#------------------------------------------------------------------------------
#$Date: 2020-06-26 02:27:38 +0300 (Fri, 26 Jun 2020) $
#$Revision: 253452 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/85/4038523.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_4038523
loop_
_publ_author_name
'Mohite, Amar Ramchandra'
'Reany, Ofer'
_publ_section_title
;
 Inherently Chiral Bambus[4]urils.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01174
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C52 H56 N16 O8 [+ solvent]'
_chemical_formula_sum            'C52 H56 N16 O8'
_chemical_formula_weight         1033.12
_chemical_name_common            ro24_sq
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 127.66(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.264(5)
_cell_length_b                   18.390(4)
_cell_length_c                   17.423(4)
_cell_measurement_reflns_used    8386
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.052
_cell_measurement_theta_min      1.565
_cell_volume                     5901(3)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13822
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.052
_diffrn_reflns_theta_max         25.052
_diffrn_reflns_theta_min         1.565
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 2174 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8386
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1347P)²+14.8296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2551
_reflns_Friedel_coverage         0.616
_reflns_Friedel_fraction_full    0.612
_reflns_Friedel_fraction_max     0.612
_reflns_number_gt                6453
_reflns_number_total             8386
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c01174_si_002.cif
_cod_data_source_block           ro24_sq
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4038523
_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_min   0.969
_shelx_estimated_absorpt_t_max   0.988
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -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
O1 O 0.4378(4) 0.6075(3) 0.0866(5) 0.0626(17) Uani 1 1 d . . . . .
O2 O 0.4241(4) 0.5068(3) 0.3977(4) 0.0445(13) Uani 1 1 d . . . . .
O3 O 0.6483(4) 0.6248(4) 0.8293(5) 0.0690(18) Uani 1 1 d . . . . .
O4 O 0.6794(4) 0.5058(3) 0.5353(5) 0.0549(15) Uani 1 1 d . . . . .
O5 O 0.7984(6) 0.1928(5) 0.5278(7) 0.104(3) Uani 1 1 d . . . . .
O6 O 0.6146(4) 0.3072(4) 0.6418(5) 0.0594(16) Uani 1 1 d . . . . .
O7 O 0.2943(6) 0.1942(5) 0.4014(7) 0.098(3) Uani 1 1 d . . . . .
O8 O 0.4810(4) 0.2989(3) 0.2914(5) 0.0472(13) Uani 1 1 d . . . . .
N1 N 0.4363(4) 0.4996(4) 0.1493(5) 0.0457(16) Uani 1 1 d . . . . .
N2 N 0.5145(4) 0.5843(4) 0.2512(5) 0.0478(16) Uani 1 1 d . . . . .
N3 N 0.5110(4) 0.5384(3) 0.3810(5) 0.0444(15) Uani 1 1 d . . . . .
N4 N 0.4231(4) 0.4625(4) 0.2717(5) 0.0429(15) Uani 1 1 d . . . . .
N5 N 0.5756(5) 0.5875(4) 0.6704(6) 0.0559(18) Uani 1 1 d . . . . .
N6 N 0.6694(4) 0.5198(4) 0.7797(5) 0.0543(18) Uani 1 1 d . . . . .
N7 N 0.6795(5) 0.4674(4) 0.6601(5) 0.0533(18) Uani 1 1 d . . . . .
N8 N 0.5965(4) 0.5474(4) 0.5561(5) 0.0437(15) Uani 1 1 d . . . . .
N9 N 0.7736(5) 0.2915(5) 0.5841(8) 0.080(2) Uani 1 1 d . . . . .
N10 N 0.6822(6) 0.2295(5) 0.4580(7) 0.076(3) Uani 1 1 d . . . . .
N11 N 0.6139(5) 0.2662(4) 0.5162(6) 0.059(2) Uani 1 1 d . . . . .
N12 N 0.6951(5) 0.3485(5) 0.6160(6) 0.058(2) Uani 1 1 d . . . . .
N13 N 0.4138(5) 0.2321(4) 0.4769(6) 0.059(2) Uani 1 1 d . . . . .
N14 N 0.3223(5) 0.2962(4) 0.3523(6) 0.060(2) Uani 1 1 d . . . . .
N15 N 0.3977(4) 0.3444(3) 0.3118(5) 0.0439(15) Uani 1 1 d . . . . .
N16 N 0.4829(5) 0.2674(4) 0.4206(5) 0.0515(17) Uani 1 1 d . . . . .
C1 C 0.4590(5) 0.5680(5) 0.1544(6) 0.0453(18) Uani 1 1 d . . . . .
C2 C 0.5293(5) 0.5233(4) 0.3160(6) 0.0439(19) Uani 1 1 d . . . . .
H2 H 0.579638 0.503715 0.351072 0.053 Uiso 1 1 calc R U . . .
C3 C 0.4699(5) 0.4670(4) 0.2433(6) 0.0417(18) Uani 1 1 d . . . . .
H3 H 0.491814 0.418714 0.248608 0.050 Uiso 1 1 calc R U . . .
C4 C 0.4499(5) 0.5036(4) 0.3540(6) 0.0389(17) Uani 1 1 d . . . . .
C5 C 0.3750(5) 0.4677(5) 0.0594(7) 0.060(2) Uani 1 1 d . . . . .
H5A H 0.329666 0.485890 0.044792 0.090 Uiso 1 1 calc R U . . .
H5B H 0.376795 0.414656 0.065876 0.090 Uiso 1 1 calc R U . . .
H5C H 0.377048 0.480987 0.006626 0.090 Uiso 1 1 calc R U . . .
C6 C 0.5615(6) 0.6453(5) 0.2807(7) 0.055(2) Uani 1 1 d . . . . .
H6A H 0.557678 0.662283 0.223774 0.066 Uiso 1 1 calc R U . . .
H6B H 0.611986 0.628324 0.329639 0.066 Uiso 1 1 calc R U . . .
C7A C 0.5491(4) 0.7091(4) 0.3220(6) 0.0796(17) Uani 1 1 d G . . . .
C8 C 0.6086(4) 0.7507(5) 0.3925(7) 0.0796(17) Uani 0.597(15) 1 d G . P A 1
H8 H 0.654554 0.742795 0.406745 0.095 Uiso 0.597(15) 1 calc R U P A 1
C9 C 0.6008(5) 0.8040(5) 0.4423(7) 0.0796(17) Uani 0.597(15) 1 d G . P A 1
H9 H 0.641480 0.832383 0.490447 0.095 Uiso 0.597(15) 1 calc R U P A 1
C10A C 0.5336(6) 0.8156(5) 0.4215(8) 0.135(4) Uani 1 1 d DG . . A .
H10A H 0.528267 0.851945 0.455440 0.162 Uiso 1 1 calc R U . B 1
C11A C 0.4741(5) 0.7740(5) 0.3509(8) 0.135(4) Uani 1 1 d G . . A .
H11A H 0.428126 0.781919 0.336731 0.162 Uiso 1 1 calc R U . . .
C12A C 0.4819(4) 0.7208(4) 0.3012(6) 0.0796(17) Uani 1 1 d G . . A .
H12A H 0.441198 0.692330 0.253028 0.095 Uiso 1 1 calc R U . . .
C8A C 0.587(2) 0.767(2) 0.328(4) 0.135(4) Uani 0.403(15) 1 d . . P A 2
H8A H 0.617410 0.773120 0.309229 0.162 Uiso 0.403(15) 1 calc R U P A 2
C9A C 0.5660(7) 0.824(2) 0.3764(9) 0.135(4) Uani 0.403(15) 1 d D . P A 2
H9A H 0.577982 0.872574 0.374019 0.162 Uiso 0.403(15) 1 calc R U P A 2
C13 C 0.5517(6) 0.5850(3) 0.4654(7) 0.0486(16) Uani 1 1 d . . . . .
H13A H 0.582929 0.617399 0.459590 0.058 Uiso 1 1 calc R U . . .
H13B H 0.517169 0.616149 0.465702 0.058 Uiso 1 1 calc R U . . .
C14 C 0.6330(5) 0.5822(5) 0.7655(6) 0.055(2) Uani 1 1 d . . . . .
C15 C 0.5742(5) 0.5290(4) 0.6157(6) 0.0405(17) Uani 1 1 d . . . . .
H15 H 0.526016 0.503908 0.576632 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6353(5) 0.4773(5) 0.6929(6) 0.049(2) Uani 1 1 d . . . . .
H16 H 0.615881 0.430252 0.697021 0.059 Uiso 1 1 calc R U . . .
C17 C 0.6541(5) 0.5060(4) 0.5791(6) 0.0447(18) Uani 1 1 d . . . . .
C18 C 0.5286(6) 0.6513(5) 0.6274(7) 0.064(3) Uani 1 1 d . . . . .
H18A H 0.512408 0.664888 0.665864 0.096 Uiso 1 1 calc R U . . .
H18B H 0.486288 0.640096 0.560947 0.096 Uiso 1 1 calc R U . . .
H18C H 0.555593 0.691865 0.626650 0.096 Uiso 1 1 calc R U . . .
C19 C 0.7302(6) 0.4936(6) 0.8781(7) 0.070(3) Uani 1 1 d D . . . .
H19A H 0.719749 0.505602 0.923819 0.084 Uiso 1 1 calc R U . C 1
H19B H 0.733402 0.439972 0.876458 0.084 Uiso 1 1 calc R U . C 1
C20 C 0.8013(10) 0.5257(12) 0.9145(19) 0.145(5) Uani 0.832(15) 1 d D . P D 1
C20A C 0.8060(12) 0.514(3) 0.921(3) 0.089(12) Uani 0.168(15) 1 d DG . P D 2
C21A C 0.8561(17) 0.495(3) 1.018(3) 0.089(12) Uani 0.168(15) 1 d DG . P D 2
H21A H 0.840061 0.474588 1.052153 0.107 Uiso 0.168(15) 1 calc R U P D 2
C22A C 0.9298(15) 0.506(3) 1.065(2) 0.089(12) Uani 0.168(15) 1 d DG . P D 2
H22A H 0.964120 0.492934 1.131785 0.107 Uiso 0.168(15) 1 calc R U P D 2
C23A C 0.9533(12) 0.536(3) 1.016(3) 0.089(12) Uani 0.168(15) 1 d DG . P D 2
H23A H 1.003710 0.543069 1.047951 0.107 Uiso 0.168(15) 1 calc R U P D 2
C24A C 0.9032(18) 0.555(3) 0.919(3) 0.089(12) Uani 0.168(15) 1 d DG . P D 2
H24A H 0.919241 0.574859 0.884486 0.107 Uiso 0.168(15) 1 calc R U P D 2
C25A C 0.8295(16) 0.544(3) 0.871(2) 0.089(12) Uani 0.168(15) 1 d DG . P D 2
H25A H 0.795181 0.556514 0.804852 0.107 Uiso 0.168(15) 1 calc R U P D 2
C21 C 0.8565(9) 0.4801(11) 0.9340(16) 0.138(6) Uani 0.832(15) 1 d D . P D 1
H21 H 0.847914 0.429432 0.921819 0.165 Uiso 0.832(15) 1 calc R U P D 1
C22 C 0.9263(9) 0.5099(12) 0.9727(17) 0.138(6) Uani 0.832(15) 1 d D . P D 1
H22 H 0.963332 0.479969 0.981669 0.165 Uiso 0.832(15) 1 calc R U P D 1
C23 C 0.9386(11) 0.5814(12) 0.9961(17) 0.145(5) Uani 0.832(15) 1 d D . P D 1
H23 H 0.986387 0.599310 1.026823 0.174 Uiso 0.832(15) 1 calc R U P D 1
C24 C 0.8874(10) 0.6294(12) 0.9786(17) 0.145(5) Uani 0.832(15) 1 d D . P D 1
H24 H 0.898869 0.678950 0.997489 0.174 Uiso 0.832(15) 1 calc R U P D 1
C25 C 0.8144(9) 0.6013(11) 0.9298(16) 0.145(5) Uani 0.832(15) 1 d D . P D 1
H25 H 0.775383 0.633740 0.908113 0.174 Uiso 0.832(15) 1 calc R U P D 1
C26 C 0.7276(6) 0.4067(6) 0.6882(8) 0.068(3) Uani 1 1 d . . . . .
H26A H 0.741720 0.386944 0.750422 0.081 Uiso 1 1 calc R U . . .
H26B H 0.772295 0.423855 0.698763 0.081 Uiso 1 1 calc R U . . .
C27 C 0.7528(8) 0.2324(6) 0.5202(9) 0.075(3) Uani 1 1 d . . . . .
C28 C 0.7077(6) 0.3363(6) 0.5441(8) 0.067(3) Uani 1 1 d . . . . .
H28 H 0.708317 0.382740 0.514714 0.081 Uiso 1 1 calc R U . . .
C29 C 0.6458(6) 0.2867(5) 0.4697(8) 0.061(3) Uani 1 1 d . . . . .
H29 H 0.610094 0.312768 0.407237 0.073 Uiso 1 1 calc R U . . .
C30 C 0.6385(6) 0.3065(5) 0.5953(7) 0.054(2) Uani 1 1 d . . . . .
C31 C 0.8447(7) 0.3183(7) 0.6498(9) 0.080(2) Uani 1 1 d . . . . .
H31A H 0.877567 0.278175 0.689211 0.120 Uiso 1 1 calc R U . . .
H31B H 0.846017 0.354595 0.692072 0.120 Uiso 1 1 calc R U . . .
H31C H 0.859956 0.340885 0.613941 0.120 Uiso 1 1 calc R U . . .
C32 C 0.6462(8) 0.1918(6) 0.3667(9) 0.081(3) Uani 1 1 d D . . . .
H32A H 0.684108 0.178041 0.360099 0.097 Uiso 1 1 calc R U . E 1
H32B H 0.614273 0.227543 0.314891 0.097 Uiso 1 1 calc R U . E 1
C33 C 0.6010(7) 0.1248(5) 0.3445(10) 0.099(5) Uani 0.75(3) 1 d DG . P F 1
C34 C 0.6309(8) 0.0703(7) 0.4143(10) 0.093(5) Uani 0.75(3) 1 d DG . P F 1
H34 H 0.677622 0.076764 0.474602 0.112 Uiso 0.75(3) 1 calc R U P F 1
C35 C 0.5926(11) 0.0064(7) 0.3959(15) 0.194(15) Uani 0.75(3) 1 d DG . P F 1
H35 H 0.613011 -0.030842 0.443631 0.232 Uiso 0.75(3) 1 calc R U P F 1
C36 C 0.5243(11) -0.0031(8) 0.3078(17) 0.196(15) Uani 0.75(3) 1 d DG . P F 1
H36 H 0.498044 -0.046752 0.295177 0.235 Uiso 0.75(3) 1 calc R U P F 1
C37 C 0.4944(8) 0.0514(10) 0.2380(13) 0.173(11) Uani 0.75(3) 1 d DG . P F 1
H37 H 0.447688 0.044944 0.177693 0.208 Uiso 0.75(3) 1 calc R U P F 1
C38 C 0.5327(7) 0.1153(7) 0.2564(9) 0.099(5) Uani 0.75(3) 1 d DG . P F 1
H38 H 0.512299 0.152551 0.208662 0.119 Uiso 0.75(3) 1 calc R U P F 1
C33A C 0.616(3) 0.126(2) 0.378(4) 0.16(2) Uani 0.25(3) 1 d D . P F 2
C34A C 0.660(3) 0.090(3) 0.468(4) 0.16(2) Uani 0.25(3) 1 d D . P F 2
H34A H 0.705577 0.109847 0.519527 0.189 Uiso 0.25(3) 1 calc R U P F 2
C35A C 0.636(4) 0.026(2) 0.481(5) 0.16(2) Uani 0.25(3) 1 d D . P F 2
H35A H 0.667765 -0.005422 0.533945 0.189 Uiso 0.25(3) 1 calc R U P F 2
C36A C 0.562(4) 0.009(3) 0.411(5) 0.16(2) Uani 0.25(3) 1 d D . P F 2
H36A H 0.540775 -0.028135 0.425138 0.189 Uiso 0.25(3) 1 calc R U P F 2
C37A C 0.518(3) 0.045(2) 0.322(5) 0.16(2) Uani 0.25(3) 1 d D . P F 2
H37A H 0.472528 0.025169 0.269567 0.189 Uiso 0.25(3) 1 calc R U P F 2
C38A C 0.543(3) 0.109(2) 0.312(4) 0.16(2) Uani 0.25(3) 1 d D . P F 2
H38A H 0.510947 0.141913 0.261343 0.189 Uiso 0.25(3) 1 calc R U P F 2
C39 C 0.5490(7) 0.2246(4) 0.4698(9) 0.062(2) Uani 1 1 d . . . . .
H39A H 0.552433 0.193796 0.519050 0.074 Uiso 1 1 calc R U . . .
H39B H 0.545400 0.191858 0.421949 0.074 Uiso 1 1 calc R U . . .
C40 C 0.3389(7) 0.2375(6) 0.4082(8) 0.067(3) Uani 1 1 d . . . . .
C41 C 0.4486(5) 0.2912(4) 0.4639(6) 0.0448(19) Uani 1 1 d . . . . .
H41 H 0.482695 0.319374 0.524985 0.054 Uiso 1 1 calc R U . . .
C42 C 0.3845(5) 0.3391(4) 0.3816(6) 0.0398(17) Uani 1 1 d . . . . .
H42 H 0.383791 0.387991 0.406142 0.048 Uiso 1 1 calc R U . . .
C43 C 0.4574(5) 0.3032(4) 0.3372(7) 0.0474(19) Uani 1 1 d . . . . .
C44 C 0.4453(9) 0.1970(6) 0.5682(9) 0.095(4) Uani 1 1 d . . . . .
H44A H 0.488945 0.223463 0.619732 0.142 Uiso 1 1 calc R U . . .
H44B H 0.458405 0.146888 0.565460 0.142 Uiso 1 1 calc R U . . .
H44C H 0.410147 0.196502 0.581696 0.142 Uiso 1 1 calc R U . . .
C45 C 0.2509(6) 0.3095(6) 0.2638(8) 0.068(3) Uani 1 1 d D . . . .
H45A H 0.216737 0.275322 0.260987 0.082 Uiso 0.597(15) 1 calc R U P A 1
H45B H 0.251344 0.297745 0.208695 0.082 Uiso 0.597(15) 1 calc R U P A 1
H45C H 0.253466 0.306631 0.209207 0.082 Uiso 0.403(15) 1 calc R U P A 2
H45D H 0.218574 0.269762 0.254950 0.082 Uiso 0.403(15) 1 calc R U P A 2
C46 C 0.2205(11) 0.3881(8) 0.2489(13) 0.117(8) Uani 0.597(15) 1 d DG . P A 1
C47 C 0.1712(11) 0.4124(10) 0.1540(11) 0.097(8) Uani 0.597(15) 1 d DG . P A 1
H47 H 0.157635 0.381649 0.101526 0.117 Uiso 0.597(15) 1 calc R U P A 1
C48 C 0.1419(9) 0.4818(10) 0.1358(10) 0.098(6) Uani 0.597(15) 1 d DG . P A 1
H48 H 0.108153 0.498476 0.070954 0.117 Uiso 0.597(15) 1 calc R U P A 1
C49 C 0.1618(10) 0.5269(8) 0.2126(13) 0.117(9) Uani 0.597(15) 1 d DG . P A 1
H49 H 0.141672 0.574340 0.200139 0.140 Uiso 0.597(15) 1 calc R U P A 1
C50 C 0.2111(10) 0.5026(10) 0.3074(11) 0.169(15) Uani 0.597(15) 1 d DG . P A 1
H50 H 0.224674 0.533378 0.359895 0.203 Uiso 0.597(15) 1 calc R U P A 1
C51 C 0.2405(9) 0.4332(10) 0.3256(10) 0.101(7) Uani 0.597(15) 1 d DG . P A 1
H51 H 0.274157 0.416552 0.390468 0.121 Uiso 0.597(15) 1 calc R U P A 1
C46A C 0.2178(13) 0.3775(10) 0.2571(16) 0.066(4) Uani 0.403(15) 1 d DG . P A 2
C47A C 0.1731(16) 0.4172(14) 0.1719(15) 0.091(11) Uani 0.403(15) 1 d DG . P A 2
H47A H 0.167575 0.402832 0.115344 0.110 Uiso 0.403(15) 1 calc R U P A 2
C48A C 0.1365(17) 0.4780(15) 0.1694(18) 0.114(15) Uani 0.403(15) 1 d DG . P A 2
H48A H 0.105914 0.505125 0.111205 0.137 Uiso 0.403(15) 1 calc R U P A 2
C49A C 0.1446(15) 0.4990(15) 0.252(2) 0.17(2) Uani 0.403(15) 1 d DG . P A 2
H49A H 0.119524 0.540563 0.250499 0.199 Uiso 0.403(15) 1 calc R U P A 2
C50A C 0.1893(13) 0.4593(17) 0.3374(16) 0.117(8) Uani 0.403(15) 1 d DG . P A 2
H50A H 0.194796 0.473708 0.393932 0.140 Uiso 0.403(15) 1 calc R U P A 2
C51A C 0.2259(12) 0.3986(14) 0.3398(14) 0.117(8) Uani 0.403(15) 1 d DG . P A 2
H51A H 0.256458 0.371414 0.398073 0.140 Uiso 0.403(15) 1 calc R U P A 2
C52 C 0.3721(5) 0.4038(4) 0.2430(6) 0.0437(18) Uani 1 1 d . . . . .
H52A H 0.358014 0.383520 0.180969 0.052 Uiso 1 1 calc R U . . .
H52B H 0.327816 0.424304 0.230599 0.052 Uiso 1 1 calc R U . . .
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'
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
C1 N1 C3 113.2(6) . . ?
C1 N1 C5 122.4(7) . . ?
C3 N1 C5 123.5(6) . . ?
C1 N2 C6 123.0(7) . . ?
C1 N2 C2 112.0(6) . . ?
C6 N2 C2 123.6(7) . . ?
C4 N3 C13 122.0(7) . . ?
C4 N3 C2 112.5(6) . . ?
C13 N3 C2 125.5(7) . . ?
C4 N4 C52 121.4(6) . . ?
C4 N4 C3 111.4(6) . . ?
C52 N4 C3 123.5(6) . . ?
C14 N5 C15 111.5(7) . . ?
C14 N5 C18 123.7(8) . . ?
C15 N5 C18 124.0(7) . . ?
C14 N6 C16 112.8(7) . . ?
C14 N6 C19 122.3(8) . . ?
C16 N6 C19 124.1(8) . . ?
C17 N7 C26 121.0(7) . . ?
C17 N7 C16 112.4(7) . . ?
C26 N7 C16 123.4(7) . . ?
C17 N8 C13 120.8(7) . . ?
C17 N8 C15 112.0(6) . . ?
C13 N8 C15 124.3(7) . . ?
C31 N9 C27 125.4(9) . . ?
C31 N9 C28 123.4(10) . . ?
C27 N9 C28 107.4(10) . . ?
C27 N10 C29 113.8(10) . . ?
C27 N10 C32 121.5(9) . . ?
C29 N10 C32 120.8(9) . . ?
C30 N11 C39 121.1(8) . . ?
C30 N11 C29 112.8(9) . . ?
C39 N11 C29 123.5(8) . . ?
C30 N12 C26 123.2(7) . . ?
C30 N12 C28 110.4(8) . . ?
C26 N12 C28 125.4(9) . . ?
C40 N13 C44 120.7(9) . . ?
C40 N13 C41 109.7(8) . . ?
C44 N13 C41 123.6(9) . . ?
C40 N14 C45 123.0(8) . . ?
C40 N14 C42 113.7(8) . . ?
C45 N14 C42 122.7(7) . . ?
C43 N15 C42 112.5(6) . . ?
C43 N15 C52 119.8(6) . . ?
C42 N15 C52 124.1(6) . . ?
C43 N16 C39 120.5(7) . . ?
C43 N16 C41 112.8(7) . . ?
C39 N16 C41 125.0(7) . . ?
O1 C1 N1 126.1(8) . . ?
O1 C1 N2 125.4(8) . . ?
N1 C1 N2 108.4(7) . . ?
N3 C2 N2 114.0(6) . . ?
N3 C2 C3 102.8(6) . . ?
N2 C2 C3 101.9(6) . . ?
N1 C3 N4 114.3(7) . . ?
N1 C3 C2 104.0(6) . . ?
N4 C3 C2 103.8(6) . . ?
O2 C4 N3 124.7(7) . . ?
O2 C4 N4 125.9(7) . . ?
N3 C4 N4 109.3(6) . . ?
N2 C6 C7A 117.4(7) . . ?
C8A C7A C12A 118.4(17) . . ?
C8 C7A C12A 120.0 . . ?
C8A C7A C6 110.6(17) . . ?
C8 C7A C6 118.5(6) . . ?
C12A C7A C6 120.9(6) . . ?
C7A C8 C9 120.0 . . ?
C10A C9 C8 120.0 . . ?
C11A C10A C9 120.0 . . ?
C11A C10A C9A 98.7(11) . . ?
C12A C11A C10A 120.0 . . ?
C11A C12A C7A 120.0 . . ?
C7A C8A C9A 99(3) . . ?
C10A C9A C8A 133(3) . . ?
N8 C13 N3 114.7(5) . . ?
O3 C14 N5 126.0(9) . . ?
O3 C14 N6 125.0(8) . . ?
N5 C14 N6 108.9(7) . . ?
N5 C15 N8 115.4(6) . . ?
N5 C15 C16 104.4(6) . . ?
N8 C15 C16 102.9(6) . . ?
N6 C16 N7 114.4(7) . . ?
N6 C16 C15 101.8(7) . . ?
N7 C16 C15 103.3(6) . . ?
O4 C17 N7 125.7(8) . . ?
O4 C17 N8 125.5(7) . . ?
N7 C17 N8 108.7(7) . . ?
C20A C19 N6 120.1(16) . . ?
C20 C19 N6 113.0(12) . . ?
C21 C20 C25 119.2(16) . . ?
C21 C20 C19 119.0(17) . . ?
C25 C20 C19 121.8(16) . . ?
C21A C20A C25A 120.0 . . ?
C21A C20A C19 114(2) . . ?
C25A C20A C19 126(2) . . ?
C20A C21A C22A 120.0 . . ?
C23A C22A C21A 120.0 . . ?
C22A C23A C24A 120.0 . . ?
C25A C24A C23A 120.0 . . ?
C24A C25A C20A 120.0 . . ?
C20 C21 C22 119.8(18) . . ?
C23 C22 C21 118.8(18) . . ?
C22 C23 C24 124.6(19) . . ?
C23 C24 C25 116.9(18) . . ?
C20 C25 C24 120.0(17) . . ?
N7 C26 N12 112.9(8) . . ?
O5 C27 N10 129.3(12) . . ?
O5 C27 N9 121.0(13) . . ?
N10 C27 N9 109.7(9) . . ?
N12 C28 N9 111.8(8) . . ?
N12 C28 C29 104.0(8) . . ?
N9 C28 C29 103.6(8) . . ?
N10 C29 N11 115.9(7) . . ?
N10 C29 C28 103.1(8) . . ?
N11 C29 C28 102.8(8) . . ?
O6 C30 N11 126.8(10) . . ?
O6 C30 N12 124.6(9) . . ?
N11 C30 N12 108.6(7) . . ?
N10 C32 C33A 105(2) . . ?
N10 C32 C33 121.3(10) . . ?
C34 C33 C38 120.0 . . ?
C34 C33 C32 117.8(9) . . ?
C38 C33 C32 122.1(9) . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C37 C36 C35 120.0 . . ?
C38 C37 C36 120.0 . . ?
C37 C38 C33 120.0 . . ?
C38A C33A C34A 120(3) . . ?
C38A C33A C32 121(3) . . ?
C34A C33A C32 117(3) . . ?
C35A C34A C33A 119(3) . . ?
C34A C35A C36A 117(3) . . ?
C37A C36A C35A 122(3) . . ?
C38A C37A C36A 118(3) . . ?
C37A C38A C33A 119(3) . . ?
N11 C39 N16 114.7(6) . . ?
O7 C40 N14 126.0(12) . . ?
O7 C40 N13 124.5(11) . . ?
N14 C40 N13 109.6(8) . . ?
N13 C41 N16 112.9(6) . . ?
N13 C41 C42 104.7(7) . . ?
N16 C41 C42 102.2(6) . . ?
N15 C42 N14 115.3(6) . . ?
N15 C42 C41 103.8(6) . . ?
N14 C42 C41 101.9(6) . . ?
O8 C43 N16 126.4(8) . . ?
O8 C43 N15 125.9(8) . . ?
N16 C43 N15 107.6(7) . . ?
C46A C45 N14 116.5(11) . . ?
N14 C45 C46 116.4(10) . . ?
C47 C46 C51 120.0 . . ?
C47 C46 C45 117.2(11) . . ?
C51 C46 C45 122.8(11) . . ?
C46 C47 C48 120.0 . . ?
C49 C48 C47 120.0 . . ?
C48 C49 C50 120.0 . . ?
C49 C50 C51 120.0 . . ?
C50 C51 C46 120.0 . . ?
C47A C46A C51A 120.0 . . ?
C47A C46A C45 124.0(14) . . ?
C51A C46A C45 115.6(14) . . ?
C46A C47A C48A 120.0 . . ?
C49A C48A C47A 120.0 . . ?
C50A C49A C48A 120.0 . . ?
C49A C50A C51A 120.0 . . ?
C50A C51A C46A 120.0 . . ?
N4 C52 N15 116.0(7) . . ?
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
O1 C1 1.204(10) . ?
O2 C4 1.225(9) . ?
O3 C14 1.222(11) . ?
O4 C17 1.214(9) . ?
O5 C27 1.224(13) . ?
O6 C30 1.232(9) . ?
O7 C40 1.254(12) . ?
O8 C43 1.217(9) . ?
N1 C1 1.347(10) . ?
N1 C3 1.445(10) . ?
N1 C5 1.450(11) . ?
N2 C1 1.393(10) . ?
N2 C6 1.425(10) . ?
N2 C2 1.475(10) . ?
N3 C4 1.355(10) . ?
N3 C13 1.446(10) . ?
N3 C2 1.460(9) . ?
N4 C4 1.387(10) . ?
N4 C52 1.448(10) . ?
N4 C3 1.449(10) . ?
N5 C14 1.354(11) . ?
N5 C15 1.426(10) . ?
N5 C18 1.460(11) . ?
N6 C14 1.356(12) . ?
N6 C16 1.436(11) . ?
N6 C19 1.487(12) . ?
N7 C17 1.351(10) . ?
N7 C26 1.439(12) . ?
N7 C16 1.460(10) . ?
N8 C17 1.371(10) . ?
N8 C13 1.433(11) . ?
N8 C15 1.457(10) . ?
N9 C31 1.404(16) . ?
N9 C27 1.414(16) . ?
N9 C28 1.487(12) . ?
N10 C27 1.304(16) . ?
N10 C29 1.440(12) . ?
N10 C32 1.444(15) . ?
N11 C30 1.345(12) . ?
N11 C39 1.425(14) . ?
N11 C29 1.443(11) . ?
N12 C30 1.371(13) . ?
N12 C26 1.461(14) . ?
N12 C28 1.467(11) . ?
N13 C40 1.389(14) . ?
N13 C44 1.435(14) . ?
N13 C41 1.453(10) . ?
N14 C40 1.344(14) . ?
N14 C45 1.438(14) . ?
N14 C42 1.439(10) . ?
N15 C43 1.396(11) . ?
N15 C42 1.429(9) . ?
N15 C52 1.453(10) . ?
N16 C43 1.356(11) . ?
N16 C39 1.451(13) . ?
N16 C41 1.461(10) . ?
C2 C3 1.564(12) . ?
C6 C7A 1.495(10) . ?
C7A C8A 1.35(4) . ?
C7A C8 1.3900 . ?
C7A C12A 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10A 1.3900 . ?
C10A C11A 1.3900 . ?
C10A C9A 1.3902(14) . ?
C11A C12A 1.3900 . ?
C8A C9A 1.59(5) . ?
C15 C16 1.548(11) . ?
C19 C20A 1.48(2) . ?
C19 C20 1.485(19) . ?
C20 C21 1.39(2) . ?
C20 C25 1.41(2) . ?
C20A C21A 1.3900 . ?
C20A C25A 1.3900 . ?
C21A C22A 1.3900 . ?
C22A C23A 1.3900 . ?
C23A C24A 1.3900 . ?
C24A C25A 1.3900 . ?
C21 C22 1.435(19) . ?
C22 C23 1.355(19) . ?
C23 C24 1.36(2) . ?
C24 C25 1.454(19) . ?
C28 C29 1.518(16) . ?
C32 C33A 1.47(3) . ?
C32 C33 1.508(15) . ?
C33 C34 1.3900 . ?
C33 C38 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C37 C38 1.3900 . ?
C33A C38A 1.38(2) . ?
C33A C34A 1.40(2) . ?
C34A C35A 1.38(2) . ?
C35A C36A 1.41(3) . ?
C36A C37A 1.40(3) . ?
C37A C38A 1.38(2) . ?
C41 C42 1.563(12) . ?
C45 C46A 1.436(18) . ?
C45 C46 1.560(15) . ?
C46 C47 1.3900 . ?
C46 C51 1.3900 . ?
C47 C48 1.3900 . ?
C48 C49 1.3900 . ?
C49 C50 1.3900 . ?
C50 C51 1.3900 . ?
C46A C47A 1.3900 . ?
C46A C51A 1.3900 . ?
C47A C48A 1.3900 . ?
C48A C49A 1.3900 . ?
C49A C50A 1.3900 . ?
C50A C51A 1.3900 . ?
