# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_171217_ys_1-2
_database_code_depnum_ccdc_archive 'CCDC 1906673'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_vrf_PLAT416_171217_ys_1-2       
;
PLOBLEM: Short Intra D-H..H-D H19 ..H21 1.83 Ang.  Short Intra D-H..H-D H17 ..H22 1.76 Ang.  Short Intra D-H..H-D H18 ..H22 1.82 Ang. 
RESPONSE: Short distances between H19 and H21, H17 and H22, and H18 and H22 are due to inner 3H of porphyrin.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
'C38 H11 F15 N4 O, C0.23 H0.23 Cl0.68, C0.76 H7.79'
_chemical_formula_sum            'C38.99 H13.02 Cl0.68 F15 N4 O'
_chemical_formula_weight         862.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1723 0.1934 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.734(2)
_cell_length_b                   15.683(3)
_cell_length_c                   18.431(3)
_cell_angle_alpha                84.631(3)
_cell_angle_beta                 80.158(3)
_cell_angle_gamma                81.477(3)
_cell_volume                     3297.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    27892
_cell_measurement_theta_min      1.238
_cell_measurement_theta_max      28.139

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             1718
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.001
_exptl_absorpt_coefficient_mu    0.277
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.7829
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'

_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            27892
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.238
_diffrn_reflns_theta_max         28.139
_diffrn_reflns_theta_full        28.017
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             11841
_reflns_number_gt                7177
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1314P)²+1.2219P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0187(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11841
_refine_ls_number_parameters     1112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.2443
_refine_ls_wR_factor_gt          0.1810
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6971(4) 0.6036(3) -0.0596(2) 0.0341(10) Uani 1 1 d . . . . .
C2 C 0.7105(4) 0.6704(3) -0.0147(2) 0.0299(10) Uani 1 1 d . . . . .
C3 C 0.6935(4) 0.7579(3) -0.0365(2) 0.0359(11) Uani 1 1 d . . . . .
H1 H 0.6799 0.7821 -0.0839 0.043 Uiso 1 1 calc R U . . .
C4 C 0.6996(4) 0.8037(3) 0.0224(2) 0.0364(11) Uani 1 1 d . . . . .
H2 H 0.6900 0.8648 0.0233 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7227(4) 0.7433(3) 0.0811(2) 0.0298(10) Uani 1 1 d . . . . .
C6 C 0.7452(4) 0.7593(3) 0.1510(2) 0.0286(9) Uani 1 1 d . . . . .
C7 C 0.7631(4) 0.6982(3) 0.2091(2) 0.0298(10) Uani 1 1 d . . . . .
C8 C 0.8033(4) 0.7163(3) 0.2753(2) 0.0344(11) Uani 1 1 d . . . . .
H3 H 0.8160 0.7712 0.2878 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8193(4) 0.6418(3) 0.3155(2) 0.0324(10) Uani 1 1 d . . . . .
H4 H 0.8465 0.6328 0.3616 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7868(4) 0.5768(3) 0.2744(2) 0.0287(9) Uani 1 1 d . . . . .
C11 C 0.7918(4) 0.4887(3) 0.2995(2) 0.0292(10) Uani 1 1 d . . . . .
C12 C 0.7617(3) 0.4244(3) 0.2623(2) 0.0280(9) Uani 1 1 d . . . . .
C13 C 0.7654(4) 0.3348(3) 0.2851(2) 0.0359(11) Uani 1 1 d . . . . .
H5 H 0.7904 0.3075 0.3290 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7275(4) 0.2954(3) 0.2339(2) 0.0358(11) Uani 1 1 d . . . . .
H6 H 0.7198 0.2358 0.2360 0.043 Uiso 1 1 calc R U . . .
C15 C 0.7007(4) 0.3578(3) 0.1759(2) 0.0340(10) Uani 1 1 d . . . . .
C16 C 0.6660(4) 0.3429(3) 0.1118(2) 0.0324(10) Uani 1 1 d . . . . .
C17 C 0.6562(4) 0.4023(3) 0.0495(2) 0.0330(10) Uani 1 1 d . . . . .
C18 C 0.5998(4) 0.3948(3) -0.0100(2) 0.0319(10) Uani 1 1 d . . . . .
H7 H 0.5590 0.3485 -0.0158 0.038 Uiso 1 1 calc R U . . .
C19 C 0.6136(3) 0.4649(3) -0.0581(2) 0.0328(10) Uani 1 1 d . . . . .
H8 H 0.5845 0.4759 -0.1035 0.039 Uiso 1 1 calc R U . . .
C20 C 0.6774(4) 0.5178(3) -0.0294(2) 0.0318(10) Uani 1 1 d . . . . .
C21 C 0.7558(4) 0.8504(3) 0.1608(3) 0.0363(11) Uani 1 1 d . . . . .
C22 C 0.6854(5) 0.8971(3) 0.2136(3) 0.0436(12) Uani 1 1 d . . . . .
C23 C 0.6964(5) 0.9835(3) 0.2210(3) 0.0562(16) Uani 1 1 d . . . . .
C24 C 0.7790(6) 1.0213(3) 0.1738(4) 0.0606(17) Uani 1 1 d . . . . .
C25 C 0.8505(5) 0.9768(3) 0.1209(3) 0.0552(15) Uani 1 1 d . . . . .
C26 C 0.8403(4) 0.8926(3) 0.1150(3) 0.0399(12) Uani 1 1 d . . . . .
C27 C 0.8386(4) 0.4594(3) 0.3689(2) 0.0283(9) Uani 1 1 d . . . . .
C28 C 0.7701(3) 0.4349(3) 0.4336(2) 0.0304(10) Uani 1 1 d . . . . .
C29 C 0.8139(4) 0.4075(3) 0.4977(2) 0.0380(11) Uani 1 1 d . . . . .
C30 C 0.9290(4) 0.4031(3) 0.4982(2) 0.0390(11) Uani 1 1 d . . . . .
C31 C 1.0015(4) 0.4269(3) 0.4352(2) 0.0348(10) Uani 1 1 d . . . . .
C32 C 0.9548(4) 0.4540(3) 0.3724(2) 0.0320(10) Uani 1 1 d . . . . .
C33 C 0.6338(4) 0.2567(3) 0.1048(2) 0.0369(11) Uani 1 1 d . . . . .
C34 C 0.5430(4) 0.2250(3) 0.1510(2) 0.0416(12) Uani 1 1 d . . . . .
C35 C 0.5079(5) 0.1468(3) 0.1435(3) 0.0498(14) Uani 1 1 d . . . . .
C36 C 0.5633(5) 0.0988(3) 0.0866(3) 0.0551(15) Uani 1 1 d . . . . .
C37 C 0.6551(5) 0.1271(3) 0.0392(3) 0.0521(14) Uani 1 1 d . . . . .
C38 C 0.6893(4) 0.2052(3) 0.0489(3) 0.0416(12) Uani 1 1 d . . . . .
C39 C 1.0155(4) 0.5081(3) 0.8940(2) 0.0288(9) Uani 1 1 d . . . . .
C40 C 0.9518(3) 0.4480(3) 0.8684(2) 0.0281(9) Uani 1 1 d . . . . .
C41 C 0.9748(4) 0.3582(3) 0.8809(3) 0.0349(10) Uani 1 1 d . . . . .
H9 H 1.0319 0.3276 0.9080 0.042 Uiso 1 1 calc R U . . .
C42 C 0.9003(4) 0.3226(3) 0.8471(2) 0.0366(11) Uani 1 1 d . . . . .
H10 H 0.8964 0.2627 0.8459 0.044 Uiso 1 1 calc R U . . .
C43 C 0.8302(4) 0.3911(3) 0.8144(2) 0.0307(10) Uani 1 1 d . . . . .
C44 C 0.7399(4) 0.3848(3) 0.7748(2) 0.0325(10) Uani 1 1 d . . . . .
C45 C 0.6781(4) 0.4496(3) 0.7373(2) 0.0326(10) Uani 1 1 d . . . . .
C46 C 0.5834(4) 0.4432(3) 0.7009(3) 0.0399(12) Uani 1 1 d . . . . .
H11 H 0.5478 0.3927 0.7006 0.048 Uiso 1 1 calc R U . . .
C47 C 0.5517(4) 0.5212(3) 0.6662(3) 0.0417(12) Uani 1 1 d . . . . .
H12 H 0.4895 0.5351 0.6385 0.050 Uiso 1 1 calc R U . . .
C48 C 0.6287(4) 0.5788(3) 0.6791(3) 0.0372(11) Uani 1 1 d . . . . .
C49 C 0.6335(4) 0.6631(3) 0.6485(3) 0.0411(12) Uani 1 1 d . . . . .
C50 C 0.7045(4) 0.7202(3) 0.6661(3) 0.0449(13) Uani 1 1 d . . . . .
C51 C 0.7147(4) 0.8049(3) 0.6317(3) 0.0426(12) Uani 1 1 d . . . . .
H13 H 0.6778 0.8310 0.5915 0.051 Uiso 1 1 calc R U . . .
C52 C 0.7851(4) 0.8408(3) 0.6661(3) 0.0430(12) Uani 1 1 d . . . . .
H14 H 0.8069 0.8972 0.6550 0.052 Uiso 1 1 calc R U . . .
C53 C 0.8220(5) 0.7792(3) 0.7227(3) 0.0524(15) Uani 1 1 d . . . . .
C54 C 0.8934(4) 0.7911(3) 0.7719(3) 0.0459(13) Uani 1 1 d . . . . .
C55 C 0.9382(4) 0.7299(3) 0.8234(3) 0.0373(11) Uani 1 1 d . . . . .
C56 C 0.9989(4) 0.7420(3) 0.8798(3) 0.0376(11) Uani 1 1 d . . . . .
H15 H 1.0149 0.7959 0.8924 0.045 Uiso 1 1 calc R U . . .
C57 C 1.0312(4) 0.6630(3) 0.9134(2) 0.0349(10) Uani 1 1 d . . . . .
H16 H 1.0729 0.6527 0.9539 0.042 Uiso 1 1 calc R U . . .
C58 C 0.9930(3) 0.6002(3) 0.8788(2) 0.0294(10) Uani 1 1 d . . . . .
C59 C 0.7143(4) 0.2952(3) 0.7681(2) 0.0330(10) Uani 1 1 d . . . . .
C60 C 0.6275(4) 0.2578(3) 0.8144(2) 0.0340(10) Uani 1 1 d . . . . .
C61 C 0.6055(4) 0.1760(3) 0.8083(2) 0.0362(11) Uani 1 1 d . . . . .
C62 C 0.6690(4) 0.1287(3) 0.7532(3) 0.0369(11) Uani 1 1 d . . . . .
C63 C 0.7553(4) 0.1633(3) 0.7056(2) 0.0321(10) Uani 1 1 d . . . . .
C64 C 0.7778(4) 0.2450(3) 0.7141(2) 0.0343(10) Uani 1 1 d . . . . .
C65 C 0.5625(4) 0.6934(3) 0.5897(3) 0.0373(11) Uani 1 1 d . . . . .
C66 C 0.4711(4) 0.7600(3) 0.5980(3) 0.0372(11) Uani 1 1 d . . . . .
C67 C 0.4041(4) 0.7859(3) 0.5437(3) 0.0413(12) Uani 1 1 d . . . . .
C68 C 0.4286(4) 0.7472(3) 0.4784(3) 0.0473(13) Uani 1 1 d . . . . .
C69 C 0.5199(4) 0.6834(3) 0.4671(3) 0.0465(13) Uani 1 1 d . . . . .
C70 C 0.5835(4) 0.6571(3) 0.5227(3) 0.0406(12) Uani 1 1 d . . . . .
C71 C 0.9309(4) 0.8789(3) 0.7660(3) 0.0472(13) Uani 1 1 d . . . . .
C72 C 0.8798(4) 0.9419(3) 0.8126(3) 0.0446(13) Uani 1 1 d . . . . .
C73 C 0.9143(5) 1.0230(3) 0.8046(3) 0.0489(14) Uani 1 1 d . . . . .
C74 C 1.0003(5) 1.0427(3) 0.7494(3) 0.0511(14) Uani 1 1 d . . . . .
C75 C 1.0548(5) 0.9814(3) 0.7019(4) 0.0588(15) Uani 1 1 d . . . . .
C76 C 1.0203(5) 0.9011(3) 0.7121(4) 0.0573(15) Uani 1 1 d . . . . .
N1 N 0.7259(3) 0.6630(2) 0.05677(18) 0.0294(8) Uani 1 1 d . . . . .
H19 H 0.7365 0.6139 0.0836 0.035 Uiso 1 1 calc R U . . .
N2 N 0.7533(3) 0.6113(2) 0.21094(18) 0.0284(8) Uani 1 1 d . . . . .
N3 N 0.7213(3) 0.4368(2) 0.19709(18) 0.0300(8) Uani 1 1 d . . . . .
H20 H 0.7097 0.4869 0.1718 0.036 Uiso 1 1 calc R U . . .
N4 N 0.7021(3) 0.4793(2) 0.03736(19) 0.0311(8) Uani 1 1 d . . . . .
H21 H 0.7405 0.5002 0.0671 0.037 Uiso 1 1 calc R U . . .
N5 N 0.8635(3) 0.4681(2) 0.82813(18) 0.0294(8) Uani 1 1 d . . . . .
H22 H 0.8333 0.5203 0.8136 0.035 Uiso 1 1 calc R U . . .
N6 N 0.6996(3) 0.5349(2) 0.72396(19) 0.0326(9) Uani 1 1 d . . . . .
H17 H 0.7522 0.5571 0.7423 0.039 Uiso 1 1 calc R U . . .
N7 N 0.7714(4) 0.7042(2) 0.7204(3) 0.0598(14) Uani 1 1 d . . . . .
N8 N 0.9363(3) 0.6427(2) 0.8245(2) 0.0338(9) Uani 1 1 d . . . . .
H18 H 0.9031 0.6176 0.7944 0.041 Uiso 1 1 calc R U . . .
O1 O 0.6914(3) 0.6218(2) -0.12668(16) 0.0448(8) Uani 1 1 d . . . . .
O2 O 1.0936(2) 0.47917(18) 0.93175(15) 0.0321(7) Uani 1 1 d . . . . .
F1 F 0.6021(2) 0.86135(19) 0.25953(15) 0.0505(7) Uani 1 1 d . . . . .
F2 F 0.6255(3) 1.0267(2) 0.2732(2) 0.0780(11) Uani 1 1 d . . . . .
F3 F 0.7913(4) 1.10387(18) 0.1823(2) 0.0859(13) Uani 1 1 d . . . . .
F4 F 0.9321(3) 1.01681(19) 0.07566(19) 0.0707(10) Uani 1 1 d . . . . .
F5 F 0.9164(2) 0.85046(18) 0.06406(15) 0.0486(7) Uani 1 1 d . . . . .
F6 F 0.6550(2) 0.43789(18) 0.43628(14) 0.0431(7) Uani 1 1 d . . . . .
F7 F 0.7423(2) 0.3856(2) 0.55886(14) 0.0556(8) Uani 1 1 d . . . . .
F8 F 0.9742(2) 0.3786(2) 0.56007(14) 0.0531(8) Uani 1 1 d . . . . .
F9 F 1.1163(2) 0.4217(2) 0.43521(14) 0.0505(8) Uani 1 1 d . . . . .
F10 F 1.0284(2) 0.47618(18) 0.31192(13) 0.0441(7) Uani 1 1 d . . . . .
F11 F 0.4840(2) 0.27116(19) 0.20615(15) 0.0506(8) Uani 1 1 d . . . . .
F12 F 0.4189(3) 0.1195(2) 0.19033(17) 0.0692(10) Uani 1 1 d . . . . .
F13 F 0.5307(3) 0.02271(19) 0.07869(19) 0.0758(11) Uani 1 1 d . . . . .
F14 F 0.7109(3) 0.07874(18) -0.01509(18) 0.0720(10) Uani 1 1 d . . . . .
F15 F 0.7807(3) 0.22943(17) 0.00228(15) 0.0522(8) Uani 1 1 d . . . . .
F16 F 0.5592(2) 0.30344(17) 0.86700(14) 0.0451(7) Uani 1 1 d . . . . .
F17 F 0.5229(2) 0.14164(17) 0.85654(14) 0.0448(7) Uani 1 1 d . . . . .
F18 F 0.6492(2) 0.04794(16) 0.74685(15) 0.0471(7) Uani 1 1 d . . . . .
F19 F 0.8189(2) 0.11675(16) 0.65137(14) 0.0437(7) Uani 1 1 d . . . . .
F20 F 0.8661(2) 0.27527(16) 0.66789(13) 0.0414(7) Uani 1 1 d . . . . .
F21 F 0.4448(2) 0.80160(16) 0.65926(14) 0.0417(7) Uani 1 1 d . . . . .
F22 F 0.3153(2) 0.84909(18) 0.55458(17) 0.0570(8) Uani 1 1 d . . . . .
F23 F 0.3661(3) 0.7729(2) 0.42438(17) 0.0654(9) Uani 1 1 d . . . . .
F24 F 0.5462(3) 0.6444(2) 0.40363(16) 0.0620(9) Uani 1 1 d . . . . .
F25 F 0.6733(2) 0.59375(18) 0.50920(17) 0.0549(8) Uani 1 1 d . . . . .
F26 F 0.7938(3) 0.92551(17) 0.86711(17) 0.0544(8) Uani 1 1 d . . . . .
F27 F 0.8634(3) 1.08281(17) 0.85127(17) 0.0566(8) Uani 1 1 d . . . . .
F28 F 1.0317(3) 1.12213(17) 0.74072(18) 0.0602(9) Uani 1 1 d . . . . .
F29 F 1.1423(3) 0.9999(2) 0.6494(2) 0.0858(12) Uani 1 1 d . . . . .
F30 F 1.0756(3) 0.8419(2) 0.6650(2) 0.0777(11) Uani 1 1 d . . . . .
C82 C 0.0480(11) 1.1106(7) 0.5153(7) 0.068(4) Uani 0.513(9) 1 d . . P . .
H23 H 0.0373 1.1053 0.5699 0.081 Uiso 0.513(9) 1 calc R U P . .
H24 H 0.1326 1.0994 0.4962 0.081 Uiso 0.513(9) 1 calc R U P . .
C83 C 0.0002(11) 1.1970(7) 0.4894(7) 0.072(4) Uani 0.513(9) 1 d . . P . .
H25 H -0.0831 1.2078 0.5094 0.108 Uiso 0.513(9) 1 calc R U P . .
H26 H 0.0103 1.2013 0.4353 0.108 Uiso 0.513(9) 1 calc R U P . .
H27 H 0.0411 1.2399 0.5059 0.108 Uiso 0.513(9) 1 calc R U P . .
C84 C -0.0166(12) 1.0459(7) 0.4873(7) 0.071(4) Uani 0.513(9) 1 d . . P . .
H28 H -0.1014 1.0617 0.5035 0.086 Uiso 0.513(9) 1 calc R U P . .
H29 H -0.0022 1.0511 0.4327 0.086 Uiso 0.513(9) 1 calc R U P . .
C85 C 0.5681(16) 0.9707(7) 0.4458(7) 0.064(4) Uani 0.451(3) 1 d . . P A -1
H85 H 0.6104 1.0178 0.4184 0.077 Uiso 0.451(3) 1 calc R U P A -1
Cl1 Cl 0.6569(3) 0.87293(19) 0.43071(16) 0.0514(9) Uani 0.451(3) 1 d . . P A -1
Cl2 Cl 0.4378(3) 0.9717(2) 0.4090(2) 0.0719(11) Uani 0.451(3) 1 d . . P A -1
Cl3 Cl 0.5381(4) 0.9916(2) 0.53768(19) 0.0785(13) Uani 0.451(3) 1 d . . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.254(5) . ?
C1 C2 1.436(6) . ?
C1 C20 1.442(6) . ?
C2 N1 1.353(5) . ?
C2 C3 1.389(6) . ?
C3 C4 1.374(6) . ?
C3 H1 0.9500 . ?
C4 C5 1.404(6) . ?
C4 H2 0.9500 . ?
C5 N1 1.370(5) . ?
C5 C6 1.410(6) . ?
C6 C7 1.392(6) . ?
C6 C21 1.481(6) . ?
C7 N2 1.382(5) . ?
C7 C8 1.447(6) . ?
C8 C9 1.330(6) . ?
C8 H3 0.9500 . ?
C9 C10 1.454(5) . ?
C9 H4 0.9500 . ?
C10 N2 1.338(5) . ?
C10 C11 1.412(6) . ?
C11 C12 1.387(5) . ?
C11 C27 1.486(6) . ?
C12 N3 1.354(5) . ?
C12 C13 1.426(6) . ?
C13 C14 1.343(6) . ?
C13 H5 0.9500 . ?
C14 C15 1.423(6) . ?
C14 H6 0.9500 . ?
C15 C16 1.364(6) . ?
C15 N3 1.399(5) . ?
C16 C17 1.418(6) . ?
C16 C33 1.479(6) . ?
C17 N4 1.379(5) . ?
C17 C18 1.396(6) . ?
C18 C19 1.357(6) . ?
C18 H7 0.9500 . ?
C19 C20 1.389(6) . ?
C19 H8 0.9500 . ?
C20 N4 1.377(5) . ?
C21 C22 1.359(7) . ?
C21 C26 1.391(7) . ?
C22 F1 1.334(6) . ?
C22 C23 1.400(7) . ?
C23 F2 1.326(6) . ?
C23 C24 1.354(9) . ?
C24 C25 1.347(9) . ?
C24 F3 1.350(5) . ?
C25 F4 1.346(6) . ?
C25 C26 1.361(7) . ?
C26 F5 1.331(6) . ?
C27 C32 1.365(6) . ?
C27 C28 1.375(6) . ?
C28 F6 1.337(4) . ?
C28 C29 1.375(6) . ?
C29 F7 1.337(5) . ?
C29 C30 1.344(6) . ?
C30 F8 1.339(5) . ?
C30 C31 1.375(6) . ?
C31 F9 1.337(5) . ?
C31 C32 1.370(6) . ?
C32 F10 1.341(5) . ?
C33 C34 1.369(6) . ?
C33 C38 1.381(7) . ?
C34 F11 1.336(6) . ?
C34 C35 1.376(6) . ?
C35 F12 1.332(6) . ?
C35 C36 1.364(8) . ?
C36 F13 1.334(5) . ?
C36 C37 1.367(8) . ?
C37 F14 1.332(6) . ?
C37 C38 1.380(6) . ?
C38 F15 1.333(5) . ?
C39 O2 1.251(5) . ?
C39 C58 1.440(6) . ?
C39 C40 1.442(5) . ?
C40 N5 1.359(5) . ?
C40 C41 1.399(6) . ?
C41 C42 1.365(6) . ?
C41 H9 0.9500 . ?
C42 C43 1.408(6) . ?
C42 H10 0.9500 . ?
C43 N5 1.380(5) . ?
C43 C44 1.404(6) . ?
C44 C45 1.363(6) . ?
C44 C59 1.501(6) . ?
C45 N6 1.389(5) . ?
C45 C46 1.412(6) . ?
C46 C47 1.357(7) . ?
C46 H11 0.9500 . ?
C47 C48 1.428(6) . ?
C47 H12 0.9500 . ?
C48 N6 1.345(6) . ?
C48 C49 1.393(7) . ?
C49 C50 1.403(6) . ?
C49 C65 1.481(6) . ?
C50 N7 1.359(6) . ?
C50 C51 1.430(7) . ?
C51 C52 1.337(6) . ?
C51 H13 0.9500 . ?
C52 C53 1.433(7) . ?
C52 H14 0.9500 . ?
C53 C54 1.377(6) . ?
C53 N7 1.400(6) . ?
C54 C55 1.397(6) . ?
C54 C71 1.496(6) . ?
C55 N8 1.369(5) . ?
C55 C56 1.397(6) . ?
C56 C57 1.363(6) . ?
C56 H15 0.9500 . ?
C57 C58 1.386(6) . ?
C57 H16 0.9500 . ?
C58 N8 1.364(5) . ?
C59 C64 1.373(6) . ?
C59 C60 1.377(6) . ?
C60 F16 1.339(5) . ?
C60 C61 1.363(6) . ?
C61 F17 1.339(5) . ?
C61 C62 1.362(6) . ?
C62 F18 1.340(5) . ?
C62 C63 1.363(6) . ?
C63 F19 1.345(5) . ?
C63 C64 1.374(6) . ?
C64 F20 1.339(5) . ?
C65 C70 1.377(6) . ?
C65 C66 1.380(6) . ?
C66 F21 1.325(5) . ?
C66 C67 1.371(6) . ?
C67 F22 1.329(5) . ?
C67 C68 1.367(7) . ?
C68 F23 1.333(5) . ?
C68 C69 1.356(7) . ?
C69 F24 1.338(5) . ?
C69 C70 1.367(7) . ?
C70 F25 1.343(5) . ?
C71 C72 1.370(7) . ?
C71 C76 1.378(8) . ?
C72 F26 1.333(6) . ?
C72 C73 1.379(6) . ?
C73 F27 1.336(6) . ?
C73 C74 1.354(8) . ?
C74 F28 1.339(5) . ?
C74 C75 1.372(8) . ?
C75 F29 1.331(7) . ?
C75 C76 1.367(7) . ?
C76 F30 1.347(6) . ?
N1 H19 0.8800 . ?
N3 H20 0.8800 . ?
N4 H21 0.8800 . ?
N5 H22 0.8800 . ?
N6 H17 0.8800 . ?
N8 H18 0.8800 . ?
C82 C83 1.457(14) . ?
C82 C84 1.528(17) . ?
C82 H23 0.9900 . ?
C82 H24 0.9900 . ?
C83 H25 0.9800 . ?
C83 H26 0.9800 . ?
C83 H27 0.9800 . ?
C84 C84 1.49(2) 2_576 ?
C84 H28 0.9900 . ?
C84 H29 0.9900 . ?
C85 Cl3 1.722(13) . ?
C85 Cl1 1.739(15) . ?
C85 Cl2 1.773(15) . ?
C85 H85 1.0000 . ?

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
O1 C1 C2 119.2(4) . . ?
O1 C1 C20 117.7(4) . . ?
C2 C1 C20 122.8(4) . . ?
N1 C2 C3 107.6(4) . . ?
N1 C2 C1 128.3(4) . . ?
C3 C2 C1 123.7(4) . . ?
C4 C3 C2 108.4(4) . . ?
C4 C3 H1 125.8 . . ?
C2 C3 H1 125.8 . . ?
C3 C4 C5 107.2(4) . . ?
C3 C4 H2 126.4 . . ?
C5 C4 H2 126.4 . . ?
N1 C5 C4 107.0(4) . . ?
N1 C5 C6 124.9(4) . . ?
C4 C5 C6 128.0(4) . . ?
C7 C6 C5 126.6(4) . . ?
C7 C6 C21 117.9(4) . . ?
C5 C6 C21 115.5(4) . . ?
N2 C7 C6 126.1(4) . . ?
N2 C7 C8 109.8(4) . . ?
C6 C7 C8 124.0(4) . . ?
C9 C8 C7 107.2(4) . . ?
C9 C8 H3 126.4 . . ?
C7 C8 H3 126.4 . . ?
C8 C9 C10 106.2(4) . . ?
C8 C9 H4 126.9 . . ?
C10 C9 H4 126.9 . . ?
N2 C10 C11 125.3(4) . . ?
N2 C10 C9 111.5(4) . . ?
C11 C10 C9 123.1(4) . . ?
C12 C11 C10 125.3(4) . . ?
C12 C11 C27 115.8(4) . . ?
C10 C11 C27 118.8(3) . . ?
N3 C12 C11 125.3(4) . . ?
N3 C12 C13 107.3(3) . . ?
C11 C12 C13 127.4(4) . . ?
C14 C13 C12 108.3(4) . . ?
C14 C13 H5 125.8 . . ?
C12 C13 H5 125.8 . . ?
C13 C14 C15 108.8(4) . . ?
C13 C14 H6 125.6 . . ?
C15 C14 H6 125.6 . . ?
C16 C15 N3 127.2(4) . . ?
C16 C15 C14 126.9(4) . . ?
N3 C15 C14 105.8(3) . . ?
C15 C16 C17 126.8(4) . . ?
C15 C16 C33 118.3(4) . . ?
C17 C16 C33 114.9(4) . . ?
N4 C17 C18 107.4(4) . . ?
N4 C17 C16 125.1(4) . . ?
C18 C17 C16 127.5(4) . . ?
C19 C18 C17 108.2(4) . . ?
C19 C18 H7 125.9 . . ?
C17 C18 H7 125.9 . . ?
C18 C19 C20 108.4(4) . . ?
C18 C19 H8 125.8 . . ?
C20 C19 H8 125.8 . . ?
N4 C20 C19 107.8(4) . . ?
N4 C20 C1 126.6(4) . . ?
C19 C20 C1 125.0(4) . . ?
C22 C21 C26 116.4(4) . . ?
C22 C21 C6 123.0(4) . . ?
C26 C21 C6 120.6(4) . . ?
F1 C22 C21 120.0(4) . . ?
F1 C22 C23 118.1(5) . . ?
C21 C22 C23 121.8(5) . . ?
F2 C23 C24 121.4(5) . . ?
F2 C23 C22 119.7(6) . . ?
C24 C23 C22 118.9(5) . . ?
C25 C24 F3 120.3(6) . . ?
C25 C24 C23 121.0(5) . . ?
F3 C24 C23 118.7(6) . . ?
F4 C25 C24 118.9(5) . . ?
F4 C25 C26 121.5(6) . . ?
C24 C25 C26 119.6(5) . . ?
F5 C26 C25 117.3(5) . . ?
F5 C26 C21 120.4(4) . . ?
C25 C26 C21 122.3(5) . . ?
C32 C27 C28 115.1(4) . . ?
C32 C27 C11 121.5(4) . . ?
C28 C27 C11 123.3(4) . . ?
F6 C28 C29 116.9(4) . . ?
F6 C28 C27 120.0(4) . . ?
C29 C28 C27 123.1(4) . . ?
F7 C29 C30 120.4(4) . . ?
F7 C29 C28 120.1(4) . . ?
C30 C29 C28 119.5(4) . . ?
F8 C30 C29 121.1(4) . . ?
F8 C30 C31 119.0(4) . . ?
C29 C30 C31 119.8(4) . . ?
F9 C31 C32 120.9(4) . . ?
F9 C31 C30 120.1(4) . . ?
C32 C31 C30 119.0(4) . . ?
F10 C32 C27 119.4(4) . . ?
F10 C32 C31 117.3(4) . . ?
C27 C32 C31 123.4(4) . . ?
C34 C33 C38 115.8(4) . . ?
C34 C33 C16 122.0(4) . . ?
C38 C33 C16 122.1(4) . . ?
F11 C34 C33 119.6(4) . . ?
F11 C34 C35 117.2(4) . . ?
C33 C34 C35 123.1(5) . . ?
F12 C35 C36 120.5(4) . . ?
F12 C35 C34 120.3(5) . . ?
C36 C35 C34 119.2(5) . . ?
F13 C36 C35 120.0(5) . . ?
F13 C36 C37 119.9(6) . . ?
C35 C36 C37 120.1(4) . . ?
F14 C37 C36 119.7(4) . . ?
F14 C37 C38 121.1(5) . . ?
C36 C37 C38 119.2(5) . . ?
F15 C38 C37 117.2(5) . . ?
F15 C38 C33 120.3(4) . . ?
C37 C38 C33 122.5(5) . . ?
O2 C39 C58 118.0(3) . . ?
O2 C39 C40 118.8(4) . . ?
C58 C39 C40 123.2(4) . . ?
N5 C40 C41 109.5(3) . . ?
N5 C40 C39 126.6(4) . . ?
C41 C40 C39 123.9(4) . . ?
C42 C41 C40 107.5(4) . . ?
C42 C41 H9 126.3 . . ?
C40 C41 H9 126.3 . . ?
C41 C42 C43 107.3(4) . . ?
C41 C42 H10 126.4 . . ?
C43 C42 H10 126.4 . . ?
N5 C43 C44 124.4(4) . . ?
N5 C43 C42 108.6(3) . . ?
C44 C43 C42 127.1(4) . . ?
C45 C44 C43 127.9(4) . . ?
C45 C44 C59 115.8(4) . . ?
C43 C44 C59 116.2(4) . . ?
C44 C45 N6 126.6(4) . . ?
C44 C45 C46 127.4(4) . . ?
N6 C45 C46 105.9(4) . . ?
C47 C46 C45 108.8(4) . . ?
C47 C46 H11 125.6 . . ?
C45 C46 H11 125.6 . . ?
C46 C47 C48 107.7(4) . . ?
C46 C47 H12 126.1 . . ?
C48 C47 H12 126.1 . . ?
N6 C48 C49 126.1(4) . . ?
N6 C48 C47 107.0(4) . . ?
C49 C48 C47 126.8(4) . . ?
C48 C49 C50 125.6(4) . . ?
C48 C49 C65 117.2(4) . . ?
C50 C49 C65 117.1(4) . . ?
N7 C50 C49 124.9(4) . . ?
N7 C50 C51 109.5(4) . . ?
C49 C50 C51 125.6(4) . . ?
C52 C51 C50 107.9(4) . . ?
C52 C51 H13 126.1 . . ?
C50 C51 H13 126.1 . . ?
C51 C52 C53 107.7(4) . . ?
C51 C52 H14 126.1 . . ?
C53 C52 H14 126.1 . . ?
C54 C53 N7 125.4(5) . . ?
C54 C53 C52 126.4(4) . . ?
N7 C53 C52 108.2(4) . . ?
C53 C54 C55 127.5(4) . . ?
C53 C54 C71 115.3(4) . . ?
C55 C54 C71 117.2(4) . . ?
N8 C55 C54 124.8(4) . . ?
N8 C55 C56 106.2(4) . . ?
C54 C55 C56 128.9(4) . . ?
C57 C56 C55 108.1(4) . . ?
C57 C56 H15 126.0 . . ?
C55 C56 H15 126.0 . . ?
C56 C57 C58 108.9(4) . . ?
C56 C57 H16 125.6 . . ?
C58 C57 H16 125.6 . . ?
N8 C58 C57 106.4(4) . . ?
N8 C58 C39 126.7(4) . . ?
C57 C58 C39 126.8(4) . . ?
C64 C59 C60 115.6(4) . . ?
C64 C59 C44 121.0(4) . . ?
C60 C59 C44 123.3(4) . . ?
F16 C60 C61 117.6(4) . . ?
F16 C60 C59 119.4(4) . . ?
C61 C60 C59 123.0(4) . . ?
F17 C61 C62 119.8(4) . . ?
F17 C61 C60 120.4(4) . . ?
C62 C61 C60 119.7(4) . . ?
F18 C62 C61 120.4(4) . . ?
F18 C62 C63 120.1(4) . . ?
C61 C62 C63 119.4(4) . . ?
F19 C63 C62 119.8(4) . . ?
F19 C63 C64 120.4(4) . . ?
C62 C63 C64 119.8(4) . . ?
F20 C64 C59 119.7(4) . . ?
F20 C64 C63 117.8(4) . . ?
C59 C64 C63 122.5(4) . . ?
C70 C65 C66 115.4(4) . . ?
C70 C65 C49 122.1(4) . . ?
C66 C65 C49 122.5(4) . . ?
F21 C66 C67 117.3(4) . . ?
F21 C66 C65 120.8(4) . . ?
C67 C66 C65 121.9(4) . . ?
F22 C67 C68 119.9(4) . . ?
F22 C67 C66 119.9(4) . . ?
C68 C67 C66 120.2(5) . . ?
F23 C68 C69 119.1(5) . . ?
F23 C68 C67 121.0(5) . . ?
C69 C68 C67 119.8(5) . . ?
F24 C69 C68 121.2(5) . . ?
F24 C69 C70 119.9(5) . . ?
C68 C69 C70 118.9(5) . . ?
F25 C70 C69 117.0(4) . . ?
F25 C70 C65 119.2(4) . . ?
C69 C70 C65 123.8(4) . . ?
C72 C71 C76 115.9(4) . . ?
C72 C71 C54 123.2(5) . . ?
C76 C71 C54 120.9(5) . . ?
F26 C72 C71 119.9(4) . . ?
F26 C72 C73 118.3(5) . . ?
C71 C72 C73 121.8(5) . . ?
F27 C73 C74 119.4(4) . . ?
F27 C73 C72 120.4(5) . . ?
C74 C73 C72 120.2(5) . . ?
F28 C74 C73 120.0(5) . . ?
F28 C74 C75 119.9(5) . . ?
C73 C74 C75 120.0(5) . . ?
F29 C75 C76 121.5(6) . . ?
F29 C75 C74 119.9(5) . . ?
C76 C75 C74 118.5(6) . . ?
F30 C76 C75 117.3(6) . . ?
F30 C76 C71 119.1(4) . . ?
C75 C76 C71 123.5(6) . . ?
C2 N1 C5 109.8(3) . . ?
C2 N1 H19 125.1 . . ?
C5 N1 H19 125.1 . . ?
C10 N2 C7 105.3(3) . . ?
C12 N3 C15 109.7(3) . . ?
C12 N3 H20 125.2 . . ?
C15 N3 H20 125.2 . . ?
C20 N4 C17 108.2(3) . . ?
C20 N4 H21 125.9 . . ?
C17 N4 H21 125.9 . . ?
C40 N5 C43 107.1(3) . . ?
C40 N5 H22 126.4 . . ?
C43 N5 H22 126.4 . . ?
C48 N6 C45 110.5(3) . . ?
C48 N6 H17 124.7 . . ?
C45 N6 H17 124.7 . . ?
C50 N7 C53 106.7(4) . . ?
C58 N8 C55 110.4(3) . . ?
C58 N8 H18 124.8 . . ?
C55 N8 H18 124.8 . . ?
C83 C82 C84 107.8(11) . . ?
C83 C82 H23 110.2 . . ?
C84 C82 H23 110.2 . . ?
C83 C82 H24 110.2 . . ?
C84 C82 H24 110.2 . . ?
H23 C82 H24 108.5 . . ?
C82 C83 H25 109.5 . . ?
C82 C83 H26 109.5 . . ?
H25 C83 H26 109.5 . . ?
C82 C83 H27 109.5 . . ?
H25 C83 H27 109.5 . . ?
H26 C83 H27 109.5 . . ?
C84 C84 C82 114.9(13) 2_576 . ?
C84 C84 H28 108.5 2_576 . ?
C82 C84 H28 108.5 . . ?
C84 C84 H29 108.5 2_576 . ?
C82 C84 H29 108.5 . . ?
H28 C84 H29 107.5 . . ?
Cl3 C85 Cl1 112.4(7) . . ?
Cl3 C85 Cl2 111.1(11) . . ?
Cl1 C85 Cl2 109.5(6) . . ?
Cl3 C85 H85 107.9 . . ?
Cl1 C85 H85 107.9 . . ?
Cl2 C85 H85 107.9 . . ?

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
O1 C1 C2 N1 -175.2(4) . . . . ?
C20 C1 C2 N1 11.5(7) . . . . ?
O1 C1 C2 C3 14.0(7) . . . . ?
C20 C1 C2 C3 -159.3(4) . . . . ?
N1 C2 C3 C4 0.4(5) . . . . ?
C1 C2 C3 C4 172.9(4) . . . . ?
C2 C3 C4 C5 1.0(5) . . . . ?
C3 C4 C5 N1 -2.0(5) . . . . ?
C3 C4 C5 C6 174.7(4) . . . . ?
N1 C5 C6 C7 -6.7(7) . . . . ?
C4 C5 C6 C7 177.2(4) . . . . ?
N1 C5 C6 C21 170.3(4) . . . . ?
C4 C5 C6 C21 -5.8(7) . . . . ?
C5 C6 C7 N2 -5.2(7) . . . . ?
C21 C6 C7 N2 177.8(4) . . . . ?
C5 C6 C7 C8 170.2(4) . . . . ?
C21 C6 C7 C8 -6.8(6) . . . . ?
N2 C7 C8 C9 1.1(5) . . . . ?
C6 C7 C8 C9 -175.0(4) . . . . ?
C7 C8 C9 C10 -1.0(5) . . . . ?
C8 C9 C10 N2 0.7(5) . . . . ?
C8 C9 C10 C11 -179.9(4) . . . . ?
N2 C10 C11 C12 -0.7(7) . . . . ?
C9 C10 C11 C12 -180.0(4) . . . . ?
N2 C10 C11 C27 175.9(4) . . . . ?
C9 C10 C11 C27 -3.4(6) . . . . ?
C10 C11 C12 N3 -1.1(7) . . . . ?
C27 C11 C12 N3 -177.7(4) . . . . ?
C10 C11 C12 C13 179.9(4) . . . . ?
C27 C11 C12 C13 3.3(6) . . . . ?
N3 C12 C13 C14 -0.1(5) . . . . ?
C11 C12 C13 C14 179.1(4) . . . . ?
C12 C13 C14 C15 1.3(5) . . . . ?
C13 C14 C15 C16 176.0(5) . . . . ?
C13 C14 C15 N3 -1.9(5) . . . . ?
N3 C15 C16 C17 7.7(8) . . . . ?
C14 C15 C16 C17 -169.8(4) . . . . ?
N3 C15 C16 C33 -171.8(4) . . . . ?
C14 C15 C16 C33 10.6(7) . . . . ?
C15 C16 C17 N4 13.7(8) . . . . ?
C33 C16 C17 N4 -166.7(4) . . . . ?
C15 C16 C17 C18 -166.3(5) . . . . ?
C33 C16 C17 C18 13.3(7) . . . . ?
N4 C17 C18 C19 1.3(5) . . . . ?
C16 C17 C18 C19 -178.7(4) . . . . ?
C17 C18 C19 C20 -0.6(5) . . . . ?
C18 C19 C20 N4 -0.4(5) . . . . ?
C18 C19 C20 C1 -171.6(4) . . . . ?
O1 C1 C20 N4 166.0(4) . . . . ?
C2 C1 C20 N4 -20.6(7) . . . . ?
O1 C1 C20 C19 -24.5(7) . . . . ?
C2 C1 C20 C19 148.9(4) . . . . ?
C7 C6 C21 C22 -62.0(6) . . . . ?
C5 C6 C21 C22 120.7(5) . . . . ?
C7 C6 C21 C26 118.2(5) . . . . ?
C5 C6 C21 C26 -59.1(6) . . . . ?
C26 C21 C22 F1 179.8(4) . . . . ?
C6 C21 C22 F1 0.0(7) . . . . ?
C26 C21 C22 C23 0.6(7) . . . . ?
C6 C21 C22 C23 -179.1(4) . . . . ?
F1 C22 C23 F2 0.7(7) . . . . ?
C21 C22 C23 F2 179.9(4) . . . . ?
F1 C22 C23 C24 -178.7(4) . . . . ?
C21 C22 C23 C24 0.5(8) . . . . ?
F2 C23 C24 C25 -180.0(5) . . . . ?
C22 C23 C24 C25 -0.6(8) . . . . ?
F2 C23 C24 F3 2.3(8) . . . . ?
C22 C23 C24 F3 -178.4(4) . . . . ?
F3 C24 C25 F4 -1.6(7) . . . . ?
C23 C24 C25 F4 -179.4(5) . . . . ?
F3 C24 C25 C26 177.3(4) . . . . ?
C23 C24 C25 C26 -0.5(8) . . . . ?
F4 C25 C26 F5 1.8(7) . . . . ?
C24 C25 C26 F5 -177.0(4) . . . . ?
F4 C25 C26 C21 -179.4(4) . . . . ?
C24 C25 C26 C21 1.7(7) . . . . ?
C22 C21 C26 F5 176.9(4) . . . . ?
C6 C21 C26 F5 -3.3(6) . . . . ?
C22 C21 C26 C25 -1.8(7) . . . . ?
C6 C21 C26 C25 178.0(4) . . . . ?
C12 C11 C27 C32 104.8(5) . . . . ?
C10 C11 C27 C32 -72.1(6) . . . . ?
C12 C11 C27 C28 -74.4(5) . . . . ?
C10 C11 C27 C28 108.8(5) . . . . ?
C32 C27 C28 F6 179.9(4) . . . . ?
C11 C27 C28 F6 -0.9(6) . . . . ?
C32 C27 C28 C29 0.5(6) . . . . ?
C11 C27 C28 C29 179.7(4) . . . . ?
F6 C28 C29 F7 -0.2(6) . . . . ?
C27 C28 C29 F7 179.2(4) . . . . ?
F6 C28 C29 C30 179.9(4) . . . . ?
C27 C28 C29 C30 -0.7(7) . . . . ?
F7 C29 C30 F8 -1.4(7) . . . . ?
C28 C29 C30 F8 178.4(4) . . . . ?
F7 C29 C30 C31 -179.1(4) . . . . ?
C28 C29 C30 C31 0.7(7) . . . . ?
F8 C30 C31 F9 3.0(7) . . . . ?
C29 C30 C31 F9 -179.2(4) . . . . ?
F8 C30 C31 C32 -178.4(4) . . . . ?
C29 C30 C31 C32 -0.6(7) . . . . ?
C28 C27 C32 F10 179.7(4) . . . . ?
C11 C27 C32 F10 0.4(6) . . . . ?
C28 C27 C32 C31 -0.4(6) . . . . ?
C11 C27 C32 C31 -179.6(4) . . . . ?
F9 C31 C32 F10 -1.0(6) . . . . ?
C30 C31 C32 F10 -179.6(4) . . . . ?
F9 C31 C32 C27 179.1(4) . . . . ?
C30 C31 C32 C27 0.5(7) . . . . ?
C15 C16 C33 C34 61.6(6) . . . . ?
C17 C16 C33 C34 -118.1(5) . . . . ?
C15 C16 C33 C38 -121.9(5) . . . . ?
C17 C16 C33 C38 58.4(6) . . . . ?
C38 C33 C34 F11 -179.5(4) . . . . ?
C16 C33 C34 F11 -2.8(7) . . . . ?
C38 C33 C34 C35 0.2(7) . . . . ?
C16 C33 C34 C35 177.0(4) . . . . ?
F11 C34 C35 F12 -0.3(7) . . . . ?
C33 C34 C35 F12 179.9(4) . . . . ?
F11 C34 C35 C36 178.0(4) . . . . ?
C33 C34 C35 C36 -1.7(7) . . . . ?
F12 C35 C36 F13 -1.9(7) . . . . ?
C34 C35 C36 F13 179.7(4) . . . . ?
F12 C35 C36 C37 -179.5(5) . . . . ?
C34 C35 C36 C37 2.2(8) . . . . ?
F13 C36 C37 F14 0.6(8) . . . . ?
C35 C36 C37 F14 178.1(5) . . . . ?
F13 C36 C37 C38 -178.7(5) . . . . ?
C35 C36 C37 C38 -1.1(8) . . . . ?
F14 C37 C38 F15 -0.6(7) . . . . ?
C36 C37 C38 F15 178.7(4) . . . . ?
F14 C37 C38 C33 -179.7(4) . . . . ?
C36 C37 C38 C33 -0.4(8) . . . . ?
C34 C33 C38 F15 -178.2(4) . . . . ?
C16 C33 C38 F15 5.1(7) . . . . ?
C34 C33 C38 C37 0.8(7) . . . . ?
C16 C33 C38 C37 -175.9(4) . . . . ?
O2 C39 C40 N5 178.8(4) . . . . ?
C58 C39 C40 N5 -0.5(7) . . . . ?
O2 C39 C40 C41 -2.5(6) . . . . ?
C58 C39 C40 C41 178.2(4) . . . . ?
N5 C40 C41 C42 0.6(5) . . . . ?
C39 C40 C41 C42 -178.2(4) . . . . ?
C40 C41 C42 C43 -0.7(5) . . . . ?
C41 C42 C43 N5 0.5(5) . . . . ?
C41 C42 C43 C44 -178.8(4) . . . . ?
N5 C43 C44 C45 7.3(7) . . . . ?
C42 C43 C44 C45 -173.6(4) . . . . ?
N5 C43 C44 C59 -178.0(4) . . . . ?
C42 C43 C44 C59 1.2(7) . . . . ?
C43 C44 C45 N6 7.0(8) . . . . ?
C59 C44 C45 N6 -167.8(4) . . . . ?
C43 C44 C45 C46 -176.5(5) . . . . ?
C59 C44 C45 C46 8.7(7) . . . . ?
C44 C45 C46 C47 -176.0(5) . . . . ?
N6 C45 C46 C47 1.1(5) . . . . ?
C45 C46 C47 C48 1.3(5) . . . . ?
C46 C47 C48 N6 -3.2(5) . . . . ?
C46 C47 C48 C49 174.2(5) . . . . ?
N6 C48 C49 C50 -7.8(8) . . . . ?
C47 C48 C49 C50 175.3(5) . . . . ?
N6 C48 C49 C65 168.7(4) . . . . ?
C47 C48 C49 C65 -8.2(7) . . . . ?
C48 C49 C50 N7 -6.3(9) . . . . ?
C65 C49 C50 N7 177.2(5) . . . . ?
C48 C49 C50 C51 176.1(5) . . . . ?
C65 C49 C50 C51 -0.4(8) . . . . ?
N7 C50 C51 C52 -1.4(6) . . . . ?
C49 C50 C51 C52 176.5(5) . . . . ?
C50 C51 C52 C53 0.5(6) . . . . ?
C51 C52 C53 C54 -178.6(6) . . . . ?
C51 C52 C53 N7 0.5(6) . . . . ?
N7 C53 C54 C55 6.7(10) . . . . ?
C52 C53 C54 C55 -174.3(5) . . . . ?
N7 C53 C54 C71 -176.5(5) . . . . ?
C52 C53 C54 C71 2.5(9) . . . . ?
C53 C54 C55 N8 12.9(9) . . . . ?
C71 C54 C55 N8 -163.8(5) . . . . ?
C53 C54 C55 C56 -171.5(6) . . . . ?
C71 C54 C55 C56 11.8(8) . . . . ?
N8 C55 C56 C57 -0.4(5) . . . . ?
C54 C55 C56 C57 -176.6(5) . . . . ?
C55 C56 C57 C58 0.6(5) . . . . ?
C56 C57 C58 N8 -0.7(5) . . . . ?
C56 C57 C58 C39 175.6(4) . . . . ?
O2 C39 C58 N8 161.4(4) . . . . ?
C40 C39 C58 N8 -19.3(7) . . . . ?
O2 C39 C58 C57 -14.1(7) . . . . ?
C40 C39 C58 C57 165.2(4) . . . . ?
C45 C44 C59 C64 91.6(5) . . . . ?
C43 C44 C59 C64 -83.8(5) . . . . ?
C45 C44 C59 C60 -88.2(5) . . . . ?
C43 C44 C59 C60 96.3(5) . . . . ?
C64 C59 C60 F16 -177.8(4) . . . . ?
C44 C59 C60 F16 2.1(7) . . . . ?
C64 C59 C60 C61 0.7(7) . . . . ?
C44 C59 C60 C61 -179.4(4) . . . . ?
F16 C60 C61 F17 -4.1(6) . . . . ?
C59 C60 C61 F17 177.4(4) . . . . ?
F16 C60 C61 C62 176.7(4) . . . . ?
C59 C60 C61 C62 -1.8(7) . . . . ?
F17 C61 C62 F18 0.1(6) . . . . ?
C60 C61 C62 F18 179.4(4) . . . . ?
F17 C61 C62 C63 -178.1(4) . . . . ?
C60 C61 C62 C63 1.2(7) . . . . ?
F18 C62 C63 F19 1.3(6) . . . . ?
C61 C62 C63 F19 179.6(4) . . . . ?
F18 C62 C63 C64 -177.7(4) . . . . ?
C61 C62 C63 C64 0.5(7) . . . . ?
C60 C59 C64 F20 -178.1(4) . . . . ?
C44 C59 C64 F20 2.0(6) . . . . ?
C60 C59 C64 C63 1.0(7) . . . . ?
C44 C59 C64 C63 -178.9(4) . . . . ?
F19 C63 C64 F20 -1.6(6) . . . . ?
C62 C63 C64 F20 177.5(4) . . . . ?
F19 C63 C64 C59 179.3(4) . . . . ?
C62 C63 C64 C59 -1.6(7) . . . . ?
C48 C49 C65 C70 -64.3(6) . . . . ?
C50 C49 C65 C70 112.5(5) . . . . ?
C48 C49 C65 C66 115.8(5) . . . . ?
C50 C49 C65 C66 -67.4(6) . . . . ?
C70 C65 C66 F21 -178.0(4) . . . . ?
C49 C65 C66 F21 1.9(7) . . . . ?
C70 C65 C66 C67 1.8(7) . . . . ?
C49 C65 C66 C67 -178.2(4) . . . . ?
F21 C66 C67 F22 -1.5(7) . . . . ?
C65 C66 C67 F22 178.6(4) . . . . ?
F21 C66 C67 C68 178.3(4) . . . . ?
C65 C66 C67 C68 -1.6(7) . . . . ?
F22 C67 C68 F23 1.4(7) . . . . ?
C66 C67 C68 F23 -178.4(4) . . . . ?
F22 C67 C68 C69 179.3(4) . . . . ?
C66 C67 C68 C69 -0.5(8) . . . . ?
F23 C68 C69 F24 -1.9(7) . . . . ?
C67 C68 C69 F24 -179.8(4) . . . . ?
F23 C68 C69 C70 -179.8(4) . . . . ?
C67 C68 C69 C70 2.2(7) . . . . ?
F24 C69 C70 F25 2.0(7) . . . . ?
C68 C69 C70 F25 -180.0(4) . . . . ?
F24 C69 C70 C65 -179.9(4) . . . . ?
C68 C69 C70 C65 -2.0(8) . . . . ?
C66 C65 C70 F25 177.9(4) . . . . ?
C49 C65 C70 F25 -2.0(7) . . . . ?
C66 C65 C70 C69 -0.1(7) . . . . ?
C49 C65 C70 C69 -180.0(4) . . . . ?
C53 C54 C71 C72 100.3(6) . . . . ?
C55 C54 C71 C72 -82.6(6) . . . . ?
C53 C54 C71 C76 -79.5(6) . . . . ?
C55 C54 C71 C76 97.6(6) . . . . ?
C76 C71 C72 F26 -179.0(4) . . . . ?
C54 C71 C72 F26 1.3(7) . . . . ?
C76 C71 C72 C73 1.5(7) . . . . ?
C54 C71 C72 C73 -178.3(4) . . . . ?
F26 C72 C73 F27 0.9(7) . . . . ?
C71 C72 C73 F27 -179.5(4) . . . . ?
F26 C72 C73 C74 -179.1(4) . . . . ?
C71 C72 C73 C74 0.4(7) . . . . ?
F27 C73 C74 F28 -1.6(7) . . . . ?
C72 C73 C74 F28 178.4(4) . . . . ?
F27 C73 C74 C75 178.8(4) . . . . ?
C72 C73 C74 C75 -1.1(8) . . . . ?
F28 C74 C75 F29 3.1(8) . . . . ?
C73 C74 C75 F29 -177.4(5) . . . . ?
F28 C74 C75 C76 -179.7(5) . . . . ?
C73 C74 C75 C76 -0.2(8) . . . . ?
F29 C75 C76 F30 -2.4(8) . . . . ?
C74 C75 C76 F30 -179.6(5) . . . . ?
F29 C75 C76 C71 179.4(5) . . . . ?
C74 C75 C76 C71 2.2(9) . . . . ?
C72 C71 C76 F30 179.0(4) . . . . ?
C54 C71 C76 F30 -1.2(7) . . . . ?
C72 C71 C76 C75 -2.8(8) . . . . ?
C54 C71 C76 C75 176.9(5) . . . . ?
C3 C2 N1 C5 -1.7(5) . . . . ?
C1 C2 N1 C5 -173.7(4) . . . . ?
C4 C5 N1 C2 2.3(5) . . . . ?
C6 C5 N1 C2 -174.5(4) . . . . ?
C11 C10 N2 C7 -179.4(4) . . . . ?
C9 C10 N2 C7 0.0(5) . . . . ?
C6 C7 N2 C10 175.3(4) . . . . ?
C8 C7 N2 C10 -0.6(5) . . . . ?
C11 C12 N3 C15 179.7(4) . . . . ?
C13 C12 N3 C15 -1.2(5) . . . . ?
C16 C15 N3 C12 -176.1(4) . . . . ?
C14 C15 N3 C12 1.9(5) . . . . ?
C19 C20 N4 C17 1.2(5) . . . . ?
C1 C20 N4 C17 172.2(4) . . . . ?
C18 C17 N4 C20 -1.5(5) . . . . ?
C16 C17 N4 C20 178.5(4) . . . . ?
C41 C40 N5 C43 -0.3(5) . . . . ?
C39 C40 N5 C43 178.5(4) . . . . ?
C44 C43 N5 C40 179.2(4) . . . . ?
C42 C43 N5 C40 -0.1(5) . . . . ?
C49 C48 N6 C45 -173.5(4) . . . . ?
C47 C48 N6 C45 4.0(5) . . . . ?
C44 C45 N6 C48 173.9(4) . . . . ?
C46 C45 N6 C48 -3.2(5) . . . . ?
C49 C50 N7 C53 -176.3(5) . . . . ?
C51 C50 N7 C53 1.7(6) . . . . ?
C54 C53 N7 C50 177.8(6) . . . . ?
C52 C53 N7 C50 -1.4(6) . . . . ?
C57 C58 N8 C55 0.4(5) . . . . ?
C39 C58 N8 C55 -175.8(4) . . . . ?
C54 C55 N8 C58 176.4(4) . . . . ?
C56 C55 N8 C58 -0.1(5) . . . . ?
C83 C82 C84 C84 -176.5(14) . . . 2_576 ?

_refine_diff_density_max         1.077
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.102



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_171217_ys_5-1
_database_code_depnum_ccdc_archive 'CCDC 1906674'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_vrf_PLAT410_171217_ys_5-1       
;
PROBLEM: Short Intra H...H Contact H38 ..H40B 1.43 Ang.
RESPONSE: Short distance between H38 and H40B is due to disordering of 
aklyl chains.
;

_vrf_PLAT973_171217_ys_5-1       
;
PROBLEM: Check Calcd Positive Resid. Density on Zn1 2.49 eA-3
RESPONSE: The large peaks around Zn atom are the ghost peak derived from 
the ripple of fourier series truncation error.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C38 H10 F15 N4 O Zn, C16 H36 N, C2.5 H3.5'
_chemical_formula_sum            'C56.50 H49.50 Cl F15 N5 O Zn'
_chemical_formula_weight         1200.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2181 1.7016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1723 0.1934 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.303(3)
_cell_length_b                   16.985(3)
_cell_length_c                   20.280(4)
_cell_angle_alpha                92.310(2)
_cell_angle_beta                 94.162(2)
_cell_angle_gamma                101.368(2)
_cell_volume                     5146.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    44052
_cell_measurement_theta_min      1.111
_cell_measurement_theta_max      28.140

_exptl_crystal_description       cube
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             2454
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.815
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.7829
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'

_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            44052
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.111
_diffrn_reflns_theta_max         28.140
_diffrn_reflns_theta_full        28.017
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             18560
_reflns_number_gt                11664
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1250P)²+24.8810P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0087(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         18560
_refine_ls_number_parameters     1425
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.2960
_refine_ls_wR_factor_gt          0.2113
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_restrained_S_all      1.196
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0466(4) 0.4676(4) 0.5626(3) 0.0237(14) Uani 1 1 d . . . . .
C2 C 0.0340(4) 0.4410(4) 0.5758(3) 0.0238(14) Uani 1 1 d . . . . .
C3 C 0.0421(5) 0.3601(4) 0.5799(3) 0.0252(15) Uani 1 1 d . . . . .
H1 H -0.0055 0.3144 0.5753 0.030 Uiso 1 1 calc R U . . .
C4 C 0.1296(5) 0.3595(4) 0.5916(3) 0.0302(16) Uani 1 1 d . . . . .
H2 H 0.1556 0.3137 0.5979 0.036 Uiso 1 1 calc R U . . .
C5 C 0.1756(4) 0.4411(4) 0.5927(3) 0.0259(15) Uani 1 1 d . . . . .
C6 C 0.2683(4) 0.4674(4) 0.5974(3) 0.0252(15) Uani 1 1 d . . . . .
C7 C 0.3152(5) 0.5433(4) 0.5930(3) 0.0250(15) Uani 1 1 d . . . . .
C8 C 0.4106(4) 0.5689(5) 0.6000(3) 0.0298(16) Uani 1 1 d . . . . .
H3 H 0.4529 0.5356 0.6081 0.036 Uiso 1 1 calc R U . . .
C9 C 0.4291(5) 0.6482(4) 0.5931(4) 0.0316(16) Uani 1 1 d . . . . .
H4 H 0.4869 0.6817 0.5945 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3459(5) 0.6732(4) 0.5830(3) 0.0286(16) Uani 1 1 d . . . . .
C11 C 0.3356(5) 0.7522(4) 0.5746(3) 0.0260(15) Uani 1 1 d . . . . .
C12 C 0.2568(5) 0.7793(4) 0.5693(4) 0.0276(15) Uani 1 1 d . . . . .
C13 C 0.2477(5) 0.8604(4) 0.5638(4) 0.0346(17) Uani 1 1 d . . . . .
H5 H 0.2945 0.9058 0.5613 0.042 Uiso 1 1 calc R U . . .
C14 C 0.1591(5) 0.8602(5) 0.5629(4) 0.0330(17) Uani 1 1 d . . . . .
H6 H 0.1326 0.9062 0.5599 0.040 Uiso 1 1 calc R U . . .
C15 C 0.1131(5) 0.7813(4) 0.5670(4) 0.0275(15) Uani 1 1 d . . . . .
C16 C 0.0232(5) 0.7563(4) 0.5704(3) 0.0272(15) Uani 1 1 d . . . . .
C17 C -0.0249(4) 0.6783(4) 0.5745(3) 0.0254(15) Uani 1 1 d . . . . .
C18 C -0.1187(5) 0.6535(4) 0.5709(3) 0.0286(16) Uani 1 1 d . . . . .
H7 H -0.1607 0.6879 0.5712 0.034 Uiso 1 1 calc R U . . .
C19 C -0.1383(5) 0.5720(4) 0.5668(3) 0.0289(16) Uani 1 1 d . . . . .
H8 H -0.1961 0.5383 0.5621 0.035 Uiso 1 1 calc R U . . .
C20 C -0.0564(4) 0.5480(4) 0.5708(3) 0.0229(14) Uani 1 1 d . . . . .
C21 C 0.3231(4) 0.4048(4) 0.6074(3) 0.0268(15) Uani 1 1 d . . . . .
C22 C 0.3502(5) 0.3641(4) 0.5551(3) 0.0311(16) Uani 1 1 d . . . . .
C23 C 0.4013(5) 0.3084(5) 0.5629(4) 0.0329(17) Uani 1 1 d . . . . .
C24 C 0.4290(5) 0.2916(4) 0.6256(4) 0.0330(17) Uani 1 1 d . . . . .
C25 C 0.4050(5) 0.3298(4) 0.6790(4) 0.0308(16) Uani 1 1 d . . . . .
C26 C 0.3495(4) 0.3843(4) 0.6688(3) 0.0273(15) Uani 1 1 d . . . . .
C27 C 0.4200(4) 0.8142(4) 0.5772(3) 0.0269(15) Uani 1 1 d . . . . .
C28 C 0.4487(5) 0.8506(5) 0.5216(4) 0.0362(18) Uani 1 1 d . . . . .
C29 C 0.5253(5) 0.9078(5) 0.5225(4) 0.0377(18) Uani 1 1 d . . . . .
C30 C 0.5755(5) 0.9291(5) 0.5807(5) 0.043(2) Uani 1 1 d . . . . .
C31 C 0.5504(5) 0.8949(5) 0.6367(4) 0.0352(18) Uani 1 1 d . . . . .
C32 C 0.4731(5) 0.8385(4) 0.6347(4) 0.0317(16) Uani 1 1 d . . . . .
C33 C -0.0321(4) 0.8191(4) 0.5626(3) 0.0259(15) Uani 1 1 d . . . . .
C34 C -0.0392(5) 0.8556(5) 0.5042(4) 0.0333(17) Uani 1 1 d . . . . .
C35 C -0.0905(5) 0.9134(5) 0.4944(4) 0.0392(19) Uani 1 1 d . . . . .
C36 C -0.1375(5) 0.9338(5) 0.5448(4) 0.0380(19) Uani 1 1 d . . . . .
C37 C -0.1320(5) 0.8990(4) 0.6028(4) 0.0334(17) Uani 1 1 d . . . . .
C38 C -0.0802(5) 0.8433(4) 0.6111(3) 0.0293(16) Uani 1 1 d . . . . .
C39 C 1.0281(4) 0.5498(4) 0.9387(3) 0.0250(15) Uani 1 1 d . . . . .
C40 C 0.9350(5) 0.5318(4) 0.9256(3) 0.0274(15) Uani 1 1 d . . . . .
C41 C 0.8802(4) 0.5894(4) 0.9252(3) 0.0248(14) Uani 1 1 d . . . . .
H9 H 0.8996 0.6458 0.9333 0.030 Uiso 1 1 calc R U . . .
C42 C 0.7945(4) 0.5494(4) 0.9111(3) 0.0273(15) Uani 1 1 d . . . . .
H10 H 0.7427 0.5722 0.9057 0.033 Uiso 1 1 calc R U . . .
C43 C 0.7979(5) 0.4668(4) 0.9060(3) 0.0260(15) Uani 1 1 d . . . . .
C44 C 0.7243(4) 0.4034(4) 0.9019(3) 0.0215(14) Uani 1 1 d . . . . .
C45 C 0.7228(4) 0.3234(4) 0.9079(4) 0.0272(15) Uani 1 1 d . . . . .
C46 C 0.6453(5) 0.2604(4) 0.9052(4) 0.0344(17) Uani 1 1 d . . . . .
H11 H 0.5849 0.2661 0.8975 0.041 Uiso 1 1 calc R U . . .
C47 C 0.6733(4) 0.1926(4) 0.9155(4) 0.0279(15) Uani 1 1 d . . . . .
H12 H 0.6361 0.1411 0.9179 0.034 Uiso 1 1 calc R U . . .
C48 C 0.7686(5) 0.2100(4) 0.9225(4) 0.0284(16) Uani 1 1 d . . . . .
C49 C 0.8238(4) 0.1569(4) 0.9286(4) 0.0268(15) Uani 1 1 d . . . . .
C50 C 0.9155(4) 0.1720(4) 0.9272(3) 0.0245(14) Uani 1 1 d . . . . .
C51 C 0.9707(5) 0.1138(4) 0.9227(3) 0.0286(15) Uani 1 1 d . . . . .
H13 H 0.9517 0.0574 0.9252 0.034 Uiso 1 1 calc R U . . .
C52 C 1.0535(4) 0.1524(4) 0.9142(3) 0.0265(15) Uani 1 1 d . . . . .
H14 H 1.1037 0.1286 0.9079 0.032 Uiso 1 1 calc R U . . .
C53 C 1.0522(4) 0.2361(4) 0.9165(3) 0.0236(14) Uani 1 1 d . . . . .
C54 C 1.1242(4) 0.2973(4) 0.9117(3) 0.0267(15) Uani 1 1 d . . . . .
C55 C 1.1266(4) 0.3798(4) 0.9170(3) 0.0211(14) Uani 1 1 d . . . . .
C56 C 1.2028(4) 0.4414(4) 0.9187(3) 0.0265(15) Uani 1 1 d . . . . .
H15 H 1.2621 0.4345 0.9138 0.032 Uiso 1 1 calc R U . . .
C57 C 1.1768(4) 0.5128(4) 0.9287(3) 0.0225(14) Uani 1 1 d . . . . .
H16 H 1.2141 0.5648 0.9332 0.027 Uiso 1 1 calc R U . . .
C58 C 1.0837(4) 0.4936(4) 0.9309(3) 0.0217(14) Uani 1 1 d . . . . .
C59 C 0.6352(4) 0.4259(4) 0.8889(3) 0.0273(15) Uani 1 1 d . . . . .
C60 C 0.6100(4) 0.4549(4) 0.8294(3) 0.0273(15) Uani 1 1 d . . . . .
C61 C 0.5291(4) 0.4758(4) 0.8172(3) 0.0246(15) Uani 1 1 d . . . . .
C62 C 0.4712(4) 0.4677(4) 0.8642(3) 0.0266(15) Uani 1 1 d . . . . .
C63 C 0.4912(4) 0.4405(4) 0.9235(3) 0.0263(15) Uani 1 1 d . . . . .
C64 C 0.5744(4) 0.4209(4) 0.9354(3) 0.0234(14) Uani 1 1 d . . . . .
C65 C 0.7797(4) 0.0707(4) 0.9342(3) 0.0248(14) Uani 1 1 d . . . . .
C66 C 0.7446(5) 0.0208(4) 0.8817(3) 0.0330(17) Uani 1 1 d . . . . .
C67 C 0.7056(5) -0.0580(4) 0.8863(4) 0.0348(17) Uani 1 1 d . . . . .
C68 C 0.6998(5) -0.0888(4) 0.9470(4) 0.0308(16) Uani 1 1 d . . . . .
C69 C 0.7333(5) -0.0410(4) 1.0013(4) 0.0332(17) Uani 1 1 d . . . . .
C70 C 0.7725(5) 0.0370(4) 0.9947(4) 0.0301(16) Uani 1 1 d . . . . .
C71 C 1.2076(4) 0.2720(4) 0.8943(3) 0.0244(14) Uani 1 1 d . . . . .
C72 C 1.2149(4) 0.2394(4) 0.8333(3) 0.0289(16) Uani 1 1 d . . . . .
C73 C 1.2907(5) 0.2138(5) 0.8157(4) 0.0341(17) Uani 1 1 d . . . . .
C74 C 1.3621(5) 0.2225(4) 0.8605(4) 0.0311(16) Uani 1 1 d . . . . .
C75 C 1.3587(4) 0.2564(4) 0.9218(4) 0.0300(16) Uani 1 1 d . . . . .
C76 C 1.2827(5) 0.2793(4) 0.9391(3) 0.0270(15) Uani 1 1 d . . . . .
C77 C 0.1461(5) 0.7957(4) 0.7429(4) 0.0360(18) Uani 1 1 d . . . . .
H41 H 0.1007 0.8295 0.7359 0.043 Uiso 1 1 calc R U . . .
H42 H 0.1561 0.7731 0.6990 0.043 Uiso 1 1 calc R U . . .
C78 C 0.2329(6) 0.8490(5) 0.7721(5) 0.049(2) Uani 1 1 d . . . . .
H43 H 0.2269 0.8634 0.8191 0.058 Uiso 1 1 calc R U . . .
H44 H 0.2815 0.8183 0.7708 0.058 Uiso 1 1 calc R U . . .
C79 C 0.2577(8) 0.9234(6) 0.7368(5) 0.066(3) Uani 1 1 d . . . . .
H45 H 0.3118 0.9553 0.7621 0.079 Uiso 1 1 calc R U . A 3
H46 H 0.2772 0.9067 0.6938 0.079 Uiso 1 1 calc R U . A 3
C80A C 0.2023(13) 0.9769(12) 0.7227(11) 0.069(7) Uiso 0.57(3) 1 d . . P B 3
H80A H 0.1486 0.9488 0.6958 0.103 Uiso 0.57(3) 1 calc R U P B 3
H80B H 0.2340 1.0207 0.6981 0.103 Uiso 0.57(3) 1 calc R U P B 3
H80C H 0.1851 0.9989 0.7641 0.103 Uiso 0.57(3) 1 calc R U P B 3
C80B C 0.1978(19) 0.9810(17) 0.7770(15) 0.073(10) Uiso 0.43(3) 1 d . . P B 4
H80D H 0.1407 0.9794 0.7512 0.110 Uiso 0.43(3) 1 calc R U P B 4
H80E H 0.2314 1.0366 0.7822 0.110 Uiso 0.43(3) 1 calc R U P B 4
H80F H 0.1866 0.9604 0.8207 0.110 Uiso 0.43(3) 1 calc R U P B 4
C81 C 0.0795(5) 0.7585(5) 0.8482(3) 0.0293(16) Uani 1 1 d . . . . .
H47 H 0.0672 0.7132 0.8775 0.035 Uiso 1 1 calc R U . . .
H48 H 0.1295 0.7991 0.8704 0.035 Uiso 1 1 calc R U . . .
C82 C -0.0024(5) 0.7956(5) 0.8406(4) 0.0344(17) Uani 1 1 d . . . . .
H49 H 0.0071 0.8386 0.8088 0.041 Uiso 1 1 calc R U . . .
H50 H -0.0547 0.7542 0.8231 0.041 Uiso 1 1 calc R U . . .
C83 C -0.0200(5) 0.8303(5) 0.9067(4) 0.0333(17) Uani 1 1 d . . . . .
H51 H -0.0215 0.7889 0.9398 0.040 Uiso 1 1 calc R U . . .
H52 H 0.0295 0.8759 0.9215 0.040 Uiso 1 1 calc R U . . .
C84 C -0.1071(6) 0.8591(6) 0.9034(4) 0.048(2) Uani 1 1 d . . . . .
H65 H -0.1082 0.8962 0.8677 0.072 Uiso 1 1 calc R U . . .
H66 H -0.1129 0.8869 0.9457 0.072 Uiso 1 1 calc R U . . .
H67 H -0.1569 0.8129 0.8947 0.072 Uiso 1 1 calc R U . . .
C85 C 0.0322(5) 0.6763(4) 0.7428(3) 0.0304(16) Uani 1 1 d . . . . .
H53 H 0.0546 0.6554 0.7024 0.036 Uiso 1 1 calc R U . . .
H54 H -0.0109 0.7101 0.7287 0.036 Uiso 1 1 calc R U . . .
C86 C -0.0161(5) 0.6063(4) 0.7782(3) 0.0294(16) Uani 1 1 d . . . . .
H55 H 0.0232 0.5668 0.7842 0.035 Uiso 1 1 calc R U . . .
H56 H -0.0280 0.6258 0.8227 0.035 Uiso 1 1 calc R U . . .
C87 C -0.1023(6) 0.5653(5) 0.7420(4) 0.0372(18) Uani 1 1 d . . . . .
H57 H -0.1259 0.5159 0.7647 0.045 Uiso 1 1 calc R U . . .
H58 H -0.0903 0.5485 0.6968 0.045 Uiso 1 1 calc R U . . .
C88 C -0.1740(5) 0.6152(5) 0.7365(4) 0.0403(19) Uani 1 1 d . . . . .
H68 H -0.1848 0.6343 0.7808 0.061 Uiso 1 1 calc R U . . .
H69 H -0.2294 0.5822 0.7151 0.061 Uiso 1 1 calc R U . . .
H70 H -0.1542 0.6614 0.7099 0.061 Uiso 1 1 calc R U . . .
C89 C 0.1794(5) 0.6807(5) 0.8033(4) 0.0349(18) Uani 1 1 d . . . . .
H59 H 0.1526 0.6365 0.8304 0.042 Uiso 1 1 calc R U . . .
H60 H 0.2280 0.7163 0.8315 0.042 Uiso 1 1 calc R U . . .
C90 C 0.2200(7) 0.6449(6) 0.7460(5) 0.058(3) Uani 1 1 d . . . . .
H61 H 0.1735 0.6044 0.7201 0.069 Uiso 1 1 calc R U . . .
H62 H 0.2430 0.6877 0.7163 0.069 Uiso 1 1 calc R U . . .
C91 C 0.2955(7) 0.6056(6) 0.7711(5) 0.059(3) Uani 1 1 d . . . . .
H63 H 0.3162 0.5778 0.7332 0.071 Uiso 1 1 calc R U . . .
H64 H 0.2722 0.5643 0.8019 0.071 Uiso 1 1 calc R U . . .
C92 C 0.3752(7) 0.6634(7) 0.8064(8) 0.088(4) Uani 1 1 d . . . . .
H71 H 0.3940 0.7086 0.7786 0.132 Uiso 1 1 calc R U . . .
H72 H 0.4246 0.6352 0.8147 0.132 Uiso 1 1 calc R U . . .
H73 H 0.3583 0.6836 0.8486 0.132 Uiso 1 1 calc R U . . .
C93 C 0.7595(5) 0.2974(5) 0.6423(4) 0.0359(18) Uani 1 1 d . . . . .
H17 H 0.8124 0.3227 0.6198 0.043 Uiso 1 1 calc R U . . .
H18 H 0.7229 0.2554 0.6110 0.043 Uiso 1 1 calc R U . . .
C94 C 0.7060(5) 0.3596(5) 0.6558(4) 0.0308(16) Uani 1 1 d . . . . .
H19 H 0.7447 0.4071 0.6800 0.037 Uiso 1 1 calc R U . . .
H20 H 0.6576 0.3379 0.6839 0.037 Uiso 1 1 calc R U . . .
C95 C 0.6650(5) 0.3852(5) 0.5904(4) 0.0354(17) Uani 1 1 d . . . . .
H21 H 0.7131 0.4020 0.5607 0.043 Uiso 1 1 calc R U . . .
H22 H 0.6223 0.3387 0.5682 0.043 Uiso 1 1 calc R U . . .
C96 C 0.6179(5) 0.4526(5) 0.6017(4) 0.0373(18) Uani 1 1 d . . . . .
H74 H 0.5736 0.4378 0.6340 0.056 Uiso 1 1 calc R U . . .
H75 H 0.5876 0.4636 0.5599 0.056 Uiso 1 1 calc R U . . .
H76 H 0.6613 0.5008 0.6187 0.056 Uiso 1 1 calc R U . . .
C97 C 0.7163(5) 0.2176(4) 0.7396(4) 0.0311(16) Uani 1 1 d . . . . .
H23 H 0.6881 0.2601 0.7586 0.037 Uiso 1 1 calc R U . . .
H24 H 0.7423 0.1918 0.7771 0.037 Uiso 1 1 calc R U . . .
C98 C 0.6435(5) 0.1550(5) 0.7023(4) 0.0363(18) Uani 1 1 d . . . . .
H25 H 0.6673 0.1066 0.6907 0.044 Uiso 1 1 calc R U . . .
H26 H 0.6225 0.1766 0.6607 0.044 Uiso 1 1 calc R U . . .
C99 C 0.5664(6) 0.1329(6) 0.7452(4) 0.052(2) Uani 1 1 d . . . . .
H27 H 0.5881 0.1103 0.7861 0.063 Uiso 1 1 calc R U . . .
H28 H 0.5454 0.1824 0.7583 0.063 Uiso 1 1 calc R U . . .
C100 C 0.4886(6) 0.0728(5) 0.7114(4) 0.045(2) Uani 1 1 d . . . . .
H77 H 0.4697 0.0929 0.6691 0.067 Uiso 1 1 calc R U . . .
H78 H 0.4388 0.0652 0.7397 0.067 Uiso 1 1 calc R U . . .
H79 H 0.5069 0.0214 0.7032 0.067 Uiso 1 1 calc R U . . .
C101 C 0.8410(6) 0.1959(6) 0.6746(4) 0.048(2) Uani 1 1 d . . . . .
H29 H 0.7985 0.1566 0.6445 0.057 Uiso 1 1 calc R U . . .
H30 H 0.8877 0.2238 0.6476 0.057 Uiso 1 1 calc R U . . .
C102 C 0.8845(6) 0.1503(5) 0.7243(4) 0.045(2) Uani 1 1 d . . . . .
H31 H 0.9210 0.1885 0.7585 0.054 Uiso 1 1 calc R U . . .
H32 H 0.8379 0.1141 0.7463 0.054 Uiso 1 1 calc R U . . .
C103 C 0.9422(7) 0.1022(6) 0.6921(5) 0.056(3) Uani 1 1 d . . . . .
H33 H 0.9926 0.1391 0.6746 0.068 Uiso 1 1 calc R U . . .
H34 H 0.9071 0.0693 0.6541 0.068 Uiso 1 1 calc R U . . .
C104 C 0.9792(7) 0.0471(6) 0.7388(5) 0.059(3) Uani 1 1 d . . . . .
H80 H 1.0187 0.0796 0.7743 0.089 Uiso 1 1 calc R U . . .
H81 H 1.0131 0.0140 0.7144 0.089 Uiso 1 1 calc R U . . .
H82 H 0.9297 0.0122 0.7580 0.089 Uiso 1 1 calc R U . . .
C105 C 0.8496(5) 0.3168(5) 0.7496(4) 0.0412(19) Uani 1 1 d . . . . .
H35 H 0.8642 0.2883 0.7893 0.049 Uiso 1 1 calc R U . . .
H36 H 0.8148 0.3570 0.7635 0.049 Uiso 1 1 calc R U . . .
C106 C 0.9364(5) 0.3612(7) 0.7258(5) 0.064(3) Uani 1 1 d . . . . .
H37 H 0.9324 0.3513 0.6771 0.077 Uiso 1 1 calc R U . C 1
H38 H 0.9388 0.4194 0.7344 0.077 Uiso 1 1 calc R U . C 1
C17A C 1.0214(10) 0.3445(10) 0.7518(8) 0.021(5) Uiso 0.40(2) 1 d . . P D 1
H39A H 1.0373 0.3009 0.7241 0.025 Uiso 0.40(2) 1 calc R U P D 1
H40A H 1.0166 0.3265 0.7975 0.025 Uiso 0.40(2) 1 calc R U P D 1
C17B C 1.0031(8) 0.3892(8) 0.7725(6) 0.029(4) Uiso 0.60(2) 1 d . . P D 2
H39B H 1.0075 0.3452 0.8024 0.035 Uiso 0.60(2) 1 calc R U P D 2
H40B H 0.9851 0.4327 0.7991 0.035 Uiso 0.60(2) 1 calc R U P D 2
C108 C 1.0951(6) 0.4212(6) 0.7520(4) 0.051(2) Uani 1 1 d . . . . .
H87 H 1.1517 0.4062 0.7425 0.076 Uiso 1 1 calc R U . D 1
H88 H 1.1021 0.4498 0.7956 0.076 Uiso 1 1 calc R U . D 1
H89 H 1.0781 0.4561 0.7181 0.076 Uiso 1 1 calc R U . D 1
C109 C 0.6199(6) 0.6814(6) 0.7472(4) 0.047(2) Uani 1 1 d . . . . .
H83 H 0.6342 0.6306 0.7297 0.057 Uiso 1 1 calc R U . . .
H84 H 0.5575 0.6826 0.7313 0.057 Uiso 1 1 calc R U . . .
C110 C 0.6811(6) 0.7505(5) 0.7228(4) 0.0419(19) Uani 1 1 d . . . . .
H85 H 0.7430 0.7518 0.7415 0.050 Uiso 1 1 calc R U . . .
H86 H 0.6638 0.8012 0.7374 0.050 Uiso 1 1 calc R U . . .
N1 N 0.1171(4) 0.4904(3) 0.5846(2) 0.0230(12) Uani 1 1 d . . . . .
N2 N 0.2758(4) 0.6090(3) 0.5828(3) 0.0261(13) Uani 1 1 d . . . . .
N3 N 0.1729(4) 0.7306(4) 0.5707(3) 0.0280(13) Uani 1 1 d . . . . .
N4 N 0.0128(4) 0.6126(3) 0.5773(3) 0.0261(13) Uani 1 1 d . . . . .
N5 N 0.8839(4) 0.4571(3) 0.9144(3) 0.0238(12) Uani 1 1 d . . . . .
N6 N 0.7978(4) 0.2916(4) 0.9178(3) 0.0297(14) Uani 1 1 d . . . . .
N7 N 0.9674(4) 0.2464(3) 0.9245(3) 0.0269(13) Uani 1 1 d . . . . .
N8 N 1.0534(4) 0.4120(4) 0.9229(3) 0.0274(13) Uani 1 1 d . . . . .
N9 N 0.1093(4) 0.7279(4) 0.7841(3) 0.0301(14) Uani 1 1 d . . . . .
N10 N 0.7914(4) 0.2572(4) 0.7010(3) 0.0318(14) Uani 1 1 d . . . . .
O1 O -0.1187(3) 0.4137(3) 0.5441(2) 0.0266(10) Uani 1 1 d . . . . .
O2 O 1.0656(3) 0.6234(3) 0.9574(2) 0.0253(10) Uani 1 1 d . . . . .
F1 F 0.3267(3) 0.3810(3) 0.4928(2) 0.0391(11) Uani 1 1 d . . . . .
F2 F 0.4254(3) 0.2701(3) 0.5106(2) 0.0472(12) Uani 1 1 d . . . . .
F3 F 0.4817(3) 0.2382(3) 0.6334(2) 0.0452(12) Uani 1 1 d . . . . .
F4 F 0.4331(3) 0.3149(3) 0.7397(2) 0.0385(10) Uani 1 1 d . . . . .
F5 F 0.3256(3) 0.4193(3) 0.72307(19) 0.0343(10) Uani 1 1 d . . . . .
F6 F 0.4009(3) 0.8305(3) 0.4635(2) 0.0418(11) Uani 1 1 d . . . . .
F7 F 0.5505(3) 0.9410(3) 0.4672(3) 0.0513(13) Uani 1 1 d . . . . .
F8 F 0.6496(3) 0.9870(3) 0.5829(3) 0.0578(14) Uani 1 1 d . . . . .
F9 F 0.5991(3) 0.9163(3) 0.6939(3) 0.0543(14) Uani 1 1 d . . . . .
F10 F 0.4498(3) 0.8066(3) 0.6910(2) 0.0450(11) Uani 1 1 d . . . . .
F11 F 0.0041(3) 0.8362(3) 0.4528(2) 0.0393(11) Uani 1 1 d . . . . .
F12 F -0.0940(3) 0.9468(3) 0.4361(2) 0.0522(13) Uani 1 1 d . . . . .
F13 F -0.1864(3) 0.9891(3) 0.5353(3) 0.0580(15) Uani 1 1 d . . . . .
F14 F -0.1785(3) 0.9190(3) 0.6519(2) 0.0485(12) Uani 1 1 d . . . . .
F15 F -0.0763(3) 0.8124(3) 0.6711(2) 0.0362(10) Uani 1 1 d . . . . .
F16 F 0.6653(3) 0.4608(3) 0.78066(19) 0.0330(10) Uani 1 1 d . . . . .
F17 F 0.5077(3) 0.5010(3) 0.7578(2) 0.0391(11) Uani 1 1 d . . . . .
F18 F 0.3912(3) 0.4877(3) 0.8524(2) 0.0365(10) Uani 1 1 d . . . . .
F19 F 0.4349(2) 0.4350(3) 0.9705(2) 0.0323(9) Uani 1 1 d . . . . .
F20 F 0.5940(3) 0.3971(3) 0.9957(2) 0.0362(10) Uani 1 1 d . . . . .
F21 F 0.7473(4) 0.0483(3) 0.8212(2) 0.0598(15) Uani 1 1 d . . . . .
F22 F 0.6736(4) -0.1035(3) 0.8327(2) 0.0661(17) Uani 1 1 d . . . . .
F23 F 0.6628(3) -0.1651(3) 0.9519(2) 0.0463(12) Uani 1 1 d . . . . .
F24 F 0.7293(4) -0.0709(3) 1.0613(2) 0.0617(15) Uani 1 1 d . . . . .
F25 F 0.8034(4) 0.0819(3) 1.0507(2) 0.0565(14) Uani 1 1 d . . . . .
F26 F 1.1466(3) 0.2304(3) 0.7870(2) 0.0412(11) Uani 1 1 d . . . . .
F27 F 1.2930(3) 0.1816(3) 0.7550(2) 0.0446(12) Uani 1 1 d . . . . .
F28 F 1.4351(3) 0.1974(3) 0.8442(2) 0.0431(11) Uani 1 1 d . . . . .
F29 F 1.4294(3) 0.2646(3) 0.9651(2) 0.0351(10) Uani 1 1 d . . . . .
F30 F 1.2811(3) 0.3102(3) 1.00050(19) 0.0331(10) Uani 1 1 d . . . . .
Zn1 Zn 0.14369(5) 0.60785(5) 0.55894(4) 0.0255(2) Uani 1 1 d . . . . .
Zn2 Zn 0.92642(5) 0.35361(5) 0.93997(4) 0.0247(2) Uani 1 1 d . . . . .
Cl1 Cl 0.63035(17) 0.68521(14) 0.83491(11) 0.0540(6) Uani 1 1 d . . . . .
Cl2 Cl 0.67630(13) 0.74234(14) 0.63611(10) 0.0451(5) Uani 1 1 d . . . . .
C201 C 0.5429(13) 0.1083(10) 0.1333(7) 0.143(7) Uiso 1 1 d G . . . .
H20A H 0.5911 0.1452 0.1145 0.215 Uiso 1 1 calc R U . . .
H20B H 0.5598 0.1025 0.1801 0.215 Uiso 1 1 calc R U . . .
H20C H 0.4880 0.1298 0.1292 0.215 Uiso 1 1 calc R U . . .
C202 C 0.5284(15) 0.0328(8) 0.0989(8) 0.172(9) Uiso 1 1 d G . . . .
H20D H 0.4744 -0.0021 0.1137 0.207 Uiso 1 1 calc R U . . .
H20E H 0.5800 0.0070 0.1092 0.207 Uiso 1 1 calc R U . . .
C203 C 0.5153(14) 0.0415(11) 0.0203(7) 0.152(7) Uiso 1 1 d G . . . .
H20F H 0.4701 0.0750 0.0112 0.183 Uiso 1 1 calc R U . . .
H20G H 0.5724 0.0699 0.0050 0.183 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.308(8) . ?
C1 C2 1.408(9) . ?
C1 C20 1.408(10) . ?
C2 N1 1.373(9) . ?
C2 C3 1.409(9) . ?
C3 C4 1.345(10) . ?
C3 H1 0.9500 . ?
C4 C5 1.423(10) . ?
C4 H2 0.9500 . ?
C5 N1 1.347(8) . ?
C5 C6 1.395(9) . ?
C6 C7 1.355(10) . ?
C6 C21 1.491(9) . ?
C7 N2 1.385(8) . ?
C7 C8 1.434(10) . ?
C8 C9 1.336(10) . ?
C8 H3 0.9500 . ?
C9 C10 1.422(9) . ?
C9 H4 0.9500 . ?
C10 N2 1.370(9) . ?
C10 C11 1.397(10) . ?
C11 C12 1.373(9) . ?
C11 C27 1.492(9) . ?
C12 N3 1.386(9) . ?
C12 C13 1.419(10) . ?
C13 C14 1.354(10) . ?
C13 H5 0.9500 . ?
C14 C15 1.395(10) . ?
C14 H6 0.9500 . ?
C15 C16 1.365(10) . ?
C15 N3 1.374(8) . ?
C16 C17 1.392(10) . ?
C16 C33 1.494(9) . ?
C17 N4 1.354(8) . ?
C17 C18 1.409(10) . ?
C18 C19 1.355(10) . ?
C18 H7 0.9500 . ?
C19 C20 1.390(9) . ?
C19 H8 0.9500 . ?
C20 N4 1.361(9) . ?
C21 C26 1.361(9) . ?
C21 C22 1.375(10) . ?
C22 F1 1.345(8) . ?
C22 C23 1.349(9) . ?
C23 F2 1.333(8) . ?
C23 C24 1.371(10) . ?
C24 F3 1.335(8) . ?
C24 C25 1.350(11) . ?
C25 F4 1.325(8) . ?
C25 C26 1.387(9) . ?
C26 F5 1.337(8) . ?
C27 C28 1.366(10) . ?
C27 C32 1.373(10) . ?
C28 F6 1.335(9) . ?
C28 C29 1.366(11) . ?
C29 F7 1.325(9) . ?
C29 C30 1.357(12) . ?
C30 C31 1.341(12) . ?
C30 F8 1.343(9) . ?
C31 F9 1.330(9) . ?
C31 C32 1.365(11) . ?
C32 F10 1.324(8) . ?
C33 C34 1.366(10) . ?
C33 C38 1.367(10) . ?
C34 F11 1.339(8) . ?
C34 C35 1.384(10) . ?
C35 F12 1.334(9) . ?
C35 C36 1.363(11) . ?
C36 F13 1.323(8) . ?
C36 C37 1.342(11) . ?
C37 F14 1.336(8) . ?
C37 C38 1.357(10) . ?
C38 F15 1.347(8) . ?
C39 O2 1.299(8) . ?
C39 C40 1.401(9) . ?
C39 C58 1.408(9) . ?
C40 N5 1.354(9) . ?
C40 C41 1.408(9) . ?
C41 C42 1.357(10) . ?
C41 H9 0.9500 . ?
C42 C43 1.413(10) . ?
C42 H10 0.9500 . ?
C43 N5 1.358(8) . ?
C43 C44 1.391(9) . ?
C44 C45 1.366(10) . ?
C44 C59 1.496(9) . ?
C45 N6 1.366(8) . ?
C45 C46 1.429(10) . ?
C46 C47 1.324(10) . ?
C46 H11 0.9500 . ?
C47 C48 1.426(9) . ?
C47 H12 0.9500 . ?
C48 C49 1.354(9) . ?
C48 N6 1.379(9) . ?
C49 C50 1.379(9) . ?
C49 C65 1.499(9) . ?
C50 N7 1.360(9) . ?
C50 C51 1.424(9) . ?
C51 C52 1.334(10) . ?
C51 H13 0.9500 . ?
C52 C53 1.425(10) . ?
C52 H14 0.9500 . ?
C53 N7 1.363(8) . ?
C53 C54 1.370(10) . ?
C54 C55 1.394(10) . ?
C54 C71 1.487(9) . ?
C55 N8 1.351(8) . ?
C55 C56 1.402(9) . ?
C56 C57 1.360(10) . ?
C56 H15 0.9500 . ?
C57 C58 1.402(9) . ?
C57 H16 0.9500 . ?
C58 N8 1.371(9) . ?
C59 C64 1.364(9) . ?
C59 C60 1.381(10) . ?
C60 F16 1.340(8) . ?
C60 C61 1.363(9) . ?
C61 F17 1.335(7) . ?
C61 C62 1.342(9) . ?
C62 F18 1.341(7) . ?
C62 C63 1.342(9) . ?
C63 F19 1.323(8) . ?
C63 C64 1.385(9) . ?
C64 F20 1.335(7) . ?
C65 C66 1.344(10) . ?
C65 C70 1.378(10) . ?
C66 F21 1.330(8) . ?
C66 C67 1.363(10) . ?
C67 F22 1.314(8) . ?
C67 C68 1.358(10) . ?
C68 F23 1.319(8) . ?
C68 C69 1.348(10) . ?
C69 F24 1.338(8) . ?
C69 C70 1.357(10) . ?
C70 F25 1.342(8) . ?
C71 C72 1.356(10) . ?
C71 C76 1.394(10) . ?
C72 F26 1.333(8) . ?
C72 C73 1.381(10) . ?
C73 F27 1.332(8) . ?
C73 C74 1.352(11) . ?
C74 F28 1.329(8) . ?
C74 C75 1.357(10) . ?
C75 F29 1.325(8) . ?
C75 C76 1.362(10) . ?
C76 F30 1.336(8) . ?
C77 N9 1.494(9) . ?
C77 C78 1.517(12) . ?
C77 H41 0.9900 . ?
C77 H42 0.9900 . ?
C78 C79 1.476(12) . ?
C78 H43 0.9900 . ?
C78 H44 0.9900 . ?
C79 C80A 1.38(2) . ?
C79 C80B 1.69(3) . ?
C79 H45 0.9900 . ?
C79 H46 0.9900 . ?
C80A H80A 0.9800 . ?
C80A H80B 0.9800 . ?
C80A H80C 0.9800 . ?
C80B H80D 0.9800 . ?
C80B H80E 0.9800 . ?
C80B H80F 0.9800 . ?
C81 C82 1.510(10) . ?
C81 N9 1.514(9) . ?
C81 H47 0.9900 . ?
C81 H48 0.9900 . ?
C82 C83 1.506(10) . ?
C82 H49 0.9900 . ?
C82 H50 0.9900 . ?
C83 C84 1.506(10) . ?
C83 H51 0.9900 . ?
C83 H52 0.9900 . ?
C84 H65 0.9800 . ?
C84 H66 0.9800 . ?
C84 H67 0.9800 . ?
C85 N9 1.500(9) . ?
C85 C86 1.509(10) . ?
C85 H53 0.9900 . ?
C85 H54 0.9900 . ?
C86 C87 1.491(10) . ?
C86 H55 0.9900 . ?
C86 H56 0.9900 . ?
C87 C88 1.514(11) . ?
C87 H57 0.9900 . ?
C87 H58 0.9900 . ?
C88 H68 0.9800 . ?
C88 H69 0.9800 . ?
C88 H70 0.9800 . ?
C89 N9 1.499(9) . ?
C89 C90 1.519(11) . ?
C89 H59 0.9900 . ?
C89 H60 0.9900 . ?
C90 C91 1.511(12) . ?
C90 H61 0.9900 . ?
C90 H62 0.9900 . ?
C91 C92 1.518(16) . ?
C91 H63 0.9900 . ?
C91 H64 0.9900 . ?
C92 H71 0.9800 . ?
C92 H72 0.9800 . ?
C92 H73 0.9800 . ?
C93 C94 1.488(10) . ?
C93 N10 1.494(9) . ?
C93 H17 0.9900 . ?
C93 H18 0.9900 . ?
C94 C95 1.539(10) . ?
C94 H19 0.9900 . ?
C94 H20 0.9900 . ?
C95 C96 1.487(10) . ?
C95 H21 0.9900 . ?
C95 H22 0.9900 . ?
C96 H74 0.9800 . ?
C96 H75 0.9800 . ?
C96 H76 0.9800 . ?
C97 N10 1.502(9) . ?
C97 C98 1.513(11) . ?
C97 H23 0.9900 . ?
C97 H24 0.9900 . ?
C98 C99 1.514(11) . ?
C98 H25 0.9900 . ?
C98 H26 0.9900 . ?
C99 C100 1.508(12) . ?
C99 H27 0.9900 . ?
C99 H28 0.9900 . ?
C100 H77 0.9800 . ?
C100 H78 0.9800 . ?
C100 H79 0.9800 . ?
C101 C102 1.491(11) . ?
C101 N10 1.508(10) . ?
C101 H29 0.9900 . ?
C101 H30 0.9900 . ?
C102 C103 1.484(12) . ?
C102 H31 0.9900 . ?
C102 H32 0.9900 . ?
C103 C104 1.515(12) . ?
C103 H33 0.9900 . ?
C103 H34 0.9900 . ?
C104 H80 0.9800 . ?
C104 H81 0.9800 . ?
C104 H82 0.9800 . ?
C105 N10 1.493(10) . ?
C105 C106 1.514(11) . ?
C105 H35 0.9900 . ?
C105 H36 0.9900 . ?
C106 C17B 1.341(15) . ?
C106 C17A 1.453(17) . ?
C106 H37 0.9900 . ?
C106 H38 0.9900 . ?
C17A C108 1.544(18) . ?
C17A H39A 0.9900 . ?
C17A H40A 0.9900 . ?
C17B C108 1.501(14) . ?
C17B H39B 0.9900 . ?
C17B H40B 0.9900 . ?
C108 H87 0.9800 . ?
C108 H88 0.9800 . ?
C108 H89 0.9800 . ?
C109 C110 1.477(12) . ?
C109 Cl1 1.772(9) . ?
C109 H83 0.9900 . ?
C109 H84 0.9900 . ?
C110 Cl2 1.753(9) . ?
C110 H85 0.9900 . ?
C110 H86 0.9900 . ?
N1 Zn1 2.052(6) . ?
N2 Zn1 2.041(5) . ?
N3 Zn1 2.045(6) . ?
N4 Zn1 2.080(6) . ?
N5 Zn2 2.063(6) . ?
N6 Zn2 2.050(6) . ?
N7 Zn2 2.058(6) . ?
N8 Zn2 2.060(6) . ?
O1 Zn1 2.100(5) 2_566 ?
O2 Zn2 2.092(5) 2_767 ?
Zn1 O1 2.100(5) 2_566 ?
Zn2 O2 2.092(5) 2_767 ?
C201 C202 1.4032 . ?
C201 H20A 0.9800 . ?
C201 H20B 0.9800 . ?
C201 H20C 0.9800 . ?
C202 C203 1.6080 . ?
C202 H20D 0.9900 . ?
C202 H20E 0.9900 . ?
C203 C203 1.57(3) 2_655 ?
C203 H20F 0.9900 . ?
C203 H20G 0.9900 . ?

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
O1 C1 C2 118.1(6) . . ?
O1 C1 C20 117.2(6) . . ?
C2 C1 C20 124.7(6) . . ?
N1 C2 C1 124.7(6) . . ?
N1 C2 C3 110.0(6) . . ?
C1 C2 C3 125.3(6) . . ?
C4 C3 C2 107.3(6) . . ?
C4 C3 H1 126.4 . . ?
C2 C3 H1 126.4 . . ?
C3 C4 C5 106.5(6) . . ?
C3 C4 H2 126.8 . . ?
C5 C4 H2 126.8 . . ?
N1 C5 C6 123.7(6) . . ?
N1 C5 C4 110.6(6) . . ?
C6 C5 C4 125.7(6) . . ?
C7 C6 C5 128.0(6) . . ?
C7 C6 C21 115.5(6) . . ?
C5 C6 C21 116.5(6) . . ?
C6 C7 N2 123.7(6) . . ?
C6 C7 C8 126.7(6) . . ?
N2 C7 C8 109.6(6) . . ?
C9 C8 C7 107.4(6) . . ?
C9 C8 H3 126.3 . . ?
C7 C8 H3 126.3 . . ?
C8 C9 C10 107.1(7) . . ?
C8 C9 H4 126.4 . . ?
C10 C9 H4 126.4 . . ?
N2 C10 C11 123.8(6) . . ?
N2 C10 C9 110.9(6) . . ?
C11 C10 C9 125.3(7) . . ?
C12 C11 C10 126.9(7) . . ?
C12 C11 C27 116.9(6) . . ?
C10 C11 C27 116.0(6) . . ?
C11 C12 N3 124.4(6) . . ?
C11 C12 C13 126.2(7) . . ?
N3 C12 C13 109.4(6) . . ?
C14 C13 C12 106.5(7) . . ?
C14 C13 H5 126.8 . . ?
C12 C13 H5 126.8 . . ?
C13 C14 C15 108.7(7) . . ?
C13 C14 H6 125.7 . . ?
C15 C14 H6 125.7 . . ?
C16 C15 N3 123.6(6) . . ?
C16 C15 C14 126.7(6) . . ?
N3 C15 C14 109.6(6) . . ?
C15 C16 C17 128.3(6) . . ?
C15 C16 C33 116.2(6) . . ?
C17 C16 C33 115.2(6) . . ?
N4 C17 C16 123.9(6) . . ?
N4 C17 C18 109.1(6) . . ?
C16 C17 C18 126.8(6) . . ?
C19 C18 C17 107.9(6) . . ?
C19 C18 H7 126.1 . . ?
C17 C18 H7 126.1 . . ?
C18 C19 C20 105.8(7) . . ?
C18 C19 H8 127.1 . . ?
C20 C19 H8 127.1 . . ?
N4 C20 C19 111.2(6) . . ?
N4 C20 C1 124.4(6) . . ?
C19 C20 C1 124.1(7) . . ?
C26 C21 C22 115.9(6) . . ?
C26 C21 C6 122.0(6) . . ?
C22 C21 C6 122.0(6) . . ?
F1 C22 C23 117.5(6) . . ?
F1 C22 C21 119.4(6) . . ?
C23 C22 C21 123.1(6) . . ?
F2 C23 C22 121.0(7) . . ?
F2 C23 C24 119.9(6) . . ?
C22 C23 C24 119.1(7) . . ?
F3 C24 C25 120.2(7) . . ?
F3 C24 C23 119.2(7) . . ?
C25 C24 C23 120.6(6) . . ?
F4 C25 C24 120.7(6) . . ?
F4 C25 C26 120.8(6) . . ?
C24 C25 C26 118.5(6) . . ?
F5 C26 C21 120.8(6) . . ?
F5 C26 C25 116.4(6) . . ?
C21 C26 C25 122.7(7) . . ?
C28 C27 C32 115.9(7) . . ?
C28 C27 C11 121.4(6) . . ?
C32 C27 C11 122.7(6) . . ?
F6 C28 C27 119.8(7) . . ?
F6 C28 C29 117.6(7) . . ?
C27 C28 C29 122.7(7) . . ?
F7 C29 C30 120.7(7) . . ?
F7 C29 C28 120.4(7) . . ?
C30 C29 C28 118.9(8) . . ?
C31 C30 F8 119.6(8) . . ?
C31 C30 C29 120.7(8) . . ?
F8 C30 C29 119.7(8) . . ?
F9 C31 C30 120.7(7) . . ?
F9 C31 C32 119.9(7) . . ?
C30 C31 C32 119.4(7) . . ?
F10 C32 C31 117.8(7) . . ?
F10 C32 C27 119.8(7) . . ?
C31 C32 C27 122.4(7) . . ?
C34 C33 C38 115.2(6) . . ?
C34 C33 C16 120.9(6) . . ?
C38 C33 C16 123.9(6) . . ?
F11 C34 C33 120.5(6) . . ?
F11 C34 C35 116.6(7) . . ?
C33 C34 C35 122.9(7) . . ?
F12 C35 C36 121.6(7) . . ?
F12 C35 C34 119.7(7) . . ?
C36 C35 C34 118.7(7) . . ?
F13 C36 C37 121.7(7) . . ?
F13 C36 C35 118.5(7) . . ?
C37 C36 C35 119.8(7) . . ?
F14 C37 C36 119.5(6) . . ?
F14 C37 C38 120.3(7) . . ?
C36 C37 C38 120.1(7) . . ?
F15 C38 C37 116.7(6) . . ?
F15 C38 C33 120.0(6) . . ?
C37 C38 C33 123.3(7) . . ?
O2 C39 C40 117.7(6) . . ?
O2 C39 C58 118.1(6) . . ?
C40 C39 C58 124.1(7) . . ?
N5 C40 C39 125.6(6) . . ?
N5 C40 C41 109.9(6) . . ?
C39 C40 C41 124.5(7) . . ?
C42 C41 C40 107.3(6) . . ?
C42 C41 H9 126.3 . . ?
C40 C41 H9 126.3 . . ?
C41 C42 C43 106.1(6) . . ?
C41 C42 H10 127.0 . . ?
C43 C42 H10 127.0 . . ?
N5 C43 C44 123.6(6) . . ?
N5 C43 C42 110.3(6) . . ?
C44 C43 C42 125.6(6) . . ?
C45 C44 C43 128.5(6) . . ?
C45 C44 C59 115.8(6) . . ?
C43 C44 C59 115.7(6) . . ?
C44 C45 N6 123.9(6) . . ?
C44 C45 C46 126.6(6) . . ?
N6 C45 C46 109.5(6) . . ?
C47 C46 C45 107.2(6) . . ?
C47 C46 H11 126.4 . . ?
C45 C46 H11 126.4 . . ?
C46 C47 C48 108.5(6) . . ?
C46 C47 H12 125.8 . . ?
C48 C47 H12 125.8 . . ?
C49 C48 N6 124.0(6) . . ?
C49 C48 C47 127.5(7) . . ?
N6 C48 C47 108.4(6) . . ?
C48 C49 C50 127.8(7) . . ?
C48 C49 C65 116.3(6) . . ?
C50 C49 C65 115.8(6) . . ?
N7 C50 C49 124.4(6) . . ?
N7 C50 C51 108.6(6) . . ?
C49 C50 C51 126.8(6) . . ?
C52 C51 C50 108.1(6) . . ?
C52 C51 H13 125.9 . . ?
C50 C51 H13 125.9 . . ?
C51 C52 C53 106.8(6) . . ?
C51 C52 H14 126.6 . . ?
C53 C52 H14 126.6 . . ?
N7 C53 C54 124.6(6) . . ?
N7 C53 C52 109.4(6) . . ?
C54 C53 C52 126.0(6) . . ?
C53 C54 C55 127.7(6) . . ?
C53 C54 C71 115.4(6) . . ?
C55 C54 C71 116.7(6) . . ?
N8 C55 C54 123.6(6) . . ?
N8 C55 C56 109.7(6) . . ?
C54 C55 C56 126.7(6) . . ?
C57 C56 C55 108.0(6) . . ?
C57 C56 H15 126.0 . . ?
C55 C56 H15 126.0 . . ?
C56 C57 C58 105.8(6) . . ?
C56 C57 H16 127.1 . . ?
C58 C57 H16 127.1 . . ?
N8 C58 C57 110.4(6) . . ?
N8 C58 C39 124.3(6) . . ?
C57 C58 C39 125.3(6) . . ?
C64 C59 C60 115.7(6) . . ?
C64 C59 C44 122.5(6) . . ?
C60 C59 C44 121.8(6) . . ?
F16 C60 C61 118.1(6) . . ?
F16 C60 C59 119.6(6) . . ?
C61 C60 C59 122.2(6) . . ?
F17 C61 C62 121.3(6) . . ?
F17 C61 C60 119.2(6) . . ?
C62 C61 C60 119.4(6) . . ?
F18 C62 C61 119.7(6) . . ?
F18 C62 C63 118.6(6) . . ?
C61 C62 C63 121.7(6) . . ?
F19 C63 C62 121.5(6) . . ?
F19 C63 C64 120.4(6) . . ?
C62 C63 C64 118.1(6) . . ?
F20 C64 C59 120.3(6) . . ?
F20 C64 C63 116.8(6) . . ?
C59 C64 C63 122.9(6) . . ?
C66 C65 C70 115.1(6) . . ?
C66 C65 C49 123.3(6) . . ?
C70 C65 C49 121.6(6) . . ?
F21 C66 C65 119.4(6) . . ?
F21 C66 C67 116.9(7) . . ?
C65 C66 C67 123.7(7) . . ?
F22 C67 C68 120.4(7) . . ?
F22 C67 C66 120.4(7) . . ?
C68 C67 C66 119.3(7) . . ?
F23 C68 C69 120.9(7) . . ?
F23 C68 C67 119.7(7) . . ?
C69 C68 C67 119.3(7) . . ?
F24 C69 C68 119.9(7) . . ?
F24 C69 C70 120.3(7) . . ?
C68 C69 C70 119.8(7) . . ?
F25 C70 C69 117.0(6) . . ?
F25 C70 C65 120.2(6) . . ?
C69 C70 C65 122.8(7) . . ?
C72 C71 C76 115.7(6) . . ?
C72 C71 C54 121.5(6) . . ?
C76 C71 C54 122.7(6) . . ?
F26 C72 C71 120.0(6) . . ?
F26 C72 C73 116.8(6) . . ?
C71 C72 C73 123.1(6) . . ?
F27 C73 C74 120.8(6) . . ?
F27 C73 C72 120.0(7) . . ?
C74 C73 C72 119.2(7) . . ?
F28 C74 C73 119.6(7) . . ?
F28 C74 C75 120.6(7) . . ?
C73 C74 C75 119.8(7) . . ?
F29 C75 C74 119.1(6) . . ?
F29 C75 C76 120.5(7) . . ?
C74 C75 C76 120.4(6) . . ?
F30 C76 C75 118.5(6) . . ?
F30 C76 C71 119.7(6) . . ?
C75 C76 C71 121.7(6) . . ?
N9 C77 C78 114.8(6) . . ?
N9 C77 H41 108.6 . . ?
C78 C77 H41 108.6 . . ?
N9 C77 H42 108.6 . . ?
C78 C77 H42 108.6 . . ?
H41 C77 H42 107.5 . . ?
C79 C78 C77 113.0(7) . . ?
C79 C78 H43 109.0 . . ?
C77 C78 H43 109.0 . . ?
C79 C78 H44 109.0 . . ?
C77 C78 H44 109.0 . . ?
H43 C78 H44 107.8 . . ?
C80A C79 C78 125.2(13) . . ?
C78 C79 C80B 98.7(13) . . ?
C80A C79 H45 106.0 . . ?
C78 C79 H45 106.0 . . ?
C80A C79 H46 106.0 . . ?
C78 C79 H46 106.0 . . ?
H45 C79 H46 106.3 . . ?
C79 C80A H80A 109.5 . . ?
C79 C80A H80B 109.5 . . ?
H80A C80A H80B 109.5 . . ?
C79 C80A H80C 109.5 . . ?
H80A C80A H80C 109.5 . . ?
H80B C80A H80C 109.5 . . ?
C79 C80B H80D 109.5 . . ?
C79 C80B H80E 109.5 . . ?
H80D C80B H80E 109.5 . . ?
C79 C80B H80F 109.5 . . ?
H80D C80B H80F 109.5 . . ?
H80E C80B H80F 109.5 . . ?
C82 C81 N9 115.1(6) . . ?
C82 C81 H47 108.5 . . ?
N9 C81 H47 108.5 . . ?
C82 C81 H48 108.5 . . ?
N9 C81 H48 108.5 . . ?
H47 C81 H48 107.5 . . ?
C83 C82 C81 109.8(6) . . ?
C83 C82 H49 109.7 . . ?
C81 C82 H49 109.7 . . ?
C83 C82 H50 109.7 . . ?
C81 C82 H50 109.7 . . ?
H49 C82 H50 108.2 . . ?
C84 C83 C82 111.8(6) . . ?
C84 C83 H51 109.3 . . ?
C82 C83 H51 109.3 . . ?
C84 C83 H52 109.3 . . ?
C82 C83 H52 109.3 . . ?
H51 C83 H52 107.9 . . ?
C83 C84 H65 109.5 . . ?
C83 C84 H66 109.5 . . ?
H65 C84 H66 109.5 . . ?
C83 C84 H67 109.5 . . ?
H65 C84 H67 109.5 . . ?
H66 C84 H67 109.5 . . ?
N9 C85 C86 113.7(5) . . ?
N9 C85 H53 108.8 . . ?
C86 C85 H53 108.8 . . ?
N9 C85 H54 108.8 . . ?
C86 C85 H54 108.8 . . ?
H53 C85 H54 107.7 . . ?
C87 C86 C85 113.0(6) . . ?
C87 C86 H55 109.0 . . ?
C85 C86 H55 109.0 . . ?
C87 C86 H56 109.0 . . ?
C85 C86 H56 109.0 . . ?
H55 C86 H56 107.8 . . ?
C86 C87 C88 115.2(7) . . ?
C86 C87 H57 108.5 . . ?
C88 C87 H57 108.5 . . ?
C86 C87 H58 108.5 . . ?
C88 C87 H58 108.5 . . ?
H57 C87 H58 107.5 . . ?
C87 C88 H68 109.5 . . ?
C87 C88 H69 109.5 . . ?
H68 C88 H69 109.5 . . ?
C87 C88 H70 109.5 . . ?
H68 C88 H70 109.5 . . ?
H69 C88 H70 109.5 . . ?
N9 C89 C90 115.3(6) . . ?
N9 C89 H59 108.4 . . ?
C90 C89 H59 108.4 . . ?
N9 C89 H60 108.4 . . ?
C90 C89 H60 108.4 . . ?
H59 C89 H60 107.5 . . ?
C91 C90 C89 110.6(8) . . ?
C91 C90 H61 109.5 . . ?
C89 C90 H61 109.5 . . ?
C91 C90 H62 109.5 . . ?
C89 C90 H62 109.5 . . ?
H61 C90 H62 108.1 . . ?
C90 C91 C92 114.5(9) . . ?
C90 C91 H63 108.6 . . ?
C92 C91 H63 108.6 . . ?
C90 C91 H64 108.6 . . ?
C92 C91 H64 108.6 . . ?
H63 C91 H64 107.6 . . ?
C91 C92 H71 109.5 . . ?
C91 C92 H72 109.5 . . ?
H71 C92 H72 109.5 . . ?
C91 C92 H73 109.5 . . ?
H71 C92 H73 109.5 . . ?
H72 C92 H73 109.5 . . ?
C94 C93 N10 116.5(6) . . ?
C94 C93 H17 108.2 . . ?
N10 C93 H17 108.2 . . ?
C94 C93 H18 108.2 . . ?
N10 C93 H18 108.2 . . ?
H17 C93 H18 107.3 . . ?
C93 C94 C95 110.4(6) . . ?
C93 C94 H19 109.6 . . ?
C95 C94 H19 109.6 . . ?
C93 C94 H20 109.6 . . ?
C95 C94 H20 109.6 . . ?
H19 C94 H20 108.1 . . ?
C96 C95 C94 111.7(6) . . ?
C96 C95 H21 109.3 . . ?
C94 C95 H21 109.3 . . ?
C96 C95 H22 109.3 . . ?
C94 C95 H22 109.3 . . ?
H21 C95 H22 107.9 . . ?
C95 C96 H74 109.5 . . ?
C95 C96 H75 109.5 . . ?
H74 C96 H75 109.5 . . ?
C95 C96 H76 109.5 . . ?
H74 C96 H76 109.5 . . ?
H75 C96 H76 109.5 . . ?
N10 C97 C98 116.9(6) . . ?
N10 C97 H23 108.1 . . ?
C98 C97 H23 108.1 . . ?
N10 C97 H24 108.1 . . ?
C98 C97 H24 108.1 . . ?
H23 C97 H24 107.3 . . ?
C97 C98 C99 109.3(7) . . ?
C97 C98 H25 109.8 . . ?
C99 C98 H25 109.8 . . ?
C97 C98 H26 109.8 . . ?
C99 C98 H26 109.8 . . ?
H25 C98 H26 108.3 . . ?
C100 C99 C98 113.4(8) . . ?
C100 C99 H27 108.9 . . ?
C98 C99 H27 108.9 . . ?
C100 C99 H28 108.9 . . ?
C98 C99 H28 108.9 . . ?
H27 C99 H28 107.7 . . ?
C99 C100 H77 109.5 . . ?
C99 C100 H78 109.5 . . ?
H77 C100 H78 109.5 . . ?
C99 C100 H79 109.5 . . ?
H77 C100 H79 109.5 . . ?
H78 C100 H79 109.5 . . ?
C102 C101 N10 117.0(7) . . ?
C102 C101 H29 108.1 . . ?
N10 C101 H29 108.1 . . ?
C102 C101 H30 108.1 . . ?
N10 C101 H30 108.1 . . ?
H29 C101 H30 107.3 . . ?
C103 C102 C101 110.8(7) . . ?
C103 C102 H31 109.5 . . ?
C101 C102 H31 109.5 . . ?
C103 C102 H32 109.5 . . ?
C101 C102 H32 109.5 . . ?
H31 C102 H32 108.1 . . ?
C102 C103 C104 112.8(8) . . ?
C102 C103 H33 109.0 . . ?
C104 C103 H33 109.0 . . ?
C102 C103 H34 109.0 . . ?
C104 C103 H34 109.0 . . ?
H33 C103 H34 107.8 . . ?
C103 C104 H80 109.5 . . ?
C103 C104 H81 109.5 . . ?
H80 C104 H81 109.5 . . ?
C103 C104 H82 109.5 . . ?
H80 C104 H82 109.5 . . ?
H81 C104 H82 109.5 . . ?
N10 C105 C106 116.2(8) . . ?
N10 C105 H35 108.2 . . ?
C106 C105 H35 108.2 . . ?
N10 C105 H36 108.2 . . ?
C106 C105 H36 108.2 . . ?
H35 C105 H36 107.4 . . ?
C17B C106 C105 116.4(9) . . ?
C17A C106 C105 120.4(9) . . ?
C17A C106 H37 107.2 . . ?
C105 C106 H37 107.2 . . ?
C17A C106 H38 107.2 . . ?
C105 C106 H38 107.2 . . ?
H37 C106 H38 106.9 . . ?
C106 C17A C108 109.8(12) . . ?
C106 C17A H39A 109.7 . . ?
C108 C17A H39A 109.7 . . ?
C106 C17A H40A 109.7 . . ?
C108 C17A H40A 109.7 . . ?
H39A C17A H40A 108.2 . . ?
C106 C17B C108 119.1(10) . . ?
C106 C17B H39B 107.5 . . ?
C108 C17B H39B 107.5 . . ?
C106 C17B H40B 107.5 . . ?
C108 C17B H40B 107.5 . . ?
H39B C17B H40B 107.0 . . ?
C17A C108 H87 109.5 . . ?
C17A C108 H88 109.5 . . ?
H87 C108 H88 109.5 . . ?
C17A C108 H89 109.5 . . ?
H87 C108 H89 109.5 . . ?
H88 C108 H89 109.5 . . ?
C110 C109 Cl1 110.2(6) . . ?
C110 C109 H83 109.6 . . ?
Cl1 C109 H83 109.6 . . ?
C110 C109 H84 109.6 . . ?
Cl1 C109 H84 109.6 . . ?
H83 C109 H84 108.1 . . ?
C109 C110 Cl2 109.8(6) . . ?
C109 C110 H85 109.7 . . ?
Cl2 C110 H85 109.7 . . ?
C109 C110 H86 109.7 . . ?
Cl2 C110 H86 109.7 . . ?
H85 C110 H86 108.2 . . ?
C5 N1 C2 105.7(6) . . ?
C5 N1 Zn1 127.4(5) . . ?
C2 N1 Zn1 124.1(4) . . ?
C10 N2 C7 104.9(6) . . ?
C10 N2 Zn1 127.3(4) . . ?
C7 N2 Zn1 127.2(5) . . ?
C15 N3 C12 105.9(5) . . ?
C15 N3 Zn1 126.8(4) . . ?
C12 N3 Zn1 125.9(4) . . ?
C17 N4 C20 105.9(5) . . ?
C17 N4 Zn1 126.2(5) . . ?
C20 N4 Zn1 124.3(4) . . ?
C40 N5 C43 106.3(6) . . ?
C40 N5 Zn2 123.6(4) . . ?
C43 N5 Zn2 126.6(5) . . ?
C45 N6 C48 106.4(6) . . ?
C45 N6 Zn2 127.0(5) . . ?
C48 N6 Zn2 125.5(4) . . ?
C50 N7 C53 107.0(6) . . ?
C50 N7 Zn2 125.5(4) . . ?
C53 N7 Zn2 127.2(5) . . ?
C55 N8 C58 106.1(6) . . ?
C55 N8 Zn2 127.8(5) . . ?
C58 N8 Zn2 124.5(4) . . ?
C77 N9 C89 110.8(6) . . ?
C77 N9 C85 106.5(5) . . ?
C89 N9 C85 111.0(6) . . ?
C77 N9 C81 111.3(6) . . ?
C89 N9 C81 106.3(5) . . ?
C85 N9 C81 111.0(6) . . ?
C105 N10 C93 111.2(6) . . ?
C105 N10 C97 104.5(6) . . ?
C93 N10 C97 112.7(6) . . ?
C105 N10 C101 111.6(6) . . ?
C93 N10 C101 106.4(6) . . ?
C97 N10 C101 110.6(6) . . ?
C1 O1 Zn1 114.4(4) . 2_566 ?
C39 O2 Zn2 113.3(4) . 2_767 ?
N2 Zn1 N3 88.2(2) . . ?
N2 Zn1 N1 87.8(2) . . ?
N3 Zn1 N1 158.7(2) . . ?
N2 Zn1 N4 156.0(2) . . ?
N3 Zn1 N4 87.7(2) . . ?
N1 Zn1 N4 87.6(2) . . ?
N2 Zn1 O1 107.9(2) . 2_566 ?
N3 Zn1 O1 103.3(2) . 2_566 ?
N1 Zn1 O1 97.86(19) . 2_566 ?
N4 Zn1 O1 96.0(2) . 2_566 ?
N6 Zn2 N7 87.6(2) . . ?
N6 Zn2 N8 157.8(2) . . ?
N7 Zn2 N8 88.1(2) . . ?
N6 Zn2 N5 88.3(2) . . ?
N7 Zn2 N5 156.8(2) . . ?
N8 Zn2 N5 87.1(2) . . ?
N6 Zn2 O2 103.6(2) . 2_767 ?
N7 Zn2 O2 106.5(2) . 2_767 ?
N8 Zn2 O2 98.5(2) . 2_767 ?
N5 Zn2 O2 96.7(2) . 2_767 ?
C202 C201 H20A 109.5 . . ?
C202 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
C202 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
C201 C202 C203 111.0 . . ?
C201 C202 H20D 109.4 . . ?
C203 C202 H20D 109.4 . . ?
C201 C202 H20E 109.4 . . ?
C203 C202 H20E 109.4 . . ?
H20D C202 H20E 108.0 . . ?
C203 C203 C202 113(2) 2_655 . ?
C203 C203 H20F 108.9 2_655 . ?
C202 C203 H20F 108.9 . . ?
C203 C203 H20G 108.9 2_655 . ?
C202 C203 H20G 108.9 . . ?
H20F C203 H20G 107.7 . . ?

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
O1 C1 C2 N1 168.3(6) . . . . ?
C20 C1 C2 N1 -14.7(10) . . . . ?
O1 C1 C2 C3 -9.5(10) . . . . ?
C20 C1 C2 C3 167.4(6) . . . . ?
N1 C2 C3 C4 0.4(8) . . . . ?
C1 C2 C3 C4 178.5(6) . . . . ?
C2 C3 C4 C5 -1.7(8) . . . . ?
C3 C4 C5 N1 2.6(8) . . . . ?
C3 C4 C5 C6 -173.9(7) . . . . ?
N1 C5 C6 C7 -2.2(12) . . . . ?
C4 C5 C6 C7 173.9(7) . . . . ?
N1 C5 C6 C21 179.0(6) . . . . ?
C4 C5 C6 C21 -4.9(10) . . . . ?
C5 C6 C7 N2 0.3(12) . . . . ?
C21 C6 C7 N2 179.1(6) . . . . ?
C5 C6 C7 C8 178.0(7) . . . . ?
C21 C6 C7 C8 -3.1(10) . . . . ?
C6 C7 C8 C9 -179.1(7) . . . . ?
N2 C7 C8 C9 -1.1(8) . . . . ?
C7 C8 C9 C10 1.2(8) . . . . ?
C8 C9 C10 N2 -0.9(9) . . . . ?
C8 C9 C10 C11 179.0(7) . . . . ?
N2 C10 C11 C12 4.6(12) . . . . ?
C9 C10 C11 C12 -175.3(7) . . . . ?
N2 C10 C11 C27 179.3(6) . . . . ?
C9 C10 C11 C27 -0.5(11) . . . . ?
C10 C11 C12 N3 -0.9(12) . . . . ?
C27 C11 C12 N3 -175.6(6) . . . . ?
C10 C11 C12 C13 176.9(7) . . . . ?
C27 C11 C12 C13 2.2(11) . . . . ?
C11 C12 C13 C14 -177.3(7) . . . . ?
N3 C12 C13 C14 0.9(9) . . . . ?
C12 C13 C14 C15 -0.6(9) . . . . ?
C13 C14 C15 C16 176.9(7) . . . . ?
C13 C14 C15 N3 0.1(9) . . . . ?
N3 C15 C16 C17 -3.7(12) . . . . ?
C14 C15 C16 C17 179.9(7) . . . . ?
N3 C15 C16 C33 -177.5(6) . . . . ?
C14 C15 C16 C33 6.2(11) . . . . ?
C15 C16 C17 N4 1.7(12) . . . . ?
C33 C16 C17 N4 175.5(6) . . . . ?
C15 C16 C17 C18 -172.7(7) . . . . ?
C33 C16 C17 C18 1.1(10) . . . . ?
N4 C17 C18 C19 -4.2(8) . . . . ?
C16 C17 C18 C19 170.8(7) . . . . ?
C17 C18 C19 C20 2.5(8) . . . . ?
C18 C19 C20 N4 0.0(8) . . . . ?
C18 C19 C20 C1 -174.1(6) . . . . ?
O1 C1 C20 N4 -166.7(6) . . . . ?
C2 C1 C20 N4 16.3(10) . . . . ?
O1 C1 C20 C19 6.5(10) . . . . ?
C2 C1 C20 C19 -170.5(7) . . . . ?
C7 C6 C21 C26 91.2(9) . . . . ?
C5 C6 C21 C26 -89.8(9) . . . . ?
C7 C6 C21 C22 -88.7(9) . . . . ?
C5 C6 C21 C22 90.3(9) . . . . ?
C26 C21 C22 F1 180.0(7) . . . . ?
C6 C21 C22 F1 -0.1(11) . . . . ?
C26 C21 C22 C23 -1.3(12) . . . . ?
C6 C21 C22 C23 178.6(7) . . . . ?
F1 C22 C23 F2 -1.8(12) . . . . ?
C21 C22 C23 F2 179.4(7) . . . . ?
F1 C22 C23 C24 177.9(7) . . . . ?
C21 C22 C23 C24 -0.9(13) . . . . ?
F2 C23 C24 F3 1.7(11) . . . . ?
C22 C23 C24 F3 -178.0(7) . . . . ?
F2 C23 C24 C25 -179.8(7) . . . . ?
C22 C23 C24 C25 0.5(12) . . . . ?
F3 C24 C25 F4 -0.1(12) . . . . ?
C23 C24 C25 F4 -178.6(7) . . . . ?
F3 C24 C25 C26 -179.5(7) . . . . ?
C23 C24 C25 C26 2.1(12) . . . . ?
C22 C21 C26 F5 -179.0(6) . . . . ?
C6 C21 C26 F5 1.1(11) . . . . ?
C22 C21 C26 C25 3.9(11) . . . . ?
C6 C21 C26 C25 -175.9(7) . . . . ?
F4 C25 C26 F5 -0.9(10) . . . . ?
C24 C25 C26 F5 178.4(7) . . . . ?
F4 C25 C26 C21 176.3(7) . . . . ?
C24 C25 C26 C21 -4.4(11) . . . . ?
C12 C11 C27 C28 -75.7(9) . . . . ?
C10 C11 C27 C28 109.0(8) . . . . ?
C12 C11 C27 C32 104.1(8) . . . . ?
C10 C11 C27 C32 -71.2(9) . . . . ?
C32 C27 C28 F6 180.0(6) . . . . ?
C11 C27 C28 F6 -0.2(11) . . . . ?
C32 C27 C28 C29 -0.2(11) . . . . ?
C11 C27 C28 C29 179.6(7) . . . . ?
F6 C28 C29 F7 -0.6(11) . . . . ?
C27 C28 C29 F7 179.6(7) . . . . ?
F6 C28 C29 C30 -179.5(7) . . . . ?
C27 C28 C29 C30 0.7(12) . . . . ?
F7 C29 C30 C31 -179.3(7) . . . . ?
C28 C29 C30 C31 -0.5(12) . . . . ?
F7 C29 C30 F8 3.1(11) . . . . ?
C28 C29 C30 F8 -178.0(7) . . . . ?
F8 C30 C31 F9 -1.7(11) . . . . ?
C29 C30 C31 F9 -179.3(7) . . . . ?
F8 C30 C31 C32 177.3(7) . . . . ?
C29 C30 C31 C32 -0.2(12) . . . . ?
F9 C31 C32 F10 -0.3(10) . . . . ?
C30 C31 C32 F10 -179.3(7) . . . . ?
F9 C31 C32 C27 179.8(7) . . . . ?
C30 C31 C32 C27 0.7(11) . . . . ?
C28 C27 C32 F10 179.6(6) . . . . ?
C11 C27 C32 F10 -0.3(10) . . . . ?
C28 C27 C32 C31 -0.5(11) . . . . ?
C11 C27 C32 C31 179.7(7) . . . . ?
C15 C16 C33 C34 65.2(9) . . . . ?
C17 C16 C33 C34 -109.4(8) . . . . ?
C15 C16 C33 C38 -116.2(8) . . . . ?
C17 C16 C33 C38 69.2(9) . . . . ?
C38 C33 C34 F11 -179.3(7) . . . . ?
C16 C33 C34 F11 -0.6(11) . . . . ?
C38 C33 C34 C35 0.5(11) . . . . ?
C16 C33 C34 C35 179.2(7) . . . . ?
F11 C34 C35 F12 -0.5(11) . . . . ?
C33 C34 C35 F12 179.7(7) . . . . ?
F11 C34 C35 C36 178.4(7) . . . . ?
C33 C34 C35 C36 -1.4(13) . . . . ?
F12 C35 C36 F13 -1.2(13) . . . . ?
C34 C35 C36 F13 179.9(8) . . . . ?
F12 C35 C36 C37 -179.8(8) . . . . ?
C34 C35 C36 C37 1.3(13) . . . . ?
F13 C36 C37 F14 1.7(12) . . . . ?
C35 C36 C37 F14 -179.8(8) . . . . ?
F13 C36 C37 C38 -179.0(8) . . . . ?
C35 C36 C37 C38 -0.4(13) . . . . ?
F14 C37 C38 F15 -2.1(11) . . . . ?
C36 C37 C38 F15 178.5(7) . . . . ?
F14 C37 C38 C33 178.9(7) . . . . ?
C36 C37 C38 C33 -0.5(12) . . . . ?
C34 C33 C38 F15 -178.5(6) . . . . ?
C16 C33 C38 F15 2.8(11) . . . . ?
C34 C33 C38 C37 0.4(11) . . . . ?
C16 C33 C38 C37 -178.2(7) . . . . ?
O2 C39 C40 N5 -170.5(6) . . . . ?
C58 C39 C40 N5 11.4(11) . . . . ?
O2 C39 C40 C41 6.4(10) . . . . ?
C58 C39 C40 C41 -171.6(6) . . . . ?
N5 C40 C41 C42 -2.2(8) . . . . ?
C39 C40 C41 C42 -179.6(6) . . . . ?
C40 C41 C42 C43 2.6(8) . . . . ?
C41 C42 C43 N5 -2.2(8) . . . . ?
C41 C42 C43 C44 169.8(6) . . . . ?
N5 C43 C44 C45 3.0(11) . . . . ?
C42 C43 C44 C45 -168.1(7) . . . . ?
N5 C43 C44 C59 -176.8(6) . . . . ?
C42 C43 C44 C59 12.1(10) . . . . ?
C43 C44 C45 N6 -1.7(12) . . . . ?
C59 C44 C45 N6 178.1(6) . . . . ?
C43 C44 C45 C46 178.0(7) . . . . ?
C59 C44 C45 C46 -2.3(11) . . . . ?
C44 C45 C46 C47 -177.8(7) . . . . ?
N6 C45 C46 C47 1.9(9) . . . . ?
C45 C46 C47 C48 -2.1(9) . . . . ?
C46 C47 C48 C49 -174.6(8) . . . . ?
C46 C47 C48 N6 1.7(9) . . . . ?
N6 C48 C49 C50 -4.4(12) . . . . ?
C47 C48 C49 C50 171.3(7) . . . . ?
N6 C48 C49 C65 178.9(6) . . . . ?
C47 C48 C49 C65 -5.4(11) . . . . ?
C48 C49 C50 N7 5.6(12) . . . . ?
C65 C49 C50 N7 -177.7(6) . . . . ?
C48 C49 C50 C51 -168.8(7) . . . . ?
C65 C49 C50 C51 8.0(11) . . . . ?
N7 C50 C51 C52 -2.9(8) . . . . ?
C49 C50 C51 C52 172.2(7) . . . . ?
C50 C51 C52 C53 2.7(8) . . . . ?
C51 C52 C53 N7 -1.6(8) . . . . ?
C51 C52 C53 C54 178.1(7) . . . . ?
N7 C53 C54 C55 3.2(12) . . . . ?
C52 C53 C54 C55 -176.5(7) . . . . ?
N7 C53 C54 C71 -172.3(6) . . . . ?
C52 C53 C54 C71 8.1(10) . . . . ?
C53 C54 C55 N8 -5.4(11) . . . . ?
C71 C54 C55 N8 170.0(6) . . . . ?
C53 C54 C55 C56 173.0(7) . . . . ?
C71 C54 C55 C56 -11.6(10) . . . . ?
N8 C55 C56 C57 2.6(8) . . . . ?
C54 C55 C56 C57 -176.0(6) . . . . ?
C55 C56 C57 C58 -1.8(7) . . . . ?
C56 C57 C58 N8 0.4(7) . . . . ?
C56 C57 C58 C39 -178.3(6) . . . . ?
O2 C39 C58 N8 168.0(6) . . . . ?
C40 C39 C58 N8 -14.0(10) . . . . ?
O2 C39 C58 C57 -13.5(10) . . . . ?
C40 C39 C58 C57 164.5(6) . . . . ?
C45 C44 C59 C64 69.4(9) . . . . ?
C43 C44 C59 C64 -110.8(8) . . . . ?
C45 C44 C59 C60 -112.2(8) . . . . ?
C43 C44 C59 C60 67.7(9) . . . . ?
C64 C59 C60 F16 -179.2(6) . . . . ?
C44 C59 C60 F16 2.3(10) . . . . ?
C64 C59 C60 C61 -1.2(11) . . . . ?
C44 C59 C60 C61 -179.8(7) . . . . ?
F16 C60 C61 F17 0.1(10) . . . . ?
C59 C60 C61 F17 -177.8(7) . . . . ?
F16 C60 C61 C62 177.6(6) . . . . ?
C59 C60 C61 C62 -0.4(11) . . . . ?
F17 C61 C62 F18 -2.2(11) . . . . ?
C60 C61 C62 F18 -179.6(6) . . . . ?
F17 C61 C62 C63 178.3(7) . . . . ?
C60 C61 C62 C63 0.9(11) . . . . ?
F18 C62 C63 F19 -1.6(11) . . . . ?
C61 C62 C63 F19 177.9(7) . . . . ?
F18 C62 C63 C64 -179.4(6) . . . . ?
C61 C62 C63 C64 0.2(11) . . . . ?
C60 C59 C64 F20 -176.9(6) . . . . ?
C44 C59 C64 F20 1.7(11) . . . . ?
C60 C59 C64 C63 2.4(11) . . . . ?
C44 C59 C64 C63 -179.1(7) . . . . ?
F19 C63 C64 F20 -0.4(10) . . . . ?
C62 C63 C64 F20 177.4(6) . . . . ?
F19 C63 C64 C59 -179.7(6) . . . . ?
C62 C63 C64 C59 -1.9(11) . . . . ?
C48 C49 C65 C66 82.3(9) . . . . ?
C50 C49 C65 C66 -94.8(9) . . . . ?
C48 C49 C65 C70 -97.7(8) . . . . ?
C50 C49 C65 C70 85.2(9) . . . . ?
C70 C65 C66 F21 179.0(7) . . . . ?
C49 C65 C66 F21 -1.0(11) . . . . ?
C70 C65 C66 C67 -1.0(11) . . . . ?
C49 C65 C66 C67 179.0(7) . . . . ?
F21 C66 C67 F22 0.7(12) . . . . ?
C65 C66 C67 F22 -179.2(7) . . . . ?
F21 C66 C67 C68 -178.9(7) . . . . ?
C65 C66 C67 C68 1.2(13) . . . . ?
F22 C67 C68 F23 1.0(12) . . . . ?
C66 C67 C68 F23 -179.5(7) . . . . ?
F22 C67 C68 C69 179.9(7) . . . . ?
C66 C67 C68 C69 -0.6(12) . . . . ?
F23 C68 C69 F24 0.0(11) . . . . ?
C67 C68 C69 F24 -178.9(7) . . . . ?
F23 C68 C69 C70 178.8(7) . . . . ?
C67 C68 C69 C70 -0.1(12) . . . . ?
F24 C69 C70 F25 -2.1(11) . . . . ?
C68 C69 C70 F25 179.0(7) . . . . ?
F24 C69 C70 C65 179.1(7) . . . . ?
C68 C69 C70 C65 0.2(12) . . . . ?
C66 C65 C70 F25 -178.5(7) . . . . ?
C49 C65 C70 F25 1.5(10) . . . . ?
C66 C65 C70 C69 0.3(11) . . . . ?
C49 C65 C70 C69 -179.7(7) . . . . ?
C53 C54 C71 C72 69.4(9) . . . . ?
C55 C54 C71 C72 -106.6(8) . . . . ?
C53 C54 C71 C76 -110.2(8) . . . . ?
C55 C54 C71 C76 73.9(9) . . . . ?
C76 C71 C72 F26 -179.7(6) . . . . ?
C54 C71 C72 F26 0.8(11) . . . . ?
C76 C71 C72 C73 0.8(11) . . . . ?
C54 C71 C72 C73 -178.7(7) . . . . ?
F26 C72 C73 F27 -0.1(11) . . . . ?
C71 C72 C73 F27 179.4(7) . . . . ?
F26 C72 C73 C74 179.2(7) . . . . ?
C71 C72 C73 C74 -1.3(12) . . . . ?
F27 C73 C74 F28 -1.1(11) . . . . ?
C72 C73 C74 F28 179.5(7) . . . . ?
F27 C73 C74 C75 179.1(7) . . . . ?
C72 C73 C74 C75 -0.2(12) . . . . ?
F28 C74 C75 F29 0.3(11) . . . . ?
C73 C74 C75 F29 -179.9(7) . . . . ?
F28 C74 C75 C76 -177.6(7) . . . . ?
C73 C74 C75 C76 2.1(11) . . . . ?
F29 C75 C76 F30 0.1(10) . . . . ?
C74 C75 C76 F30 178.0(6) . . . . ?
F29 C75 C76 C71 179.5(6) . . . . ?
C74 C75 C76 C71 -2.6(11) . . . . ?
C72 C71 C76 F30 -179.5(6) . . . . ?
C54 C71 C76 F30 0.0(10) . . . . ?
C72 C71 C76 C75 1.1(11) . . . . ?
C54 C71 C76 C75 -179.4(7) . . . . ?
N9 C77 C78 C79 -169.0(8) . . . . ?
C77 C78 C79 C80A 51.6(17) . . . . ?
C77 C78 C79 C80B 85.5(13) . . . . ?
N9 C81 C82 C83 -174.8(6) . . . . ?
C81 C82 C83 C84 -173.1(7) . . . . ?
N9 C85 C86 C87 168.8(6) . . . . ?
C85 C86 C87 C88 -66.0(8) . . . . ?
N9 C89 C90 C91 174.6(8) . . . . ?
C89 C90 C91 C92 -64.5(12) . . . . ?
N10 C93 C94 C95 -170.6(6) . . . . ?
C93 C94 C95 C96 -174.9(7) . . . . ?
N10 C97 C98 C99 -169.9(7) . . . . ?
C97 C98 C99 C100 177.9(7) . . . . ?
N10 C101 C102 C103 -171.0(8) . . . . ?
C101 C102 C103 C104 -173.1(9) . . . . ?
N10 C105 C106 C17B -154.7(10) . . . . ?
N10 C105 C106 C17A -109.6(13) . . . . ?
C105 C106 C17A C108 -149.3(11) . . . . ?
C105 C106 C17B C108 169.7(10) . . . . ?
Cl1 C109 C110 Cl2 175.7(4) . . . . ?
C6 C5 N1 C2 174.3(6) . . . . ?
C4 C5 N1 C2 -2.3(7) . . . . ?
C6 C5 N1 Zn1 13.2(10) . . . . ?
C4 C5 N1 Zn1 -163.4(5) . . . . ?
C1 C2 N1 C5 -177.0(6) . . . . ?
C3 C2 N1 C5 1.2(7) . . . . ?
C1 C2 N1 Zn1 -15.1(9) . . . . ?
C3 C2 N1 Zn1 163.0(4) . . . . ?
C11 C10 N2 C7 -179.7(7) . . . . ?
C9 C10 N2 C7 0.2(8) . . . . ?
C11 C10 N2 Zn1 8.6(10) . . . . ?
C9 C10 N2 Zn1 -171.5(5) . . . . ?
C6 C7 N2 C10 178.6(6) . . . . ?
C8 C7 N2 C10 0.6(7) . . . . ?
C6 C7 N2 Zn1 -9.7(10) . . . . ?
C8 C7 N2 Zn1 172.3(5) . . . . ?
C16 C15 N3 C12 -176.5(7) . . . . ?
C14 C15 N3 C12 0.4(8) . . . . ?
C16 C15 N3 Zn1 16.3(10) . . . . ?
C14 C15 N3 Zn1 -166.8(5) . . . . ?
C11 C12 N3 C15 177.4(7) . . . . ?
C13 C12 N3 C15 -0.8(8) . . . . ?
C11 C12 N3 Zn1 -15.3(10) . . . . ?
C13 C12 N3 Zn1 166.6(5) . . . . ?
C16 C17 N4 C20 -171.1(6) . . . . ?
C18 C17 N4 C20 4.1(7) . . . . ?
C16 C17 N4 Zn1 -12.1(9) . . . . ?
C18 C17 N4 Zn1 163.1(4) . . . . ?
C19 C20 N4 C17 -2.5(7) . . . . ?
C1 C20 N4 C17 171.5(6) . . . . ?
C19 C20 N4 Zn1 -162.1(5) . . . . ?
C1 C20 N4 Zn1 11.9(9) . . . . ?
C39 C40 N5 C43 178.2(6) . . . . ?
C41 C40 N5 C43 0.8(7) . . . . ?
C39 C40 N5 Zn2 18.2(9) . . . . ?
C41 C40 N5 Zn2 -159.2(4) . . . . ?
C44 C43 N5 C40 -171.4(6) . . . . ?
C42 C43 N5 C40 0.9(7) . . . . ?
C44 C43 N5 Zn2 -12.2(9) . . . . ?
C42 C43 N5 Zn2 160.1(5) . . . . ?
C44 C45 N6 C48 178.9(7) . . . . ?
C46 C45 N6 C48 -0.8(8) . . . . ?
C44 C45 N6 Zn2 9.8(10) . . . . ?
C46 C45 N6 Zn2 -169.9(5) . . . . ?
C49 C48 N6 C45 176.0(7) . . . . ?
C47 C48 N6 C45 -0.4(8) . . . . ?
C49 C48 N6 Zn2 -14.8(10) . . . . ?
C47 C48 N6 Zn2 168.8(5) . . . . ?
C49 C50 N7 C53 -173.4(6) . . . . ?
C51 C50 N7 C53 1.8(7) . . . . ?
C49 C50 N7 Zn2 12.5(10) . . . . ?
C51 C50 N7 Zn2 -172.3(4) . . . . ?
C54 C53 N7 C50 -179.9(6) . . . . ?
C52 C53 N7 C50 -0.2(7) . . . . ?
C54 C53 N7 Zn2 -5.9(10) . . . . ?
C52 C53 N7 Zn2 173.8(4) . . . . ?
C54 C55 N8 C58 176.4(6) . . . . ?
C56 C55 N8 C58 -2.3(7) . . . . ?
C54 C55 N8 Zn2 10.3(9) . . . . ?
C56 C55 N8 Zn2 -168.4(4) . . . . ?
C57 C58 N8 C55 1.2(7) . . . . ?
C39 C58 N8 C55 179.9(6) . . . . ?
C57 C58 N8 Zn2 167.8(4) . . . . ?
C39 C58 N8 Zn2 -13.4(9) . . . . ?
C78 C77 N9 C89 -51.2(9) . . . . ?
C78 C77 N9 C85 -172.0(7) . . . . ?
C78 C77 N9 C81 66.8(8) . . . . ?
C90 C89 N9 C77 -58.2(9) . . . . ?
C90 C89 N9 C85 59.9(9) . . . . ?
C90 C89 N9 C81 -179.2(7) . . . . ?
C86 C85 N9 C77 -177.3(6) . . . . ?
C86 C85 N9 C89 62.0(8) . . . . ?
C86 C85 N9 C81 -56.0(8) . . . . ?
C82 C81 N9 C77 69.5(8) . . . . ?
C82 C81 N9 C89 -169.8(6) . . . . ?
C82 C81 N9 C85 -49.0(8) . . . . ?
C106 C105 N10 C93 -63.5(9) . . . . ?
C106 C105 N10 C97 174.7(7) . . . . ?
C106 C105 N10 C101 55.1(9) . . . . ?
C94 C93 N10 C105 -59.8(8) . . . . ?
C94 C93 N10 C97 57.1(9) . . . . ?
C94 C93 N10 C101 178.5(7) . . . . ?
C98 C97 N10 C105 178.0(6) . . . . ?
C98 C97 N10 C93 57.2(8) . . . . ?
C98 C97 N10 C101 -61.7(8) . . . . ?
C102 C101 N10 C105 55.1(10) . . . . ?
C102 C101 N10 C93 176.6(8) . . . . ?
C102 C101 N10 C97 -60.8(10) . . . . ?
C2 C1 O1 Zn1 -91.9(6) . . . 2_566 ?
C20 C1 O1 Zn1 91.0(6) . . . 2_566 ?
C40 C39 O2 Zn2 88.6(6) . . . 2_767 ?
C58 C39 O2 Zn2 -93.3(6) . . . 2_767 ?
C201 C202 C203 C203 -172(3) . . . 2_655 ?

_refine_diff_density_max         2.216
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.173



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_180131_ys-4-1_rev
_database_code_depnum_ccdc_archive 'CCDC 1906679'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H8 F15 N4 O Pd, C28 H30 N3'
_chemical_formula_sum            'C66 H38 F15 N7 O Pd'
_chemical_formula_weight         1336.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.7734 1.2009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.8987(2)
_cell_length_b                   18.5720(5)
_cell_length_c                   32.3929(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.213(2)
_cell_angle_gamma                90
_cell_volume                     5353.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    22814
_cell_measurement_theta_min      1.390
_cell_measurement_theta_max      28.101

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_F_000             2688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.576
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.78192
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            22814
_diffrn_reflns_av_unetI/netI     0.1690
_diffrn_reflns_av_R_equivalents  0.1270
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.390
_diffrn_reflns_theta_max         28.101
_diffrn_reflns_theta_full        27.979
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             9642
_reflns_number_gt                5342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1339P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9642
_refine_ls_number_parameters     814
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.0878
_refine_ls_wR_factor_ref         0.2495
_refine_ls_wR_factor_gt          0.2039
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C3 C 0.4192(9) 0.7105(5) 0.2640(3) 0.0352(19) Uani 1 1 d . . . . .
C5 C 0.4516(8) 0.5800(4) 0.2803(2) 0.0301(18) Uani 1 1 d . . . . .
F10 F 0.3979(5) 0.4441(2) 0.43935(14) 0.0394(11) Uani 1 1 d . . . . .
F12 F 1.1785(5) 0.7085(3) 0.53272(15) 0.0494(13) Uani 1 1 d . . . . .
Pd1 Pd 0.57635(6) 0.68172(3) 0.34623(2) 0.0320(2) Uani 1 1 d . . . . .
C16 C 0.8005(8) 0.8527(5) 0.4076(2) 0.0359(19) Uani 1 1 d . . . . .
H16 H 0.8679 0.8712 0.4278 0.043 Uiso 1 1 calc R U . . .
F1 F 0.1104(5) 0.6298(3) 0.22610(14) 0.0432(12) Uani 1 1 d . . . . .
C15 C 0.7431(8) 0.7811(4) 0.4058(2) 0.0337(19) Uani 1 1 d . . . . .
C23 C 0.1754(9) 0.5964(4) 0.1593(3) 0.039(2) Uani 1 1 d . . . . .
C27 C 0.5818(8) 0.4277(4) 0.3874(2) 0.0322(18) Uani 1 1 d . . . . .
C31 C 0.4886(9) 0.3280(4) 0.4291(3) 0.036(2) Uani 1 1 d . . . . .
C34 C 0.9746(9) 0.7186(5) 0.4864(2) 0.0362(19) Uani 1 1 d . . . . .
F4 F 0.5362(6) 0.5644(3) 0.11348(15) 0.0529(13) Uani 1 1 d . . . . .
F6 F 0.7660(5) 0.3976(2) 0.33777(13) 0.0381(11) Uani 1 1 d . . . . .
C21 C 0.3673(8) 0.6162(4) 0.2114(3) 0.0347(19) Uani 1 1 d . . . . .
C28 C 0.6715(8) 0.3763(4) 0.3679(2) 0.0322(18) Uani 1 1 d . . . . .
F7 F 0.7638(5) 0.2589(3) 0.35875(14) 0.0442(12) Uani 1 1 d . . . . .
C14 C 0.7644(8) 0.7264(4) 0.4347(2) 0.0304(18) Uani 1 1 d . . . . .
F5 F 0.6185(5) 0.5984(3) 0.19045(14) 0.0461(12) Uani 1 1 d . . . . .
C10 C 0.6338(8) 0.5543(5) 0.4035(2) 0.0343(19) Uani 1 1 d . . . . .
F8 F 0.5781(6) 0.2106(3) 0.41945(14) 0.0470(12) Uani 1 1 d . . . . .
F9 F 0.3986(5) 0.3048(3) 0.45962(14) 0.0456(12) Uani 1 1 d . . . . .
C9 C 0.5785(8) 0.5039(4) 0.3750(2) 0.0281(17) Uani 1 1 d . . . . .
F3 F 0.2414(6) 0.5634(3) 0.09137(14) 0.0497(13) Uani 1 1 d . . . . .
C33 C 0.8396(8) 0.7484(4) 0.4738(2) 0.0343(19) Uani 1 1 d . . . . .
F2 F 0.0280(5) 0.5956(3) 0.14895(15) 0.0511(13) Uani 1 1 d . . . . .
F11 F 1.0358(5) 0.6662(3) 0.46415(14) 0.0436(12) Uani 1 1 d . . . . .
C32 C 0.4900(8) 0.3996(4) 0.4188(2) 0.0349(19) Uani 1 1 d . . . . .
F13 F 1.0522(6) 0.8090(3) 0.58215(15) 0.0552(14) Uani 1 1 d . . . . .
C4 C 0.4138(8) 0.6359(5) 0.2539(2) 0.0327(19) Uani 1 1 d . . . . .
C13 C 0.7190(8) 0.6559(4) 0.4306(2) 0.0298(17) Uani 1 1 d . . . . .
C17 C 0.7412(9) 0.8897(5) 0.3751(3) 0.039(2) Uani 1 1 d . . . . .
H17 H 0.7601 0.9386 0.3683 0.047 Uiso 1 1 calc R U . . .
F14 F 0.7856(6) 0.8705(3) 0.56092(16) 0.0570(14) Uani 1 1 d . . . . .
F15 F 0.6451(5) 0.8306(3) 0.49101(14) 0.0435(12) Uani 1 1 d . . . . .
N1 N 0.6559(6) 0.6269(3) 0.39526(19) 0.0290(15) Uani 1 1 d . . . . .
N2 N 0.5059(7) 0.5878(4) 0.31999(19) 0.0328(16) Uani 1 1 d . . . . .
N3 N 0.4883(6) 0.7374(4) 0.2987(2) 0.0317(15) Uani 1 1 d . . . . .
N4 N 0.6553(7) 0.7745(4) 0.3710(2) 0.0398(17) Uani 1 1 d . . . . .
O1 O 0.5281(6) 0.9304(3) 0.31461(17) 0.0427(14) Uani 1 1 d . . . . .
C22 C 0.2178(9) 0.6130(5) 0.1986(3) 0.037(2) Uani 1 1 d . . . . .
C44 C 0.8339(9) 0.5807(5) 0.2798(3) 0.038(2) Uani 1 1 d . . . . .
H44 H 0.7712 0.5456 0.2671 0.046 Uiso 1 1 calc R U . . .
C55 C 1.0073(8) 0.6820(5) 0.3187(2) 0.0330(18) Uani 1 1 d . . . . .
C57 C 1.0917(9) 0.7349(4) 0.3399(3) 0.036(2) Uani 1 1 d . . . . .
N5 N 1.1233(7) 0.5905(4) 0.3601(2) 0.0373(16) Uani 1 1 d . . . . .
N6 N 0.8981(7) 0.7754(4) 0.2750(2) 0.0376(17) Uani 1 1 d . . . . .
N7 N 1.2507(8) 0.8405(4) 0.3827(2) 0.0404(17) Uani 1 1 d . . . . .
C2 C 0.3584(8) 0.7662(4) 0.2399(2) 0.0330(18) Uani 1 1 d . . . . .
H2 H 0.3054 0.7609 0.2146 0.040 Uiso 1 1 calc R U . . .
C1 C 0.3896(8) 0.8296(4) 0.2597(2) 0.0356(19) Uani 1 1 d . . . . .
H1 H 0.3614 0.8766 0.2510 0.043 Uiso 1 1 calc R U . . .
C6 C 0.4345(9) 0.5056(5) 0.2709(2) 0.0368(19) Uani 1 1 d . . . . .
H6 H 0.4012 0.4856 0.2454 0.044 Uiso 1 1 calc R U . . .
C7 C 0.4754(8) 0.4688(4) 0.3055(2) 0.0343(19) Uani 1 1 d . . . . .
H7 H 0.4730 0.4180 0.3090 0.041 Uiso 1 1 calc R U . . .
C8 C 0.5230(8) 0.5209(4) 0.3360(2) 0.0302(18) Uani 1 1 d . . . . .
C11 C 0.6828(8) 0.5387(5) 0.4452(2) 0.0361(19) Uani 1 1 d . . . . .
H11 H 0.6805 0.4931 0.4584 0.043 Uiso 1 1 calc R U . . .
C12 C 0.7325(8) 0.6012(4) 0.4618(2) 0.0335(18) Uani 1 1 d . . . . .
H12 H 0.7695 0.6078 0.4891 0.040 Uiso 1 1 calc R U . . .
C18 C 0.6459(9) 0.8415(4) 0.3534(2) 0.0356(19) Uani 1 1 d . . . . .
C19 C 0.5462(9) 0.8631(5) 0.3208(3) 0.040(2) Uani 1 1 d . . . . .
C20 C 0.4724(9) 0.8112(4) 0.2955(2) 0.0327(18) Uani 1 1 d . . . . .
C24 C 0.2831(9) 0.5805(4) 0.1298(3) 0.0362(19) Uani 1 1 d . . . . .
C25 C 0.4318(10) 0.5812(4) 0.1413(3) 0.040(2) Uani 1 1 d . . . . .
C26 C 0.4705(9) 0.5996(5) 0.1812(3) 0.0365(19) Uani 1 1 d . . . . .
C29 C 0.6694(9) 0.3047(5) 0.3776(2) 0.0341(19) Uani 1 1 d . . . . .
C30 C 0.5790(9) 0.2803(4) 0.4093(3) 0.0364(19) Uani 1 1 d . . . . .
C35 C 1.0459(9) 0.7397(5) 0.5218(3) 0.040(2) Uani 1 1 d . . . . .
C36 C 0.9827(10) 0.7915(5) 0.5470(3) 0.041(2) Uani 1 1 d . . . . .
C37 C 0.8493(10) 0.8206(5) 0.5360(3) 0.043(2) Uani 1 1 d . . . . .
C38 C 0.7793(9) 0.8002(4) 0.5001(3) 0.036(2) Uani 1 1 d . . . . .
C39 C 1.0649(10) 0.9499(5) 0.3029(3) 0.046(2) Uani 1 1 d . . . . .
H39 H 1.0624 0.9985 0.2936 0.055 Uiso 1 1 calc R U . . .
C40 C 0.9806(9) 0.8986(5) 0.2815(3) 0.044(2) Uani 1 1 d . . . . .
H40 H 0.9217 0.9124 0.2583 0.052 Uiso 1 1 calc R U . . .
C41 C 0.9835(9) 0.8277(5) 0.2942(3) 0.039(2) Uani 1 1 d . . . . .
C42 C 0.9061(9) 0.7031(4) 0.2863(3) 0.0355(19) Uani 1 1 d . . . . .
C43 C 0.8191(9) 0.6503(5) 0.2666(3) 0.041(2) Uani 1 1 d . . . . .
H43 H 0.7520 0.6625 0.2448 0.050 Uiso 1 1 calc R U . . .
C45 C 0.9308(9) 0.5574(5) 0.3095(3) 0.039(2) Uani 1 1 d . . . . .
H45 H 0.9371 0.5079 0.3166 0.047 Uiso 1 1 calc R U . . .
C46 C 1.0217(9) 0.6094(5) 0.3295(3) 0.040(2) Uani 1 1 d . . . . .
C47 C 1.1980(9) 0.6407(5) 0.3835(3) 0.038(2) Uani 1 1 d . . . . .
C48 C 1.2880(9) 0.6227(5) 0.4170(3) 0.040(2) Uani 1 1 d . . . . .
H48 H 1.3036 0.5736 0.4241 0.048 Uiso 1 1 calc R U . . .
C49 C 1.3555(9) 0.6775(5) 0.4400(3) 0.044(2) Uani 1 1 d . . . . .
H49 H 1.4126 0.6645 0.4637 0.052 Uiso 1 1 calc R U . . .
C50 C 1.3436(9) 0.7491(5) 0.4302(3) 0.045(2) Uani 1 1 d . . . . .
H50 H 1.3917 0.7845 0.4468 0.054 Uiso 1 1 calc R U . . .
C51 C 1.2603(9) 0.7693(5) 0.3958(3) 0.038(2) Uani 1 1 d . . . . .
C52 C 1.1616(9) 0.8620(5) 0.3500(3) 0.040(2) Uani 1 1 d . . . . .
C53 C 1.1531(10) 0.9329(5) 0.3376(3) 0.046(2) Uani 1 1 d . . . . .
H53 H 1.2058 0.9695 0.3522 0.055 Uiso 1 1 calc R U . . .
C54 C 1.0769(9) 0.8082(5) 0.3276(3) 0.037(2) Uani 1 1 d . . . . .
C56 C 1.1835(9) 0.7155(5) 0.3728(3) 0.0363(19) Uani 1 1 d . . . . .
C58 C 0.7961(10) 0.7943(5) 0.2408(3) 0.044(2) Uani 1 1 d . . . . .
H58 H 0.7671 0.8456 0.2431 0.053 Uiso 1 1 calc R U . . .
H58A H 0.7036 0.7649 0.2427 0.053 Uiso 1 1 calc R U . . .
C59 C 0.8696(9) 0.7816(5) 0.1992(2) 0.045(2) Uani 1 1 d . . . . .
H59 H 0.9148 0.7329 0.1989 0.054 Uiso 1 1 calc R U . . .
H59A H 0.9513 0.8171 0.1953 0.054 Uiso 1 1 calc R U . . .
C60 C 0.7560(10) 0.7882(6) 0.1635(3) 0.058(3) Uani 1 1 d . . . . .
H60 H 0.6710 0.7558 0.1685 0.086 Uiso 1 1 calc R U . . .
H60A H 0.8049 0.7751 0.1375 0.086 Uiso 1 1 calc R U . . .
H60B H 0.7197 0.8380 0.1618 0.086 Uiso 1 1 calc R U . . .
C61 C 1.1422(9) 0.5133(4) 0.3707(3) 0.042(2) Uani 1 1 d . . . . .
H61 H 1.2452 0.5050 0.3813 0.051 Uiso 1 1 calc R U . . .
H61A H 1.1284 0.4836 0.3456 0.051 Uiso 1 1 calc R U . . .
C62 C 1.0295(9) 0.4915(5) 0.4027(3) 0.045(2) Uani 1 1 d . . . . .
H62 H 0.9275 0.5046 0.3930 0.054 Uiso 1 1 calc R U . . .
H62A H 1.0497 0.5182 0.4285 0.054 Uiso 1 1 calc R U . . .
C63 C 1.0348(10) 0.4105(5) 0.4116(3) 0.057(3) Uani 1 1 d . . . . .
H63 H 1.0180 0.3838 0.3859 0.086 Uiso 1 1 calc R U . . .
H63A H 0.9564 0.3981 0.4315 0.086 Uiso 1 1 calc R U . . .
H63B H 1.1335 0.3979 0.4230 0.086 Uiso 1 1 calc R U . . .
C64 C 1.3335(10) 0.8952(5) 0.4065(3) 0.045(2) Uani 1 1 d . . . . .
H64 H 1.3593 0.9359 0.3881 0.054 Uiso 1 1 calc R U . . .
H64A H 1.4284 0.8741 0.4169 0.054 Uiso 1 1 calc R U . . .
C65 C 1.2412(11) 0.9230(6) 0.4428(3) 0.061(3) Uani 1 1 d . . . . .
H65 H 1.1588 0.9539 0.4323 0.073 Uiso 1 1 calc R U . . .
H65A H 1.1955 0.8818 0.4575 0.073 Uiso 1 1 calc R U . . .
C66 C 1.3381(12) 0.9661(6) 0.4728(3) 0.069(3) Uani 1 1 d . . . . .
H66 H 1.4264 0.9376 0.4806 0.104 Uiso 1 1 calc R U . . .
H66A H 1.2795 0.9775 0.4975 0.104 Uiso 1 1 calc R U . . .
H66B H 1.3706 1.0109 0.4595 0.104 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C3 N3 1.372(10) . ?
C3 C2 1.404(11) . ?
C3 C4 1.424(12) . ?
C5 N2 1.379(9) . ?
C5 C4 1.386(11) . ?
C5 C6 1.422(11) . ?
F10 C32 1.342(9) . ?
F12 C35 1.360(9) . ?
Pd1 N3 2.011(6) . ?
Pd1 N1 2.013(6) . ?
Pd1 N4 2.025(7) . ?
Pd1 N2 2.038(7) . ?
C16 C17 1.360(11) . ?
C16 C15 1.425(11) . ?
C16 H16 0.9500 . ?
F1 C22 1.345(9) . ?
C15 N4 1.374(10) . ?
C15 C14 1.395(11) . ?
C23 F2 1.353(9) . ?
C23 C22 1.362(11) . ?
C23 C24 1.389(12) . ?
C27 C28 1.397(11) . ?
C27 C32 1.407(11) . ?
C27 C9 1.471(11) . ?
C31 F9 1.346(9) . ?
C31 C30 1.359(12) . ?
C31 C32 1.371(11) . ?
C34 F11 1.329(9) . ?
C34 C35 1.366(11) . ?
C34 C33 1.383(11) . ?
F4 C25 1.334(9) . ?
F6 C28 1.351(8) . ?
C21 C26 1.379(11) . ?
C21 C22 1.393(10) . ?
C21 C4 1.483(11) . ?
C28 C29 1.366(11) . ?
F7 C29 1.344(9) . ?
C14 C13 1.376(11) . ?
C14 C33 1.485(11) . ?
F5 C26 1.349(9) . ?
C10 N1 1.388(10) . ?
C10 C9 1.402(11) . ?
C10 C11 1.449(11) . ?
F8 C30 1.335(9) . ?
C9 C8 1.391(10) . ?
F3 C24 1.335(9) . ?
C33 C38 1.395(11) . ?
F13 C36 1.333(9) . ?
C13 N1 1.381(9) . ?
C13 C12 1.440(11) . ?
C17 C18 1.418(11) . ?
C17 H17 0.9500 . ?
F14 C37 1.355(10) . ?
F15 C38 1.352(9) . ?
N2 C8 1.356(10) . ?
N3 C20 1.383(10) . ?
N4 C18 1.372(11) . ?
O1 C19 1.276(10) . ?
C44 C45 1.360(11) . ?
C44 C43 1.368(12) . ?
C44 H44 0.9500 . ?
C55 C46 1.398(12) . ?
C55 C57 1.414(11) . ?
C55 C42 1.436(11) . ?
C57 C56 1.387(11) . ?
C57 C54 1.425(12) . ?
N5 C47 1.373(10) . ?
N5 C46 1.385(10) . ?
N5 C61 1.482(10) . ?
N6 C41 1.380(10) . ?
N6 C42 1.394(11) . ?
N6 C58 1.473(10) . ?
N7 C52 1.380(11) . ?
N7 C51 1.391(11) . ?
N7 C64 1.470(10) . ?
C2 C1 1.369(11) . ?
C2 H2 0.9500 . ?
C1 C20 1.415(11) . ?
C1 H1 0.9500 . ?
C6 C7 1.363(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.445(11) . ?
C7 H7 0.9500 . ?
C11 C12 1.353(11) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C18 C19 1.435(11) . ?
C19 C20 1.423(11) . ?
C24 C25 1.374(11) . ?
C25 C26 1.380(11) . ?
C29 C30 1.383(11) . ?
C35 C36 1.382(12) . ?
C36 C37 1.351(12) . ?
C37 C38 1.371(11) . ?
C39 C40 1.396(12) . ?
C39 C53 1.405(12) . ?
C39 H39 0.9500 . ?
C40 C41 1.381(12) . ?
C40 H40 0.9500 . ?
C41 C54 1.407(11) . ?
C42 C43 1.401(11) . ?
C43 H43 0.9500 . ?
C45 C46 1.414(11) . ?
C45 H45 0.9500 . ?
C47 C48 1.386(11) . ?
C47 C56 1.438(12) . ?
C48 C49 1.396(12) . ?
C48 H48 0.9500 . ?
C49 C50 1.371(13) . ?
C49 H49 0.9500 . ?
C50 C51 1.388(12) . ?
C50 H50 0.9500 . ?
C51 C56 1.419(11) . ?
C52 C53 1.380(12) . ?
C52 C54 1.446(12) . ?
C53 H53 0.9500 . ?
C58 C59 1.516(11) . ?
C58 H58 0.9900 . ?
C58 H58A 0.9900 . ?
C59 C60 1.538(11) . ?
C59 H59 0.9900 . ?
C59 H59A 0.9900 . ?
C60 H60 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C61 C62 1.502(11) . ?
C61 H61 0.9900 . ?
C61 H61A 0.9900 . ?
C62 C63 1.531(12) . ?
C62 H62 0.9900 . ?
C62 H62A 0.9900 . ?
C63 H63 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C64 C65 1.527(13) . ?
C64 H64 0.9900 . ?
C64 H64A 0.9900 . ?
C65 C66 1.524(13) . ?
C65 H65 0.9900 . ?
C65 H65A 0.9900 . ?
C66 H66 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?

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
N3 C3 C2 111.0(7) . . ?
N3 C3 C4 123.8(7) . . ?
C2 C3 C4 125.2(8) . . ?
N2 C5 C4 125.4(7) . . ?
N2 C5 C6 109.9(7) . . ?
C4 C5 C6 124.7(7) . . ?
N3 Pd1 N1 177.4(2) . . ?
N3 Pd1 N4 90.0(3) . . ?
N1 Pd1 N4 89.8(3) . . ?
N3 Pd1 N2 90.1(2) . . ?
N1 Pd1 N2 90.2(2) . . ?
N4 Pd1 N2 177.4(3) . . ?
C17 C16 C15 107.6(7) . . ?
C17 C16 H16 126.2 . . ?
C15 C16 H16 126.2 . . ?
N4 C15 C14 124.1(7) . . ?
N4 C15 C16 108.6(7) . . ?
C14 C15 C16 127.2(7) . . ?
F2 C23 C22 120.0(8) . . ?
F2 C23 C24 119.8(7) . . ?
C22 C23 C24 120.2(7) . . ?
C28 C27 C32 114.1(7) . . ?
C28 C27 C9 123.1(7) . . ?
C32 C27 C9 122.8(7) . . ?
F9 C31 C30 119.5(8) . . ?
F9 C31 C32 119.7(7) . . ?
C30 C31 C32 120.8(8) . . ?
F11 C34 C35 118.4(7) . . ?
F11 C34 C33 119.2(7) . . ?
C35 C34 C33 122.3(8) . . ?
C26 C21 C22 114.7(7) . . ?
C26 C21 C4 122.0(7) . . ?
C22 C21 C4 123.3(8) . . ?
F6 C28 C29 117.4(7) . . ?
F6 C28 C27 119.0(7) . . ?
C29 C28 C27 123.6(7) . . ?
C13 C14 C15 126.0(7) . . ?
C13 C14 C33 118.5(7) . . ?
C15 C14 C33 115.5(7) . . ?
N1 C10 C9 125.0(7) . . ?
N1 C10 C11 109.3(7) . . ?
C9 C10 C11 125.6(8) . . ?
C8 C9 C10 124.6(7) . . ?
C8 C9 C27 118.2(7) . . ?
C10 C9 C27 117.3(7) . . ?
C34 C33 C38 115.5(7) . . ?
C34 C33 C14 122.1(7) . . ?
C38 C33 C14 122.5(7) . . ?
F10 C32 C31 118.1(7) . . ?
F10 C32 C27 119.2(7) . . ?
C31 C32 C27 122.7(8) . . ?
C5 C4 C3 125.4(7) . . ?
C5 C4 C21 117.0(7) . . ?
C3 C4 C21 117.5(7) . . ?
C14 C13 N1 124.8(7) . . ?
C14 C13 C12 125.3(7) . . ?
N1 C13 C12 109.9(7) . . ?
C16 C17 C18 107.1(8) . . ?
C16 C17 H17 126.5 . . ?
C18 C17 H17 126.5 . . ?
C13 N1 C10 106.1(6) . . ?
C13 N1 Pd1 126.6(5) . . ?
C10 N1 Pd1 126.3(5) . . ?
C8 N2 C5 107.4(7) . . ?
C8 N2 Pd1 126.2(5) . . ?
C5 N2 Pd1 125.8(5) . . ?
C3 N3 C20 104.7(6) . . ?
C3 N3 Pd1 127.7(5) . . ?
C20 N3 Pd1 127.3(5) . . ?
C18 N4 C15 107.0(7) . . ?
C18 N4 Pd1 125.9(6) . . ?
C15 N4 Pd1 126.7(6) . . ?
F1 C22 C23 118.4(7) . . ?
F1 C22 C21 118.2(7) . . ?
C23 C22 C21 123.3(8) . . ?
C45 C44 C43 125.6(8) . . ?
C45 C44 H44 117.2 . . ?
C43 C44 H44 117.2 . . ?
C46 C55 C57 120.1(7) . . ?
C46 C55 C42 120.1(7) . . ?
C57 C55 C42 119.7(8) . . ?
C56 C57 C55 120.2(8) . . ?
C56 C57 C54 121.2(8) . . ?
C55 C57 C54 118.6(8) . . ?
C47 N5 C46 122.5(7) . . ?
C47 N5 C61 118.4(7) . . ?
C46 N5 C61 118.9(7) . . ?
C41 N6 C42 122.2(7) . . ?
C41 N6 C58 120.6(7) . . ?
C42 N6 C58 117.3(7) . . ?
C52 N7 C51 122.9(7) . . ?
C52 N7 C64 119.1(7) . . ?
C51 N7 C64 117.9(7) . . ?
C1 C2 C3 107.2(7) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 H2 126.4 . . ?
C2 C1 C20 106.3(7) . . ?
C2 C1 H1 126.9 . . ?
C20 C1 H1 126.9 . . ?
C7 C6 C5 106.3(7) . . ?
C7 C6 H6 126.8 . . ?
C5 C6 H6 126.8 . . ?
C6 C7 C8 107.7(7) . . ?
C6 C7 H7 126.1 . . ?
C8 C7 H7 126.1 . . ?
N2 C8 C9 126.5(7) . . ?
N2 C8 C7 108.6(7) . . ?
C9 C8 C7 124.9(7) . . ?
C12 C11 C10 107.2(8) . . ?
C12 C11 H11 126.4 . . ?
C10 C11 H11 126.4 . . ?
C11 C12 C13 107.4(7) . . ?
C11 C12 H12 126.3 . . ?
C13 C12 H12 126.3 . . ?
N4 C18 C17 109.3(7) . . ?
N4 C18 C19 126.7(8) . . ?
C17 C18 C19 123.8(8) . . ?
O1 C19 C20 121.0(7) . . ?
O1 C19 C18 117.8(8) . . ?
C20 C19 C18 121.1(8) . . ?
N3 C20 C1 110.7(7) . . ?
N3 C20 C19 125.6(7) . . ?
C1 C20 C19 123.1(7) . . ?
F3 C24 C25 121.3(8) . . ?
F3 C24 C23 120.2(7) . . ?
C25 C24 C23 118.5(8) . . ?
F4 C25 C24 119.1(7) . . ?
F4 C25 C26 121.3(7) . . ?
C24 C25 C26 119.6(8) . . ?
F5 C26 C21 119.9(7) . . ?
F5 C26 C25 116.3(7) . . ?
C21 C26 C25 123.7(7) . . ?
F7 C29 C28 120.1(7) . . ?
F7 C29 C30 119.8(8) . . ?
C28 C29 C30 119.9(8) . . ?
F8 C30 C31 120.8(7) . . ?
F8 C30 C29 120.3(7) . . ?
C31 C30 C29 118.9(8) . . ?
F12 C35 C34 119.7(8) . . ?
F12 C35 C36 119.8(7) . . ?
C34 C35 C36 120.4(7) . . ?
F13 C36 C37 122.1(8) . . ?
F13 C36 C35 119.1(7) . . ?
C37 C36 C35 118.8(8) . . ?
C36 C37 F14 119.0(8) . . ?
C36 C37 C38 120.6(8) . . ?
F14 C37 C38 120.3(7) . . ?
F15 C38 C37 117.9(7) . . ?
F15 C38 C33 119.8(7) . . ?
C37 C38 C33 122.3(7) . . ?
C40 C39 C53 122.8(9) . . ?
C40 C39 H39 118.6 . . ?
C53 C39 H39 118.6 . . ?
C41 C40 C39 119.5(8) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
N6 C41 C40 121.8(8) . . ?
N6 C41 C54 119.2(8) . . ?
C40 C41 C54 119.0(8) . . ?
N6 C42 C43 121.8(8) . . ?
N6 C42 C55 119.1(7) . . ?
C43 C42 C55 119.1(8) . . ?
C44 C43 C42 117.7(8) . . ?
C44 C43 H43 121.1 . . ?
C42 C43 H43 121.1 . . ?
C44 C45 C46 117.8(8) . . ?
C44 C45 H45 121.1 . . ?
C46 C45 H45 121.1 . . ?
N5 C46 C55 118.8(8) . . ?
N5 C46 C45 121.7(8) . . ?
C55 C46 C45 119.5(8) . . ?
N5 C47 C48 123.0(8) . . ?
N5 C47 C56 118.7(7) . . ?
C48 C47 C56 118.3(8) . . ?
C47 C48 C49 119.2(8) . . ?
C47 C48 H48 120.4 . . ?
C49 C48 H48 120.4 . . ?
C50 C49 C48 123.4(8) . . ?
C50 C49 H49 118.3 . . ?
C48 C49 H49 118.3 . . ?
C49 C50 C51 119.3(8) . . ?
C49 C50 H50 120.4 . . ?
C51 C50 H50 120.4 . . ?
C50 C51 N7 122.2(8) . . ?
C50 C51 C56 119.1(8) . . ?
N7 C51 C56 118.7(7) . . ?
C53 C52 N7 122.1(8) . . ?
C53 C52 C54 119.0(8) . . ?
N7 C52 C54 118.9(8) . . ?
C52 C53 C39 118.5(8) . . ?
C52 C53 H53 120.7 . . ?
C39 C53 H53 120.7 . . ?
C41 C54 C57 121.0(8) . . ?
C41 C54 C52 121.0(8) . . ?
C57 C54 C52 118.0(8) . . ?
C57 C56 C51 120.1(8) . . ?
C57 C56 C47 119.2(8) . . ?
C51 C56 C47 120.7(7) . . ?
N6 C58 C59 111.4(7) . . ?
N6 C58 H58 109.4 . . ?
C59 C58 H58 109.4 . . ?
N6 C58 H58A 109.4 . . ?
C59 C58 H58A 109.4 . . ?
H58 C58 H58A 108.0 . . ?
C58 C59 C60 111.7(7) . . ?
C58 C59 H59 109.3 . . ?
C60 C59 H59 109.3 . . ?
C58 C59 H59A 109.3 . . ?
C60 C59 H59A 109.3 . . ?
H59 C59 H59A 107.9 . . ?
C59 C60 H60 109.5 . . ?
C59 C60 H60A 109.5 . . ?
H60 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N5 C61 C62 110.2(7) . . ?
N5 C61 H61 109.6 . . ?
C62 C61 H61 109.6 . . ?
N5 C61 H61A 109.6 . . ?
C62 C61 H61A 109.6 . . ?
H61 C61 H61A 108.1 . . ?
C61 C62 C63 112.0(8) . . ?
C61 C62 H62 109.2 . . ?
C63 C62 H62 109.2 . . ?
C61 C62 H62A 109.2 . . ?
C63 C62 H62A 109.2 . . ?
H62 C62 H62A 107.9 . . ?
C62 C63 H63 109.5 . . ?
C62 C63 H63A 109.5 . . ?
H63 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
N7 C64 C65 111.5(7) . . ?
N7 C64 H64 109.3 . . ?
C65 C64 H64 109.3 . . ?
N7 C64 H64A 109.3 . . ?
C65 C64 H64A 109.3 . . ?
H64 C64 H64A 108.0 . . ?
C66 C65 C64 111.4(8) . . ?
C66 C65 H65 109.4 . . ?
C64 C65 H65 109.4 . . ?
C66 C65 H65A 109.4 . . ?
C64 C65 H65A 109.4 . . ?
H65 C65 H65A 108.0 . . ?
C65 C66 H66 109.5 . . ?
C65 C66 H66A 109.5 . . ?
H66 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?

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
_geom_torsion_publ_flag
C17 C16 C15 N4 3.0(9) . . . . ?
C17 C16 C15 C14 -174.5(8) . . . . ?
C32 C27 C28 F6 -178.8(6) . . . . ?
C9 C27 C28 F6 3.6(11) . . . . ?
C32 C27 C28 C29 1.3(11) . . . . ?
C9 C27 C28 C29 -176.3(7) . . . . ?
N4 C15 C14 C13 9.1(13) . . . . ?
C16 C15 C14 C13 -173.8(8) . . . . ?
N4 C15 C14 C33 -169.1(7) . . . . ?
C16 C15 C14 C33 8.0(11) . . . . ?
N1 C10 C9 C8 -7.2(12) . . . . ?
C11 C10 C9 C8 175.6(7) . . . . ?
N1 C10 C9 C27 171.9(7) . . . . ?
C11 C10 C9 C27 -5.2(11) . . . . ?
C28 C27 C9 C8 65.1(10) . . . . ?
C32 C27 C9 C8 -112.2(8) . . . . ?
C28 C27 C9 C10 -114.1(8) . . . . ?
C32 C27 C9 C10 68.6(10) . . . . ?
F11 C34 C33 C38 176.5(7) . . . . ?
C35 C34 C33 C38 -1.5(12) . . . . ?
F11 C34 C33 C14 -3.4(12) . . . . ?
C35 C34 C33 C14 178.6(8) . . . . ?
C13 C14 C33 C34 62.0(10) . . . . ?
C15 C14 C33 C34 -119.6(8) . . . . ?
C13 C14 C33 C38 -117.9(9) . . . . ?
C15 C14 C33 C38 60.5(10) . . . . ?
F9 C31 C32 F10 -1.4(11) . . . . ?
C30 C31 C32 F10 179.8(7) . . . . ?
F9 C31 C32 C27 179.7(7) . . . . ?
C30 C31 C32 C27 0.8(13) . . . . ?
C28 C27 C32 F10 -179.3(6) . . . . ?
C9 C27 C32 F10 -1.8(11) . . . . ?
C28 C27 C32 C31 -0.4(11) . . . . ?
C9 C27 C32 C31 177.2(7) . . . . ?
N2 C5 C4 C3 -2.6(13) . . . . ?
C6 C5 C4 C3 174.9(8) . . . . ?
N2 C5 C4 C21 175.9(7) . . . . ?
C6 C5 C4 C21 -6.7(11) . . . . ?
N3 C3 C4 C5 12.3(13) . . . . ?
C2 C3 C4 C5 -169.1(8) . . . . ?
N3 C3 C4 C21 -166.2(7) . . . . ?
C2 C3 C4 C21 12.5(12) . . . . ?
C26 C21 C4 C5 -79.9(10) . . . . ?
C22 C21 C4 C5 100.1(9) . . . . ?
C26 C21 C4 C3 98.6(9) . . . . ?
C22 C21 C4 C3 -81.3(10) . . . . ?
C15 C14 C13 N1 5.8(12) . . . . ?
C33 C14 C13 N1 -176.0(6) . . . . ?
C15 C14 C13 C12 -175.4(7) . . . . ?
C33 C14 C13 C12 2.8(11) . . . . ?
C15 C16 C17 C18 0.6(9) . . . . ?
C14 C13 N1 C10 177.2(7) . . . . ?
C12 C13 N1 C10 -1.8(8) . . . . ?
C14 C13 N1 Pd1 -13.2(10) . . . . ?
C12 C13 N1 Pd1 167.8(5) . . . . ?
C9 C10 N1 C13 -176.7(7) . . . . ?
C11 C10 N1 C13 0.9(8) . . . . ?
C9 C10 N1 Pd1 13.7(11) . . . . ?
C11 C10 N1 Pd1 -168.8(5) . . . . ?
C4 C5 N2 C8 177.5(7) . . . . ?
C6 C5 N2 C8 -0.3(8) . . . . ?
C4 C5 N2 Pd1 -10.8(11) . . . . ?
C6 C5 N2 Pd1 171.5(5) . . . . ?
C2 C3 N3 C20 -1.1(8) . . . . ?
C4 C3 N3 C20 177.7(7) . . . . ?
C2 C3 N3 Pd1 173.7(5) . . . . ?
C4 C3 N3 Pd1 -7.4(11) . . . . ?
C14 C15 N4 C18 172.1(7) . . . . ?
C16 C15 N4 C18 -5.4(9) . . . . ?
C14 C15 N4 Pd1 -14.9(11) . . . . ?
C16 C15 N4 Pd1 167.5(5) . . . . ?
F2 C23 C22 F1 -1.4(12) . . . . ?
C24 C23 C22 F1 178.4(7) . . . . ?
F2 C23 C22 C21 -178.7(8) . . . . ?
C24 C23 C22 C21 1.0(13) . . . . ?
C26 C21 C22 F1 -178.8(7) . . . . ?
C4 C21 C22 F1 1.2(12) . . . . ?
C26 C21 C22 C23 -1.4(12) . . . . ?
C4 C21 C22 C23 178.5(8) . . . . ?
C46 C55 C57 C56 -3.1(11) . . . . ?
C42 C55 C57 C56 176.5(7) . . . . ?
C46 C55 C57 C54 178.5(7) . . . . ?
C42 C55 C57 C54 -1.8(11) . . . . ?
N3 C3 C2 C1 0.0(9) . . . . ?
C4 C3 C2 C1 -178.8(8) . . . . ?
C3 C2 C1 C20 1.1(9) . . . . ?
N2 C5 C6 C7 1.5(9) . . . . ?
C4 C5 C6 C7 -176.3(7) . . . . ?
C5 C6 C7 C8 -2.0(9) . . . . ?
C5 N2 C8 C9 178.4(7) . . . . ?
Pd1 N2 C8 C9 6.7(11) . . . . ?
C5 N2 C8 C7 -0.9(8) . . . . ?
Pd1 N2 C8 C7 -172.7(5) . . . . ?
C10 C9 C8 N2 -3.6(12) . . . . ?
C27 C9 C8 N2 177.2(7) . . . . ?
C10 C9 C8 C7 175.6(7) . . . . ?
C27 C9 C8 C7 -3.6(11) . . . . ?
C6 C7 C8 N2 1.9(9) . . . . ?
C6 C7 C8 C9 -177.4(7) . . . . ?
N1 C10 C11 C12 0.4(9) . . . . ?
C9 C10 C11 C12 178.0(7) . . . . ?
C10 C11 C12 C13 -1.5(8) . . . . ?
C14 C13 C12 C11 -176.9(7) . . . . ?
N1 C13 C12 C11 2.1(9) . . . . ?
C15 N4 C18 C17 5.8(9) . . . . ?
Pd1 N4 C18 C17 -167.2(5) . . . . ?
C15 N4 C18 C19 -168.7(8) . . . . ?
Pd1 N4 C18 C19 18.3(12) . . . . ?
C16 C17 C18 N4 -4.0(9) . . . . ?
C16 C17 C18 C19 170.7(8) . . . . ?
N4 C18 C19 O1 164.3(8) . . . . ?
C17 C18 C19 O1 -9.5(12) . . . . ?
N4 C18 C19 C20 -17.0(13) . . . . ?
C17 C18 C19 C20 169.2(8) . . . . ?
C3 N3 C20 C1 1.8(8) . . . . ?
Pd1 N3 C20 C1 -173.1(5) . . . . ?
C3 N3 C20 C19 -169.4(8) . . . . ?
Pd1 N3 C20 C19 15.7(11) . . . . ?
C2 C1 C20 N3 -1.9(9) . . . . ?
C2 C1 C20 C19 169.7(8) . . . . ?
O1 C19 C20 N3 177.7(7) . . . . ?
C18 C19 C20 N3 -1.0(13) . . . . ?
O1 C19 C20 C1 7.4(13) . . . . ?
C18 C19 C20 C1 -171.2(7) . . . . ?
F2 C23 C24 F3 -1.0(12) . . . . ?
C22 C23 C24 F3 179.2(7) . . . . ?
F2 C23 C24 C25 -179.5(7) . . . . ?
C22 C23 C24 C25 0.8(12) . . . . ?
F3 C24 C25 F4 0.1(12) . . . . ?
C23 C24 C25 F4 178.5(7) . . . . ?
F3 C24 C25 C26 179.5(7) . . . . ?
C23 C24 C25 C26 -2.1(12) . . . . ?
C22 C21 C26 F5 -177.6(7) . . . . ?
C4 C21 C26 F5 2.5(12) . . . . ?
C22 C21 C26 C25 0.0(12) . . . . ?
C4 C21 C26 C25 -179.9(8) . . . . ?
F4 C25 C26 F5 -1.2(12) . . . . ?
C24 C25 C26 F5 179.4(8) . . . . ?
F4 C25 C26 C21 -178.9(8) . . . . ?
C24 C25 C26 C21 1.7(13) . . . . ?
F6 C28 C29 F7 3.0(11) . . . . ?
C27 C28 C29 F7 -177.1(7) . . . . ?
F6 C28 C29 C30 177.5(6) . . . . ?
C27 C28 C29 C30 -2.5(12) . . . . ?
F9 C31 C30 F8 0.9(12) . . . . ?
C32 C31 C30 F8 179.7(7) . . . . ?
F9 C31 C30 C29 179.1(7) . . . . ?
C32 C31 C30 C29 -2.0(12) . . . . ?
F7 C29 C30 F8 -4.3(11) . . . . ?
C28 C29 C30 F8 -178.9(7) . . . . ?
F7 C29 C30 C31 177.4(7) . . . . ?
C28 C29 C30 C31 2.9(12) . . . . ?
F11 C34 C35 F12 2.1(12) . . . . ?
C33 C34 C35 F12 -179.9(8) . . . . ?
F11 C34 C35 C36 -176.8(8) . . . . ?
C33 C34 C35 C36 1.2(13) . . . . ?
F12 C35 C36 F13 -1.3(12) . . . . ?
C34 C35 C36 F13 177.6(7) . . . . ?
F12 C35 C36 C37 -178.7(8) . . . . ?
C34 C35 C36 C37 0.2(13) . . . . ?
F13 C36 C37 F14 1.6(13) . . . . ?
C35 C36 C37 F14 178.8(8) . . . . ?
F13 C36 C37 C38 -178.5(8) . . . . ?
C35 C36 C37 C38 -1.2(14) . . . . ?
C36 C37 C38 F15 179.2(8) . . . . ?
F14 C37 C38 F15 -0.9(12) . . . . ?
C36 C37 C38 C33 0.9(14) . . . . ?
F14 C37 C38 C33 -179.2(8) . . . . ?
C34 C33 C38 F15 -177.8(7) . . . . ?
C14 C33 C38 F15 2.1(12) . . . . ?
C34 C33 C38 C37 0.4(12) . . . . ?
C14 C33 C38 C37 -179.7(8) . . . . ?
C53 C39 C40 C41 -0.5(13) . . . . ?
C42 N6 C41 C40 176.6(8) . . . . ?
C58 N6 C41 C40 -2.1(12) . . . . ?
C42 N6 C41 C54 -2.9(12) . . . . ?
C58 N6 C41 C54 178.3(7) . . . . ?
C39 C40 C41 N6 177.6(7) . . . . ?
C39 C40 C41 C54 -2.8(13) . . . . ?
C41 N6 C42 C43 -179.9(7) . . . . ?
C58 N6 C42 C43 -1.2(11) . . . . ?
C41 N6 C42 C55 -0.5(11) . . . . ?
C58 N6 C42 C55 178.2(6) . . . . ?
C46 C55 C42 N6 -177.4(7) . . . . ?
C57 C55 C42 N6 2.9(11) . . . . ?
C46 C55 C42 C43 2.0(11) . . . . ?
C57 C55 C42 C43 -177.6(7) . . . . ?
C45 C44 C43 C42 -2.8(13) . . . . ?
N6 C42 C43 C44 -179.8(8) . . . . ?
C55 C42 C43 C44 0.8(11) . . . . ?
C43 C44 C45 C46 1.8(13) . . . . ?
C47 N5 C46 C55 7.5(11) . . . . ?
C61 N5 C46 C55 -178.1(7) . . . . ?
C47 N5 C46 C45 -171.3(7) . . . . ?
C61 N5 C46 C45 3.2(11) . . . . ?
C57 C55 C46 N5 -2.1(11) . . . . ?
C42 C55 C46 N5 178.3(7) . . . . ?
C57 C55 C46 C45 176.6(7) . . . . ?
C42 C55 C46 C45 -3.0(11) . . . . ?
C44 C45 C46 N5 179.9(7) . . . . ?
C44 C45 C46 C55 1.2(11) . . . . ?
C46 N5 C47 C48 173.3(7) . . . . ?
C61 N5 C47 C48 -1.2(11) . . . . ?
C46 N5 C47 C56 -7.3(11) . . . . ?
C61 N5 C47 C56 178.3(7) . . . . ?
N5 C47 C48 C49 -177.7(7) . . . . ?
C56 C47 C48 C49 2.9(11) . . . . ?
C47 C48 C49 C50 -3.2(13) . . . . ?
C48 C49 C50 C51 0.2(13) . . . . ?
C49 C50 C51 N7 -176.2(8) . . . . ?
C49 C50 C51 C56 3.1(12) . . . . ?
C52 N7 C51 C50 -176.2(7) . . . . ?
C64 N7 C51 C50 0.5(12) . . . . ?
C52 N7 C51 C56 4.5(12) . . . . ?
C64 N7 C51 C56 -178.8(7) . . . . ?
C51 N7 C52 C53 179.8(8) . . . . ?
C64 N7 C52 C53 3.1(12) . . . . ?
C51 N7 C52 C54 -1.5(12) . . . . ?
C64 N7 C52 C54 -178.2(7) . . . . ?
N7 C52 C53 C39 177.3(7) . . . . ?
C54 C52 C53 C39 -1.4(12) . . . . ?
C40 C39 C53 C52 2.6(13) . . . . ?
N6 C41 C54 C57 4.1(12) . . . . ?
C40 C41 C54 C57 -175.5(8) . . . . ?
N6 C41 C54 C52 -176.4(7) . . . . ?
C40 C41 C54 C52 4.0(12) . . . . ?
C56 C57 C54 C41 -180.0(7) . . . . ?
C55 C57 C54 C41 -1.7(12) . . . . ?
C56 C57 C54 C52 0.5(12) . . . . ?
C55 C57 C54 C52 178.8(7) . . . . ?
C53 C52 C54 C41 -1.8(12) . . . . ?
N7 C52 C54 C41 179.4(7) . . . . ?
C53 C52 C54 C57 177.7(8) . . . . ?
N7 C52 C54 C57 -1.1(11) . . . . ?
C55 C57 C56 C51 -175.8(7) . . . . ?
C54 C57 C56 C51 2.5(12) . . . . ?
C55 C57 C56 C47 3.3(11) . . . . ?
C54 C57 C56 C47 -178.4(7) . . . . ?
C50 C51 C56 C57 175.7(7) . . . . ?
N7 C51 C56 C57 -4.9(12) . . . . ?
C50 C51 C56 C47 -3.3(12) . . . . ?
N7 C51 C56 C47 176.0(7) . . . . ?
N5 C47 C56 C57 1.7(11) . . . . ?
C48 C47 C56 C57 -178.7(7) . . . . ?
N5 C47 C56 C51 -179.2(7) . . . . ?
C48 C47 C56 C51 0.3(12) . . . . ?
C41 N6 C58 C59 96.2(9) . . . . ?
C42 N6 C58 C59 -82.6(9) . . . . ?
N6 C58 C59 C60 169.9(8) . . . . ?
C47 N5 C61 C62 87.3(9) . . . . ?
C46 N5 C61 C62 -87.3(9) . . . . ?
N5 C61 C62 C63 174.6(7) . . . . ?
C52 N7 C64 C65 90.4(9) . . . . ?
C51 N7 C64 C65 -86.4(10) . . . . ?
N7 C64 C65 C66 166.9(8) . . . . ?

_refine_diff_density_max         1.356
_refine_diff_density_min         -1.748
_refine_diff_density_rms         0.143



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_180131_ys-3-2
_database_code_depnum_ccdc_archive 'CCDC 1906675'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H8 F15 N4 O Pd, C16 H36 N'
_chemical_formula_sum            'C54 H44 F15 N5 O Pd'
_chemical_formula_weight         1170.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
Pd Pd -0.7734 1.2009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.2881(3)
_cell_length_b                   22.4879(6)
_cell_length_c                   26.3395(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4909.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    27310
_cell_measurement_theta_min      1.310
_cell_measurement_theta_max      28.101

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             2368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.611
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.509
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.78192
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            27310
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.310
_diffrn_reflns_theta_max         28.101
_diffrn_reflns_theta_full        27.979
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8719
_reflns_number_gt                6394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0943P)²+13.0340P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0060(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.18(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8719
_refine_ls_number_parameters     691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1982
_refine_ls_wR_factor_gt          0.1539
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5331(17) 0.4890(4) 0.7857(4) 0.035(3) Uani 1 1 d . . . . .
C2 C 0.5696(15) 0.4867(4) 0.7324(4) 0.030(3) Uani 1 1 d . . . . .
C3 C 0.6047(14) 0.4339(4) 0.7061(5) 0.034(3) Uani 1 1 d . . . . .
H3 H 0.6169 0.3955 0.7206 0.041 Uiso 1 1 calc R U . . .
C4 C 0.6182(14) 0.4477(5) 0.6558(4) 0.030(3) Uani 1 1 d . . . . .
H4 H 0.6466 0.4214 0.6291 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5815(15) 0.5093(5) 0.6512(4) 0.034(3) Uani 1 1 d . . . . .
C6 C 0.5608(18) 0.5408(4) 0.6058(4) 0.034(3) Uani 1 1 d . . . . .
C7 C 0.5302(17) 0.6001(5) 0.6017(4) 0.032(3) Uani 1 1 d . . . . .
C8 C 0.5039(16) 0.6327(5) 0.5549(5) 0.042(4) Uani 1 1 d . . . . .
H8 H 0.4983 0.6164 0.5217 0.051 Uiso 1 1 calc R U . . .
C9 C 0.4890(19) 0.6903(5) 0.5674(4) 0.048(4) Uani 1 1 d . . . . .
H9 H 0.4680 0.7220 0.5445 0.058 Uiso 1 1 calc R U . . .
C10 C 0.5100(16) 0.6958(5) 0.6208(4) 0.036(3) Uani 1 1 d . . . . .
C11 C 0.5239(17) 0.7492(4) 0.6476(4) 0.032(3) Uani 1 1 d . . . . .
C12 C 0.5532(15) 0.7551(4) 0.6990(4) 0.028(2) Uani 1 1 d . . . . .
C13 C 0.5787(14) 0.8093(5) 0.7261(4) 0.033(3) Uani 1 1 d . . . . .
H13 H 0.5810 0.8481 0.7120 0.039 Uiso 1 1 calc R U . . .
C14 C 0.5990(13) 0.7952(5) 0.7756(5) 0.033(3) Uani 1 1 d . . . . .
H14 H 0.6207 0.8224 0.8024 0.040 Uiso 1 1 calc R U . . .
C15 C 0.5818(12) 0.7322(5) 0.7805(5) 0.029(3) Uani 1 1 d . . . . .
C16 C 0.5788(15) 0.7013(5) 0.8248(4) 0.030(3) Uani 1 1 d . . . . .
C17 C 0.5492(18) 0.6404(4) 0.8297(4) 0.033(3) Uani 1 1 d . . . . .
C18 C 0.5198(19) 0.6090(5) 0.8753(5) 0.047(4) Uani 1 1 d . . . . .
H18 H 0.5140 0.6260 0.9083 0.057 Uiso 1 1 calc R U . . .
C19 C 0.5016(18) 0.5512(5) 0.8643(4) 0.044(4) Uani 1 1 d . . . . .
H19 H 0.4803 0.5200 0.8877 0.053 Uiso 1 1 calc R U . . .
C20 C 0.5197(19) 0.5454(5) 0.8123(4) 0.041(3) Uani 1 1 d . . . . .
C21 C 0.5628(19) 0.5053(5) 0.5576(4) 0.040(3) Uani 1 1 d . . . . .
C22 C 0.428(2) 0.4939(5) 0.5312(5) 0.046(4) Uani 1 1 d . . . . .
C23 C 0.428(3) 0.4600(6) 0.4866(5) 0.058(5) Uani 1 1 d . . . . .
C24 C 0.569(3) 0.4363(6) 0.4707(5) 0.062(5) Uani 1 1 d . . . . .
C25 C 0.711(2) 0.4456(6) 0.4958(6) 0.054(4) Uani 1 1 d . . . . .
C26 C 0.7102(19) 0.4809(5) 0.5390(5) 0.044(3) Uani 1 1 d . . . . .
C27 C 0.5097(16) 0.8058(4) 0.6176(4) 0.035(3) Uani 1 1 d . . . . .
C28 C 0.3671(17) 0.8316(5) 0.6056(5) 0.039(3) Uani 1 1 d . . . . .
C29 C 0.3534(18) 0.8833(6) 0.5767(5) 0.047(3) Uani 1 1 d . . . . .
C30 C 0.495(2) 0.9093(5) 0.5600(5) 0.048(4) Uani 1 1 d . . . . .
C31 C 0.6397(19) 0.8855(5) 0.5722(5) 0.046(3) Uani 1 1 d . . . . .
C32 C 0.6434(19) 0.8340(5) 0.6010(5) 0.043(3) Uani 1 1 d . . . . .
C33 C 0.6047(15) 0.7350(5) 0.8730(5) 0.035(3) Uani 1 1 d . . . . .
C34 C 0.4849(18) 0.7658(5) 0.8975(5) 0.046(4) Uani 1 1 d . . . . .
C35 C 0.511(2) 0.7950(6) 0.9430(5) 0.058(5) Uani 1 1 d . . . . .
C36 C 0.662(3) 0.7953(6) 0.9632(5) 0.066(5) Uani 1 1 d . . . . .
C37 C 0.789(2) 0.7651(6) 0.9408(6) 0.055(4) Uani 1 1 d . . . . .
C38 C 0.7570(18) 0.7354(5) 0.8949(5) 0.043(3) Uani 1 1 d . . . . .
C39 C 1.1419(18) 0.6497(6) 0.7338(6) 0.050(4) Uani 1 1 d . . . . .
H39 H 1.2065 0.6366 0.7634 0.060 Uiso 1 1 calc R U . . .
H39A H 1.2188 0.6619 0.7070 0.060 Uiso 1 1 calc R U . . .
C40 C 1.0462(19) 0.7032(6) 0.7492(7) 0.060(4) Uani 1 1 d . . . . .
H40 H 0.9764 0.7156 0.7206 0.072 Uiso 1 1 calc R U . . .
H40A H 0.9754 0.6926 0.7781 0.072 Uiso 1 1 calc R U . . .
C41 C 1.1500(19) 0.7536(7) 0.7641(7) 0.067(5) Uani 1 1 d . . . . .
H41 H 1.2214 0.7639 0.7353 0.080 Uiso 1 1 calc R U . . .
H41A H 1.2194 0.7412 0.7928 0.080 Uiso 1 1 calc R U . . .
C42 C 1.057(2) 0.8082(7) 0.7795(8) 0.093(7) Uani 1 1 d . . . . .
H42 H 1.0168 0.8285 0.7491 0.139 Uiso 1 1 calc R U . . .
H42A H 1.1274 0.8351 0.7985 0.139 Uiso 1 1 calc R U . . .
H42B H 0.9653 0.7965 0.8009 0.139 Uiso 1 1 calc R U . . .
C43 C 0.9449(16) 0.6177(5) 0.6700(4) 0.040(3) Uani 1 1 d . . . . .
H43 H 0.8860 0.5829 0.6562 0.048 Uiso 1 1 calc R U . . .
H43A H 0.8636 0.6463 0.6828 0.048 Uiso 1 1 calc R U . . .
C44 C 1.0365(19) 0.6466(5) 0.6274(5) 0.045(3) Uani 1 1 d . . . . .
H44 H 1.1251 0.6200 0.6164 0.054 Uiso 1 1 calc R U . . .
H44A H 1.0847 0.6843 0.6395 0.054 Uiso 1 1 calc R U . . .
C45 C 0.9252(18) 0.6591(5) 0.5827(5) 0.047(4) Uani 1 1 d . . . . .
H45 H 0.8882 0.6209 0.5682 0.056 Uiso 1 1 calc R U . . .
H45A H 0.8290 0.6808 0.5950 0.056 Uiso 1 1 calc R U . . .
C46 C 1.004(2) 0.6949(6) 0.5417(5) 0.057(5) Uani 1 1 d . . . . .
H46 H 1.0167 0.7360 0.5532 0.086 Uiso 1 1 calc R U . . .
H46A H 0.9359 0.6941 0.5112 0.086 Uiso 1 1 calc R U . . .
H46B H 1.1096 0.6779 0.5338 0.086 Uiso 1 1 calc R U . . .
C47 C 1.1567(17) 0.5489(5) 0.6975(6) 0.046(3) Uani 1 1 d . . . . .
H47 H 1.2065 0.5306 0.7279 0.055 Uiso 1 1 calc R U . . .
H47A H 1.2448 0.5668 0.6772 0.055 Uiso 1 1 calc R U . . .
C48 C 1.0785(16) 0.4994(5) 0.6658(5) 0.044(3) Uani 1 1 d . . . . .
H48 H 0.9740 0.4881 0.6813 0.053 Uiso 1 1 calc R U . . .
H48A H 1.0568 0.5144 0.6311 0.053 Uiso 1 1 calc R U . . .
C49 C 1.1852(17) 0.4454(5) 0.6627(6) 0.047(3) Uani 1 1 d . . . . .
H49 H 1.1888 0.4258 0.6963 0.056 Uiso 1 1 calc R U . . .
H49A H 1.2962 0.4580 0.6539 0.056 Uiso 1 1 calc R U . . .
C50 C 1.126(2) 0.4014(6) 0.6234(6) 0.062(4) Uani 1 1 d . . . . .
H50 H 1.0156 0.3894 0.6316 0.093 Uiso 1 1 calc R U . . .
H50A H 1.1965 0.3664 0.6235 0.093 Uiso 1 1 calc R U . . .
H50B H 1.1284 0.4200 0.5898 0.093 Uiso 1 1 calc R U . . .
C51 C 0.9328(18) 0.5733(6) 0.7558(5) 0.049(3) Uani 1 1 d . . . . .
H51 H 0.8527 0.6046 0.7637 0.059 Uiso 1 1 calc R U . . .
H51A H 0.8734 0.5388 0.7418 0.059 Uiso 1 1 calc R U . . .
C52 C 1.016(2) 0.5543(7) 0.8053(5) 0.056(4) Uani 1 1 d . . . . .
H52A H 1.1292 0.5444 0.7968 0.067 Uiso 1 1 calc R U . A 1
H52B H 1.0191 0.5896 0.8278 0.067 Uiso 1 1 calc R U . A 1
C53A C 0.953(4) 0.5055(10) 0.8349(9) 0.054(7) Uiso 0.61(3) 1 d . . P B 1
H53A H 0.8349 0.5106 0.8391 0.065 Uiso 0.61(3) 1 calc R U P B 1
H53B H 1.0026 0.5060 0.8691 0.065 Uiso 0.61(3) 1 calc R U P B 1
C54A C 0.986(3) 0.4449(12) 0.8094(10) 0.060(8) Uiso 0.61(3) 1 d . . P B 1
H54A H 0.9397 0.4447 0.7752 0.090 Uiso 0.61(3) 1 calc R U P B 1
H54B H 0.9372 0.4131 0.8297 0.090 Uiso 0.61(3) 1 calc R U P B 1
H54C H 1.1029 0.4384 0.8073 0.090 Uiso 0.61(3) 1 calc R U P B 1
C53B C 0.994(4) 0.4807(16) 0.8029(14) 0.044(10) Uiso 0.39(3) 1 d . . P B 2
H53C H 0.8786 0.4699 0.8017 0.053 Uiso 0.39(3) 1 calc R U P B 2
H53D H 1.0479 0.4645 0.7723 0.053 Uiso 0.39(3) 1 calc R U P B 2
C54B C 1.076(6) 0.4552(18) 0.8526(16) 0.068(14) Uiso 0.39(3) 1 d . . P B 2
H54D H 1.1890 0.4675 0.8539 0.102 Uiso 0.39(3) 1 calc R U P B 2
H54E H 1.0696 0.4116 0.8523 0.102 Uiso 0.39(3) 1 calc R U P B 2
H54F H 1.0188 0.4704 0.8825 0.102 Uiso 0.39(3) 1 calc R U P B 2
F1 F 0.2803(11) 0.5157(3) 0.5464(3) 0.055(2) Uani 1 1 d . . . . .
F2 F 0.2894(13) 0.4499(4) 0.4608(4) 0.073(3) Uani 1 1 d . . . . .
F3 F 0.5722(16) 0.4006(3) 0.4294(3) 0.087(4) Uani 1 1 d . . . . .
F4 F 0.8512(13) 0.4211(4) 0.4824(3) 0.073(3) Uani 1 1 d . . . . .
F5 F 0.8456(10) 0.4908(3) 0.5646(3) 0.051(2) Uani 1 1 d . . . . .
F6 F 0.2249(10) 0.8071(4) 0.6216(3) 0.058(2) Uani 1 1 d . . . . .
F7 F 0.2093(12) 0.9065(4) 0.5653(4) 0.069(3) Uani 1 1 d . . . . .
F8 F 0.4840(13) 0.9583(3) 0.5306(3) 0.062(3) Uani 1 1 d . . . . .
F9 F 0.7767(13) 0.9115(4) 0.5548(4) 0.078(3) Uani 1 1 d . . . . .
F10 F 0.7947(10) 0.8124(3) 0.6105(4) 0.060(2) Uani 1 1 d . . . . .
F11 F 0.3356(12) 0.7662(4) 0.8792(3) 0.072(3) Uani 1 1 d . . . . .
F12 F 0.3888(16) 0.8238(5) 0.9655(4) 0.097(4) Uani 1 1 d . . . . .
F13 F 0.6939(16) 0.8251(4) 1.0069(3) 0.091(4) Uani 1 1 d . . . . .
F14 F 0.9414(14) 0.7674(4) 0.9590(3) 0.078(3) Uani 1 1 d . . . . .
F15 F 0.8802(10) 0.7072(4) 0.8730(3) 0.054(2) Uani 1 1 d . . . . .
N1 N 0.5585(12) 0.5328(4) 0.6991(3) 0.026(2) Uani 1 1 d . . . . .
N2 N 0.5325(13) 0.6410(4) 0.6424(4) 0.034(2) Uani 1 1 d . . . . .
N3 N 0.5580(13) 0.7079(4) 0.7331(3) 0.028(2) Uani 1 1 d . . . . .
N4 N 0.5460(12) 0.6003(3) 0.7890(4) 0.032(2) Uani 1 1 d . . . . .
N5 N 1.0489(13) 0.5971(4) 0.7145(4) 0.042(2) Uani 1 1 d . . . . .
O1 O 0.5149(13) 0.4420(3) 0.8103(3) 0.049(3) Uani 1 1 d . . . . .
Pd1 Pd 0.54695(11) 0.62059(3) 0.71586(3) 0.0301(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.249(12) . ?
C1 C2 1.437(16) . ?
C1 C20 1.453(15) . ?
C2 N1 1.363(13) . ?
C2 C3 1.405(15) . ?
C3 C4 1.364(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.423(15) . ?
C4 H4 0.9500 . ?
C5 N1 1.381(14) . ?
C5 C6 1.401(16) . ?
C6 C7 1.361(15) . ?
C6 C21 1.500(15) . ?
C7 N2 1.413(13) . ?
C7 C8 1.451(15) . ?
C8 C9 1.343(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.422(16) . ?
C9 H9 0.9500 . ?
C10 N2 1.371(14) . ?
C10 C11 1.398(15) . ?
C11 C12 1.382(16) . ?
C11 C27 1.502(14) . ?
C12 N3 1.391(13) . ?
C12 C13 1.429(15) . ?
C13 C14 1.351(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.429(15) . ?
C14 H14 0.9500 . ?
C15 C16 1.361(16) . ?
C15 N3 1.375(14) . ?
C16 C17 1.397(15) . ?
C16 C33 1.494(16) . ?
C17 N4 1.400(13) . ?
C17 C18 1.415(16) . ?
C18 C19 1.341(16) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(16) . ?
C19 H19 0.9500 . ?
C20 N4 1.395(14) . ?
C21 C22 1.342(19) . ?
C21 C26 1.43(2) . ?
C22 F1 1.375(18) . ?
C22 C23 1.402(18) . ?
C23 C24 1.35(3) . ?
C23 F2 1.354(19) . ?
C24 F3 1.351(15) . ?
C24 C25 1.37(3) . ?
C25 F4 1.334(19) . ?
C25 C26 1.387(19) . ?
C26 F5 1.329(17) . ?
C27 C32 1.350(19) . ?
C27 C28 1.354(18) . ?
C28 F6 1.368(16) . ?
C28 C29 1.394(18) . ?
C29 F7 1.337(16) . ?
C29 C30 1.38(2) . ?
C30 C31 1.35(2) . ?
C30 F8 1.352(13) . ?
C31 F9 1.357(16) . ?
C31 C32 1.385(17) . ?
C32 F10 1.368(17) . ?
C33 C34 1.371(18) . ?
C33 C38 1.388(19) . ?
C34 F11 1.327(17) . ?
C34 C35 1.385(18) . ?
C35 F12 1.342(17) . ?
C35 C36 1.36(2) . ?
C36 F13 1.357(15) . ?
C36 C37 1.39(2) . ?
C37 F14 1.351(19) . ?
C37 C38 1.406(19) . ?
C38 F15 1.333(16) . ?
C39 C40 1.499(18) . ?
C39 N5 1.500(15) . ?
C39 H39 0.9900 . ?
C39 H39A 0.9900 . ?
C40 C41 1.476(19) . ?
C40 H40 0.9900 . ?
C40 H40A 0.9900 . ?
C41 C42 1.51(2) . ?
C41 H41 0.9900 . ?
C41 H41A 0.9900 . ?
C42 H42 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C43 C44 1.501(17) . ?
C43 N5 1.529(16) . ?
C43 H43 0.9900 . ?
C43 H43A 0.9900 . ?
C44 C45 1.523(19) . ?
C44 H44 0.9900 . ?
C44 H44A 0.9900 . ?
C45 C46 1.493(18) . ?
C45 H45 0.9900 . ?
C45 H45A 0.9900 . ?
C46 H46 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 N5 1.474(16) . ?
C47 C48 1.535(17) . ?
C47 H47 0.9900 . ?
C47 H47A 0.9900 . ?
C48 C49 1.503(17) . ?
C48 H48 0.9900 . ?
C48 H48A 0.9900 . ?
C49 C50 1.512(19) . ?
C49 H49 0.9900 . ?
C49 H49A 0.9900 . ?
C50 H50 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C51 C52 1.537(19) . ?
C51 N5 1.545(17) . ?
C51 H51 0.9900 . ?
C51 H51A 0.9900 . ?
C52 C53A 1.44(3) . ?
C52 C53B 1.67(4) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53A C54A 1.54(4) . ?
C53A H53A 0.9900 . ?
C53A H53B 0.9900 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C53B C54B 1.58(6) . ?
C53B H53C 0.9900 . ?
C53B H53D 0.9900 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
N1 Pd1 2.024(8) . ?
N2 Pd1 1.991(10) . ?
N3 Pd1 2.018(8) . ?
N4 Pd1 1.980(10) . ?

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
O1 C1 C2 120.1(10) . . ?
O1 C1 C20 118.8(11) . . ?
C2 C1 C20 121.2(9) . . ?
N1 C2 C3 109.8(10) . . ?
N1 C2 C1 126.0(9) . . ?
C3 C2 C1 123.8(9) . . ?
C4 C3 C2 107.7(9) . . ?
C4 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
C3 C4 C5 106.8(10) . . ?
C3 C4 H4 126.6 . . ?
C5 C4 H4 126.6 . . ?
N1 C5 C6 124.8(10) . . ?
N1 C5 C4 108.9(10) . . ?
C6 C5 C4 126.3(11) . . ?
C7 C6 C5 125.8(10) . . ?
C7 C6 C21 117.3(10) . . ?
C5 C6 C21 116.9(9) . . ?
C6 C7 N2 125.1(10) . . ?
C6 C7 C8 126.1(10) . . ?
N2 C7 C8 108.6(9) . . ?
C9 C8 C7 107.0(10) . . ?
C9 C8 H8 126.5 . . ?
C7 C8 H8 126.5 . . ?
C8 C9 C10 108.4(10) . . ?
C8 C9 H9 125.8 . . ?
C10 C9 H9 125.8 . . ?
N2 C10 C11 123.6(11) . . ?
N2 C10 C9 110.4(10) . . ?
C11 C10 C9 125.7(10) . . ?
C12 C11 C10 126.2(10) . . ?
C12 C11 C27 116.6(9) . . ?
C10 C11 C27 117.2(10) . . ?
C11 C12 N3 124.5(9) . . ?
C11 C12 C13 126.7(9) . . ?
N3 C12 C13 108.8(9) . . ?
C14 C13 C12 107.6(9) . . ?
C14 C13 H13 126.2 . . ?
C12 C13 H13 126.2 . . ?
C13 C14 C15 107.8(10) . . ?
C13 C14 H14 126.1 . . ?
C15 C14 H14 126.1 . . ?
C16 C15 N3 124.9(9) . . ?
C16 C15 C14 125.9(11) . . ?
N3 C15 C14 109.1(10) . . ?
C15 C16 C17 125.7(10) . . ?
C15 C16 C33 117.8(9) . . ?
C17 C16 C33 116.4(10) . . ?
C16 C17 N4 124.3(10) . . ?
C16 C17 C18 126.7(10) . . ?
N4 C17 C18 109.0(9) . . ?
C19 C18 C17 108.6(11) . . ?
C19 C18 H18 125.7 . . ?
C17 C18 H18 125.7 . . ?
C18 C19 C20 107.0(11) . . ?
C18 C19 H19 126.5 . . ?
C20 C19 H19 126.5 . . ?
C19 C20 N4 111.7(10) . . ?
C19 C20 C1 124.4(11) . . ?
N4 C20 C1 123.4(11) . . ?
C22 C21 C26 117.7(12) . . ?
C22 C21 C6 122.0(14) . . ?
C26 C21 C6 120.4(13) . . ?
C21 C22 F1 121.6(12) . . ?
C21 C22 C23 122.4(16) . . ?
F1 C22 C23 116.0(14) . . ?
C24 C23 F2 120.7(13) . . ?
C24 C23 C22 118.6(16) . . ?
F2 C23 C22 120.7(17) . . ?
C23 C24 F3 120.3(18) . . ?
C23 C24 C25 122.3(13) . . ?
F3 C24 C25 117.4(18) . . ?
F4 C25 C24 124.0(14) . . ?
F4 C25 C26 117.3(15) . . ?
C24 C25 C26 118.7(16) . . ?
F5 C26 C25 120.6(14) . . ?
F5 C26 C21 119.0(11) . . ?
C25 C26 C21 120.4(14) . . ?
C32 C27 C28 116.1(11) . . ?
C32 C27 C11 120.2(12) . . ?
C28 C27 C11 123.6(12) . . ?
C27 C28 F6 120.5(10) . . ?
C27 C28 C29 123.7(13) . . ?
F6 C28 C29 115.8(12) . . ?
F7 C29 C30 121.5(12) . . ?
F7 C29 C28 121.4(14) . . ?
C30 C29 C28 117.1(13) . . ?
C31 C30 F8 121.4(14) . . ?
C31 C30 C29 120.7(11) . . ?
F8 C30 C29 117.9(13) . . ?
C30 C31 F9 119.5(11) . . ?
C30 C31 C32 118.7(14) . . ?
F9 C31 C32 121.8(14) . . ?
C27 C32 F10 121.8(11) . . ?
C27 C32 C31 123.5(14) . . ?
F10 C32 C31 114.7(13) . . ?
C34 C33 C38 117.4(12) . . ?
C34 C33 C16 123.5(12) . . ?
C38 C33 C16 119.1(11) . . ?
F11 C34 C33 120.6(11) . . ?
F11 C34 C35 117.2(13) . . ?
C33 C34 C35 122.2(14) . . ?
F12 C35 C36 121.3(13) . . ?
F12 C35 C34 119.6(15) . . ?
C36 C35 C34 119.1(14) . . ?
F13 C36 C35 120.8(18) . . ?
F13 C36 C37 117.1(17) . . ?
C35 C36 C37 122.0(12) . . ?
F14 C37 C36 122.7(14) . . ?
F14 C37 C38 120.0(16) . . ?
C36 C37 C38 117.1(15) . . ?
F15 C38 C33 120.9(11) . . ?
F15 C38 C37 116.9(14) . . ?
C33 C38 C37 122.2(14) . . ?
C40 C39 N5 116.9(12) . . ?
C40 C39 H39 108.1 . . ?
N5 C39 H39 108.1 . . ?
C40 C39 H39A 108.1 . . ?
N5 C39 H39A 108.1 . . ?
H39 C39 H39A 107.3 . . ?
C41 C40 C39 112.4(13) . . ?
C41 C40 H40 109.1 . . ?
C39 C40 H40 109.1 . . ?
C41 C40 H40A 109.1 . . ?
C39 C40 H40A 109.1 . . ?
H40 C40 H40A 107.9 . . ?
C40 C41 C42 113.4(14) . . ?
C40 C41 H41 108.9 . . ?
C42 C41 H41 108.9 . . ?
C40 C41 H41A 108.9 . . ?
C42 C41 H41A 108.9 . . ?
H41 C41 H41A 107.7 . . ?
C41 C42 H42 109.5 . . ?
C41 C42 H42A 109.5 . . ?
H42 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C44 C43 N5 114.8(11) . . ?
C44 C43 H43 108.6 . . ?
N5 C43 H43 108.6 . . ?
C44 C43 H43A 108.6 . . ?
N5 C43 H43A 108.6 . . ?
H43 C43 H43A 107.5 . . ?
C43 C44 C45 110.6(12) . . ?
C43 C44 H44 109.5 . . ?
C45 C44 H44 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C45 C44 H44A 109.5 . . ?
H44 C44 H44A 108.1 . . ?
C46 C45 C44 113.3(13) . . ?
C46 C45 H45 108.9 . . ?
C44 C45 H45 108.9 . . ?
C46 C45 H45A 108.9 . . ?
C44 C45 H45A 108.9 . . ?
H45 C45 H45A 107.7 . . ?
C45 C46 H46 109.5 . . ?
C45 C46 H46A 109.5 . . ?
H46 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N5 C47 C48 116.3(11) . . ?
N5 C47 H47 108.2 . . ?
C48 C47 H47 108.2 . . ?
N5 C47 H47A 108.2 . . ?
C48 C47 H47A 108.2 . . ?
H47 C47 H47A 107.4 . . ?
C49 C48 C47 111.5(11) . . ?
C49 C48 H48 109.3 . . ?
C47 C48 H48 109.3 . . ?
C49 C48 H48A 109.3 . . ?
C47 C48 H48A 109.3 . . ?
H48 C48 H48A 108.0 . . ?
C48 C49 C50 112.1(12) . . ?
C48 C49 H49 109.2 . . ?
C50 C49 H49 109.2 . . ?
C48 C49 H49A 109.2 . . ?
C50 C49 H49A 109.2 . . ?
H49 C49 H49A 107.9 . . ?
C49 C50 H50 109.5 . . ?
C49 C50 H50A 109.5 . . ?
H50 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C52 C51 N5 114.4(12) . . ?
C52 C51 H51 108.7 . . ?
N5 C51 H51 108.7 . . ?
C52 C51 H51A 108.7 . . ?
N5 C51 H51A 108.7 . . ?
H51 C51 H51A 107.6 . . ?
C53A C52 C51 120.5(16) . . ?
C51 C52 C53B 101.3(16) . . ?
C53A C52 H52A 107.2 . . ?
C51 C52 H52A 107.2 . . ?
C53A C52 H52B 107.2 . . ?
C51 C52 H52B 107.2 . . ?
H52A C52 H52B 106.8 . . ?
C52 C53A C54A 112(2) . . ?
C52 C53A H53A 109.3 . . ?
C54A C53A H53A 109.3 . . ?
C52 C53A H53B 109.3 . . ?
C54A C53A H53B 109.3 . . ?
H53A C53A H53B 107.9 . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C54B C53B C52 106(3) . . ?
C54B C53B H53C 110.4 . . ?
C52 C53B H53C 110.4 . . ?
C54B C53B H53D 110.4 . . ?
C52 C53B H53D 110.4 . . ?
H53C C53B H53D 108.6 . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C2 N1 C5 106.7(8) . . ?
C2 N1 Pd1 127.3(7) . . ?
C5 N1 Pd1 125.3(7) . . ?
C10 N2 C7 105.6(9) . . ?
C10 N2 Pd1 128.2(8) . . ?
C7 N2 Pd1 126.1(7) . . ?
C15 N3 C12 106.7(9) . . ?
C15 N3 Pd1 126.7(7) . . ?
C12 N3 Pd1 126.5(7) . . ?
C20 N4 C17 103.7(9) . . ?
C20 N4 Pd1 129.1(8) . . ?
C17 N4 Pd1 126.6(6) . . ?
C47 N5 C39 111.7(10) . . ?
C47 N5 C43 109.3(10) . . ?
C39 N5 C43 108.0(10) . . ?
C47 N5 C51 109.7(10) . . ?
C39 N5 C51 110.8(10) . . ?
C43 N5 C51 107.1(10) . . ?
N4 Pd1 N2 176.3(5) . . ?
N4 Pd1 N3 90.3(3) . . ?
N2 Pd1 N3 89.9(3) . . ?
N4 Pd1 N1 89.3(3) . . ?
N2 Pd1 N1 90.9(3) . . ?
N3 Pd1 N1 174.7(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
_geom_torsion_publ_flag
O1 C1 C2 N1 165.0(12) . . . . ?
C20 C1 C2 N1 -16(2) . . . . ?
O1 C1 C2 C3 -7(2) . . . . ?
C20 C1 C2 C3 171.4(13) . . . . ?
N1 C2 C3 C4 1.0(14) . . . . ?
C1 C2 C3 C4 174.4(12) . . . . ?
C2 C3 C4 C5 -3.3(14) . . . . ?
C3 C4 C5 N1 4.5(14) . . . . ?
C3 C4 C5 C6 -171.4(13) . . . . ?
N1 C5 C6 C7 7(2) . . . . ?
C4 C5 C6 C7 -178.0(14) . . . . ?
N1 C5 C6 C21 -169.5(13) . . . . ?
C4 C5 C6 C21 6(2) . . . . ?
C5 C6 C7 N2 8(2) . . . . ?
C21 C6 C7 N2 -176.2(12) . . . . ?
C5 C6 C7 C8 -178.1(13) . . . . ?
C21 C6 C7 C8 -2(2) . . . . ?
C6 C7 C8 C9 -175.9(14) . . . . ?
N2 C7 C8 C9 -0.8(16) . . . . ?
C7 C8 C9 C10 1.8(16) . . . . ?
C8 C9 C10 N2 -2.2(17) . . . . ?
C8 C9 C10 C11 171.2(13) . . . . ?
N2 C10 C11 C12 -4(2) . . . . ?
C9 C10 C11 C12 -176.2(14) . . . . ?
N2 C10 C11 C27 174.9(12) . . . . ?
C9 C10 C11 C27 2(2) . . . . ?
C10 C11 C12 N3 -7(2) . . . . ?
C27 C11 C12 N3 175.0(12) . . . . ?
C10 C11 C12 C13 175.4(13) . . . . ?
C27 C11 C12 C13 -3(2) . . . . ?
C11 C12 C13 C14 178.5(13) . . . . ?
N3 C12 C13 C14 0.2(14) . . . . ?
C12 C13 C14 C15 -1.6(13) . . . . ?
C13 C14 C15 C16 -173.4(12) . . . . ?
C13 C14 C15 N3 2.6(13) . . . . ?
N3 C15 C16 C17 -1(2) . . . . ?
C14 C15 C16 C17 174.5(13) . . . . ?
N3 C15 C16 C33 -179.1(11) . . . . ?
C14 C15 C16 C33 -3.6(18) . . . . ?
C15 C16 C17 N4 12(2) . . . . ?
C33 C16 C17 N4 -170.1(12) . . . . ?
C15 C16 C17 C18 -169.1(14) . . . . ?
C33 C16 C17 C18 9(2) . . . . ?
C16 C17 C18 C19 -178.3(15) . . . . ?
N4 C17 C18 C19 1.1(18) . . . . ?
C17 C18 C19 C20 0.3(18) . . . . ?
C18 C19 C20 N4 -1.5(18) . . . . ?
C18 C19 C20 C1 170.2(15) . . . . ?
O1 C1 C20 C19 6(2) . . . . ?
C2 C1 C20 C19 -173.0(14) . . . . ?
O1 C1 C20 N4 176.6(13) . . . . ?
C2 C1 C20 N4 -2(2) . . . . ?
C7 C6 C21 C22 -70.5(17) . . . . ?
C5 C6 C21 C22 106.0(15) . . . . ?
C7 C6 C21 C26 111.2(15) . . . . ?
C5 C6 C21 C26 -72.3(16) . . . . ?
C26 C21 C22 F1 -179.9(11) . . . . ?
C6 C21 C22 F1 1.7(17) . . . . ?
C26 C21 C22 C23 -0.7(18) . . . . ?
C6 C21 C22 C23 -179.1(11) . . . . ?
C21 C22 C23 C24 2(2) . . . . ?
F1 C22 C23 C24 -178.3(12) . . . . ?
C21 C22 C23 F2 -179.5(11) . . . . ?
F1 C22 C23 F2 -0.2(17) . . . . ?
F2 C23 C24 F3 -2(2) . . . . ?
C22 C23 C24 F3 176.3(11) . . . . ?
F2 C23 C24 C25 180.0(13) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?
C23 C24 C25 F4 177.4(13) . . . . ?
F3 C24 C25 F4 -1(2) . . . . ?
C23 C24 C25 C26 0(2) . . . . ?
F3 C24 C25 C26 -178.5(12) . . . . ?
F4 C25 C26 F5 1.9(19) . . . . ?
C24 C25 C26 F5 179.7(12) . . . . ?
F4 C25 C26 C21 -175.8(11) . . . . ?
C24 C25 C26 C21 2(2) . . . . ?
C22 C21 C26 F5 -179.3(11) . . . . ?
C6 C21 C26 F5 -0.9(17) . . . . ?
C22 C21 C26 C25 -1.5(18) . . . . ?
C6 C21 C26 C25 176.9(11) . . . . ?
C12 C11 C27 C32 82.8(15) . . . . ?
C10 C11 C27 C32 -95.8(15) . . . . ?
C12 C11 C27 C28 -97.3(16) . . . . ?
C10 C11 C27 C28 84.1(16) . . . . ?
C32 C27 C28 F6 -178.6(12) . . . . ?
C11 C27 C28 F6 1.5(19) . . . . ?
C32 C27 C28 C29 1.7(19) . . . . ?
C11 C27 C28 C29 -178.3(11) . . . . ?
C27 C28 C29 F7 179.0(12) . . . . ?
F6 C28 C29 F7 -0.7(18) . . . . ?
C27 C28 C29 C30 -1(2) . . . . ?
F6 C28 C29 C30 179.7(11) . . . . ?
F7 C29 C30 C31 179.6(12) . . . . ?
C28 C29 C30 C31 -0.8(19) . . . . ?
F7 C29 C30 F8 -1.7(18) . . . . ?
C28 C29 C30 F8 177.9(11) . . . . ?
F8 C30 C31 F9 0.5(19) . . . . ?
C29 C30 C31 F9 179.2(12) . . . . ?
F8 C30 C31 C32 -177.7(11) . . . . ?
C29 C30 C31 C32 0.9(19) . . . . ?
C28 C27 C32 F10 -179.7(12) . . . . ?
C11 C27 C32 F10 0.2(18) . . . . ?
C28 C27 C32 C31 -1.6(19) . . . . ?
C11 C27 C32 C31 178.4(12) . . . . ?
C30 C31 C32 C27 0(2) . . . . ?
F9 C31 C32 C27 -177.9(12) . . . . ?
C30 C31 C32 F10 178.6(12) . . . . ?
F9 C31 C32 F10 0.4(19) . . . . ?
C15 C16 C33 C34 82.3(16) . . . . ?
C17 C16 C33 C34 -96.0(16) . . . . ?
C15 C16 C33 C38 -98.2(14) . . . . ?
C17 C16 C33 C38 83.4(16) . . . . ?
C38 C33 C34 F11 -178.4(12) . . . . ?
C16 C33 C34 F11 1(2) . . . . ?
C38 C33 C34 C35 -2(2) . . . . ?
C16 C33 C34 C35 177.8(12) . . . . ?
F11 C34 C35 F12 -2(2) . . . . ?
C33 C34 C35 F12 -179.2(13) . . . . ?
F11 C34 C35 C36 179.5(14) . . . . ?
C33 C34 C35 C36 3(2) . . . . ?
F12 C35 C36 F13 0(2) . . . . ?
C34 C35 C36 F13 177.9(13) . . . . ?
F12 C35 C36 C37 179.1(13) . . . . ?
C34 C35 C36 C37 -3(2) . . . . ?
F13 C36 C37 F14 -4(2) . . . . ?
C35 C36 C37 F14 176.6(14) . . . . ?
F13 C36 C37 C38 -178.6(12) . . . . ?
C35 C36 C37 C38 2(2) . . . . ?
C34 C33 C38 F15 -179.0(11) . . . . ?
C16 C33 C38 F15 1.5(17) . . . . ?
C34 C33 C38 C37 0.9(19) . . . . ?
C16 C33 C38 C37 -178.6(11) . . . . ?
F14 C37 C38 F15 4.1(18) . . . . ?
C36 C37 C38 F15 178.9(12) . . . . ?
F14 C37 C38 C33 -175.8(12) . . . . ?
C36 C37 C38 C33 -1.0(19) . . . . ?
N5 C39 C40 C41 -176.0(13) . . . . ?
C39 C40 C41 C42 179.6(16) . . . . ?
N5 C43 C44 C45 173.7(9) . . . . ?
C43 C44 C45 C46 172.5(11) . . . . ?
N5 C47 C48 C49 -164.5(12) . . . . ?
C47 C48 C49 C50 -168.5(12) . . . . ?
N5 C51 C52 C53A -146.9(16) . . . . ?
N5 C51 C52 C53B -109.8(17) . . . . ?
C51 C52 C53A C54A 73(3) . . . . ?
C51 C52 C53B C54B -180(2) . . . . ?
C3 C2 N1 C5 1.8(14) . . . . ?
C1 C2 N1 C5 -171.4(12) . . . . ?
C3 C2 N1 Pd1 -169.1(8) . . . . ?
C1 C2 N1 Pd1 17.6(19) . . . . ?
C6 C5 N1 C2 172.2(12) . . . . ?
C4 C5 N1 C2 -3.9(14) . . . . ?
C6 C5 N1 Pd1 -16.7(18) . . . . ?
C4 C5 N1 Pd1 167.3(8) . . . . ?
C11 C10 N2 C7 -172.0(13) . . . . ?
C9 C10 N2 C7 1.6(15) . . . . ?
C11 C10 N2 Pd1 12.8(19) . . . . ?
C9 C10 N2 Pd1 -173.6(10) . . . . ?
C6 C7 N2 C10 174.6(13) . . . . ?
C8 C7 N2 C10 -0.5(15) . . . . ?
C6 C7 N2 Pd1 -10(2) . . . . ?
C8 C7 N2 Pd1 174.9(9) . . . . ?
C16 C15 N3 C12 173.6(12) . . . . ?
C14 C15 N3 C12 -2.5(13) . . . . ?
C16 C15 N3 Pd1 -10.0(17) . . . . ?
C14 C15 N3 Pd1 173.9(8) . . . . ?
C11 C12 N3 C15 -177.0(12) . . . . ?
C13 C12 N3 C15 1.4(14) . . . . ?
C11 C12 N3 Pd1 6.7(19) . . . . ?
C13 C12 N3 Pd1 -174.9(8) . . . . ?
C19 C20 N4 C17 2.1(16) . . . . ?
C1 C20 N4 C17 -169.7(14) . . . . ?
C19 C20 N4 Pd1 -169.8(9) . . . . ?
C1 C20 N4 Pd1 18(2) . . . . ?
C16 C17 N4 C20 177.4(14) . . . . ?
C18 C17 N4 C20 -1.9(16) . . . . ?
C16 C17 N4 Pd1 -10(2) . . . . ?
C18 C17 N4 Pd1 170.2(9) . . . . ?
C48 C47 N5 C39 -166.1(11) . . . . ?
C48 C47 N5 C43 -46.6(15) . . . . ?
C48 C47 N5 C51 70.5(15) . . . . ?
C40 C39 N5 C47 176.3(13) . . . . ?
C40 C39 N5 C43 56.0(16) . . . . ?
C40 C39 N5 C51 -61.0(16) . . . . ?
C44 C43 N5 C47 -65.5(13) . . . . ?
C44 C43 N5 C39 56.3(14) . . . . ?
C44 C43 N5 C51 175.7(10) . . . . ?
C52 C51 N5 C47 65.4(14) . . . . ?
C52 C51 N5 C39 -58.5(14) . . . . ?
C52 C51 N5 C43 -176.1(10) . . . . ?

_refine_diff_density_max         1.378
_refine_diff_density_min         -2.332
_refine_diff_density_rms         0.145



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_171217_ys7-1_180906
_database_code_depnum_ccdc_archive 'CCDC 1906676'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_vrf_PLAT971_171217_ys7-1_180906 
;
PROBLEM: Check Calcd Resid. Dens. 1.34A From C47 5.51 eA-3  
RESPONSE: The large peaks around Pt atom are the ghost peak derived from 
the ripple of fourier series truncation error.
;

_vrf_PLAT973_171217_ys7-1_180906 
;
PROBLEM: Check Calcd Positive Resid. Density on Pt1 2.36 eA-3 
RESPONSE: The large peaks around Pt atom are the ghost peak derived from 
the ripple of fourier series truncation error.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H8 F15 N4 O Pt, C16 H36 N'
_chemical_formula_sum            'C54 H44 F15 N5 O Pt'
_chemical_formula_weight         1259.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -2.7169 9.8130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.1911(16)
_cell_length_b                   22.065(4)
_cell_length_c                   25.559(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4619.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    25047
_cell_measurement_theta_min      1.343
_cell_measurement_theta_max      27.498

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_F_000             2496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    4.001
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.7829
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            25047
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.343
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        27.498
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7915
_reflns_number_gt                6753
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.

 The large peaks around Pt atom are the ghost peak derived from 
 the ripple of Fourier series truncation errortruncation.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0270P)²+73.2969P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.472(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7915
_refine_ls_number_parameters     529
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1609
_refine_ls_wR_factor_gt          0.1351
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.551(2) 0.5071(7) 0.2141(8) 0.025(2) Uani 1 1 d . . . . .
C2 C 0.595(3) 0.5109(8) 0.2670(7) 0.025(2) Uani 1 1 d . . . . .
C3 C 0.642(2) 0.5626(8) 0.2911(8) 0.025(2) Uani 1 1 d . . . . .
H1 H 0.658056 0.600780 0.274730 0.031 Uiso 1 1 calc R U . . .
C4 C 0.661(3) 0.5503(9) 0.3425(8) 0.029(5) Uani 1 1 d . . . . .
H2 H 0.691084 0.578028 0.369236 0.035 Uiso 1 1 calc R U . . .
C5 C 0.628(2) 0.4880(9) 0.3484(7) 0.026(5) Uani 1 1 d . . . . .
C6 C 0.623(2) 0.4570(8) 0.3944(7) 0.0241(17) Uani 1 1 d . . . . .
C7 C 0.592(3) 0.3975(8) 0.4017(7) 0.0241(17) Uani 1 1 d . . . . .
C8 C 0.583(2) 0.3681(8) 0.4482(6) 0.0241(17) Uani 1 1 d . . . . .
H3 H 0.580857 0.386181 0.481940 0.029 Uiso 1 1 calc R U . . .
C9 C 0.577(3) 0.3088(8) 0.4376(7) 0.0241(17) Uani 1 1 d . . . . .
H4 H 0.573175 0.276729 0.462349 0.029 Uiso 1 1 calc R U . . .
C10 C 0.577(3) 0.3027(8) 0.3828(6) 0.0241(17) Uani 1 1 d . . . . .
C11 C 0.563(3) 0.2490(7) 0.3559(7) 0.022(2) Uani 1 1 d . . . . .
C12 C 0.565(3) 0.2429(7) 0.3034(7) 0.022(2) Uani 1 1 d . . . . .
C13 C 0.569(3) 0.1884(7) 0.2757(7) 0.022(2) Uani 1 1 d . . . . .
H5 H 0.568622 0.148908 0.290432 0.027 Uiso 1 1 calc R U . . .
C14 C 0.573(3) 0.2014(8) 0.2258(7) 0.028(4) Uani 1 1 d . . . . .
H6 H 0.576138 0.172910 0.197905 0.033 Uiso 1 1 calc R U . . .
C15 C 0.572(3) 0.2632(7) 0.2207(6) 0.022(4) Uani 1 1 d . . . . .
C16 C 0.557(3) 0.2952(8) 0.1760(7) 0.025(4) Uani 1 1 d . . . . .
C17 C 0.543(3) 0.3556(8) 0.1709(8) 0.034(3) Uani 1 1 d . . . . .
C18 C 0.496(3) 0.3870(9) 0.1238(8) 0.034(3) Uani 1 1 d . . . . .
H7 H 0.470818 0.369568 0.090793 0.041 Uiso 1 1 calc R U . . .
C19 C 0.494(3) 0.4460(9) 0.1364(8) 0.034(3) Uani 1 1 d . . . . .
H8 H 0.473300 0.478513 0.112991 0.041 Uiso 1 1 calc R U . . .
C20 C 0.528(3) 0.4516(8) 0.1887(7) 0.028(5) Uani 1 1 d . . . . .
C21 C 0.6336(16) 0.4941(5) 0.4418(4) 0.030(5) Uani 1 1 d G . . . .
C22 C 0.4936(14) 0.5057(6) 0.4708(5) 0.038(6) Uani 1 1 d G . . . .
C23 C 0.5021(16) 0.5420(7) 0.5152(5) 0.039(6) Uani 1 1 d G . . . .
C24 C 0.651(2) 0.5666(6) 0.5306(4) 0.041(6) Uani 1 1 d G . . . .
C25 C 0.7909(15) 0.5550(6) 0.5016(5) 0.037(5) Uani 1 1 d G . . . .
C26 C 0.7823(14) 0.5187(6) 0.4572(5) 0.032(5) Uani 1 1 d G . . . .
C27 C 0.5661(19) 0.1925(4) 0.3864(4) 0.024(4) Uani 1 1 d G . . . .
C28 C 0.4195(16) 0.1635(6) 0.3977(5) 0.038(5) Uani 1 1 d G . . . .
C29 C 0.4195(18) 0.1102(6) 0.4267(5) 0.034(5) Uani 1 1 d G . . . .
C30 C 0.566(2) 0.0858(4) 0.4443(5) 0.037(5) Uani 1 1 d G . . . .
C31 C 0.7125(18) 0.1148(6) 0.4331(5) 0.051(7) Uani 1 1 d G . . . .
C32 C 0.7125(16) 0.1681(6) 0.4041(6) 0.038(5) Uani 1 1 d G . . . .
C33 C 0.5651(18) 0.2603(6) 0.1267(4) 0.030(5) Uani 1 1 d G . . . .
C34 C 0.4283(15) 0.2332(6) 0.1046(5) 0.036(5) Uani 1 1 d G . . . .
C35 C 0.4415(18) 0.2027(6) 0.0572(5) 0.045(6) Uani 1 1 d G . . . .
C36 C 0.591(2) 0.1993(6) 0.0319(4) 0.044(6) Uani 1 1 d G . . . .
C37 C 0.7282(17) 0.2263(6) 0.0540(5) 0.042(6) Uani 1 1 d G . . . .
C38 C 0.7151(15) 0.2569(6) 0.1014(5) 0.032(5) Uani 1 1 d G . . . .
C39 C 0.192(3) 0.4610(10) 0.2844(11) 0.047(3) Uani 1 1 d . . . . .
H9 H 0.241033 0.481060 0.253538 0.057 Uiso 1 1 calc R U . . .
H10 H 0.281059 0.440845 0.303930 0.057 Uiso 1 1 calc R U . . .
C40 C 0.116(3) 0.5092(10) 0.3192(11) 0.052(7) Uani 1 1 d . . . . .
H11 H 0.016064 0.525227 0.302557 0.062 Uiso 1 1 calc R U . . .
H12 H 0.085357 0.491047 0.353260 0.062 Uiso 1 1 calc R U . . .
C41 C 0.231(4) 0.5582(12) 0.3278(11) 0.065(9) Uani 1 1 d . . . . .
H13 H 0.241785 0.581959 0.295119 0.078 Uiso 1 1 calc R U . . .
H14 H 0.339202 0.540939 0.336264 0.078 Uiso 1 1 calc R U . . .
C42 C 0.179(4) 0.5986(11) 0.3704(10) 0.059(8) Uani 1 1 d . . . . .
H33 H 0.072837 0.616357 0.361828 0.089 Uiso 1 1 calc R U . . .
H34 H 0.259911 0.631018 0.374706 0.089 Uiso 1 1 calc R U . . .
H35 H 0.170575 0.575429 0.402948 0.089 Uiso 1 1 calc R U . . .
C43 C -0.051(3) 0.4393(10) 0.2295(8) 0.038(2) Uani 1 1 d . . . . .
H15 H -0.104037 0.474686 0.246054 0.046 Uiso 1 1 calc R U . . .
H16 H -0.135541 0.408133 0.223251 0.046 Uiso 1 1 calc R U . . .
C44 C 0.023(3) 0.4583(10) 0.1776(9) 0.038(2) Uani 1 1 d . . . . .
H17 H 0.026621 0.422846 0.153920 0.046 Uiso 1 1 calc R U . . .
H18 H 0.136326 0.472206 0.183383 0.046 Uiso 1 1 calc R U . . .
C45 C -0.074(3) 0.5088(9) 0.1514(8) 0.038(2) Uani 1 1 d . . . . .
H19 H -0.191722 0.499606 0.152912 0.046 Uiso 1 1 calc R U . . .
H20 H -0.041329 0.512199 0.114170 0.046 Uiso 1 1 calc R U . . .
C46 C -0.039(4) 0.5683(13) 0.1795(10) 0.073(10) Uani 1 1 d . . . . .
H36 H -0.105183 0.570465 0.211430 0.109 Uiso 1 1 calc R U . . .
H37 H -0.066774 0.602272 0.156521 0.109 Uiso 1 1 calc R U . . .
H38 H 0.076925 0.570321 0.188751 0.109 Uiso 1 1 calc R U . . .
C47 C 0.179(3) 0.3684(11) 0.2402(9) 0.047(3) Uani 1 1 d . . . . .
H21 H 0.260929 0.353348 0.265377 0.057 Uiso 1 1 calc R U . . .
H22 H 0.237248 0.387511 0.210630 0.057 Uiso 1 1 calc R U . . .
C48 C 0.072(3) 0.3122(9) 0.2188(9) 0.047(3) Uani 1 1 d . . . . .
H23 H -0.045393 0.321954 0.221303 0.057 Uiso 1 1 calc R U . . .
H24 H 0.098641 0.304842 0.181491 0.057 Uiso 1 1 calc R U . . .
C49 C 0.108(3) 0.2565(10) 0.2498(9) 0.047(3) Uani 1 1 d . . . . .
H25 H 0.066111 0.261549 0.285906 0.057 Uiso 1 1 calc R U . . .
H26 H 0.227416 0.250193 0.251746 0.057 Uiso 1 1 calc R U . . .
C50 C 0.029(3) 0.2027(10) 0.2250(12) 0.060(8) Uani 1 1 d . . . . .
H39 H -0.088899 0.209343 0.222570 0.090 Uiso 1 1 calc R U . . .
H40 H 0.050581 0.166578 0.246219 0.090 Uiso 1 1 calc R U . . .
H41 H 0.074102 0.196787 0.189797 0.090 Uiso 1 1 calc R U . . .
C51 C -0.008(2) 0.3872(10) 0.3115(8) 0.038(2) Uani 1 1 d . . . . .
H27 H -0.077791 0.353608 0.298815 0.046 Uiso 1 1 calc R U . . .
H28 H -0.081081 0.418204 0.326868 0.046 Uiso 1 1 calc R U . . .
C52 C 0.099(3) 0.3635(9) 0.3534(8) 0.038(2) Uani 1 1 d . . . . .
H29 H 0.166567 0.329964 0.339470 0.046 Uiso 1 1 calc R U . . .
H30 H 0.173516 0.396029 0.365451 0.046 Uiso 1 1 calc R U . . .
C53 C 0.001(3) 0.3414(14) 0.3980(12) 0.068(9) Uani 1 1 d . . . . .
H31 H -0.064502 0.375690 0.411781 0.082 Uiso 1 1 calc R U . . .
H32 H -0.076945 0.310540 0.384892 0.082 Uiso 1 1 calc R U . . .
C54 C 0.093(4) 0.3153(11) 0.4408(10) 0.057(7) Uani 1 1 d . . . . .
H42 H 0.115063 0.272442 0.433443 0.085 Uiso 1 1 calc R U . . .
H43 H 0.030461 0.318714 0.473312 0.085 Uiso 1 1 calc R U . . .
H44 H 0.196981 0.337000 0.444619 0.085 Uiso 1 1 calc R U . . .
N1 N 0.5944(18) 0.4640(6) 0.3008(5) 0.0206(16) Uani 1 1 d . . . . .
N2 N 0.5806(19) 0.3583(6) 0.3607(5) 0.0206(16) Uani 1 1 d . . . . .
N3 N 0.568(2) 0.2891(6) 0.2689(5) 0.0206(16) Uani 1 1 d . . . . .
N4 N 0.5518(16) 0.3961(6) 0.2101(6) 0.0206(16) Uani 1 1 d . . . . .
N5 N 0.075(2) 0.4142(7) 0.2661(6) 0.038(2) Uani 1 1 d . . . . .
O1 O 0.5283(19) 0.5543(6) 0.1892(5) 0.037(4) Uani 1 1 d . . . . .
F1 F 0.3559(16) 0.4851(6) 0.4575(5) 0.044(3) Uani 1 1 d . . . . .
F2 F 0.3747(17) 0.5527(6) 0.5425(5) 0.048(4) Uani 1 1 d . . . . .
F3 F 0.6553(17) 0.6011(6) 0.5696(5) 0.048(3) Uani 1 1 d . . . . .
F4 F 0.926(2) 0.5796(5) 0.5128(4) 0.048(3) Uani 1 1 d . . . . .
F5 F 0.9120(18) 0.5069(5) 0.4316(4) 0.042(3) Uani 1 1 d . . . . .
F6 F 0.2832(18) 0.1843(6) 0.3814(6) 0.052(4) Uani 1 1 d . . . . .
F7 F 0.287(2) 0.0834(6) 0.4368(6) 0.057(4) Uani 1 1 d . . . . .
F8 F 0.565(2) 0.0374(5) 0.4715(4) 0.053(4) Uani 1 1 d . . . . .
F9 F 0.8512(19) 0.0914(6) 0.4482(7) 0.062(5) Uani 1 1 d . . . . .
F10 F 0.8460(18) 0.1929(6) 0.3931(7) 0.056(4) Uani 1 1 d . . . . .
F11 F 0.2931(17) 0.2359(7) 0.1272(5) 0.054(4) Uani 1 1 d . . . . .
F12 F 0.316(2) 0.1776(8) 0.0378(6) 0.069(5) Uani 1 1 d . . . . .
F13 F 0.604(2) 0.1708(6) -0.0115(5) 0.060(4) Uani 1 1 d . . . . .
F14 F 0.8675(18) 0.2207(7) 0.0317(5) 0.059(4) Uani 1 1 d . . . . .
F15 F 0.8440(15) 0.2813(6) 0.1204(5) 0.039(3) Uani 1 1 d . . . . .
PT1 Pt 0.57465(8) 0.37668(3) 0.28558(3) 0.0193(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.23(2) . ?
C1 C20 1.40(2) . ?
C1 C2 1.40(3) . ?
C2 N1 1.35(2) . ?
C2 C3 1.35(3) . ?
C3 C4 1.35(3) . ?
C3 H1 0.9500 . ?
C4 C5 1.41(3) . ?
C4 H2 0.9500 . ?
C5 N1 1.35(2) . ?
C5 C6 1.36(3) . ?
C6 C7 1.35(2) . ?
C6 C21 1.47(2) . ?
C7 C8 1.36(2) . ?
C7 N2 1.36(2) . ?
C8 C9 1.34(2) . ?
C8 H3 0.9500 . ?
C9 C10 1.40(2) . ?
C9 H4 0.9500 . ?
C10 N2 1.35(2) . ?
C10 C11 1.38(2) . ?
C11 C12 1.35(2) . ?
C11 C27 1.471(18) . ?
C12 N3 1.35(2) . ?
C12 C13 1.40(2) . ?
C13 C14 1.31(2) . ?
C13 H5 0.9500 . ?
C14 C15 1.37(2) . ?
C14 H6 0.9500 . ?
C15 C16 1.35(2) . ?
C15 N3 1.36(2) . ?
C16 C17 1.34(3) . ?
C16 C33 1.480(19) . ?
C17 N4 1.34(2) . ?
C17 C18 1.44(3) . ?
C18 C19 1.34(3) . ?
C18 H7 0.9500 . ?
C19 C20 1.37(3) . ?
C19 H8 0.9500 . ?
C20 N4 1.36(2) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 F1 1.263(16) . ?
C22 C23 1.3900 . ?
C23 F2 1.277(16) . ?
C23 C24 1.3900 . ?
C24 F3 1.254(15) . ?
C24 C25 1.3900 . ?
C25 F4 1.263(18) . ?
C25 C26 1.3900 . ?
C26 F5 1.276(17) . ?
C27 C28 1.3900 . ?
C27 C32 1.3900 . ?
C28 F6 1.277(18) . ?
C28 C29 1.3900 . ?
C29 F7 1.260(17) . ?
C29 C30 1.3900 . ?
C30 F8 1.274(13) . ?
C30 C31 1.3900 . ?
C31 F9 1.306(17) . ?
C31 C32 1.3900 . ?
C32 F10 1.254(18) . ?
C33 C34 1.3900 . ?
C33 C38 1.3900 . ?
C34 F11 1.251(17) . ?
C34 C35 1.3900 . ?
C35 F12 1.266(18) . ?
C35 C36 1.3900 . ?
C36 F13 1.279(14) . ?
C36 C37 1.3900 . ?
C37 F14 1.282(17) . ?
C37 C38 1.3900 . ?
C38 F15 1.281(16) . ?
C39 N5 1.48(3) . ?
C39 C40 1.52(3) . ?
C39 H9 0.9900 . ?
C39 H10 0.9900 . ?
C40 C41 1.45(3) . ?
C40 H11 0.9900 . ?
C40 H12 0.9900 . ?
C41 C42 1.47(3) . ?
C41 H13 0.9900 . ?
C41 H14 0.9900 . ?
C42 H33 0.9800 . ?
C42 H34 0.9800 . ?
C42 H35 0.9800 . ?
C43 N5 1.50(3) . ?
C43 C44 1.52(3) . ?
C43 H15 0.9900 . ?
C43 H16 0.9900 . ?
C44 C45 1.52(3) . ?
C44 H17 0.9900 . ?
C44 H18 0.9900 . ?
C45 C46 1.52(3) . ?
C45 H19 0.9900 . ?
C45 H20 0.9900 . ?
C46 H36 0.9800 . ?
C46 H37 0.9800 . ?
C46 H38 0.9800 . ?
C47 N5 1.47(3) . ?
C47 C48 1.61(3) . ?
C47 H21 0.9900 . ?
C47 H22 0.9900 . ?
C48 C49 1.49(3) . ?
C48 H23 0.9900 . ?
C48 H24 0.9900 . ?
C49 C50 1.49(3) . ?
C49 H25 0.9900 . ?
C49 H26 0.9900 . ?
C50 H39 0.9800 . ?
C50 H40 0.9800 . ?
C50 H41 0.9800 . ?
C51 N5 1.47(3) . ?
C51 C52 1.48(3) . ?
C51 H27 0.9900 . ?
C51 H28 0.9900 . ?
C52 C53 1.48(3) . ?
C52 H29 0.9900 . ?
C52 H30 0.9900 . ?
C53 C54 1.45(3) . ?
C53 H31 0.9900 . ?
C53 H32 0.9900 . ?
C54 H42 0.9800 . ?
C54 H43 0.9800 . ?
C54 H44 0.9800 . ?
N1 PT1 1.972(14) . ?
N2 PT1 1.962(14) . ?
N3 PT1 1.980(13) . ?
N4 PT1 1.985(15) . ?

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
O1 C1 C20 118.6(19) . . ?
O1 C1 C2 119.1(16) . . ?
C20 C1 C2 122.3(16) . . ?
N1 C2 C3 111.0(16) . . ?
N1 C2 C1 124.8(16) . . ?
C3 C2 C1 124.2(17) . . ?
C2 C3 C4 107.8(17) . . ?
C2 C3 H1 126.1 . . ?
C4 C3 H1 126.1 . . ?
C3 C4 C5 106.1(18) . . ?
C3 C4 H2 127.0 . . ?
C5 C4 H2 127.0 . . ?
N1 C5 C6 124.9(18) . . ?
N1 C5 C4 109.0(17) . . ?
C6 C5 C4 126.1(18) . . ?
C7 C6 C5 127.9(18) . . ?
C7 C6 C21 116.1(15) . . ?
C5 C6 C21 115.7(16) . . ?
C6 C7 C8 126.6(17) . . ?
C6 C7 N2 121.7(16) . . ?
C8 C7 N2 111.5(15) . . ?
C9 C8 C7 106.9(15) . . ?
C9 C8 H3 126.5 . . ?
C7 C8 H3 126.5 . . ?
C8 C9 C10 107.2(15) . . ?
C8 C9 H4 126.4 . . ?
C10 C9 H4 126.4 . . ?
N2 C10 C11 125.1(16) . . ?
N2 C10 C9 109.3(15) . . ?
C11 C10 C9 125.4(16) . . ?
C12 C11 C10 125.6(16) . . ?
C12 C11 C27 116.3(14) . . ?
C10 C11 C27 117.6(15) . . ?
C11 C12 N3 125.2(15) . . ?
C11 C12 C13 126.2(16) . . ?
N3 C12 C13 108.5(15) . . ?
C14 C13 C12 107.9(15) . . ?
C14 C13 H5 126.0 . . ?
C12 C13 H5 126.0 . . ?
C13 C14 C15 108.0(16) . . ?
C13 C14 H6 126.0 . . ?
C15 C14 H6 126.0 . . ?
C16 C15 N3 123.0(15) . . ?
C16 C15 C14 127.0(16) . . ?
N3 C15 C14 109.5(15) . . ?
C17 C16 C15 127.5(17) . . ?
C17 C16 C33 116.0(16) . . ?
C15 C16 C33 116.4(15) . . ?
N4 C17 C16 125.6(17) . . ?
N4 C17 C18 108.5(16) . . ?
C16 C17 C18 125.5(19) . . ?
C19 C18 C17 105.5(18) . . ?
C19 C18 H7 127.2 . . ?
C17 C18 H7 127.2 . . ?
C18 C19 C20 108.7(18) . . ?
C18 C19 H8 125.7 . . ?
C20 C19 H8 125.7 . . ?
N4 C20 C19 109.9(16) . . ?
N4 C20 C1 125.9(18) . . ?
C19 C20 C1 124.0(18) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 C6 119.6(12) . . ?
C26 C21 C6 120.4(12) . . ?
F1 C22 C23 118.3(12) . . ?
F1 C22 C21 121.7(12) . . ?
C23 C22 C21 120.0 . . ?
F2 C23 C22 120.7(12) . . ?
F2 C23 C24 119.3(12) . . ?
C22 C23 C24 120.0 . . ?
F3 C24 C25 120.8(13) . . ?
F3 C24 C23 119.2(13) . . ?
C25 C24 C23 120.0 . . ?
F4 C25 C24 121.3(12) . . ?
F4 C25 C26 118.5(12) . . ?
C24 C25 C26 120.0 . . ?
F5 C26 C25 119.7(11) . . ?
F5 C26 C21 120.3(11) . . ?
C25 C26 C21 120.0 . . ?
C28 C27 C32 120.0 . . ?
C28 C27 C11 118.9(13) . . ?
C32 C27 C11 121.1(13) . . ?
F6 C28 C29 118.6(12) . . ?
F6 C28 C27 121.4(12) . . ?
C29 C28 C27 120.0 . . ?
F7 C29 C28 120.5(13) . . ?
F7 C29 C30 119.5(13) . . ?
C28 C29 C30 120.0 . . ?
F8 C30 C31 120.3(15) . . ?
F8 C30 C29 119.7(15) . . ?
C31 C30 C29 120.0 . . ?
F9 C31 C32 119.4(12) . . ?
F9 C31 C30 120.6(12) . . ?
C32 C31 C30 120.0 . . ?
F10 C32 C31 119.3(12) . . ?
F10 C32 C27 120.7(12) . . ?
C31 C32 C27 120.0 . . ?
C34 C33 C38 120.0 . . ?
C34 C33 C16 122.4(13) . . ?
C38 C33 C16 117.6(13) . . ?
F11 C34 C35 119.6(11) . . ?
F11 C34 C33 120.4(11) . . ?
C35 C34 C33 120.0 . . ?
F12 C35 C34 119.3(13) . . ?
F12 C35 C36 120.7(13) . . ?
C34 C35 C36 120.0 . . ?
F13 C36 C37 119.9(14) . . ?
F13 C36 C35 120.1(14) . . ?
C37 C36 C35 120.0 . . ?
F14 C37 C36 119.6(13) . . ?
F14 C37 C38 120.3(13) . . ?
C36 C37 C38 120.0 . . ?
F15 C38 C37 118.0(11) . . ?
F15 C38 C33 122.0(11) . . ?
C37 C38 C33 120.0 . . ?
N5 C39 C40 114.2(19) . . ?
N5 C39 H9 108.7 . . ?
C40 C39 H9 108.7 . . ?
N5 C39 H10 108.7 . . ?
C40 C39 H10 108.7 . . ?
H9 C39 H10 107.6 . . ?
C41 C40 C39 110(2) . . ?
C41 C40 H11 109.6 . . ?
C39 C40 H11 109.6 . . ?
C41 C40 H12 109.6 . . ?
C39 C40 H12 109.6 . . ?
H11 C40 H12 108.1 . . ?
C40 C41 C42 112(2) . . ?
C40 C41 H13 109.2 . . ?
C42 C41 H13 109.2 . . ?
C40 C41 H14 109.2 . . ?
C42 C41 H14 109.2 . . ?
H13 C41 H14 107.9 . . ?
C41 C42 H33 109.5 . . ?
C41 C42 H34 109.5 . . ?
H33 C42 H34 109.5 . . ?
C41 C42 H35 109.5 . . ?
H33 C42 H35 109.5 . . ?
H34 C42 H35 109.5 . . ?
N5 C43 C44 112.0(18) . . ?
N5 C43 H15 109.2 . . ?
C44 C43 H15 109.2 . . ?
N5 C43 H16 109.2 . . ?
C44 C43 H16 109.2 . . ?
H15 C43 H16 107.9 . . ?
C43 C44 C45 112.5(19) . . ?
C43 C44 H17 109.1 . . ?
C45 C44 H17 109.1 . . ?
C43 C44 H18 109.1 . . ?
C45 C44 H18 109.1 . . ?
H17 C44 H18 107.8 . . ?
C44 C45 C46 109(2) . . ?
C44 C45 H19 109.9 . . ?
C46 C45 H19 109.9 . . ?
C44 C45 H20 109.9 . . ?
C46 C45 H20 109.9 . . ?
H19 C45 H20 108.3 . . ?
C45 C46 H36 109.5 . . ?
C45 C46 H37 109.5 . . ?
H36 C46 H37 109.5 . . ?
C45 C46 H38 109.5 . . ?
H36 C46 H38 109.5 . . ?
H37 C46 H38 109.5 . . ?
N5 C47 C48 111.8(19) . . ?
N5 C47 H21 109.3 . . ?
C48 C47 H21 109.3 . . ?
N5 C47 H22 109.3 . . ?
C48 C47 H22 109.3 . . ?
H21 C47 H22 107.9 . . ?
C49 C48 C47 110.3(19) . . ?
C49 C48 H23 109.6 . . ?
C47 C48 H23 109.6 . . ?
C49 C48 H24 109.6 . . ?
C47 C48 H24 109.6 . . ?
H23 C48 H24 108.1 . . ?
C48 C49 C50 110.1(19) . . ?
C48 C49 H25 109.6 . . ?
C50 C49 H25 109.6 . . ?
C48 C49 H26 109.6 . . ?
C50 C49 H26 109.6 . . ?
H25 C49 H26 108.2 . . ?
C49 C50 H39 109.5 . . ?
C49 C50 H40 109.5 . . ?
H39 C50 H40 109.5 . . ?
C49 C50 H41 109.5 . . ?
H39 C50 H41 109.5 . . ?
H40 C50 H41 109.5 . . ?
N5 C51 C52 116.0(17) . . ?
N5 C51 H27 108.3 . . ?
C52 C51 H27 108.3 . . ?
N5 C51 H28 108.3 . . ?
C52 C51 H28 108.3 . . ?
H27 C51 H28 107.4 . . ?
C53 C52 C51 110.5(18) . . ?
C53 C52 H29 109.6 . . ?
C51 C52 H29 109.6 . . ?
C53 C52 H30 109.6 . . ?
C51 C52 H30 109.6 . . ?
H29 C52 H30 108.1 . . ?
C54 C53 C52 115(2) . . ?
C54 C53 H31 108.5 . . ?
C52 C53 H31 108.5 . . ?
C54 C53 H32 108.5 . . ?
C52 C53 H32 108.5 . . ?
H31 C53 H32 107.5 . . ?
C53 C54 H42 109.5 . . ?
C53 C54 H43 109.5 . . ?
H42 C54 H43 109.5 . . ?
C53 C54 H44 109.5 . . ?
H42 C54 H44 109.5 . . ?
H43 C54 H44 109.5 . . ?
C2 N1 C5 105.9(15) . . ?
C2 N1 PT1 128.6(12) . . ?
C5 N1 PT1 125.2(12) . . ?
C10 N2 C7 104.8(14) . . ?
C10 N2 PT1 126.7(11) . . ?
C7 N2 PT1 128.5(11) . . ?
C12 N3 C15 106.0(13) . . ?
C12 N3 PT1 126.6(11) . . ?
C15 N3 PT1 127.3(11) . . ?
C17 N4 C20 107.1(15) . . ?
C17 N4 PT1 125.8(11) . . ?
C20 N4 PT1 126.9(12) . . ?
C51 N5 C47 110.0(18) . . ?
C51 N5 C39 109.4(17) . . ?
C47 N5 C39 104.5(18) . . ?
C51 N5 C43 108.7(17) . . ?
C47 N5 C43 111.6(16) . . ?
C39 N5 C43 112.6(17) . . ?
N2 PT1 N1 90.4(5) . . ?
N2 PT1 N3 90.5(5) . . ?
N1 PT1 N3 176.8(7) . . ?
N2 PT1 N4 176.0(6) . . ?
N1 PT1 N4 89.3(5) . . ?
N3 PT1 N4 89.9(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
_geom_torsion_publ_flag
O1 C1 C2 N1 167.3(19) . . . . ?
C20 C1 C2 N1 -11(3) . . . . ?
O1 C1 C2 C3 -12(3) . . . . ?
C20 C1 C2 C3 170(2) . . . . ?
N1 C2 C3 C4 -4(2) . . . . ?
C1 C2 C3 C4 175(2) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
C3 C4 C5 N1 2(2) . . . . ?
C3 C4 C5 C6 -175.6(19) . . . . ?
N1 C5 C6 C7 3(3) . . . . ?
C4 C5 C6 C7 -180(2) . . . . ?
N1 C5 C6 C21 -169.2(17) . . . . ?
C4 C5 C6 C21 8(3) . . . . ?
C5 C6 C7 C8 -178(2) . . . . ?
C21 C6 C7 C8 -5(3) . . . . ?
C5 C6 C7 N2 8(3) . . . . ?
C21 C6 C7 N2 -179.4(17) . . . . ?
C6 C7 C8 C9 -170(2) . . . . ?
N2 C7 C8 C9 4(3) . . . . ?
C7 C8 C9 C10 -2(3) . . . . ?
C8 C9 C10 N2 -1(3) . . . . ?
C8 C9 C10 C11 -176(2) . . . . ?
N2 C10 C11 C12 6(4) . . . . ?
C9 C10 C11 C12 -179(2) . . . . ?
N2 C10 C11 C27 178(2) . . . . ?
C9 C10 C11 C27 -7(4) . . . . ?
C10 C11 C12 N3 -6(4) . . . . ?
C27 C11 C12 N3 -177.7(19) . . . . ?
C10 C11 C12 C13 172(2) . . . . ?
C27 C11 C12 C13 0(4) . . . . ?
C11 C12 C13 C14 -179(2) . . . . ?
N3 C12 C13 C14 0(3) . . . . ?
C12 C13 C14 C15 0(3) . . . . ?
C13 C14 C15 C16 -172(2) . . . . ?
C13 C14 C15 N3 0(3) . . . . ?
N3 C15 C16 C17 3(4) . . . . ?
C14 C15 C16 C17 174(3) . . . . ?
N3 C15 C16 C33 180(2) . . . . ?
C14 C15 C16 C33 -9(4) . . . . ?
C15 C16 C17 N4 5(4) . . . . ?
C33 C16 C17 N4 -172.2(19) . . . . ?
C15 C16 C17 C18 -167(2) . . . . ?
C33 C16 C17 C18 16(4) . . . . ?
N4 C17 C18 C19 6(3) . . . . ?
C16 C17 C18 C19 179(2) . . . . ?
C17 C18 C19 C20 -3(3) . . . . ?
C18 C19 C20 N4 0(3) . . . . ?
C18 C19 C20 C1 174(2) . . . . ?
O1 C1 C20 N4 178.4(19) . . . . ?
C2 C1 C20 N4 -3(3) . . . . ?
O1 C1 C20 C19 6(3) . . . . ?
C2 C1 C20 C19 -176(2) . . . . ?
C7 C6 C21 C22 -70.2(19) . . . . ?
C5 C6 C21 C22 103.2(17) . . . . ?
C7 C6 C21 C26 111.3(17) . . . . ?
C5 C6 C21 C26 -75.3(19) . . . . ?
C26 C21 C22 F1 178.6(16) . . . . ?
C6 C21 C22 F1 0.2(16) . . . . ?
C26 C21 C22 C23 0.0 . . . . ?
C6 C21 C22 C23 -178.5(13) . . . . ?
F1 C22 C23 F2 1.9(15) . . . . ?
C21 C22 C23 F2 -179.4(15) . . . . ?
F1 C22 C23 C24 -178.7(15) . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
F2 C23 C24 F3 -3.2(16) . . . . ?
C22 C23 C24 F3 177.3(15) . . . . ?
F2 C23 C24 C25 179.4(15) . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
F3 C24 C25 F4 -1.5(16) . . . . ?
C23 C24 C25 F4 175.8(15) . . . . ?
F3 C24 C25 C26 -177.3(15) . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
F4 C25 C26 F5 6.0(15) . . . . ?
C24 C25 C26 F5 -178.1(14) . . . . ?
F4 C25 C26 C21 -175.9(15) . . . . ?
C24 C25 C26 C21 0.0 . . . . ?
C22 C21 C26 F5 178.1(14) . . . . ?
C6 C21 C26 F5 -3.4(16) . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
C6 C21 C26 C25 178.5(13) . . . . ?
C12 C11 C27 C28 -87(2) . . . . ?
C10 C11 C27 C28 101(2) . . . . ?
C12 C11 C27 C32 93(2) . . . . ?
C10 C11 C27 C32 -79(2) . . . . ?
C32 C27 C28 F6 -179.0(16) . . . . ?
C11 C27 C28 F6 1.2(17) . . . . ?
C32 C27 C28 C29 0.0 . . . . ?
C11 C27 C28 C29 -179.8(13) . . . . ?
F6 C28 C29 F7 -0.5(17) . . . . ?
C27 C28 C29 F7 -179.6(16) . . . . ?
F6 C28 C29 C30 179.1(15) . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
F7 C29 C30 F8 -1.4(16) . . . . ?
C28 C29 C30 F8 179.0(13) . . . . ?
F7 C29 C30 C31 179.6(16) . . . . ?
C28 C29 C30 C31 0.0 . . . . ?
F8 C30 C31 F9 2.9(17) . . . . ?
C29 C30 C31 F9 -178.1(16) . . . . ?
F8 C30 C31 C32 -179.0(13) . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
F9 C31 C32 F10 -0.1(16) . . . . ?
C30 C31 C32 F10 -178.2(16) . . . . ?
F9 C31 C32 C27 178.1(16) . . . . ?
C30 C31 C32 C27 0.0 . . . . ?
C28 C27 C32 F10 178.2(16) . . . . ?
C11 C27 C32 F10 -2.1(17) . . . . ?
C28 C27 C32 C31 0.0 . . . . ?
C11 C27 C32 C31 179.7(13) . . . . ?
C17 C16 C33 C34 -96(2) . . . . ?
C15 C16 C33 C34 87(2) . . . . ?
C17 C16 C33 C38 82(2) . . . . ?
C15 C16 C33 C38 -96(2) . . . . ?
C38 C33 C34 F11 179.8(16) . . . . ?
C16 C33 C34 F11 -2.5(17) . . . . ?
C38 C33 C34 C35 0.0 . . . . ?
C16 C33 C34 C35 177.7(14) . . . . ?
F11 C34 C35 F12 -0.6(18) . . . . ?
C33 C34 C35 F12 179.2(16) . . . . ?
F11 C34 C35 C36 -179.8(16) . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
F12 C35 C36 F13 0.3(17) . . . . ?
C34 C35 C36 F13 179.5(15) . . . . ?
F12 C35 C36 C37 -179.2(17) . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
F13 C36 C37 F14 -2.6(16) . . . . ?
C35 C36 C37 F14 176.9(15) . . . . ?
F13 C36 C37 C38 -179.5(15) . . . . ?
C35 C36 C37 C38 0.0 . . . . ?
F14 C37 C38 F15 3.2(16) . . . . ?
C36 C37 C38 F15 -179.9(14) . . . . ?
F14 C37 C38 C33 -176.9(15) . . . . ?
C36 C37 C38 C33 0.0 . . . . ?
C34 C33 C38 F15 179.9(14) . . . . ?
C16 C33 C38 F15 2.1(15) . . . . ?
C34 C33 C38 C37 0.0 . . . . ?
C16 C33 C38 C37 -177.8(14) . . . . ?
N5 C39 C40 C41 -170(2) . . . . ?
C39 C40 C41 C42 -167(3) . . . . ?
N5 C43 C44 C45 -152.4(18) . . . . ?
C43 C44 C45 C46 75(3) . . . . ?
N5 C47 C48 C49 -111(2) . . . . ?
C47 C48 C49 C50 -171(2) . . . . ?
N5 C51 C52 C53 176(2) . . . . ?
C51 C52 C53 C54 178(2) . . . . ?
C3 C2 N1 C5 5(2) . . . . ?
C1 C2 N1 C5 -174(2) . . . . ?
C3 C2 N1 PT1 -168.3(13) . . . . ?
C1 C2 N1 PT1 12(3) . . . . ?
C6 C5 N1 C2 173(2) . . . . ?
C4 C5 N1 C2 -4(2) . . . . ?
C6 C5 N1 PT1 -13(3) . . . . ?
C4 C5 N1 PT1 169.6(14) . . . . ?
C11 C10 N2 C7 179(2) . . . . ?
C9 C10 N2 C7 3(3) . . . . ?
C11 C10 N2 PT1 -2(4) . . . . ?
C9 C10 N2 PT1 -177.6(14) . . . . ?
C6 C7 N2 C10 170(2) . . . . ?
C8 C7 N2 C10 -5(2) . . . . ?
C6 C7 N2 PT1 -9(3) . . . . ?
C8 C7 N2 PT1 176.3(14) . . . . ?
C11 C12 N3 C15 179(2) . . . . ?
C13 C12 N3 C15 0(2) . . . . ?
C11 C12 N3 PT1 1(3) . . . . ?
C13 C12 N3 PT1 -176.9(14) . . . . ?
C16 C15 N3 C12 172(2) . . . . ?
C14 C15 N3 C12 0(3) . . . . ?
C16 C15 N3 PT1 -11(3) . . . . ?
C14 C15 N3 PT1 177.0(15) . . . . ?
C16 C17 N4 C20 -179(2) . . . . ?
C18 C17 N4 C20 -6(2) . . . . ?
C16 C17 N4 PT1 -4(3) . . . . ?
C18 C17 N4 PT1 169.1(13) . . . . ?
C19 C20 N4 C17 4(2) . . . . ?
C1 C20 N4 C17 -170(2) . . . . ?
C19 C20 N4 PT1 -171.1(14) . . . . ?
C1 C20 N4 PT1 15(3) . . . . ?
C52 C51 N5 C47 61(2) . . . . ?
C52 C51 N5 C39 -53(3) . . . . ?
C52 C51 N5 C43 -176.3(18) . . . . ?
C48 C47 N5 C51 61(2) . . . . ?
C48 C47 N5 C39 178.5(19) . . . . ?
C48 C47 N5 C43 -60(2) . . . . ?
C40 C39 N5 C51 -54(3) . . . . ?
C40 C39 N5 C47 -172(2) . . . . ?
C40 C39 N5 C43 67(3) . . . . ?
C44 C43 N5 C51 -170.3(17) . . . . ?
C44 C43 N5 C47 -49(2) . . . . ?
C44 C43 N5 C39 68(2) . . . . ?

_refine_diff_density_max         6.392
_refine_diff_density_min         -2.545
_refine_diff_density_rms         0.228



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_171217_ys_8-1
_database_code_depnum_ccdc_archive 'CCDC 1906677'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H42 F15 N7 O2'
_chemical_formula_weight         1250.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.389(2)
_cell_length_b                   13.345(4)
_cell_length_c                   26.551(8)
_cell_angle_alpha                103.059(4)
_cell_angle_beta                 93.168(4)
_cell_angle_gamma                93.947(4)
_cell_volume                     2537.6(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    20573
_cell_measurement_theta_min      1.732
_cell_measurement_theta_max      28.139

_exptl_crystal_description       rod
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_F_000             1276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.173
_shelx_estimated_absorpt_T_min   0.998
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.7829
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            20573
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.732
_diffrn_reflns_theta_max         28.139
_diffrn_reflns_theta_full        28.017
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             9086
_reflns_number_gt                5951
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0795P)²+1.9652P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9086
_refine_ls_number_parameters     820
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1752
_refine_ls_wR_factor_gt          0.1427
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4041(5) 0.1597(3) 0.19617(13) 0.0328(8) Uani 1 1 d . . . . .
C2 C 0.4777(5) 0.1789(2) 0.24846(13) 0.0301(7) Uani 1 1 d . . . . .
C3 C 0.5233(5) 0.1044(3) 0.27415(13) 0.0338(8) Uani 1 1 d . . . . .
H1 H 0.5193 0.0323 0.2597 0.041 Uiso 1 1 calc R U . . .
C4 C 0.5749(5) 0.1532(3) 0.32373(13) 0.0334(8) Uani 1 1 d . . . . .
H2 H 0.6133 0.1213 0.3506 0.040 Uiso 1 1 calc R U . . .
C5 C 0.5619(5) 0.2581(2) 0.32840(12) 0.0307(7) Uani 1 1 d . . . . .
C6 C 0.5980(5) 0.3356(2) 0.37344(12) 0.0290(7) Uani 1 1 d . . . . .
C7 C 0.6082(5) 0.4389(2) 0.37730(12) 0.0303(7) Uani 1 1 d . . . . .
C8 C 0.6510(5) 0.5161(3) 0.42356(13) 0.0326(8) Uani 1 1 d . . . . .
H3 H 0.6704 0.5049 0.4575 0.039 Uiso 1 1 calc R U . . .
C9 C 0.6591(5) 0.6063(3) 0.41093(13) 0.0319(8) Uani 1 1 d . . . . .
H4 H 0.6871 0.6719 0.4339 0.038 Uiso 1 1 calc R U . . .
C10 C 0.6183(5) 0.5870(2) 0.35667(12) 0.0294(7) Uani 1 1 d . . . . .
C11 C 0.6057(4) 0.6620(2) 0.32913(12) 0.0277(7) Uani 1 1 d . . . . .
C12 C 0.5486(5) 0.6456(2) 0.27771(12) 0.0297(7) Uani 1 1 d . . . . .
C13 C 0.5307(5) 0.7212(3) 0.24854(13) 0.0318(8) Uani 1 1 d . . . . .
H5 H 0.5564 0.7935 0.2612 0.038 Uiso 1 1 calc R U . . .
C14 C 0.4725(5) 0.6741(3) 0.20078(13) 0.0322(8) Uani 1 1 d . . . . .
H6 H 0.4502 0.7064 0.1729 0.039 Uiso 1 1 calc R U . . .
C15 C 0.4490(5) 0.5672(2) 0.19828(13) 0.0318(8) Uani 1 1 d . . . . .
C16 C 0.3835(5) 0.4929(3) 0.15614(12) 0.0315(8) Uani 1 1 d . . . . .
C17 C 0.3555(5) 0.3877(3) 0.15252(13) 0.0325(8) Uani 1 1 d . . . . .
C18 C 0.2869(5) 0.3134(3) 0.10841(13) 0.0369(8) Uani 1 1 d . . . . .
H7 H 0.2449 0.3260 0.0761 0.044 Uiso 1 1 calc R U . . .
C19 C 0.2915(5) 0.2214(3) 0.12021(13) 0.0365(8) Uani 1 1 d . . . . .
H8 H 0.2530 0.1562 0.0980 0.044 Uiso 1 1 calc R U . . .
C20 C 0.3634(5) 0.2395(2) 0.17126(12) 0.0314(8) Uani 1 1 d . . . . .
C21 C 0.6315(5) 0.3011(2) 0.42180(12) 0.0300(7) Uani 1 1 d . . . . .
C22 C 0.7965(5) 0.3148(3) 0.44857(13) 0.0346(8) Uani 1 1 d . . . . .
C23 C 0.8255(5) 0.2853(3) 0.49364(13) 0.0364(8) Uani 1 1 d . . . . .
C24 C 0.6863(5) 0.2404(3) 0.51321(13) 0.0362(8) Uani 1 1 d . . . . .
C25 C 0.5213(5) 0.2241(2) 0.48772(12) 0.0324(8) Uani 1 1 d . . . . .
C26 C 0.4947(5) 0.2561(2) 0.44347(13) 0.0309(8) Uani 1 1 d . . . . .
C27 C 0.6535(5) 0.7692(2) 0.35713(12) 0.0294(7) Uani 1 1 d . . . . .
C28 C 0.8258(5) 0.8039(2) 0.37601(13) 0.0320(8) Uani 1 1 d . . . . .
C29 C 0.8736(5) 0.9016(3) 0.40278(13) 0.0352(8) Uani 1 1 d . . . . .
C30 C 0.7453(5) 0.9689(2) 0.41137(14) 0.0362(8) Uani 1 1 d . . . . .
C31 C 0.5718(5) 0.9383(3) 0.39381(13) 0.0341(8) Uani 1 1 d . . . . .
C32 C 0.5285(5) 0.8407(3) 0.36642(13) 0.0316(8) Uani 1 1 d . . . . .
C33 C 0.3388(5) 0.5309(3) 0.10984(13) 0.0338(8) Uani 1 1 d . . . . .
C34 C 0.4702(5) 0.5608(3) 0.08109(14) 0.0387(9) Uani 1 1 d . . . . .
C35 C 0.4314(6) 0.5999(3) 0.03917(14) 0.0408(9) Uani 1 1 d . . . . .
C36 C 0.2577(6) 0.6088(3) 0.02504(13) 0.0423(9) Uani 1 1 d . . . . .
C37 C 0.1242(5) 0.5809(3) 0.05231(13) 0.0388(9) Uani 1 1 d . . . . .
C38 C 0.1659(5) 0.5426(3) 0.09418(13) 0.0371(8) Uani 1 1 d . . . . .
C39 C -0.0753(5) 0.0897(3) 0.18902(13) 0.0328(8) Uani 1 1 d . . . . .
C40 C -0.1005(5) -0.0007(3) 0.15057(13) 0.0338(8) Uani 1 1 d . . . . .
C41 C -0.1769(5) 0.0009(3) 0.10203(13) 0.0365(8) Uani 1 1 d . . . . .
C42 C -0.2036(5) -0.0890(3) 0.06443(14) 0.0431(9) Uani 1 1 d . . . . .
H9 H -0.2522 -0.0887 0.0306 0.052 Uiso 1 1 calc R U . . .
C43 C -0.1597(6) -0.1783(3) 0.07628(15) 0.0449(9) Uani 1 1 d . . . . .
H10 H -0.1816 -0.2405 0.0503 0.054 Uiso 1 1 calc R U . . .
C44 C -0.0858(5) -0.1830(3) 0.12374(14) 0.0395(9) Uani 1 1 d . . . . .
H11 H -0.0590 -0.2474 0.1308 0.047 Uiso 1 1 calc R U . . .
C45 C -0.0505(5) -0.0931(3) 0.16132(14) 0.0369(8) Uani 1 1 d . . . . .
C46 C -0.0047(5) 0.0869(3) 0.23786(13) 0.0310(8) Uani 1 1 d . . . . .
C47 C 0.0433(5) -0.0059(2) 0.24822(13) 0.0323(8) Uani 1 1 d . . . . .
C48 C 0.1014(5) -0.0079(3) 0.29784(13) 0.0374(8) Uani 1 1 d . . . . .
H12 H 0.1292 -0.0711 0.3061 0.045 Uiso 1 1 calc R U . . .
C49 C 0.1188(5) 0.0807(3) 0.33487(14) 0.0381(8) Uani 1 1 d . . . . .
H13 H 0.1608 0.0783 0.3690 0.046 Uiso 1 1 calc R U . . .
C50 C 0.0791(5) 0.1733(3) 0.32566(14) 0.0359(8) Uani 1 1 d . . . . .
H14 H 0.0963 0.2342 0.3526 0.043 Uiso 1 1 calc R U . . .
C51 C 0.0145(5) 0.1774(2) 0.27723(13) 0.0310(8) Uani 1 1 d . . . . .
C52 C -0.1194(5) 0.1812(3) 0.17829(13) 0.0327(8) Uani 1 1 d . . . . .
C53 C -0.0925(5) 0.2717(3) 0.21724(13) 0.0343(8) Uani 1 1 d . . . . .
C54 C -0.1292(5) 0.3632(3) 0.20563(14) 0.0387(9) Uani 1 1 d . . . . .
H15 H -0.1063 0.4262 0.2311 0.046 Uiso 1 1 calc R U . . .
C55 C -0.1988(5) 0.3627(3) 0.15714(14) 0.0392(9) Uani 1 1 d . . . . .
H16 H -0.2254 0.4265 0.1495 0.047 Uiso 1 1 calc R U . . .
C56 C -0.2322(5) 0.2752(3) 0.11917(14) 0.0388(9) Uani 1 1 d . . . . .
H17 H -0.2830 0.2779 0.0859 0.047 Uiso 1 1 calc R U . . .
C57 C -0.1920(5) 0.1840(3) 0.12944(13) 0.0348(8) Uani 1 1 d . . . . .
C58 C -0.3180(6) 0.0934(3) 0.04382(14) 0.0444(9) Uani 1 1 d . . . . .
H18 H -0.4028 0.1485 0.0491 0.053 Uiso 1 1 calc R U . . .
H19 H -0.3909 0.0267 0.0304 0.053 Uiso 1 1 calc R U . . .
C59 C -0.1909(6) 0.1109(3) 0.00459(14) 0.0464(10) Uani 1 1 d . . . . .
H20 H -0.1067 0.0555 -0.0012 0.056 Uiso 1 1 calc R U . . .
H21 H -0.1175 0.1775 0.0178 0.056 Uiso 1 1 calc R U . . .
C60 C -0.2918(6) 0.1121(3) -0.04587(15) 0.0508(10) Uani 1 1 d . . . . .
H30 H -0.3493 0.0429 -0.0617 0.076 Uiso 1 1 calc R U . . .
H31 H -0.2065 0.1332 -0.0693 0.076 Uiso 1 1 calc R U . . .
H32 H -0.3855 0.1611 -0.0396 0.076 Uiso 1 1 calc R U . . .
C61 C 0.1024(5) -0.1857(3) 0.21778(14) 0.0365(8) Uani 1 1 d . . . . .
H22 H 0.2087 -0.1669 0.2435 0.044 Uiso 1 1 calc R U . . .
H23 H 0.1444 -0.2257 0.1850 0.044 Uiso 1 1 calc R U . . .
C62 C -0.0362(5) -0.2509(3) 0.23714(14) 0.0392(9) Uani 1 1 d . . . . .
H24 H -0.1394 -0.2727 0.2106 0.047 Uiso 1 1 calc R U . . .
H25 H -0.0833 -0.2094 0.2688 0.047 Uiso 1 1 calc R U . . .
C63 C 0.0386(5) -0.3443(3) 0.24936(15) 0.0403(9) Uani 1 1 d . . . . .
H33 H 0.0828 -0.3864 0.2180 0.060 Uiso 1 1 calc R U . . .
H34 H -0.0571 -0.3847 0.2620 0.060 Uiso 1 1 calc R U . . .
H35 H 0.1394 -0.3231 0.2761 0.060 Uiso 1 1 calc R U . . .
C64 C -0.0320(5) 0.3582(3) 0.30733(14) 0.0358(8) Uani 1 1 d . . . . .
H26 H -0.0575 0.3372 0.3399 0.043 Uiso 1 1 calc R U . . .
H27 H -0.1310 0.3998 0.2993 0.043 Uiso 1 1 calc R U . . .
C65 C 0.1434(5) 0.4238(3) 0.31572(14) 0.0392(9) Uani 1 1 d . . . . .
H28 H 0.1693 0.4464 0.2836 0.047 Uiso 1 1 calc R U . . .
H29 H 0.2434 0.3832 0.3240 0.047 Uiso 1 1 calc R U . . .
C66 C 0.1339(5) 0.5166(3) 0.35934(15) 0.0442(9) Uani 1 1 d . . . . .
H36 H 0.0293 0.5538 0.3522 0.066 Uiso 1 1 calc R U . . .
H37 H 0.2459 0.5621 0.3625 0.066 Uiso 1 1 calc R U . . .
H38 H 0.1204 0.4943 0.3918 0.066 Uiso 1 1 calc R U . . .
N1 N 0.5045(4) 0.2716(2) 0.28161(10) 0.0294(6) Uani 1 1 d . . . . .
H41 H 0.4875 0.3313 0.2740 0.035 Uiso 1 1 calc R U . . .
N2 N 0.5882(4) 0.4853(2) 0.33690(10) 0.0301(6) Uani 1 1 d . . . . .
N3 N 0.4992(4) 0.5530(2) 0.24593(10) 0.0309(6) Uani 1 1 d . . . . .
H40 H 0.4994 0.4931 0.2546 0.037 Uiso 1 1 calc R U . . .
N4 N 0.3994(4) 0.3411(2) 0.19118(10) 0.0318(6) Uani 1 1 d . . . . .
N5 N -0.2257(4) 0.0924(2) 0.09304(11) 0.0395(7) Uani 1 1 d . . . . .
N6 N 0.0295(4) -0.0918(2) 0.20874(11) 0.0358(7) Uani 1 1 d . . . . .
N7 N -0.0332(4) 0.2664(2) 0.26579(11) 0.0345(7) Uani 1 1 d . . . . .
O1 O 0.3736(4) 0.06915(18) 0.17091(9) 0.0434(6) Uani 1 1 d . . . . .
F1 F 0.9393(3) 0.35743(16) 0.43049(8) 0.0411(5) Uani 1 1 d . . . . .
F2 F 0.9896(3) 0.29900(18) 0.51765(8) 0.0502(6) Uani 1 1 d . . . . .
F3 F 0.7131(3) 0.20946(17) 0.55643(8) 0.0480(6) Uani 1 1 d . . . . .
F4 F 0.3850(3) 0.17762(15) 0.50634(7) 0.0404(5) Uani 1 1 d . . . . .
F5 F 0.3284(3) 0.24350(15) 0.42117(7) 0.0386(5) Uani 1 1 d . . . . .
F6 F 0.9578(3) 0.74040(14) 0.36802(7) 0.0357(5) Uani 1 1 d . . . . .
F7 F 1.0445(3) 0.93210(15) 0.42000(8) 0.0429(5) Uani 1 1 d . . . . .
F8 F 0.7901(3) 1.06445(14) 0.43759(8) 0.0477(6) Uani 1 1 d . . . . .
F9 F 0.4444(3) 1.00385(14) 0.40327(8) 0.0413(5) Uani 1 1 d . . . . .
F10 F 0.3564(3) 0.81390(14) 0.34903(7) 0.0358(5) Uani 1 1 d . . . . .
F11 F 0.6431(3) 0.55187(17) 0.09335(8) 0.0482(6) Uani 1 1 d . . . . .
F12 F 0.5629(3) 0.62826(17) 0.01224(8) 0.0521(6) Uani 1 1 d . . . . .
F13 F 0.2158(4) 0.64368(17) -0.01669(8) 0.0544(6) Uani 1 1 d . . . . .
F14 F -0.0477(3) 0.59018(16) 0.03864(8) 0.0483(6) Uani 1 1 d . . . . .
F15 F 0.0306(3) 0.51812(17) 0.12066(8) 0.0451(5) Uani 1 1 d . . . . .
O2 O 0.4732(4) -0.1192(2) 0.16865(12) 0.0552(8) Uani 1 1 d . . . . .
H2A H 0.446(7) -0.043(4) 0.1729(19) 0.083 Uiso 1 1 d . U . . .
H2B H 0.565(7) -0.118(4) 0.153(2) 0.083 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.241(4) . ?
C1 C20 1.415(5) . ?
C1 C2 1.423(5) . ?
C2 N1 1.341(4) . ?
C2 C3 1.377(4) . ?
C3 C4 1.351(5) . ?
C3 H1 0.9500 . ?
C4 C5 1.388(5) . ?
C4 H2 0.9500 . ?
C5 N1 1.345(4) . ?
C5 C6 1.392(5) . ?
C6 C7 1.356(5) . ?
C6 C21 1.473(4) . ?
C7 N2 1.360(4) . ?
C7 C8 1.418(5) . ?
C8 C9 1.319(5) . ?
C8 H3 0.9500 . ?
C9 C10 1.416(5) . ?
C9 H4 0.9500 . ?
C10 N2 1.337(4) . ?
C10 C11 1.373(4) . ?
C11 C12 1.370(4) . ?
C11 C27 1.465(4) . ?
C12 N3 1.344(4) . ?
C12 C13 1.412(4) . ?
C13 C14 1.315(5) . ?
C13 H5 0.9500 . ?
C14 C15 1.412(5) . ?
C14 H6 0.9500 . ?
C15 N3 1.357(4) . ?
C15 C16 1.358(5) . ?
C16 C17 1.384(5) . ?
C16 C33 1.462(4) . ?
C17 N4 1.351(4) . ?
C17 C18 1.397(5) . ?
C18 C19 1.336(5) . ?
C18 H7 0.9500 . ?
C19 C20 1.390(5) . ?
C19 H8 0.9500 . ?
C20 N4 1.342(4) . ?
C21 C22 1.357(5) . ?
C21 C26 1.360(5) . ?
C22 F1 1.328(4) . ?
C22 C23 1.352(5) . ?
C23 F2 1.320(4) . ?
C23 C24 1.342(5) . ?
C24 F3 1.314(4) . ?
C24 C25 1.341(5) . ?
C25 F4 1.323(4) . ?
C25 C26 1.347(5) . ?
C26 F5 1.317(4) . ?
C27 C28 1.352(5) . ?
C27 C32 1.366(5) . ?
C28 F6 1.330(4) . ?
C28 C29 1.350(5) . ?
C29 F7 1.323(4) . ?
C29 C30 1.343(5) . ?
C30 F8 1.318(4) . ?
C30 C31 1.343(5) . ?
C31 F9 1.325(4) . ?
C31 C32 1.348(5) . ?
C32 F10 1.325(4) . ?
C33 C38 1.352(5) . ?
C33 C34 1.360(5) . ?
C34 F11 1.321(4) . ?
C34 C35 1.357(5) . ?
C35 F12 1.322(4) . ?
C35 C36 1.338(6) . ?
C36 F13 1.325(4) . ?
C36 C37 1.336(5) . ?
C37 F14 1.323(4) . ?
C37 C38 1.354(5) . ?
C38 F15 1.318(4) . ?
C39 C52 1.371(5) . ?
C39 C46 1.380(5) . ?
C39 C40 1.387(5) . ?
C40 C41 1.383(5) . ?
C40 C45 1.396(5) . ?
C41 N5 1.364(4) . ?
C41 C42 1.371(5) . ?
C42 C43 1.355(5) . ?
C42 H9 0.9500 . ?
C43 C44 1.362(5) . ?
C43 H10 0.9500 . ?
C44 C45 1.375(5) . ?
C44 H11 0.9500 . ?
C45 N6 1.357(4) . ?
C46 C47 1.392(4) . ?
C46 C51 1.400(5) . ?
C47 N6 1.361(4) . ?
C47 C48 1.370(5) . ?
C48 C49 1.350(5) . ?
C48 H12 0.9500 . ?
C49 C50 1.361(5) . ?
C49 H13 0.9500 . ?
C50 C51 1.361(5) . ?
C50 H14 0.9500 . ?
C51 N7 1.355(4) . ?
C52 C57 1.385(5) . ?
C52 C53 1.396(5) . ?
C53 N7 1.357(4) . ?
C53 C54 1.366(5) . ?
C54 C55 1.358(5) . ?
C54 H15 0.9500 . ?
C55 C56 1.357(5) . ?
C55 H16 0.9500 . ?
C56 C57 1.355(5) . ?
C56 H17 0.9500 . ?
C57 N5 1.375(5) . ?
C58 N5 1.444(4) . ?
C58 C59 1.486(5) . ?
C58 H18 0.9900 . ?
C58 H19 0.9900 . ?
C59 C60 1.501(5) . ?
C59 H20 0.9900 . ?
C59 H21 0.9900 . ?
C60 H30 0.9800 . ?
C60 H31 0.9800 . ?
C60 H32 0.9800 . ?
C61 N6 1.461(4) . ?
C61 C62 1.486(5) . ?
C61 H22 0.9900 . ?
C61 H23 0.9900 . ?
C62 C63 1.491(5) . ?
C62 H24 0.9900 . ?
C62 H25 0.9900 . ?
C63 H33 0.9800 . ?
C63 H34 0.9800 . ?
C63 H35 0.9800 . ?
C64 N7 1.451(4) . ?
C64 C65 1.489(5) . ?
C64 H26 0.9900 . ?
C64 H27 0.9900 . ?
C65 C66 1.500(5) . ?
C65 H28 0.9900 . ?
C65 H29 0.9900 . ?
C66 H36 0.9800 . ?
C66 H37 0.9800 . ?
C66 H38 0.9800 . ?
N1 H41 0.8800 . ?
N3 H40 0.8800 . ?
O2 H2A 1.03(5) . ?
O2 H2B 0.82(5) . ?

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
O1 C1 C20 117.9(3) . . ?
O1 C1 C2 119.1(3) . . ?
C20 C1 C2 123.0(3) . . ?
N1 C2 C3 108.8(3) . . ?
N1 C2 C1 125.8(3) . . ?
C3 C2 C1 125.3(3) . . ?
C4 C3 C2 107.1(3) . . ?
C4 C3 H1 126.5 . . ?
C2 C3 H1 126.5 . . ?
C3 C4 C5 107.9(3) . . ?
C3 C4 H2 126.1 . . ?
C5 C4 H2 126.1 . . ?
N1 C5 C4 107.6(3) . . ?
N1 C5 C6 125.9(3) . . ?
C4 C5 C6 126.5(3) . . ?
C7 C6 C5 127.0(3) . . ?
C7 C6 C21 116.9(3) . . ?
C5 C6 C21 116.2(3) . . ?
C6 C7 N2 125.4(3) . . ?
C6 C7 C8 125.7(3) . . ?
N2 C7 C8 108.9(3) . . ?
C9 C8 C7 107.5(3) . . ?
C9 C8 H3 126.3 . . ?
C7 C8 H3 126.3 . . ?
C8 C9 C10 107.2(3) . . ?
C8 C9 H4 126.4 . . ?
C10 C9 H4 126.4 . . ?
N2 C10 C11 125.5(3) . . ?
N2 C10 C9 109.8(3) . . ?
C11 C10 C9 124.7(3) . . ?
C12 C11 C10 125.6(3) . . ?
C12 C11 C27 116.9(3) . . ?
C10 C11 C27 117.5(3) . . ?
N3 C12 C11 125.3(3) . . ?
N3 C12 C13 107.7(3) . . ?
C11 C12 C13 127.0(3) . . ?
C14 C13 C12 108.2(3) . . ?
C14 C13 H5 125.9 . . ?
C12 C13 H5 125.9 . . ?
C13 C14 C15 108.0(3) . . ?
C13 C14 H6 126.0 . . ?
C15 C14 H6 126.0 . . ?
N3 C15 C16 126.5(3) . . ?
N3 C15 C14 107.5(3) . . ?
C16 C15 C14 126.0(3) . . ?
C15 C16 C17 127.6(3) . . ?
C15 C16 C33 114.6(3) . . ?
C17 C16 C33 117.8(3) . . ?
N4 C17 C16 124.3(3) . . ?
N4 C17 C18 109.6(3) . . ?
C16 C17 C18 126.0(3) . . ?
C19 C18 C17 107.1(3) . . ?
C19 C18 H7 126.4 . . ?
C17 C18 H7 126.4 . . ?
C18 C19 C20 106.8(3) . . ?
C18 C19 H8 126.6 . . ?
C20 C19 H8 126.6 . . ?
N4 C20 C19 110.4(3) . . ?
N4 C20 C1 126.0(3) . . ?
C19 C20 C1 123.4(3) . . ?
C22 C21 C26 115.6(3) . . ?
C22 C21 C6 123.1(3) . . ?
C26 C21 C6 121.3(3) . . ?
F1 C22 C23 116.9(3) . . ?
F1 C22 C21 120.2(3) . . ?
C23 C22 C21 122.8(3) . . ?
F2 C23 C24 120.4(3) . . ?
F2 C23 C22 120.3(3) . . ?
C24 C23 C22 119.3(3) . . ?
F3 C24 C25 120.0(3) . . ?
F3 C24 C23 120.0(3) . . ?
C25 C24 C23 119.9(3) . . ?
F4 C25 C24 119.9(3) . . ?
F4 C25 C26 120.3(3) . . ?
C24 C25 C26 119.8(3) . . ?
F5 C26 C25 117.7(3) . . ?
F5 C26 C21 119.7(3) . . ?
C25 C26 C21 122.6(3) . . ?
C28 C27 C32 115.4(3) . . ?
C28 C27 C11 121.9(3) . . ?
C32 C27 C11 122.8(3) . . ?
F6 C28 C29 116.9(3) . . ?
F6 C28 C27 119.8(3) . . ?
C29 C28 C27 123.3(3) . . ?
F7 C29 C30 119.9(3) . . ?
F7 C29 C28 121.0(3) . . ?
C30 C29 C28 119.1(3) . . ?
F8 C30 C31 120.3(3) . . ?
F8 C30 C29 119.7(3) . . ?
C31 C30 C29 120.0(3) . . ?
F9 C31 C30 120.1(3) . . ?
F9 C31 C32 120.3(3) . . ?
C30 C31 C32 119.6(3) . . ?
F10 C32 C31 117.8(3) . . ?
F10 C32 C27 119.6(3) . . ?
C31 C32 C27 122.6(3) . . ?
C38 C33 C34 115.9(3) . . ?
C38 C33 C16 122.3(3) . . ?
C34 C33 C16 121.7(3) . . ?
F11 C34 C35 117.3(3) . . ?
F11 C34 C33 120.2(3) . . ?
C35 C34 C33 122.5(4) . . ?
F12 C35 C36 120.1(3) . . ?
F12 C35 C34 120.7(4) . . ?
C36 C35 C34 119.2(4) . . ?
F13 C36 C37 119.2(4) . . ?
F13 C36 C35 120.3(4) . . ?
C37 C36 C35 120.4(3) . . ?
F14 C37 C36 120.6(3) . . ?
F14 C37 C38 119.9(4) . . ?
C36 C37 C38 119.4(4) . . ?
F15 C38 C33 119.9(3) . . ?
F15 C38 C37 117.5(3) . . ?
C33 C38 C37 122.6(4) . . ?
C52 C39 C46 120.4(3) . . ?
C52 C39 C40 120.0(3) . . ?
C46 C39 C40 119.6(3) . . ?
C41 C40 C39 119.9(3) . . ?
C41 C40 C45 120.4(3) . . ?
C39 C40 C45 119.7(3) . . ?
N5 C41 C42 121.6(3) . . ?
N5 C41 C40 118.8(3) . . ?
C42 C41 C40 119.6(3) . . ?
C43 C42 C41 119.0(3) . . ?
C43 C42 H9 120.5 . . ?
C41 C42 H9 120.5 . . ?
C42 C43 C44 123.1(4) . . ?
C42 C43 H10 118.5 . . ?
C44 C43 H10 118.5 . . ?
C43 C44 C45 118.9(3) . . ?
C43 C44 H11 120.6 . . ?
C45 C44 H11 120.6 . . ?
N6 C45 C44 121.9(3) . . ?
N6 C45 C40 119.1(3) . . ?
C44 C45 C40 119.0(3) . . ?
C39 C46 C47 120.1(3) . . ?
C39 C46 C51 119.7(3) . . ?
C47 C46 C51 120.2(3) . . ?
N6 C47 C48 122.2(3) . . ?
N6 C47 C46 118.8(3) . . ?
C48 C47 C46 119.0(3) . . ?
C49 C48 C47 119.3(3) . . ?
C49 C48 H12 120.3 . . ?
C47 C48 H12 120.3 . . ?
C48 C49 C50 123.2(3) . . ?
C48 C49 H13 118.4 . . ?
C50 C49 H13 118.4 . . ?
C51 C50 C49 119.0(3) . . ?
C51 C50 H14 120.5 . . ?
C49 C50 H14 120.5 . . ?
N7 C51 C50 122.1(3) . . ?
N7 C51 C46 118.6(3) . . ?
C50 C51 C46 119.3(3) . . ?
C39 C52 C57 120.5(3) . . ?
C39 C52 C53 119.4(3) . . ?
C57 C52 C53 120.0(3) . . ?
N7 C53 C54 121.7(3) . . ?
N7 C53 C52 119.2(3) . . ?
C54 C53 C52 119.1(3) . . ?
C55 C54 C53 118.9(3) . . ?
C55 C54 H15 120.5 . . ?
C53 C54 H15 120.5 . . ?
C56 C55 C54 123.0(3) . . ?
C56 C55 H16 118.5 . . ?
C54 C55 H16 118.5 . . ?
C57 C56 C55 119.0(3) . . ?
C57 C56 H17 120.5 . . ?
C55 C56 H17 120.5 . . ?
C56 C57 N5 121.9(3) . . ?
C56 C57 C52 119.9(3) . . ?
N5 C57 C52 118.2(3) . . ?
N5 C58 C59 112.9(3) . . ?
N5 C58 H18 109.0 . . ?
C59 C58 H18 109.0 . . ?
N5 C58 H19 109.0 . . ?
C59 C58 H19 109.0 . . ?
H18 C58 H19 107.8 . . ?
C58 C59 C60 111.3(4) . . ?
C58 C59 H20 109.4 . . ?
C60 C59 H20 109.4 . . ?
C58 C59 H21 109.4 . . ?
C60 C59 H21 109.4 . . ?
H20 C59 H21 108.0 . . ?
C59 C60 H30 109.5 . . ?
C59 C60 H31 109.5 . . ?
H30 C60 H31 109.5 . . ?
C59 C60 H32 109.5 . . ?
H30 C60 H32 109.5 . . ?
H31 C60 H32 109.5 . . ?
N6 C61 C62 111.5(3) . . ?
N6 C61 H22 109.3 . . ?
C62 C61 H22 109.3 . . ?
N6 C61 H23 109.3 . . ?
C62 C61 H23 109.3 . . ?
H22 C61 H23 108.0 . . ?
C61 C62 C63 112.3(3) . . ?
C61 C62 H24 109.1 . . ?
C63 C62 H24 109.1 . . ?
C61 C62 H25 109.1 . . ?
C63 C62 H25 109.1 . . ?
H24 C62 H25 107.9 . . ?
C62 C63 H33 109.5 . . ?
C62 C63 H34 109.5 . . ?
H33 C63 H34 109.5 . . ?
C62 C63 H35 109.5 . . ?
H33 C63 H35 109.5 . . ?
H34 C63 H35 109.5 . . ?
N7 C64 C65 113.5(3) . . ?
N7 C64 H26 108.9 . . ?
C65 C64 H26 108.9 . . ?
N7 C64 H27 108.9 . . ?
C65 C64 H27 108.9 . . ?
H26 C64 H27 107.7 . . ?
C64 C65 C66 110.2(3) . . ?
C64 C65 H28 109.6 . . ?
C66 C65 H28 109.6 . . ?
C64 C65 H29 109.6 . . ?
C66 C65 H29 109.6 . . ?
H28 C65 H29 108.1 . . ?
C65 C66 H36 109.5 . . ?
C65 C66 H37 109.5 . . ?
H36 C66 H37 109.5 . . ?
C65 C66 H38 109.5 . . ?
H36 C66 H38 109.5 . . ?
H37 C66 H38 109.5 . . ?
C2 N1 C5 108.6(3) . . ?
C2 N1 H41 125.7 . . ?
C5 N1 H41 125.7 . . ?
C10 N2 C7 106.6(3) . . ?
C12 N3 C15 108.6(3) . . ?
C12 N3 H40 125.7 . . ?
C15 N3 H40 125.7 . . ?
C20 N4 C17 105.9(3) . . ?
C41 N5 C57 122.4(3) . . ?
C41 N5 C58 119.1(3) . . ?
C57 N5 C58 118.5(3) . . ?
C45 N6 C47 122.1(3) . . ?
C45 N6 C61 118.9(3) . . ?
C47 N6 C61 118.9(3) . . ?
C51 N7 C53 122.5(3) . . ?
C51 N7 C64 119.1(3) . . ?
C53 N7 C64 118.3(3) . . ?
H2A O2 H2B 99(4) . . ?

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
O1 C1 C2 N1 -174.6(3) . . . . ?
C20 C1 C2 N1 5.4(6) . . . . ?
O1 C1 C2 C3 1.6(6) . . . . ?
C20 C1 C2 C3 -178.5(3) . . . . ?
N1 C2 C3 C4 1.2(4) . . . . ?
C1 C2 C3 C4 -175.5(3) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C3 C4 C5 N1 -0.6(4) . . . . ?
C3 C4 C5 C6 178.2(3) . . . . ?
N1 C5 C6 C7 -10.4(6) . . . . ?
C4 C5 C6 C7 171.0(4) . . . . ?
N1 C5 C6 C21 170.7(3) . . . . ?
C4 C5 C6 C21 -7.9(5) . . . . ?
C5 C6 C7 N2 -1.4(6) . . . . ?
C21 C6 C7 N2 177.5(3) . . . . ?
C5 C6 C7 C8 -177.8(3) . . . . ?
C21 C6 C7 C8 1.1(5) . . . . ?
C6 C7 C8 C9 176.0(3) . . . . ?
N2 C7 C8 C9 -0.9(4) . . . . ?
C7 C8 C9 C10 1.0(4) . . . . ?
C8 C9 C10 N2 -0.7(4) . . . . ?
C8 C9 C10 C11 177.1(3) . . . . ?
N2 C10 C11 C12 4.6(6) . . . . ?
C9 C10 C11 C12 -173.0(3) . . . . ?
N2 C10 C11 C27 -176.8(3) . . . . ?
C9 C10 C11 C27 5.7(5) . . . . ?
C10 C11 C12 N3 -1.3(6) . . . . ?
C27 C11 C12 N3 -180.0(3) . . . . ?
C10 C11 C12 C13 178.7(3) . . . . ?
C27 C11 C12 C13 0.0(5) . . . . ?
N3 C12 C13 C14 -0.1(4) . . . . ?
C11 C12 C13 C14 179.9(3) . . . . ?
C12 C13 C14 C15 0.8(4) . . . . ?
C13 C14 C15 N3 -1.3(4) . . . . ?
C13 C14 C15 C16 177.1(4) . . . . ?
N3 C15 C16 C17 -0.6(6) . . . . ?
C14 C15 C16 C17 -178.7(4) . . . . ?
N3 C15 C16 C33 179.5(3) . . . . ?
C14 C15 C16 C33 1.3(5) . . . . ?
C15 C16 C17 N4 -3.6(6) . . . . ?
C33 C16 C17 N4 176.3(3) . . . . ?
C15 C16 C17 C18 179.7(4) . . . . ?
C33 C16 C17 C18 -0.3(6) . . . . ?
N4 C17 C18 C19 -0.8(4) . . . . ?
C16 C17 C18 C19 176.3(4) . . . . ?
C17 C18 C19 C20 -0.3(4) . . . . ?
C18 C19 C20 N4 1.2(4) . . . . ?
C18 C19 C20 C1 -174.3(3) . . . . ?
O1 C1 C20 N4 -174.9(3) . . . . ?
C2 C1 C20 N4 5.2(6) . . . . ?
O1 C1 C20 C19 0.0(5) . . . . ?
C2 C1 C20 C19 -180.0(3) . . . . ?
C7 C6 C21 C22 -67.9(5) . . . . ?
C5 C6 C21 C22 111.2(4) . . . . ?
C7 C6 C21 C26 109.7(4) . . . . ?
C5 C6 C21 C26 -71.2(4) . . . . ?
C26 C21 C22 F1 179.6(3) . . . . ?
C6 C21 C22 F1 -2.7(5) . . . . ?
C26 C21 C22 C23 0.5(5) . . . . ?
C6 C21 C22 C23 178.3(3) . . . . ?
F1 C22 C23 F2 -0.2(5) . . . . ?
C21 C22 C23 F2 178.9(3) . . . . ?
F1 C22 C23 C24 -179.0(3) . . . . ?
C21 C22 C23 C24 0.1(6) . . . . ?
F2 C23 C24 F3 -0.2(5) . . . . ?
C22 C23 C24 F3 178.7(3) . . . . ?
F2 C23 C24 C25 -178.1(3) . . . . ?
C22 C23 C24 C25 0.8(5) . . . . ?
F3 C24 C25 F4 0.5(5) . . . . ?
C23 C24 C25 F4 178.4(3) . . . . ?
F3 C24 C25 C26 179.9(3) . . . . ?
C23 C24 C25 C26 -2.2(5) . . . . ?
F4 C25 C26 F5 2.9(5) . . . . ?
C24 C25 C26 F5 -176.5(3) . . . . ?
F4 C25 C26 C21 -177.7(3) . . . . ?
C24 C25 C26 C21 2.9(5) . . . . ?
C22 C21 C26 F5 177.4(3) . . . . ?
C6 C21 C26 F5 -0.4(5) . . . . ?
C22 C21 C26 C25 -2.0(5) . . . . ?
C6 C21 C26 C25 -179.8(3) . . . . ?
C12 C11 C27 C28 -114.1(4) . . . . ?
C10 C11 C27 C28 67.2(4) . . . . ?
C12 C11 C27 C32 66.5(4) . . . . ?
C10 C11 C27 C32 -112.2(4) . . . . ?
C32 C27 C28 F6 -178.7(3) . . . . ?
C11 C27 C28 F6 1.9(5) . . . . ?
C32 C27 C28 C29 0.7(5) . . . . ?
C11 C27 C28 C29 -178.8(3) . . . . ?
F6 C28 C29 F7 0.1(5) . . . . ?
C27 C28 C29 F7 -179.3(3) . . . . ?
F6 C28 C29 C30 179.3(3) . . . . ?
C27 C28 C29 C30 -0.1(5) . . . . ?
F7 C29 C30 F8 -1.0(5) . . . . ?
C28 C29 C30 F8 179.8(3) . . . . ?
F7 C29 C30 C31 179.8(3) . . . . ?
C28 C29 C30 C31 0.6(5) . . . . ?
F8 C30 C31 F9 -0.7(5) . . . . ?
C29 C30 C31 F9 178.4(3) . . . . ?
F8 C30 C31 C32 179.1(3) . . . . ?
C29 C30 C31 C32 -1.7(5) . . . . ?
F9 C31 C32 F10 0.9(5) . . . . ?
C30 C31 C32 F10 -178.9(3) . . . . ?
F9 C31 C32 C27 -177.7(3) . . . . ?
C30 C31 C32 C27 2.5(5) . . . . ?
C28 C27 C32 F10 179.5(3) . . . . ?
C11 C27 C32 F10 -1.0(5) . . . . ?
C28 C27 C32 C31 -1.9(5) . . . . ?
C11 C27 C32 C31 177.5(3) . . . . ?
C15 C16 C33 C38 -102.0(4) . . . . ?
C17 C16 C33 C38 78.0(5) . . . . ?
C15 C16 C33 C34 75.1(4) . . . . ?
C17 C16 C33 C34 -104.9(4) . . . . ?
C38 C33 C34 F11 -179.8(3) . . . . ?
C16 C33 C34 F11 2.9(5) . . . . ?
C38 C33 C34 C35 -0.1(5) . . . . ?
C16 C33 C34 C35 -177.4(3) . . . . ?
F11 C34 C35 F12 -0.4(5) . . . . ?
C33 C34 C35 F12 179.9(3) . . . . ?
F11 C34 C35 C36 179.1(3) . . . . ?
C33 C34 C35 C36 -0.6(6) . . . . ?
F12 C35 C36 F13 1.6(5) . . . . ?
C34 C35 C36 F13 -177.9(3) . . . . ?
F12 C35 C36 C37 -179.5(3) . . . . ?
C34 C35 C36 C37 1.0(6) . . . . ?
F13 C36 C37 F14 -1.5(5) . . . . ?
C35 C36 C37 F14 179.6(3) . . . . ?
F13 C36 C37 C38 178.2(3) . . . . ?
C35 C36 C37 C38 -0.7(6) . . . . ?
C34 C33 C38 F15 -178.2(3) . . . . ?
C16 C33 C38 F15 -0.9(5) . . . . ?
C34 C33 C38 C37 0.5(5) . . . . ?
C16 C33 C38 C37 177.8(3) . . . . ?
F14 C37 C38 F15 -1.7(5) . . . . ?
C36 C37 C38 F15 178.6(3) . . . . ?
F14 C37 C38 C33 179.7(3) . . . . ?
C36 C37 C38 C33 -0.1(6) . . . . ?
C52 C39 C40 C41 -2.5(5) . . . . ?
C46 C39 C40 C41 177.8(3) . . . . ?
C52 C39 C40 C45 178.2(3) . . . . ?
C46 C39 C40 C45 -1.5(5) . . . . ?
C39 C40 C41 N5 0.1(5) . . . . ?
C45 C40 C41 N5 179.4(3) . . . . ?
C39 C40 C41 C42 -179.1(3) . . . . ?
C45 C40 C41 C42 0.1(6) . . . . ?
N5 C41 C42 C43 -177.2(4) . . . . ?
C40 C41 C42 C43 2.1(6) . . . . ?
C41 C42 C43 C44 -1.6(6) . . . . ?
C42 C43 C44 C45 -1.2(6) . . . . ?
C43 C44 C45 N6 -177.4(4) . . . . ?
C43 C44 C45 C40 3.4(6) . . . . ?
C41 C40 C45 N6 177.9(3) . . . . ?
C39 C40 C45 N6 -2.8(5) . . . . ?
C41 C40 C45 C44 -2.9(6) . . . . ?
C39 C40 C45 C44 176.4(3) . . . . ?
C52 C39 C46 C47 -178.7(3) . . . . ?
C40 C39 C46 C47 1.0(5) . . . . ?
C52 C39 C46 C51 2.7(5) . . . . ?
C40 C39 C46 C51 -177.6(3) . . . . ?
C39 C46 C47 N6 3.8(5) . . . . ?
C51 C46 C47 N6 -177.6(3) . . . . ?
C39 C46 C47 C48 -175.6(3) . . . . ?
C51 C46 C47 C48 2.9(5) . . . . ?
N6 C47 C48 C49 177.5(3) . . . . ?
C46 C47 C48 C49 -3.1(5) . . . . ?
C47 C48 C49 C50 0.8(6) . . . . ?
C48 C49 C50 C51 1.6(6) . . . . ?
C49 C50 C51 N7 177.9(3) . . . . ?
C49 C50 C51 C46 -1.8(5) . . . . ?
C39 C46 C51 N7 -1.6(5) . . . . ?
C47 C46 C51 N7 179.9(3) . . . . ?
C39 C46 C51 C50 178.1(3) . . . . ?
C47 C46 C51 C50 -0.5(5) . . . . ?
C46 C39 C52 C57 -179.4(3) . . . . ?
C40 C39 C52 C57 1.0(5) . . . . ?
C46 C39 C52 C53 0.0(5) . . . . ?
C40 C39 C52 C53 -179.7(3) . . . . ?
C39 C52 C53 N7 -3.8(5) . . . . ?
C57 C52 C53 N7 175.5(3) . . . . ?
C39 C52 C53 C54 177.1(3) . . . . ?
C57 C52 C53 C54 -3.6(5) . . . . ?
N7 C53 C54 C55 -176.0(3) . . . . ?
C52 C53 C54 C55 3.1(5) . . . . ?
C53 C54 C55 C56 -0.8(6) . . . . ?
C54 C55 C56 C57 -1.1(6) . . . . ?
C55 C56 C57 N5 178.7(3) . . . . ?
C55 C56 C57 C52 0.6(6) . . . . ?
C39 C52 C57 C56 -178.9(3) . . . . ?
C53 C52 C57 C56 1.7(5) . . . . ?
C39 C52 C57 N5 2.9(5) . . . . ?
C53 C52 C57 N5 -176.4(3) . . . . ?
N5 C58 C59 C60 -179.6(3) . . . . ?
N6 C61 C62 C63 -176.8(3) . . . . ?
N7 C64 C65 C66 -179.7(3) . . . . ?
C3 C2 N1 C5 -1.6(4) . . . . ?
C1 C2 N1 C5 175.1(3) . . . . ?
C4 C5 N1 C2 1.4(4) . . . . ?
C6 C5 N1 C2 -177.5(3) . . . . ?
C11 C10 N2 C7 -177.7(3) . . . . ?
C9 C10 N2 C7 0.1(4) . . . . ?
C6 C7 N2 C10 -176.5(3) . . . . ?
C8 C7 N2 C10 0.5(4) . . . . ?
C11 C12 N3 C15 179.3(3) . . . . ?
C13 C12 N3 C15 -0.8(4) . . . . ?
C16 C15 N3 C12 -177.2(3) . . . . ?
C14 C15 N3 C12 1.2(4) . . . . ?
C19 C20 N4 C17 -1.7(4) . . . . ?
C1 C20 N4 C17 173.7(3) . . . . ?
C16 C17 N4 C20 -175.6(3) . . . . ?
C18 C17 N4 C20 1.5(4) . . . . ?
C42 C41 N5 C57 -176.8(4) . . . . ?
C40 C41 N5 C57 3.9(5) . . . . ?
C42 C41 N5 C58 3.9(5) . . . . ?
C40 C41 N5 C58 -175.3(3) . . . . ?
C56 C57 N5 C41 176.4(3) . . . . ?
C52 C57 N5 C41 -5.4(5) . . . . ?
C56 C57 N5 C58 -4.3(5) . . . . ?
C52 C57 N5 C58 173.8(3) . . . . ?
C59 C58 N5 C41 -91.0(4) . . . . ?
C59 C58 N5 C57 89.7(4) . . . . ?
C44 C45 N6 C47 -171.3(3) . . . . ?
C40 C45 N6 C47 7.9(5) . . . . ?
C44 C45 N6 C61 8.5(5) . . . . ?
C40 C45 N6 C61 -172.3(3) . . . . ?
C48 C47 N6 C45 171.0(3) . . . . ?
C46 C47 N6 C45 -8.4(5) . . . . ?
C48 C47 N6 C61 -8.7(5) . . . . ?
C46 C47 N6 C61 171.8(3) . . . . ?
C62 C61 N6 C45 -90.2(4) . . . . ?
C62 C61 N6 C47 89.6(4) . . . . ?
C50 C51 N7 C53 177.9(3) . . . . ?
C46 C51 N7 C53 -2.4(5) . . . . ?
C50 C51 N7 C64 -6.0(5) . . . . ?
C46 C51 N7 C64 173.6(3) . . . . ?
C54 C53 N7 C51 -175.8(3) . . . . ?
C52 C53 N7 C51 5.1(5) . . . . ?
C54 C53 N7 C64 8.1(5) . . . . ?
C52 C53 N7 C64 -170.9(3) . . . . ?
C65 C64 N7 C51 92.3(4) . . . . ?
C65 C64 N7 C53 -91.5(4) . . . . ?

_refine_diff_density_max         0.264
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.071



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1906678'
loop_
_audit_author_name
_audit_author_address
'Nobuhiro Yasuda'
;Japan Synchrotron Radiation Research Institute
Japan
;
_audit_update_record             
;
2019-03-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C68 H41 F15 N8 Ni O'
_chemical_formula_sum            'C68 H41 F15 N8 Ni O'
_chemical_formula_weight         1329.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 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'
F F 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3232 1.3233 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4930(4)
_cell_length_b                   28.6109(13)
_cell_length_c                   22.8426(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.787(3)
_cell_angle_gamma                90
_cell_volume                     5511.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    29443
_cell_measurement_theta_min      1.260
_cell_measurement_theta_max      27.952

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_F_000             2704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.589
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.78192
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            29443
_diffrn_reflns_av_unetI/netI     0.1506
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.260
_diffrn_reflns_theta_max         27.952
_diffrn_reflns_theta_full        27.952
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             9787
_reflns_number_gt                5721
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1076P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9787
_refine_ls_number_parameters     840
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1726
_refine_ls_R_factor_gt           0.0956
_refine_ls_wR_factor_ref         0.2334
_refine_ls_wR_factor_gt          0.1942
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8902(7) 0.5939(2) 0.3626(3) 0.0278(15) Uani 1 1 d . . . . .
C2 C 0.8257(7) 0.6402(2) 0.3611(2) 0.0261(15) Uani 1 1 d . . . . .
C3 C 0.8392(8) 0.6688(2) 0.4118(3) 0.0352(17) Uani 1 1 d . . . . .
H1 H 0.8733 0.6593 0.4511 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7943(8) 0.7124(2) 0.3938(2) 0.0356(17) Uani 1 1 d . . . . .
H2 H 0.7937 0.7394 0.4180 0.043 Uiso 1 1 calc R U . . .
C5 C 0.7482(7) 0.7102(2) 0.3321(2) 0.0255(15) Uani 1 1 d . . . . .
C6 C 0.6905(7) 0.7469(2) 0.2964(2) 0.0261(15) Uani 1 1 d . . . . .
C7 C 0.6199(7) 0.74139(19) 0.2395(2) 0.0218(14) Uani 1 1 d . . . . .
C8 C 0.5215(8) 0.7755(2) 0.2069(2) 0.0301(16) Uani 1 1 d . . . . .
H3 H 0.5142 0.8076 0.2166 0.036 Uiso 1 1 calc R U . . .
C9 C 0.4414(7) 0.75391(19) 0.1603(2) 0.0233(14) Uani 1 1 d . . . . .
H4 H 0.3649 0.7675 0.1316 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4944(7) 0.70631(19) 0.1623(2) 0.0223(14) Uani 1 1 d . . . . .
C11 C 0.4427(7) 0.6726(2) 0.1199(2) 0.0242(14) Uani 1 1 d . . . . .
C12 C 0.5270(8) 0.6306(2) 0.1156(2) 0.0274(15) Uani 1 1 d . . . . .
C13 C 0.5052(8) 0.5997(2) 0.0662(2) 0.0271(15) Uani 1 1 d . . . . .
H5 H 0.4219 0.6008 0.0346 0.033 Uiso 1 1 calc R U . . .
C14 C 0.6246(7) 0.5692(2) 0.0730(2) 0.0288(16) Uani 1 1 d . . . . .
H6 H 0.6452 0.5454 0.0459 0.035 Uiso 1 1 calc R U . . .
C15 C 0.7160(8) 0.5787(2) 0.1284(2) 0.0256(15) Uani 1 1 d . . . . .
C16 C 0.8428(7) 0.5531(2) 0.1535(2) 0.0241(14) Uani 1 1 d . . . . .
C17 C 0.9042(7) 0.5562(2) 0.2134(2) 0.0272(15) Uani 1 1 d . . . . .
C18 C 1.0099(8) 0.5245(2) 0.2433(3) 0.0358(17) Uani 1 1 d . . . . .
H7 H 1.0686 0.5008 0.2263 0.043 Uiso 1 1 calc R U . . .
C19 C 1.0119(8) 0.5343(2) 0.3025(2) 0.0316(16) Uani 1 1 d . . . . .
H8 H 1.0701 0.5180 0.3342 0.038 Uiso 1 1 calc R U . . .
C20 C 0.9145(7) 0.5720(2) 0.3070(2) 0.0254(15) Uani 1 1 d . . . . .
C21 C 0.6847(7) 0.7951(2) 0.3224(2) 0.0250(15) Uani 1 1 d . . . . .
C22 C 0.7818(8) 0.8307(2) 0.3075(2) 0.0302(16) Uani 1 1 d . . . . .
C23 C 0.7681(8) 0.8760(2) 0.3268(2) 0.0284(16) Uani 1 1 d . . . . .
C24 C 0.6524(8) 0.8871(2) 0.3623(2) 0.0318(16) Uani 1 1 d . . . . .
C25 C 0.5558(8) 0.8525(2) 0.3788(3) 0.0302(16) Uani 1 1 d . . . . .
C26 C 0.5716(8) 0.8074(2) 0.3587(2) 0.0319(16) Uani 1 1 d . . . . .
C27 C 0.2998(7) 0.6812(2) 0.0774(2) 0.0254(15) Uani 1 1 d . . . . .
C28 C 0.3071(8) 0.6980(2) 0.0200(2) 0.0282(15) Uani 1 1 d . . . . .
C29 C 0.1754(8) 0.7017(2) -0.0205(2) 0.0299(16) Uani 1 1 d . . . . .
C30 C 0.0316(8) 0.6888(2) -0.0052(3) 0.0304(16) Uani 1 1 d . . . . .
C31 C 0.0159(8) 0.6736(2) 0.0512(2) 0.0256(15) Uani 1 1 d . . . . .
C32 C 0.1509(8) 0.6712(2) 0.0914(2) 0.0277(15) Uani 1 1 d . . . . .
C33 C 0.9112(7) 0.5164(2) 0.1178(2) 0.0239(14) Uani 1 1 d . . . . .
C34 C 1.0497(8) 0.5253(2) 0.0928(2) 0.0269(15) Uani 1 1 d . . . . .
C35 C 1.1211(7) 0.4914(2) 0.0605(2) 0.0281(15) Uani 1 1 d . . . . .
C36 C 1.0515(8) 0.4484(2) 0.0524(2) 0.0292(16) Uani 1 1 d . . . . .
C37 C 0.9135(8) 0.4384(2) 0.0759(3) 0.0328(16) Uani 1 1 d . . . . .
C38 C 0.8473(8) 0.4725(2) 0.1085(2) 0.0310(16) Uani 1 1 d . . . . .
C39 C 0.5489(8) 0.5537(2) 0.3922(2) 0.0322(16) Uani 1 1 d . . . . .
C40 C 0.4972(8) 0.5919(2) 0.4238(3) 0.0371(17) Uani 1 1 d . . . . .
C41 C 0.5499(10) 0.5956(3) 0.4860(3) 0.052(2) Uani 1 1 d . . . . .
C42 C 0.5003(10) 0.6350(2) 0.5154(3) 0.052(2) Uani 1 1 d . . . . .
H9 H 0.5350 0.6392 0.5562 0.062 Uiso 1 1 calc R U . . .
C43 C 0.4019(10) 0.6676(3) 0.4861(3) 0.054(2) Uani 1 1 d . . . . .
H10 H 0.3673 0.6933 0.5076 0.065 Uiso 1 1 calc R U . . .
C44 C 0.3520(9) 0.6646(3) 0.4272(3) 0.050(2) Uani 1 1 d . . . . .
H11 H 0.2842 0.6878 0.4083 0.060 Uiso 1 1 calc R U . . .
C45 C 0.4023(9) 0.6266(2) 0.3949(3) 0.0406(19) Uani 1 1 d . . . . .
C46 C 0.5001(8) 0.5497(2) 0.3312(2) 0.0319(16) Uani 1 1 d . . . . .
C47 C 0.4061(8) 0.5849(2) 0.3015(3) 0.0350(17) Uani 1 1 d . . . . .
C48 C 0.3626(8) 0.5818(2) 0.2405(2) 0.0343(17) Uani 1 1 d . . . . .
H12 H 0.2981 0.6051 0.2201 0.041 Uiso 1 1 calc R U . . .
C49 C 0.4154(8) 0.5441(2) 0.2107(3) 0.0323(16) Uani 1 1 d . . . . .
H13 H 0.3868 0.5421 0.1693 0.039 Uiso 1 1 calc R U . . .
C50 C 0.5082(8) 0.5089(2) 0.2385(3) 0.0324(16) Uani 1 1 d . . . . .
H14 H 0.5403 0.4832 0.2165 0.039 Uiso 1 1 calc R U . . .
C51 C 0.5539(7) 0.5118(2) 0.2989(2) 0.0276(15) Uani 1 1 d . . . . .
C52 C 0.6423(8) 0.5181(2) 0.4216(3) 0.0339(16) Uani 1 1 d . . . . .
C53 C 0.6956(8) 0.4803(2) 0.3896(3) 0.0324(16) Uani 1 1 d . . . . .
C54 C 0.7821(8) 0.4449(2) 0.4195(3) 0.0365(17) Uani 1 1 d . . . . .
H15 H 0.8107 0.4178 0.3990 0.044 Uiso 1 1 calc R U . . .
C55 C 0.8270(8) 0.4492(2) 0.4800(3) 0.0423(19) Uani 1 1 d . . . . .
H16 H 0.8890 0.4252 0.5000 0.051 Uiso 1 1 calc R U . . .
C56 C 0.7842(9) 0.4872(3) 0.5116(3) 0.049(2) Uani 1 1 d . . . . .
H17 H 0.8185 0.4895 0.5526 0.059 Uiso 1 1 calc R U . . .
C57 C 0.6902(9) 0.5222(3) 0.4830(3) 0.049(2) Uani 1 1 d . . . . .
C58A C 0.6512(14) 0.5599(4) 0.5802(5) 0.038(4) Uiso 0.633(19) 1 d . . P A 2
H58A H 0.5573 0.5747 0.5943 0.046 Uiso 0.633(19) 1 calc R U P A 2
H58B H 0.6609 0.5274 0.5951 0.046 Uiso 0.633(19) 1 calc R U P A 2
C59A C 0.7987(15) 0.5873(4) 0.5989(6) 0.048(4) Uiso 0.633(19) 1 d . . P A 2
H59A H 0.7952 0.6174 0.5775 0.057 Uiso 0.633(19) 1 calc R U P A 2
H59B H 0.8928 0.5697 0.5895 0.057 Uiso 0.633(19) 1 calc R U P A 2
C60A C 0.8111(17) 0.5964(5) 0.6666(5) 0.048(4) Uiso 0.633(19) 1 d . . P A 2
H60A H 0.7221 0.6160 0.6753 0.072 Uiso 0.633(19) 1 calc R U P A 2
H60B H 0.9112 0.6124 0.6796 0.072 Uiso 0.633(19) 1 calc R U P A 2
H60C H 0.8079 0.5666 0.6875 0.072 Uiso 0.633(19) 1 calc R U P A 2
C58B C 0.768(3) 0.5778(7) 0.5661(10) 0.045(7) Uiso 0.367(19) 1 d . . P A 3
H58C H 0.8699 0.5613 0.5655 0.054 Uiso 0.367(19) 1 calc R U P A 3
H58D H 0.7858 0.6120 0.5646 0.054 Uiso 0.367(19) 1 calc R U P A 3
C59B C 0.688(2) 0.5644(6) 0.6193(8) 0.030(6) Uiso 0.367(19) 1 d . . P A 3
H59C H 0.5791 0.5770 0.6141 0.036 Uiso 0.367(19) 1 calc R U P A 3
H59D H 0.6804 0.5299 0.6204 0.036 Uiso 0.367(19) 1 calc R U P A 3
C60B C 0.766(2) 0.5803(7) 0.6764(7) 0.025(5) Uiso 0.367(19) 1 d . . P A 3
H60D H 0.8721 0.5664 0.6837 0.038 Uiso 0.367(19) 1 calc R U P A 3
H60E H 0.7030 0.5707 0.7076 0.038 Uiso 0.367(19) 1 calc R U P A 3
H60F H 0.7753 0.6144 0.6763 0.038 Uiso 0.367(19) 1 calc R U P A 3
C61A C 0.2063(12) 0.6500(4) 0.3072(4) 0.026(3) Uiso 0.633(18) 1 d . . P B 4
H61A H 0.1449 0.6319 0.2753 0.031 Uiso 0.633(18) 1 calc R U P B 4
H61B H 0.1359 0.6571 0.3376 0.031 Uiso 0.633(18) 1 calc R U P B 4
C62A C 0.2632(13) 0.6941(4) 0.2831(4) 0.032(3) Uiso 0.633(18) 1 d . . P B 4
H62A H 0.3448 0.7084 0.3122 0.038 Uiso 0.633(18) 1 calc R U P B 4
H62B H 0.3120 0.6875 0.2467 0.038 Uiso 0.633(18) 1 calc R U P B 4
C63A C 0.1300(16) 0.7263(4) 0.2700(6) 0.027(4) Uiso 0.633(18) 1 d . . P B 4
H63A H 0.0405 0.7097 0.2482 0.041 Uiso 0.633(18) 1 calc R U P B 4
H63B H 0.1620 0.7523 0.2461 0.041 Uiso 0.633(18) 1 calc R U P B 4
H63C H 0.0982 0.7385 0.3069 0.041 Uiso 0.633(18) 1 calc R U P B 4
C61B C 0.332(3) 0.6701(7) 0.3011(9) 0.046(7) Uiso 0.367(18) 1 d . . P B 5
H61C H 0.3844 0.6955 0.3256 0.055 Uiso 0.367(18) 1 calc R U P B 5
H61D H 0.3774 0.6689 0.2631 0.055 Uiso 0.367(18) 1 calc R U P B 5
C62B C 0.154(3) 0.6762(8) 0.2919(8) 0.043(6) Uiso 0.367(18) 1 d . . P B 5
H62C H 0.1131 0.6768 0.3307 0.052 Uiso 0.367(18) 1 calc R U P B 5
H62D H 0.1057 0.6492 0.2694 0.052 Uiso 0.367(18) 1 calc R U P B 5
C63B C 0.103(3) 0.7252(8) 0.2556(12) 0.036(7) Uiso 0.367(18) 1 d . . P B 5
H63D H 0.1521 0.7520 0.2776 0.054 Uiso 0.367(18) 1 calc R U P B 5
H63E H -0.0125 0.7286 0.2514 0.054 Uiso 0.367(18) 1 calc R U P B 5
H63F H 0.1395 0.7241 0.2165 0.054 Uiso 0.367(18) 1 calc R U P B 5
C64 C 0.7368(8) 0.4446(2) 0.2939(3) 0.0330(16) Uani 1 1 d . . . . .
H26 H 0.8417 0.4377 0.3159 0.040 Uiso 1 1 calc R U . . .
H27 H 0.7556 0.4592 0.2560 0.040 Uiso 1 1 calc R U . . .
C65 C 0.6515(8) 0.3994(2) 0.2807(3) 0.0352(17) Uani 1 1 d . . . . .
H28 H 0.5462 0.4055 0.2585 0.042 Uiso 1 1 calc R U . . .
H29 H 0.6352 0.3835 0.3180 0.042 Uiso 1 1 calc R U . . .
C66 C 0.7491(9) 0.3680(2) 0.2443(3) 0.0462(19) Uani 1 1 d . . . . .
H48 H 0.7609 0.3833 0.2066 0.069 Uiso 1 1 calc R U . . .
H49 H 0.6947 0.3380 0.2368 0.069 Uiso 1 1 calc R U . . .
H50 H 0.8540 0.3627 0.2660 0.069 Uiso 1 1 calc R U . . .
C67 C -0.1670(11) 0.7699(3) 0.1139(4) 0.083(3) Uani 1 1 d . . . . .
H39 H -0.2358 0.7675 0.0765 0.125 Uiso 1 1 calc R U . . .
H40 H -0.2217 0.7876 0.1422 0.125 Uiso 1 1 calc R U . . .
H41 H -0.1416 0.7386 0.1295 0.125 Uiso 1 1 calc R U . . .
C68 C -0.0216(12) 0.7940(3) 0.1044(4) 0.061(2) Uani 1 1 d . . . . .
N1 N 0.7693(6) 0.66477(16) 0.31164(18) 0.0240(12) Uani 1 1 d . . . . .
N2 N 0.6051(6) 0.69847(16) 0.20982(19) 0.0247(12) Uani 1 1 d . . . . .
N3 N 0.6543(6) 0.61730(16) 0.15528(18) 0.0226(12) Uani 1 1 d . . . . .
N4 N 0.8451(6) 0.58727(16) 0.25267(19) 0.0243(12) Uani 1 1 d . . . . .
N5 N 0.6400(9) 0.5611(2) 0.5131(2) 0.071(2) Uani 1 1 d . . . . .
N6 N 0.3502(8) 0.6210(2) 0.3346(2) 0.0565(19) Uani 1 1 d . . . . .
N7 N 0.6544(6) 0.47921(17) 0.3284(2) 0.0294(13) Uani 1 1 d . . . . .
N8 N 0.0892(10) 0.8116(3) 0.0965(4) 0.097(3) Uani 1 1 d . . . . .
O1 O 0.9385(5) 0.57314(15) 0.41051(17) 0.0401(12) Uani 1 1 d . . . . .
F1 F 0.8955(4) 0.82125(12) 0.27232(14) 0.0368(9) Uani 1 1 d . . . . .
F2 F 0.8655(5) 0.90953(12) 0.31126(15) 0.0405(10) Uani 1 1 d . . . . .
F3 F 0.6325(4) 0.93119(12) 0.37899(14) 0.0384(10) Uani 1 1 d . . . . .
F4 F 0.4421(4) 0.86306(12) 0.41284(15) 0.0401(10) Uani 1 1 d . . . . .
F5 F 0.4702(4) 0.77477(12) 0.37441(15) 0.0404(10) Uani 1 1 d . . . . .
F6 F 0.4496(4) 0.71045(12) 0.00391(13) 0.0365(9) Uani 1 1 d . . . . .
F7 F 0.1862(4) 0.71696(12) -0.07558(13) 0.0408(10) Uani 1 1 d . . . . .
F8 F -0.0986(4) 0.68919(12) -0.04529(14) 0.0385(10) Uani 1 1 d . . . . .
F9 F -0.1260(4) 0.66138(12) 0.06647(14) 0.0376(9) Uani 1 1 d . . . . .
F10 F 0.1327(4) 0.65609(12) 0.14647(13) 0.0342(9) Uani 1 1 d . . . . .
F11 F 1.1201(4) 0.56693(12) 0.09920(13) 0.0320(9) Uani 1 1 d . . . . .
F12 F 1.2541(4) 0.50189(11) 0.03714(14) 0.0349(9) Uani 1 1 d . . . . .
F13 F 1.1178(4) 0.41582(11) 0.02058(14) 0.0340(9) Uani 1 1 d . . . . .
F14 F 0.8477(4) 0.39584(12) 0.06753(16) 0.0427(10) Uani 1 1 d . . . . .
F15 F 0.7125(4) 0.46073(12) 0.13092(15) 0.0396(9) Uani 1 1 d . . . . .
Ni1 Ni 0.71815(9) 0.64179(3) 0.23242(3) 0.0244(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.269(7) . ?
C1 C2 1.434(8) . ?
C1 C20 1.452(8) . ?
C2 N1 1.367(7) . ?
C2 C3 1.413(8) . ?
C3 C4 1.353(8) . ?
C3 H1 0.9500 . ?
C4 C5 1.419(7) . ?
C4 H2 0.9500 . ?
C5 C6 1.384(8) . ?
C5 N1 1.400(7) . ?
C6 C7 1.374(7) . ?
C6 C21 1.504(8) . ?
C7 N2 1.401(7) . ?
C7 C8 1.433(8) . ?
C8 C9 1.345(8) . ?
C8 H3 0.9500 . ?
C9 C10 1.433(7) . ?
C9 H4 0.9500 . ?
C10 N2 1.368(7) . ?
C10 C11 1.401(7) . ?
C11 C12 1.407(8) . ?
C11 C27 1.484(8) . ?
C12 N3 1.380(7) . ?
C12 C13 1.428(8) . ?
C13 C14 1.333(8) . ?
C13 H5 0.9500 . ?
C14 C15 1.430(8) . ?
C14 H6 0.9500 . ?
C15 C16 1.371(8) . ?
C15 N3 1.396(7) . ?
C16 C17 1.409(8) . ?
C16 C33 1.489(8) . ?
C17 N4 1.397(7) . ?
C17 C18 1.398(8) . ?
C18 C19 1.379(8) . ?
C18 H7 0.9500 . ?
C19 C20 1.370(8) . ?
C19 H8 0.9500 . ?
C20 N4 1.381(7) . ?
C21 C22 1.380(8) . ?
C21 C26 1.386(8) . ?
C22 F1 1.355(7) . ?
C22 C23 1.377(8) . ?
C23 F2 1.341(7) . ?
C23 C24 1.383(9) . ?
C24 F3 1.333(7) . ?
C24 C25 1.367(9) . ?
C25 F4 1.344(7) . ?
C25 C26 1.383(8) . ?
C26 F5 1.347(7) . ?
C27 C32 1.371(8) . ?
C27 C28 1.403(8) . ?
C28 F6 1.354(7) . ?
C28 C29 1.368(8) . ?
C29 F7 1.346(6) . ?
C29 C30 1.360(9) . ?
C30 F8 1.350(7) . ?
C30 C31 1.381(8) . ?
C31 F9 1.340(7) . ?
C31 C32 1.383(8) . ?
C32 F10 1.356(6) . ?
C33 C38 1.374(8) . ?
C33 C34 1.390(8) . ?
C34 F11 1.334(6) . ?
C34 C35 1.399(8) . ?
C35 F12 1.339(7) . ?
C35 C36 1.367(8) . ?
C36 F13 1.346(7) . ?
C36 C37 1.377(9) . ?
C37 F14 1.343(7) . ?
C37 C38 1.387(8) . ?
C38 F15 1.351(7) . ?
C39 C40 1.406(9) . ?
C39 C46 1.410(8) . ?
C39 C52 1.413(8) . ?
C40 C45 1.395(9) . ?
C40 C41 1.443(8) . ?
C41 N5 1.354(9) . ?
C41 C42 1.403(9) . ?
C42 C43 1.373(9) . ?
C42 H9 0.9500 . ?
C43 C44 1.363(9) . ?
C43 H10 0.9500 . ?
C44 C45 1.408(9) . ?
C44 H11 0.9500 . ?
C45 N6 1.405(8) . ?
C46 C47 1.410(8) . ?
C46 C51 1.418(8) . ?
C47 N6 1.394(8) . ?
C47 C48 1.402(8) . ?
C48 C49 1.378(8) . ?
C48 H12 0.9500 . ?
C49 C50 1.384(8) . ?
C49 H13 0.9500 . ?
C50 C51 1.392(8) . ?
C50 H14 0.9500 . ?
C51 N7 1.383(7) . ?
C52 C53 1.409(9) . ?
C52 C57 1.417(8) . ?
C53 C54 1.385(8) . ?
C53 N7 1.401(7) . ?
C54 C55 1.394(8) . ?
C54 H15 0.9500 . ?
C55 C56 1.376(9) . ?
C55 H16 0.9500 . ?
C56 C57 1.395(9) . ?
C56 H17 0.9500 . ?
C57 N5 1.400(9) . ?
C58A C59A 1.50(2) . ?
C58A N5 1.523(13) . ?
C58A H58A 0.9900 . ?
C58A H58B 0.9900 . ?
C59A C60A 1.560(18) . ?
C59A H59A 0.9900 . ?
C59A H59B 0.9900 . ?
C60A H60A 0.9800 . ?
C60A H60B 0.9800 . ?
C60A H60C 0.9800 . ?
C58B C59B 1.51(3) . ?
C58B N5 1.60(2) . ?
C58B H58C 0.9900 . ?
C58B H58D 0.9900 . ?
C59B C60B 1.46(2) . ?
C59B H59C 0.9900 . ?
C59B H59D 0.9900 . ?
C60B H60D 0.9800 . ?
C60B H60E 0.9800 . ?
C60B H60F 0.9800 . ?
C61A C62A 1.479(18) . ?
C61A N6 1.548(12) . ?
C61A H61A 0.9900 . ?
C61A H61B 0.9900 . ?
C62A C63A 1.463(18) . ?
C62A H62A 0.9900 . ?
C62A H62B 0.9900 . ?
C63A H63A 0.9800 . ?
C63A H63B 0.9800 . ?
C63A H63C 0.9800 . ?
C61B C62B 1.51(4) . ?
C61B N6 1.60(2) . ?
C61B H61C 0.9900 . ?
C61B H61D 0.9900 . ?
C62B C63B 1.66(3) . ?
C62B H62C 0.9900 . ?
C62B H62D 0.9900 . ?
C63B H63D 0.9800 . ?
C63B H63E 0.9800 . ?
C63B H63F 0.9800 . ?
C64 N7 1.491(7) . ?
C64 C65 1.495(8) . ?
C64 H26 0.9900 . ?
C64 H27 0.9900 . ?
C65 C66 1.533(9) . ?
C65 H28 0.9900 . ?
C65 H29 0.9900 . ?
C66 H48 0.9800 . ?
C66 H49 0.9800 . ?
C66 H50 0.9800 . ?
C67 C68 1.452(12) . ?
C67 H39 0.9800 . ?
C67 H40 0.9800 . ?
C67 H41 0.9800 . ?
C68 N8 1.101(10) . ?
N1 Ni1 1.926(4) . ?
N2 Ni1 1.923(5) . ?
N3 Ni1 1.914(4) . ?
N4 Ni1 1.921(5) . ?

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
O1 C1 C2 122.5(5) . . ?
O1 C1 C20 119.2(6) . . ?
C2 C1 C20 118.1(5) . . ?
N1 C2 C3 111.5(5) . . ?
N1 C2 C1 126.3(5) . . ?
C3 C2 C1 121.4(5) . . ?
C4 C3 C2 106.9(5) . . ?
C4 C3 H1 126.5 . . ?
C2 C3 H1 126.5 . . ?
C3 C4 C5 107.2(6) . . ?
C3 C4 H2 126.4 . . ?
C5 C4 H2 126.4 . . ?
C6 C5 N1 123.9(5) . . ?
C6 C5 C4 126.1(6) . . ?
N1 C5 C4 110.0(5) . . ?
C7 C6 C5 123.7(5) . . ?
C7 C6 C21 116.6(5) . . ?
C5 C6 C21 119.2(5) . . ?
C6 C7 N2 124.2(5) . . ?
C6 C7 C8 125.1(5) . . ?
N2 C7 C8 109.4(5) . . ?
C9 C8 C7 108.0(5) . . ?
C9 C8 H3 126.0 . . ?
C7 C8 H3 126.0 . . ?
C8 C9 C10 106.4(5) . . ?
C8 C9 H4 126.8 . . ?
C10 C9 H4 126.8 . . ?
N2 C10 C11 124.4(5) . . ?
N2 C10 C9 111.5(5) . . ?
C11 C10 C9 124.1(5) . . ?
C10 C11 C12 121.1(5) . . ?
C10 C11 C27 120.2(5) . . ?
C12 C11 C27 118.7(5) . . ?
N3 C12 C11 123.7(5) . . ?
N3 C12 C13 111.5(5) . . ?
C11 C12 C13 124.3(6) . . ?
C14 C13 C12 106.7(6) . . ?
C14 C13 H5 126.6 . . ?
C12 C13 H5 126.6 . . ?
C13 C14 C15 107.7(5) . . ?
C13 C14 H6 126.1 . . ?
C15 C14 H6 126.1 . . ?
C16 C15 N3 123.8(5) . . ?
C16 C15 C14 125.9(5) . . ?
N3 C15 C14 110.3(5) . . ?
C15 C16 C17 123.7(5) . . ?
C15 C16 C33 119.0(5) . . ?
C17 C16 C33 117.0(5) . . ?
N4 C17 C18 111.0(5) . . ?
N4 C17 C16 123.0(5) . . ?
C18 C17 C16 125.1(6) . . ?
C19 C18 C17 106.2(6) . . ?
C19 C18 H7 126.9 . . ?
C17 C18 H7 126.9 . . ?
C20 C19 C18 107.3(5) . . ?
C20 C19 H8 126.3 . . ?
C18 C19 H8 126.3 . . ?
C19 C20 N4 112.3(5) . . ?
C19 C20 C1 123.7(5) . . ?
N4 C20 C1 124.0(5) . . ?
C22 C21 C26 115.9(6) . . ?
C22 C21 C6 122.1(5) . . ?
C26 C21 C6 121.8(6) . . ?
F1 C22 C23 118.1(6) . . ?
F1 C22 C21 119.1(5) . . ?
C23 C22 C21 122.8(6) . . ?
F2 C23 C22 120.6(6) . . ?
F2 C23 C24 119.6(6) . . ?
C22 C23 C24 119.8(6) . . ?
F3 C24 C25 120.4(6) . . ?
F3 C24 C23 120.5(6) . . ?
C25 C24 C23 119.1(6) . . ?
F4 C25 C24 119.5(6) . . ?
F4 C25 C26 120.4(6) . . ?
C24 C25 C26 120.0(6) . . ?
F5 C26 C25 117.9(6) . . ?
F5 C26 C21 119.6(5) . . ?
C25 C26 C21 122.5(6) . . ?
C32 C27 C28 115.7(5) . . ?
C32 C27 C11 121.1(5) . . ?
C28 C27 C11 123.1(6) . . ?
F6 C28 C29 118.8(5) . . ?
F6 C28 C27 118.9(5) . . ?
C29 C28 C27 122.3(6) . . ?
F7 C29 C30 119.3(5) . . ?
F7 C29 C28 121.1(6) . . ?
C30 C29 C28 119.5(5) . . ?
F8 C30 C29 120.8(5) . . ?
F8 C30 C31 118.3(6) . . ?
C29 C30 C31 120.9(6) . . ?
F9 C31 C30 120.9(5) . . ?
F9 C31 C32 121.0(5) . . ?
C30 C31 C32 118.1(6) . . ?
F10 C32 C27 119.5(5) . . ?
F10 C32 C31 117.1(6) . . ?
C27 C32 C31 123.3(5) . . ?
C38 C33 C34 116.2(5) . . ?
C38 C33 C16 123.7(6) . . ?
C34 C33 C16 120.0(5) . . ?
F11 C34 C33 120.5(5) . . ?
F11 C34 C35 117.5(6) . . ?
C33 C34 C35 122.0(6) . . ?
F12 C35 C36 121.3(5) . . ?
F12 C35 C34 119.5(6) . . ?
C36 C35 C34 119.2(6) . . ?
F13 C36 C35 119.6(6) . . ?
F13 C36 C37 119.7(6) . . ?
C35 C36 C37 120.6(6) . . ?
F14 C37 C36 119.5(6) . . ?
F14 C37 C38 121.8(6) . . ?
C36 C37 C38 118.7(6) . . ?
F15 C38 C33 120.5(5) . . ?
F15 C38 C37 116.3(6) . . ?
C33 C38 C37 123.2(6) . . ?
C40 C39 C46 119.8(6) . . ?
C40 C39 C52 120.5(5) . . ?
C46 C39 C52 119.6(6) . . ?
C45 C40 C39 120.5(6) . . ?
C45 C40 C41 120.5(6) . . ?
C39 C40 C41 118.9(6) . . ?
N5 C41 C42 123.6(6) . . ?
N5 C41 C40 119.3(6) . . ?
C42 C41 C40 117.1(7) . . ?
C43 C42 C41 120.8(7) . . ?
C43 C42 H9 119.6 . . ?
C41 C42 H9 119.6 . . ?
C44 C43 C42 122.6(7) . . ?
C44 C43 H10 118.7 . . ?
C42 C43 H10 118.7 . . ?
C43 C44 C45 119.2(7) . . ?
C43 C44 H11 120.4 . . ?
C45 C44 H11 120.4 . . ?
C40 C45 N6 118.6(6) . . ?
C40 C45 C44 119.7(6) . . ?
N6 C45 C44 121.5(6) . . ?
C39 C46 C47 120.1(6) . . ?
C39 C46 C51 120.1(6) . . ?
C47 C46 C51 119.7(5) . . ?
N6 C47 C48 121.4(6) . . ?
N6 C47 C46 118.5(5) . . ?
C48 C47 C46 120.0(6) . . ?
C49 C48 C47 118.6(6) . . ?
C49 C48 H12 120.7 . . ?
C47 C48 H12 120.7 . . ?
C48 C49 C50 122.9(6) . . ?
C48 C49 H13 118.6 . . ?
C50 C49 H13 118.6 . . ?
C49 C50 C51 119.3(6) . . ?
C49 C50 H14 120.4 . . ?
C51 C50 H14 120.4 . . ?
N7 C51 C50 121.8(6) . . ?
N7 C51 C46 118.7(5) . . ?
C50 C51 C46 119.5(6) . . ?
C53 C52 C39 120.2(5) . . ?
C53 C52 C57 120.4(6) . . ?
C39 C52 C57 119.3(6) . . ?
C54 C53 N7 122.1(6) . . ?
C54 C53 C52 119.3(5) . . ?
N7 C53 C52 118.6(5) . . ?
C53 C54 C55 119.4(6) . . ?
C53 C54 H15 120.3 . . ?
C55 C54 H15 120.3 . . ?
C56 C55 C54 122.1(6) . . ?
C56 C55 H16 118.9 . . ?
C54 C55 H16 118.9 . . ?
C55 C56 C57 119.6(6) . . ?
C55 C56 H17 120.2 . . ?
C57 C56 H17 120.2 . . ?
C56 C57 N5 122.1(6) . . ?
C56 C57 C52 119.0(6) . . ?
N5 C57 C52 119.0(6) . . ?
C59A C58A N5 103.1(9) . . ?
C59A C58A H58A 111.1 . . ?
N5 C58A H58A 111.1 . . ?
C59A C58A H58B 111.1 . . ?
N5 C58A H58B 111.1 . . ?
H58A C58A H58B 109.1 . . ?
C58A C59A C60A 109.1(12) . . ?
C58A C59A H59A 109.9 . . ?
C60A C59A H59A 109.9 . . ?
C58A C59A H59B 109.9 . . ?
C60A C59A H59B 109.9 . . ?
H59A C59A H59B 108.3 . . ?
C59A C60A H60A 109.5 . . ?
C59A C60A H60B 109.5 . . ?
H60A C60A H60B 109.5 . . ?
C59A C60A H60C 109.5 . . ?
H60A C60A H60C 109.5 . . ?
H60B C60A H60C 109.5 . . ?
C59B C58B N5 101.9(15) . . ?
C59B C58B H58C 111.4 . . ?
N5 C58B H58C 111.4 . . ?
C59B C58B H58D 111.4 . . ?
N5 C58B H58D 111.4 . . ?
H58C C58B H58D 109.2 . . ?
C60B C59B C58B 116.4(19) . . ?
C60B C59B H59C 108.2 . . ?
C58B C59B H59C 108.2 . . ?
C60B C59B H59D 108.2 . . ?
C58B C59B H59D 108.2 . . ?
H59C C59B H59D 107.3 . . ?
C59B C60B H60D 109.5 . . ?
C59B C60B H60E 109.5 . . ?
H60D C60B H60E 109.5 . . ?
C59B C60B H60F 109.5 . . ?
H60D C60B H60F 109.5 . . ?
H60E C60B H60F 109.5 . . ?
C62A C61A N6 109.3(9) . . ?
C62A C61A H61A 109.8 . . ?
N6 C61A H61A 109.8 . . ?
C62A C61A H61B 109.8 . . ?
N6 C61A H61B 109.8 . . ?
H61A C61A H61B 108.3 . . ?
C63A C62A C61A 109.5(10) . . ?
C63A C62A H62A 109.8 . . ?
C61A C62A H62A 109.8 . . ?
C63A C62A H62B 109.8 . . ?
C61A C62A H62B 109.8 . . ?
H62A C62A H62B 108.2 . . ?
C62A C63A H63A 109.5 . . ?
C62A C63A H63B 109.5 . . ?
H63A C63A H63B 109.5 . . ?
C62A C63A H63C 109.5 . . ?
H63A C63A H63C 109.5 . . ?
H63B C63A H63C 109.5 . . ?
C62B C61B N6 101.8(15) . . ?
C62B C61B H61C 111.4 . . ?
N6 C61B H61C 111.4 . . ?
C62B C61B H61D 111.4 . . ?
N6 C61B H61D 111.4 . . ?
H61C C61B H61D 109.3 . . ?
C61B C62B C63B 111.4(19) . . ?
C61B C62B H62C 109.3 . . ?
C63B C62B H62C 109.3 . . ?
C61B C62B H62D 109.3 . . ?
C63B C62B H62D 109.3 . . ?
H62C C62B H62D 108.0 . . ?
C62B C63B H63D 109.5 . . ?
C62B C63B H63E 109.5 . . ?
H63D C63B H63E 109.5 . . ?
C62B C63B H63F 109.5 . . ?
H63D C63B H63F 109.5 . . ?
H63E C63B H63F 109.5 . . ?
N7 C64 C65 115.7(5) . . ?
N7 C64 H26 108.3 . . ?
C65 C64 H26 108.3 . . ?
N7 C64 H27 108.3 . . ?
C65 C64 H27 108.3 . . ?
H26 C64 H27 107.4 . . ?
C64 C65 C66 109.6(5) . . ?
C64 C65 H28 109.7 . . ?
C66 C65 H28 109.7 . . ?
C64 C65 H29 109.7 . . ?
C66 C65 H29 109.7 . . ?
H28 C65 H29 108.2 . . ?
C65 C66 H48 109.5 . . ?
C65 C66 H49 109.5 . . ?
H48 C66 H49 109.5 . . ?
C65 C66 H50 109.5 . . ?
H48 C66 H50 109.5 . . ?
H49 C66 H50 109.5 . . ?
C68 C67 H39 109.5 . . ?
C68 C67 H40 109.5 . . ?
H39 C67 H40 109.5 . . ?
C68 C67 H41 109.5 . . ?
H39 C67 H41 109.5 . . ?
H40 C67 H41 109.5 . . ?
N8 C68 C67 178.7(12) . . ?
C2 N1 C5 104.3(4) . . ?
C2 N1 Ni1 128.2(4) . . ?
C5 N1 Ni1 127.4(4) . . ?
C10 N2 C7 104.7(4) . . ?
C10 N2 Ni1 128.7(4) . . ?
C7 N2 Ni1 126.6(4) . . ?
C12 N3 C15 103.6(4) . . ?
C12 N3 Ni1 128.2(4) . . ?
C15 N3 Ni1 127.9(4) . . ?
C20 N4 C17 103.2(5) . . ?
C20 N4 Ni1 129.9(4) . . ?
C17 N4 Ni1 126.6(4) . . ?
C41 N5 C57 122.8(5) . . ?
C41 N5 C58A 116.2(7) . . ?
C57 N5 C58A 119.3(6) . . ?
C41 N5 C58B 115.0(9) . . ?
C57 N5 C58B 113.0(9) . . ?
C47 N6 C45 121.9(6) . . ?
C47 N6 C61A 118.7(6) . . ?
C45 N6 C61A 118.5(6) . . ?
C47 N6 C61B 114.2(8) . . ?
C45 N6 C61B 111.7(9) . . ?
C51 N7 C53 122.5(5) . . ?
C51 N7 C64 119.5(5) . . ?
C53 N7 C64 117.7(5) . . ?
N3 Ni1 N4 90.8(2) . . ?
N3 Ni1 N2 89.1(2) . . ?
N4 Ni1 N2 175.6(2) . . ?
N3 Ni1 N1 176.1(2) . . ?
N4 Ni1 N1 89.6(2) . . ?
N2 Ni1 N1 90.8(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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -179.1(6) . . . . ?
C20 C1 C2 N1 6.8(9) . . . . ?
O1 C1 C2 C3 12.1(10) . . . . ?
C20 C1 C2 C3 -162.0(6) . . . . ?
N1 C2 C3 C4 -1.5(7) . . . . ?
C1 C2 C3 C4 168.8(6) . . . . ?
C2 C3 C4 C5 1.9(7) . . . . ?
C3 C4 C5 C6 178.3(6) . . . . ?
C3 C4 C5 N1 -1.7(7) . . . . ?
N1 C5 C6 C7 12.7(10) . . . . ?
C4 C5 C6 C7 -167.3(6) . . . . ?
N1 C5 C6 C21 -175.3(5) . . . . ?
C4 C5 C6 C21 4.7(9) . . . . ?
C5 C6 C7 N2 -3.4(10) . . . . ?
C21 C6 C7 N2 -175.6(5) . . . . ?
C5 C6 C7 C8 161.9(6) . . . . ?
C21 C6 C7 C8 -10.3(9) . . . . ?
C6 C7 C8 C9 -164.0(6) . . . . ?
N2 C7 C8 C9 3.2(7) . . . . ?
C7 C8 C9 C10 -2.1(6) . . . . ?
C8 C9 C10 N2 0.3(7) . . . . ?
C8 C9 C10 C11 -177.8(6) . . . . ?
N2 C10 C11 C12 -14.6(9) . . . . ?
C9 C10 C11 C12 163.2(6) . . . . ?
N2 C10 C11 C27 167.3(5) . . . . ?
C9 C10 C11 C27 -14.8(9) . . . . ?
C10 C11 C12 N3 6.8(9) . . . . ?
C27 C11 C12 N3 -175.1(5) . . . . ?
C10 C11 C12 C13 -164.8(6) . . . . ?
C27 C11 C12 C13 13.3(9) . . . . ?
N3 C12 C13 C14 -4.1(7) . . . . ?
C11 C12 C13 C14 168.4(6) . . . . ?
C12 C13 C14 C15 3.7(7) . . . . ?
C13 C14 C15 C16 175.4(6) . . . . ?
C13 C14 C15 N3 -2.3(7) . . . . ?
N3 C15 C16 C17 13.9(10) . . . . ?
C14 C15 C16 C17 -163.5(6) . . . . ?
N3 C15 C16 C33 -172.4(5) . . . . ?
C14 C15 C16 C33 10.2(9) . . . . ?
C15 C16 C17 N4 -2.5(10) . . . . ?
C33 C16 C17 N4 -176.4(5) . . . . ?
C15 C16 C17 C18 166.0(6) . . . . ?
C33 C16 C17 C18 -7.9(9) . . . . ?
N4 C17 C18 C19 2.7(7) . . . . ?
C16 C17 C18 C19 -167.0(6) . . . . ?
C17 C18 C19 C20 -2.1(7) . . . . ?
C18 C19 C20 N4 0.9(8) . . . . ?
C18 C19 C20 C1 -177.7(6) . . . . ?
O1 C1 C20 C19 -12.5(10) . . . . ?
C2 C1 C20 C19 161.7(6) . . . . ?
O1 C1 C20 N4 169.0(5) . . . . ?
C2 C1 C20 N4 -16.8(9) . . . . ?
C7 C6 C21 C22 -76.3(8) . . . . ?
C5 C6 C21 C22 111.1(7) . . . . ?
C7 C6 C21 C26 97.9(7) . . . . ?
C5 C6 C21 C26 -74.7(8) . . . . ?
C26 C21 C22 F1 179.7(5) . . . . ?
C6 C21 C22 F1 -5.8(9) . . . . ?
C26 C21 C22 C23 -0.5(9) . . . . ?
C6 C21 C22 C23 173.9(5) . . . . ?
F1 C22 C23 F2 -0.4(8) . . . . ?
C21 C22 C23 F2 179.9(5) . . . . ?
F1 C22 C23 C24 179.4(5) . . . . ?
C21 C22 C23 C24 -0.4(9) . . . . ?
F2 C23 C24 F3 3.0(8) . . . . ?
C22 C23 C24 F3 -176.8(5) . . . . ?
F2 C23 C24 C25 -178.7(5) . . . . ?
C22 C23 C24 C25 1.5(9) . . . . ?
F3 C24 C25 F4 -1.1(9) . . . . ?
C23 C24 C25 F4 -179.4(5) . . . . ?
F3 C24 C25 C26 176.6(5) . . . . ?
C23 C24 C25 C26 -1.7(9) . . . . ?
F4 C25 C26 F5 -0.1(9) . . . . ?
C24 C25 C26 F5 -177.7(5) . . . . ?
F4 C25 C26 C21 178.5(5) . . . . ?
C24 C25 C26 C21 0.8(10) . . . . ?
C22 C21 C26 F5 178.8(5) . . . . ?
C6 C21 C26 F5 4.3(9) . . . . ?
C22 C21 C26 C25 0.3(9) . . . . ?
C6 C21 C26 C25 -174.2(6) . . . . ?
C10 C11 C27 C32 -85.8(7) . . . . ?
C12 C11 C27 C32 96.1(7) . . . . ?
C10 C11 C27 C28 97.1(7) . . . . ?
C12 C11 C27 C28 -81.0(8) . . . . ?
C32 C27 C28 F6 177.4(5) . . . . ?
C11 C27 C28 F6 -5.4(9) . . . . ?
C32 C27 C28 C29 -3.5(9) . . . . ?
C11 C27 C28 C29 173.8(6) . . . . ?
F6 C28 C29 F7 0.6(9) . . . . ?
C27 C28 C29 F7 -178.6(5) . . . . ?
F6 C28 C29 C30 179.3(5) . . . . ?
C27 C28 C29 C30 0.1(9) . . . . ?
F7 C29 C30 F8 3.1(9) . . . . ?
C28 C29 C30 F8 -175.7(5) . . . . ?
F7 C29 C30 C31 -179.0(5) . . . . ?
C28 C29 C30 C31 2.3(9) . . . . ?
F8 C30 C31 F9 -2.6(9) . . . . ?
C29 C30 C31 F9 179.4(5) . . . . ?
F8 C30 C31 C32 176.9(5) . . . . ?
C29 C30 C31 C32 -1.1(9) . . . . ?
C28 C27 C32 F10 -178.1(5) . . . . ?
C11 C27 C32 F10 4.6(8) . . . . ?
C28 C27 C32 C31 4.8(9) . . . . ?
C11 C27 C32 C31 -172.5(5) . . . . ?
F9 C31 C32 F10 -0.3(8) . . . . ?
C30 C31 C32 F10 -179.9(5) . . . . ?
F9 C31 C32 C27 176.9(5) . . . . ?
C30 C31 C32 C27 -2.6(9) . . . . ?
C15 C16 C33 C38 -80.3(7) . . . . ?
C17 C16 C33 C38 93.9(7) . . . . ?
C15 C16 C33 C34 101.3(7) . . . . ?
C17 C16 C33 C34 -84.5(7) . . . . ?
C38 C33 C34 F11 179.8(5) . . . . ?
C16 C33 C34 F11 -1.7(8) . . . . ?
C38 C33 C34 C35 -0.6(8) . . . . ?
C16 C33 C34 C35 177.8(5) . . . . ?
F11 C34 C35 F12 -0.7(8) . . . . ?
C33 C34 C35 F12 179.7(5) . . . . ?
F11 C34 C35 C36 -179.3(5) . . . . ?
C33 C34 C35 C36 1.1(9) . . . . ?
F12 C35 C36 F13 0.3(8) . . . . ?
C34 C35 C36 F13 178.9(5) . . . . ?
F12 C35 C36 C37 -179.0(5) . . . . ?
C34 C35 C36 C37 -0.4(9) . . . . ?
F13 C36 C37 F14 1.0(9) . . . . ?
C35 C36 C37 F14 -179.7(5) . . . . ?
F13 C36 C37 C38 -180.0(5) . . . . ?
C35 C36 C37 C38 -0.7(9) . . . . ?
C34 C33 C38 F15 -179.7(5) . . . . ?
C16 C33 C38 F15 1.8(9) . . . . ?
C34 C33 C38 C37 -0.5(9) . . . . ?
C16 C33 C38 C37 -179.0(6) . . . . ?
F14 C37 C38 F15 -0.6(9) . . . . ?
C36 C37 C38 F15 -179.6(5) . . . . ?
F14 C37 C38 C33 -179.8(5) . . . . ?
C36 C37 C38 C33 1.2(9) . . . . ?
C46 C39 C40 C45 -2.2(10) . . . . ?
C52 C39 C40 C45 -178.7(6) . . . . ?
C46 C39 C40 C41 -179.3(6) . . . . ?
C52 C39 C40 C41 4.2(10) . . . . ?
C45 C40 C41 N5 179.1(7) . . . . ?
C39 C40 C41 N5 -3.8(11) . . . . ?
C45 C40 C41 C42 0.7(11) . . . . ?
C39 C40 C41 C42 177.8(7) . . . . ?
N5 C41 C42 C43 -176.5(8) . . . . ?
C40 C41 C42 C43 1.8(12) . . . . ?
C41 C42 C43 C44 -2.3(13) . . . . ?
C42 C43 C44 C45 0.1(12) . . . . ?
C39 C40 C45 N6 4.6(11) . . . . ?
C41 C40 C45 N6 -178.4(7) . . . . ?
C39 C40 C45 C44 -179.8(7) . . . . ?
C41 C40 C45 C44 -2.8(11) . . . . ?
C43 C44 C45 C40 2.4(12) . . . . ?
C43 C44 C45 N6 177.8(7) . . . . ?
C40 C39 C46 C47 3.1(10) . . . . ?
C52 C39 C46 C47 179.6(6) . . . . ?
C40 C39 C46 C51 178.9(6) . . . . ?
C52 C39 C46 C51 -4.6(10) . . . . ?
C39 C46 C47 N6 -6.3(10) . . . . ?
C51 C46 C47 N6 177.8(6) . . . . ?
C39 C46 C47 C48 177.6(6) . . . . ?
C51 C46 C47 C48 1.7(10) . . . . ?
N6 C47 C48 C49 -176.8(6) . . . . ?
C46 C47 C48 C49 -0.9(10) . . . . ?
C47 C48 C49 C50 0.7(10) . . . . ?
C48 C49 C50 C51 -1.4(10) . . . . ?
C49 C50 C51 N7 -176.0(6) . . . . ?
C49 C50 C51 C46 2.2(9) . . . . ?
C39 C46 C51 N7 0.0(9) . . . . ?
C47 C46 C51 N7 175.9(6) . . . . ?
C39 C46 C51 C50 -178.3(6) . . . . ?
C47 C46 C51 C50 -2.4(9) . . . . ?
C40 C39 C52 C53 -179.1(6) . . . . ?
C46 C39 C52 C53 4.5(10) . . . . ?
C40 C39 C52 C57 -3.2(10) . . . . ?
C46 C39 C52 C57 -179.7(6) . . . . ?
C39 C52 C53 C54 -177.7(6) . . . . ?
C57 C52 C53 C54 6.5(10) . . . . ?
C39 C52 C53 N7 0.2(10) . . . . ?
C57 C52 C53 N7 -175.7(6) . . . . ?
N7 C53 C54 C55 176.5(6) . . . . ?
C52 C53 C54 C55 -5.7(10) . . . . ?
C53 C54 C55 C56 1.9(11) . . . . ?
C54 C55 C56 C57 1.4(12) . . . . ?
C55 C56 C57 N5 178.5(8) . . . . ?
C55 C56 C57 C52 -0.7(12) . . . . ?
C53 C52 C57 C56 -3.2(11) . . . . ?
C39 C52 C57 C56 -179.1(7) . . . . ?
C53 C52 C57 N5 177.6(7) . . . . ?
C39 C52 C57 N5 1.7(11) . . . . ?
N5 C58A C59A C60A 170.5(9) . . . . ?
N5 C58B C59B C60B -172.7(13) . . . . ?
N6 C61A C62A C63A -166.6(9) . . . . ?
N6 C61B C62B C63B -178.6(15) . . . . ?
N7 C64 C65 C66 179.0(5) . . . . ?
C3 C2 N1 C5 0.5(7) . . . . ?
C1 C2 N1 C5 -169.3(6) . . . . ?
C3 C2 N1 Ni1 -176.2(4) . . . . ?
C1 C2 N1 Ni1 14.0(9) . . . . ?
C6 C5 N1 C2 -179.3(6) . . . . ?
C4 C5 N1 C2 0.7(7) . . . . ?
C6 C5 N1 Ni1 -2.6(8) . . . . ?
C4 C5 N1 Ni1 177.4(4) . . . . ?
C11 C10 N2 C7 179.7(5) . . . . ?
C9 C10 N2 C7 1.6(6) . . . . ?
C11 C10 N2 Ni1 -0.3(8) . . . . ?
C9 C10 N2 Ni1 -178.3(4) . . . . ?
C6 C7 N2 C10 164.4(6) . . . . ?
C8 C7 N2 C10 -2.9(6) . . . . ?
C6 C7 N2 Ni1 -15.6(8) . . . . ?
C8 C7 N2 Ni1 177.1(4) . . . . ?
C11 C12 N3 C15 -170.0(5) . . . . ?
C13 C12 N3 C15 2.6(6) . . . . ?
C11 C12 N3 Ni1 15.8(8) . . . . ?
C13 C12 N3 Ni1 -171.7(4) . . . . ?
C16 C15 N3 C12 -178.0(6) . . . . ?
C14 C15 N3 C12 -0.2(6) . . . . ?
C16 C15 N3 Ni1 -3.7(9) . . . . ?
C14 C15 N3 Ni1 174.0(4) . . . . ?
C19 C20 N4 C17 0.7(7) . . . . ?
C1 C20 N4 C17 179.3(6) . . . . ?
C19 C20 N4 Ni1 -172.6(4) . . . . ?
C1 C20 N4 Ni1 6.0(9) . . . . ?
C18 C17 N4 C20 -2.0(7) . . . . ?
C16 C17 N4 C20 167.9(6) . . . . ?
C18 C17 N4 Ni1 171.6(4) . . . . ?
C16 C17 N4 Ni1 -18.5(8) . . . . ?
C42 C41 N5 C57 -179.2(8) . . . . ?
C40 C41 N5 C57 2.5(13) . . . . ?
C42 C41 N5 C58A 15.4(13) . . . . ?
C40 C41 N5 C58A -162.9(8) . . . . ?
C42 C41 N5 C58B -34.6(14) . . . . ?
C40 C41 N5 C58B 147.1(11) . . . . ?
C56 C57 N5 C41 179.4(8) . . . . ?
C52 C57 N5 C41 -1.4(13) . . . . ?
C56 C57 N5 C58A -15.7(13) . . . . ?
C52 C57 N5 C58A 163.5(8) . . . . ?
C56 C57 N5 C58B 34.1(13) . . . . ?
C52 C57 N5 C58B -146.7(10) . . . . ?
C59A C58A N5 C41 -93.7(10) . . . . ?
C59A C58A N5 C57 100.4(10) . . . . ?
C59B C58B N5 C41 102.1(13) . . . . ?
C59B C58B N5 C57 -109.8(13) . . . . ?
C48 C47 N6 C45 -175.0(7) . . . . ?
C46 C47 N6 C45 8.9(11) . . . . ?
C48 C47 N6 C61A 15.9(11) . . . . ?
C46 C47 N6 C61A -160.1(7) . . . . ?
C48 C47 N6 C61B -35.9(13) . . . . ?
C46 C47 N6 C61B 148.0(10) . . . . ?
C40 C45 N6 C47 -8.1(11) . . . . ?
C44 C45 N6 C47 176.4(7) . . . . ?
C40 C45 N6 C61A 161.0(7) . . . . ?
C44 C45 N6 C61A -14.5(11) . . . . ?
C40 C45 N6 C61B -148.1(10) . . . . ?
C44 C45 N6 C61B 36.4(13) . . . . ?
C62A C61A N6 C47 -98.5(9) . . . . ?
C62A C61A N6 C45 92.1(9) . . . . ?
C62B C61B N6 C47 111.3(13) . . . . ?
C62B C61B N6 C45 -105.4(13) . . . . ?
C50 C51 N7 C53 -176.9(6) . . . . ?
C46 C51 N7 C53 4.8(9) . . . . ?
C50 C51 N7 C64 10.0(9) . . . . ?
C46 C51 N7 C64 -168.3(6) . . . . ?
C54 C53 N7 C51 172.9(6) . . . . ?
C52 C53 N7 C51 -4.9(9) . . . . ?
C54 C53 N7 C64 -13.9(9) . . . . ?
C52 C53 N7 C64 168.3(6) . . . . ?
C65 C64 N7 C51 -91.1(7) . . . . ?
C65 C64 N7 C53 95.5(7) . . . . ?

_refine_diff_density_max         0.493
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.100



