#------------------------------------------------------------------------------
#$Date: 2019-06-11 10:36:04 +0300 (Tue, 11 Jun 2019) $
#$Revision: 215822 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/13/1551325.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_1551325
loop_
_publ_author_name
'Marc A. Little'
'Michael E. Briggs'
'James T. A. Jones'
'Marc Schmidtmann'
'Tom Hasell'
'Samantha Y. Chong'
'Kim E. Jelfs'
'Linjiang Chen'
'Andrew I. Cooper'
_publ_section_title
;
 Trapping virtual pores by crystal retro-engineering
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              153
_journal_page_last               159
_journal_paper_doi               10.1038/nchem.2156
_journal_volume                  7
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety
'2(C72 H84 N12), C72 H72 N11, 2(C0.25 H0.25 Cl0.75), 1.5 (C1 O1 H4)'
_chemical_formula_sum            'C218.02 H246.5 Cl1.5 N35 O1.5'
_chemical_formula_weight         3432.40
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.718(2)
_cell_length_b                   20.718(2)
_cell_length_c                   44.992(5)
_cell_measurement_reflns_used    9140
_cell_measurement_temperature    300
_cell_measurement_theta_max      21.638
_cell_measurement_theta_min      2.315
_cell_volume                     16725(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            92330
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.6949.
The λ/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5511
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6816
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1479P)²+3.8550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2282
_reflns_number_gt                4858
_reflns_number_total             6816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s10.cif
_cod_data_source_block           2(CC3-R)(3+2#5)_350K
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_original_formula_sum        'C218.02 H246.50 Cl1.50 N35 O1.50'
_cod_database_code               1551325
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C50
 1.43 with sigma of 0.005
 O1-C49
 1.43 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(O2) = Uiso(C50)
Uiso(C49) = Uiso(O1)
4. Others
 Fixed Sof: N6(0.5) C42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5)
 H45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5) N7(0.5) C36(0.5) C35(0.5)
 H35(0.5) C34(0.5) H34(0.5) C33(0.5) C38(0.5) H38(0.5) C37(0.5) H37(0.5)
 C39(0.5) H39(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5) H41B(0.5)
 N5(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 C26(0.5) H26(0.5) C27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5)
 C31(0.5) H31(0.5) C32(0.5) H32(0.5) Cl1(0.25) C48(0.08333) H48(0.08333)
 O1(0.16667) C49(0.17) O2(0.08333) C50(0.08333)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C18(H18), C22(H22), C48(H48)
5.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C19(H19A,
 H19B), C20(H20A,H20B), C23(H23A,H23B), C40(H40A,H40B), C41(H41A,H41B),
 C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C12(H12), C14(H14), C16(H16), C17(H17), C21(H21),
 C031(H031), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C35(H35),
 C34(H34), C38(H38), C37(H37), C39(H39), C26(H26), C28(H28), C29(H29), C31(H31),
  C32(H32)
5.d Fitted hexagon refined as free rotating group:
 C42(C43,C44,C45,C46,C47), C36(C35,C34,C33,C38,C37), C27(C28,C29,C30,C31,C32)
5.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 'x-y, -y, -z'
5 '-x, -x+y, -z'
6 'y, x, -z'
7 'x+2/3, y+1/3, z+1/3'
8 '-y+2/3, x-y+1/3, z+1/3'
9 '-x+y+2/3, -x+1/3, z+1/3'
10 'x-y+2/3, -y+1/3, -z+1/3'
11 '-x+2/3, -x+y+1/3, -z+1/3'
12 'y+2/3, x+1/3, -z+1/3'
13 'x+1/3, y+2/3, z+2/3'
14 '-y+1/3, x-y+2/3, z+2/3'
15 '-x+y+1/3, -x+2/3, z+2/3'
16 'x-y+1/3, -y+2/3, -z+2/3'
17 '-x+1/3, -x+y+2/3, -z+2/3'
18 'y+1/3, x+2/3, -z+2/3'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
N1 N 0.49596(17) 0.64133(16) 0.41390(7) 0.0859(7) Uani 1 1 d . . . .
N2 N 0.56073(16) 0.61148(15) 0.36312(7) 0.0838(8) Uani 1 1 d . . . .
N3 N 0.60533(17) 0.81940(17) 0.25175(6) 0.0857(8) Uani 1 1 d . . . .
N4 N 0.37352(17) 0.46367(16) 0.24406(7) 0.0844(7) Uani 1 1 d . . . .
C1 C 0.4094(2) 0.7127(2) 0.40600(7) 0.0812(8) Uani 1 1 d . . . .
H1 H 0.4609 0.7435 0.4059 0.097 Uiso 1 1 calc . . R .
C1A C 0.7442(3) 0.9720(3) 0.20140(12) 0.1264(17) Uani 1 1 d . . . .
H1AA H 0.7230 0.9532 0.1819 0.152 Uiso 1 1 calc . . R .
H1AB H 0.7978 0.9931 0.2000 0.152 Uiso 1 1 calc . . R .
C2 C 0.37919(19) 0.6351(2) 0.40608(7) 0.0781(8) Uani 1 1 d . . . .
C3 C 0.5403(2) 0.60495(19) 0.41661(8) 0.0809(8) Uani 1 1 d . . . .
H3 H 0.5078 0.5509 0.4146 0.097 Uiso 1 1 calc . . R .
C5 C 0.5770(3) 0.6222(3) 0.44690(10) 0.1060(12) Uani 1 1 d . . . .
H5A H 0.5388 0.6016 0.4622 0.127 Uiso 1 1 calc . . R .
H5B H 0.6055 0.6758 0.4497 0.127 Uiso 1 1 calc . . R .
C6 C 0.6281(4) 0.5899(3) 0.45024(12) 0.1273(17) Uani 1 1 d . . . .
H6A H 0.6527 0.6041 0.4694 0.153 Uiso 1 1 calc . . R .
H6B H 0.5988 0.5360 0.4495 0.153 Uiso 1 1 calc . . R .
C7 C 0.6859(3) 0.6174(3) 0.42602(13) 0.1208(16) Uani 1 1 d . . . .
H7A H 0.7157 0.5933 0.4278 0.145 Uiso 1 1 calc . . R .
H7B H 0.7189 0.6707 0.4281 0.145 Uiso 1 1 calc . . R .
C8 C 0.6483(2) 0.6003(3) 0.39550(11) 0.1034(12) Uani 1 1 d . . . .
H8A H 0.6864 0.6197 0.3802 0.124 Uiso 1 1 calc . . R .
H8B H 0.6188 0.5467 0.3930 0.124 Uiso 1 1 calc . . R .
C9 C 0.59879(19) 0.63356(18) 0.39167(8) 0.0823(9) Uani 1 1 d . . . .
H9 H 0.6289 0.6880 0.3927 0.099 Uiso 1 1 calc . . R .
C10 C 0.56984(19) 0.6616(2) 0.34528(8) 0.0823(9) Uani 1 1 d . . . .
H10 H 0.5994 0.7108 0.3513 0.099 Uiso 1 1 calc . . R .
C11 C 0.53676(18) 0.6474(2) 0.31542(8) 0.0829(9) Uani 1 1 d . . . .
C12 C 0.55713(19) 0.70508(19) 0.29569(8) 0.0815(8) Uani 1 1 d . . . .
H12 H 0.5909 0.7535 0.3016 0.098 Uiso 1 1 calc . . R .
C13 C 0.5279(2) 0.6920(2) 0.26687(8) 0.0845(9) Uani 1 1 d . . . .
C14 C 0.4763(2) 0.6201(2) 0.25807(8) 0.0843(9) Uani 1 1 d . . . .
H14 H 0.4564 0.6114 0.2390 0.101 Uiso 1 1 calc . . R .
C15 C 0.4542(2) 0.56062(19) 0.27788(8) 0.0816(8) Uani 1 1 d . . . .
C16 C 0.4849(2) 0.5747(2) 0.30630(9) 0.0852(9) Uani 1 1 d . . . .
H16 H 0.4708 0.5353 0.3195 0.102 Uiso 1 1 calc . . R .
C17 C 0.5541(2) 0.7541(2) 0.24557(8) 0.0895(10) Uani 1 1 d . . . .
H17 H 0.5322 0.7449 0.2269 0.107 Uiso 1 1 calc . . R .
C18 C 0.62968(19) 0.8761(2) 0.22883(8) 0.0809(8) Uani 1 1 d . . . .
H18 H 0.6020 0.8541 0.2104 0.097 Uiso 1 1 calc . . R .
C19 C 0.7130(3) 0.9087(3) 0.22334(11) 0.1079(12) Uani 1 1 d . . . .
H19A H 0.7394 0.9263 0.2420 0.130 Uiso 1 1 calc . . R .
H19B H 0.7216 0.8696 0.2160 0.130 Uiso 1 1 calc . . R .
C20 C 0.7268(3) 1.0327(3) 0.21084(12) 0.1171(15) Uani 1 1 d . . . .
H20A H 0.7536 1.0562 0.2290 0.141 Uiso 1 1 calc . . R .
H20B H 0.7433 1.0706 0.1955 0.141 Uiso 1 1 calc . . R .
C21 C 0.40052(19) 0.48381(19) 0.26936(8) 0.0799(8) Uani 1 1 d . . . .
H21 H 0.3855 0.4473 0.2840 0.096 Uiso 1 1 calc . . R .
C22 C 0.3221(2) 0.38411(17) 0.23911(7) 0.0785(8) Uani 1 1 d . . . .
H22 H 0.3158 0.3573 0.2578 0.094 Uiso 1 1 calc . . R .
C23 C 0.3555(3) 0.3556(2) 0.21590(9) 0.0984(11) Uani 1 1 d . . . .
H23A H 0.3620 0.3820 0.1973 0.118 Uiso 1 1 calc . . R .
H23B H 0.4041 0.3654 0.2225 0.118 Uiso 1 1 calc . . R .
C031 C 0.4285(2) 0.60304(19) 0.40841(7) 0.0804(8) Uani 1 1 d . . . .
H031 H 0.4081 0.5520 0.4056 0.096 Uiso 1 1 calc . . R .
N6 N 0.4724(4) 0.3534(6) 0.3369(3) 0.091(3) Uani 0.50 1 d . . . .
C42 C 0.4025(3) 0.3509(5) 0.3375(2) 0.081(4) Uani 0.50 1 d A . . .
C43 C 0.3413(5) 0.2942(5) 0.3228(2) 0.114(4) Uani 0.50 1 d A 2 G .
H43 H 0.3458 0.2572 0.3129 0.137 Uiso 0.50 1 calc A 2 R .
C44 C 0.2735(4) 0.2928(11) 0.3230(4) 0.128(6) Uani 0.50 1 d A 2 G .
H44 H 0.2326 0.2549 0.3132 0.154 Uiso 0.50 1 calc A 2 R .
C45 C 0.2669(7) 0.3481(14) 0.3378(5) 0.131(8) Uani 0.50 1 d . . G .
H45 H 0.2236 0.3508 0.3392 0.157 Uiso 0.50 1 calc A 1 R .
C46 C 0.3281(8) 0.4048(10) 0.3525(4) 0.126(6) Uani 0.50 1 d A 1 G .
H46 H 0.3237 0.4417 0.3624 0.152 Uiso 0.50 1 calc A 1 R .
C47 C 0.3959(5) 0.4062(5) 0.35233(17) 0.098(3) Uani 0.50 1 d A 1 G .
H47 H 0.4368 0.4441 0.3621 0.117 Uiso 0.50 1 calc A 1 R .
N7 N 0.6307(6) 0.4298(6) 0.4660(3) 0.092(3) Uani 0.50 1 d . 1 . .
N8 N 0.6667 0.3333 0.50381(13) 0.0939(15) Uani 1 3 d . 1 S T
C36 C 0.6062(4) 0.4076(4) 0.41360(18) 0.073(2) Uani 0.50 1 d . 1 . .
C35 C 0.5294(4) 0.3755(4) 0.41643(13) 0.085(2) Uani 0.50 1 d . 1 G .
H35 H 0.5077 0.3664 0.4352 0.102 Uiso 0.50 1 calc . 1 R .
C34 C 0.4849(3) 0.3570(4) 0.39120(15) 0.092(3) Uani 0.50 1 d . 1 G .
H34 H 0.4335 0.3355 0.3931 0.110 Uiso 0.50 1 calc . 1 R .
C33 C 0.5172(5) 0.3705(4) 0.36314(13) 0.083(3) Uani 0.50 1 d . 1 G .
C38 C 0.5940(5) 0.4026(5) 0.36032(16) 0.084(3) Uani 0.50 1 d . 1 G .
H38 H 0.6156 0.4117 0.3415 0.101 Uiso 0.50 1 calc . 1 R .
C37 C 0.6385(3) 0.4212(5) 0.3855(2) 0.083(3) Uani 0.50 1 d . 1 G .
H37 H 0.6898 0.4427 0.3837 0.099 Uiso 0.50 1 calc . 1 R .
C39 C 0.6538(6) 0.4307(6) 0.4403(3) 0.073(3) Uani 0.50 1 d . 1 . .
H39 H 0.7042 0.4470 0.4378 0.088 Uiso 0.50 1 calc . 1 R .
C40 C 0.6794(6) 0.4518(5) 0.4907(3) 0.088(3) Uani 0.50 1 d . 1 . .
H40A H 0.6851 0.4980 0.4986 0.105 Uiso 0.50 1 calc . 1 R .
H40B H 0.7280 0.4618 0.4840 0.105 Uiso 0.50 1 calc . 1 R .
C41 C 0.6525(8) 0.3929(9) 0.5161(3) 0.092(4) Uani 0.50 1 d . 1 . .
H41A H 0.6807 0.4142 0.5342 0.110 Uiso 0.50 1 calc . 1 R .
H41B H 0.5999 0.3730 0.5203 0.110 Uiso 0.50 1 calc . 1 R .
N5 N 0.5290(7) 0.2708(10) 0.2039(3) 0.132(5) Uani 0.50 1 d . 2 . .
C24 C 0.5867(14) 0.2894(19) 0.1571(4) 0.192(14) Uani 0.50 1 d . 2 . .
H24A H 0.5614 0.2780 0.1383 0.288 Uiso 0.50 1 calc . 2 GR .
H24B H 0.6301 0.2841 0.1555 0.288 Uiso 0.50 1 calc . 2 GR .
H24C H 0.6014 0.3396 0.1626 0.288 Uiso 0.50 1 calc . 2 GR .
C25 C 0.5376(10) 0.2390(13) 0.1793(4) 0.185(10) Uani 0.50 1 d . 2 . .
H25A H 0.4890 0.2083 0.1703 0.222 Uiso 0.50 1 calc . 2 R .
H25B H 0.5562 0.2062 0.1851 0.222 Uiso 0.50 1 calc . 2 R .
C26 C 0.5453(8) 0.2591(10) 0.2306(4) 0.110(5) Uani 0.50 1 d . 2 . .
H26 H 0.5673 0.2297 0.2323 0.131 Uiso 0.50 1 calc . 2 R .
C27 C 0.5319(5) 0.2881(6) 0.25786(17) 0.094(4) Uani 0.50 1 d . 2 . .
C28 C 0.5366(6) 0.2583(6) 0.2849(2) 0.091(3) Uani 0.50 1 d . 2 G .
H28 H 0.5521 0.2232 0.2855 0.109 Uiso 0.50 1 calc . 2 R .
C29 C 0.5181(6) 0.2808(5) 0.31109(17) 0.097(4) Uani 0.50 1 d . 2 G .
H29 H 0.5212 0.2609 0.3292 0.117 Uiso 0.50 1 calc . 2 R .
C30 C 0.4949(5) 0.3332(5) 0.31022(14) 0.093(3) Uani 0.50 1 d . 2 G .
C31 C 0.4902(5) 0.3631(6) 0.28318(16) 0.128(4) Uani 0.50 1 d . 2 G .
H31 H 0.4747 0.3981 0.2826 0.154 Uiso 0.50 1 calc . 2 R .
C32 C 0.5087(5) 0.3405(6) 0.25700(14) 0.136(5) Uani 0.50 1 d . 2 G .
H32 H 0.5056 0.3605 0.2389 0.163 Uiso 0.50 1 calc . 2 R .
Cl1 Cl 0.4214(3) 0.7420(3) 0.32503(12) 0.1218(14) Uiso 0.25 1 d B 1 . .
C48 C 0.3333 0.6667 0.3308(9) 0.127(10) Uiso 0.25 3 d . 1 S T
H48 H 0.3333 0.6667 0.3526 0.152 Uiso 0.25 3 calc . 1 RS T
O1 O 0.3333 0.6667 0.2731(2) 0.115(3) Uiso 0.17 1 d C 2 DS T
C49 C 0.3318(16) 0.6262(14) 0.2991(4) 0.115(3) Uiso 0.17 1 d C 2 D .
O2 O 0.3333 0.6667 0.19853(11) 0.240(16) Uiso 0.25 3 d . . DS T
C50 C 0.3333 0.6667 0.1667 0.240(16) Uiso 0.50 6 d . . DS T
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'
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
C031 N1 C3 119.2(3) . .
C10 N2 C9 118.2(3) . .
C17 N3 C18 118.4(3) . .
C21 N4 C22 117.9(3) . .
C2 C1 H1 119.2 2_665 .
C2 C1 H1 119.2 . .
C2 C1 C2 121.6(3) 2_665 .
H1AA C1A H1AB 108.0 . .
C19 C1A H1AA 109.4 . .
C19 C1A H1AB 109.4 . .
C19 C1A C20 111.0(4) . .
C20 C1A H1AA 109.4 . .
C20 C1A H1AB 109.4 . .
C1 C2 C1 118.4(3) 3_565 .
C1 C2 C031 120.2(3) . .
C1 C2 C031 121.3(3) 3_565 .
N1 C3 H3 109.4 . .
N1 C3 C5 109.0(3) . .
N1 C3 C9 108.6(3) . .
C5 C3 H3 109.4 . .
C5 C3 C9 111.1(3) . .
C9 C3 H3 109.4 . .
C3 C5 H5A 109.4 . .
C3 C5 H5B 109.4 . .
C3 C5 C6 111.4(4) . .
H5A C5 H5B 108.0 . .
C6 C5 H5A 109.4 . .
C6 C5 H5B 109.4 . .
C5 C6 H6A 109.4 . .
C5 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
C7 C6 C5 111.2(4) . .
C7 C6 H6A 109.4 . .
C7 C6 H6B 109.4 . .
C6 C7 H7A 109.6 . .
C6 C7 H7B 109.6 . .
C6 C7 C8 110.2(4) . .
H7A C7 H7B 108.1 . .
C8 C7 H7A 109.6 . .
C8 C7 H7B 109.6 . .
C7 C8 H8A 109.1 . .
C7 C8 H8B 109.1 . .
H8A C8 H8B 107.9 . .
C9 C8 C7 112.4(4) . .
C9 C8 H8A 109.1 . .
C9 C8 H8B 109.1 . .
N2 C9 C3 108.9(3) . .
N2 C9 C8 110.1(3) . .
N2 C9 H9 109.6 . .
C3 C9 H9 109.6 . .
C8 C9 C3 109.1(3) . .
C8 C9 H9 109.6 . .
N2 C10 H10 118.0 . .
N2 C10 C11 124.1(3) . .
C11 C10 H10 118.0 . .
C12 C11 C10 120.5(3) . .
C12 C11 C16 118.8(3) . .
C16 C11 C10 120.7(3) . .
C11 C12 H12 119.5 . .
C11 C12 C13 121.0(3) . .
C13 C12 H12 119.5 . .
C12 C13 C17 119.9(3) . .
C14 C13 C12 119.9(3) . .
C14 C13 C17 120.1(4) . .
C13 C14 H14 120.0 . .
C13 C14 C15 120.0(4) . .
C15 C14 H14 120.0 . .
C14 C15 C21 121.7(3) . .
C16 C15 C14 119.1(3) . .
C16 C15 C21 119.2(3) . .
C11 C16 H16 119.4 . .
C15 C16 C11 121.1(3) . .
C15 C16 H16 119.4 . .
N3 C17 C13 122.5(4) . .
N3 C17 H17 118.8 . .
C13 C17 H17 118.8 . .
N3 C18 H18 109.7 . .
N3 C18 C19 109.3(3) . .
N3 C18 C22 109.3(3) . 2_665
C19 C18 H18 109.7 . .
C22 C18 H18 109.7 2_665 .
C22 C18 C19 109.0(3) 2_665 .
C1A C19 C18 112.9(4) . .
C1A C19 H19A 109.0 . .
C1A C19 H19B 109.0 . .
C18 C19 H19A 109.0 . .
C18 C19 H19B 109.0 . .
H19A C19 H19B 107.8 . .
C1A C20 H20A 109.5 . .
C1A C20 H20B 109.5 . .
H20A C20 H20B 108.1 . .
C23 C20 C1A 110.5(4) 2_665 .
C23 C20 H20A 109.5 2_665 .
C23 C20 H20B 109.5 2_665 .
N4 C21 C15 125.0(3) . .
N4 C21 H21 117.5 . .
C15 C21 H21 117.5 . .
N4 C22 C18 111.1(3) . 3_565
N4 C22 H22 108.9 . .
N4 C22 C23 108.9(3) . .
C18 C22 H22 108.9 3_565 .
C18 C22 C23 110.1(3) 3_565 .
C23 C22 H22 108.9 . .
C20 C23 C22 111.0(3) 3_565 .
C20 C23 H23A 109.4 3_565 .
C20 C23 H23B 109.4 3_565 .
C22 C23 H23A 109.4 . .
C22 C23 H23B 109.4 . .
H23A C23 H23B 108.0 . .
N1 C031 C2 122.7(3) . .
N1 C031 H031 118.7 . .
C2 C031 H031 118.7 . .
N6 N6 C42 88.8(4) 16 .
N6 N6 C42 62.0(3) 16 16
N6 N6 C33 38.1(14) 16 16
N6 N6 C33 122.1(19) 16 .
N6 N6 C30 55.0(14) 16 .
N6 N6 C30 91(2) 16 16
C42 N6 C42 27.1(5) . 16
C42 N6 C33 87.3(7) 16 16
C42 N6 C33 112.3(7) . 16
C42 N6 C33 120.9(8) . .
C42 N6 C30 118.9(8) . .
C33 N6 C42 136.8(10) . 16
C33 N6 C33 122.8(9) . 16
C30 N6 C42 97.5(6) . 16
C30 N6 C42 123.1(13) 16 16
C30 N6 C42 123.7(12) 16 .
C30 N6 C33 17.0(7) . 16
C30 N6 C33 30.7(9) 16 .
C30 N6 C33 120.1(5) . .
C30 N6 C33 101.2(9) 16 16
C30 N6 C30 106.5(10) 16 .
C43 C42 N6 120.2(6) . .
C43 C42 C47 120.0 . .
C47 C42 N6 119.8(6) . .
C42 C43 H43 120.0 . .
C42 C43 C44 120.0 . .
C44 C43 H43 120.0 . .
C43 C44 H44 120.0 . .
C45 C44 C43 120.0 . .
C45 C44 H44 120.0 . .
C44 C45 C44 96.1(12) 16 .
C44 C45 H45 138.5 16 .
C44 C45 H45 125.4 . .
C44 C45 C46 10.8(2) . 16
C44 C45 C46 120.0 . .
C44 C45 C46 24.0(12) 16 .
C44 C45 C46 106.8(9) 16 16
C46 C45 H45 114.6 16 .
C46 C45 H45 114.6 . .
C46 C45 C46 130.8(3) . 16
C45 C46 H46 120.0 . .
C47 C46 C45 120.0 . .
C47 C46 H46 120.0 . .
C42 C47 H47 120.0 . .
C46 C47 C42 120.0 . .
C46 C47 H47 120.0 . .
C39 N7 C40 121.2(10) . .
C41 N8 C41 107.3(6) 2_655 .
C41 N8 C41 107.3(7) 3_665 .
C41 N8 C41 107.3(7) 3_665 2_655
C35 C36 C37 120.0 . .
C35 C36 C39 120.1(7) . .
C37 C36 C39 119.8(7) . .
C36 C35 H35 120.0 . .
C36 C35 C34 120.0 . .
C34 C35 H35 120.0 . .
C35 C34 H34 120.0 . .
C33 C34 C35 120.0 . .
C33 C34 H34 120.0 . .
N6 C33 N6 19.8(7) . 16
C34 C33 N6 120.8(6) . .
C34 C33 N6 117.1(5) . 16
C34 C33 C38 120.0 . .
C38 C33 N6 119.5(5) . 16
C38 C33 N6 119.2(6) . .
C33 C38 H38 120.0 . .
C37 C38 C33 120.0 . .
C37 C38 H38 120.0 . .
C36 C37 H37 120.0 . .
C38 C37 C36 120.0 . .
C38 C37 H37 120.0 . .
N7 C39 C36 124.2(10) . .
N7 C39 H39 117.9 . .
C36 C39 H39 117.9 . .
N7 C40 H40A 108.8 . .
N7 C40 H40B 108.8 . .
N7 C40 C41 113.9(10) . .
H40A C40 H40B 107.7 . .
C41 C40 H40A 108.8 . .
C41 C40 H40B 108.8 . .
N8 C41 C40 103.4(9) . .
N8 C41 H41A 111.1 . .
N8 C41 H41B 111.1 . .
C40 C41 H41A 111.1 . .
C40 C41 H41B 111.1 . .
H41A C41 H41B 109.1 . .
C26 N5 C25 124(2) . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C25 C24 H24A 109.5 . .
C25 C24 H24B 109.5 . .
C25 C24 H24C 109.5 . .
N5 C25 C24 116(2) . .
N5 C25 H25A 108.3 . .
N5 C25 H25B 108.3 . .
C24 C25 H25A 108.3 . .
C24 C25 H25B 108.3 . .
H25A C25 H25B 107.4 . .
N5 C26 H26 117.2 . .
N5 C26 C27 125.5(16) . .
C27 C26 H26 117.2 . .
C28 C27 C26 119.0(9) . .
C28 C27 C32 120.0 . .
C32 C27 C26 120.8(9) . .
C27 C28 H28 120.0 . .
C27 C28 C29 120.0 . .
C29 C28 H28 120.0 . .
C28 C29 H29 120.0 . .
C28 C29 C30 120.0 . .
C30 C29 H29 120.0 . .
N6 C30 N6 33.5(8) 16 .
N6 C30 C29 101.4(8) 16 .
N6 C30 C31 127.6(7) 16 .
C29 C30 N6 119.8(7) . .
C31 C30 N6 120.1(6) . .
C31 C30 C29 120.0 . .
C30 C31 H31 120.0 . .
C32 C31 C30 120.0 . .
C32 C31 H31 120.0 . .
C27 C32 H32 120.0 . .
C31 C32 C27 120.0 . .
C31 C32 H32 120.0 . .
Cl1 C48 Cl1 117.8(7) . 3_565
Cl1 C48 Cl1 117.8(7) 2_665 3_565
Cl1 C48 Cl1 117.8(7) 2_665 .
Cl1 C48 H48 98.6 3_565 .
Cl1 C48 H48 98.6 . .
Cl1 C48 H48 98.6 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C3 1.456(4) .
N1 C031 1.239(5) .
N2 C9 1.456(5) .
N2 C10 1.249(4) .
N3 C17 1.265(5) .
N3 C18 1.452(4) .
N4 C21 1.245(5) .
N4 C22 1.465(4) .
C1 H1 0.9300 .
C1 C2 1.368(5) 2_665
C1 C2 1.403(5) .
C1A H1AA 0.9700 .
C1A H1AB 0.9700 .
C1A C19 1.504(7) .
C1A C20 1.532(8) .
C2 C1 1.368(5) 3_565
C2 C031 1.474(5) .
C3 H3 0.9800 .
C3 C5 1.513(6) .
C3 C9 1.537(5) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C6 1.517(7) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.505(8) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.530(7) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C9 1.505(5) .
C9 H9 0.9800 .
C10 H10 0.9300 .
C10 C11 1.470(5) .
C11 C12 1.374(5) .
C11 C16 1.405(5) .
C12 H12 0.9300 .
C12 C13 1.399(5) .
C13 C14 1.388(5) .
C13 C17 1.473(5) .
C14 H14 0.9300 .
C14 C15 1.399(5) .
C15 C16 1.392(5) .
C15 C21 1.465(5) .
C16 H16 0.9300 .
C17 H17 0.9300 .
C18 H18 0.9800 .
C18 C19 1.527(6) .
C18 C22 1.517(5) 2_665
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C20 C23 1.506(6) 2_665
C21 H21 0.9300 .
C22 C18 1.517(5) 3_565
C22 H22 0.9800 .
C22 C23 1.526(5) .
C23 C20 1.506(6) 3_565
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C031 H031 0.9300 .
N6 N6 0.787(14) 16
N6 C42 1.612(7) 16
N6 C42 1.423(7) .
N6 C33 1.967(12) 16
N6 C33 1.433(11) .
N6 C30 1.166(17) 16
N6 C30 1.423(11) .
C42 C43 1.3900 .
C42 C47 1.3900 .
C43 H43 0.9300 .
C43 C44 1.3900 .
C44 H44 0.9300 .
C44 C45 1.3900 .
C45 C44 0.887(15) 16
C45 H45 0.9300 .
C45 C46 2.00(2) 16
C45 C46 1.3900 .
C46 H46 0.9300 .
C46 C47 1.3900 .
C47 H47 0.9300 .
N7 C39 1.250(19) .
N7 C40 1.414(17) .
N8 C41 1.509(17) .
N8 C41 1.509(17) 2_655
N8 C41 1.509(17) 3_665
C36 C35 1.3900 .
C36 C37 1.3900 .
C36 C39 1.473(13) .
C35 H35 0.9300 .
C35 C34 1.3900 .
C34 H34 0.9300 .
C34 C33 1.3900 .
C33 N6 1.967(10) 16
C33 C38 1.3900 .
C38 H38 0.9300 .
C38 C37 1.3900 .
C37 H37 0.9300 .
C39 H39 0.9300 .
C40 H40A 0.9700 .
C40 H40B 0.9700 .
C40 C41 1.559(18) .
C41 H41A 0.9700 .
C41 H41B 0.9700 .
N5 C25 1.35(2) .
N5 C26 1.30(2) .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C24 C25 1.43(3) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 H26 0.9300 .
C26 C27 1.452(17) .
C27 C28 1.3900 .
C27 C32 1.3900 .
C28 H28 0.9300 .
C28 C29 1.3900 .
C29 H29 0.9300 .
C29 C30 1.3900 .
C30 N6 1.166(13) 16
C30 C31 1.3900 .
C31 H31 0.9300 .
C31 C32 1.3900 .
C32 H32 0.9300 .
Cl1 C48 1.728(8) .
C48 Cl1 1.728(9) 3_565
C48 Cl1 1.728(9) 2_665
C48 H48 0.9800 .
O1 C49 1.433(5) .
O2 C50 1.433(5) .
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
N1 C3 C5 C6 -176.2(4) . . . .
N1 C3 C9 N2 -63.7(3) . . . .
N1 C3 C9 C8 176.2(3) . . . .
N2 C10 C11 C12 -171.4(3) . . . .
N2 C10 C11 C16 7.3(5) . . . .
N3 C18 C19 C1A -175.9(4) . . . .
N4 C22 C23 C20 177.9(4) . . . 3_565
C1 C2 C031 N1 8.8(5) . . . .
C1 C2 C031 N1 -166.6(3) 3_565 . . .
C2 C1 C2 C1 0.5(6) 2_665 . . 3_565
C2 C1 C2 C031 -175.1(2) 2_665 . . .
C3 N1 C031 C2 178.4(3) . . . .
C3 C5 C6 C7 56.1(6) . . . .
C5 C3 C9 N2 176.4(3) . . . .
C5 C3 C9 C8 56.3(4) . . . .
C5 C6 C7 C8 -55.2(6) . . . .
C6 C7 C8 C9 57.0(5) . . . .
C7 C8 C9 N2 -176.2(3) . . . .
C7 C8 C9 C3 -56.8(4) . . . .
C9 N2 C10 C11 178.1(3) . . . .
C9 C3 C5 C6 -56.5(5) . . . .
C10 N2 C9 C3 118.6(3) . . . .
C10 N2 C9 C8 -121.9(3) . . . .
C10 C11 C12 C13 177.8(3) . . . .
C10 C11 C16 C15 -178.9(3) . . . .
C11 C12 C13 C14 1.4(5) . . . .
C11 C12 C13 C17 -176.2(3) . . . .
C12 C11 C16 C15 -0.1(5) . . . .
C12 C13 C14 C15 -0.8(5) . . . .
C12 C13 C17 N3 3.4(6) . . . .
C13 C14 C15 C16 -0.2(5) . . . .
C13 C14 C15 C21 -179.3(3) . . . .
C14 C13 C17 N3 -174.2(4) . . . .
C14 C15 C16 C11 0.7(5) . . . .
C14 C15 C21 N4 4.5(5) . . . .
C16 C11 C12 C13 -0.9(5) . . . .
C16 C15 C21 N4 -174.6(4) . . . .
C17 N3 C18 C19 -121.8(4) . . . .
C17 N3 C18 C22 119.0(4) . . . 2_665
C17 C13 C14 C15 176.8(3) . . . .
C18 N3 C17 C13 177.3(3) . . . .
C18 C22 C23 C20 -60.0(4) 3_565 . . 3_565
C19 C1A C20 C23 -53.9(6) . . . 2_665
C20 C1A C19 C18 54.4(6) . . . .
C21 N4 C22 C18 120.8(3) . . . 3_565
C21 N4 C22 C23 -117.7(4) . . . .
C21 C15 C16 C11 179.8(3) . . . .
C22 N4 C21 C15 178.2(3) . . . .
C22 C18 C19 C1A -56.4(5) 2_665 . . .
C031 N1 C3 C5 -122.6(4) . . . .
C031 N1 C3 C9 116.2(4) . . . .
N6 N6 C42 C43 -10(2) 16 . . .
N6 N6 C42 C47 171.2(18) 16 . . .
N6 N6 C33 C34 -85.0(16) 16 . . .
N6 N6 C33 C38 96.4(19) 16 . . .
N6 N6 C30 C29 -63.1(12) 16 . . .
N6 N6 C30 C31 113.7(14) 16 . . .
N6 C42 C43 C44 -178.7(14) . . . .
N6 C42 C47 C46 178.7(14) . . . .
N6 C33 C38 C37 -158.7(6) 16 . . .
N6 C33 C38 C37 178.6(7) . . . .
N6 C30 C31 C32 -176.8(8) . . . .
N6 C30 C31 C32 -137.1(10) 16 . . .
C42 N6 C42 C43 -3.3(14) 16 . . .
C42 N6 C42 C47 178(2) 16 . . .
C42 N6 C33 N6 110(3) . . . 16
C42 N6 C33 N6 82(2) 16 . . 16
C42 N6 C33 C34 -3.2(13) 16 . . .
C42 N6 C33 C34 25.3(13) . . . .
C42 N6 C33 C38 -153.3(9) . . . .
C42 N6 C33 C38 178.2(8) 16 . . .
C42 N6 C30 N6 -47.8(9) 16 . . 16
C42 N6 C30 N6 -65.5(8) . . . 16
C42 N6 C30 C29 -128.6(10) . . . .
C42 N6 C30 C29 -110.9(8) 16 . . .
C42 N6 C30 C31 48.2(12) . . . .
C42 N6 C30 C31 65.9(9) 16 . . .
C42 C43 C44 C45 0.0 . . . .
C43 C42 C47 C46 0.0 . . . .
C43 C44 C45 C44 2(3) . . . 16
C43 C44 C45 C46 0.0 . . . .
C43 C44 C45 C46 176(8) . . . 16
C44 C45 C46 C47 0.0 . . . .
C44 C45 C46 C47 -4(7) 16 . . .
C45 C46 C47 C42 0.0 . . . .
C46 C45 C46 C47 -1.0(18) 16 . . .
C47 C42 C43 C44 0.0 . . . .
N7 C40 C41 N8 73.9(13) . . . .
C36 C35 C34 C33 0.0 . . . .
C35 C36 C37 C38 0.0 . . . .
C35 C36 C39 N7 -6.8(16) . . . .
C35 C34 C33 N6 -178.6(7) . . . .
C35 C34 C33 N6 159.1(6) . . . 16
C35 C34 C33 C38 0.0 . . . .
C34 C33 C38 C37 0.0 . . . .
C33 N6 C42 C43 -137.5(8) . . . .
C33 N6 C42 C43 20.7(14) 16 . . .
C33 N6 C42 C47 43.8(14) . . . .
C33 N6 C42 C47 -158.0(8) 16 . . .
C33 N6 C33 N6 -45.5(11) 16 . . 16
C33 N6 C33 C34 -130.5(11) 16 . . .
C33 N6 C33 C38 50.9(11) 16 . . .
C33 N6 C30 N6 6(3) 16 . . 16
C33 N6 C30 N6 110(2) . . . 16
C33 N6 C30 C29 47.0(11) . . . .
C33 N6 C30 C29 -57(2) 16 . . .
C33 N6 C30 C31 -136.2(8) . . . .
C33 N6 C30 C31 119(3) 16 . . .
C33 C38 C37 C36 0.0 . . . .
C37 C36 C35 C34 0.0 . . . .
C37 C36 C39 N7 170.2(10) . . . .
C39 N7 C40 C41 -126.6(13) . . . .
C39 C36 C35 C34 177.0(9) . . . .
C39 C36 C37 C38 -177.0(9) . . . .
C40 N7 C39 C36 179.2(10) . . . .
C41 N8 C41 C40 97.2(15) 3_665 . . .
C41 N8 C41 C40 -147.7(9) 2_655 . . .
N5 C26 C27 C28 165.9(13) . . . .
N5 C26 C27 C32 -9(2) . . . .
C25 N5 C26 C27 -175.4(15) . . . .
C26 N5 C25 C24 -120(2) . . . .
C26 C27 C28 C29 -174.7(10) . . . .
C26 C27 C32 C31 174.6(11) . . . .
C27 C28 C29 C30 0.0 . . . .
C28 C27 C32 C31 0.0 . . . .
C28 C29 C30 N6 146.6(7) . . . 16
C28 C29 C30 N6 176.8(8) . . . .
C28 C29 C30 C31 0.0 . . . .
C29 C30 C31 C32 0.0 . . . .
C30 N6 C42 C43 38.0(15) . . . .
C30 N6 C42 C43 -101.1(12) 16 . . .
C30 N6 C42 C47 80.2(15) 16 . . .
C30 N6 C42 C47 -140.7(8) . . . .
C30 N6 C33 N6 -65.2(11) . . . 16
C30 N6 C33 N6 5(2) 16 . . 16
C30 N6 C33 C34 -150.2(8) . . . .
C30 N6 C33 C34 -79.6(16) 16 . . .
C30 N6 C33 C38 31.3(12) . . . .
C30 N6 C33 C38 101.8(18) 16 . . .
C30 N6 C30 N6 80.0(19) 16 . . 16
C30 N6 C30 C29 16.9(11) 16 . . .
C30 N6 C30 C31 -166.3(11) 16 . . .
C30 C31 C32 C27 0.0 . . . .
C32 C27 C28 C29 0.0 . . . .
