#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:12:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179098 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/60/4306055.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_4306055
loop_
_publ_author_name
'Massimo Casanova'
'Ennio Zangrando'
'Elisabetta Iengo'
'Enzo Alessio'
'Maria Teresa Indelli'
'Franco Scandola'
'Michele Orlandi'
_publ_section_title
;
Structural and Photophysical Characterization of Multichromophoric
Pyridylporphyrin-Rhenium(I) Conjugates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10407
_journal_page_last               10418
_journal_paper_doi               10.1021/ic800971e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'C92 H58 N16 O12 Re4 4+, 4(C F3 S O3 1-), 6(C3 H6 O)'
_chemical_formula_sum            'C114 H94 F12 N16 O30 Re4 S4'
_chemical_formula_weight         3269.09
_chemical_name_systematic
;
 tetra[(fac-tricarbonyl-(2,2'bipyridine)-rhenium(I)]-
 -(5-10-15-20-tetra(3'pyridyl)porphyrine)
 tetratriflate acetone solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 108.733(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.479(4)
_cell_length_b                   15.689(3)
_cell_length_c                   22.865(4)
_cell_measurement_temperature    100(2)
_cell_volume                     6957(2)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.70.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'CCD MarResearch'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0000
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36421
_diffrn_reflns_theta_full        30.17
_diffrn_reflns_theta_max         30.17
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    7.330
_exptl_absorpt_correction_T_max  0.1786
_exptl_absorpt_correction_T_min  0.1033
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3204
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         6815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0370P)²+8.3560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                5450
_reflns_number_total             6815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800971e_si_002_4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4306055
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.455879(16) 0.111100(18) 0.362916(15) 0.03054(13) Uani 1 1 d . . .
Re2 Re 0.160362(16) -0.399275(19) -0.203917(16) 0.03328(13) Uani 1 1 d . . .
C1A C 0.3901(4) 0.0201(5) 0.3709(3) 0.0369(19) Uani 1 1 d . . .
C2A C 0.5138(4) 0.0144(5) 0.3460(3) 0.0373(19) Uani 1 1 d . . .
C3A C 0.5077(4) 0.0972(4) 0.4530(4) 0.040(2) Uani 1 1 d . . .
C4A C 0.1942(4) -0.5215(5) -0.1936(4) 0.042(2) Uani 1 1 d . . .
C5A C 0.2335(4) -0.3848(4) -0.2443(4) 0.0384(19) Uani 1 1 d . . .
C6A C 0.0962(4) -0.4322(5) -0.2858(4) 0.043(2) Uani 1 1 d . . .
O1 O 0.3509(3) -0.0353(3) 0.3754(2) 0.0477(14) Uani 1 1 d . . .
O2 O 0.5489(3) -0.0426(3) 0.3387(3) 0.0510(14) Uani 1 1 d . . .
O3 O 0.5357(3) 0.0890(3) 0.5077(3) 0.0517(15) Uani 1 1 d . . .
O4 O 0.2141(3) -0.5939(3) -0.1893(3) 0.0527(15) Uani 1 1 d . . .
O5 O 0.2784(3) -0.3846(3) -0.2687(3) 0.0541(15) Uani 1 1 d . . .
O6 O 0.0596(3) -0.4523(4) -0.3380(3) 0.0603(16) Uani 1 1 d . . .
N1 N 0.5136(3) 0.2238(3) 0.3414(3) 0.0324(15) Uani 1 1 d . . .
N2 N 0.4028(3) 0.2276(3) 0.3853(3) 0.0350(15) Uani 1 1 d . . .
N3 N 0.3927(3) 0.1348(3) 0.2599(3) 0.0308(15) Uani 1 1 d . . .
N4 N 0.1135(3) -0.2670(3) -0.2093(3) 0.0366(15) Uani 1 1 d . . .
C21 C 0.5681(4) 0.2168(4) 0.3157(3) 0.0353(19) Uani 1 1 d . . .
H21 H 0.5879 0.1624 0.3146 0.042 Uiso 1 1 calc R . .
C22 C 0.5941(4) 0.2877(4) 0.2917(4) 0.041(2) Uani 1 1 d . . .
H22 H 0.6305 0.2808 0.2748 0.049 Uiso 1 1 calc R . .
C23 C 0.5641(4) 0.3707(4) 0.2934(4) 0.040(2) Uani 1 1 d . . .
H23 H 0.5808 0.4190 0.2774 0.049 Uiso 1 1 calc R . .
C24 C 0.5087(4) 0.3805(4) 0.3192(3) 0.0365(19) Uani 1 1 d . . .
H24 H 0.4884 0.4347 0.3204 0.044 Uiso 1 1 calc R . .
C25 C 0.4850(3) 0.3059(4) 0.3433(3) 0.0307(18) Uani 1 1 d . . .
C26 C 0.4264(4) 0.3083(4) 0.3730(3) 0.0332(18) Uani 1 1 d . . .
C27 C 0.3983(4) 0.3869(4) 0.3882(3) 0.0351(19) Uani 1 1 d . . .
H27 H 0.4145 0.4403 0.3789 0.042 Uiso 1 1 calc R . .
C28 C 0.3459(4) 0.3838(4) 0.4175(3) 0.0388(19) Uani 1 1 d . . .
H28 H 0.3268 0.4347 0.4275 0.047 Uiso 1 1 calc R . .
C29 C 0.3229(4) 0.3014(5) 0.4316(4) 0.048(2) Uani 1 1 d . . .
H29 H 0.2891 0.2978 0.4519 0.057 Uiso 1 1 calc R . .
C30 C 0.3512(4) 0.2250(5) 0.4145(3) 0.040(2) Uani 1 1 d . . .
H30 H 0.3350 0.1713 0.4231 0.048 Uiso 1 1 calc R . .
C31 C 0.1322(4) -0.1956(5) -0.2386(4) 0.047(2) Uani 1 1 d . . .
H31 H 0.1693 -0.2015 -0.2548 0.056 Uiso 1 1 calc R . .
C32 C 0.0980(5) -0.1161(5) -0.2447(4) 0.060(3) Uani 1 1 d . . .
H32 H 0.1121 -0.0695 -0.2644 0.073 Uiso 1 1 calc R . .
C33 C 0.0413(5) -0.1072(5) -0.2204(5) 0.067(3) Uani 1 1 d . . .
H33 H 0.0168 -0.0548 -0.2251 0.081 Uiso 1 1 calc R . .
C34 C 0.0220(5) -0.1775(5) -0.1893(5) 0.064(3) Uani 1 1 d . . .
H34 H -0.0147 -0.1723 -0.1725 0.077 Uiso 1 1 calc R . .
C35 C 0.0600(4) -0.2567(5) -0.1839(4) 0.045(2) Uani 1 1 d . . .
C36 C 0.0414(4) -0.3374(5) -0.1519(4) 0.043(2) Uani 1 1 d . . .
C37 C -0.0109(4) -0.3381(5) -0.1220(4) 0.054(2) Uani 1 1 d . . .
H37 H -0.0351 -0.2874 -0.1194 0.065 Uiso 1 1 calc R . .
C38 C -0.0259(4) -0.4163(5) -0.0962(4) 0.060(3) Uani 1 1 d . . .
H38 H -0.0603 -0.4181 -0.0766 0.072 Uiso 1 1 calc R . .
C39 C 0.0124(4) -0.4921(5) -0.1006(4) 0.050(2) Uani 1 1 d . . .
H39 H 0.0026 -0.5448 -0.0847 0.060 Uiso 1 1 calc R . .
C40 C 0.0649(4) -0.4872(5) -0.1289(4) 0.043(2) Uani 1 1 d . . .
H40 H 0.0907 -0.5370 -0.1303 0.051 Uiso 1 1 calc R . .
N10 N 0.5188(3) 0.1164(3) 0.0589(3) 0.0292(14) Uani 1 1 d . . .
H10 H 0.5148 0.0693 0.0371 0.035 Uiso 1 1 calc R . .
N20 N 0.4145(3) -0.0364(3) 0.0266(2) 0.0271(14) Uani 1 1 d . . .
C1 C 0.5705(3) 0.1803(4) 0.0647(3) 0.0270(17) Uani 1 1 d . . .
C2 C 0.5573(3) 0.2482(4) 0.1046(3) 0.0299(17) Uani 1 1 d . . .
H2 H 0.5828 0.2995 0.1160 0.036 Uiso 1 1 calc R . .
C3 C 0.5004(4) 0.2234(4) 0.1226(3) 0.0287(17) Uani 1 1 d . . .
H3 H 0.4817 0.2549 0.1489 0.034 Uiso 1 1 calc R . .
C4 C 0.4744(3) 0.1403(4) 0.0937(3) 0.0263(17) Uani 1 1 d . . .
C5 C 0.4161(3) 0.0913(4) 0.0982(3) 0.0273(17) Uani 1 1 d . . .
C6 C 0.3872(4) 0.0109(4) 0.0665(3) 0.0301(18) Uani 1 1 d . . .
C7 C 0.3225(3) -0.0322(4) 0.0719(3) 0.0345(18) Uani 1 1 d . . .
H7 H 0.2954 -0.0130 0.0960 0.041 Uiso 1 1 calc R . .
C8 C 0.3107(3) -0.1047(4) 0.0350(3) 0.0360(19) Uani 1 1 d . . .
H8 H 0.2738 -0.1440 0.0286 0.043 Uiso 1 1 calc R . .
C9 C 0.3692(3) -0.1085(4) 0.0066(3) 0.0292(17) Uani 1 1 d . . .
C10 C 0.3763(3) -0.1773(4) -0.0348(3) 0.0290(17) Uani 1 1 d . . .
N5 N 0.0799(3) -0.4116(4) -0.1549(3) 0.0384(16) Uani 1 1 d . . .
N6 N 0.2341(3) -0.3533(3) -0.1086(3) 0.0321(14) Uani 1 1 d . . .
C51 C 0.3821(3) 0.1250(4) 0.1465(3) 0.0295(18) Uani 1 1 d . . .
C52 C 0.4194(4) 0.1141(4) 0.2113(4) 0.0310(18) Uani 1 1 d . . .
H52 H 0.4649 0.0917 0.2223 0.037 Uiso 1 1 calc R . .
C53 C 0.3258(4) 0.1685(4) 0.2432(3) 0.0330(18) Uani 1 1 d . . .
H53 H 0.3068 0.1824 0.2748 0.040 Uiso 1 1 calc R . .
C54 C 0.2846(4) 0.1829(4) 0.1791(4) 0.0355(19) Uani 1 1 d . . .
H54 H 0.2395 0.2061 0.1689 0.043 Uiso 1 1 calc R . .
C55 C 0.3138(4) 0.1610(4) 0.1311(3) 0.0338(19) Uani 1 1 d . . .
H55 H 0.2877 0.1704 0.0891 0.041 Uiso 1 1 calc R . .
C56 C 0.3266(3) -0.2563(4) -0.0428(3) 0.0288(17) Uani 1 1 d . . .
C57 C 0.2778(3) -0.2797(4) -0.1012(3) 0.0326(18) Uani 1 1 d . . .
H57 H 0.2742 -0.2452 -0.1363 0.039 Uiso 1 1 calc R . .
C58 C 0.2405(4) -0.4031(4) -0.0557(4) 0.0359(19) Uani 1 1 d . . .
H58 H 0.2126 -0.4525 -0.0601 0.043 Uiso 1 1 calc R . .
C59 C 0.2868(4) -0.3828(4) 0.0039(4) 0.040(2) Uani 1 1 d . . .
H59 H 0.2889 -0.4173 0.0386 0.048 Uiso 1 1 calc R . .
C60 C 0.3300(4) -0.3092(4) 0.0104(4) 0.0372(19) Uani 1 1 d . . .
H60 H 0.3612 -0.2947 0.0498 0.045 Uiso 1 1 calc R . .
S1 S 0.84307(12) 0.80723(14) 0.52364(11) 0.0633(7) Uani 1 1 d . . .
S2 S 0.67786(10) 0.07963(11) 0.22534(10) 0.0420(5) Uani 1 1 d . . .
O11 O 0.8173(3) 0.7165(3) 0.5062(3) 0.0605(16) Uani 1 1 d . . .
O12 O 0.9172(3) 0.8225(4) 0.5294(3) 0.0723(18) Uani 1 1 d . . .
O13 O 0.8181(4) 0.8474(5) 0.5737(3) 0.108(3) Uani 1 1 d . . .
O21 O 0.7065(3) 0.1639(3) 0.2540(3) 0.0625(17) Uani 1 1 d . . .
O22 O 0.6019(2) 0.0663(3) 0.2145(2) 0.0424(13) Uani 1 1 d . . .
O23 O 0.7034(3) 0.0520(3) 0.1738(2) 0.0527(15) Uani 1 1 d . . .
C17 C 0.7944(5) 0.8721(5) 0.4581(5) 0.067(3) Uani 1 1 d . . .
C18 C 0.7188(4) -0.0007(6) 0.2883(4) 0.054(2) Uani 1 1 d . . .
F1 F 0.8062(3) 0.8457(3) 0.4018(3) 0.0792(16) Uani 1 1 d . . .
F2 F 0.7226(3) 0.8664(4) 0.4431(3) 0.0977(19) Uani 1 1 d . . .
F3 F 0.8132(3) 0.9579(3) 0.4636(3) 0.0764(15) Uani 1 1 d . . .
F4 F 0.6958(2) -0.0832(3) 0.2722(2) 0.0675(14) Uani 1 1 d . . .
F5 F 0.7907(2) -0.0001(3) 0.3062(2) 0.0700(14) Uani 1 1 d . . .
F6 F 0.7013(3) 0.0200(4) 0.3420(2) 0.0793(16) Uani 1 1 d . . .
O7 O 0.8473(3) 0.2651(4) 0.5072(3) 0.0766(19) Uani 1 1 d . . .
O8 O 0.8940(4) 0.6529(5) 0.3791(4) 0.089(2) Uani 1 1 d . . .
O9 O 0.9424(4) 0.8939(4) 0.2238(4) 0.089(2) Uani 1 1 d . . .
C61 C 0.8884(5) 0.1512(6) 0.4523(6) 0.088(3) Uani 1 1 d . . .
H61A H 0.9060 0.1256 0.4935 0.133 Uiso 1 1 calc R . .
H61B H 0.9266 0.1602 0.4360 0.133 Uiso 1 1 calc R . .
H61C H 0.8544 0.1130 0.4248 0.133 Uiso 1 1 calc R . .
C62 C 0.8540(4) 0.2376(6) 0.4566(5) 0.062(3) Uani 1 1 d . . .
C63 C 0.8242(6) 0.2879(7) 0.3958(5) 0.088(3) Uani 1 1 d . . .
H63A H 0.8038 0.3412 0.4040 0.132 Uiso 1 1 calc R . .
H63B H 0.7887 0.2537 0.3662 0.132 Uiso 1 1 calc R . .
H63C H 0.8612 0.3008 0.3786 0.132 Uiso 1 1 calc R . .
C64 C 0.8599(5) 0.5383(6) 0.4366(5) 0.078(3) Uani 1 1 d . . .
H64A H 0.8207 0.5344 0.3985 0.117 Uiso 1 1 calc R . .
H64B H 0.8433 0.5514 0.4713 0.117 Uiso 1 1 calc R . .
H64C H 0.8847 0.4838 0.4442 0.117 Uiso 1 1 calc R . .
C65 C 0.9090(5) 0.6095(6) 0.4300(6) 0.076(3) Uani 1 1 d . . .
C66 C 0.9754(6) 0.6282(7) 0.4834(6) 0.114(4) Uani 1 1 d . . .
H66A H 1.0000 0.6756 0.4721 0.171 Uiso 1 1 calc R . .
H66B H 1.0049 0.5774 0.4919 0.171 Uiso 1 1 calc R . .
H66C H 0.9637 0.6434 0.5204 0.171 Uiso 1 1 calc R . .
C67 C 0.8354(5) 0.8139(7) 0.2101(5) 0.091(3) Uani 1 1 d . . .
H67A H 0.8633 0.7843 0.2476 0.136 Uiso 1 1 calc R . .
H67B H 0.8173 0.7724 0.1768 0.136 Uiso 1 1 calc R . .
H67C H 0.7969 0.8430 0.2183 0.136 Uiso 1 1 calc R . .
C68 C 0.8813(6) 0.8812(6) 0.1903(5) 0.076(3) Uani 1 1 d . . .
C69 C 0.8467(6) 0.9357(7) 0.1300(5) 0.089(3) Uani 1 1 d . . .
H69A H 0.8809 0.9747 0.1232 0.134 Uiso 1 1 calc R . .
H69B H 0.8082 0.9687 0.1351 0.134 Uiso 1 1 calc R . .
H69C H 0.8296 0.8975 0.0944 0.134 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0074 0.0035 '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 0.0136 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0227 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -7.2020 10.7760 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.2073 0.2439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0347 0.0215 '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
_geom_angle_publ_flag
C3A Re1 C1A 88.8(3) . . ?
C3A Re1 C2A 88.0(3) . . ?
C1A Re1 C2A 86.3(3) . . ?
C3A Re1 N1 99.6(2) . . ?
C1A Re1 N1 169.9(2) . . ?
C2A Re1 N1 99.4(2) . . ?
C3A Re1 N2 89.4(3) . . ?
C1A Re1 N2 99.7(2) . . ?
C2A Re1 N2 173.4(2) . . ?
N1 Re1 N2 75.0(2) . . ?
C3A Re1 N3 176.4(3) . . ?
C1A Re1 N3 91.9(2) . . ?
C2A Re1 N3 95.5(2) . . ?
N1 Re1 N3 79.32(19) . . ?
N2 Re1 N3 87.0(2) . . ?
C6A Re2 C5A 87.8(3) . . ?
C6A Re2 C4A 87.8(3) . . ?
C5A Re2 C4A 83.3(3) . . ?
C6A Re2 N4 92.6(3) . . ?
C5A Re2 N4 103.7(2) . . ?
C4A Re2 N4 173.0(2) . . ?
C6A Re2 N5 94.5(3) . . ?
C5A Re2 N5 177.5(2) . . ?
C4A Re2 N5 97.9(2) . . ?
N4 Re2 N5 75.2(2) . . ?
C6A Re2 N6 177.1(3) . . ?
C5A Re2 N6 92.3(2) . . ?
C4A Re2 N6 95.1(3) . . ?
N4 Re2 N6 84.5(2) . . ?
N5 Re2 N6 85.4(2) . . ?
O1 C1A Re1 179.3(6) . . ?
O2 C2A Re1 177.3(6) . . ?
O3 C3A Re1 176.7(7) . . ?
O4 C4A Re2 178.1(6) . . ?
O5 C5A Re2 173.7(5) . . ?
O6 C6A Re2 176.2(6) . . ?
C25 N1 C21 117.8(5) . . ?
C25 N1 Re1 116.9(4) . . ?
C21 N1 Re1 124.3(4) . . ?
C26 N2 C30 118.2(5) . . ?
C26 N2 Re1 117.2(4) . . ?
C30 N2 Re1 124.5(4) . . ?
C53 N3 C52 117.4(6) . . ?
C53 N3 Re1 120.9(5) . . ?
C52 N3 Re1 121.7(4) . . ?
C35 N4 C31 118.0(6) . . ?
C35 N4 Re2 117.1(4) . . ?
C31 N4 Re2 124.9(5) . . ?
C22 C21 N1 122.9(6) . . ?
C21 C22 C23 118.7(6) . . ?
C24 C23 C22 120.2(6) . . ?
C25 C24 C23 118.2(6) . . ?
N1 C25 C24 122.2(6) . . ?
N1 C25 C26 114.7(5) . . ?
C24 C25 C26 123.1(6) . . ?
N2 C26 C27 121.8(6) . . ?
N2 C26 C25 115.1(6) . . ?
C27 C26 C25 123.1(6) . . ?
C28 C27 C26 119.7(6) . . ?
C27 C28 C29 118.7(6) . . ?
C30 C29 C28 119.7(7) . . ?
N2 C30 C29 122.0(6) . . ?
C32 C31 N4 122.8(7) . . ?
C31 C32 C33 118.7(7) . . ?
C34 C33 C32 119.9(7) . . ?
C33 C34 C35 118.3(7) . . ?
N4 C35 C34 122.2(6) . . ?
N4 C35 C36 115.9(6) . . ?
C34 C35 C36 121.8(7) . . ?
N5 C36 C37 121.7(7) . . ?
N5 C36 C35 114.6(6) . . ?
C37 C36 C35 123.7(7) . . ?
C38 C37 C36 119.3(7) . . ?
C37 C38 C39 118.8(7) . . ?
C40 C39 C38 119.5(7) . . ?
N5 C40 C39 122.5(7) . . ?
C1 N10 C4 110.3(5) . . ?
C6 N20 C9 105.5(5) . . ?
N10 C1 C10 125.1(5) . 3_655 ?
N10 C1 C2 106.5(5) . . ?
C10 C1 C2 128.4(6) 3_655 . ?
C3 C2 C1 108.2(5) . . ?
C2 C3 C4 109.0(5) . . ?
N10 C4 C5 125.6(6) . . ?
N10 C4 C3 106.0(5) . . ?
C5 C4 C3 128.4(6) . . ?
C4 C5 C6 128.8(6) . . ?
C4 C5 C51 115.5(5) . . ?
C6 C5 C51 115.6(5) . . ?
N20 C6 C5 125.5(6) . . ?
N20 C6 C7 110.5(5) . . ?
C5 C6 C7 124.0(6) . . ?
C8 C7 C6 107.5(6) . . ?
C7 C8 C9 106.3(6) . . ?
N20 C9 C10 126.3(6) . . ?
N20 C9 C8 110.2(5) . . ?
C10 C9 C8 123.5(6) . . ?
C1 C10 C9 124.5(6) 3_655 . ?
C1 C10 C56 118.1(5) 3_655 . ?
C9 C10 C56 117.2(6) . . ?
C40 N5 C36 118.1(6) . . ?
C40 N5 Re2 124.8(5) . . ?
C36 N5 Re2 117.1(4) . . ?
C58 N6 C57 117.5(6) . . ?
C58 N6 Re2 119.0(4) . . ?
C57 N6 Re2 123.4(5) . . ?
C52 C51 C55 116.7(6) . . ?
C52 C51 C5 118.2(6) . . ?
C55 C51 C5 124.9(6) . . ?
N3 C52 C51 124.3(6) . . ?
N3 C53 C54 122.2(6) . . ?
C55 C54 C53 118.6(6) . . ?
C51 C55 C54 120.8(6) . . ?
C57 C56 C60 117.7(6) . . ?
C57 C56 C10 122.7(6) . . ?
C60 C56 C10 119.6(6) . . ?
C56 C57 N6 122.4(6) . . ?
N6 C58 C59 123.2(6) . . ?
C58 C59 C60 118.6(7) . . ?
C59 C60 C56 120.7(7) . . ?
O12 S1 O11 115.3(4) . . ?
O12 S1 O13 116.1(4) . . ?
O11 S1 O13 114.2(3) . . ?
O12 S1 C17 104.7(4) . . ?
O11 S1 C17 104.7(4) . . ?
O13 S1 C17 99.2(5) . . ?
O23 S2 O21 114.3(3) . . ?
O23 S2 O22 115.6(3) . . ?
O21 S2 O22 115.4(3) . . ?
O23 S2 C18 102.9(3) . . ?
O21 S2 C18 103.7(4) . . ?
O22 S2 C18 102.4(3) . . ?
F3 C17 F2 108.8(7) . . ?
F3 C17 F1 103.7(7) . . ?
F2 C17 F1 103.1(8) . . ?
F3 C17 S1 113.8(7) . . ?
F2 C17 S1 114.7(7) . . ?
F1 C17 S1 111.6(6) . . ?
F4 C18 F5 108.7(7) . . ?
F4 C18 F6 106.5(6) . . ?
F5 C18 F6 106.3(7) . . ?
F4 C18 S2 112.9(6) . . ?
F5 C18 S2 112.7(5) . . ?
F6 C18 S2 109.4(6) . . ?
O7 C62 C63 121.0(8) . . ?
O7 C62 C61 122.3(9) . . ?
C63 C62 C61 116.6(9) . . ?
O8 C65 C66 120.5(10) . . ?
O8 C65 C64 119.5(9) . . ?
C66 C65 C64 119.9(11) . . ?
O9 C68 C67 120.1(10) . . ?
O9 C68 C69 121.6(9) . . ?
C67 C68 C69 118.1(9) . . ?
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
Re1 C3A 2.003(9) . ?
Re1 C1A 2.010(8) . ?
Re1 C2A 2.037(9) . ?
Re1 N1 2.266(5) . ?
Re1 N2 2.268(5) . ?
Re1 N3 2.324(6) . ?
Re2 C6A 1.979(9) . ?
Re2 C5A 2.010(9) . ?
Re2 C4A 2.027(8) . ?
Re2 N4 2.273(6) . ?
Re2 N5 2.278(5) . ?
Re2 N6 2.331(6) . ?
C1A O1 1.211(8) . ?
C2A O2 1.194(8) . ?
C3A O3 1.203(9) . ?
C4A O4 1.200(8) . ?
C5A O5 1.218(9) . ?
C6A O6 1.230(9) . ?
N1 C25 1.421(8) . ?
N1 C21 1.422(8) . ?
N2 C26 1.416(9) . ?
N2 C30 1.419(9) . ?
N3 C53 1.401(9) . ?
N3 C52 1.426(9) . ?
N4 C35 1.404(9) . ?
N4 C31 1.420(9) . ?
C21 C22 1.418(10) . ?
C22 C23 1.446(10) . ?
C23 C24 1.446(10) . ?
C24 C25 1.442(9) . ?
C25 C26 1.559(10) . ?
C26 C27 1.450(9) . ?
C27 C28 1.436(10) . ?
C28 C29 1.446(10) . ?
C29 C30 1.439(10) . ?
C31 C32 1.415(11) . ?
C32 C33 1.447(12) . ?
C33 C34 1.436(11) . ?
C34 C35 1.450(11) . ?
C35 C36 1.570(10) . ?
C36 N5 1.419(9) . ?
C36 C37 1.444(10) . ?
C37 C38 1.436(11) . ?
C38 C39 1.445(11) . ?
C39 C40 1.424(10) . ?
C40 N5 1.405(9) . ?
N10 C1 1.432(8) . ?
N10 C4 1.437(8) . ?
N20 C6 1.423(8) . ?
N20 C9 1.442(8) . ?
C1 C10 1.461(9) 3_655 ?
C1 C2 1.482(9) . ?
C2 C3 1.410(9) . ?
C3 C4 1.480(9) . ?
C4 C5 1.452(9) . ?
C5 C6 1.480(9) . ?
C5 C51 1.574(10) . ?
C6 C7 1.526(9) . ?
C7 C8 1.390(9) . ?
C8 C9 1.535(9) . ?
C9 C10 1.473(9) . ?
C10 C1 1.461(9) 3_655 ?
C10 C56 1.577(9) . ?
N6 C58 1.410(9) . ?
N6 C57 1.437(8) . ?
C51 C52 1.442(10) . ?
C51 C55 1.444(9) . ?
C53 C54 1.456(10) . ?
C54 C55 1.448(10) . ?
C56 C57 1.436(10) . ?
C56 C60 1.455(10) . ?
C58 C59 1.424(11) . ?
C59 C60 1.434(10) . ?
S1 O12 1.501(6) . ?
S1 O11 1.526(6) . ?
S1 O13 1.532(6) . ?
S1 C17 1.822(11) . ?
S2 O23 1.499(5) . ?
S2 O21 1.508(5) . ?
S2 O22 1.508(5) . ?
S2 C18 1.894(9) . ?
C17 F3 1.394(9) . ?
C17 F2 1.402(10) . ?
C17 F1 1.444(10) . ?
C18 F4 1.388(10) . ?
C18 F5 1.396(9) . ?
C18 F6 1.423(9) . ?
O7 C62 1.283(10) . ?
O8 C65 1.298(12) . ?
O9 C68 1.256(12) . ?
C61 C62 1.546(13) . ?
C62 C63 1.544(13) . ?
C64 C65 1.543(13) . ?
C65 C66 1.536(15) . ?
C67 C68 1.574(13) . ?
C68 C69 1.584(14) . ?
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
C3A Re1 C1A O1 -102(63) . . . . ?
C2A Re1 C1A O1 -14(63) . . . . ?
N1 Re1 C1A O1 111(63) . . . . ?
N2 Re1 C1A O1 168(100) . . . . ?
N3 Re1 C1A O1 81(63) . . . . ?
C3A Re1 C2A O2 4(12) . . . . ?
C1A Re1 C2A O2 -84(13) . . . . ?
N1 Re1 C2A O2 104(13) . . . . ?
N2 Re1 C2A O2 72(13) . . . . ?
N3 Re1 C2A O2 -176(100) . . . . ?
C1A Re1 C3A O3 -47(10) . . . . ?
C2A Re1 C3A O3 -133(10) . . . . ?
N1 Re1 C3A O3 128(10) . . . . ?
N2 Re1 C3A O3 53(10) . . . . ?
N3 Re1 C3A O3 55(12) . . . . ?
C6A Re2 C4A O4 41(19) . . . . ?
C5A Re2 C4A O4 -47(19) . . . . ?
N4 Re2 C4A O4 135(18) . . . . ?
N5 Re2 C4A O4 135(19) . . . . ?
N6 Re2 C4A O4 -139(19) . . . . ?
C6A Re2 C5A O5 -77(6) . . . . ?
C4A Re2 C5A O5 11(6) . . . . ?
N4 Re2 C5A O5 -170(6) . . . . ?
N5 Re2 C5A O5 128(6) . . . . ?
N6 Re2 C5A O5 106(6) . . . . ?
C5A Re2 C6A O6 5(10) . . . . ?
C4A Re2 C6A O6 -78(10) . . . . ?
N4 Re2 C6A O6 109(10) . . . . ?
N5 Re2 C6A O6 -176(100) . . . . ?
N6 Re2 C6A O6 96(11) . . . . ?
C3A Re1 N1 C25 -95.1(5) . . . . ?
C1A Re1 N1 C25 51.0(16) . . . . ?
C2A Re1 N1 C25 175.3(5) . . . . ?
N2 Re1 N1 C25 -8.4(5) . . . . ?
N3 Re1 N1 C25 81.4(5) . . . . ?
C3A Re1 N1 C21 96.7(5) . . . . ?
C1A Re1 N1 C21 -117.2(14) . . . . ?
C2A Re1 N1 C21 7.1(5) . . . . ?
N2 Re1 N1 C21 -176.5(5) . . . . ?
N3 Re1 N1 C21 -86.8(5) . . . . ?
C3A Re1 N2 C26 103.2(5) . . . . ?
C1A Re1 N2 C26 -168.1(5) . . . . ?
C2A Re1 N2 C26 36(2) . . . . ?
N1 Re1 N2 C26 3.1(5) . . . . ?
N3 Re1 N2 C26 -76.7(5) . . . . ?
C3A Re1 N2 C30 -72.1(6) . . . . ?
C1A Re1 N2 C30 16.6(6) . . . . ?
C2A Re1 N2 C30 -139(2) . . . . ?
N1 Re1 N2 C30 -172.2(6) . . . . ?
N3 Re1 N2 C30 108.0(5) . . . . ?
C3A Re1 N3 C53 -36(4) . . . . ?
C1A Re1 N3 C53 66.0(5) . . . . ?
C2A Re1 N3 C53 152.5(5) . . . . ?
N1 Re1 N3 C53 -108.9(5) . . . . ?
N2 Re1 N3 C53 -33.6(4) . . . . ?
C3A Re1 N3 C52 146(4) . . . . ?
C1A Re1 N3 C52 -112.7(5) . . . . ?
C2A Re1 N3 C52 -26.2(5) . . . . ?
N1 Re1 N3 C52 72.4(4) . . . . ?
N2 Re1 N3 C52 147.7(4) . . . . ?
C6A Re2 N4 C35 92.0(5) . . . . ?
C5A Re2 N4 C35 -179.7(5) . . . . ?
C4A Re2 N4 C35 -1(2) . . . . ?
N5 Re2 N4 C35 -1.9(5) . . . . ?
N6 Re2 N4 C35 -88.7(5) . . . . ?
C6A Re2 N4 C31 -85.2(6) . . . . ?
C5A Re2 N4 C31 3.2(6) . . . . ?
C4A Re2 N4 C31 -179(23) . . . . ?
N5 Re2 N4 C31 -179.1(6) . . . . ?
N6 Re2 N4 C31 94.2(6) . . . . ?
C25 N1 C21 C22 -0.7(10) . . . . ?
Re1 N1 C21 C22 167.4(5) . . . . ?
N1 C21 C22 C23 0.1(11) . . . . ?
C21 C22 C23 C24 0.1(11) . . . . ?
C22 C23 C24 C25 0.3(11) . . . . ?
C21 N1 C25 C24 1.1(10) . . . . ?
Re1 N1 C25 C24 -167.8(5) . . . . ?
C21 N1 C25 C26 -179.0(5) . . . . ?
Re1 N1 C25 C26 12.0(7) . . . . ?
C23 C24 C25 N1 -1.0(10) . . . . ?
C23 C24 C25 C26 179.2(6) . . . . ?
C30 N2 C26 C27 -1.5(10) . . . . ?
Re1 N2 C26 C27 -177.1(5) . . . . ?
C30 N2 C26 C25 177.7(6) . . . . ?
Re1 N2 C26 C25 2.1(7) . . . . ?
N1 C25 C26 N2 -9.2(9) . . . . ?
C24 C25 C26 N2 170.6(6) . . . . ?
N1 C25 C26 C27 169.9(6) . . . . ?
C24 C25 C26 C27 -10.2(10) . . . . ?
N2 C26 C27 C28 1.2(10) . . . . ?
C25 C26 C27 C28 -177.9(6) . . . . ?
C26 C27 C28 C29 0.4(11) . . . . ?
C27 C28 C29 C30 -1.6(11) . . . . ?
C26 N2 C30 C29 0.2(10) . . . . ?
Re1 N2 C30 C29 175.5(6) . . . . ?
C28 C29 C30 N2 1.4(12) . . . . ?
C35 N4 C31 C32 -1.9(11) . . . . ?
Re2 N4 C31 C32 175.2(6) . . . . ?
N4 C31 C32 C33 -0.3(13) . . . . ?
C31 C32 C33 C34 1.8(14) . . . . ?
C32 C33 C34 C35 -0.9(14) . . . . ?
C31 N4 C35 C34 2.8(11) . . . . ?
Re2 N4 C35 C34 -174.5(7) . . . . ?
C31 N4 C35 C36 -179.8(7) . . . . ?
Re2 N4 C35 C36 2.9(8) . . . . ?
C33 C34 C35 N4 -1.4(14) . . . . ?
C33 C34 C35 C36 -178.7(8) . . . . ?
N4 C35 C36 N5 -2.3(10) . . . . ?
C34 C35 C36 N5 175.1(8) . . . . ?
N4 C35 C36 C37 178.4(7) . . . . ?
C34 C35 C36 C37 -4.2(12) . . . . ?
N5 C36 C37 C38 -1.8(12) . . . . ?
C35 C36 C37 C38 177.4(8) . . . . ?
C36 C37 C38 C39 0.5(13) . . . . ?
C37 C38 C39 C40 1.5(13) . . . . ?
C38 C39 C40 N5 -2.1(12) . . . . ?
C4 N10 C1 C10 -179.2(6) . . . 3_655 ?
C4 N10 C1 C2 -0.7(7) . . . . ?
N10 C1 C2 C3 1.3(7) . . . . ?
C10 C1 C2 C3 179.7(6) 3_655 . . . ?
C1 C2 C3 C4 -1.3(7) . . . . ?
C1 N10 C4 C5 179.5(6) . . . . ?
C1 N10 C4 C3 -0.1(7) . . . . ?
C2 C3 C4 N10 0.9(7) . . . . ?
C2 C3 C4 C5 -178.7(6) . . . . ?
N10 C4 C5 C6 -3.7(11) . . . . ?
C3 C4 C5 C6 175.8(6) . . . . ?
N10 C4 C5 C51 171.9(6) . . . . ?
C3 C4 C5 C51 -8.7(10) . . . . ?
C9 N20 C6 C5 -179.4(6) . . . . ?
C9 N20 C6 C7 0.0(7) . . . . ?
C4 C5 C6 N20 3.2(11) . . . . ?
C51 C5 C6 N20 -172.3(6) . . . . ?
C4 C5 C6 C7 -176.1(6) . . . . ?
C51 C5 C6 C7 8.4(9) . . . . ?
N20 C6 C7 C8 -0.6(8) . . . . ?
C5 C6 C7 C8 178.8(6) . . . . ?
C6 C7 C8 C9 0.9(8) . . . . ?
C6 N20 C9 C10 -179.0(6) . . . . ?
C6 N20 C9 C8 0.6(7) . . . . ?
C7 C8 C9 N20 -0.9(8) . . . . ?
C7 C8 C9 C10 178.7(6) . . . . ?
N20 C9 C10 C1 -3.5(10) . . . 3_655 ?
C8 C9 C10 C1 177.0(6) . . . 3_655 ?
N20 C9 C10 C56 171.5(6) . . . . ?
C8 C9 C10 C56 -8.1(9) . . . . ?
C39 C40 N5 C36 0.8(11) . . . . ?
C39 C40 N5 Re2 -177.8(6) . . . . ?
C37 C36 N5 C40 1.2(11) . . . . ?
C35 C36 N5 C40 -178.1(6) . . . . ?
C37 C36 N5 Re2 179.9(6) . . . . ?
C35 C36 N5 Re2 0.6(8) . . . . ?
C6A Re2 N5 C40 87.7(6) . . . . ?
C5A Re2 N5 C40 -118(6) . . . . ?
C4A Re2 N5 C40 -0.7(6) . . . . ?
N4 Re2 N5 C40 179.2(6) . . . . ?
N6 Re2 N5 C40 -95.3(6) . . . . ?
C6A Re2 N5 C36 -90.9(6) . . . . ?
C5A Re2 N5 C36 64(6) . . . . ?
C4A Re2 N5 C36 -179.3(5) . . . . ?
N4 Re2 N5 C36 0.6(5) . . . . ?
N6 Re2 N5 C36 86.1(5) . . . . ?
C6A Re2 N6 C58 139(5) . . . . ?
C5A Re2 N6 C58 -129.8(5) . . . . ?
C4A Re2 N6 C58 -46.4(5) . . . . ?
N4 Re2 N6 C58 126.6(5) . . . . ?
N5 Re2 N6 C58 51.1(5) . . . . ?
C6A Re2 N6 C57 -46(5) . . . . ?
C5A Re2 N6 C57 45.4(5) . . . . ?
C4A Re2 N6 C57 128.8(5) . . . . ?
N4 Re2 N6 C57 -58.2(5) . . . . ?
N5 Re2 N6 C57 -133.7(5) . . . . ?
C4 C5 C51 C52 -72.0(7) . . . . ?
C6 C5 C51 C52 104.1(7) . . . . ?
C4 C5 C51 C55 112.6(7) . . . . ?
C6 C5 C51 C55 -71.2(8) . . . . ?
C53 N3 C52 C51 -0.5(8) . . . . ?
Re1 N3 C52 C51 178.2(4) . . . . ?
C55 C51 C52 N3 1.3(9) . . . . ?
C5 C51 C52 N3 -174.4(5) . . . . ?
C52 N3 C53 C54 -0.4(8) . . . . ?
Re1 N3 C53 C54 -179.1(5) . . . . ?
N3 C53 C54 C55 0.4(9) . . . . ?
C52 C51 C55 C54 -1.3(9) . . . . ?
C5 C51 C55 C54 174.2(6) . . . . ?
C53 C54 C55 C51 0.5(9) . . . . ?
C1 C10 C56 C57 -66.5(8) 3_655 . . . ?
C9 C10 C56 C57 118.2(7) . . . . ?
C1 C10 C56 C60 112.9(7) 3_655 . . . ?
C9 C10 C56 C60 -62.4(8) . . . . ?
C60 C56 C57 N6 -1.3(9) . . . . ?
C10 C56 C57 N6 178.1(5) . . . . ?
C58 N6 C57 C56 0.2(9) . . . . ?
Re2 N6 C57 C56 -175.1(4) . . . . ?
C57 N6 C58 C59 1.2(9) . . . . ?
Re2 N6 C58 C59 176.6(5) . . . . ?
N6 C58 C59 C60 -1.2(10) . . . . ?
C58 C59 C60 C56 0.0(10) . . . . ?
C57 C56 C60 C59 1.2(9) . . . . ?
C10 C56 C60 C59 -178.2(6) . . . . ?
O12 S1 C17 F3 -55.1(7) . . . . ?
O11 S1 C17 F3 -176.8(6) . . . . ?
O13 S1 C17 F3 65.1(7) . . . . ?
O12 S1 C17 F2 178.7(6) . . . . ?
O11 S1 C17 F2 57.1(7) . . . . ?
O13 S1 C17 F2 -61.1(7) . . . . ?
O12 S1 C17 F1 61.8(6) . . . . ?
O11 S1 C17 F1 -59.8(6) . . . . ?
O13 S1 C17 F1 -177.9(6) . . . . ?
O23 S2 C18 F4 -64.2(6) . . . . ?
O21 S2 C18 F4 176.5(5) . . . . ?
O22 S2 C18 F4 56.1(6) . . . . ?
O23 S2 C18 F5 59.5(7) . . . . ?
O21 S2 C18 F5 -59.8(7) . . . . ?
O22 S2 C18 F5 179.8(6) . . . . ?
O23 S2 C18 F6 177.5(5) . . . . ?
O21 S2 C18 F6 58.2(6) . . . . ?
O22 S2 C18 F6 -62.2(6) . . . . ?
