#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Kaden, Thomas A.' 'Kircher, Peter' 'Meyer, Franc' 'Pritzkow, Hans' 'Siegfried, Liselotte' _publ_contact_author 'Dr Franc Meyer' _publ_contact_author_address ; Dr Franc Meyer Anorganisch-Chemisches Institut der Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg GERMANY ; _publ_contact_author_email d61@ix.urz.uni-heidelberg.de _publ_requested_journal 'JCS Dalton' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Complexes of a bis(tetradentate)compartmental pyrazolate ligand: solution studies and solid state structures ; loop_ _publ_author_name _publ_author_address 'Siegfried, Liselotte' ; Institut fuer Anorg.Chemie Universitaet Basel Spitalstr.51 CH-4056 Basel ; 'Kaden, Thomas A.' ; Institut fuer Anorg.Chemie Universitaet Basel Spitalstr.51 CH-4056 Basel ; 'Meyer, Franc' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Kircher, Peter' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Pritzkow, Hans' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; #============================================================================== data_fmpe _database_code_CSD 160993 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C16H33N5Ni 2C3H5N)2 (C16H33N5Ni=B7C3H5N=B7CH3OH)2 CH3OH' _chemical_formula_sum 'C86 H178 Cl8 N26 Ni4 O36' _chemical_formula_weight 2670.98 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.017(3) _cell_length_b 13.449(3) _cell_length_c 18.704(4) _cell_angle_alpha 97.65(3) _cell_angle_beta 106.04(3) _cell_angle_gamma 100.10(3) _cell_volume 3040.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.871 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23834 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11939 _reflns_number_gt 8935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski and Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; One of the not-coordinating diethylaminogroups is heavily disordered. The structure contains disordered methanol. 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^)+(0.1024P)^2^+3.9762P] 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 11939 _refine_ls_number_parameters 852 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.002 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 0.61629(3) 0.92464(3) 0.48578(2) 0.02032(13) Uani 1 1 d . . . Ni2 Ni 0.46813(4) 1.12710(3) 0.05359(2) 0.02377(14) Uani 1 1 d . . . Cl10 Cl 0.43476(9) 1.44888(8) 0.29911(6) 0.0398(3) Uani 1 1 d . . . O10 O 0.3516(4) 1.3898(4) 0.3227(3) 0.0896(15) Uani 1 1 d . . . O11 O 0.4789(4) 1.5469(3) 0.3450(2) 0.0800(14) Uani 1 1 d . . . O12 O 0.5172(3) 1.3913(3) 0.3036(3) 0.0849(15) Uani 1 1 d . . . O13 O 0.3861(4) 1.4559(3) 0.2227(2) 0.0773(13) Uani 1 1 d . . . Cl20 Cl 0.03103(8) 0.76744(8) -0.43296(6) 0.0368(2) Uani 1 1 d . . . O20 O 0.1374(4) 0.7799(6) -0.3835(4) 0.0713(19) Uani 0.80 1 d P A 1 O21 O 0.0133(6) 0.8575(4) -0.4631(4) 0.0658(17) Uani 0.80 1 d P A 1 O22 O 0.0087(5) 0.6805(4) -0.4936(3) 0.0765(16) Uani 0.80 1 d P A 1 O23 O -0.0473(7) 0.7425(6) -0.3929(5) 0.059(2) Uani 0.80 1 d P A 1 O120 O 0.111(2) 0.839(2) -0.3709(15) 0.087(9) Uani 0.20 1 d P A 2 O121 O -0.022(2) 0.8245(19) -0.4792(15) 0.052(7) Uiso 0.20 1 d P A 2 O122 O 0.088(2) 0.7117(17) -0.4734(13) 0.069(6) Uiso 0.20 1 d P A 2 O123 O -0.044(2) 0.7009(19) -0.4124(18) 0.046(7) Uani 0.20 1 d P A 2 Cl30 Cl 0.2579(14) 1.5196(10) 0.0342(9) 0.070(4) Uani 0.45 1 d P B 1 O30 O 0.3742(10) 1.5844(9) 0.0643(8) 0.056(3) Uiso 0.45 1 d P B 1 O31 O 0.2819(10) 1.4184(8) 0.0290(7) 0.067(3) Uiso 0.45 1 d P B 1 O32 O 0.2084(16) 1.5291(13) -0.0429(11) 0.084 Uiso 0.45 1 d P B 1 O33 O 0.1827(10) 1.5069(10) 0.0661(7) 0.088 Uiso 0.45 1 d P B 1 Cl40 Cl 0.2585(10) 1.5164(10) 0.0240(12) 0.074(6) Uani 0.30 1 d P C 2 O430 O 0.3672(12) 1.5592(11) 0.0268(9) 0.063(4) Uiso 0.30 1 d P C 2 O431 O 0.2518(15) 1.4099(12) -0.0055(10) 0.070(4) Uiso 0.30 1 d P C 2 O432 O 0.2250(14) 1.5516(12) -0.0471(10) 0.051(4) Uiso 0.30 1 d P C 2 O433 O 0.2255(16) 1.5720(15) 0.0844(12) 0.074(5) Uiso 0.30 1 d P C 2 Cl50 Cl 0.272(2) 1.5275(19) 0.0302(15) 0.049(4) Uiso 0.25 1 d P D 3 O530 O 0.3531(15) 1.5940(13) 0.0763(9) 0.040(5) Uiso 0.25 1 d P D 3 O531 O 0.2382(16) 1.4181(13) 0.0362(10) 0.058(4) Uiso 0.25 1 d P D 3 O532 O 0.1848(16) 1.5564(16) -0.0220(11) 0.070(5) Uiso 0.25 1 d P D 3 O533 O 0.2226(19) 1.551(2) 0.1047(13) 0.076(7) Uiso 0.25 1 d P D 3 Cl40 Cl 0.05308(9) 1.03784(9) -0.14952(6) 0.0421(3) Uani 1 1 d . E 3 O40 O 0.1486(3) 1.0040(3) -0.1152(2) 0.0693(11) Uani 1 1 d . E 3 O41 O -0.0393(6) 0.9479(6) -0.1816(5) 0.0609(18) Uiso 0.55 1 d P F 1 O42 O 0.0658(7) 1.0989(6) -0.2037(5) 0.056(2) Uiso 0.55 1 d P G 1 O43 O 0.0148(8) 1.0986(7) -0.0951(5) 0.078(2) Uiso 0.55 1 d P H 1 O141 O -0.016(2) 0.998(2) -0.1130(15) 0.037(6) Uiso 0.15 1 d P I 2 O142 O 0.0272(14) 1.016(2) -0.2299(9) 0.021(4) Uiso 0.15 1 d P J 2 O143 O 0.146(2) 1.1224(19) -0.1062(14) 0.056(6) Uiso 0.15 1 d P K 2 O241 O -0.0314(17) 1.0335(19) -0.1243(12) 0.017(4) Uiso 0.12 1 d P E 3 O242 O 0.026(3) 0.953(4) -0.225(2) 0.088 Uiso 0.12 1 d P E 3 O243 O 0.097(3) 1.154(2) -0.1377(18) 0.052(7) Uiso 0.12 1 d P E 3 O341 O -0.0435(13) 0.9784(15) -0.1460(12) 0.027(4) Uiso 0.18 1 d P L 4 O342 O 0.0409(13) 1.0636(18) -0.2222(9) 0.013(3) Uiso 0.18 1 d P M 4 O343 O 0.083(2) 1.1398(17) -0.0940(13) 0.059(5) Uiso 0.18 1 d P N 4 O170 O 0.3500(3) 1.1551(2) -0.04453(17) 0.0370(7) Uani 1 1 d . . . N1 N 0.4843(2) 0.8898(2) 0.52325(16) 0.0215(6) Uani 1 1 d . . . N2 N 0.4171(2) 0.9444(2) 0.54819(15) 0.0193(6) Uani 1 1 d . . . N3 N 0.6461(2) 0.7802(2) 0.52769(17) 0.0242(6) Uani 1 1 d . . . N4 N 0.7358(2) 1.0005(2) 0.59774(16) 0.0217(6) Uani 1 1 d . . . N5 N 0.7812(3) 0.5580(3) 0.4862(2) 0.0306(7) Uani 1 1 d . . . N60 N 0.7474(2) 0.9298(2) 0.44025(17) 0.0253(7) Uani 1 1 d . . . N70 N 0.5242(3) 0.8281(2) 0.37486(18) 0.0280(7) Uani 1 1 d . . . N101 N 0.3905(2) 0.9762(2) 0.02516(16) 0.0233(6) Uani 1 1 d . . . N102 N 0.4193(3) 0.8869(2) 0.00244(17) 0.0264(7) Uani 1 1 d . . . N103 N 0.3390(3) 1.1357(2) 0.11035(18) 0.0282(7) Uani 1 1 d . . . N104 N 0.5674(3) 1.1114(2) 0.16727(17) 0.0269(7) Uani 1 1 d . . . N105 N 0.1423(5) 1.3097(5) 0.1294(4) 0.0440(15) Uani 0.75 1 d P O 1 C111 C 0.0522(9) 1.2653(8) 0.0404(6) 0.075(3) Uiso 0.75 1 d P O 1 H11A H 0.0929 1.2402 0.0082 0.19(5) Uiso 0.75 1 calc PR O 1 H11B H -0.0006 1.2062 0.0429 0.19(5) Uiso 0.75 1 calc PR O 1 C112 C 0.1164(17) 1.3770(17) 0.1895(13) 0.056(5) Uiso 0.33 1 d P O 1 H11F H 0.0821 1.4302 0.1695 0.19(5) Uiso 0.33 1 calc PR O 1 H11G H 0.1817 1.4089 0.2318 0.19(5) Uiso 0.33 1 calc PR O 1 C115 C -0.0126(17) 1.3374(16) -0.0001(12) 0.080 Uiso 0.35 1 d P O 1 H11C H -0.0750 1.3405 0.0174 0.052(9) Uiso 0.35 1 calc PR O 1 H11D H -0.0370 1.3118 -0.0538 0.052(9) Uiso 0.35 1 calc PR O 1 H11E H 0.0335 1.4051 0.0109 0.052(9) Uiso 0.35 1 calc PR O 1 C116 C 0.038(2) 1.301(2) 0.2121(16) 0.064(6) Uiso 0.33 1 d P O 1 H11H H -0.0166 1.2598 0.1674 0.052(9) Uiso 0.33 1 calc PR O 1 H11I H 0.0037 1.3370 0.2431 0.052(9) Uiso 0.33 1 calc PR O 1 H11J H 0.0776 1.2572 0.2401 0.052(9) Uiso 0.33 1 calc PR O 1 N140 N 0.1303(18) 1.3115(17) 0.0912(10) 0.038(5) Uani 0.25 1 d P O 2 C141 C 0.0500(14) 1.2764(12) 0.0669(10) 0.017(3) Uiso 0.25 1 d P O 2 C142 C -0.0196(16) 1.3538(15) 0.0487(11) 0.045(4) Uiso 0.25 1 d P O 2 C143 C 0.0907(19) 1.3716(17) 0.1512(14) 0.051(5) Uiso 0.25 1 d P O 2 C144 C 0.017(3) 1.304(2) 0.1806(18) 0.068(8) Uiso 0.25 1 d P O 2 C125 C -0.0230(15) 1.1757(14) 0.0450(9) 0.076 Uiso 0.40 1 d P P 3 C122 C 0.1010(13) 1.3370(13) 0.1996(8) 0.052(3) Uiso 0.43 1 d P Q 4 C126 C 0.040(2) 1.266(2) 0.2251(16) 0.068(7) Uiso 0.27 1 d P Q 4 H12D H 0.0774 1.2116 0.2355 0.052(9) Uiso 0.27 1 calc PR Q 4 H12E H -0.0298 1.2383 0.1872 0.052(9) Uiso 0.27 1 calc PR Q 4 H12F H 0.0290 1.2979 0.2707 0.052(9) Uiso 0.27 1 calc PR Q 4 C127 C 0.029(2) 1.4066(19) 0.1842(14) 0.028(5) Uiso 0.15 1 d P Q 3 H12G H -0.0018 1.4173 0.2248 0.052(9) Uiso 0.15 1 calc PR Q 3 H12H H -0.0285 1.3778 0.1376 0.052(9) Uiso 0.15 1 calc PR Q 3 H12I H 0.0700 1.4711 0.1800 0.052(9) Uiso 0.15 1 calc PR Q 3 N160 N 0.5192(3) 1.2871(3) 0.08098(18) 0.0315(7) Uani 1 1 d . . . C1 C 0.3658(3) 0.8856(3) 0.58652(19) 0.0229(7) Uani 1 1 d . . . H1 H 0.3152 0.9046 0.6093 0.029(5) Uiso 1 1 calc R . . C2 C 0.3984(3) 0.7933(3) 0.5874(2) 0.0251(8) Uani 1 1 d . . . H2 H 0.3759 0.7398 0.6103 0.029(5) Uiso 1 1 calc R . . C3 C 0.4725(3) 0.7991(3) 0.54629(19) 0.0224(7) Uani 1 1 d . . . C4 C 0.5345(3) 0.7233(3) 0.5233(2) 0.0268(8) Uani 1 1 d . . . H4A H 0.5405 0.6740 0.5568 0.0290(19) Uiso 1 1 calc R . . H4B H 0.4961 0.6862 0.4720 0.0290(19) Uiso 1 1 calc R . . C5 C 0.7162(3) 0.8161(3) 0.6082(2) 0.0257(8) Uani 1 1 d . . . H5A H 0.7573 0.7650 0.6239 0.0290(19) Uiso 1 1 calc R . . H5B H 0.6702 0.8244 0.6405 0.0290(19) Uiso 1 1 calc R . . C6 C 0.7946(3) 0.9173(3) 0.6172(2) 0.0269(8) Uani 1 1 d . . . H6A H 0.8423 0.9374 0.6692 0.0290(19) Uiso 1 1 calc R . . H6B H 0.8402 0.9088 0.5847 0.0290(19) Uiso 1 1 calc R . . C7 C 0.6977(3) 0.7149(3) 0.4838(2) 0.0278(8) Uani 1 1 d . . . H7A H 0.7732 0.7498 0.4926 0.0290(19) Uiso 1 1 calc R . . H7B H 0.6594 0.7062 0.4302 0.0290(19) Uiso 1 1 calc R . . C8 C 0.6956(3) 0.6084(3) 0.5054(2) 0.0319(9) Uani 1 1 d . . . H8A H 0.7065 0.6155 0.5594 0.0290(19) Uiso 1 1 calc R . . H8B H 0.6239 0.5642 0.4792 0.0290(19) Uiso 1 1 calc R . . C9 C 0.6788(3) 1.0291(3) 0.65401(19) 0.0238(8) Uani 1 1 d . . . H9A H 0.6245 0.9691 0.6530 0.0290(19) Uiso 1 1 calc R . . H9B H 0.6399 1.0814 0.6377 0.0290(19) Uiso 1 1 calc R . . C10 C 0.8215(3) 1.0912(3) 0.5975(2) 0.0273(8) Uani 1 1 d . . . H10A H 0.8452 1.0754 0.5533 0.0290(19) Uiso 1 1 calc R . . H10B H 0.8844 1.0990 0.6418 0.0290(19) Uiso 1 1 calc R . . C11 C 0.7877(4) 0.4622(3) 0.5198(3) 0.0467(12) Uani 1 1 d . . . H11A H 0.7153 0.4171 0.5036 0.0290(19) Uiso 1 1 calc R . . H11B H 0.8355 0.4260 0.5003 0.0290(19) Uiso 1 1 calc R . . C12 C 0.7622(4) 0.5364(4) 0.4016(3) 0.0502(12) Uani 1 1 d . . . H12A H 0.6922 0.4883 0.3774 0.0290(19) Uiso 1 1 calc R . . H12B H 0.7575 0.5999 0.3829 0.0290(19) Uiso 1 1 calc R . . C13 C 0.7518(3) 1.0692(3) 0.7359(2) 0.0324(9) Uani 1 1 d . . . H13A H 0.7857 1.0159 0.7546 0.053(3) Uiso 1 1 calc R . . H13B H 0.7080 1.0891 0.7667 0.053(3) Uiso 1 1 calc R . . H13C H 0.8074 1.1276 0.7378 0.053(3) Uiso 1 1 calc R . . C14 C 0.7885(3) 1.1937(3) 0.5971(2) 0.0306(9) Uani 1 1 d . . . H14A H 0.7205 1.1854 0.5577 0.053(3) Uiso 1 1 calc R . . H14B H 0.8444 1.2427 0.5881 0.053(3) Uiso 1 1 calc R . . H14C H 0.7796 1.2178 0.6452 0.053(3) Uiso 1 1 calc R . . C15 C 0.8290(6) 0.4847(4) 0.6033(3) 0.0662(16) Uani 1 1 d . . . H15A H 0.8933 0.5397 0.6200 0.053(3) Uiso 1 1 calc R . . H15B H 0.8472 0.4244 0.6212 0.053(3) Uiso 1 1 calc R . . H15C H 0.7736 0.5047 0.6232 0.053(3) Uiso 1 1 calc R . . C16 C 0.8496(6) 0.4932(5) 0.3785(3) 0.0714(18) Uani 1 1 d . . . H16A H 0.9198 0.5386 0.4039 0.053(3) Uiso 1 1 calc R . . H16B H 0.8350 0.4864 0.3246 0.053(3) Uiso 1 1 calc R . . H16C H 0.8499 0.4268 0.3921 0.053(3) Uiso 1 1 calc R . . C60 C 0.8124(3) 0.9248(3) 0.4109(2) 0.0267(8) Uani 1 1 d . . . C61 C 0.8940(4) 0.9134(4) 0.3723(3) 0.0413(11) Uani 1 1 d . . . H61A H 0.9670 0.9342 0.4085 0.082(7) Uiso 1 1 calc R . . H61B H 0.8895 0.9570 0.3347 0.082(7) Uiso 1 1 calc R . . C62 C 0.8721(4) 0.7964(4) 0.3323(3) 0.054 Uiso 1 1 d . . . C70 C 0.4818(3) 0.7818(3) 0.3159(2) 0.0337(9) Uani 1 1 d . S . C71 C 0.4240(4) 0.7215(4) 0.2394(3) 0.0515(13) Uani 1 1 d . . . H71A H 0.4622 0.6686 0.2279 0.082(7) Uiso 1 1 calc R R 1 H71B H 0.4230 0.7660 0.2025 0.082(7) Uiso 1 1 calc R R 1 C72 C 0.3067(7) 0.6717(7) 0.2341(5) 0.049 Uiso 0.60 1 d P S 1 H72A H 0.2726 0.6251 0.1864 0.090 Uiso 0.60 1 calc PR S 1 H72B H 0.2660 0.7241 0.2380 0.090 Uiso 0.60 1 calc PR S 1 H72C H 0.3077 0.6346 0.2747 0.090 Uiso 0.60 1 calc PR S 1 C73 C 0.4931(12) 0.7234(11) 0.2004(8) 0.058 Uiso 0.40 1 d P S 2 H73A H 0.4602 0.6754 0.1532 0.090 Uiso 0.40 1 calc PR S 2 H73B H 0.5582 0.7048 0.2288 0.090 Uiso 0.40 1 calc PR S 2 H73C H 0.5120 0.7914 0.1906 0.090 Uiso 0.40 1 calc PR S 2 C101 C 0.3544(4) 0.8098(3) 0.0190(2) 0.0348(9) Uani 1 1 d . . . H101 H 0.3569 0.7408 0.0091 0.029(5) Uiso 1 1 calc R T . C102 C 0.2837(4) 0.8472(3) 0.0527(2) 0.0375(10) Uani 1 1 d . T . H102 H 0.2314 0.8104 0.0702 0.029(5) Uiso 1 1 calc R . . C103 C 0.3079(3) 0.9521(3) 0.0545(2) 0.0283(8) Uani 1 1 d . T . C104 C 0.2568(3) 1.0350(3) 0.0796(2) 0.0300(8) Uani 1 1 d . T . H10C H 0.2254 1.0161 0.1186 0.0290(19) Uiso 1 1 calc R . . H10D H 0.1980 1.0427 0.0372 0.0290(19) Uiso 1 1 calc R . . C105 C 0.3985(3) 1.1454(3) 0.1922(2) 0.0333(9) Uani 1 1 d . T . H10E H 0.3461 1.1247 0.2186 0.0290(19) Uiso 1 1 calc R . . H10F H 0.4345 1.2169 0.2137 0.0290(19) Uiso 1 1 calc R . . C106 C 0.4830(3) 1.0801(3) 0.2046(2) 0.0316(9) Uani 1 1 d . T . H10G H 0.5183 1.0871 0.2586 0.0290(19) Uiso 1 1 calc R . . H10H H 0.4470 1.0084 0.1843 0.0290(19) Uiso 1 1 calc R . . C107 C 0.2846(3) 1.2227(3) 0.0985(3) 0.0363(9) Uani 1 1 d . O . H10I H 0.2448 1.2140 0.0451 0.0290(19) Uiso 1 1 calc R . . H10J H 0.3401 1.2862 0.1124 0.0290(19) Uiso 1 1 calc R . . C108 C 0.2051(4) 1.2317(4) 0.1446(3) 0.0504(12) Uani 1 1 d . . . H10K H 0.1544 1.1656 0.1344 0.082(7) Uiso 1 1 calc R O 1 H10L H 0.2465 1.2466 0.1981 0.082(7) Uiso 1 1 calc R O 1 C109 C 0.6242(3) 1.0262(3) 0.1581(2) 0.0331(9) Uani 1 1 d . T . H10C H 0.6754 1.0453 0.1305 0.0290(19) Uiso 1 1 calc R . . H10D H 0.5700 0.9658 0.1270 0.0290(19) Uiso 1 1 calc R . . C110 C 0.6470(3) 1.2065(3) 0.2159(2) 0.0312(9) Uani 1 1 d . T . H11C H 0.6731 1.1943 0.2671 0.0290(19) Uiso 1 1 calc R . . H11D H 0.6086 1.2620 0.2177 0.0290(19) Uiso 1 1 calc R . . C113 C 0.6871(4) 0.9962(4) 0.2314(2) 0.0415(11) Uani 1 1 d . . . H11E H 0.7449 1.0535 0.2613 0.053(3) Uiso 1 1 calc R T . H11F H 0.7179 0.9388 0.2191 0.053(3) Uiso 1 1 calc R . . H11G H 0.6379 0.9774 0.2598 0.053(3) Uiso 1 1 calc R . . C114 C 0.7444(3) 1.2406(3) 0.1894(2) 0.0368(10) Uani 1 1 d . . . H11H H 0.7902 1.1917 0.1959 0.053(3) Uiso 1 1 calc R T . H11I H 0.7855 1.3069 0.2187 0.053(3) Uiso 1 1 calc R . . H11J H 0.7196 1.2449 0.1368 0.053(3) Uiso 1 1 calc R . . C160 C 0.5437(4) 1.3741(3) 0.0966(2) 0.0376(10) Uani 1 1 d . T . C161 C 0.5761(5) 1.4862(4) 0.1192(4) 0.0638(15) Uani 1 1 d . . . H16D H 0.5917 1.5144 0.0772 0.082(7) Uiso 1 1 calc R T . H16E H 0.5144 1.5112 0.1281 0.082(7) Uiso 1 1 calc R . . C162 C 0.6690(5) 1.5251(4) 0.1850(3) 0.058 Uiso 1 1 d . T . H16F H 0.6696 1.5948 0.2052 0.090 Uiso 1 1 calc R . . H16G H 0.7349 1.5234 0.1717 0.090 Uiso 1 1 calc R . . H16H H 0.6650 1.4834 0.2225 0.090 Uiso 1 1 calc R . . C170 C 0.3664(7) 1.2368(6) -0.0869(4) 0.047(2) Uiso 0.70 1 d P T 1 H17A H 0.3232 1.2130 -0.1391 0.052(9) Uiso 0.70 1 calc PR T 1 H17B H 0.4425 1.2554 -0.0836 0.052(9) Uiso 0.70 1 calc PR T 1 H17C H 0.3444 1.2957 -0.0661 0.052(9) Uiso 0.70 1 calc PR T 1 C171 C 0.3306(13) 1.2377(11) -0.0790(8) 0.028(3) Uiso 0.30 1 d P T 2 H17D H 0.3986 1.2766 -0.0813 0.052(9) Uiso 0.30 1 calc PR T 2 H17E H 0.2988 1.2808 -0.0503 0.052(9) Uiso 0.30 1 calc PR T 2 H17F H 0.2811 1.2129 -0.1295 0.052(9) Uiso 0.30 1 calc PR T 2 H5 H 0.839(4) 0.597(4) 0.514(3) 0.041(13) Uiso 1 1 d . . . H170 H 0.299(4) 1.118(4) -0.064(3) 0.032(14) Uiso 1 1 d . . . O80 O -0.0173(17) 1.6016(17) 0.2065(13) 0.061(5) Uiso 0.23 1 d P U 1 C80 C -0.047(3) 1.541(3) 0.2319(19) 0.081(9) Uiso 0.23 1 d P U 1 O81 O -0.009(3) 1.593(3) 0.2503(18) 0.048(7) Uiso 0.12 1 d P V 2 C81 C -0.018(5) 1.658(5) 0.237(3) 0.072(14) Uiso 0.12 1 d P V 2 O82 O -0.005(3) 1.662(2) 0.1372(16) 0.069(7) Uiso 0.17 1 d P W 3 C82 C 0.013(3) 1.630(2) 0.1982(16) 0.035(6) Uiso 0.17 1 d P W 3 O83 O -0.198(3) 1.681(2) 0.2484(17) 0.053(7) Uiso 0.12 1 d P X 4 C83 C -0.107(5) 1.659(4) 0.180(3) 0.066(13) Uiso 0.12 1 d P Y 4 O84 O -0.246(3) 1.696(2) 0.2703(16) 0.088(8) Uiso 0.18 1 d P . 5 C84 C -0.138(4) 1.673(3) 0.223(2) 0.081(11) Uiso 0.18 1 d P . 5 O85 O -0.040(3) 1.669(2) 0.1705(19) 0.089(8) Uiso 0.18 1 d P Z 6 C85 C 0.047(4) 1.668(3) 0.134(2) 0.065(9) Uiso 0.18 1 d P Z 6 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 0.0151(2) 0.0226(2) 0.0247(2) 0.00328(18) 0.00716(18) 0.00707(18) Ni2 0.0251(3) 0.0215(3) 0.0232(2) 0.00287(18) 0.00733(19) 0.00244(19) Cl10 0.0431(6) 0.0345(5) 0.0411(6) 0.0060(4) 0.0120(5) 0.0099(4) O10 0.083(3) 0.111(4) 0.089(3) 0.034(3) 0.051(3) 0.008(3) O11 0.099(3) 0.046(2) 0.065(2) -0.0190(18) -0.020(2) 0.032(2) O12 0.058(3) 0.045(2) 0.138(4) -0.015(2) 0.016(3) 0.0209(19) O13 0.118(4) 0.052(2) 0.0374(19) 0.0093(16) 0.001(2) -0.009(2) Cl20 0.0234(5) 0.0366(5) 0.0485(6) 0.0082(4) 0.0079(4) 0.0072(4) O20 0.019(2) 0.110(6) 0.073(4) 0.030(4) -0.003(2) 0.001(3) O21 0.088(5) 0.040(3) 0.080(4) 0.029(3) 0.032(4) 0.017(3) O22 0.071(4) 0.067(3) 0.073(3) -0.020(3) 0.006(3) 0.019(3) O23 0.034(3) 0.068(5) 0.089(6) 0.037(4) 0.027(4) 0.015(4) O120 0.062(18) 0.09(2) 0.064(15) 0.020(15) -0.025(13) -0.034(14) O123 0.020(10) 0.045(15) 0.061(13) -0.002(11) 0.018(8) -0.019(11) Cl30 0.071(6) 0.058(5) 0.104(8) 0.054(5) 0.038(5) 0.028(4) Cl40 0.028(5) 0.029(6) 0.138(15) -0.008(6) 0.008(6) -0.011(4) Cl40 0.0360(6) 0.0466(6) 0.0401(6) 0.0113(5) 0.0063(4) 0.0064(5) O40 0.043(2) 0.093(3) 0.070(3) 0.031(2) 0.0030(18) 0.022(2) O170 0.0444(19) 0.0288(16) 0.0327(16) 0.0073(13) 0.0018(14) 0.0101(15) N1 0.0162(14) 0.0233(15) 0.0252(15) 0.0018(12) 0.0066(12) 0.0070(12) N2 0.0125(14) 0.0228(15) 0.0229(14) 0.0002(11) 0.0064(11) 0.0062(11) N3 0.0183(15) 0.0246(16) 0.0297(16) 0.0029(12) 0.0072(12) 0.0070(12) N4 0.0161(14) 0.0224(15) 0.0270(15) 0.0050(12) 0.0069(12) 0.0044(12) N5 0.0236(18) 0.0235(17) 0.043(2) -0.0001(15) 0.0069(15) 0.0112(14) N60 0.0206(16) 0.0285(17) 0.0274(16) 0.0039(13) 0.0069(13) 0.0091(13) N70 0.0231(16) 0.0274(17) 0.0327(18) 0.0008(14) 0.0076(14) 0.0095(13) N101 0.0270(16) 0.0207(15) 0.0210(15) 0.0020(11) 0.0080(12) 0.0026(12) N102 0.0331(18) 0.0209(16) 0.0241(15) 0.0029(12) 0.0095(13) 0.0032(13) N103 0.0245(17) 0.0272(17) 0.0315(17) 0.0011(13) 0.0098(13) 0.0035(13) N104 0.0266(17) 0.0296(17) 0.0234(15) 0.0022(13) 0.0082(13) 0.0045(13) N105 0.033(3) 0.043(3) 0.056(4) 0.000(4) 0.012(4) 0.017(2) N140 0.048(12) 0.052(10) 0.027(9) 0.014(10) 0.020(10) 0.024(8) N160 0.0332(18) 0.0281(19) 0.0324(18) 0.0046(14) 0.0101(14) 0.0057(14) C1 0.0198(18) 0.0295(19) 0.0212(17) 0.0025(14) 0.0097(14) 0.0064(14) C2 0.0248(19) 0.0266(19) 0.0249(18) 0.0060(15) 0.0090(15) 0.0056(15) C3 0.0176(17) 0.0228(18) 0.0246(18) 0.0012(14) 0.0044(14) 0.0047(14) C4 0.0223(19) 0.0236(19) 0.035(2) 0.0035(15) 0.0096(15) 0.0072(15) C5 0.0227(19) 0.0250(19) 0.0297(19) 0.0055(15) 0.0054(15) 0.0104(15) C6 0.0190(18) 0.029(2) 0.033(2) 0.0034(16) 0.0070(15) 0.0084(15) C7 0.0223(19) 0.0270(19) 0.038(2) 0.0064(16) 0.0119(16) 0.0121(15) C8 0.027(2) 0.028(2) 0.044(2) 0.0052(17) 0.0152(17) 0.0120(16) C9 0.0201(18) 0.0264(19) 0.0255(18) 0.0052(14) 0.0068(14) 0.0071(15) C10 0.0179(18) 0.030(2) 0.032(2) 0.0034(16) 0.0062(15) 0.0033(15) C11 0.050(3) 0.024(2) 0.071(3) 0.008(2) 0.023(2) 0.015(2) C12 0.052(3) 0.058(3) 0.041(3) -0.003(2) 0.012(2) 0.030(2) C13 0.028(2) 0.038(2) 0.029(2) 0.0043(17) 0.0086(16) 0.0049(17) C14 0.029(2) 0.029(2) 0.0283(19) 0.0037(16) 0.0029(16) 0.0017(16) C15 0.102(5) 0.047(3) 0.072(4) 0.027(3) 0.036(3) 0.046(3) C16 0.090(5) 0.084(4) 0.068(4) 0.015(3) 0.042(3) 0.061(4) C60 0.0227(19) 0.032(2) 0.0292(19) 0.0084(15) 0.0098(16) 0.0109(16) C61 0.034(2) 0.060(3) 0.044(2) 0.016(2) 0.024(2) 0.022(2) C70 0.032(2) 0.027(2) 0.042(2) 0.0047(18) 0.0076(18) 0.0122(17) C71 0.065(3) 0.039(3) 0.039(3) -0.001(2) -0.001(2) 0.016(2) C101 0.045(2) 0.0207(19) 0.039(2) 0.0048(16) 0.0199(19) -0.0017(17) C102 0.040(2) 0.030(2) 0.044(2) 0.0057(18) 0.024(2) -0.0048(18) C103 0.026(2) 0.029(2) 0.0245(19) -0.0001(15) 0.0044(15) -0.0006(16) C104 0.0240(19) 0.031(2) 0.030(2) -0.0002(16) 0.0077(16) -0.0008(16) C105 0.029(2) 0.040(2) 0.0256(19) -0.0032(17) 0.0112(16) -0.0013(17) C106 0.033(2) 0.039(2) 0.0199(18) 0.0059(16) 0.0088(16) -0.0008(17) C107 0.031(2) 0.030(2) 0.048(2) 0.0018(18) 0.0141(19) 0.0087(17) C108 0.036(3) 0.040(3) 0.075(3) -0.006(2) 0.024(2) 0.010(2) C109 0.038(2) 0.035(2) 0.0231(19) 0.0026(16) 0.0037(16) 0.0123(18) C110 0.027(2) 0.035(2) 0.0258(19) -0.0019(16) 0.0052(16) 0.0023(17) C113 0.050(3) 0.045(3) 0.029(2) 0.0074(18) 0.0048(19) 0.022(2) C114 0.027(2) 0.039(2) 0.038(2) -0.0022(18) 0.0076(17) 0.0026(18) C160 0.037(2) 0.029(2) 0.044(2) 0.0017(18) 0.0129(19) 0.0053(18) C161 0.068(4) 0.028(3) 0.086(4) -0.007(2) 0.021(3) 0.005(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 N2 2.027(3) 2_676 ? Ni1 N1 2.033(3) . ? Ni1 N60 2.102(3) . ? Ni1 N70 2.188(3) . ? Ni1 N4 2.219(3) . ? Ni1 N3 2.246(3) . ? Ni1 Ni1 4.0389(13) 2_676 ? Ni2 N101 2.029(3) . ? Ni2 N102 2.043(3) 2_675 ? Ni2 N160 2.086(3) . ? Ni2 O170 2.168(3) . ? Ni2 N104 2.221(3) . ? Ni2 N103 2.233(3) . ? Ni2 Ni2 4.0600(15) 2_675 ? Cl10 O11 1.401(4) . ? Cl10 O13 1.417(4) . ? Cl10 O12 1.420(4) . ? Cl10 O10 1.432(4) . ? Cl20 O121 1.36(3) . ? Cl20 O123 1.38(3) . ? Cl20 O20 1.404(5) . ? Cl20 O120 1.43(2) . ? Cl20 O21 1.430(5) . ? Cl20 O122 1.43(2) . ? Cl20 O22 1.443(5) . ? Cl20 O23 1.443(8) . ? Cl30 O33 1.28(2) . ? Cl30 O32 1.44(2) . ? Cl30 O31 1.446(18) . ? Cl30 O30 1.52(2) . ? Cl40 O430 1.41(2) . ? Cl40 O431 1.44(2) . ? Cl40 O432 1.45(3) . ? Cl40 O433 1.47(3) . ? Cl50 O530 1.27(3) . ? Cl50 O532 1.43(3) . ? Cl50 O531 1.49(3) . ? Cl50 O533 1.70(3) . ? Cl40 O241 1.31(2) . ? Cl40 O40 1.415(4) . ? Cl40 O243 1.53(3) . ? Cl40 O242 1.60(4) . ? O170 C171 1.383(14) . ? O170 C170 1.457(8) . ? O170 H170 0.72(5) . ? N1 C3 1.345(5) . ? N1 N2 1.372(4) . ? N2 C1 1.347(5) . ? N2 Ni1 2.027(3) 2_676 ? N3 C7 1.488(5) . ? N3 C5 1.493(5) . ? N3 C4 1.493(5) . ? N4 C6 1.492(5) . ? N4 C9 1.493(4) . ? N4 C10 1.503(5) . ? N5 C8 1.499(5) . ? N5 C11 1.512(6) . ? N5 C12 1.513(6) . ? N5 H5 0.83(5) . ? N60 C60 1.136(5) . ? N70 C70 1.127(5) . ? N101 C103 1.347(5) . ? N101 N102 1.369(4) . ? N102 C101 1.345(5) . ? N102 Ni2 2.043(3) 2_675 ? N103 C107 1.481(5) . ? N103 C105 1.489(5) . ? N103 C104 1.500(5) . ? N104 C109 1.484(5) . ? N104 C106 1.487(5) . ? N104 C110 1.497(5) . ? N105 C108 1.449(8) . ? N105 C112 1.50(2) . ? N105 C111 1.708(12) . ? C111 C115 1.54(2) . ? C111 H11A 0.9700 . ? C111 H11B 0.9700 . ? C112 C116 1.50(3) . ? C112 H11F 0.9700 . ? C112 H11G 0.9700 . ? C115 H11C 0.9600 . ? C115 H11D 0.9600 . ? C115 H11E 0.9600 . ? C116 H11H 0.9600 . ? C116 H11I 0.9600 . ? C116 H11J 0.9600 . ? N140 C141 1.01(2) . ? N140 C143 1.55(3) . ? N140 C108 1.79(2) . ? C141 C142 1.51(2) . ? C141 C143 1.78(3) . ? C142 C143 2.01(3) . ? C143 C144 1.47(4) . ? C122 C126 1.35(3) . ? C122 C127 1.44(3) . ? C126 H12D 0.9600 . ? C126 H12E 0.9600 . ? C126 H12F 0.9600 . ? C127 H12G 0.9600 . ? C127 H12H 0.9600 . ? C127 H12I 0.9600 . ? N160 C160 1.133(5) . ? C1 C2 1.381(5) . ? C1 H1 0.9300 . ? C2 C3 1.389(5) . ? C2 H2 0.9300 . ? C3 C4 1.496(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.510(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.536(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C13 1.528(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C14 1.514(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C15 1.476(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C16 1.503(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C60 C61 1.458(5) . ? C61 C62 1.589(7) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 O84 1.85(3) 1_645 ? C70 C71 1.467(6) . ? C71 C73 1.304(14) . ? C71 C72 1.527(10) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C101 C102 1.377(6) . ? C101 H101 0.9300 . ? C102 C103 1.384(6) . ? C102 H102 0.9300 . ? C103 C104 1.483(5) . ? C104 H10C 0.9700 . ? C104 H10D 0.9700 . ? C105 C106 1.513(6) . ? C105 H10E 0.9700 . ? C105 H10F 0.9700 . ? C106 H10G 0.9700 . ? C106 H10H 0.9700 . ? C107 C108 1.529(6) . ? C107 H10I 0.9700 . ? C107 H10J 0.9700 . ? C108 H10K 0.9700 . ? C108 H10L 0.9700 . ? C109 C113 1.535(5) . ? C109 H10C 0.9700 . ? C109 H10D 0.9700 . ? C110 C114 1.506(6) . ? C110 H11C 0.9700 . ? C110 H11D 0.9700 . ? C113 H11E 0.9600 . ? C113 H11F 0.9600 . ? C113 H11G 0.9600 . ? C114 H11H 0.9600 . ? C114 H11I 0.9600 . ? C114 H11J 0.9600 . ? C160 C161 1.463(6) . ? C161 C162 1.427(8) . ? C161 H16D 0.9700 . ? C161 H16E 0.9700 . ? C162 H16F 0.9600 . ? C162 H16G 0.9600 . ? C162 H16H 0.9600 . ? C170 H17A 0.9600 . ? C170 H17B 0.9600 . ? C170 H17C 0.9600 . ? C171 H17D 0.9600 . ? C171 H17E 0.9600 . ? C171 H17F 0.9600 . ? O80 C80 1.07(4) . ? O81 C81 0.95(6) . ? O82 C82 1.25(4) . ? O84 C62 1.85(3) 1_465 ? O84 C84 1.90(5) . ? O85 C85 1.49(5) . ? 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 N1 96.27(12) 2_676 . ? N2 Ni1 N60 92.66(12) 2_676 . ? N1 Ni1 N60 168.94(12) . . ? N2 Ni1 N70 93.34(12) 2_676 . ? N1 Ni1 N70 90.49(12) . . ? N60 Ni1 N70 82.46(12) . . ? N2 Ni1 N4 96.30(11) 2_676 . ? N1 Ni1 N4 96.62(11) . . ? N60 Ni1 N4 88.85(11) . . ? N70 Ni1 N4 167.31(11) . . ? N2 Ni1 N3 176.45(11) 2_676 . ? N1 Ni1 N3 80.34(11) . . ? N60 Ni1 N3 90.83(12) . . ? N70 Ni1 N3 87.77(12) . . ? N4 Ni1 N3 83.11(11) . . ? N2 Ni1 Ni1 50.41(8) 2_676 2_676 ? N1 Ni1 Ni1 46.34(8) . 2_676 ? N60 Ni1 Ni1 143.06(9) . 2_676 ? N70 Ni1 Ni1 98.31(9) . 2_676 ? N4 Ni1 Ni1 94.19(8) . 2_676 ? N3 Ni1 Ni1 126.10(8) . 2_676 ? N101 Ni2 N102 95.90(12) . 2_675 ? N101 Ni2 N160 169.45(13) . . ? N102 Ni2 N160 92.70(13) 2_675 . ? N101 Ni2 O170 89.01(13) . . ? N102 Ni2 O170 93.15(13) 2_675 . ? N160 Ni2 O170 84.43(13) . . ? N101 Ni2 N104 93.07(12) . . ? N102 Ni2 N104 98.37(12) 2_675 . ? N160 Ni2 N104 91.70(13) . . ? O170 Ni2 N104 168.02(12) . . ? N101 Ni2 N103 81.55(12) . . ? N102 Ni2 N103 177.04(11) 2_675 . ? N160 Ni2 N103 89.68(13) . . ? O170 Ni2 N103 85.33(12) . . ? N104 Ni2 N103 83.31(12) . . ? N101 Ni2 Ni2 46.85(9) . 2_675 ? N102 Ni2 Ni2 49.47(9) 2_675 2_675 ? N160 Ni2 Ni2 142.16(10) . 2_675 ? O170 Ni2 Ni2 96.70(9) . 2_675 ? N104 Ni2 Ni2 93.32(9) . 2_675 ? N103 Ni2 Ni2 128.15(9) . 2_675 ? O11 Cl10 O13 111.0(2) . . ? O11 Cl10 O12 110.4(3) . . ? O13 Cl10 O12 110.0(3) . . ? O11 Cl10 O10 112.3(3) . . ? O13 Cl10 O10 107.1(3) . . ? O12 Cl10 O10 105.9(3) . . ? O121 Cl20 O123 109.8(18) . . ? O121 Cl20 O20 135.4(10) . . ? O123 Cl20 O20 111.0(15) . . ? O121 Cl20 O120 106.0(15) . . ? O123 Cl20 O120 114.3(17) . . ? O20 Cl20 O120 39.3(13) . . ? O121 Cl20 O21 22.9(9) . . ? O123 Cl20 O21 126.2(14) . . ? O20 Cl20 O21 113.1(4) . . ? O120 Cl20 O21 83.9(12) . . ? O121 Cl20 O122 107.9(15) . . ? O123 Cl20 O122 110.6(14) . . ? O20 Cl20 O122 73.3(10) . . ? O120 Cl20 O122 107.9(17) . . ? O21 Cl20 O122 110.3(9) . . ? O121 Cl20 O22 93.6(11) . . ? O123 Cl20 O22 81.4(10) . . ? O20 Cl20 O22 109.5(4) . . ? O120 Cl20 O22 147.6(15) . . ? O21 Cl20 O22 110.4(4) . . ? O122 Cl20 O22 40.3(9) . . ? O121 Cl20 O23 99.6(12) . . ? O123 Cl20 O23 26.2(9) . . ? O20 Cl20 O23 109.2(5) . . ? O120 Cl20 O23 95.8(14) . . ? O21 Cl20 O23 108.3(4) . . ? O122 Cl20 O23 136.3(10) . . ? O22 Cl20 O23 106.2(4) . . ? O33 Cl30 O32 108.2(16) . . ? O33 Cl30 O31 100.2(11) . . ? O32 Cl30 O31 105.3(13) . . ? O33 Cl30 O30 130.2(14) . . ? O32 Cl30 O30 110.1(13) . . ? O31 Cl30 O30 99.1(12) . . ? O430 Cl40 O431 99.7(14) . . ? O430 Cl40 O432 86.2(13) . . ? O431 Cl40 O432 98.9(16) . . ? O430 Cl40 O433 112.2(14) . . ? O431 Cl40 O433 135.6(16) . . ? O432 Cl40 O433 112.8(14) . . ? O530 Cl50 O532 122(2) . . ? O530 Cl50 O531 126(2) . . ? O532 Cl50 O531 110(2) . . ? O530 Cl50 O533 79.7(17) . . ? O532 Cl50 O533 94.3(19) . . ? O531 Cl50 O533 83.6(16) . . ? O241 Cl40 O40 124.5(10) . . ? O241 Cl40 O243 101.7(16) . . ? O40 Cl40 O243 102.2(12) . . ? O241 Cl40 O242 111.3(18) . . ? O40 Cl40 O242 91.1(16) . . ? O243 Cl40 O242 128(2) . . ? C171 O170 C170 21.2(7) . . ? C171 O170 Ni2 137.4(6) . . ? C170 O170 Ni2 127.0(4) . . ? C171 O170 H170 100(4) . . ? C170 O170 H170 111(4) . . ? Ni2 O170 H170 121(4) . . ? C3 N1 N2 108.0(3) . . ? C3 N1 Ni1 114.5(2) . . ? N2 N1 Ni1 135.4(2) . . ? C1 N2 N1 107.0(3) . . ? C1 N2 Ni1 127.9(2) . 2_676 ? N1 N2 Ni1 124.1(2) . 2_676 ? C7 N3 C5 111.4(3) . . ? C7 N3 C4 110.5(3) . . ? C5 N3 C4 110.7(3) . . ? C7 N3 Ni1 115.4(2) . . ? C5 N3 Ni1 104.7(2) . . ? C4 N3 Ni1 103.7(2) . . ? C6 N4 C9 111.6(3) . . ? C6 N4 C10 106.3(3) . . ? C9 N4 C10 110.2(3) . . ? C6 N4 Ni1 101.2(2) . . ? C9 N4 Ni1 111.2(2) . . ? C10 N4 Ni1 115.9(2) . . ? C8 N5 C11 111.1(3) . . ? C8 N5 C12 111.2(3) . . ? C11 N5 C12 112.1(3) . . ? C8 N5 H5 103(3) . . ? C11 N5 H5 100(3) . . ? C12 N5 H5 119(3) . . ? C60 N60 Ni1 173.7(3) . . ? C70 N70 Ni1 175.4(3) . . ? C103 N101 N102 107.9(3) . . ? C103 N101 Ni2 114.5(2) . . ? N102 N101 Ni2 134.4(2) . . ? C101 N102 N101 107.3(3) . . ? C101 N102 Ni2 126.6(3) . 2_675 ? N101 N102 Ni2 126.0(2) . 2_675 ? C107 N103 C105 110.3(3) . . ? C107 N103 C104 110.4(3) . . ? C105 N103 C104 111.4(3) . . ? C107 N103 Ni2 114.9(2) . . ? C105 N103 Ni2 104.0(2) . . ? C104 N103 Ni2 105.6(2) . . ? C109 N104 C106 108.8(3) . . ? C109 N104 C110 110.6(3) . . ? C106 N104 C110 108.6(3) . . ? C109 N104 Ni2 108.9(2) . . ? C106 N104 Ni2 103.0(2) . . ? C110 N104 Ni2 116.4(2) . . ? C108 N105 C112 123.7(11) . . ? C108 N105 C111 105.9(6) . . ? C112 N105 C111 122.3(10) . . ? C115 C111 N105 119.8(11) . . ? C115 C111 H11A 107.4 . . ? N105 C111 H11A 107.4 . . ? C115 C111 H11B 107.4 . . ? N105 C111 H11B 107.4 . . ? H11A C111 H11B 106.9 . . ? N105 C112 C116 101.5(17) . . ? N105 C112 H11F 111.5 . . ? C116 C112 H11F 111.5 . . ? N105 C112 H11G 111.5 . . ? C116 C112 H11G 111.5 . . ? H11F C112 H11G 109.3 . . ? C141 N140 C143 85.2(19) . . ? C141 N140 C108 111.7(18) . . ? C143 N140 C108 102.3(13) . . ? N140 C141 C142 111.3(18) . . ? N140 C141 C143 60.2(15) . . ? C142 C141 C143 74.7(12) . . ? C141 C142 C143 58.8(11) . . ? C144 C143 N140 113(2) . . ? C144 C143 C141 88.4(17) . . ? N140 C143 C141 34.6(10) . . ? C144 C143 C142 94.7(18) . . ? N140 C143 C142 71.1(13) . . ? C141 C143 C142 46.5(10) . . ? C126 C122 C127 100(2) . . ? C160 N160 Ni2 177.5(4) . . ? N2 C1 C2 110.9(3) . . ? N2 C1 H1 124.6 . . ? C2 C1 H1 124.6 . . ? C1 C2 C3 103.9(3) . . ? C1 C2 H2 128.0 . . ? C3 C2 H2 128.0 . . ? N1 C3 C2 110.2(3) . . ? N1 C3 C4 118.3(3) . . ? C2 C3 C4 131.6(3) . . ? N3 C4 C3 108.8(3) . . ? N3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N3 C5 C6 110.5(3) . . ? N3 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N3 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N4 C6 C5 111.9(3) . . ? N4 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N4 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C8 112.7(3) . . ? N3 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N5 C8 C7 113.4(3) . . ? N5 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? N5 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N4 C9 C13 116.1(3) . . ? N4 C9 H9A 108.3 . . ? C13 C9 H9A 108.3 . . ? N4 C9 H9B 108.3 . . ? C13 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N4 C10 C14 116.8(3) . . ? N4 C10 H10A 108.1 . . ? C14 C10 H10A 108.1 . . ? N4 C10 H10B 108.1 . . ? C14 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? C15 C11 N5 112.9(4) . . ? C15 C11 H11A 109.0 . . ? N5 C11 H11A 109.0 . . ? C15 C11 H11B 109.0 . . ? N5 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C16 C12 N5 114.2(4) . . ? C16 C12 H12A 108.7 . . ? N5 C12 H12A 108.7 . . ? C16 C12 H12B 108.7 . . ? N5 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N60 C60 C61 177.4(4) . . ? C60 C61 C62 109.2(4) . . ? C60 C61 H61A 109.8 . . ? C62 C61 H61A 109.9 . . ? C60 C61 H61B 109.8 . . ? C62 C61 H61B 109.8 . . ? H61A C61 H61B 108.3 . . ? C61 C62 O84 137.3(10) . 1_645 ? N70 C70 C71 178.6(5) . . ? C73 C71 C70 108.5(7) . . ? C73 C71 C72 141.4(8) . . ? C70 C71 C72 110.0(5) . . ? C73 C71 H71A 51.9 . . ? C70 C71 H71A 109.7 . . ? C72 C71 H71A 109.7 . . ? C73 C71 H71B 59.6 . . ? C70 C71 H71B 109.7 . . ? C72 C71 H71B 109.7 . . ? H71A C71 H71B 108.2 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N102 C101 C102 110.6(4) . . ? N102 C101 H101 124.7 . . ? C102 C101 H101 124.7 . . ? C101 C102 C103 104.4(4) . . ? C101 C102 H102 127.8 . . ? C103 C102 H102 127.8 . . ? N101 C103 C102 109.9(3) . . ? N101 C103 C104 118.8(3) . . ? C102 C103 C104 131.3(4) . . ? C103 C104 N103 111.5(3) . . ? C103 C104 H10C 109.3 . . ? N103 C104 H10C 109.3 . . ? C103 C104 H10D 109.3 . . ? N103 C104 H10D 109.3 . . ? H10C C104 H10D 108.0 . . ? N103 C105 C106 112.0(3) . . ? N103 C105 H10E 109.2 . . ? C106 C105 H10E 109.2 . . ? N103 C105 H10F 109.2 . . ? C106 C105 H10F 109.2 . . ? H10E C105 H10F 107.9 . . ? N104 C106 C105 111.2(3) . . ? N104 C106 H10G 109.4 . . ? C105 C106 H10G 109.4 . . ? N104 C106 H10H 109.4 . . ? C105 C106 H10H 109.4 . . ? H10G C106 H10H 108.0 . . ? N103 C107 C108 113.0(4) . . ? N103 C107 H10I 109.0 . . ? C108 C107 H10I 109.0 . . ? N103 C107 H10J 109.0 . . ? C108 C107 H10J 109.0 . . ? H10I C107 H10J 107.8 . . ? N105 C108 C107 114.9(5) . . ? N105 C108 N140 21.5(6) . . ? C107 C108 N140 96.9(7) . . ? N105 C108 H10K 108.5 . . ? C107 C108 H10K 108.5 . . ? N140 C108 H10K 105.8 . . ? N105 C108 H10L 108.5 . . ? C107 C108 H10L 108.5 . . ? N140 C108 H10L 128.1 . . ? H10K C108 H10L 107.5 . . ? N104 C109 C113 116.3(3) . . ? N104 C109 H10C 108.2 . . ? C113 C109 H10C 108.2 . . ? N104 C109 H10D 108.2 . . ? C113 C109 H10D 108.2 . . ? H10C C109 H10D 107.4 . . ? N104 C110 C114 114.5(3) . . ? N104 C110 H11C 108.6 . . ? C114 C110 H11C 108.6 . . ? N104 C110 H11D 108.6 . . ? C114 C110 H11D 108.6 . . ? H11C C110 H11D 107.6 . . ? C109 C113 H11E 109.5 . . ? C109 C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? C109 C113 H11G 109.5 . . ? H11E C113 H11G 109.5 . . ? H11F C113 H11G 109.5 . . ? C110 C114 H11H 109.5 . . ? C110 C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? C110 C114 H11J 109.5 . . ? H11H C114 H11J 109.5 . . ? H11I C114 H11J 109.5 . . ? N160 C160 C161 178.3(5) . . ? C162 C161 C160 115.5(5) . . ? C162 C161 H16D 108.4 . . ? C160 C161 H16D 108.4 . . ? C162 C161 H16E 108.4 . . ? C160 C161 H16E 108.4 . . ? H16D C161 H16E 107.5 . . ? C161 C162 H16F 109.5 . . ? C161 C162 H16G 109.5 . . ? H16F C162 H16G 109.5 . . ? C161 C162 H16H 109.5 . . ? H16F C162 H16H 109.5 . . ? H16G C162 H16H 109.5 . . ? O170 C170 H17A 109.5 . . ? O170 C170 H17B 109.5 . . ? O170 C170 H17C 109.5 . . ? O170 C171 H17D 109.5 . . ? O170 C171 H17E 109.5 . . ? H17D C171 H17E 109.5 . . ? O170 C171 H17F 109.5 . . ? H17D C171 H17F 109.5 . . ? H17E C171 H17F 109.5 . . ? C62 O84 C84 79.8(17) 1_465 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.706 _refine_diff_density_min -2.357 _refine_diff_density_rms 0.099 #================================================================ data_fm21 _database_code_CSD 160994 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H64 Cl2 N8 Ni2 O10' _chemical_formula_weight 873.20 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.4373(6) _cell_length_b 24.0949(18) _cell_length_c 19.2556(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.828(1) _cell_angle_gamma 90.00 _cell_volume 3909.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13555 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8163 _reflns_number_gt 7655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0688P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(9) _refine_ls_number_reflns 8163 _refine_ls_number_parameters 634 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.56771(4) 0.797253(14) 0.50848(2) 0.02030(9) Uani 1 1 d . . . Ni2 Ni 0.62486(4) 0.934972(14) 0.65602(2) 0.02182(9) Uani 1 1 d . . . Cl1 Cl 0.10303(9) 0.73133(3) 0.69028(4) 0.02996(16) Uani 1 1 d . . . Cl2 Cl 0.05473(13) 0.98027(4) 0.95313(5) 0.0459(2) Uani 1 1 d . . . O1 O 0.3833(2) 0.82452(9) 0.55686(12) 0.0229(4) Uani 1 1 d . . . O2 O 0.4155(3) 0.91217(9) 0.61630(12) 0.0265(4) Uani 1 1 d D . . O3 O 0.0195(6) 0.71037(18) 0.6299(2) 0.0845(14) Uani 1 1 d . . . O4 O 0.1851(5) 0.68605(13) 0.72392(16) 0.0622(10) Uani 1 1 d . . . O5 O 0.2155(5) 0.77070(13) 0.6687(2) 0.0714(11) Uani 1 1 d . . . O6 O 0.0023(5) 0.75776(16) 0.7371(2) 0.0658(10) Uani 1 1 d . . . O7 O -0.0073(9) 1.01783(19) 0.9019(3) 0.122(2) Uani 1 1 d . . . O8 O 0.1190(8) 0.93444(17) 0.9177(2) 0.1024(19) Uani 1 1 d . . . O9 O -0.0606(10) 0.9601(3) 0.9941(4) 0.153(3) Uani 1 1 d . . . O10 O 0.1703(5) 1.0104(2) 0.9955(2) 0.0780(12) Uani 1 1 d . . . N1 N 0.7464(3) 0.83816(11) 0.55723(14) 0.0271(5) Uani 1 1 d . . . N2 N 0.7615(3) 0.88438(11) 0.59840(14) 0.0253(5) Uani 1 1 d . . . N3 N 0.7508(3) 0.76253(11) 0.45159(15) 0.0290(5) Uani 1 1 d . . . N4 N 0.5408(3) 0.85453(10) 0.42131(13) 0.0230(5) Uani 1 1 d . . . N5 N 0.5614(3) 0.71396(10) 0.55340(16) 0.0284(6) Uani 1 1 d . . . N6 N 0.8530(3) 0.96072(12) 0.69295(15) 0.0333(6) Uani 1 1 d . . . N7 N 0.6160(3) 0.89351(11) 0.75412(15) 0.0288(6) Uani 1 1 d . . . N8 N 0.5869(3) 1.02528(11) 0.64302(18) 0.0362(7) Uani 1 1 d . . . C1 C 0.9179(4) 0.89852(14) 0.59940(17) 0.0277(6) Uani 1 1 d . . . C2 C 1.0021(4) 0.86373(13) 0.55924(18) 0.0291(6) Uani 1 1 d . . . C3 C 0.8896(4) 0.82616(13) 0.53384(17) 0.0276(6) Uani 1 1 d . . . C4 C 0.9051(4) 0.77655(14) 0.48817(19) 0.0329(7) Uani 1 1 d . . . H4A H 0.9851 0.7841 0.4535 0.045(4) Uiso 1 1 calc R . . H4B H 0.9424 0.7445 0.5167 0.045(4) Uiso 1 1 calc R . . C5 C 0.7396(5) 0.78829(16) 0.38126(19) 0.0337(7) Uani 1 1 d . . . C6 C 0.6955(4) 0.84905(14) 0.38726(18) 0.0304(6) Uani 1 1 d . . . C7 C 0.7256(5) 0.70191(14) 0.4488(2) 0.0352(8) Uani 1 1 d . . . C8 C 0.6858(4) 0.68048(14) 0.5197(2) 0.0365(8) Uani 1 1 d . . . C9 C 0.4091(4) 0.84035(16) 0.36973(18) 0.0289(7) Uani 1 1 d . . . C10 C 0.2438(4) 0.84924(17) 0.3942(2) 0.0382(8) Uani 1 1 d . . . C11 C 0.5231(5) 0.91201(12) 0.44829(17) 0.0292(6) Uani 1 1 d . . . C12 C 0.5223(7) 0.95811(16) 0.3941(2) 0.0450(10) Uani 1 1 d . . . C13 C 0.4015(4) 0.68879(14) 0.54101(19) 0.0326(7) Uani 1 1 d . . . H13A H 0.3272 0.7069 0.5721 0.045(4) Uiso 1 1 calc R . . H13B H 0.4075 0.6490 0.5539 0.045(4) Uiso 1 1 calc R . . C14 C 0.3346(5) 0.69340(17) 0.4673(2) 0.0403(8) Uani 1 1 d . . . H14A H 0.3281 0.7326 0.4538 0.063(4) Uiso 1 1 calc R . . H14B H 0.2283 0.6769 0.4638 0.063(4) Uiso 1 1 calc R . . H14C H 0.4038 0.6737 0.4362 0.063(4) Uiso 1 1 calc R . . C15 C 0.6002(5) 0.71891(14) 0.62890(19) 0.0337(7) Uani 1 1 d . . . C16 C 0.6080(6) 0.66375(16) 0.6695(2) 0.0465(10) Uani 1 1 d . . . H16A H 0.5016 0.6475 0.6700 0.063(4) Uiso 1 1 calc R . . H16B H 0.6480 0.6707 0.7174 0.063(4) Uiso 1 1 calc R . . H16C H 0.6793 0.6380 0.6470 0.063(4) Uiso 1 1 calc R . . C17 C 0.9684(4) 0.94936(15) 0.6394(2) 0.0359(7) Uani 1 1 d . . . C18 C 0.8946(5) 0.9256(2) 0.7552(2) 0.0450(9) Uani 1 1 d . . . H18A H 0.9791 0.9440 0.7843 0.045(4) Uiso 1 1 calc R . . H18B H 0.9358 0.8893 0.7400 0.045(4) Uiso 1 1 calc R . . C19 C 0.7515(5) 0.91630(17) 0.7978(2) 0.0420(8) Uani 1 1 d . . . H19A H 0.7793 0.8901 0.8361 0.045(4) Uiso 1 1 calc R . . H19B H 0.7197 0.9519 0.8187 0.045(4) Uiso 1 1 calc R . . C20 C 0.8467(5) 1.02072(15) 0.7106(2) 0.0393(8) Uani 1 1 d . . . C21 C 0.7498(5) 1.04973(16) 0.6536(2) 0.0384(8) Uani 1 1 d . . . C22 C 0.6237(6) 0.83365(14) 0.7373(2) 0.0377(8) Uani 1 1 d . . . C23 C 0.6387(7) 0.79423(18) 0.8000(3) 0.0518(12) Uani 1 1 d . . . C24 C 0.4759(6) 0.90576(15) 0.7980(2) 0.0455(10) Uani 1 1 d . . . C25 C 0.3206(5) 0.8797(2) 0.7730(3) 0.0506(10) Uani 1 1 d . . . C26 C 0.4846(5) 1.05280(16) 0.6955(3) 0.0442(9) Uani 1 1 d . . . C27 C 0.3173(5) 1.03049(16) 0.6958(3) 0.0482(10) Uani 1 1 d . . . H27A H 0.2614 1.0388 0.6511 0.063(4) Uiso 1 1 calc R . . H27B H 0.2614 1.0479 0.7335 0.063(4) Uiso 1 1 calc R . . H27C H 0.3205 0.9902 0.7028 0.063(4) Uiso 1 1 calc R . . C28 C 0.5347(5) 1.03119(15) 0.5691(3) 0.0481(10) Uani 1 1 d . . . H28A H 0.4253 1.0165 0.5631 0.045(4) Uiso 1 1 calc R . . H28B H 0.6034 1.0075 0.5413 0.045(4) Uiso 1 1 calc R . . C29 C 0.5361(7) 1.08918(19) 0.5391(3) 0.0658(14) Uani 1 1 d . . . H29A H 0.4666 1.1132 0.5652 0.063(4) Uiso 1 1 calc R . . H29B H 0.4980 1.0880 0.4902 0.063(4) Uiso 1 1 calc R . . H29C H 0.6445 1.1039 0.5424 0.063(4) Uiso 1 1 calc R . . H1O H 0.346(6) 0.807(2) 0.582(3) 0.048(14) Uiso 1 1 d . . . H2OO H 0.381(6) 0.9366(16) 0.594(3) 0.065(16) Uiso 1 1 d D . . H2O H 0.406(6) 0.866(2) 0.589(3) 0.050(13) Uiso 1 1 d . . . H2 H 1.103(5) 0.8702(14) 0.5525(19) 0.022(9) Uiso 1 1 d . . . H5A H 0.819(6) 0.7846(19) 0.368(3) 0.045(13) Uiso 1 1 d . . . H5B H 0.650(6) 0.7674(19) 0.354(2) 0.040(11) Uiso 1 1 d . . . H6B H 0.775(5) 0.8696(18) 0.413(2) 0.039(11) Uiso 1 1 d . . . H6A H 0.709(5) 0.8657(15) 0.339(2) 0.025(9) Uiso 1 1 d . . . H7A H 0.807(5) 0.6844(17) 0.431(2) 0.032(10) Uiso 1 1 d . . . H7B H 0.613(5) 0.6887(17) 0.416(2) 0.037(10) Uiso 1 1 d . . . H8A H 0.791(5) 0.6847(17) 0.550(2) 0.036(10) Uiso 1 1 d . . . H8B H 0.665(6) 0.638(2) 0.518(3) 0.048(13) Uiso 1 1 d . . . H9A H 0.419(6) 0.8156(19) 0.366(3) 0.030(13) Uiso 1 1 d . . . H9B H 0.437(5) 0.8658(16) 0.321(2) 0.029(9) Uiso 1 1 d . . . H10A H 0.170(5) 0.8295(18) 0.364(2) 0.039(11) Uiso 1 1 d . . . H10B H 0.216(7) 0.895(2) 0.394(3) 0.068(16) Uiso 1 1 d . . . H10C H 0.232(6) 0.834(2) 0.445(3) 0.057(14) Uiso 1 1 d . . . H11A H 0.615(7) 0.922(2) 0.479(3) 0.056(14) Uiso 1 1 d . . . H11B H 0.437(5) 0.9125(16) 0.470(2) 0.027(9) Uiso 1 1 d . . . H12A H 0.451(5) 0.9501(16) 0.362(2) 0.026(10) Uiso 1 1 d . . . H12B H 0.626(7) 0.958(2) 0.375(3) 0.058(15) Uiso 1 1 d . . . H12C H 0.503(8) 0.983(3) 0.417(4) 0.075(19) Uiso 1 1 d . . . H15A H 0.511(5) 0.7383(16) 0.649(2) 0.026(9) Uiso 1 1 d . . . H15B H 0.685(6) 0.7334(17) 0.630(2) 0.033(11) Uiso 1 1 d . . . H17A H 0.980(4) 0.9822(15) 0.606(2) 0.025(9) Uiso 1 1 d . . . H17B H 1.093(5) 0.9431(16) 0.663(2) 0.038(11) Uiso 1 1 d . . . H20A H 0.947(4) 1.0371(15) 0.712(2) 0.022(8) Uiso 1 1 d . . . H20B H 0.779(5) 1.0290(16) 0.755(2) 0.034(10) Uiso 1 1 d . . . H21A H 0.752(6) 1.0798(19) 0.665(3) 0.041(12) Uiso 1 1 d . . . H21B H 0.811(4) 1.0447(15) 0.606(2) 0.020(8) Uiso 1 1 d . . . H22A H 0.549(4) 0.8255(12) 0.7090(17) 0.003(7) Uiso 1 1 d . . . H22B H 0.710(6) 0.8321(18) 0.710(3) 0.044(12) Uiso 1 1 d . . . H23A H 0.600(7) 0.760(3) 0.777(3) 0.069(17) Uiso 1 1 d . . . H23B H 0.544(5) 0.7952(16) 0.832(2) 0.031(10) Uiso 1 1 d . . . H24A H 0.498(4) 0.8905(13) 0.8449(19) 0.017(8) Uiso 1 1 d . . . H24B H 0.481(7) 0.952(2) 0.798(3) 0.066(16) Uiso 1 1 d . . . H25A H 0.331(6) 0.841(2) 0.781(3) 0.041(11) Uiso 1 1 d . . . H25B H 0.300(7) 0.894(2) 0.729(3) 0.063(15) Uiso 1 1 d . . . H25C H 0.227(6) 0.893(2) 0.804(3) 0.063(15) Uiso 1 1 d . . . H26A H 0.498(4) 1.0919(16) 0.684(2) 0.024(9) Uiso 1 1 d . . . H26B H 0.528(5) 1.0546(17) 0.738(3) 0.032(10) Uiso 1 1 d . . . H23C H 0.729(6) 0.8010(19) 0.838(3) 0.048(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01787(16) 0.02223(17) 0.02089(17) -0.00041(14) 0.00193(12) 0.00097(14) Ni2 0.02260(18) 0.02246(17) 0.02039(17) -0.00085(14) 0.00078(13) -0.00612(14) Cl1 0.0364(4) 0.0280(3) 0.0255(4) 0.0029(3) 0.0020(3) -0.0031(3) Cl2 0.0592(6) 0.0388(5) 0.0401(5) -0.0010(4) 0.0062(4) 0.0056(4) O1 0.0190(10) 0.0224(10) 0.0277(11) 0.0026(8) 0.0065(8) -0.0006(8) O2 0.0240(11) 0.0240(10) 0.0313(12) 0.0016(9) -0.0024(9) -0.0055(8) O3 0.089(3) 0.083(3) 0.077(3) -0.018(2) -0.045(3) -0.001(2) O4 0.105(3) 0.0438(16) 0.0371(16) 0.0051(12) -0.0036(17) 0.0275(17) O5 0.080(2) 0.0445(17) 0.095(3) 0.0038(17) 0.049(2) -0.0121(16) O6 0.065(2) 0.076(2) 0.059(2) 0.0128(17) 0.0314(17) 0.0250(18) O7 0.181(6) 0.067(3) 0.110(4) -0.003(3) -0.076(4) 0.025(3) O8 0.190(6) 0.070(3) 0.048(2) -0.0004(18) 0.022(3) 0.058(3) O9 0.201(7) 0.120(4) 0.150(6) -0.063(4) 0.120(5) -0.097(5) O10 0.050(2) 0.105(3) 0.078(3) -0.019(2) -0.0061(19) 0.007(2) N1 0.0204(12) 0.0350(14) 0.0260(13) -0.0023(10) 0.0013(10) -0.0021(10) N2 0.0196(12) 0.0362(13) 0.0203(12) 0.0003(10) 0.0015(9) -0.0054(10) N3 0.0248(13) 0.0301(13) 0.0326(14) -0.0011(10) 0.0063(11) 0.0058(10) N4 0.0266(12) 0.0210(11) 0.0216(12) 0.0000(9) 0.0040(9) -0.0005(9) N5 0.0257(13) 0.0198(11) 0.0394(16) -0.0047(10) -0.0014(11) 0.0010(9) N6 0.0321(15) 0.0382(15) 0.0293(14) -0.0019(11) -0.0033(11) -0.0109(11) N7 0.0315(14) 0.0260(13) 0.0284(14) 0.0055(10) -0.0031(11) -0.0041(10) N8 0.0296(15) 0.0221(12) 0.057(2) -0.0046(12) 0.0007(13) -0.0041(10) C1 0.0225(14) 0.0359(16) 0.0246(15) 0.0048(12) 0.0001(11) -0.0048(12) C2 0.0180(14) 0.0335(16) 0.0357(17) 0.0027(12) 0.0012(12) 0.0003(11) C3 0.0202(14) 0.0359(16) 0.0270(15) 0.0043(12) 0.0029(11) 0.0000(11) C4 0.0227(15) 0.0345(16) 0.0415(19) 0.0006(14) 0.0019(13) 0.0066(12) C5 0.0323(18) 0.0422(19) 0.0276(17) -0.0017(13) 0.0114(14) 0.0089(14) C6 0.0291(16) 0.0363(17) 0.0266(16) 0.0016(13) 0.0088(12) -0.0016(12) C7 0.0320(17) 0.0294(16) 0.045(2) -0.0133(14) 0.0083(15) 0.0044(13) C8 0.0354(18) 0.0258(16) 0.048(2) -0.0089(14) 0.0024(16) 0.0046(13) C9 0.0354(18) 0.0257(17) 0.0254(16) -0.0013(13) -0.0006(12) 0.0009(13) C10 0.0295(18) 0.051(2) 0.0340(19) -0.0033(16) 0.0008(14) 0.0001(15) C11 0.044(2) 0.0188(13) 0.0252(15) -0.0016(11) 0.0058(14) -0.0002(12) C12 0.079(3) 0.0219(17) 0.035(2) 0.0050(15) 0.011(2) -0.0030(17) C13 0.0327(17) 0.0265(15) 0.0386(19) 0.0001(13) 0.0007(14) -0.0052(12) C14 0.0321(18) 0.044(2) 0.045(2) 0.0008(16) -0.0041(15) -0.0097(15) C15 0.041(2) 0.0259(15) 0.0337(18) 0.0005(13) -0.0031(14) 0.0007(14) C16 0.060(3) 0.0300(17) 0.049(2) 0.0046(15) -0.003(2) 0.0011(17) C17 0.0258(16) 0.0393(17) 0.042(2) -0.0021(15) -0.0021(14) -0.0081(13) C18 0.0325(19) 0.069(3) 0.0321(19) 0.0032(17) -0.0102(15) -0.0068(17) C19 0.047(2) 0.046(2) 0.0328(18) -0.0007(16) -0.0008(16) 0.0000(17) C20 0.0337(18) 0.0421(19) 0.042(2) -0.0156(15) 0.0026(15) -0.0176(15) C21 0.041(2) 0.0287(18) 0.046(2) -0.0110(15) 0.0085(16) -0.0134(14) C22 0.055(2) 0.0240(15) 0.0356(19) 0.0037(14) 0.0137(18) 0.0113(15) C23 0.077(3) 0.038(2) 0.042(2) 0.0172(17) 0.018(2) 0.014(2) C24 0.082(3) 0.0307(17) 0.0255(18) -0.0028(13) 0.0147(18) 0.0041(18) C25 0.043(2) 0.058(3) 0.053(3) 0.016(2) 0.024(2) 0.0077(18) C26 0.043(2) 0.0269(17) 0.063(3) -0.0155(17) -0.0019(19) -0.0023(14) C27 0.035(2) 0.0358(19) 0.074(3) -0.0059(18) 0.0030(19) 0.0037(15) C28 0.047(2) 0.0298(17) 0.066(3) 0.0023(17) -0.013(2) -0.0057(15) C29 0.060(3) 0.041(2) 0.095(4) 0.023(2) -0.017(3) -0.005(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 O1 1.966(2) . ? Ni1 N1 1.997(3) . ? Ni1 N3 2.110(3) . ? Ni1 N4 2.176(2) . ? Ni1 N5 2.187(3) . ? Ni1 Ni2 4.3795(5) . ? Ni2 O2 1.968(2) . ? Ni2 N2 2.043(3) . ? Ni2 N6 2.112(3) . ? Ni2 N7 2.141(3) . ? Ni2 N8 2.212(3) . ? Cl1 O5 1.419(3) . ? Cl1 O6 1.420(3) . ? Cl1 O3 1.423(4) . ? Cl1 O4 1.430(3) . ? Cl2 O9 1.371(5) . ? Cl2 O7 1.420(5) . ? Cl2 O8 1.420(4) . ? Cl2 O10 1.437(4) . ? O1 O2 2.411(3) . ? O1 O5 2.936(4) . ? O1 H1O 0.74(6) . ? O1 H2O 1.19(5) . ? O2 H2O 1.23(5) . ? O2 H2OO 0.78(2) . ? O2 H2O 1.23(5) . ? O5 H1O 2.21(6) . ? N1 C3 1.342(4) . ? N1 N2 1.369(4) . ? N2 C1 1.362(4) . ? N3 C7 1.477(4) . ? N3 C5 1.489(5) . ? N3 C4 1.488(4) . ? N4 C11 1.489(4) . ? N4 C9 1.493(4) . ? N4 C6 1.495(4) . ? N5 C15 1.479(5) . ? N5 C13 1.488(4) . ? N5 C8 1.497(4) . ? N6 C17 1.478(5) . ? N6 C20 1.487(5) . ? N6 C18 1.496(5) . ? N7 C22 1.480(4) . ? N7 C19 1.490(5) . ? N7 C24 1.515(5) . ? N8 C28 1.476(6) . ? N8 C21 1.500(5) . ? N8 C26 1.514(5) . ? C1 C2 1.364(5) . ? C1 C17 1.498(5) . ? C2 C3 1.384(4) . ? C2 H2 0.88(4) . ? C3 C4 1.493(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.516(5) . ? C5 H5A 0.74(5) . ? C5 H5B 1.03(5) . ? C6 H6B 0.95(5) . ? C6 H6A 1.02(4) . ? C7 C8 1.513(6) . ? C7 H7A 0.89(4) . ? C7 H7B 1.16(4) . ? C8 H8A 1.05(4) . ? C8 H8B 1.04(5) . ? C9 C10 1.509(5) . ? C9 H9A 0.61(4) . ? C9 H9B 1.16(4) . ? C10 H10A 0.95(5) . ? C10 H10B 1.12(6) . ? C10 H10C 1.05(6) . ? C11 C12 1.523(5) . ? C11 H11A 0.98(6) . ? C11 H11B 0.86(5) . ? C12 H12A 0.86(4) . ? C12 H12B 0.97(6) . ? C12 H12C 0.77(7) . ? C13 C14 1.506(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.542(5) . ? C15 H15A 0.98(4) . ? C15 H15B 0.80(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 1.03(4) . ? C17 H17B 1.14(4) . ? C18 C19 1.509(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.507(6) . ? C20 H20A 0.94(4) . ? C20 H20B 1.08(5) . ? C21 H21A 0.76(5) . ? C21 H21B 1.07(4) . ? C22 C23 1.536(5) . ? C22 H22A 0.84(3) . ? C22 H22B 0.92(5) . ? C23 H23A 0.98(6) . ? C23 H23B 1.03(5) . ? C23 H23C 1.04(5) . ? C24 C25 1.510(7) . ? C24 H24A 0.99(4) . ? C24 H24B 1.13(6) . ? C25 H25A 0.94(5) . ? C25 H25B 0.92(6) . ? C25 H25C 1.07(6) . ? C26 C27 1.511(6) . ? C26 H26A 0.97(4) . ? C26 H26B 0.89(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.513(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 O1 Ni1 N1 102.08(10) . . ? O1 Ni1 N3 174.50(10) . . ? N1 Ni1 N3 83.38(11) . . ? O1 Ni1 N4 95.66(9) . . ? N1 Ni1 N4 95.58(10) . . ? N3 Ni1 N4 84.39(10) . . ? O1 Ni1 N5 94.82(10) . . ? N1 Ni1 N5 107.43(11) . . ? N3 Ni1 N5 82.77(11) . . ? N4 Ni1 N5 152.05(10) . . ? O1 Ni1 Ni2 60.25(6) . . ? N1 Ni1 Ni2 42.65(8) . . ? N3 Ni1 Ni2 125.25(8) . . ? N4 Ni1 Ni2 91.36(7) . . ? N5 Ni1 Ni2 116.28(8) . . ? O2 Ni2 N2 98.18(10) . . ? O2 Ni2 N6 176.78(11) . . ? N2 Ni2 N6 80.14(11) . . ? O2 Ni2 N7 98.21(10) . . ? N2 Ni2 N7 104.24(11) . . ? N6 Ni2 N7 84.89(11) . . ? O2 Ni2 N8 96.22(10) . . ? N2 Ni2 N8 127.46(12) . . ? N6 Ni2 N8 82.74(11) . . ? N7 Ni2 N8 123.20(12) . . ? O2 Ni2 Ni1 57.89(7) . . ? N2 Ni2 Ni1 40.76(7) . . ? N6 Ni2 Ni1 120.69(9) . . ? N7 Ni2 Ni1 102.20(7) . . ? N8 Ni2 Ni1 131.40(9) . . ? O5 Cl1 O6 108.4(2) . . ? O5 Cl1 O3 108.0(3) . . ? O6 Cl1 O3 113.0(3) . . ? O5 Cl1 O4 109.1(3) . . ? O6 Cl1 O4 110.2(2) . . ? O3 Cl1 O4 108.0(2) . . ? O9 Cl2 O7 112.2(6) . . ? O9 Cl2 O8 107.4(4) . . ? O7 Cl2 O8 107.3(3) . . ? O9 Cl2 O10 109.5(4) . . ? O7 Cl2 O10 106.8(3) . . ? O8 Cl2 O10 113.6(3) . . ? Ni1 O1 O2 116.39(11) . . ? Ni1 O1 O5 128.42(12) . . ? O2 O1 O5 94.93(12) . . ? Ni1 O1 H1O 120(4) . . ? O2 O1 H1O 104(4) . . ? O5 O1 H1O 10(4) . . ? Ni1 O1 H2O 114(2) . . ? O2 O1 H2O 4(2) . . ? O5 O1 H2O 94(2) . . ? H1O O1 H2O 102(5) . . ? H2O O2 Ni2 117(2) . . ? H2O O2 O1 4(2) . . ? Ni2 O2 O1 120.45(12) . . ? H2O O2 H2OO 115(5) . . ? Ni2 O2 H2OO 108(4) . . ? O1 O2 H2OO 111(4) . . ? H2O O2 H2O 0(6) . . ? Ni2 O2 H2O 117(2) . . ? O1 O2 H2O 4(2) . . ? H2OO O2 H2O 115(5) . . ? Cl1 O5 H1O 147.8(14) . . ? Cl1 O5 O1 149.8(3) . . ? H1O O5 O1 3.2(13) . . ? C3 N1 N2 108.1(2) . . ? C3 N1 Ni1 114.0(2) . . ? N2 N1 Ni1 136.1(2) . . ? C1 N2 N1 105.9(3) . . ? C1 N2 Ni2 114.5(2) . . ? N1 N2 Ni2 139.5(2) . . ? C7 N3 C5 112.1(3) . . ? C7 N3 C4 111.3(3) . . ? C5 N3 C4 110.5(3) . . ? C7 N3 Ni1 107.7(2) . . ? C5 N3 Ni1 107.0(2) . . ? C4 N3 Ni1 108.1(2) . . ? C11 N4 C9 111.2(3) . . ? C11 N4 C6 109.9(3) . . ? C9 N4 C6 109.0(3) . . ? C11 N4 Ni1 109.21(19) . . ? C9 N4 Ni1 114.4(2) . . ? C6 N4 Ni1 102.83(19) . . ? C15 N5 C13 110.2(3) . . ? C15 N5 C8 110.1(3) . . ? C13 N5 C8 111.1(3) . . ? C15 N5 Ni1 107.83(19) . . ? C13 N5 Ni1 110.5(2) . . ? C8 N5 Ni1 107.0(2) . . ? C17 N6 C20 111.8(3) . . ? C17 N6 C18 108.5(3) . . ? C20 N6 C18 112.1(3) . . ? C17 N6 Ni2 109.37(19) . . ? C20 N6 Ni2 108.7(2) . . ? C18 N6 Ni2 106.1(2) . . ? C22 N7 C19 116.2(3) . . ? C22 N7 C24 110.8(3) . . ? C19 N7 C24 102.2(3) . . ? C22 N7 Ni2 105.0(2) . . ? C19 N7 Ni2 105.5(2) . . ? C24 N7 Ni2 117.6(2) . . ? C28 N8 C21 108.7(3) . . ? C28 N8 C26 116.7(3) . . ? C21 N8 C26 106.6(3) . . ? C28 N8 Ni2 103.8(2) . . ? C21 N8 Ni2 104.1(2) . . ? C26 N8 Ni2 116.1(2) . . ? N2 C1 C2 111.7(3) . . ? N2 C1 C17 117.6(3) . . ? C2 C1 C17 130.6(3) . . ? C1 C2 C3 103.6(3) . . ? C1 C2 H2 121(2) . . ? C3 C2 H2 136(2) . . ? N1 C3 C2 110.7(3) . . ? N1 C3 C4 118.5(3) . . ? C2 C3 C4 130.8(3) . . ? N3 C4 C3 111.1(3) . . ? N3 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N3 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 109.8(3) . . ? N3 C5 H5A 104(4) . . ? C6 C5 H5A 112(4) . . ? N3 C5 H5B 106(3) . . ? C6 C5 H5B 109(3) . . ? H5A C5 H5B 115(5) . . ? N4 C6 C5 110.0(3) . . ? N4 C6 H6B 110(3) . . ? C5 C6 H6B 112(3) . . ? N4 C6 H6A 120(2) . . ? C5 C6 H6A 106(2) . . ? H6B C6 H6A 99(3) . . ? N3 C7 C8 110.0(3) . . ? N3 C7 H7A 112(3) . . ? C8 C7 H7A 113(3) . . ? N3 C7 H7B 114(2) . . ? C8 C7 H7B 101(2) . . ? H7A C7 H7B 107(3) . . ? N5 C8 C7 113.5(3) . . ? N5 C8 H8A 107(2) . . ? C7 C8 H8A 105(3) . . ? N5 C8 H8B 115(3) . . ? C7 C8 H8B 111(3) . . ? H8A C8 H8B 104(3) . . ? N4 C9 C10 115.4(3) . . ? N4 C9 H9A 102(5) . . ? C10 C9 H9A 108(5) . . ? N4 C9 H9B 104.2(19) . . ? C10 C9 H9B 114(2) . . ? H9A C9 H9B 113(5) . . ? C9 C10 H10A 109(3) . . ? C9 C10 H10B 109(3) . . ? H10A C10 H10B 111(4) . . ? C9 C10 H10C 112(3) . . ? H10A C10 H10C 107(4) . . ? H10B C10 H10C 108(4) . . ? N4 C11 C12 115.9(3) . . ? N4 C11 H11A 110(3) . . ? C12 C11 H11A 102(3) . . ? N4 C11 H11B 107(3) . . ? C12 C11 H11B 111(3) . . ? H11A C11 H11B 112(4) . . ? C11 C12 H12A 108(3) . . ? C11 C12 H12B 106(3) . . ? H12A C12 H12B 110(4) . . ? C11 C12 H12C 100(5) . . ? H12A C12 H12C 115(6) . . ? H12B C12 H12C 117(6) . . ? N5 C13 C14 114.6(3) . . ? N5 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? N5 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 C16 115.5(3) . . ? N5 C15 H15A 107(2) . . ? C16 C15 H15A 103(2) . . ? N5 C15 H15B 103(3) . . ? C16 C15 H15B 110(3) . . ? H15A C15 H15B 119(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 C1 109.2(3) . . ? N6 C17 H17A 113(2) . . ? C1 C17 H17A 110(2) . . ? N6 C17 H17B 112(2) . . ? C1 C17 H17B 109(2) . . ? H17A C17 H17B 103(3) . . ? N6 C18 C19 110.9(3) . . ? N6 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.0 . . ? N7 C19 C18 111.1(3) . . ? N7 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? N7 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N6 C20 C21 108.0(3) . . ? N6 C20 H20A 112(2) . . ? C21 C20 H20A 107(2) . . ? N6 C20 H20B 113(2) . . ? C21 C20 H20B 102(2) . . ? H20A C20 H20B 114(3) . . ? N8 C21 C20 112.2(3) . . ? N8 C21 H21A 115(4) . . ? C20 C21 H21A 103(4) . . ? N8 C21 H21B 108.3(19) . . ? C20 C21 H21B 107.5(19) . . ? H21A C21 H21B 111(4) . . ? N7 C22 C23 115.7(3) . . ? N7 C22 H22A 109(2) . . ? C23 C22 H22A 113(2) . . ? N7 C22 H22B 102(3) . . ? C23 C22 H22B 113(3) . . ? H22A C22 H22B 102(4) . . ? C22 C23 H23A 98(3) . . ? C22 C23 H23B 114(2) . . ? H23A C23 H23B 92(4) . . ? C22 C23 H23C 119(3) . . ? H23A C23 H23C 132(4) . . ? H23B C23 H23C 99(4) . . ? C25 C24 N7 115.5(3) . . ? C25 C24 H24A 105(2) . . ? N7 C24 H24A 109(2) . . ? C25 C24 H24B 117(3) . . ? N7 C24 H24B 99(3) . . ? H24A C24 H24B 112(4) . . ? C24 C25 H25A 107(3) . . ? C24 C25 H25B 105(4) . . ? H25A C25 H25B 121(5) . . ? C24 C25 H25C 110(3) . . ? H25A C25 H25C 106(4) . . ? H25B C25 H25C 108(5) . . ? C27 C26 N8 114.2(3) . . ? C27 C26 H26A 117(2) . . ? N8 C26 H26A 101(2) . . ? C27 C26 H26B 111(3) . . ? N8 C26 H26B 115(3) . . ? H26A C26 H26B 97(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C29 116.8(4) . . ? N8 C28 H28A 108.1 . . ? C29 C28 H28A 108.1 . . ? N8 C28 H28B 108.1 . . ? C29 C28 H28B 108.1 . . ? H28A C28 H28B 107.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.862 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.074 #================================================== data_mey _database_code_CSD 160995 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H122 B2 Cu2 N8 O5' _chemical_formula_weight 1496.62 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' 'B' 'B' 0.0013 0.0007 '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' 'Cu' 'Cu' 0.3201 1.2651 '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)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.740(3) _cell_length_b 26.747(5) _cell_length_c 18.024(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.44(2) _cell_angle_gamma 90.00 _cell_volume 8550(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 3 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Syntex R3' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 147 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9322 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8833 _reflns_number_gt 5397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3 (Siemens)' _computing_cell_refinement 'XDISK (Siemens)' _computing_data_reduction 'XDISK (Siemens)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0690P)^2^+15.5694P] 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 8833 _refine_ls_number_parameters 934 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.32318(5) 0.07674(3) 0.75912(5) 0.0485(3) Uani 1 1 d . . . Cu2 Cu 0.27810(5) -0.08458(3) 0.72958(5) 0.0548(3) Uani 1 1 d . . . O1 O 0.2433(3) 0.04245(19) 0.8060(3) 0.0610(16) Uani 1 1 d . . . O2 O 0.2019(3) -0.03624(18) 0.7497(3) 0.0695(16) Uani 1 1 d . . . N1 N 0.3759(4) 0.0148(2) 0.7236(3) 0.0430(15) Uani 1 1 d . . . N2 N 0.3605(3) -0.0346(2) 0.7104(3) 0.0449(16) Uani 1 1 d . . . N3 N 0.4120(3) 0.1109(2) 0.7102(3) 0.0478(16) Uani 1 1 d . . . N4 N 0.2576(4) 0.1074(2) 0.6528(3) 0.0547(17) Uani 1 1 d . . . N5 N 0.3406(4) 0.1295(2) 0.8454(3) 0.0515(17) Uani 1 1 d . . . N6 N 0.3632(4) -0.1343(2) 0.7086(4) 0.0577(18) Uani 1 1 d . . . N7 N 0.3027(4) -0.1110(2) 0.8534(4) 0.0648(19) Uani 1 1 d . . . N8 N 0.2116(4) -0.1331(3) 0.6619(4) 0.068(2) Uani 1 1 d . . . C1 C 0.4225(5) -0.0554(3) 0.6817(4) 0.048(2) Uani 1 1 d . . . C2 C 0.4786(5) -0.0199(3) 0.6754(4) 0.054(2) Uani 1 1 d . . . H2 H 0.5268 -0.0241 0.6571 0.07(3) Uiso 1 1 calc R . . C3 C 0.4462(5) 0.0236(3) 0.7026(4) 0.048(2) Uani 1 1 d . . . C4 C 0.4764(4) 0.0754(3) 0.7145(4) 0.059(2) Uani 1 1 d . . . H4A H 0.5016 0.0778 0.7627 0.069(5) Uiso 1 1 calc R . . H4B H 0.5125 0.0834 0.6768 0.069(5) Uiso 1 1 calc R . . C5 C 0.3920(5) 0.1216(3) 0.6317(4) 0.064(2) Uani 1 1 d . . . H5A H 0.4274 0.1457 0.6125 0.069(5) Uiso 1 1 calc R . . H5B H 0.3965 0.0911 0.6030 0.069(5) Uiso 1 1 calc R . . C6 C 0.3147(5) 0.1414(3) 0.6222(5) 0.071(3) Uani 1 1 d . . . H6A H 0.3037 0.1465 0.5697 0.069(5) Uiso 1 1 calc R . . H6B H 0.3116 0.1735 0.6468 0.069(5) Uiso 1 1 calc R . . C7 C 0.4292(5) 0.1581(3) 0.7504(4) 0.058(2) Uani 1 1 d . . . H7A H 0.3966 0.1846 0.7316 0.069(5) Uiso 1 1 calc R . . H7B H 0.4810 0.1677 0.7424 0.069(5) Uiso 1 1 calc R . . C8 C 0.4173(4) 0.1509(3) 0.8322(4) 0.059(2) Uani 1 1 d . . . H8A H 0.4556 0.1286 0.8526 0.069(5) Uiso 1 1 calc R . . H8B H 0.4222 0.1828 0.8574 0.069(5) Uiso 1 1 calc R . . C9 C 0.1862(5) 0.1354(3) 0.6608(5) 0.078(3) Uani 1 1 d . . . H9A H 0.1708 0.1483 0.6124 0.075(7) Uiso 1 1 calc R . . H9B H 0.1961 0.1639 0.6929 0.075(7) Uiso 1 1 calc R . . C10 C 0.1220(6) 0.1064(4) 0.6914(6) 0.114(4) Uani 1 1 d . . . H10A H 0.1078 0.0803 0.6574 0.162(10) Uiso 1 1 calc R . . H10B H 0.0798 0.1283 0.6981 0.162(10) Uiso 1 1 calc R . . H10C H 0.1371 0.0921 0.7382 0.162(10) Uiso 1 1 calc R . . C11 C 0.2462(5) 0.0627(3) 0.6057(4) 0.068(2) Uani 1 1 d . . . H11A H 0.2141 0.0396 0.6318 0.075(7) Uiso 1 1 calc R . . H11B H 0.2947 0.0466 0.6001 0.075(7) Uiso 1 1 calc R . . C12 C 0.2108(5) 0.0716(3) 0.5267(5) 0.091(3) Uani 1 1 d . . . H12A H 0.1607 0.0847 0.5310 0.162(10) Uiso 1 1 calc R . . H12B H 0.2087 0.0405 0.5001 0.162(10) Uiso 1 1 calc R . . H12C H 0.2411 0.0950 0.5003 0.162(10) Uiso 1 1 calc R . . C13 C 0.3386(5) 0.1066(3) 0.9200(4) 0.068(2) Uani 1 1 d . . . H13A H 0.2873 0.0962 0.9291 0.075(7) Uiso 1 1 calc R . . H13B H 0.3520 0.1319 0.9565 0.075(7) Uiso 1 1 calc R . . C14 C 0.3897(6) 0.0625(3) 0.9318(5) 0.089(3) Uani 1 1 d . . . H14A H 0.3852 0.0405 0.8898 0.162(10) Uiso 1 1 calc R . . H14B H 0.3757 0.0450 0.9758 0.162(10) Uiso 1 1 calc R . . H14C H 0.4409 0.0738 0.9372 0.162(10) Uiso 1 1 calc R . . C15 C 0.2816(5) 0.1692(3) 0.8385(4) 0.059(2) Uani 1 1 d . . . H15A H 0.2327 0.1532 0.8412 0.075(7) Uiso 1 1 calc R . . H15B H 0.2848 0.1839 0.7895 0.075(7) Uiso 1 1 calc R . . C16 C 0.2844(5) 0.2116(3) 0.8954(5) 0.091(3) Uani 1 1 d . . . H16A H 0.2782 0.1982 0.9442 0.162(10) Uiso 1 1 calc R . . H16B H 0.2446 0.2350 0.8844 0.162(10) Uiso 1 1 calc R . . H16C H 0.3321 0.2284 0.8932 0.162(10) Uiso 1 1 calc R . . C17 C 0.4177(5) -0.1089(3) 0.6606(4) 0.059(2) Uani 1 1 d . . . H17A H 0.4015 -0.1119 0.6090 0.069(5) Uiso 1 1 calc R . . H17B H 0.4669 -0.1244 0.6665 0.069(5) Uiso 1 1 calc R . . C18 C 0.4029(5) -0.1482(3) 0.7795(5) 0.069(3) Uani 1 1 d . . . H18A H 0.4386 -0.1221 0.7931 0.069(5) Uiso 1 1 calc R . . H18B H 0.4309 -0.1789 0.7724 0.069(5) Uiso 1 1 calc R . . C19 C 0.3490(5) -0.1553(3) 0.8412(5) 0.076(3) Uani 1 1 d . . . H19A H 0.3164 -0.1835 0.8296 0.069(5) Uiso 1 1 calc R . . H19B H 0.3772 -0.1631 0.8865 0.069(5) Uiso 1 1 calc R . . C20 C 0.3317(6) -0.1793(3) 0.6723(5) 0.079(3) Uani 1 1 d . . . H20A H 0.3143 -0.2026 0.7094 0.069(5) Uiso 1 1 calc R . . H20B H 0.3701 -0.1957 0.6438 0.069(5) Uiso 1 1 calc R . . C21 C 0.2680(6) -0.1639(3) 0.6228(6) 0.097(3) Uani 1 1 d . . . H21A H 0.2434 -0.1935 0.6026 0.069(5) Uiso 1 1 calc R . . H21B H 0.2874 -0.1448 0.5816 0.069(5) Uiso 1 1 calc R . . C22 C 0.2397(6) -0.1268(4) 0.9004(5) 0.097(3) Uani 1 1 d . . . H22A H 0.2602 -0.1419 0.9455 0.075(7) Uiso 1 1 calc R . . H22B H 0.2102 -0.1521 0.8742 0.075(7) Uiso 1 1 calc R . . C23 C 0.1871(7) -0.0828(5) 0.9215(7) 0.151(5) Uani 1 1 d . . . H23A H 0.2139 -0.0604 0.9543 0.162(10) Uiso 1 1 calc R . . H23B H 0.1436 -0.0957 0.9458 0.162(10) Uiso 1 1 calc R . . H23C H 0.1713 -0.0652 0.8774 0.162(10) Uiso 1 1 calc R . . C24 C 0.3473(5) -0.0693(3) 0.8875(5) 0.076(3) Uani 1 1 d . . . H24A H 0.3137 -0.0411 0.8937 0.075(7) Uiso 1 1 calc R . . H24B H 0.3851 -0.0592 0.8525 0.075(7) Uiso 1 1 calc R . . C25 C 0.3868(7) -0.0788(4) 0.9608(5) 0.123(4) Uani 1 1 d . . . H25A H 0.3502 -0.0805 0.9992 0.162(10) Uiso 1 1 calc R . . H25B H 0.4215 -0.0521 0.9715 0.162(10) Uiso 1 1 calc R . . H25C H 0.4138 -0.1098 0.9587 0.162(10) Uiso 1 1 calc R . . C26 C 0.1648(6) -0.1684(4) 0.7041(6) 0.103(3) Uani 1 1 d . . . H26A H 0.1444 -0.1932 0.6697 0.075(7) Uiso 1 1 calc R . . H26B H 0.1974 -0.1859 0.7394 0.075(7) Uiso 1 1 calc R . . C27 C 0.1027(7) -0.1470(4) 0.7441(7) 0.129(4) Uani 1 1 d . . . H27A H 0.1195 -0.1173 0.7694 0.162(10) Uiso 1 1 calc R . . H27B H 0.0851 -0.1708 0.7797 0.162(10) Uiso 1 1 calc R . . H27C H 0.0623 -0.1387 0.7098 0.162(10) Uiso 1 1 calc R . . C28 C 0.1639(6) -0.1070(4) 0.6063(5) 0.092(3) Uani 1 1 d . . . H28A H 0.1224 -0.0912 0.6314 0.075(7) Uiso 1 1 calc R . . H28B H 0.1426 -0.1315 0.5721 0.075(7) Uiso 1 1 calc R . . C29 C 0.2049(6) -0.0679(4) 0.5625(6) 0.111(4) Uani 1 1 d . . . H29A H 0.2331 -0.0466 0.5960 0.162(10) Uiso 1 1 calc R . . H29B H 0.1689 -0.0482 0.5346 0.162(10) Uiso 1 1 calc R . . H29C H 0.2386 -0.0839 0.5292 0.162(10) Uiso 1 1 calc R . . H100 H 0.225(5) 0.017(3) 0.797(5) 0.070 Uiso 1 1 d . . . B1 B 0.1727(5) -0.3430(3) 0.8086(5) 0.051(2) Uani 1 1 d . . . C30 C 0.2595(4) -0.3212(3) 0.8077(5) 0.051(2) Uani 1 1 d . . . C31 C 0.2956(5) -0.3070(3) 0.8747(5) 0.069(2) Uani 1 1 d . . . H31 H 0.2689 -0.3087 0.9184 0.071(4) Uiso 1 1 calc R . . C32 C 0.3691(6) -0.2905(3) 0.8778(6) 0.076(3) Uani 1 1 d . . . H32 H 0.3908 -0.2816 0.9234 0.071(4) Uiso 1 1 calc R . . C33 C 0.4104(5) -0.2871(3) 0.8159(7) 0.077(3) Uani 1 1 d . . . H33 H 0.4602 -0.2762 0.8185 0.071(4) Uiso 1 1 calc R . . C34 C 0.3766(6) -0.3001(3) 0.7485(6) 0.082(3) Uani 1 1 d . . . H34 H 0.4038 -0.2981 0.7052 0.071(4) Uiso 1 1 calc R . . C35 C 0.3027(5) -0.3161(3) 0.7456(5) 0.060(2) Uani 1 1 d . . . H35 H 0.2810 -0.3238 0.6995 0.071(4) Uiso 1 1 calc R . . C36 C 0.1236(4) -0.3127(3) 0.8697(4) 0.046(2) Uani 1 1 d . . . C37 C 0.0700(4) -0.3339(3) 0.9151(4) 0.052(2) Uani 1 1 d . . . H37 H 0.0605 -0.3680 0.9109 0.071(4) Uiso 1 1 calc R . . C38 C 0.0304(4) -0.3068(3) 0.9658(4) 0.060(2) Uani 1 1 d . . . H38 H -0.0053 -0.3229 0.9943 0.071(4) Uiso 1 1 calc R . . C39 C 0.0424(5) -0.2560(3) 0.9755(5) 0.064(2) Uani 1 1 d . . . H39 H 0.0164 -0.2380 1.0108 0.071(4) Uiso 1 1 calc R . . C40 C 0.0938(5) -0.2335(3) 0.9315(5) 0.067(2) Uani 1 1 d . . . H40 H 0.1025 -0.1993 0.9362 0.071(4) Uiso 1 1 calc R . . C41 C 0.1329(5) -0.2607(3) 0.8803(5) 0.064(2) Uani 1 1 d . . . H41 H 0.1673 -0.2440 0.8512 0.071(4) Uiso 1 1 calc R . . C42 C 0.1340(4) -0.3366(3) 0.7250(4) 0.050(2) Uani 1 1 d . . . C43 C 0.0886(5) -0.2970(3) 0.7046(4) 0.060(2) Uani 1 1 d . . . H43 H 0.0767 -0.2739 0.7410 0.071(4) Uiso 1 1 calc R . . C44 C 0.0593(5) -0.2891(3) 0.6336(5) 0.070(3) Uani 1 1 d . . . H44 H 0.0299 -0.2611 0.6234 0.071(4) Uiso 1 1 calc R . . C45 C 0.0739(5) -0.3226(4) 0.5790(5) 0.078(3) Uani 1 1 d . . . H45 H 0.0542 -0.3178 0.5312 0.071(4) Uiso 1 1 calc R . . C46 C 0.1179(6) -0.3632(4) 0.5953(5) 0.080(3) Uani 1 1 d . . . H46 H 0.1280 -0.3866 0.5586 0.071(4) Uiso 1 1 calc R . . C47 C 0.1476(5) -0.3696(3) 0.6673(5) 0.069(2) Uani 1 1 d . . . H47 H 0.1780 -0.3972 0.6770 0.071(4) Uiso 1 1 calc R . . C48 C 0.1758(5) -0.4027(3) 0.8307(4) 0.053(2) Uani 1 1 d . . . C49 C 0.2360(5) -0.4253(3) 0.8681(5) 0.082(3) Uani 1 1 d . . . H49 H 0.2781 -0.4063 0.8812 0.071(4) Uiso 1 1 calc R . . C50 C 0.2348(7) -0.4755(4) 0.8863(6) 0.115(4) Uani 1 1 d . . . H50 H 0.2765 -0.4891 0.9113 0.071(4) Uiso 1 1 calc R . . C51 C 0.1763(8) -0.5054(4) 0.8697(6) 0.102(4) Uani 1 1 d . . . H51 H 0.1767 -0.5392 0.8822 0.071(4) Uiso 1 1 calc R . . C52 C 0.1164(7) -0.4843(4) 0.8336(6) 0.101(4) Uani 1 1 d . . . H52 H 0.0747 -0.5040 0.8212 0.071(4) Uiso 1 1 calc R . . C53 C 0.1157(6) -0.4341(3) 0.8149(5) 0.073(3) Uani 1 1 d . . . H53 H 0.0731 -0.4210 0.7907 0.071(4) Uiso 1 1 calc R . . B2 B 0.6860(5) 0.1790(3) 0.6372(5) 0.052(2) Uani 1 1 d . . . C54 C 0.6465(4) 0.1894(3) 0.7161(4) 0.047(2) Uani 1 1 d . . . C55 C 0.6426(4) 0.1534(3) 0.7708(5) 0.061(2) Uani 1 1 d . . . H55 H 0.6572 0.1210 0.7593 0.071(4) Uiso 1 1 calc R . . C56 C 0.6186(5) 0.1629(4) 0.8412(5) 0.082(3) Uani 1 1 d . . . H56 H 0.6171 0.1370 0.8756 0.071(4) Uiso 1 1 calc R . . C57 C 0.5970(5) 0.2094(5) 0.8611(5) 0.079(3) Uani 1 1 d . . . H57 H 0.5824 0.2160 0.9094 0.071(4) Uiso 1 1 calc R . . C58 C 0.5969(5) 0.2466(4) 0.8091(5) 0.074(3) Uani 1 1 d . . . H58 H 0.5803 0.2785 0.8210 0.071(4) Uiso 1 1 calc R . . C59 C 0.6216(4) 0.2364(3) 0.7386(5) 0.059(2) Uani 1 1 d . . . H59 H 0.6218 0.2624 0.7042 0.071(4) Uiso 1 1 calc R . . C60 C 0.6606(5) 0.1237(3) 0.6048(4) 0.054(2) Uani 1 1 d . . . C61 C 0.6039(5) 0.1156(3) 0.5517(4) 0.067(2) Uani 1 1 d . . . H61 H 0.5795 0.1433 0.5314 0.071(4) Uiso 1 1 calc R . . C62 C 0.5817(6) 0.0688(4) 0.5274(5) 0.085(3) Uani 1 1 d . . . H62 H 0.5423 0.0658 0.4927 0.071(4) Uiso 1 1 calc R . . C63 C 0.6162(7) 0.0276(4) 0.5533(7) 0.095(4) Uani 1 1 d . . . H63 H 0.6026 -0.0038 0.5351 0.071(4) Uiso 1 1 calc R . . C64 C 0.6723(7) 0.0325(4) 0.6073(7) 0.094(3) Uani 1 1 d . . . H64 H 0.6950 0.0041 0.6279 0.071(4) Uiso 1 1 calc R . . C65 C 0.6948(5) 0.0797(4) 0.6309(5) 0.078(3) Uani 1 1 d . . . H65 H 0.7343 0.0823 0.6656 0.071(4) Uiso 1 1 calc R . . C66 C 0.7775(5) 0.1812(3) 0.6514(5) 0.058(2) Uani 1 1 d . . . C67 C 0.8117(5) 0.2079(3) 0.7088(5) 0.065(2) Uani 1 1 d . . . H67 H 0.7816 0.2234 0.7435 0.071(4) Uiso 1 1 calc R . . C68 C 0.8896(6) 0.2123(3) 0.7165(6) 0.085(3) Uani 1 1 d . . . H68 H 0.9104 0.2310 0.7554 0.071(4) Uiso 1 1 calc R . . C69 C 0.9348(6) 0.1900(4) 0.6686(8) 0.105(4) Uani 1 1 d . . . H69 H 0.9869 0.1927 0.6745 0.071(4) Uiso 1 1 calc R . . C70 C 0.9043(7) 0.1631(4) 0.6109(7) 0.105(4) Uani 1 1 d . . . H70 H 0.9353 0.1481 0.5765 0.071(4) Uiso 1 1 calc R . . C71 C 0.8274(6) 0.1583(4) 0.6043(5) 0.085(3) Uani 1 1 d . . . H71 H 0.8077 0.1385 0.5660 0.071(4) Uiso 1 1 calc R . . C72 C 0.6621(5) 0.2221(3) 0.5756(4) 0.058(2) Uani 1 1 d . . . C73 C 0.7134(6) 0.2463(3) 0.5307(5) 0.070(3) Uani 1 1 d . . . H73 H 0.7641 0.2377 0.5359 0.071(4) Uiso 1 1 calc R . . C74 C 0.6936(8) 0.2822(4) 0.4790(5) 0.093(4) Uani 1 1 d . . . H74 H 0.7304 0.2975 0.4510 0.071(4) Uiso 1 1 calc R . . C75 C 0.6199(10) 0.2950(4) 0.4695(6) 0.104(4) Uani 1 1 d . . . H75 H 0.6061 0.3186 0.4337 0.071(4) Uiso 1 1 calc R . . C76 C 0.5658(7) 0.2737(4) 0.5118(6) 0.093(3) Uani 1 1 d . . . H76 H 0.5156 0.2833 0.5059 0.071(4) Uiso 1 1 calc R . . C77 C 0.5866(6) 0.2373(3) 0.5643(5) 0.072(3) Uani 1 1 d . . . H77 H 0.5494 0.2227 0.5927 0.071(4) Uiso 1 1 calc R . . O3A O -0.0040(17) -0.0358(11) 0.7102(16) 0.257(15) Uiso 0.52(2) 1 d PD A 1 C78A C -0.0603(17) -0.0511(9) 0.7385(17) 0.24(2) Uiso 0.52(2) 1 d PD A 1 C79A C -0.1275(19) -0.0529(18) 0.694(3) 0.28(2) Uiso 0.52(2) 1 d PD A 1 C80A C -0.0537(19) -0.0662(12) 0.8134(16) 0.219(17) Uiso 0.52(2) 1 d PD A 1 O4A O 0.1264(9) 0.0947(5) 0.8888(9) 0.168(7) Uiso 0.70(2) 1 d PD B 1 C81A C 0.0955(14) 0.0869(9) 0.9459(15) 0.48(5) Uiso 0.70(2) 1 d PD B 1 C82A C 0.0634(15) 0.1289(10) 0.9812(15) 0.240(15) Uiso 0.70(2) 1 d PD B 1 C83A C 0.0922(19) 0.0364(10) 0.9709(18) 0.279(17) Uiso 0.70(2) 1 d PD B 1 O5A O 0.0936(11) -0.0645(8) 1.0960(10) 0.179(10) Uiso 0.519(18) 1 d PD C 1 C84A C 0.1272(13) -0.0947(9) 1.1347(14) 0.162(12) Uiso 0.519(18) 1 d PD C 1 C85A C 0.142(2) -0.0811(12) 1.2099(14) 0.191(14) Uiso 0.519(18) 1 d PD C 1 C86A C 0.149(3) -0.1407(14) 1.101(3) 0.44(5) Uiso 0.519(18) 1 d PD C 1 O3B O -0.0863(19) -0.0480(19) 0.664(3) 0.41(3) Uiso 0.48(2) 1 d PD A 2 C78B C -0.034(2) -0.0229(14) 0.6476(18) 0.55(7) Uiso 0.48(2) 1 d PD A 2 C79B C 0.0335(14) -0.0273(9) 0.6931(14) 0.104(9) Uiso 0.48(2) 1 d PD A 2 C80B C -0.041(3) 0.008(2) 0.584(3) 0.46(5) Uiso 0.48(2) 1 d PD A 2 O4B O 0.1613(19) 0.0765(15) 0.932(2) 0.208(19) Uiso 0.30(2) 1 d PD B 2 C81B C 0.0953(14) 0.0744(8) 0.9450(12) 0.045(9) Uiso 0.30(2) 1 d PD B 2 C82B C 0.064(2) 0.0266(15) 0.915(3) 0.20(3) Uiso 0.30(2) 1 d PD B 2 C83B C 0.076(2) 0.0872(17) 1.0206(17) 0.144(19) Uiso 0.30(2) 1 d PD B 2 O5B O 0.0460(17) -0.1395(15) 1.108(2) 0.40(3) Uiso 0.481(18) 1 d PD C 2 C84B C 0.0987(18) -0.1204(11) 1.1391(17) 0.353 Uiso 0.481(18) 1 d PD C 2 C85B C 0.083(3) -0.0848(15) 1.196(2) 0.24(2) Uiso 0.481(18) 1 d PD C 2 C86B C 0.1722(15) -0.1369(11) 1.1190(18) 0.147(13) Uiso 0.481(18) 1 d PD C 2 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 Cu1 0.0506(6) 0.0424(5) 0.0526(6) -0.0019(5) -0.0001(5) -0.0030(5) Cu2 0.0554(7) 0.0428(6) 0.0668(7) -0.0051(5) 0.0091(5) -0.0036(5) O1 0.059(4) 0.051(3) 0.074(4) -0.009(3) 0.005(3) -0.012(3) O2 0.053(4) 0.054(3) 0.102(4) -0.015(3) 0.008(3) -0.004(3) N1 0.040(4) 0.041(4) 0.048(4) 0.001(3) 0.000(3) -0.005(3) N2 0.049(4) 0.037(4) 0.050(4) 0.001(3) 0.003(3) 0.000(3) N3 0.051(4) 0.037(4) 0.055(4) 0.008(3) -0.007(3) 0.000(3) N4 0.057(5) 0.052(4) 0.055(4) -0.001(3) -0.008(4) 0.008(4) N5 0.060(5) 0.046(4) 0.049(4) -0.001(3) -0.006(3) 0.000(4) N6 0.071(5) 0.042(4) 0.061(4) 0.001(3) 0.007(4) 0.000(4) N7 0.078(5) 0.049(4) 0.069(5) 0.000(4) 0.016(4) 0.002(4) N8 0.078(5) 0.055(4) 0.069(5) 0.008(4) -0.010(5) -0.018(4) C1 0.046(5) 0.050(5) 0.046(5) 0.011(4) 0.009(4) 0.009(5) C2 0.047(6) 0.060(6) 0.057(5) 0.009(4) 0.014(5) 0.004(5) C3 0.047(6) 0.045(5) 0.053(5) 0.006(4) -0.003(4) -0.003(5) C4 0.056(6) 0.062(5) 0.060(5) 0.003(4) 0.000(4) -0.010(5) C5 0.075(7) 0.056(5) 0.060(6) 0.014(4) 0.000(5) -0.012(5) C6 0.095(8) 0.059(6) 0.057(6) 0.007(4) -0.011(5) 0.002(6) C7 0.066(6) 0.038(5) 0.069(6) 0.008(4) 0.001(5) -0.008(4) C8 0.058(6) 0.050(5) 0.067(6) -0.003(4) -0.015(5) -0.006(5) C9 0.078(7) 0.088(7) 0.067(6) -0.015(5) -0.026(6) 0.025(6) C10 0.075(8) 0.138(10) 0.130(10) 0.016(8) 0.011(7) 0.046(8) C11 0.085(7) 0.047(5) 0.070(6) 0.003(4) -0.013(5) -0.005(5) C12 0.116(8) 0.090(7) 0.065(6) -0.004(5) -0.031(6) 0.000(6) C13 0.088(7) 0.064(6) 0.053(6) -0.001(5) -0.010(5) -0.019(6) C14 0.122(8) 0.074(7) 0.070(6) 0.015(5) -0.016(6) -0.014(7) C15 0.065(6) 0.053(5) 0.061(5) -0.008(4) 0.000(5) -0.005(5) C16 0.103(8) 0.083(7) 0.086(7) -0.034(6) -0.008(6) 0.010(6) C17 0.073(6) 0.043(5) 0.062(5) 0.000(4) 0.022(5) -0.003(5) C18 0.066(6) 0.058(5) 0.084(7) 0.012(5) 0.020(6) 0.013(5) C19 0.098(7) 0.056(6) 0.075(6) 0.005(5) -0.002(6) 0.010(6) C20 0.090(7) 0.049(5) 0.098(7) -0.015(5) 0.009(6) -0.003(6) C21 0.125(10) 0.063(6) 0.102(8) -0.037(6) 0.008(8) -0.014(7) C22 0.113(9) 0.099(8) 0.080(7) 0.015(6) 0.032(7) 0.004(7) C23 0.161(12) 0.149(12) 0.146(12) 0.018(9) 0.078(10) 0.016(11) C24 0.105(8) 0.058(6) 0.065(6) 0.004(5) 0.005(6) 0.009(6) C25 0.206(13) 0.088(7) 0.074(7) -0.002(6) -0.035(8) 0.025(8) C26 0.099(9) 0.093(8) 0.117(9) -0.008(7) 0.003(8) -0.024(8) C27 0.117(10) 0.099(9) 0.170(12) 0.029(8) 0.012(10) -0.004(8) C28 0.107(8) 0.082(7) 0.086(7) -0.007(6) -0.009(7) -0.015(7) C29 0.152(11) 0.083(7) 0.098(8) 0.009(6) -0.025(8) -0.015(7) B1 0.053(6) 0.054(6) 0.048(6) 0.001(5) 0.003(5) 0.001(5) C30 0.053(5) 0.047(5) 0.055(5) 0.002(4) -0.006(5) 0.002(4) C31 0.058(7) 0.091(7) 0.060(6) -0.004(5) 0.003(5) -0.014(5) C32 0.069(8) 0.079(7) 0.078(7) -0.006(5) -0.018(6) -0.008(6) C33 0.042(6) 0.062(6) 0.126(9) 0.012(6) -0.008(7) -0.006(5) C34 0.066(8) 0.090(7) 0.090(8) 0.015(6) 0.020(7) 0.004(6) C35 0.054(6) 0.064(6) 0.062(6) 0.008(4) 0.006(5) -0.002(5) C36 0.044(5) 0.050(5) 0.044(5) 0.011(4) -0.010(4) -0.007(4) C37 0.051(5) 0.051(5) 0.054(5) 0.005(4) -0.001(5) -0.010(5) C38 0.049(6) 0.074(6) 0.059(6) 0.003(5) 0.002(5) -0.006(5) C39 0.056(6) 0.072(7) 0.064(6) -0.006(5) 0.006(5) 0.014(5) C40 0.076(7) 0.057(5) 0.069(6) -0.008(5) 0.012(6) 0.003(5) C41 0.068(6) 0.054(6) 0.069(6) 0.008(5) 0.013(5) -0.004(5) C42 0.050(5) 0.048(5) 0.054(5) 0.005(4) 0.004(4) -0.006(5) C43 0.064(6) 0.063(6) 0.054(6) 0.005(4) -0.009(5) -0.008(5) C44 0.077(7) 0.070(6) 0.063(6) 0.017(5) -0.014(6) -0.015(5) C45 0.074(7) 0.111(8) 0.049(6) 0.021(6) -0.017(5) -0.025(7) C46 0.085(8) 0.105(8) 0.051(6) -0.012(6) -0.003(6) -0.017(7) C47 0.066(6) 0.076(6) 0.064(6) 0.001(5) -0.001(5) -0.003(5) C48 0.059(6) 0.051(5) 0.048(5) -0.003(4) -0.004(4) -0.001(5) C49 0.075(7) 0.070(7) 0.101(7) 0.024(6) -0.015(6) -0.007(6) C50 0.124(10) 0.075(8) 0.144(11) 0.045(7) -0.031(8) 0.015(8) C51 0.149(12) 0.057(7) 0.101(9) 0.024(6) 0.009(9) -0.012(8) C52 0.134(11) 0.072(8) 0.096(8) 0.001(6) -0.027(8) -0.031(8) C53 0.092(7) 0.054(6) 0.071(6) 0.004(5) -0.015(5) -0.009(6) B2 0.046(6) 0.058(6) 0.051(6) -0.002(5) 0.002(5) -0.008(5) C54 0.036(5) 0.055(5) 0.051(5) 0.003(4) -0.001(4) -0.009(4) C55 0.054(6) 0.072(6) 0.058(6) -0.005(5) 0.002(5) -0.003(5) C56 0.076(7) 0.100(8) 0.069(7) 0.015(6) -0.001(6) 0.001(6) C57 0.066(7) 0.122(9) 0.049(6) -0.003(7) 0.009(5) -0.015(7) C58 0.070(7) 0.081(7) 0.071(7) -0.028(6) 0.009(6) -0.007(5) C59 0.056(6) 0.065(6) 0.057(6) 0.001(5) 0.005(5) -0.010(5) C60 0.052(6) 0.061(6) 0.048(5) -0.002(4) 0.010(5) -0.015(5) C61 0.074(7) 0.072(6) 0.054(6) 0.001(5) 0.008(5) -0.033(5) C62 0.102(9) 0.093(8) 0.061(6) -0.004(6) 0.003(6) -0.042(8) C63 0.117(10) 0.083(9) 0.089(9) -0.025(7) 0.039(8) -0.052(8) C64 0.110(9) 0.061(7) 0.113(9) 0.003(6) 0.028(8) -0.009(7) C65 0.076(7) 0.075(7) 0.084(7) -0.013(6) 0.014(5) -0.012(6) C66 0.055(6) 0.057(5) 0.064(6) -0.002(5) 0.015(5) -0.006(5) C67 0.064(7) 0.048(5) 0.082(7) -0.005(5) -0.013(5) -0.004(5) C68 0.058(8) 0.061(6) 0.135(10) -0.014(6) -0.026(7) 0.005(6) C69 0.047(7) 0.080(8) 0.188(13) 0.002(8) -0.019(9) -0.006(7) C70 0.065(9) 0.116(9) 0.137(11) -0.029(8) 0.037(7) -0.007(7) C71 0.073(8) 0.100(8) 0.083(7) -0.024(6) 0.004(6) -0.027(6) C72 0.069(6) 0.057(5) 0.047(5) -0.016(4) 0.004(5) -0.021(5) C73 0.098(8) 0.056(5) 0.055(6) -0.005(5) 0.000(6) -0.009(6) C74 0.162(12) 0.066(7) 0.050(7) -0.004(5) 0.009(8) -0.033(8) C75 0.180(14) 0.076(8) 0.055(7) -0.004(6) -0.027(9) -0.005(10) C76 0.121(10) 0.085(8) 0.072(7) -0.012(6) -0.039(7) 0.020(7) C77 0.079(8) 0.070(6) 0.068(6) -0.004(5) -0.017(6) -0.001(6) _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 Cu1 O1 1.904(5) . ? Cu1 N1 2.015(6) . ? Cu1 N3 2.040(6) . ? Cu1 N5 2.117(6) . ? Cu1 N4 2.364(6) . ? Cu1 Cu2 4.4182(15) . ? Cu2 O2 1.912(5) . ? Cu2 N2 2.018(6) . ? Cu2 N6 2.054(6) . ? Cu2 N8 2.119(7) . ? Cu2 N7 2.370(7) . ? O1 O2 2.442(7) . ? N1 C3 1.334(9) . ? N1 N2 1.368(7) . ? N2 C1 1.347(8) . ? N3 C5 1.478(9) . ? N3 C7 1.482(8) . ? N3 C4 1.486(9) . ? N4 C11 1.475(9) . ? N4 C6 1.479(9) . ? N4 C9 1.482(10) . ? N5 C13 1.478(9) . ? N5 C15 1.494(9) . ? N5 C8 1.500(9) . ? N6 C20 1.474(9) . ? N6 C17 1.479(9) . ? N6 C18 1.490(10) . ? N7 C19 1.463(9) . ? N7 C22 1.482(10) . ? N7 C24 1.492(10) . ? N8 C28 1.471(10) . ? N8 C26 1.481(11) . ? N8 C21 1.487(11) . ? C1 C2 1.382(10) . ? C1 C17 1.483(10) . ? C2 C3 1.393(10) . ? C3 C4 1.499(10) . ? C5 C6 1.476(10) . ? C7 C8 1.507(10) . ? C9 C10 1.496(12) . ? C11 C12 1.560(10) . ? C13 C14 1.498(11) . ? C15 C16 1.529(10) . ? C18 C19 1.495(10) . ? C20 C21 1.481(12) . ? C22 C23 1.556(13) . ? C24 C25 1.501(11) . ? C26 C27 1.451(13) . ? C28 C29 1.509(12) . ? B1 C36 1.637(11) . ? B1 C30 1.646(12) . ? B1 C42 1.648(11) . ? B1 C48 1.648(11) . ? C30 C35 1.379(10) . ? C30 C31 1.405(10) . ? C31 C32 1.376(11) . ? C32 C33 1.353(12) . ? C33 C34 1.385(12) . ? C34 C35 1.378(11) . ? C36 C37 1.392(9) . ? C36 C41 1.412(10) . ? C37 C38 1.373(10) . ? C38 C39 1.386(10) . ? C39 C40 1.364(10) . ? C40 C41 1.377(10) . ? C42 C43 1.376(10) . ? C42 C47 1.390(10) . ? C43 C44 1.384(10) . ? C44 C45 1.360(11) . ? C45 C46 1.366(12) . ? C46 C47 1.399(11) . ? C48 C53 1.381(10) . ? C48 C49 1.386(11) . ? C49 C50 1.383(12) . ? C50 C51 1.338(13) . ? C51 C52 1.356(13) . ? C52 C53 1.384(12) . ? B2 C54 1.627(11) . ? B2 C66 1.637(12) . ? B2 C60 1.648(11) . ? B2 C72 1.648(12) . ? C54 C55 1.381(10) . ? C54 C59 1.397(10) . ? C55 C56 1.371(11) . ? C56 C57 1.355(12) . ? C57 C58 1.366(12) . ? C58 C59 1.382(10) . ? C60 C61 1.386(10) . ? C60 C65 1.400(11) . ? C61 C62 1.382(11) . ? C62 C63 1.338(13) . ? C63 C64 1.381(14) . ? C64 C65 1.389(12) . ? C66 C71 1.384(11) . ? C66 C67 1.386(10) . ? C67 C68 1.391(11) . ? C68 C69 1.334(13) . ? C69 C70 1.365(13) . ? C70 C71 1.373(12) . ? C72 C73 1.393(11) . ? C72 C77 1.410(11) . ? C73 C74 1.376(12) . ? C74 C75 1.359(14) . ? C75 C76 1.366(14) . ? C76 C77 1.401(12) . ? O3A C78A 1.21(2) . ? C78A C80A 1.410(18) . ? C78A C79A 1.425(18) . ? O4A C81A 1.20(2) . ? C81A C82A 1.417(18) . ? C81A C83A 1.427(18) . ? O5A C84A 1.21(2) . ? C84A C85A 1.422(17) . ? C84A C86A 1.427(18) . ? O3B C78B 1.20(2) . ? C78B C80B 1.426(18) . ? C78B C79B 1.432(18) . ? O4B C81B 1.20(2) . ? C81B C83B 1.456(18) . ? C81B C82B 1.492(18) . ? O5B C84B 1.19(2) . ? C84B C86B 1.432(18) . ? C84B C85B 1.432(18) . ? 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 O1 Cu1 N1 95.8(2) . . ? O1 Cu1 N3 177.4(2) . . ? N1 Cu1 N3 82.1(2) . . ? O1 Cu1 N5 95.2(2) . . ? N1 Cu1 N5 136.1(2) . . ? N3 Cu1 N5 85.4(2) . . ? O1 Cu1 N4 99.8(2) . . ? N1 Cu1 N4 104.5(2) . . ? N3 Cu1 N4 82.2(2) . . ? N5 Cu1 N4 115.2(2) . . ? O1 Cu1 Cu2 56.53(16) . . ? N1 Cu1 Cu2 40.74(18) . . ? N3 Cu1 Cu2 121.65(16) . . ? N5 Cu1 Cu2 139.62(16) . . ? N4 Cu1 Cu2 99.02(15) . . ? O2 Cu2 N2 95.9(2) . . ? O2 Cu2 N6 177.7(2) . . ? N2 Cu2 N6 81.9(2) . . ? O2 Cu2 N8 97.9(3) . . ? N2 Cu2 N8 134.6(3) . . ? N6 Cu2 N8 84.2(3) . . ? O2 Cu2 N7 97.9(2) . . ? N2 Cu2 N7 104.0(2) . . ? N6 Cu2 N7 82.0(2) . . ? N8 Cu2 N7 116.5(3) . . ? O2 Cu2 Cu1 56.18(15) . . ? N2 Cu2 Cu1 40.84(18) . . ? N6 Cu2 Cu1 121.51(18) . . ? N8 Cu2 Cu1 139.8(2) . . ? N7 Cu2 Cu1 98.56(16) . . ? Cu1 O1 O2 116.7(3) . . ? Cu2 O2 O1 117.1(3) . . ? C3 N1 N2 107.8(6) . . ? C3 N1 Cu1 112.9(5) . . ? N2 N1 Cu1 139.2(5) . . ? C1 N2 N1 107.7(6) . . ? C1 N2 Cu2 113.2(5) . . ? N1 N2 Cu2 138.8(5) . . ? C5 N3 C7 110.2(5) . . ? C5 N3 C4 109.8(6) . . ? C7 N3 C4 111.6(6) . . ? C5 N3 Cu1 109.3(5) . . ? C7 N3 Cu1 108.7(4) . . ? C4 N3 Cu1 107.0(4) . . ? C11 N4 C6 111.6(6) . . ? C11 N4 C9 111.2(6) . . ? C6 N4 C9 108.6(7) . . ? C11 N4 Cu1 104.1(4) . . ? C6 N4 Cu1 100.8(4) . . ? C9 N4 Cu1 120.0(5) . . ? C13 N5 C15 109.7(6) . . ? C13 N5 C8 110.2(6) . . ? C15 N5 C8 110.5(6) . . ? C13 N5 Cu1 112.7(4) . . ? C15 N5 Cu1 108.9(4) . . ? C8 N5 Cu1 104.7(4) . . ? C20 N6 C17 111.2(6) . . ? C20 N6 C18 110.0(6) . . ? C17 N6 C18 108.3(6) . . ? C20 N6 Cu2 109.8(5) . . ? C17 N6 Cu2 107.7(4) . . ? C18 N6 Cu2 109.7(5) . . ? C19 N7 C22 106.8(7) . . ? C19 N7 C24 111.9(7) . . ? C22 N7 C24 112.2(7) . . ? C19 N7 Cu2 101.0(5) . . ? C22 N7 Cu2 120.0(6) . . ? C24 N7 Cu2 104.4(5) . . ? C28 N8 C26 109.4(8) . . ? C28 N8 C21 108.8(8) . . ? C26 N8 C21 106.4(7) . . ? C28 N8 Cu2 113.8(5) . . ? C26 N8 Cu2 114.0(6) . . ? C21 N8 Cu2 103.9(5) . . ? N2 C1 C2 110.2(7) . . ? N2 C1 C17 117.0(7) . . ? C2 C1 C17 132.7(8) . . ? C1 C2 C3 103.9(7) . . ? N1 C3 C2 110.5(7) . . ? N1 C3 C4 117.1(7) . . ? C2 C3 C4 132.3(8) . . ? N3 C4 C3 108.2(6) . . ? C6 C5 N3 112.3(7) . . ? C5 C6 N4 112.3(6) . . ? N3 C7 C8 109.8(6) . . ? N5 C8 C7 110.7(6) . . ? N4 C9 C10 115.7(8) . . ? N4 C11 C12 116.7(6) . . ? N5 C13 C14 115.2(7) . . ? N5 C15 C16 117.5(7) . . ? N6 C17 C1 109.1(6) . . ? N6 C18 C19 111.9(7) . . ? N7 C19 C18 112.4(7) . . ? N6 C20 C21 108.4(7) . . ? C20 C21 N8 112.4(8) . . ? N7 C22 C23 112.8(8) . . ? N7 C24 C25 117.9(7) . . ? C27 C26 N8 116.5(9) . . ? N8 C28 C29 114.1(8) . . ? C36 B1 C30 110.2(6) . . ? C36 B1 C42 110.4(6) . . ? C30 B1 C42 108.9(6) . . ? C36 B1 C48 109.4(6) . . ? C30 B1 C48 108.7(6) . . ? C42 B1 C48 109.4(6) . . ? C35 C30 C31 114.8(8) . . ? C35 C30 B1 125.6(7) . . ? C31 C30 B1 119.6(7) . . ? C32 C31 C30 122.1(8) . . ? C33 C32 C31 121.4(9) . . ? C32 C33 C34 118.3(9) . . ? C35 C34 C33 120.1(9) . . ? C34 C35 C30 123.2(8) . . ? C37 C36 C41 113.7(7) . . ? C37 C36 B1 125.2(7) . . ? C41 C36 B1 121.1(7) . . ? C38 C37 C36 123.0(7) . . ? C37 C38 C39 121.4(8) . . ? C40 C39 C38 117.6(8) . . ? C39 C40 C41 120.7(8) . . ? C40 C41 C36 123.5(8) . . ? C43 C42 C47 113.5(7) . . ? C43 C42 B1 123.5(7) . . ? C47 C42 B1 122.9(7) . . ? C42 C43 C44 124.7(8) . . ? C45 C44 C43 119.6(9) . . ? C44 C45 C46 119.1(9) . . ? C45 C46 C47 119.7(9) . . ? C42 C47 C46 123.3(9) . . ? C53 C48 C49 114.6(7) . . ? C53 C48 B1 121.2(7) . . ? C49 C48 B1 124.1(8) . . ? C50 C49 C48 121.5(9) . . ? C51 C50 C49 122.9(10) . . ? C50 C51 C52 116.9(10) . . ? C51 C52 C53 121.6(10) . . ? C48 C53 C52 122.5(9) . . ? C54 B2 C66 107.7(7) . . ? C54 B2 C60 110.0(6) . . ? C66 B2 C60 110.4(7) . . ? C54 B2 C72 111.1(7) . . ? C66 B2 C72 108.6(7) . . ? C60 B2 C72 109.0(6) . . ? C55 C54 C59 113.6(7) . . ? C55 C54 B2 122.4(7) . . ? C59 C54 B2 123.6(7) . . ? C56 C55 C54 123.6(8) . . ? C57 C56 C55 120.8(9) . . ? C56 C57 C58 118.8(9) . . ? C57 C58 C59 119.6(9) . . ? C58 C59 C54 123.6(8) . . ? C61 C60 C65 113.7(8) . . ? C61 C60 B2 124.9(8) . . ? C65 C60 B2 121.5(8) . . ? C62 C61 C60 123.8(9) . . ? C63 C62 C61 120.8(10) . . ? C62 C63 C64 118.9(10) . . ? C63 C64 C65 119.9(10) . . ? C64 C65 C60 122.9(9) . . ? C71 C66 C67 114.2(8) . . ? C71 C66 B2 122.4(8) . . ? C67 C66 B2 123.3(8) . . ? C66 C67 C68 122.3(9) . . ? C69 C68 C67 120.6(10) . . ? C68 C69 C70 119.7(10) . . ? C69 C70 C71 119.3(10) . . ? C70 C71 C66 123.7(9) . . ? C73 C72 C77 114.5(8) . . ? C73 C72 B2 123.7(8) . . ? C77 C72 B2 121.8(7) . . ? C74 C73 C72 123.9(10) . . ? C75 C74 C73 119.4(11) . . ? C74 C75 C76 120.7(12) . . ? C75 C76 C77 119.4(11) . . ? C76 C77 C72 122.1(10) . . ? O3A C78A C80A 116.8(17) . . ? O3A C78A C79A 117.5(17) . . ? C80A C78A C79A 126(3) . . ? O4A C81A C82A 116.6(17) . . ? O4A C81A C83A 117.3(17) . . ? C82A C81A C83A 126(2) . . ? O5A C84A C85A 117.1(16) . . ? O5A C84A C86A 117.7(17) . . ? C85A C84A C86A 125(2) . . ? O3B C78B C80B 118.2(18) . . ? O3B C78B C79B 117.0(17) . . ? C80B C78B C79B 125(3) . . ? O4B C81B C83B 115.6(18) . . ? O4B C81B C82B 108.9(16) . . ? C83B C81B C82B 116(2) . . ? O5B C84B C86B 117.3(17) . . ? O5B C84B C85B 117.2(17) . . ? C86B C84B C85B 125(3) . . ? _diffrn_measured_fraction_theta_max 0.587 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.371 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.060 #========END