#------------------------------------------------------------------------------
#$Date: 2020-02-05 01:43:11 +0200 (Wed, 05 Feb 2020) $
#$Revision: 247853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/41/4134127.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_4134127
loop_
_publ_author_name
'Liu, Wenqi'
'Bobbala, Sharan'
'Stern, Charlotte L.'
'Hornick, Jessica'
'Liu, Yugang'
'Enciso, Alan Enrique'
'Scott, Evan A.'
'Stoddart, J. Fraser'
_publ_section_title
;
 XCage: A Tricyclic Octacationic Receptor for Perylene Diimide with
 Picomolar Affinity in Water.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12982
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C96 H76 N8, C32 H28 N4 O4, 7(F6 P), 4(C2 H3 N), 2(H O)'
_chemical_formula_sum            'C136 H118 F42 N16 O6 P7'
_chemical_formula_weight         3087.25
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.109(4)
_cell_length_b                   40.109(4)
_cell_length_c                   10.8259(13)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      53.390
_cell_measurement_theta_min      2.463
_cell_volume                     17416(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            37061
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        54.261
_diffrn_reflns_theta_max         54.261
_diffrn_reflns_theta_min         1.558
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.6158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1224 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.8203. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       needle
_exptl_crystal_F_000             6308
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 2409 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.128(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         10132
_refine_ls_number_restraints     1320
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2703
_refine_ls_wR_factor_ref         0.2963
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                7288
_reflns_number_total             10132
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12982_si_003.cif
_cod_data_source_block           cx1582a
_cod_original_cell_volume        17416(4)
_cod_database_code               4134127
_shelx_shelxl_version_number     2017/1
_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_max   0.966
_shelx_estimated_absorpt_t_min   0.405
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P4-F20 = P4-F24 = P4-F22 = P4-F23 = P4-F19 = P4-F21
 1.6 with sigma of 0.02
 C69-C68
 2.4 with sigma of 0.02
 O2S-H2S = O1S-H1S
 1 with sigma of 0.02
 C67_$1-C66 \\sim C67-C66 \\sim C63_$1-C62_$1 \\sim C63-C62
 with sigma of 0.01
 F7-F9 \\sim F7-F10 \\sim F7-F11 \\sim F7-F12 \\sim F8-F9 \\sim F8-F10 \\sim
F8-F11 \\sim F8-F12 \\sim F9-F10
 \\sim F9-F12 \\sim F10-F11 \\sim F11-F12
 with sigma of 0.02
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12
 with sigma of 0.01
 F7A-F9A \\sim F7A-F10A \\sim F7A-F11A \\sim F7A-F12A \\sim F8A-F9A \\sim
F8A-F10A \\sim F8A-F11A ~
 F8A-F12A \\sim F9A-F10A \\sim F9A-F12A \\sim F10A-F11A \\sim F11A-F12A
 with sigma of 0.02
 P2A-F7A \\sim P2A-F8A \\sim P2A-F9A \\sim P2A-F10A \\sim P2A-F11A \\sim
P2A-F12A
 with sigma of 0.01
 F19-F21 \\sim F19-F22 \\sim F19-F23 \\sim F19-F24 \\sim F20-F21 \\sim F20-F22
\\sim F20-F23 \\sim F20-F24
 \\sim F21-F22 \\sim F21-F24 \\sim F22-F23 \\sim F23-F24
 with sigma of 0.02
 P4-F19 \\sim P4-F20 \\sim P4-F21 \\sim P4-F22 \\sim P4-F23 \\sim P4-F24
 with sigma of 0.01
 N7-C66 \\sim N8_$1-C69_$1 \\sim N8_$1-C67_$1 \\sim N8_$1-C68_$1 \\sim N8-C68
\\sim N8-C67 \\sim N8-
 C69 \\sim N6-C63 \\sim N6-C63_$1 \\sim N5-C62 \\sim N5-C62_$1 \\sim N6-C64_$1
\\sim N6-C64
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C69) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(O2S) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Fixed Sof: N8(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5)
 H66A(0.5) H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5) C68(0.5) H68A(0.5) H68B(0.5)
 H68C(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) P4(0.5) F19(0.5) F20(0.5)
 F21(0.5) F22(0.5) F23(0.5) F24(0.5) H2S(0.5) H1S(0.5) O1S(0.5) O2S(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C18(H18A,H18B), C25(H25A,H25B), C42(H42A,H42B), C62(H62A,H62B),
 C63(H63A,H63B), C66(H66A,H66B), C67(H67A,H67B)
6.b Me refined with riding coordinates:
 C69(H69A,H69B,H69C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C34(H34), C36(H36), C38(H38),
 C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50),
  C51(H51), C56(H56), C57(H57)
6.d Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,
 H4SC)
;
_olex2_date_sample_data_collection 2019-06-10
_olex2_date_sample_submission    2019-06-06
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id cx1582a
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5645(2) 0.2785(3) 0.4140(9) 0.066(2) Uani 1 1 d . U . . .
N2 N 0.7556(3) 0.4316(2) 0.4917(8) 0.056(2) Uani 1 1 d . U . . .
N3 N 0.7210(3) 0.0880(2) 0.5127(9) 0.061(2) Uani 1 1 d . U . . .
N4 N 0.9080(2) 0.2366(3) 0.4064(9) 0.059(2) Uani 1 1 d . U . . .
C1 C 0.5296(3) 0.2715(4) 0.4435(12) 0.072(3) Uani 1 1 d . U . . .
H1A H 0.520549 0.254563 0.385915 0.086 Uiso 1 1 calc R . . . .
H1B H 0.516089 0.292042 0.435473 0.086 Uiso 1 1 calc R . . . .
C2 C 0.5865(3) 0.2556(4) 0.3826(13) 0.073(3) Uani 1 1 d . U . . .
H2 H 0.578539 0.233996 0.362200 0.088 Uiso 1 1 calc R . . . .
C3 C 0.6196(3) 0.2613(3) 0.3777(11) 0.058(3) Uani 1 1 d . U . . .
H3 H 0.634007 0.243394 0.355982 0.070 Uiso 1 1 calc R . . . .
C4 C 0.6330(3) 0.2915(3) 0.4027(9) 0.049(2) Uani 1 1 d . U . . .
C5 C 0.6102(3) 0.3179(4) 0.4229(14) 0.075(3) Uani 1 1 d . U . . .
H5 H 0.618033 0.340140 0.430722 0.090 Uiso 1 1 calc R . . . .
C6 C 0.5759(3) 0.3110(4) 0.4313(14) 0.076(3) Uani 1 1 d . U . . .
H6 H 0.560508 0.328462 0.448711 0.091 Uiso 1 1 calc R . . . .
C7 C 0.6699(3) 0.2981(3) 0.4046(11) 0.052(2) Uani 1 1 d . U . . .
C8 C 0.6910(3) 0.2700(3) 0.4036(9) 0.043(2) Uani 1 1 d . U . . .
H8 H 0.681900 0.248211 0.395147 0.052 Uiso 1 1 calc R . . . .
C9 C 0.7257(2) 0.2744(2) 0.4151(8) 0.0376(18) Uani 1 1 d . U . . .
C10 C 0.7384(3) 0.3059(2) 0.4293(8) 0.0371(19) Uani 1 1 d . U . . .
H10 H 0.761789 0.308579 0.439307 0.045 Uiso 1 1 calc R . . . .
C11 C 0.7180(3) 0.3346(2) 0.4296(9) 0.044(2) Uani 1 1 d . U . . .
C12 C 0.6830(3) 0.3292(3) 0.4213(10) 0.049(2) Uani 1 1 d . U . . .
H12 H 0.668421 0.347788 0.427465 0.059 Uiso 1 1 calc R . . . .
C13 C 0.7317(3) 0.3679(3) 0.4498(10) 0.051(2) Uani 1 1 d . U . . .
C14 C 0.7637(3) 0.3729(3) 0.4932(11) 0.056(3) Uani 1 1 d . U . . .
H14 H 0.777368 0.353958 0.508886 0.067 Uiso 1 1 calc R . . . .
C15 C 0.7770(3) 0.4050(3) 0.5154(12) 0.066(3) Uani 1 1 d . U . . .
H15 H 0.799142 0.408294 0.544553 0.079 Uiso 1 1 calc R . . . .
C16 C 0.7261(3) 0.4287(3) 0.4484(11) 0.061(3) Uani 1 1 d . U . . .
H16 H 0.712880 0.447804 0.432074 0.073 Uiso 1 1 calc R . . . .
C17 C 0.7136(3) 0.3962(3) 0.4254(11) 0.061(3) Uani 1 1 d . U . . .
H17 H 0.691803 0.393908 0.391763 0.073 Uiso 1 1 calc R . . . .
C18 C 0.7668(4) 0.4649(3) 0.5391(12) 0.075(3) Uani 1 1 d . U . . .
H18A H 0.791068 0.467583 0.526810 0.090 Uiso 1 1 calc R . . . .
H18B H 0.755204 0.483006 0.493794 0.090 Uiso 1 1 calc R . . . .
C19 C 0.7585(4) 0.4668(3) 0.6741(12) 0.065(2) Uani 1 1 d . U . . .
C20 C 0.7814(4) 0.4659(3) 0.7622(12) 0.070(3) Uani 1 1 d . U . . .
H20 H 0.804187 0.464148 0.739562 0.083 Uiso 1 1 calc R . . . .
C21 C 0.7729(4) 0.4674(3) 0.8888(12) 0.071(3) Uani 1 1 d . U . . .
H21 H 0.789924 0.465068 0.949432 0.085 Uiso 1 1 calc R . . . .
C22 C 0.7415(4) 0.4720(3) 0.9242(11) 0.065(3) Uani 1 1 d . U . . .
C23 C 0.7135(4) 0.4747(3) 0.8273(11) 0.072(3) Uani 1 1 d . U . . .
H23 H 0.690701 0.477229 0.849141 0.086 Uiso 1 1 calc R . . . .
C24 C 0.7244(4) 0.4730(3) 0.7024(11) 0.066(3) Uani 1 1 d . U . . .
H24 H 0.708832 0.476102 0.637325 0.079 Uiso 1 1 calc R . . . .
C25 C 0.7102(4) 0.0530(3) 0.5619(10) 0.067(3) Uani 1 1 d . U . . .
H25A H 0.685659 0.050712 0.560949 0.080 Uiso 1 1 calc R . . . .
H25B H 0.720057 0.035023 0.510856 0.080 Uiso 1 1 calc R . . . .
C26 C 0.7497(3) 0.0913(3) 0.4499(10) 0.060(3) Uani 1 1 d . U . . .
H26 H 0.762263 0.072319 0.426142 0.072 Uiso 1 1 calc R . . . .
C27 C 0.7604(3) 0.1228(2) 0.4209(10) 0.053(2) Uani 1 1 d . U . . .
H27 H 0.780046 0.125600 0.373260 0.063 Uiso 1 1 calc R . . . .
C28 C 0.7427(3) 0.1507(3) 0.4603(10) 0.050(2) Uani 1 1 d . U . . .
C29 C 0.7126(3) 0.1453(3) 0.5209(12) 0.056(3) Uani 1 1 d . U . . .
H29 H 0.699159 0.163718 0.544920 0.068 Uiso 1 1 calc R . . . .
C30 C 0.7024(3) 0.1131(3) 0.5459(11) 0.057(2) Uani 1 1 d . U . . .
H30 H 0.681830 0.109280 0.587195 0.068 Uiso 1 1 calc R . . . .
C31 C 0.7576(3) 0.1851(3) 0.4410(10) 0.046(2) Uani 1 1 d . U . . .
C32 C 0.7909(3) 0.1905(3) 0.4212(10) 0.047(2) Uani 1 1 d . U . . .
H32 H 0.805503 0.171813 0.421096 0.057 Uiso 1 1 calc R . . . .
C33 C 0.8041(2) 0.2213(2) 0.4015(9) 0.0401(19) Uani 1 1 d . U . . .
C34 C 0.7817(2) 0.2485(2) 0.3943(9) 0.041(2) Uani 1 1 d . U . . .
H34 H 0.790181 0.270027 0.374877 0.049 Uiso 1 1 calc R . . . .
C35 C 0.7476(2) 0.2447(2) 0.4150(9) 0.0394(19) Uani 1 1 d . U . . .
C36 C 0.7359(2) 0.2126(2) 0.4391(8) 0.0364(19) Uani 1 1 d . U . . .
H36 H 0.712776 0.209290 0.454563 0.044 Uiso 1 1 calc R . . . .
C37 C 0.8395(3) 0.2264(3) 0.3938(10) 0.050(2) Uani 1 1 d . U . . .
C38 C 0.8630(3) 0.2000(3) 0.3831(10) 0.050(2) Uani 1 1 d . U . . .
H38 H 0.855250 0.177882 0.371049 0.060 Uiso 1 1 calc R . . . .
C39 C 0.8963(3) 0.2060(3) 0.3900(10) 0.056(2) Uani 1 1 d . U . . .
H39 H 0.911537 0.187933 0.382817 0.067 Uiso 1 1 calc R . . . .
C40 C 0.8870(3) 0.2622(3) 0.4130(13) 0.067(3) Uani 1 1 d . U . . .
H40 H 0.895819 0.283968 0.423575 0.080 Uiso 1 1 calc R . . . .
C41 C 0.8543(3) 0.2582(3) 0.4053(13) 0.064(3) Uani 1 1 d . U . . .
H41 H 0.840396 0.277383 0.407499 0.077 Uiso 1 1 calc R . . . .
C42 C 0.9461(3) 0.2439(4) 0.4293(11) 0.069(3) Uani 1 1 d . U . . .
H42A H 0.959533 0.223420 0.417828 0.083 Uiso 1 1 calc R . . . .
H42B H 0.954278 0.261225 0.371694 0.083 Uiso 1 1 calc R . . . .
C43 C 0.9480(3) 0.2558(3) 0.5607(11) 0.061(2) Uani 1 1 d . U . . .
C44 C 0.9452(3) 0.2325(3) 0.6597(11) 0.060(3) Uani 1 1 d . U . . .
H44 H 0.942658 0.209457 0.641820 0.072 Uiso 1 1 calc R . . . .
C45 C 0.9461(3) 0.2430(3) 0.7805(11) 0.059(2) Uani 1 1 d . U . . .
H45 H 0.945073 0.227228 0.845972 0.070 Uiso 1 1 calc R . . . .
C46 C 0.9485(3) 0.2764(3) 0.8055(11) 0.059(3) Uani 1 1 d . U . . .
C47 C 0.9526(3) 0.2987(3) 0.7120(11) 0.064(3) Uani 1 1 d . U . . .
H47 H 0.955366 0.321651 0.730312 0.077 Uiso 1 1 calc R . . . .
C48 C 0.9527(3) 0.2877(3) 0.5871(11) 0.064(3) Uani 1 1 d . U . . .
H48 H 0.956052 0.303360 0.522342 0.077 Uiso 1 1 calc R . . . .
O1 O 0.8587(3) 0.2221(3) 0.7235(16) 0.139(5) Uani 1 1 d . U . . .
O2 O 0.6570(3) 0.4210(3) 0.7747(15) 0.136(4) Uani 1 1 d . U . . .
N5 N 0.8178(3) 0.1822(3) 0.750000 0.117(6) Uani 1 2 d DS TU P . .
N6 N 0.8849(3) 0.1151(3) 0.750000 0.129(6) Uani 1 2 d DS TU P . .
N7 N 0.6201(3) 0.3799(3) 0.750000 0.133(7) Uani 1 2 d DS TU P . .
N8 N 0.6139(11) 0.4350(12) 0.544(3) 0.193(12) Uani 0.5 1 d D U . A -2
C49 C 0.8018(4) 0.2395(4) 0.7332(13) 0.084(3) Uani 1 1 d . U . . .
C50 C 0.8112(4) 0.2722(4) 0.7193(11) 0.072(3) Uani 1 1 d . U . . .
H50 H 0.833893 0.277327 0.703260 0.087 Uiso 1 1 calc R . . . .
C51 C 0.7868(4) 0.2993(4) 0.7286(12) 0.080(3) Uani 1 1 d . U . . .
H51 H 0.792943 0.322114 0.723433 0.096 Uiso 1 1 calc R . . . .
C52 C 0.7535(3) 0.2891(3) 0.7457(10) 0.067(2) Uani 1 1 d . U . . .
C53 C 0.7434(3) 0.2566(3) 0.750000 0.065(3) Uani 1 2 d S TU P . .
C54 C 0.7687(3) 0.2313(3) 0.750000 0.073(4) Uani 1 2 d S TU P . .
C55 C 0.7271(4) 0.3165(4) 0.7536(13) 0.077(3) Uani 1 1 d . U . . .
C56 C 0.7359(4) 0.3505(4) 0.7664(13) 0.082(3) Uani 1 1 d . U . . .
H56 H 0.758648 0.357004 0.772058 0.098 Uiso 1 1 calc R . . . .
C57 C 0.7106(4) 0.3741(4) 0.7705(12) 0.080(3) Uani 1 1 d . U . . .
H57 H 0.716576 0.396805 0.782706 0.096 Uiso 1 1 calc R . . . .
C58 C 0.6783(4) 0.3666(4) 0.7582(15) 0.091(4) Uani 1 1 d . U . . .
C59 C 0.6679(3) 0.3321(3) 0.750000 0.071(4) Uani 1 2 d S TU P . .
C60 C 0.6934(3) 0.3066(3) 0.750000 0.071(4) Uani 1 2 d S TU P . .
C61 C 0.8297(5) 0.2132(5) 0.725(2) 0.114(5) Uani 1 1 d . U . . .
C62 C 0.8427(8) 0.1558(8) 0.682(3) 0.111(8) Uani 0.5 1 d D U . B -1
H62A H 0.830535 0.138220 0.636261 0.133 Uiso 0.5 1 calc R . . B -1
H62B H 0.858935 0.166939 0.626348 0.133 Uiso 0.5 1 calc R . . B -1
C63 C 0.8585(16) 0.1432(15) 0.799(3) 0.18(2) Uani 0.5 1 d D U . B -1
H63A H 0.841615 0.133160 0.854673 0.221 Uiso 0.5 1 calc R . . B -1
H63B H 0.870132 0.161353 0.843766 0.221 Uiso 0.5 1 calc R . . B -1
C64 C 0.8795(8) 0.0896(7) 0.633(3) 0.204(12) Uani 1 1 d D U . . .
H64A H 0.856517 0.081311 0.633663 0.307 Uiso 1 1 calc GR . . . .
H64B H 0.894930 0.070715 0.641196 0.307 Uiso 1 1 calc GR . . . .
H64C H 0.883885 0.101379 0.555926 0.307 Uiso 1 1 calc GR . . . .
C65 C 0.6508(5) 0.3903(5) 0.772(2) 0.124(6) Uani 1 1 d . U . . .
C66 C 0.5913(3) 0.4087(3) 0.750000 0.162(10) Uani 1 2 d DS TU P . .
H66A H 0.570070 0.397002 0.767264 0.194 Uiso 0.5 1 calc R . . A .
H66B H 0.595871 0.422802 0.823119 0.194 Uiso 0.5 1 calc R . . . .
C67 C 0.5839(11) 0.4325(12) 0.646(4) 0.168(16) Uani 0.5 1 d D U . A -2
H67A H 0.579886 0.454994 0.680504 0.202 Uiso 0.5 1 calc R . . A -2
H67B H 0.563224 0.425315 0.603624 0.202 Uiso 0.5 1 calc R . . A -2
C68 C 0.6332(11) 0.4070(11) 0.460(5) 0.142(12) Uani 0.5 1 d D U . A -2
H68A H 0.629207 0.384821 0.494888 0.213 Uiso 0.5 1 calc GR . . A -2
H68B H 0.657209 0.411690 0.460544 0.213 Uiso 0.5 1 calc GR . . A -2
H68C H 0.624856 0.407836 0.375215 0.213 Uiso 0.5 1 calc GR . . A -2
C69 C 0.5941(15) 0.4520(14) 0.428(5) 0.197(17) Uani 0.5 1 d D U . A -2
H69A H 0.609493 0.455017 0.358217 0.295 Uiso 0.5 1 calc R . . A -2
H69B H 0.575639 0.437553 0.402187 0.295 Uiso 0.5 1 calc R . . A -2
H69C H 0.585252 0.473785 0.452826 0.295 Uiso 0.5 1 calc R . . A -2
P1 P 0.86492(15) 0.35401(18) 0.5961(5) 0.1322(18) Uani 1 1 d . U . . .
F1 F 0.8912(4) 0.3763(6) 0.6730(16) 0.232(6) Uani 1 1 d . U . . .
F2 F 0.8397(3) 0.3315(3) 0.5233(10) 0.134(3) Uani 1 1 d . U . . .
F3 F 0.8947(3) 0.3436(3) 0.5093(13) 0.158(4) Uani 1 1 d . U . . .
F4 F 0.8725(3) 0.3239(5) 0.6911(15) 0.220(6) Uani 1 1 d . U . . .
F5 F 0.8354(3) 0.3654(4) 0.6841(14) 0.185(4) Uani 1 1 d . U . . .
F6 F 0.8570(4) 0.3849(4) 0.5011(17) 0.193(5) Uani 1 1 d . U . . .
P2 P 0.83056(10) 0.46160(10) 0.2508(4) 0.0611(13) Uani 0.666(5) 1 d D U . C 1
F7 F 0.8675(2) 0.4500(3) 0.2312(10) 0.084(3) Uani 0.666(5) 1 d D U . C 1
F8 F 0.7933(2) 0.4725(2) 0.2690(10) 0.073(3) Uani 0.666(5) 1 d D U . C 1
F9 F 0.8173(3) 0.4294(3) 0.1882(16) 0.174(6) Uani 0.666(5) 1 d D U . C 1
F10 F 0.8304(3) 0.4444(4) 0.3771(10) 0.153(5) Uani 0.666(5) 1 d D U . C 1
F11 F 0.8424(3) 0.4947(3) 0.3080(16) 0.162(6) Uani 0.666(5) 1 d D U . C 1
F12 F 0.8301(3) 0.4788(4) 0.1210(11) 0.185(6) Uani 0.666(5) 1 d D U . C 1
P2A P 0.9516(2) 0.3369(3) 0.2434(9) 0.092(3) Uani 0.334(5) 1 d D U . C 2
F7A F 0.9770(5) 0.3380(5) 0.1478(18) 0.117(6) Uani 0.334(5) 1 d D U . C 2
F8A F 0.9264(5) 0.3354(5) 0.3411(18) 0.119(6) Uani 0.334(5) 1 d D U . C 2
F9A F 0.9471(5) 0.3015(4) 0.2271(16) 0.091(5) Uani 0.334(5) 1 d D U . C 2
F10A F 0.9778(5) 0.3312(5) 0.3351(18) 0.121(6) Uani 0.334(5) 1 d D U . C 2
F11A F 0.9550(6) 0.3726(4) 0.2662(19) 0.119(6) Uani 0.334(5) 1 d D U . C 2
F12A F 0.9260(5) 0.3438(5) 0.1518(17) 0.108(6) Uani 0.334(5) 1 d D U . C 2
P3 P 0.68133(10) 0.51904(9) 0.3527(3) 0.0730(9) Uani 1 1 d . U . . .
F13 F 0.6917(2) 0.5499(2) 0.4326(9) 0.113(3) Uani 1 1 d . U . . .
F14 F 0.6754(3) 0.4870(3) 0.2735(9) 0.134(3) Uani 1 1 d . U . . .
F15 F 0.6803(3) 0.4963(2) 0.4693(8) 0.113(3) Uani 1 1 d . U . . .
F16 F 0.7207(2) 0.5125(2) 0.3321(10) 0.108(2) Uani 1 1 d . U . . .
F17 F 0.6818(2) 0.5402(3) 0.2318(8) 0.113(3) Uani 1 1 d . U . . .
F18 F 0.6426(2) 0.5280(2) 0.3688(9) 0.109(3) Uani 1 1 d . U . . .
P4 P 0.6120(2) 0.4085(2) 0.3538(14) 0.176(5) Uani 0.5 1 d D U . D -1
F19 F 0.6425(4) 0.4324(4) 0.336(3) 0.230(10) Uani 0.5 1 d D U . D -1
F20 F 0.5817(3) 0.3846(3) 0.369(2) 0.163(7) Uani 0.5 1 d D U . D -1
F21 F 0.6312(4) 0.3814(4) 0.278(2) 0.166(7) Uani 0.5 1 d D U . D -1
F22 F 0.6281(5) 0.3951(4) 0.4757(18) 0.164(7) Uani 0.5 1 d D U . D -1
F23 F 0.5937(5) 0.4364(4) 0.428(2) 0.193(8) Uani 0.5 1 d D U . D -1
F24 F 0.5973(4) 0.4219(5) 0.2300(18) 0.209(8) Uani 0.5 1 d D U . D -1
N1S N 0.8503(8) 0.4069(6) 0.906(3) 0.246(13) Uani 1 1 d . U . . .
C1S C 0.8289(6) 0.3812(5) 0.915(2) 0.130(6) Uani 1 1 d . U . . .
C2S C 0.8049(5) 0.3570(4) 0.9581(13) 0.101(5) Uani 1 1 d . U . . .
H2SA H 0.812827 0.347012 1.035329 0.152 Uiso 1 1 calc GR . . . .
H2SB H 0.802144 0.339512 0.895638 0.152 Uiso 1 1 calc GR . . . .
H2SC H 0.783455 0.368021 0.972463 0.152 Uiso 1 1 calc GR . . . .
N2S N 0.8050(3) 0.3271(3) 0.2536(11) 0.086(3) Uani 1 1 d . U . . .
C3S C 0.8302(3) 0.3428(4) 0.2455(19) 0.101(6) Uani 1 1 d . U . . .
C4S C 0.8595(4) 0.3631(4) 0.2260(16) 0.096(5) Uani 1 1 d . U . . .
H4SA H 0.855436 0.378542 0.157312 0.144 Uiso 1 1 calc GR . . . .
H4SB H 0.878540 0.348812 0.206233 0.144 Uiso 1 1 calc GR . . . .
H4SC H 0.864290 0.375887 0.301115 0.144 Uiso 1 1 calc GR . . . .
H2S H 0.962(5) 0.136(3) 0.533(13) 0.05(5) Uiso 0.5 1 d D . . . .
H1S H 0.863(3) 0.103(4) 0.38(2) 0.055 Uiso 0.5 1 d DR . . . .
O1S O 0.8441(4) 0.1196(3) 0.3794(15) 0.059(4) Uani 0.5 1 d D U . . .
O2S O 0.9625(6) 0.1544(6) 0.467(2) 0.121(8) Uani 0.5 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
C2 N1 C1 124.2(12) . .
C2 N1 C6 118.0(11) . .
C6 N1 C1 117.5(11) . .
C15 N2 C18 115.7(11) . .
C16 N2 C15 124.8(10) . .
C16 N2 C18 118.9(10) . .
C26 N3 C25 119.9(10) . .
C30 N3 C25 116.2(10) . .
C30 N3 C26 123.6(10) . .
C39 N4 C40 120.0(10) . .
C39 N4 C42 122.4(10) . .
C40 N4 C42 117.4(11) . .
N1 C1 C22 108.1(9) . 8_666
N1 C2 C3 123.5(13) . .
C2 C3 C4 122.3(12) . .
C3 C4 C5 116.2(11) . .
C3 C4 C7 123.6(10) . .
C5 C4 C7 120.1(11) . .
C6 C5 C4 119.8(13) . .
N1 C6 C5 119.5(12) . .
C8 C7 C4 116.7(10) . .
C12 C7 C4 123.0(10) . .
C12 C7 C8 119.9(10) . .
C9 C8 C7 119.5(10) . .
C8 C9 C35 119.2(9) . .
C10 C9 C8 119.6(9) . .
C10 C9 C35 121.3(9) . .
C9 C10 C11 122.3(9) . .
C10 C11 C12 116.8(9) . .
C10 C11 C13 121.6(9) . .
C12 C11 C13 121.3(9) . .
C7 C12 C11 121.8(10) . .
C14 C13 C11 122.3(10) . .
C17 C13 C11 121.7(11) . .
C17 C13 C14 116.0(11) . .
C13 C14 C15 122.6(11) . .
N2 C15 C14 115.6(11) . .
N2 C16 C17 118.5(11) . .
C13 C17 C16 122.4(12) . .
C19 C18 N2 108.1(10) . .
C20 C19 C18 123.1(14) . .
C20 C19 C24 121.0(12) . .
C24 C19 C18 115.5(13) . .
C19 C20 C21 122.1(14) . .
C22 C21 C20 120.7(14) . .
C1 C22 C23 113.3(12) 8_666 .
C21 C22 C1 125.9(13) . 8_666
C21 C22 C23 120.3(12) . .
C24 C23 C22 114.8(13) . .
C19 C24 C23 120.6(13) . .
C46 C25 N3 104.8(9) 8_666 .
N3 C26 C27 118.4(11) . .
C26 C27 C28 120.8(11) . .
C27 C28 C29 117.5(10) . .
C27 C28 C31 119.2(10) . .
C29 C28 C31 123.2(10) . .
C30 C29 C28 119.6(11) . .
N3 C30 C29 119.8(12) . .
C32 C31 C28 123.3(9) . .
C32 C31 C36 118.6(9) . .
C36 C31 C28 118.0(9) . .
C33 C32 C31 123.1(10) . .
C32 C33 C34 117.6(9) . .
C32 C33 C37 121.5(9) . .
C34 C33 C37 120.8(9) . .
C35 C34 C33 121.9(9) . .
C34 C35 C9 119.8(9) . .
C34 C35 C36 117.5(9) . .
C36 C35 C9 122.7(9) . .
C35 C36 C31 121.1(9) . .
C38 C37 C33 123.6(10) . .
C41 C37 C33 122.6(10) . .
C41 C37 C38 113.7(10) . .
C39 C38 C37 121.0(11) . .
N4 C39 C38 121.1(11) . .
C41 C40 N4 122.1(12) . .
C40 C41 C37 121.9(11) . .
C43 C42 N4 105.0(9) . .
C44 C43 C42 119.8(12) . .
C48 C43 C42 121.3(12) . .
C48 C43 C44 118.9(12) . .
C45 C44 C43 120.8(12) . .
C46 C45 C44 119.2(12) . .
C45 C46 C25 121.6(11) . 8_666
C47 C46 C25 118.1(12) . 8_666
C47 C46 C45 120.3(12) . .
C46 C47 C48 120.4(13) . .
C43 C48 C47 120.2(12) . .
C61 N5 C61 133(2) 8_666 .
C61 N5 C62 114.9(18) 8_666 .
C61 N5 C62 114.9(18) . 8_666
C61 N5 C62 106.7(18) . .
C61 N5 C62 106.7(18) 8_666 8_666
C62 N5 C62 54(2) . 8_666
C63 N6 C63 38(3) 8_666 .
C63 N6 C64 127(2) 8_666 8_666
C63 N6 C64 94(2) . 8_666
C63 N6 C64 127(2) . .
C63 N6 C64 94(2) 8_666 .
C64 N6 C64 139(2) 8_666 .
C65 N7 C65 128(2) . 8_666
C65 N7 C66 115.8(11) 8_666 .
C65 N7 C66 115.8(11) . .
C67 N8 C68 133(4) . .
C67 N8 C69 101(4) . .
C68 N8 C69 95.3(18) . .
C50 C49 C54 120.3(14) . .
C50 C49 C61 116.7(15) . .
C54 C49 C61 123.0(17) . .
C49 C50 C51 121.2(14) . .
C52 C51 C50 115.2(14) . .
C51 C52 C55 117.0(13) . .
C53 C52 C51 124.2(13) . .
C53 C52 C55 118.8(13) . .
C52 C53 C52 124.4(17) 8_666 .
C52 C53 C54 117.8(9) 8_666 .
C52 C53 C54 117.8(9) . .
C49 C54 C49 118.2(19) 8_666 .
C49 C54 C53 120.9(10) . .
C49 C54 C53 120.9(10) 8_666 .
C56 C55 C52 121.8(13) . .
C60 C55 C52 117.4(14) . .
C60 C55 C56 120.8(13) . .
C57 C56 C55 118.5(15) . .
C58 C57 C56 123.5(15) . .
C57 C58 C59 119.9(14) . .
C57 C58 C65 125.0(16) . .
C59 C58 C65 114.3(16) . .
C58 C59 C58 123.4(19) 8_666 .
C60 C59 C58 118.3(9) . 8_666
C60 C59 C58 118.3(9) . .
C55 C60 C55 122.6(18) 8_666 .
C55 C60 C59 118.7(9) 8_666 .
C55 C60 C59 118.7(9) . .
O1 C61 N5 127.6(17) . .
O1 C61 C49 119.5(18) . .
N5 C61 C49 111.1(18) . .
C63 C62 N5 95.3(19) . .
C62 C63 N6 103(2) . .
O2 C65 N7 119.9(17) . .
O2 C65 C58 119.2(19) . .
N7 C65 C58 118.6(19) . .
C67 C66 N7 125.9(16) . .
C67 C66 N7 125.9(16) 8_666 .
C67 C66 C67 108(3) 8_666 .
C66 C67 N8 114(3) . .
F1 P1 F4 88.0(11) . .
F1 P1 F6 91.7(11) . .
F2 P1 F1 178.5(11) . .
F2 P1 F3 92.1(7) . .
F2 P1 F4 90.6(8) . .
F2 P1 F5 89.1(7) . .
F2 P1 F6 89.7(8) . .
F3 P1 F1 87.8(9) . .
F3 P1 F4 92.3(9) . .
F3 P1 F5 178.5(9) . .
F3 P1 F6 88.4(8) . .
F4 P1 F6 179.2(11) . .
F5 P1 F1 91.0(8) . .
F5 P1 F4 88.5(10) . .
F5 P1 F6 90.8(9) . .
F7 P2 F8 178.8(6) . .
F9 P2 F7 91.0(6) . .
F9 P2 F8 87.8(5) . .
F9 P2 F12 88.3(8) . .
F10 P2 F7 89.5(6) . .
F10 P2 F8 90.5(6) . .
F10 P2 F9 90.8(8) . .
F10 P2 F11 91.7(8) . .
F10 P2 F12 178.9(9) . .
F11 P2 F7 91.1(6) . .
F11 P2 F8 90.2(6) . .
F11 P2 F9 176.8(8) . .
F11 P2 F12 89.1(8) . .
F12 P2 F7 91.1(6) . .
F12 P2 F8 88.9(6) . .
F7A P2A F8A 178.9(12) . .
F7A P2A F10A 89.0(9) . .
F7A P2A F11A 91.5(9) . .
F8A P2A F10A 90.0(9) . .
F9A P2A F7A 91.6(9) . .
F9A P2A F8A 87.9(9) . .
F9A P2A F10A 91.0(9) . .
F9A P2A F11A 176.9(11) . .
F9A P2A F12A 90.9(9) . .
F11A P2A F8A 89.0(9) . .
F11A P2A F10A 88.4(9) . .
F12A P2A F7A 90.3(9) . .
F12A P2A F8A 90.7(9) . .
F12A P2A F10A 178.0(11) . .
F12A P2A F11A 89.8(9) . .
F13 P3 F16 87.0(5) . .
F13 P3 F18 91.1(6) . .
F14 P3 F13 173.3(6) . .
F14 P3 F16 86.4(6) . .
F14 P3 F18 95.5(6) . .
F15 P3 F13 91.3(6) . .
F15 P3 F14 87.6(6) . .
F15 P3 F16 92.4(5) . .
F15 P3 F17 177.0(6) . .
F15 P3 F18 90.9(5) . .
F17 P3 F13 91.7(6) . .
F17 P3 F14 89.4(6) . .
F17 P3 F16 87.8(5) . .
F17 P3 F18 88.9(5) . .
F18 P3 F16 176.2(5) . .
F19 P4 F21 88.7(8) . .
F19 P4 F22 89.4(9) . .
F20 P4 F19 179.1(11) . .
F20 P4 F21 90.7(8) . .
F20 P4 F22 91.2(9) . .
F20 P4 F23 91.1(8) . .
F20 P4 F24 90.4(9) . .
F22 P4 F21 89.8(8) . .
F23 P4 F19 89.5(9) . .
F23 P4 F21 178.2(10) . .
F23 P4 F22 90.3(8) . .
F24 P4 F19 89.0(9) . .
F24 P4 F21 88.7(9) . .
F24 P4 F22 177.8(10) . .
F24 P4 F23 91.2(8) . .
N1S C1S C2S 164(3) . .
N2S C3S C4S 174.8(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.466(15) .
N1 C2 1.315(16) .
N1 C6 1.395(17) .
N2 C15 1.393(15) .
N2 C16 1.277(15) .
N2 C18 1.502(15) .
N3 C25 1.563(15) .
N3 C26 1.343(15) .
N3 C30 1.304(15) .
N4 C39 1.323(15) .
N4 C40 1.328(15) .
N4 C42 1.576(15) .
C1 C22 1.524(18) 8_666
C2 C3 1.349(17) .
C3 C4 1.354(16) .
C4 C5 1.418(17) .
C4 C7 1.500(16) .
C5 C6 1.407(18) .
C7 C8 1.413(15) .
C7 C12 1.366(15) .
C8 C9 1.406(15) .
C9 C10 1.375(14) .
C9 C35 1.479(14) .
C10 C11 1.411(14) .
C11 C12 1.420(15) .
C11 C13 1.463(15) .
C13 C14 1.381(16) .
C13 C17 1.375(16) .
C14 C15 1.417(16) .
C16 C17 1.418(17) .
C18 C19 1.501(18) .
C19 C20 1.324(18) .
C19 C24 1.422(19) .
C20 C21 1.413(19) .
C21 C22 1.333(18) .
C22 C23 1.540(19) .
C23 C24 1.423(18) .
C25 C46 1.534(17) 8_666
C26 C27 1.368(16) .
C27 C28 1.391(15) .
C28 C29 1.391(16) .
C28 C31 1.518(15) .
C29 C30 1.383(15) .
C31 C32 1.369(15) .
C31 C36 1.409(14) .
C32 C33 1.361(14) .
C33 C34 1.416(14) .
C33 C37 1.439(15) .
C34 C35 1.394(14) .
C35 C36 1.397(14) .
C37 C38 1.419(15) .
C37 C41 1.414(16) .
C38 C39 1.362(15) .
C40 C41 1.324(16) .
C42 C43 1.504(17) .
C43 C44 1.427(17) .
C43 C48 1.323(17) .
C44 C45 1.374(17) .
C45 C46 1.370(17) .
C46 C47 1.360(17) .
C47 C48 1.422(18) .
O1 C61 1.22(2) .
O2 C65 1.26(2) .
N5 C61 1.36(2) 8_666
N5 C61 1.36(2) .
N5 C62 1.632(16) .
N5 C62 1.632(16) 8_666
N6 C63 1.636(16) 8_666
N6 C63 1.636(16) .
N6 C64 1.639(15) 8_666
N6 C64 1.639(15) .
N7 C65 1.32(2) .
N7 C65 1.32(2) 8_666
N7 C66 1.633(17) .
N8 C67 1.634(16) .
N8 C68 1.636(16) .
N8 C69 1.636(16) .
C49 C50 1.37(2) .
C49 C54 1.381(17) .
C49 C61 1.54(2) .
C50 C51 1.468(19) .
C51 C52 1.408(19) .
C52 C53 1.366(15) .
C52 C55 1.529(18) .
C53 C54 1.43(3) .
C55 C56 1.41(2) .
C55 C60 1.412(16) .
C56 C57 1.39(2) .
C57 C58 1.34(2) .
C58 C59 1.449(17) .
C58 C65 1.46(2) .
C59 C60 1.44(3) .
C62 C63 1.51(3) .
C66 C67 1.51(3) 8_666
C66 C67 1.51(3) .
P1 F1 1.612(15) .
P1 F2 1.570(12) .
P1 F3 1.575(13) .
P1 F4 1.616(16) .
P1 F5 1.587(14) .
P1 F6 1.642(16) .
P2 F7 1.568(8) .
P2 F8 1.571(8) .
P2 F9 1.552(9) .
P2 F10 1.531(9) .
P2 F11 1.538(9) .
P2 F12 1.566(9) .
P2A F7A 1.455(14) .
P2A F8A 1.463(14) .
P2A F9A 1.441(14) .
P2A F10A 1.465(14) .
P2A F11A 1.458(14) .
P2A F12A 1.454(14) .
P3 F13 1.568(9) .
P3 F14 1.562(9) .
P3 F15 1.558(9) .
P3 F16 1.615(9) .
P3 F17 1.560(9) .
P3 F18 1.603(9) .
P4 F19 1.565(12) .
P4 F20 1.557(11) .
P4 F21 1.566(11) .
P4 F22 1.566(12) .
P4 F23 1.559(11) .
P4 F24 1.559(12) .
N1S C1S 1.34(3) .
C1S C2S 1.45(3) .
N2S C3S 1.193(17) .
C3S C4S 1.45(2) .
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
N1 C2 C3 C4 -1(2) . .
N2 C16 C17 C13 1.1(18) . .
N2 C18 C19 C20 109.0(13) . .
N2 C18 C19 C24 -77.3(13) . .
N3 C26 C27 C28 2.8(17) . .
N4 C40 C41 C37 2(2) . .
N4 C42 C43 C44 75.5(13) . .
N4 C42 C43 C48 -105.2(13) . .
C1 N1 C2 C3 -167.4(12) . .
C1 N1 C6 C5 170.2(12) . .
C1 C22 C23 C24 -174.3(10) 8_666 .
C2 N1 C1 C22 79.7(16) . 8_666
C2 N1 C6 C5 -4.2(19) . .
C2 C3 C4 C5 -5.8(18) . .
C2 C3 C4 C7 176.7(11) . .
C3 C4 C5 C6 7.7(19) . .
C3 C4 C7 C8 -12.4(16) . .
C3 C4 C7 C12 175.2(11) . .
C4 C5 C6 N1 -3(2) . .
C4 C7 C8 C9 -175.0(9) . .
C4 C7 C12 C11 176.4(10) . .
C5 C4 C7 C8 170.1(11) . .
C5 C4 C7 C12 -2.2(17) . .
C6 N1 C1 C22 -94.2(14) . 8_666
C6 N1 C2 C3 7(2) . .
C7 C4 C5 C6 -174.7(12) . .
C7 C8 C9 C10 1.1(14) . .
C7 C8 C9 C35 179.5(9) . .
C8 C7 C12 C11 4.3(16) . .
C8 C9 C10 C11 -1.7(14) . .
C8 C9 C35 C34 163.5(9) . .
C8 C9 C35 C36 -18.8(14) . .
C9 C10 C11 C12 3.4(14) . .
C9 C10 C11 C13 177.5(9) . .
C9 C35 C36 C31 -178.5(9) . .
C10 C9 C35 C34 -18.1(14) . .
C10 C9 C35 C36 159.6(9) . .
C10 C11 C12 C7 -4.7(15) . .
C10 C11 C13 C14 -13.0(16) . .
C10 C11 C13 C17 166.4(10) . .
C11 C13 C14 C15 -178.7(11) . .
C11 C13 C17 C16 177.8(10) . .
C12 C7 C8 C9 -2.4(16) . .
C12 C11 C13 C14 160.9(10) . .
C12 C11 C13 C17 -19.7(16) . .
C13 C11 C12 C7 -178.8(10) . .
C13 C14 C15 N2 0.6(18) . .
C14 C13 C17 C16 -2.8(17) . .
C15 N2 C16 C17 1.8(18) . .
C15 N2 C18 C19 -80.6(14) . .
C16 N2 C15 C14 -2.6(18) . .
C16 N2 C18 C19 90.5(14) . .
C17 C13 C14 C15 1.9(17) . .
C18 N2 C15 C14 167.9(10) . .
C18 N2 C16 C17 -168.4(10) . .
C18 C19 C20 C21 -179.6(11) . .
C18 C19 C24 C23 178.9(10) . .
C19 C20 C21 C22 -4.5(18) . .
C20 C19 C24 C23 -7.2(17) . .
C20 C21 C22 C1 173.0(11) . 8_666
C20 C21 C22 C23 2.0(17) . .
C21 C22 C23 C24 -2.2(16) . .
C22 C23 C24 C19 4.6(16) . .
C24 C19 C20 C21 7.0(17) . .
C25 N3 C26 C27 -172.4(10) . .
C25 N3 C30 C29 171.1(10) . .
C25 C46 C47 C48 -177.3(10) 8_666 .
C26 N3 C25 C46 93.4(12) . 8_666
C26 N3 C30 C29 -2.7(18) . .
C26 C27 C28 C29 -5.2(16) . .
C26 C27 C28 C31 172.0(10) . .
C27 C28 C29 C30 3.7(17) . .
C27 C28 C31 C32 -19.9(16) . .
C27 C28 C31 C36 157.7(10) . .
C28 C29 C30 N3 0.1(17) . .
C28 C31 C32 C33 178.6(10) . .
C28 C31 C36 C35 -176.4(9) . .
C29 C28 C31 C32 157.1(11) . .
C29 C28 C31 C36 -25.3(16) . .
C30 N3 C25 C46 -80.6(13) . 8_666
C30 N3 C26 C27 1.2(17) . .
C31 C28 C29 C30 -173.3(10) . .
C31 C32 C33 C34 -3.8(16) . .
C31 C32 C33 C37 173.4(10) . .
C32 C31 C36 C35 1.3(15) . .
C32 C33 C34 C35 4.4(15) . .
C32 C33 C37 C38 11.9(17) . .
C32 C33 C37 C41 -163.3(11) . .
C33 C34 C35 C9 175.7(9) . .
C33 C34 C35 C36 -2.1(14) . .
C33 C37 C38 C39 -172.6(10) . .
C33 C37 C41 C40 171.7(12) . .
C34 C33 C37 C38 -171.0(10) . .
C34 C33 C37 C41 13.8(17) . .
C34 C35 C36 C31 -0.7(14) . .
C35 C9 C10 C11 179.9(9) . .
C36 C31 C32 C33 1.0(16) . .
C37 C33 C34 C35 -172.9(10) . .
C37 C38 C39 N4 -0.2(17) . .
C38 C37 C41 C40 -4.0(19) . .
C39 N4 C40 C41 0.9(19) . .
C39 N4 C42 C43 -111.8(12) . .
C40 N4 C39 C38 -1.9(17) . .
C40 N4 C42 C43 63.4(14) . .
C41 C37 C38 C39 3.0(16) . .
C42 N4 C39 C38 173.2(10) . .
C42 N4 C40 C41 -174.4(12) . .
C42 C43 C44 C45 -178.4(10) . .
C42 C43 C48 C47 176.5(10) . .
C43 C44 C45 C46 2.5(17) . .
C44 C43 C48 C47 -4.1(17) . .
C44 C45 C46 C25 175.5(10) . 8_666
C44 C45 C46 C47 -5.2(17) . .
C45 C46 C47 C48 3.3(17) . .
C46 C47 C48 C43 1.5(18) . .
C48 C43 C44 C45 2.2(17) . .
N5 C62 C63 N6 179(4) . .
N7 C66 C67 N8 -17(5) . .
C49 C50 C51 C52 -3.3(18) . .
C50 C49 C54 C49 -178.4(15) . 8_666
C50 C49 C54 C53 1.6(15) . .
C50 C49 C61 O1 9(3) . .
C50 C49 C61 N5 175.3(13) . .
C50 C51 C52 C53 -2.0(17) . .
C50 C51 C52 C55 -179.0(10) . .
C51 C52 C53 C52 -173.2(13) . 8_666
C51 C52 C53 C54 6.8(13) . .
C51 C52 C55 C56 -11.5(19) . .
C51 C52 C55 C60 169.7(10) . .
C52 C53 C54 C49 -6.6(9) . .
C52 C53 C54 C49 173.4(9) 8_666 .
C52 C53 C54 C49 -6.6(9) 8_666 8_666
C52 C53 C54 C49 173.4(9) . 8_666
C52 C55 C56 C57 178.7(12) . .
C52 C55 C60 C55 3.6(7) . 8_666
C52 C55 C60 C59 -176.4(7) . .
C53 C52 C55 C56 171.4(11) . .
C53 C52 C55 C60 -7.5(15) . .
C54 C49 C50 C51 3.4(19) . .
C54 C49 C61 O1 -172.3(16) . .
C54 C49 C61 N5 -7(2) . .
C55 C52 C53 C52 3.7(8) . 8_666
C55 C52 C53 C54 -176.3(8) . .
C55 C56 C57 C58 -3(2) . .
C56 C55 C60 C55 -175.3(15) . 8_666
C56 C55 C60 C59 4.7(15) . .
C56 C57 C58 C59 5(2) . .
C56 C57 C58 C65 174.5(17) . .
C57 C58 C59 C58 177.3(17) . 8_666
C57 C58 C59 C60 -2.7(17) . .
C57 C58 C65 O2 13(3) . .
C57 C58 C65 N7 175.9(16) . .
C58 C59 C60 C55 177.8(10) . 8_666
C58 C59 C60 C55 177.8(10) 8_666 .
C58 C59 C60 C55 -2.2(10) . .
C58 C59 C60 C55 -2.2(10) 8_666 8_666
C59 C58 C65 O2 -176.9(17) . .
C59 C58 C65 N7 -14(2) . .
C60 C55 C56 C57 -2(2) . .
C61 N5 C61 O1 167(3) 8_666 .
C61 N5 C61 C49 2.9(10) 8_666 .
C61 N5 C62 C63 108(4) . .
C61 N5 C62 C63 -94(4) 8_666 .
C61 C49 C50 C51 -178.3(13) . .
C61 C49 C54 C49 3.4(12) . 8_666
C61 C49 C54 C53 -176.6(12) . .
C62 N5 C61 O1 -41(3) . .
C62 N5 C61 O1 17(3) 8_666 .
C62 N5 C61 C49 155.1(18) . .
C62 N5 C61 C49 -147.5(18) 8_666 .
C62 N5 C62 C63 -1(4) 8_666 .
C63 N6 C63 C62 -1(5) 8_666 .
C64 N6 C63 C62 151(4) 8_666 .
C64 N6 C63 C62 -36(6) . .
C65 N7 C65 O2 170(2) 8_666 .
C65 N7 C65 C58 7.7(14) 8_666 .
C65 N7 C66 C67 -101(3) 8_666 .
C65 N7 C66 C67 79(3) . .
C65 N7 C66 C67 79(3) 8_666 8_666
C65 N7 C66 C67 -101(3) . 8_666
C65 C58 C59 C58 6.9(12) . 8_666
C65 C58 C59 C60 -173.1(12) . .
C66 N7 C65 O2 -10(2) . .
C66 N7 C65 C58 -172.3(14) . .
C67 C66 C67 N8 163(5) 8_666 .
C68 N8 C67 C66 55(6) . .
C69 N8 C67 C66 163(4) . .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.000 -0.183 833.1 202.1
2 0.000 0.500 -0.406 1204.1 311.0
3 0.500 0.500 -0.010 833.1 202.1
4 0.500 0.000 -0.875 1204.1 310.9
