#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:42:43 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266045 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707138.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_7707138
loop_
_publ_author_name
'Pitarch-Jarque, Javier'
'Zaragozá, Ramón J'
'Ballesteros, Rafael'
'Abarca, Belen'
'Garcia-España, Enrique'
'Verdejo, Begoña'
'Ballesteros-Garrido, Rafael'
_publ_section_title
;
 About the relevance of anion-π interactions in water.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6834
_journal_page_last               6839
_journal_paper_doi               10.1039/d1dt00771h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '6(Br), 2(C39 H30 N9), 3(H2 O)'
_chemical_formula_sum            'C78 H66 Br6 N18 O3'
_chemical_formula_weight         1782.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-07-09 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3635(9)
_cell_length_b                   23.3233(15)
_cell_length_c                   13.8839(12)
_cell_measurement_reflns_used    3300
_cell_measurement_temperature    119.9(3)
_cell_measurement_theta_max      24.4530
_cell_measurement_theta_min      3.6910
_cell_volume                     3674.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0133
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  90.00   1.00   45.00    --   20.73  57.00  30.00   90
  2  ω     -6.00  63.00   1.00   45.00    --   20.73  77.00  60.00   69
  3  ω    -48.00  42.00   1.00   45.00    --   20.73 -57.00-120.00   90
  4  ω    -82.00 -38.00   1.00   45.00    --  -19.95 178.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0063757000
_diffrn_orient_matrix_UB_12      0.0300787000
_diffrn_orient_matrix_UB_13      -0.0026527000
_diffrn_orient_matrix_UB_21      0.0046157000
_diffrn_orient_matrix_UB_22      0.0027320000
_diffrn_orient_matrix_UB_23      0.0524270000
_diffrn_orient_matrix_UB_31      0.0620286000
_diffrn_orient_matrix_UB_32      -0.0032664000
_diffrn_orient_matrix_UB_33      0.0186761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17947
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water, methanol'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6452
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0588
_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)+(0.0355P)²+7.9776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4654
_reflns_number_total             6452
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00771h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707136--7707138.cif.'
_cod_original_cell_volume        3674.0(5)
_cod_database_code               7707138
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'raf qui I 1'
_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.
;
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Br2_$1-H2a
 3.5 with sigma of 0.01
 Br2_$1-H3b
 3.2 with sigma of 0.01
 Br3-H3a
 3.2 with sigma of 0.01
 H2a-H8_$1
 2.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O2(0.75) H2a(0.75) H2b(0.75) O1(0.5) H1a(0.5) H1b(0.5) O3(0.25)
 H3a(0.25) H3b(0.25)
5.a Free rotating group:
 O2(H2a,H2b), O1(H1a,H1b), O3(H3a,H3b)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C18(H18a,H18b), C29(H29a,H29b)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C24(H24), C8(H8), C26(H26), C19(H19), C22(H22),
 C27(H27), C15(H15), C14(H14), C21(H21), C30(H30), C10(H10), C16(H16), C25(H25),
  C32(H32), C11(H11), C13(H13), C35(H35), C38(H38), C36(H36), C37(H37), C33(H33)
;
_olex2_date_sample_data_collection 2017-07-10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.869
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Br2 Br 0.60555(5) 0.37254(3) 0.64249(5) 0.03475(18) Uani 1 1 d D . . . .
Br3 Br 0.71539(5) 0.48073(3) 0.23152(5) 0.03603(19) Uani 1 1 d D . . . .
Br1 Br 0.39162(5) 0.13035(3) 0.75183(5) 0.03618(19) Uani 1 1 d . . . . .
N1 N 0.3099(4) 0.2784(2) 0.5092(3) 0.0212(11) Uani 1 1 d . . . . .
N6 N 0.8890(4) 0.31948(18) 0.5045(3) 0.0185(10) Uani 1 1 d . . . . .
O2 O 0.7091(4) 0.5339(2) 0.4496(4) 0.0195(11) Uani 0.75 1 d . . P A 1
H2A H 0.6420 0.5380 0.4521 0.029 Uiso 0.75 1 d DG . P A 1
H2B H 0.7000 0.5255 0.3872 0.029 Uiso 0.75 1 d G . P A 1
N5 N 0.8224(4) 0.27472(19) 0.4555(3) 0.0212(11) Uani 1 1 d . . . . .
N2 N 0.2180(4) 0.2466(2) 0.4506(3) 0.0232(11) Uani 1 1 d . . . . .
N3 N 0.1373(4) 0.2870(2) 0.4013(3) 0.0229(11) Uani 1 1 d . . . . .
N4 N 0.7202(4) 0.29961(19) 0.3977(3) 0.0194(10) Uani 1 1 d . . . . .
N7 N 0.6378(4) 0.0499(2) 0.4170(4) 0.0254(12) Uani 1 1 d . . . . .
N9 N 0.8026(4) 0.05049(19) 0.4087(4) 0.0251(12) Uani 1 1 d . . . . .
N8 N 0.7476(4) 0.0690(2) 0.4684(4) 0.0282(12) Uani 1 1 d . . . . .
C7 C 0.4176(4) 0.2481(2) 0.5770(4) 0.0223(13) Uani 1 1 d . . . . .
H7A H 0.3979 0.2197 0.6185 0.027 Uiso 1 1 calc R . . . .
H7B H 0.4722 0.2752 0.6248 0.027 Uiso 1 1 calc R . . . .
C3 C 0.5718(4) 0.2271(2) 0.3930(4) 0.0186(12) Uani 1 1 d . . . . .
C2 C 0.5184(4) 0.2529(2) 0.4534(4) 0.0192(13) Uani 1 1 d . . . . .
H2 H 0.5113 0.2926 0.4538 0.023 Uiso 1 1 calc R . . . .
C18 C 0.6212(4) 0.2628(2) 0.3296(4) 0.0220(13) Uani 1 1 d . . . . .
H18A H 0.6487 0.2377 0.2884 0.026 Uiso 1 1 calc R . . . .
H18B H 0.5592 0.2869 0.2814 0.026 Uiso 1 1 calc R . . . .
C23 C 1.0641(4) 0.3645(2) 0.6224(4) 0.0217(13) Uani 1 1 d . . . . .
C4 C 0.5803(4) 0.1676(2) 0.3918(4) 0.0224(13) Uani 1 1 d . . . . .
H4 H 0.6140 0.1503 0.3500 0.027 Uiso 1 1 calc R . . . .
C28 C 1.0069(4) 0.3136(2) 0.5771(4) 0.0207(13) Uani 1 1 d . . . . .
C6 C 0.4872(4) 0.1605(2) 0.5138(4) 0.0206(13) Uani 1 1 d . . . . .
H6 H 0.4603 0.1384 0.5555 0.025 Uiso 1 1 calc R . . . .
C5 C 0.5388(4) 0.1336(2) 0.4526(4) 0.0228(13) Uani 1 1 d . . . . .
C24 C 1.1815(5) 0.3598(3) 0.6974(4) 0.0274(14) Uani 1 1 d . . . . .
H24 H 1.2227 0.3925 0.7299 0.033 Uiso 1 1 calc R . . . .
C8 C 0.2932(5) 0.3349(2) 0.4999(4) 0.0261(14) Uani 1 1 d . . . . .
H8 H 0.3470 0.3635 0.5343 0.031 Uiso 1 1 calc DR . . . .
C9 C 0.1773(5) 0.3416(2) 0.4275(4) 0.0239(13) Uani 1 1 d . . . . .
C26 C 1.1758(5) 0.2573(3) 0.6757(4) 0.0263(14) Uani 1 1 d . . . . .
H26 H 1.2137 0.2221 0.6942 0.032 Uiso 1 1 calc R . . . .
C19 C 0.7194(5) 0.3561(2) 0.4072(4) 0.0253(14) Uani 1 1 d . . . . .
H19 H 0.6567 0.3808 0.3731 0.030 Uiso 1 1 calc R . . . .
C1 C 0.4755(4) 0.2190(2) 0.5133(4) 0.0209(13) Uani 1 1 d . . . . .
C22 C 1.0051(5) 0.4184(3) 0.5928(4) 0.0279(14) Uani 1 1 d . . . . .
H22 H 1.0461 0.4518 0.6217 0.034 Uiso 1 1 calc R . . . .
C17 C 0.0226(5) 0.2730(3) 0.3305(4) 0.0252(14) Uani 1 1 d . . . . .
C27 C 1.0605(5) 0.2596(3) 0.6016(4) 0.0246(13) Uani 1 1 d . . . . .
H27 H 1.0203 0.2265 0.5694 0.030 Uiso 1 1 calc R . . . .
C20 C 0.8312(5) 0.3708(2) 0.4784(4) 0.0228(13) Uani 1 1 d . . . . .
C15 C -0.1266(5) 0.2061(3) 0.2377(4) 0.0311(15) Uani 1 1 d . . . . .
H15 H -0.1539 0.1686 0.2223 0.037 Uiso 1 1 calc R . . . .
C12 C -0.0514(5) 0.3201(3) 0.2836(4) 0.0282(14) Uani 1 1 d . . . . .
C14 C -0.2006(5) 0.2520(3) 0.1871(5) 0.0333(16) Uani 1 1 d . . . . .
H14 H -0.2757 0.2443 0.1371 0.040 Uiso 1 1 calc R . . . .
C21 C 0.8916(5) 0.4223(2) 0.5243(5) 0.0290(15) Uani 1 1 d . . . . .
H21 H 0.8539 0.4576 0.5076 0.035 Uiso 1 1 calc R . . . .
C30 C 0.6233(5) 0.0198(2) 0.3309(5) 0.0282(14) Uani 1 1 d . . . . .
H30 H 0.5542 0.0026 0.2850 0.034 Uiso 1 1 calc R . . . .
C10 C 0.1005(5) 0.3884(3) 0.3833(5) 0.0330(16) Uani 1 1 d . . . . .
H10 H 0.1257 0.4259 0.4026 0.040 Uiso 1 1 calc R . . . .
C16 C -0.0141(5) 0.2161(3) 0.3100(4) 0.0289(15) Uani 1 1 d . . . . .
H16 H 0.0358 0.1861 0.3440 0.035 Uiso 1 1 calc R . . . .
C39 C 0.9225(5) 0.0628(3) 0.4328(5) 0.0290(15) Uani 1 1 d . . . . .
C25 C 1.2350(5) 0.3070(3) 0.7226(4) 0.0289(15) Uani 1 1 d . . . . .
H25 H 1.3122 0.3045 0.7719 0.035 Uiso 1 1 calc R . . . .
C31 C 0.7313(5) 0.0196(2) 0.3239(5) 0.0290(14) Uani 1 1 d . . . . .
C29 C 0.5496(5) 0.0689(2) 0.4564(5) 0.0302(15) Uani 1 1 d . . . . .
H29A H 0.5723 0.0558 0.5282 0.036 Uiso 1 1 calc R . . . .
H29B H 0.4738 0.0519 0.4142 0.036 Uiso 1 1 calc R . . . .
C32 C 0.7776(6) -0.0011(3) 0.2527(5) 0.0344(16) Uani 1 1 d . . . . .
H32 H 0.7304 -0.0216 0.1934 0.041 Uiso 1 1 calc R . . . .
C11 C -0.0106(5) 0.3777(3) 0.3124(5) 0.0331(16) Uani 1 1 d . . . . .
H11 H -0.0611 0.4082 0.2819 0.040 Uiso 1 1 calc R . . . .
C34 C 0.9663(5) 0.0412(2) 0.3619(5) 0.0305(15) Uani 1 1 d . . . . .
C13 C -0.1662(5) 0.3074(3) 0.2086(5) 0.0365(17) Uani 1 1 d . . . . .
H13 H -0.2177 0.3369 0.1743 0.044 Uiso 1 1 calc R . . . .
C35 C 1.0877(5) 0.0519(3) 0.3858(5) 0.0373(17) Uani 1 1 d . . . . .
H35 H 1.1217 0.0384 0.3412 0.045 Uiso 1 1 calc R . . . .
C38 C 0.9898(5) 0.0930(3) 0.5219(5) 0.0317(15) Uani 1 1 d . . . . .
H38 H 0.9571 0.1064 0.5674 0.038 Uiso 1 1 calc R . . . .
C36 C 1.1545(6) 0.0820(3) 0.4741(5) 0.0410(18) Uani 1 1 d . . . . .
H36 H 1.2337 0.0885 0.4889 0.049 Uiso 1 1 calc R . . . .
C37 C 1.1067(6) 0.1030(3) 0.5419(5) 0.0406(18) Uani 1 1 d . . . . .
H37 H 1.1533 0.1238 0.6010 0.049 Uiso 1 1 calc R . . . .
C33 C 0.8917(6) 0.0094(3) 0.2724(5) 0.0360(16) Uani 1 1 d . . . . .
H33 H 0.9229 -0.0046 0.2261 0.043 Uiso 1 1 calc R . . . .
O1 O 0.5148(9) 0.4606(4) 0.4307(8) 0.051(3) Uani 0.5 1 d . . P B 3
H1A H 0.5678 0.4496 0.4886 0.076 Uiso 0.5 1 d G . P B 3
H1B H 0.4954 0.4328 0.3875 0.076 Uiso 0.5 1 d G . P B 3
O3 O 0.6201(14) 0.5070(7) 0.4652(13) 0.035(4) Uani 0.25 1 d . U P C 2
H3A H 0.6068 0.4933 0.4048 0.053 Uiso 0.25 1 d DG . P C 2
H3B H 0.5560 0.5193 0.4666 0.053 Uiso 0.25 1 d DG . P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
N2 N1 C7 117.3(4) . . ?
N2 N1 C8 115.5(4) . . ?
C8 N1 C7 127.1(5) . . ?
N5 N6 C28 122.7(4) . . ?
N5 N6 C20 113.5(4) . . ?
C20 N6 C28 123.8(4) . . ?
H2A O2 H2B 109.4 . . ?
N4 N5 N6 102.2(4) . . ?
N1 N2 N3 101.6(4) . . ?
N2 N3 C9 113.7(4) . . ?
N2 N3 C17 122.0(5) . . ?
C9 N3 C17 124.3(5) . . ?
N5 N4 C18 118.5(4) . . ?
C19 N4 N5 114.6(4) . . ?
C19 N4 C18 126.9(4) . . ?
N8 N7 C30 113.7(5) . . ?
N8 N7 C29 116.6(5) . . ?
C30 N7 C29 129.5(5) . . ?
N8 N9 C39 122.2(5) . . ?
N8 N9 C31 113.1(5) . . ?
C31 N9 C39 124.7(5) . . ?
N7 N8 N9 102.7(4) . . ?
N1 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
N1 C7 C1 111.2(4) . . ?
H7A C7 H7B 108.0 . . ?
C1 C7 H7A 109.4 . . ?
C1 C7 H7B 109.4 . . ?
C2 C3 C18 120.8(5) . . ?
C2 C3 C4 119.6(5) . . ?
C4 C3 C18 119.6(5) . . ?
C3 C2 H2 120.1 . . ?
C3 C2 C1 119.8(5) . . ?
C1 C2 H2 120.1 . . ?
N4 C18 C3 111.7(4) . . ?
N4 C18 H18A 109.3 . . ?
N4 C18 H18B 109.3 . . ?
C3 C18 H18A 109.3 . . ?
C3 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
C28 C23 C24 116.9(5) . . ?
C28 C23 C22 120.6(5) . . ?
C24 C23 C22 122.5(5) . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.8(5) . . ?
C5 C4 H4 119.6 . . ?
C23 C28 N6 115.7(5) . . ?
C23 C28 C27 123.4(5) . . ?
C27 C28 N6 120.9(5) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C1 C6 C5 121.1(5) . . ?
C4 C5 C6 118.6(5) . . ?
C4 C5 C29 122.7(5) . . ?
C6 C5 C29 118.8(5) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(5) . . ?
C25 C24 H24 119.8 . . ?
N1 C8 H8 127.6 . . ?
N1 C8 C9 104.9(5) . . ?
C9 C8 H8 127.6 . . ?
N3 C9 C8 104.3(5) . . ?
N3 C9 C10 119.7(5) . . ?
C8 C9 C10 136.0(6) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.7(5) . . ?
N4 C19 H19 127.1 . . ?
N4 C19 C20 105.8(5) . . ?
C20 C19 H19 127.1 . . ?
C2 C1 C7 118.5(5) . . ?
C6 C1 C7 121.3(5) . . ?
C6 C1 C2 120.2(5) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 C23 122.1(5) . . ?
C21 C22 H22 119.0 . . ?
N3 C17 C12 115.4(5) . . ?
C16 C17 N3 121.4(5) . . ?
C16 C17 C12 123.1(5) . . ?
C28 C27 H27 121.3 . . ?
C26 C27 C28 117.4(5) . . ?
C26 C27 H27 121.3 . . ?
N6 C20 C19 103.9(5) . . ?
N6 C20 C21 119.6(5) . . ?
C19 C20 C21 136.5(5) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C16 C15 C14 120.3(6) . . ?
C17 C12 C11 120.6(5) . . ?
C17 C12 C13 116.8(6) . . ?
C13 C12 C11 122.6(5) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 C15 122.2(5) . . ?
C13 C14 H14 118.9 . . ?
C22 C21 C20 118.2(5) . . ?
C22 C21 H21 120.9 . . ?
C20 C21 H21 120.9 . . ?
N7 C30 H30 127.0 . . ?
N7 C30 C31 106.0(5) . . ?
C31 C30 H30 127.0 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 118.9(6) . . ?
C11 C10 H10 120.5 . . ?
C17 C16 H16 121.1 . . ?
C15 C16 C17 117.7(6) . . ?
C15 C16 H16 121.1 . . ?
C34 C39 N9 115.2(5) . . ?
C38 C39 N9 121.3(6) . . ?
C38 C39 C34 123.6(6) . . ?
C24 C25 C26 121.2(5) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
N9 C31 C30 104.5(5) . . ?
N9 C31 C32 118.9(6) . . ?
C30 C31 C32 136.6(6) . . ?
N7 C29 C5 110.8(5) . . ?
N7 C29 H29A 109.5 . . ?
N7 C29 H29B 109.5 . . ?
C5 C29 H29A 109.5 . . ?
C5 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
C31 C32 H32 120.7 . . ?
C33 C32 C31 118.6(6) . . ?
C33 C32 H32 120.7 . . ?
C12 C11 H11 119.5 . . ?
C10 C11 C12 121.1(5) . . ?
C10 C11 H11 119.5 . . ?
C39 C34 C35 116.2(6) . . ?
C39 C34 C33 120.4(6) . . ?
C35 C34 C33 123.4(6) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.7(6) . . ?
C14 C13 H13 120.1 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.2(7) . . ?
C36 C35 H35 119.9 . . ?
C39 C38 H38 120.7 . . ?
C37 C38 C39 118.6(6) . . ?
C37 C38 H38 120.7 . . ?
C35 C36 H36 119.3 . . ?
C35 C36 C37 121.4(6) . . ?
C37 C36 H36 119.3 . . ?
C38 C37 C36 119.9(6) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C33 C34 122.2(6) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
H1A O1 H1B 109.5 . . ?
H3A O3 H3B 109.5 . . ?
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 N2 1.330(6) . ?
N1 C7 1.471(6) . ?
N1 C8 1.331(7) . ?
N6 N5 1.336(6) . ?
N6 C28 1.412(6) . ?
N6 C20 1.367(7) . ?
O2 H2A 0.8500 . ?
O2 H2B 0.8503 . ?
N5 N4 1.331(6) . ?
N2 N3 1.346(6) . ?
N3 C9 1.361(7) . ?
N3 C17 1.406(7) . ?
N4 C18 1.486(6) . ?
N4 C19 1.324(7) . ?
N7 N8 1.334(6) . ?
N7 C30 1.334(7) . ?
N7 C29 1.470(7) . ?
N9 N8 1.335(7) . ?
N9 C39 1.413(7) . ?
N9 C31 1.363(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C1 1.504(8) . ?
C3 C2 1.392(7) . ?
C3 C18 1.506(8) . ?
C3 C4 1.393(7) . ?
C2 H2 0.9300 . ?
C2 C1 1.396(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C23 C28 1.397(8) . ?
C23 C24 1.415(7) . ?
C23 C22 1.429(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.395(8) . ?
C28 C27 1.402(8) . ?
C6 H6 0.9300 . ?
C6 C5 1.398(8) . ?
C6 C1 1.372(7) . ?
C5 C29 1.514(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.376(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.394(7) . ?
C9 C10 1.417(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.389(7) . ?
C26 C25 1.386(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.386(7) . ?
C22 H22 0.9300 . ?
C22 C21 1.349(7) . ?
C17 C12 1.414(8) . ?
C17 C16 1.393(8) . ?
C27 H27 0.9300 . ?
C20 C21 1.424(8) . ?
C15 H15 0.9300 . ?
C15 C14 1.403(8) . ?
C15 C16 1.374(7) . ?
C12 C11 1.435(8) . ?
C12 C13 1.419(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.354(9) . ?
C21 H21 0.9300 . ?
C30 H30 0.9300 . ?
C30 C31 1.376(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.358(8) . ?
C16 H16 0.9300 . ?
C39 C34 1.392(9) . ?
C39 C38 1.379(8) . ?
C25 H25 0.9300 . ?
C31 C32 1.411(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C32 H32 0.9300 . ?
C32 C33 1.349(8) . ?
C11 H11 0.9300 . ?
C34 C35 1.425(8) . ?
C34 C33 1.426(8) . ?
C13 H13 0.9300 . ?
C35 H35 0.9300 . ?
C35 C36 1.369(9) . ?
C38 H38 0.9300 . ?
C38 C37 1.378(8) . ?
C36 H36 0.9300 . ?
C36 C37 1.385(9) . ?
C37 H37 0.9300 . ?
C33 H33 0.9300 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8499 . ?
O3 H3A 0.8498 . ?
O3 H3B 0.8502 . ?
