Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Vitaly V. Pavlishchuk' 'A. Addison' 'Eugeny A. Goreshnik' 'Sergey V. Kolotilov' ; M.J.Prushan ; 'Dieter Schollmeyer' 'Laurence K. Thompson' 'Thomas Weyhermuller' _publ_contact_author_name 'Dr Vitaly V Pavlishchuk' _publ_contact_author_address ; L.V Pisarzhevskii Institute of Physical Chemistry of the National Academy of Sci Prospekt Nauki 31 Kiev 03039 UKRAINE ; _publ_contact_author_email PAVLISVV@PHYCHE.FREENET.KIEV.UA _publ_section_title ; Structural, magnetic and related attributes of some tetranuclear nickel rhombs and a dinuclear congener ; data_3625 _database_code_CSD 193550 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical '[C24 H52 N10 Ni4 O10]2+, 2 (ClO4)-,H2O' _chemical_formula_sum 'C24 H54 Cl2 N10 Ni4 O19' _chemical_formula_weight 1092.51 _chemical_melting_point ? _chemical_compound_source ? 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' Cl Cl 0.1484 0.1585 '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 P2(1)/c 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 10.6517(3) _cell_length_b 17.5058(6) _cell_length_c 22.5440(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.53(1) _cell_angle_gamma 90.00 _cell_volume 4199.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used 16390 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque block' _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method ? _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.977 _exptl_absorpt_correction_type 'DELrefABS, Platon99 Prog. Suite' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 Nonius-Kappa-CCD-Detector _diffrn_measurement_method '\-scan,258 images a 0.5 deg./60 sec' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34327 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12100 _reflns_number_observed 10068 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 37 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+4.2253P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12063 _refine_ls_number_parameters 548 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_obs 0.0393 _refine_ls_wR_factor_all 0.1158 _refine_ls_wR_factor_obs 0.0994 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.123 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni -0.16406(3) 0.31608(2) 0.267167(12) 0.01125(7) Uani 1 d . . Ni2 Ni 0.05061(2) 0.19324(2) 0.328490(12) 0.01108(7) Uani 1 d . . Ni3 Ni 0.26314(3) 0.23210(2) 0.440495(12) 0.01246(7) Uani 1 d . . Ni4 Ni 0.05104(2) 0.35594(2) 0.377642(12) 0.01150(7) Uani 1 d . . O1 O -0.22431(14) 0.22272(9) 0.31520(7) 0.0144(3) Uani 1 d . . O2 O 0.04544(14) 0.08526(9) 0.36838(7) 0.0154(3) Uani 1 d . . O3 O 0.05494(14) 0.14549(9) 0.24307(7) 0.0151(3) Uani 1 d . . O4 O 0.32314(14) 0.19136(9) 0.35907(7) 0.0151(3) Uani 1 d . . O5 O 0.32031(15) 0.33592(9) 0.41012(7) 0.0166(3) Uani 1 d . . O6 O 0.04019(15) 0.39232(9) 0.46782(7) 0.0178(3) Uani 1 d . . O7 O 0.06386(15) 0.45896(9) 0.32869(7) 0.0156(3) Uani 1 d . . O8 O -0.21212(14) 0.37997(9) 0.33929(7) 0.0159(3) Uani 1 d . . O9 O 0.01731(14) 0.30024(8) 0.29877(7) 0.0114(3) Uani 1 d D . H9 H 0.0649(30) 0.3135(18) 0.2767(14) 0.027(9) Uiso 1 d D . O10 O 0.08325(14) 0.24796(9) 0.40771(7) 0.0124(3) Uani 1 d D . H10 H 0.0348(32) 0.2333(21) 0.4287(15) 0.041(11) Uiso 1 d D . N1 N -0.1176(2) 0.41696(11) 0.22205(9) 0.0163(4) Uani 1 d . . H1A H -0.0859(2) 0.45149(11) 0.24821(9) 0.020 Uiso 1 calc R . H1B H -0.0586(2) 0.40672(11) 0.19582(9) 0.020 Uiso 1 calc R . N2 N -0.3447(2) 0.34056(11) 0.23136(8) 0.0142(3) Uani 1 d . . H2 H -0.4028(2) 0.32790(11) 0.25808(8) 0.017 Uiso 1 calc R . N3 N -0.1599(2) 0.24245(11) 0.19380(9) 0.0161(4) Uani 1 d . . H3A H -0.1260(2) 0.26592(11) 0.16280(9) 0.019 Uiso 1 calc R . H3B H -0.1148(2) 0.20023(11) 0.20288(9) 0.019 Uiso 1 calc R . N4 N -0.1365(2) 0.17589(10) 0.33498(8) 0.0123(3) Uani 1 d . . N5 N 0.2368(2) 0.17814(10) 0.31794(8) 0.0128(3) Uani 1 d . . N6 N 0.2272(2) 0.12014(11) 0.46839(9) 0.0174(4) Uani 1 d . . H6A H 0.1608(2) 0.11989(11) 0.49177(9) 0.021 Uiso 1 calc R . H6B H 0.2087(2) 0.09039(11) 0.43664(9) 0.021 Uiso 1 calc R . N7 N 0.4435(2) 0.20932(12) 0.47606(8) 0.0166(4) Uani 1 d . . H7 H 0.5008(2) 0.22893(12) 0.45146(8) 0.020 Uiso 1 calc R . N8 N 0.2440(2) 0.28618(12) 0.52355(9) 0.0186(4) Uani 1 d . . H8A H 0.1907(2) 0.32598(12) 0.52027(9) 0.022 Uiso 1 calc R . H8B H 0.2160(2) 0.25316(12) 0.55054(9) 0.022 Uiso 1 calc R . N9 N 0.2376(2) 0.37466(10) 0.37892(8) 0.0131(3) Uani 1 d . . N10 N -0.1332(2) 0.37820(10) 0.38471(8) 0.0138(3) Uani 1 d . . C1 C -0.2305(2) 0.44882(13) 0.19049(10) 0.0170(4) Uani 1 d . . H1A' H -0.2347(2) 0.43101(13) 0.14971(10) 0.020 Uiso 1 calc R . H1B' H -0.2255(2) 0.50415(13) 0.19007(10) 0.020 Uiso 1 calc R . C2 C -0.3474(2) 0.42409(13) 0.22117(11) 0.0171(4) Uani 1 d . . H2A H -0.3517(2) 0.45049(13) 0.25886(11) 0.021 Uiso 1 calc R . H2B H -0.4214(2) 0.43749(13) 0.19680(11) 0.021 Uiso 1 calc R . C3 C -0.3681(2) 0.29614(13) 0.17620(10) 0.0168(4) Uani 1 d . . H3A' H -0.3439(2) 0.32594(13) 0.14228(10) 0.020 Uiso 1 calc R . H3B' H -0.4569(2) 0.28429(13) 0.17112(10) 0.020 Uiso 1 calc R . C4 C -0.2924(2) 0.22293(13) 0.17991(11) 0.0177(4) Uani 1 d . . H4A H -0.3237(2) 0.19013(13) 0.21063(11) 0.021 Uiso 1 calc R . H4B H -0.3001(2) 0.19584(13) 0.14239(11) 0.021 Uiso 1 calc R . C5 C -0.1693(2) 0.11439(12) 0.36337(9) 0.0133(4) Uani 1 d . . C6 C -0.0620(2) 0.06699(12) 0.38219(9) 0.0139(4) Uani 1 d . . C7 C -0.0818(2) -0.00318(13) 0.41744(11) 0.0196(4) Uani 1 d . . H7A H -0.0023(2) -0.02758(13) 0.42612(11) 0.029 Uiso 1 calc R . H7B H -0.1360(2) -0.03746(13) 0.39512(11) 0.029 Uiso 1 calc R . H7C H -0.1197(2) 0.01008(13) 0.45389(11) 0.029 Uiso 1 calc R . C8 C -0.3009(2) 0.09547(14) 0.37605(11) 0.0192(4) Uani 1 d . . H8A' H -0.3558(2) 0.13430(14) 0.35966(11) 0.029 Uiso 1 calc R . H8B' H -0.3093(2) 0.09280(14) 0.41822(11) 0.029 Uiso 1 calc R . H8C H -0.3228(2) 0.04705(14) 0.35850(11) 0.029 Uiso 1 calc R . C9 C 0.1634(2) 0.13144(12) 0.22782(10) 0.0143(4) Uani 1 d . . C10 C 0.2706(2) 0.14983(12) 0.26734(10) 0.0135(4) Uani 1 d . . C11 C 0.4039(2) 0.13534(14) 0.25406(11) 0.0202(5) Uani 1 d . . H11A H 0.4575(2) 0.15230(14) 0.28681(11) 0.030 Uiso 1 calc R . H11B H 0.4242(2) 0.16273(14) 0.21886(11) 0.030 Uiso 1 calc R . H11C H 0.4162(2) 0.08164(14) 0.24794(11) 0.030 Uiso 1 calc R . C12 C 0.1811(2) 0.09267(14) 0.16962(11) 0.0212(5) Uani 1 d . . H12A H 0.1008(2) 0.08502(14) 0.14949(11) 0.032 Uiso 1 calc R . H12B H 0.2212(2) 0.04415(14) 0.17644(11) 0.032 Uiso 1 calc R . H12C H 0.2327(2) 0.12396(14) 0.14560(11) 0.032 Uiso 1 calc R . C13 C 0.3387(2) 0.08994(14) 0.50149(11) 0.0217(5) Uani 1 d . . H13A H 0.3419(2) 0.03481(14) 0.49747(11) 0.026 Uiso 1 calc R . H13B H 0.3343(2) 0.10219(14) 0.54331(11) 0.026 Uiso 1 calc R . C14 C 0.4553(2) 0.12533(15) 0.47696(11) 0.0217(5) Uani 1 d . . H14A H 0.5286(2) 0.11074(15) 0.50144(11) 0.026 Uiso 1 calc R . H14B H 0.4664(2) 0.10667(15) 0.43701(11) 0.026 Uiso 1 calc R . C15 C 0.4615(2) 0.2450(2) 0.53486(11) 0.0222(5) Uani 1 d . . H15A H 0.5477(2) 0.2623(2) 0.54050(11) 0.027 Uiso 1 calc R . H15B H 0.4455(2) 0.2078(2) 0.56548(11) 0.027 Uiso 1 calc R . C16 C 0.3729(2) 0.31215(15) 0.54013(11) 0.0229(5) Uani 1 d . . H16A H 0.3766(2) 0.33128(15) 0.58055(11) 0.028 Uiso 1 calc R . H16B H 0.3972(2) 0.35307(15) 0.51397(11) 0.028 Uiso 1 calc R . C17 C 0.2766(2) 0.43343(12) 0.34864(10) 0.0151(4) Uani 1 d . . C18 C 0.1745(2) 0.47382(12) 0.31801(10) 0.0148(4) Uani 1 d . . C19 C 0.2028(2) 0.53273(13) 0.27283(12) 0.0226(5) Uani 1 d . . H19A H 0.1256(2) 0.55410(13) 0.25668(12) 0.034 Uiso 1 calc R . H19B H 0.2479(2) 0.50961(13) 0.24154(12) 0.034 Uiso 1 calc R . H19C H 0.2531(2) 0.57244(13) 0.29113(12) 0.034 Uiso 1 calc R . C20 C 0.4119(2) 0.45401(14) 0.34599(13) 0.0240(5) Uani 1 d . . H20A H 0.4616(2) 0.41896(14) 0.36987(13) 0.036 Uiso 1 calc R . H20B H 0.4246(2) 0.50498(14) 0.36076(13) 0.036 Uiso 1 calc R . H20C H 0.4367(2) 0.45137(14) 0.30561(13) 0.036 Uiso 1 calc R . C21 C -0.0705(2) 0.40297(13) 0.48155(10) 0.0178(4) Uani 1 d . . C22 C -0.1713(2) 0.40088(13) 0.43648(10) 0.0175(4) Uani 1 d . . C23 C -0.3044(2) 0.4220(2) 0.44581(12) 0.0301(6) Uani 1 d . . H23A H -0.3532(2) 0.4159(2) 0.40927(12) 0.045 Uiso 1 calc R . H23B H -0.3084(2) 0.4742(2) 0.45853(12) 0.045 Uiso 1 calc R . H23C H -0.3376(2) 0.3895(2) 0.47563(12) 0.045 Uiso 1 calc R . C24 C -0.0988(3) 0.4188(2) 0.54485(11) 0.0266(5) Uani 1 d . . H24A H -0.0221(3) 0.4181(2) 0.56886(11) 0.040 Uiso 1 calc R . H24B H -0.1547(3) 0.3803(2) 0.55866(11) 0.040 Uiso 1 calc R . H24C H -0.1378(3) 0.4680(2) 0.54761(11) 0.040 Uiso 1 calc R . Cl1 Cl 0.28154(5) 0.34051(3) 0.18910(2) 0.01620(10) Uani 1 d . . O11 O 0.1585(2) 0.36572(11) 0.20454(8) 0.0260(4) Uani 1 d . . O12 O 0.3387(2) 0.39963(11) 0.15549(9) 0.0284(4) Uani 1 d . . O13 O 0.2716(2) 0.27219(11) 0.15408(9) 0.0313(4) Uani 1 d . . O14 O 0.3558(2) 0.32516(11) 0.24225(8) 0.0257(4) Uani 1 d . . Cl2 Cl -0.14039(6) 0.16998(4) 0.53529(3) 0.02443(13) Uani 1 d . . O20 O -0.0530(2) 0.15780(11) 0.48942(9) 0.0282(4) Uani 1 d . . O21 O -0.0702(2) 0.1707(2) 0.59158(10) 0.0479(6) Uani 1 d . . O22 O -0.2251(2) 0.10661(14) 0.53628(10) 0.0393(5) Uani 1 d . . O23 O -0.2074(3) 0.23871(15) 0.5269(2) 0.0602(8) Uani 1 d . . O30 O 0.5569(2) 0.27573(12) 0.36457(11) 0.0349(5) Uani 1 d D . H30A H 0.6243(32) 0.2546(22) 0.3528(17) 0.047(11) Uiso 1 d D . H30B H 0.4919(36) 0.2493(26) 0.3535(22) 0.076(15) Uiso 1 d 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 Ni1 0.01045(13) 0.01213(12) 0.01114(12) 0.00115(10) 0.00017(9) 0.00002(9) Ni2 0.00989(13) 0.01103(12) 0.01237(13) 0.00089(10) 0.00113(10) -0.00040(9) Ni3 0.01057(13) 0.01552(13) 0.01129(13) 0.00253(10) 0.00041(10) 0.00047(9) Ni4 0.01036(13) 0.01195(12) 0.01216(13) 0.00040(10) 0.00025(10) 0.00004(9) O1 0.0105(7) 0.0162(7) 0.0164(7) 0.0060(6) 0.0001(6) 0.0009(6) O2 0.0143(7) 0.0132(7) 0.0187(7) 0.0019(6) 0.0015(6) 0.0005(6) O3 0.0131(7) 0.0157(7) 0.0164(7) -0.0011(6) 0.0006(6) -0.0002(6) O4 0.0117(7) 0.0199(8) 0.0136(7) 0.0000(6) 0.0002(6) -0.0010(6) O5 0.0135(7) 0.0176(7) 0.0184(8) 0.0052(6) -0.0022(6) -0.0006(6) O6 0.0166(8) 0.0197(8) 0.0171(7) -0.0041(6) -0.0003(6) 0.0021(6) O7 0.0164(7) 0.0112(7) 0.0191(8) 0.0010(6) -0.0005(6) 0.0007(6) O8 0.0123(7) 0.0202(8) 0.0150(7) -0.0025(6) -0.0012(6) 0.0017(6) O9 0.0110(7) 0.0117(7) 0.0115(7) 0.0011(6) 0.0016(5) -0.0009(5) O10 0.0108(7) 0.0142(7) 0.0121(7) 0.0018(6) 0.0008(6) -0.0004(5) N1 0.0151(9) 0.0151(8) 0.0187(9) 0.0043(7) 0.0008(7) 0.0006(7) N2 0.0126(8) 0.0153(8) 0.0146(8) 0.0001(7) 0.0007(7) 0.0005(7) N3 0.0170(9) 0.0166(9) 0.0147(8) 0.0002(7) 0.0005(7) 0.0030(7) N4 0.0125(8) 0.0135(8) 0.0110(8) 0.0009(6) 0.0008(6) 0.0006(6) N5 0.0122(8) 0.0119(8) 0.0141(8) 0.0020(7) -0.0004(7) -0.0004(6) N6 0.0140(9) 0.0186(9) 0.0197(9) 0.0064(8) 0.0009(7) 0.0006(7) N7 0.0122(8) 0.0236(9) 0.0141(8) 0.0028(7) 0.0011(7) 0.0013(7) N8 0.0176(9) 0.0239(10) 0.0142(8) 0.0021(8) 0.0012(7) 0.0036(8) N9 0.0129(8) 0.0128(8) 0.0136(8) 0.0012(7) -0.0003(6) 0.0015(6) N10 0.0127(8) 0.0145(8) 0.0141(8) -0.0004(7) -0.0004(7) -0.0005(6) C1 0.0191(10) 0.0134(9) 0.0184(10) 0.0027(8) -0.0002(8) 0.0007(8) C2 0.0151(10) 0.0148(10) 0.0213(10) -0.0023(8) 0.0000(8) 0.0034(8) C3 0.0163(10) 0.0171(10) 0.0165(10) -0.0019(8) -0.0036(8) 0.0006(8) C4 0.0177(10) 0.0161(10) 0.0190(10) -0.0020(8) -0.0017(8) -0.0008(8) C5 0.0133(9) 0.0128(9) 0.0138(9) -0.0012(8) 0.0009(7) -0.0021(7) C6 0.0173(10) 0.0114(9) 0.0129(9) -0.0017(7) 0.0005(8) -0.0016(8) C7 0.0198(11) 0.0137(10) 0.0253(11) 0.0053(9) 0.0014(9) -0.0020(8) C8 0.0132(10) 0.0204(11) 0.0243(11) 0.0054(9) 0.0033(8) -0.0026(8) C9 0.0161(10) 0.0111(9) 0.0157(10) 0.0016(8) 0.0009(8) 0.0007(7) C10 0.0127(9) 0.0123(9) 0.0155(9) 0.0012(8) 0.0022(8) 0.0002(7) C11 0.0158(10) 0.0238(11) 0.0212(11) -0.0052(9) 0.0035(9) 0.0005(9) C12 0.0209(11) 0.0237(11) 0.0191(11) -0.0055(9) 0.0022(9) -0.0010(9) C13 0.0189(11) 0.0232(11) 0.0228(11) 0.0078(9) -0.0009(9) 0.0027(9) C14 0.0166(11) 0.0263(12) 0.0223(11) 0.0056(10) 0.0008(9) 0.0071(9) C15 0.0167(11) 0.0318(13) 0.0177(11) 0.0002(10) -0.0044(9) 0.0005(9) C16 0.0208(11) 0.0283(12) 0.0193(11) -0.0019(10) -0.0028(9) -0.0002(9) C17 0.0141(10) 0.0127(9) 0.0184(10) 0.0004(8) 0.0003(8) -0.0022(7) C18 0.0178(10) 0.0097(9) 0.0170(10) -0.0012(8) 0.0007(8) -0.0008(7) C19 0.0224(12) 0.0152(10) 0.0302(13) 0.0088(10) 0.0011(10) 0.0003(9) C20 0.0157(11) 0.0214(11) 0.0350(14) 0.0060(10) 0.0009(10) -0.0036(9) C21 0.0182(10) 0.0202(10) 0.0150(10) -0.0030(8) 0.0017(8) 0.0010(8) C22 0.0164(10) 0.0197(10) 0.0164(10) -0.0040(9) 0.0004(8) 0.0010(8) C23 0.0161(11) 0.053(2) 0.0217(12) -0.0109(12) 0.0027(9) 0.0068(11) C24 0.0242(12) 0.0401(15) 0.0154(10) -0.0072(10) -0.0002(9) 0.0031(11) Cl1 0.0177(2) 0.0155(2) 0.0157(2) 0.0009(2) 0.0036(2) 0.0010(2) O11 0.0193(8) 0.0314(10) 0.0279(9) 0.0057(8) 0.0086(7) 0.0050(7) O12 0.0267(9) 0.0271(9) 0.0322(10) 0.0136(8) 0.0084(8) -0.0014(7) O13 0.0432(12) 0.0229(9) 0.0275(10) -0.0092(8) -0.0012(9) -0.0006(8) O14 0.0269(9) 0.0291(9) 0.0209(9) 0.0020(7) -0.0031(7) 0.0018(7) Cl2 0.0223(3) 0.0277(3) 0.0238(3) -0.0034(2) 0.0074(2) 0.0015(2) O20 0.0301(10) 0.0309(10) 0.0246(9) 0.0014(8) 0.0141(8) -0.0042(8) O21 0.0515(15) 0.062(2) 0.0302(11) -0.0170(11) -0.0028(11) 0.0061(12) O22 0.0308(11) 0.0455(13) 0.0424(12) 0.0083(10) 0.0104(9) -0.0122(10) O23 0.051(2) 0.0378(13) 0.094(2) 0.0146(14) 0.017(2) 0.0206(12) O30 0.0176(9) 0.0298(10) 0.0584(15) -0.0056(10) 0.0139(9) -0.0028(8) _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 O9 2.048(2) . ? Ni1 O8 2.057(2) . ? Ni1 O1 2.078(2) . ? Ni1 N2 2.098(2) . ? Ni1 N3 2.099(2) . ? Ni1 N1 2.108(2) . ? Ni2 O9 2.015(2) . ? Ni2 N5 2.026(2) . ? Ni2 N4 2.028(2) . ? Ni2 O10 2.043(2) . ? Ni2 O2 2.095(2) . ? Ni2 O3 2.102(2) . ? Ni3 O10 2.042(2) . ? Ni3 O5 2.044(2) . ? Ni3 N7 2.087(2) . ? Ni3 O4 2.095(2) . ? Ni3 N6 2.099(2) . ? Ni3 N8 2.116(2) . ? Ni4 N9 2.013(2) . ? Ni4 N10 2.014(2) . ? Ni4 O10 2.032(2) . ? Ni4 O9 2.046(2) . ? Ni4 O7 2.122(2) . ? Ni4 O6 2.138(2) . ? O1 N4 1.307(2) . ? O2 C6 1.241(3) . ? O3 C9 1.244(3) . ? O4 N5 1.297(2) . ? O5 N9 1.295(2) . ? O6 C21 1.247(3) . ? O7 C18 1.241(3) . ? O8 N10 1.296(2) . ? N1 C1 1.479(3) . ? N2 C3 1.478(3) . ? N2 C2 1.480(3) . ? N3 C4 1.473(3) . ? N4 C5 1.308(3) . ? N5 C10 1.309(3) . ? N6 C13 1.473(3) . ? N7 C15 1.470(3) . ? N7 C14 1.476(3) . ? N8 C16 1.479(3) . ? N9 C17 1.313(3) . ? N10 C22 1.314(3) . ? C1 C2 1.513(3) . ? C3 C4 1.514(3) . ? C5 C6 1.460(3) . ? C5 C8 1.481(3) . ? C6 C7 1.483(3) . ? C9 C10 1.453(3) . ? C9 C12 1.497(3) . ? C10 C11 1.487(3) . ? C13 C14 1.514(3) . ? C15 C16 1.515(4) . ? C17 C18 1.447(3) . ? C17 C20 1.489(3) . ? C18 C19 1.490(3) . ? C21 C22 1.445(3) . ? C21 C24 1.497(3) . ? C22 C23 1.490(3) . ? Cl1 O14 1.431(2) . ? Cl1 O12 1.434(2) . ? Cl1 O13 1.434(2) . ? Cl1 O11 1.440(2) . ? Cl2 O23 1.407(2) . ? Cl2 O22 1.431(2) . ? Cl2 O20 1.437(2) . ? Cl2 O21 1.444(2) . ? 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 O9 Ni1 O8 93.58(6) . . ? O9 Ni1 O1 91.18(6) . . ? O8 Ni1 O1 85.54(6) . . ? O9 Ni1 N2 175.24(7) . . ? O8 Ni1 N2 86.39(7) . . ? O1 Ni1 N2 93.56(7) . . ? O9 Ni1 N3 97.97(7) . . ? O8 Ni1 N3 166.30(7) . . ? O1 Ni1 N3 86.87(7) . . ? N2 Ni1 N3 82.71(7) . . ? O9 Ni1 N1 92.50(7) . . ? O8 Ni1 N1 89.87(7) . . ? O1 Ni1 N1 174.30(7) . . ? N2 Ni1 N1 82.75(7) . . ? N3 Ni1 N1 96.93(8) . . ? O9 Ni2 N5 103.95(7) . . ? O9 Ni2 N4 90.23(7) . . ? N5 Ni2 N4 163.68(7) . . ? O9 Ni2 O10 82.85(6) . . ? N5 Ni2 O10 91.95(7) . . ? N4 Ni2 O10 97.88(7) . . ? O9 Ni2 O2 166.82(6) . . ? N5 Ni2 O2 88.69(7) . . ? N4 Ni2 O2 77.84(7) . . ? O10 Ni2 O2 93.12(6) . . ? O9 Ni2 O3 94.34(6) . . ? N5 Ni2 O3 77.25(7) . . ? N4 Ni2 O3 93.89(7) . . ? O10 Ni2 O3 167.90(6) . . ? O2 Ni2 O3 92.09(6) . . ? O10 Ni3 O5 92.67(6) . . ? O10 Ni3 N7 176.42(7) . . ? O5 Ni3 N7 90.91(7) . . ? O10 Ni3 O4 92.68(6) . . ? O5 Ni3 O4 84.39(6) . . ? N7 Ni3 O4 87.73(7) . . ? O10 Ni3 N6 93.13(7) . . ? O5 Ni3 N6 172.55(7) . . ? N7 Ni3 N6 83.31(8) . . ? O4 Ni3 N6 90.66(7) . . ? O10 Ni3 N8 97.71(7) . . ? O5 Ni3 N8 86.58(7) . . ? N7 Ni3 N8 82.44(8) . . ? O4 Ni3 N8 166.53(7) . . ? N6 Ni3 N8 97.28(8) . . ? N9 Ni4 N10 158.77(7) . . ? N9 Ni4 O10 89.69(7) . . ? N10 Ni4 O10 107.72(7) . . ? N9 Ni4 O9 103.03(7) . . ? N10 Ni4 O9 91.53(7) . . ? O10 Ni4 O9 82.36(6) . . ? N9 Ni4 O7 77.46(7) . . ? N10 Ni4 O7 87.82(7) . . ? O10 Ni4 O7 161.86(6) . . ? O9 Ni4 O7 88.05(6) . . ? N9 Ni4 O6 91.87(7) . . ? N10 Ni4 O6 76.90(7) . . ? O10 Ni4 O6 88.59(6) . . ? O9 Ni4 O6 162.46(6) . . ? O7 Ni4 O6 104.40(6) . . ? N4 O1 Ni1 116.00(12) . . ? C6 O2 Ni2 112.47(14) . . ? C9 O3 Ni2 112.96(14) . . ? N5 O4 Ni3 116.94(13) . . ? N9 O5 Ni3 116.23(13) . . ? C21 O6 Ni4 111.85(14) . . ? C18 O7 Ni4 111.25(14) . . ? N10 O8 Ni1 115.85(13) . . ? Ni2 O9 Ni4 97.61(7) . . ? Ni2 O9 Ni1 113.01(7) . . ? Ni4 O9 Ni1 111.38(7) . . ? Ni4 O10 Ni3 112.90(7) . . ? Ni4 O10 Ni2 97.17(7) . . ? Ni3 O10 Ni2 111.93(7) . . ? C1 N1 Ni1 110.19(14) . . ? C3 N2 C2 112.8(2) . . ? C3 N2 Ni1 109.52(13) . . ? C2 N2 Ni1 105.81(13) . . ? C4 N3 Ni1 104.88(14) . . ? O1 N4 C5 118.8(2) . . ? O1 N4 Ni2 124.89(13) . . ? C5 N4 Ni2 116.28(15) . . ? O4 N5 C10 118.5(2) . . ? O4 N5 Ni2 124.02(14) . . ? C10 N5 Ni2 117.37(15) . . ? C13 N6 Ni3 109.45(14) . . ? C15 N7 C14 113.8(2) . . ? C15 N7 Ni3 110.28(14) . . ? C14 N7 Ni3 105.82(14) . . ? C16 N8 Ni3 103.70(14) . . ? O5 N9 C17 118.0(2) . . ? O5 N9 Ni4 124.77(14) . . ? C17 N9 Ni4 117.10(15) . . ? O8 N10 C22 118.7(2) . . ? O8 N10 Ni4 122.85(14) . . ? C22 N10 Ni4 118.0(2) . . ? N1 C1 C2 109.9(2) . . ? N2 C2 C1 110.1(2) . . ? N2 C3 C4 109.2(2) . . ? N3 C4 C3 108.6(2) . . ? N4 C5 C6 112.8(2) . . ? N4 C5 C8 123.6(2) . . ? C6 C5 C8 123.5(2) . . ? O2 C6 C5 119.9(2) . . ? O2 C6 C7 120.1(2) . . ? C5 C6 C7 119.9(2) . . ? O3 C9 C10 120.0(2) . . ? O3 C9 C12 119.1(2) . . ? C10 C9 C12 120.8(2) . . ? N5 C10 C9 112.3(2) . . ? N5 C10 C11 122.8(2) . . ? C9 C10 C11 124.8(2) . . ? N6 C13 C14 108.9(2) . . ? N7 C14 C13 110.0(2) . . ? N7 C15 C16 110.1(2) . . ? N8 C16 C15 108.4(2) . . ? N9 C17 C18 112.5(2) . . ? N9 C17 C20 122.7(2) . . ? C18 C17 C20 124.8(2) . . ? O7 C18 C17 120.4(2) . . ? O7 C18 C19 120.0(2) . . ? C17 C18 C19 119.6(2) . . ? O6 C21 C22 120.2(2) . . ? O6 C21 C24 119.8(2) . . ? C22 C21 C24 120.0(2) . . ? N10 C22 C21 112.6(2) . . ? N10 C22 C23 122.3(2) . . ? C21 C22 C23 125.2(2) . . ? O14 Cl1 O12 110.26(12) . . ? O14 Cl1 O13 109.20(12) . . ? O12 Cl1 O13 109.49(12) . . ? O14 Cl1 O11 109.28(11) . . ? O12 Cl1 O11 108.56(11) . . ? O13 Cl1 O11 110.04(13) . . ? O23 Cl2 O22 110.4(2) . . ? O23 Cl2 O20 111.8(2) . . ? O22 Cl2 O20 108.96(13) . . ? O23 Cl2 O21 110.5(2) . . ? O22 Cl2 O21 107.2(2) . . ? O20 Cl2 O21 107.86(14) . . ? _refine_diff_density_max 1.104 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.133 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Vitaly V, Pavlishchuk' 'A. Addison' 'Eugeny A. Goreshnik' 'Sergey V. Kolotilov' 'Michael J. Prushan' 'Dieter Schollmeyer' 'Laurence K. Thompson' 'Thomas Weyhermuller' _publ_contact_author_name 'Dr Vitaly V Pavlishchuk' _publ_contact_author_address ; L.V Pisarzhevskii Institute of Physical Chemistry of the National Academy of Sci Prospekt Nauki 31 Kiev 03039 UKRAINE ; _publ_contact_author_email 'PAVLISVV@PHYCHE.FREENET.KIEV.UA' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Structural, magnetic and related attributes of some tetranuclear nickel rhombs and a dinuclear congener ; data_ST3594 _database_code_CSD 192596 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C16 H36 N6 Ni2 O6]2+, 2 (ClO4)-' _chemical_formula_analytical ? _chemical_formula_sum 'C16 H36 Cl2 N6 Ni2 O14' _chemical_formula_weight 724.83 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5117(6) _cell_length_b 9.9561(8) _cell_length_c 10.3216(9) _cell_angle_alpha 62.35(2) _cell_angle_beta 75.05(2) _cell_angle_gamma 66.71(2) _cell_volume 708.67(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5911 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method ? _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type 'SADABS, G.M. Sheldrick 1994' _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.814 _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 'Siemens, SMART CCD-Detector' _diffrn_measurement_method '\w, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7625 _diffrn_reflns_av_R_equivalents 0.0141 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 33.70 _reflns_number_total 4602 _reflns_number_observed 3915 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4602 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_obs 0.0289 _refine_ls_wR_factor_all 0.0727 _refine_ls_wR_factor_obs 0.0715 _refine_ls_goodness_of_fit_all 0.974 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 0.974 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.98051(2) 0.96408(2) 0.69543(2) 0.01031(5) Uani 1 d . . O10 O 0.86097(13) 1.09135(12) 0.82883(11) 0.0138(2) Uani 1 d . . O2 O 0.89658(13) 1.17885(12) 0.52720(11) 0.0136(2) Uani 1 d . . O3 O 0.93472(14) 1.24394(13) 0.11827(11) 0.0161(2) Uani 1 d . . N2 N 0.90355(15) 1.20075(14) 0.39078(12) 0.0113(2) Uani 1 d . . N5 N 1.1813(2) 1.0388(2) 0.68505(14) 0.0154(2) Uani 1 d . . H5A H 1.2803(2) 0.9526(2) 0.70859(14) 0.018 Uiso 1 calc R . H5B H 1.2002(2) 1.1115(2) 0.59144(14) 0.018 Uiso 1 calc R . N8 N 0.7334(2) 0.9532(2) 0.72402(14) 0.0148(2) Uani 1 d . . H8A H 0.6835(2) 1.0145(2) 0.63675(14) 0.018 Uiso 1 calc R . H8B H 0.7381(2) 0.8492(2) 0.75394(14) 0.018 Uiso 1 calc R . C1 C 0.7602(2) 1.4839(2) 0.3450(2) 0.0188(3) Uani 1 d . . H1A H 0.7106(14) 1.5832(3) 0.2619(4) 0.028 Uiso 1 calc R . H1B H 0.8491(4) 1.4960(10) 0.3792(13) 0.028 Uiso 1 calc R . H1C H 0.6700(11) 1.4613(7) 0.4250(10) 0.028 Uiso 1 calc R . C2 C 0.8382(2) 1.3486(2) 0.2974(2) 0.0130(2) Uani 1 d . . C3 C 0.8527(2) 1.3628(2) 0.1476(2) 0.0145(3) Uani 1 d . . C4 C 0.7697(2) 1.5200(2) 0.0288(2) 0.0234(3) Uani 1 d . . H4A H 0.8089(14) 1.6026(4) 0.0240(10) 0.035 Uiso 1 calc R . H4B H 0.6447(2) 1.5495(8) 0.0504(8) 0.035 Uiso 1 calc R . H4C H 0.8014(14) 1.5107(5) -0.0656(3) 0.035 Uiso 1 calc R . C5 C 1.1343(2) 1.1137(2) 0.7903(2) 0.0178(3) Uani 1 d . . H5C H 1.2016(2) 1.1864(2) 0.7613(2) 0.021 Uiso 1 calc R . H5D H 1.1620(2) 1.0297(2) 0.8897(2) 0.021 Uiso 1 calc R . C6 C 0.9450(2) 1.2068(2) 0.7931(2) 0.0169(3) Uani 1 d . . H6A H 0.9104(2) 1.2509(2) 0.8685(2) 0.020 Uiso 1 calc R . H6B H 0.9161(2) 1.2962(2) 0.6963(2) 0.020 Uiso 1 calc R . C7 C 0.6787(2) 1.1537(2) 0.8179(2) 0.0169(3) Uani 1 d . . H7A H 0.6506(2) 1.2434(2) 0.7210(2) 0.020 Uiso 1 calc R . H7B H 0.6168(2) 1.1922(2) 0.8958(2) 0.020 Uiso 1 calc R . C8 C 0.6308(2) 1.0141(2) 0.8365(2) 0.0180(3) Uani 1 d . . H8C H 0.6535(2) 0.9278(2) 0.9358(2) 0.022 Uiso 1 calc R . H8D H 0.5069(2) 1.0492(2) 0.8257(2) 0.022 Uiso 1 calc R . Cl1 Cl 0.59417(4) 0.68514(4) 0.65078(4) 0.01598(7) Uani 1 d . . O11 O 0.77007(15) 0.6840(2) 0.62581(13) 0.0241(2) Uani 1 d . . O12 O 0.5143(2) 0.7831(2) 0.51517(14) 0.0326(3) Uani 1 d . . O13 O 0.5910(2) 0.52479(15) 0.7066(2) 0.0295(3) Uani 1 d . . O14 O 0.5031(2) 0.75147(15) 0.75837(14) 0.0250(3) Uani 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 Ni1 0.01117(9) 0.01020(9) 0.00881(9) -0.00344(6) -0.00093(6) -0.00323(6) O10 0.0143(5) 0.0145(5) 0.0142(5) -0.0069(4) -0.0004(4) -0.0054(4) O2 0.0169(5) 0.0138(5) 0.0090(5) -0.0045(4) -0.0019(3) -0.0038(4) O3 0.0185(5) 0.0152(5) 0.0125(5) -0.0046(4) -0.0012(4) -0.0048(4) N2 0.0110(5) 0.0122(5) 0.0096(5) -0.0029(4) -0.0011(4) -0.0045(4) N5 0.0143(6) 0.0149(6) 0.0149(6) -0.0042(5) -0.0020(4) -0.0045(4) N8 0.0157(6) 0.0145(6) 0.0151(6) -0.0059(5) -0.0016(4) -0.0057(4) C1 0.0234(8) 0.0122(6) 0.0191(7) -0.0067(6) -0.0046(6) -0.0022(5) C2 0.0137(6) 0.0118(6) 0.0124(6) -0.0036(5) -0.0016(5) -0.0044(5) C3 0.0143(6) 0.0139(6) 0.0127(6) -0.0028(5) -0.0014(5) -0.0050(5) C4 0.0299(9) 0.0158(7) 0.0143(7) -0.0012(6) -0.0060(6) -0.0009(6) C5 0.0203(7) 0.0188(7) 0.0182(7) -0.0070(6) -0.0055(5) -0.0084(6) C6 0.0209(7) 0.0158(7) 0.0188(7) -0.0089(6) -0.0017(5) -0.0083(5) C7 0.0131(7) 0.0183(7) 0.0188(7) -0.0104(6) 0.0018(5) -0.0031(5) C8 0.0141(7) 0.0204(7) 0.0191(7) -0.0091(6) 0.0032(5) -0.0069(5) Cl1 0.0138(2) 0.0135(2) 0.0190(2) -0.00410(13) -0.00376(12) -0.00448(12) O11 0.0147(5) 0.0283(6) 0.0281(6) -0.0085(5) -0.0011(4) -0.0100(5) O12 0.0275(7) 0.0383(8) 0.0233(7) -0.0021(6) -0.0128(5) -0.0084(6) O13 0.0275(7) 0.0164(6) 0.0450(8) -0.0117(6) -0.0013(5) -0.0097(5) O14 0.0211(6) 0.0240(6) 0.0295(6) -0.0148(5) -0.0023(5) -0.0021(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 N2 2.0201(13) 2_776 ? Ni1 O2 2.0208(12) . ? Ni1 N5 2.0789(13) . ? Ni1 O3 2.0846(13) 2_776 ? Ni1 N8 2.0868(13) . ? Ni1 O10 2.1008(11) . ? O10 C7 1.438(2) . ? O10 C6 1.446(2) . ? O2 N2 1.3099(15) . ? O3 C3 1.245(2) . ? O3 Ni1 2.0846(13) 2_776 ? N2 C2 1.310(2) . ? N2 Ni1 2.0200(12) 2_776 ? N5 C5 1.479(2) . ? N8 C8 1.479(2) . ? C1 C2 1.496(2) . ? C2 C3 1.462(2) . ? C3 C4 1.497(2) . ? C5 C6 1.509(2) . ? C7 C8 1.515(2) . ? Cl1 O13 1.4331(13) . ? Cl1 O12 1.4395(13) . ? Cl1 O11 1.4486(12) . ? Cl1 O14 1.4499(13) . ? 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 N2 Ni1 O2 107.24(4) 2_776 . ? N2 Ni1 N5 102.42(5) 2_776 . ? O2 Ni1 N5 85.37(5) . . ? N2 Ni1 O3 78.51(5) 2_776 2_776 ? O2 Ni1 O3 173.89(4) . 2_776 ? N5 Ni1 O3 91.41(5) . 2_776 ? N2 Ni1 N8 96.26(5) 2_776 . ? O2 Ni1 N8 86.21(5) . . ? N5 Ni1 N8 161.07(5) . . ? O3 Ni1 N8 95.31(5) 2_776 . ? N2 Ni1 O10 167.42(4) 2_776 . ? O2 Ni1 O10 84.94(4) . . ? N5 Ni1 O10 81.30(5) . . ? O3 Ni1 O10 89.44(4) 2_776 . ? N8 Ni1 O10 81.10(5) . . ? C7 O10 C6 116.37(11) . . ? C7 O10 Ni1 109.14(8) . . ? C6 O10 Ni1 108.95(8) . . ? N2 O2 Ni1 124.98(9) . . ? C3 O3 Ni1 112.40(9) . 2_776 ? O2 N2 C2 116.28(12) . . ? O2 N2 Ni1 127.49(9) . 2_776 ? C2 N2 Ni1 116.05(9) . 2_776 ? C5 N5 Ni1 108.36(9) . . ? C8 N8 Ni1 108.40(9) . . ? N2 C2 C3 112.81(13) . . ? N2 C2 C1 121.47(13) . . ? C3 C2 C1 125.71(13) . . ? O3 C3 C2 119.95(13) . . ? O3 C3 C4 119.73(13) . . ? C2 C3 C4 120.32(13) . . ? N5 C5 C6 110.14(12) . . ? O10 C6 C5 104.65(12) . . ? O10 C7 C8 104.99(12) . . ? N8 C8 C7 109.33(12) . . ? O13 Cl1 O12 110.45(9) . . ? O13 Cl1 O11 109.81(8) . . ? O12 Cl1 O11 109.39(8) . . ? O13 Cl1 O14 109.11(8) . . ? O12 Cl1 O14 109.61(8) . . ? O11 Cl1 O14 108.45(8) . . ? _refine_diff_density_max 0.978 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.081 data_ST3784 _database_code_CSD 192597 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C24 H50 N8 Ni4 O12]2+, 2 (ClO4)-, 0.6 H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C24 H51.20 Cl2 N8 Ni4 O20.60' _chemical_formula_weight 1087.27 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7838(6) _cell_length_b 20.327(2) _cell_length_c 11.1143(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.50(1) _cell_angle_gamma 90.00 _cell_volume 2056.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20067 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method ? _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 2.020 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Nonius KappaCCD' _diffrn_measurement_method '\391 images at 1 deg. in \w and 120 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20067 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5995 _reflns_number_observed 4691 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.5692P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5986 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_obs 0.0379 _refine_ls_wR_factor_all 0.0927 _refine_ls_wR_factor_obs 0.0847 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni -0.18364(3) -0.035388(13) 0.22430(3) 0.01394(8) Uani 1 d . . Ni2 Ni 0.12203(3) 0.025327(13) 0.45594(3) 0.01297(8) Uani 1 d . . N1 N -0.0472(2) -0.07382(10) 0.1315(2) 0.0209(4) Uani 1 d . . H1A H 0.0359(2) -0.04993(10) 0.1541(2) 0.025 Uiso 1 calc R . H1B H -0.0224(2) -0.11549(10) 0.1579(2) 0.025 Uiso 1 calc R . C2 C -0.1227(3) -0.07262(13) -0.0118(2) 0.0244(5) Uani 1 d . . H2A H -0.1633(3) -0.11571(13) -0.0422(2) 0.029 Uiso 1 calc R . H2B H -0.0527(3) -0.06181(13) -0.0518(2) 0.029 Uiso 1 calc R . C3 C -0.2452(3) -0.02176(12) -0.0495(2) 0.0242(5) Uani 1 d . . H3A H -0.2030(3) 0.02205(12) -0.0374(2) 0.029 Uiso 1 calc R . H3B H -0.3058(3) -0.02689(12) -0.1402(2) 0.029 Uiso 1 calc R . O4 O -0.3332(2) -0.02899(7) 0.0262(2) 0.0182(3) Uani 1 d . . C5 C -0.4295(3) -0.08644(12) -0.0071(2) 0.0212(5) Uani 1 d . . H5A H -0.3863(3) -0.12097(12) -0.0419(2) 0.025 Uiso 1 calc R . H5B H -0.5241(3) -0.07483(12) -0.0717(2) 0.025 Uiso 1 calc R . C6 C -0.4482(3) -0.10973(12) 0.1145(2) 0.0221(5) Uani 1 d . . H6A H -0.4992(3) -0.07652(12) 0.1448(2) 0.026 Uiso 1 calc R . H6B H -0.5063(3) -0.14972(12) 0.0971(2) 0.026 Uiso 1 calc R . N7 N -0.3011(2) -0.12241(10) 0.2148(2) 0.0200(4) Uani 1 d . . H7A H -0.2570(2) -0.15652(10) 0.1921(2) 0.024 Uiso 1 calc R . H7B H -0.3083(2) -0.13132(10) 0.2916(2) 0.024 Uiso 1 calc R . O11 O 0.2253(2) -0.02277(8) 0.3427(2) 0.0177(3) Uani 1 d . . C12 C 0.3173(2) -0.06376(11) 0.4089(2) 0.0172(4) Uani 1 d . . C13 C 0.3644(2) -0.06402(11) 0.5486(2) 0.0169(4) Uani 1 d . . N14 N 0.2919(2) -0.02161(9) 0.5917(2) 0.0151(4) Uani 1 d . . O15 O 0.3312(2) -0.01341(8) 0.71616(15) 0.0188(3) Uani 1 d . . C16 C 0.3804(3) -0.11294(13) 0.3433(2) 0.0257(5) Uani 1 d . . H16A H 0.3624(18) -0.15658(13) 0.3671(14) 0.038 Uiso 1 calc R . H16B H 0.4843(4) -0.1060(6) 0.3696(14) 0.038 Uiso 1 calc R . H16C H 0.3349(15) -0.1078(6) 0.2513(3) 0.038 Uiso 1 calc R . C17 C 0.4799(3) -0.10861(13) 0.6357(2) 0.0275(6) Uani 1 d . . H17A H 0.5733(5) -0.0867(4) 0.6641(15) 0.041 Uiso 1 calc R . H17B H 0.4850(15) -0.1479(4) 0.5895(6) 0.041 Uiso 1 calc R . H17C H 0.4557(11) -0.1199(8) 0.7094(10) 0.041 Uiso 1 calc R . O21 O 0.2365(2) 0.11535(7) 0.48883(15) 0.0170(3) Uani 1 d . . C22 C 0.1733(2) 0.15750(11) 0.4052(2) 0.0164(4) Uani 1 d . . C23 C 0.0395(2) 0.14091(10) 0.2973(2) 0.0167(4) Uani 1 d . . N24 N -0.0009(2) 0.07969(9) 0.3006(2) 0.0148(4) Uani 1 d . . O25 O -0.1132(2) 0.05737(8) 0.20336(15) 0.0186(3) Uani 1 d . . C26 C 0.2373(3) 0.22463(11) 0.4147(2) 0.0225(5) Uani 1 d . . H26A H 0.1724(10) 0.2560(2) 0.4304(18) 0.034 Uiso 1 calc R . H26B H 0.2497(19) 0.2353(4) 0.3352(7) 0.034 Uiso 1 calc R . H26C H 0.3309(10) 0.2259(3) 0.4846(12) 0.034 Uiso 1 calc R . C27 C -0.0436(3) 0.18762(12) 0.1919(2) 0.0267(6) Uani 1 d . . H27A H 0.0041(12) 0.1908(7) 0.1304(10) 0.040 Uiso 1 calc R . H27B H -0.0461(18) 0.2302(3) 0.2283(3) 0.040 Uiso 1 calc R . H27C H -0.1421(7) 0.1718(5) 0.1493(12) 0.040 Uiso 1 calc R . O30 O -0.0347(2) -0.04686(8) 0.40814(15) 0.0143(3) Uani 1 d . . H30 H -0.0030(29) -0.0820(14) 0.4148(26) 0.017 Uiso 1 d . . Cl1X Cl 0.1000(4) -0.23528(13) 0.4277(5) 0.0327(8) Uani 0.299(4) d P 2 O41X O 0.1298(10) -0.2384(4) 0.5610(8) 0.050(2) Uani 0.299(4) d P 2 O45X O -0.1146(12) -0.2194(6) 0.1050(12) 0.084(4) Uiso 0.299(4) d P 2 Cl1 Cl 0.0591(2) -0.23053(5) 0.3559(2) 0.0307(4) Uani 0.701(4) d P 1 O41 O -0.0134(4) -0.2137(2) 0.2219(3) 0.0518(10) Uani 0.701(4) d P 1 O44 O 0.1873(3) -0.27233(10) 0.3751(3) 0.0514(7) Uani 1 d . . O43 O 0.1084(3) -0.17023(11) 0.4163(3) 0.0619(8) Uani 1 d . . O42 O -0.0435(3) -0.26397(13) 0.3901(3) 0.0710(9) Uani 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 Ni1 0.01502(14) 0.01348(14) 0.01157(14) 0.00015(10) 0.00282(10) -0.00015(10) Ni2 0.01293(14) 0.01321(14) 0.01167(14) 0.00119(10) 0.00322(10) 0.00061(10) N1 0.0214(10) 0.0221(10) 0.0197(10) 0.0015(8) 0.0081(8) -0.0005(8) C2 0.0253(12) 0.0324(13) 0.0194(12) -0.0062(10) 0.0129(10) -0.0066(10) C3 0.0289(13) 0.0260(12) 0.0165(12) 0.0027(9) 0.0070(10) -0.0061(10) O4 0.0161(8) 0.0158(8) 0.0180(8) -0.0019(6) 0.0006(6) -0.0017(6) C5 0.0208(11) 0.0209(11) 0.0181(11) -0.0027(9) 0.0026(9) -0.0027(9) C6 0.0185(11) 0.0252(12) 0.0205(12) -0.0008(9) 0.0048(9) -0.0059(9) N7 0.0234(10) 0.0175(9) 0.0182(10) -0.0001(7) 0.0067(8) -0.0033(7) O11 0.0170(8) 0.0215(8) 0.0143(8) 0.0030(6) 0.0054(6) 0.0017(6) C12 0.0124(10) 0.0199(11) 0.0195(11) 0.0007(9) 0.0061(8) -0.0008(8) C13 0.0154(10) 0.0178(10) 0.0163(11) 0.0001(8) 0.0045(8) 0.0016(8) N14 0.0148(9) 0.0161(9) 0.0131(9) 0.0009(7) 0.0034(7) -0.0005(7) O15 0.0189(8) 0.0216(8) 0.0119(8) -0.0005(6) 0.0011(6) 0.0033(6) C16 0.0225(12) 0.0314(13) 0.0224(13) -0.0025(10) 0.0075(10) 0.0079(10) C17 0.0269(13) 0.0307(14) 0.0215(13) 0.0017(10) 0.0048(10) 0.0141(10) O21 0.0159(8) 0.0172(7) 0.0165(8) 0.0025(6) 0.0042(6) 0.0000(6) C22 0.0186(11) 0.0160(10) 0.0165(11) -0.0018(8) 0.0086(8) -0.0008(8) C23 0.0184(11) 0.0138(10) 0.0162(11) 0.0019(8) 0.0041(8) 0.0008(8) N24 0.0143(9) 0.0160(9) 0.0130(9) 0.0002(7) 0.0036(7) -0.0002(7) O25 0.0192(8) 0.0164(8) 0.0144(8) 0.0014(6) -0.0007(6) -0.0032(6) C26 0.0246(12) 0.0167(11) 0.0244(13) 0.0000(9) 0.0068(10) -0.0044(9) C27 0.0299(14) 0.0194(12) 0.0232(13) 0.0068(9) 0.0009(10) 0.0018(10) O30 0.0151(8) 0.0126(7) 0.0132(8) 0.0005(6) 0.0029(6) 0.0013(6) Cl1X 0.042(2) 0.0196(11) 0.042(2) -0.0009(12) 0.022(2) 0.0003(10) O41X 0.073(6) 0.044(4) 0.043(5) 0.005(4) 0.033(4) 0.005(4) Cl1 0.0365(6) 0.0159(4) 0.0473(10) 0.0035(5) 0.0243(7) 0.0050(4) O41 0.073(3) 0.034(2) 0.043(2) 0.0058(14) 0.015(2) 0.015(2) O44 0.066(2) 0.0246(10) 0.084(2) 0.0105(11) 0.0516(14) 0.0180(10) O43 0.0488(14) 0.0227(11) 0.114(2) -0.0125(13) 0.0296(15) 0.0062(10) O42 0.049(2) 0.053(2) 0.119(3) 0.020(2) 0.041(2) -0.0040(13) _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 O30 2.0421(15) . ? Ni1 O25 2.050(2) . ? Ni1 O15 2.051(2) 3_556 ? Ni1 N7 2.091(2) . ? Ni1 N1 2.113(2) . ? Ni1 O4 2.155(2) . ? Ni2 N14 2.028(2) . ? Ni2 N24 2.032(2) . ? Ni2 O30 2.037(2) 3_556 ? Ni2 O30 2.047(2) . ? Ni2 O21 2.106(2) . ? Ni2 O11 2.120(2) . ? N1 C2 1.490(3) . ? C2 C3 1.520(4) . ? C3 O4 1.415(3) . ? O4 C5 1.461(3) . ? C5 C6 1.505(3) . ? C6 N7 1.485(3) . ? O11 C12 1.249(3) . ? C12 C13 1.449(3) . ? C12 C16 1.497(3) . ? C13 N14 1.313(3) . ? C13 C17 1.494(3) . ? N14 O15 1.303(2) . ? O15 Ni1 2.051(2) 3_556 ? O21 C22 1.249(3) . ? C22 C23 1.454(3) . ? C22 C26 1.489(3) . ? C23 N24 1.310(3) . ? C23 C27 1.495(3) . ? N24 O25 1.308(2) . ? O30 Ni2 2.037(2) 3_556 ? Cl1X O43 1.334(3) . ? Cl1X O41X 1.402(10) . ? Cl1X O44 1.415(3) . ? Cl1X O42 1.434(4) . ? Cl1 O42 1.376(3) . ? Cl1 O43 1.396(3) . ? Cl1 O41 1.436(4) . ? Cl1 O44 1.464(2) . ? 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 O30 Ni1 O25 94.16(6) . . ? O30 Ni1 O15 93.48(6) . 3_556 ? O25 Ni1 O15 84.11(7) . 3_556 ? O30 Ni1 N7 97.54(7) . . ? O25 Ni1 N7 166.88(7) . . ? O15 Ni1 N7 89.24(8) 3_556 . ? O30 Ni1 N1 95.70(7) . . ? O25 Ni1 N1 89.20(7) . . ? O15 Ni1 N1 169.00(7) 3_556 . ? N7 Ni1 N1 95.53(8) . . ? O30 Ni1 O4 175.92(6) . . ? O25 Ni1 O4 87.65(6) . . ? O15 Ni1 O4 90.33(6) 3_556 . ? N7 Ni1 O4 81.07(7) . . ? N1 Ni1 O4 80.65(7) . . ? N14 Ni2 N24 163.13(8) . . ? N14 Ni2 O30 90.08(7) . 3_556 ? N24 Ni2 O30 103.59(7) . 3_556 ? N14 Ni2 O30 100.82(7) . . ? N24 Ni2 O30 90.88(7) . . ? O30 Ni2 O30 82.45(7) 3_556 . ? N14 Ni2 O21 92.34(7) . . ? N24 Ni2 O21 77.68(7) . . ? O30 Ni2 O21 91.46(6) 3_556 . ? O30 Ni2 O21 165.46(6) . . ? N14 Ni2 O11 77.63(7) . . ? N24 Ni2 O11 90.50(7) . . ? O30 Ni2 O11 163.79(6) 3_556 . ? O30 Ni2 O11 89.44(6) . . ? O21 Ni2 O11 99.48(6) . . ? C2 N1 Ni1 111.14(14) . . ? N1 C2 C3 109.8(2) . . ? O4 C3 C2 110.8(2) . . ? C3 O4 C5 114.1(2) . . ? C3 O4 Ni1 106.31(13) . . ? C5 O4 Ni1 110.12(13) . . ? O4 C5 C6 107.7(2) . . ? N7 C6 C5 109.0(2) . . ? C6 N7 Ni1 104.75(14) . . ? C12 O11 Ni2 110.80(15) . . ? O11 C12 C13 120.8(2) . . ? O11 C12 C16 119.7(2) . . ? C13 C12 C16 119.5(2) . . ? N14 C13 C12 112.7(2) . . ? N14 C13 C17 122.9(2) . . ? C12 C13 C17 124.4(2) . . ? O15 N14 C13 118.8(2) . . ? O15 N14 Ni2 124.89(14) . . ? C13 N14 Ni2 116.27(15) . . ? N14 O15 Ni1 115.82(12) . 3_556 ? C22 O21 Ni2 112.34(14) . . ? O21 C22 C23 120.3(2) . . ? O21 C22 C26 119.7(2) . . ? C23 C22 C26 119.9(2) . . ? N24 C23 C22 112.8(2) . . ? N24 C23 C27 122.8(2) . . ? C22 C23 C27 124.4(2) . . ? O25 N24 C23 118.5(2) . . ? O25 N24 Ni2 124.74(13) . . ? C23 N24 Ni2 116.71(14) . . ? N24 O25 Ni1 116.17(12) . . ? Ni2 O30 Ni1 112.22(7) 3_556 . ? Ni2 O30 Ni2 97.55(7) 3_556 . ? Ni1 O30 Ni2 111.70(7) . . ? O43 Cl1X O41X 98.5(4) . . ? O43 Cl1X O44 114.9(3) . . ? O41X Cl1X O44 119.3(5) . . ? O43 Cl1X O42 117.6(3) . . ? O41X Cl1X O42 95.3(4) . . ? O44 Cl1X O42 109.7(3) . . ? O42 Cl1 O43 117.3(2) . . ? O42 Cl1 O41 105.8(2) . . ? O43 Cl1 O41 104.0(2) . . ? O42 Cl1 O44 110.2(2) . . ? O43 Cl1 O44 108.2(2) . . ? O41 Cl1 O44 111.2(2) . . ? _refine_diff_density_max 0.636 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.096 data_ST3778 _database_code_CSD 192598 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C24 H50 N8 Ni4 O10 S2]2+, 2 (ClO4)-, 2 H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C24 H54 Cl2 N8 Ni4 O20 S2' _chemical_formula_weight 1144.61 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6136(6) _cell_length_b 13.7058(9) _cell_length_c 16.8831(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.52(1) _cell_angle_gamma 90.00 _cell_volume 2214.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6430 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method ? _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.971 _exptl_absorpt_correction_type 'Not corrected' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius Kappa-CCD' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20491 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6463 _reflns_number_observed 4532 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect' _computing_cell_refinement 'DENZO, Nonius Collect' _computing_data_reduction 'DENZO, Nonius Collect' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 33 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+4.5500P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6430 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_obs 0.0593 _refine_ls_wR_factor_all 0.1604 _refine_ls_wR_factor_obs 0.1419 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.044 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni -0.39948(5) 0.04960(4) -0.15959(3) 0.02009(13) Uani 1 d . . Ni2 Ni -0.56655(5) 0.10167(4) 0.00313(3) 0.01935(13) Uani 1 d . . O1 O -0.5311(3) -0.0021(2) -0.0799(2) 0.0212(5) Uani 1 d . . H1 H -0.6160(48) -0.0254(32) -0.1109(28) 0.025 Uiso 1 d . . N1 N -0.4224(3) -0.0761(3) -0.2317(2) 0.0250(7) Uani 1 d . . H1A H -0.4340(3) -0.1289(3) -0.2013(2) 0.030 Uiso 1 calc R . H1B H -0.4986(3) -0.0701(3) -0.2668(2) 0.030 Uiso 1 calc R . C2 C -0.2972(6) -0.0888(4) -0.2747(3) 0.0423(12) Uani 1 d . . H2A H -0.3130(6) -0.1426(4) -0.3118(3) 0.051 Uiso 1 calc R . H2B H -0.2188(6) -0.1062(4) -0.2368(3) 0.051 Uiso 1 calc R . C3 C -0.2594(5) 0.0001(4) -0.3195(3) 0.0406(11) Uani 1 d . . H3A H -0.3288(5) 0.0101(4) -0.3644(3) 0.049 Uiso 1 calc R . H3B H -0.1699(5) -0.0103(4) -0.3401(3) 0.049 Uiso 1 calc R . S4 S -0.24948(11) 0.10878(9) -0.25760(6) 0.0304(2) Uani 1 d . . C5 C -0.3803(5) 0.1872(4) -0.3100(3) 0.0411(11) Uani 1 d . . H5A H -0.3716(5) 0.2521(4) -0.2873(3) 0.049 Uiso 1 calc R . H5B H -0.3611(5) 0.1919(4) -0.3653(3) 0.049 Uiso 1 calc R . C6 C -0.5293(5) 0.1527(4) -0.3072(3) 0.0356(10) Uani 1 d . . H6A H -0.5931(5) 0.2028(4) -0.3290(3) 0.043 Uiso 1 calc R . H6B H -0.5448(5) 0.0947(4) -0.3398(3) 0.043 Uiso 1 calc R . N7 N -0.5592(3) 0.1303(3) -0.2248(2) 0.0255(7) Uani 1 d . . H7A H -0.6395(3) 0.0962(3) -0.2263(2) 0.031 Uiso 1 calc R . H7B H -0.5718(3) 0.1866(3) -0.1990(2) 0.031 Uiso 1 calc R . O11 O -0.7028(3) 0.1806(2) -0.0771(2) 0.0247(6) Uani 1 d . . C12 C -0.8276(4) 0.1714(3) -0.0635(2) 0.0252(8) Uani 1 d . . C13 C -0.8633(4) 0.1158(3) 0.0046(2) 0.0219(8) Uani 1 d . . N14 N -0.7564(3) 0.0687(2) 0.0401(2) 0.0206(6) Uani 1 d . . O15 O -0.7737(3) 0.0169(2) 0.1038(2) 0.0235(6) Uani 1 d . . C16 C -0.9405(5) 0.2176(4) -0.1182(3) 0.0389(11) Uani 1 d . . H16A H -0.8996(5) 0.2515(4) -0.1599(3) 0.058 Uiso 1 calc R . H16B H -0.9918(5) 0.2630(4) -0.0888(3) 0.058 Uiso 1 calc R . H16C H -1.0027(5) 0.1681(4) -0.1408(3) 0.058 Uiso 1 calc R . C17 C -1.0067(4) 0.1152(3) 0.0332(3) 0.0264(8) Uani 1 d . . H17A H -1.0067(4) 0.0736(3) 0.0789(3) 0.040 Uiso 1 calc R . H17B H -1.0731(4) 0.0912(3) -0.0084(3) 0.040 Uiso 1 calc R . H17C H -1.0318(4) 0.1803(3) 0.0472(3) 0.040 Uiso 1 calc R . O21 O -0.5524(3) 0.2119(2) 0.0902(2) 0.0227(5) Uani 1 d . . C22 C -0.4573(4) 0.2710(3) 0.0810(2) 0.0237(8) Uani 1 d . . C23 C -0.3747(4) 0.2623(3) 0.0132(2) 0.0230(8) Uani 1 d . . N24 N -0.4053(3) 0.1845(2) -0.0298(2) 0.0210(6) Uani 1 d . . O25 O -0.3429(3) 0.1715(2) -0.0942(2) 0.0244(6) Uani 1 d . . C26 C -0.4287(5) 0.3524(3) 0.1390(3) 0.0353(10) Uani 1 d . . H26A H -0.4915(5) 0.3478(3) 0.1798(3) 0.053 Uiso 1 calc R . H26B H -0.4422(5) 0.4137(3) 0.1119(3) 0.053 Uiso 1 calc R . H26C H -0.3341(5) 0.3480(3) 0.1627(3) 0.053 Uiso 1 calc R . C27 C -0.2711(4) 0.3366(3) -0.0088(3) 0.0296(9) Uani 1 d . . H27A H -0.2297(4) 0.3152(3) -0.0553(3) 0.044 Uiso 1 calc R . H27B H -0.1994(4) 0.3444(3) 0.0345(3) 0.044 Uiso 1 calc R . H27C H -0.3175(4) 0.3978(3) -0.0195(3) 0.044 Uiso 1 calc R . Cl1 Cl -0.31173(13) 0.58365(9) 0.25143(9) 0.0448(3) Uani 1 d . . O41 O -0.2347(5) 0.6548(4) 0.2996(4) 0.092(2) Uani 1 d . . O42 O -0.3338(5) 0.5004(3) 0.2967(3) 0.0739(14) Uani 1 d . . O43 O -0.4421(4) 0.6245(3) 0.2194(3) 0.0645(12) Uani 1 d . . O44 O -0.2297(4) 0.5544(3) 0.1878(2) 0.0459(9) Uani 1 d . . O50 O -0.3240(12) 0.5978(8) 0.0301(7) 0.080(3) Uiso 0.48 d P . O50X O -0.1485(34) 0.5889(22) 0.0149(19) 0.075(8) Uiso 0.17 d P . O50Y O -0.0518(29) 0.5714(19) 0.0111(16) 0.076(7) Uiso 0.20 d P . O50Z O -0.4199(37) 0.5651(25) 0.0214(21) 0.074(9) Uiso 0.15 d P . 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 0.0183(2) 0.0258(3) 0.0170(2) -0.0019(2) 0.0059(2) -0.0005(2) Ni2 0.0170(2) 0.0232(3) 0.0189(2) -0.0025(2) 0.0064(2) -0.0008(2) O1 0.0177(12) 0.0248(14) 0.0217(13) -0.0043(11) 0.0051(10) -0.0014(10) N1 0.023(2) 0.033(2) 0.0195(15) -0.0034(14) 0.0057(13) 0.0010(14) C2 0.054(3) 0.035(3) 0.043(3) -0.003(2) 0.026(2) 0.005(2) C3 0.044(3) 0.045(3) 0.036(2) -0.009(2) 0.021(2) 0.000(2) S4 0.0274(5) 0.0397(6) 0.0257(5) -0.0036(4) 0.0109(4) -0.0068(4) C5 0.040(3) 0.044(3) 0.040(3) 0.013(2) 0.010(2) 0.002(2) C6 0.032(2) 0.045(3) 0.030(2) 0.010(2) 0.002(2) -0.001(2) N7 0.024(2) 0.031(2) 0.022(2) -0.0037(14) 0.0070(13) 0.0024(14) O11 0.0232(13) 0.0272(14) 0.0250(13) 0.0017(11) 0.0083(11) 0.0021(11) C12 0.026(2) 0.026(2) 0.025(2) -0.002(2) 0.005(2) 0.002(2) C13 0.020(2) 0.023(2) 0.022(2) -0.0055(15) 0.0048(14) -0.0016(14) N14 0.0199(14) 0.024(2) 0.0187(14) -0.0049(12) 0.0071(12) -0.0016(12) O15 0.0196(12) 0.0321(15) 0.0199(12) 0.0023(11) 0.0072(10) -0.0004(11) C16 0.028(2) 0.052(3) 0.038(2) 0.010(2) 0.007(2) 0.010(2) C17 0.018(2) 0.031(2) 0.030(2) -0.006(2) 0.005(2) -0.001(2) O21 0.0219(12) 0.0231(13) 0.0243(13) -0.0053(11) 0.0084(11) -0.0013(11) C22 0.021(2) 0.027(2) 0.024(2) -0.002(2) 0.0067(15) 0.0002(15) C23 0.022(2) 0.025(2) 0.023(2) -0.001(2) 0.0070(15) -0.0011(15) N24 0.0186(14) 0.028(2) 0.0176(14) -0.0006(13) 0.0054(12) 0.0017(12) O25 0.0262(13) 0.0296(15) 0.0191(12) -0.0034(11) 0.0106(11) -0.0034(11) C26 0.036(2) 0.039(3) 0.035(2) -0.014(2) 0.019(2) -0.011(2) C27 0.033(2) 0.028(2) 0.030(2) -0.005(2) 0.015(2) -0.006(2) Cl1 0.0368(6) 0.0381(6) 0.0573(8) -0.0076(6) -0.0078(6) 0.0052(5) O41 0.046(2) 0.092(4) 0.133(5) -0.076(4) -0.011(3) 0.006(2) O42 0.107(4) 0.060(3) 0.060(3) 0.009(2) 0.033(3) 0.026(3) O43 0.034(2) 0.073(3) 0.084(3) 0.006(2) -0.007(2) 0.011(2) O44 0.040(2) 0.044(2) 0.052(2) 0.000(2) -0.004(2) -0.002(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 Ni1 O15 2.046(3) 3_455 ? Ni1 O25 2.048(3) . ? Ni1 O1 2.059(3) . ? Ni1 N1 2.110(3) . ? Ni1 N7 2.113(3) . ? Ni1 S4 2.4361(12) . ? Ni2 N14 2.036(3) . ? Ni2 N24 2.041(3) . ? Ni2 O1 2.046(3) 3_455 ? Ni2 O1 2.048(3) . ? Ni2 O11 2.093(3) . ? Ni2 O21 2.104(3) . ? O1 Ni2 2.047(3) 3_455 ? N1 C2 1.475(6) . ? C2 C3 1.497(7) . ? C3 S4 1.817(5) . ? S4 C5 1.818(5) . ? C5 C6 1.514(6) . ? C6 N7 1.479(5) . ? O11 C12 1.249(5) . ? C12 C13 1.448(6) . ? C12 C16 1.496(6) . ? C13 N14 1.310(5) . ? C13 C17 1.503(5) . ? N14 O15 1.312(4) . ? O15 Ni1 2.046(3) 3_455 ? O21 C22 1.242(5) . ? C22 C23 1.460(5) . ? C22 C26 1.492(6) . ? C23 N24 1.308(5) . ? C23 C27 1.495(5) . ? N24 O25 1.304(4) . ? Cl1 O42 1.401(5) . ? Cl1 O41 1.430(4) . ? Cl1 O43 1.431(4) . ? Cl1 O44 1.449(4) . ? O50 O50Z 1.02(3) . ? O50 O50X 1.74(3) . ? O50X O50Y 0.97(3) . ? 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 O15 Ni1 O25 87.31(11) 3_455 . ? O15 Ni1 O1 93.99(11) 3_455 . ? O25 Ni1 O1 94.40(10) . . ? O15 Ni1 N1 86.42(12) 3_455 . ? O25 Ni1 N1 170.31(12) . . ? O1 Ni1 N1 93.40(12) . . ? O15 Ni1 N7 172.26(12) 3_455 . ? O25 Ni1 N7 89.75(12) . . ? O1 Ni1 N7 93.38(12) . . ? N1 Ni1 N7 95.53(13) . . ? O15 Ni1 S4 87.29(8) 3_455 . ? O25 Ni1 S4 87.16(8) . . ? O1 Ni1 S4 178.03(8) . . ? N1 Ni1 S4 85.16(10) . . ? N7 Ni1 S4 85.42(10) . . ? N14 Ni2 N24 159.02(13) . . ? N14 Ni2 O1 91.59(12) . 3_455 ? N24 Ni2 O1 103.24(11) . 3_455 ? N14 Ni2 O1 105.60(12) . . ? N24 Ni2 O1 91.11(12) . . ? O1 Ni2 O1 82.76(11) 3_455 . ? N14 Ni2 O11 77.86(12) . . ? N24 Ni2 O11 88.90(12) . . ? O1 Ni2 O11 167.15(11) 3_455 . ? O1 Ni2 O11 92.93(11) . . ? N14 Ni2 O21 86.82(11) . . ? N24 Ni2 O21 77.94(11) . . ? O1 Ni2 O21 92.37(11) 3_455 . ? O1 Ni2 O21 166.71(10) . . ? O11 Ni2 O21 94.33(11) . . ? Ni2 O1 Ni2 97.24(11) 3_455 . ? Ni2 O1 Ni1 111.72(12) 3_455 . ? Ni2 O1 Ni1 111.17(12) . . ? C2 N1 Ni1 109.6(3) . . ? N1 C2 C3 113.7(4) . . ? C2 C3 S4 112.3(3) . . ? C3 S4 C5 102.1(3) . . ? C3 S4 Ni1 96.6(2) . . ? C5 S4 Ni1 95.8(2) . . ? C6 C5 S4 114.3(3) . . ? N7 C6 C5 111.4(4) . . ? C6 N7 Ni1 113.6(3) . . ? C12 O11 Ni2 112.4(3) . . ? O11 C12 C13 120.3(4) . . ? O11 C12 C16 119.8(4) . . ? C13 C12 C16 119.9(4) . . ? N14 C13 C12 112.8(3) . . ? N14 C13 C17 123.6(4) . . ? C12 C13 C17 123.6(4) . . ? C13 N14 O15 119.1(3) . . ? C13 N14 Ni2 115.9(3) . . ? O15 N14 Ni2 124.0(2) . . ? N14 O15 Ni1 117.2(2) . 3_455 ? C22 O21 Ni2 112.3(2) . . ? O21 C22 C23 120.6(4) . . ? O21 C22 C26 119.7(4) . . ? C23 C22 C26 119.7(3) . . ? N24 C23 C22 113.0(3) . . ? N24 C23 C27 122.5(3) . . ? C22 C23 C27 124.4(3) . . ? O25 N24 C23 118.4(3) . . ? O25 N24 Ni2 125.0(2) . . ? C23 N24 Ni2 116.1(3) . . ? N24 O25 Ni1 116.2(2) . . ? O42 Cl1 O41 110.0(4) . . ? O42 Cl1 O43 110.6(3) . . ? O41 Cl1 O43 109.6(3) . . ? O42 Cl1 O44 107.5(2) . . ? O41 Cl1 O44 108.7(3) . . ? O43 Cl1 O44 110.3(3) . . ? O50Z O50 O50X 145.5(25) . . ? O50Y O50X O50 168.8(35) . . ? _refine_diff_density_max 1.567 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.162 data_1a' _database_code_CSD 190465 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Cl2 N10 Ni4 O19' _chemical_formula_weight 1082.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 10.7475(6) _cell_length_b 17.8722(16) _cell_length_c 22.8691(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.903(5) _cell_angle_gamma 90.00 _cell_volume 4387.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 3.758 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'Corinc (Drager, 1971)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf Nonius' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method \q/2\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_reflns_number 8878 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 73.87 _reflns_number_total 8878 _reflns_number_gt 4954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius Software V5' _computing_cell_refinement 'Enraf Nonius Software V5' _computing_data_reduction 'Corinc (Drager, 1971)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1180P)^2^+0.0173P] 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_extinction_coef ? _refine_ls_number_reflns 8878 _refine_ls_number_parameters 586 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.1478 _refine_ls_R_factor_obs 0.0810 _refine_ls_wR_factor_ref 0.2389 _refine_ls_wR_factor_obs 0.1950 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.025 _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 Ni1 Ni 0.65747(11) 0.31384(7) 0.23137(5) 0.0284(3) Uani 1 1 d . . . Ni2 Ni 0.44305(11) 0.35079(7) 0.12122(5) 0.0292(3) Uani 1 1 d . . . Ni3 Ni 0.44565(10) 0.19111(7) 0.17044(5) 0.0279(3) Uani 1 1 d . . . Ni4 Ni 0.23177(11) 0.22806(7) 0.06010(5) 0.0323(3) Uani 1 1 d . . . N1 N 0.6490(6) 0.2455(4) 0.3065(3) 0.0387(15) Uani 1 1 d . . . C2 C 0.7805(8) 0.2263(5) 0.3200(4) 0.048(2) Uani 1 1 d . . . H2A H 0.8094 0.1929 0.2902 0.057 Uiso 1 1 calc R . . H2B H 0.7881 0.2005 0.3573 0.057 Uiso 1 1 calc R . . C3 C 0.8606(8) 0.2960(5) 0.3227(4) 0.043(2) Uani 1 1 d . . . H3A H 0.8396 0.3265 0.3558 0.052 Uiso 1 1 calc R . . H3B H 0.9478 0.2822 0.3276 0.052 Uiso 1 1 calc R . . N4 N 0.8386(6) 0.3389(4) 0.2674(3) 0.0328(14) Uani 1 1 d . . . C5 C 0.8405(8) 0.4201(4) 0.2765(4) 0.044(2) Uani 1 1 d . . . H5A H 0.8460 0.4452 0.2391 0.053 Uiso 1 1 calc R . . H5B H 0.9132 0.4337 0.3010 0.053 Uiso 1 1 calc R . . C6 C 0.7223(8) 0.4454(5) 0.3055(4) 0.045(2) Uani 1 1 d . . . H6A H 0.7243 0.4278 0.3457 0.054 Uiso 1 1 calc R . . H6B H 0.7186 0.4996 0.3060 0.054 Uiso 1 1 calc R . . N7 N 0.6111(6) 0.4154(4) 0.2731(3) 0.0417(16) Uani 1 1 d . . . O8 O 0.7071(5) 0.3737(3) 0.1591(2) 0.0427(14) Uani 1 1 d . . . N9 N 0.6253(5) 0.3729(4) 0.1143(3) 0.0330(14) Uani 1 1 d . . . C10 C 0.6618(7) 0.3977(5) 0.0636(4) 0.045(2) Uani 1 1 d . . . C11 C 0.5605(8) 0.3997(5) 0.0194(3) 0.043(2) Uani 1 1 d . . . O12 O 0.4523(5) 0.3877(3) 0.0319(2) 0.0439(14) Uani 1 1 d . . . C13 C 0.7927(9) 0.4216(8) 0.0539(5) 0.086(4) Uani 1 1 d . . . H13A H 0.8431 0.4151 0.0894 0.128 Uiso 1 1 calc R . . H13B H 0.7933 0.4733 0.0426 0.128 Uiso 1 1 calc R . . H13C H 0.8256 0.3917 0.0234 0.128 Uiso 1 1 calc R . . C14 C 0.5879(10) 0.4172(7) -0.0427(4) 0.067(3) Uani 1 1 d . . . H14A H 0.5117 0.4167 -0.0665 0.101 Uiso 1 1 calc R . . H14B H 0.6439 0.3803 -0.0569 0.101 Uiso 1 1 calc R . . H14C H 0.6255 0.4658 -0.0445 0.101 Uiso 1 1 calc R . . O15 O 0.4319(5) 0.4542(3) 0.1660(2) 0.0383(13) Uani 1 1 d . . . C16 C 0.3224(7) 0.4712(4) 0.1757(4) 0.0386(18) Uani 1 1 d . . . C17 C 0.2201(7) 0.4291(4) 0.1476(4) 0.0363(17) Uani 1 1 d . . . N18 N 0.2577(5) 0.3702(3) 0.1203(3) 0.0313(13) Uani 1 1 d . . . O19 O 0.1748(5) 0.3292(3) 0.0916(3) 0.0442(14) Uani 1 1 d . . . C20 C 0.2967(9) 0.5339(5) 0.2161(5) 0.064(3) Uani 1 1 d . . . H20A H 0.3740 0.5552 0.2309 0.096 Uiso 1 1 calc R . . H20B H 0.2511 0.5155 0.2481 0.096 Uiso 1 1 calc R . . H20C H 0.2485 0.5715 0.1953 0.096 Uiso 1 1 calc R . . C21 C 0.0870(8) 0.4500(6) 0.1500(6) 0.076(4) Uani 1 1 d . . . H21A H 0.0367 0.4144 0.1281 0.114 Uiso 1 1 calc R . . H21B H 0.0743 0.4989 0.1334 0.114 Uiso 1 1 calc R . . H21C H 0.0639 0.4503 0.1900 0.114 Uiso 1 1 calc R . . N22 N 0.2511(7) 0.2820(5) -0.0213(3) 0.0474(18) Uani 1 1 d . . . C23 C 0.1233(10) 0.3046(6) -0.0401(4) 0.063(3) Uani 1 1 d . . . H23A H 0.1212 0.3200 -0.0809 0.076 Uiso 1 1 calc R . . H23B H 0.0981 0.3469 -0.0169 0.076 Uiso 1 1 calc R . . C24 C 0.0354(9) 0.2419(7) -0.0331(5) 0.072(3) Uani 1 1 d . . . H24A H -0.0493 0.2605 -0.0383 0.086 Uiso 1 1 calc R . . H24B H 0.0475 0.2050 -0.0634 0.086 Uiso 1 1 calc R . . N25 N 0.0514(6) 0.2058(5) 0.0242(3) 0.0471(18) Uani 1 1 d . . . C26 C 0.0412(9) 0.1237(6) 0.0226(5) 0.066(3) Uani 1 1 d . . . H26A H -0.0306 0.1096 -0.0024 0.079 Uiso 1 1 calc R . . H26B H 0.0283 0.1052 0.0617 0.079 Uiso 1 1 calc R . . C27 C 0.1555(9) 0.0881(6) 0.0001(5) 0.066(3) Uani 1 1 d . . . H27A H 0.1513 0.0343 0.0054 0.079 Uiso 1 1 calc R . . H27B H 0.1594 0.0982 -0.0414 0.079 Uiso 1 1 calc R . . N28 N 0.2687(6) 0.1176(4) 0.0317(3) 0.0481(18) Uani 1 1 d . . . O29 O 0.1741(5) 0.1859(3) 0.1390(2) 0.0405(13) Uani 1 1 d . . . N30 N 0.2612(5) 0.1744(3) 0.1806(3) 0.0303(13) Uani 1 1 d . . . C31 C 0.2275(7) 0.1478(4) 0.2309(3) 0.0313(16) Uani 1 1 d . . . C32 C 0.3349(7) 0.1328(4) 0.2709(3) 0.0326(16) Uani 1 1 d . . . O33 O 0.4415(5) 0.1457(3) 0.2555(2) 0.0357(12) Uani 1 1 d . . . C34 C 0.0958(7) 0.1328(5) 0.2440(4) 0.050(2) Uani 1 1 d . . . H34A H 0.0422 0.1469 0.2110 0.075 Uiso 1 1 calc R . . H34B H 0.0745 0.1612 0.2776 0.075 Uiso 1 1 calc R . . H34C H 0.0854 0.0804 0.2518 0.075 Uiso 1 1 calc R . . C35 C 0.3168(9) 0.0996(6) 0.3298(4) 0.058(3) Uani 1 1 d . . . H35A H 0.3963 0.0933 0.3503 0.087 Uiso 1 1 calc R . . H35B H 0.2767 0.0518 0.3252 0.087 Uiso 1 1 calc R . . H35C H 0.2658 0.1322 0.3517 0.087 Uiso 1 1 calc R . . O36 O 0.4528(5) 0.0850(3) 0.1310(2) 0.0377(12) Uani 1 1 d . . . C37 C 0.5615(7) 0.0666(4) 0.1195(3) 0.0339(16) Uani 1 1 d . . . C38 C 0.6649(7) 0.1142(4) 0.1398(3) 0.0291(15) Uani 1 1 d . . . N39 N 0.6313(5) 0.1743(3) 0.1658(2) 0.0272(12) Uani 1 1 d . . . O40 O 0.7188(4) 0.2202(3) 0.1871(2) 0.0364(12) Uani 1 1 d . . . C41 C 0.5811(9) -0.0004(5) 0.0842(4) 0.056(2) Uani 1 1 d . . . H41A H 0.5021 -0.0230 0.0735 0.084 Uiso 1 1 calc R . . H41B H 0.6319 -0.0354 0.1065 0.084 Uiso 1 1 calc R . . H41C H 0.6222 0.0132 0.0494 0.084 Uiso 1 1 calc R . . C42 C 0.7962(8) 0.0939(5) 0.1291(4) 0.051(2) Uani 1 1 d . . . H42A H 0.8513 0.1307 0.1467 0.076 Uiso 1 1 calc R . . H42B H 0.8069 0.0922 0.0877 0.076 Uiso 1 1 calc R . . H42C H 0.8149 0.0458 0.1459 0.076 Uiso 1 1 calc R . . O43 O 0.4760(4) 0.2972(3) 0.1999(2) 0.0277(10) Uani 1 1 d . . . H43 H 0.4335 0.3127 0.2297 0.041 Uiso 1 1 d R . . O44 O 0.4123(4) 0.2442(3) 0.0923(2) 0.0282(10) Uani 1 1 d . . . H44 H 0.4474 0.2246 0.0632 0.042 Uiso 1 1 d R . . Cl1 Cl 0.6355(3) 0.17796(19) -0.03035(12) 0.0724(8) Uani 1 1 d D . . O11L O 0.7039(16) 0.2417(8) -0.0218(10) 0.167(8) Uani 0.70 1 d PDU A 1 O12L O 0.7166(15) 0.1141(8) -0.0327(8) 0.127(7) Uani 0.70 1 d PDU A 1 O13L O 0.5550(16) 0.1628(11) 0.0123(7) 0.101(7) Uani 0.70 1 d PDU A 1 O14L O 0.574(2) 0.1788(14) -0.0853(7) 0.190(9) Uani 0.70 1 d PDU A 1 O15L O 0.593(4) 0.2409(17) -0.0613(16) 0.17(2) Uani 0.30 1 d PDU A 2 O16L O 0.688(3) 0.1260(17) -0.0643(14) 0.114(13) Uani 0.30 1 d PDU A 2 O17L O 0.718(3) 0.2072(18) 0.0149(11) 0.104(11) Uani 0.30 1 d PDU A 2 O18L O 0.537(3) 0.148(2) -0.0009(14) 0.076(12) Uani 0.30 1 d PDU A 2 Cl2 Cl 0.2256(3) 0.34263(15) 0.31373(12) 0.0611(7) Uani 1 1 d D . . O21L O 0.3397(13) 0.3631(12) 0.2963(6) 0.097(9) Uani 0.70 1 d PDU B 1 O22L O 0.2325(13) 0.2781(7) 0.3458(6) 0.183(6) Uani 1 1 d DU B 1 O23L O 0.1488(11) 0.3206(7) 0.2638(5) 0.143(5) Uani 1 1 d DU B 1 O24L O 0.1618(13) 0.4006(8) 0.3382(6) 0.083(5) Uani 0.70 1 d PDU B 1 O25L O 0.202(5) 0.377(2) 0.3658(16) 0.17(3) Uani 0.30 1 d PDU B 2 O26L O 0.328(4) 0.377(3) 0.292(2) 0.12(2) Uani 0.30 1 d PDU B 2 O1W O -0.0608(8) 0.2751(5) 0.1397(6) 0.151(5) Uani 1 1 d . . . H1W H -0.0809 0.2602 0.1070 0.226 Uiso 1 1 d R . . H2W H -0.1267 0.2588 0.1544 0.226 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0269(6) 0.0323(7) 0.0257(6) -0.0040(5) -0.0006(5) -0.0018(5) Ni2 0.0251(6) 0.0319(7) 0.0303(7) -0.0013(5) -0.0012(5) -0.0007(5) Ni3 0.0230(6) 0.0310(7) 0.0296(7) -0.0033(5) 0.0019(5) 0.0001(5) Ni4 0.0285(6) 0.0418(8) 0.0263(6) -0.0071(6) -0.0012(5) -0.0027(6) N1 0.037(3) 0.043(4) 0.036(4) 0.004(3) -0.002(3) -0.012(3) C2 0.059(5) 0.038(5) 0.045(5) 0.007(4) -0.015(4) -0.004(4) C3 0.043(5) 0.040(5) 0.045(5) 0.004(4) -0.012(4) -0.004(4) N4 0.030(3) 0.036(3) 0.033(3) -0.004(3) -0.002(2) 0.001(3) C5 0.051(5) 0.032(4) 0.048(5) 0.004(4) -0.008(4) -0.010(4) C6 0.054(5) 0.030(4) 0.051(5) -0.004(4) -0.007(4) 0.003(4) N7 0.039(4) 0.038(4) 0.048(4) -0.012(3) -0.004(3) -0.001(3) O8 0.026(3) 0.063(4) 0.039(3) 0.009(3) -0.006(2) -0.012(3) N9 0.026(3) 0.041(4) 0.032(3) 0.001(3) -0.004(2) -0.002(3) C10 0.032(4) 0.063(6) 0.039(5) 0.011(4) 0.001(3) -0.007(4) C11 0.051(5) 0.049(5) 0.027(4) 0.005(4) -0.002(3) -0.012(4) O12 0.038(3) 0.054(4) 0.039(3) 0.006(3) -0.005(2) -0.007(3) C13 0.040(5) 0.160(13) 0.058(7) 0.033(8) 0.007(5) -0.029(7) C14 0.079(7) 0.088(8) 0.035(5) 0.014(5) 0.001(5) -0.011(6) O15 0.029(3) 0.035(3) 0.050(3) -0.001(3) -0.002(2) -0.002(2) C16 0.038(4) 0.028(4) 0.050(5) 0.004(4) -0.002(4) -0.002(3) C17 0.026(4) 0.036(4) 0.047(5) -0.007(4) 0.000(3) 0.000(3) N18 0.033(3) 0.036(3) 0.025(3) -0.004(3) -0.001(2) 0.001(3) O19 0.032(3) 0.054(4) 0.045(3) -0.019(3) -0.010(2) -0.003(3) C20 0.057(6) 0.036(5) 0.097(9) -0.026(5) -0.007(6) 0.003(4) C21 0.037(5) 0.063(7) 0.128(11) -0.033(7) -0.002(6) 0.010(5) N22 0.042(4) 0.067(5) 0.033(4) 0.005(4) 0.001(3) -0.009(4) C23 0.072(7) 0.072(7) 0.043(5) 0.019(5) -0.023(5) -0.004(6) C24 0.043(5) 0.112(10) 0.058(7) 0.021(7) -0.011(5) -0.007(6) N25 0.028(3) 0.071(5) 0.042(4) -0.001(4) -0.006(3) -0.008(3) C26 0.043(5) 0.076(7) 0.077(8) -0.018(6) -0.002(5) -0.029(5) C27 0.057(6) 0.056(6) 0.084(8) -0.028(6) -0.015(5) -0.008(5) N28 0.039(4) 0.047(4) 0.058(5) -0.020(4) 0.001(3) -0.005(3) O29 0.026(3) 0.060(4) 0.036(3) 0.003(3) -0.001(2) 0.000(3) N30 0.029(3) 0.035(3) 0.026(3) -0.009(3) -0.002(2) 0.005(3) C31 0.028(4) 0.033(4) 0.033(4) -0.001(3) 0.006(3) 0.003(3) C32 0.034(4) 0.028(4) 0.036(4) 0.001(3) -0.004(3) -0.002(3) O33 0.029(3) 0.039(3) 0.039(3) 0.007(2) -0.002(2) -0.004(2) C34 0.034(4) 0.065(6) 0.052(5) 0.010(5) 0.013(4) -0.007(4) C35 0.050(5) 0.081(7) 0.044(5) 0.017(5) 0.002(4) -0.003(5) O36 0.032(3) 0.036(3) 0.044(3) -0.004(2) 0.001(2) -0.004(2) C37 0.034(4) 0.033(4) 0.035(4) -0.002(3) 0.000(3) 0.002(3) C38 0.030(4) 0.027(4) 0.030(4) -0.003(3) 0.001(3) 0.003(3) N39 0.024(3) 0.039(3) 0.018(3) 0.001(2) -0.002(2) -0.004(2) O40 0.022(2) 0.045(3) 0.042(3) -0.013(3) 0.000(2) -0.002(2) C41 0.056(6) 0.045(5) 0.067(7) -0.019(5) -0.003(5) 0.004(4) C42 0.040(5) 0.040(5) 0.073(7) -0.017(4) 0.007(4) 0.011(4) O43 0.024(2) 0.034(3) 0.025(2) -0.008(2) 0.0034(19) -0.0012(19) O44 0.024(2) 0.037(3) 0.024(2) -0.007(2) 0.0049(18) 0.000(2) Cl1 0.0752(18) 0.087(2) 0.0567(16) -0.0019(14) 0.0243(14) -0.0148(16) O11L 0.141(13) 0.111(12) 0.250(17) -0.004(13) 0.008(13) -0.065(11) O12L 0.102(11) 0.150(13) 0.132(13) -0.038(11) 0.030(10) 0.047(10) O13L 0.118(13) 0.112(12) 0.077(10) -0.024(9) 0.055(9) 0.011(10) O14L 0.222(17) 0.220(17) 0.123(13) 0.055(13) -0.032(12) -0.050(15) O15L 0.21(3) 0.16(3) 0.15(2) 0.011(18) -0.010(18) -0.006(19) O16L 0.12(2) 0.14(2) 0.087(18) -0.068(15) 0.058(15) -0.004(16) O17L 0.117(19) 0.088(17) 0.106(18) -0.011(15) 0.005(15) -0.030(15) O18L 0.056(15) 0.097(19) 0.075(18) -0.034(15) 0.011(13) -0.025(13) Cl2 0.0681(16) 0.0562(14) 0.0616(15) -0.0074(12) 0.0278(13) -0.0055(12) O21L 0.074(13) 0.150(19) 0.071(11) -0.054(12) 0.043(9) -0.026(11) O22L 0.213(15) 0.161(13) 0.179(13) 0.103(11) 0.037(11) 0.035(11) O23L 0.155(10) 0.158(11) 0.114(9) -0.063(8) 0.002(8) -0.057(9) O24L 0.076(8) 0.081(10) 0.095(10) -0.045(8) 0.026(7) 0.026(7) O25L 0.28(6) 0.13(3) 0.12(3) -0.09(3) 0.13(4) -0.17(4) O26L 0.07(3) 0.13(4) 0.16(4) 0.06(3) 0.04(3) -0.04(3) O1W 0.075(7) 0.089(7) 0.296(16) 0.015(9) 0.083(9) 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 O8 2.061(6) . ? Ni1 O43 2.066(5) . ? Ni1 O40 2.080(5) . ? Ni1 N1 2.113(7) . ? Ni1 N7 2.121(7) . ? Ni1 N4 2.123(6) . ? Ni2 N9 2.012(6) . ? Ni2 N18 2.022(6) . ? Ni2 O44 2.037(5) . ? Ni2 O43 2.053(5) . ? Ni2 O15 2.119(6) . ? Ni2 O12 2.153(6) . ? Ni3 N39 2.026(6) . ? Ni3 N30 2.030(6) . ? Ni3 O43 2.032(5) . ? Ni3 O44 2.039(5) . ? Ni3 O36 2.102(5) . ? Ni3 O33 2.110(5) . ? Ni4 O19 2.052(6) . ? Ni4 O44 2.060(5) . ? Ni4 O29 2.079(6) . ? Ni4 N25 2.104(6) . ? Ni4 N22 2.116(7) . ? Ni4 N28 2.122(7) . ? N1 C2 1.472(10) . ? C2 C3 1.513(11) . ? C3 N4 1.487(10) . ? N4 C5 1.466(9) . ? C5 C6 1.532(12) . ? C6 N7 1.476(10) . ? O8 N9 1.317(7) . ? N9 C10 1.318(10) . ? C10 C11 1.448(11) . ? C10 C13 1.498(11) . ? C11 O12 1.231(9) . ? C11 C14 1.498(11) . ? O15 C16 1.247(9) . ? C16 C17 1.456(10) . ? C16 C20 1.486(12) . ? C17 N18 1.298(9) . ? C17 C21 1.481(11) . ? N18 O19 1.305(7) . ? N22 C23 1.475(11) . ? C23 C24 1.480(14) . ? C24 N25 1.465(12) . ? N25 C26 1.472(13) . ? C26 C27 1.497(13) . ? C27 N28 1.480(10) . ? O29 N30 1.317(7) . ? N30 C31 1.313(9) . ? C31 C32 1.461(10) . ? C31 C34 1.486(10) . ? C32 O33 1.237(9) . ? C32 C35 1.492(11) . ? O36 C37 1.254(8) . ? C37 C38 1.458(10) . ? C37 C41 1.466(11) . ? C38 N39 1.287(9) . ? C38 C42 1.489(10) . ? N39 O40 1.322(7) . ? Cl1 O16L 1.350(13) . ? Cl1 O13L 1.362(10) . ? Cl1 O11L 1.364(11) . ? Cl1 O14L 1.388(12) . ? Cl1 O18L 1.390(14) . ? Cl1 O15L 1.394(15) . ? Cl1 O17L 1.426(14) . ? Cl1 O12L 1.440(11) . ? Cl2 O21L 1.358(10) . ? Cl2 O22L 1.368(9) . ? Cl2 O25L 1.374(15) . ? Cl2 O24L 1.377(9) . ? Cl2 O26L 1.379(15) . ? Cl2 O23L 1.430(9) . ? 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 O8 Ni1 O43 94.2(2) . . ? O8 Ni1 O40 85.8(2) . . ? O43 Ni1 O40 91.76(19) . . ? O8 Ni1 N1 167.2(2) . . ? O43 Ni1 N1 97.0(2) . . ? O40 Ni1 N1 87.6(3) . . ? O8 Ni1 N7 89.6(3) . . ? O43 Ni1 N7 92.4(2) . . ? O40 Ni1 N7 174.0(2) . . ? N1 Ni1 N7 96.2(3) . . ? O8 Ni1 N4 86.1(2) . . ? O43 Ni1 N4 175.3(2) . . ? O40 Ni1 N4 93.0(2) . . ? N1 Ni1 N4 83.3(2) . . ? N7 Ni1 N4 82.9(2) . . ? N9 Ni2 N18 158.1(3) . . ? N9 Ni2 O44 107.5(2) . . ? N18 Ni2 O44 90.8(2) . . ? N9 Ni2 O43 92.0(2) . . ? N18 Ni2 O43 102.4(2) . . ? O44 Ni2 O43 82.30(19) . . ? N9 Ni2 O15 86.9(2) . . ? N18 Ni2 O15 77.0(2) . . ? O44 Ni2 O15 163.7(2) . . ? O43 Ni2 O15 89.7(2) . . ? N9 Ni2 O12 76.9(2) . . ? N18 Ni2 O12 91.8(2) . . ? O44 Ni2 O12 89.6(2) . . ? O43 Ni2 O12 163.7(2) . . ? O15 Ni2 O12 101.4(2) . . ? N39 Ni3 N30 162.6(3) . . ? N39 Ni3 O43 90.8(2) . . ? N30 Ni3 O43 103.9(2) . . ? N39 Ni3 O44 98.8(2) . . ? N30 Ni3 O44 92.3(2) . . ? O43 Ni3 O44 82.76(19) . . ? N39 Ni3 O36 77.6(2) . . ? N30 Ni3 O36 88.5(2) . . ? O43 Ni3 O36 167.0(2) . . ? O44 Ni3 O36 93.0(2) . . ? N39 Ni3 O33 93.3(2) . . ? N30 Ni3 O33 76.8(2) . . ? O43 Ni3 O33 93.7(2) . . ? O44 Ni3 O33 167.4(2) . . ? O36 Ni3 O33 92.9(2) . . ? O19 Ni4 O44 92.5(2) . . ? O19 Ni4 O29 84.7(2) . . ? O44 Ni4 O29 93.28(19) . . ? O19 Ni4 N25 91.0(3) . . ? O44 Ni4 N25 176.4(3) . . ? O29 Ni4 N25 87.7(2) . . ? O19 Ni4 N22 87.2(3) . . ? O44 Ni4 N22 96.8(2) . . ? O29 Ni4 N22 167.3(3) . . ? N25 Ni4 N22 82.7(3) . . ? O19 Ni4 N28 172.5(3) . . ? O44 Ni4 N28 93.0(2) . . ? O29 Ni4 N28 89.9(3) . . ? N25 Ni4 N28 83.5(3) . . ? N22 Ni4 N28 97.2(3) . . ? C2 N1 Ni1 103.0(5) . . ? N1 C2 C3 110.8(7) . . ? N4 C3 C2 108.9(6) . . ? C5 N4 C3 113.0(6) . . ? C5 N4 Ni1 105.6(5) . . ? C3 N4 Ni1 108.9(5) . . ? N4 C5 C6 110.4(7) . . ? N7 C6 C5 110.0(7) . . ? C6 N7 Ni1 109.6(5) . . ? N9 O8 Ni1 115.4(4) . . ? O8 N9 C10 117.6(6) . . ? O8 N9 Ni2 123.7(5) . . ? C10 N9 Ni2 118.0(5) . . ? N9 C10 C11 112.0(7) . . ? N9 C10 C13 123.4(8) . . ? C11 C10 C13 124.5(8) . . ? O12 C11 C10 121.2(7) . . ? O12 C11 C14 119.4(8) . . ? C10 C11 C14 119.4(8) . . ? C11 O12 Ni2 111.4(5) . . ? C16 O15 Ni2 112.1(5) . . ? O15 C16 C17 119.6(7) . . ? O15 C16 C20 120.1(8) . . ? C17 C16 C20 120.3(7) . . ? N18 C17 C16 112.6(7) . . ? N18 C17 C21 123.1(7) . . ? C16 C17 C21 124.2(8) . . ? C17 N18 O19 118.4(6) . . ? C17 N18 Ni2 117.7(5) . . ? O19 N18 Ni2 123.8(5) . . ? N18 O19 Ni4 117.6(4) . . ? C23 N22 Ni4 104.5(5) . . ? N22 C23 C24 110.6(8) . . ? N25 C24 C23 112.6(8) . . ? C24 N25 C26 114.3(9) . . ? C24 N25 Ni4 109.3(6) . . ? C26 N25 Ni4 105.3(5) . . ? N25 C26 C27 111.8(8) . . ? N28 C27 C26 110.5(8) . . ? C27 N28 Ni4 108.6(6) . . ? N30 O29 Ni4 116.8(4) . . ? C31 N30 O29 118.2(6) . . ? C31 N30 Ni3 117.9(5) . . ? O29 N30 Ni3 123.8(5) . . ? N30 C31 C32 111.8(6) . . ? N30 C31 C34 123.3(7) . . ? C32 C31 C34 124.9(7) . . ? O33 C32 C31 120.0(7) . . ? O33 C32 C35 119.8(7) . . ? C31 C32 C35 120.1(7) . . ? C32 O33 Ni3 113.5(5) . . ? C37 O36 Ni3 112.4(5) . . ? O36 C37 C38 118.9(7) . . ? O36 C37 C41 119.5(7) . . ? C38 C37 C41 121.6(7) . . ? N39 C38 C37 114.0(6) . . ? N39 C38 C42 124.7(7) . . ? C37 C38 C42 121.3(7) . . ? C38 N39 O40 118.5(6) . . ? C38 N39 Ni3 116.6(5) . . ? O40 N39 Ni3 124.9(4) . . ? N39 O40 Ni1 116.2(4) . . ? Ni3 O43 Ni2 97.34(19) . . ? Ni3 O43 Ni1 112.5(2) . . ? Ni2 O43 Ni1 110.9(2) . . ? Ni2 O44 Ni3 97.6(2) . . ? Ni2 O44 Ni4 112.4(2) . . ? Ni3 O44 Ni4 111.6(2) . . ? O16L Cl1 O13L 124.9(19) . . ? O16L Cl1 O11L 115(2) . . ? O13L Cl1 O11L 114.9(11) . . ? O16L Cl1 O14L 71.3(17) . . ? O13L Cl1 O14L 111.1(11) . . ? O11L Cl1 O14L 110.4(12) . . ? O16L Cl1 O18L 111(2) . . ? O13L Cl1 O18L 18.4(19) . . ? O11L Cl1 O18L 132.2(18) . . ? O14L Cl1 O18L 96.1(18) . . ? O16L Cl1 O15L 113.5(18) . . ? O13L Cl1 O15L 109(2) . . ? O11L Cl1 O15L 63.9(18) . . ? O14L Cl1 O15L 53.4(18) . . ? O18L Cl1 O15L 108.8(19) . . ? O16L Cl1 O17L 114.1(17) . . ? O13L Cl1 O17L 86.9(16) . . ? O11L Cl1 O17L 44.0(13) . . ? O14L Cl1 O17L 154.3(15) . . ? O18L Cl1 O17L 104.4(15) . . ? O15L Cl1 O17L 104.4(18) . . ? O16L Cl1 O12L 33.1(16) . . ? O13L Cl1 O12L 106.1(11) . . ? O11L Cl1 O12L 110.1(9) . . ? O14L Cl1 O12L 103.6(12) . . ? O18L Cl1 O12L 101(2) . . ? O15L Cl1 O12L 143.6(19) . . ? O17L Cl1 O12L 87.9(16) . . ? O21L Cl2 O22L 111.0(10) . . ? O21L Cl2 O25L 110(2) . . ? O22L Cl2 O25L 85(2) . . ? O21L Cl2 O24L 113.1(10) . . ? O22L Cl2 O24L 115.6(9) . . ? O25L Cl2 O24L 36(3) . . ? O21L Cl2 O26L 13(4) . . ? O22L Cl2 O26L 124(3) . . ? O25L Cl2 O26L 108(2) . . ? O24L Cl2 O26L 103(3) . . ? O21L Cl2 O23L 109.4(7) . . ? O22L Cl2 O23L 102.1(8) . . ? O25L Cl2 O23L 133(3) . . ? O24L Cl2 O23L 104.7(8) . . ? O26L Cl2 O23L 106(2) . . ? 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 O8 Ni1 N1 C2 6.8(14) . . . . ? O43 Ni1 N1 C2 157.2(5) . . . . ? O40 Ni1 N1 C2 65.7(5) . . . . ? N7 Ni1 N1 C2 -109.6(5) . . . . ? N4 Ni1 N1 C2 -27.5(5) . . . . ? Ni1 N1 C2 C3 51.2(8) . . . . ? N1 C2 C3 N4 -53.7(10) . . . . ? C2 C3 N4 C5 143.2(7) . . . . ? C2 C3 N4 Ni1 26.2(8) . . . . ? O8 Ni1 N4 C5 66.4(5) . . . . ? O43 Ni1 N4 C5 -28(3) . . . . ? O40 Ni1 N4 C5 151.9(5) . . . . ? N1 Ni1 N4 C5 -120.8(5) . . . . ? N7 Ni1 N4 C5 -23.7(5) . . . . ? O8 Ni1 N4 C3 -172.0(5) . . . . ? O43 Ni1 N4 C3 94(3) . . . . ? O40 Ni1 N4 C3 -86.5(5) . . . . ? N1 Ni1 N4 C3 0.8(5) . . . . ? N7 Ni1 N4 C3 98.0(5) . . . . ? C3 N4 C5 C6 -72.9(8) . . . . ? Ni1 N4 C5 C6 46.0(7) . . . . ? N4 C5 C6 N7 -50.9(9) . . . . ? C5 C6 N7 Ni1 28.0(8) . . . . ? O8 Ni1 N7 C6 -88.8(6) . . . . ? O43 Ni1 N7 C6 177.0(5) . . . . ? O40 Ni1 N7 C6 -50(3) . . . . ? N1 Ni1 N7 C6 79.7(6) . . . . ? N4 Ni1 N7 C6 -2.7(6) . . . . ? O43 Ni1 O8 N9 -10.5(5) . . . . ? O40 Ni1 O8 N9 81.0(5) . . . . ? N1 Ni1 O8 N9 140.2(10) . . . . ? N7 Ni1 O8 N9 -102.8(5) . . . . ? N4 Ni1 O8 N9 174.3(5) . . . . ? Ni1 O8 N9 C10 -167.2(6) . . . . ? Ni1 O8 N9 Ni2 22.2(7) . . . . ? N18 Ni2 N9 O8 110.8(8) . . . . ? O44 Ni2 N9 O8 -103.6(6) . . . . ? O43 Ni2 N9 O8 -21.1(6) . . . . ? O15 Ni2 N9 O8 68.6(6) . . . . ? O12 Ni2 N9 O8 171.0(6) . . . . ? N18 Ni2 N9 C10 -59.7(10) . . . . ? O44 Ni2 N9 C10 85.8(7) . . . . ? O43 Ni2 N9 C10 168.4(7) . . . . ? O15 Ni2 N9 C10 -102.0(7) . . . . ? O12 Ni2 N9 C10 0.5(6) . . . . ? O8 N9 C10 C11 -175.2(7) . . . . ? Ni2 N9 C10 C11 -4.0(10) . . . . ? O8 N9 C10 C13 4.3(14) . . . . ? Ni2 N9 C10 C13 175.4(9) . . . . ? N9 C10 C11 O12 8.0(13) . . . . ? C13 C10 C11 O12 -171.4(10) . . . . ? N9 C10 C11 C14 -172.3(9) . . . . ? C13 C10 C11 C14 8.3(16) . . . . ? C10 C11 O12 Ni2 -7.4(11) . . . . ? C14 C11 O12 Ni2 172.9(7) . . . . ? N9 Ni2 O12 C11 3.7(6) . . . . ? N18 Ni2 O12 C11 164.9(6) . . . . ? O44 Ni2 O12 C11 -104.4(6) . . . . ? O43 Ni2 O12 C11 -44.4(11) . . . . ? O15 Ni2 O12 C11 87.8(6) . . . . ? N9 Ni2 O15 C16 172.9(6) . . . . ? N18 Ni2 O15 C16 7.8(5) . . . . ? O44 Ni2 O15 C16 -34.5(10) . . . . ? O43 Ni2 O15 C16 -95.0(5) . . . . ? O12 Ni2 O15 C16 97.0(6) . . . . ? Ni2 O15 C16 C17 -11.2(9) . . . . ? Ni2 O15 C16 C20 168.6(7) . . . . ? O15 C16 C17 N18 8.7(11) . . . . ? C20 C16 C17 N18 -171.1(8) . . . . ? O15 C16 C17 C21 -172.0(9) . . . . ? C20 C16 C17 C21 8.2(14) . . . . ? C16 C17 N18 O19 -177.7(7) . . . . ? C21 C17 N18 O19 3.0(13) . . . . ? C16 C17 N18 Ni2 -1.1(9) . . . . ? C21 C17 N18 Ni2 179.6(8) . . . . ? N9 Ni2 N18 C17 -46.8(10) . . . . ? O44 Ni2 N18 C17 165.8(6) . . . . ? O43 Ni2 N18 C17 83.5(6) . . . . ? O15 Ni2 N18 C17 -3.3(6) . . . . ? O12 Ni2 N18 C17 -104.6(6) . . . . ? N9 Ni2 N18 O19 129.6(7) . . . . ? O44 Ni2 N18 O19 -17.8(6) . . . . ? O43 Ni2 N18 O19 -100.1(6) . . . . ? O15 Ni2 N18 O19 173.1(6) . . . . ? O12 Ni2 N18 O19 71.8(6) . . . . ? C17 N18 O19 Ni4 -170.4(6) . . . . ? Ni2 N18 O19 Ni4 13.2(8) . . . . ? O44 Ni4 O19 N18 -0.7(5) . . . . ? O29 Ni4 O19 N18 92.3(5) . . . . ? N25 Ni4 O19 N18 179.9(5) . . . . ? N22 Ni4 O19 N18 -97.4(5) . . . . ? N28 Ni4 O19 N18 136.0(19) . . . . ? O19 Ni4 N22 C23 -64.5(6) . . . . ? O44 Ni4 N22 C23 -156.7(6) . . . . ? O29 Ni4 N22 C23 -14.3(16) . . . . ? N25 Ni4 N22 C23 26.9(6) . . . . ? N28 Ni4 N22 C23 109.4(6) . . . . ? Ni4 N22 C23 C24 -46.8(10) . . . . ? N22 C23 C24 N25 47.6(13) . . . . ? C23 C24 N25 C26 -139.7(10) . . . . ? C23 C24 N25 Ni4 -21.9(12) . . . . ? O19 Ni4 N25 C24 83.7(7) . . . . ? O44 Ni4 N25 C24 -85(4) . . . . ? O29 Ni4 N25 C24 168.3(7) . . . . ? N22 Ni4 N25 C24 -3.3(7) . . . . ? N28 Ni4 N25 C24 -101.5(7) . . . . ? O19 Ni4 N25 C26 -153.1(6) . . . . ? O44 Ni4 N25 C26 38(4) . . . . ? O29 Ni4 N25 C26 -68.4(6) . . . . ? N22 Ni4 N25 C26 119.9(6) . . . . ? N28 Ni4 N25 C26 21.7(6) . . . . ? C24 N25 C26 C27 75.5(10) . . . . ? Ni4 N25 C26 C27 -44.4(10) . . . . ? N25 C26 C27 N28 50.2(13) . . . . ? C26 C27 N28 Ni4 -28.3(11) . . . . ? O19 Ni4 N28 C27 48(2) . . . . ? O44 Ni4 N28 C27 -175.5(7) . . . . ? O29 Ni4 N28 C27 91.2(7) . . . . ? N25 Ni4 N28 C27 3.5(7) . . . . ? N22 Ni4 N28 C27 -78.3(7) . . . . ? O19 Ni4 O29 N30 -99.0(5) . . . . ? O44 Ni4 O29 N30 -6.9(5) . . . . ? N25 Ni4 O29 N30 169.7(5) . . . . ? N22 Ni4 O29 N30 -149.4(11) . . . . ? N28 Ni4 O29 N30 86.2(5) . . . . ? Ni4 O29 N30 C31 -179.9(5) . . . . ? Ni4 O29 N30 Ni3 -2.8(7) . . . . ? N39 Ni3 N30 C31 58.2(10) . . . . ? O43 Ni3 N30 C31 -88.8(6) . . . . ? O44 Ni3 N30 C31 -171.9(5) . . . . ? O36 Ni3 N30 C31 95.1(6) . . . . ? O33 Ni3 N30 C31 1.7(5) . . . . ? N39 Ni3 N30 O29 -118.9(8) . . . . ? O43 Ni3 N30 O29 94.0(5) . . . . ? O44 Ni3 N30 O29 10.9(5) . . . . ? O36 Ni3 N30 O29 -82.1(5) . . . . ? O33 Ni3 N30 O29 -175.4(6) . . . . ? O29 N30 C31 C32 175.7(6) . . . . ? Ni3 N30 C31 C32 -1.6(8) . . . . ? O29 N30 C31 C34 -2.5(11) . . . . ? Ni3 N30 C31 C34 -179.8(6) . . . . ? N30 C31 C32 O33 0.1(10) . . . . ? C34 C31 C32 O33 178.3(8) . . . . ? N30 C31 C32 C35 -177.7(8) . . . . ? C34 C31 C32 C35 0.4(12) . . . . ? C31 C32 O33 Ni3 1.3(9) . . . . ? C35 C32 O33 Ni3 179.2(6) . . . . ? N39 Ni3 O33 C32 -167.1(5) . . . . ? N30 Ni3 O33 C32 -1.6(5) . . . . ? O43 Ni3 O33 C32 101.9(5) . . . . ? O44 Ni3 O33 C32 28.7(12) . . . . ? O36 Ni3 O33 C32 -89.3(5) . . . . ? N39 Ni3 O36 C37 -5.8(5) . . . . ? N30 Ni3 O36 C37 -175.2(5) . . . . ? O43 Ni3 O36 C37 21.9(12) . . . . ? O44 Ni3 O36 C37 92.6(5) . . . . ? O33 Ni3 O36 C37 -98.6(5) . . . . ? Ni3 O36 C37 C38 6.8(9) . . . . ? Ni3 O36 C37 C41 -171.0(7) . . . . ? O36 C37 C38 N39 -3.6(11) . . . . ? C41 C37 C38 N39 174.2(8) . . . . ? O36 C37 C38 C42 178.0(7) . . . . ? C41 C37 C38 C42 -4.2(12) . . . . ? C37 C38 N39 O40 178.4(6) . . . . ? C42 C38 N39 O40 -3.2(11) . . . . ? C37 C38 N39 Ni3 -1.9(8) . . . . ? C42 C38 N39 Ni3 176.5(6) . . . . ? N30 Ni3 N39 C38 41.9(11) . . . . ? O43 Ni3 N39 C38 -169.9(5) . . . . ? O44 Ni3 N39 C38 -87.2(5) . . . . ? O36 Ni3 N39 C38 4.1(5) . . . . ? O33 Ni3 N39 C38 96.3(5) . . . . ? N30 Ni3 N39 O40 -138.4(7) . . . . ? O43 Ni3 N39 O40 9.7(5) . . . . ? O44 Ni3 N39 O40 92.5(5) . . . . ? O36 Ni3 N39 O40 -176.3(6) . . . . ? O33 Ni3 N39 O40 -84.0(5) . . . . ? C38 N39 O40 Ni1 -177.6(5) . . . . ? Ni3 N39 O40 Ni1 2.7(7) . . . . ? O8 Ni1 O40 N39 -107.5(5) . . . . ? O43 Ni1 O40 N39 -13.4(5) . . . . ? N1 Ni1 O40 N39 83.5(5) . . . . ? N7 Ni1 O40 N39 -147(2) . . . . ? N4 Ni1 O40 N39 166.6(5) . . . . ? N39 Ni3 O43 Ni2 98.6(2) . . . . ? N30 Ni3 O43 Ni2 -90.7(2) . . . . ? O44 Ni3 O43 Ni2 -0.18(18) . . . . ? O36 Ni3 O43 Ni2 71.6(10) . . . . ? O33 Ni3 O43 Ni2 -168.01(19) . . . . ? N39 Ni3 O43 Ni1 -17.6(3) . . . . ? N30 Ni3 O43 Ni1 153.0(2) . . . . ? O44 Ni3 O43 Ni1 -116.4(2) . . . . ? O36 Ni3 O43 Ni1 -44.6(10) . . . . ? O33 Ni3 O43 Ni1 75.7(2) . . . . ? N9 Ni2 O43 Ni3 -107.2(2) . . . . ? N18 Ni2 O43 Ni3 89.3(2) . . . . ? O44 Ni2 O43 Ni3 0.18(19) . . . . ? O15 Ni2 O43 Ni3 165.9(2) . . . . ? O12 Ni2 O43 Ni3 -60.6(8) . . . . ? N9 Ni2 O43 Ni1 10.3(3) . . . . ? N18 Ni2 O43 Ni1 -153.2(2) . . . . ? O44 Ni2 O43 Ni1 117.7(2) . . . . ? O15 Ni2 O43 Ni1 -76.5(2) . . . . ? O12 Ni2 O43 Ni1 56.9(8) . . . . ? O8 Ni1 O43 Ni3 104.8(3) . . . . ? O40 Ni1 O43 Ni3 18.9(3) . . . . ? N1 Ni1 O43 Ni3 -68.9(3) . . . . ? N7 Ni1 O43 Ni3 -165.5(3) . . . . ? N4 Ni1 O43 Ni3 -161(3) . . . . ? O8 Ni1 O43 Ni2 -3.1(3) . . . . ? O40 Ni1 O43 Ni2 -88.9(2) . . . . ? N1 Ni1 O43 Ni2 -176.8(3) . . . . ? N7 Ni1 O43 Ni2 86.7(3) . . . . ? N4 Ni1 O43 Ni2 91(3) . . . . ? N9 Ni2 O44 Ni3 89.5(2) . . . . ? N18 Ni2 O44 Ni3 -102.6(2) . . . . ? O43 Ni2 O44 Ni3 -0.18(18) . . . . ? O15 Ni2 O44 Ni3 -61.6(8) . . . . ? O12 Ni2 O44 Ni3 165.6(2) . . . . ? N9 Ni2 O44 Ni4 -153.2(2) . . . . ? N18 Ni2 O44 Ni4 14.6(3) . . . . ? O43 Ni2 O44 Ni4 117.0(2) . . . . ? O15 Ni2 O44 Ni4 55.6(8) . . . . ? O12 Ni2 O44 Ni4 -77.2(2) . . . . ? N39 Ni3 O44 Ni2 -89.5(2) . . . . ? N30 Ni3 O44 Ni2 103.9(2) . . . . ? O43 Ni3 O44 Ni2 0.18(19) . . . . ? O36 Ni3 O44 Ni2 -167.5(2) . . . . ? O33 Ni3 O44 Ni2 74.5(10) . . . . ? N39 Ni3 O44 Ni4 152.7(2) . . . . ? N30 Ni3 O44 Ni4 -13.9(3) . . . . ? O43 Ni3 O44 Ni4 -117.7(2) . . . . ? O36 Ni3 O44 Ni4 74.7(2) . . . . ? O33 Ni3 O44 Ni4 -43.4(10) . . . . ? O19 Ni4 O44 Ni2 -10.5(3) . . . . ? O29 Ni4 O44 Ni2 -95.3(3) . . . . ? N25 Ni4 O44 Ni2 158(4) . . . . ? N22 Ni4 O44 Ni2 76.9(3) . . . . ? N28 Ni4 O44 Ni2 174.6(3) . . . . ? O19 Ni4 O44 Ni3 98.0(3) . . . . ? O29 Ni4 O44 Ni3 13.2(3) . . . . ? N25 Ni4 O44 Ni3 -93(4) . . . . ? N22 Ni4 O44 Ni3 -174.5(3) . . . . ? N28 Ni4 O44 Ni3 -76.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 73.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.697 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.128 data_1b _database_code_CSD 190466 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H22 Cl N6 Ni2 O11' _chemical_formula_weight 591.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' 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' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 15.137(5) _cell_length_b 14.921(7) _cell_length_c 21.516(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4860(4) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 3.511 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Corinc (Drager, 1971)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf Nonius' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method \q/2\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 20 _diffrn_reflns_number 7142 _diffrn_reflns_av_R_equivalents 0.1239 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 73.93 _reflns_number_total 2568 _reflns_number_gt 1190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius Software V5' _computing_cell_refinement 'Enraf Nonius Software V5' _computing_data_reduction 'Corinc (Drager, 1971)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1819P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2568 _refine_ls_number_parameters 155 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1755 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.3200 _refine_ls_wR_factor_obs 0.2572 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Ni1 Ni 0.39848(11) 0.5000 0.0000 0.0396(5) Uani 1 2 d S . . O12 O 0.5000 0.4222(5) -0.0352(4) 0.0385(17) Uani 1 2 d S . . Ni2 Ni 0.5000 0.29698(14) 0.00379(10) 0.0434(6) Uani 1 2 d S . . O1 O 0.3079(4) 0.5685(5) 0.0585(3) 0.0563(16) Uani 1 1 d . . . C2 C 0.2922(6) 0.5284(7) 0.1072(4) 0.052(2) Uani 1 1 d . . . C3 C 0.3250(5) 0.4354(7) 0.1154(4) 0.050(2) Uani 1 1 d . . . N4 N 0.3776(4) 0.4116(5) 0.0699(3) 0.0433(16) Uani 1 1 d . . . O5 O 0.4091(4) 0.3302(4) 0.0706(3) 0.0549(16) Uani 1 1 d . . . C6 C 0.2434(9) 0.5693(9) 0.1596(6) 0.087(4) Uani 1 1 d . . . C7 C 0.3007(8) 0.3762(8) 0.1681(5) 0.075(3) Uani 1 1 d . . . H7A H 0.3299 0.3194 0.1635 0.112 Uiso 1 1 d R . . H7B H 0.2377 0.3672 0.1687 0.112 Uiso 1 1 d R . . H7C H 0.3189 0.4038 0.2065 0.112 Uiso 1 1 d R . . N8 N 0.3951(5) 0.2459(6) -0.0508(4) 0.058(2) Uani 1 1 d . A . H8A H 0.3507 0.2862 -0.0525 0.070 Uiso 1 1 d R . . H8B H 0.4140 0.2354 -0.0900 0.070 Uiso 1 1 d R . . C9 C 0.3643(8) 0.1641(9) -0.0230(7) 0.086(4) Uani 1 1 d . . . H9A H 0.3689 0.1179 -0.0548 0.103 Uiso 1 1 d R A . H9B H 0.3021 0.1709 -0.0128 0.103 Uiso 1 1 d R . . C10A C 0.4075(16) 0.1354(16) 0.0331(12) 0.072(6) Uani 0.55 1 d P A 1 H10A H 0.4133 0.0706 0.0316 0.087 Uiso 0.55 1 d PR A 1 H10B H 0.3728 0.1505 0.0697 0.087 Uiso 0.55 1 d PR A 1 C10B C 0.4371(17) 0.1100(18) 0.0038(15) 0.065(6) Uani 0.45 1 d P . 2 H10C H 0.4132 0.0624 0.0298 0.078 Uiso 0.45 1 d PR . 2 H10D H 0.4704 0.0829 -0.0300 0.078 Uiso 0.45 1 d PR . 2 N11 N 0.5000 0.1671(8) 0.0389(6) 0.056(3) Uani 1 2 d S . . H13 H 0.5000 0.2038 0.0703 0.067 Uiso 1 2 d SR A . Cl1 Cl 0.0000 0.4401(3) 0.1833(2) 0.0803(13) Uani 1 2 d SD . . O1L O 0.0000 0.5084(10) 0.1410(7) 0.138(6) Uani 1 2 d SD . . O2L O 0.0650(12) 0.3795(12) 0.1734(8) 0.206(8) Uani 1 1 d D . . O3L O 0.0000 0.4666(17) 0.2435(9) 0.218(11) Uiso 1 2 d SD . . N1L N 0.0000 0.1629(17) 0.1920(10) 0.145(8) Uiso 1 2 d SG . . C1L C 0.020(2) 0.198(2) 0.2566(13) 0.184(18) Uiso 0.50 1 d PG . . H1L1 H -0.0329 0.1989 0.2812 0.277 Uiso 0.50 1 d PR . . H1L2 H 0.0432 0.2583 0.2535 0.277 Uiso 0.50 1 d PR . . H1L3 H 0.0635 0.1605 0.2763 0.277 Uiso 0.50 1 d PR . . O5L O -0.08341(10) 0.164(2) 0.1951(12) 0.327(14) Uiso 1 1 d G . . 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 0.0359(9) 0.0455(11) 0.0375(10) 0.0005(10) 0.000 0.000 O12 0.034(3) 0.039(4) 0.042(4) -0.001(4) 0.000 0.000 Ni2 0.0446(10) 0.0405(11) 0.0450(11) 0.0009(10) 0.000 0.000 O1 0.049(3) 0.060(4) 0.059(4) -0.001(3) 0.010(3) 0.012(3) C2 0.047(4) 0.062(6) 0.047(5) -0.002(4) 0.008(4) 0.002(4) C3 0.044(4) 0.068(6) 0.037(4) 0.005(4) 0.004(3) 0.000(4) N4 0.039(3) 0.050(4) 0.041(4) -0.001(3) -0.001(3) 0.001(3) O5 0.065(4) 0.049(4) 0.050(4) 0.008(3) 0.009(3) 0.005(3) C6 0.096(8) 0.086(8) 0.079(8) 0.007(7) 0.048(7) 0.011(7) C7 0.089(8) 0.080(8) 0.055(6) 0.016(6) 0.032(6) -0.002(7) N8 0.062(5) 0.054(5) 0.059(5) -0.002(4) -0.008(4) -0.010(4) C9 0.068(7) 0.068(7) 0.123(11) 0.028(8) -0.017(7) -0.015(6) C10A 0.069(14) 0.057(13) 0.092(18) -0.002(13) 0.000(12) -0.036(11) C10B 0.065(13) 0.055(14) 0.075(17) 0.022(16) 0.011(15) 0.002(11) N11 0.064(7) 0.046(6) 0.057(7) 0.004(6) 0.000 0.000 Cl1 0.101(3) 0.076(3) 0.064(2) 0.004(2) 0.000 0.000 O1L 0.214(18) 0.099(12) 0.102(12) 0.032(10) 0.000 0.000 O2L 0.227(16) 0.187(15) 0.204(17) 0.014(12) 0.056(13) 0.121(12) _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 N4 2.026(7) 3_565 ? Ni1 N4 2.026(7) . ? Ni1 O12 2.069(5) 9_665 ? Ni1 O12 2.069(5) . ? Ni1 O1 2.123(6) . ? Ni1 O1 2.124(6) 3_565 ? O12 Ni2 2.049(8) . ? O12 Ni1 2.069(5) 9_665 ? Ni2 O5 2.051(7) 11_655 ? Ni2 O5 2.051(7) . ? Ni2 N11 2.080(12) . ? Ni2 N8 2.116(8) . ? Ni2 N8 2.116(8) 11_655 ? O1 C2 1.230(11) . ? C2 C6 1.479(13) . ? C2 C3 1.484(14) . ? C3 N4 1.310(10) . ? C3 C7 1.484(12) . ? N4 O5 1.305(9) . ? N8 C9 1.437(14) . ? C9 C10A 1.44(3) . ? C9 C10B 1.48(3) . ? C10A N11 1.48(2) . ? C10B N11 1.48(3) . ? C10B C10B 1.90(5) 11_655 ? N11 C10A 1.48(2) 11_655 ? N11 C10B 1.48(3) 11_655 ? Cl1 O2L 1.354(12) 11 ? Cl1 O2L 1.354(12) . ? Cl1 O3L 1.355(17) . ? Cl1 O1L 1.366(12) . ? N1L O5L 1.2644 . ? N1L O5L 1.264(3) 11 ? N1L C1L 1.5201 . ? N1L C1L 1.520(13) 11 ? C1L C1L 0.62(7) 11 ? C1L O5L 1.7111(18) 11 ? O5L C1L 1.71(4) 11 ? 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 Ni1 N4 162.0(4) 3_565 . ? N4 Ni1 O12 91.3(3) 3_565 9_665 ? N4 Ni1 O12 102.1(3) . 9_665 ? N4 Ni1 O12 102.1(3) 3_565 . ? N4 Ni1 O12 91.3(3) . . ? O12 Ni1 O12 84.1(3) 9_665 . ? N4 Ni1 O1 91.5(3) 3_565 . ? N4 Ni1 O1 76.8(3) . . ? O12 Ni1 O1 89.6(2) 9_665 . ? O12 Ni1 O1 165.1(3) . . ? N4 Ni1 O1 76.8(3) 3_565 3_565 ? N4 Ni1 O1 91.5(3) . 3_565 ? O12 Ni1 O1 165.1(3) 9_665 3_565 ? O12 Ni1 O1 89.6(2) . 3_565 ? O1 Ni1 O1 99.6(4) . 3_565 ? Ni2 O12 Ni1 111.2(3) . 9_665 ? Ni2 O12 Ni1 111.2(3) . . ? Ni1 O12 Ni1 95.9(3) 9_665 . ? O12 Ni2 O5 93.8(3) . 11_655 ? O12 Ni2 O5 93.8(3) . . ? O5 Ni2 O5 84.3(4) 11_655 . ? O12 Ni2 N11 177.1(4) . . ? O5 Ni2 N11 88.3(3) 11_655 . ? O5 Ni2 N11 88.3(3) . . ? O12 Ni2 N8 95.8(3) . . ? O5 Ni2 N8 168.3(3) 11_655 . ? O5 Ni2 N8 88.4(3) . . ? N11 Ni2 N8 82.3(3) . . ? O12 Ni2 N8 95.8(3) . 11_655 ? O5 Ni2 N8 88.4(3) 11_655 11_655 ? O5 Ni2 N8 168.3(3) . 11_655 ? N11 Ni2 N8 82.3(3) . 11_655 ? N8 Ni2 N8 97.2(5) . 11_655 ? C2 O1 Ni1 113.3(6) . . ? O1 C2 C6 123.0(10) . . ? O1 C2 C3 119.4(8) . . ? C6 C2 C3 117.6(9) . . ? N4 C3 C7 124.1(9) . . ? N4 C3 C2 111.6(8) . . ? C7 C3 C2 124.3(8) . . ? O5 N4 C3 117.8(8) . . ? O5 N4 Ni1 123.9(5) . . ? C3 N4 Ni1 118.2(6) . . ? N4 O5 Ni2 117.5(5) . . ? C9 N8 Ni2 108.6(7) . . ? N8 C9 C10A 117.0(12) . . ? N8 C9 C10B 112.5(13) . . ? C10A C9 C10B 34.2(13) . . ? C9 C10A N11 113.9(17) . . ? C9 C10B N11 111.2(19) . . ? C9 C10B C10B 138.0(11) . 11_655 ? N11 C10B C10B 50.1(12) . 11_655 ? C10A N11 C10A 141(2) . 11_655 ? C10A N11 C10B 33.7(12) . . ? C10A N11 C10B 112(2) 11_655 . ? C10A N11 C10B 112(2) . 11_655 ? C10A N11 C10B 33.7(12) 11_655 11_655 ? C10B N11 C10B 80(2) . 11_655 ? C10A N11 Ni2 105.5(11) . . ? C10A N11 Ni2 105.5(11) 11_655 . ? C10B N11 Ni2 110.5(11) . . ? C10B N11 Ni2 110.5(11) 11_655 . ? O2L Cl1 O2L 93(2) 11 . ? O2L Cl1 O3L 110.2(10) 11 . ? O2L Cl1 O3L 110.2(10) . . ? O2L Cl1 O1L 113.2(8) 11 . ? O2L Cl1 O1L 113.2(8) . . ? O3L Cl1 O1L 114.8(13) . . ? O5L N1L O5L 173.7 . 11 ? O5L N1L C1L 98.6 . . ? O5L N1L C1L 75.2 11 . ? O5L N1L C1L 75(2) . 11 ? O5L N1L C1L 99(2) 11 11 ? C1L N1L C1L 23(2) . 11 ? C1L C1L N1L 78.3 11 . ? C1L C1L O5L 123.93(9) 11 11 ? N1L C1L O5L 45.60(9) . 11 ? N1L O5L C1L 59.2(18) . 11 ? 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 N4 Ni1 O12 Ni2 -154.5(3) 3_565 . . . ? N4 Ni1 O12 Ni2 13.5(3) . . . . ? O12 Ni1 O12 Ni2 115.5(4) 9_665 . . . ? O1 Ni1 O12 Ni2 50.2(11) . . . . ? O1 Ni1 O12 Ni2 -78.0(3) 3_565 . . . ? N4 Ni1 O12 Ni1 90.1(3) 3_565 . . 9_665 ? N4 Ni1 O12 Ni1 -102.0(3) . . . 9_665 ? O12 Ni1 O12 Ni1 -0.003(1) 9_665 . . 9_665 ? O1 Ni1 O12 Ni1 -65.2(11) . . . 9_665 ? O1 Ni1 O12 Ni1 166.5(3) 3_565 . . 9_665 ? Ni1 O12 Ni2 O5 10.5(3) 9_665 . . 11_655 ? Ni1 O12 Ni2 O5 -95.1(3) . . . 11_655 ? Ni1 O12 Ni2 O5 95.1(3) 9_665 . . . ? Ni1 O12 Ni2 O5 -10.5(3) . . . . ? Ni1 O12 Ni2 N11 -127.2(3) 9_665 . . . ? Ni1 O12 Ni2 N11 127.2(3) . . . . ? Ni1 O12 Ni2 N8 -176.1(3) 9_665 . . . ? Ni1 O12 Ni2 N8 78.3(4) . . . . ? Ni1 O12 Ni2 N8 -78.3(4) 9_665 . . 11_655 ? Ni1 O12 Ni2 N8 176.1(3) . . . 11_655 ? N4 Ni1 O1 C2 172.0(7) 3_565 . . . ? N4 Ni1 O1 C2 5.8(6) . . . . ? O12 Ni1 O1 C2 -96.7(7) 9_665 . . . ? O12 Ni1 O1 C2 -32.1(14) . . . . ? O1 Ni1 O1 C2 95.1(7) 3_565 . . . ? Ni1 O1 C2 C6 169.4(9) . . . . ? Ni1 O1 C2 C3 -9.0(11) . . . . ? O1 C2 C3 N4 7.7(12) . . . . ? C6 C2 C3 N4 -170.8(9) . . . . ? O1 C2 C3 C7 -171.7(10) . . . . ? C6 C2 C3 C7 9.8(15) . . . . ? C7 C3 N4 O5 1.3(13) . . . . ? C2 C3 N4 O5 -178.1(7) . . . . ? C7 C3 N4 Ni1 177.2(8) . . . . ? C2 C3 N4 Ni1 -2.2(9) . . . . ? N4 Ni1 N4 O5 123.5(6) 3_565 . . . ? O12 Ni1 N4 O5 -99.2(6) 9_665 . . . ? O12 Ni1 N4 O5 -15.0(6) . . . . ? O1 Ni1 N4 O5 174.1(7) . . . . ? O1 Ni1 N4 O5 74.6(6) 3_565 . . . ? N4 Ni1 N4 C3 -52.2(6) 3_565 . . . ? O12 Ni1 N4 C3 85.1(6) 9_665 . . . ? O12 Ni1 N4 C3 169.4(6) . . . . ? O1 Ni1 N4 C3 -1.5(6) . . . . ? O1 Ni1 N4 C3 -101.0(6) 3_565 . . . ? C3 N4 O5 Ni2 -174.6(6) . . . . ? Ni1 N4 O5 Ni2 9.7(8) . . . . ? O12 Ni2 O5 N4 1.3(6) . . . . ? O5 Ni2 O5 N4 94.8(6) 11_655 . . . ? N11 Ni2 O5 N4 -176.7(6) . . . . ? N8 Ni2 O5 N4 -94.4(6) . . . . ? N8 Ni2 O5 N4 146.6(14) 11_655 . . . ? O12 Ni2 N8 C9 -165.5(8) . . . . ? O5 Ni2 N8 C9 -20(2) 11_655 . . . ? O5 Ni2 N8 C9 -71.9(8) . . . . ? N11 Ni2 N8 C9 16.6(8) . . . . ? N8 Ni2 N8 C9 97.9(8) 11_655 . . . ? Ni2 N8 C9 C10A 0.5(19) . . . . ? Ni2 N8 C9 C10B -37.0(19) . . . . ? N8 C9 C10A N11 -27(3) . . . . ? C10B C9 C10A N11 64(3) . . . . ? N8 C9 C10B N11 44(3) . . . . ? C10A C9 C10B N11 -62(3) . . . . ? N8 C9 C10B C10B -10(3) . . . 11_655 ? C10A C9 C10B C10B -115(3) . . . 11_655 ? C9 C10A N11 C10A -104(3) . . . 11_655 ? C9 C10A N11 C10B -65(3) . . . . ? C9 C10A N11 C10B -82(2) . . . 11_655 ? C9 C10A N11 Ni2 38(2) . . . . ? C9 C10B N11 C10A 60(3) . . . . ? C10B C10B N11 C10A -164(2) 11_655 . . . ? C9 C10B N11 C10A -145(2) . . . 11_655 ? C10B C10B N11 C10A -9.2(13) 11_655 . . 11_655 ? C9 C10B N11 C10B -135.6(14) . . . 11_655 ? C9 C10B N11 Ni2 -27(2) . . . . ? C10B C10B N11 Ni2 108.2(13) 11_655 . . . ? O12 Ni2 N11 C10A -78.3(13) . . . . ? O5 Ni2 N11 C10A 143.8(13) 11_655 . . . ? O5 Ni2 N11 C10A 59.5(13) . . . . ? N8 Ni2 N11 C10A -29.1(13) . . . . ? N8 Ni2 N11 C10A -127.5(13) 11_655 . . . ? O12 Ni2 N11 C10A 78.3(13) . . . 11_655 ? O5 Ni2 N11 C10A -59.5(13) 11_655 . . 11_655 ? O5 Ni2 N11 C10A -143.8(13) . . . 11_655 ? N8 Ni2 N11 C10A 127.5(13) . . . 11_655 ? N8 Ni2 N11 C10A 29.1(13) 11_655 . . 11_655 ? O12 Ni2 N11 C10B -43.2(13) . . . . ? O5 Ni2 N11 C10B 179.0(13) 11_655 . . . ? O5 Ni2 N11 C10B 94.6(13) . . . . ? N8 Ni2 N11 C10B 6.0(13) . . . . ? N8 Ni2 N11 C10B -92.4(14) 11_655 . . . ? O12 Ni2 N11 C10B 43.2(13) . . . 11_655 ? O5 Ni2 N11 C10B -94.6(13) 11_655 . . 11_655 ? O5 Ni2 N11 C10B -179.0(13) . . . 11_655 ? N8 Ni2 N11 C10B 92.4(14) . . . 11_655 ? N8 Ni2 N11 C10B -6.0(13) 11_655 . . 11_655 ? O5L N1L C1L C1L -0.3 . . . 11 ? O5L N1L C1L C1L -179.6 11 . . 11 ? O5L N1L C1L O5L 179.3 . . . 11 ? C1L N1L C1L O5L 179.6 11 . . 11 ? O5L N1L O5L C1L 6.3(3) 11 . . 11 ? C1L N1L O5L C1L 0.1 . . . 11 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 73.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.062 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.137 data_sk31199 _database_code_CSD 155327 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 Cl2 N10 Ni4 O24' _chemical_formula_weight 1286.74 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 10.4880(7) _cell_length_b 16.1935(10) _cell_length_c 16.2944(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.9580(10) _cell_angle_gamma 90.00 _cell_volume 2647.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2745 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 20.7 _exptl_crystal_description quader _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7598 _exptl_absorpt_correction_T_max 0.9319 _exptl_absorpt_process_details 'Corinc (Dr\"ager, 1971)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD Bruker AXS' _diffrn_measurement_device '3-circle diffractometer' _diffrn_measurement_method \q/\f-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24155 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.1606 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6524 _reflns_number_gt 3061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'smart software V5' _computing_cell_refinement 'saint V5' _computing_data_reduction 'saint V5' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0380P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6524 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_obs 0.0537 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_obs 0.0904 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _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 Ni1 Ni 0.91188(6) 0.32277(3) 0.45500(3) 0.03260(16) Uani 1 1 d . . . Ni2 Ni 0.85412(5) 0.52857(3) 0.47137(3) 0.02988(16) Uani 1 1 d . . . O123 O 0.9715(3) 0.44188(15) 0.43874(16) 0.0291(7) Uani 1 1 d . . . H123 H 0.9724 0.4466 0.3781 0.044 Uiso 1 1 d R . . N1A N 0.7503(4) 0.3214(2) 0.3415(2) 0.0467(10) Uani 1 1 d . . . H1A1 H 0.7084 0.3705 0.3334 0.056 Uiso 1 1 calc R . . H1A2 H 0.7790 0.3103 0.2957 0.056 Uiso 1 1 calc R . . C2A C 0.6610(5) 0.2564(3) 0.3537(4) 0.0691(17) Uani 1 1 d . . . H2A1 H 0.6093 0.2774 0.3898 0.083 Uiso 1 1 calc R . . H2A2 H 0.5993 0.2423 0.2985 0.083 Uiso 1 1 calc R . . C3A C 0.7301(5) 0.1820(3) 0.3926(4) 0.0715(17) Uani 1 1 d . . . H3A1 H 0.7541 0.1501 0.3489 0.086 Uiso 1 1 calc R . . H3A2 H 0.6700 0.1487 0.4142 0.086 Uiso 1 1 calc R . . N4A N 0.8501(4) 0.1991(2) 0.4626(2) 0.0408(9) Uani 1 1 d . . . H4A H 0.8329 0.1911 0.5136 0.049 Uiso 1 1 calc R . . C5A C 0.9647(5) 0.1472(3) 0.4593(3) 0.0575(15) Uani 1 1 d . . . H5A1 H 0.9354 0.0905 0.4469 0.069 Uiso 1 1 calc R . . H5A2 H 1.0318 0.1482 0.5147 0.069 Uiso 1 1 calc R . . C6A C 1.0243(5) 0.1777(3) 0.3917(3) 0.0604(15) Uani 1 1 d . . . H6A1 H 1.1074 0.1489 0.3969 0.072 Uiso 1 1 calc R . . H6A2 H 0.9639 0.1660 0.3354 0.072 Uiso 1 1 calc R . . N7A N 1.0494(4) 0.2670(2) 0.4008(2) 0.0419(10) Uani 1 1 d . . . H7A1 H 1.0417 0.2894 0.3490 0.050 Uiso 1 1 calc R . . H7A2 H 1.1329 0.2762 0.4345 0.050 Uiso 1 1 calc R . . O1B O 0.7835(3) 0.36239(17) 0.52392(18) 0.0421(8) Uani 1 1 d . . . N2B N 0.7716(3) 0.4423(2) 0.5318(2) 0.0319(8) Uani 1 1 d . . . C3B C 0.6958(4) 0.4695(3) 0.5769(3) 0.0353(10) Uani 1 1 d . . . C4B C 0.6855(4) 0.5595(3) 0.5757(3) 0.0381(11) Uani 1 1 d . . . O5B O 0.7386(3) 0.60111(18) 0.53060(19) 0.0401(8) Uani 1 1 d . . . C6B C 0.6262(5) 0.4145(3) 0.6229(3) 0.0586(15) Uani 1 1 d . . . H6B1 H 0.6479 0.3580 0.6150 0.088 Uiso 1 1 calc R . . H6B2 H 0.5316 0.4223 0.6004 0.088 Uiso 1 1 calc R . . H6B3 H 0.6540 0.4276 0.6830 0.088 Uiso 1 1 calc R . . C7B C 0.6094(5) 0.6006(3) 0.6282(3) 0.0642(16) Uani 1 1 d . . . H7B1 H 0.6113 0.6593 0.6204 0.096 Uiso 1 1 calc R . . H7B2 H 0.6491 0.5874 0.6876 0.096 Uiso 1 1 calc R . . H7B3 H 0.5188 0.5817 0.6104 0.096 Uiso 1 1 calc R . . O1C O 0.9513(3) 0.68994(18) 0.42543(18) 0.0414(8) Uani 1 1 d . . . N2C N 0.8694(3) 0.6281(2) 0.3982(2) 0.0310(8) Uani 1 1 d . . . C3C C 0.7850(4) 0.6325(3) 0.3219(3) 0.0330(10) Uani 1 1 d . . . C4C C 0.6972(4) 0.5613(3) 0.3019(3) 0.0361(11) Uani 1 1 d . . . O5C O 0.6987(3) 0.50789(18) 0.35700(18) 0.0384(8) Uani 1 1 d . . . C6C C 0.7790(5) 0.7031(3) 0.2630(3) 0.0545(14) Uani 1 1 d . . . H6C1 H 0.8464 0.7427 0.2899 0.082 Uiso 1 1 calc R . . H6C2 H 0.6928 0.7286 0.2501 0.082 Uiso 1 1 calc R . . H6C3 H 0.7940 0.6838 0.2109 0.082 Uiso 1 1 calc R . . C7C C 0.6028(5) 0.5517(3) 0.2143(3) 0.0676(17) Uani 1 1 d . . . H7C1 H 0.5521 0.5019 0.2119 0.101 Uiso 1 1 calc R . . H7C2 H 0.6519 0.5487 0.1731 0.101 Uiso 1 1 calc R . . H7C3 H 0.5435 0.5981 0.2016 0.101 Uiso 1 1 calc R . . Cl1 Cl 1.00057(18) 0.95567(9) 0.29505(10) 0.0712(5) Uani 1 1 d . . . O1I O 0.9537(6) 0.8821(3) 0.2581(4) 0.178(3) Uani 1 1 d . . . O2I O 1.0753(7) 0.9523(4) 0.3762(3) 0.181(3) Uani 1 1 d . . . O3I O 0.8862(6) 1.0023(4) 0.2925(5) 0.201(3) Uani 1 1 d . . . O4I O 1.0665(8) 0.9915(5) 0.2471(4) 0.232(4) Uani 1 1 d . . . O1L O 0.4332(5) 0.3592(3) 0.1608(3) 0.0897(13) Uani 1 1 d . . . C2L C 0.4698(8) 0.2964(5) 0.1139(5) 0.116(3) Uani 1 1 d . . . H2L1 H 0.4000 0.2549 0.0993 0.139 Uiso 1 1 calc R . . H2L2 H 0.5506 0.2702 0.1488 0.139 Uiso 1 1 calc R . . C3L C 0.4918(11) 0.3277(6) 0.0363(6) 0.156(4) Uani 1 1 d . . . H3L1 H 0.5657 0.3662 0.0513 0.188 Uiso 1 1 calc R . . H3L2 H 0.5162 0.2822 0.0052 0.188 Uiso 1 1 calc R . . O4L O 0.3809(8) 0.3670(5) -0.0164(3) 0.155(3) Uani 1 1 d . . . C5L C 0.3427(9) 0.4313(5) 0.0317(6) 0.132(3) Uani 1 1 d . . . H5L1 H 0.2620 0.4577 -0.0033 0.159 Uiso 1 1 calc R . . H5L2 H 0.4125 0.4727 0.0471 0.159 Uiso 1 1 calc R . . C6L C 0.3196(8) 0.3980(5) 0.1093(6) 0.113(3) Uani 1 1 d . . . H6L1 H 0.2942 0.4424 0.1413 0.136 Uiso 1 1 calc R . . H6L2 H 0.2468 0.3587 0.0937 0.136 Uiso 1 1 calc R . . O5I O 0.8359(5) 0.2550(3) 0.1714(3) 0.1141(17) Uani 1 1 d . . . H5I H 0.8568 0.2174 0.1286 0.171 Uiso 1 1 d R . . H6I H 0.9014 0.3255 0.1875 0.171 Uiso 0.50 1 d PR . . H7I H 0.8225 0.2177 0.2377 0.171 Uiso 0.50 1 d PR . . 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 0.0374(3) 0.0283(3) 0.0346(3) -0.0033(3) 0.0143(3) -0.0024(3) Ni2 0.0310(3) 0.0290(3) 0.0312(3) 0.0009(3) 0.0116(2) -0.0001(3) O123 0.0346(17) 0.0289(16) 0.0258(15) -0.0018(12) 0.0116(13) -0.0009(13) N1A 0.048(3) 0.048(2) 0.045(2) 0.000(2) 0.013(2) 0.001(2) C2A 0.045(3) 0.053(4) 0.096(5) -0.007(3) 0.001(3) -0.015(3) C3A 0.064(4) 0.053(4) 0.086(4) 0.000(3) 0.004(3) -0.021(3) N4A 0.046(2) 0.037(2) 0.041(2) -0.0047(18) 0.015(2) -0.007(2) C5A 0.070(4) 0.034(3) 0.073(4) 0.005(3) 0.029(3) 0.004(3) C6A 0.068(4) 0.038(3) 0.087(4) -0.009(3) 0.042(3) 0.009(3) N7A 0.045(2) 0.038(2) 0.046(2) -0.0046(19) 0.018(2) -0.0007(19) O1B 0.053(2) 0.0275(17) 0.054(2) -0.0004(15) 0.0285(17) -0.0020(15) N2B 0.033(2) 0.032(2) 0.032(2) 0.0011(17) 0.0111(17) 0.0024(17) C3B 0.036(3) 0.037(3) 0.037(3) 0.000(2) 0.018(2) 0.001(2) C4B 0.032(3) 0.042(3) 0.040(3) -0.006(2) 0.011(2) 0.001(2) O5B 0.0383(19) 0.0352(18) 0.052(2) -0.0005(16) 0.0207(17) 0.0009(15) C6B 0.068(4) 0.050(3) 0.078(4) 0.005(3) 0.052(3) 0.002(3) C7B 0.072(4) 0.058(4) 0.080(4) -0.016(3) 0.048(3) 0.007(3) O1C 0.053(2) 0.0335(18) 0.0374(18) 0.0019(15) 0.0131(16) -0.0110(16) N2C 0.032(2) 0.032(2) 0.031(2) -0.0022(17) 0.0122(18) 0.0002(17) C3C 0.037(3) 0.039(3) 0.027(2) 0.001(2) 0.014(2) 0.003(2) C4C 0.032(3) 0.040(3) 0.035(3) 0.001(2) 0.008(2) 0.005(2) O5C 0.0335(18) 0.0414(19) 0.0373(18) 0.0028(15) 0.0059(15) -0.0026(14) C6C 0.069(4) 0.050(3) 0.040(3) 0.011(2) 0.009(3) -0.002(3) C7C 0.066(4) 0.071(4) 0.048(3) 0.008(3) -0.011(3) -0.014(3) Cl1 0.1043(13) 0.0607(10) 0.0589(10) -0.0153(8) 0.0399(9) -0.0271(9) O1I 0.171(6) 0.093(4) 0.251(7) -0.089(5) 0.031(5) -0.009(4) O2I 0.256(8) 0.196(7) 0.062(4) 0.002(4) 0.001(4) 0.008(6) O3I 0.144(6) 0.162(6) 0.296(9) -0.096(6) 0.060(6) 0.021(5) O4I 0.294(9) 0.299(9) 0.154(6) 0.002(6) 0.145(6) -0.161(8) O1L 0.098(4) 0.102(4) 0.069(3) -0.011(3) 0.023(3) 0.004(3) C2L 0.156(8) 0.107(6) 0.092(6) 0.004(5) 0.046(6) 0.035(5) C3L 0.218(12) 0.169(10) 0.114(8) 0.004(7) 0.099(8) 0.058(9) O4L 0.240(8) 0.153(6) 0.065(4) 0.005(4) 0.032(4) 0.004(6) C5L 0.162(9) 0.105(7) 0.099(7) 0.007(6) -0.010(6) -0.003(6) C6L 0.081(6) 0.141(8) 0.112(7) -0.005(6) 0.020(5) 0.014(5) O5I 0.128(4) 0.113(4) 0.123(4) -0.054(3) 0.072(3) -0.021(3) _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 O1C 2.066(3) 3_766 ? Ni1 O123 2.068(3) . ? Ni1 O1B 2.089(3) . ? Ni1 N7A 2.102(3) . ? Ni1 N1A 2.113(3) . ? Ni1 N4A 2.120(3) . ? Ni2 O123 2.038(3) . ? Ni2 O123 2.038(3) 3_766 ? Ni2 N2C 2.039(3) . ? Ni2 N2B 2.041(3) . ? Ni2 O5B 2.112(3) . ? Ni2 O5C 2.114(3) . ? O123 Ni2 2.038(3) 3_766 ? N1A C2A 1.461(6) . ? C2A C3A 1.451(7) . ? C3A N4A 1.457(6) . ? N4A C5A 1.481(6) . ? C5A C6A 1.499(6) . ? C6A N7A 1.471(5) . ? O1B N2B 1.310(4) . ? N2B C3B 1.308(5) . ? C3B C4B 1.460(6) . ? C3B C6B 1.486(6) . ? C4B O5B 1.243(5) . ? C4B C7B 1.486(6) . ? O1C N2C 1.309(4) . ? O1C Ni1 2.066(3) 3_766 ? N2C C3C 1.301(5) . ? C3C C4C 1.452(6) . ? C3C C6C 1.482(6) . ? C4C O5C 1.244(5) . ? C4C C7C 1.489(6) . ? Cl1 O4I 1.319(5) . ? Cl1 O2I 1.327(5) . ? Cl1 O1I 1.360(5) . ? Cl1 O3I 1.408(6) . ? O1L C6L 1.391(8) . ? O1L C2L 1.392(7) . ? C2L C3L 1.441(10) . ? C3L O4L 1.383(10) . ? O4L C5L 1.430(9) . ? C5L C6L 1.459(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 O1C Ni1 O123 93.48(11) 3_766 . ? O1C Ni1 O1B 84.43(12) 3_766 . ? O123 Ni1 O1B 92.80(11) . . ? O1C Ni1 N7A 88.88(13) 3_766 . ? O123 Ni1 N7A 94.38(12) . . ? O1B Ni1 N7A 170.47(13) . . ? O1C Ni1 N1A 169.66(13) 3_766 . ? O123 Ni1 N1A 95.35(13) . . ? O1B Ni1 N1A 89.76(13) . . ? N7A Ni1 N1A 95.79(14) . . ? O1C Ni1 N4A 89.50(13) 3_766 . ? O123 Ni1 N4A 175.98(12) . . ? O1B Ni1 N4A 90.17(13) . . ? N7A Ni1 N4A 82.98(14) . . ? N1A Ni1 N4A 81.95(14) . . ? O123 Ni2 O123 82.27(11) . 3_766 ? O123 Ni2 N2C 103.65(12) . . ? O123 Ni2 N2C 91.57(12) 3_766 . ? O123 Ni2 N2B 91.59(12) . . ? O123 Ni2 N2B 103.41(12) 3_766 . ? N2C Ni2 N2B 160.00(14) . . ? O123 Ni2 O5B 166.72(11) . . ? O123 Ni2 O5B 93.16(10) 3_766 . ? N2C Ni2 O5B 88.88(12) . . ? N2B Ni2 O5B 77.29(13) . . ? O123 Ni2 O5C 91.73(11) . . ? O123 Ni2 O5C 165.90(11) 3_766 . ? N2C Ni2 O5C 77.39(13) . . ? N2B Ni2 O5C 89.44(12) . . ? O5B Ni2 O5C 95.35(11) . . ? Ni2 O123 Ni2 97.73(11) . 3_766 ? Ni2 O123 Ni1 112.37(12) . . ? Ni2 O123 Ni1 111.61(12) 3_766 . ? C2A N1A Ni1 105.7(3) . . ? C3A C2A N1A 113.5(4) . . ? C2A C3A N4A 113.0(4) . . ? C3A N4A C5A 112.9(4) . . ? C3A N4A Ni1 110.0(3) . . ? C5A N4A Ni1 105.6(3) . . ? N4A C5A C6A 110.9(4) . . ? N7A C6A C5A 110.6(4) . . ? C6A N7A Ni1 109.9(3) . . ? N2B O1B Ni1 116.8(2) . . ? C3B N2B O1B 118.6(4) . . ? C3B N2B Ni2 117.0(3) . . ? O1B N2B Ni2 124.3(3) . . ? N2B C3B C4B 112.6(4) . . ? N2B C3B C6B 123.4(4) . . ? C4B C3B C6B 124.0(4) . . ? O5B C4B C3B 120.3(4) . . ? O5B C4B C7B 120.3(4) . . ? C3B C4B C7B 119.3(4) . . ? C4B O5B Ni2 112.6(3) . . ? N2C O1C Ni1 116.7(2) . 3_766 ? C3C N2C O1C 118.6(3) . . ? C3C N2C Ni2 117.0(3) . . ? O1C N2C Ni2 124.2(2) . . ? N2C C3C C4C 112.4(4) . . ? N2C C3C C6C 123.3(4) . . ? C4C C3C C6C 124.3(4) . . ? O5C C4C C3C 121.1(4) . . ? O5C C4C C7C 118.9(4) . . ? C3C C4C C7C 120.0(4) . . ? C4C O5C Ni2 111.7(3) . . ? O4I Cl1 O2I 110.4(5) . . ? O4I Cl1 O1I 107.9(4) . . ? O2I Cl1 O1I 115.9(4) . . ? O4I Cl1 O3I 109.6(5) . . ? O2I Cl1 O3I 107.6(4) . . ? O1I Cl1 O3I 105.2(4) . . ? C6L O1L C2L 108.9(5) . . ? O1L C2L C3L 111.4(7) . . ? O4L C3L C2L 112.7(8) . . ? C3L O4L C5L 108.3(6) . . ? O4L C5L C6L 110.5(7) . . ? O1L C6L C5L 111.1(7) . . ? 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 O123 Ni2 O123 Ni2 0.0 3_766 . . 3_766 ? N2C Ni2 O123 Ni2 89.74(13) . . . 3_766 ? N2B Ni2 O123 Ni2 -103.32(12) . . . 3_766 ? O5B Ni2 O123 Ni2 -70.5(5) . . . 3_766 ? O5C Ni2 O123 Ni2 167.19(12) . . . 3_766 ? O123 Ni2 O123 Ni1 117.25(16) 3_766 . . . ? N2C Ni2 O123 Ni1 -153.01(14) . . . . ? N2B Ni2 O123 Ni1 13.93(14) . . . . ? O5B Ni2 O123 Ni1 46.7(5) . . . . ? O5C Ni2 O123 Ni1 -75.56(13) . . . . ? O1C Ni1 O123 Ni2 -96.59(14) 3_766 . . . ? O1B Ni1 O123 Ni2 -12.00(14) . . . . ? N7A Ni1 O123 Ni2 174.27(14) . . . . ? N1A Ni1 O123 Ni2 78.02(15) . . . . ? N4A Ni1 O123 Ni2 125.6(18) . . . . ? O1C Ni1 O123 Ni2 12.04(14) 3_766 . . 3_766 ? O1B Ni1 O123 Ni2 96.63(13) . . . 3_766 ? N7A Ni1 O123 Ni2 -77.10(15) . . . 3_766 ? N1A Ni1 O123 Ni2 -173.34(14) . . . 3_766 ? N4A Ni1 O123 Ni2 -125.8(18) . . . 3_766 ? O1C Ni1 N1A C2A -10.3(9) 3_766 . . . ? O123 Ni1 N1A C2A -158.9(3) . . . . ? O1B Ni1 N1A C2A -66.1(3) . . . . ? N7A Ni1 N1A C2A 106.2(3) . . . . ? N4A Ni1 N1A C2A 24.1(3) . . . . ? Ni1 N1A C2A C3A -42.4(6) . . . . ? N1A C2A C3A N4A 42.0(7) . . . . ? C2A C3A N4A C5A -136.0(5) . . . . ? C2A C3A N4A Ni1 -18.3(6) . . . . ? O1C Ni1 N4A C3A 170.4(3) 3_766 . . . ? O123 Ni1 N4A C3A -51.7(19) . . . . ? O1B Ni1 N4A C3A 85.9(3) . . . . ? N7A Ni1 N4A C3A -100.7(3) . . . . ? N1A Ni1 N4A C3A -3.8(3) . . . . ? O1C Ni1 N4A C5A -67.5(3) 3_766 . . . ? O123 Ni1 N4A C5A 70.4(19) . . . . ? O1B Ni1 N4A C5A -152.0(3) . . . . ? N7A Ni1 N4A C5A 21.4(3) . . . . ? N1A Ni1 N4A C5A 118.3(3) . . . . ? C3A N4A C5A C6A 76.5(5) . . . . ? Ni1 N4A C5A C6A -43.8(5) . . . . ? N4A C5A C6A N7A 49.9(6) . . . . ? C5A C6A N7A Ni1 -28.9(5) . . . . ? O1C Ni1 N7A C6A 93.5(3) 3_766 . . . ? O123 Ni1 N7A C6A -173.1(3) . . . . ? O1B Ni1 N7A C6A 48.2(9) . . . . ? N1A Ni1 N7A C6A -77.2(3) . . . . ? N4A Ni1 N7A C6A 3.9(3) . . . . ? O1C Ni1 O1B N2B 97.1(3) 3_766 . . . ? O123 Ni1 O1B N2B 3.9(3) . . . . ? N7A Ni1 O1B N2B 142.7(7) . . . . ? N1A Ni1 O1B N2B -91.5(3) . . . . ? N4A Ni1 O1B N2B -173.4(3) . . . . ? Ni1 O1B N2B C3B -177.7(3) . . . . ? Ni1 O1B N2B Ni2 6.6(4) . . . . ? O123 Ni2 N2B C3B 170.9(3) . . . . ? O123 Ni2 N2B C3B 88.5(3) 3_766 . . . ? N2C Ni2 N2B C3B -49.1(5) . . . . ? O5B Ni2 N2B C3B -1.8(3) . . . . ? O5C Ni2 N2B C3B -97.4(3) . . . . ? O123 Ni2 N2B O1B -13.3(3) . . . . ? O123 Ni2 N2B O1B -95.7(3) 3_766 . . . ? N2C Ni2 N2B O1B 126.7(4) . . . . ? O5B Ni2 N2B O1B 174.0(3) . . . . ? O5C Ni2 N2B O1B 78.4(3) . . . . ? O1B N2B C3B C4B -176.5(3) . . . . ? Ni2 N2B C3B C4B -0.5(5) . . . . ? O1B N2B C3B C6B 2.5(6) . . . . ? Ni2 N2B C3B C6B 178.5(3) . . . . ? N2B C3B C4B O5B 4.4(6) . . . . ? C6B C3B C4B O5B -174.6(4) . . . . ? N2B C3B C4B C7B -176.4(4) . . . . ? C6B C3B C4B C7B 4.6(7) . . . . ? C3B C4B O5B Ni2 -5.8(5) . . . . ? C7B C4B O5B Ni2 175.0(3) . . . . ? O123 Ni2 O5B C4B -29.6(6) . . . . ? O123 Ni2 O5B C4B -99.0(3) 3_766 . . . ? N2C Ni2 O5B C4B 169.5(3) . . . . ? N2B Ni2 O5B C4B 4.1(3) . . . . ? O5C Ni2 O5B C4B 92.3(3) . . . . ? Ni1 O1C N2C C3C -177.4(3) 3_766 . . . ? Ni1 O1C N2C Ni2 7.8(4) 3_766 . . . ? O123 Ni2 N2C C3C 88.3(3) . . . . ? O123 Ni2 N2C C3C 170.7(3) 3_766 . . . ? N2B Ni2 N2C C3C -50.3(5) . . . . ? O5B Ni2 N2C C3C -96.1(3) . . . . ? O5C Ni2 N2C C3C -0.4(3) . . . . ? O123 Ni2 N2C O1C -96.8(3) . . . . ? O123 Ni2 N2C O1C -14.4(3) 3_766 . . . ? N2B Ni2 N2C O1C 124.5(4) . . . . ? O5B Ni2 N2C O1C 78.7(3) . . . . ? O5C Ni2 N2C O1C 174.5(3) . . . . ? O1C N2C C3C C4C -177.6(3) . . . . ? Ni2 N2C C3C C4C -2.5(5) . . . . ? O1C N2C C3C C6C 1.5(6) . . . . ? Ni2 N2C C3C C6C 176.7(3) . . . . ? N2C C3C C4C O5C 6.2(6) . . . . ? C6C C3C C4C O5C -173.0(4) . . . . ? N2C C3C C4C C7C -174.2(4) . . . . ? C6C C3C C4C C7C 6.6(7) . . . . ? C3C C4C O5C Ni2 -6.4(5) . . . . ? C7C C4C O5C Ni2 174.0(3) . . . . ? O123 Ni2 O5C C4C -100.0(3) . . . . ? O123 Ni2 O5C C4C -35.6(6) 3_766 . . . ? N2C Ni2 O5C C4C 3.6(3) . . . . ? N2B Ni2 O5C C4C 168.4(3) . . . . ? O5B Ni2 O5C C4C 91.3(3) . . . . ? C6L O1L C2L C3L 57.1(9) . . . . ? O1L C2L C3L O4L -58.2(11) . . . . ? C2L C3L O4L C5L 56.2(11) . . . . ? C3L O4L C5L C6L -56.0(10) . . . . ? C2L O1L C6L C5L -58.2(8) . . . . ? O4L C5L C6L O1L 58.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.550 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.092