# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address ; L.V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine Prospekt Nauki 31 03028 Kiev Ukraine ; ; L.V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine Prospekt Nauki 31 03028 Kiev Ukraine ; ; L.V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine Prospekt Nauki 31 03028 Kiev Ukraine ; ; L.V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine Prospekt Nauki 31 03028 Kiev Ukraine ; ; Petru Poni Institute of Macromolecular Chemistry, Aleea Grigore Ghica Voda 41A RO-700487 Iasi Romania and Institute of Applied Physics of the Academy of Sciences of Moldova, Academiei str. 5, 2028 Chisinau Moldova ; ; Institut fuer Anorganische Chemie, Universitaet Wien Waehringer Strasse 42 A-1090 Vienna Austria ; _publ_contact_author_address ; L.V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine Prospekt Nauki 31 03028 Kiev Ukraine ; _publ_contact_author_email lampeka@adamant.net _publ_contact_author_name Ya.D.Lampeka _publ_section_title ; Catenation control by ligand size in the two-dimensional coordination polymers based on tritopic carboxylate linkers and azamacrocyclic nickel(II) complexes ; _publ_author_name Y.Lampeka data_NiL1_BTB _database_code_depnum_ccdc_archive 'CCDC 834622' #TrackingRef '8684_web_deposit_cif_file_0_YaroslawD.Lampeka_ #1324039133.NiL1_BTB.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(\m~3~(4,4',4''-benzene-1,3,5-triyl-tribenzoato)-O,O',O'') -tris((1,4,8,11-tetra-azacyclotetradecane)-nickel(ii)) hexahydrate) ; _chemical_name_common ; catena-(bis(mu!3$(4,4',4''-benzene-1,3,5-triyl-tribenzoato)- O,O',O'') -tris((1,4,8,11-tetra-azacyclotetradecane)-nickel(ii)) hexahydrate) ; _chemical_formula_moiety '2n(C42 H51 N6 Ni1.5 O6), 6n(H2 O)' _chemical_formula_sum 'C84 H114 N12 Ni3 O18' _chemical_formula_weight 1756.00 _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 293(2) _chemical_oxdiff_formula C31H30N4O6Ni1 _chemical_oxdiff_usercomment ? 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 7.1953(15) _cell_length_b 20.339(3) _cell_length_c 29.599(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.67(2) _cell_angle_gamma 90.00 _cell_volume 4317.3(14) _cell_formula_units_Z 2 _cell_measurement_reflns_used 893 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.8117 _cell_measurement_theta_min 2.8611 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_unetI/netI 0.2256 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 20298 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_min 2.88 _diffrn_detector_area_resol_mean 15.9914 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -52.00 67.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 20.4664 0.0000 150.0000 119 #__ type_ start__ end____ width___ exp.time_ 2 omega -26.00 -1.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 20.4664 104.0000 -104.0000 25 #__ type_ start__ end____ width___ exp.time_ 3 omega 7.00 85.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 20.4664 37.0000 0.0000 78 #__ type_ start__ end____ width___ exp.time_ 4 omega 60.00 100.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 20.4664 179.0000 150.0000 40 #__ type_ start__ end____ width___ exp.time_ 5 omega 60.00 93.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 20.4664 179.0000 -30.0000 33 #__ type_ start__ end____ width___ exp.time_ 6 omega -18.00 15.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - -21.2476 -104.0000 -25.0000 33 #__ type_ start__ end____ width___ exp.time_ 7 omega -104.00 -32.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - -21.2476 179.0000 30.0000 72 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0391750000 _diffrn_orient_matrix_UB_12 -0.0041397000 _diffrn_orient_matrix_UB_13 0.0209992000 _diffrn_orient_matrix_UB_21 0.0863982000 _diffrn_orient_matrix_UB_22 -0.0123401000 _diffrn_orient_matrix_UB_23 0.0097348000 _diffrn_orient_matrix_UB_31 0.0279785000 _diffrn_orient_matrix_UB_32 0.0323234000 _diffrn_orient_matrix_UB_33 0.0064049000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2330 _reflns_number_total 7536 _reflns_odcompleteness_completeness 74.89 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.481 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.092 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 529 _refine_ls_number_reflns 7536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3022 _refine_ls_R_factor_gt 0.0852 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0100P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1261 _refine_ls_wR_factor_ref 0.1948 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ni1 Ni 0.0000 1.5000 0.5000 0.0348(5) Uani 1 2 d S . . Ni2 Ni 0.71454(19) 0.72172(6) 0.73739(4) 0.0323(4) Uani 1 1 d . . . N3 N 0.9030(11) 0.7892(4) 0.7160(2) 0.033(2) Uani 1 1 d . . . H3 H 1.0192 0.7764 0.7270 0.039 Uiso 1 1 calc R . . N4 N 0.6684(12) 0.7893(4) 0.7870(3) 0.038(2) Uani 1 1 d . . . H4 H 0.5648 0.8124 0.7770 0.046 Uiso 1 1 calc R . . O4 O 0.0914(11) 0.8922(3) 0.2466(2) 0.050(2) Uani 1 1 d . . . O1 O 0.4953(10) 0.7633(3) 0.6922(2) 0.0422(19) Uani 1 1 d . . . C11 C 0.3998(14) 0.8150(5) 0.6967(4) 0.039(3) Uani 1 1 d . . . O2 O 0.3330(10) 0.8319(3) 0.7328(2) 0.045(2) Uani 1 1 d . . . C9 C 0.4836(17) 0.7127(6) 0.8300(4) 0.065(4) Uani 1 1 d . . . H9A H 0.3735 0.7309 0.8134 0.078 Uiso 1 1 calc R . . H9B H 0.4523 0.7042 0.8607 0.078 Uiso 1 1 calc R . . O5 O 0.1139(10) 1.4046(3) 0.5018(2) 0.043(2) Uani 1 1 d . . . N1 N 0.5338(12) 0.6526(4) 0.7586(3) 0.041(2) Uani 1 1 d . . . H1 H 0.4176 0.6652 0.7475 0.049 Uiso 1 1 calc R . . C36 C 0.1162(15) 1.2022(5) 0.4845(3) 0.047(3) Uani 1 1 d . . . H36 H 0.0299 1.1825 0.4636 0.056 Uiso 1 1 calc R . . O3 O -0.0673(10) 0.8174(3) 0.2826(2) 0.0404(19) Uani 1 1 d . . . C12 C 0.3696(13) 0.8582(5) 0.6554(3) 0.032(3) Uani 1 1 d . . . C32 C 0.3809(15) 1.1953(4) 0.5387(3) 0.038(3) Uani 1 1 d . . . H32 H 0.4741 1.1711 0.5547 0.046 Uiso 1 1 calc R . . C24 C 0.1676(14) 0.9621(4) 0.4120(3) 0.027(2) Uani 1 1 d . . . C33 C 0.3728(15) 1.2629(5) 0.5449(3) 0.043(3) Uani 1 1 d . . . H33 H 0.4619 1.2833 0.5647 0.051 Uiso 1 1 calc R . . C29 C 0.0940(14) 0.8993(5) 0.4092(3) 0.035(3) Uani 1 1 d . . . H29 H 0.0731 0.8764 0.4355 0.042 Uiso 1 1 calc R . . C8 C 0.6361(16) 0.7646(5) 0.8319(3) 0.047(3) Uani 1 1 d . . . H8A H 0.6012 0.8009 0.8507 0.056 Uiso 1 1 calc R . . H8B H 0.7509 0.7458 0.8458 0.056 Uiso 1 1 calc R . . N2 N 0.7624(12) 0.6547(4) 0.6869(3) 0.039(2) Uani 1 1 d . . . H2 H 0.8694 0.6329 0.6959 0.047 Uiso 1 1 calc R . . C35 C 0.1098(15) 1.2687(4) 0.4912(3) 0.043(3) Uani 1 1 d . . . H35 H 0.0193 1.2931 0.4745 0.051 Uiso 1 1 calc R . . C15 C 0.3166(13) 0.9396(4) 0.5788(3) 0.028(2) Uani 1 1 d . . . C14 C 0.3786(14) 0.8748(5) 0.5752(3) 0.039(3) Uani 1 1 d . . . H14 H 0.4037 0.8580 0.5471 0.047 Uiso 1 1 calc R . . C4 C 0.9435(14) 0.7319(5) 0.6445(3) 0.045(3) Uani 1 1 d . . . H4A H 0.9769 0.7405 0.6140 0.054 Uiso 1 1 calc R . . H4B H 1.0513 0.7122 0.6611 0.054 Uiso 1 1 calc R . . C25 C 0.1939(13) 0.9937(4) 0.3715(3) 0.029(2) Uani 1 1 d . . . H25 H 0.2424 1.0361 0.3727 0.035 Uiso 1 1 calc R . . C3 C 0.7862(16) 0.6820(5) 0.6419(4) 0.052(3) Uani 1 1 d . . . H3A H 0.6713 0.7030 0.6301 0.062 Uiso 1 1 calc R . . H3B H 0.8139 0.6469 0.6213 0.062 Uiso 1 1 calc R . . C18 C 0.2886(13) 0.9821(4) 0.5378(3) 0.028(2) Uani 1 1 d . . . C26 C 0.1512(14) 0.9650(5) 0.3288(3) 0.035(3) Uani 1 1 d . . . H26 H 0.1703 0.9882 0.3026 0.041 Uiso 1 1 calc R . . C13 C 0.4028(14) 0.8351(5) 0.6139(3) 0.034(3) Uani 1 1 d . . . H13 H 0.4425 0.7919 0.6111 0.041 Uiso 1 1 calc R . . C34 C 0.2332(14) 1.3007(4) 0.5219(3) 0.029(2) Uani 1 1 d U . . C28 C 0.0507(13) 0.8700(5) 0.3666(3) 0.035(3) Uani 1 1 d . . . H28 H 0.0003 0.8279 0.3654 0.042 Uiso 1 1 calc R . . C10 C 0.5291(15) 0.6469(5) 0.8081(3) 0.048(3) Uani 1 1 d . . . H10A H 0.6492 0.6314 0.8211 0.058 Uiso 1 1 calc R . . H10B H 0.4359 0.6146 0.8148 0.058 Uiso 1 1 calc R . . C17 C 0.3077(13) 0.9213(5) 0.6589(3) 0.038(3) Uani 1 1 d . . . H17 H 0.2799 0.9373 0.6871 0.046 Uiso 1 1 calc R . . C31 C 0.2513(15) 1.1632(5) 0.5088(3) 0.034(3) Uani 1 1 d . . . C30 C 0.0322(14) 0.8689(5) 0.2811(4) 0.038(3) Uani 1 1 d . . . C5 C 0.9045(15) 0.7973(5) 0.6667(3) 0.045(3) Uani 1 1 d . . . H5A H 0.9996 0.8289 0.6601 0.055 Uiso 1 1 calc R . . H5B H 0.7847 0.8141 0.6543 0.055 Uiso 1 1 calc R . . N7 N -0.0509(12) 1.4873(4) 0.4309(3) 0.039(2) Uani 1 1 d . . . H7 H -0.1245 1.5213 0.4204 0.047 Uiso 1 1 calc R . . O6 O 0.3020(11) 1.3968(3) 0.5642(3) 0.058(2) Uani 1 1 d . . . C27 C 0.0804(13) 0.9016(5) 0.3262(3) 0.027(2) Uani 1 1 d U . . C7 C 0.8279(15) 0.8353(5) 0.7872(3) 0.047(3) Uani 1 1 d . . . H7A H 0.9389 0.8151 0.8020 0.056 Uiso 1 1 calc R . . H7B H 0.8013 0.8751 0.8036 0.056 Uiso 1 1 calc R . . C16 C 0.2859(14) 0.9614(5) 0.6218(3) 0.034(3) Uani 1 1 d U . . H16 H 0.2491 1.0047 0.6256 0.041 Uiso 1 1 calc R . . N6 N -0.2518(12) 1.4602(4) 0.5144(3) 0.039(2) Uani 1 1 d . . . H6 H -0.3374 1.4931 0.5104 0.047 Uiso 1 1 calc R . . C6 C 0.8585(16) 0.8516(5) 0.7387(4) 0.052(3) Uani 1 1 d . . . H6A H 0.7471 0.8712 0.7237 0.063 Uiso 1 1 calc R . . H6B H 0.9607 0.8825 0.7375 0.063 Uiso 1 1 calc R . . C2 C 0.6068(16) 0.6065(5) 0.6873(4) 0.057(4) Uani 1 1 d . . . H2A H 0.6382 0.5668 0.6714 0.069 Uiso 1 1 calc R . . H2B H 0.4946 0.6249 0.6720 0.069 Uiso 1 1 calc R . . C40 C -0.1462(15) 1.4261(5) 0.4160(4) 0.049(3) Uani 1 1 d . . . H40A H -0.0671 1.3889 0.4250 0.059 Uiso 1 1 calc R . . H40B H -0.1653 1.4260 0.3832 0.059 Uiso 1 1 calc R . . C21 C 0.2105(12) 1.0610(4) 0.4618(3) 0.030(2) Uani 1 1 d . . . H21 H 0.1794 1.0873 0.4366 0.035 Uiso 1 1 calc R . . C37 C 0.2176(15) 1.3725(5) 0.5302(4) 0.038(3) Uani 1 1 d . . . C38 C -0.3232(15) 1.4053(5) 0.4858(4) 0.046(3) Uani 1 1 d . . . H38A H -0.4479 1.3946 0.4937 0.055 Uiso 1 1 calc R . . H38B H -0.2451 1.3671 0.4927 0.055 Uiso 1 1 calc R . . C20 C 0.2541(13) 1.0908(4) 0.5036(3) 0.025(2) Uani 1 1 d . . . C19 C 0.2957(13) 1.0504(4) 0.5409(3) 0.031(3) Uani 1 1 d . . . H19 H 0.3295 1.0696 0.5689 0.037 Uiso 1 1 calc R . . C1 C 0.5722(16) 0.5898(5) 0.7363(4) 0.057(4) Uani 1 1 d . . . H1A H 0.4665 0.5603 0.7371 0.069 Uiso 1 1 calc R . . H1B H 0.6810 0.5687 0.7515 0.069 Uiso 1 1 calc R . . C23 C 0.2470(13) 0.9544(5) 0.4957(3) 0.031(2) Uani 1 1 d U . . H23 H 0.2420 0.9089 0.4932 0.037 Uiso 1 1 calc R . . C39 C -0.3304(16) 1.4181(6) 0.4355(4) 0.058(4) Uani 1 1 d . . . H39A H -0.3964 1.3821 0.4199 0.070 Uiso 1 1 calc R . . H39B H -0.4030 1.4577 0.4290 0.070 Uiso 1 1 calc R . . C22 C 0.2121(12) 0.9928(4) 0.4566(3) 0.021(2) Uani 1 1 d U . . C41 C 0.1360(17) 1.4967(5) 0.4130(3) 0.056(3) Uani 1 1 d . . . H41A H 0.2106 1.4573 0.4180 0.067 Uiso 1 1 calc R . . H41B H 0.1211 1.5052 0.3807 0.067 Uiso 1 1 calc R . . C42 C 0.2313(16) 1.5537(6) 0.4371(4) 0.059(4) Uani 1 1 d . . . H42A H 0.3529 1.5606 0.4259 0.071 Uiso 1 1 calc R . . H42B H 0.1581 1.5933 0.4314 0.071 Uiso 1 1 calc R . . O2W O 0.3847(10) 1.4596(3) 0.6512(2) 0.061(2) Uani 1 1 d D . . H2WA H 0.4978 1.4466 0.6628 0.091 Uiso 1 1 d RD . . H2WB H 0.3636 1.4318 0.6275 0.091 Uiso 1 1 d RD . . O1W O 0.2864(12) 0.9293(4) 0.7985(3) 0.100(3) Uani 1 1 d D . . H1WA H 0.3066 0.8975 0.7785 0.149 Uiso 1 1 d RD . . H1WB H 0.1689 0.9223 0.8048 0.149 Uiso 1 1 d RD . . O3W O 0.0597(11) 1.0056(3) 0.1987(2) 0.072(3) Uani 1 1 d D . . H3WA H 0.0996 0.9724 0.2165 0.108 Uiso 1 1 d RD . . H3WB H 0.1555 1.0138 0.1821 0.108 Uiso 1 1 d RD . . 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 Ni1 0.0400(13) 0.0265(11) 0.0378(12) -0.0021(9) 0.0028(9) -0.0002(10) Ni2 0.0361(8) 0.0298(8) 0.0305(8) 0.0010(6) 0.0006(6) 0.0004(7) N3 0.033(5) 0.043(6) 0.023(5) 0.003(4) 0.008(4) 0.001(5) N4 0.054(6) 0.035(5) 0.026(5) 0.003(4) 0.000(4) 0.005(5) O4 0.071(6) 0.050(5) 0.030(5) -0.001(4) 0.013(4) -0.021(4) O1 0.048(5) 0.036(4) 0.043(5) 0.012(4) 0.003(4) 0.005(4) C11 0.023(7) 0.046(8) 0.046(8) 0.009(6) -0.012(6) -0.002(6) O2 0.045(5) 0.065(5) 0.026(4) 0.012(4) 0.013(4) 0.016(4) C9 0.076(10) 0.083(10) 0.037(8) 0.020(7) 0.017(7) 0.008(9) O5 0.049(5) 0.024(4) 0.054(5) 0.000(4) -0.015(4) 0.008(4) N1 0.042(6) 0.040(6) 0.040(6) 0.007(5) 0.001(5) -0.002(5) C36 0.059(8) 0.038(7) 0.040(7) 0.008(5) -0.020(6) 0.021(6) O3 0.048(5) 0.042(5) 0.031(4) -0.008(3) -0.002(4) -0.007(4) C12 0.022(6) 0.041(7) 0.032(7) 0.004(5) -0.010(5) 0.007(5) C32 0.051(8) 0.022(6) 0.040(7) -0.004(5) -0.003(6) 0.003(6) C24 0.039(7) 0.016(5) 0.028(6) 0.004(4) 0.007(5) -0.002(5) C33 0.051(8) 0.034(7) 0.040(7) -0.004(5) -0.013(6) -0.001(6) C29 0.049(8) 0.035(6) 0.021(6) 0.005(5) 0.000(5) 0.006(6) C8 0.061(9) 0.053(8) 0.024(7) -0.003(6) -0.007(6) 0.015(7) N2 0.044(6) 0.036(5) 0.038(6) -0.004(4) 0.001(5) 0.013(5) C35 0.066(8) 0.018(6) 0.042(7) -0.004(5) -0.007(6) 0.015(6) C15 0.033(6) 0.024(6) 0.026(6) -0.003(5) -0.004(5) 0.002(5) C14 0.052(8) 0.039(7) 0.027(6) -0.001(5) 0.007(5) -0.008(6) C4 0.042(7) 0.064(8) 0.030(7) 0.017(6) 0.014(5) 0.005(7) C25 0.032(6) 0.017(5) 0.038(7) -0.010(5) -0.002(5) -0.006(5) C3 0.061(9) 0.046(8) 0.049(8) -0.008(6) 0.005(7) 0.000(7) C18 0.036(6) 0.020(6) 0.027(6) 0.003(4) -0.001(5) 0.015(5) C26 0.047(7) 0.029(6) 0.027(6) -0.002(5) 0.001(5) 0.005(5) C13 0.037(7) 0.033(6) 0.032(7) 0.015(5) 0.002(5) 0.003(5) C34 0.034(6) 0.023(5) 0.030(5) 0.002(4) 0.005(4) 0.015(4) C28 0.039(7) 0.025(6) 0.040(7) 0.002(5) -0.007(5) -0.003(5) C10 0.039(7) 0.069(9) 0.039(7) 0.019(6) 0.018(6) -0.007(7) C17 0.035(7) 0.046(7) 0.033(7) -0.004(5) -0.009(5) 0.007(6) C31 0.059(8) 0.029(6) 0.018(6) 0.004(5) 0.015(5) -0.010(6) C30 0.024(6) 0.036(7) 0.050(8) -0.016(6) -0.017(6) -0.003(6) C5 0.037(7) 0.055(8) 0.045(8) 0.011(6) 0.008(6) -0.007(6) N7 0.046(6) 0.034(6) 0.035(5) 0.002(4) -0.003(5) 0.000(5) O6 0.058(6) 0.046(5) 0.067(6) -0.021(4) -0.020(5) 0.011(4) C27 0.024(4) 0.031(4) 0.026(4) -0.004(3) 0.003(3) 0.005(4) C7 0.047(8) 0.041(7) 0.053(8) -0.018(6) 0.007(6) -0.010(6) C16 0.038(4) 0.031(4) 0.033(4) -0.007(4) 0.005(4) 0.002(4) N6 0.036(6) 0.047(6) 0.036(6) -0.003(4) 0.016(4) -0.006(5) C6 0.060(9) 0.038(7) 0.060(9) -0.005(6) 0.017(7) -0.021(6) C2 0.055(9) 0.032(7) 0.084(10) -0.013(7) -0.001(7) -0.005(7) C40 0.058(9) 0.031(7) 0.060(8) -0.009(6) 0.012(7) 0.001(6) C21 0.022(6) 0.024(6) 0.044(7) -0.001(5) 0.005(5) 0.007(5) C37 0.033(7) 0.022(6) 0.058(8) -0.008(6) -0.006(6) 0.007(5) C38 0.035(7) 0.042(7) 0.064(9) -0.005(6) 0.017(6) -0.012(6) C20 0.032(6) 0.014(5) 0.030(6) 0.008(4) -0.003(5) 0.006(5) C19 0.032(6) 0.031(6) 0.030(6) 0.007(5) 0.003(5) 0.000(5) C1 0.064(9) 0.029(7) 0.078(10) 0.002(6) 0.005(8) -0.016(7) C23 0.038(4) 0.027(4) 0.027(4) 0.004(4) 0.007(4) 0.004(4) C39 0.054(9) 0.055(8) 0.066(9) -0.002(7) 0.004(7) -0.022(7) C22 0.022(4) 0.019(4) 0.024(4) -0.005(3) 0.005(3) -0.004(3) C41 0.081(10) 0.061(8) 0.029(7) -0.005(6) 0.018(6) -0.011(8) C42 0.056(9) 0.076(10) 0.050(8) -0.015(7) 0.035(7) -0.014(7) O2W 0.056(6) 0.069(5) 0.055(5) -0.007(4) -0.009(4) 0.007(5) O1W 0.074(7) 0.118(8) 0.104(8) -0.055(6) -0.008(6) 0.002(6) O3W 0.095(7) 0.046(5) 0.079(6) 0.002(4) 0.026(5) -0.006(5) _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 Ni1 O5 2.106(6) . ? Ni1 O5 2.106(6) 3_586 ? Ni1 N7 2.064(8) . ? Ni1 N7 2.064(8) 3_586 ? Ni1 N6 2.060(8) . ? Ni1 N6 2.060(8) 3_586 ? Ni2 N3 2.065(8) . ? Ni2 N4 2.058(8) . ? Ni2 O1 2.156(7) . ? Ni2 N1 2.048(8) . ? Ni2 O3 2.132(7) 4_676 ? Ni2 N2 2.073(8) . ? N3 C5 1.470(11) . ? N3 C6 1.482(11) . ? N4 C8 1.455(11) . ? N4 C7 1.481(12) . ? O4 C30 1.233(12) . ? O1 C11 1.269(11) . ? C11 O2 1.254(12) . ? C11 C12 1.510(13) . ? C9 C8 1.520(14) . ? C9 C10 1.534(14) . ? O5 C37 1.261(11) . ? N1 C10 1.473(11) . ? N1 C1 1.474(11) . ? C36 C35 1.368(12) . ? C36 C31 1.406(12) . ? O3 Ni2 2.132(7) 4_475 ? O3 C30 1.271(11) . ? C12 C13 1.353(12) . ? C12 C17 1.366(12) . ? C32 C33 1.388(12) . ? C32 C31 1.394(12) . ? C24 C29 1.384(12) . ? C24 C25 1.388(12) . ? C24 C22 1.470(11) . ? C33 C34 1.397(12) . ? C29 C28 1.406(12) . ? N2 C3 1.467(12) . ? N2 C2 1.490(12) . ? C35 C34 1.382(12) . ? C15 C14 1.398(12) . ? C15 C18 1.490(11) . ? C15 C16 1.383(12) . ? C14 C13 1.402(12) . ? C4 C3 1.516(13) . ? C4 C5 1.519(12) . ? C25 C26 1.403(11) . ? C18 C19 1.393(12) . ? C18 C23 1.377(11) . ? C26 C27 1.385(12) . ? C34 C37 1.486(12) . ? C28 C27 1.390(12) . ? C17 C16 1.366(12) . ? C31 C20 1.480(12) . ? C30 C27 1.506(13) . ? N7 C40 1.472(11) . ? N7 C41 1.498(13) . ? O6 C37 1.235(11) . ? C7 C6 1.508(13) . ? N6 C38 1.469(11) . ? N6 C42 1.460(12) 3_586 ? C2 C1 1.529(14) . ? C40 C39 1.497(14) . ? C21 C20 1.392(11) . ? C21 C22 1.396(11) . ? C38 C39 1.509(13) . ? C20 C19 1.388(11) . ? C23 C22 1.403(11) . ? C41 C42 1.497(13) . ? C42 N6 1.460(12) 3_586 ? 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 O5 Ni1 O5 179.998(5) . 3_586 ? N7 Ni1 O5 86.9(3) . . ? N7 Ni1 O5 93.1(3) 3_586 . ? N7 Ni1 O5 86.9(3) 3_586 3_586 ? N7 Ni1 O5 93.1(3) . 3_586 ? N7 Ni1 N7 179.998(5) 3_586 . ? N6 Ni1 O5 88.9(3) 3_586 3_586 ? N6 Ni1 O5 91.1(3) . 3_586 ? N6 Ni1 O5 91.1(3) 3_586 . ? N6 Ni1 O5 88.9(3) . . ? N6 Ni1 N7 93.9(3) 3_586 3_586 ? N6 Ni1 N7 86.1(3) . 3_586 ? N6 Ni1 N7 86.1(3) 3_586 . ? N6 Ni1 N7 93.9(3) . . ? N6 Ni1 N6 179.999(1) . 3_586 ? N3 Ni2 O1 90.9(3) . . ? N3 Ni2 O3 88.4(3) . 4_676 ? N3 Ni2 N2 93.7(3) . . ? N4 Ni2 N3 85.6(3) . . ? N4 Ni2 O1 91.7(3) . . ? N4 Ni2 O3 87.4(3) . 4_676 ? N4 Ni2 N2 179.2(4) . . ? N1 Ni2 N3 178.2(3) . . ? N1 Ni2 N4 95.5(3) . . ? N1 Ni2 O1 90.5(3) . . ? N1 Ni2 O3 90.3(3) . 4_676 ? N1 Ni2 N2 85.2(3) . . ? O3 Ni2 O1 178.9(3) 4_676 . ? N2 Ni2 O1 88.1(3) . . ? N2 Ni2 O3 92.9(3) . 4_676 ? C5 N3 Ni2 115.9(6) . . ? C5 N3 C6 111.9(8) . . ? C6 N3 Ni2 105.0(6) . . ? C8 N4 Ni2 117.9(6) . . ? C8 N4 C7 113.3(8) . . ? C7 N4 Ni2 104.7(6) . . ? C11 O1 Ni2 129.3(7) . . ? O1 C11 C12 116.1(10) . . ? O2 C11 O1 124.5(10) . . ? O2 C11 C12 119.4(10) . . ? C8 C9 C10 116.3(10) . . ? C37 O5 Ni1 134.6(7) . . ? C10 N1 Ni2 115.2(6) . . ? C10 N1 C1 113.4(8) . . ? C1 N1 Ni2 108.2(7) . . ? C35 C36 C31 120.9(10) . . ? C30 O3 Ni2 132.3(7) . 4_475 ? C13 C12 C11 120.5(9) . . ? C13 C12 C17 118.7(9) . . ? C17 C12 C11 120.7(10) . . ? C33 C32 C31 121.0(10) . . ? C29 C24 C25 116.9(9) . . ? C29 C24 C22 120.1(8) . . ? C25 C24 C22 123.0(8) . . ? C32 C33 C34 121.1(9) . . ? C24 C29 C28 120.1(9) . . ? N4 C8 C9 111.9(8) . . ? C3 N2 Ni2 116.4(6) . . ? C3 N2 C2 113.7(8) . . ? C2 N2 Ni2 104.9(6) . . ? C36 C35 C34 122.3(10) . . ? C14 C15 C18 120.5(9) . . ? C16 C15 C14 116.6(9) . . ? C16 C15 C18 122.9(9) . . ? C15 C14 C13 120.0(9) . . ? C3 C4 C5 116.4(9) . . ? C24 C25 C26 123.4(9) . . ? N2 C3 C4 110.4(9) . . ? C19 C18 C15 121.5(8) . . ? C23 C18 C15 120.3(8) . . ? C23 C18 C19 118.1(8) . . ? C27 C26 C25 119.4(9) . . ? C12 C13 C14 121.4(10) . . ? C33 C34 C37 121.4(9) . . ? C35 C34 C33 117.3(8) . . ? C35 C34 C37 121.3(9) . . ? C27 C28 C29 122.5(9) . . ? N1 C10 C9 112.0(8) . . ? C12 C17 C16 120.9(10) . . ? C36 C31 C20 121.5(9) . . ? C32 C31 C36 117.3(9) . . ? C32 C31 C20 121.2(9) . . ? O4 C30 O3 125.3(10) . . ? O4 C30 C27 119.6(10) . . ? O3 C30 C27 115.0(10) . . ? N3 C5 C4 110.3(8) . . ? C40 N7 Ni1 116.4(6) . . ? C40 N7 C41 114.3(8) . . ? C41 N7 Ni1 104.0(6) . . ? C26 C27 C28 117.6(9) . . ? C26 C27 C30 121.2(9) . . ? C28 C27 C30 121.2(9) . . ? N4 C7 C6 108.0(8) . . ? C17 C16 C15 122.2(10) . . ? C38 N6 Ni1 116.8(6) . . ? C42 N6 Ni1 105.1(7) 3_586 . ? C42 N6 C38 115.0(8) 3_586 . ? N3 C6 C7 107.3(8) . . ? N2 C2 C1 109.6(9) . . ? N7 C40 C39 112.4(9) . . ? C20 C21 C22 121.9(8) . . ? O5 C37 C34 116.5(9) . . ? O6 C37 O5 124.1(9) . . ? O6 C37 C34 119.4(9) . . ? N6 C38 C39 114.8(9) . . ? C21 C20 C31 121.4(8) . . ? C19 C20 C31 120.7(9) . . ? C19 C20 C21 117.9(8) . . ? C20 C19 C18 122.3(9) . . ? N1 C1 C2 106.4(8) . . ? C18 C23 C22 122.0(9) . . ? C40 C39 C38 116.0(10) . . ? C21 C22 C24 121.2(8) . . ? C21 C22 C23 117.7(8) . . ? C23 C22 C24 121.0(8) . . ? C42 C41 N7 108.7(9) . . ? N6 C42 C41 108.9(9) 3_586 . ? _symmetry_cell_setting ? _symmetry_space_group_name_h-m ? _symmetry_int_tables_number ? _chemical_absolute_configuration ? # Attachment '8685_web_deposit_cif_file_1_YaroslawD.Lampeka_ #1324039133.NiL2_BTC.cif' data_NiL2_BTC _database_code_depnum_ccdc_archive 'CCDC 834623' #TrackingRef '8685_web_deposit_cif_file_1_YaroslawD.Lampeka_ #1324039133.NiL2_BTC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(\m~3~-Benzene-1,3,5-tricarboxylato-O,O',O'')-tris((3-methyl-1, 3,5,8,12-penta-azacyclotetradecane)-nickel(ii)) decahydrate) ; _chemical_name_common ; catena-(bis(mu!3$-Benzene-1,3,5-tricarboxylato-O,O',O'')- tris((3-methyl-1, 3,5,8,12-penta-azacyclotetradecane)-nickel(ii)) decahydrate) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H101.50 N15 Ni3 O22.25' _chemical_formula_weight 1421.07 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 9.2825(7) _cell_length_b 27.248(2) _cell_length_c 16.1584(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.808(4) _cell_angle_gamma 90.00 _cell_volume 4038.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6930 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 29.55 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1513 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6183 _exptl_absorpt_correction_T_max 0.9279 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95328 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.10 _reflns_number_total 6365 _reflns_number_gt 5348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; DELU 0.01 0.01 SIMU 0.04 0.08 1.7 ISOR 0.001 0.002 O7 ISOR 0.001 0.002 O8 ISOR 0.001 0.002 O9 ISOR 0.001 0.002 O10 EADP N8 C24 EXYZ N8 C24 Most restraints were needed because of the presence of disordered water molecules, EADP and EXYZ were used because of the disorder observed in the macrocyclic ligand. Both DELU and SIMU were used to improve the data to parameter ratio. 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^)+(0.0802P)^2^+90.9843P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6365 _refine_ls_number_parameters 449 _refine_ls_number_restraints 393 _refine_ls_R_factor_all 0.1456 _refine_ls_R_factor_gt 0.1299 _refine_ls_wR_factor_ref 0.3195 _refine_ls_wR_factor_gt 0.3133 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni2 Ni 0.56712(13) 0.24774(5) 0.87340(8) 0.0297(4) Uani 1 1 d U . . N1 N 0.6955(12) 0.2570(5) 0.7814(6) 0.063(2) Uani 1 1 d U . . H1 H 0.7919 0.2593 0.8074 0.076 Uiso 1 1 calc R . . N2 N 0.5232(10) 0.3215(4) 0.8582(7) 0.057(2) Uani 1 1 d U . . H2 H 0.4336 0.3239 0.8238 0.069 Uiso 1 1 calc R . . N3 N 0.4337(9) 0.2377(4) 0.9622(5) 0.051(2) Uani 1 1 d U . . H3 H 0.3385 0.2336 0.9352 0.062 Uiso 1 1 calc R . . N4 N 0.6129(10) 0.1738(4) 0.8864(6) 0.052(2) Uani 1 1 d U . . H4 H 0.7035 0.1710 0.9198 0.062 Uiso 1 1 calc R . . N5 N 0.7229(15) 0.1679(6) 0.7593(10) 0.096(4) Uani 1 1 d U . . C10 C 0.6538(18) 0.3041(6) 0.7448(9) 0.083(4) Uani 1 1 d U . . H10A H 0.5627 0.3006 0.7045 0.099 Uiso 1 1 calc R . . H10B H 0.7309 0.3161 0.7138 0.099 Uiso 1 1 calc R . . C11 C 0.6309(16) 0.3406(5) 0.8103(9) 0.077(3) Uani 1 1 d U . . H11A H 0.7239 0.3466 0.8478 0.093 Uiso 1 1 calc R . . H11B H 0.5967 0.3720 0.7837 0.093 Uiso 1 1 calc R . . C12 C 0.5085(14) 0.3481(5) 0.9344(10) 0.079(3) Uani 1 1 d U . . H12A H 0.4806 0.3825 0.9198 0.094 Uiso 1 1 calc R . . H12B H 0.6042 0.3488 0.9712 0.094 Uiso 1 1 calc R . . C13 C 0.3979(15) 0.3261(7) 0.9814(11) 0.093(4) Uani 1 1 d U . . H13A H 0.3777 0.3500 1.0244 0.112 Uiso 1 1 calc R . . H13B H 0.3063 0.3216 0.9418 0.112 Uiso 1 1 calc R . . C14 C 0.4365(15) 0.2790(7) 1.0230(9) 0.082(4) Uani 1 1 d U . . H14A H 0.3672 0.2719 1.0623 0.098 Uiso 1 1 calc R . . H14B H 0.5353 0.2815 1.0560 0.098 Uiso 1 1 calc R . . C15 C 0.4851(17) 0.1902(6) 1.0015(9) 0.078(3) Uani 1 1 d U . . H15A H 0.4130 0.1776 1.0355 0.094 Uiso 1 1 calc R . . H15B H 0.5788 0.1952 1.0390 0.094 Uiso 1 1 calc R . . C16 C 0.5051(16) 0.1534(5) 0.9338(9) 0.072(3) Uani 1 1 d U . . H16A H 0.5397 0.1217 0.9592 0.086 Uiso 1 1 calc R . . H16B H 0.4115 0.1479 0.8965 0.086 Uiso 1 1 calc R . . C17 C 0.6208(15) 0.1470(5) 0.8096(9) 0.072(3) Uani 1 1 d U . . H17A H 0.5226 0.1461 0.7756 0.086 Uiso 1 1 calc R . . H17B H 0.6500 0.1127 0.8239 0.086 Uiso 1 1 calc R . . C18 C 0.6864(17) 0.2162(7) 0.7218(9) 0.085(4) Uani 1 1 d U . . H18A H 0.7528 0.2231 0.6808 0.102 Uiso 1 1 calc R . . H18B H 0.5859 0.2149 0.6906 0.102 Uiso 1 1 calc R . . C19 C 0.8761(18) 0.1651(9) 0.7961(14) 0.127(7) Uani 1 1 d U . . H19A H 0.9360 0.1801 0.7580 0.191 Uiso 1 1 calc R . . H19B H 0.9043 0.1306 0.8055 0.191 Uiso 1 1 calc R . . H19C H 0.8912 0.1827 0.8497 0.191 Uiso 1 1 calc R . . Ni1 Ni 1.0000 0.5000 1.0000 0.0331(5) Uani 1 2 d SU . . N6 N 1.1274(12) 0.5264(3) 1.1049(7) 0.061(2) Uani 1 1 d U . . H6 H 1.1536 0.4998 1.1401 0.073 Uiso 1 1 calc R . . N7 N 1.1845(11) 0.5025(4) 0.9459(7) 0.065(2) Uani 1 1 d U . . H7 H 1.1793 0.5305 0.9124 0.077 Uiso 1 1 calc R . . N8 N 1.093(2) 0.4551(6) 0.8234(10) 0.097(4) Uani 0.50 1 d PU . 1 C24 C 1.093(2) 0.4551(6) 0.8234(10) 0.097(4) Uani 0.50 1 d PU . 2 H24A H 1.0040 0.4514 0.8451 0.116 Uiso 0.50 1 d PR . 2 H24B H 1.1104 0.4260 0.7934 0.116 Uiso 0.50 1 d PR . 2 C20 C 1.049(2) 0.5637(5) 1.1541(9) 0.087(4) Uani 1 1 d U . . H20A H 1.0321 0.5936 1.1226 0.105 Uiso 1 1 d R . . H20B H 1.1122 0.5711 1.2053 0.105 Uiso 1 1 d R . . C21 C 1.2597(16) 0.5456(6) 1.0802(11) 0.088(4) Uani 1 1 d U . . H21A H 1.3378 0.5479 1.1291 0.106 Uiso 1 1 calc R . . H21B H 1.2425 0.5787 1.0554 0.106 Uiso 1 1 calc R . . C22 C 1.3026(13) 0.5098(5) 1.0156(11) 0.079(3) Uani 1 1 d U . . H22A H 1.3895 0.5225 0.9939 0.094 Uiso 1 1 calc R . . H22B H 1.3287 0.4778 1.0429 0.094 Uiso 1 1 calc R . . C23 C 1.213(2) 0.4613(6) 0.8949(11) 0.094(4) Uani 1 1 d U . . H23A H 1.2229 0.4321 0.9287 0.113 Uiso 1 1 d R . . H23B H 1.3028 0.4665 0.8739 0.113 Uiso 1 1 d R . . C25 C 1.076(4) 0.4946(12) 0.7679(18) 0.096(8) Uani 0.50 1 d PU . . H25A H 0.9978 0.4873 0.7235 0.115 Uiso 0.50 1 d PR . . H25B H 1.0536 0.5240 0.7960 0.115 Uiso 0.50 1 d PR . . H25C H 1.1645 0.4992 0.7450 0.115 Uiso 0.50 1 d PR . . O1 O 0.7470(7) 0.2689(3) 0.9663(4) 0.0352(15) Uani 1 1 d U . . O2 O 1.1681(10) 0.4277(3) 1.1664(5) 0.061(2) Uani 1 1 d U . . O3 O 1.3843(7) 0.2711(3) 1.2781(4) 0.0359(16) Uani 1 1 d U . . O4 O 0.8724(9) 0.1994(3) 1.0006(6) 0.063(2) Uani 1 1 d U . . O5 O 1.0360(8) 0.4257(2) 1.0378(5) 0.0422(17) Uani 1 1 d U . . O6 O 1.2506(9) 0.2028(3) 1.2558(6) 0.068(3) Uani 1 1 d U . . C1 C 0.8521(11) 0.2450(4) 1.0065(7) 0.036(2) Uani 1 1 d U . . C2 C 0.9655(10) 0.2742(4) 1.0659(6) 0.032(2) Uani 1 1 d U . . C3 C 1.0646(10) 0.2490(4) 1.1233(6) 0.0311(19) Uani 1 1 d U . . H3A H 1.0611 0.2141 1.1253 0.037 Uiso 1 1 calc R . . C4 C 1.1717(10) 0.2747(4) 1.1795(6) 0.0285(19) Uani 1 1 d U . . C5 C 1.1787(10) 0.3253(4) 1.1715(6) 0.0294(19) Uani 1 1 d U . . H5 H 1.2504 0.3431 1.2079 0.035 Uiso 1 1 calc R . . C6 C 1.0832(10) 0.3508(4) 1.1114(6) 0.031(2) Uani 1 1 d U . . C7 C 0.9761(10) 0.3245(3) 1.0587(6) 0.0296(19) Uani 1 1 d U . . H7A H 0.9103 0.3415 1.0177 0.035 Uiso 1 1 calc R . . C8 C 1.0964(11) 0.4058(4) 1.1048(6) 0.037(2) Uani 1 1 d U . . C9 C 1.2764(10) 0.2473(4) 1.2416(7) 0.037(2) Uani 1 1 d U . . O7 O 0.3125(17) 0.5918(6) 0.8725(10) 0.049(4) Uani 0.50 1 d PU . . O8 O 0.0090(19) 0.2848(7) 0.8507(11) 0.058(4) Uani 0.50 1 d PU . . O9 O 0.878(4) 0.1273(13) 1.126(2) 0.055(9) Uani 0.25 1 d PU . . O10 O 0.142(2) 0.1893(9) 0.9247(15) 0.022(5) Uiso 0.25 1 d PU A 1 O10X O 0.147(3) 0.1699(11) 0.9644(19) 0.042(7) Uiso 0.25 1 d PU B 2 O11 O 1.158(2) 0.4054(7) 1.3406(11) 0.061(5) Uiso 0.50 1 d PU . . O12 O 0.5276(19) 0.5430(7) 0.7992(11) 0.061(5) Uiso 0.50 1 d P . . O13 O 1.230(4) 0.1261(14) 1.143(2) 0.062(9) Uiso 0.25 1 d PU . . O14 O 0.684(4) 0.0597(15) 1.138(2) 0.070(10) Uiso 0.25 1 d P . . O15 O -0.027(5) 0.3152(16) 0.801(3) 0.077(11) Uiso 0.25 1 d PU . . O O 1.190(4) 0.1154(13) 1.200(2) 0.062(9) Uiso 0.25 1 d PU . . O0AA O 0.885(4) 0.1156(15) 1.087(3) 0.065(10) Uiso 0.25 1 d PU . . O1AA O 0.467(5) 0.4463(19) 0.724(3) 0.098(14) Uiso 0.25 1 d P . . O3AA O 0.381(5) 0.4328(18) 0.607(3) 0.094(14) Uiso 0.25 1 d P . . O2AA O 1.351(6) 0.465(2) 1.432(3) 0.036(12) Uiso 0.13 1 d PU . . O4AA O 0.901(8) 0.049(3) 0.945(4) 0.059(18) Uiso 0.13 1 d P . . O5AA O 0.613(6) 0.026(2) 0.869(4) 0.043(14) Uiso 0.13 1 d P . . O6AA O 1.272(6) 0.499(2) 1.493(3) 0.034(12) Uiso 0.13 1 d PU . . O7AA O 1.217(12) 0.437(4) 1.328(7) 0.11(3) Uiso 0.13 1 d PU . . 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 Ni2 0.0220(6) 0.0382(7) 0.0276(7) -0.0111(5) -0.0007(5) -0.0046(5) N1 0.048(6) 0.103(6) 0.039(5) -0.007(4) 0.009(4) -0.020(5) N2 0.040(5) 0.047(4) 0.073(6) -0.012(4) -0.032(4) -0.005(4) N3 0.023(4) 0.099(6) 0.028(4) -0.011(4) -0.009(3) -0.009(4) N4 0.042(5) 0.045(4) 0.062(6) -0.013(4) -0.015(4) -0.003(4) N5 0.062(7) 0.126(8) 0.100(9) -0.065(7) 0.010(6) 0.011(7) C10 0.085(10) 0.108(8) 0.047(7) 0.015(5) -0.012(6) -0.055(8) C11 0.074(8) 0.066(6) 0.076(8) 0.018(5) -0.039(6) -0.038(6) C12 0.044(7) 0.057(7) 0.121(9) -0.049(6) -0.030(6) 0.012(6) C13 0.044(7) 0.122(9) 0.108(10) -0.081(8) -0.006(6) 0.023(7) C14 0.047(7) 0.152(9) 0.049(7) -0.051(7) 0.019(6) -0.010(8) C15 0.066(9) 0.110(8) 0.056(7) 0.020(6) 0.003(6) -0.033(7) C16 0.065(8) 0.061(6) 0.081(8) 0.018(6) -0.016(6) -0.030(6) C17 0.056(7) 0.063(7) 0.087(8) -0.047(6) -0.022(6) 0.013(6) C18 0.063(8) 0.145(9) 0.050(8) -0.043(6) 0.016(6) -0.016(8) C19 0.057(7) 0.18(2) 0.138(17) -0.066(14) 0.005(9) 0.021(10) Ni1 0.0263(9) 0.0263(9) 0.0413(10) 0.0036(8) -0.0113(7) 0.0017(7) N6 0.079(7) 0.032(5) 0.058(5) 0.008(4) -0.031(4) -0.010(4) N7 0.049(5) 0.062(6) 0.084(6) 0.032(5) 0.015(4) 0.017(5) N8 0.157(13) 0.064(8) 0.075(8) 0.012(6) 0.035(7) 0.041(9) C24 0.157(13) 0.064(8) 0.075(8) 0.012(6) 0.035(7) 0.041(9) C20 0.150(12) 0.041(7) 0.053(8) -0.010(6) -0.041(8) 0.013(8) C21 0.065(7) 0.068(9) 0.110(10) 0.031(6) -0.054(6) -0.030(6) C22 0.028(5) 0.068(8) 0.135(10) 0.066(6) -0.002(5) 0.007(5) C23 0.113(11) 0.087(9) 0.091(9) 0.037(6) 0.043(6) 0.058(8) C25 0.16(2) 0.081(15) 0.054(12) 0.015(11) 0.050(12) 0.056(17) O1 0.030(3) 0.038(4) 0.034(4) -0.006(3) -0.006(3) 0.002(3) O2 0.079(6) 0.030(4) 0.058(5) 0.002(4) -0.034(4) -0.001(4) O3 0.021(3) 0.043(4) 0.039(4) 0.015(3) -0.012(3) 0.003(3) O4 0.047(5) 0.036(4) 0.093(7) -0.005(4) -0.025(4) 0.004(4) O5 0.047(4) 0.025(3) 0.048(4) 0.008(3) -0.014(3) 0.005(3) O6 0.049(5) 0.042(4) 0.100(7) 0.036(5) -0.032(5) -0.005(4) C1 0.033(5) 0.036(5) 0.034(5) 0.001(4) -0.004(4) -0.008(4) C2 0.018(4) 0.038(4) 0.039(5) 0.003(4) -0.001(3) -0.002(4) C3 0.028(5) 0.028(4) 0.034(5) 0.005(4) -0.004(3) 0.001(4) C4 0.024(4) 0.036(4) 0.022(5) 0.007(4) -0.004(3) 0.000(4) C5 0.022(4) 0.034(4) 0.029(5) 0.003(4) -0.003(3) 0.000(4) C6 0.029(5) 0.030(4) 0.033(5) 0.007(4) -0.002(4) 0.005(4) C7 0.030(5) 0.032(4) 0.023(5) 0.006(4) -0.006(4) 0.005(4) C8 0.038(6) 0.036(4) 0.032(5) 0.002(4) -0.010(4) 0.001(4) C9 0.015(4) 0.043(5) 0.048(6) 0.021(5) -0.012(4) 0.001(4) O7 0.050(4) 0.049(4) 0.049(4) 0.003(2) 0.008(2) -0.002(2) O8 0.057(5) 0.059(5) 0.057(5) -0.001(2) 0.010(2) -0.001(2) O9 0.055(9) 0.055(9) 0.055(9) 0.000(2) 0.009(2) 0.000(2) _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 Ni2 N3 2.053(9) . ? Ni2 N2 2.058(10) . ? Ni2 N1 2.059(10) . ? Ni2 N4 2.063(10) . ? Ni2 O1 2.147(6) . ? Ni2 O3 2.171(6) 4_465 ? N1 C10 1.442(19) . ? N1 C18 1.463(18) . ? N1 H1 0.9300 . ? N2 C11 1.451(18) . ? N2 C12 1.453(17) . ? N2 H2 0.9300 . ? N3 C15 1.486(19) . ? N3 C14 1.492(17) . ? N3 H3 0.9300 . ? N4 C17 1.452(16) . ? N4 C16 1.460(17) . ? N4 H4 0.9300 . ? N5 C17 1.46(2) . ? N5 C19 1.46(2) . ? N5 C18 1.47(2) . ? C10 C11 1.49(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.49(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.47(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.52(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Ni1 N7 2.040(10) 3_767 ? Ni1 N7 2.040(10) . ? Ni1 N6 2.043(9) . ? Ni1 N6 2.043(9) 3_767 ? Ni1 O5 2.126(6) 3_767 ? Ni1 O5 2.126(6) . ? N6 C21 1.447(19) . ? N6 C20 1.54(2) . ? N6 H6 0.9300 . ? N7 C23 1.44(2) . ? N7 C22 1.460(18) . ? N7 H7 0.9300 . ? N8 C25 1.40(3) . ? N8 C23 1.48(2) . ? N8 C20 1.51(2) 3_767 ? N8 H24A 0.9535 . ? N8 H24B 0.9544 . ? C20 C24 1.51(2) 3_767 ? C20 N8 1.51(2) 3_767 ? C20 H20A 0.9601 . ? C20 H20B 0.9605 . ? C21 C22 1.53(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9602 . ? C23 H23B 0.9599 . ? C25 H25A 0.9597 . ? C25 H25B 0.9601 . ? C25 H25C 0.9601 . ? O1 C1 1.267(12) . ? O2 C8 1.259(12) . ? O3 C9 1.261(12) . ? O3 Ni2 2.171(6) 4_666 ? O4 C1 1.261(13) . ? O5 C8 1.263(12) . ? O6 C9 1.263(13) . ? C1 C2 1.534(13) . ? C2 C7 1.382(14) . ? C2 C3 1.385(14) . ? C3 C4 1.425(13) . ? C3 H3A 0.9500 . ? C4 C5 1.388(14) . ? C4 C9 1.487(13) . ? C5 C6 1.395(13) . ? C5 H5 0.9500 . ? C6 C7 1.402(13) . ? C6 C8 1.510(14) . ? C7 H7A 0.9500 . ? O8 O15 1.17(4) . ? O9 O0AA 0.72(4) . ? O11 O7AA 1.04(12) . ? O13 O 1.09(4) . ? O2AA O6AA 1.60(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni2 N2 94.8(5) . . ? N3 Ni2 N1 178.1(4) . . ? N2 Ni2 N1 85.5(5) . . ? N3 Ni2 N4 86.3(4) . . ? N2 Ni2 N4 178.8(5) . . ? N1 Ni2 N4 93.4(5) . . ? N3 Ni2 O1 92.0(3) . . ? N2 Ni2 O1 86.5(3) . . ? N1 Ni2 O1 89.9(4) . . ? N4 Ni2 O1 93.8(3) . . ? N3 Ni2 O3 88.5(3) . 4_465 ? N2 Ni2 O3 91.6(3) . 4_465 ? N1 Ni2 O3 89.6(4) . 4_465 ? N4 Ni2 O3 88.1(3) . 4_465 ? O1 Ni2 O3 178.1(3) . 4_465 ? C10 N1 C18 114.9(12) . . ? C10 N1 Ni2 104.8(9) . . ? C18 N1 Ni2 113.6(9) . . ? C10 N1 H1 107.7 . . ? C18 N1 H1 107.7 . . ? Ni2 N1 H1 107.7 . . ? C11 N2 C12 115.8(11) . . ? C11 N2 Ni2 105.8(9) . . ? C12 N2 Ni2 115.4(9) . . ? C11 N2 H2 106.4 . . ? C12 N2 H2 106.4 . . ? Ni2 N2 H2 106.4 . . ? C15 N3 C14 113.8(11) . . ? C15 N3 Ni2 103.1(8) . . ? C14 N3 Ni2 114.0(8) . . ? C15 N3 H3 108.6 . . ? C14 N3 H3 108.6 . . ? Ni2 N3 H3 108.6 . . ? C17 N4 C16 112.7(11) . . ? C17 N4 Ni2 116.2(9) . . ? C16 N4 Ni2 106.1(8) . . ? C17 N4 H4 107.1 . . ? C16 N4 H4 107.1 . . ? Ni2 N4 H4 107.1 . . ? C17 N5 C19 115.5(17) . . ? C17 N5 C18 116.9(12) . . ? C19 N5 C18 111.4(17) . . ? N1 C10 C11 111.2(11) . . ? N1 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N1 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C10 109.0(11) . . ? N2 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? N2 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N2 C12 C13 113.0(11) . . ? N2 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N2 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 116.5(12) . . ? C14 C13 H13A 108.2 . . ? C12 C13 H13A 108.2 . . ? C14 C13 H13B 108.2 . . ? C12 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? C13 C14 N3 112.4(12) . . ? C13 C14 H14A 109.1 . . ? N3 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? N3 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? N3 C15 C16 109.5(11) . . ? N3 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? N3 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C15 107.2(10) . . ? N4 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? N4 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.5 . . ? N4 C17 N5 113.7(11) . . ? N4 C17 H17A 108.8 . . ? N5 C17 H17A 108.8 . . ? N4 C17 H17B 108.8 . . ? N5 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N1 C18 N5 114.9(12) . . ? N1 C18 H18A 108.5 . . ? N5 C18 H18A 108.5 . . ? N1 C18 H18B 108.5 . . ? N5 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N7 Ni1 N7 179.999(3) 3_767 . ? N7 Ni1 N6 94.2(5) 3_767 . ? N7 Ni1 N6 85.8(5) . . ? N7 Ni1 N6 85.8(5) 3_767 3_767 ? N7 Ni1 N6 94.2(5) . 3_767 ? N6 Ni1 N6 179.999(3) . 3_767 ? N7 Ni1 O5 92.9(4) 3_767 3_767 ? N7 Ni1 O5 87.1(4) . 3_767 ? N6 Ni1 O5 87.1(3) . 3_767 ? N6 Ni1 O5 92.9(3) 3_767 3_767 ? N7 Ni1 O5 87.1(4) 3_767 . ? N7 Ni1 O5 92.9(4) . . ? N6 Ni1 O5 92.9(3) . . ? N6 Ni1 O5 87.1(3) 3_767 . ? O5 Ni1 O5 180.0(4) 3_767 . ? C21 N6 C20 113.2(12) . . ? C21 N6 Ni1 107.9(9) . . ? C20 N6 Ni1 113.5(8) . . ? C21 N6 H6 107.3 . . ? C20 N6 H6 107.3 . . ? Ni1 N6 H6 107.3 . . ? C23 N7 C22 111.4(12) . . ? C23 N7 Ni1 117.2(11) . . ? C22 N7 Ni1 104.7(9) . . ? C23 N7 H7 107.7 . . ? C22 N7 H7 107.7 . . ? Ni1 N7 H7 107.7 . . ? C25 N8 C23 114(2) . . ? C25 N8 C20 113(2) . 3_767 ? C23 N8 C20 115.3(13) . 3_767 ? C25 N8 H24A 107.2 . . ? C23 N8 H24A 108.3 . . ? C25 N8 H24B 109.0 . . ? C23 N8 H24B 109.1 . . ? C20 N8 H24B 93.5 3_767 . ? H24A N8 H24B 108.9 . . ? C24 C20 N6 113.7(11) 3_767 . ? N8 C20 N6 113.7(11) 3_767 . ? C24 C20 H20A 110.0 3_767 . ? N8 C20 H20A 110.0 3_767 . ? N6 C20 H20A 109.6 . . ? C24 C20 H20B 107.9 3_767 . ? N8 C20 H20B 107.9 3_767 . ? N6 C20 H20B 107.6 . . ? H20A C20 H20B 107.9 . . ? N6 C21 C22 106.1(11) . . ? N6 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? N6 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? N7 C22 C21 111.7(10) . . ? N7 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? N7 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? N7 C23 N8 110.8(12) . . ? N7 C23 H23A 109.3 . . ? N8 C23 H23A 110.2 . . ? N7 C23 H23B 109.2 . . ? N8 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? N8 C25 H25A 108.6 . . ? N8 C25 H25B 110.6 . . ? H25A C25 H25B 109.5 . . ? N8 C25 H25C 109.2 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.4 . . ? C1 O1 Ni2 132.5(6) . . ? C9 O3 Ni2 133.5(6) . 4_666 ? C8 O5 Ni1 133.2(7) . . ? O4 C1 O1 125.5(9) . . ? O4 C1 C2 117.5(9) . . ? O1 C1 C2 117.0(9) . . ? C7 C2 C3 120.0(9) . . ? C7 C2 C1 120.9(9) . . ? C3 C2 C1 118.9(9) . . ? C2 C3 C4 120.7(9) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 118.0(8) . . ? C5 C4 C9 121.8(9) . . ? C3 C4 C9 120.2(9) . . ? C4 C5 C6 121.6(9) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 119.1(9) . . ? C5 C6 C8 119.5(9) . . ? C7 C6 C8 121.4(8) . . ? C2 C7 C6 120.5(8) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? O2 C8 O5 125.8(10) . . ? O2 C8 C6 117.0(9) . . ? O5 C8 C6 117.2(9) . . ? O3 C9 O6 124.6(9) . . ? O3 C9 C4 116.6(9) . . ? O6 C9 C4 118.8(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni2 N1 C10 -14.2(8) . . . . ? N4 Ni2 N1 C10 165.6(8) . . . . ? O1 Ni2 N1 C10 -100.7(8) . . . . ? O3 Ni2 N1 C10 77.5(8) 4_465 . . . ? N2 Ni2 N1 C18 -140.4(11) . . . . ? N4 Ni2 N1 C18 39.4(11) . . . . ? O1 Ni2 N1 C18 133.1(11) . . . . ? O3 Ni2 N1 C18 -48.8(11) 4_465 . . . ? N3 Ni2 N2 C11 167.7(7) . . . . ? N1 Ni2 N2 C11 -14.1(7) . . . . ? O1 Ni2 N2 C11 76.0(7) . . . . ? O3 Ni2 N2 C11 -103.6(7) 4_465 . . . ? N3 Ni2 N2 C12 38.3(9) . . . . ? N1 Ni2 N2 C12 -143.6(9) . . . . ? O1 Ni2 N2 C12 -53.5(8) . . . . ? O3 Ni2 N2 C12 126.9(8) 4_465 . . . ? N2 Ni2 N3 C15 -162.5(8) . . . . ? N4 Ni2 N3 C15 17.8(8) . . . . ? O1 Ni2 N3 C15 -75.9(8) . . . . ? O3 Ni2 N3 C15 106.0(8) 4_465 . . . ? N2 Ni2 N3 C14 -38.7(9) . . . . ? N4 Ni2 N3 C14 141.6(9) . . . . ? O1 Ni2 N3 C14 48.0(9) . . . . ? O3 Ni2 N3 C14 -130.1(9) 4_465 . . . ? N3 Ni2 N4 C17 138.8(9) . . . . ? N1 Ni2 N4 C17 -39.3(9) . . . . ? O1 Ni2 N4 C17 -129.4(9) . . . . ? O3 Ni2 N4 C17 50.2(9) 4_465 . . . ? N3 Ni2 N4 C16 12.7(8) . . . . ? N1 Ni2 N4 C16 -165.5(8) . . . . ? O1 Ni2 N4 C16 104.4(8) . . . . ? O3 Ni2 N4 C16 -76.0(8) 4_465 . . . ? C18 N1 C10 C11 166.0(12) . . . . ? Ni2 N1 C10 C11 40.5(13) . . . . ? C12 N2 C11 C10 168.7(11) . . . . ? Ni2 N2 C11 C10 39.5(12) . . . . ? N1 C10 C11 N2 -56.2(15) . . . . ? C11 N2 C12 C13 -179.0(12) . . . . ? Ni2 N2 C12 C13 -54.6(14) . . . . ? N2 C12 C13 C14 70.8(16) . . . . ? C12 C13 C14 N3 -71.9(16) . . . . ? C15 N3 C14 C13 174.7(12) . . . . ? Ni2 N3 C14 C13 56.9(13) . . . . ? C14 N3 C15 C16 -169.4(10) . . . . ? Ni2 N3 C15 C16 -45.4(11) . . . . ? C17 N4 C16 C15 -168.4(11) . . . . ? Ni2 N4 C16 C15 -40.2(12) . . . . ? N3 C15 C16 N4 59.8(14) . . . . ? C16 N4 C17 N5 177.5(12) . . . . ? Ni2 N4 C17 N5 54.7(14) . . . . ? C19 N5 C17 N4 67.1(18) . . . . ? C18 N5 C17 N4 -66.9(16) . . . . ? C10 N1 C18 N5 -177.6(12) . . . . ? Ni2 N1 C18 N5 -56.9(15) . . . . ? C17 N5 C18 N1 69.4(17) . . . . ? C19 N5 C18 N1 -66.4(17) . . . . ? N7 Ni1 N6 C21 -163.9(9) 3_767 . . . ? N7 Ni1 N6 C21 16.1(9) . . . . ? O5 Ni1 N6 C21 -71.2(9) 3_767 . . . ? O5 Ni1 N6 C21 108.8(9) . . . . ? N7 Ni1 N6 C20 -37.7(10) 3_767 . . . ? N7 Ni1 N6 C20 142.3(10) . . . . ? O5 Ni1 N6 C20 55.0(9) 3_767 . . . ? O5 Ni1 N6 C20 -125.0(9) . . . . ? N6 Ni1 N7 C23 137.0(10) . . . . ? N6 Ni1 N7 C23 -43.0(10) 3_767 . . . ? O5 Ni1 N7 C23 -135.7(10) 3_767 . . . ? O5 Ni1 N7 C23 44.3(10) . . . . ? N6 Ni1 N7 C22 13.0(8) . . . . ? N6 Ni1 N7 C22 -167.0(8) 3_767 . . . ? O5 Ni1 N7 C22 100.3(8) 3_767 . . . ? O5 Ni1 N7 C22 -79.7(8) . . . . ? C21 N6 C20 C24 177.2(12) . . . 3_767 ? Ni1 N6 C20 C24 53.8(14) . . . 3_767 ? C21 N6 C20 N8 177.2(12) . . . 3_767 ? Ni1 N6 C20 N8 53.8(14) . . . 3_767 ? C20 N6 C21 C22 -166.6(10) . . . . ? Ni1 N6 C21 C22 -40.1(11) . . . . ? C23 N7 C22 C21 -167.5(12) . . . . ? Ni1 N7 C22 C21 -39.9(12) . . . . ? N6 C21 C22 N7 55.4(14) . . . . ? C22 N7 C23 N8 -178.9(13) . . . . ? Ni1 N7 C23 N8 60.6(15) . . . . ? C25 N8 C23 N7 62(2) . . . . ? C20 N8 C23 N7 -71.6(17) 3_767 . . . ? N3 Ni2 O1 C1 93.8(10) . . . . ? N2 Ni2 O1 C1 -171.5(10) . . . . ? N1 Ni2 O1 C1 -86.0(10) . . . . ? N4 Ni2 O1 C1 7.4(10) . . . . ? N7 Ni1 O5 C8 -85.6(10) 3_767 . . . ? N7 Ni1 O5 C8 94.4(10) . . . . ? N6 Ni1 O5 C8 8.5(11) . . . . ? N6 Ni1 O5 C8 -171.5(11) 3_767 . . . ? Ni2 O1 C1 O4 -1.6(17) . . . . ? Ni2 O1 C1 C2 177.1(6) . . . . ? O4 C1 C2 C7 161.2(10) . . . . ? O1 C1 C2 C7 -17.7(14) . . . . ? O4 C1 C2 C3 -14.3(15) . . . . ? O1 C1 C2 C3 166.9(9) . . . . ? C7 C2 C3 C4 4.4(15) . . . . ? C1 C2 C3 C4 179.9(9) . . . . ? C2 C3 C4 C5 -3.6(15) . . . . ? C2 C3 C4 C9 179.3(9) . . . . ? C3 C4 C5 C6 0.9(14) . . . . ? C9 C4 C5 C6 177.9(9) . . . . ? C4 C5 C6 C7 1.0(15) . . . . ? C4 C5 C6 C8 -179.4(9) . . . . ? C3 C2 C7 C6 -2.5(15) . . . . ? C1 C2 C7 C6 -177.9(9) . . . . ? C5 C6 C7 C2 -0.2(14) . . . . ? C8 C6 C7 C2 -179.8(9) . . . . ? Ni1 O5 C8 O2 -8.5(18) . . . . ? Ni1 O5 C8 C6 172.2(7) . . . . ? C5 C6 C8 O2 -17.2(15) . . . . ? C7 C6 C8 O2 162.4(10) . . . . ? C5 C6 C8 O5 162.1(9) . . . . ? C7 C6 C8 O5 -18.3(15) . . . . ? Ni2 O3 C9 O6 0.8(18) 4_666 . . . ? Ni2 O3 C9 C4 178.9(6) 4_666 . . . ? C5 C4 C9 O3 -9.9(15) . . . . ? C3 C4 C9 O3 167.0(9) . . . . ? C5 C4 C9 O6 168.4(11) . . . . ? C3 C4 C9 O6 -14.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.387 _refine_diff_density_min -2.743 _refine_diff_density_rms 0.156 # Attachment '8686_web_deposit_cif_file_2_YaroslawD.Lampeka_ #1324039133.NiL2_BTB.cif' data_NiL2_BTB _database_code_depnum_ccdc_archive 'CCDC 834624' #TrackingRef '8686_web_deposit_cif_file_2_YaroslawD.Lampeka_ #1324039133.NiL2_BTB.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(\m~3~-(4,4',4''-benzene-1,3,5-triyl-tribenzoato)-O,O',O'')- tris((3-methyl-1,3,5,8,12-penta-azacyclotetradecane)-nickel(ii)) hexahydrate) ; _chemical_name_common ; catena-(bis(mu!3$-(4,4',4''-benzene-1,3,5-triyl-tribenzoato)- O,O',O'')-tris((3-methyl-1,3,5,8,12-penta-azacyclotetradecane)- nickel(ii)) hexahydrate) ; _chemical_formula_moiety '2n(C42 H52.5 N7.5 Ni1.5 O6), 6n(H2 O)' _chemical_formula_sum 'C84 H117 N15 Ni3 O18' _chemical_formula_weight 1801.06 _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 293(2) 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 7.3051(3) _cell_length_b 20.3203(8) _cell_length_c 29.5008(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.816(5) _cell_angle_gamma 90.00 _cell_volume 4373.9(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.1250 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16726 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.88 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4106 _reflns_number_total 8559 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.659 _refine_diff_density_min -1.400 _refine_diff_density_rms 0.091 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 551 _refine_ls_number_reflns 8559 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0654 _refine_ls_restrained_S_all 1.010 _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/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1617 _refine_ls_wR_factor_ref 0.1738 _refine_special_details ; SIMU C43 N8 ISOR 0.001 0.2 C43 EADP C4X N5 EADP C4 N5X EADP N8 C39 EXYZ C4X N5 EXYZ C4 N5X EXYZ N8 C3 Most restraints were needed because of the presence of disordered water molecules, EADP and EXYZ were used because of the disorder observed in the macrocyclic ligand. Both DELU and SIMU were used to improve the data to parameter ratio. 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ni2 Ni 0.73090(8) 0.73521(3) 0.74394(2) 0.0354(2) Uani 1 1 d . . . O1 O 0.5308(5) 0.78037(15) 0.69887(11) 0.0425(9) Uani 1 1 d . . . N4 N 0.7033(6) 0.80734(19) 0.79277(13) 0.0412(10) Uani 1 1 d . B . H4 H 0.6048 0.8324 0.7838 0.062 Uiso 1 1 calc R . . N3 N 0.9319(5) 0.79550(19) 0.71863(13) 0.0427(11) Uani 1 1 d . A . H3 H 1.0431 0.7797 0.7287 0.064 Uiso 1 1 calc R . . N2 N 0.7618(6) 0.66382(19) 0.69567(14) 0.0453(11) Uani 1 1 d . A . H2 H 0.8616 0.6396 0.7048 0.068 Uiso 1 1 calc R . . C4 C 0.9503(8) 0.7338(3) 0.64754(18) 0.0643(15) Uani 0.50 1 d P A 2 H4A H 0.9751 0.7401 0.6158 0.077 Uiso 0.50 1 calc PR A 2 H4B H 1.0571 0.7127 0.6619 0.077 Uiso 0.50 1 calc PR A 2 C4X C 0.5151(8) 0.7388(3) 0.84070(17) 0.0597(15) Uani 0.50 1 d P B 2 H4XA H 0.4101 0.7600 0.8255 0.072 Uiso 0.50 1 calc PR B 2 H4XB H 0.4870 0.7328 0.8722 0.072 Uiso 0.50 1 calc PR B 2 O2 O 0.3766(6) 0.8517(2) 0.73912(13) 0.0735(13) Uani 1 1 d . . . C15 C 0.3191(6) 0.94359(19) 0.58071(15) 0.0259(10) Uani 1 1 d . . . C11 C 0.4361(7) 0.8311(2) 0.70332(18) 0.0392(13) Uani 1 1 d . . . C12 C 0.3923(6) 0.8696(2) 0.66007(15) 0.0325(11) Uani 1 1 d . . . N1 N 0.5331(6) 0.6746(2) 0.77000(15) 0.0495(12) Uani 1 1 d . A . H1 H 0.4214 0.6901 0.7600 0.074 Uiso 1 1 calc R . . C5 C 0.9301(8) 0.7994(3) 0.66849(18) 0.0542(15) Uani 1 1 d . . . H5A H 0.8157 0.8191 0.6572 0.065 Uiso 1 1 calc R A 1 H5B H 1.0294 0.8276 0.6597 0.065 Uiso 1 1 calc R A 1 C17 C 0.3177(6) 0.9329(2) 0.66234(16) 0.0348(12) Uani 1 1 d . . . H17 H 0.2923 0.9509 0.6903 0.042 Uiso 1 1 calc R . . C23 C 0.2485(6) 0.9534(2) 0.49724(15) 0.0291(11) Uani 1 1 d . . . H23 H 0.2451 0.9077 0.4956 0.035 Uiso 1 1 calc R . . C20 C 0.2561(6) 1.0898(2) 0.50202(14) 0.0280(11) Uani 1 1 d . . . C18 C 0.2869(6) 0.9833(2) 0.53875(15) 0.0278(11) Uani 1 1 d . . . C13 C 0.4284(7) 0.8447(2) 0.61810(16) 0.0378(12) Uani 1 1 d . . . H13 H 0.4783 0.8028 0.6160 0.045 Uiso 1 1 calc R . . C16 C 0.2817(7) 0.9685(2) 0.62322(15) 0.0353(12) Uani 1 1 d . . . H16 H 0.2311 1.0103 0.6252 0.042 Uiso 1 1 calc R . . C14 C 0.3922(6) 0.8808(2) 0.57910(15) 0.0346(12) Uani 1 1 d . . . H14 H 0.4172 0.8626 0.5512 0.041 Uiso 1 1 calc R . . C21 C 0.2155(6) 1.0581(2) 0.46107(15) 0.0296(11) Uani 1 1 d . . . H21 H 0.1883 1.0832 0.4352 0.036 Uiso 1 1 calc R . . C9 C 0.5377(8) 0.6737(3) 0.82032(19) 0.0591(17) Uani 1 1 d . . . H9A H 0.4411 0.6450 0.8301 0.071 Uiso 1 1 calc R B 1 H9B H 0.6538 0.6553 0.8315 0.071 Uiso 1 1 calc R B 1 C8 C 0.6716(8) 0.7828(3) 0.83891(17) 0.0546(15) Uani 1 1 d . . . H8A H 0.7804 0.7597 0.8505 0.066 Uiso 1 1 calc R B 1 H8B H 0.6527 0.8200 0.8587 0.066 Uiso 1 1 calc R B 1 C7 C 0.8681(8) 0.8487(3) 0.7897(2) 0.0599(16) Uani 1 1 d . . . H7A H 0.9726 0.8272 0.8048 0.072 Uiso 1 1 calc R B . H7B H 0.8495 0.8906 0.8045 0.072 Uiso 1 1 calc R . . C3 C 0.7949(8) 0.6883(3) 0.64982(18) 0.0520(15) Uani 1 1 d . . . H3A H 0.8161 0.6510 0.6303 0.062 Uiso 1 1 calc R A 1 H3B H 0.6851 0.7105 0.6379 0.062 Uiso 1 1 calc R A 1 C6 C 0.9047(8) 0.8598(2) 0.74013(19) 0.0567(16) Uani 1 1 d . A . H6A H 0.8018 0.8824 0.7251 0.068 Uiso 1 1 calc R . . H6B H 1.0132 0.8868 0.7376 0.068 Uiso 1 1 calc R . . C19 C 0.2918(6) 1.0519(2) 0.54026(15) 0.0300(11) Uani 1 1 d . . . H19 H 0.3200 1.0727 0.5678 0.036 Uiso 1 1 calc R . . C2 C 0.5998(8) 0.6204(3) 0.6986(2) 0.0624(17) Uani 1 1 d . . . H2A H 0.6236 0.5782 0.6847 0.075 Uiso 1 1 calc R A . H2B H 0.4944 0.6402 0.6826 0.075 Uiso 1 1 calc R . . C1 C 0.5608(8) 0.6107(3) 0.7481(2) 0.0630(17) Uani 1 1 d . A . H1A H 0.4520 0.5838 0.7504 0.076 Uiso 1 1 calc R . . H1B H 0.6628 0.5879 0.7634 0.076 Uiso 1 1 calc R . . O1W O 0.2859(7) 0.9499(3) 0.79991(19) 0.125(2) Uani 1 1 d . . . H1WA H 0.1912 0.9663 0.7970 0.150 Uiso 1 1 d R . . H1WB H 0.3334 0.9294 0.7804 0.150 Uiso 1 1 d R . . C10 C 0.3471(12) 0.7725(5) 0.8384(3) 0.041(2) Uani 0.50 1 d P B 1 H10A H 0.3121 0.7821 0.8073 0.061 Uiso 0.50 1 d PR B 1 H10B H 0.3580 0.8129 0.8553 0.061 Uiso 0.50 1 d PR B 1 H10C H 0.2555 0.7452 0.8512 0.061 Uiso 0.50 1 d PR B 1 C10X C 1.127(2) 0.7057(7) 0.6524(5) 0.097(5) Uani 0.50 1 d P A 1 H10D H 1.2181 0.7385 0.6470 0.146 Uiso 0.50 1 d PR A 1 H10E H 1.1379 0.6703 0.6311 0.146 Uiso 0.50 1 d PR A 1 H10F H 1.1451 0.6890 0.6827 0.146 Uiso 0.50 1 d PR A 1 C33 C 0.3647(8) 1.2629(2) 0.54308(18) 0.0524(15) Uani 1 1 d . . . H33 H 0.4423 1.2829 0.5649 0.063 Uiso 1 1 calc R . . C34 C 0.2424(8) 1.3007(2) 0.51686(19) 0.0516(15) Uani 1 1 d . . . C31 C 0.2561(7) 1.1629(2) 0.50557(15) 0.0338(12) Uani 1 1 d . . . C35 C 0.1313(9) 1.2687(3) 0.4846(2) 0.0633(18) Uani 1 1 d . . . H35 H 0.0496 1.2933 0.4663 0.076 Uiso 1 1 calc R . . C32 C 0.3718(7) 1.1951(2) 0.53692(16) 0.0441(14) Uani 1 1 d . . . H32 H 0.4568 1.1707 0.5544 0.053 Uiso 1 1 calc R . . C36 C 0.1376(8) 1.2010(2) 0.47852(19) 0.0543(16) Uani 1 1 d . . . H36 H 0.0620 1.1811 0.4562 0.065 Uiso 1 1 calc R . . O3 O -0.0680(5) 0.80899(16) 0.28895(11) 0.0462(9) Uani 1 1 d . . . O4 O 0.0926(6) 0.88098(19) 0.25091(13) 0.0675(12) Uani 1 1 d . . . C24 C 0.1723(6) 0.9569(2) 0.41354(15) 0.0273(11) Uani 1 1 d . . . C27 C 0.0805(6) 0.8944(2) 0.33068(16) 0.0339(12) Uani 1 1 d . . . C25 C 0.2084(7) 0.9860(2) 0.37224(16) 0.0346(12) Uani 1 1 d . . . H25 H 0.2652 1.0269 0.3721 0.042 Uiso 1 1 calc R . . C26 C 0.1621(6) 0.9556(2) 0.33180(16) 0.0369(12) Uani 1 1 d . . . H26 H 0.1861 0.9766 0.3047 0.044 Uiso 1 1 calc R . . C22 C 0.2146(6) 0.9901(2) 0.45777(15) 0.0278(11) Uani 1 1 d . . . C30 C 0.0309(7) 0.8593(3) 0.28625(18) 0.0412(13) Uani 1 1 d . . . C28 C 0.0460(6) 0.8649(2) 0.37158(16) 0.0348(12) Uani 1 1 d . . . H28 H -0.0091 0.8236 0.3715 0.042 Uiso 1 1 calc R . . C29 C 0.0907(6) 0.8948(2) 0.41230(16) 0.0347(12) Uani 1 1 d . . . H29 H 0.0666 0.8736 0.4393 0.042 Uiso 1 1 calc R . . Ni1 Ni 0.0000 1.5000 0.5000 0.0663(4) Uani 1 2 d S . . O6 O 0.1316(7) 1.40598(18) 0.49695(16) 0.0843(15) Uani 1 1 d . . . C37 C 0.2296(9) 1.3749(3) 0.5259(2) 0.0630(18) Uani 1 1 d . . . O5 O 0.3091(7) 1.39712(19) 0.55934(18) 0.0917(16) Uani 1 1 d . . . O2W O 0.0695(8) 0.9905(2) 0.2005(2) 0.132(2) Uani 1 1 d . . . H2WA H 0.1432 0.9897 0.1762 0.158 Uiso 1 1 d R . . H2WB H 0.1288 0.9614 0.2187 0.158 Uiso 1 1 d R . . O3W O 0.3870(8) 1.4693(2) 0.64953(19) 0.1171(19) Uani 1 1 d . . . H3WA H 0.4049 1.4380 0.6196 0.140 Uiso 1 1 d R . . H3WB H 0.4012 1.4388 0.6711 0.140 Uiso 1 1 d R . . N7 N -0.0651(8) 1.4874(2) 0.43169(19) 0.0795(17) Uani 1 1 d . F . H7 H -0.1451 1.5200 0.4232 0.095 Uiso 1 1 calc R . . N6 N -0.2376(8) 1.4563(3) 0.5194(2) 0.0870(18) Uani 1 1 d . . . H6 H -0.3297 1.4864 0.5164 0.104 Uiso 1 1 calc R . . C41 C 0.1061(11) 1.4993(4) 0.4074(3) 0.097(2) Uani 1 1 d . . . H41A H 0.0770 1.5089 0.3756 0.117 Uiso 1 1 calc R . . H41B H 0.1845 1.4608 0.4093 0.117 Uiso 1 1 calc R . . C40 C -0.1537(12) 1.4253(3) 0.4197(3) 0.098(3) Uani 1 1 d . . . H40A H -0.0696 1.3892 0.4263 0.117 Uiso 1 1 calc R C 1 H40B H -0.1866 1.4247 0.3874 0.117 Uiso 1 1 calc R C 1 C42 C 0.2027(12) 1.5583(4) 0.4305(3) 0.110(3) Uani 1 1 d . . . H42A H 0.3180 1.5666 0.4166 0.132 Uiso 1 1 calc R . . H42B H 0.1267 1.5972 0.4268 0.132 Uiso 1 1 calc R . . C38 C -0.2961(12) 1.3962(4) 0.4946(3) 0.104(3) Uani 1 1 d . . . H38A H -0.4087 1.3790 0.5061 0.124 Uiso 1 1 calc R D 1 H38B H -0.2023 1.3624 0.4976 0.124 Uiso 1 1 calc R D 1 C43 C -0.441(3) 1.3730(11) 0.4324(8) 0.187(10) Uiso 0.50 1 d PU E 1 H43A H -0.4629 1.3754 0.4001 0.281 Uiso 0.50 1 d PR E 1 H43B H -0.5542 1.3788 0.4470 0.281 Uiso 0.50 1 d PR E 1 H43C H -0.3898 1.3307 0.4404 0.281 Uiso 0.50 1 d PR E 1 C39 C -0.3250(11) 1.4166(4) 0.4464(3) 0.117(3) Uani 0.50 1 d P F 2 H39A H -0.3916 1.4579 0.4457 0.140 Uiso 0.50 1 calc PR F 2 H39B H -0.4027 1.3841 0.4310 0.140 Uiso 0.50 1 calc PR F 2 N5 N 0.5151(8) 0.7388(3) 0.84070(17) 0.0597(15) Uani 0.50 1 d P B 1 N5X N 0.9503(8) 0.7338(3) 0.64754(18) 0.0643(15) Uani 0.50 1 d P A 1 N8 N -0.3250(11) 1.4166(4) 0.4464(3) 0.117(3) Uani 0.50 1 d PU E 1 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 Ni2 0.0360(4) 0.0383(4) 0.0315(4) 0.0105(3) -0.0011(3) 0.0038(3) O1 0.049(2) 0.040(2) 0.037(2) 0.0129(16) -0.0046(17) 0.0103(17) N4 0.041(3) 0.048(2) 0.035(3) 0.008(2) 0.008(2) 0.007(2) N3 0.041(3) 0.052(3) 0.035(3) 0.009(2) 0.006(2) -0.002(2) N2 0.045(3) 0.042(2) 0.048(3) 0.008(2) -0.006(2) 0.012(2) C4 0.057(4) 0.093(4) 0.044(3) 0.007(3) 0.009(3) 0.011(4) C4X 0.071(4) 0.066(4) 0.044(3) 0.020(3) 0.023(3) 0.015(3) O2 0.085(3) 0.104(3) 0.033(2) 0.026(2) 0.019(2) 0.056(3) C15 0.028(3) 0.021(2) 0.028(3) 0.0040(19) -0.003(2) 0.000(2) C11 0.036(3) 0.046(3) 0.035(3) 0.014(3) 0.000(3) 0.007(3) C12 0.030(3) 0.041(3) 0.026(3) 0.009(2) 0.001(2) 0.005(2) N1 0.040(3) 0.051(3) 0.057(3) 0.023(2) -0.004(2) -0.002(2) C5 0.057(4) 0.063(4) 0.044(4) 0.015(3) 0.011(3) -0.009(3) C17 0.040(3) 0.039(3) 0.025(3) 0.002(2) -0.001(2) 0.008(2) C23 0.033(3) 0.024(2) 0.031(3) 0.002(2) -0.002(2) 0.003(2) C20 0.033(3) 0.027(3) 0.024(3) -0.001(2) 0.001(2) 0.002(2) C18 0.024(3) 0.033(3) 0.026(3) -0.001(2) -0.001(2) 0.005(2) C13 0.049(3) 0.027(2) 0.038(3) 0.007(2) 0.001(3) 0.008(2) C16 0.046(3) 0.030(3) 0.029(3) 0.002(2) 0.000(2) 0.008(2) C14 0.041(3) 0.038(3) 0.024(3) 0.000(2) 0.000(2) 0.005(2) C21 0.035(3) 0.030(3) 0.024(3) 0.006(2) -0.002(2) 0.006(2) C9 0.046(4) 0.075(4) 0.057(4) 0.037(3) 0.010(3) -0.007(3) C8 0.069(4) 0.061(4) 0.035(3) 0.007(3) 0.005(3) 0.018(3) C7 0.072(5) 0.051(3) 0.057(4) -0.010(3) 0.006(3) -0.004(3) C3 0.057(4) 0.062(4) 0.036(3) -0.010(3) -0.005(3) 0.004(3) C6 0.067(4) 0.051(3) 0.053(4) 0.005(3) 0.011(3) -0.019(3) C19 0.038(3) 0.027(2) 0.025(3) -0.001(2) 0.002(2) 0.003(2) C2 0.068(4) 0.043(3) 0.075(5) -0.007(3) -0.011(4) -0.001(3) C1 0.061(4) 0.047(4) 0.080(5) 0.013(3) -0.007(4) -0.011(3) O1W 0.110(5) 0.136(4) 0.128(5) -0.050(4) -0.005(4) -0.010(4) C10 0.024(5) 0.052(6) 0.047(6) 0.019(5) 0.007(5) 0.004(5) C10X 0.085(12) 0.124(12) 0.084(12) 0.018(10) 0.016(9) -0.009(10) C33 0.078(4) 0.034(3) 0.044(3) -0.004(3) -0.009(3) 0.002(3) C34 0.068(4) 0.038(3) 0.050(4) 0.003(3) 0.002(3) 0.004(3) C31 0.050(3) 0.025(3) 0.027(3) 0.003(2) 0.006(2) 0.006(2) C35 0.093(5) 0.033(3) 0.061(4) 0.009(3) -0.022(4) 0.021(3) C32 0.066(4) 0.033(3) 0.032(3) 0.002(2) -0.008(3) 0.005(3) C36 0.070(4) 0.038(3) 0.053(4) 0.000(3) -0.016(3) 0.013(3) O3 0.046(2) 0.048(2) 0.043(2) -0.0114(17) -0.0085(18) -0.0133(19) O4 0.078(3) 0.089(3) 0.036(2) -0.013(2) 0.008(2) -0.043(2) C24 0.025(3) 0.031(3) 0.026(3) -0.003(2) -0.001(2) 0.001(2) C27 0.026(3) 0.042(3) 0.034(3) -0.009(2) 0.000(2) -0.003(2) C25 0.043(3) 0.028(2) 0.032(3) -0.006(2) -0.005(2) -0.010(2) C26 0.040(3) 0.045(3) 0.026(3) 0.001(2) 0.003(2) -0.007(2) C22 0.026(3) 0.031(3) 0.026(3) -0.004(2) -0.004(2) 0.002(2) C30 0.036(3) 0.052(3) 0.035(3) -0.012(3) -0.003(3) -0.004(3) C28 0.039(3) 0.030(3) 0.035(3) -0.007(2) 0.000(2) -0.010(2) C29 0.039(3) 0.031(3) 0.034(3) 0.001(2) 0.000(2) 0.001(2) Ni1 0.0815(9) 0.0501(6) 0.0674(8) 0.0003(6) 0.0047(7) 0.0053(6) O6 0.112(4) 0.038(2) 0.100(4) -0.002(2) -0.025(3) 0.014(2) C37 0.088(5) 0.036(3) 0.064(5) 0.002(3) -0.005(4) 0.016(4) O5 0.127(4) 0.046(2) 0.098(4) -0.023(3) -0.038(3) 0.015(3) O2W 0.152(5) 0.083(3) 0.163(6) 0.036(4) 0.032(5) 0.016(4) O3W 0.140(5) 0.106(4) 0.104(4) -0.011(3) -0.004(4) -0.007(4) N7 0.105(5) 0.059(3) 0.073(4) -0.009(3) -0.004(4) 0.002(3) N6 0.089(5) 0.080(4) 0.093(5) -0.006(4) 0.012(4) -0.006(3) C41 0.105(7) 0.115(6) 0.074(6) -0.007(5) 0.025(5) -0.012(5) C40 0.129(8) 0.058(4) 0.104(7) -0.017(4) -0.028(6) 0.009(5) C42 0.108(7) 0.142(7) 0.082(6) 0.025(6) 0.021(5) -0.012(6) C38 0.117(7) 0.108(6) 0.086(6) 0.008(5) 0.002(5) -0.040(5) C39 0.090(6) 0.123(6) 0.137(8) -0.022(6) 0.012(6) -0.044(5) N5 0.071(4) 0.066(4) 0.044(3) 0.020(3) 0.023(3) 0.015(3) N5X 0.057(4) 0.093(4) 0.044(3) 0.007(3) 0.009(3) 0.011(4) N8 0.090(6) 0.123(6) 0.137(8) -0.022(6) 0.012(6) -0.044(5) _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 Ni2 O1 2.135(3) . ? Ni2 N4 2.072(4) . ? Ni2 N3 2.079(4) . ? Ni2 N2 2.053(4) . ? Ni2 N1 2.075(4) . ? Ni2 O3 2.130(3) 4_676 ? O1 C11 1.251(5) . ? N4 C8 1.479(6) . ? N4 C7 1.475(7) . ? N3 C5 1.481(6) . ? N3 C6 1.470(6) . ? N2 C3 1.473(6) . ? N2 C2 1.483(7) . ? C4 C5 1.480(7) . ? C4 C3 1.467(7) . ? C4X C9 1.466(7) . ? C4X C8 1.454(7) . ? O2 C11 1.235(6) . ? C15 C18 1.487(6) . ? C15 C16 1.392(6) . ? C15 C14 1.385(6) . ? C11 C12 1.518(6) . ? C12 C17 1.399(6) . ? C12 C13 1.375(6) . ? N1 C9 1.483(7) . ? N1 C1 1.470(7) . ? C17 C16 1.376(6) . ? C23 C18 1.384(6) . ? C23 C22 1.395(6) . ? C20 C21 1.388(6) . ? C20 C19 1.379(6) . ? C20 C31 1.491(6) . ? C18 C19 1.395(6) . ? C13 C14 1.379(6) . ? C21 C22 1.385(6) . ? C7 C6 1.515(7) . ? C2 C1 1.513(8) . ? C33 C34 1.385(7) . ? C33 C32 1.390(6) . ? C34 C35 1.384(7) . ? C34 C37 1.535(7) . ? C31 C32 1.386(6) . ? C31 C36 1.384(6) . ? C35 C36 1.388(7) . ? O3 Ni2 2.130(3) 4_475 ? O3 C30 1.257(6) . ? O4 C30 1.237(6) . ? C24 C25 1.391(6) . ? C24 C22 1.488(6) . ? C24 C29 1.395(6) . ? C27 C26 1.379(6) . ? C27 C30 1.520(6) . ? C27 C28 1.382(6) . ? C25 C26 1.371(6) . ? C28 C29 1.372(6) . ? Ni1 O6 2.143(4) 3_586 ? Ni1 O6 2.143(4) . ? Ni1 N7 2.064(5) . ? Ni1 N7 2.063(5) 3_586 ? Ni1 N6 2.055(6) . ? Ni1 N6 2.056(6) 3_586 ? O6 C37 1.257(7) . ? C37 O5 1.208(7) . ? N7 C41 1.492(8) . ? N7 C40 1.453(8) . ? N6 C42 1.515(9) 3_586 ? N6 C38 1.478(9) . ? C41 C42 1.534(10) . ? C40 C39 1.523(10) . ? C42 N6 1.515(8) 3_586 ? C38 C39 1.485(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni2 O1 92.40(14) . . ? N4 Ni2 N3 85.84(16) . . ? N4 Ni2 N1 93.94(17) . . ? N4 Ni2 O3 87.29(15) . 4_676 ? N3 Ni2 O1 89.83(14) . . ? N3 Ni2 O3 89.70(15) . 4_676 ? N2 Ni2 O1 88.10(14) . . ? N2 Ni2 N4 179.29(17) . . ? N2 Ni2 N3 93.65(17) . . ? N2 Ni2 N1 86.56(18) . . ? N2 Ni2 O3 92.21(15) . 4_676 ? N1 Ni2 O1 91.01(14) . . ? N1 Ni2 N3 179.14(17) . . ? N1 Ni2 O3 89.45(15) . 4_676 ? O3 Ni2 O1 179.46(13) 4_676 . ? C11 O1 Ni2 130.8(3) . . ? C8 N4 Ni2 115.2(3) . . ? C7 N4 Ni2 104.6(3) . . ? C7 N4 C8 114.5(4) . . ? C5 N3 Ni2 114.8(3) . . ? C6 N3 Ni2 104.8(3) . . ? C6 N3 C5 112.9(4) . . ? C3 N2 Ni2 115.3(3) . . ? C3 N2 C2 115.0(4) . . ? C2 N2 Ni2 105.4(3) . . ? C3 C4 C5 117.1(5) . . ? C8 C4X C9 115.8(5) . . ? C16 C15 C18 121.5(4) . . ? C14 C15 C18 121.2(4) . . ? C14 C15 C16 117.3(4) . . ? O1 C11 C12 115.6(5) . . ? O2 C11 O1 126.1(5) . . ? O2 C11 C12 118.3(5) . . ? C17 C12 C11 120.1(4) . . ? C13 C12 C11 121.6(4) . . ? C13 C12 C17 118.3(4) . . ? C9 N1 Ni2 113.3(3) . . ? C1 N1 Ni2 104.4(3) . . ? C1 N1 C9 115.6(4) . . ? C4 C5 N3 111.9(4) . . ? C16 C17 C12 120.1(4) . . ? C18 C23 C22 121.6(4) . . ? C21 C20 C31 121.5(4) . . ? C19 C20 C21 118.5(4) . . ? C19 C20 C31 119.9(4) . . ? C23 C18 C15 121.0(4) . . ? C23 C18 C19 118.1(4) . . ? C19 C18 C15 120.9(4) . . ? C12 C13 C14 121.2(4) . . ? C17 C16 C15 121.8(4) . . ? C13 C14 C15 121.3(4) . . ? C22 C21 C20 121.6(4) . . ? C4X C9 N1 113.7(4) . . ? C4X C8 N4 113.6(4) . . ? N4 C7 C6 109.2(4) . . ? C4 C3 N2 114.7(4) . . ? N3 C6 C7 108.5(4) . . ? C20 C19 C18 121.8(4) . . ? N2 C2 C1 108.8(4) . . ? N1 C1 C2 110.2(4) . . ? C34 C33 C32 120.2(5) . . ? C33 C34 C37 119.4(5) . . ? C35 C34 C33 117.7(5) . . ? C35 C34 C37 122.9(5) . . ? C32 C31 C20 121.0(4) . . ? C36 C31 C20 121.2(4) . . ? C36 C31 C32 117.7(4) . . ? C34 C35 C36 122.1(5) . . ? C31 C32 C33 122.0(5) . . ? C31 C36 C35 120.2(5) . . ? C30 O3 Ni2 133.2(3) . 4_475 ? C25 C24 C22 122.4(4) . . ? C25 C24 C29 117.4(4) . . ? C29 C24 C22 120.2(4) . . ? C26 C27 C30 121.9(5) . . ? C26 C27 C28 117.9(4) . . ? C28 C27 C30 120.2(4) . . ? C26 C25 C24 121.5(4) . . ? C25 C26 C27 121.0(5) . . ? C23 C22 C24 120.7(4) . . ? C21 C22 C23 118.4(4) . . ? C21 C22 C24 120.9(4) . . ? O3 C30 C27 116.1(5) . . ? O4 C30 O3 125.2(5) . . ? O4 C30 C27 118.6(5) . . ? C29 C28 C27 121.8(4) . . ? C28 C29 C24 120.5(4) . . ? O6 Ni1 O6 179.999(3) 3_586 . ? N7 Ni1 O6 86.01(19) 3_586 3_586 ? N7 Ni1 O6 93.99(19) . 3_586 ? N7 Ni1 O6 93.99(19) 3_586 . ? N7 Ni1 O6 86.01(19) . . ? N7 Ni1 N7 179.999(3) 3_586 . ? N6 Ni1 O6 89.2(2) 3_586 . ? N6 Ni1 O6 90.8(2) 3_586 3_586 ? N6 Ni1 O6 89.2(2) . 3_586 ? N6 Ni1 O6 90.8(2) . . ? N6 Ni1 N7 86.5(2) . 3_586 ? N6 Ni1 N7 93.5(2) 3_586 3_586 ? N6 Ni1 N7 93.5(2) . . ? N6 Ni1 N7 86.5(2) 3_586 . ? N6 Ni1 N6 179.997(1) . 3_586 ? C37 O6 Ni1 131.4(4) . . ? O6 C37 C34 114.4(6) . . ? O5 C37 C34 118.6(5) . . ? O5 C37 O6 126.9(5) . . ? C41 N7 Ni1 106.9(4) . . ? C40 N7 Ni1 115.1(5) . . ? C40 N7 C41 113.4(6) . . ? C42 N6 Ni1 104.6(4) 3_586 . ? C38 N6 Ni1 116.5(5) . . ? C38 N6 C42 110.6(6) . 3_586 ? N7 C41 C42 106.9(6) . . ? N7 C40 C39 110.0(6) . . ? N6 C42 C41 109.4(6) 3_586 . ? N6 C38 C39 105.5(6) . . ? C38 C39 C40 116.5(7) . . ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m ? _symmetry_int_tables_number ? _chemical_absolute_configuration ?