# CIF produced by WinGX routine CIF_UPDATE # Created on 2003-01-23 at 15:53:49 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : e:\wingx\files\archive.dat # CIF files read : 3 # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_global _publ_requested_journal J.Am.Chem.Soc. # #------------------------------------------------------------------------- #2 Person making the deposition # _audit_creation_date 'Apr 19 12:58:11 2002' _audit_creation_method WinGX _publ_contact_author_name 'Sekiya, Ryo' _publ_contact_author_address ; Department of Basic Science, Graduate School of Arts and Sciences, The University of Tokyo, Komaba3-8-1, Meguro, Tokyo 153-8902, Japan ; _publ_contact_author_email csekiya@mail.ecc.u-tokyo.ac.jp _publ_contact_author_fax +81-3-5454-6569 _publ_contact_author_phone +81-3-5454-6569 #------------------------------------------------------------------------- #3 Publication details # # Provide these details if the structure has been published, # accepted or submitted for publication # # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal # loop_ _publ_author_name _publ_author_address 'Sekiya, Ryo' ; Department of Basic Science, Graduate School of Arts and Sciences, The University of Tokyo, Komaba3-8-1, Meguro, Tokyo 153-8902, Japan ; 'Nishikiori, Shin-ichi' ; Department of Basic Science, Graduate School of Arts and Sciences, The University of Tokyo, Komaba3-8-1, Meguro, Tokyo 153-8902, Japan ; 'Ogura, Katsuyuki' ; Department of Materials and Technology, Faculty of Engineering, Chiba University, 1-33, Yayoicho, Inageku, Chiba 263-8522, Japan ; # #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_triphenylene #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; catena-bis(N-isonicotinic acid)nickel(II) -bis(/m-thiocyanato-N,N',S,S')(triphenylene)1/3 ; _chemical_formula_moiety 'C60 H42 N12 Ni3 O12 S6' _chemical_formula_sum 'C60 H42 N12 Ni3 O12 S6' _chemical_formula_weight 1491.55 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.8740(8) _cell_length_b 11.1970(5) _cell_length_c 16.9305(7) _cell_angle_alpha 103.836(3) _cell_angle_beta 78.041(4) _cell_angle_gamma 86.770(2) _cell_volume 3198.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 29.98 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8988 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w' _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.1558 _diffrn_reflns_number 15190 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 29.98 _reflns_number_total 15190 _reflns_number_observed 5524 _reflns_observed_criterion >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'RAPID-AUTO' _computing_cell_refinement 'RAPID-AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1029P)^2^+20.2065P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 15190 _refine_ls_number_parameters 841 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3059 _refine_ls_R_factor_obs 0.1448 _refine_ls_wR_factor_all 0.3699 _refine_ls_wR_factor_obs 0.289 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.854 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.14 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_thermal_displace_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni4 Ni 0.32416(10) -0.10869(15) 0.16254(10) 0.0447(4) Uani 1 1 d . . . S2 S 0.1196(2) 0.1052(3) -0.0027(3) 0.0617(10) Uani 1 1 d . . . S1 S -0.12547(19) 0.4071(3) 0.0350(2) 0.0514(9) Uani 1 1 d . . . S4 S 0.2003(2) 0.3058(3) 0.2165(2) 0.0601(9) Uani 1 1 d . . . N2 N 0.0638(6) 0.3474(10) 0.0038(6) 0.048(3) Uani 1 1 d . . . N1 N -0.0705(7) 0.1603(10) 0.0212(6) 0.051(3) Uani 1 1 d . . . C1 C -0.0928(7) 0.2638(12) 0.0276(7) 0.045(3) Uani 1 1 d . . . C2 C 0.0857(7) 0.2464(12) 0.0019(8) 0.046(3) Uani 1 1 d . . . N4 N 0.2559(6) 0.0555(10) 0.1873(6) 0.045(2) Uani 1 1 d . . . C4 C 0.2326(8) 0.1567(13) 0.1993(8) 0.055(3) Uani 1 1 d . . . N41 N 0.3127(7) -0.0889(10) 0.2944(7) 0.059(3) Uani 1 1 d . . . N61 N 0.3369(6) 0.8641(10) 1.0305(7) 0.053(3) Uani 1 1 d . . . O51 O 0.4068(6) 0.6381(11) 0.5597(6) 0.085(3) Uani 1 1 d . . . O52 O 0.2835(6) 0.7241(10) 0.5865(5) 0.075(3) Uani 1 1 d . . . H252 H 0.2913 0.7525 0.633 0.112 Uiso 1 1 calc R . . C66 C 0.3468(10) 0.7807(16) 0.7685(9) 0.069(4) Uani 1 1 d . . . O61 O 0.4093(6) 0.7242(10) 0.7186(6) 0.078(3) Uani 1 1 d . . . H261 H 0.4045 0.7122 0.6703 0.117 Uiso 1 1 calc R . . O62 O 0.2868(6) 0.8046(11) 0.7449(6) 0.079(3) Uani 1 1 d . . . C64 C 0.4043(8) 0.7728(13) 0.8895(8) 0.056(3) Uani 1 1 d . . . H64 H 0.4483 0.728 0.8525 0.067 Uiso 1 1 calc R . . C63 C 0.3440(7) 0.8111(13) 0.8596(7) 0.052(3) Uani 1 1 d . . . C44 C 0.2396(8) -0.0110(14) 0.4378(9) 0.061(4) Uani 1 1 d . . . H44 H 0.1935 0.0242 0.4754 0.074 Uiso 1 1 calc R . . C42 C 0.3760(10) -0.0920(15) 0.4080(8) 0.073(5) Uani 1 1 d . . . H42 H 0.4205 -0.1097 0.4253 0.088 Uiso 1 1 calc R . . C53 C 0.3399(9) 0.5998(13) 0.4505(8) 0.056(4) Uani 1 1 d . . . C56 C 0.3457(10) 0.6554(14) 0.5377(9) 0.060(4) Uani 1 1 d . . . C62 C 0.2802(8) 0.8768(15) 0.9159(9) 0.067(4) Uani 1 1 d . . . H62 H 0.2383 0.9044 0.8978 0.08 Uiso 1 1 calc R . . C65 C 0.3997(7) 0.8008(12) 0.9746(8) 0.051(3) Uani 1 1 d . . . H65 H 0.4413 0.7749 0.9938 0.061 Uiso 1 1 calc R . . C32 C 0.3693(9) 0.1581(16) 0.9049(9) 0.079(5) Uani 1 1 d . . . H32 H 0.4054 0.0921 0.8728 0.094 Uiso 1 1 calc R . . C41 C 0.3743(9) -0.1156(13) 0.3241(9) 0.063(4) Uani 1 1 d . . . H41 H 0.4193 -0.1527 0.2852 0.075 Uiso 1 1 calc R . . C61 C 0.2790(8) 0.9019(13) 1.0011(7) 0.058(4) Uani 1 1 d . . . H61 H 0.2355 0.9471 1.0389 0.069 Uiso 1 1 calc R . . O42 O 0.2430(7) 0.0585(11) 0.6071(6) 0.083(3) Uani 1 1 d . . . O41 O 0.3652(7) -0.0226(11) 0.5792(6) 0.084(3) Uani 1 1 d . . . H441 H 0.3591 0.0035 0.63 0.127 Uiso 1 1 calc R . . C46 C 0.3024(10) 0.0027(14) 0.5578(8) 0.062(4) Uani 1 1 d . . . C106 C 0.3446(11) 0.3189(16) 0.5458(10) 0.077(5) Uani 1 1 d . . . C105 C 0.3472(11) 0.3705(16) 0.6318(11) 0.077(5) Uani 1 1 d . . . C111 C 0.2773(15) 0.3451(19) 0.5190(11) 0.100(7) Uani 1 1 d . . . C43 C 0.3070(9) -0.0401(13) 0.4645(8) 0.061(4) Uani 1 1 d . . . C112 C 0.2097(15) 0.4215(19) 0.5808(13) 0.094(6) Uani 1 1 d . . . C114 C 0.087(2) 0.522(4) 0.606(2) 0.151(13) Uani 1 1 d . . . H114 H 0.0415 0.5373 0.5889 0.181 Uiso 1 1 calc R . . C107 C 0.4066(14) 0.2506(17) 0.4844(12) 0.103(7) Uani 1 1 d . . . H107 H 0.4527 0.2352 0.4995 0.123 Uiso 1 1 calc R . . C113 C 0.141(2) 0.455(3) 0.5498(18) 0.147(12) Uani 1 1 d . . . H113 H 0.1382 0.4276 0.4942 0.177 Uiso 1 1 calc R . . C103 C 0.2885(17) 0.493(2) 0.7702(14) 0.119(9) Uani 1 1 d . . . H103 H 0.2467 0.5434 0.8077 0.143 Uiso 1 1 calc R . . C45 C 0.2472(8) -0.0390(13) 0.3503(8) 0.060(4) Uani 1 1 d . . . H45 H 0.2042 -0.0218 0.3304 0.072 Uiso 1 1 calc R . . C104 C 0.2842(12) 0.4439(16) 0.6881(11) 0.078(5) Uani 1 1 d . . . C108 C 0.4029(14) 0.2044(18) 0.4014(14) 0.099(7) Uani 1 1 d . . . H108 H 0.4456 0.1605 0.3615 0.119 Uiso 1 1 calc R . . C117 C 0.2157(14) 0.4722(19) 0.6604(13) 0.097(6) Uani 1 1 d . . . C110 C 0.2724(15) 0.2934(19) 0.4355(15) 0.111(7) Uani 1 1 d . . . H110 H 0.2273 0.3054 0.4178 0.134 Uiso 1 1 calc R . . C118 C 0.4118(13) 0.347(2) 0.6590(14) 0.108(7) Uani 1 1 d . . . H118 H 0.4538 0.2968 0.6214 0.13 Uiso 1 1 calc R . . C116 C 0.152(2) 0.553(2) 0.7164(19) 0.149(12) Uani 1 1 d . . . H116 H 0.1544 0.59 0.7711 0.179 Uiso 1 1 calc R . . C115 C 0.0855(19) 0.577(3) 0.688(3) 0.173(17) Uani 1 1 d . . . H115 H 0.0426 0.6277 0.7238 0.207 Uiso 1 1 calc R . . C101 C 0.4168(19) 0.394(3) 0.7401(19) 0.143(11) Uani 1 1 d . . . H101 H 0.4614 0.377 0.7575 0.171 Uiso 1 1 calc R . . C109 C 0.3373(18) 0.225(2) 0.3815(13) 0.112(8) Uani 1 1 d . . . H109 H 0.3343 0.1899 0.3267 0.135 Uiso 1 1 calc R . . C102 C 0.353(2) 0.467(2) 0.7960(14) 0.131(12) Uani 1 1 d . . . H102 H 0.3542 0.4993 0.8515 0.157 Uiso 1 1 calc R . . Ni1 Ni 0 0 0 0.0447(6) Uani 1 2 d S . . Ni2 Ni 0 0.5 0 0.0440(6) Uani 1 2 d S . . Ni3 Ni 0.32513(10) 0.39498(15) 0.16220(10) 0.0452(4) Uani 1 1 d . . . S3 S 0.4451(2) -0.0022(3) 0.1533(2) 0.0570(9) Uani 1 1 d . . . S5 S 0.2028(2) 0.7888(3) 0.1694(2) 0.0569(9) Uani 1 1 d . . . S6 S 0.4479(2) 0.4780(3) 0.1064(2) 0.0560(9) Uani 1 1 d . . . N21 N 0.0056(7) 0.4208(10) 0.8686(6) 0.050(3) Uani 1 1 d . . . N5 N 0.2576(6) 0.5467(9) 0.1617(6) 0.050(3) Uani 1 1 d . . . C16 C -0.0226(11) 0.1115(14) 0.3967(9) 0.070(5) Uani 1 1 d . . . N11 N -0.0150(6) 0.0220(10) 0.1325(6) 0.050(3) Uani 1 1 d . . . O22 O 0.0457(7) 0.1668(10) 0.5737(6) 0.084(3) Uani 1 1 d . . . H222 H 0.0352 0.1427 0.5279 0.126 Uiso 1 1 calc R . . N3 N 0.3910(6) 0.2424(10) 0.1648(7) 0.050(3) Uani 1 1 d . . . C11 C 0.0436(9) -0.0051(14) 0.1626(9) 0.067(4) Uani 1 1 d . . . H11 H 0.0891 -0.0428 0.1248 0.08 Uiso 1 1 calc R . . O21 O -0.0670(7) 0.2738(11) 0.5968(6) 0.092(4) Uani 1 1 d . . . N6 N 0.3939(7) 0.7289(10) 0.1403(7) 0.053(3) Uani 1 1 d . . . O11 O -0.0841(6) 0.1694(11) 0.4450(6) 0.084(4) Uani 1 1 d . . . H211 H -0.08 0.1811 0.4936 0.126 Uiso 1 1 calc R . . O12 O 0.0371(7) 0.0861(12) 0.4175(6) 0.094(4) Uani 1 1 d . . . C6 C 0.4168(7) 0.6260(12) 0.1257(7) 0.044(3) Uani 1 1 d . . . C14 C -0.0882(10) 0.1033(15) 0.2752(9) 0.073(5) Uani 1 1 d . . . H14 H -0.135 0.1375 0.3117 0.087 Uiso 1 1 calc R . . C13 C -0.0236(9) 0.0783(14) 0.3042(9) 0.062(4) Uani 1 1 d . . . C26 C -0.0064(9) 0.2478(14) 0.6205(8) 0.059(4) Uani 1 1 d . . . N31 N 0.3197(6) 0.3105(10) 1.0354(6) 0.052(3) Uani 1 1 d . . . C23 C -0.0002(8) 0.3053(12) 0.7062(8) 0.054(3) Uani 1 1 d . . . C25 C 0.0585(8) 0.3330(13) 0.8196(8) 0.057(4) Uani 1 1 d . . . H25 H 0.0984 0.3089 0.842 0.068 Uiso 1 1 calc R . . O32 O 0.2472(6) 0.1692(11) 0.7619(6) 0.083(3) Uani 1 1 d . . . H232 H 0.2498 0.1326 0.7131 0.125 Uiso 1 1 calc R . . C34 C 0.2587(8) 0.2982(13) 0.9221(8) 0.056(4) Uani 1 1 d . . . H34 H 0.2193 0.3292 0.9018 0.067 Uiso 1 1 calc R . . N51 N 0.3308(6) 0.4844(10) 0.2869(6) 0.050(3) Uani 1 1 d . . . C3 C 0.4130(7) 0.1416(12) 0.1599(7) 0.045(3) Uani 1 1 d . . . C5 C 0.2357(7) 0.6460(11) 0.1635(7) 0.043(3) Uani 1 1 d . . . C33 C 0.3115(7) 0.2020(13) 0.8720(8) 0.049(3) Uani 1 1 d . . . C24 C 0.0598(9) 0.2741(14) 0.7388(9) 0.068(4) Uani 1 1 d . . . H24 H 0.1001 0.2147 0.707 0.082 Uiso 1 1 calc R . . C15 C -0.0799(8) 0.0753(14) 0.1892(9) 0.061(4) Uani 1 1 d . . . H15 H -0.1224 0.0949 0.1692 0.073 Uiso 1 1 calc R . . C55 C 0.2703(8) 0.5564(13) 0.3421(8) 0.060(4) Uani 1 1 d . . . H55 H 0.2246 0.5669 0.3251 0.072 Uiso 1 1 calc R . . C12 C 0.0426(9) 0.0186(15) 0.2477(8) 0.074(5) Uani 1 1 d . . . H12 H 0.0854 -0.0053 0.2657 0.089 Uiso 1 1 calc R . . C36 C 0.3079(10) 0.1403(16) 0.7825(9) 0.066(4) Uani 1 1 d . . . C35 C 0.2649(8) 0.3478(13) 1.0024(8) 0.057(4) Uani 1 1 d . . . H35 H 0.2281 0.4118 1.0358 0.068 Uiso 1 1 calc R . . C22 C -0.0575(9) 0.4021(13) 0.7555(8) 0.064(4) Uani 1 1 d . . . H22 H -0.0974 0.4296 0.7344 0.076 Uiso 1 1 calc R . . C51 C 0.3948(7) 0.4693(12) 0.3141(8) 0.051(3) Uani 1 1 d . . . H51 H 0.4368 0.4184 0.2771 0.061 Uiso 1 1 calc R . . C21 C -0.0514(8) 0.4542(13) 0.8368(8) 0.056(3) Uani 1 1 d . . . H21 H -0.0895 0.5159 0.8707 0.067 Uiso 1 1 calc R . . O31 O 0.3642(7) 0.0667(12) 0.7376(6) 0.094(4) Uani 1 1 d . . . C31 C 0.3722(10) 0.2143(15) 0.9857(9) 0.080(5) Uani 1 1 d . . . H31 H 0.4113 0.1859 1.0075 0.096 Uiso 1 1 calc R . . C54 C 0.2733(9) 0.6156(12) 0.4234(8) 0.061(4) Uani 1 1 d . . . H54 H 0.2305 0.6656 0.4594 0.073 Uiso 1 1 calc R . . C52 C 0.4028(8) 0.5251(13) 0.3945(8) 0.057(4) Uani 1 1 d . . . H52 H 0.4489 0.5128 0.4102 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni4 0.0493(10) 0.0366(9) 0.0474(9) 0.0065(7) -0.0172(7) 0.0048(7) S2 0.055(2) 0.042(2) 0.092(3) 0.0204(19) -0.027(2) 0.0046(17) S1 0.048(2) 0.0318(18) 0.074(2) 0.0130(16) -0.0147(17) 0.0071(15) S4 0.052(2) 0.0401(19) 0.082(2) 0.0111(18) -0.0113(18) 0.0093(16) N2 0.052(7) 0.046(7) 0.050(6) 0.010(5) -0.026(5) 0.000(5) N1 0.065(8) 0.033(6) 0.059(7) 0.010(5) -0.024(6) -0.004(5) C1 0.051(8) 0.051(8) 0.036(6) 0.013(6) -0.013(6) -0.007(7) C2 0.043(7) 0.045(8) 0.052(7) 0.011(6) -0.019(6) -0.001(6) N4 0.036(6) 0.043(6) 0.058(6) 0.015(5) -0.016(5) 0.002(5) C4 0.057(9) 0.056(9) 0.055(8) 0.015(7) -0.026(7) 0.016(7) N41 0.070(8) 0.048(7) 0.060(7) 0.012(6) -0.021(6) 0.006(6) N61 0.054(7) 0.044(6) 0.060(7) 0.005(5) -0.023(6) 0.007(5) O51 0.072(8) 0.113(10) 0.064(6) 0.004(6) -0.032(6) 0.010(7) O52 0.092(8) 0.086(8) 0.039(5) 0.000(5) -0.023(5) 0.014(6) C66 0.065(10) 0.084(12) 0.050(8) 0.002(8) -0.012(8) -0.002(9) O61 0.076(8) 0.101(9) 0.043(5) 0.003(5) -0.006(5) 0.010(7) O62 0.076(7) 0.101(9) 0.050(6) -0.002(5) -0.024(5) 0.020(6) C64 0.050(8) 0.059(9) 0.062(8) 0.020(7) -0.018(7) 0.004(7) C63 0.047(8) 0.059(9) 0.044(7) 0.003(6) -0.014(6) 0.012(7) C44 0.050(9) 0.068(10) 0.068(9) 0.019(8) -0.020(7) 0.001(7) C42 0.097(13) 0.079(11) 0.042(7) 0.005(7) -0.030(8) 0.015(10) C53 0.073(10) 0.057(9) 0.042(7) 0.017(6) -0.013(7) -0.010(8) C56 0.070(11) 0.052(9) 0.054(8) 0.009(7) -0.012(8) -0.015(8) C62 0.045(8) 0.090(12) 0.062(9) 0.022(8) -0.008(7) 0.016(8) C65 0.045(7) 0.048(8) 0.055(8) 0.009(6) -0.011(6) 0.011(6) C32 0.079(11) 0.088(12) 0.056(9) -0.010(8) -0.030(8) 0.030(9) C41 0.064(10) 0.056(9) 0.064(9) 0.013(7) -0.014(7) 0.014(7) C61 0.061(9) 0.070(10) 0.036(6) -0.001(6) -0.021(6) 0.023(7) O42 0.084(8) 0.101(9) 0.050(6) -0.008(6) -0.015(6) -0.009(7) O41 0.099(9) 0.100(9) 0.053(6) 0.000(6) -0.039(6) 0.005(7) C46 0.076(11) 0.064(10) 0.044(8) 0.008(7) -0.015(8) -0.006(9) C106 0.091(13) 0.079(12) 0.059(10) 0.013(9) -0.013(9) -0.021(10) C105 0.089(13) 0.072(12) 0.073(11) 0.022(9) -0.024(10) -0.014(10) C111 0.17(2) 0.097(15) 0.052(10) 0.041(10) -0.023(12) -0.067(15) C43 0.081(11) 0.053(9) 0.053(8) 0.010(7) -0.031(8) -0.002(8) C112 0.13(2) 0.094(15) 0.070(13) 0.035(11) -0.033(13) -0.042(14) C114 0.16(3) 0.19(4) 0.13(2) 0.09(3) -0.01(2) -0.05(3) C107 0.14(2) 0.077(13) 0.086(13) 0.030(11) -0.008(13) -0.037(13) C113 0.20(3) 0.14(3) 0.100(18) 0.033(18) -0.01(2) -0.08(2) C103 0.18(3) 0.080(15) 0.081(15) 0.003(11) -0.003(15) -0.049(17) C45 0.063(9) 0.070(10) 0.041(7) 0.006(7) -0.013(7) 0.010(8) C104 0.103(15) 0.054(10) 0.078(11) 0.018(9) -0.018(11) -0.027(10) C108 0.111(18) 0.077(13) 0.095(16) 0.030(12) 0.024(13) -0.026(13) C117 0.117(18) 0.078(14) 0.096(14) 0.040(12) 0.000(14) -0.032(13) C110 0.16(2) 0.071(14) 0.126(18) 0.047(13) -0.043(17) -0.031(14) C118 0.122(19) 0.116(18) 0.105(16) 0.046(14) -0.041(14) -0.033(15) C116 0.16(3) 0.089(19) 0.16(2) 0.024(17) 0.04(2) -0.03(2) C115 0.12(3) 0.09(2) 0.28(5) 0.09(3) 0.05(3) 0.004(19) C101 0.20(3) 0.14(2) 0.14(2) 0.06(2) -0.09(2) -0.07(2) C109 0.18(3) 0.073(15) 0.072(13) 0.001(11) -0.016(16) -0.036(17) C102 0.23(4) 0.11(2) 0.062(13) 0.007(12) -0.041(18) -0.09(2) Ni1 0.0513(15) 0.0349(13) 0.0485(13) 0.0083(10) -0.0179(11) 0.0042(11) Ni2 0.0500(14) 0.0328(13) 0.0484(13) 0.0056(10) -0.0177(11) 0.0052(11) Ni3 0.0522(10) 0.0354(9) 0.0479(9) 0.0073(7) -0.0184(7) 0.0059(7) S3 0.047(2) 0.0347(18) 0.088(3) 0.0119(17) -0.0217(18) 0.0087(15) S5 0.054(2) 0.0328(17) 0.086(2) 0.0119(17) -0.0258(18) 0.0042(15) S6 0.057(2) 0.0408(19) 0.066(2) 0.0142(16) -0.0065(17) 0.0064(16) N21 0.062(7) 0.042(6) 0.044(6) -0.001(5) -0.022(5) -0.002(6) N5 0.067(8) 0.031(6) 0.052(6) 0.006(5) -0.018(5) 0.001(5) C16 0.101(14) 0.055(9) 0.057(9) -0.001(7) -0.049(9) 0.008(9) N11 0.058(7) 0.045(6) 0.044(6) 0.005(5) -0.016(5) 0.010(5) O22 0.107(9) 0.078(8) 0.055(6) -0.008(5) -0.027(6) 0.026(7) N3 0.052(7) 0.037(6) 0.065(7) 0.012(5) -0.024(5) -0.007(5) C11 0.066(10) 0.067(10) 0.062(9) 0.015(8) -0.014(8) 0.028(8) O21 0.082(8) 0.112(10) 0.061(6) -0.022(6) -0.036(6) 0.032(7) N6 0.063(7) 0.032(6) 0.063(7) 0.011(5) -0.014(6) 0.012(5) O11 0.068(7) 0.111(10) 0.054(6) -0.006(6) -0.016(5) 0.028(7) O12 0.086(8) 0.126(11) 0.055(6) -0.004(6) -0.029(6) 0.039(7) C6 0.043(7) 0.043(7) 0.044(7) 0.008(6) -0.013(5) 0.008(6) C14 0.079(12) 0.088(12) 0.050(8) 0.010(8) -0.026(8) 0.010(9) C13 0.060(9) 0.068(10) 0.059(8) 0.025(8) -0.009(7) -0.003(8) C26 0.071(10) 0.058(9) 0.047(8) 0.008(7) -0.018(7) 0.008(8) N31 0.044(6) 0.057(7) 0.054(6) 0.015(6) -0.012(5) 0.000(5) C23 0.069(10) 0.039(7) 0.055(8) 0.001(6) -0.029(7) -0.007(7) C25 0.066(9) 0.059(9) 0.045(7) 0.006(6) -0.026(7) 0.017(7) O32 0.078(8) 0.110(9) 0.051(6) -0.005(6) -0.024(5) 0.014(7) C34 0.043(8) 0.061(9) 0.064(9) 0.013(7) -0.021(7) 0.013(7) N51 0.047(7) 0.049(7) 0.052(6) 0.011(5) -0.013(5) 0.006(5) C3 0.052(8) 0.042(7) 0.044(7) 0.014(6) -0.012(6) -0.011(6) C5 0.047(7) 0.033(7) 0.056(7) 0.011(6) -0.025(6) -0.007(6) C33 0.028(6) 0.063(9) 0.064(8) 0.021(7) -0.019(6) -0.008(6) C24 0.065(10) 0.063(10) 0.073(10) 0.004(8) -0.031(8) 0.017(8) C15 0.041(8) 0.075(10) 0.071(9) 0.023(8) -0.020(7) 0.000(7) C55 0.052(9) 0.065(10) 0.055(8) 0.002(7) -0.014(7) -0.001(7) C12 0.069(10) 0.097(13) 0.049(8) 0.001(8) -0.027(7) 0.031(9) C36 0.069(11) 0.083(12) 0.050(8) 0.013(8) -0.026(8) -0.014(9) C35 0.054(8) 0.066(9) 0.048(7) 0.000(7) -0.028(6) 0.018(7) C22 0.079(11) 0.057(9) 0.060(9) 0.013(7) -0.032(8) 0.005(8) C51 0.046(8) 0.054(8) 0.053(7) 0.009(6) -0.017(6) -0.004(6) C21 0.057(9) 0.048(8) 0.054(8) -0.002(6) -0.012(7) 0.006(7) O31 0.093(9) 0.111(10) 0.057(6) -0.007(6) -0.020(6) 0.049(8) C31 0.083(12) 0.081(12) 0.067(10) 0.001(8) -0.030(8) 0.040(9) C54 0.080(11) 0.046(8) 0.046(7) -0.001(6) -0.010(7) 0.002(8) C52 0.054(8) 0.060(9) 0.051(7) -0.001(7) -0.021(6) 0.009(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ni4 N4 2.052(10) . ? Ni4 N6 2.055(10) 1_545 ? Ni4 N61 2.144(11) 1_544 ? Ni4 N41 2.155(11) . ? Ni4 S5 2.506(4) 1_545 ? Ni4 S3 2.522(4) . ? S2 C2 1.639(13) . ? S2 Ni1 2.496(4) . ? S1 C1 1.643(14) . ? S1 Ni2 2.544(3) . ? S4 C4 1.671(14) . ? S4 Ni3 2.580(4) . ? N2 C2 1.167(15) . ? N2 Ni2 2.022(11) . ? N1 C1 1.176(15) . ? N1 Ni1 2.046(11) . ? N4 C4 1.141(15) . ? N41 C45 1.338(16) . ? N41 C41 1.348(16) . ? N61 C61 1.329(15) . ? N61 C65 1.344(15) . ? N61 Ni4 2.144(11) 1_566 ? O51 C56 1.244(17) . ? O52 C56 1.316(17) . ? C66 O62 1.255(17) . ? C66 O61 1.279(17) . ? C66 C63 1.487(18) . ? C64 C63 1.371(16) . ? C64 C65 1.384(17) . ? C63 C62 1.367(17) . ? C44 C45 1.416(18) . ? C44 C43 1.418(18) . ? C42 C41 1.388(18) . ? C42 C43 1.39(2) . ? C53 C54 1.380(19) . ? C53 C52 1.391(19) . ? C53 C56 1.486(18) . ? C62 C61 1.397(17) . ? C32 C31 1.375(19) . ? C32 C33 1.390(18) . ? O42 C46 1.234(17) . ? O41 C46 1.285(17) . ? C46 C43 1.521(18) . ? C106 C107 1.39(3) . ? C106 C111 1.41(3) . ? C106 C105 1.44(2) . ? C105 C118 1.36(2) . ? C105 C104 1.39(2) . ? C111 C110 1.42(3) . ? C111 C112 1.49(3) . ? C112 C117 1.36(3) . ? C112 C113 1.49(4) . ? C114 C113 1.27(4) . ? C114 C115 1.38(4) . ? C107 C108 1.39(3) . ? C103 C102 1.35(4) . ? C103 C104 1.39(3) . ? C104 C117 1.44(3) . ? C108 C109 1.31(3) . ? C117 C116 1.43(3) . ? C110 C109 1.38(3) . ? C118 C101 1.37(3) . ? C116 C115 1.40(4) . ? C101 C102 1.40(4) . ? Ni1 N1 2.046(11) 2 ? Ni1 N11 2.155(10) . ? Ni1 N11 2.155(10) 2 ? Ni1 S2 2.496(4) 2 ? Ni2 N2 2.022(11) 2_565 ? Ni2 N21 2.168(10) 1_554 ? Ni2 N21 2.168(10) 2_566 ? Ni2 S1 2.544(3) 2_565 ? Ni3 N5 2.030(11) . ? Ni3 N3 2.034(11) . ? Ni3 N51 2.136(10) . ? Ni3 N31 2.154(10) 1_554 ? Ni3 S6 2.523(4) . ? S3 C3 1.648(13) . ? S5 C5 1.645(12) . ? S5 Ni4 2.506(4) 1_565 ? S6 C6 1.650(13) . ? N21 C25 1.315(16) . ? N21 C21 1.322(16) . ? N21 Ni2 2.168(10) 1_556 ? N5 C5 1.150(14) . ? C16 O12 1.231(17) . ? C16 O11 1.261(18) . ? C16 C13 1.524(19) . ? N11 C11 1.308(16) . ? N11 C15 1.344(17) . ? O22 C26 1.254(16) . ? N3 C3 1.152(15) . ? C11 C12 1.397(18) . ? O21 C26 1.272(16) . ? N6 C6 1.151(14) . ? N6 Ni4 2.055(10) 1_565 ? C14 C13 1.384(19) . ? C14 C15 1.390(18) . ? C13 C12 1.377(19) . ? C26 C23 1.469(17) . ? N31 C35 1.317(14) . ? N31 C31 1.369(17) . ? N31 Ni3 2.154(10) 1_556 ? C23 C24 1.369(18) . ? C23 C22 1.417(19) . ? C25 C24 1.365(18) . ? O32 C36 1.254(17) . ? C34 C35 1.370(17) . ? C34 C33 1.374(18) . ? N51 C51 1.336(15) . ? N51 C55 1.347(16) . ? C33 C36 1.524(18) . ? C55 C54 1.391(17) . ? C36 O31 1.250(18) . ? C22 C21 1.391(17) . ? C51 C52 1.395(16) . ? 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 N4 Ni4 N6 178.5(4) . 1_545 ? N4 Ni4 N61 91.7(4) . 1_544 ? N6 Ni4 N61 89.5(4) 1_545 1_544 ? N4 Ni4 N41 90.4(4) . . ? N6 Ni4 N41 88.4(4) 1_545 . ? N61 Ni4 N41 177.8(4) 1_544 . ? N4 Ni4 S5 86.8(3) . 1_545 ? N6 Ni4 S5 94.1(3) 1_545 1_545 ? N61 Ni4 S5 89.8(3) 1_544 1_545 ? N41 Ni4 S5 89.6(3) . 1_545 ? N4 Ni4 S3 92.1(3) . . ? N6 Ni4 S3 87.0(3) 1_545 . ? N61 Ni4 S3 89.2(3) 1_544 . ? N41 Ni4 S3 91.4(3) . . ? S5 Ni4 S3 178.50(14) 1_545 . ? C2 S2 Ni1 100.6(5) . . ? C1 S1 Ni2 100.8(5) . . ? C4 S4 Ni3 101.1(5) . . ? C2 N2 Ni2 164.1(10) . . ? C1 N1 Ni1 162.4(11) . . ? N1 C1 S1 178.6(12) . . ? N2 C2 S2 177.9(13) . . ? C4 N4 Ni4 165.4(11) . . ? N4 C4 S4 178.8(14) . . ? C45 N41 C41 117.5(12) . . ? C45 N41 Ni4 121.9(9) . . ? C41 N41 Ni4 120.3(10) . . ? C61 N61 C65 117.4(11) . . ? C61 N61 Ni4 119.9(9) . 1_566 ? C65 N61 Ni4 122.5(8) . 1_566 ? O62 C66 O61 123.4(13) . . ? O62 C66 C63 118.7(13) . . ? O61 C66 C63 117.7(14) . . ? C63 C64 C65 120.0(13) . . ? C62 C63 C64 118.3(12) . . ? C62 C63 C66 120.5(12) . . ? C64 C63 C66 121.3(13) . . ? C45 C44 C43 115.6(14) . . ? C41 C42 C43 115.9(14) . . ? C54 C53 C52 118.3(12) . . ? C54 C53 C56 122.5(14) . . ? C52 C53 C56 119.2(13) . . ? O51 C56 O52 124.4(13) . . ? O51 C56 C53 120.4(14) . . ? O52 C56 C53 115.1(14) . . ? C63 C62 C61 119.0(13) . . ? N61 C65 C64 122.2(12) . . ? C31 C32 C33 118.6(14) . . ? N41 C41 C42 125.2(14) . . ? N61 C61 C62 123.1(13) . . ? O42 C46 O41 124.3(13) . . ? O42 C46 C43 121.4(14) . . ? O41 C46 C43 114.3(14) . . ? C107 C106 C111 116.3(18) . . ? C107 C106 C105 124.4(19) . . ? C111 C106 C105 119.1(18) . . ? C118 C105 C104 119.1(19) . . ? C118 C105 C106 120(2) . . ? C104 C105 C106 120.8(18) . . ? C106 C111 C110 120(2) . . ? C106 C111 C112 119.2(17) . . ? C110 C111 C112 120(2) . . ? C42 C43 C44 121.9(13) . . ? C42 C43 C46 121.5(13) . . ? C44 C43 C46 116.2(14) . . ? C117 C112 C111 120(2) . . ? C117 C112 C113 122(2) . . ? C111 C112 C113 118(2) . . ? C113 C114 C115 129(4) . . ? C106 C107 C108 123(2) . . ? C114 C113 C112 114(3) . . ? C102 C103 C104 120(3) . . ? N41 C45 C44 123.8(13) . . ? C103 C104 C105 120(2) . . ? C103 C104 C117 120(2) . . ? C105 C104 C117 120.1(18) . . ? C109 C108 C107 118(2) . . ? C112 C117 C116 118(3) . . ? C112 C117 C104 121(2) . . ? C116 C117 C104 121(2) . . ? C109 C110 C111 117(2) . . ? C105 C118 C101 122(3) . . ? C115 C116 C117 120(3) . . ? C114 C115 C116 117(3) . . ? C118 C101 C102 118(3) . . ? C108 C109 C110 125(2) . . ? C103 C102 C101 121(2) . . ? N1 Ni1 N1 180.0(6) . 2 ? N1 Ni1 N11 90.6(4) . . ? N1 Ni1 N11 89.4(4) 2 . ? N1 Ni1 N11 89.4(4) . 2 ? N1 Ni1 N11 90.6(4) 2 2 ? N11 Ni1 N11 180.00(8) . 2 ? N1 Ni1 S2 85.8(3) . 2 ? N1 Ni1 S2 94.2(3) 2 2 ? N11 Ni1 S2 89.9(3) . 2 ? N11 Ni1 S2 90.1(3) 2 2 ? N1 Ni1 S2 94.2(3) . . ? N1 Ni1 S2 85.8(3) 2 . ? N11 Ni1 S2 90.1(3) . . ? N11 Ni1 S2 89.9(3) 2 . ? S2 Ni1 S2 180.0(3) 2 . ? N2 Ni2 N2 180.0(6) . 2_565 ? N2 Ni2 N21 90.0(4) . 1_554 ? N2 Ni2 N21 90.0(4) 2_565 1_554 ? N2 Ni2 N21 90.0(4) . 2_566 ? N2 Ni2 N21 90.0(4) 2_565 2_566 ? N21 Ni2 N21 180.0(2) 1_554 2_566 ? N2 Ni2 S1 92.5(3) . . ? N2 Ni2 S1 87.5(3) 2_565 . ? N21 Ni2 S1 88.9(3) 1_554 . ? N21 Ni2 S1 91.1(3) 2_566 . ? N2 Ni2 S1 87.5(3) . 2_565 ? N2 Ni2 S1 92.5(3) 2_565 2_565 ? N21 Ni2 S1 91.1(3) 1_554 2_565 ? N21 Ni2 S1 88.9(3) 2_566 2_565 ? S1 Ni2 S1 180.00(16) . 2_565 ? N5 Ni3 N3 178.7(5) . . ? N5 Ni3 N51 88.4(4) . . ? N3 Ni3 N51 91.0(4) . . ? N5 Ni3 N31 90.1(4) . 1_554 ? N3 Ni3 N31 90.5(4) . 1_554 ? N51 Ni3 N31 178.1(4) . 1_554 ? N5 Ni3 S6 93.3(3) . . ? N3 Ni3 S6 87.8(3) . . ? N51 Ni3 S6 90.1(3) . . ? N31 Ni3 S6 88.8(3) 1_554 . ? N5 Ni3 S4 87.4(3) . . ? N3 Ni3 S4 91.5(3) . . ? N51 Ni3 S4 90.9(3) . . ? N31 Ni3 S4 90.2(3) 1_554 . ? S6 Ni3 S4 178.74(14) . . ? C3 S3 Ni4 102.7(5) . . ? C5 S5 Ni4 100.9(4) . 1_565 ? C6 S6 Ni3 100.3(5) . . ? C25 N21 C21 117.1(11) . . ? C25 N21 Ni2 124.3(9) . 1_556 ? C21 N21 Ni2 118.3(9) . 1_556 ? C5 N5 Ni3 163.0(10) . . ? O12 C16 O11 125.9(13) . . ? O12 C16 C13 119.0(15) . . ? O11 C16 C13 115.0(13) . . ? C11 N11 C15 115.9(11) . . ? C11 N11 Ni1 119.8(9) . . ? C15 N11 Ni1 123.9(9) . . ? C3 N3 Ni3 162.6(10) . . ? N11 C11 C12 124.4(13) . . ? C6 N6 Ni4 163.5(11) . 1_565 ? N6 C6 S6 178.7(13) . . ? C13 C14 C15 117.0(15) . . ? C12 C13 C14 119.1(14) . . ? C12 C13 C16 118.0(14) . . ? C14 C13 C16 122.9(14) . . ? O22 C26 O21 120.7(13) . . ? O22 C26 C23 119.4(13) . . ? O21 C26 C23 119.7(13) . . ? C35 N31 C31 116.9(12) . . ? C35 N31 Ni3 121.5(9) . 1_556 ? C31 N31 Ni3 121.6(9) . 1_556 ? C24 C23 C22 118.8(12) . . ? C24 C23 C26 123.3(14) . . ? C22 C23 C26 117.8(12) . . ? N21 C25 C24 125.5(12) . . ? C35 C34 C33 119.1(12) . . ? C51 N51 C55 116.9(11) . . ? C51 N51 Ni3 121.0(9) . . ? C55 N51 Ni3 122.1(9) . . ? N3 C3 S3 179.5(13) . . ? N5 C5 S5 178.0(13) . . ? C34 C33 C32 118.6(13) . . ? C34 C33 C36 122.3(12) . . ? C32 C33 C36 119.0(13) . . ? C25 C24 C23 117.8(14) . . ? N11 C15 C14 125.1(13) . . ? N51 C55 C54 122.7(13) . . ? C13 C12 C11 118.3(13) . . ? O31 C36 O32 126.7(14) . . ? O31 C36 C33 117.8(13) . . ? O32 C36 C33 115.5(14) . . ? N31 C35 C34 124.1(13) . . ? C21 C22 C23 117.1(12) . . ? N51 C51 C52 124.1(13) . . ? N21 C21 C22 123.5(13) . . ? N31 C31 C32 122.6(13) . . ? C53 C54 C55 119.7(14) . . ? C53 C52 C51 118.2(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O11 H211 O21 0.8200 1.8700 2.645(14) 156.00 1_555 yes O22 H222 O12 0.8200 1.8200 2.622(14) 166.00 1_555 yes O32 H232 O42 0.8200 1.8200 2.636(14) 173.00 1_555 yes O52 H252 O62 0.8200 1.8300 2.630(13) 167.00 1_555 yes O61 H261 O51 0.8200 1.8500 2.643(14) 163.00 1_555 yes O41 H441 O31 0.8200 1.8100 2.624(14) 169.00 1_555 yes #===END