#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:21:22 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229960.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_7229960
loop_
_publ_author_name
'Aghabali, Amineh'
'Jun, Sharon'
'Olmstead, Marilyn M.'
'Balch, Alan L.'
_publ_section_title
;
 The directional character of the piperazine double addition product,
 e{N(CH2CH2)2N}2C60, as a building block for forming crystalline fullerene
 polymers
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              924
_journal_paper_doi               10.1039/C7CE02117H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'2(C34 H8 N2), 2(I2), 2(C3 H3), 0.5(C S2), 0.5(C S2)'
_chemical_formula_sum            'C72 H19 I4 N4 S2'
_chemical_formula_weight         1511.63
_chemical_name_systematic        'e{N(CH2CH2)2N}2C60?3I2?CS2?C6H6 '
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-15 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.744(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4566(7)
_cell_length_b                   10.6707(5)
_cell_length_c                   16.0942(7)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.948
_cell_measurement_theta_min      2.585
_cell_volume                     2390.99(19)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex 2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 with Photon 100 CMOS detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61791
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         43.971
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'Advanced Light Source, beamline 11.3.1'
_exptl_absorpt_coefficient_mu    3.428
_exptl_absorpt_correction_T_max  0.4458
_exptl_absorpt_correction_T_min  0.3944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_description       block
_exptl_crystal_F_000             1446
_exptl_crystal_recrystallization_method
'diffusion of a CS2 solution of the fullerene with a solution of I2 in benzene'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.182
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         14780
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0351P)²+6.1659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12163
_reflns_number_total             14780
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce02117h1.cif
_cod_data_source_block           aa96
_cod_depositor_comments
'Adding full bibliography for 7229960--7229961.cif.'
_cod_database_code               7229960
_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   0.279
_shelx_estimated_absorpt_t_max   0.821
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
I1 I 0.68498(2) 1.12178(2) 0.90842(2) 0.01468(3) Uani 1 1 d . . . . .
I2 I 0.41672(2) 0.7500 0.54063(2) 0.01208(3) Uani 1 2 d S T P . .
I3 I 0.30903(2) 0.7500 0.64092(2) 0.02315(5) Uani 1 2 d S T P . .
N1 N 0.69864(12) 0.86871(16) 0.90060(11) 0.0123(3) Uani 1 1 d . . . . .
N2 N 0.61571(17) 0.7500 0.35415(16) 0.0150(4) Uani 1 2 d S T P . .
N3 N 0.52138(15) 0.7500 0.45150(15) 0.0106(3) Uani 1 2 d S T P . .
C1 C 0.75217(13) 0.82567(18) 0.84698(12) 0.0106(3) Uani 1 1 d . . . . .
C2 C 0.85281(13) 0.88473(18) 0.88555(12) 0.0117(3) Uani 1 1 d . . . . .
C3 C 0.93671(13) 0.81953(19) 0.93149(12) 0.0128(3) Uani 1 1 d . . . . .
C4 C 1.02448(13) 0.8602(2) 0.92759(13) 0.0143(3) Uani 1 1 d . . . . .
C5 C 1.07775(19) 0.7500 0.92501(18) 0.0143(4) Uani 1 2 d S T P . .
C6 C 1.12984(19) 0.7500 0.87242(19) 0.0152(5) Uani 1 2 d S T P . .
C7 C 1.12952(13) 0.8601(2) 0.81950(14) 0.0158(3) Uani 1 1 d . . . . .
C8 C 1.12856(13) 0.8181(2) 0.73341(14) 0.0156(3) Uani 1 1 d . . . . .
C9 C 1.07464(14) 0.8833(2) 0.65212(14) 0.0153(3) Uani 1 1 d . . . . .
C10 C 1.01831(13) 0.8150(2) 0.56784(14) 0.0150(3) Uani 1 1 d . . . . .
C11 C 0.92920(13) 0.8835(2) 0.51811(13) 0.0147(3) Uani 1 1 d . . . . .
C12 C 0.84306(13) 0.8179(2) 0.47090(13) 0.0135(3) Uani 1 1 d . . . . .
C13 C 0.75543(13) 0.86027(19) 0.47219(12) 0.0125(3) Uani 1 1 d . . . . .
C14 C 0.68543(18) 0.7500 0.45275(17) 0.0116(4) Uani 1 2 d S T P . .
C15 C 0.62744(17) 0.7500 0.51581(17) 0.0096(4) Uani 1 2 d S T P . .
C16 C 0.65201(12) 0.85981(17) 0.58345(12) 0.0098(3) Uani 1 1 d . . . . .
C17 C 0.65661(12) 0.81862(17) 0.66996(12) 0.0090(2) Uani 1 1 d . . . . .
C18 C 0.70778(12) 0.88422(17) 0.75048(12) 0.0099(3) Uani 1 1 d . . . . .
C19 C 0.76265(13) 0.99035(17) 0.74755(13) 0.0114(3) Uani 1 1 d . . . . .
C20 C 0.85233(13) 0.99181(18) 0.83090(13) 0.0120(3) Uani 1 1 d . . . . .
C21 C 0.93610(14) 1.03384(19) 0.82727(14) 0.0138(3) Uani 1 1 d . . . . .
C22 C 1.02452(14) 0.9664(2) 0.87711(13) 0.0140(3) Uani 1 1 d . . . . .
C23 C 1.07805(14) 0.9659(2) 0.82178(14) 0.0154(3) Uani 1 1 d . . . . .
C24 C 1.02187(14) 1.0340(2) 0.73706(15) 0.0157(3) Uani 1 1 d . . . . .
C25 C 1.02036(14) 0.9936(2) 0.65388(14) 0.0157(3) Uani 1 1 d . . . . .
C26 C 0.93042(14) 0.9931(2) 0.57057(14) 0.0149(3) Uani 1 1 d . . . . .
C27 C 0.84580(14) 1.03200(19) 0.57412(14) 0.0139(3) Uani 1 1 d . . . . .
C28 C 0.75732(13) 0.96345(19) 0.52352(13) 0.0123(3) Uani 1 1 d . . . . .
C29 C 0.70423(13) 0.96276(18) 0.58099(13) 0.0111(3) Uani 1 1 d . . . . .
C30 C 0.76031(13) 1.03067(17) 0.66396(13) 0.0120(3) Uani 1 1 d . . . . .
C31 C 0.84793(14) 1.07374(18) 0.66044(14) 0.0134(3) Uani 1 1 d . . . . .
C32 C 0.93396(14) 1.07567(19) 0.74042(14) 0.0147(3) Uani 1 1 d . . . . .
C33 C 0.74775(16) 0.8227(2) 0.99639(14) 0.0168(3) Uani 1 1 d . . . . .
H33A H 0.7143 0.8541 1.0326 0.020 Uiso 1 1 calc R U . . .
H33B H 0.8146 0.8541 1.0254 0.020 Uiso 1 1 calc R U . . .
C34 C 0.59921(14) 0.8226(2) 0.85753(14) 0.0153(3) Uani 1 1 d . . . . .
H34A H 0.5662 0.8539 0.7934 0.018 Uiso 1 1 calc R U . . .
H34B H 0.5641 0.8539 0.8922 0.018 Uiso 1 1 calc R U . . .
C35 C 0.49656(13) 0.6368(2) 0.39208(13) 0.0147(3) Uani 1 1 d . . . . .
H35A H 0.4269 0.6361 0.3509 0.018 Uiso 1 1 calc R U . . .
H35B H 0.5122 0.5605 0.4309 0.018 Uiso 1 1 calc R U . . .
C36 C 0.55446(14) 0.6376(2) 0.33354(14) 0.0174(4) Uani 1 1 d . . . . .
H36A H 0.5950 0.5616 0.3473 0.021 Uiso 1 1 calc R U . . .
H36B H 0.5095 0.6365 0.2671 0.021 Uiso 1 1 calc R U . . .
C37 C 0.6125(7) 0.3777(7) 0.1102(6) 0.0192(14) Uiso 0.25 1 d D . P A 1
S1 S 0.61852(13) 0.2500 0.09659(13) 0.0340(5) Uani 0.5 2 d DS T P A 1
S2 S 0.6071(4) 0.5164(4) 0.1282(4) 0.0544(12) Uani 0.25 1 d D . P A 1
C38 C 0.6906(7) 0.6767(11) 0.1864(7) 0.0262(18) Uiso 0.25 1 d D . P B 2
S3 S 0.7915(2) 0.7500 0.23988(15) 0.0392(6) Uani 0.5 2 d DS T P B 2
S4 S 0.5851(3) 0.6244(6) 0.1243(3) 0.0580(14) Uani 0.25 1 d D . P B 2
C39 C 0.5807(6) 0.7551(16) 0.1233(7) 0.061(3) Uiso 0.25 1 d G . P C -3
H39 H 0.5149 0.7657 0.0819 0.073 Uiso 0.25 1 d G U P C -3
C40 C 0.6186(7) 0.6353(13) 0.1478(8) 0.042(4) Uiso 0.25 1 d G . P C -3
H40 H 0.5787 0.5641 0.1232 0.050 Uiso 0.25 1 d G U P C -3
C41 C 0.7149(8) 0.6197(8) 0.2084(8) 0.033(2) Uiso 0.25 1 d G . P C -3
H41 H 0.7408 0.5378 0.2251 0.040 Uiso 0.25 1 d G U P C -3
C42 C 0.7732(5) 0.7239(8) 0.2444(6) 0.028(3) Uiso 0.25 1 d G . P C -3
H42 H 0.8390 0.7132 0.2858 0.034 Uiso 0.25 1 d G U P C -3
C43 C 0.7353(8) 0.8437(7) 0.2199(9) 0.035(2) Uiso 0.25 1 d G . P C -3
H43 H 0.7752 0.9149 0.2445 0.042 Uiso 0.25 1 d G U P C -3
C44 C 0.6391(9) 0.8593(12) 0.1593(9) 0.094(10) Uiso 0.25 1 d G . P C -3
H44 H 0.6132 0.9412 0.1426 0.112 Uiso 0.25 1 d G U P C -3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
I I -0.3071 2.1212 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1430 0.1480 '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
C34 N1 C33 109.83(16) . .
C34 N1 C1 110.51(15) . .
C33 N1 C1 109.66(15) . .
C36 N2 C36 108.9(2) . 4_575
C36 N2 C14 109.79(14) . .
C36 N2 C14 109.79(14) 4_575 .
C35 N3 C35 109.0(2) . 4_575
C35 N3 C15 109.95(13) . .
C35 N3 C15 109.95(13) 4_575 .
N1 C1 C18 109.97(14) . .
N1 C1 C2 110.83(14) . .
C18 C1 C2 99.86(15) . .
N1 C1 C1 107.78(10) . 4_575
C18 C1 C1 114.06(10) . 4_575
C2 C1 C1 114.20(10) . 4_575
C3 C2 C20 119.00(17) . .
C3 C2 C1 124.33(18) . .
C20 C2 C1 110.05(15) . .
C2 C3 C4 120.53(18) . .
C2 C3 C3 120.50(12) . 4_575
C4 C3 C3 107.39(12) . 4_575
C22 C4 C5 119.98(19) . .
C22 C4 C3 120.33(18) . .
C5 C4 C3 108.22(19) . .
C6 C5 C4 120.12(15) . .
C6 C5 C4 120.12(15) . 4_575
C4 C5 C4 108.8(2) . 4_575
C5 C6 C7 119.96(15) . .
C5 C6 C7 119.96(15) . 4_575
C7 C6 C7 108.3(3) . 4_575
C23 C7 C6 119.9(2) . .
C23 C7 C8 120.50(19) . .
C6 C7 C8 107.9(2) . .
C9 C8 C7 119.8(2) . .
C9 C8 C8 119.92(13) . 4_575
C7 C8 C8 107.99(13) . 4_575
C8 C9 C10 119.9(2) . .
C8 C9 C25 120.05(19) . .
C10 C9 C25 107.95(17) . .
C10 C10 C9 120.17(12) 4_575 .
C10 C10 C11 120.19(12) 4_575 .
C9 C10 C11 107.61(19) . .
C12 C11 C26 119.48(18) . .
C12 C11 C10 119.8(2) . .
C26 C11 C10 108.55(17) . .
C11 C12 C13 121.00(19) . .
C11 C12 C12 119.99(12) . 4_575
C13 C12 C12 108.34(12) . 4_575
C28 C13 C12 119.24(17) . .
C28 C13 C14 124.58(17) . .
C12 C13 C14 109.94(18) . .
N2 C14 C13 109.79(15) . .
N2 C14 C13 109.80(15) . 4_575
C13 C14 C13 100.0(2) . 4_575
N2 C14 C15 109.2(2) . .
C13 C14 C15 113.88(14) . .
C13 C14 C15 113.88(14) 4_575 .
N3 C15 C16 110.32(14) . .
N3 C15 C16 110.32(14) . 4_575
C16 C15 C16 99.90(19) . 4_575
N3 C15 C14 107.56(19) . .
C16 C15 C14 114.31(13) . .
C16 C15 C14 114.31(13) 4_575 .
C29 C16 C17 119.45(16) . .
C29 C16 C15 123.99(17) . .
C17 C16 C15 110.41(15) . .
C18 C17 C16 121.57(16) . .
C18 C17 C17 120.48(10) . 4_575
C16 C17 C17 107.87(10) . 4_575
C17 C18 C19 118.53(16) . .
C17 C18 C1 124.52(16) . .
C19 C18 C1 110.24(15) . .
C30 C19 C18 120.56(17) . .
C30 C19 C20 120.09(17) . .
C18 C19 C20 108.70(16) . .
C21 C20 C2 121.47(18) . .
C21 C20 C19 119.74(18) . .
C2 C20 C19 107.79(16) . .
C20 C21 C22 119.29(18) . .
C20 C21 C32 120.32(17) . .
C22 C21 C32 107.97(17) . .
C4 C22 C21 119.32(18) . .
C4 C22 C23 119.83(19) . .
C21 C22 C23 108.38(18) . .
C7 C23 C24 119.79(19) . .
C7 C23 C22 120.2(2) . .
C24 C23 C22 107.77(18) . .
C25 C24 C32 120.23(18) . .
C25 C24 C23 119.9(2) . .
C32 C24 C23 107.78(18) . .
C24 C25 C26 119.77(19) . .
C24 C25 C9 119.95(19) . .
C26 C25 C9 107.95(19) . .
C27 C26 C11 119.46(18) . .
C27 C26 C25 119.92(19) . .
C11 C26 C25 107.95(18) . .
C26 C27 C31 119.99(18) . .
C26 C27 C28 119.92(19) . .
C31 C27 C28 108.52(17) . .
C13 C28 C27 120.84(18) . .
C13 C28 C29 120.07(17) . .
C27 C28 C29 107.18(16) . .
C16 C29 C30 120.17(17) . .
C16 C29 C28 120.95(17) . .
C30 C29 C28 107.75(16) . .
C19 C30 C29 119.56(17) . .
C19 C30 C31 119.97(17) . .
C29 C30 C31 108.66(16) . .
C32 C31 C27 120.47(19) . .
C32 C31 C30 120.01(18) . .
C27 C31 C30 107.89(16) . .
C31 C32 C24 119.62(19) . .
C31 C32 C21 119.87(18) . .
C24 C32 C21 108.11(18) . .
N1 C33 C33 109.44(11) . 4_575
N1 C33 H33A 109.8 . .
C33 C33 H33A 109.8 4_575 .
N1 C33 H33B 109.8 . .
C33 C33 H33B 109.8 4_575 .
H33A C33 H33B 108.2 . .
N1 C34 C34 109.57(11) . 4_575
N1 C34 H34A 109.8 . .
C34 C34 H34A 109.8 4_575 .
N1 C34 H34B 109.8 . .
C34 C34 H34B 109.8 4_575 .
H34A C34 H34B 108.2 . .
N3 C35 C36 109.27(17) . .
N3 C35 H35A 109.8 . .
C36 C35 H35A 109.8 . .
N3 C35 H35B 109.8 . .
C36 C35 H35B 109.8 . .
H35A C35 H35B 108.3 . .
N2 C36 C35 110.51(18) . .
N2 C36 H36A 109.5 . .
C35 C36 H36A 109.5 . .
N2 C36 H36B 109.5 . .
C35 C36 H36B 109.5 . .
H36A C36 H36B 108.1 . .
S1 C37 S2 178.3(8) . .
C37 S1 C37 157.3(8) 4_565 .
C38 C38 S4 110.4(5) 4_575 .
C38 C38 S3 61.1(4) 4_575 .
S4 C38 S3 170.9(9) . .
C38 S3 C38 57.8(8) 4_575 .
C40 C39 C44 120.0 . .
C40 C39 H39 120.0 . .
C44 C39 H39 120.0 . .
C41 C40 C39 120.0 . .
C41 C40 H40 120.0 . .
C39 C40 H40 120.0 . .
C40 C41 C42 120.0 . .
C40 C41 H41 120.0 . .
C42 C41 H41 120.0 . .
C43 C42 C41 120.0 . .
C43 C42 H42 120.0 . .
C41 C42 H42 120.0 . .
C44 C43 C42 120.0 . .
C44 C43 H43 120.0 . .
C42 C43 H43 120.0 . .
C43 C44 C39 120.0 . .
C43 C44 H44 120.0 . .
C39 C44 H44 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 I1 2.7363(3) 4_585
I2 I3 2.7766(3) .
N1 C34 1.469(3) .
N1 C33 1.476(3) .
N1 C1 1.504(2) .
N2 C36 1.474(3) .
N2 C36 1.474(3) 4_575
N2 C14 1.481(3) .
N3 C35 1.484(2) .
N3 C35 1.484(2) 4_575
N3 C15 1.511(3) .
C1 C18 1.532(3) .
C1 C2 1.537(3) .
C1 C1 1.615(4) 4_575
C2 C3 1.371(3) .
C2 C20 1.440(3) .
C3 C4 1.452(3) .
C3 C3 1.484(4) 4_575
C4 C22 1.395(3) .
C4 C5 1.446(3) .
C5 C6 1.399(4) .
C5 C4 1.446(3) 4_575
C6 C7 1.450(3) .
C6 C7 1.450(3) 4_575
C7 C23 1.390(3) .
C7 C8 1.450(3) .
C8 C9 1.394(3) .
C8 C8 1.454(5) 4_575
C9 C10 1.450(3) .
C9 C25 1.453(3) .
C10 C10 1.387(5) 4_575
C10 C11 1.454(3) .
C11 C12 1.400(3) .
C11 C26 1.438(3) .
C12 C13 1.437(3) .
C12 C12 1.449(4) 4_575
C13 C28 1.369(3) .
C13 C14 1.536(3) .
C14 C13 1.536(3) 4_575
C14 C15 1.620(4) .
C15 C16 1.531(2) .
C15 C16 1.531(2) 4_575
C16 C29 1.374(3) .
C16 C17 1.432(2) .
C17 C18 1.380(2) .
C17 C17 1.465(4) 4_575
C18 C19 1.428(3) .
C19 C30 1.398(3) .
C19 C20 1.451(3) .
C20 C21 1.395(3) .
C21 C22 1.441(3) .
C21 C32 1.454(3) .
C22 C23 1.455(3) .
C23 C24 1.454(3) .
C24 C25 1.397(3) .
C24 C32 1.453(3) .
C25 C26 1.453(3) .
C26 C27 1.397(3) .
C27 C31 1.446(3) .
C27 C28 1.449(3) .
C28 C29 1.479(3) .
C29 C30 1.433(3) .
C30 C31 1.454(3) .
C31 C32 1.392(3) .
C33 C33 1.551(5) 4_575
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C34 C34 1.549(4) 4_575
C34 H34A 0.9900 .
C34 H34B 0.9900 .
C35 C36 1.556(3) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C36 H36A 0.9900 .
C36 H36B 0.9900 .
C37 S1 1.390(8) .
C37 S2 1.518(9) .
S1 C37 1.390(8) 4_565
C38 C38 1.56(2) 4_575
C38 S4 1.598(10) .
C38 S3 1.618(9) .
S3 C38 1.618(9) 4_575
C39 C40 1.3900 .
C39 C44 1.3900 .
C39 H39 0.9500 .
C40 C41 1.3900 .
C40 H40 0.9500 .
C41 C42 1.3900 .
C41 H41 0.9500 .
C42 C43 1.3900 .
C42 H42 0.9500 .
C43 C44 1.3900 .
C43 H43 0.9500 .
C44 H44 0.9500 .
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_4
C34 N1 C1 C18 64.6(2) . .
C33 N1 C1 C18 -174.16(16) . .
C34 N1 C1 C2 174.08(16) . .
C33 N1 C1 C2 -64.7(2) . .
C34 N1 C1 C1 -60.28(15) . 4_575
C33 N1 C1 C1 60.94(15) . 4_575
N1 C1 C2 C3 110.7(2) . .
C18 C1 C2 C3 -133.42(19) . .
C1 C1 C2 C3 -11.3(2) 4_575 .
N1 C1 C2 C20 -98.40(18) . .
C18 C1 C2 C20 17.51(19) . .
C1 C1 C2 C20 139.65(12) 4_575 .
C20 C2 C3 C4 2.0(3) . .
C1 C2 C3 C4 150.55(18) . .
C20 C2 C3 C3 -136.59(13) . 4_575
C1 C2 C3 C3 12.0(2) . 4_575
C2 C3 C4 C22 0.1(3) . .
C3 C3 C4 C22 143.46(16) 4_575 .
C2 C3 C4 C5 -143.2(2) . .
C3 C3 C4 C5 0.12(17) 4_575 .
C22 C4 C5 C6 0.4(3) . .
C3 C4 C5 C6 143.9(2) . .
C22 C4 C5 C4 -143.69(16) . 4_575
C3 C4 C5 C4 -0.2(3) . 4_575
C4 C5 C6 C7 -0.7(3) . .
C4 C5 C6 C7 139.3(2) 4_575 .
C4 C5 C6 C7 -139.3(2) . 4_575
C4 C5 C6 C7 0.7(3) 4_575 4_575
C5 C6 C7 C23 0.5(3) . .
C7 C6 C7 C23 143.41(17) 4_575 .
C5 C6 C7 C8 -142.6(2) . .
C7 C6 C7 C8 0.3(3) 4_575 .
C23 C7 C8 C9 -0.8(3) . .
C6 C7 C8 C9 142.0(2) . .
C23 C7 C8 C8 -143.04(16) . 4_575
C6 C7 C8 C8 -0.16(17) . 4_575
C7 C8 C9 C10 -137.4(2) . .
C8 C8 C9 C10 0.3(2) 4_575 .
C7 C8 C9 C25 0.6(3) . .
C8 C8 C9 C25 138.33(15) 4_575 .
C8 C9 C10 C10 -0.3(2) . 4_575
C25 C9 C10 C10 -142.83(12) . 4_575
C8 C9 C10 C11 142.32(19) . .
C25 C9 C10 C11 -0.2(2) . .
C10 C10 C11 C12 0.7(2) 4_575 .
C9 C10 C11 C12 -141.96(19) . .
C10 C10 C11 C26 142.89(12) 4_575 .
C9 C10 C11 C26 0.3(2) . .
C26 C11 C12 C13 1.6(3) . .
C10 C11 C12 C13 139.77(19) . .
C26 C11 C12 C12 -138.82(15) . 4_575
C10 C11 C12 C12 -0.7(2) . 4_575
C11 C12 C13 C28 -2.7(3) . .
C12 C12 C13 C28 141.75(15) 4_575 .
C11 C12 C13 C14 -156.23(19) . .
C12 C12 C13 C14 -11.78(16) 4_575 .
C36 N2 C14 C13 174.65(17) . .
C36 N2 C14 C13 -65.6(2) 4_575 .
C36 N2 C14 C13 65.6(2) . 4_575
C36 N2 C14 C13 -174.65(17) 4_575 4_575
C36 N2 C14 C15 -59.87(15) . .
C36 N2 C14 C15 59.87(15) 4_575 .
C28 C13 C14 N2 110.3(2) . .
C12 C13 C14 N2 -97.86(19) . .
C28 C13 C14 C13 -134.26(16) . 4_575
C12 C13 C14 C13 17.6(2) . 4_575
C28 C13 C14 C15 -12.4(3) . .
C12 C13 C14 C15 139.41(16) . .
C35 N3 C15 C16 -174.73(16) . .
C35 N3 C15 C16 65.3(2) 4_575 .
C35 N3 C15 C16 -65.3(2) . 4_575
C35 N3 C15 C16 174.73(16) 4_575 4_575
C35 N3 C15 C14 59.99(14) . .
C35 N3 C15 C14 -59.99(14) 4_575 .
N2 C14 C15 N3 0.000(1) . .
C13 C14 C15 N3 123.08(14) . .
C13 C14 C15 N3 -123.08(14) 4_575 .
N2 C14 C15 C16 -122.86(14) . .
C13 C14 C15 C16 0.2(2) . .
C13 C14 C15 C16 114.05(16) 4_575 .
N2 C14 C15 C16 122.87(14) . 4_575
C13 C14 C15 C16 -114.05(16) . 4_575
C13 C14 C15 C16 -0.2(2) 4_575 4_575
N3 C15 C16 C29 -109.7(2) . .
C16 C15 C16 C29 134.16(15) 4_575 .
C14 C15 C16 C29 11.7(3) . .
N3 C15 C16 C17 98.22(17) . .
C16 C15 C16 C17 -17.9(2) 4_575 .
C14 C15 C16 C17 -140.43(16) . .
C29 C16 C17 C18 3.9(3) . .
C15 C16 C17 C18 157.45(17) . .
C29 C16 C17 C17 -141.52(14) . 4_575
C15 C16 C17 C17 12.00(16) . 4_575
C16 C17 C18 C19 -4.5(3) . .
C17 C17 C18 C19 136.68(13) 4_575 .
C16 C17 C18 C1 -152.96(17) . .
C17 C17 C18 C1 -11.7(2) 4_575 .
N1 C1 C18 C17 -110.13(19) . .
C2 C1 C18 C17 133.31(18) . .
C1 C1 C18 C17 11.1(2) 4_575 .
N1 C1 C18 C19 99.23(17) . .
C2 C1 C18 C19 -17.34(18) . .
C1 C1 C18 C19 -139.57(11) 4_575 .
C17 C18 C19 C30 3.4(3) . .
C1 C18 C19 C30 156.02(17) . .
C17 C18 C19 C20 -141.15(17) . .
C1 C18 C19 C20 11.5(2) . .
C3 C2 C20 C21 -3.1(3) . .
C1 C2 C20 C21 -155.75(17) . .
C3 C2 C20 C19 140.75(18) . .
C1 C2 C20 C19 -11.9(2) . .
C30 C19 C20 C21 0.1(3) . .
C18 C19 C20 C21 144.87(18) . .
C30 C19 C20 C2 -144.42(18) . .
C18 C19 C20 C2 0.3(2) . .
C2 C20 C21 C22 1.9(3) . .
C19 C20 C21 C22 -137.76(19) . .
C2 C20 C21 C32 139.4(2) . .
C19 C20 C21 C32 -0.2(3) . .
C5 C4 C22 C21 137.8(2) . .
C3 C4 C22 C21 -1.3(3) . .
C5 C4 C22 C23 0.1(3) . .
C3 C4 C22 C23 -138.94(19) . .
C20 C21 C22 C4 0.3(3) . .
C32 C21 C22 C4 -141.92(19) . .
C20 C21 C22 C23 142.28(19) . .
C32 C21 C22 C23 0.1(2) . .
C6 C7 C23 C24 -137.8(2) . .
C8 C7 C23 C24 0.8(3) . .
C6 C7 C23 C22 0.0(3) . .
C8 C7 C23 C22 138.5(2) . .
C4 C22 C23 C7 -0.4(3) . .
C21 C22 C23 C7 -142.10(19) . .
C4 C22 C23 C24 141.88(19) . .
C21 C22 C23 C24 0.1(2) . .
C7 C23 C24 C25 -0.5(3) . .
C22 C23 C24 C25 -142.88(19) . .
C7 C23 C24 C32 142.17(19) . .
C22 C23 C24 C32 -0.3(2) . .
C32 C24 C25 C26 -0.1(3) . .
C23 C24 C25 C26 137.9(2) . .
C32 C24 C25 C9 -137.8(2) . .
C23 C24 C25 C9 0.2(3) . .
C8 C9 C25 C24 -0.3(3) . .
C10 C9 C25 C24 142.16(19) . .
C8 C9 C25 C26 -142.41(19) . .
C10 C9 C25 C26 0.1(2) . .
C12 C11 C26 C27 0.4(3) . .
C10 C11 C26 C27 -141.98(19) . .
C12 C11 C26 C25 142.14(19) . .
C10 C11 C26 C25 -0.2(2) . .
C24 C25 C26 C27 -0.5(3) . .
C9 C25 C26 C27 141.6(2) . .
C24 C25 C26 C11 -142.1(2) . .
C9 C25 C26 C11 0.1(2) . .
C11 C26 C27 C31 137.7(2) . .
C25 C26 C27 C31 0.6(3) . .
C11 C26 C27 C28 -1.3(3) . .
C25 C26 C27 C28 -138.5(2) . .
C12 C13 C28 C27 1.8(3) . .
C14 C13 C28 C27 151.18(19) . .
C12 C13 C28 C29 -136.22(18) . .
C14 C13 C28 C29 13.2(3) . .
C26 C27 C28 C13 0.2(3) . .
C31 C27 C28 C13 -143.03(18) . .
C26 C27 C28 C29 142.89(18) . .
C31 C27 C28 C29 -0.3(2) . .
C17 C16 C29 C30 -2.0(3) . .
C15 C16 C29 C30 -151.77(18) . .
C17 C16 C29 C28 137.41(18) . .
C15 C16 C29 C28 -12.3(3) . .
C13 C28 C29 C16 -0.4(3) . .
C27 C28 C29 C16 -143.44(18) . .
C13 C28 C29 C30 143.42(18) . .
C27 C28 C29 C30 0.4(2) . .
C18 C19 C30 C29 -1.6(3) . .
C20 C19 C30 C29 138.96(19) . .
C18 C19 C30 C31 -140.36(19) . .
C20 C19 C30 C31 0.2(3) . .
C16 C29 C30 C19 1.0(3) . .
C28 C29 C30 C19 -143.20(18) . .
C16 C29 C30 C31 143.87(18) . .
C28 C29 C30 C31 -0.3(2) . .
C26 C27 C31 C32 0.1(3) . .
C28 C27 C31 C32 143.26(19) . .
C26 C27 C31 C30 -143.04(19) . .
C28 C27 C31 C30 0.2(2) . .
C19 C30 C31 C32 -0.5(3) . .
C29 C30 C31 C32 -143.21(19) . .
C19 C30 C31 C27 142.82(18) . .
C29 C30 C31 C27 0.1(2) . .
C27 C31 C32 C24 -0.7(3) . .
C30 C31 C32 C24 138.0(2) . .
C27 C31 C32 C21 -138.3(2) . .
C30 C31 C32 C21 0.4(3) . .
C25 C24 C32 C31 0.7(3) . .
C23 C24 C32 C31 -141.76(19) . .
C25 C24 C32 C21 142.8(2) . .
C23 C24 C32 C21 0.3(2) . .
C20 C21 C32 C31 0.0(3) . .
C22 C21 C32 C31 141.73(19) . .
C20 C21 C32 C24 -141.98(19) . .
C22 C21 C32 C24 -0.2(2) . .
C34 N1 C33 C33 59.67(15) . 4_575
C1 N1 C33 C33 -61.96(14) . 4_575
C33 N1 C34 C34 -59.75(15) . 4_575
C1 N1 C34 C34 61.37(14) . 4_575
C35 N3 C35 C36 60.0(2) 4_575 .
C15 N3 C35 C36 -60.6(2) . .
C36 N2 C36 C35 -59.1(3) 4_575 .
C14 N2 C36 C35 61.2(2) . .
N3 C35 C36 N2 -0.3(2) . .
C44 C39 C40 C41 0.0 . .
C39 C40 C41 C42 0.0 . .
C40 C41 C42 C43 0.0 . .
C41 C42 C43 C44 0.0 . .
C42 C43 C44 C39 0.0 . .
C40 C39 C44 C43 0.0 . .
