#------------------------------------------------------------------------------
#$Date: 2025-01-06 12:18:29 +0200 (Mon, 06 Jan 2025) $
#$Revision: 297071 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/39/7133956.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_7133956
loop_
_publ_author_name
'Nakagawa, Aoi'
'Ota, Wataru'
'Ehara, Takumi'
'Matsuo, Yusuke'
'Miyata, Kiyoshi'
'Onda, Ken'
'Sato, Tohru'
'Seki, Shu'
'Tanaka, Takayuki'
_publ_section_title
;
 Synthesis of substituent-free dioxadiaza[8]circulene to investigate
 intermolecular interactions and photophysical properties.
;
_journal_issue                   99
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14770
_journal_page_last               14773
_journal_paper_doi               10.1039/d4cc05539j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C20 H21 N O), 2(C4 H8 O), 3.5[C4H8O]'
_chemical_formula_sum            'C62 H86 N2 O7.5'
_chemical_formula_weight         979.383
_chemical_name_common            tetra-tert-butyl-opp-dioxadiaza[8]circulene
_chemical_name_systematic        tetra-tert-butyldioxadiaza[8]circulene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-05-14
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.05.14 svn.rc2abdb5a for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-10-17 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                109.901(2)
_cell_angle_beta                 90.100(1)
_cell_angle_gamma                106.501(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2049(1)
_cell_length_b                   16.5666(3)
_cell_length_c                   17.5296(2)
_cell_measurement_reflns_used    40778
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      74.1940
_cell_measurement_theta_min      3.2160
_cell_volume                     2655.85(8)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9815
_diffrn_measured_fraction_theta_max 0.9815
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.9815
_diffrn_reflns_Laue_measured_fraction_max 0.9815
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33819
_diffrn_reflns_point_group_measured_fraction_full 0.9815
_diffrn_reflns_point_group_measured_fraction_max 0.9815
_diffrn_reflns_theta_full        65.9949
_diffrn_reflns_theta_max         65.99
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       prism
_exptl_crystal_F_000             1067.297
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.2832
_refine_diff_density_min         -0.2865
_refine_diff_density_rms         0.0739
_refine_ls_d_res_high            0.8439
_refine_ls_d_res_low             13.6861
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0369
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0369
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0970P)²+1.3486P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7752
_reflns_number_total             9071
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc05539j2.cif
_cod_data_source_block           210703nakagawa
_cod_depositor_comments
'Adding full bibliography for 7133954--7133956.cif.'
_cod_database_code               7133956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
3. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed X: Hh(-10) Hi(10) Hj(10) Hk(-10) Hl(-10) Hm(-10) Ho(10) Hn(-10)
 Fixed Y: Hh(-10) Hi(-10) Hj(10) Hk(10) Hl(-10) Hm(10) Hn(10) Ho(10)
 Fixed Z: Hh(-10) Hi(-10) Hj(10) Hk(-10) Hl(10) Hm(10) Hn(-10) Ho(10)
6.a Secondary CH2 refined with riding coordinates:
 C41(H41a,H41b), C42(H42a,H42b), C43(H43a,H43b), C44(H44a,H44b), C45(H45a,
 H45b), C46(H46a,H46b), C47(H47a,H47b), C48(H48a,H48b)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), N1(H1), C24(H24), C29(H29), N2(H2)
6.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C36(H36a,H36b,H36c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c),
 C40(H40a,H40b,H40c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -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_refinement_flags_posn
C1 C 0.10270(19) 0.97106(13) 0.56894(11) 0.0295(4) Uani 1.000000 .
C2 C 0.1682(2) 0.95053(14) 0.62653(11) 0.0308(4) Uani 1.000000 .
C3 C 0.2825(2) 0.91717(14) 0.61413(12) 0.0326(4) Uani 1.000000 .
C4 C 0.3294(2) 0.90572(14) 0.53731(12) 0.0345(4) Uani 1.000000 .
H4 H 0.4066(2) 0.88416(14) 0.52496(12) 0.0414(5) Uiso 1.000000 R
C5 C 0.2648(2) 0.92545(14) 0.47823(12) 0.0324(4) Uani 1.000000 .
C6 C 0.15012(19) 0.95774(13) 0.49224(11) 0.0301(4) Uani 1.000000 .
C7 C 0.11060(19) 0.96886(13) 0.41890(11) 0.0297(4) Uani 1.000000 .
C8 C 0.2025(2) 0.94324(13) 0.36251(12) 0.0312(4) Uani 1.000000 .
C9 C 0.1932(2) 0.94535(13) 0.28366(11) 0.0314(4) Uani 1.000000 .
H9 H 0.2572(2) 0.92690(13) 0.24760(11) 0.0377(5) Uiso 1.000000 R
C10 C 0.09180(19) 0.97401(13) 0.25698(11) 0.0290(4) Uani 1.000000 .
C11 C 0.00185(19) 1.00031(13) 0.31513(11) 0.0293(4) Uani 1.000000 .
C12 C 0.00758(19) 0.99790(13) 0.39334(11) 0.0291(4) Uani 1.000000 .
O1 O 0.10543(13) 0.96796(9) 0.69860(8) 0.0313(3) Uani 1.000000 .
N1 N 0.29583(17) 0.91729(12) 0.39936(10) 0.0341(4) Uani 1.000000 .
H1 H 0.36371(17) 0.89868(12) 0.37643(10) 0.0410(5) Uiso 1.000000 R
C13 C 0.3484(2) 0.89496(15) 0.67965(12) 0.0356(5) Uani 1.000000 .
C14 C 0.4009(2) 0.97949(16) 0.75599(13) 0.0424(5) Uani 1.000000 .
H14a H 0.4641(13) 1.0275(4) 0.7415(2) 0.0636(8) Uiso 1.000000 GR
H14b H 0.3230(3) 0.9991(7) 0.7792(6) 0.0636(8) Uiso 1.000000 GR
H14c H 0.4494(15) 0.9661(3) 0.7963(4) 0.0636(8) Uiso 1.000000 GR
C15 C 0.2407(2) 0.82181(17) 0.70142(14) 0.0441(5) Uani 1.000000 .
H15a H 0.1614(8) 0.8428(5) 0.7194(10) 0.0661(8) Uiso 1.000000 GR
H15b H 0.2106(13) 0.7664(4) 0.6533(3) 0.0661(8) Uiso 1.000000 GR
H15c H 0.2816(6) 0.8097(8) 0.7454(7) 0.0661(8) Uiso 1.000000 GR
C16 C 0.4694(2) 0.85937(17) 0.65019(13) 0.0414(5) Uani 1.000000 .
H16a H 0.4372(4) 0.8050(6) 0.6012(6) 0.0621(8) Uiso 1.000000 GR
H16b H 0.5401(8) 0.9055(4) 0.6373(10) 0.0621(8) Uiso 1.000000 GR
H16c H 0.5082(11) 0.8448(11) 0.6932(4) 0.0621(8) Uiso 1.000000 GR
C17 C 0.0791(2) 0.97816(14) 0.17156(11) 0.0320(4) Uani 1.000000 .
C18 C 0.1841(2) 0.94129(14) 0.11943(12) 0.0354(4) Uani 1.000000 .
H18a H 0.2773(2) 0.9782(6) 0.1449(5) 0.0531(7) Uiso 1.000000 GR
H18b H 0.1704(10) 0.8789(4) 0.1154(8) 0.0531(7) Uiso 1.000000 GR
H18c H 0.1716(10) 0.9432(10) 0.0647(3) 0.0531(7) Uiso 1.000000 GR
C19 C -0.0644(2) 0.92118(17) 0.12772(13) 0.0437(5) Uani 1.000000 .
H19a H -0.0796(7) 0.8584(3) 0.1229(9) 0.0656(8) Uiso 1.000000 GR
H19b H -0.1338(2) 0.9442(7) 0.1590(5) 0.0656(8) Uiso 1.000000 GR
H19c H -0.0717(6) 0.9244(9) 0.0732(4) 0.0656(8) Uiso 1.000000 GR
C20 C 0.1047(2) 1.07654(15) 0.17920(14) 0.0424(5) Uani 1.000000 .
H20a H 0.0353(11) 1.1000(4) 0.2101(9) 0.0636(8) Uiso 1.000000 GR
H20b H 0.1964(7) 1.1125(3) 0.2077(9) 0.0636(8) Uiso 1.000000 GR
H20c H 0.0986(17) 1.0800(2) 0.12464(14) 0.0636(8) Uiso 1.000000 GR
C21 C 0.37100(19) 0.43707(13) 0.05103(11) 0.0289(4) Uani 1.000000 .
C22 C 0.28346(19) 0.38355(12) 0.08700(11) 0.0290(4) Uani 1.000000 .
C23 C 0.16212(19) 0.39878(13) 0.11984(11) 0.0300(4) Uani 1.000000 .
C24 C 0.1350(2) 0.47489(13) 0.11521(12) 0.0323(4) Uani 1.000000 .
H24 H 0.0558(2) 0.48937(13) 0.13668(12) 0.0388(5) Uiso 1.000000 R
C25 C 0.22243(19) 0.53055(13) 0.07949(12) 0.0305(4) Uani 1.000000 .
C26 C 0.34232(19) 0.51360(13) 0.04683(11) 0.0291(4) Uani 1.000000 .
C27 C 0.59584(19) 0.41790(13) -0.01504(11) 0.0289(4) Uani 1.000000 .
C28 C 0.32040(19) 0.63935(13) 0.02894(12) 0.0301(4) Uani 1.000000 .
C29 C 0.35123(19) 0.71492(13) 0.00556(12) 0.0307(4) Uani 1.000000 .
H29 H 0.29145(19) 0.75128(13) 0.01615(12) 0.0368(5) Uiso 1.000000 R
C30 C 0.46839(19) 0.73780(13) -0.03309(11) 0.0294(4) Uani 1.000000 .
C31 C 0.47854(19) 0.39659(13) 0.02498(11) 0.0282(4) Uani 1.000000 .
C32 C 0.45025(19) 0.32122(13) 0.04682(11) 0.0282(4) Uani 1.000000 .
O2 O 0.32940(13) 0.31109(8) 0.08464(8) 0.0291(3) Uani 1.000000 .
N2 N 0.20998(16) 0.60678(11) 0.06749(10) 0.0324(4) Uani 1.000000 .
H2 H 0.14290(16) 0.63058(11) 0.08199(10) 0.0389(4) Uiso 1.000000 R
C33 C 0.0656(2) 0.33401(13) 0.15472(12) 0.0321(4) Uani 1.000000 .
C34 C 0.0135(2) 0.23999(14) 0.08806(13) 0.0373(5) Uani 1.000000 .
H34a H -0.0369(14) 0.2433(2) 0.0421(4) 0.0560(7) Uiso 1.000000 GR
H34b H 0.0919(2) 0.2184(5) 0.0691(7) 0.0560(7) Uiso 1.000000 GR
H34c H -0.0477(13) 0.1983(3) 0.1104(3) 0.0560(7) Uiso 1.000000 GR
C35 C -0.0604(2) 0.36436(14) 0.18381(14) 0.0378(5) Uani 1.000000 .
H35a H -0.0303(2) 0.4229(5) 0.2284(7) 0.0568(7) Uiso 1.000000 GR
H35b H -0.1093(9) 0.3696(10) 0.1384(3) 0.0568(7) Uiso 1.000000 GR
H35c H -0.1219(8) 0.3199(5) 0.2032(9) 0.0568(7) Uiso 1.000000 GR
C36 C 0.1429(2) 0.32925(15) 0.22782(13) 0.0384(5) Uani 1.000000 .
H36a H 0.2202(10) 0.3062(10) 0.2096(2) 0.0576(7) Uiso 1.000000 GR
H36b H 0.1775(14) 0.3896(2) 0.2696(4) 0.0576(7) Uiso 1.000000 GR
H36c H 0.0801(5) 0.2890(8) 0.2509(6) 0.0576(7) Uiso 1.000000 GR
C37 C 0.50733(19) 0.82020(13) -0.05843(12) 0.0305(4) Uani 1.000000 .
C38 C 0.6451(2) 0.88467(13) -0.01020(13) 0.0355(4) Uani 1.000000 .
H38a H 0.6354(5) 0.9035(8) 0.04834(13) 0.0533(7) Uiso 1.000000 GR
H38b H 0.7158(4) 0.8539(3) -0.0219(7) 0.0533(7) Uiso 1.000000 GR
H38c H 0.6719(8) 0.9377(5) -0.0263(7) 0.0533(7) Uiso 1.000000 GR
C39 C 0.5205(2) 0.79219(14) -0.15022(12) 0.0355(4) Uani 1.000000 .
H39a H 0.5935(11) 0.7635(9) -0.16288(19) 0.0533(7) Uiso 1.000000 GR
H39b H 0.4332(5) 0.7496(8) -0.18059(12) 0.0533(7) Uiso 1.000000 GR
H39c H 0.5431(16) 0.84558(19) -0.1659(2) 0.0533(7) Uiso 1.000000 GR
C40 C 0.3998(2) 0.87088(14) -0.04036(14) 0.0366(5) Uani 1.000000 .
H40a H 0.3104(4) 0.8303(3) -0.0694(8) 0.0549(7) Uiso 1.000000 GR
H40b H 0.3927(12) 0.8923(9) 0.01847(17) 0.0549(7) Uiso 1.000000 GR
H40c H 0.4275(8) 0.9224(6) -0.0586(9) 0.0549(7) Uiso 1.000000 GR
C41 C -0.1697(2) 0.59349(16) 0.14701(14) 0.0452(5) Uani 1.000000 .
H41a H -0.1546(2) 0.53547(16) 0.11492(14) 0.0542(6) Uiso 1.000000 R
H41b H -0.2696(2) 0.58404(16) 0.14939(14) 0.0542(6) Uiso 1.000000 R
C42 C -0.0928(2) 0.63240(16) 0.23299(14) 0.0462(5) Uani 1.000000 .
H42a H -0.1539(2) 0.65049(16) 0.27503(14) 0.0554(6) Uiso 1.000000 R
H42b H -0.0546(2) 0.58823(16) 0.24391(14) 0.0554(6) Uiso 1.000000 R
C43 C 0.0215(3) 0.7138(2) 0.23126(16) 0.0606(7) Uani 1.000000 .
H43a H 0.0002(3) 0.7701(2) 0.26227(16) 0.0727(8) Uiso 1.000000 R
H43b H 0.1098(3) 0.7156(2) 0.25621(16) 0.0727(8) Uiso 1.000000 R
O3 O 0.03032(15) 0.70540(10) 0.14805(9) 0.0423(4) Uani 1.000000 .
C44 C -0.1083(2) 0.66415(16) 0.11052(15) 0.0456(5) Uani 1.000000 .
H44a H -0.1107(2) 0.63638(16) 0.05059(15) 0.0547(6) Uiso 1.000000 R
H44b H -0.1592(2) 0.70905(16) 0.12259(15) 0.0547(6) Uiso 1.000000 R
C45 C 0.5935(2) 0.81994(18) 0.34633(15) 0.0497(6) Uani 1.000000 .
H45a H 0.5771(2) 0.77221(18) 0.37026(15) 0.0596(7) Uiso 1.000000 R
H45b H 0.6391(2) 0.87883(18) 0.38957(15) 0.0596(7) Uiso 1.000000 R
C46 C 0.6810(3) 0.8019(2) 0.27626(16) 0.0593(7) Uani 1.000000 .
H46a H 0.7454(3) 0.8589(2) 0.27558(16) 0.0712(8) Uiso 1.000000 R
H46b H 0.7348(3) 0.7623(2) 0.28115(16) 0.0712(8) Uiso 1.000000 R
C47 C 0.5831(3) 0.7572(3) 0.20171(19) 0.0817(11) Uani 1.000000 .
H47a H 0.6093(3) 0.7885(3) 0.16238(19) 0.0981(13) Uiso 1.000000 R
H47b H 0.5817(3) 0.6937(3) 0.17536(19) 0.0981(13) Uiso 1.000000 R
C48 C 0.4457(3) 0.76193(19) 0.22801(15) 0.0540(6) Uani 1.000000 .
H48a H 0.4013(3) 0.78607(19) 0.19415(15) 0.0648(8) Uiso 1.000000 R
H48b H 0.3852(3) 0.70123(19) 0.22223(15) 0.0648(8) Uiso 1.000000 R
O4 O 0.46828(17) 0.82014(13) 0.31132(10) 0.0570(5) Uani 1.000000 .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
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
C6 C1 C2 119.19(17) . . ?
C12 C1 C2 106.37(16) 2_576 . ?
C12 C1 C6 134.44(18) 2_576 . ?
C3 C2 C1 124.95(17) . . ?
O1 C2 C1 110.44(15) . . ?
O1 C2 C3 124.61(16) . . ?
C4 C3 C2 114.81(17) . . ?
C13 C3 C2 122.27(17) . . ?
C13 C3 C4 122.93(17) . . ?
H4 C4 C3 119.36(11) . . ?
C5 C4 C3 121.27(17) . . ?
C5 C4 H4 119.36(11) . . ?
C6 C5 C4 122.51(17) . . ?
N1 C5 C4 129.13(17) . . ?
N1 C5 C6 108.36(16) . . ?
C5 C6 C1 117.27(17) . . ?
C7 C6 C1 135.62(17) . . ?
C7 C6 C5 107.11(16) . . ?
C8 C7 C6 107.16(16) . . ?
C12 C7 C6 135.55(17) . . ?
C12 C7 C8 117.29(17) . . ?
C9 C8 C7 122.47(17) . . ?
N1 C8 C7 108.36(16) . . ?
N1 C8 C9 129.17(16) . . ?
H9 C9 C8 119.39(10) . . ?
C10 C9 C8 121.22(17) . . ?
C10 C9 H9 119.39(11) . . ?
C11 C10 C9 115.14(17) . . ?
C17 C10 C9 122.81(16) . . ?
C17 C10 C11 122.04(16) . . ?
C12 C11 C10 124.88(17) . . ?
O1 C11 C10 124.47(16) 2_576 . ?
O1 C11 C12 110.65(15) 2_576 . ?
C7 C12 C1 134.39(17) . 2_576 ?
C11 C12 C1 106.62(16) . 2_576 ?
C11 C12 C7 118.98(16) . . ?
C11 O1 C2 105.92(13) 2_576 . ?
C8 N1 C5 109.01(15) . . ?
H1 N1 C5 125.50(10) . . ?
H1 N1 C8 125.50(10) . . ?
C14 C13 C3 109.74(17) . . ?
C15 C13 C3 109.44(17) . . ?
C15 C13 C14 109.35(17) . . ?
C16 C13 C3 111.57(16) . . ?
C16 C13 C14 108.53(17) . . ?
C16 C13 C15 108.18(17) . . ?
H14a C14 C13 109.5 . . ?
H14b C14 C13 109.5 . . ?
H14b C14 H14a 109.5 . . ?
H14c C14 C13 109.5 . . ?
H14c C14 H14a 109.5 . . ?
H14c C14 H14b 109.5 . . ?
H15a C15 C13 109.5 . . ?
H15b C15 C13 109.5 . . ?
H15b C15 H15a 109.5 . . ?
H15c C15 C13 109.5 . . ?
H15c C15 H15a 109.5 . . ?
H15c C15 H15b 109.5 . . ?
H16a C16 C13 109.5 . . ?
H16b C16 C13 109.5 . . ?
H16b C16 H16a 109.5 . . ?
H16c C16 C13 109.5 . . ?
H16c C16 H16a 109.5 . . ?
H16c C16 H16b 109.5 . . ?
C18 C17 C10 111.42(16) . . ?
C19 C17 C10 110.06(16) . . ?
C19 C17 C18 107.64(16) . . ?
C20 C17 C10 108.94(16) . . ?
C20 C17 C18 108.69(16) . . ?
C20 C17 C19 110.08(18) . . ?
H18a C18 C17 109.5 . . ?
H18b C18 C17 109.5 . . ?
H18b C18 H18a 109.5 . . ?
H18c C18 C17 109.5 . . ?
H18c C18 H18a 109.5 . . ?
H18c C18 H18b 109.5 . . ?
H19a C19 C17 109.5 . . ?
H19b C19 C17 109.5 . . ?
H19b C19 H19a 109.5 . . ?
H19c C19 C17 109.5 . . ?
H19c C19 H19a 109.5 . . ?
H19c C19 H19b 109.5 . . ?
H20a C20 C17 109.5 . . ?
H20b C20 C17 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 C17 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
C26 C21 C22 119.44(16) . . ?
C31 C21 C22 106.43(16) . . ?
C31 C21 C26 134.13(17) . . ?
C23 C22 C21 124.81(17) . . ?
O2 C22 C21 110.53(15) . . ?
O2 C22 C23 124.64(16) . . ?
C24 C23 C22 115.08(17) . . ?
C33 C23 C22 122.15(16) . . ?
C33 C23 C24 122.73(16) . . ?
H24 C24 C23 119.36(11) . . ?
C25 C24 C23 121.28(17) . . ?
C25 C24 H24 119.36(10) . . ?
C26 C25 C24 122.51(17) . . ?
N2 C25 C24 129.26(17) . . ?
N2 C25 C26 108.22(16) . . ?
C25 C26 C21 116.87(17) . . ?
C27 C26 C21 135.77(17) 2_665 . ?
C27 C26 C25 107.34(16) 2_665 . ?
C28 C27 C26 107.13(16) 2_665 2_665 ?
C31 C27 C26 135.92(17) . 2_665 ?
C31 C27 C28 116.94(17) . 2_665 ?
C29 C28 C27 122.62(17) . 2_665 ?
N2 C28 C27 108.36(16) . 2_665 ?
N2 C28 C29 129.02(16) . . ?
H29 C29 C28 119.42(10) . . ?
C30 C29 C28 121.16(17) . . ?
C30 C29 H29 119.42(11) . . ?
C32 C30 C29 114.96(17) 2_665 . ?
C37 C30 C29 123.01(16) . . ?
C37 C30 C32 122.03(16) . 2_665 ?
C27 C31 C21 134.17(17) . . ?
C32 C31 C21 106.70(16) . . ?
C32 C31 C27 119.13(16) . . ?
C31 C32 C30 125.19(17) . 2_665 ?
O2 C32 C30 124.39(16) . 2_665 ?
O2 C32 C31 110.42(15) . . ?
C32 O2 C22 105.91(13) . . ?
C28 N2 C25 108.94(15) . . ?
H2 N2 C25 125.53(10) . . ?
H2 N2 C28 125.53(10) . . ?
C34 C33 C23 109.31(15) . . ?
C35 C33 C23 111.76(15) . . ?
C35 C33 C34 107.77(16) . . ?
C36 C33 C23 109.70(16) . . ?
C36 C33 C34 109.90(16) . . ?
C36 C33 C35 108.37(16) . . ?
H34a C34 C33 109.5 . . ?
H34b C34 C33 109.5 . . ?
H34b C34 H34a 109.5 . . ?
H34c C34 C33 109.5 . . ?
H34c C34 H34a 109.5 . . ?
H34c C34 H34b 109.5 . . ?
H35a C35 C33 109.5 . . ?
H35b C35 C33 109.5 . . ?
H35b C35 H35a 109.5 . . ?
H35c C35 C33 109.5 . . ?
H35c C35 H35a 109.5 . . ?
H35c C35 H35b 109.5 . . ?
H36a C36 C33 109.5 . . ?
H36b C36 C33 109.5 . . ?
H36b C36 H36a 109.5 . . ?
H36c C36 C33 109.5 . . ?
H36c C36 H36a 109.5 . . ?
H36c C36 H36b 109.5 . . ?
C38 C37 C30 108.54(16) . . ?
C39 C37 C30 110.37(16) . . ?
C39 C37 C38 109.87(16) . . ?
C40 C37 C30 112.07(15) . . ?
C40 C37 C38 108.22(16) . . ?
C40 C37 C39 107.74(16) . . ?
H38a C38 C37 109.5 . . ?
H38b C38 C37 109.5 . . ?
H38b C38 H38a 109.5 . . ?
H38c C38 C37 109.5 . . ?
H38c C38 H38a 109.5 . . ?
H38c C38 H38b 109.5 . . ?
H39a C39 C37 109.5 . . ?
H39b C39 C37 109.5 . . ?
H39b C39 H39a 109.5 . . ?
H39c C39 C37 109.5 . . ?
H39c C39 H39a 109.5 . . ?
H39c C39 H39b 109.5 . . ?
H40a C40 C37 109.5 . . ?
H40b C40 C37 109.5 . . ?
H40b C40 H40a 109.5 . . ?
H40c C40 C37 109.5 . . ?
H40c C40 H40a 109.5 . . ?
H40c C40 H40b 109.5 . . ?
H41b C41 H41a 109.0 . . ?
C42 C41 H41a 110.98(12) . . ?
C42 C41 H41b 110.98(12) . . ?
C44 C41 H41a 110.98(12) . . ?
C44 C41 H41b 110.98(12) . . ?
C44 C41 C42 103.91(19) . . ?
H42a C42 C41 111.10(12) . . ?
H42b C42 C41 111.10(12) . . ?
H42b C42 H42a 109.1 . . ?
C43 C42 C41 103.29(19) . . ?
C43 C42 H42a 111.10(13) . . ?
C43 C42 H42b 111.10(15) . . ?
H43a C43 C42 110.25(14) . . ?
H43b C43 C42 110.25(15) . . ?
H43b C43 H43a 108.5 . . ?
O3 C43 C42 107.3(2) . . ?
O3 C43 H43a 110.25(14) . . ?
O3 C43 H43b 110.25(13) . . ?
C44 O3 C43 104.66(17) . . ?
O3 C44 C41 105.10(18) . . ?
H44a C44 C41 110.72(13) . . ?
H44a C44 O3 110.72(11) . . ?
H44b C44 C41 110.72(12) . . ?
H44b C44 O3 110.72(11) . . ?
H44b C44 H44a 108.8 . . ?
H45b C45 H45a 108.8 . . ?
C46 C45 H45a 110.72(16) . . ?
C46 C45 H45b 110.72(15) . . ?
O4 C45 H45a 110.72(14) . . ?
O4 C45 H45b 110.72(13) . . ?
O4 C45 C46 105.1(2) . . ?
H46a C46 C45 110.65(15) . . ?
H46b C46 C45 110.65(15) . . ?
H46b C46 H46a 108.8 . . ?
C47 C46 C45 105.5(2) . . ?
C47 C46 H46a 110.7(2) . . ?
C47 C46 H46b 110.65(18) . . ?
H47a C47 C46 110.5(2) . . ?
H47b C47 C46 110.47(19) . . ?
H47b C47 H47a 108.7 . . ?
C48 C47 C46 106.3(2) . . ?
C48 C47 H47a 110.5(2) . . ?
C48 C47 H47b 110.47(19) . . ?
H48a C48 C47 110.35(19) . . ?
H48b C48 C47 110.3(2) . . ?
H48b C48 H48a 108.6 . . ?
O4 C48 C47 106.9(2) . . ?
O4 C48 H48a 110.35(13) . . ?
O4 C48 H48b 110.35(15) . . ?
C48 O4 C45 108.31(17) . . ?
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
C1 C2 1.393(3) . ?
C1 C6 1.397(3) . ?
C1 C12 1.438(2) 2_576 ?
C2 C3 1.414(3) . ?
C2 O1 1.396(2) . ?
C3 C4 1.400(3) . ?
C3 C13 1.527(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.402(3) . ?
C5 C6 1.408(3) . ?
C5 N1 1.389(2) . ?
C6 C7 1.432(3) . ?
C7 C8 1.407(3) . ?
C7 C12 1.404(3) . ?
C8 C9 1.398(3) . ?
C8 N1 1.389(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(3) . ?
C10 C11 1.414(3) . ?
C10 C17 1.529(3) . ?
C11 C12 1.387(3) . ?
C11 O1 1.394(2) 2_576 ?
N1 H1 0.8800 . ?
C13 C14 1.528(3) . ?
C13 C15 1.544(3) . ?
C13 C16 1.532(3) . ?
C14 H14a 0.9800 . ?
C14 H14b 0.9800 . ?
C14 H14c 0.9800 . ?
C15 H15a 0.9800 . ?
C15 H15b 0.9800 . ?
C15 H15c 0.9800 . ?
C16 H16a 0.9800 . ?
C16 H16b 0.9800 . ?
C16 H16c 0.9800 . ?
C17 C18 1.533(3) . ?
C17 C19 1.530(3) . ?
C17 C20 1.534(3) . ?
C18 H18a 0.9800 . ?
C18 H18b 0.9800 . ?
C18 H18c 0.9800 . ?
C19 H19a 0.9800 . ?
C19 H19b 0.9800 . ?
C19 H19c 0.9800 . ?
C20 H20a 0.9800 . ?
C20 H20b 0.9800 . ?
C20 H20c 0.9800 . ?
C21 C22 1.384(3) . ?
C21 C26 1.405(3) . ?
C21 C31 1.440(2) . ?
C22 C23 1.417(3) . ?
C22 O2 1.396(2) . ?
C23 C24 1.393(3) . ?
C23 C33 1.531(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.402(3) . ?
C25 C26 1.411(3) . ?
C25 N2 1.388(2) . ?
C26 C27 1.422(3) 2_665 ?
C27 C28 1.412(2) 2_665 ?
C27 C31 1.408(3) . ?
C28 C29 1.400(3) . ?
C28 N2 1.387(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.397(3) . ?
C30 C32 1.416(2) 2_665 ?
C30 C37 1.524(3) . ?
C31 C32 1.382(3) . ?
C32 O2 1.396(2) . ?
N2 H2 0.8800 . ?
C33 C34 1.537(3) . ?
C33 C35 1.536(2) . ?
C33 C36 1.540(3) . ?
C34 H34a 0.9800 . ?
C34 H34b 0.9800 . ?
C34 H34c 0.9800 . ?
C35 H35a 0.9800 . ?
C35 H35b 0.9800 . ?
C35 H35c 0.9800 . ?
C36 H36a 0.9800 . ?
C36 H36b 0.9800 . ?
C36 H36c 0.9800 . ?
C37 C38 1.536(3) . ?
C37 C39 1.533(3) . ?
C37 C40 1.534(2) . ?
C38 H38a 0.9800 . ?
C38 H38b 0.9800 . ?
C38 H38c 0.9800 . ?
C39 H39a 0.9800 . ?
C39 H39b 0.9800 . ?
C39 H39c 0.9800 . ?
C40 H40a 0.9800 . ?
C40 H40b 0.9800 . ?
C40 H40c 0.9800 . ?
C41 H41a 0.9900 . ?
C41 H41b 0.9900 . ?
C41 C42 1.533(3) . ?
C41 C44 1.505(3) . ?
C42 H42a 0.9900 . ?
C42 H42b 0.9900 . ?
C42 C43 1.521(4) . ?
C43 H43a 0.9900 . ?
C43 H43b 0.9900 . ?
C43 O3 1.423(3) . ?
O3 C44 1.429(3) . ?
C44 H44a 0.9900 . ?
C44 H44b 0.9900 . ?
C45 H45a 0.9900 . ?
C45 H45b 0.9900 . ?
C45 C46 1.517(3) . ?
C45 O4 1.418(3) . ?
C46 H46a 0.9900 . ?
C46 H46b 0.9900 . ?
C46 C47 1.473(4) . ?
C47 H47a 0.9900 . ?
C47 H47b 0.9900 . ?
C47 C48 1.492(4) . ?
C48 H48a 0.9900 . ?
C48 H48b 0.9900 . ?
C48 O4 1.425(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O4 0.8800 1.979(2) 2.828(2) 161.64(8) .
N2 H2 O3 0.8800 2.008(2) 2.857(2) 161.75(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.4(2) . . . . ?
C1 C2 C3 C13 -179.3(2) . . . . ?
C1 C2 O1 C11 0.25(19) . . . 2_576 ?
C1 C6 C5 C4 0.9(2) . . . . ?
C1 C6 C5 N1 -179.70(19) . . . . ?
C1 C6 C7 C8 179.9(3) . . . . ?
C1 C6 C7 C12 0.0(3) . . . . ?
C1 C12 C7 C6 -0.0(3) 2_576 . . . ?
C1 C12 C7 C8 -179.9(2) 2_576 . . . ?
C1 C12 C11 C10 -179.24(15) 2_576 . . . ?
C1 C12 C11 O1 -0.56(17) . 2_576 2_576 . ?
C2 C3 C4 C5 -0.7(2) . . . . ?
C2 C3 C13 C14 -60.1(2) . . . . ?
C2 C3 C13 C15 59.9(2) . . . . ?
C2 C3 C13 C16 179.5(2) . . . . ?
C2 O1 C11 C10 -179.60(15) . . 2_576 2_576 ?
C2 O1 C11 C12 0.20(16) . . 2_576 2_576 ?
C3 C4 C5 C6 0.1(3) . . . . ?
C3 C4 C5 N1 -179.18(19) . . . . ?
C4 C5 C6 C7 -179.1(2) . . . . ?
C4 C5 N1 C8 179.0(2) . . . . ?
C5 C6 C7 C8 -0.14(18) . . . . ?
C5 C6 C7 C12 -179.98(16) . . . . ?
C5 N1 C8 C7 0.30(18) . . . . ?
C5 N1 C8 C9 -179.43(16) . . . . ?
C6 C7 C8 C9 179.66(16) . . . . ?
C6 C7 C8 N1 -0.10(18) . . . . ?
C6 C7 C12 C11 179.5(2) . . . . ?
C7 C8 C9 C10 0.5(2) . . . . ?
C7 C12 C11 C10 1.1(2) . . . . ?
C7 C12 C11 O1 -179.12(18) . . . 2_576 ?
C8 C9 C10 C11 0.2(2) . . . . ?
C8 C9 C10 C17 179.39(18) . . . . ?
C9 C10 C11 C12 -1.0(2) . . . . ?
C9 C10 C11 O1 179.23(16) . . . 2_576 ?
C9 C10 C17 C18 3.8(2) . . . . ?
C9 C10 C17 C19 123.1(2) . . . . ?
C9 C10 C17 C20 -116.1(2) . . . . ?
C21 C22 C23 C24 -1.1(2) . . . . ?
C21 C22 C23 C33 176.64(19) . . . . ?
C21 C22 O2 C32 0.76(18) . . . . ?
C21 C26 C25 C24 0.4(2) . . . . ?
C21 C26 C25 N2 -178.27(18) . . . . ?
C21 C26 C27 C28 178.4(3) . . 2_665 . ?
C21 C26 C27 C31 -0.9(3) . . 2_665 2_665 ?
C21 C31 C27 C26 -0.4(3) . . . 2_665 ?
C21 C31 C27 C28 178.9(2) . . . 2_665 ?
C21 C31 C32 C30 -179.34(15) . . . 2_665 ?
C21 C31 C32 O2 0.65(17) . . . . ?
C22 C23 C24 C25 0.7(2) . . . . ?
C22 C23 C33 C34 -59.0(2) . . . . ?
C22 C23 C33 C35 -178.2(2) . . . . ?
C22 C23 C33 C36 61.6(2) . . . . ?
C22 O2 C32 C30 179.12(14) . . . 2_665 ?
C22 O2 C32 C31 -0.87(15) . . . . ?
C23 C24 C25 C26 -0.4(2) . . . . ?
C23 C24 C25 N2 177.96(18) . . . . ?
C24 C25 C26 C27 179.2(2) . . . 2_665 ?
C24 C25 N2 C28 -179.4(2) . . . . ?
C25 C26 C27 C28 -0.08(18) . . 2_665 . ?
C25 C26 C27 C31 -179.44(15) . . 2_665 2_665 ?
C25 N2 C28 C27 0.78(17) . . . 2_665 ?
C25 N2 C28 C29 -179.33(16) . . . . ?
C26 C27 C28 C29 179.68(15) . 2_665 . . ?
C26 C27 C28 N2 -0.43(17) . 2_665 . . ?
C26 C27 C31 C32 179.4(2) 2_665 . . . ?
C27 C28 C29 C30 -0.2(2) 2_665 . . . ?
C27 C31 C32 C30 0.8(2) . . . 2_665 ?
C27 C31 C32 O2 -179.23(18) . . . . ?
C28 C29 C30 C32 0.6(2) . . . 2_665 ?
C28 C29 C30 C37 -179.00(18) . . . . ?
C29 C30 C32 C31 -0.2(2) . . 2_665 2_665 ?
C29 C30 C32 O2 179.80(15) . . 2_665 2_665 ?
C29 C30 C37 C38 116.6(2) . . . . ?
C29 C30 C37 C39 -122.9(2) . . . . ?
C29 C30 C37 C40 -2.9(2) . . . . ?
C41 C42 C43 O3 -14.89(19) . . . . ?
C41 C44 O3 C43 -40.8(2) . . . . ?
C42 C43 O3 C44 34.8(2) . . . . ?
C45 C46 C47 C48 7.9(3) . . . . ?
C45 O4 C48 C47 -24.6(3) . . . . ?
C46 C47 C48 O4 9.5(3) . . . . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-16T01:10:56+02:00
;
 Replaced the '^A\/Y' character sequence with the backslash character ('\')
 in the '_diffrn_measurement_method' data value.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.447 0.500 0.500 837.5 284.5 '7 THF'
2 0.201 0.936 0.878 11.3 0.0 ?
3 0.799 0.064 0.122 11.3 0.0 ?
