#------------------------------------------------------------------------------
#$Date: 2023-05-05 06:22:04 +0300 (Fri, 05 May 2023) $
#$Revision: 283470 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/92/7159256.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_7159256
loop_
_publ_author_name
'Sierra, Sonia'
'López, Rosa'
'Gómez-Bengoa, Enrique'
'Falvello, Larry R.'
'Urriolabeitia, Esteban P.'
_publ_section_title
;
 Synthesis of 1,2-diaminotruxinic δ-cyclobutanes by
 BF₃-controlled [2 + 2]-photocycloaddition of
 5(4H)-oxazolones and stereoselective expansion of
 δ-cyclobutanes to give highly substituted
 pyrrolidine-2,5-dicarboxylates.
;
_journal_issue                   15
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              3203
_journal_page_last               3213
_journal_paper_doi               10.1039/d3ob00284e
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C34 H26 F4 N2 O6, C H Cl3'
_chemical_formula_sum            'C35 H27 Cl3 F4 N2 O6'
_chemical_formula_weight         753.93
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                99.183(2)
_cell_angle_beta                 93.990(2)
_cell_angle_gamma                108.186(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4722(13)
_cell_length_b                   10.4254(15)
_cell_length_c                   18.483(3)
_cell_measurement_reflns_used    3825
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.704
_cell_measurement_theta_min      2.180
_cell_volume                     1697.9(4)
_computing_cell_refinement       'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (farrugia, 2012)'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17823
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         1.125
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       plate
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         6931
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      447.202
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0495P)²+0.5915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4584
_reflns_number_total             6931
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ob00284e2.cif
_cod_data_source_block           cmpnd_2s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct method' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7159254--7159256.cif.
;
_cod_database_code               7159256
_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.
;
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
N1 N 0.7256(2) 0.7810(2) 0.32969(10) 0.0203(4) Uani 1 1 d . . . . .
N2 N 0.4842(2) 0.48527(18) 0.18482(10) 0.0200(4) Uani 1 1 d . . . . .
O1 O 0.75369(18) 0.47460(17) 0.23209(10) 0.0371(4) Uani 1 1 d . . . . .
O2 O 0.93412(16) 0.66981(15) 0.28418(9) 0.0288(4) Uani 1 1 d . . . . .
O3 O 0.72006(19) 0.61630(16) 0.39491(9) 0.0321(4) Uani 1 1 d . . . . .
O4 O 0.39360(17) 0.68246(16) 0.33919(9) 0.0286(4) Uani 1 1 d . . . . .
O5 O 0.39783(17) 0.46481(16) 0.31659(9) 0.0290(4) Uani 1 1 d . . . . .
O6 O 0.23524(16) 0.45014(15) 0.17008(9) 0.0251(4) Uani 1 1 d . . . . .
F1 F 0.77439(17) 1.22619(14) 0.15484(9) 0.0459(4) Uani 1 1 d . . . . .
F2 F 1.18433(15) 1.10035(16) 0.23214(9) 0.0479(4) Uani 1 1 d . . . . .
F3 F 0.32729(15) 0.54933(15) -0.05920(7) 0.0365(4) Uani 1 1 d . . . . .
F4 F 0.04718(17) 0.75301(18) 0.09030(9) 0.0542(5) Uani 1 1 d . . . . .
C1 C 0.6925(2) 0.6848(2) 0.26049(12) 0.0195(5) Uani 1 1 d . . . . .
C2 C 0.6862(2) 0.7617(2) 0.19448(12) 0.0194(5) Uani 1 1 d . . . . .
C3 C 0.5176(2) 0.7362(2) 0.20096(12) 0.0202(5) Uani 1 1 d . . . . .
C4 C 0.5166(2) 0.6106(2) 0.23828(12) 0.0197(5) Uani 1 1 d . . . . .
C5 C 0.7929(2) 0.5950(2) 0.25758(12) 0.0232(5) Uani 1 1 d . . . . .
C6 C 1.0383(3) 0.5921(3) 0.2829(2) 0.0437(8) Uani 1 1 d . . . . .
C7 C 0.7361(2) 0.7375(2) 0.39453(12) 0.0233(5) Uani 1 1 d . . . . .
C8 C 0.7699(2) 0.8432(2) 0.46355(12) 0.0239(5) Uani 1 1 d . . . . .
C9 C 0.7085(3) 0.9485(3) 0.47130(14) 0.0317(6) Uani 1 1 d . . . . .
C10 C 0.7398(3) 1.0412(3) 0.53810(15) 0.0405(7) Uani 1 1 d . . . . .
C11 C 0.8332(3) 1.0290(3) 0.59529(16) 0.0420(7) Uani 1 1 d . . . . .
C12 C 0.8955(3) 0.9250(3) 0.58721(14) 0.0361(6) Uani 1 1 d . . . . .
C13 C 0.8628(3) 0.8316(3) 0.52172(13) 0.0297(6) Uani 1 1 d . . . . .
C14 C 0.7897(2) 0.9055(2) 0.19831(12) 0.0207(5) Uani 1 1 d . . . . .
C15 C 0.7326(3) 1.0049(2) 0.17971(13) 0.0257(5) Uani 1 1 d . . . . .
C16 C 0.8312(3) 1.1331(2) 0.17718(14) 0.0302(6) Uani 1 1 d . . . . .
C17 C 0.9834(3) 1.1701(3) 0.19440(13) 0.0304(6) Uani 1 1 d . . . . .
C18 C 1.0350(3) 1.0693(3) 0.21370(13) 0.0302(6) Uani 1 1 d . . . . .
C19 C 0.9440(3) 0.9387(2) 0.21571(13) 0.0261(5) Uani 1 1 d . . . . .
C20 C 0.4079(2) 0.7137(2) 0.13366(12) 0.0201(5) Uani 1 1 d . . . . .
C21 C 0.4252(3) 0.6489(2) 0.06466(13) 0.0238(5) Uani 1 1 d . . . . .
C22 C 0.3124(3) 0.6179(2) 0.00713(12) 0.0261(5) Uani 1 1 d . . . . .
C23 C 0.1841(3) 0.6511(3) 0.01310(14) 0.0305(6) Uani 1 1 d . . . . .
C24 C 0.1726(3) 0.7188(3) 0.08153(14) 0.0312(6) Uani 1 1 d . . . . .
C25 C 0.2804(3) 0.7519(2) 0.14166(14) 0.0267(5) Uani 1 1 d . . . . .
C26 C 0.4268(2) 0.5918(2) 0.30355(12) 0.0224(5) Uani 1 1 d . . . . .
C27 C 0.3180(4) 0.4351(4) 0.37889(18) 0.0435(7) Uani 1 1 d . . . . .
C28 C 0.3414(2) 0.4106(2) 0.15575(12) 0.0208(5) Uani 1 1 d . . . . .
C29 C 0.3220(2) 0.2793(2) 0.10399(12) 0.0213(5) Uani 1 1 d . . . . .
C30 C 0.4151(3) 0.2016(2) 0.11261(14) 0.0276(5) Uani 1 1 d . . . . .
C31 C 0.3888(3) 0.0772(3) 0.06495(14) 0.0332(6) Uani 1 1 d . . . . .
C32 C 0.2720(3) 0.0322(3) 0.00788(14) 0.0332(6) Uani 1 1 d . . . . .
C33 C 0.1815(3) 0.1108(2) -0.00177(14) 0.0297(6) Uani 1 1 d . . . . .
C34 C 0.2060(3) 0.2328(2) 0.04627(13) 0.0260(5) Uani 1 1 d . . . . .
Cl1 Cl 0.59095(12) 0.28488(11) 0.45602(5) 0.0768(3) Uani 1 1 d . . . . .
C50A C 0.6536(4) 0.2918(4) 0.3710(2) 0.0371(9) Uiso 0.726(2) 1 d . . P A 1
Cl3A Cl 0.52099(13) 0.15965(12) 0.30716(7) 0.0624(4) Uani 0.726(2) 1 d . . P A 1
C50B C 0.7277(17) 0.3388(13) 0.4064(7) 0.058(3) Uiso 0.274(2) 1 d . . P A 2
Cl3B Cl 0.8885(4) 0.4174(4) 0.4794(2) 0.0811(14) Uani 0.274(2) 1 d . . P A 2
Cl2A Cl 0.8345(4) 0.2748(7) 0.3743(4) 0.0448(11) Uiso 0.472(17) 1 d . . P B 3
Cl2B Cl 0.8156(7) 0.2406(9) 0.3565(5) 0.0496(14) Uiso 0.364(17) 1 d . . P C 4
Cl2C Cl 0.836(3) 0.329(3) 0.406(2) 0.083(10) Uiso 0.057(7) 1 d . . P D 5
Cl2D Cl 0.7344(13) 0.2042(9) 0.3328(5) 0.049(3) Uiso 0.105(4) 1 d . . P E 6
H1N H 0.748(3) 0.863(3) 0.3300(13) 0.026(7) Uiso 1 1 d . . . . .
H2N H 0.555(3) 0.451(2) 0.1802(13) 0.029(7) Uiso 1 1 d . . . . .
H2 H 0.698(2) 0.702(2) 0.1516(12) 0.013(5) Uiso 1 1 d . . . . .
H3 H 0.507(3) 0.812(2) 0.2386(13) 0.031(7) Uiso 1 1 d . . . . .
H6A H 1.044(3) 0.553(3) 0.2330(18) 0.061(10) Uiso 1 1 d . . . . .
H6B H 1.000(3) 0.520(3) 0.3118(16) 0.054(9) Uiso 1 1 d . . . . .
H6C H 1.125(3) 0.651(3) 0.3071(15) 0.041(8) Uiso 1 1 d . . . . .
H9 H 0.646(3) 0.957(3) 0.4315(15) 0.038(7) Uiso 1 1 d . . . . .
H10 H 0.695(3) 1.109(3) 0.5438(14) 0.035(7) Uiso 1 1 d . . . . .
H11 H 0.851(3) 1.089(3) 0.6369(17) 0.056(9) Uiso 1 1 d . . . . .
H12 H 0.963(3) 0.919(3) 0.6288(15) 0.040(7) Uiso 1 1 d . . . . .
H13 H 0.899(3) 0.758(3) 0.5155(13) 0.032(7) Uiso 1 1 d . . . . .
H15 H 0.629(3) 0.989(2) 0.1665(13) 0.033(7) Uiso 1 1 d . . . . .
H17 H 1.050(3) 1.261(3) 0.1899(14) 0.040(7) Uiso 1 1 d . . . . .
H19 H 0.986(2) 0.871(2) 0.2279(12) 0.020(6) Uiso 1 1 d . . . . .
H21 H 0.507(3) 0.621(2) 0.0572(12) 0.024(6) Uiso 1 1 d . . . . .
H23 H 0.107(3) 0.625(2) -0.0271(14) 0.035(7) Uiso 1 1 d . . . . .
H25 H 0.267(3) 0.800(2) 0.1878(14) 0.028(6) Uiso 1 1 d . . . . .
H27A H 0.383(4) 0.487(3) 0.4225(18) 0.062(10) Uiso 1 1 d . . . . .
H27B H 0.295(4) 0.344(4) 0.3795(18) 0.066(10) Uiso 1 1 d . . . . .
H27C H 0.230(3) 0.458(3) 0.3753(16) 0.051(9) Uiso 1 1 d . . . . .
H30 H 0.495(3) 0.227(2) 0.1523(13) 0.023(6) Uiso 1 1 d . . . . .
H31 H 0.449(3) 0.024(3) 0.0713(13) 0.035(7) Uiso 1 1 d . . . . .
H32 H 0.256(3) -0.051(3) -0.0266(14) 0.036(7) Uiso 1 1 d . . . . .
H33 H 0.105(3) 0.083(2) -0.0386(14) 0.031(7) Uiso 1 1 d . . . . .
H34 H 0.148(2) 0.283(2) 0.0423(12) 0.016(6) Uiso 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C7 N1 C1 120.34(19) . . ?
C7 N1 H1N 119.2(17) . . ?
C1 N1 H1N 120.0(17) . . ?
C28 N2 C4 120.82(18) . . ?
C28 N2 H2N 121.1(17) . . ?
C4 N2 H2N 116.5(17) . . ?
C5 O2 C6 114.64(19) . . ?
C26 O5 C27 116.1(2) . . ?
N1 C1 C5 111.30(18) . . ?
N1 C1 C2 109.91(17) . . ?
C5 C1 C2 117.08(17) . . ?
N1 C1 C4 111.59(16) . . ?
C5 C1 C4 118.00(17) . . ?
C2 C1 C4 86.75(15) . . ?
C14 C2 C3 119.66(18) . . ?
C14 C2 C1 120.75(18) . . ?
C3 C2 C1 88.34(15) . . ?
C14 C2 H2 109.6(12) . . ?
C3 C2 H2 110.6(12) . . ?
C1 C2 H2 105.9(12) . . ?
C20 C3 C2 120.76(19) . . ?
C20 C3 C4 119.17(18) . . ?
C2 C3 C4 88.18(15) . . ?
C20 C3 H3 108.6(13) . . ?
C2 C3 H3 109.1(14) . . ?
C4 C3 H3 109.4(13) . . ?
N2 C4 C26 112.83(17) . . ?
N2 C4 C3 112.17(17) . . ?
C26 C4 C3 116.27(17) . . ?
N2 C4 C1 111.59(17) . . ?
C26 C4 C1 114.72(17) . . ?
C3 C4 C1 86.76(15) . . ?
O1 C5 O2 123.5(2) . . ?
O1 C5 C1 125.4(2) . . ?
O2 C5 C1 110.99(19) . . ?
O2 C6 H6A 110.4(19) . . ?
O2 C6 H6B 106.6(17) . . ?
H6A C6 H6B 111(3) . . ?
O2 C6 H6C 105.7(17) . . ?
H6A C6 H6C 114(3) . . ?
H6B C6 H6C 108(2) . . ?
O3 C7 N1 120.4(2) . . ?
O3 C7 C8 122.6(2) . . ?
N1 C7 C8 117.02(19) . . ?
C13 C8 C9 120.1(2) . . ?
C13 C8 C7 117.8(2) . . ?
C9 C8 C7 122.1(2) . . ?
C8 C9 C10 119.4(2) . . ?
C8 C9 H9 120.0(16) . . ?
C10 C9 H9 120.6(16) . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.9(16) . . ?
C9 C10 H10 119.2(16) . . ?
C10 C11 C12 120.7(3) . . ?
C10 C11 H11 118.2(19) . . ?
C12 C11 H11 121(2) . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 H12 121.0(15) . . ?
C11 C12 H12 119.3(15) . . ?
C12 C13 C8 120.2(2) . . ?
C12 C13 H13 121.6(15) . . ?
C8 C13 H13 118.1(15) . . ?
C15 C14 C19 119.2(2) . . ?
C15 C14 C2 119.7(2) . . ?
C19 C14 C2 120.95(19) . . ?
C16 C15 C14 118.8(2) . . ?
C16 C15 H15 117.5(14) . . ?
C14 C15 H15 123.7(14) . . ?
F1 C16 C17 118.2(2) . . ?
F1 C16 C15 118.0(2) . . ?
C17 C16 C15 123.8(2) . . ?
C16 C17 C18 115.5(2) . . ?
C16 C17 H17 121.3(15) . . ?
C18 C17 H17 123.0(15) . . ?
F2 C18 C19 117.9(2) . . ?
F2 C18 C17 118.2(2) . . ?
C19 C18 C17 123.9(2) . . ?
C18 C19 C14 118.8(2) . . ?
C18 C19 H19 120.8(13) . . ?
C14 C19 H19 120.4(13) . . ?
C21 C20 C25 119.1(2) . . ?
C21 C20 C3 122.05(19) . . ?
C25 C20 C3 118.8(2) . . ?
C22 C21 C20 119.0(2) . . ?
C22 C21 H21 119.0(15) . . ?
C20 C21 H21 121.8(15) . . ?
F3 C22 C23 117.7(2) . . ?
F3 C22 C21 118.7(2) . . ?
C23 C22 C21 123.6(2) . . ?
C22 C23 C24 115.8(2) . . ?
C22 C23 H23 121.3(15) . . ?
C24 C23 H23 122.9(15) . . ?
F4 C24 C23 118.0(2) . . ?
F4 C24 C25 118.4(2) . . ?
C23 C24 C25 123.6(2) . . ?
C24 C25 C20 118.8(2) . . ?
C24 C25 H25 120.0(14) . . ?
C20 C25 H25 121.3(14) . . ?
O4 C26 O5 125.8(2) . . ?
O4 C26 C4 123.6(2) . . ?
O5 C26 C4 110.58(18) . . ?
O5 C27 H27A 107.6(19) . . ?
O5 C27 H27B 109(2) . . ?
H27A C27 H27B 109(3) . . ?
O5 C27 H27C 110.3(17) . . ?
H27A C27 H27C 111(3) . . ?
H27B C27 H27C 110(3) . . ?
O6 C28 N2 122.0(2) . . ?
O6 C28 C29 122.4(2) . . ?
N2 C28 C29 115.61(19) . . ?
C34 C29 C30 119.2(2) . . ?
C34 C29 C28 118.8(2) . . ?
C30 C29 C28 122.0(2) . . ?
C31 C30 C29 119.9(2) . . ?
C31 C30 H30 117.3(13) . . ?
C29 C30 H30 122.7(13) . . ?
C32 C31 C30 120.0(2) . . ?
C32 C31 H31 120.0(16) . . ?
C30 C31 H31 119.9(16) . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 118.9(15) . . ?
C31 C32 H32 120.9(15) . . ?
C34 C33 C32 119.8(2) . . ?
C34 C33 H33 118.8(15) . . ?
C32 C33 H33 121.4(15) . . ?
C33 C34 C29 120.9(2) . . ?
C33 C34 H34 121.3(15) . . ?
C29 C34 H34 117.8(15) . . ?
Cl1 C50A Cl3A 106.8(2) . . ?
Cl1 C50B Cl3B 100.9(7) . . ?
C50B Cl3B Cl3B 148.6(5) . 2_766 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C7 1.356(3) . ?
N1 C1 1.442(3) . ?
N1 H1N 0.81(2) . ?
N2 C28 1.354(3) . ?
N2 C4 1.440(3) . ?
N2 H2N 0.86(2) . ?
O1 C5 1.197(3) . ?
O2 C5 1.332(3) . ?
O2 C6 1.458(3) . ?
O3 C7 1.225(3) . ?
O4 C26 1.201(3) . ?
O5 C26 1.331(3) . ?
O5 C27 1.443(3) . ?
O6 C28 1.229(3) . ?
F1 C16 1.351(3) . ?
F2 C18 1.354(3) . ?
F3 C22 1.357(3) . ?
F4 C24 1.356(3) . ?
C1 C5 1.526(3) . ?
C1 C2 1.571(3) . ?
C1 C4 1.594(3) . ?
C2 C14 1.501(3) . ?
C2 C3 1.551(3) . ?
C2 H2 0.96(2) . ?
C3 C20 1.502(3) . ?
C3 C4 1.573(3) . ?
C3 H3 1.00(2) . ?
C4 C26 1.527(3) . ?
C6 H6A 0.96(3) . ?
C6 H6B 0.98(3) . ?
C6 H6C 0.89(3) . ?
C7 C8 1.490(3) . ?
C8 C13 1.386(3) . ?
C8 C9 1.387(3) . ?
C9 C10 1.391(4) . ?
C9 H9 0.94(3) . ?
C10 C11 1.378(4) . ?
C10 H10 0.92(2) . ?
C11 C12 1.380(4) . ?
C11 H11 0.88(3) . ?
C12 C13 1.376(4) . ?
C12 H12 0.99(3) . ?
C13 H13 0.93(2) . ?
C14 C15 1.386(3) . ?
C14 C19 1.394(3) . ?
C15 C16 1.381(3) . ?
C15 H15 0.95(2) . ?
C16 C17 1.371(3) . ?
C17 C18 1.373(3) . ?
C17 H17 0.98(3) . ?
C18 C19 1.373(3) . ?
C19 H19 0.96(2) . ?
C20 C21 1.390(3) . ?
C20 C25 1.395(3) . ?
C21 C22 1.376(3) . ?
C21 H21 0.92(2) . ?
C22 C23 1.371(3) . ?
C23 C24 1.375(3) . ?
C23 H23 0.94(3) . ?
C24 C25 1.377(3) . ?
C25 H25 0.96(2) . ?
C27 H27A 0.95(3) . ?
C27 H27B 0.91(3) . ?
C27 H27C 0.94(3) . ?
C28 C29 1.491(3) . ?
C29 C34 1.386(3) . ?
C29 C30 1.389(3) . ?
C30 C31 1.387(3) . ?
C30 H30 0.95(2) . ?
C31 C32 1.383(4) . ?
C31 H31 0.92(2) . ?
C32 C33 1.379(4) . ?
C32 H32 0.95(3) . ?
C33 C34 1.374(3) . ?
C33 H33 0.90(3) . ?
C34 H34 0.88(2) . ?
Cl1 C50B 1.647(14) . ?
Cl1 C50A 1.722(4) . ?
C50A Cl3A 1.751(4) . ?
C50B Cl3B 1.842(15) . ?
Cl3B Cl3B 2.257(8) 2_766 ?
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
C7 N1 C1 C5 -48.9(3) . . . . ?
C7 N1 C1 C2 179.77(18) . . . . ?
C7 N1 C1 C4 85.3(2) . . . . ?
N1 C1 C2 C14 35.7(3) . . . . ?
C5 C1 C2 C14 -92.5(2) . . . . ?
C4 C1 C2 C14 147.55(19) . . . . ?
N1 C1 C2 C3 -88.23(18) . . . . ?
C5 C1 C2 C3 143.51(19) . . . . ?
C4 C1 C2 C3 23.57(15) . . . . ?
C14 C2 C3 C20 88.0(3) . . . . ?
C1 C2 C3 C20 -147.14(19) . . . . ?
C14 C2 C3 C4 -148.8(2) . . . . ?
C1 C2 C3 C4 -23.87(15) . . . . ?
C28 N2 C4 C26 52.7(3) . . . . ?
C28 N2 C4 C3 -80.9(2) . . . . ?
C28 N2 C4 C1 -176.41(17) . . . . ?
C20 C3 C4 N2 36.1(3) . . . . ?
C2 C3 C4 N2 -88.49(19) . . . . ?
C20 C3 C4 C26 -95.8(2) . . . . ?
C2 C3 C4 C26 139.58(19) . . . . ?
C20 C3 C4 C1 148.16(19) . . . . ?
C2 C3 C4 C1 23.53(15) . . . . ?
N1 C1 C4 N2 -160.52(17) . . . . ?
C5 C1 C4 N2 -29.8(2) . . . . ?
C2 C1 C4 N2 89.34(18) . . . . ?
N1 C1 C4 C26 -30.6(2) . . . . ?
C5 C1 C4 C26 100.1(2) . . . . ?
C2 C1 C4 C26 -140.76(18) . . . . ?
N1 C1 C4 C3 86.89(18) . . . . ?
C5 C1 C4 C3 -142.34(19) . . . . ?
C2 C1 C4 C3 -23.25(15) . . . . ?
C6 O2 C5 O1 -2.5(3) . . . . ?
C6 O2 C5 C1 -179.5(2) . . . . ?
N1 C1 C5 O1 139.8(2) . . . . ?
C2 C1 C5 O1 -92.6(3) . . . . ?
C4 C1 C5 O1 9.0(3) . . . . ?
N1 C1 C5 O2 -43.2(2) . . . . ?
C2 C1 C5 O2 84.4(2) . . . . ?
C4 C1 C5 O2 -174.08(17) . . . . ?
C1 N1 C7 O3 1.2(3) . . . . ?
C1 N1 C7 C8 -179.72(18) . . . . ?
O3 C7 C8 C13 36.1(3) . . . . ?
N1 C7 C8 C13 -142.9(2) . . . . ?
O3 C7 C8 C9 -142.2(2) . . . . ?
N1 C7 C8 C9 38.8(3) . . . . ?
C13 C8 C9 C10 -0.7(4) . . . . ?
C7 C8 C9 C10 177.6(2) . . . . ?
C8 C9 C10 C11 1.1(4) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C10 C11 C12 C13 -0.7(4) . . . . ?
C11 C12 C13 C8 1.2(4) . . . . ?
C9 C8 C13 C12 -0.5(4) . . . . ?
C7 C8 C13 C12 -178.8(2) . . . . ?
C3 C2 C14 C15 -24.4(3) . . . . ?
C1 C2 C14 C15 -131.8(2) . . . . ?
C3 C2 C14 C19 159.8(2) . . . . ?
C1 C2 C14 C19 52.4(3) . . . . ?
C19 C14 C15 C16 1.6(3) . . . . ?
C2 C14 C15 C16 -174.2(2) . . . . ?
C14 C15 C16 F1 176.3(2) . . . . ?
C14 C15 C16 C17 -2.2(4) . . . . ?
F1 C16 C17 C18 -177.3(2) . . . . ?
C15 C16 C17 C18 1.1(4) . . . . ?
C16 C17 C18 F2 -179.2(2) . . . . ?
C16 C17 C18 C19 0.5(4) . . . . ?
F2 C18 C19 C14 178.8(2) . . . . ?
C17 C18 C19 C14 -1.0(4) . . . . ?
C15 C14 C19 C18 -0.2(3) . . . . ?
C2 C14 C19 C18 175.7(2) . . . . ?
C2 C3 C20 C21 32.4(3) . . . . ?
C4 C3 C20 C21 -74.5(3) . . . . ?
C2 C3 C20 C25 -151.4(2) . . . . ?
C4 C3 C20 C25 101.7(2) . . . . ?
C25 C20 C21 C22 -3.3(3) . . . . ?
C3 C20 C21 C22 172.9(2) . . . . ?
C20 C21 C22 F3 -177.15(19) . . . . ?
C20 C21 C22 C23 2.1(4) . . . . ?
F3 C22 C23 C24 179.1(2) . . . . ?
C21 C22 C23 C24 -0.1(4) . . . . ?
C22 C23 C24 F4 -179.6(2) . . . . ?
C22 C23 C24 C25 -0.5(4) . . . . ?
F4 C24 C25 C20 178.3(2) . . . . ?
C23 C24 C25 C20 -0.9(4) . . . . ?
C21 C20 C25 C24 2.8(3) . . . . ?
C3 C20 C25 C24 -173.5(2) . . . . ?
C27 O5 C26 O4 0.7(3) . . . . ?
C27 O5 C26 C4 177.8(2) . . . . ?
N2 C4 C26 O4 -152.4(2) . . . . ?
C3 C4 C26 O4 -20.8(3) . . . . ?
C1 C4 C26 O4 78.3(3) . . . . ?
N2 C4 C26 O5 30.4(2) . . . . ?
C3 C4 C26 O5 162.01(17) . . . . ?
C1 C4 C26 O5 -98.9(2) . . . . ?
C4 N2 C28 O6 4.5(3) . . . . ?
C4 N2 C28 C29 -176.92(18) . . . . ?
O6 C28 C29 C34 30.5(3) . . . . ?
N2 C28 C29 C34 -148.2(2) . . . . ?
O6 C28 C29 C30 -148.6(2) . . . . ?
N2 C28 C29 C30 32.8(3) . . . . ?
C34 C29 C30 C31 -1.8(3) . . . . ?
C28 C29 C30 C31 177.2(2) . . . . ?
C29 C30 C31 C32 1.5(4) . . . . ?
C30 C31 C32 C33 0.0(4) . . . . ?
C31 C32 C33 C34 -1.2(4) . . . . ?
C32 C33 C34 C29 0.9(4) . . . . ?
C30 C29 C34 C33 0.6(3) . . . . ?
C28 C29 C34 C33 -178.4(2) . . . . ?
Cl1 C50B Cl3B Cl3B -146.7(6) . . . 2_766 ?
