# CIF produced by WinGX routine CIF_UPDATE # Created on 2003-01-06 at 17:18:52 # 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 : new # # 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_dihydroanthracene #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; catena-bis(N-isonicotinic acid)nickel(II) -bis(/m-thiocyanato-N,N',S,S')(9,10-dihydroanthracene)1/2 ; _chemical_formula_moiety 'C42 H32 N8 Ni2 O8 S4' _chemical_formula_sum 'C42 H32 N8 Ni2 O8 S4' _chemical_formula_weight 1022.42 #----------------------------------------------------------------------------# # 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 14.8275(7) _cell_length_b 11.0772(4) _cell_length_c 16.5228(10) _cell_angle_alpha 101.697(4) _cell_angle_beta 64.114(5) _cell_angle_gamma 74.884(3) _cell_volume 2194.89(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 1.47 _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 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.111 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8331 _exptl_absorpt_correction_T_max 0.9354 #----------------------------------------------------------------------------# # 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 0.0508 _diffrn_reflns_av_sigmaI/netI 0.107 _diffrn_reflns_number 11109 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 29.98 _reflns_number_total 11109 _reflns_number_observed 5625 _reflns_observed_criterion >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'RAPID-AUTO' _computing_cell_refinement 'RAPID-AUTO' _computing_structure_solution 'SIR-92' _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^)+(0.0631P)^2^+4.0254P] 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 11109 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1844 _refine_ls_R_factor_obs 0.0902 _refine_ls_wR_factor_all 0.2045 _refine_ls_wR_factor_obs 0.164 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/esd_max 0.00 _refine_ls_shift/esd_mean 0.00 _refine_diff_density_max 0.484 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # 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 C1 C 0.3713(5) 0.0677(6) -0.0260(4) 0.0325(13) Uani 1 1 d . . . C2 C 0.1130(5) 0.1804(6) 0.0791(4) 0.0337(13) Uani 1 1 d . . . C3 C 0.1178(5) 0.6627(6) 0.0345(4) 0.0318(13) Uani 1 1 d . . . C4 C 0.3745(5) 0.5524(6) -0.0695(4) 0.0343(13) Uani 1 1 d . . . C11 C 0.3450(6) 0.4029(7) 0.1254(5) 0.0478(17) Uani 1 1 d . . . H11 H 0.407 0.336 0.0701 0.057 Uiso 1 1 calc R . . C12 C 0.3504(6) 0.4489(7) 0.2062(5) 0.0499(17) Uani 1 1 d . . . H12 H 0.4152 0.4131 0.2052 0.06 Uiso 1 1 calc R . . C13 C 0.2613(6) 0.5465(7) 0.2872(5) 0.0453(16) Uani 1 1 d . . . C14 C 0.1670(6) 0.5990(7) 0.2859(5) 0.0496(17) Uani 1 1 d . . . H14 H 0.105 0.6675 0.3402 0.06 Uiso 1 1 calc R . . C15 C 0.1657(6) 0.5487(7) 0.2029(5) 0.0472(17) Uani 1 1 d . . . H15 H 0.1018 0.5838 0.2025 0.057 Uiso 1 1 calc R . . C16 C 0.2641(7) 0.5943(8) 0.3770(5) 0.0523(18) Uani 1 1 d . . . C21 C 0.3200(6) 0.1677(7) 0.8044(5) 0.0512(18) Uani 1 1 d . . . H21 H 0.3839 0.132 0.8049 0.061 Uiso 1 1 calc R . . C22 C 0.3150(6) 0.1055(7) 0.7268(5) 0.056(2) Uani 1 1 d . . . H22 H 0.3741 0.0295 0.6763 0.068 Uiso 1 1 calc R . . C23 C 0.2208(5) 0.1574(6) 0.7248(4) 0.0400(15) Uani 1 1 d . . . C24 C 0.1360(5) 0.2717(7) 0.7996(5) 0.0450(16) Uani 1 1 d . . . H24 H 0.0722 0.3099 0.7997 0.054 Uiso 1 1 calc R . . C25 C 0.1488(5) 0.3281(6) 0.8749(5) 0.0415(15) Uani 1 1 d . . . H25 H 0.092 0.4061 0.9252 0.05 Uiso 1 1 calc R . . C26 C 0.2092(7) 0.0943(8) 0.6436(5) 0.0525(18) Uani 1 1 d . . . C31 C 0.3035(6) -0.1809(7) 0.1578(5) 0.0474(17) Uani 1 1 d . . . H31 H 0.3681 -0.2436 0.1026 0.057 Uiso 1 1 calc R . . C32 C 0.2968(6) -0.1597(7) 0.2452(5) 0.0471(17) Uani 1 1 d . . . H32 H 0.3562 -0.2057 0.2489 0.057 Uiso 1 1 calc R . . C33 C 0.2011(6) -0.0696(7) 0.3272(5) 0.0456(16) Uani 1 1 d . . . C34 C 0.1118(6) -0.0038(7) 0.3199(5) 0.0493(17) Uani 1 1 d . . . H34 H 0.0452 0.0553 0.3747 0.059 Uiso 1 1 calc R . . C35 C 0.1259(6) -0.0296(7) 0.2289(5) 0.0450(16) Uani 1 1 d . . . H35 H 0.0674 0.014 0.2233 0.054 Uiso 1 1 calc R . . C36 C 0.1958(7) -0.0371(8) 0.4217(5) 0.0528(18) Uani 1 1 d . . . C41 C 0.3557(6) 0.7536(7) 0.7880(5) 0.0471(17) Uani 1 1 d . . . H41 H 0.4177 0.7161 0.7907 0.056 Uiso 1 1 calc R . . C42 C 0.3619(6) 0.7155(7) 0.7007(5) 0.0471(16) Uani 1 1 d . . . H42 H 0.4267 0.6534 0.6455 0.056 Uiso 1 1 calc R . . C43 C 0.2694(6) 0.7715(7) 0.6962(5) 0.0428(15) Uani 1 1 d . . . C44 C 0.1773(6) 0.8679(8) 0.7774(5) 0.0570(19) Uani 1 1 d . . . H44 H 0.1154 0.9104 0.7759 0.068 Uiso 1 1 calc R . . C45 C 0.1788(6) 0.9004(7) 0.8616(5) 0.0523(18) Uani 1 1 d . . . H45 H 0.1164 0.9671 0.9166 0.063 Uiso 1 1 calc R . . C46 C 0.2700(6) 0.7246(7) 0.6043(6) 0.0512(18) Uani 1 1 d . . . C101 C 0.1774(13) 0.2691(13) 0.3005(11) 0.107(4) Uani 1 1 d . . . H101 H 0.1326 0.289 0.2752 0.129 Uiso 1 1 calc R . . C102 C 0.2824(14) 0.1769(12) 0.2411(9) 0.108(5) Uani 1 1 d . . . H102 H 0.3089 0.1325 0.1761 0.13 Uiso 1 1 calc R . . C103 C 0.3475(10) 0.1511(11) 0.2784(7) 0.096(4) Uani 1 1 d . . . H103 H 0.4192 0.0885 0.238 0.115 Uiso 1 1 calc R . . C104 C 0.3102(8) 0.2157(9) 0.3756(6) 0.068(2) Uani 1 1 d . . . C105 C 0.2039(8) 0.3082(9) 0.4335(7) 0.072(2) Uani 1 1 d . . . C106 C 0.1375(11) 0.3317(11) 0.3949(9) 0.102(4) Uani 1 1 d . . . H106 H 0.0647 0.3913 0.4347 0.123 Uiso 1 1 calc R . . C107 C 0.1573(8) 0.3823(10) 0.5377(7) 0.089(3) Uani 1 1 d . . . H502 H 0.1054 0.3484 0.5749 0.107 Uiso 1 1 calc R . . H503 H 0.1168 0.4761 0.5528 0.107 Uiso 1 1 calc R . . C108 C 0.2373(8) 0.3746(9) 0.5712(6) 0.071(2) Uani 1 1 d . . . C109 C 0.2065(10) 0.4586(11) 0.6594(7) 0.092(3) Uani 1 1 d . . . H109 H 0.1357 0.5238 0.6985 0.11 Uiso 1 1 calc R . . C110 C 0.2784(15) 0.4489(14) 0.6918(9) 0.114(5) Uani 1 1 d . . . H110 H 0.2544 0.5059 0.7533 0.137 Uiso 1 1 calc R . . C111 C 0.3839(14) 0.3577(16) 0.6359(12) 0.122(5) Uani 1 1 d . . . H111 H 0.4327 0.3533 0.6573 0.146 Uiso 1 1 calc R . . C112 C 0.4153(10) 0.2731(12) 0.5472(9) 0.096(3) Uani 1 1 d . . . H112 H 0.4865 0.2088 0.5087 0.115 Uiso 1 1 calc R . . C113 C 0.3450(9) 0.2790(10) 0.5121(7) 0.074(3) Uani 1 1 d . . . C114 C 0.3835(8) 0.1843(10) 0.4162(7) 0.084(3) Uani 1 1 d . . . H501 H 0.3937 0.0957 0.4196 0.101 Uiso 1 1 calc R . . H504 H 0.4545 0.1802 0.3712 0.101 Uiso 1 1 calc R . . N1 N 0.3410(4) 0.1799(5) -0.0176(4) 0.0390(12) Uani 1 1 d . . . N2 N 0.1460(4) 0.0642(5) 0.0589(4) 0.0408(12) Uani 1 1 d . . . N3 N 0.1501(4) 0.5488(5) 0.0200(4) 0.0374(12) Uani 1 1 d . . . N4 N 0.3414(4) 0.6694(5) -0.0421(4) 0.0379(12) Uani 1 1 d . . . N11 N 0.2531(4) 0.4514(5) 0.1236(4) 0.0386(12) Uani 1 1 d . . . N21 N 0.2388(4) 0.2761(5) 0.8789(4) 0.0399(12) Uani 1 1 d . . . N31 N 0.2203(4) -0.1147(5) 0.1482(4) 0.0415(13) Uani 1 1 d . . . N41 N 0.2644(5) 0.8420(5) 0.8691(4) 0.0429(13) Uani 1 1 d . . . O11 O 0.3547(5) 0.5463(6) 0.3723(4) 0.0719(16) Uani 1 1 d . . . H211 H 0.3472 0.5789 0.4252 0.108 Uiso 1 1 calc R . . O12 O 0.1768(5) 0.6808(6) 0.4515(4) 0.0711(16) Uani 1 1 d . . . O21 O 0.2917(5) -0.0068(5) 0.5752(4) 0.0678(16) Uani 1 1 d . . . H221 H 0.2783 -0.0348 0.5336 0.102 Uiso 1 1 calc R . . O22 O 0.1200(5) 0.1411(6) 0.6470(4) 0.0688(15) Uani 1 1 d . . . O31 O 0.1069(5) 0.0493(6) 0.4948(4) 0.0713(16) Uani 1 1 d . . . H231 H 0.1125 0.0599 0.5428 0.107 Uiso 1 1 calc R . . O32 O 0.2810(5) -0.0966(6) 0.4220(4) 0.0716(17) Uani 1 1 d . . . O41 O 0.3580(5) 0.6411(6) 0.5307(4) 0.0655(15) Uani 1 1 d . . . O42 O 0.1797(5) 0.7728(6) 0.6084(4) 0.0719(16) Uani 1 1 d . . . H242 H 0.1882 0.7422 0.5548 0.108 Uiso 1 1 calc R . . S1 S 0.41408(14) -0.09020(15) -0.03749(13) 0.0424(4) Uani 1 1 d . . . S2 S 0.06925(14) 0.34304(16) 0.10695(13) 0.0453(4) Uani 1 1 d . . . S3 S 0.07183(14) 0.82417(16) 0.05569(14) 0.0481(4) Uani 1 1 d . . . S004 S 0.41826(14) 0.38956(16) -0.10752(13) 0.0482(4) Uani 1 1 d . . . Ni01 Ni 0.24550(7) 0.36467(8) 0.00071(6) 0.0334(2) Uani 1 1 d . . . Ni2 Ni 0.24360(7) -0.13268(8) 0.00899(6) 0.0329(2) Uani 1 1 d . . . 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 C1 0.032(3) 0.038(3) 0.031(3) 0.011(3) -0.019(3) -0.014(3) C2 0.038(4) 0.036(3) 0.034(3) 0.013(3) -0.024(3) -0.014(3) C3 0.022(3) 0.038(3) 0.031(3) 0.010(2) -0.012(3) -0.010(3) C4 0.026(3) 0.039(3) 0.035(3) 0.016(3) -0.014(3) -0.012(3) C11 0.044(4) 0.048(4) 0.049(4) 0.013(3) -0.027(4) -0.013(3) C12 0.048(5) 0.055(4) 0.052(4) 0.018(3) -0.035(4) -0.012(4) C13 0.055(5) 0.045(4) 0.046(4) 0.016(3) -0.032(4) -0.024(3) C14 0.047(4) 0.051(4) 0.044(4) 0.008(3) -0.026(4) -0.011(3) C15 0.041(4) 0.054(4) 0.043(4) 0.010(3) -0.025(4) -0.013(3) C16 0.055(5) 0.063(5) 0.047(4) 0.015(4) -0.035(4) -0.024(4) C21 0.047(5) 0.050(4) 0.048(4) 0.007(3) -0.030(4) -0.005(3) C22 0.059(5) 0.046(4) 0.047(4) 0.001(3) -0.032(4) -0.001(4) C23 0.041(4) 0.045(4) 0.034(3) 0.016(3) -0.020(3) -0.016(3) C24 0.031(4) 0.058(4) 0.043(4) 0.014(3) -0.020(3) -0.014(3) C25 0.036(4) 0.041(4) 0.043(4) 0.009(3) -0.022(3) -0.010(3) C26 0.061(5) 0.060(5) 0.039(4) 0.016(3) -0.029(4) -0.026(4) C31 0.044(4) 0.045(4) 0.044(4) 0.013(3) -0.024(3) -0.004(3) C32 0.051(5) 0.049(4) 0.041(4) 0.016(3) -0.030(4) -0.010(3) C33 0.055(5) 0.050(4) 0.038(4) 0.016(3) -0.026(4) -0.025(4) C34 0.038(4) 0.055(4) 0.041(4) 0.010(3) -0.018(3) -0.011(3) C35 0.035(4) 0.052(4) 0.048(4) 0.017(3) -0.026(3) -0.011(3) C36 0.066(5) 0.058(4) 0.041(4) 0.016(3) -0.033(4) -0.026(4) C41 0.034(4) 0.050(4) 0.046(4) 0.013(3) -0.020(3) -0.004(3) C42 0.047(4) 0.048(4) 0.036(4) 0.009(3) -0.019(3) -0.012(3) C43 0.045(4) 0.047(4) 0.043(4) 0.017(3) -0.030(3) -0.015(3) C44 0.051(5) 0.063(5) 0.059(5) 0.020(4) -0.039(4) -0.010(4) C45 0.051(5) 0.056(4) 0.046(4) 0.013(3) -0.033(4) -0.006(4) C46 0.047(5) 0.056(4) 0.060(5) 0.023(4) -0.036(4) -0.018(4) C101 0.161(14) 0.092(9) 0.134(12) 0.072(8) -0.103(11) -0.071(9) C102 0.193(15) 0.089(8) 0.084(8) 0.045(7) -0.080(10) -0.089(10) C103 0.119(10) 0.090(7) 0.059(6) 0.023(5) -0.021(6) -0.063(7) C104 0.066(6) 0.062(5) 0.057(5) 0.023(4) -0.017(5) -0.025(5) C105 0.079(7) 0.068(6) 0.066(6) 0.031(5) -0.033(5) -0.028(5) C106 0.125(11) 0.086(7) 0.092(8) 0.036(6) -0.061(8) -0.027(7) C107 0.063(7) 0.092(7) 0.071(6) 0.024(5) -0.022(5) 0.003(5) C108 0.072(7) 0.072(6) 0.051(5) 0.032(4) -0.016(5) -0.026(5) C109 0.111(9) 0.090(7) 0.062(6) 0.034(6) -0.030(6) -0.046(7) C110 0.192(15) 0.120(11) 0.086(9) 0.057(8) -0.075(11) -0.121(12) C111 0.144(13) 0.152(14) 0.150(14) 0.102(12) -0.091(12) -0.111(12) C112 0.088(8) 0.090(8) 0.107(9) 0.040(7) -0.041(8) -0.046(7) C113 0.077(7) 0.088(7) 0.066(6) 0.034(5) -0.035(6) -0.045(6) C114 0.057(6) 0.088(7) 0.080(7) 0.022(5) -0.024(5) -0.018(5) N1 0.041(3) 0.036(3) 0.048(3) 0.017(2) -0.028(3) -0.016(3) N2 0.045(3) 0.034(3) 0.048(3) 0.014(2) -0.028(3) -0.015(3) N3 0.038(3) 0.027(3) 0.047(3) 0.011(2) -0.023(3) -0.011(2) N4 0.035(3) 0.034(3) 0.051(3) 0.019(2) -0.025(3) -0.014(2) N11 0.037(3) 0.038(3) 0.039(3) 0.011(2) -0.022(3) -0.010(3) N21 0.041(3) 0.036(3) 0.044(3) 0.014(2) -0.024(3) -0.013(3) N31 0.039(3) 0.044(3) 0.038(3) 0.013(2) -0.021(3) -0.013(3) N41 0.049(4) 0.040(3) 0.042(3) 0.013(2) -0.030(3) -0.011(3) O11 0.067(4) 0.091(4) 0.058(3) 0.008(3) -0.047(3) -0.022(3) O12 0.059(4) 0.085(4) 0.045(3) -0.003(3) -0.029(3) -0.011(3) O21 0.081(4) 0.062(3) 0.052(3) 0.003(3) -0.046(3) -0.009(3) O22 0.060(4) 0.092(4) 0.057(3) 0.014(3) -0.039(3) -0.029(3) O31 0.072(4) 0.096(4) 0.039(3) 0.009(3) -0.031(3) -0.031(4) O32 0.085(5) 0.075(4) 0.057(3) 0.014(3) -0.053(3) -0.013(3) O41 0.063(4) 0.079(4) 0.049(3) 0.010(3) -0.034(3) -0.021(3) O42 0.067(4) 0.091(4) 0.050(3) 0.007(3) -0.041(3) -0.013(3) S1 0.0387(10) 0.0304(8) 0.0589(11) 0.0179(7) -0.0267(9) -0.0110(7) S2 0.0412(10) 0.0299(8) 0.0514(10) 0.0124(7) -0.0178(8) -0.0079(7) S3 0.0393(10) 0.0298(8) 0.0757(13) 0.0195(8) -0.0310(10) -0.0121(7) S004 0.0387(10) 0.0287(8) 0.0591(11) 0.0112(7) -0.0155(9) -0.0090(7) Ni01 0.0364(4) 0.0279(4) 0.0379(4) 0.0114(3) -0.0225(4) -0.0101(3) Ni2 0.0365(4) 0.0284(4) 0.0363(4) 0.0119(3) -0.0222(4) -0.0105(3) #----------------------------------------------------------------------------# # 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 C1 N1 1.163(7) . ? C1 S1 1.637(6) . ? C2 N2 1.168(7) . ? C2 S2 1.635(6) . ? C3 N3 1.158(7) . ? C3 S3 1.640(6) . ? C4 N4 1.167(7) . ? C4 S004 1.626(6) . ? C11 N11 1.344(8) . ? C11 C12 1.373(9) . ? C12 C13 1.353(9) . ? C13 C14 1.379(9) . ? C13 C16 1.494(9) . ? C14 C15 1.382(9) . ? C15 N11 1.332(8) . ? C16 O12 1.261(9) . ? C16 O11 1.271(9) . ? C21 N21 1.327(8) . ? C21 C22 1.369(9) . ? C22 C23 1.384(9) . ? C23 C24 1.374(9) . ? C23 C26 1.483(9) . ? C24 C25 1.388(9) . ? C25 N21 1.345(8) . ? C26 O22 1.261(9) . ? C26 O21 1.262(9) . ? C31 N31 1.354(8) . ? C31 C32 1.369(9) . ? C32 C33 1.371(9) . ? C33 C34 1.404(9) . ? C33 C36 1.491(9) . ? C34 C35 1.381(9) . ? C35 N31 1.341(8) . ? C36 O31 1.264(9) . ? C36 O32 1.265(9) . ? C41 N41 1.334(8) . ? C41 C42 1.373(9) . ? C42 C43 1.390(9) . ? C43 C44 1.366(9) . ? C43 C46 1.498(9) . ? C44 C45 1.375(9) . ? C45 N41 1.337(8) . ? C46 O41 1.251(9) . ? C46 O42 1.272(8) . ? C101 C106 1.344(15) . ? C101 C102 1.364(16) . ? C102 C103 1.358(16) . ? C103 C104 1.396(12) . ? C104 C105 1.376(12) . ? C104 C114 1.513(13) . ? C105 C106 1.388(14) . ? C105 C107 1.486(12) . ? C107 C108 1.504(13) . ? C108 C109 1.358(13) . ? C108 C113 1.401(12) . ? C109 C110 1.377(16) . ? C110 C111 1.362(17) . ? C111 C112 1.364(16) . ? C112 C113 1.390(14) . ? C113 C114 1.470(12) . ? N1 Ni01 2.037(5) . ? N2 Ni2 2.028(5) . ? N3 Ni01 2.025(5) . ? N4 Ni2 2.036(5) 1_565 ? N11 Ni01 2.127(5) . ? N21 Ni01 2.109(5) 1_556 ? N31 Ni2 2.129(5) . ? N41 Ni2 2.141(5) 1_566 ? S1 Ni2 2.5047(19) . ? S2 Ni01 2.542(2) . ? S3 Ni2 2.526(2) 1_565 ? S004 Ni01 2.531(2) . ? Ni01 N21 2.109(5) 1_554 ? Ni2 N4 2.036(5) 1_545 ? Ni2 N41 2.141(5) 1_544 ? Ni2 S3 2.526(2) 1_545 ? 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 N1 C1 S1 179.8(6) . . ? N2 C2 S2 178.8(6) . . ? N3 C3 S3 179.6(6) . . ? N4 C4 S004 178.9(6) . . ? N11 C11 C12 122.2(7) . . ? C13 C12 C11 119.8(7) . . ? C12 C13 C14 118.7(6) . . ? C12 C13 C16 120.7(7) . . ? C14 C13 C16 120.5(7) . . ? C13 C14 C15 119.1(7) . . ? N11 C15 C14 122.1(6) . . ? O12 C16 O11 124.8(6) . . ? O12 C16 C13 117.7(7) . . ? O11 C16 C13 117.5(7) . . ? N21 C21 C22 123.6(7) . . ? C21 C22 C23 119.0(7) . . ? C24 C23 C22 119.0(6) . . ? C24 C23 C26 119.1(6) . . ? C22 C23 C26 121.9(6) . . ? C23 C24 C25 117.9(6) . . ? N21 C25 C24 123.5(6) . . ? O22 C26 O21 124.2(7) . . ? O22 C26 C23 119.8(7) . . ? O21 C26 C23 116.0(7) . . ? N31 C31 C32 122.9(6) . . ? C31 C32 C33 119.0(6) . . ? C32 C33 C34 119.4(6) . . ? C32 C33 C36 119.4(7) . . ? C34 C33 C36 121.1(7) . . ? C35 C34 C33 117.9(6) . . ? N31 C35 C34 123.0(6) . . ? O31 C36 O32 125.3(7) . . ? O31 C36 C33 117.1(7) . . ? O32 C36 C33 117.5(7) . . ? N41 C41 C42 122.8(6) . . ? C41 C42 C43 118.8(6) . . ? C44 C43 C42 119.0(6) . . ? C44 C43 C46 120.5(6) . . ? C42 C43 C46 120.5(6) . . ? C43 C44 C45 118.0(7) . . ? N41 C45 C44 124.0(7) . . ? O41 C46 O42 125.5(7) . . ? O41 C46 C43 118.0(6) . . ? O42 C46 C43 116.5(7) . . ? C106 C101 C102 121.1(13) . . ? C103 C102 C101 118.9(12) . . ? C102 C103 C104 122.0(12) . . ? C105 C104 C103 117.7(10) . . ? C105 C104 C114 121.1(8) . . ? C103 C104 C114 121.2(10) . . ? C104 C105 C106 119.8(10) . . ? C104 C105 C107 121.4(9) . . ? C106 C105 C107 118.8(10) . . ? C101 C106 C105 120.6(12) . . ? C105 C107 C108 116.4(8) . . ? C109 C108 C113 118.8(10) . . ? C109 C108 C107 120.8(10) . . ? C113 C108 C107 120.3(9) . . ? C108 C109 C110 121.1(12) . . ? C111 C110 C109 121.5(13) . . ? C110 C111 C112 117.6(14) . . ? C111 C112 C113 122.7(12) . . ? C112 C113 C108 118.3(10) . . ? C112 C113 C114 120.1(10) . . ? C108 C113 C114 121.6(9) . . ? C113 C114 C104 116.1(8) . . ? C1 N1 Ni01 161.5(5) . . ? C2 N2 Ni2 164.1(5) . . ? C3 N3 Ni01 160.7(5) . . ? C4 N4 Ni2 163.1(5) . 1_565 ? C15 N11 C11 118.0(6) . . ? C15 N11 Ni01 121.4(4) . . ? C11 N11 Ni01 120.5(4) . . ? C21 N21 C25 117.0(6) . . ? C21 N21 Ni01 122.9(5) . 1_556 ? C25 N21 Ni01 120.2(4) . 1_556 ? C35 N31 C31 117.8(6) . . ? C35 N31 Ni2 121.3(4) . . ? C31 N31 Ni2 120.7(4) . . ? C41 N41 C45 117.0(6) . . ? C41 N41 Ni2 122.4(4) . 1_566 ? C45 N41 Ni2 119.7(5) . 1_566 ? C1 S1 Ni2 101.6(2) . . ? C2 S2 Ni01 100.5(2) . . ? C3 S3 Ni2 101.4(2) . 1_565 ? C4 S004 Ni01 99.8(2) . . ? N3 Ni01 N1 179.6(2) . . ? N3 Ni01 N21 90.9(2) . 1_554 ? N1 Ni01 N21 89.5(2) . 1_554 ? N3 Ni01 N11 89.8(2) . . ? N1 Ni01 N11 89.8(2) . . ? N21 Ni01 N11 179.2(2) 1_554 . ? N3 Ni01 S004 92.09(15) . . ? N1 Ni01 S004 88.10(15) . . ? N21 Ni01 S004 90.07(16) 1_554 . ? N11 Ni01 S004 90.11(15) . . ? N3 Ni01 S2 86.58(15) . . ? N1 Ni01 S2 93.23(15) . . ? N21 Ni01 S2 88.83(15) 1_554 . ? N11 Ni01 S2 91.01(15) . . ? S004 Ni01 S2 178.26(7) . . ? N2 Ni2 N4 179.5(2) . 1_545 ? N2 Ni2 N31 90.9(2) . . ? N4 Ni2 N31 89.6(2) 1_545 . ? N2 Ni2 N41 90.5(2) . 1_544 ? N4 Ni2 N41 89.0(2) 1_545 1_544 ? N31 Ni2 N41 177.4(2) . 1_544 ? N2 Ni2 S1 93.95(16) . . ? N4 Ni2 S1 86.22(15) 1_545 . ? N31 Ni2 S1 89.91(15) . . ? N41 Ni2 S1 92.14(16) 1_544 . ? N2 Ni2 S3 86.12(16) . 1_545 ? N4 Ni2 S3 93.72(15) 1_545 1_545 ? N31 Ni2 S3 90.12(15) . 1_545 ? N41 Ni2 S3 87.83(16) 1_544 1_545 ? S1 Ni2 S3 179.93(10) . 1_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D...A symm(A) # O11 H211 O41 2.641(7) . yes O32 H232 O21 2.614(7) . yes O22 H221 O31 2.623(7) . yes O42 H242 O12 2.609(7) . yes #===END