data_yb058j

_publ_section_related_literature ?

_publ_contact_author_name 'Yassine Beldjoudi'

_publ_contact_letter 
;
Please consider this CIF for publication. I certify that this contibution is the
original work of those listed as authors; that it has not been published
before (in any language or medium) and is not being considered for publication
elsewhere; that all authors concur with and are aware of the submission; that
all workers involved in the study are listed as authors or given proper credit
in the acknowledgements; that I have obtained permission for and acknowledged
the source of any excerpts from other copyright works; and that to the best of
my knowledge the paper contains no statements which are libellous, unlawful or
in any way actionable. All coauthors have made significant scientific
contributions to the work reported, including the ideas and their execution,
and share responsibility and accountability for the results.
;


_publ_requested_category ?

_publ_requested_journal ?

_publ_contact_author_fax ?

_publ_contact_author_phone ?

_publ_contact_author_email 'Yassine.beldjoudi@northwestern.edu'

_publ_contact_author_address

;
2145 Sheridan Rd, Evanston, IL 60208
;


_publ_section_title
;
Supramolecular Tessellations by a Rigid Naphthalene Diimide Triangle
;

_publ_section_abstract
;
?
;


# Loop of author details

loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
_publ_author_email
'Beldjoudi, Yassine'
;
2145 Sheridan Rd, Evanston, IL 60208
;
.
;
Yassine.Beldjoud@northwestern.edu
;
'Stoddart, Fraser'
;
2145 Sheridan Rd, Evanston, IL 60208
;
.
;
stoddart@northwestern.edu
;




_audit_update_record
;
2019-07-24 # Formatted by publCIF

;
_publcif_datablock.id '{07854da5-e58b-4c6c-a784-0a52f1e336c3}'

# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents

 section 
;
Chemical context
; 
;

;
 section 
;
Structural commentary
; 
;

;
 section 
;
Supramolecular features
; 
;

;
 section 
;
Database survey
; 
;

;
 section 
;
Synthesis and crystallization
; 
;

;
 section 
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;

# publcif _publ_body_element loop end
_audit_creation_date               2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Bourhis, L. J., Dolomanov, O. V., Gildea, R. J., Howard, J. A. K. & Puschmann,
H. (2015). Acta Cryst. A71, 59--75.

Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann,
H. (2009). J. Appl. Cryst. 42, 339--341.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           '3(C6 H4 S4), C60 H42 N6 O12, 1(C H2 Cl2)'
_chemical_formula_sum              'C79 H52 Cl2 N6 O12 S12'
_chemical_formula_weight           1732.88
_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'
 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        monoclinic
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/n 1'
_space_group_name_Hall             '-P 2yn'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                     18.1136(10)
_cell_length_b                     15.6480(9)
_cell_length_c                     27.3059(15)
_cell_angle_alpha                  90
_cell_angle_beta                   91.229(4)
_cell_angle_gamma                  90
_cell_volume                       7737.8(7)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      9498
_cell_measurement_temperature      100(2)
_cell_measurement_theta_max        67.454
_cell_measurement_theta_min        3.740
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      4.339
_exptl_absorpt_correction_T_max    1.0000
_exptl_absorpt_correction_T_min    0.6191
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details    
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1034 before and 0.0737 after correction. The Ratio of minimum to maximum transmission is 0.6191. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              green
_exptl_crystal_colour_primary      green
_exptl_crystal_density_diffrn      1.488
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         Needle
_exptl_crystal_F_000               3560
_exptl_crystal_size_max            0.09
_exptl_crystal_size_mid            0.061
_exptl_crystal_size_min            0.061
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1025
_diffrn_reflns_av_unetI/netI       0.1045
_diffrn_reflns_Laue_measured_fraction_full  0.945
_diffrn_reflns_Laue_measured_fraction_max  0.945
_diffrn_reflns_limit_h_max         21
_diffrn_reflns_limit_h_min         -21
_diffrn_reflns_limit_k_max         9
_diffrn_reflns_limit_k_min         -18
_diffrn_reflns_limit_l_max         31
_diffrn_reflns_limit_l_min         -32
_diffrn_reflns_number              37431
_diffrn_reflns_point_group_measured_fraction_full  0.945
_diffrn_reflns_point_group_measured_fraction_max  0.945
_diffrn_reflns_theta_full          65.402
_diffrn_reflns_theta_max           65.402
_diffrn_reflns_theta_min           3.255
_diffrn_ambient_temperature        99.99
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.945
_diffrn_measured_fraction_theta_max  0.945
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         '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                  10990
_reflns_number_total               12570
_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 V8.38A (?, 2016)'
_computing_data_collection         'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction          'SAINT V8.38A (?, 2016)'
_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      'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max           0.779
_refine_diff_density_min           -0.546
_refine_diff_density_rms           0.128
_refine_ls_extinction_coef         9891(122)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.044
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       1077
_refine_ls_number_reflns           12570
_refine_ls_number_restraints       277
_refine_ls_R_factor_all            0.2057
_refine_ls_R_factor_gt             0.1947
_refine_ls_restrained_S_all        1.043
_refine_ls_shift/su_max            0.929
_refine_ls_shift/su_mean           0.012
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0400P)²+45.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.3720
_refine_ls_wR_factor_ref           0.3780
_refine_special_details            
'Distance restraints and rigid-bond restrains (ShELX Keyword RIGU) were imposed on the highly disordered cyclohexane moeities of the NDI triangle.  Displacement restrains where imposed on both the macrocycle and the TTF molecules. A Shelx FLAT command was imposed on the disordered TTF rings. ADP restraints using ISOR were imposed. The solvent (dichloromethane) inside the cavity is disordered and refined using an occ of 0.33. Restrains are used to stabilise the dischloromethane molecules.'

_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl2-C79
 1.78 with sigma of 0.02
 C80-Cl4
 1.78 with sigma of 0.02
 Cl3-C80
 1.78 with sigma of 0.02
 C79-Cl1
 1.78 with sigma of 0.02
 S8-C72
 1.76 with sigma of 0.02
 C71-C72
 1.36 with sigma of 0.02
 S10-C75
 1.76 with sigma of 0.02
 C78-C77
 1.36 with sigma of 0.02
 C47-C46
 1.36 with sigma of 0.02
 C49-C50
 1.54 with sigma of 0.01
 C44-C43
 1.54 with sigma of 0.01
 C56-C55
 1.54 with sigma of 0.02
 C45-C46
 1.54 with sigma of 0.02
 C48-C47
 1.54 with sigma of 0.02
 C43-C48
 1.54 with sigma of 0.02
 C44-C45
 1.54 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C54-C53
 1.54 with sigma of 0.02
 C56-C57
 1.54 with sigma of 0.02
 C58-C59
 1.54 with sigma of 0.02
 C60-C55
 1.54 with sigma of 0.02
 S10-C73
 1.76 with sigma of 0.02
 C75-S9
 1.76 with sigma of 0.02
 C75-S10
 1.76 with sigma of 0.02
 S9-C74
 1.76 with sigma of 0.02
 S4-C66
 1.76 with sigma of 0.02
 C75-C73
 2.6 with sigma of 0.02
 S11-C77
 1.76 with sigma of 0.02
 C64-C63
 1.36 with sigma of 0.02
 C76-C75
 1.36 with sigma of 0.02
 S5-C69
 1.72 with sigma of 0.02
 C69-S6
 1.72 with sigma of 0.02
 C49-C54
 1.54 with sigma of 0.02
 C53-C52
 1.54 with sigma of 0.02
 C51-C50
 1.54 with sigma of 0.02
 C46-C47
 1.54 with sigma of 0.02
 C0AA-Cl0A
 1.78 with sigma of 0.02
 C15-O5
 1.24 with sigma of 0.02
 Cl18-C0AA
 1.78 with sigma of 0.02
 Cl1-Cl2
 2.6 with sigma of 0.02
 C42-O12
 1.24 with sigma of 0.02
 N1-C44
 1.48 with sigma of 0.02
 N6-C43
 1.48 with sigma of 0.02
 C56-N5
 1.48 with sigma of 0.02
 C55-N4
 1.48 with sigma of 0.02
 N3-C50
 1.48 with sigma of 0.02
 C49-N2
 1.48 with sigma of 0.02
 C1AA-C2AA
 1.54 with sigma of 0.02
 C2AA-C1AA
 1.54 with sigma of 0.02
 C54-C2AA
 1.54 with sigma of 0.02
 N2-C2AA
 1.48 with sigma of 0.02
 C44-C3AA
 1.55 with sigma of 0.02
3. Restrained angles
 C75-S10-C73
 fixed at 0.66 with sigma of 0.02
4. Restrained planarity
 S10, C73, C74, S9
 with sigma of 0.01
 S5, C67, C68, S6
 with sigma of 0.005
5. Uiso/Uaniso restraints and constraints
Cl0A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C52) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(C50) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(C55) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(Cl2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.1
Uanis(C79) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(Cl1) \\sim Ueq: with sigma of 0.25 and sigma for terminal atoms of 0.1
Uanis(C72) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.1
Uanis(C47) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(Cl4) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.1
Uanis(Cl3) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.2
Uanis(C80) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(C75) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C0AA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C2AA) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C1AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C3AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
6. Rigid body (RIGU) restrains
 C44, C43, C48, C47, C46, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C49, C54, C53, C52, C51, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C57, C58, C59, C60, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C47, C48, C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50, C51, C52, C53, C54, C49
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: H51A(0.5) H51B(0.5) H51D(0.5) H51C(0.5) H54D(0.5) H54C(0.5)
 H54B(0.5) H54A(0.5) C43(0.5) H43(0.5) H44(0.5) H44A(0.5) H48A(0.5) H48B(0.5)
 H48C(0.5) H48D(0.5) C50(0.5) H50(0.5) C49(0.5) H49(0.5) Cl2(0.33333)
 C79(0.33333) H79A(0.33333) H79B(0.33333) Cl1(0.33333) C80(0.33333)
 H80A(0.33333) H80B(0.33333) Cl3(0.33333) Cl4(0.33333) C0AA(0.33333)
 H0AA(0.33333) H0AB(0.33333) Cl0A(0.33333) Cl18(0.33333) C1AA(0.5) H1AA(0.5)
 C2AA(0.5) H2AA(0.5) C3AA(0.5) H3AA(0.5)
8.a Ternary CH refined with riding coordinates:
 C43(H43), C44(H44), C44(H44A), C56(H56), C50(H50), C49(H49), C55(H55),
 C1AA(H1AA), C2AA(H2AA), C3AA(H3AA)
8.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C60(H60A,H60B), C53(H53A,H53B), C51(H51A,H51B), C51(H51D,
 H51C), C54(H54D,H54C), C54(H54B,H54A), C59(H59A,H59B), C58(H58A,H58B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C48(H48C,H48D),
  C52(H52A,H52B), C79(H79A,H79B), C80(H80A,H80B), C0AA(H0AA,H0AB)
8.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C7(H7), C35(H35), C6(H6), C36(H36), C20(H20), C34(H34),
 C37(H37), C25(H25), C21(H21), C26(H26), C66(H66), C62(H62), C78(H78), C61(H61),
  C68(H68), C71(H71), C67(H67), C65(H65), C72(H72), C77(H77), C73(H73), C74(H74)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       iterative
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 S4 S 0.4239(4) 0.4536(5) 0.0122(3) 0.144(2) Uani 1 1 d D . . . .
 S3 S 0.2647(4) 0.4752(4) -0.0136(3) 0.134(2) Uani 1 1 d . . . . .
 S11 S 0.5674(4) 0.2681(4) 0.4338(3) 0.143(2) Uani 1 1 d D . . . .
 S1 S 0.2478(4) 0.2745(5) -0.0205(3) 0.140(2) Uani 1 1 d . . . . .
 S7 S -0.1159(4) 0.2675(5) 0.3722(3) 0.142(2) Uani 1 1 d . . . . .
 S2 S 0.4045(5) 0.2493(5) 0.0050(3) 0.154(3) Uani 1 1 d . . . . .
 S5 S -0.1102(4) 0.4680(5) 0.3635(3) 0.151(3) Uani 1 1 d D . . . .
 S8 S -0.1685(4) 0.2520(6) 0.2683(3) 0.164(3) Uani 1 1 d D . . . .
 S6 S -0.1626(4) 0.4575(6) 0.2596(3) 0.147(3) Uani 1 1 d D . . . .
 N2 N 0.4787(7) 0.3688(11) 0.1487(5) 0.090(4) Uani 1 1 d D . . . .
 C18 C 0.4415(9) 0.3693(10) 0.3268(6) 0.077(4) Uani 1 1 d . . . . .
 N1 N 0.0980(7) 0.3668(11) 0.0909(5) 0.089(4) Uani 1 1 d D . . . .
 C4 C 0.2473(9) 0.3639(10) 0.1165(6) 0.080(4) Uani 1 1 d . . . . .
 O9 O 0.1120(8) 0.2251(10) 0.4092(6) 0.124(5) Uani 1 1 d . . . . .
 N6 N -0.0103(11) 0.3722(12) 0.1653(6) 0.097(5) Uani 1 1 d D . . . .
 N5 N 0.1222(8) 0.3655(11) 0.4095(5) 0.089(4) Uani 1 1 d D . . . .
 C23 C 0.3897(8) 0.3688(10) 0.3629(6) 0.073(4) Uani 1 1 d . . . . .
 C9 C 0.3219(8) 0.3682(9) 0.1286(5) 0.066(4) Uani 1 1 d . . . . .
 C5 C 0.2084(9) 0.4456(10) 0.1098(6) 0.080(4) Uani 1 1 d . . . . .
 C32 C 0.0690(10) 0.3695(10) 0.3108(6) 0.079(4) Uani 1 1 d . . . . .
 C39 C 0.0414(9) 0.3706(11) 0.2660(5) 0.074(4) Uani 1 1 d . . . . .
 C3 C 0.2116(8) 0.2927(9) 0.1066(7) 0.076(4) Uani 1 1 d . . . . .
 C33 C 0.0824(10) 0.4452(12) 0.3391(8) 0.093(5) Uani 1 1 d . . . . .
 O1 O 0.0979(8) 0.5148(11) 0.0910(6) 0.133(5) Uani 1 1 d . . . . .
 O12 O -0.0207(10) 0.5082(11) 0.1646(7) 0.147(6) Uani 1 1 d D . . . .
 C29 C 0.1051(10) 0.2934(12) 0.3856(9) 0.095(6) Uani 1 1 d . . . . .
 C8 C 0.3601(9) 0.4421(11) 0.1319(7) 0.083(5) Uani 1 1 d . . . . .
 O4 O 0.4788(8) 0.2205(11) 0.1440(6) 0.134(5) Uani 1 1 d . . . . .
 C11 C 0.3259(11) 0.2190(11) 0.1203(8) 0.106(6) Uani 1 1 d . . . . .
 H11 H 0.352829 0.167017 0.122745 0.127 Uiso 1 1 calc R . . . .
 C10 C 0.3610(8) 0.2918(11) 0.1288(6) 0.078(4) Uani 1 1 d . . . . .
 C31 C 0.0765(9) 0.2905(11) 0.3385(7) 0.085(5) Uani 1 1 d . . . . .
 O3 O 0.4798(8) 0.5137(11) 0.1478(7) 0.139(6) Uani 1 1 d . . . . .
 C14 C 0.4399(11) 0.2939(15) 0.1408(7) 0.100(6) Uani 1 1 d . . . . .
 O10 O 0.1188(8) 0.5083(11) 0.4079(6) 0.133(5) Uani 1 1 d . . . . .
 C13 C 0.4383(11) 0.4517(14) 0.1424(7) 0.094(5) Uani 1 1 d . . . . .
 C17 C 0.4673(10) 0.2914(13) 0.3083(7) 0.092(5) Uani 1 1 d . . . . .
 C19 C 0.4662(10) 0.4465(12) 0.3069(7) 0.090(5) Uani 1 1 d . . . . .
 C24 C 0.3638(10) 0.2940(13) 0.3851(7) 0.094(5) Uani 1 1 d . . . . .
 C22 C 0.3651(9) 0.4436(11) 0.3861(7) 0.088(5) Uani 1 1 d . . . . .
 O8 O 0.2834(8) 0.2251(12) 0.4382(6) 0.138(6) Uani 1 1 d . . . . .
 C40 C 0.0231(10) 0.2909(14) 0.2400(7) 0.096(5) Uani 1 1 d . . . . .
 C30 C 0.1098(10) 0.4451(12) 0.3851(8) 0.092(6) Uani 1 1 d . . . . .
 C1 C 0.1296(10) 0.4448(15) 0.0973(7) 0.092(5) Uani 1 1 d . . . . .
 C12 C 0.2513(12) 0.2156(12) 0.1081(8) 0.110(7) Uani 1 1 d . . . . .
 H12 H 0.227685 0.162647 0.101012 0.133 Uiso 1 1 calc R . . . .
 C7 C 0.3229(10) 0.5186(11) 0.1275(8) 0.106(7) Uani 1 1 d . . . . .
 H7 H 0.348536 0.571098 0.131719 0.128 Uiso 1 1 calc R . . . .
 O7 O 0.2870(9) 0.5177(14) 0.4395(6) 0.154(7) Uani 1 1 d . . . . .
 N3 N 0.5389(8) 0.3639(14) 0.2477(5) 0.101(5) Uani 1 1 d D . . . .
 C38 C 0.0283(12) 0.4444(12) 0.2410(9) 0.106(6) Uani 1 1 d . . . . .
 C27 C 0.3068(12) 0.2905(18) 0.4224(9) 0.136(10) Uani 1 1 d . . . . .
 C41 C -0.0056(13) 0.298(2) 0.1881(10) 0.143(11) Uani 1 1 d . . . . .
 C35 C 0.0565(11) 0.2207(13) 0.3135(7) 0.097(5) Uani 1 1 d . . . . .
 H35 H 0.060561 0.167991 0.330583 0.117 Uiso 1 1 calc R . . . .
 O2 O 0.0999(9) 0.2286(11) 0.0841(7) 0.138(5) Uani 1 1 d . . . . .
 C2 C 0.1348(14) 0.2933(14) 0.0944(8) 0.112(7) Uani 1 1 d . . . . .
 C42 C 0.0010(13) 0.442(2) 0.1875(9) 0.156(13) Uani 1 1 d D . . . .
 O11 O -0.0245(8) 0.2251(11) 0.1653(6) 0.133(5) Uani 1 1 d . . . . .
 C16 C 0.5162(11) 0.2896(18) 0.2696(8) 0.106(6) Uani 1 1 d . . . . .
 S9 S 0.5601(7) 0.4705(6) 0.4446(5) 0.263(8) Uani 1 1 d D . . . .
 C6 C 0.2471(11) 0.5185(10) 0.1166(6) 0.092(5) Uani 1 1 d . . . . .
 H6 H 0.221974 0.571663 0.114028 0.111 Uiso 1 1 calc R . . . .
 C57 C 0.0869(12) 0.3521(17) 0.4966(8) 0.132(8) Uani 1 1 d D U . . .
 H57A H 0.047426 0.393901 0.488561 0.158 Uiso 1 1 calc R . . . .
 H57B H 0.065241 0.294231 0.493458 0.158 Uiso 1 1 calc R . . . .
 O5 O 0.5463(7) 0.5143(13) 0.2556(6) 0.152(7) Uani 1 1 d D . . . .
 C36 C 0.0315(13) 0.2163(13) 0.2674(9) 0.116(7) Uani 1 1 d . . . . .
 H36 H 0.019412 0.162533 0.253279 0.139 Uiso 1 1 calc R . . . .
 C60 C 0.2470(12) 0.3652(11) 0.5283(7) 0.103(5) Uani 1 1 d D U . . .
 H60A H 0.275176 0.311949 0.534437 0.123 Uiso 1 1 calc R . . . .
 H60B H 0.281699 0.413155 0.534239 0.123 Uiso 1 1 calc R . . . .
 C15 C 0.5197(11) 0.4498(17) 0.2710(8) 0.121(8) Uani 1 1 d D . . . .
 C20 C 0.4435(11) 0.5207(13) 0.3285(8) 0.100(6) Uani 1 1 d . . . . .
 H20 H 0.461665 0.573958 0.317197 0.120 Uiso 1 1 calc R . . . .
 C53 C 0.6896(11) 0.3699(17) 0.1236(8) 0.137(8) Uani 1 1 d D U . . .
 H53A H 0.712346 0.324513 0.103673 0.164 Uiso 1 1 calc R . . . .
 H53B H 0.706772 0.425806 0.111331 0.164 Uiso 1 1 calc R . . . .
 C34 C 0.0666(12) 0.5285(13) 0.3133(9) 0.116(7) Uani 1 1 d . . . . .
 H34 H 0.073088 0.582040 0.329227 0.139 Uiso 1 1 calc R . . . .
 O6 O 0.5457(8) 0.2215(14) 0.2543(7) 0.165(8) Uani 1 1 d . . . . .
 C37 C 0.0419(15) 0.5225(18) 0.2643(10) 0.146(10) Uani 1 1 d . . . . .
 H37 H 0.034091 0.573713 0.246233 0.175 Uiso 1 1 calc R . . . .
 C25 C 0.3946(11) 0.2209(11) 0.3681(9) 0.110(7) Uani 1 1 d . . . . .
 H25 H 0.382729 0.168771 0.383998 0.132 Uiso 1 1 calc R . . . .
 C51 C 0.6666(10) 0.3533(18) 0.2214(7) 0.140(9) Uani 1 1 d D U . . .
 H51A H 0.668901 0.408025 0.239575 0.168 Uiso 0.5 1 calc R . P A 1
 H51B H 0.686220 0.307852 0.243328 0.168 Uiso 0.5 1 calc R . P A 1
 H51D H 0.687413 0.389293 0.248144 0.168 Uiso 0.5 1 calc R . P B 2
 H51C H 0.664628 0.293436 0.233107 0.168 Uiso 0.5 1 calc R . P B 2
 C21 C 0.3964(10) 0.5188(12) 0.3650(8) 0.099(6) Uani 1 1 d . . . . .
 H21 H 0.382089 0.572178 0.378422 0.119 Uiso 1 1 calc R . . . .
 C64 C 0.3402(14) 0.4095(11) -0.0003(7) 0.112(7) Uani 1 1 d D . . . .
 C63 C 0.3306(13) 0.3260(13) -0.0044(6) 0.112(7) Uani 1 1 d D . . . .
 C26 C 0.4408(12) 0.2176(12) 0.3302(9) 0.107(7) Uani 1 1 d . . . . .
 H26 H 0.455822 0.163530 0.318183 0.128 Uiso 1 1 calc R . . . .
 C54 C 0.6046(10) 0.3646(17) 0.1181(7) 0.133(8) Uani 1 1 d D U . . .
 H54D H 0.587630 0.421485 0.106588 0.159 Uiso 0.5 1 calc R . P C 2
 H54C H 0.593954 0.324134 0.090955 0.159 Uiso 0.5 1 calc R . P C 2
 H54B H 0.589251 0.405942 0.092341 0.159 Uiso 0.5 1 calc R . P D 1
 H54A H 0.592292 0.306921 0.105446 0.159 Uiso 0.5 1 calc R . P D 1
 C66 C 0.3879(15) 0.5532(10) 0.0204(11) 0.146(10) Uani 1 1 d D . . . .
 H66 H 0.416181 0.599833 0.032749 0.175 Uiso 1 1 calc R . . . .
 C59 C 0.1901(13) 0.370(3) 0.5668(11) 0.218(19) Uani 1 1 d D U . . .
 H59A H 0.196564 0.425066 0.584663 0.262 Uiso 1 1 calc R . . . .
 H59B H 0.198666 0.323516 0.590497 0.262 Uiso 1 1 calc R . . . .
 C62 C 0.2710(18) 0.1688(17) -0.0090(14) 0.179(15) Uani 1 1 d . . . . .
 H62 H 0.236373 0.123182 -0.009155 0.215 Uiso 1 1 calc R . . . .
 C58 C 0.1114(12) 0.3652(18) 0.5478(8) 0.139(9) Uani 1 1 d D U . . .
 H58A H 0.088202 0.318705 0.566639 0.167 Uiso 1 1 calc R . . . .
 H58B H 0.087460 0.418796 0.558333 0.167 Uiso 1 1 calc R . . . .
 C70 C -0.1378(10) 0.3210(16) 0.3168(12) 0.140(11) Uani 1 1 d . . . . .
 C43 C -0.0383(11) 0.348(2) 0.1166(7) 0.099(8) Uani 0.5 1 d D U P E 1
 H43 H -0.035686 0.284082 0.117899 0.118 Uiso 0.5 1 calc R . P E 1
 C44 C 0.0195(8) 0.3694(17) 0.0783(6) 0.130(8) Uani 1 1 d D U . . .
 H44 H 0.014235 0.432905 0.080741 0.156 Uiso 0.5 1 calc R . P E 1
 H44A H 0.012682 0.306735 0.083649 0.156 Uiso 0.5 1 calc R . P E 2
 C45 C 0.0012(11) 0.3637(15) 0.0241(7) 0.127(7) Uani 1 1 d D U . . .
 H45A H 0.026593 0.410983 0.007304 0.152 Uiso 1 1 calc R . . . .
 H45B H 0.021575 0.309415 0.011556 0.152 Uiso 1 1 calc R . . . .
 C46 C -0.0795(11) 0.3674(19) 0.0105(8) 0.151(10) Uani 1 1 d D U . . .
 H46A H -0.087786 0.419668 -0.009245 0.181 Uiso 1 1 calc R . . . .
 H46B H -0.090666 0.318042 -0.011067 0.181 Uiso 1 1 calc R . . . .
 C47 C -0.1322(14) 0.367(2) 0.0484(7) 0.153(8) Uani 1 1 d D U . . .
 H47A H -0.165485 0.318708 0.040799 0.184 Uiso 1 1 calc R . . . .
 H47B H -0.162066 0.419587 0.042952 0.184 Uiso 1 1 calc R . . . .
 C48 C -0.1185(10) 0.3633(15) 0.1022(7) 0.116(6) Uani 1 1 d D U . . .
 H48A H -0.148938 0.316872 0.115863 0.140 Uiso 0.5 1 calc R . P E 1
 H48B H -0.134805 0.417707 0.116965 0.140 Uiso 0.5 1 calc R . P E 1
 H48C H -0.126028 0.303996 0.113649 0.140 Uiso 0.5 1 calc R . P E 2
 H48D H -0.154420 0.400468 0.118811 0.140 Uiso 0.5 1 calc R . P E 2
 C52 C 0.7140(13) 0.359(2) 0.1767(7) 0.153(8) Uani 1 1 d D U . . .
 H52A H 0.744947 0.307259 0.177404 0.184 Uiso 1 1 calc R . . . .
 H52B H 0.748099 0.407678 0.183351 0.184 Uiso 1 1 calc R . . . .
 C56 C 0.1462(10) 0.3610(19) 0.4603(6) 0.138(9) Uani 1 1 d D U . . .
 H56 H 0.150100 0.297444 0.457813 0.165 Uiso 1 1 calc R . . . .
 C78 C 0.6232(17) 0.1883(19) 0.3688(12) 0.151(10) Uani 1 1 d D . . . .
 H78 H 0.629238 0.143426 0.345864 0.182 Uiso 1 1 calc R . . . .
 C61 C 0.3382(18) 0.1598(16) -0.0004(10) 0.141(10) Uani 1 1 d . . . . .
 H61 H 0.356619 0.103392 0.003685 0.170 Uiso 1 1 calc R . . . .
 C76 C 0.6174(11) 0.3350(12) 0.3933(8) 0.112(7) Uani 1 1 d D . . F 2
 C50 C 0.5857(12) 0.333(2) 0.2075(10) 0.085(8) Uani 0.5 1 d D U P G 1
 H50 H 0.579124 0.270161 0.203152 0.102 Uiso 0.5 1 calc R . P G 1
 C68 C -0.1318(11) 0.547(2) 0.2769(11) 0.157(10) Uani 1 1 d . U . . .
 H68 H -0.130725 0.594161 0.254724 0.189 Uiso 1 1 calc R . . . .
 C69 C -0.1348(12) 0.4113(15) 0.3121(6) 0.145(10) Uani 1 1 d D . . . .
 C71 C -0.123(2) 0.164(2) 0.3503(12) 0.177(13) Uani 1 1 d D . . . .
 H71 H -0.112191 0.115022 0.369828 0.213 Uiso 1 1 calc R . . . .
 C67 C -0.1082(11) 0.557(2) 0.3215(11) 0.167(11) Uani 1 1 d . U . . .
 H67 H -0.089595 0.610316 0.332254 0.200 Uiso 1 1 calc R . . . .
 C49 C 0.5551(13) 0.340(3) 0.1595(13) 0.122(12) Uani 0.5 1 d D U P G 2
 H49 H 0.556004 0.276228 0.164185 0.147 Uiso 0.5 1 calc R . P G 2
 C65 C 0.3134(17) 0.5603(14) 0.0073(13) 0.178(14) Uani 1 1 d . . . . .
 H65 H 0.289506 0.614075 0.010155 0.214 Uiso 1 1 calc R . . . .
 C55 C 0.2269(10) 0.3665(19) 0.4744(7) 0.144(8) Uani 1 1 d D U . . .
 H55 H 0.223871 0.430285 0.475006 0.173 Uiso 1 1 calc R . . . .
 S10 S 0.6660(8) 0.4837(11) 0.3596(5) 0.341(12) Uani 1 1 d D . . . .
 C72 C -0.1446(17) 0.1593(17) 0.3035(11) 0.169(11) Uani 1 1 d D U . . .
 H72 H -0.147550 0.104783 0.288283 0.203 Uiso 1 1 calc R . . . .
 N4 N 0.2792(9) 0.3703(13) 0.4356(6) 0.099(5) Uiso 1 1 d D . . . .
 C28 C 0.3107(13) 0.4484(19) 0.4215(7) 0.127(10) Uani 1 1 d . . . . .
 S12 S 0.6714(5) 0.2832(12) 0.3531(3) 0.247(7) Uani 1 1 d . . . . .
 C75 C 0.6126(11) 0.4201(12) 0.3994(7) 0.145(9) Uani 1 1 d D U . . .
 C77 C 0.581(2) 0.1674(15) 0.4053(14) 0.207(18) Uani 1 1 d D . . . .
 H77 H 0.563167 0.112753 0.414171 0.248 Uiso 1 1 calc R . . . .
 Cl2 Cl 0.246(3) 0.291(3) 0.2456(14) 0.25(2) Uani 0.3333 1 d D U P H 1
 C79 C 0.232(5) 0.213(3) 0.292(2) 0.13(3) Uani 0.3333 1 d D U P H 1
 H79A H 0.253832 0.229365 0.323923 0.150 Uiso 0.3333 1 calc R . P H 1
 H79B H 0.179617 0.196707 0.295081 0.150 Uiso 0.3333 1 calc R . P H 1
 Cl1 Cl 0.284(2) 0.134(2) 0.2613(11) 0.243(18) Uani 0.3333 1 d D U P H 1
 C80 C 0.255(4) 0.356(4) 0.288(3) 0.099(18) Uani 0.3333 1 d D U P I 2
 H80A H 0.209869 0.362750 0.307424 0.118 Uiso 0.3333 1 calc R . P I 2
 H80B H 0.296910 0.358033 0.311647 0.118 Uiso 0.3333 1 calc R . P I 2
 Cl3 Cl 0.252(4) 0.247(4) 0.267(3) 0.43(5) Uani 0.3333 1 d D U P I 2
 Cl4 Cl 0.262(4) 0.451(5) 0.253(3) 0.42(5) Uani 0.3333 1 d D U P I 2
 C73 C 0.6171(18) 0.5782(14) 0.3706(13) 0.32(3) Uani 1 1 d D U . . .
 H73 H 0.622669 0.629071 0.352082 0.379 Uiso 1 1 calc R . . . .
 C74 C 0.566(2) 0.5697(18) 0.4125(12) 0.220(16) Uani 1 1 d D U . . .
 H74 H 0.536317 0.616855 0.421932 0.264 Uiso 1 1 calc R . . . .
 C0AA C 0.247(7) 0.486(2) 0.249(5) 0.19(5) Uani 0.3333 1 d D U P J 3
 H0AA H 0.253562 0.491087 0.213051 0.225 Uiso 0.3333 1 calc R . P J 3
 H0AB H 0.193261 0.489374 0.253139 0.225 Uiso 0.3333 1 calc R . P J 3
 Cl0A Cl 0.274(3) 0.590(4) 0.2681(16) 0.42(5) Uani 0.3333 1 d D U P J 3
 Cl18 Cl 0.2611(17) 0.374(2) 0.2565(11) 0.148(9) Uani 0.3333 1 d D . P J 3
 C1AA C 0.5863(16) 0.385(2) 0.2063(11) 0.069(8) Uani 0.5 1 d D U P G 2
 H1AA H 0.586754 0.448618 0.201067 0.083 Uiso 0.5 1 calc R . P G 2
 C2AA C 0.5576(11) 0.380(3) 0.1615(9) 0.090(11) Uani 0.5 1 d D U P G 1
 H2AA H 0.563410 0.442566 0.169089 0.108 Uiso 0.5 1 calc R . P G 1
 C3AA C -0.0358(16) 0.394(2) 0.1164(10) 0.071(9) Uani 0.5 1 d D U P E 2
 H3AA H -0.037612 0.457479 0.115742 0.085 Uiso 0.5 1 calc R . P E 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
 S4 C64 1.69(3) . ?
 S4 C66 1.707(16) . ?
 S3 C64 1.74(2) . ?
 S3 C65 1.69(3) . ?
 S11 C76 1.78(2) . ?
 S11 C77 1.778(17) . ?
 S1 C63 1.75(2) . ?
 S1 C62 1.73(3) . ?
 S7 C70 1.77(3) . ?
 S7 C71 1.73(3) . ?
 S2 C63 1.81(2) . ?
 S2 C61 1.85(3) . ?
 S5 C69 1.712(17) . ?
 S5 C67 1.80(3) . ?
 S8 C70 1.79(3) . ?
 S8 C72 1.788(18) . ?
 S6 C68 1.58(3) . ?
 S6 C69 1.672(16) . ?
 N2 C14 1.38(3) . ?
 N2 C13 1.50(2) . ?
 N2 C49 1.480(19) . ?
 N2 C2AA 1.474(19) . ?
 C18 C23 1.38(2) . ?
 C18 C17 1.40(2) . ?
 C18 C19 1.40(2) . ?
 N1 C1 1.36(2) . ?
 N1 C2 1.33(3) . ?
 N1 C44 1.458(15) . ?
 C4 C9 1.39(2) . ?
 C4 C5 1.47(2) . ?
 C4 C3 1.31(2) . ?
 O9 C29 1.25(2) . ?
 N6 C41 1.33(4) . ?
 N6 C42 1.27(3) . ?
 N6 C43 1.463(18) . ?
 N6 C3AA 1.44(4) . ?
 N5 C29 1.34(2) . ?
 N5 C30 1.43(2) . ?
 N5 C56 1.445(16) . ?
 C23 C24 1.41(2) . ?
 C23 C22 1.41(2) . ?
 C9 C8 1.35(2) . ?
 C9 C10 1.39(2) . ?
 C5 C1 1.46(2) . ?
 C5 C6 1.35(2) . ?
 C32 C39 1.31(2) . ?
 C32 C33 1.43(2) . ?
 C32 C31 1.46(2) . ?
 C39 C40 1.47(3) . ?
 C39 C38 1.36(2) . ?
 C3 C12 1.40(2) . ?
 C3 C2 1.42(3) . ?
 C33 C30 1.34(2) . ?
 C33 C34 1.51(3) . ?
 O1 C1 1.25(2) . ?
 O12 C42 1.262(17) . ?
 C29 C31 1.38(3) . ?
 C8 C13 1.45(2) . ?
 C8 C7 1.38(2) . ?
 O4 C14 1.35(2) . ?
 C11 C10 1.32(2) . ?
 C11 C12 1.39(3) . ?
 C10 C14 1.46(2) . ?
 C31 C35 1.34(2) . ?
 O3 C13 1.23(2) . ?
 O10 C30 1.18(2) . ?
 C17 C16 1.39(3) . ?
 C17 C26 1.39(3) . ?
 C19 C15 1.39(3) . ?
 C19 C20 1.37(3) . ?
 C24 C27 1.47(3) . ?
 C24 C25 1.36(3) . ?
 C22 C21 1.43(3) . ?
 C22 C28 1.40(3) . ?
 O8 C27 1.19(2) . ?
 C40 C41 1.50(3) . ?
 C40 C36 1.39(3) . ?
 C7 C6 1.40(2) . ?
 O7 C28 1.27(3) . ?
 N3 C16 1.37(3) . ?
 N3 C15 1.53(3) . ?
 N3 C50 1.481(18) . ?
 N3 C1AA 1.47(3) . ?
 C38 C42 1.53(3) . ?
 C38 C37 1.40(3) . ?
 C27 N4 1.40(3) . ?
 C41 O11 1.33(3) . ?
 C35 C36 1.33(3) . ?
 O2 C2 1.22(2) . ?
 C16 O6 1.27(3) . ?
 S9 C75 1.762(16) . ?
 S9 C74 1.788(19) . ?
 C57 C58 1.47(3) . ?
 C57 C56 1.484(17) . ?
 O5 C15 1.197(16) . ?
 C60 C59 1.49(3) . ?
 C60 C55 1.509(17) . ?
 C20 C21 1.33(3) . ?
 C53 C54 1.547(17) . ?
 C53 C52 1.514(13) . ?
 C34 C37 1.41(3) . ?
 C25 C26 1.35(3) . ?
 C51 C52 1.512(17) . ?
 C51 C50 1.539(18) . ?
 C51 C1AA 1.58(4) . ?
 C64 C63 1.323(17) . ?
 C54 C49 1.51(2) . ?
 C54 C2AA 1.495(19) . ?
 C66 C65 1.39(3) . ?
 C59 C58 1.508(18) . ?
 C62 C61 1.24(4) . ?
 C70 C69 1.42(3) . ?
 C43 C44 1.532(10) . ?
 C43 C48 1.517(18) . ?
 C44 C45 1.511(17) . ?
 C44 C3AA 1.508(18) . ?
 C45 C46 1.502(17) . ?
 C46 C47 1.422(13) . ?
 C47 C48 1.484(17) . ?
 C48 C3AA 1.61(4) . ?
 C56 C55 1.505(17) . ?
 C78 S12 1.78(3) . ?
 C78 C77 1.305(19) . ?
 C76 S12 1.69(3) . ?
 C76 C75 1.345(17) . ?
 C50 C2AA 1.54(5) . ?
 C68 C67 1.29(3) . ?
 C71 C72 1.330(18) . ?
 C49 C1AA 1.56(6) . ?
 C55 N4 1.437(16) . ?
 S10 C75 1.775(13) . ?
 S10 C73 1.752(19) . ?
 N4 C28 1.41(3) . ?
 Cl2 C79 1.78(2) . ?
 C79 Cl1 1.77(2) . ?
 C80 Cl3 1.79(2) . ?
 C80 Cl4 1.78(2) . ?
 C73 C74 1.49(5) . ?
 C0AA Cl0A 1.77(2) . ?
 C0AA Cl18 1.78(2) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 C64 S4 C66 93.1(12) . . ?
 C65 S3 C64 89.6(12) . . ?
 C77 S11 C76 99.8(14) . . ?
 C62 S1 C63 101.0(14) . . ?
 C71 S7 C70 97.8(14) . . ?
 C63 S2 C61 90.8(13) . . ?
 C69 S5 C67 83.4(13) . . ?
 C70 S8 C72 91.3(16) . . ?
 C68 S6 C69 91.8(14) . . ?
 C14 N2 C13 118.1(15) . . ?
 C14 N2 C49 104(3) . . ?
 C14 N2 C2AA 129(2) . . ?
 C49 N2 C13 138(3) . . ?
 C2AA N2 C13 113(2) . . ?
 C23 C18 C17 119.3(15) . . ?
 C23 C18 C19 120.7(16) . . ?
 C19 C18 C17 119.9(17) . . ?
 C1 N1 C44 114.3(17) . . ?
 C2 N1 C1 124.0(16) . . ?
 C2 N1 C44 121.8(19) . . ?
 C9 C4 C5 116.7(14) . . ?
 C3 C4 C9 124.2(15) . . ?
 C3 C4 C5 118.8(15) . . ?
 C41 N6 C43 102.4(19) . . ?
 C41 N6 C3AA 131(2) . . ?
 C42 N6 C41 122.0(19) . . ?
 C42 N6 C43 135(2) . . ?
 C42 N6 C3AA 107(2) . . ?
 C29 N5 C30 118.4(15) . . ?
 C29 N5 C56 119.3(19) . . ?
 C30 N5 C56 122.1(18) . . ?
 C18 C23 C24 123.7(16) . . ?
 C18 C23 C22 123.1(15) . . ?
 C24 C23 C22 112.7(16) . . ?
 C4 C9 C10 117.0(14) . . ?
 C8 C9 C4 123.6(15) . . ?
 C8 C9 C10 118.4(15) . . ?
 C1 C5 C4 119.0(15) . . ?
 C6 C5 C4 118.2(15) . . ?
 C6 C5 C1 122.8(17) . . ?
 C39 C32 C33 123.4(16) . . ?
 C39 C32 C31 121.8(15) . . ?
 C33 C32 C31 114.0(15) . . ?
 C32 C39 C40 121.1(16) . . ?
 C32 C39 C38 122.6(17) . . ?
 C38 C39 C40 116.3(16) . . ?
 C4 C3 C12 118.3(16) . . ?
 C4 C3 C2 121.0(15) . . ?
 C12 C3 C2 120.7(16) . . ?
 C32 C33 C34 115.7(17) . . ?
 C30 C33 C32 124.2(17) . . ?
 C30 C33 C34 120.1(18) . . ?
 O9 C29 N5 117(2) . . ?
 O9 C29 C31 119.0(19) . . ?
 N5 C29 C31 124.2(17) . . ?
 C9 C8 C13 126.9(16) . . ?
 C9 C8 C7 119.3(15) . . ?
 C7 C8 C13 113.7(17) . . ?
 C10 C11 C12 122.6(16) . . ?
 C9 C10 C14 118.6(17) . . ?
 C11 C10 C9 119.8(15) . . ?
 C11 C10 C14 121.5(17) . . ?
 C29 C31 C32 119.2(16) . . ?
 C35 C31 C32 114.0(17) . . ?
 C35 C31 C29 126.7(18) . . ?
 N2 C14 C10 123.1(18) . . ?
 O4 C14 N2 116.6(18) . . ?
 O4 C14 C10 120(2) . . ?
 C8 C13 N2 114.0(17) . . ?
 O3 C13 N2 111.8(17) . . ?
 O3 C13 C8 134.2(19) . . ?
 C16 C17 C18 121(2) . . ?
 C26 C17 C18 116.5(18) . . ?
 C26 C17 C16 123(2) . . ?
 C15 C19 C18 122.4(18) . . ?
 C20 C19 C18 117.6(17) . . ?
 C20 C19 C15 119(2) . . ?
 C23 C24 C27 125(2) . . ?
 C25 C24 C23 114.2(17) . . ?
 C25 C24 C27 120(2) . . ?
 C23 C22 C21 111.7(16) . . ?
 C28 C22 C23 126.3(19) . . ?
 C28 C22 C21 121.6(19) . . ?
 C39 C40 C41 118(2) . . ?
 C36 C40 C39 115.4(17) . . ?
 C36 C40 C41 127(2) . . ?
 C33 C30 N5 119.3(15) . . ?
 O10 C30 N5 117.8(19) . . ?
 O10 C30 C33 123(2) . . ?
 N1 C1 C5 116.4(17) . . ?
 O1 C1 N1 125.5(17) . . ?
 O1 C1 C5 118.0(19) . . ?
 C11 C12 C3 118.0(16) . . ?
 C8 C7 C6 119.7(15) . . ?
 C16 N3 C15 119.3(15) . . ?
 C16 N3 C50 103(2) . . ?
 C16 N3 C1AA 135(2) . . ?
 C50 N3 C15 137(2) . . ?
 C1AA N3 C15 105(2) . . ?
 C39 C38 C42 120.7(19) . . ?
 C39 C38 C37 119(2) . . ?
 C37 C38 C42 120(2) . . ?
 O8 C27 C24 123(3) . . ?
 O8 C27 N4 123(3) . . ?
 N4 C27 C24 114.1(17) . . ?
 N6 C41 C40 121(2) . . ?
 N6 C41 O11 121(2) . . ?
 O11 C41 C40 117(3) . . ?
 C36 C35 C31 128(2) . . ?
 N1 C2 C3 120.5(17) . . ?
 O2 C2 N1 116(2) . . ?
 O2 C2 C3 123(2) . . ?
 N6 C42 C38 121(2) . . ?
 O12 C42 N6 115(2) . . ?
 O12 C42 C38 123(3) . . ?
 N3 C16 C17 121(2) . . ?
 O6 C16 C17 123(3) . . ?
 O6 C16 N3 116(2) . . ?
 C75 S9 C74 90.4(18) . . ?
 C5 C6 C7 122.3(16) . . ?
 C58 C57 C56 114(2) . . ?
 C35 C36 C40 119.8(19) . . ?
 C59 C60 C55 122.1(18) . . ?
 C19 C15 N3 115.3(16) . . ?
 O5 C15 C19 125(3) . . ?
 O5 C15 N3 120(2) . . ?
 C21 C20 C19 120.6(18) . . ?
 C52 C53 C54 111.0(19) . . ?
 C37 C34 C33 116.2(19) . . ?
 C38 C37 C34 123(2) . . ?
 C26 C25 C24 124.2(18) . . ?
 C52 C51 C50 111.6(18) . . ?
 C52 C51 C1AA 108(2) . . ?
 C20 C21 C22 125.9(18) . . ?
 S4 C64 S3 119.8(11) . . ?
 C63 C64 S4 122.2(19) . . ?
 C63 C64 S3 118(2) . . ?
 S1 C63 S2 110.9(11) . . ?
 C64 C63 S1 125.9(19) . . ?
 C64 C63 S2 123.2(19) . . ?
 C25 C26 C17 121.7(18) . . ?
 C49 C54 C53 123(2) . . ?
 C2AA C54 C53 119.7(17) . . ?
 C65 C66 S4 114.3(18) . . ?
 C60 C59 C58 115(2) . . ?
 C61 C62 S1 112(2) . . ?
 C57 C58 C59 127(2) . . ?
 S7 C70 S8 114.1(15) . . ?
 C69 C70 S7 122.9(18) . . ?
 C69 C70 S8 123(2) . . ?
 N6 C43 C44 109.6(17) . . ?
 N6 C43 C48 120.3(19) . . ?
 C48 C43 C44 116.9(17) . . ?
 N1 C44 C43 120.7(16) . . ?
 N1 C44 C45 114.9(15) . . ?
 N1 C44 C3AA 120.2(18) . . ?
 C45 C44 C43 121.1(16) . . ?
 C3AA C44 C45 123.8(19) . . ?
 C46 C45 C44 115.5(18) . . ?
 C47 C46 C45 119(2) . . ?
 C46 C47 C48 128(2) . . ?
 C47 C48 C43 113.7(18) . . ?
 C47 C48 C3AA 111.2(19) . . ?
 C51 C52 C53 128(2) . . ?
 N5 C56 C57 116.0(16) . . ?
 N5 C56 C55 120.8(15) . . ?
 C57 C56 C55 123.2(17) . . ?
 C77 C78 S12 134(2) . . ?
 C62 C61 S2 124(2) . . ?
 S12 C76 S11 115.4(12) . . ?
 C75 C76 S11 118.0(18) . . ?
 C75 C76 S12 126.5(19) . . ?
 N3 C50 C51 107.9(17) . . ?
 N3 C50 C2AA 105(2) . . ?
 C2AA C50 C51 114(2) . . ?
 C67 C68 S6 119(3) . . ?
 S6 C69 S5 123.2(14) . . ?
 C70 C69 S5 116.7(17) . . ?
 C70 C69 S6 119.8(18) . . ?
 C72 C71 S7 114(3) . . ?
 C68 C67 S5 120(3) . . ?
 N2 C49 C54 109.8(19) . . ?
 N2 C49 C1AA 110(3) . . ?
 C54 C49 C1AA 106(3) . . ?
 C66 C65 S3 121.3(17) . . ?
 C56 C55 C60 117.5(16) . . ?
 N4 C55 C60 124.7(17) . . ?
 N4 C55 C56 117.8(16) . . ?
 C73 S10 C75 94.8(12) . . ?
 C71 C72 S8 122(3) . . ?
 C27 N4 C55 113(2) . . ?
 C27 N4 C28 123.8(17) . . ?
 C28 N4 C55 121(2) . . ?
 C22 C28 N4 116.1(18) . . ?
 O7 C28 C22 124(3) . . ?
 O7 C28 N4 119(2) . . ?
 C76 S12 C78 87.1(12) . . ?
 S9 C75 S10 119.2(14) . . ?
 C76 C75 S9 124.6(15) . . ?
 C76 C75 S10 116.2(16) . . ?
 C78 C77 S11 102(2) . . ?
 Cl1 C79 Cl2 93.7(14) . . ?
 Cl4 C80 Cl3 129(6) . . ?
 C74 C73 S10 112(2) . . ?
 C73 C74 S9 120(3) . . ?
 Cl0A C0AA Cl18 146(7) . . ?
 N3 C1AA C51 106(2) . . ?
 N3 C1AA C49 108(2) . . ?
 C49 C1AA C51 113(2) . . ?
 N2 C2AA C54 110.9(18) . . ?
 N2 C2AA C50 116(2) . . ?
 C54 C2AA C50 113(2) . . ?
 N6 C3AA C44 112(2) . . ?
 N6 C3AA C48 116(2) . . ?
 C44 C3AA C48 113(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

loop_
# start Validation Reply Form
_vrf_SHFSU01_yb058j
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: The struture could not be converged due to the high disorder 
of the guest solvent inside the cavity of the macrocycle.
;
_vrf_PLAT080_yb058j
;
PROBLEM: Maximum Shift/Error ............................       0.93 Why ? 
RESPONSE: High disorder of solvent inside the macrocycle cavity
;
_vrf_PLAT029_yb058j
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.945 Why?  
RESPONSE: Several crystals are tested . The crystal of limited quality does 
not diffract X-ray well and hence the numbers of observed reflections are 
rather low. We cut off the data at 0.85 Ang due to the low intensity at higher 
angles. However we are confident on the quality of the struture and its packing.
;
_vrf_PLAT082_yb058j
;
PROBLEM: High R1 Value ..................................       0.19 Report
RESPONSE: Due to the disorder. Several atoms are contrained to be isotropic.
;
_vrf_PLAT084_yb058j
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: High disorder in the lattice
;
_vrf_PLAT201_yb058j
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: Due to the disorder.
;
_vrf_PLAT230_yb058j
;
PROBLEM: Hirshfeld Test Diff for    N6       --C41      .        8.5 s.u.  
RESPONSE: Due to the disorder.
;
_vrf_PLAT234_yb058j
;
PROBLEM: Large Hirshfeld Difference O10      --C30      .       0.26 Ang.  
RESPONSE: ...
;
_vrf_PLAT241_yb058j
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C59 Check 
RESPONSE: Due to the disorder.
;
_vrf_PLAT242_yb058j
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C60 Check 
RESPONSE: Due to the disorder.
;
_vrf_PLAT260_yb058j
;
PROBLEM: Large Average Ueq of Residue Including       Cl3      0.316 Check 
RESPONSE: Due to the disorder.
;
_vrf_PLAT340_yb058j
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0291 Ang.  
RESPONSE: Due to the disorder.
;
_vrf_PLAT410_yb058j
;
PROBLEM: Short Intra H...H Contact  H56      ..H57B     .       1.84 Ang.  
RESPONSE: due to the slight elongation of the Carbonyl bond.
;
# end Validation Reply Form
