T C16U 108.0(5) . . ?
C14T C13T C61 114.4(5) . . ?
C14T C13T C15T 117.8(6) . . ?
C14T C13T C16T 103.5(5) . . ?
C15T C13T C61 109.2(4) . . ?
C15T C13T C16T 99.0(5) . . ?
C14U C13T C61 114.0(5) . . ?
C14U C13T C15U 124.8(7) . . ?
C14U C13T C16U 103.9(7) . . ?
C15U C13T C61 104.9(5) . . ?
C15U C13T C16U 99.3(7) . . ?
C51 O2 C58 113.9(3) . . ?
C100 O3 C55 114.5(3) . . ?
C63 O4 C53 112.7(3) . . ?
C56 O7 C60 116.6(3) . . ?
C44 O9 C48 116.6(3) . . ?
C108 O13 C72 117.8(4) . . ?
C62 O14 C86 118.8(3) . . ?
C71 O15 C78 115.5(3) . . ?
O9 C44 C56 115.6(3) . . ?
O9 C44 C66 124.3(4) . . ?
C66 C44 C56 120.0(4) . . ?
O9 C48 C55 107.3(3) . . ?
O2 C51 C53 110.1(3) . . ?
O4 C53 C51 109.3(3) . . ?
O3 C55 C48 109.1(3) . . ?
O7 C56 C44 116.8(4) . . ?
O7 C56 C91 124.0(4) . . ?
C91 C56 C44 119.2(4) . . ?
O2 C58 C86 108.9(3) . . ?
O7 C60 C63 110.1(3) . . ?
O14 C62 C71 116.6(3) . . ?
O14 C62 C88 125.2(4) . . ?
C71 C62 C88 118.1(4) . . ?
O4 C63 C60 109.5(4) . . ?
C44 C66 C104 120.1(5) . . ?
O15 C71 C62 115.8(4) . . ?
C82 C71 O15 123.3(4) . . ?
C82 C71 C62 120.8(4) . . ?
O13 C72 C78 111.2(4) . . ?
O15 C78 C72 108.6(4) . . ?
C71 C82 C99 119.6(5) . . ?
O14 C86 C58 111.6(3) . . ?
C95 C88 C62 120.5(5) . . ?
C101 C91 C56 120.5(5) . . ?
C99 C95 C88 121.5(5) . . ?
C95 C99 C82 119.3(5) . . ?
C108 C100 O3 118.8(4) . . ?
C104 C101 C91 120.3(5) . . ?
C101 C104 C66 119.9(5) . . ?
O13 C108 C100 119.7(4) . . ?
F1 B1 F2 106.9(5) . . ?
F4 B1 F1 111.3(5) . . ?
F4 B1 F2 110.6(5) . . ?
F4 B1 F3 112.7(6) . . ?
F3 B1 F1 110.7(4) . . ?
F3 B1 F2 104.4(4) . . ?
C80 C74 C90 120.3(5) . . ?
C89 C80 C74 120.7(6) . . ?
C80 C89 C97 119.9(7) . . ?
C74 C90 C109 117.9(6) . . ?
C74 C90 C14 121.5(8) . . ?
C109 C90 C14 120.6(8) . . ?
C109 C97 C89 120.4(7) . . ?
C97 C109 C90 120.7(7) . . ?
C68 C9T C11T 108.6(6) . . ?
C68 C9T C12T 111.3(6) . . ?
C68 C9T C11U 105.6(7) . . ?
C10T C9T C68 115.5(6) . . ?
C10T C9T C11T 111.0(9) . . ?
C10T C9T C12T 106.3(8) . . ?
C12T C9T C11T 103.5(8) . . ?
C10U C9T C68 111.7(6) . . ?
C10U C9T C11U 116.4(10) . . ?
C10U C9T C12U 112.4(11) . . ?
C12U C9T C68 105.2(6) . . ?
C12U C9T C11U 104.6(9) . . ?
C7W C2W C1W 121.0(12) . . ?
C7W C2W C3W 120.0 . . ?
C3W C2W C1W 118.7(11) . . ?
C2W C7W C6W 120.0 . . ?
C5W C6W C7W 120.0 . . ?
C6W C5W C4W 120.0 . . ?
C3W C4W C5W 120.0 . . ?
C4W C3W C2W 120.0 . . ?
C5 C3 C2 118.0(12) . . ?
C5 C3 C13 120.0 . . ?
C13 C3 C2 122.0(12) . . ?
C6 C5 C3 120.0 . . ?
C5 C6 C8 120.0 . . ?
C6 C8 C9 120.0 . . ?
C13 C9 C8 120.0 . . ?
C9 C13 C3 120.0 . . ?
C15 C1A C1F 125.6(13) . . ?
C15 C1A C1B 114.1(13) . . ?
C1F C1A C1B 120.0 . . ?
C1E C1F C1A 120.0 . . ?
C1F C1E C1D 120.0 . . ?
C1C C1D C1E 120.0 . . ?
C1D C1C C1B 120.0 . . ?
C1C C1B C1A 120.0 . . ?
F9 B3 F12 105.0(7) . . ?
F10 B3 F9 106.5(9) . . ?
F10 B3 F11 108.4(9) . . ?
F10 B3 F12 113.8(10) . . ?
F11 B3 F9 111.8(9) . . ?
F11 B3 F12 111.3(8) . . ?
F10A B3 F9A 101.1(13) . . ?
F11A B3 F9A 113.8(11) . . ?
F11A B3 F10A 105.6(12) . . ?
F12A B3 F9A 108.9(14) . . ?
F12A B3 F10A 112.1(14) . . ?
F12A B3 F11A 114.6(12) . . ?
F9B B3 F10B 101.3(13) . . ?
F9B B3 F11B 114.4(15) . . ?
F9B B3 F12B 112.9(14) . . ?
F11B B3 F10B 102.2(12) . . ?
F12B B3 F10B 112.4(13) . . ?
F12B B3 F11B 112.5(12) . . ?
F3 B1A F1 111.9(10) . . ?
F3 B1A F2A 108.6(13) . . ?
F2A B1A F1 112.4(12) . . ?
F4A B1A F1 110.1(14) . . ?
F4A B1A F3 101.4(13) . . ?
F4A B1A F2A 112.0(15) . . ?
C7X C2X C1X 118.3(16) . . ?
C3X C2X C1X 118.5(15) . . ?
C3X C2X C7X 121.9(12) . . ?
C6X C7X C2X 117.9(13) . . ?
C5X C6X C7X 120.2(14) . . ?
C4X C5X C6X 120.6(14) . . ?
C5X C4X C3X 119.3(13) . . ?
C2X C3X C4X 118.8(12) . . ?
C7Y C2Y C1Y 118(2) . . ?
C3Y C2Y C1Y 118.6(18) . . ?
C3Y C2Y C7Y 120.9(14) . . ?
C6Y C7Y C2Y 118.5(16) . . ?
C5Y C6Y C7Y 119.2(15) . . ?
C4Y C5Y C6Y 120.7(14) . . ?
C5Y C4Y C3Y 120.0(14) . . ?
C2Y C3Y C4Y 118.7(14) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
