#------------------------------------------------------------------------------
#$Date: 2021-09-06 15:34:37 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158141.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_7158141
loop_
_publ_author_name
'Zhan, Shao-Cong'
'Fang, Ren-Jie'
'Sun, Jing'
'Yan, Chao-Guo'
_publ_section_title
;
 Diastereoselective synthesis of spiro[carbazole-3,5'-pyrimidines] and
 spiro[carbazole-3,1'-cyclohexanes] via four-component reaction.
;
_journal_issue                   28
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              6322
_journal_page_last               6327
_journal_paper_doi               10.1039/d1ob01113h
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C34 H31 N3 O8'
_chemical_formula_sum            'C34 H31 N3 O8'
_chemical_formula_weight         609.62
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-04-20 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                105.432(2)
_cell_angle_beta                 103.175(2)
_cell_angle_gamma                103.079(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8318(6)
_cell_length_b                   11.4013(7)
_cell_length_c                   15.4837(8)
_cell_measurement_reflns_used    3969
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      2.34
_cell_volume                     1708.80(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17530
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.946
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6537
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1818
_refine_ls_R_factor_gt           0.0946
_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)+(0.1043P)²+2.4570P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2299
_refine_ls_wR_factor_ref         0.2804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3219
_reflns_number_total             6537
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ob01113h2.cif
_cod_data_source_block           3oo
_cod_depositor_comments
'Adding full bibliography for 7158139--7158148.cif.'
_cod_original_cell_volume        1708.79(17)
_cod_database_code               7158141
_shelx_shelxl_version_number     2014/7
_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   0.981
_shelx_estimated_absorpt_t_max   0.985
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
C1 C 0.6194(5) -0.0097(4) 0.2784(4) 0.0616(13) Uani 1 1 d . . . . .
C2 C 0.6950(5) -0.0932(5) 0.2696(5) 0.0800(17) Uani 1 1 d . . . . .
H2 H 0.7102 -0.1366 0.3120 0.096 Uiso 1 1 calc R U . . .
C3 C 0.7463(6) -0.1090(6) 0.1954(5) 0.0905(19) Uani 1 1 d . . . . .
H3 H 0.7992 -0.1626 0.1888 0.109 Uiso 1 1 calc R U . . .
C4 C 0.7219(6) -0.0477(6) 0.1304(5) 0.0871(18) Uani 1 1 d . . . . .
H4 H 0.7576 -0.0617 0.0807 0.104 Uiso 1 1 calc R U . . .
C5 C 0.6454(5) 0.0339(5) 0.1381(4) 0.0743(15) Uani 1 1 d . . . . .
H5 H 0.6289 0.0745 0.0939 0.089 Uiso 1 1 calc R U . . .
C6 C 0.5930(5) 0.0546(4) 0.2135(3) 0.0591(13) Uani 1 1 d . . . . .
C7 C 0.5110(4) 0.1295(4) 0.2449(3) 0.0506(11) Uani 1 1 d . . . . .
C8 C 0.4911(4) 0.1074(4) 0.3227(3) 0.0516(11) Uani 1 1 d . . . . .
C9 C 0.4064(4) 0.1613(4) 0.3756(3) 0.0518(11) Uani 1 1 d . . . . .
H9 H 0.4632 0.2410 0.4258 0.062 Uiso 1 1 calc R U . . .
C10 C 0.3422(6) 0.0714(5) 0.4203(5) 0.0670(14) Uani 1 1 d . . . . .
C11 C 0.1490(16) -0.1231(14) 0.3798(12) 0.099(2) Uani 0.487(10) 1 d D U P A 1
H11A H 0.2029 -0.1582 0.4189 0.119 Uiso 0.487(10) 1 calc R U P A 1
H11B H 0.0957 -0.1901 0.3208 0.119 Uiso 0.487(10) 1 calc R U P A 1
C12 C 0.0616(14) -0.0621(14) 0.4303(12) 0.105(3) Uani 0.487(10) 1 d D U P A 1
H12A H 0.1171 0.0101 0.4844 0.158 Uiso 0.487(10) 1 calc R U P A 1
H12B H 0.0087 -0.1236 0.4498 0.158 Uiso 0.487(10) 1 calc R U P A 1
H12C H 0.0042 -0.0346 0.3882 0.158 Uiso 0.487(10) 1 calc R U P A 1
C11' C 0.1741(11) -0.0821(14) 0.4253(11) 0.098(2) Uani 0.513(10) 1 d D U P A 2
H11C H 0.2170 -0.1449 0.4369 0.117 Uiso 0.513(10) 1 calc R U P A 2
H11D H 0.1803 -0.0219 0.4849 0.117 Uiso 0.513(10) 1 calc R U P A 2
C12' C 0.0302(10) -0.1450(14) 0.3621(11) 0.108(3) Uani 0.513(10) 1 d D U P A 2
H12D H -0.0028 -0.0829 0.3409 0.162 Uiso 0.513(10) 1 calc R U P A 2
H12E H -0.0235 -0.1780 0.3969 0.162 Uiso 0.513(10) 1 calc R U P A 2
H12F H 0.0263 -0.2136 0.3088 0.162 Uiso 0.513(10) 1 calc R U P A 2
C13 C 0.4507(4) 0.2123(4) 0.1995(3) 0.0493(11) Uani 1 1 d . . . . .
H13 H 0.3841 0.1543 0.1401 0.059 Uiso 1 1 calc R U . . .
C14 C 0.5515(5) 0.3006(4) 0.1729(3) 0.0536(12) Uani 1 1 d . . . . .
C15 C 0.6802(5) 0.3619(5) 0.2320(3) 0.0615(13) Uani 1 1 d . . . . .
H15 H 0.7060 0.3469 0.2886 0.074 Uiso 1 1 calc R U . . .
C16 C 0.7711(6) 0.4442(5) 0.2099(4) 0.0779(16) Uani 1 1 d . . . . .
H16 H 0.8571 0.4850 0.2508 0.094 Uiso 1 1 calc R U . . .
C17 C 0.7327(6) 0.4651(6) 0.1264(4) 0.0837(17) Uani 1 1 d . . . . .
C18 C 0.6075(7) 0.4040(6) 0.0640(4) 0.0833(17) Uani 1 1 d . . . . .
H18 H 0.5838 0.4180 0.0069 0.100 Uiso 1 1 calc R U . . .
C19 C 0.5175(5) 0.3216(5) 0.0872(3) 0.0678(14) Uani 1 1 d . . . . .
H19 H 0.4324 0.2792 0.0450 0.081 Uiso 1 1 calc R U . . .
C20 C 0.2595(5) 0.3059(5) 0.1869(3) 0.0580(12) Uani 1 1 d . . . . .
C21 C 0.2294(6) 0.4271(6) 0.2086(5) 0.1069(19) Uani 1 1 d . U . . .
H21A H 0.1616 0.4189 0.2400 0.128 Uiso 1 1 calc R U . . .
H21B H 0.1890 0.4363 0.1490 0.128 Uiso 1 1 calc R U . . .
C22 C 0.3354(6) 0.5487(5) 0.2660(4) 0.0803(13) Uani 1 1 d . U . . .
C23 C 0.2813(12) 0.6626(10) 0.3064(9) 0.096(3) Uani 0.571(8) 1 d . U P B 1
H23A H 0.2126 0.6334 0.3324 0.143 Uiso 0.571(8) 1 calc R U P B 1
H23B H 0.2456 0.6924 0.2566 0.143 Uiso 0.571(8) 1 calc R U P B 1
H23C H 0.3528 0.7311 0.3548 0.143 Uiso 0.571(8) 1 calc R U P B 1
C24 C 0.4160(13) 0.5856(12) 0.2056(9) 0.102(3) Uani 0.571(8) 1 d . U P B 1
H24A H 0.4807 0.6680 0.2399 0.153 Uiso 0.571(8) 1 calc R U P B 1
H24B H 0.3585 0.5892 0.1498 0.153 Uiso 0.571(8) 1 calc R U P B 1
H24C H 0.4608 0.5235 0.1884 0.153 Uiso 0.571(8) 1 calc R U P B 1
C23' C 0.2759(17) 0.5739(16) 0.3446(12) 0.110(3) Uani 0.429(8) 1 d . U P B 2
H23D H 0.2924 0.5196 0.3809 0.165 Uiso 0.429(8) 1 calc R U P B 2
H23E H 0.1816 0.5567 0.3191 0.165 Uiso 0.429(8) 1 calc R U P B 2
H23F H 0.3154 0.6617 0.3843 0.165 Uiso 0.429(8) 1 calc R U P B 2
C24' C 0.3477(15) 0.6523(14) 0.2202(11) 0.089(3) Uani 0.429(8) 1 d . U P B 2
H24D H 0.3951 0.7341 0.2677 0.133 Uiso 0.429(8) 1 calc R U P B 2
H24E H 0.2605 0.6523 0.1887 0.133 Uiso 0.429(8) 1 calc R U P B 2
H24F H 0.3954 0.6354 0.1754 0.133 Uiso 0.429(8) 1 calc R U P B 2
C25 C 0.4440(8) 0.5296(7) 0.3278(6) 0.143(2) Uani 1 1 d . U . . .
H25A H 0.5236 0.5758 0.3180 0.172 Uiso 1 1 calc R U . . .
H25B H 0.4466 0.5761 0.3909 0.172 Uiso 1 1 calc R U . . .
C26 C 0.4642(5) 0.4126(4) 0.3324(3) 0.0508(11) Uani 1 1 d . . . . .
C27 C 0.3724(4) 0.2854(4) 0.2579(3) 0.0466(11) Uani 1 1 d . . . . .
C28 C 0.3026(4) 0.1941(4) 0.3062(3) 0.0479(11) Uani 1 1 d . . . . .
H28 H 0.2506 0.1134 0.2554 0.057 Uiso 1 1 calc R U . . .
C29 C 0.2052(4) 0.2393(4) 0.3523(3) 0.0461(10) Uani 1 1 d . . . . .
C30 C 0.2462(4) 0.3263(4) 0.4429(3) 0.0513(11) Uani 1 1 d . . . . .
H30 H 0.3369 0.3622 0.4747 0.062 Uiso 1 1 calc R U . . .
C31 C 0.1575(5) 0.3611(4) 0.4871(3) 0.0565(12) Uani 1 1 d . . . . .
H31 H 0.1871 0.4197 0.5478 0.068 Uiso 1 1 calc R U . . .
C32 C 0.0234(4) 0.3071(4) 0.4394(3) 0.0504(11) Uani 1 1 d . . . . .
C33 C -0.0225(5) 0.2217(4) 0.3487(4) 0.0585(12) Uani 1 1 d . . . . .
H33 H -0.1133 0.1876 0.3169 0.070 Uiso 1 1 calc R U . . .
C34 C 0.0693(4) 0.1882(4) 0.3065(3) 0.0554(12) Uani 1 1 d . . . . .
H34 H 0.0394 0.1298 0.2456 0.067 Uiso 1 1 calc R U . . .
N1 N 0.5567(4) 0.0236(4) 0.3451(3) 0.0597(11) Uani 1 1 d . . . . .
H1 H 0.5581 -0.0029 0.3922 0.072 Uiso 1 1 calc R U . . .
N3 N -0.0728(4) 0.3411(4) 0.4871(3) 0.0640(11) Uani 1 1 d . . . . .
O1 O 0.3909(5) 0.0791(5) 0.5001(3) 0.1066(15) Uani 1 1 d . . . . .
O2 O 0.2327(4) -0.0143(4) 0.3638(3) 0.0957(13) Uani 1 1 d . U . . .
N2 N 0.821(2) 0.566(2) 0.1066(16) 0.119(4) Uani 0.617(16) 1 d . U P C 1
O3 O 0.7763(13) 0.5979(13) 0.0392(9) 0.117(3) Uani 0.617(16) 1 d . U P C 1
O4 O 0.9337(13) 0.6227(15) 0.1662(9) 0.137(4) Uani 0.617(16) 1 d . U P C 1
N2' N 0.844(4) 0.528(3) 0.093(3) 0.122(4) Uani 0.383(16) 1 d . U P C 1
O3' O 0.817(2) 0.544(2) 0.0207(15) 0.126(4) Uani 0.383(16) 1 d . U P C 1
O4' O 0.955(2) 0.554(2) 0.1320(15) 0.125(4) Uani 0.383(16) 1 d . U P C 1
O5 O 0.1918(5) 0.2199(5) 0.1188(3) 0.1247(19) Uani 1 1 d . . . . .
O6 O 0.5521(4) 0.4171(3) 0.3954(2) 0.0799(11) Uani 1 1 d . . . . .
O7 O -0.0284(4) 0.4141(4) 0.5689(3) 0.0835(11) Uani 1 1 d . . . . .
O8 O -0.1907(4) 0.2956(4) 0.4437(3) 0.0920(13) Uani 1 1 d . . . . .
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
N1 C1 C2 129.5(5) . . ?
N1 C1 C6 108.5(4) . . ?
C2 C1 C6 122.1(5) . . ?
C3 C2 C1 117.2(6) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C2 C3 C4 122.2(6) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 120.9(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.9(6) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C1 118.8(5) . . ?
C5 C6 C7 135.4(5) . . ?
C1 C6 C7 105.9(4) . . ?
C8 C7 C6 107.4(4) . . ?
C8 C7 C13 124.5(4) . . ?
C6 C7 C13 128.0(4) . . ?
C7 C8 N1 110.5(4) . . ?
C7 C8 C9 125.2(4) . . ?
N1 C8 C9 124.3(4) . . ?
C8 C9 C10 111.9(4) . . ?
C8 C9 C28 107.5(4) . . ?
C10 C9 C28 112.6(4) . . ?
C8 C9 H9 108.2 . . ?
C10 C9 H9 108.2 . . ?
C28 C9 H9 108.2 . . ?
O1 C10 O2 124.2(5) . . ?
O1 C10 C9 122.3(5) . . ?
O2 C10 C9 113.6(5) . . ?
O2 C11 C12 102.7(10) . . ?
O2 C11 H11A 111.2 . . ?
C12 C11 H11A 111.2 . . ?
O2 C11 H11B 111.2 . . ?
C12 C11 H11B 111.2 . . ?
H11A C11 H11B 109.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C12' C11' O2 100.1(10) . . ?
C12' C11' H11C 111.7 . . ?
O2 C11' H11C 111.7 . . ?
C12' C11' H11D 111.7 . . ?
O2 C11' H11D 111.7 . . ?
H11C C11' H11D 109.5 . . ?
C11' C12' H12D 109.5 . . ?
C11' C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
C11' C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
C7 C13 C14 112.0(4) . . ?
C7 C13 C27 113.3(3) . . ?
C14 C13 C27 112.7(4) . . ?
C7 C13 H13 106.0 . . ?
C14 C13 H13 106.0 . . ?
C27 C13 H13 106.0 . . ?
C15 C14 C19 117.6(4) . . ?
C15 C14 C13 121.4(4) . . ?
C19 C14 C13 121.0(4) . . ?
C16 C15 C14 122.0(5) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C17 C16 C15 118.6(5) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C18 121.8(5) . . ?
C16 C17 N2 119.8(11) . . ?
C18 C17 N2 118.1(11) . . ?
C16 C17 N2' 116.4(18) . . ?
C18 C17 N2' 119.6(17) . . ?
N2 C17 N2' 21.3(15) . . ?
C17 C18 C19 119.0(5) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C14 121.0(5) . . ?
C18 C19 H19 119.5 . . ?
C14 C19 H19 119.5 . . ?
O5 C20 C21 120.0(5) . . ?
O5 C20 C27 119.4(5) . . ?
C21 C20 C27 120.4(5) . . ?
C20 C21 C22 120.9(5) . . ?
C20 C21 H21A 107.1 . . ?
C22 C21 H21A 107.1 . . ?
C20 C21 H21B 107.1 . . ?
C22 C21 H21B 107.1 . . ?
H21A C21 H21B 106.8 . . ?
C25 C22 C21 112.1(5) . . ?
C25 C22 C24 93.5(8) . . ?
C21 C22 C24 108.0(7) . . ?
C25 C22 C23' 88.8(9) . . ?
C21 C22 C23' 94.3(8) . . ?
C25 C22 C24' 125.3(8) . . ?
C21 C22 C24' 114.9(8) . . ?
C23' C22 C24' 113.6(9) . . ?
C25 C22 C23 118.5(7) . . ?
C21 C22 C23 113.9(6) . . ?
C24 C22 C23 108.4(7) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C23' H23D 109.5 . . ?
C22 C23' H23E 109.5 . . ?
H23D C23' H23E 109.5 . . ?
C22 C23' H23F 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C22 C24' H24D 109.5 . . ?
C22 C24' H24E 109.5 . . ?
H24D C24' H24E 109.5 . . ?
C22 C24' H24F 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
C26 C25 C22 128.2(6) . . ?
C26 C25 H25A 105.2 . . ?
C22 C25 H25A 105.2 . . ?
C26 C25 H25B 105.2 . . ?
C22 C25 H25B 105.2 . . ?
H25A C25 H25B 106.0 . . ?
O6 C26 C25 117.7(5) . . ?
O6 C26 C27 122.0(4) . . ?
C25 C26 C27 120.3(5) . . ?
C26 C27 C20 111.5(4) . . ?
C26 C27 C13 112.1(3) . . ?
C20 C27 C13 107.6(3) . . ?
C26 C27 C28 110.4(3) . . ?
C20 C27 C28 106.9(3) . . ?
C13 C27 C28 108.0(3) . . ?
C29 C28 C9 110.8(3) . . ?
C29 C28 C27 115.5(3) . . ?
C9 C28 C27 111.6(3) . . ?
C29 C28 H28 106.1 . . ?
C9 C28 H28 106.1 . . ?
C27 C28 H28 106.1 . . ?
C34 C29 C30 117.5(4) . . ?
C34 C29 C28 120.2(4) . . ?
C30 C29 C28 122.1(4) . . ?
C31 C30 C29 122.2(4) . . ?
C31 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
C30 C31 C32 118.4(4) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
C33 C32 C31 121.7(4) . . ?
C33 C32 N3 119.4(4) . . ?
C31 C32 N3 118.8(4) . . ?
C34 C33 C32 118.4(4) . . ?
C34 C33 H33 120.8 . . ?
C32 C33 H33 120.8 . . ?
C33 C34 C29 121.7(4) . . ?
C33 C34 H34 119.1 . . ?
C29 C34 H34 119.1 . . ?
C1 N1 C8 107.8(4) . . ?
C1 N1 H1 126.1 . . ?
C8 N1 H1 126.1 . . ?
O8 N3 O7 124.0(5) . . ?
O8 N3 C32 118.4(5) . . ?
O7 N3 C32 117.6(4) . . ?
C10 O2 C11 128.9(8) . . ?
C10 O2 C11' 105.3(6) . . ?
O3 N2 O4 124.1(16) . . ?
O3 N2 C17 118.7(17) . . ?
O4 N2 C17 116.7(16) . . ?
O4' N2' O3' 117(3) . . ?
O4' N2' C17 124(3) . . ?
O3' N2' C17 119(3) . . ?
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 N1 1.378(6) . ?
C1 C2 1.389(7) . ?
C1 C6 1.410(7) . ?
C2 C3 1.373(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.441(6) . ?
C7 C8 1.347(6) . ?
C7 C13 1.495(6) . ?
C8 N1 1.381(5) . ?
C8 C9 1.491(6) . ?
C9 C10 1.513(7) . ?
C9 C28 1.554(6) . ?
C9 H9 0.9800 . ?
C10 O1 1.198(6) . ?
C10 O2 1.294(6) . ?
C11 O2 1.475(14) . ?
C11 C12 1.528(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C11' C12' 1.526(5) . ?
C11' O2 1.534(15) . ?
C11' H11C 0.9700 . ?
C11' H11D 0.9700 . ?
C12' H12D 0.9600 . ?
C12' H12E 0.9600 . ?
C12' H12F 0.9600 . ?
C13 C14 1.518(6) . ?
C13 C27 1.581(6) . ?
C13 H13 0.9800 . ?
C14 C15 1.381(6) . ?
C14 C19 1.393(6) . ?
C15 C16 1.369(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.366(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(8) . ?
C17 N2 1.47(2) . ?
C17 N2' 1.52(4) . ?
C18 C19 1.374(7) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 O5 1.176(6) . ?
C20 C21 1.462(8) . ?
C20 C27 1.553(6) . ?
C21 C22 1.479(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C25 1.435(8) . ?
C22 C24 1.493(12) . ?
C22 C23' 1.494(16) . ?
C22 C24' 1.528(14) . ?
C22 C23 1.581(12) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?
C25 C26 1.418(8) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 O6 1.178(5) . ?
C26 C27 1.535(6) . ?
C27 C28 1.591(6) . ?
C28 C29 1.510(6) . ?
C28 H28 0.9800 . ?
C29 C34 1.388(6) . ?
C29 C30 1.388(6) . ?
C30 C31 1.369(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.379(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.378(6) . ?
C32 N3 1.471(6) . ?
C33 C34 1.378(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N1 H1 0.8600 . ?
N3 O8 1.215(5) . ?
N3 O7 1.228(5) . ?
N2 O3 1.23(2) . ?
N2 O4 1.25(2) . ?
N2' O4' 1.14(3) . ?
N2' O3' 1.17(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 O1 0.86 2.10 2.937(5) 163.9 2_656
