#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:18:45 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267024 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/83/7128360.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_7128360
loop_
_publ_author_name
'He, Donglin'
'Clowes, Rob'
'Little, Marc A.'
'Liu, Ming'
'Cooper, Andrew I.'
_publ_section_title
;
 Creating porosity in a trianglimine macrocycle by heterochiral pairing.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6141
_journal_page_last               6144
_journal_paper_doi               10.1039/d1cc01650d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C42 H48 N6, 2(C8 H10)'
_chemical_formula_sum            'C58 H68 N6'
_chemical_formula_weight         849.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                104.5050(4)
_cell_angle_beta                 91.5770(5)
_cell_angle_gamma                105.6390(5)
_cell_formula_units_Z            2
_cell_length_a                   11.19190(7)
_cell_length_b                   15.18470(8)
_cell_length_c                   15.73550(8)
_cell_measurement_reflns_used    31076
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.7188703978
_cell_measurement_theta_min      1.40837131993
_cell_volume                     2480.11(3)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.6.4-g47a579eb-release'
_computing_data_collection       'Diamond I19 GDA, (Diamond, RAL, Didcot, UK)'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.6.4-g47a579eb-release
pointless (Evans, P., 2006)
XIA2 0.5.340-g5578c4a7-dials-1.6 (Winter, G., 2010)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean PILATUS_2M_S_N_24_0107_Diamond
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32622
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.847
_diffrn_reflns_theta_min         1.302
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10349
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0674
_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)+(0.1218P)²+0.5184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9404
_reflns_number_total             10349
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01650d2.cif
_cod_data_source_block           2oX_1-rac_100K_publ
_cod_depositor_comments
'Adding full bibliography for 7128359--7128364.cif.'
_cod_original_cell_volume        2480.11(2)
_cod_database_code               7128360
_shelx_shelxl_version_number     2018/3
_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   0.999
_shelx_estimated_absorpt_t_min   0.994
_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 C(H,H,H) groups
2. Restrained distances
 C57-C53 = C58-C54
 1.49 with sigma of 0.01
 C62-C65 = C66-C61
 1.49 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C63, C62, C60, C59, C64, C61, C66, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C50, C43, C44, C48, C49, C45, C47, C46
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C62)=Sof(C61)=Sof(C60)=Sof(H1ca)=Sof(C59)=Sof(H2ca)=Sof(C64)=Sof(H3ca)=
 Sof(C63)=Sof(H4ca)=Sof(C66)=Sof(H5ca)=Sof(H6ca)=Sof(H7ca)=Sof(C65)=Sof(H8ca)=
 Sof(H9ca)=Sof(H0da)=1-FVAR(1)
 Sof(C53)=Sof(C54)=Sof(C55)=Sof(H1da)=Sof(C56)=Sof(H2da)=Sof(C51)=Sof(H3da)=
 Sof(C52)=Sof(H4da)=Sof(C57)=Sof(H5da)=Sof(H6da)=Sof(H7da)=Sof(C58)=Sof(H8da)=
 Sof(H9da)=Sof(H0ea)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(Hb), C15(Hd), C4(Hg), C34(Hi), C29(Hn), C20(Hu)
5.b Secondary CH2 refined with riding coordinates:
 C16(Hj,Hk), C17(Hs,Ht), C19(Hv,Hw), C30(Hx,Hy), C2(Hz,H0aa), C32(H1aa,H2aa),
 C3(H5aa,H6aa), C18(H0ba,H1ba), C6(H2ba,H3ba), C33(H4ba,H5ba), C1(H7ba,H8ba),
 C31(H9ba,H0ca)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H), C21(Ha), C37(Hc), C14(He), C9(Hf), C39(Hh), C27(Hl), C35(Hm), C28(Ho),
  C11(Hp), C38(Hq), C41(Hr), C7(H3aa), C13(H4aa), C23(H7aa), C25(H8aa),
 C10(H9aa), C24(H6ba), C48(H48), C45(H45), C46(H46), C47(H47), C60(H1ca),
 C59(H2ca), C64(H3ca), C63(H4ca), C55(H1da), C56(H2da), C51(H3da), C52(H4da)
5.d Fitted hexagon refined as free rotating group:
 C62(C61,C60,C59,C64,C63), C53(C54,C55,C56,C51,C52)
5.e Idealised Me refined as rotating group:
 C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C66(H5ca,H6ca,H7ca), C65(H8ca,H9ca,
 H0da), C57(H5da,H6da,H7da), C58(H8da,H9da,H0ea)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
N6 N 0.05885(10) 0.85494(8) 0.53041(7) 0.0239(2) Uani 1 1 d . . . . .
N5 N 0.30089(11) 0.87585(8) 0.62785(8) 0.0264(3) Uani 1 1 d . . . . .
N4 N 0.71681(10) 0.67208(8) 0.50206(7) 0.0256(2) Uani 1 1 d . . . . .
N2 N 0.08800(11) 0.42497(8) 0.10396(8) 0.0271(3) Uani 1 1 d . . . . .
N3 N 0.60400(10) 0.51080(8) 0.34962(8) 0.0280(3) Uani 1 1 d . . . . .
N1 N -0.09019(10) 0.52451(8) 0.17303(7) 0.0253(2) Uani 1 1 d . . . . .
C12 C -0.04561(12) 0.69360(9) 0.21908(8) 0.0242(3) Uani 1 1 d . . . . .
C42 C 0.39566(13) 0.94057(9) 0.62145(8) 0.0259(3) Uani 1 1 d . . . . .
H H 0.393968 1.004802 0.637781 0.031 Uiso 1 1 calc R . . . .
C21 C 0.17145(13) 0.44324(9) 0.16671(9) 0.0268(3) Uani 1 1 d . . . . .
HA H 0.148590 0.424472 0.218609 0.032 Uiso 1 1 calc R . . . .
C22 C 0.30346(12) 0.49281(9) 0.16222(9) 0.0264(3) Uani 1 1 d . . . . .
C36 C 0.62613(13) 0.80255(9) 0.54612(9) 0.0275(3) Uani 1 1 d . . . . .
C5 C 0.07325(12) 0.83739(9) 0.61701(8) 0.0234(3) Uani 1 1 d . . . . .
HB H 0.075272 0.770262 0.608070 0.028 Uiso 1 1 calc R . . . .
C37 C 0.72270(12) 0.87206(10) 0.52527(9) 0.0277(3) Uani 1 1 d . . . . .
HC H 0.794818 0.856650 0.503288 0.033 Uiso 1 1 calc R . . . .
C15 C -0.12483(12) 0.43633(9) 0.10252(8) 0.0236(3) Uani 1 1 d . . . . .
HD H -0.115230 0.451057 0.044166 0.028 Uiso 1 1 calc R . . . .
C14 C -0.07526(12) 0.60157(9) 0.15139(8) 0.0247(3) Uani 1 1 d . . . . .
HE H -0.083276 0.600059 0.090744 0.030 Uiso 1 1 calc R . . . .
C9 C 0.00434(12) 0.86684(9) 0.34903(9) 0.0255(3) Uani 1 1 d . . . . .
HF H 0.019340 0.925414 0.392979 0.031 Uiso 1 1 calc R . . . .
C4 C 0.19603(12) 0.90369(9) 0.66896(8) 0.0246(3) Uani 1 1 d . . . . .
HG H 0.202509 0.970981 0.670161 0.030 Uiso 1 1 calc R . . . .
C39 C 0.60742(13) 0.98646(9) 0.56980(9) 0.0277(3) Uani 1 1 d . . . . .
HH H 0.602519 1.049643 0.579383 0.033 Uiso 1 1 calc R . . . .
C26 C 0.52122(13) 0.54084(9) 0.21960(9) 0.0266(3) Uani 1 1 d . . . . .
C34 C 0.70740(12) 0.57354(9) 0.50018(9) 0.0254(3) Uani 1 1 d . . . . .
HI H 0.625848 0.544352 0.520446 0.030 Uiso 1 1 calc R . . . .
C16 C -0.26153(12) 0.38376(10) 0.10663(9) 0.0267(3) Uani 1 1 d . . . . .
HJ H -0.272143 0.374399 0.166311 0.032 Uiso 1 1 calc R . . . .
HK H -0.315244 0.423013 0.096231 0.032 Uiso 1 1 calc R . . . .
C40 C 0.50931(12) 0.91758(9) 0.58883(9) 0.0256(3) Uani 1 1 d . . . . .
C27 C 0.39545(12) 0.49723(9) 0.22561(9) 0.0263(3) Uani 1 1 d . . . . .
HL H 0.372899 0.470475 0.273405 0.032 Uiso 1 1 calc R . . . .
C35 C 0.63077(13) 0.70415(10) 0.53576(10) 0.0285(3) Uani 1 1 d . . . . .
HM H 0.564996 0.662390 0.555652 0.034 Uiso 1 1 calc R . . . .
C29 C 0.71472(12) 0.51785(9) 0.40570(9) 0.0259(3) Uani 1 1 d . . . . .
HN H 0.791261 0.551440 0.382626 0.031 Uiso 1 1 calc R . . . .
C28 C 0.62242(12) 0.54543(9) 0.28406(9) 0.0270(3) Uani 1 1 d . . . . .
HO H 0.705726 0.575923 0.276059 0.032 Uiso 1 1 calc R . . . .
C11 C -0.04332(13) 0.77658(10) 0.19603(9) 0.0277(3) Uani 1 1 d . . . . .
HP H -0.058951 0.774639 0.135843 0.033 Uiso 1 1 calc R . . . .
C38 C 0.71277(13) 0.96333(10) 0.53680(9) 0.0288(3) Uani 1 1 d . . . . .
HQ H 0.777863 1.010244 0.522191 0.035 Uiso 1 1 calc R . . . .
C41 C 0.52019(13) 0.82585(9) 0.57689(9) 0.0268(3) Uani 1 1 d . . . . .
HR H 0.454095 0.778521 0.590016 0.032 Uiso 1 1 calc R . . . .
C17 C -0.30290(13) 0.28733(10) 0.03810(9) 0.0282(3) Uani 1 1 d . . . . .
HS H -0.389860 0.253993 0.044646 0.034 Uiso 1 1 calc R . . . .
HT H -0.300370 0.296709 -0.021936 0.034 Uiso 1 1 calc R . . . .
C20 C -0.03968(12) 0.37556(9) 0.11487(8) 0.0252(3) Uani 1 1 d . . . . .
HU H -0.043187 0.365977 0.175457 0.030 Uiso 1 1 calc R . . . .
C19 C -0.08130(13) 0.27895(10) 0.04610(9) 0.0284(3) Uani 1 1 d . . . . .
HV H -0.070169 0.288348 -0.013531 0.034 Uiso 1 1 calc R . . . .
HW H -0.028014 0.239462 0.056653 0.034 Uiso 1 1 calc R . . . .
C30 C 0.71853(13) 0.41717(10) 0.40276(11) 0.0333(3) Uani 1 1 d . . . . .
HX H 0.637115 0.381192 0.416749 0.040 Uiso 1 1 calc R . . . .
HY H 0.731237 0.384925 0.342168 0.040 Uiso 1 1 calc R . . . .
C2 C 0.09146(16) 0.90563(11) 0.81108(9) 0.0346(3) Uani 1 1 d . . . . .
HZ H 0.087226 0.971548 0.819766 0.041 Uiso 1 1 calc R . . . .
H0AA H 0.099653 0.894163 0.869898 0.041 Uiso 1 1 calc R . . . .
C32 C 0.81354(15) 0.47181(11) 0.56051(11) 0.0362(3) Uani 1 1 d . . . . .
H1AA H 0.885097 0.473518 0.599926 0.043 Uiso 1 1 calc R . . . .
H2AA H 0.735964 0.440017 0.582455 0.043 Uiso 1 1 calc R . . . .
C7 C 0.03078(12) 0.78236(9) 0.46490(8) 0.0233(3) Uani 1 1 d . . . . .
H3AA H 0.026135 0.722765 0.475684 0.028 Uiso 1 1 calc R . . . .
C8 C 0.00483(11) 0.78395(9) 0.37307(8) 0.0230(3) Uani 1 1 d . . . . .
C13 C -0.02019(12) 0.69838(9) 0.30798(8) 0.0236(3) Uani 1 1 d . . . . .
H4AA H -0.020007 0.642198 0.324176 0.028 Uiso 1 1 calc R . . . .
C3 C 0.20461(14) 0.89344(10) 0.76334(9) 0.0312(3) Uani 1 1 d . . . . .
H5AA H 0.213801 0.829904 0.761217 0.037 Uiso 1 1 calc R . . . .
H6AA H 0.280195 0.941398 0.797346 0.037 Uiso 1 1 calc R . . . .
C23 C 0.33747(13) 0.53458(10) 0.09304(9) 0.0299(3) Uani 1 1 d . . . . .
H7AA H 0.275039 0.532221 0.049710 0.036 Uiso 1 1 calc R . . . .
C25 C 0.55295(13) 0.58126(10) 0.15016(9) 0.0296(3) Uani 1 1 d . . . . .
H8AA H 0.638048 0.610571 0.145461 0.035 Uiso 1 1 calc R . . . .
C10 C -0.01813(13) 0.86286(10) 0.26092(9) 0.0294(3) Uani 1 1 d . . . . .
H9AA H -0.016395 0.919244 0.244484 0.035 Uiso 1 1 calc R . . . .
C18 C -0.21772(13) 0.22694(9) 0.04979(9) 0.0287(3) Uani 1 1 d . . . . .
H0BA H -0.242411 0.166480 0.002662 0.034 Uiso 1 1 calc R . . . .
H1BA H -0.227421 0.211740 0.107288 0.034 Uiso 1 1 calc R . . . .
C6 C -0.03971(13) 0.85035(10) 0.66579(9) 0.0287(3) Uani 1 1 d . . . . .
H2BA H -0.047176 0.914816 0.670251 0.034 Uiso 1 1 calc R . . . .
H3BA H -0.116416 0.803816 0.631858 0.034 Uiso 1 1 calc R . . . .
C33 C 0.81423(13) 0.57307(10) 0.56287(9) 0.0293(3) Uani 1 1 d . . . . .
H4BA H 0.894812 0.606557 0.545688 0.035 Uiso 1 1 calc R . . . .
H5BA H 0.805840 0.607488 0.623747 0.035 Uiso 1 1 calc R . . . .
C24 C 0.46112(14) 0.57914(10) 0.08747(10) 0.0322(3) Uani 1 1 d . . . . .
H6BA H 0.483365 0.608208 0.041051 0.039 Uiso 1 1 calc R . . . .
C1 C -0.02766(15) 0.83670(12) 0.75825(10) 0.0370(3) Uani 1 1 d . . . . .
H7BA H -0.100586 0.847350 0.789001 0.044 Uiso 1 1 calc R . . . .
H8BA H -0.026532 0.770739 0.753815 0.044 Uiso 1 1 calc R . . . .
C31 C 0.82177(14) 0.41547(11) 0.46726(11) 0.0355(3) Uani 1 1 d . . . . .
H9BA H 0.814834 0.348950 0.466758 0.043 Uiso 1 1 calc R . . . .
H0CA H 0.903969 0.442683 0.448150 0.043 Uiso 1 1 calc R . . . .
C43 C 0.43373(15) 0.77204(10) 0.29822(10) 0.0345(3) Uani 1 1 d . U . . .
C44 C 0.41019(14) 0.80759(10) 0.22797(10) 0.0339(3) Uani 1 1 d . U . . .
C48 C 0.55371(17) 0.77199(12) 0.32140(12) 0.0452(4) Uani 1 1 d . U . . .
H48 H 0.568699 0.747445 0.369298 0.054 Uiso 1 1 calc R . . . .
C45 C 0.50923(18) 0.84198(11) 0.18236(11) 0.0451(4) Uani 1 1 d . U . . .
H45 H 0.494842 0.866142 0.134076 0.054 Uiso 1 1 calc R . . . .
C46 C 0.63106(17) 0.84120(12) 0.20740(14) 0.0541(5) Uani 1 1 d . U . . .
H46 H 0.698511 0.864656 0.176108 0.065 Uiso 1 1 calc R . . . .
C49 C 0.3300(2) 0.73240(13) 0.34965(13) 0.0518(5) Uani 1 1 d . U . . .
H49A H 0.288426 0.780944 0.374066 0.078 Uiso 1 1 calc GR . . . .
H49B H 0.364892 0.713680 0.397865 0.078 Uiso 1 1 calc GR . . . .
H49C H 0.269420 0.676863 0.310372 0.078 Uiso 1 1 calc GR . . . .
C47 C 0.65118(17) 0.80632(14) 0.27723(14) 0.0537(5) Uani 1 1 d . U . . .
H47 H 0.732935 0.806058 0.294829 0.064 Uiso 1 1 calc R . . . .
C50 C 0.27806(19) 0.80471(16) 0.20301(13) 0.0536(5) Uani 1 1 d . U . . .
H50A H 0.225877 0.738640 0.185098 0.080 Uiso 1 1 calc GR . . . .
H50B H 0.276165 0.833412 0.153904 0.080 Uiso 1 1 calc GR . . . .
H50C H 0.246143 0.840196 0.253800 0.080 Uiso 1 1 calc GR . . . .
C62 C 0.3405(5) 0.1551(4) 0.0628(4) 0.0379(19) Uani 0.175(2) 1 d D U P A 2
C61 C 0.4166(6) 0.1756(4) 0.1406(3) 0.0409(19) Uani 0.175(2) 1 d DG U P A 2
C60 C 0.4963(6) 0.1210(4) 0.1477(3) 0.0405(19) Uani 0.175(2) 1 d G U P A 2
H1CA H 0.548330 0.135056 0.200897 0.049 Uiso 0.175(2) 1 calc R . P A 2
C59 C 0.4998(6) 0.0460(4) 0.0769(4) 0.045(2) Uani 0.175(2) 1 d G U P A 2
H2CA H 0.554230 0.008684 0.081728 0.054 Uiso 0.175(2) 1 calc R . P A 2
C64 C 0.4236(6) 0.0255(4) -0.0009(3) 0.045(2) Uani 0.175(2) 1 d G U P A 2
H3CA H 0.426043 -0.025844 -0.049322 0.054 Uiso 0.175(2) 1 calc R . P A 2
C63 C 0.3440(6) 0.0800(4) -0.0080(3) 0.043(2) Uani 0.175(2) 1 d G U P A 2
H4CA H 0.291955 0.066000 -0.061203 0.052 Uiso 0.175(2) 1 calc R . P A 2
C66 C 0.4145(14) 0.2578(8) 0.2153(8) 0.050(3) Uani 0.175(2) 1 d D U P A 2
H5CA H 0.466659 0.316568 0.204887 0.076 Uiso 0.175(2) 1 calc GR . P A 2
H6CA H 0.446829 0.249654 0.270425 0.076 Uiso 0.175(2) 1 calc GR . P A 2
H7CA H 0.328638 0.261339 0.219568 0.076 Uiso 0.175(2) 1 calc GR . P A 2
C65 C 0.2616(17) 0.2181(13) 0.0550(9) 0.069(5) Uani 0.175(2) 1 d D U P A 2
H8CA H 0.236797 0.243900 0.113084 0.104 Uiso 0.175(2) 1 calc GR . P A 2
H9CA H 0.187013 0.181529 0.014127 0.104 Uiso 0.175(2) 1 calc GR . P A 2
H0DA H 0.309199 0.270348 0.032521 0.104 Uiso 0.175(2) 1 calc GR . P A 2
C53 C 0.36689(11) 0.20269(9) 0.13788(7) 0.0378(5) Uani 0.825(2) 1 d D . P A 1
C54 C 0.29039(14) 0.10999(8) 0.11984(8) 0.0439(5) Uani 0.825(2) 1 d DG . P A 1
C55 C 0.19662(13) 0.07573(7) 0.05011(9) 0.0504(6) Uani 0.825(2) 1 d G . P A 1
H1DA H 0.144331 0.012368 0.037787 0.060 Uiso 0.825(2) 1 calc R . P A 1
C56 C 0.17936(13) 0.13418(10) -0.00157(8) 0.0516(6) Uani 0.825(2) 1 d G . P A 1
H2DA H 0.115274 0.110770 -0.049229 0.062 Uiso 0.825(2) 1 calc R . P A 1
C51 C 0.25587(15) 0.22689(9) 0.01646(9) 0.0476(6) Uani 0.825(2) 1 d G . P A 1
H3DA H 0.244069 0.266840 -0.018866 0.057 Uiso 0.825(2) 1 calc R . P A 1
C52 C 0.34963(13) 0.26115(7) 0.08619(9) 0.0400(5) Uani 0.825(2) 1 d G . P A 1
H4DA H 0.401922 0.324511 0.098514 0.048 Uiso 0.825(2) 1 calc R . P A 1
C57 C 0.4668(3) 0.2434(2) 0.21462(18) 0.0525(7) Uani 0.825(2) 1 d D . P A 1
H5DA H 0.428781 0.240159 0.269544 0.079 Uiso 0.825(2) 1 calc GR . P A 1
H6DA H 0.509047 0.309713 0.217337 0.079 Uiso 0.825(2) 1 calc GR . P A 1
H7DA H 0.527505 0.206760 0.206910 0.079 Uiso 0.825(2) 1 calc GR . P A 1
C58 C 0.3050(3) 0.0472(2) 0.1777(2) 0.0671(7) Uani 0.825(2) 1 d D . P A 1
H8DA H 0.387615 0.036746 0.173896 0.101 Uiso 0.825(2) 1 calc GR . P A 1
H9DA H 0.240571 -0.013900 0.157731 0.101 Uiso 0.825(2) 1 calc GR . P A 1
H0EA H 0.296413 0.077937 0.238918 0.101 Uiso 0.825(2) 1 calc GR . P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0028 0.0015 '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 0.0056 0.0031 '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
C7 N6 C5 115.98(10) . . ?
C42 N5 C4 118.23(11) . . ?
C35 N4 C34 116.12(11) . . ?
C21 N2 C20 118.10(11) . . ?
C28 N3 C29 116.83(11) . . ?
C14 N1 C15 117.64(11) . . ?
C11 C12 C14 120.88(12) . . ?
C11 C12 C13 118.86(12) . . ?
C13 C12 C14 120.26(12) . . ?
N5 C42 C40 120.81(12) . . ?
N2 C21 C22 122.33(12) . . ?
C27 C22 C21 120.39(12) . . ?
C27 C22 C23 119.27(13) . . ?
C23 C22 C21 120.33(12) . . ?
C37 C36 C35 122.76(12) . . ?
C41 C36 C37 119.34(12) . . ?
C41 C36 C35 117.90(12) . . ?
N6 C5 C4 110.26(10) . . ?
N6 C5 C6 108.71(10) . . ?
C6 C5 C4 111.94(10) . . ?
C38 C37 C36 119.92(13) . . ?
N1 C15 C16 108.46(10) . . ?
N1 C15 C20 109.26(10) . . ?
C20 C15 C16 110.50(10) . . ?
N1 C14 C12 121.00(12) . . ?
C10 C9 C8 119.71(12) . . ?
N5 C4 C5 109.34(10) . . ?
N5 C4 C3 106.44(10) . . ?
C5 C4 C3 110.40(11) . . ?
C40 C39 C38 120.54(12) . . ?
C27 C26 C28 122.57(12) . . ?
C25 C26 C27 119.23(12) . . ?
C25 C26 C28 118.20(12) . . ?
N4 C34 C29 109.33(11) . . ?
N4 C34 C33 108.49(10) . . ?
C33 C34 C29 110.90(11) . . ?
C17 C16 C15 111.70(11) . . ?
C39 C40 C42 121.05(12) . . ?
C39 C40 C41 118.76(12) . . ?
C41 C40 C42 120.19(12) . . ?
C22 C27 C26 120.54(12) . . ?
N4 C35 C36 124.06(12) . . ?
N3 C29 C34 109.39(10) . . ?
N3 C29 C30 108.12(11) . . ?
C30 C29 C34 110.78(11) . . ?
N3 C28 C26 123.41(12) . . ?
C12 C11 C10 120.35(12) . . ?
C37 C38 C39 120.21(12) . . ?
C36 C41 C40 121.19(12) . . ?
C18 C17 C16 110.44(11) . . ?
N2 C20 C15 108.73(10) . . ?
N2 C20 C19 109.32(11) . . ?
C19 C20 C15 110.22(10) . . ?
C18 C19 C20 111.71(11) . . ?
C31 C30 C29 112.84(12) . . ?
C3 C2 C1 110.58(12) . . ?
C31 C32 C33 111.00(12) . . ?
N6 C7 C8 124.51(11) . . ?
C9 C8 C7 123.18(12) . . ?
C13 C8 C9 119.33(12) . . ?
C13 C8 C7 117.49(11) . . ?
C8 C13 C12 121.19(12) . . ?
C2 C3 C4 113.16(11) . . ?
C24 C23 C22 120.54(13) . . ?
C26 C25 C24 120.63(13) . . ?
C9 C10 C11 120.54(12) . . ?
C17 C18 C19 111.08(11) . . ?
C1 C6 C5 111.17(12) . . ?
C32 C33 C34 111.10(12) . . ?
C23 C24 C25 119.76(13) . . ?
C2 C1 C6 110.50(12) . . ?
C32 C31 C30 111.25(12) . . ?
C44 C43 C49 121.27(16) . . ?
C48 C43 C44 119.85(15) . . ?
C48 C43 C49 118.88(17) . . ?
C43 C44 C50 118.62(15) . . ?
C45 C44 C43 118.63(15) . . ?
C45 C44 C50 122.73(17) . . ?
C47 C48 C43 121.65(18) . . ?
C44 C45 C46 120.42(17) . . ?
C47 C46 C45 119.48(16) . . ?
C48 C47 C46 119.96(17) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 C65 119.0(8) . . ?
C63 C62 C65 120.9(8) . . ?
C62 C61 C60 120.0 . . ?
C62 C61 C66 119.5(7) . . ?
C60 C61 C66 120.5(7) . . ?
C59 C60 C61 120.0 . . ?
C64 C59 C60 120.0 . . ?
C59 C64 C63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 C57 121.56(15) . . ?
C52 C53 C57 118.41(15) . . ?
C53 C54 C58 120.42(15) . . ?
C55 C54 C53 120.0 . . ?
C55 C54 C58 119.53(15) . . ?
C54 C55 C56 120.0 . . ?
C51 C56 C55 120.0 . . ?
C56 C51 C52 120.0 . . ?
C51 C52 C53 120.0 . . ?
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
N6 C5 1.4652(16) . ?
N6 C7 1.2658(17) . ?
N5 C42 1.2627(18) . ?
N5 C4 1.4652(17) . ?
N4 C34 1.4640(16) . ?
N4 C35 1.2638(18) . ?
N2 C21 1.2635(18) . ?
N2 C20 1.4609(17) . ?
N3 C29 1.4651(17) . ?
N3 C28 1.2682(19) . ?
N1 C15 1.4583(16) . ?
N1 C14 1.2692(17) . ?
C12 C14 1.4773(18) . ?
C12 C11 1.3899(18) . ?
C12 C13 1.3996(18) . ?
C42 C40 1.4793(18) . ?
C21 C22 1.4789(19) . ?
C22 C27 1.3901(19) . ?
C22 C23 1.404(2) . ?
C36 C37 1.4028(19) . ?
C36 C35 1.4771(18) . ?
C36 C41 1.3918(19) . ?
C5 C4 1.5331(18) . ?
C5 C6 1.5291(18) . ?
C37 C38 1.3872(19) . ?
C15 C16 1.5345(18) . ?
C15 C20 1.5335(18) . ?
C9 C8 1.4033(18) . ?
C9 C10 1.3856(19) . ?
C4 C3 1.5345(18) . ?
C39 C40 1.3946(19) . ?
C39 C38 1.396(2) . ?
C26 C27 1.4017(19) . ?
C26 C28 1.4749(19) . ?
C26 C25 1.392(2) . ?
C34 C29 1.5318(19) . ?
C34 C33 1.5317(18) . ?
C16 C17 1.5289(18) . ?
C40 C41 1.3972(18) . ?
C29 C30 1.5300(18) . ?
C11 C10 1.398(2) . ?
C17 C18 1.5263(19) . ?
C20 C19 1.5325(19) . ?
C19 C18 1.528(2) . ?
C30 C31 1.527(2) . ?
C2 C3 1.520(2) . ?
C2 C1 1.521(2) . ?
C32 C33 1.5267(19) . ?
C32 C31 1.521(2) . ?
C7 C8 1.4735(18) . ?
C8 C13 1.3919(18) . ?
C23 C24 1.383(2) . ?
C25 C24 1.393(2) . ?
C6 C1 1.5275(19) . ?
C43 C44 1.394(2) . ?
C43 C48 1.382(2) . ?
C43 C49 1.511(2) . ?
C44 C45 1.391(2) . ?
C44 C50 1.506(2) . ?
C48 C47 1.364(3) . ?
C45 C46 1.413(3) . ?
C46 C47 1.371(3) . ?
C62 C61 1.3900 . ?
C62 C63 1.3900 . ?
C62 C65 1.489(8) . ?
C61 C60 1.3900 . ?
C61 C66 1.491(8) . ?
C60 C59 1.3900 . ?
C59 C64 1.3900 . ?
C64 C63 1.3900 . ?
C53 C54 1.3900 . ?
C53 C52 1.3900 . ?
C53 C57 1.506(3) . ?
C54 C55 1.3900 . ?
C54 C58 1.508(3) . ?
C55 C56 1.3900 . ?
C56 C51 1.3900 . ?
C51 C52 1.3900 . ?
