#------------------------------------------------------------------------------
#$Date: 2019-06-12 12:40:06 +0300 (Wed, 12 Jun 2019) $
#$Revision: 215893 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/13/1551375.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1551375
loop_
_publ_author_name
'Max J. Kory'
'Michael Worle'
'Thomas Weber'
'Payam Payamyar'
'Stan W. van de Poll'
'Julia Dshemuchadse'
'Nils Trapp'
'Dieter Schluter'
_publ_section_title
;
 Gram-scale synthesis of two-dimensional polymer crystals and their
 structure analysis by X-ray diffraction
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              779
_journal_page_last               784
_journal_paper_doi               10.1038/nchem.2007
_journal_volume                  6
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         '1.5(C96 H48 N12 O12), 4(C6 H4.01 N2)'
_chemical_formula_sum            'C168 H88 N26 O18'
_chemical_formula_weight         2758.64
_chemical_name_systematic
poly(1,5,10-(1,8)trianthracena-2,4,5,8,9,11-hexaoxa-3,7(1,3,5)ditriazinabicyclo[3.3.3]undecaphane)
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.4976(6)
_cell_length_b                   19.4976(6)
_cell_length_c                   29.0508(16)
_cell_measurement_reflns_used    5284
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      63.472
_cell_measurement_theta_min      3.027
_cell_volume                     9564.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    OLEX2
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'D8 ApexII Dual Source with Cu-radiation'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'double mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18657
_diffrn_reflns_point_group_measured_fraction_full 0.876
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.002
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0827 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.7730.
The λ/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             4266
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 1822 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.17(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         6751
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0987
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.3055
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.791
_reflns_Friedel_fraction_max     0.803
_reflns_number_gt                4672
_reflns_number_total             6751
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nchem.2007-s4.cif
_cod_data_source_block           3
_cod_original_cell_volume        9564.2(8)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               1551375
_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.
;
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N3, N3C}
{C17, C17C}
{C18, C18C}
{N19, C23C}
{C20, C20C}
{C21, C21C}
{C22, C22C}
{C23, N19C}
{N3A, N3D}
{C17A, C17D}
{C18A, C18D}
{N19A, C23D}
{C20A, C20D}
{C21A, C21D}
{C22A, C22D}
{C23A, N19D}
{N3B, N3E}
{C17B, C17E}
{C18B, C18E}
{N19B, C23E}
{C20B, C20E}
{C21B, C21E}
{C22B, C22E}
{C23B, N19E}
3. Restrained planarity
 N3A, C17A, C18A, N19A, C20A, C21A, C22A, C23A
 with sigma of 0.1
 N3A, C17A, C18A, N19A, C20A, C21A, C22A, C23A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C17B) = Uiso(C18B) = Uiso(N19B) = Uiso(C20B) = Uiso(C21B) = Uiso(C22B) =
Uiso(C23B) = Uiso(C17E) = Uiso(C18E) = Uiso(C23E) = Uiso(C20E) = Uiso(C21E) =
Uiso(C22E) = Uiso(N19E) = Uiso(N3B) = Uiso(N3E)
Uiso(N3) = Uiso(C17) = Uiso(C18) = Uiso(N19) = Uiso(C20) = Uiso(C21) =
Uiso(C22) = Uiso(C23) = Uiso(N3C) = Uiso(C17C) = Uiso(C18C) = Uiso(C23C) =
Uiso(C20C) = Uiso(C21C) = Uiso(C22C) = Uiso(N19C) = Uiso(N3A) = Uiso(C17A) =
Uiso(C18A) = Uiso(N19A) = Uiso(C20A) = Uiso(C21A) = Uiso(C22A) = Uiso(C23A) =
Uiso(N3D) = Uiso(C17D) = Uiso(C18D) = Uiso(C23D) = Uiso(C20D) = Uiso(C21D) =
Uiso(C22D) = Uiso(N19D)
5. Same fragment restrains
{N3B, C17B, C18B, N19B, C20B, C21B, C22B, C23B}
as
{N3, C17, C18, N19, C20, C21, C22, C23}
6. Others
 Sof(H21D)=0.505*(1-FVAR(2))
 Sof(N3A)=Sof(C17A)=Sof(C18A)=Sof(N19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=
 Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(N3D)=Sof(C17D)=Sof(C18D)=
 Sof(N19D)=Sof(C20D)=Sof(H20D)=Sof(C21D)=Sof(C22D)=Sof(H22D)=Sof(C23D)=
 Sof(H23D)=0.5*(1-FVAR(2))
 Sof(N3)=Sof(C17)=Sof(C18)=Sof(N19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23)=Sof(N3C)=Sof(C17C)=Sof(C18C)=Sof(N19C)=Sof(C20C)=
 Sof(H20C)=Sof(C21C)=Sof(H21C)=Sof(C22C)=Sof(H22C)=Sof(C23C)=Sof(H23C)=0.5*
 FVAR(2)
 Sof(H21)=0.505*FVAR(2)
 Fixed Sof: N3B(0.16667) C17B(0.16667) C18B(0.16667) N19B(0.16667)
 C20B(0.16667) H20B(0.16667) C21B(0.16667) H21B(0.16667) C22B(0.16667)
 H22B(0.16667) C23B(0.16667) H23B(0.16667) N3E(0.16667) C17E(0.16667)
 C18E(0.16667) N19E(0.16667) C20E(0.16667) H20E(0.16667) C21E(0.16667)
 H21E(0.16667) C22E(0.16667) H22E(0.16667) C23E(0.16667) H23E(0.16667)
7.a Ternary CH refined with riding coordinates:
 C6(H6), C6A(H6A), C13(H13), C13A(H13A)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A), C3(H3), C3A(H3A), C4(H4), C4A(H4A), C8(H8), C8A(H8A),
 C9(H9), C9A(H9A), C10(H10), C10A(H10A), C2B(H2B), C3B(H3B), C4B(H4B), C6B(H6B),
  C8B(H8B), C9B(H9B), C10B(H10B), C13B(H13B), C20(H20), C21(H21), C22(H22),
 C23(H23), C20C(H20C), C21C(H21C), C22C(H22C), C23C(H23C), C20A(H20A),
 C21A(H21A), C22A(H22A), C23A(H23A), C20D(H20D), C21D(H21D), C22D(H22D),
 C23D(H23D), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C20E(H20E),
 C21E(H21E), C22E(H22E), C23E(H23E)
7.c Fitted hexagon refined as free rotating group:
 C18(N19,C20,C21,C22,C23), C18A(N19A,C20A,C21A,C22A,C23A), C18B(N19B,C20B,C21B,
 C22B,C23B)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4310(3) 0.6118(4) 0.2051(3) 0.071(2) Uani 1 1 d . . . . .
O1A O 0.5544(3) 0.3690(3) 0.2003(3) 0.071(2) Uani 1 1 d . . . . .
O2 O 0.4452(4) 0.6298(4) 0.3699(3) 0.078(2) Uani 1 1 d . . . . .
O2A O 0.5689(4) 0.3875(4) 0.3659(3) 0.077(2) Uani 1 1 d . . . . .
N1 N 0.3018(4) 0.5859(4) 0.2058(3) 0.060(2) Uani 1 1 d . . . . .
N1A N 0.6869(4) 0.4114(3) 0.1995(4) 0.066(3) Uani 1 1 d . . . . .
N2 N 0.4128(4) 0.7239(4) 0.3697(3) 0.066(2) Uani 1 1 d . . . . .
N2A N 0.6973(5) 0.4143(4) 0.3651(4) 0.071(2) Uani 1 1 d . . . . .
C1 C 0.4026(5) 0.5297(5) 0.2086(4) 0.068(3) Uani 1 1 d . . . . .
C1A C 0.5737(5) 0.4493(6) 0.1990(5) 0.074(3) Uani 1 1 d . . . . .
C2 C 0.3646(6) 0.4787(7) 0.1706(4) 0.078(3) Uani 1 1 d . . . . .
H2 H 0.3517 0.4976 0.1437 0.094 Uiso 1 1 calc R U . . .
C2A C 0.5946(6) 0.4884(6) 0.1575(5) 0.078(3) Uani 1 1 d . . . . .
H2A H 0.5988 0.4632 0.1305 0.093 Uiso 1 1 calc R U . . .
C3 C 0.3468(7) 0.4007(7) 0.1738(5) 0.083(3) Uani 1 1 d . . . . .
H3 H 0.3216 0.3655 0.1488 0.099 Uiso 1 1 calc R U . . .
C3A C 0.6096(7) 0.5666(7) 0.1564(6) 0.094(4) Uani 1 1 d . . . . .
H3A H 0.6249 0.5957 0.1284 0.112 Uiso 1 1 calc R U . . .
C4 C 0.3649(5) 0.3743(5) 0.2122(5) 0.082(4) Uani 1 1 d . . . . .
H4 H 0.3518 0.3204 0.2138 0.098 Uiso 1 1 calc R U . . .
C4A C 0.6022(6) 0.6004(6) 0.1952(5) 0.083(4) Uani 1 1 d . . . . .
H4A H 0.6145 0.6541 0.1941 0.100 Uiso 1 1 calc R U . . .
C5 C 0.4036(5) 0.4253(5) 0.2509(5) 0.073(3) Uani 1 1 d . . . . .
C5A C 0.5772(5) 0.5598(5) 0.2368(4) 0.070(3) Uani 1 1 d . . . . .
C6 C 0.4368(5) 0.4034(6) 0.2904(4) 0.072(3) Uani 1 1 d . . . . .
H6 H 0.4101 0.3443 0.2923 0.086 Uiso 1 1 calc R U . . .
C6A C 0.5614(6) 0.5922(5) 0.2806(5) 0.077(3) Uani 1 1 d . . . . .
H6A H 0.5890 0.6512 0.2780 0.092 Uiso 1 1 calc R U . . .
C7 C 0.4180(6) 0.4348(6) 0.3343(5) 0.086(4) Uani 1 1 d . . . . .
C7A C 0.5931(5) 0.5723(5) 0.3210(4) 0.074(3) Uani 1 1 d . . . . .
C8 C 0.3940(6) 0.3952(7) 0.3747(6) 0.085(4) Uani 1 1 d . . . . .
H8 H 0.3837 0.3423 0.3764 0.102 Uiso 1 1 calc R U . . .
C8A C 0.6290(6) 0.6217(6) 0.3562(5) 0.082(3) Uani 1 1 d . . . . .
H8A H 0.6406 0.6751 0.3542 0.098 Uiso 1 1 calc R U . . .
C9 C 0.3841(7) 0.4303(8) 0.4133(5) 0.089(4) Uani 1 1 d . . . . .
H9 H 0.3664 0.4012 0.4412 0.106 Uiso 1 1 calc R U . . .
C9A C 0.6500(7) 0.5958(7) 0.3963(5) 0.091(4) Uani 1 1 d . . . . .
H9A H 0.6752 0.6313 0.4211 0.110 Uiso 1 1 calc R U . . .
C10 C 0.4004(7) 0.5098(8) 0.4116(6) 0.092(4) Uani 1 1 d . . . . .
H10 H 0.3942 0.5348 0.4381 0.111 Uiso 1 1 calc R U . . .
C10A C 0.6334(7) 0.5177(7) 0.3992(5) 0.090(4) Uani 1 1 d . . . . .
H10A H 0.6470 0.4986 0.4257 0.108 Uiso 1 1 calc R U . . .
C11 C 0.4246(5) 0.5483(6) 0.3716(5) 0.075(3) Uani 1 1 d . . . . .
C11A C 0.5968(6) 0.4697(6) 0.3623(4) 0.072(3) Uani 1 1 d . . . . .
C12 C 0.4355(5) 0.5153(6) 0.3317(5) 0.074(3) Uani 1 1 d . . . . .
C12A C 0.5777(5) 0.4933(6) 0.3227(4) 0.069(3) Uani 1 1 d . . . . .
C13 C 0.4676(5) 0.5599(5) 0.2867(5) 0.073(3) Uani 1 1 d . . . . .
H13 H 0.4587 0.6062 0.2862 0.088 Uiso 1 1 calc R U . . .
C13A C 0.5326(5) 0.4393(5) 0.2852(4) 0.073(3) Uani 1 1 d . . . . .
H13A H 0.5427 0.3938 0.2861 0.087 Uiso 1 1 calc R U . . .
C14 C 0.4212(5) 0.5047(5) 0.2478(4) 0.069(3) Uani 1 1 d . . . . .
C14A C 0.5627(5) 0.4813(5) 0.2392(5) 0.075(3) Uani 1 1 d . . . . .
C15 C 0.3790(5) 0.6367(5) 0.2065(4) 0.057(2) Uani 1 1 d . . . . .
C15A C 0.6126(4) 0.3533(5) 0.1995(4) 0.058(3) Uani 1 1 d . . . . .
C16 C 0.3849(5) 0.6468(6) 0.3699(4) 0.067(3) Uani 1 1 d . . . . .
C16A C 0.6214(5) 0.3613(6) 0.3658(4) 0.064(3) Uani 1 1 d . . . . .
O1B O 0.5375(4) 0.3415(4) 0.4821(3) 0.086(2) Uani 1 1 d . . . . .
O2B O 0.5431(4) 0.3539(4) 0.6497(3) 0.0817(19) Uani 1 1 d . . . . .
N1B N 0.6694(5) 0.4047(5) 0.4830(3) 0.079(2) Uani 1 1 d . . . . .
N2B N 0.6747(5) 0.4071(5) 0.6476(4) 0.078(2) Uani 1 1 d . . . . .
C1B C 0.4621(6) 0.2741(6) 0.4833(5) 0.082(3) Uani 1 1 d . . . . .
C2B C 0.4246(8) 0.2414(8) 0.4431(5) 0.098(4) Uani 1 1 d . . . . .
H2B H 0.4496 0.2636 0.4145 0.117 Uiso 1 1 calc R U . . .
C3B C 0.3482(11) 0.1741(12) 0.4439(9) 0.125(7) Uani 1 1 d . . . . .
H3B H 0.3228 0.1497 0.4159 0.150 Uiso 1 1 calc R U . . .
C4B C 0.3125(9) 0.1453(8) 0.4825(7) 0.106(6) Uani 1 1 d . . . . .
H4B H 0.2604 0.1008 0.4824 0.127 Uiso 1 1 calc R U . . .
C5B C 0.3504(6) 0.1798(6) 0.5254(5) 0.091(4) Uani 1 1 d . . . . .
C6B C 0.3101(6) 0.1532(6) 0.5693(6) 0.091(4) Uani 1 1 d . . . . .
H6B H 0.2565 0.1115 0.5694 0.109 Uiso 1 1 calc R U . . .
C7B C 0.3461(7) 0.1857(6) 0.6111(6) 0.095(4) Uani 1 1 d . . . . .
C8B C 0.3081(8) 0.1656(7) 0.6532(8) 0.110(5) Uani 1 1 d . . . . .
H8B H 0.2540 0.1254 0.6542 0.132 Uiso 1 1 calc R U . . .
C9B C 0.3444(9) 0.2006(9) 0.6926(7) 0.112(5) Uani 1 1 d . . . . .
H9B H 0.3174 0.1834 0.7212 0.135 Uiso 1 1 calc R U . . .
C10B C 0.4242(7) 0.2639(7) 0.6910(6) 0.101(4) Uani 1 1 d . . . . .
H10B H 0.4493 0.2910 0.7185 0.122 Uiso 1 1 calc R U . . .
C11B C 0.4650(6) 0.2864(6) 0.6507(5) 0.083(3) Uani 1 1 d . . . . .
C12B C 0.4280(6) 0.2529(6) 0.6099(4) 0.074(3) Uani 1 1 d . . . . .
C13B C 0.4661(5) 0.2802(5) 0.5676(4) 0.075(3) Uani 1 1 d . . . . .
H13B H 0.5190 0.3232 0.5667 0.090 Uiso 1 1 calc R U . . .
C14B C 0.4276(6) 0.2453(6) 0.5271(5) 0.079(3) Uani 1 1 d . . . . .
C15B C 0.6025(6) 0.3347(6) 0.4825(4) 0.078(3) Uani 1 1 d . . . . .
C16B C 0.6060(5) 0.3407(6) 0.6482(4) 0.071(2) Uani 1 1 d . . . . .
N3_a N 0.6464(14) 0.5272(14) 0.7111(7) 0.114(2) Uiso 0.275(5) 1 d D . P A 1
C17_a C 0.6190(18) 0.5249(18) 0.6797(10) 0.114(2) Uiso 0.275(5) 1 d D . P A 1
C18_a C 0.5791(11) 0.5260(13) 0.6389(5) 0.114(2) Uiso 0.275(5) 1 d DG . P A 1
N19_a N 0.5153(11) 0.5383(12) 0.6449(5) 0.114(2) Uiso 0.275(5) 1 d DG . P A 1
C20_a C 0.4758(11) 0.5448(14) 0.6067(6) 0.114(2) Uiso 0.275(5) 1 d DG . P A 1
H20_a H 0.4322 0.5532 0.6108 0.136 Uiso 0.275(5) 1 calc R U P A 1
C21_a C 0.5002(12) 0.5390(14) 0.5626(5) 0.114(2) Uiso 0.275(5) 1 d DG . P A 1
H21_a H 0.4732 0.5434 0.5366 0.136 Uiso 0.278(5) 1 calc R U P A 1
C22_a C 0.5640(12) 0.5267(14) 0.5567(5) 0.114(2) Uiso 0.275(5) 1 d DG . P A 1
H22_a H 0.5806 0.5227 0.5266 0.136 Uiso 0.275(5) 1 calc R U P A 1
C23_a C 0.6034(11) 0.5202(14) 0.5948(6) 0.114(2) Uiso 0.275(5) 1 d DG . P A 1
H23_a H 0.6470 0.5118 0.5908 0.136 Uiso 0.275(5) 1 calc R U P A 1
N3C_c N 0.6464(14) 0.5272(14) 0.7111(7) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
C17C_c C 0.6190(18) 0.5249(18) 0.6797(10) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
C18C_c C 0.5791(11) 0.5260(13) 0.6389(5) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
N19C_c N 0.6034(11) 0.5202(14) 0.5948(6) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
C20C_c C 0.4758(11) 0.5448(14) 0.6067(6) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
H20C_c H 0.4322 0.5532 0.6108 0.136 Uiso 0.275(5) 1 calc R U P A 3
C21C_c C 0.5002(12) 0.5390(14) 0.5626(5) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
H21C_c H 0.4732 0.5434 0.5366 0.136 Uiso 0.275(5) 1 calc R U P A 3
C22C_c C 0.5640(12) 0.5267(14) 0.5567(5) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
H22C_c H 0.5806 0.5227 0.5266 0.136 Uiso 0.275(5) 1 calc R U P A 3
C23C_c C 0.5153(11) 0.5383(12) 0.6449(5) 0.114(2) Uiso 0.275(5) 1 d . . P A 3
H23C_c H 0.4986 0.5423 0.6750 0.136 Uiso 0.275(5) 1 calc R U P A 3
N3A_b N 0.4850(17) 0.4753(17) 0.6857(10) 0.114(2) Uiso 0.225(5) 1 d . . P A 2
C17A_b C 0.5025(17) 0.4929(15) 0.6518(14) 0.114(2) Uiso 0.225(5) 1 d . . P A 2
C18A_b C 0.5342(13) 0.5208(15) 0.6054(5) 0.114(2) Uiso 0.225(5) 1 d G . P A 2
N19A_b N 0.4796(12) 0.5280(15) 0.5782(8) 0.114(2) Uiso 0.225(5) 1 d G . P A 2
C20A_b C 0.4865(13) 0.5299(16) 0.5305(7) 0.114(2) Uiso 0.225(5) 1 d G . P A 2
H20A_b H 0.4492 0.5349 0.5119 0.136 Uiso 0.225(5) 1 calc R U P A 2
C21A_b C 0.5481(14) 0.5246(15) 0.5101(5) 0.114(2) Uiso 0.225(5) 1 d G . P A 2
H21A_b H 0.5529 0.5259 0.4775 0.136 Uiso 0.225(5) 1 calc R U P A 2
C22A_b C 0.6028(13) 0.5174(16) 0.5373(7) 0.114(2) Uiso 0.225(5) 1 d G . P A 2
H22A_b H 0.6449 0.5137 0.5233 0.136 Uiso 0.225(5) 1 calc R U P A 2
C23A_b C 0.5959(13) 0.5155(17) 0.5849(7) 0.114(2) Uiso 0.225(5) 1 d G . P A 2
H23A_b H 0.6332 0.5105 0.6035 0.136 Uiso 0.225(5) 1 calc R U P A 2
N3D_d N 0.4850(17) 0.4753(17) 0.6857(10) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
C17D_d C 0.5025(17) 0.4929(15) 0.6518(14) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
C18D_d C 0.5342(13) 0.5208(15) 0.6054(5) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
N19D_d N 0.5959(13) 0.5155(17) 0.5849(7) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
C20D_d C 0.4865(13) 0.5299(16) 0.5305(7) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
H20D_d H 0.4492 0.5349 0.5119 0.136 Uiso 0.225(5) 1 calc R U P A 4
C21D_d C 0.5481(14) 0.5246(15) 0.5101(5) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
H21D_d H 0.5529 0.5259 0.4775 0.136 Uiso 0.227(5) 1 calc R U P A 4
C22D_d C 0.6028(13) 0.5174(16) 0.5373(7) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
H22D_d H 0.6449 0.5137 0.5233 0.136 Uiso 0.225(5) 1 calc R U P A 4
C23D_d C 0.4796(12) 0.5280(15) 0.5782(8) 0.114(2) Uiso 0.225(5) 1 d . . P A 4
H23D_d H 0.4374 0.5317 0.5921 0.136 Uiso 0.225(5) 1 calc R U P A 4
N3B N 0.686(3) 0.534(2) 0.7526(16) 0.137(7) Uiso 0.1667 1 d D . P A -1
C17B C 0.690(3) 0.483(3) 0.7564(19) 0.137(7) Uiso 0.1667 1 d D . P A -1
C18B C 0.691(2) 0.410(2) 0.7548(17) 0.137(7) Uiso 0.1667 1 d DG . P A -1
N19B N 0.7638(15) 0.414(2) 0.7574(16) 0.137(7) Uiso 0.1667 1 d DG . P A -1
C20B C 0.7678(17) 0.345(3) 0.7617(14) 0.137(7) Uiso 0.1667 1 d DG . P A -1
H20B H 0.8178 0.3479 0.7635 0.165 Uiso 0.1667 1 calc R U P A -1
C21B C 0.699(3) 0.272(2) 0.7635(18) 0.137(7) Uiso 0.1667 1 d DG . P A -1
H21B H 0.7013 0.2248 0.7664 0.165 Uiso 0.1667 1 calc R U P A -1
C22B C 0.6254(19) 0.2677(19) 0.7609(16) 0.137(7) Uiso 0.1667 1 d DG . P A -1
H22B H 0.5781 0.2178 0.7620 0.165 Uiso 0.1667 1 calc R U P A -1
C23B C 0.6214(14) 0.337(2) 0.7565(12) 0.137(7) Uiso 0.1667 1 d DG . P A -1
H23B H 0.5714 0.3338 0.7548 0.165 Uiso 0.1667 1 calc R U P A -1
N3E N 0.686(3) 0.534(2) 0.7526(16) 0.137(7) Uiso 0.1667 1 d . . P B -2
C17E C 0.690(3) 0.483(3) 0.7564(19) 0.137(7) Uiso 0.1667 1 d . . P B -2
C18E C 0.691(2) 0.410(2) 0.7548(17) 0.137(7) Uiso 0.1667 1 d . . P B -2
N19E N 0.6214(14) 0.337(2) 0.7565(12) 0.137(7) Uiso 0.1667 1 d . . P B -2
C20E C 0.7678(17) 0.345(3) 0.7617(14) 0.137(7) Uiso 0.1667 1 d . . P B -2
H20E H 0.8178 0.3479 0.7635 0.165 Uiso 0.1667 1 calc R U P B -2
C21E C 0.699(3) 0.272(2) 0.7635(18) 0.137(7) Uiso 0.1667 1 d . . P B -2
H21E H 0.7013 0.2248 0.7664 0.165 Uiso 0.1667 1 calc R U P B -2
C22E C 0.6254(19) 0.2677(19) 0.7609(16) 0.137(7) Uiso 0.1667 1 d . . P B -2
H22E H 0.5781 0.2178 0.7620 0.165 Uiso 0.1667 1 calc R U P B -2
C23E C 0.7638(15) 0.414(2) 0.7574(16) 0.137(7) Uiso 0.1667 1 d . . P B -2
H23E H 0.8111 0.4639 0.7563 0.165 Uiso 0.1667 1 calc R U P B -2
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'
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
C15 O1 C1 118.4(6) . .
C15A O1A C1A 118.3(6) . .
C16 O2 C11 118.0(7) . .
C16A O2A C11A 119.5(7) . .
C15 N1 C15 113.3(8) . 3_565
C15A N1A C15A 114.5(7) . 3_665
C16 N2 C16 109.6(8) . 2_665
C16A N2A C16A 110.1(8) . 3_665
O1 C1 C2 120.6(10) . .
C14 C1 O1 116.4(9) . .
C14 C1 C2 122.7(9) . .
C2A C1A O1A 118.4(10) . .
C2A C1A C14A 124.0(9) . .
C14A C1A O1A 117.3(10) . .
C3 C2 C1 118.2(11) . .
C1A C2A C3A 117.7(12) . .
C4 C3 C2 120.4(11) . .
C4A C3A C2A 119.7(12) . .
C3 C4 C5 122.0(9) . .
C3A C4A C5A 122.7(10) . .
C4 C5 C6 124.0(9) . .
C14 C5 C4 117.5(10) . .
C14 C5 C6 117.7(10) . .
C4A C5A C6A 125.2(8) . .
C4A C5A C14A 118.8(11) . .
C14A C5A C6A 116.0(10) . .
C5 C6 C7 107.6(8) . .
C5 C6 C13A 112.0(9) . .
C7 C6 C13A 110.7(9) . .
C5A C6A C13 110.8(9) . .
C7A C6A C5A 111.1(8) . .
C7A C6A C13 110.7(9) . .
C8 C7 C6 125.2(10) . .
C8 C7 C12 119.6(13) . .
C12 C7 C6 114.9(11) . .
C8A C7A C6A 124.1(9) . .
C8A C7A C12A 120.4(11) . .
C12A C7A C6A 115.3(9) . .
C7 C8 C9 121.3(11) . .
C7A C8A C9A 121.0(10) . .
C8 C9 C10 120.3(12) . .
C10A C9A C8A 119.5(12) . .
C11 C10 C9 117.8(13) . .
C11A C10A C9A 117.2(13) . .
C10 C11 O2 118.5(12) . .
C10 C11 C12 123.8(10) . .
C12 C11 O2 117.6(10) . .
C10A C11A O2A 119.4(11) . .
C12A C11A O2A 115.5(10) . .
C12A C11A C10A 124.7(10) . .
C7 C12 C13 118.4(11) . .
C11 C12 C7 117.2(12) . .
C11 C12 C13 124.4(8) . .
C7A C12A C13A 118.8(10) . .
C11A C12A C7A 117.0(10) . .
C11A C12A C13A 123.6(9) . .
C12 C13 C6A 112.2(9) . .
C14 C13 C6A 110.6(9) . .
C14 C13 C12 107.9(8) . .
C12A C13A C6 112.6(9) . .
C12A C13A C14A 109.5(8) . .
C14A C13A C6 111.1(8) . .
C1 C14 C5 119.1(10) . .
C1 C14 C13 123.0(8) . .
C5 C14 C13 117.7(10) . .
C1A C14A C5A 117.0(11) . .
C1A C14A C13A 126.9(8) . .
C5A C14A C13A 116.1(11) . .
O1 C15 N1 112.2(7) . 2_665
N1 C15 O1 121.0(7) . .
N1 C15 N1 126.6(8) . 2_665
O1A C15A N1A 120.3(7) . .
O1A C15A N1A 114.1(6) . 2_655
N1A C15A N1A 125.5(7) . 2_655
N2 C16 O2 111.1(8) . .
N2 C16 O2 118.4(8) 3_565 .
N2 C16 N2 130.4(8) . 3_565
N2A C16A O2A 112.0(8) 2_655 .
N2A C16A O2A 118.0(8) . .
N2A C16A N2A 129.9(8) . 2_655
C15B O1B C1B 120.6(7) . .
C16B O2B C11B 117.8(7) . .
C15B N1B C15B 112.5(11) 3_665 .
C16B N2B C16B 111.9(9) 3_665 .
O1B C1B C14B 117.5(10) . .
C2B C1B O1B 119.2(12) . .
C2B C1B C14B 123.3(12) . .
C1B C2B C3B 119.5(17) . .
C4B C3B C2B 120.7(18) . .
C3B C4B C5B 120.7(14) . .
C4B C5B C6B 122.4(12) . .
C14B C5B C4B 121.5(14) . .
C14B C5B C6B 115.9(12) . .
C7B C6B C5B 123.1(10) . .
C6B C7B C12B 117.4(13) . .
C8B C7B C6B 124.7(13) . .
C8B C7B C12B 117.5(14) . .
C9B C8B C7B 122.7(13) . .
C8B C9B C10B 118.9(15) . .
C11B C10B C9B 121.3(15) . .
C10B C11B O2B 119.8(12) . .
C10B C11B C12B 120.5(11) . .
C12B C11B O2B 119.0(10) . .
C11B C12B C7B 118.7(11) . .
C11B C12B C13B 121.8(9) . .
C13B C12B C7B 119.5(11) . .
C14B C13B C12B 120.6(9) . .
C5B C14B C1B 114.2(11) . .
C13B C14B C1B 122.5(10) . .
C13B C14B C5B 123.3(12) . .
N1B C15B O1B 119.6(9) 2_655 .
N1B C15B O1B 113.0(9) . .
N1B C15B N1B 127.5(11) 2_655 .
N2B C16B O2B 119.7(8) 2_655 .
N2B C16B O2B 112.3(9) . .
N2B C16B N2B 128.0(9) 2_655 .
C17_a N3_a N3B 177(4) . .
N3_a C17_a C18_a 175(3) . .
N19_a C18_a C17_a 116.3(15) . .
N19_a C18_a C23_a 120.0 . .
C23_a C18_a C17_a 123.6(15) . .
C18_a N19_a C20_a 120.0 . .
C21_a C20_a N19_a 120.0 . .
C20_a C21_a C22_a 120.0 . .
C21_a C22_a C23_a 120.0 . .
C22_a C23_a C18_a 120.0 . .
N3A_b C17A_b C18A_b 175(2) . .
N19A_b C18A_b C17A_b 110.9(17) . .
N19A_b C18A_b C23A_b 120.0 . .
C23A_b C18A_b C17A_b 125.7(17) . .
C18A_b N19A_b C20A_b 120.0 . .
N19A_b C20A_b C21A_b 120.0 . .
C22A_b C21A_b C20A_b 120.0 . .
C21A_b C22A_b C23A_b 120.0 . .
C22A_b C23A_b C18A_b 120.0 . .
C17B N3B N3_a 107(5) . .
N3B C17B C18B 171(6) . .
N19B C18B C17B 118(2) . .
N19B C18B C23B 120.0 . .
C23B C18B C17B 122(2) . .
C18B N19B C20B 120.00(7) . .
C21B C20B N19B 120.0 . .
C22B C21B C20B 120.0 . .
C21B C22B C23B 120.00(5) . .
C22B C23B C18B 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.412(11) .
O1 C15 1.327(10) .
O1A C1A 1.416(11) .
O1A C15A 1.315(10) .
O2 C11 1.432(12) .
O2 C16 1.370(10) .
O2A C11A 1.415(12) .
O2A C16A 1.354(11) .
N1 C15 1.325(11) .
N1 C15 1.340(11) 3_565
N1A C15A 1.320(10) .
N1A C15A 1.347(10) 3_665
N2 C16 1.318(12) .
N2 C16 1.324(12) 2_665
N2A C16A 1.316(12) .
N2A C16A 1.322(12) 3_665
C1 C2 1.421(15) .
C1 C14 1.356(15) .
C1A C2A 1.374(17) .
C1A C14A 1.388(17) .
C2 C3 1.383(16) .
C2A C3A 1.403(15) .
C3 C4 1.348(18) .
C3A C4A 1.350(19) .
C4 C5 1.439(17) .
C4A C5A 1.393(17) .
C5 C6 1.480(16) .
C5 C14 1.412(12) .
C5A C6A 1.519(16) .
C5A C14A 1.412(12) .
C6 C7 1.536(18) .
C6 C13A 1.642(12) .
C6A C7A 1.465(16) .
C6A C13 1.619(13) .
C7 C8 1.352(18) .
C7 C12 1.432(14) .
C7A C8A 1.338(16) .
C7A C12A 1.415(12) .
C8 C9 1.377(19) .
C8A C9A 1.408(19) .
C9 C10 1.420(17) .
C9A C10A 1.392(17) .
C10 C11 1.336(18) .
C10A C11A 1.365(16) .
C11 C12 1.392(18) .
C11A C12A 1.359(16) .
C12 C13 1.522(18) .
C12A C13A 1.463(16) .
C13 C14 1.511(16) .
C13A C14A 1.525(17) .
C15 N1 1.340(11) 2_665
C15A N1A 1.347(10) 2_655
C16 N2 1.324(12) 3_565
C16A N2A 1.322(12) 2_655
O1B C1B 1.398(13) .
O1B C15B 1.339(13) .
O2B C11B 1.432(12) .
O2B C16B 1.375(11) .
N1B C15B 1.300(12) 3_665
N1B C15B 1.335(13) .
N2B C16B 1.316(12) 3_665
N2B C16B 1.318(12) .
C1B C2B 1.357(17) .
C1B C14B 1.417(17) .
C2B C3B 1.41(2) .
C3B C4B 1.29(3) .
C4B C5B 1.43(2) .
C5B C6B 1.450(19) .
C5B C14B 1.407(14) .
C6B C7B 1.389(19) .
C7B C8B 1.38(2) .
C7B C12B 1.475(14) .
C8B C9B 1.34(2) .
C9B C10B 1.42(2) .
C10B C11B 1.357(18) .
C11B C12B 1.373(16) .
C12B C13B 1.397(15) .
C13B C14B 1.379(16) .
C15B N1B 1.300(12) 2_655
C16B N2B 1.316(12) 2_655
N3_a C17_a 1.05(3) .
N3_a N3B 1.40(5) .
C17_a C18_a 1.42(3) .
C18_a N19_a 1.3900 .
C18_a C23_a 1.3900 .
N19_a C20_a 1.3900 .
C20_a C21_a 1.3900 .
C21_a C22_a 1.3900 .
C22_a C23_a 1.3900 .
N3A_b C17A_b 1.04(4) .
C17A_b C18A_b 1.47(5) .
C18A_b N19A_b 1.3900 .
C18A_b C23A_b 1.3900 .
N19A_b C20A_b 1.3900 .
C20A_b C21A_b 1.3900 .
C21A_b C22A_b 1.3900 .
C22A_b C23A_b 1.3900 .
N3B C17B 1.05(3) .
C17B C18B 1.43(3) .
C18B N19B 1.3900 .
C18B C23B 1.3900 .
N19B C20B 1.3900 .
C20B C21B 1.3900 .
C21B C22B 1.3900 .
C22B C23B 1.3900 .
