#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:29:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178784 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/38/4103838.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4103838
loop_
_publ_author_name
'Carlos Peinador'
'Víctor Blanco'
'José M. Quintela'
_publ_section_title
;
 A New Doubly Interlocked [2]Catenane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              920
_journal_page_last               921
_journal_paper_doi               10.1021/ja8088372
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C130 H144 F36 N16 O36 P4 Pd2 S4'
_chemical_formula_weight         3655.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 114.204(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   44.661(5)
_cell_length_b                   13.570(5)
_cell_length_c                   29.304(5)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.880
_cell_measurement_theta_min      5.212
_cell_volume                     16198(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            82038
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_correction_T_min  0.8747
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7456
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         16451
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.1182
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3223
_refine_ls_wR_factor_ref         0.3910
_reflns_number_gt                8348
_reflns_number_total             16451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8088372_si_002.cif
_cod_data_source_block           matrix_60s_0s
_cod_database_code               4103838
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.6043(2) 0.2019(6) 0.6601(3) 0.0416(19) Uani 1 1 d .
H1 H 0.6164 0.1430 0.6723 0.050 Uiso 1 1 calc R
C2 C 0.5710(2) 0.1970(6) 0.6285(3) 0.0381(18) Uani 1 1 d .
C3 C 0.55344(19) 0.2836(5) 0.6107(3) 0.0337(17) Uani 1 1 d .
C4 C 0.56920(19) 0.3760(6) 0.6244(3) 0.0364(18) Uani 1 1 d .
C5 C 0.6027(2) 0.3759(6) 0.6569(3) 0.043(2) Uani 1 1 d .
H5 H 0.6139 0.4368 0.6674 0.052 Uiso 1 1 calc R
C6 C 0.5537(2) 0.1017(6) 0.6139(3) 0.044(2) Uani 1 1 d .
H6 H 0.5655 0.0417 0.6248 0.053 Uiso 1 1 calc R
C7 C 0.5213(2) 0.1000(6) 0.5851(3) 0.043(2) Uani 1 1 d .
H7 H 0.5102 0.0386 0.5762 0.052 Uiso 1 1 calc R
C8 C 0.5032(2) 0.1892(6) 0.5677(3) 0.0390(19) Uani 1 1 d .
C9 C 0.5193(2) 0.2803(6) 0.5795(3) 0.0383(19) Uani 1 1 d .
C10 C 0.5015(2) 0.3710(6) 0.5611(3) 0.0414(19) Uani 1 1 d .
C11 C 0.5189(2) 0.4624(7) 0.5742(3) 0.046(2) Uani 1 1 d .
H11 H 0.5076 0.5222 0.5609 0.055 Uiso 1 1 calc R
C12 C 0.5514(2) 0.4647(6) 0.6056(3) 0.047(2) Uani 1 1 d .
H12 H 0.5623 0.5263 0.6150 0.056 Uiso 1 1 calc R
C13 C 0.4684(2) 0.3649(7) 0.5323(3) 0.044(2) Uani 1 1 d .
H13 H 0.4562 0.4230 0.5185 0.053 Uiso 1 1 calc R
C14 C 0.4696(2) 0.1889(6) 0.5400(3) 0.0410(19) Uani 1 1 d .
H14 H 0.4579 0.1283 0.5325 0.049 Uiso 1 1 calc R
C15 C 0.4161(3) 0.2695(7) 0.4950(4) 0.060(3) Uani 1 1 d .
H15A H 0.4077 0.3238 0.4705 0.072 Uiso 1 1 calc R
H15B H 0.4099 0.2059 0.4769 0.072 Uiso 1 1 calc R
C16 C 0.3948(2) 0.1909(7) 0.5502(3) 0.052(2) Uani 1 1 d .
H16 H 0.3980 0.1301 0.5368 0.063 Uiso 1 1 calc R
C17 C 0.3827(2) 0.1920(6) 0.5862(3) 0.049(2) Uani 1 1 d .
C18 C 0.37886(18) 0.2839(6) 0.6051(3) 0.0380(18) Uani 1 1 d .
C19 C 0.3862(2) 0.3735(7) 0.5862(3) 0.048(2) Uani 1 1 d .
C20 C 0.3980(2) 0.3647(7) 0.5504(3) 0.046(2) Uani 1 1 d .
H20 H 0.4033 0.4225 0.5370 0.056 Uiso 1 1 calc R
C21 C 0.3749(3) 0.1049(8) 0.6055(4) 0.070(3) Uani 1 1 d .
H21 H 0.3770 0.0428 0.5921 0.084 Uiso 1 1 calc R
C22 C 0.3644(3) 0.1087(7) 0.6427(4) 0.064(3) Uani 1 1 d .
H22 H 0.3598 0.0491 0.6556 0.077 Uiso 1 1 calc R
C23 C 0.3601(2) 0.2007(6) 0.6628(3) 0.045(2) Uani 1 1 d .
C24 C 0.36719(18) 0.2891(6) 0.6437(3) 0.0397(19) Uani 1 1 d .
C25 C 0.3814(3) 0.4673(7) 0.6060(4) 0.060(3) Uani 1 1 d .
H25 H 0.3857 0.5271 0.5929 0.071 Uiso 1 1 calc R
C26 C 0.3707(2) 0.4697(7) 0.6428(4) 0.056(2) Uani 1 1 d .
H26 H 0.3678 0.5317 0.6555 0.068 Uiso 1 1 calc R
C27 C 0.36375(19) 0.3825(6) 0.6633(3) 0.0399(19) Uani 1 1 d .
C28 C 0.35309(18) 0.3821(6) 0.7019(3) 0.0403(19) Uani 1 1 d .
H28 H 0.3502 0.4430 0.7157 0.048 Uiso 1 1 calc R
C29 C 0.3502(2) 0.2089(6) 0.7011(3) 0.049(2) Uani 1 1 d .
H29 H 0.3456 0.1506 0.7150 0.059 Uiso 1 1 calc R
C30 C 0.7356(3) 0.2833(11) 0.7419(5) 0.088(4) Uani 1 1 d .
H30A H 0.7556 0.3242 0.7568 0.106 Uiso 1 1 calc R
H30B H 0.7426 0.2134 0.7470 0.106 Uiso 1 1 calc R
C31 C 0.7218(3) 0.3007(12) 0.6935(6) 0.105(5) Uani 1 1 d .
H31A H 0.7323 0.2574 0.6770 0.127 Uiso 1 1 calc R
H31B H 0.7267 0.3696 0.6878 0.127 Uiso 1 1 calc R
C32 C 0.4798(3) 0.2944(10) 0.6656(4) 0.076(3) Uani 1 1 d .
H32 H 0.4574 0.3052 0.6443 0.092 Uiso 1 1 calc R
C33 C 0.4908(3) 0.2045(11) 0.6756(4) 0.074(3) Uani 1 1 d .
C34 C 0.5219(4) 0.1828(11) 0.7060(5) 0.088(4) Uani 1 1 d .
H34 H 0.5289 0.1164 0.7137 0.106 Uiso 1 1 calc R
C35 C 0.5440(4) 0.2628(15) 0.7264(5) 0.102(5) Uani 1 1 d .
H35 H 0.5664 0.2498 0.7471 0.122 Uiso 1 1 calc R
C36 C 0.5331(4) 0.3603(12) 0.7164(5) 0.088(4) Uani 1 1 d .
C37 C 0.5004(3) 0.3748(11) 0.6857(5) 0.087(4) Uani 1 1 d .
H37 H 0.4919 0.4398 0.6782 0.104 Uiso 1 1 calc R
C38 C 0.4785(4) 0.0360(11) 0.6609(6) 0.096(5) Uani 1 1 d .
H38A H 0.4852 0.0196 0.6967 0.115 Uiso 1 1 calc R
H38B H 0.4979 0.0291 0.6530 0.115 Uiso 1 1 calc R
C39 C 0.4531(4) -0.0302(11) 0.6304(7) 0.117(6) Uani 1 1 d .
H39A H 0.4334 -0.0218 0.6374 0.140 Uiso 1 1 calc R
H39B H 0.4608 -0.0992 0.6381 0.140 Uiso 1 1 calc R
C40 C 0.4281(4) -0.0848(10) 0.5401(7) 0.115(6) Uani 1 1 d .
H40A H 0.4064 -0.0975 0.5406 0.139 Uiso 1 1 calc R
H40B H 0.4411 -0.1463 0.5499 0.139 Uiso 1 1 calc R
C41 C 0.4236(6) -0.0573(12) 0.4898(9) 0.151(10) Uani 1 1 d .
H41A H 0.4453 -0.0471 0.4888 0.182 Uiso 1 1 calc R
H41B H 0.4122 -0.1110 0.4662 0.182 Uiso 1 1 calc R
C42 C 0.5440(4) 0.5383(11) 0.7219(6) 0.092(4) Uani 1 1 d .
H42A H 0.5334 0.5423 0.6850 0.110 Uiso 1 1 calc R
H42B H 0.5273 0.5550 0.7349 0.110 Uiso 1 1 calc R
C43 C 0.5699(4) 0.6064(14) 0.7403(6) 0.122(6) Uani 1 1 d .
H43A H 0.5612 0.6745 0.7335 0.147 Uiso 1 1 calc R
H43B H 0.5821 0.5984 0.7769 0.147 Uiso 1 1 calc R
C44 C 0.3868(4) 0.6634(11) 0.7748(6) 0.109(5) Uani 1 1 d .
H44A H 0.3987 0.7259 0.7877 0.131 Uiso 1 1 calc R
H44B H 0.3744 0.6710 0.7382 0.131 Uiso 1 1 calc R
C45 C 0.3658(4) 0.6503(11) 0.7949(11) 0.193(13) Uani 1 1 d .
H45A H 0.3480 0.6995 0.7805 0.232 Uiso 1 1 calc R
H45B H 0.3771 0.6638 0.8312 0.232 Uiso 1 1 calc R
C46 C 0.3206(3) 0.5592(10) 0.7944(5) 0.088(4) Uani 1 1 d .
H46A H 0.3166 0.4930 0.8050 0.105 Uiso 1 1 calc R
H46B H 0.3225 0.6062 0.8213 0.105 Uiso 1 1 calc R
C47 C 0.2941(3) 0.5854(9) 0.7514(6) 0.085(4) Uani 1 1 d .
H47A H 0.2970 0.6535 0.7418 0.101 Uiso 1 1 calc R
H47B H 0.2739 0.5837 0.7575 0.101 Uiso 1 1 calc R
C48 C 0.2667(3) 0.5508(13) 0.6642(5) 0.104(5) Uani 1 1 d .
H48A H 0.2450 0.5223 0.6585 0.124 Uiso 1 1 calc R
H48B H 0.2648 0.6235 0.6639 0.124 Uiso 1 1 calc R
C49 C 0.2760(4) 0.5205(13) 0.6264(7) 0.118(6) Uani 1 1 d .
H49A H 0.2991 0.5393 0.6347 0.142 Uiso 1 1 calc R
H49B H 0.2618 0.5515 0.5942 0.142 Uiso 1 1 calc R
C50 C 0.2813(2) 0.3685(13) 0.5872(4) 0.155(10) Uani 1 1 d G
C51 C 0.2925(3) 0.4164(11) 0.5553(5) 0.151(9) Uani 1 1 d G
H51 H 0.2941 0.4862 0.5559 0.181 Uiso 1 1 calc R
C52 C 0.3014(2) 0.3621(16) 0.5225(4) 0.211(16) Uani 1 1 d G
H52 H 0.3090 0.3948 0.5007 0.253 Uiso 1 1 calc R
C53 C 0.2990(2) 0.2599(15) 0.5217(4) 0.28(3) Uani 1 1 d G
C54 C 0.2878(3) 0.2120(11) 0.5537(6) 0.28(2) Uani 1 1 d G
H54 H 0.2862 0.1422 0.5531 0.334 Uiso 1 1 calc R
C55 C 0.2790(2) 0.2663(13) 0.5864(5) 0.190(13) Uani 1 1 d G
H55 H 0.2713 0.2336 0.6083 0.227 Uiso 1 1 calc R
C56 C 0.3131(7) 0.273(3) 0.4521(15) 0.331(14) Uani 1 1 d U
H56A H 0.2943 0.3189 0.4395 0.398 Uiso 1 1 calc R
H56B H 0.3331 0.3121 0.4708 0.398 Uiso 1 1 calc R
C57 C 0.3165(7) 0.227(3) 0.4088(14) 0.250(11) Uani 1 1 d U
H57A H 0.2997 0.1748 0.3938 0.300 Uiso 1 1 calc R
H57B H 0.3143 0.2764 0.3829 0.300 Uiso 1 1 calc R
C58 C 0.3521(15) 0.095(3) 0.3940(11) 0.38(4) Uani 1 1 d .
H58A H 0.3318 0.0564 0.3767 0.455 Uiso 1 1 calc R
H58B H 0.3597 0.1206 0.3689 0.455 Uiso 1 1 calc R
C59 C 0.3814(4) 0.026(2) 0.4370(12) 0.194(14) Uani 1 1 d .
H59A H 0.3674 -0.0216 0.4452 0.233 Uiso 1 1 calc R
H59B H 0.3891 -0.0119 0.4150 0.233 Uiso 1 1 calc R
C60 C 0.6142(5) 0.3505(18) 0.5294(9) 0.164(10) Uani 1 1 d .
C61 C 0.3230(12) 0.0699(19) 0.245(2) 0.39(4) Uani 1 1 d .
C66 C 0.5398(4) 0.3147(9) 0.3529(7) 0.107(5) Uani 1 1 d .
H66A H 0.5349 0.3301 0.3179 0.161 Uiso 1 1 calc R
H66B H 0.5217 0.2763 0.3546 0.161 Uiso 1 1 calc R
H66C H 0.5601 0.2763 0.3672 0.161 Uiso 1 1 calc R
C67 C 0.5436(4) 0.4034(12) 0.3802(6) 0.097(4) Uani 1 1 d .
C68 C 0.4389(5) 0.1051(9) 0.2514(5) 0.110(6) Uani 1 1 d .
H68A H 0.4577 0.0741 0.2482 0.166 Uiso 1 1 calc R
H68B H 0.4466 0.1479 0.2809 0.166 Uiso 1 1 calc R
H68C H 0.4267 0.1446 0.2215 0.166 Uiso 1 1 calc R
C69 C 0.4183(5) 0.0321(16) 0.2565(6) 0.122(6) Uani 1 1 d .
N1 N 0.61923(16) 0.2904(5) 0.6735(2) 0.0391(15) Uani 1 1 d .
N2 N 0.45318(17) 0.2765(5) 0.5234(3) 0.0443(17) Uani 1 1 d .
N3 N 0.40229(17) 0.2768(6) 0.5338(3) 0.0468(18) Uani 1 1 d .
N4 N 0.34683(16) 0.2976(5) 0.7200(2) 0.0384(15) Uani 1 1 d .
N5 N 0.7152(2) 0.3023(6) 0.7687(3) 0.062(2) Uani 1 1 d .
H5A H 0.7199 0.3638 0.7831 0.074 Uiso 1 1 calc R
H5B H 0.7197 0.2566 0.7939 0.074 Uiso 1 1 calc R
N6 N 0.6847(2) 0.2855(5) 0.6677(3) 0.055(2) Uani 1 1 d .
H6A H 0.6799 0.2247 0.6525 0.066 Uiso 1 1 calc R
H6B H 0.6752 0.3332 0.6437 0.066 Uiso 1 1 calc R
N9 N 0.5469(4) 0.4726(12) 0.4011(7) 0.145(6) Uani 1 1 d .
N10 N 0.4048(4) -0.0392(17) 0.2624(7) 0.184(8) Uani 1 1 d .
O1 O 0.4672(2) 0.1305(7) 0.6522(3) 0.086(2) Uani 1 1 d .
O2 O 0.4447(2) -0.0081(6) 0.5756(4) 0.100(3) Uani 1 1 d .
O3 O 0.4065(6) 0.0227(11) 0.4766(5) 0.171(7) Uani 1 1 d .
O4 O 0.5558(2) 0.4380(9) 0.7369(4) 0.106(3) Uani 1 1 d .
O5 O 0.5903(3) 0.5894(9) 0.7168(5) 0.127(4) Uani 1 1 d .
O6 O 0.35178(17) 0.5578(5) 0.7886(3) 0.073(2) Uani 1 1 d .
O7 O 0.29064(18) 0.5190(6) 0.7112(3) 0.077(2) Uani 1 1 d .
O8 O 0.27238(19) 0.4134(11) 0.6231(3) 0.115(4) Uani 1 1 d .
O9 O 0.3455(4) 0.1891(18) 0.4271(7) 0.232(9) Uani 1 1 d U
O10 O 0.3073(3) 0.191(3) 0.4934(6) 0.38(2) Uani 1 1 d U
O11 O 0.6471(2) 0.4874(9) 0.5207(4) 0.133(4) Uani 1 1 d .
O12 O 0.6472(3) 0.4335(8) 0.6009(3) 0.113(3) Uani 1 1 d .
O13 O 0.5986(2) 0.5074(6) 0.5399(3) 0.091(3) Uani 1 1 d .
O14 O 0.3285(3) -0.0668(8) 0.2988(7) 0.205(7) Uani 1 1 d U
O15 O 0.2858(8) -0.066(2) 0.2252(8) 0.340(14) Uani 1 1 d DU
O16 O 0.2835(4) 0.0294(12) 0.2731(9) 0.240(9) Uani 1 1 d U
F1 F 0.46299(18) 0.1286(4) 0.4423(2) 0.0801(19) Uani 1 1 d .
F2 F 0.49524(16) 0.2616(5) 0.4524(2) 0.086(2) Uani 1 1 d .
F3 F 0.4903(2) 0.1440(5) 0.3927(3) 0.103(3) Uani 1 1 d .
F4 F 0.46996(17) 0.2945(4) 0.3700(2) 0.0739(18) Uani 1 1 d .
F5 F 0.43648(19) 0.1642(6) 0.3605(2) 0.095(2) Uani 1 1 d .
F6 F 0.44169(17) 0.2810(4) 0.4179(2) 0.0729(17) Uani 1 1 d .
F7 F 0.5956(4) 0.2965(6) 0.5459(5) 0.176(6) Uani 1 1 d .
F8 F 0.6403(5) 0.2756(10) 0.5310(5) 0.220(8) Uani 1 1 d .
F9 F 0.6004(3) 0.3359(9) 0.4768(4) 0.165(5) Uani 1 1 d .
F10 F 0.3391(7) 0.1263(16) 0.2564(10) 0.331(18) Uani 1 1 d .
F11 F 0.2905(9) 0.1345(16) 0.1935(19) 0.59(4) Uani 1 1 d .
F12 F 0.3257(4) 0.0213(9) 0.2005(8) 0.264(10) Uani 1 1 d .
F13 F 0.6127(3) 0.2864(8) 0.3570(7) 0.181(6) Uani 1 1 d .
F14 F 0.6300(5) 0.1579(12) 0.4123(10) 0.307(13) Uani 1 1 d .
F15 F 0.6331(6) 0.1368(12) 0.3425(8) 0.321(12) Uani 1 1 d .
F16 F 0.6800(6) 0.1675(15) 0.4091(8) 0.319(12) Uani 1 1 d .
F17 F 0.6677(5) 0.2863(12) 0.3702(13) 0.337(16) Uani 1 1 d .
F18 F 0.6445(13) 0.2985(16) 0.4204(8) 0.48(3) Uani 1 1 d .
P1 P 0.46618(7) 0.21212(16) 0.40576(9) 0.0508(6) Uani 1 1 d .
P2 P 0.64076(15) 0.2157(3) 0.38266(18) 0.1086(15) Uani 1 1 d .
S1 S 0.62794(11) 0.4534(3) 0.55114(13) 0.0976(12) Uani 1 1 d .
S2 S 0.30573(16) -0.0070(5) 0.2704(3) 0.164(3) Uani 1 1 d DU
Pd1 Pd 0.667354(16) 0.29518(5) 0.72218(3) 0.0427(3) Uani 1 1 d .
O18 O 0.2561(4) -0.1330(14) 0.1616(7) 0.212(7) Uiso 1 1 d .
O17 O 0.3150(6) -0.0173(18) 0.4797(9) 0.282(10) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C2 120.1(8) . .
C3 C2 C1 119.5(7) . .
C3 C2 C6 119.0(7) . .
C1 C2 C6 121.5(7) . .
C2 C3 C4 120.3(7) . .
C2 C3 C9 120.4(7) . .
C4 C3 C9 119.2(7) . .
C5 C4 C3 117.3(7) . .
C5 C4 C12 122.3(8) . .
C3 C4 C12 120.4(7) . .
N1 C5 C4 121.1(7) . .
C7 C6 C2 119.7(8) . .
C6 C7 C8 121.1(8) . .
C14 C8 C9 118.1(8) . .
C14 C8 C7 121.7(8) . .
C9 C8 C7 120.2(8) . .
C8 C9 C3 119.5(7) . .
C8 C9 C10 120.9(8) . .
C3 C9 C10 119.7(7) . .
C13 C10 C11 123.2(8) . .
C13 C10 C9 117.8(8) . .
C11 C10 C9 118.9(8) . .
C12 C11 C10 120.8(8) . .
C11 C12 C4 120.9(8) . .
N2 C13 C10 120.3(8) . .
N2 C14 C8 119.8(8) . .
N3 C15 N2 106.0(7) . .
N3 C16 C17 119.8(9) . .
C16 C17 C18 117.6(8) . .
C16 C17 C21 122.6(9) . .
C18 C17 C21 119.7(9) . .
C17 C18 C24 120.0(8) . .
C17 C18 C19 121.2(8) . .
C24 C18 C19 118.8(7) . .
C20 C19 C18 116.6(8) . .
C20 C19 C25 123.7(9) . .
C18 C19 C25 119.7(8) . .
N3 C20 C19 121.4(9) . .
C22 C21 C17 120.8(9) . .
C21 C22 C23 121.1(9) . .
C29 C23 C24 117.2(8) . .
C29 C23 C22 123.6(8) . .
C24 C23 C22 119.2(8) . .
C23 C24 C18 119.1(7) . .
C23 C24 C27 121.0(8) . .
C18 C24 C27 119.8(7) . .
C26 C25 C19 120.0(9) . .
C25 C26 C27 122.0(9) . .
C28 C27 C26 123.5(8) . .
C28 C27 C24 116.9(7) . .
C26 C27 C24 119.6(8) . .
N4 C28 C27 121.2(7) . .
N4 C29 C23 122.2(8) . .
C31 C30 N5 115.6(11) . .
C30 C31 N6 116.3(11) . .
C33 C32 C37 121.1(14) . .
C32 C33 C34 123.3(15) . .
C32 C33 O1 114.8(12) . .
C34 C33 O1 121.9(14) . .
C33 C34 C35 117.6(14) . .
C36 C35 C34 120.7(14) . .
C37 C36 C35 117.2(15) . .
C37 C36 O4 123.6(14) . .
C35 C36 O4 119.2(14) . .
C36 C37 C32 120.1(14) . .
O1 C38 C39 109.6(13) . .
C38 C39 O2 109.0(11) . .
O2 C40 C41 111.3(11) . .
O3 C41 C40 109.8(13) . .
C43 C42 O4 111.1(13) . .
O5 C43 C42 108.1(13) . .
C45 C44 O5 115.8(14) . 2_656
C44 C45 O6 115.7(19) . .
C47 C46 O6 113.5(11) . .
C46 C47 O7 110.5(11) . .
C49 C48 O7 109.2(11) . .
C48 C49 O8 106.5(15) . .
C51 C50 C55 120.0 . .
C51 C50 O8 126.2(13) . .
C55 C50 O8 113.7(13) . .
C52 C51 C50 120.0 . .
C51 C52 C53 120.0 . .
C52 C53 C54 120.0 . .
C52 C53 O10 130(2) . .
C54 C53 O10 110(2) . .
C53 C54 C55 120.0 . .
C54 C55 C50 120.0 . .
C57 C56 O10 115(3) . .
O9 C57 C56 104(3) . .
C59 C58 O9 104.8(19) . .
O3 C59 C58 148(3) . .
F7 C60 F9 105.0(17) . .
F7 C60 F8 101.6(16) . .
F9 C60 F8 85.7(19) . .
F7 C60 S1 123(2) . .
F9 C60 S1 119.6(12) . .
F8 C60 S1 114.6(14) . .
F10 C61 F12 109(3) . .
F10 C61 F11 97(3) . .
F12 C61 F11 79(3) . .
F10 C61 S2 137(6) . .
F12 C61 S2 109(2) . .
F11 C61 S2 108(3) . .
N9 C67 C66 178.9(19) . .
N10 C69 C68 170(2) . .
C1 N1 C5 121.6(7) . .
C1 N1 Pd1 119.1(5) . .
C5 N1 Pd1 119.3(6) . .
C13 N2 C14 123.0(7) . .
C13 N2 C15 120.8(7) . .
C14 N2 C15 116.2(7) . .
C20 N3 C16 123.3(8) . .
C20 N3 C15 120.1(8) . .
C16 N3 C15 116.6(8) . .
C28 N4 C29 121.5(7) . .
C28 N4 Pd1 121.8(5) . 2_656
C29 N4 Pd1 116.7(5) . 2_656
C30 N5 Pd1 110.7(7) . .
C31 N6 Pd1 106.7(7) . .
C38 O1 C33 115.7(11) . .
C40 O2 C39 116.8(11) . .
C59 O3 C41 120.3(19) . .
C36 O4 C42 117.4(11) . .
C43 O5 C44 112.7(14) . 2_656
C45 O6 C46 111.9(11) . .
C48 O7 C47 112.9(10) . .
C50 O8 C49 114.9(14) . .
C57 O9 C58 116(3) . .
C53 O10 C56 98(3) . .
F3 P1 F5 88.7(5) . .
F3 P1 F6 179.1(4) . .
F5 P1 F6 90.7(4) . .
F3 P1 F4 89.2(3) . .
F5 P1 F4 90.9(4) . .
F6 P1 F4 90.2(3) . .
F3 P1 F2 93.3(5) . .
F5 P1 F2 177.8(4) . .
F6 P1 F2 87.3(4) . .
F4 P1 F2 90.0(4) . .
F3 P1 F1 90.2(3) . .
F5 P1 F1 89.7(4) . .
F6 P1 F1 90.5(3) . .
F4 P1 F1 179.1(4) . .
F2 P1 F1 89.4(4) . .
F14 P2 F13 103.9(9) . .
F14 P2 F15 93.4(13) . .
F13 P2 F15 100.6(12) . .
F14 P2 F18 85.8(16) . .
F13 P2 F18 73.6(15) . .
F15 P2 F18 174(2) . .
F14 P2 F17 155.6(16) . .
F13 P2 F17 92.9(8) . .
F15 P2 F17 100.7(16) . .
F18 P2 F17 82.2(17) . .
F14 P2 F16 93.0(11) . .
F13 P2 F16 160.9(9) . .
F15 P2 F16 86.9(12) . .
F18 P2 F16 99(2) . .
F17 P2 F16 68.3(10) . .
O12 S1 O13 117.6(6) . .
O12 S1 O11 114.6(7) . .
O13 S1 O11 113.0(5) . .
O12 S1 C60 103.2(9) . .
O13 S1 C60 101.3(10) . .
O11 S1 C60 104.6(10) . .
O16 S2 O14 134.5(14) . .
O16 S2 O15 94.2(17) . .
O14 S2 O15 105.0(15) . .
O16 S2 C61 109.8(11) . .
O14 S2 C61 107.3(17) . .
O15 S2 C61 99(3) . .
N5 Pd1 N1 178.3(3) . .
N5 Pd1 N4 92.3(3) . 2_656
N1 Pd1 N4 89.1(3) . 2_656
N5 Pd1 N6 84.0(4) . .
N1 Pd1 N6 94.6(3) . .
N4 Pd1 N6 175.3(3) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.352(10) .
C1 C2 1.394(12) .
C2 C3 1.390(10) .
C2 C6 1.476(11) .
C3 C4 1.414(11) .
C3 C9 1.422(11) .
C4 C5 1.405(12) .
C4 C12 1.423(11) .
C5 N1 1.354(10) .
C6 C7 1.346(12) .
C7 C8 1.428(12) .
C8 C14 1.382(12) .
C8 C9 1.399(11) .
C9 C10 1.444(11) .
C10 C13 1.369(12) .
C10 C11 1.430(12) .
C11 C12 1.363(12) .
C13 N2 1.351(11) .
C14 N2 1.377(11) .
C15 N3 1.502(11) .
C15 N2 1.522(13) .
C16 N3 1.353(12) .
C16 C17 1.371(13) .
C17 C18 1.403(12) .
C17 C21 1.414(13) .
C18 C24 1.427(11) .
C18 C19 1.430(12) .
C19 C20 1.357(12) .
C19 C25 1.452(13) .
C20 N3 1.331(11) .
C21 C22 1.353(13) .
C22 C23 1.427(12) .
C23 C29 1.367(12) .
C23 C24 1.414(11) .
C24 C27 1.426(11) .
C25 C26 1.347(13) .
C26 C27 1.418(12) .
C27 C28 1.398(12) .
C28 N4 1.340(10) .
C29 N4 1.359(11) .
C30 C31 1.316(18) .
C30 N5 1.451(15) .
C31 N6 1.528(15) .
C32 C33 1.302(16) .
C32 C37 1.393(17) .
C33 C34 1.338(18) .
C33 O1 1.413(15) .
C34 C35 1.42(2) .
C35 C36 1.40(2) .
C36 C37 1.378(18) .
C36 O4 1.415(17) .
C38 O1 1.362(15) .
C38 C39 1.44(2) .
C39 O2 1.520(17) .
C40 O2 1.445(16) .
C40 C41 1.45(2) .
C41 O3 1.29(2) .
C42 C43 1.40(2) .
C42 O4 1.460(16) .
C43 O5 1.366(18) .
C44 C45 1.31(2) .
C44 O5 1.380(18) 2_656
C45 O6 1.381(16) .
C46 C47 1.376(17) .
C46 O6 1.470(15) .
C47 O7 1.439(15) .
C48 C49 1.40(2) .
C48 O7 1.421(14) .
C49 O8 1.462(18) .
C50 C51 1.3900 .
C50 C55 1.3900 .
C50 O8 1.407(13) .
C51 C52 1.3900 .
C52 C53 1.3900 .
C53 C54 1.3900 .
C53 O10 1.40(2) .
C54 C55 1.3900 .
C56 C57 1.48(4) .
C56 O10 1.74(6) .
C57 O9 1.29(3) .
C58 C59 1.68(5) .
C58 O9 1.70(4) .
C59 O3 1.24(2) .
C60 F7 1.337(17) .
C60 F9 1.42(2) .
C60 F8 1.53(3) .
C60 S1 1.55(3) .
C61 F10 1.01(4) .
C61 F12 1.51(5) .
C61 F11 1.83(7) .
C61 S2 1.65(3) .
C66 C67 1.42(2) .
C67 N9 1.098(18) .
C68 C69 1.40(2) .
C69 N10 1.19(2) .
N1 Pd1 2.035(7) .
N4 Pd1 2.039(7) 2_656
N5 Pd1 2.011(8) .
N6 Pd1 2.045(8) .
O5 C44 1.380(18) 2_656
O11 S1 1.538(10) .
O12 S1 1.382(9) .
O13 S1 1.416(8) .
O14 S2 1.300(13) .
O15 S2 1.493(17) .
O16 S2 1.142(12) .
F1 P1 1.605(6) .
F2 P1 1.597(7) .
F3 P1 1.579(7) .
F4 P1 1.589(6) .
F5 P1 1.580(7) .
F6 P1 1.587(6) .
F13 P2 1.511(12) .
F14 P2 1.392(12) .
F15 P2 1.522(15) .
F16 P2 1.73(2) .
F17 P2 1.691(18) .
F18 P2 1.537(17) .
Pd1 N4 2.039(7) 2_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 0.5(11) . .
N1 C1 C2 C6 -178.9(7) . .
C1 C2 C3 C4 0.1(11) . .
C6 C2 C3 C4 179.4(7) . .
C1 C2 C3 C9 -178.3(7) . .
C6 C2 C3 C9 1.1(11) . .
C2 C3 C4 C5 -1.0(11) . .
C9 C3 C4 C5 177.4(7) . .
C2 C3 C4 C12 179.1(7) . .
C9 C3 C4 C12 -2.5(11) . .
C3 C4 C5 N1 1.4(11) . .
C12 C4 C5 N1 -178.7(7) . .
C3 C2 C6 C7 -2.2(11) . .
C1 C2 C6 C7 177.1(7) . .
C2 C6 C7 C8 0.9(12) . .
C6 C7 C8 C14 -177.0(7) . .
C6 C7 C8 C9 1.5(12) . .
C14 C8 C9 C3 175.9(7) . .
C7 C8 C9 C3 -2.7(11) . .
C14 C8 C9 C10 -3.1(11) . .
C7 C8 C9 C10 178.4(7) . .
C2 C3 C9 C8 1.3(11) . .
C4 C3 C9 C8 -177.0(7) . .
C2 C3 C9 C10 -179.7(7) . .
C4 C3 C9 C10 1.9(10) . .
C8 C9 C10 C13 0.7(11) . .
C3 C9 C10 C13 -178.3(7) . .
C8 C9 C10 C11 179.8(7) . .
C3 C9 C10 C11 0.8(11) . .
C13 C10 C11 C12 175.9(8) . .
C9 C10 C11 C12 -3.2(12) . .
C10 C11 C12 C4 2.7(13) . .
C5 C4 C12 C11 -179.7(8) . .
C3 C4 C12 C11 0.2(12) . .
C11 C10 C13 N2 -176.6(8) . .
C9 C10 C13 N2 2.5(11) . .
C9 C8 C14 N2 2.4(11) . .
C7 C8 C14 N2 -179.1(7) . .
N3 C16 C17 C18 -0.8(13) . .
N3 C16 C17 C21 -179.0(9) . .
C16 C17 C18 C24 -178.2(8) . .
C21 C17 C18 C24 0.1(13) . .
C16 C17 C18 C19 2.3(13) . .
C21 C17 C18 C19 -179.4(9) . .
C17 C18 C19 C20 -2.1(12) . .
C24 C18 C19 C20 178.4(7) . .
C17 C18 C19 C25 178.8(8) . .
C24 C18 C19 C25 -0.7(12) . .
C18 C19 C20 N3 0.4(12) . .
C25 C19 C20 N3 179.4(8) . .
C16 C17 C21 C22 176.9(10) . .
C18 C17 C21 C22 -1.4(16) . .
C17 C21 C22 C23 1.6(17) . .
C21 C22 C23 C29 -178.5(11) . .
C21 C22 C23 C24 -0.5(16) . .
C29 C23 C24 C18 177.4(8) . .
C22 C23 C24 C18 -0.8(13) . .
C29 C23 C24 C27 -0.8(13) . .
C22 C23 C24 C27 -178.9(8) . .
C17 C18 C24 C23 1.0(11) . .
C19 C18 C24 C23 -179.6(7) . .
C17 C18 C24 C27 179.2(7) . .
C19 C18 C24 C27 -1.3(11) . .
C20 C19 C25 C26 -177.5(9) . .
C18 C19 C25 C26 1.5(14) . .
C19 C25 C26 C27 -0.3(15) . .
C25 C26 C27 C28 179.1(9) . .
C25 C26 C27 C24 -1.7(14) . .
C23 C24 C27 C28 0.0(11) . .
C18 C24 C27 C28 -178.2(7) . .
C23 C24 C27 C26 -179.3(8) . .
C18 C24 C27 C26 2.6(12) . .
C26 C27 C28 N4 180.0(8) . .
C24 C27 C28 N4 0.8(11) . .
C24 C23 C29 N4 0.9(13) . .
C22 C23 C29 N4 179.0(9) . .
N5 C30 C31 N6 -31(2) . .
C37 C32 C33 C34 1.5(18) . .
C37 C32 C33 O1 -179.5(9) . .
C32 C33 C34 C35 -2.9(17) . .
O1 C33 C34 C35 178.1(10) . .
C33 C34 C35 C36 2.5(17) . .
C34 C35 C36 C37 -0.8(17) . .
C34 C35 C36 O4 -179.4(10) . .
C35 C36 C37 C32 -0.7(17) . .
O4 C36 C37 C32 177.9(11) . .
C33 C32 C37 C36 0.4(18) . .
O1 C38 C39 O2 63.0(14) . .
O2 C40 C41 O3 -59(2) . .
O4 C42 C43 O5 66.8(17) . .
O5 C44 C45 O6 -46(3) 2_656 .
O6 C46 C47 O7 58.1(14) . .
O7 C48 C49 O8 69.8(16) . .
C55 C50 C51 C52 0.0 . .
O8 C50 C51 C52 178.1(8) . .
C50 C51 C52 C53 0.0 . .
C51 C52 C53 C54 0.0 . .
C51 C52 C53 O10 -177.9(10) . .
C52 C53 C54 C55 0.0 . .
O10 C53 C54 C55 178.3(8) . .
C53 C54 C55 C50 0.0 . .
C51 C50 C55 C54 0.0 . .
O8 C50 C55 C54 -178.4(7) . .
O10 C56 C57 O9 -74(3) . .
O9 C58 C59 O3 -35(7) . .
C2 C1 N1 C5 -0.1(12) . .
C2 C1 N1 Pd1 177.3(6) . .
C4 C5 N1 C1 -0.8(12) . .
C4 C5 N1 Pd1 -178.3(5) . .
C10 C13 N2 C14 -3.3(12) . .
C10 C13 N2 C15 175.0(7) . .
C8 C14 N2 C13 0.8(11) . .
C8 C14 N2 C15 -177.6(7) . .
N3 C15 N2 C13 -89.0(9) . .
N3 C15 N2 C14 89.5(8) . .
C19 C20 N3 C16 1.2(13) . .
C19 C20 N3 C15 -178.7(8) . .
C17 C16 N3 C20 -1.0(14) . .
C17 C16 N3 C15 178.9(9) . .
N2 C15 N3 C20 82.6(9) . .
N2 C15 N3 C16 -97.2(9) . .
C27 C28 N4 C29 -0.7(12) . .
C27 C28 N4 Pd1 178.0(6) . 2_656
C23 C29 N4 C28 -0.2(13) . .
C23 C29 N4 Pd1 -179.0(7) . 2_656
C31 C30 N5 Pd1 23.7(16) . .
C30 C31 N6 Pd1 21.8(16) . .
C39 C38 O1 C33 -173.0(10) . .
C32 C33 O1 C38 178.0(10) . .
C34 C33 O1 C38 -2.9(15) . .
C41 C40 O2 C39 -175.8(14) . .
C38 C39 O2 C40 160.4(12) . .
C58 C59 O3 C41 -168(5) . .
C40 C41 O3 C59 -126(2) . .
C37 C36 O4 C42 -3.8(17) . .
C35 C36 O4 C42 174.7(11) . .
C43 C42 O4 C36 -173.0(12) . .
C42 C43 O5 C44 168.8(14) . 2_656
C44 C45 O6 C46 -158.2(17) . .
C47 C46 O6 C45 84.1(18) . .
C49 C48 O7 C47 148.2(14) . .
C46 C47 O7 C48 -171.3(11) . .
C51 C50 O8 C49 -0.9(12) . .
C55 C50 O8 C49 177.4(9) . .
C48 C49 O8 C50 -178.9(9) . .
C56 C57 O9 C58 157(3) . .
C59 C58 O9 C57 -151(3) . .
C52 C53 O10 C56 -11.4(15) . .
C54 C53 O10 C56 170.5(11) . .
C57 C56 O10 C53 -169(2) . .
F7 C60 S1 O12 60.6(19) . .
F9 C60 S1 O12 -163.0(16) . .
F8 C60 S1 O12 -63.6(16) . .
F7 C60 S1 O13 -61.6(18) . .
F9 C60 S1 O13 74.7(19) . .
F8 C60 S1 O13 174.2(12) . .
F7 C60 S1 O11 -179.3(16) . .
F9 C60 S1 O11 -43(2) . .
F8 C60 S1 O11 56.6(15) . .
F10 C61 S2 O16 83(6) . .
F12 C61 S2 O16 -126(3) . .
F11 C61 S2 O16 -41(4) . .
F10 C61 S2 O14 -70(5) . .
F12 C61 S2 O14 81(4) . .
F11 C61 S2 O14 166(2) . .
F10 C61 S2 O15 -179(5) . .
F12 C61 S2 O15 -28(3) . .
F11 C61 S2 O15 57(3) . .
C30 N5 Pd1 N1 -45(11) . .
C30 N5 Pd1 N4 169.0(8) . 2_656
C30 N5 Pd1 N6 -8.0(8) . .
C1 N1 Pd1 N5 125(10) . .
C5 N1 Pd1 N5 -58(11) . .
C1 N1 Pd1 N4 -88.6(6) . 2_656
C5 N1 Pd1 N4 88.9(6) . 2_656
C1 N1 Pd1 N6 88.5(6) . .
C5 N1 Pd1 N6 -94.0(6) . .
C31 N6 Pd1 N5 -6.1(8) . .
C31 N6 Pd1 N1 172.9(8) . .
C31 N6 Pd1 N4 -45(4) . 2_656
