# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1473 ## Supplementary data for m/s 9/01659G/DAP Gahan et al. ##[Ni3(tren)4(H2O)2][Cr(ox)3]2.10H2O data_1111lg22 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H88 Cr2 N16 Ni3 O32' _chemical_formula_weight 1537.35 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0430(10) _cell_length_b 24.151(3) _cell_length_c 15.318(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.619(7) _cell_angle_gamma 90.00 _cell_volume 3323.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method ? _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6220 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.1541 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5829 _reflns_number_observed 2493 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'XTAL3.2' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5829 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2008 _refine_ls_R_factor_obs 0.0775 _refine_ls_wR_factor_all 0.2746 _refine_ls_wR_factor_obs 0.2013 _refine_ls_goodness_of_fit_all 1.005 _refine_ls_goodness_of_fit_obs 1.160 _refine_ls_restrained_S_all 1.005 _refine_ls_restrained_S_obs 1.160 _refine_ls_shift/esd_max -0.057 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr -0.4507(2) 0.15796(7) 0.82594(11) 0.0402(5) Uani 1 d . . O1 O -0.2992(9) 0.1849(3) 0.9186(5) 0.051(2) Uani 1 d . . O2 O -0.5670(8) 0.1482(3) 0.9261(5) 0.052(2) Uani 1 d . . O3 O -0.3185(9) 0.1779(3) 0.7369(5) 0.048(2) Uani 1 d . . O4 O -0.5279(9) 0.2339(3) 0.8033(5) 0.049(2) Uani 1 d . . O5 O -0.3744(9) 0.0820(3) 0.8324(5) 0.051(2) Uani 1 d . . O6 O -0.6016(8) 0.1248(3) 0.7382(5) 0.044(2) Uani 1 d . . O7 O -0.2719(13) 0.2051(5) 1.0614(6) 0.094(4) Uani 1 d . . O8 O -0.5448(12) 0.1555(5) 1.0713(5) 0.084(3) Uani 1 d . . O9 O -0.2375(11) 0.2514(4) 0.6734(6) 0.072(3) Uani 1 d . . O10 O -0.4793(10) 0.3082(3) 0.7257(7) 0.076(3) Uani 1 d . . O11 O -0.4022(10) 0.0008(3) 0.7604(6) 0.071(3) Uani 1 d . . O12 O -0.6515(10) 0.0472(3) 0.6639(5) 0.063(2) Uani 1 d . . C1 C -0.3412(14) 0.1868(5) 0.9946(8) 0.054(3) Uani 1 d . . C2 C -0.5002(15) 0.1619(5) 1.0007(9) 0.052(3) Uani 1 d . . C3 C -0.3249(12) 0.2287(4) 0.7157(7) 0.041(3) Uani 1 d . . C4 C -0.4547(13) 0.2606(5) 0.7503(8) 0.048(3) Uani 1 d . . C5 C -0.4373(14) 0.0491(5) 0.7737(8) 0.051(3) Uani 1 d . . C6 C -0.5760(13) 0.0747(4) 0.7195(7) 0.043(3) Uani 1 d . . Ni1 Ni 0.0000 0.0000 0.0000 0.0312(5) Uani 1 d S . N11 N 0.0561(9) -0.0770(3) 0.0643(5) 0.036(2) Uani 1 d . . H11C H 0.0194(9) -0.1048(3) 0.0291(5) 0.044 Uiso 1 d R . H11D H 0.1558(9) -0.0806(3) 0.0726(5) 0.044 Uiso 1 d R . N12 N -0.1962(9) -0.0321(3) -0.0679(5) 0.035(2) Uani 1 d . . H12C H -0.1892(9) -0.0692(3) -0.0721(5) 0.042 Uiso 1 d R . H12D H -0.2106(9) -0.0179(3) -0.1225(5) 0.042 Uiso 1 d R . N13 N -0.1356(9) 0.0053(3) 0.1063(5) 0.036(2) Uani 1 d . . N14 N -0.2726(11) 0.1298(4) 0.2284(6) 0.054(3) Uani 1 d . . H14C H -0.3286(11) 0.1420(4) 0.1798(6) 0.064 Uiso 1 d R . H14D H -0.1866(11) 0.1489(4) 0.2332(6) 0.064 Uiso 1 d R . C11 C -0.0542(14) -0.0267(5) 0.1794(7) 0.052(3) Uani 1 d . . H11A H -0.1162(14) -0.0315(5) 0.2265(7) 0.062 Uiso 1 d R . H11B H 0.0333(14) -0.0058(5) 0.2025(7) 0.062 Uiso 1 d R . C12 C -0.0039(14) -0.0818(5) 0.1484(8) 0.054(3) Uani 1 d . . H12A H -0.0886(14) -0.1067(5) 0.1429(8) 0.064 Uiso 1 d R . H12B H 0.0719(14) -0.0972(5) 0.1916(8) 0.064 Uiso 1 d R . C13 C -0.1565(14) 0.0628(4) 0.1324(7) 0.047(3) Uani 1 d . . H13C H -0.2108(14) 0.0825(4) 0.0837(7) 0.057 Uiso 1 d R . H13D H -0.0587(14) 0.0796(4) 0.1435(7) 0.057 Uiso 1 d R . C14 C -0.2351(16) 0.0718(4) 0.2155(8) 0.060(4) Uani 1 d . . H14A H -0.3268(16) 0.0506(4) 0.2090(8) 0.072 Uiso 1 d R . H14B H -0.1733(16) 0.0582(4) 0.2669(8) 0.072 Uiso 1 d R . C15 C -0.2809(13) -0.0233(6) 0.0778(7) 0.059(3) Uani 1 d . . H15A H -0.3578(13) -0.0072(6) 0.1091(7) 0.071 Uiso 1 d R . H15B H -0.2729(13) -0.0623(6) 0.0933(7) 0.071 Uiso 1 d R . C16 C -0.3204(11) -0.0173(5) -0.0187(7) 0.050(3) Uani 1 d . . H16A H -0.4041(11) -0.0415(5) -0.0360(7) 0.060 Uiso 1 d R . H16B H -0.3513(11) 0.0205(5) -0.0326(7) 0.060 Uiso 1 d R . Ni2 Ni -0.3802(2) 0.14895(5) 0.33530(9) 0.0409(4) Uani 1 d . . N21 N -0.3907(12) 0.2344(4) 0.3098(7) 0.063(3) Uani 1 d . . H21C H -0.2981(12) 0.2479(4) 0.3093(7) 0.076 Uiso 1 d R . H21D H -0.4410(12) 0.2400(4) 0.2563(7) 0.076 Uiso 1 d R . N22 N -0.3583(13) 0.0731(4) 0.4041(6) 0.060(3) Uani 1 d . . H22C H -0.3950(13) 0.0452(4) 0.3691(6) 0.072 Uiso 1 d R . H22D H -0.2611(13) 0.0663(4) 0.4203(6) 0.072 Uiso 1 d R . N23 N -0.4985(12) 0.1712(4) 0.4392(6) 0.049(2) Uani 1 d . . O13 O -0.1556(10) 0.1676(4) 0.4050(6) 0.082(3) Uani 1 d . . H13A H -0.1657(10) 0.1793(4) 0.4639(6) 0.099 Uiso 1 d R . H13B H -0.1105(10) 0.1966(4) 0.3745(6) 0.099 Uiso 1 d R . N24 N -0.5905(13) 0.1313(5) 0.2698(7) 0.069(3) Uani 1 d . . H24C H -0.6237(13) 0.1601(5) 0.2358(7) 0.083 Uiso 1 d R . H24D H -0.5868(13) 0.1012(5) 0.2355(7) 0.083 Uiso 1 d R . C21 C -0.4609(16) 0.2295(5) 0.4585(9) 0.067(4) Uani 1 d . . H21A H -0.3614(16) 0.2317(5) 0.4896(9) 0.080 Uiso 1 d R . H21B H -0.5296(16) 0.2446(5) 0.4965(9) 0.080 Uiso 1 d R . C22 C -0.4648(18) 0.2639(5) 0.3762(9) 0.075(4) Uani 1 d . . H22A H -0.5678(18) 0.2709(5) 0.3538(9) 0.090 Uiso 1 d R . H22B H -0.4164(18) 0.2992(5) 0.3895(9) 0.090 Uiso 1 d R . C23 C -0.4468(18) 0.1338(6) 0.5142(8) 0.072(4) Uani 1 d . . H23A H -0.5189(18) 0.1352(6) 0.5564(8) 0.086 Uiso 1 d R . H23B H -0.3520(18) 0.1465(6) 0.5435(8) 0.086 Uiso 1 d R . C24 C -0.4310(19) 0.0758(6) 0.4840(9) 0.077(4) Uani 1 d . . H24A H -0.3767(19) 0.0545(6) 0.5309(9) 0.092 Uiso 1 d R . H24B H -0.5290(19) 0.0594(6) 0.4708(9) 0.092 Uiso 1 d R . C25 C -0.6604(16) 0.1652(6) 0.4100(9) 0.073(4) Uani 1 d . . H25A H -0.7119(16) 0.1536(6) 0.4591(9) 0.088 Uiso 1 d R . H25B H -0.7012(16) 0.2006(6) 0.3892(9) 0.088 Uiso 1 d R . C26 C -0.6912(16) 0.1220(7) 0.3368(10) 0.083(5) Uani 1 d . . H26A H -0.6727(16) 0.0853(7) 0.3612(10) 0.099 Uiso 1 d R . H26B H -0.7940(16) 0.1235(7) 0.3105(10) 0.099 Uiso 1 d R . O14 O -0.8615(10) 0.1532(3) 1.0647(6) 0.069(3) Uani 1 d . . O15A O -0.2933(22) 0.3023(8) 1.1349(13) 0.063(6) Uiso 0.416(13) d P . O15B O -0.0630(25) 0.1819(9) 0.5819(14) 0.069(7) Uiso 0.416(13) d P . O15C O 0.0199(54) 0.2076(19) 0.6240(31) 0.054(20) Uiso 0.17(3) d P . O16A O 0.0659(28) 0.0825(11) 0.5987(16) 0.097(8) Uiso 0.427(10) d P . O16B O 0.0045(35) 0.0573(13) 0.4244(19) 0.119(10) Uiso 0.427(10) d P . O16C O 0.1482(51) -0.0081(19) 0.3758(29) 0.041(17) Uiso 0.15(2) d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0448(11) 0.0338(10) 0.0412(10) 0.0018(8) 0.0015(8) -0.0001(8) O1 0.052(5) 0.057(5) 0.044(5) 0.000(4) 0.003(4) -0.019(4) O2 0.049(5) 0.059(5) 0.051(5) -0.002(4) 0.015(4) -0.009(4) O3 0.066(5) 0.033(4) 0.046(4) 0.005(3) 0.017(4) 0.003(4) O4 0.060(5) 0.034(4) 0.054(5) 0.005(4) 0.013(4) 0.008(4) O5 0.060(5) 0.036(4) 0.051(5) 0.010(4) -0.013(4) 0.002(4) O6 0.047(5) 0.036(4) 0.046(4) -0.002(3) -0.012(4) 0.005(4) O7 0.112(9) 0.123(9) 0.048(6) -0.018(6) 0.006(6) -0.047(7) O8 0.100(8) 0.116(8) 0.041(5) -0.006(5) 0.022(5) -0.021(7) O9 0.083(7) 0.062(6) 0.074(6) 0.029(5) 0.031(5) 0.007(5) O10 0.068(6) 0.044(5) 0.116(8) 0.026(5) 0.014(6) 0.018(5) O11 0.091(7) 0.041(5) 0.077(6) -0.005(5) -0.007(5) 0.020(5) O12 0.075(6) 0.049(5) 0.061(5) -0.016(4) -0.014(5) 0.004(4) C1 0.061(9) 0.050(7) 0.052(8) 0.001(6) 0.006(7) 0.004(7) C2 0.055(7) 0.050(7) 0.050(7) -0.004(6) 0.005(6) -0.009(6) C3 0.043(7) 0.038(6) 0.043(6) 0.012(5) 0.006(5) -0.003(5) C4 0.043(7) 0.033(6) 0.064(8) -0.001(6) -0.015(6) 0.011(5) C5 0.057(8) 0.049(7) 0.047(7) 0.010(6) 0.001(6) 0.009(6) C6 0.057(8) 0.039(6) 0.033(6) 0.000(5) 0.010(5) -0.003(6) Ni1 0.0312(10) 0.0242(9) 0.0382(10) -0.0021(8) 0.0039(8) 0.0024(8) N11 0.038(5) 0.025(4) 0.045(5) -0.004(4) 0.004(4) 0.001(4) N12 0.032(5) 0.027(4) 0.045(5) -0.005(4) 0.000(4) -0.002(4) N13 0.030(5) 0.036(5) 0.043(5) -0.003(4) 0.003(4) 0.002(4) N14 0.058(7) 0.052(6) 0.053(6) -0.009(5) 0.018(5) 0.004(5) C11 0.066(8) 0.057(7) 0.037(6) 0.013(5) 0.026(6) 0.017(6) C12 0.058(8) 0.041(6) 0.066(8) 0.011(6) 0.026(6) 0.015(6) C13 0.057(8) 0.042(6) 0.046(6) -0.018(5) 0.016(6) 0.008(6) C14 0.092(10) 0.036(6) 0.061(8) -0.006(6) 0.039(7) 0.019(6) C15 0.046(8) 0.084(9) 0.050(7) -0.012(7) 0.013(6) 0.000(7) C16 0.016(6) 0.069(8) 0.065(8) 0.002(6) 0.003(5) 0.002(5) Ni2 0.0529(10) 0.0327(7) 0.0380(8) -0.0034(6) 0.0088(6) 0.0039(7) N21 0.067(8) 0.052(6) 0.074(7) 0.011(5) 0.021(6) 0.004(6) N22 0.092(9) 0.034(5) 0.054(6) 0.001(5) 0.012(6) 0.004(5) N23 0.071(7) 0.042(5) 0.038(5) -0.009(4) 0.021(5) 0.004(5) O13 0.072(7) 0.115(8) 0.062(6) -0.001(5) 0.015(5) -0.013(6) N24 0.078(8) 0.074(8) 0.053(6) -0.006(6) 0.002(6) -0.004(6) C21 0.081(10) 0.049(7) 0.071(9) -0.028(7) 0.004(8) 0.005(7) C22 0.104(12) 0.042(7) 0.079(10) -0.003(7) 0.007(9) 0.011(8) C23 0.095(12) 0.074(10) 0.050(8) -0.002(7) 0.020(8) 0.006(8) C24 0.119(13) 0.059(9) 0.055(8) 0.008(7) 0.025(8) -0.001(9) C25 0.071(10) 0.078(10) 0.074(10) -0.013(8) 0.026(8) 0.023(8) C26 0.053(9) 0.094(11) 0.098(12) -0.033(10) -0.004(9) 0.001(8) O14 0.079(6) 0.042(5) 0.082(6) -0.011(4) -0.007(5) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O5 1.959(7) . ? Cr1 O1 1.966(7) . ? Cr1 O6 1.971(7) . ? Cr1 O2 1.972(8) . ? Cr1 O3 1.975(7) . ? Cr1 O4 1.980(7) . ? O1 C1 1.267(14) . ? O2 C2 1.273(14) . ? O3 C3 1.268(12) . ? O4 C4 1.280(14) . ? O5 C5 1.283(14) . ? O6 C6 1.272(12) . ? O7 C1 1.220(14) . ? O8 C2 1.208(14) . ? O9 C3 1.209(12) . ? O10 C4 1.221(13) . ? O11 C5 1.231(13) . ? O12 C6 1.224(12) . ? C1 C2 1.57(2) . ? C3 C4 1.55(2) . ? C5 C6 1.55(2) . ? Ni1 N12 2.099(7) . ? Ni1 N12 2.099(7) 3 ? Ni1 N11 2.139(8) 3 ? Ni1 N11 2.139(8) . ? Ni1 N13 2.152(8) 3 ? Ni1 N13 2.152(8) . ? N11 C12 1.458(13) . ? N12 C16 1.468(13) . ? N13 C13 1.462(12) . ? N13 C11 1.485(13) . ? N13 C15 1.505(14) . ? N14 C14 1.459(13) . ? N14 Ni2 2.052(9) . ? C11 C12 1.501(15) . ? C13 C14 1.543(14) . ? C15 C16 1.487(15) . ? Ni2 N23 2.088(9) . ? Ni2 N24 2.089(11) . ? Ni2 N21 2.100(10) . ? Ni2 N22 2.111(9) . ? Ni2 O13 2.229(9) . ? N21 C22 1.47(2) . ? N22 C24 1.46(2) . ? N23 C21 1.470(14) . ? N23 C25 1.49(2) . ? N23 C23 1.49(2) . ? N24 C26 1.47(2) . ? C21 C22 1.51(2) . ? C23 C24 1.49(2) . ? C25 C26 1.53(2) . ? O15A O15C 1.69(5) 4_566 ? O15B O15C 1.12(5) . ? O15C O15A 1.69(5) 4_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cr1 O1 93.5(3) . . ? O5 Cr1 O6 82.3(3) . . ? O1 Cr1 O6 175.1(3) . . ? O5 Cr1 O2 93.7(3) . . ? O1 Cr1 O2 82.4(3) . . ? O6 Cr1 O2 95.3(3) . . ? O5 Cr1 O3 91.5(3) . . ? O1 Cr1 O3 89.5(3) . . ? O6 Cr1 O3 93.2(3) . . ? O2 Cr1 O3 170.6(3) . . ? O5 Cr1 O4 172.9(3) . . ? O1 Cr1 O4 91.2(3) . . ? O6 Cr1 O4 93.1(3) . . ? O2 Cr1 O4 92.2(3) . . ? O3 Cr1 O4 83.2(3) . . ? C1 O1 Cr1 114.7(8) . . ? C2 O2 Cr1 115.2(8) . . ? C3 O3 Cr1 113.6(7) . . ? C4 O4 Cr1 112.3(7) . . ? C5 O5 Cr1 114.8(7) . . ? C6 O6 Cr1 114.2(7) . . ? O7 C1 O1 127.2(12) . . ? O7 C1 C2 118.4(12) . . ? O1 C1 C2 114.4(11) . . ? O8 C2 O2 126.7(12) . . ? O8 C2 C1 120.3(12) . . ? O2 C2 C1 113.0(11) . . ? O9 C3 O3 124.2(11) . . ? O9 C3 C4 121.8(10) . . ? O3 C3 C4 114.1(9) . . ? O10 C4 O4 125.5(11) . . ? O10 C4 C3 118.8(12) . . ? O4 C4 C3 115.8(9) . . ? O11 C5 O5 126.8(11) . . ? O11 C5 C6 119.8(11) . . ? O5 C5 C6 113.3(10) . . ? O12 C6 O6 124.8(11) . . ? O12 C6 C5 120.6(10) . . ? O6 C6 C5 114.6(10) . . ? N12 Ni1 N12 180.0 . 3 ? N12 Ni1 N11 87.2(3) . 3 ? N12 Ni1 N11 92.8(3) 3 3 ? N12 Ni1 N11 92.8(3) . . ? N12 Ni1 N11 87.2(3) 3 . ? N11 Ni1 N11 180.0 3 . ? N12 Ni1 N13 97.2(3) . 3 ? N12 Ni1 N13 82.8(3) 3 3 ? N11 Ni1 N13 80.1(3) 3 3 ? N11 Ni1 N13 99.9(3) . 3 ? N12 Ni1 N13 82.8(3) . . ? N12 Ni1 N13 97.2(3) 3 . ? N11 Ni1 N13 99.9(3) 3 . ? N11 Ni1 N13 80.1(3) . . ? N13 Ni1 N13 180.0 3 . ? C12 N11 Ni1 112.5(6) . . ? C16 N12 Ni1 107.9(6) . . ? C13 N13 C11 110.9(8) . . ? C13 N13 C15 112.3(9) . . ? C11 N13 C15 108.7(9) . . ? C13 N13 Ni1 111.5(6) . . ? C11 N13 Ni1 105.3(6) . . ? C15 N13 Ni1 107.9(6) . . ? C14 N14 Ni2 117.6(7) . . ? N13 C11 C12 111.4(9) . . ? N11 C12 C11 111.5(9) . . ? N13 C13 C14 116.5(9) . . ? N14 C14 C13 112.6(9) . . ? C16 C15 N13 110.1(10) . . ? N12 C16 C15 112.1(9) . . ? N14 Ni2 N23 176.6(4) . . ? N14 Ni2 N24 93.4(4) . . ? N23 Ni2 N24 84.3(4) . . ? N14 Ni2 N21 95.1(4) . . ? N23 Ni2 N21 82.7(4) . . ? N24 Ni2 N21 95.3(4) . . ? N14 Ni2 N22 100.2(4) . . ? N23 Ni2 N22 82.5(4) . . ? N24 Ni2 N22 95.2(4) . . ? N21 Ni2 N22 160.9(4) . . ? N14 Ni2 O13 86.4(4) . . ? N23 Ni2 O13 95.8(4) . . ? N24 Ni2 O13 179.8(3) . . ? N21 Ni2 O13 84.8(4) . . ? N22 Ni2 O13 84.7(4) . . ? C22 N21 Ni2 111.3(8) . . ? C24 N22 Ni2 110.8(8) . . ? C21 N23 C25 110.6(10) . . ? C21 N23 C23 112.3(10) . . ? C25 N23 C23 112.4(10) . . ? C21 N23 Ni2 105.9(7) . . ? C25 N23 Ni2 108.6(7) . . ? C23 N23 Ni2 106.7(7) . . ? C26 N24 Ni2 107.5(8) . . ? N23 C21 C22 112.1(10) . . ? N21 C22 C21 110.2(10) . . ? C24 C23 N23 111.3(10) . . ? N22 C24 C23 111.9(11) . . ? N23 C25 C26 112.1(10) . . ? N24 C26 C25 109.5(12) . . ? O15B O15C O15A 125.0(39) . 4_665 ? _refine_diff_density_max 0.952 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.139 #===END ## {[Ni2(tren)3][ClO4]4.H2O}n data_1162lg27 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H56 Cl4 N12 Ni2 O17' _chemical_formula_weight 971.97 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.784(3) _cell_length_b 23.414(2) _cell_length_c 10.310(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.060(10) _cell_angle_gamma 90.00 _cell_volume 2016.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method ? _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 125 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3893 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.1439 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3647 _reflns_number_observed 1705 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'XTAL3.2' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1770P)^2^+4.4414P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3647 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1989 _refine_ls_R_factor_obs 0.0900 _refine_ls_wR_factor_all 0.3188 _refine_ls_wR_factor_obs 0.2421 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.197 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.197 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.1975(2) 0.2500 0.0356(2) 0.0303(6) Uani 1 d S . N11 N 0.0540(26) 0.2948(10) -0.1321(20) 0.040(5) Uani 0.50 d P . N12 N 0.3899(24) 0.2769(8) -0.0409(23) 0.055(6) Uani 0.50 d P . H12A H 0.4704(24) 0.2929(8) 0.0257(23) 0.065 Uiso 0.50 d PR . H12B H 0.4286(24) 0.2500(8) -0.0737(23) 0.065 Uiso 1 d SR . N13 N -0.0190(17) 0.2500 0.0830(15) 0.058(4) Uani 1 d S . H13A H -0.0252(17) 0.2187 0.1317(15) 0.069 Uiso 0.50 d PR . H13B H -0.0252(17) 0.2813 0.1317(15) 0.069 Uiso 0.50 d PR . N14 N 0.1442(30) 0.1775(12) -0.1101(29) 0.042(7) Uani 0.50 d P . H14A H 0.2249(30) 0.1520(12) -0.0911(29) 0.050 Uiso 0.50 d PR . H14B H 0.0552(30) 0.1596(12) -0.1057(29) 0.050 Uiso 0.50 d PR . C11 C 0.1594(59) 0.3419(17) -0.1511(42) 0.072(14) Uani 0.50 d P . H11A H 0.1069(59) 0.3654(17) -0.2297(42) 0.087 Uiso 0.50 d PR . H11B H 0.1799(59) 0.3653(17) -0.0698(42) 0.087 Uiso 0.50 d PR . C12 C 0.3232(37) 0.3189(12) -0.1513(27) 0.059(7) Uani 0.50 d P . H12C H 0.3982(37) 0.3500(12) -0.1439(27) 0.071 Uiso 0.50 d PR . H12D H 0.3050(37) 0.3007(12) -0.2394(27) 0.071 Uiso 0.50 d PR . C13 C -0.0865(26) 0.3150(11) -0.0991(28) 0.053(7) Uani 0.50 d P . H13C H -0.1694(26) 0.3267(11) -0.1812(28) 0.064 Uiso 0.50 d PR . H13D H -0.0672(26) 0.3454(11) -0.0322(28) 0.064 Uiso 0.50 d PR . C14 C -0.1507(28) 0.2500 -0.0264(29) 0.127(14) Uani 1 d S . H14C H -0.2571(28) 0.2500 -0.0169(29) 0.153 Uiso 1 d SR . H14D H -0.1425(28) 0.2173 -0.0815(29) 0.153 Uiso 0.50 d PR . C15 C 0.0101(27) 0.2500 -0.2534(19) 0.073(7) Uani 1 d S . H15A H -0.0929(27) 0.2346 -0.2548(19) 0.088 Uiso 0.50 d PR . H15B H -0.0042(27) 0.2700 -0.3387(19) 0.088 Uiso 0.50 d PR . C16 C 0.1034(46) 0.2043(12) -0.2436(35) 0.086(12) Uani 0.50 d P . H16A H 0.0593(46) 0.1759(12) -0.3135(35) 0.103 Uiso 0.50 d PR . H16B H 0.2033(46) 0.2183(12) -0.2533(35) 0.103 Uiso 0.50 d PR . Ni2 Ni 0.5000 0.5000 0.5000 0.0281(5) Uani 1 d S . N21A N 0.3121(21) 0.4468(8) 0.3726(18) 0.035(4) Uani 0.50 d P 1 N22A N 0.3453(29) 0.3076(11) 0.1883(27) 0.049(7) Uani 0.50 d P 1 H22A H 0.3910(29) 0.2870(11) 0.2640(27) 0.059 Uiso 0.50 d PR 1 H22B H 0.4248(29) 0.3208(11) 0.1586(27) 0.059 Uiso 0.50 d PR 1 N23A N 0.3504(20) 0.5659(8) 0.3867(20) 0.037(4) Uani 0.50 d P 1 H23A H 0.3274(20) 0.5908(8) 0.4446(20) 0.044 Uiso 0.50 d PR 1 H23B H 0.4024(20) 0.5849(8) 0.3373(20) 0.044 Uiso 0.50 d PR 1 N24A N 0.3633(22) 0.4923(9) 0.6333(18) 0.039(4) Uani 0.50 d P 1 H24A H 0.4275(22) 0.4924(9) 0.7204(18) 0.046 Uiso 0.50 d PR 1 H24B H 0.2937(22) 0.5215(9) 0.6217(18) 0.046 Uiso 0.50 d PR 1 C21A C 0.3720(31) 0.3953(11) 0.3326(25) 0.025(6) Uiso 0.50 d P 1 H21A H 0.4149(31) 0.3721(11) 0.4138(25) 0.030 Uiso 0.50 d PR 1 H21B H 0.4606(31) 0.4054(11) 0.2996(25) 0.030 Uiso 0.50 d PR 1 C22A C 0.2664(29) 0.3561(12) 0.2269(26) 0.048(6) Uiso 0.50 d P 1 H22C H 0.2176(29) 0.3794(12) 0.1470(26) 0.057 Uiso 0.50 d PR 1 H22D H 0.1820(29) 0.3428(12) 0.2618(26) 0.057 Uiso 0.50 d PR 1 C23A C 0.2342(28) 0.4802(10) 0.2558(24) 0.043(6) Uiso 0.50 d P 1 H23C H 0.1320(28) 0.4630(10) 0.2068(24) 0.052 Uiso 0.50 d PR 1 H23D H 0.2988(28) 0.4816(10) 0.1947(24) 0.052 Uiso 0.50 d PR 1 C24A C 0.2023(31) 0.5416(11) 0.2963(28) 0.045(6) Uiso 0.50 d P 1 H24C H 0.1626(31) 0.5653(11) 0.2157(28) 0.054 Uiso 0.50 d PR 1 H24D H 0.1217(31) 0.5408(11) 0.3427(28) 0.054 Uiso 0.50 d PR 1 C25A C 0.1930(33) 0.4319(12) 0.4452(27) 0.059(7) Uiso 0.50 d P 1 H25A H 0.1564(33) 0.3929(12) 0.4242(27) 0.071 Uiso 0.50 d PR 1 H25B H 0.1005(33) 0.4569(12) 0.4163(27) 0.071 Uiso 0.50 d PR 1 C26A C 0.2765(34) 0.4381(12) 0.6060(27) 0.056(7) Uiso 0.50 d P 1 H26A H 0.1959(34) 0.4359(12) 0.6523(27) 0.067 Uiso 0.50 d PR 1 H26B H 0.3512(34) 0.4068(12) 0.6385(27) 0.067 Uiso 0.50 d PR 1 N21B N 0.4596(19) 0.5658(7) 0.6293(18) 0.035(4) Uani 0.50 d P 2 N22B N 0.4126(25) 0.4446(8) 0.6255(21) 0.045(5) Uani 0.50 d P 2 H22E H 0.3315(25) 0.4232(8) 0.5734(21) 0.054 Uiso 0.50 d PR 2 H22F H 0.4907(25) 0.4212(8) 0.6744(21) 0.054 Uiso 0.50 d PR 2 N23B N 0.7434(30) 0.6838(11) 0.8206(22) 0.040(5) Uani 0.50 d P 2 H23E H 0.7500(30) 0.6996(11) 0.7429(22) 0.048 Uiso 0.50 d PR 2 H23F H 0.8237(30) 0.6583(11) 0.8470(22) 0.048 Uiso 0.50 d PR 2 N24B N 0.2656(25) 0.5248(9) 0.3772(24) 0.052(5) Uani 0.50 d P 2 H24E H 0.2566(25) 0.5247(9) 0.2878(24) 0.063 Uiso 0.50 d PR 2 H24F H 0.1924(25) 0.5008(9) 0.3915(24) 0.063 Uiso 0.50 d PR 2 C21B C 0.4502(33) 0.5356(12) 0.7503(29) 0.058(7) Uiso 0.50 d P 2 H21C H 0.4042(33) 0.5606(12) 0.8033(29) 0.069 Uiso 0.50 d PR 2 H21D H 0.5575(33) 0.5257(12) 0.8068(29) 0.069 Uiso 0.50 d PR 2 C22B C 0.3520(33) 0.4811(13) 0.7132(32) 0.057(7) Uiso 0.50 d P 2 H22G H 0.2408(33) 0.4911(13) 0.6691(32) 0.069 Uiso 0.50 d PR 2 H22H H 0.3587(33) 0.4608(13) 0.7967(32) 0.069 Uiso 0.50 d PR 2 C23B C 0.5829(33) 0.6061(12) 0.6659(28) 0.031(7) Uiso 0.50 d P 2 H23G H 0.5820(33) 0.6263(12) 0.5834(28) 0.037 Uiso 0.50 d PR 2 H23H H 0.6819(33) 0.5845(12) 0.6955(28) 0.037 Uiso 0.50 d PR 2 C24B C 0.5940(26) 0.6494(10) 0.7767(23) 0.039(5) Uiso 0.50 d P 2 H24G H 0.5038(26) 0.6751(10) 0.7433(23) 0.047 Uiso 0.50 d PR 2 H24H H 0.5836(26) 0.6305(10) 0.8573(23) 0.047 Uiso 0.50 d PR 2 C25B C 0.3071(34) 0.5934(13) 0.5678(28) 0.062(7) Uiso 0.50 d P 2 H25C H 0.2304(34) 0.5812(13) 0.6125(28) 0.074 Uiso 0.50 d PR 2 H25D H 0.3201(34) 0.6344(13) 0.5792(28) 0.074 Uiso 0.50 d PR 2 C26B C 0.2375(38) 0.5803(13) 0.4187(31) 0.068(8) Uiso 0.50 d P 2 H26C H 0.2869(38) 0.6066(13) 0.3710(31) 0.081 Uiso 0.50 d PR 2 H26D H 0.1237(38) 0.5887(13) 0.3891(31) 0.081 Uiso 0.50 d PR 2 Cl1A Cl -0.0238(7) 0.3831(3) 0.4094(7) 0.052(2) Uani 0.50 d P . O11A O -0.1625(28) 0.3731(11) 0.4378(24) 0.090(7) Uiso 0.50 d P 1 O12A O -0.0395(32) 0.3573(12) 0.2826(28) 0.109(8) Uiso 0.50 d P 1 O13A O 0.1033(37) 0.3597(14) 0.4988(32) 0.123(9) Uiso 0.50 d P 1 O14A O -0.0019(32) 0.4425(12) 0.4036(28) 0.106(8) Uiso 0.50 d P 1 Cl1B Cl 0.4998(6) 0.7500 0.4165(5) 0.0631(14) Uani 1 d S . O11B O 0.3916(46) 0.7143(16) 0.4638(39) 0.165(14) Uiso 0.50 d P 2 O12B O 0.5267(40) 0.7119(14) 0.3065(34) 0.137(11) Uiso 0.50 d P 2 O13B O 0.6413(24) 0.7500 0.5256(21) 0.112(6) Uiso 1 d S 2 O14B O 0.4455(28) 0.7027(10) 0.3551(25) 0.080(6) Uiso 0.50 d P 2 Cl2A Cl -0.2241(9) 0.4099(3) 0.0004(7) 0.062(2) Uani 0.50 d P 1 O21 O -0.3734(24) 0.4223(9) -0.1037(21) 0.169(7) Uiso 1 d . . O22A O -0.2651(51) 0.3663(19) 0.0869(45) 0.182(16) Uiso 0.50 d P 1 O23A O -0.1888(47) 0.4690(19) 0.0673(40) 0.167(14) Uiso 0.50 d P 1 O24A O -0.1044(54) 0.3951(21) -0.0540(46) 0.194(17) Uiso 0.50 d P 1 Cl2B Cl -0.4541(9) 0.4063(3) -0.0059(7) 0.060(2) Uani 0.50 d P 2 O22B O -0.4514(36) 0.3447(15) 0.0190(31) 0.125(10) Uiso 0.50 d P 2 O23B O -0.6153(49) 0.4280(17) -0.0473(39) 0.164(14) Uiso 0.50 d P 2 O24B O -0.3888(46) 0.4336(18) 0.1147(42) 0.165(14) Uiso 0.50 d P 2 O1 O -0.2938(29) 0.2500 0.2923(27) 0.157(9) Uiso 1 d S . H1 H -0.2287(29) 0.2500 0.3952(27) 0.235 Uiso 1 d SR . H2 H -0.2981(29) 0.2500 0.2350(27) 0.235 Uiso 1 d SR . 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 0.0343(11) 0.0244(10) 0.0297(11) 0.000 0.0061(8) 0.000 N11 0.039(12) 0.045(13) 0.029(11) 0.016(10) 0.003(9) 0.026(11) N12 0.055(12) 0.035(10) 0.087(17) -0.005(11) 0.041(12) 0.001(9) N13 0.049(9) 0.076(12) 0.049(9) 0.000 0.016(8) 0.000 N14 0.021(12) 0.036(17) 0.056(19) -0.014(12) -0.007(11) -0.007(11) C11 0.119(35) 0.039(22) 0.047(24) 0.012(15) 0.008(20) -0.015(22) C12 0.083(20) 0.046(16) 0.053(16) 0.009(13) 0.029(15) -0.004(15) C13 0.034(13) 0.043(14) 0.062(16) 0.011(12) -0.015(12) 0.011(11) C14 0.039(13) 0.247(44) 0.098(22) 0.000 0.025(14) 0.000 C15 0.083(15) 0.092(18) 0.024(9) 0.000 -0.013(10) 0.000 C16 0.123(28) 0.029(14) 0.077(23) -0.005(14) -0.013(22) 0.015(17) Ni2 0.0301(10) 0.0223(10) 0.0300(10) -0.0019(8) 0.0067(8) -0.0023(8) N21A 0.038(10) 0.032(10) 0.035(10) 0.001(8) 0.014(8) -0.001(8) N22A 0.036(13) 0.034(13) 0.056(15) 0.003(10) -0.017(13) 0.003(12) N23A 0.032(10) 0.027(10) 0.056(12) -0.011(9) 0.021(9) 0.002(8) N24A 0.044(11) 0.050(13) 0.018(9) -0.009(9) 0.004(8) -0.009(9) N21B 0.027(9) 0.025(9) 0.045(11) -0.011(8) 0.000(8) -0.013(7) N22B 0.054(13) 0.022(10) 0.066(14) -0.018(9) 0.028(11) -0.011(9) N23B 0.050(15) 0.043(14) 0.022(10) -0.005(9) 0.004(12) -0.015(13) N24B 0.048(13) 0.037(12) 0.063(15) 0.003(11) 0.005(11) 0.000(11) Cl1A 0.045(3) 0.053(4) 0.059(4) -0.004(3) 0.021(3) -0.002(3) Cl1B 0.062(3) 0.073(3) 0.047(3) 0.000 0.006(2) 0.000 Cl2A 0.068(4) 0.059(4) 0.056(4) 0.003(3) 0.015(3) 0.024(4) Cl2B 0.083(5) 0.053(4) 0.051(4) 0.001(3) 0.029(4) -0.009(4) _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 N11 2.08(2) 4_565 ? Ni1 N11 2.08(2) . ? Ni1 N23B 2.09(2) 3_666 ? Ni1 N23B 2.09(2) 2_646 ? Ni1 N13 2.106(15) . ? Ni1 N12 2.17(2) . ? Ni1 N12 2.17(2) 4_565 ? Ni1 N22A 2.17(2) . ? Ni1 N22A 2.17(2) 4_565 ? Ni1 N14 2.22(3) 4_565 ? Ni1 N14 2.22(3) . ? N11 N14 1.00(3) 4_565 ? N11 C16 1.35(4) 4_565 ? N11 C13 1.46(3) . ? N11 C11 1.49(4) . ? N11 C15 1.58(3) . ? N12 N12 1.26(4) 4_565 ? N12 C12 1.48(3) . ? N13 C14 1.34(3) . ? N14 C11 0.66(3) 4_565 ? N14 N11 1.00(3) 4_565 ? N14 C16 1.45(4) . ? N14 C12 1.75(4) 4_565 ? C11 N14 0.66(3) 4_565 ? C11 C16 1.42(5) 4_565 ? C11 C12 1.54(5) . ? C12 N14 1.75(4) 4_565 ? C12 C16 1.95(4) 4_565 ? C13 C14 1.86(3) . ? C14 C13 1.86(3) 4_565 ? C15 C16 1.33(3) 4_565 ? C15 C16 1.33(3) . ? C15 N11 1.58(3) 4_565 ? C16 N11 1.35(4) 4_565 ? C16 C11 1.42(5) 4_565 ? C16 C12 1.95(4) 4_565 ? Ni2 N24A 2.09(2) . ? Ni2 N24A 2.09(2) 3_666 ? Ni2 N23A 2.13(2) . ? Ni2 N23A 2.13(2) 3_666 ? Ni2 N22B 2.14(2) 3_666 ? Ni2 N22B 2.14(2) . ? Ni2 N24B 2.14(2) . ? Ni2 N24B 2.14(2) 3_666 ? Ni2 N21B 2.14(2) . ? Ni2 N21B 2.14(2) 3_666 ? Ni2 N21A 2.16(2) 3_666 ? Ni2 N21A 2.16(2) . ? N21A C23A 1.42(3) . ? N21A C21A 1.43(3) . ? N21A C25A 1.50(3) . ? N22A C22A 1.45(3) . ? N23A C24A 1.46(3) . ? N24A C26A 1.46(3) . ? C21A C22A 1.51(4) . ? C23A C24A 1.55(3) . ? C25A C26A 1.60(4) . ? C25A O14A 1.65(4) . ? C25A Cl1A 2.15(3) . ? N21B C23B 1.40(3) . ? N21B C25B 1.44(3) . ? N21B C21B 1.46(3) . ? N22B C22B 1.46(3) . ? N23B C24B 1.49(3) . ? N23B Ni1 2.09(2) 3_666 ? N24B C26B 1.41(3) . ? C21B C22B 1.52(4) . ? C21B O24B 1.79(5) 3_566 ? C23B C24B 1.51(4) . ? C25B C26B 1.50(4) . ? Cl1A O13A 1.33(3) . ? Cl1A O11A 1.36(2) . ? Cl1A O12A 1.41(3) . ? Cl1A O14A 1.41(3) . ? Cl1B O14B 1.29(2) . ? Cl1B O14B 1.29(2) 4_575 ? Cl1B O13B 1.39(2) . ? Cl1B O11B 1.46(4) 4_575 ? Cl1B O11B 1.46(4) . ? Cl1B O12B 1.52(3) . ? Cl1B O12B 1.52(3) 4_575 ? O11B O14B 1.37(4) . ? O11B O11B 1.67(8) 4_575 ? O12B O14B 1.01(3) . ? O12B O12B 1.78(7) 4_575 ? Cl2A O24A 1.38(5) . ? Cl2A O21 1.44(2) . ? Cl2A O22A 1.47(4) . ? Cl2A O23A 1.53(4) . ? O21 Cl2B 1.45(2) . ? Cl2B O24B 1.36(4) . ? Cl2B O23B 1.44(4) . ? Cl2B O22B 1.46(4) . ? O24B C21B 1.79(5) 3_566 ? 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 N11 Ni1 N11 60.5(14) 4_565 . ? N11 Ni1 N23B 156.1(10) 4_565 3_666 ? N11 Ni1 N23B 99.7(10) . 3_666 ? N11 Ni1 N23B 99.7(10) 4_565 2_646 ? N11 Ni1 N23B 156.1(10) . 2_646 ? N23B Ni1 N23B 95.4(13) 3_666 2_646 ? N11 Ni1 N13 80.5(7) 4_565 . ? N11 Ni1 N13 80.5(7) . . ? N23B Ni1 N13 83.1(7) 3_666 . ? N23B Ni1 N13 83.1(7) 2_646 . ? N11 Ni1 N12 100.6(8) 4_565 . ? N11 Ni1 N12 83.7(9) . . ? N23B Ni1 N12 89.6(9) 3_666 . ? N23B Ni1 N12 115.0(9) 2_646 . ? N13 Ni1 N12 161.2(5) . . ? N11 Ni1 N12 83.7(9) 4_565 4_565 ? N11 Ni1 N12 100.6(8) . 4_565 ? N23B Ni1 N12 115.0(9) 3_666 4_565 ? N23B Ni1 N12 89.6(9) 2_646 4_565 ? N13 Ni1 N12 161.2(5) . 4_565 ? N12 Ni1 N12 33.8(10) . 4_565 ? N11 Ni1 N22A 171.0(9) 4_565 . ? N11 Ni1 N22A 111.2(9) . . ? N13 Ni1 N22A 102.2(8) . . ? N12 Ni1 N22A 74.0(10) . . ? N12 Ni1 N22A 94.9(9) 4_565 . ? N11 Ni1 N22A 111.2(9) 4_565 4_565 ? N11 Ni1 N22A 171.0(9) . 4_565 ? N13 Ni1 N22A 102.2(8) . 4_565 ? N12 Ni1 N22A 94.9(9) . 4_565 ? N12 Ni1 N22A 74.0(10) 4_565 4_565 ? N22A Ni1 N22A 76.8(12) . 4_565 ? N11 Ni1 N14 82.9(11) 4_565 4_565 ? N11 Ni1 N14 26.5(8) . 4_565 ? N23B Ni1 N14 82.4(10) 3_666 4_565 ? N23B Ni1 N14 177.3(11) 2_646 4_565 ? N13 Ni1 N14 98.1(8) . 4_565 ? N12 Ni1 N14 63.6(9) . 4_565 ? N12 Ni1 N14 90.1(9) 4_565 4_565 ? N22A Ni1 N14 88.2(10) . 4_565 ? N22A Ni1 N14 156.8(10) 4_565 4_565 ? N11 Ni1 N14 26.5(8) 4_565 . ? N11 Ni1 N14 82.9(11) . . ? N23B Ni1 N14 177.3(11) 3_666 . ? N23B Ni1 N14 82.4(10) 2_646 . ? N13 Ni1 N14 98.1(8) . . ? N12 Ni1 N14 90.1(9) . . ? N12 Ni1 N14 63.6(9) 4_565 . ? N22A Ni1 N14 156.8(10) . . ? N22A Ni1 N14 88.2(10) 4_565 . ? N14 Ni1 N14 99.9(16) 4_565 . ? N14 N11 C16 74.9(25) 4_565 4_565 ? N14 N11 C13 114.0(26) 4_565 . ? C16 N11 C13 135.6(22) 4_565 . ? N14 N11 C11 20.6(25) 4_565 . ? C16 N11 C11 60.0(24) 4_565 . ? C13 N11 C11 113.4(27) . . ? N14 N11 C15 126.4(27) 4_565 . ? C16 N11 C15 53.3(16) 4_565 . ? C13 N11 C15 112.5(20) . . ? C11 N11 C15 113.3(24) . . ? N14 N11 Ni1 84.5(20) 4_565 . ? C16 N11 Ni1 116.3(19) 4_565 . ? C13 N11 Ni1 107.9(14) . . ? C11 N11 Ni1 103.9(19) . . ? C15 N11 Ni1 105.0(11) . . ? N12 N12 C12 131.6(14) 4_565 . ? N12 N12 Ni1 73.1(5) 4_565 . ? C12 N12 Ni1 107.8(15) . . ? C14 N13 Ni1 114.2(15) . . ? C11 N14 N11 127.3(67) 4_565 4_565 ? C11 N14 C16 74.3(60) 4_565 . ? N11 N14 C16 63.7(24) 4_565 . ? C11 N14 C12 60.3(56) 4_565 4_565 ? N11 N14 C12 128.6(28) 4_565 4_565 ? C16 N14 C12 74.1(23) . 4_565 ? C11 N14 Ni1 156.3(62) 4_565 . ? N11 N14 Ni1 69.0(18) 4_565 . ? C16 N14 Ni1 104.4(19) . . ? C12 N14 Ni1 96.3(13) 4_565 . ? N14 C11 C16 79.2(58) 4_565 4_565 ? N14 C11 N11 32.1(44) 4_565 . ? C16 C11 N11 55.1(23) 4_565 . ? N14 C11 C12 97.8(60) 4_565 . ? C16 C11 C12 82.1(32) 4_565 . ? N11 C11 C12 111.2(29) . . ? N12 C12 C11 112.2(21) . . ? N12 C12 N14 91.0(16) . 4_565 ? C11 C12 N14 21.9(12) . 4_565 ? N12 C12 C16 106.7(19) . 4_565 ? C11 C12 C16 46.5(21) . 4_565 ? N14 C12 C16 45.9(17) 4_565 4_565 ? N11 C13 C14 102.4(17) . . ? N13 C14 C13 92.8(12) . . ? N13 C14 C13 92.8(12) . 4_565 ? C13 C14 C13 109.8(22) . 4_565 ? C16 C15 C16 106.8(38) 4_565 . ? C16 C15 N11 54.2(19) 4_565 . ? C16 C15 N11 118.6(19) . . ? C16 C15 N11 118.6(19) 4_565 4_565 ? C16 C15 N11 54.2(19) . 4_565 ? N11 C15 N11 82.9(16) . 4_565 ? C15 C16 N11 72.5(26) . 4_565 ? C15 C16 C11 137.4(40) . 4_565 ? N11 C16 C11 65.0(24) 4_565 4_565 ? C15 C16 N14 112.6(33) . . ? N11 C16 N14 41.4(16) 4_565 . ? C11 C16 N14 26.5(14) 4_565 . ? C15 C16 C12 139.0(24) . 4_565 ? N11 C16 C12 96.9(21) 4_565 4_565 ? C11 C16 C12 51.5(24) 4_565 4_565 ? N14 C16 C12 60.0(18) . 4_565 ? N24A Ni2 N24A 180.000(3) . 3_666 ? N24A Ni2 N23A 92.3(8) . . ? N24A Ni2 N23A 87.7(8) 3_666 . ? N24A Ni2 N23A 87.7(8) . 3_666 ? N24A Ni2 N23A 92.3(8) 3_666 3_666 ? N23A Ni2 N23A 180.000(4) . 3_666 ? N22B Ni2 N22B 180.000(4) 3_666 . ? N22B Ni2 N24B 86.4(9) 3_666 . ? N22B Ni2 N24B 93.6(9) . . ? N22B Ni2 N24B 93.6(9) 3_666 3_666 ? N22B Ni2 N24B 86.4(9) . 3_666 ? N24B Ni2 N24B 180.000(3) . 3_666 ? N22B Ni2 N21B 95.8(7) 3_666 . ? N22B Ni2 N21B 84.2(7) . . ? N24B Ni2 N21B 81.8(7) . . ? N24B Ni2 N21B 98.2(7) 3_666 . ? N22B Ni2 N21B 84.2(7) 3_666 3_666 ? N22B Ni2 N21B 95.8(7) . 3_666 ? N24B Ni2 N21B 98.2(7) . 3_666 ? N24B Ni2 N21B 81.8(7) 3_666 3_666 ? N21B Ni2 N21B 180.000(3) . 3_666 ? N24A Ni2 N21A 97.8(7) . 3_666 ? N24A Ni2 N21A 82.2(7) 3_666 3_666 ? N23A Ni2 N21A 98.1(7) . 3_666 ? N23A Ni2 N21A 81.9(7) 3_666 3_666 ? N24A Ni2 N21A 82.2(7) . . ? N24A Ni2 N21A 97.8(7) 3_666 . ? N23A Ni2 N21A 81.9(7) . . ? N23A Ni2 N21A 98.1(7) 3_666 . ? N21A Ni2 N21A 180.000(2) 3_666 . ? C23A N21A C21A 110.2(18) . . ? C23A N21A C25A 108.8(18) . . ? C21A N21A C25A 108.9(19) . . ? C23A N21A Ni2 105.9(14) . . ? C21A N21A Ni2 112.5(14) . . ? C25A N21A Ni2 110.4(14) . . ? C22A N22A Ni1 117.2(17) . . ? C24A N23A Ni2 110.1(15) . . ? C26A N24A Ni2 108.6(16) . . ? N21A C21A C22A 121.7(22) . . ? N22A C22A C21A 115.9(21) . . ? N21A C23A C24A 111.3(20) . . ? N23A C24A C23A 109.6(21) . . ? N21A C25A C26A 109.2(21) . . ? N21A C25A O14A 131.4(22) . . ? C26A C25A O14A 111.2(21) . . ? N21A C25A Cl1A 138.8(18) . . ? C26A C25A Cl1A 108.9(17) . . ? O14A C25A Cl1A 40.8(12) . . ? N24A C26A C25A 108.8(22) . . ? C23B N21B C25B 110.6(20) . . ? C23B N21B C21B 110.0(19) . . ? C25B N21B C21B 107.6(20) . . ? C23B N21B Ni2 113.0(15) . . ? C25B N21B Ni2 111.0(15) . . ? C21B N21B Ni2 104.4(14) . . ? C22B N22B Ni2 106.7(16) . . ? C24B N23B Ni1 128.2(18) . 3_666 ? C26B N24B Ni2 107.3(18) . . ? N21B C21B C22B 111.7(23) . . ? N21B C21B O24B 125.4(23) . 3_566 ? C22B C21B O24B 104.4(23) . 3_566 ? N22B C22B C21B 111.1(23) . . ? N21B C23B C24B 121.4(22) . . ? N23B C24B C23B 116.0(20) . . ? N21B C25B C26B 112.8(24) . . ? N24B C26B C25B 116.3(26) . . ? O13A Cl1A O11A 113.4(17) . . ? O13A Cl1A O12A 106.8(18) . . ? O11A Cl1A O12A 106.9(16) . . ? O13A Cl1A O14A 109.9(19) . . ? O11A Cl1A O14A 108.7(16) . . ? O12A Cl1A O14A 111.1(17) . . ? O13A Cl1A C25A 65.8(15) . . ? O11A Cl1A C25A 149.2(13) . . ? O12A Cl1A C25A 102.4(13) . . ? O14A Cl1A C25A 50.0(13) . . ? Cl1A O14A C25A 89.2(18) . . ? O14B Cl1B O14B 118.1(20) . 4_575 ? O14B Cl1B O13B 119.8(10) . . ? O14B Cl1B O13B 119.8(10) 4_575 . ? O14B Cl1B O11B 118.4(19) . 4_575 ? O14B Cl1B O11B 59.5(16) 4_575 4_575 ? O13B Cl1B O11B 103.9(16) . 4_575 ? O14B Cl1B O11B 59.5(16) . . ? O14B Cl1B O11B 118.4(19) 4_575 . ? O13B Cl1B O11B 103.9(16) . . ? O11B Cl1B O11B 69.9(30) 4_575 . ? O14B Cl1B O12B 41.3(14) . . ? O14B Cl1B O12B 104.9(17) 4_575 . ? O13B Cl1B O12B 107.3(14) . . ? O11B Cl1B O12B 148.8(20) 4_575 . ? O11B Cl1B O12B 100.5(19) . . ? O14B Cl1B O12B 104.9(17) . 4_575 ? O14B Cl1B O12B 41.3(14) 4_575 4_575 ? O13B Cl1B O12B 107.3(15) . 4_575 ? O11B Cl1B O12B 100.5(19) 4_575 4_575 ? O11B Cl1B O12B 148.8(20) . 4_575 ? O12B Cl1B O12B 72.0(26) . 4_575 ? O14B O11B Cl1B 54.2(18) . . ? O14B O11B O11B 101.4(19) . 4_575 ? Cl1B O11B O11B 55.1(15) . 4_575 ? O14B O12B Cl1B 57.3(23) . . ? O14B O12B O12B 102.3(25) . 4_575 ? Cl1B O12B O12B 54.0(13) . 4_575 ? O12B O14B Cl1B 81.4(26) . . ? O12B O14B O11B 146.6(37) . . ? Cl1B O14B O11B 66.3(20) . . ? O24A Cl2A O21 112.3(21) . . ? O24A Cl2A O22A 115.6(27) . . ? O21 Cl2A O22A 104.7(20) . . ? O24A Cl2A O23A 109.6(25) . . ? O21 Cl2A O23A 99.4(17) . . ? O22A Cl2A O23A 114.0(23) . . ? O24B Cl2B O23B 101.7(23) . . ? O24B Cl2B O21 110.8(19) . . ? O23B Cl2B O21 110.5(19) . . ? O24B Cl2B O22B 109.0(22) . . ? O23B Cl2B O22B 111.2(21) . . ? O21 Cl2B O22B 113.1(15) . . ? Cl2B O24B C21B 139.2(29) . 3_566 ? _refine_diff_density_max 1.682 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.177 #===END ## {[Ni2(tren)2(aepd)][ClO4]4.2H2O data_1132lg25 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H56 Cl4 N12 Ni2 O18' _chemical_formula_weight 987.97 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.968(2) _cell_length_b 15.4800(10) _cell_length_c 15.684(2) _cell_angle_alpha 118.552(7) _cell_angle_beta 104.250(10) _cell_angle_gamma 97.470(10) _cell_volume 1971.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description purple _exptl_crystal_colour prism _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method ? _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7353 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6916 _reflns_number_observed 4761 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'XTAL3.2' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+2.5281P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6916 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_obs 0.0470 _refine_ls_wR_factor_all 0.1503 _refine_ls_wR_factor_obs 0.1283 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.23963(6) 0.87015(4) 0.12605(4) 0.0293(2) Uani 1 d . . Ni2 Ni 0.21650(6) 1.30932(4) 0.52739(4) 0.0291(2) Uani 1 d . . N11 N 0.3494(4) 1.4229(3) 0.6792(3) 0.0362(9) Uani 1 d . . N12 N 0.1017(5) 1.2659(3) 0.6068(3) 0.0422(10) Uani 1 d . . H12A H 0.0136(5) 1.2755(3) 0.5938(3) 0.051 Uiso 1 d R . H12B H 0.0900(5) 1.1989(3) 0.5837(3) 0.051 Uiso 1 d R . N13 N 0.1155(4) 1.4236(3) 0.5414(3) 0.0388(10) Uani 1 d . . H13A H 0.1508(4) 1.4574(3) 0.5145(3) 0.047 Uiso 1 d R . H13B H 0.0196(4) 1.3950(3) 0.5064(3) 0.047 Uiso 1 d R . N14 N 0.3768(5) 1.3696(3) 0.4877(4) 0.0448(11) Uani 1 d . . H14A H 0.4176(5) 1.3210(3) 0.4548(4) 0.054 Uiso 1 d R . H14B H 0.3369(5) 1.3900(3) 0.4450(4) 0.054 Uiso 1 d R . C12A C 0.3408(7) 1.3751(4) 0.7401(4) 0.0483(14) Uani 1 d . . H12C H 0.3889(7) 1.4266(4) 0.8134(4) 0.058 Uiso 1 d R . H12D H 0.3897(7) 1.3221(4) 0.7218(4) 0.058 Uiso 1 d R . C12B C 0.1840(7) 1.3286(5) 0.7192(4) 0.054(2) Uani 1 d . . H12E H 0.1787(7) 1.2861(5) 0.7485(4) 0.065 Uiso 1 d R . H12F H 0.1417(7) 1.3831(5) 0.7522(4) 0.065 Uiso 1 d R . C13A C 0.2994(6) 1.5162(4) 0.7143(4) 0.0457(13) Uani 1 d . . H13C H 0.3613(6) 1.5667(4) 0.7101(4) 0.055 Uiso 1 d R . H13D H 0.3089(6) 1.5453(4) 0.7865(4) 0.055 Uiso 1 d R . C13B C 0.1431(6) 1.4942(4) 0.6506(4) 0.0449(13) Uani 1 d . . H13E H 0.0784(6) 1.4648(4) 0.6733(4) 0.054 Uiso 1 d R . H13F H 0.1248(6) 1.5580(4) 0.6610(4) 0.054 Uiso 1 d R . C14A C 0.4960(6) 1.4447(4) 0.6744(5) 0.0504(14) Uani 1 d . . H14C H 0.5359(6) 1.3885(4) 0.6663(5) 0.061 Uiso 1 d R . H14D H 0.5592(6) 1.5069(4) 0.7386(5) 0.061 Uiso 1 d R . C14B C 0.4877(6) 1.4580(5) 0.5842(5) 0.0535(15) Uani 1 d . . H14E H 0.4635(6) 1.5209(5) 0.5979(5) 0.064 Uiso 1 d R . H14F H 0.5811(6) 1.4632(5) 0.5759(5) 0.064 Uiso 1 d R . N21 N 0.3381(5) 0.8015(3) 0.0160(3) 0.0385(10) Uani 1 d . . N22 N 0.4208(5) 0.9994(3) 0.1931(3) 0.0408(10) Uani 1 d . . H22A H 0.3942(5) 1.0575(3) 0.2185(3) 0.049 Uiso 1 d R . H22B H 0.4890(5) 1.0031(3) 0.2455(3) 0.049 Uiso 1 d R . N23 N 0.3562(5) 0.7995(3) 0.1959(3) 0.0432(10) Uani 1 d . . H23A H 0.4187(5) 0.8481(3) 0.2599(3) 0.052 Uiso 1 d R . H23B H 0.2939(5) 0.7569(3) 0.2020(3) 0.052 Uiso 1 d R . N24 N 0.1316(5) 0.9057(3) 0.0143(3) 0.0414(10) Uani 1 d . . H24A H 0.0352(5) 0.8829(3) -0.0039(3) 0.050 Uiso 1 d R . H24B H 0.1565(5) 0.9742(3) 0.0431(3) 0.050 Uiso 1 d R . C22A C 0.4768(6) 0.8780(5) 0.0461(5) 0.0524(15) Uani 1 d . . H22C H 0.4923(6) 0.8673(5) -0.0165(5) 0.063 Uiso 1 d R . H22D H 0.5564(6) 0.8656(5) 0.0843(5) 0.063 Uiso 1 d R . C22B C 0.4776(6) 0.9871(4) 0.1108(5) 0.0498(14) Uani 1 d . . H22E H 0.5757(6) 1.0319(4) 0.1418(5) 0.060 Uiso 1 d R . H22F H 0.4187(6) 1.0063(4) 0.0673(5) 0.060 Uiso 1 d R . C23A C 0.3663(7) 0.7121(4) 0.0192(4) 0.0469(13) Uani 1 d . . H23C H 0.4300(7) 0.6864(4) -0.0187(4) 0.056 Uiso 1 d R . H23D H 0.2759(7) 0.6579(4) -0.0141(4) 0.056 Uiso 1 d R . C23B C 0.4357(7) 0.7415(5) 0.1315(4) 0.0520(14) Uani 1 d . . H23E H 0.4354(7) 0.6797(5) 0.1332(4) 0.062 Uiso 1 d R . H23F H 0.5354(7) 0.7828(5) 0.1595(4) 0.062 Uiso 1 d R . C24A C 0.2329(7) 0.7704(4) -0.0850(4) 0.0498(14) Uani 1 d . . H24C H 0.1547(7) 0.7113(4) -0.1073(4) 0.060 Uiso 1 d R . H24D H 0.2798(7) 0.7502(4) -0.1361(4) 0.060 Uiso 1 d R . C24B C 0.1719(6) 0.8567(5) -0.0787(4) 0.0511(14) Uani 1 d . . H24E H 0.2433(6) 0.9076(5) -0.0762(4) 0.061 Uiso 1 d R . H24F H 0.0873(6) 0.8297(5) -0.1403(4) 0.061 Uiso 1 d R . N31 N 0.1473(4) 0.9419(3) 0.2450(3) 0.0339(9) Uani 1 d . . N32 N 0.0503(5) 0.7439(3) 0.0597(3) 0.0432(11) Uani 1 d . . H32A H 0.0050(5) 0.7216(3) -0.0074(3) 0.052 Uiso 1 d R . H32B H 0.0750(5) 0.6916(3) 0.0634(3) 0.052 Uiso 1 d R . N33 N 0.3156(4) 1.1848(3) 0.5062(3) 0.0347(9) Uani 1 d . . H33A H 0.4126(4) 1.2086(3) 0.5293(3) 0.042 Uiso 0.60(2) d PR 1 H33B H 0.2910(4) 1.1562(3) 0.5405(3) 0.042 Uiso 0.60(2) d PR 1 H33C H 0.3985(4) 1.1954(3) 0.4947(3) 0.042 Uiso 0.40(2) d PR 2 H33D H 0.3337(4) 1.1788(3) 0.5620(3) 0.042 Uiso 0.40(2) d PR 2 N34 N 0.0775(4) 1.1988(3) 0.3714(3) 0.0391(10) Uani 1 d . . H34A H -0.0153(4) 1.1968(3) 0.3648(3) 0.047 Uiso 0.60(2) d PR 1 H34B H 0.0997(4) 1.2151(3) 0.3277(3) 0.047 Uiso 0.60(2) d PR 1 H34C H -0.0087(4) 1.1697(3) 0.3691(3) 0.047 Uiso 0.40(2) d PR 2 H34D H 0.0635(4) 1.2276(3) 0.3332(3) 0.047 Uiso 0.40(2) d PR 2 C32A C 0.0453(6) 0.8532(4) 0.2324(4) 0.0455(13) Uani 1 d . . H32C H -0.0163(6) 0.8782(4) 0.2725(4) 0.055 Uiso 1 d R . H32D H 0.0993(6) 0.8174(4) 0.2579(4) 0.055 Uiso 1 d R . C32B C -0.0461(6) 0.7806(5) 0.1196(4) 0.0533(15) Uani 1 d . . H32E H -0.1122(6) 0.7227(5) 0.1108(4) 0.064 Uiso 1 d R . H32F H -0.1026(6) 0.8156(5) 0.0944(4) 0.064 Uiso 1 d R . C33A C 0.2604(6) 1.0025(4) 0.3529(4) 0.0376(11) Uani 1 d . . H33E H 0.2366(6) 0.9786(4) 0.3958(4) 0.045 Uiso 0.60(2) d PR 1 H33F H 0.3550(6) 0.9960(4) 0.3503(4) 0.045 Uiso 0.60(2) d PR 1 H33G H 0.3543(6) 1.0261(4) 0.3514(4) 0.045 Uiso 0.40(2) d PR 2 H33H H 0.2674(6) 0.9607(4) 0.3832(4) 0.045 Uiso 0.40(2) d PR 2 C33B C 0.2564(15) 1.1092(8) 0.3940(9) 0.035(3) Uani 0.60(2) d P 1 H33I H 0.3087(15) 1.1362(8) 0.3624(9) 0.042 Uiso 0.60(2) d PR 1 C33C C 0.2044(21) 1.0939(11) 0.4151(11) 0.026(4) Uani 0.40(2) d P 2 H33J H 0.1241(21) 1.0720(11) 0.4327(11) 0.031 Uiso 0.40(2) d PR 2 C34A C 0.0675(6) 1.0149(4) 0.2363(4) 0.0426(12) Uani 1 d . . H34E H 0.1028(6) 1.0434(4) 0.2000(4) 0.051 Uiso 0.60(2) d PR 1 H34F H -0.0355(6) 0.9807(4) 0.2001(4) 0.051 Uiso 0.60(2) d PR 1 H34G H -0.0305(6) 0.9948(4) 0.2335(4) 0.051 Uiso 0.40(2) d PR 2 H34H H 0.0634(6) 1.0147(4) 0.1738(4) 0.051 Uiso 0.40(2) d PR 2 C34B C 0.1001(15) 1.0975(9) 0.3468(8) 0.034(3) Uani 0.60(2) d P 1 H34I H 0.0453(15) 1.0699(9) 0.3768(8) 0.041 Uiso 0.60(2) d PR 1 C34C C 0.1564(23) 1.1267(14) 0.3359(11) 0.034(4) Uani 0.40(2) d P 2 H34J H 0.2397(23) 1.1563(14) 0.3258(11) 0.041 Uiso 0.40(2) d PR 2 Cl1 Cl 0.29370(14) 0.72241(10) 0.59465(11) 0.0453(3) Uani 1 d . . O11 O 0.4295(5) 0.7750(4) 0.6043(4) 0.0758(14) Uani 1 d . . O12 O 0.1844(6) 0.7292(6) 0.5233(6) 0.125(3) Uani 1 d . . O13 O 0.2843(8) 0.6190(4) 0.5569(6) 0.119(3) Uani 1 d . . O14 O 0.2702(9) 0.7673(5) 0.6885(5) 0.127(3) Uani 1 d . . Cl2 Cl -0.24801(13) 0.98568(10) 0.37884(10) 0.0420(3) Uani 1 d . . O21 O -0.3814(5) 0.9961(4) 0.3945(4) 0.0763(14) Uani 1 d . . O22 O -0.2384(7) 0.8875(4) 0.3552(4) 0.089(2) Uani 1 d . . O23 O -0.2458(6) 0.9954(5) 0.2941(4) 0.084(2) Uani 1 d . . O24 O -0.1323(5) 1.0587(4) 0.4705(4) 0.095(2) Uani 1 d . . Cl3 Cl 0.1062(2) 0.54122(11) 0.17244(11) 0.0493(3) Uani 1 d . . O31 O 0.1673(10) 0.5760(7) 0.2831(6) 0.069(3) Uiso 0.618(12) d P 3 O32 O -0.0274(10) 0.4681(7) 0.1326(7) 0.078(3) Uiso 0.618(12) d P 3 O33 O 0.0910(10) 0.6232(7) 0.1611(7) 0.085(3) Uiso 0.618(12) d P 3 O34 O 0.2008(12) 0.4899(9) 0.1226(8) 0.104(4) Uiso 0.618(12) d P 3 O31' O 0.1903(20) 0.5973(14) 0.1462(13) 0.106(6) Uiso 0.382(12) d P 4 O32' O 0.1484(21) 0.4518(15) 0.1505(15) 0.117(7) Uiso 0.382(12) d P 4 O33' O -0.0503(17) 0.5000(13) 0.1087(13) 0.088(5) Uiso 0.382(12) d P 4 O34' O 0.1214(20) 0.6092(14) 0.2816(13) 0.097(6) Uiso 0.382(12) d P 4 Cl4 Cl 0.2741(2) 0.21303(11) 0.13516(12) 0.0544(4) Uani 1 d . . O41 O 0.1714(7) 0.2680(4) 0.1341(4) 0.100(2) Uani 1 d . . O42 O 0.2228(6) 0.1184(4) 0.0366(5) 0.089(2) Uani 1 d . . O43 O 0.2794(10) 0.1905(7) 0.2122(6) 0.154(3) Uani 1 d . . O44 O 0.4050(7) 0.2691(5) 0.1514(6) 0.151(3) Uani 1 d . . O1 O 0.6420(5) 1.1979(4) 0.5989(3) 0.0707(13) Uani 1 d . . H11 H 0.6541(5) 1.1547(4) 0.5491(3) 0.106 Uiso 1 d R . H12 H 0.6943(5) 1.2524(4) 0.6137(3) 0.106 Uiso 1 d R . O2 O 0.1460(5) 0.4045(4) 0.3333(4) 0.0806(15) Uani 1 d . . H21 H 0.1448(5) 0.3785(4) 0.2850(4) 0.121 Uiso 1 d R . H22 H 0.1215(5) 0.4645(4) 0.3341(4) 0.121 Uiso 1 d R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0333(3) 0.0276(3) 0.0263(3) 0.0142(3) 0.0105(2) 0.0075(2) Ni2 0.0284(3) 0.0278(3) 0.0321(3) 0.0162(3) 0.0109(2) 0.0090(2) N11 0.037(2) 0.029(2) 0.036(2) 0.015(2) 0.009(2) 0.008(2) N12 0.042(2) 0.037(2) 0.056(3) 0.028(2) 0.025(2) 0.012(2) N13 0.035(2) 0.036(2) 0.047(3) 0.024(2) 0.013(2) 0.013(2) N14 0.044(3) 0.048(3) 0.058(3) 0.035(2) 0.026(2) 0.017(2) C12A 0.068(4) 0.039(3) 0.031(3) 0.017(2) 0.011(3) 0.016(3) C12B 0.082(4) 0.047(3) 0.051(3) 0.031(3) 0.039(3) 0.023(3) C13A 0.058(3) 0.029(3) 0.048(3) 0.017(2) 0.020(3) 0.016(2) C13B 0.047(3) 0.039(3) 0.054(3) 0.024(3) 0.024(3) 0.021(2) C14A 0.032(3) 0.044(3) 0.060(4) 0.022(3) 0.004(3) 0.007(2) C14B 0.043(3) 0.048(3) 0.076(4) 0.035(3) 0.028(3) 0.008(3) N21 0.043(2) 0.043(2) 0.033(2) 0.020(2) 0.017(2) 0.013(2) N22 0.040(2) 0.037(2) 0.039(2) 0.019(2) 0.009(2) 0.007(2) N23 0.057(3) 0.039(2) 0.036(2) 0.022(2) 0.015(2) 0.016(2) N24 0.044(3) 0.042(2) 0.040(2) 0.025(2) 0.011(2) 0.011(2) C22A 0.045(3) 0.066(4) 0.053(3) 0.031(3) 0.031(3) 0.015(3) C22B 0.047(3) 0.051(3) 0.053(3) 0.030(3) 0.022(3) 0.004(3) C23A 0.060(4) 0.038(3) 0.039(3) 0.014(2) 0.021(3) 0.023(3) C23B 0.062(4) 0.049(3) 0.049(3) 0.026(3) 0.018(3) 0.029(3) C24A 0.065(4) 0.052(3) 0.029(3) 0.017(3) 0.020(3) 0.016(3) C24B 0.054(3) 0.064(4) 0.035(3) 0.029(3) 0.011(3) 0.013(3) N31 0.038(2) 0.031(2) 0.028(2) 0.012(2) 0.012(2) 0.009(2) N32 0.054(3) 0.033(2) 0.034(2) 0.014(2) 0.014(2) 0.003(2) N33 0.034(2) 0.033(2) 0.031(2) 0.014(2) 0.009(2) 0.011(2) N34 0.036(2) 0.041(2) 0.038(2) 0.018(2) 0.011(2) 0.019(2) C32A 0.046(3) 0.047(3) 0.043(3) 0.021(3) 0.024(2) 0.007(2) C32B 0.046(3) 0.053(4) 0.050(3) 0.024(3) 0.018(3) -0.002(3) C33A 0.040(3) 0.040(3) 0.029(2) 0.015(2) 0.011(2) 0.018(2) C33B 0.037(7) 0.030(5) 0.031(5) 0.012(4) 0.009(4) 0.010(4) C33C 0.035(8) 0.025(7) 0.024(7) 0.012(5) 0.017(6) 0.014(6) C34A 0.036(3) 0.045(3) 0.034(3) 0.015(2) 0.006(2) 0.015(2) C34B 0.028(6) 0.033(5) 0.035(5) 0.014(4) 0.007(4) 0.008(4) C34C 0.037(9) 0.029(8) 0.027(7) 0.010(6) 0.008(6) 0.009(7) Cl1 0.0427(7) 0.0439(7) 0.0515(8) 0.0276(7) 0.0150(6) 0.0128(6) O11 0.043(2) 0.074(3) 0.092(4) 0.039(3) 0.014(2) 0.002(2) O12 0.059(3) 0.181(7) 0.148(6) 0.121(6) -0.006(4) 0.016(4) O13 0.172(6) 0.057(3) 0.186(7) 0.075(4) 0.118(6) 0.055(4) O14 0.178(7) 0.116(5) 0.097(5) 0.042(4) 0.096(5) 0.042(5) Cl2 0.0373(7) 0.0424(7) 0.0499(8) 0.0283(6) 0.0133(6) 0.0114(5) O21 0.045(2) 0.102(4) 0.084(3) 0.047(3) 0.028(2) 0.028(3) O22 0.142(5) 0.066(3) 0.102(4) 0.059(3) 0.067(4) 0.057(3) O23 0.090(4) 0.124(5) 0.092(4) 0.085(4) 0.048(3) 0.048(3) O24 0.058(3) 0.095(4) 0.080(4) 0.031(3) -0.005(3) -0.012(3) Cl3 0.0506(8) 0.0425(7) 0.0526(8) 0.0244(7) 0.0183(6) 0.0104(6) Cl4 0.0436(8) 0.0480(8) 0.0674(10) 0.0321(8) 0.0107(7) 0.0125(6) O41 0.110(4) 0.087(4) 0.074(3) 0.026(3) 0.007(3) 0.058(3) O42 0.078(3) 0.051(3) 0.103(4) 0.023(3) 0.022(3) 0.012(3) O43 0.218(9) 0.187(8) 0.143(6) 0.139(7) 0.068(6) 0.092(7) O44 0.096(5) 0.089(5) 0.168(7) 0.001(4) 0.065(5) -0.030(4) O1 0.079(3) 0.072(3) 0.060(3) 0.031(2) 0.031(2) 0.019(3) O2 0.081(3) 0.112(4) 0.084(3) 0.068(3) 0.040(3) 0.046(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N21 2.103(4) . ? Ni1 N22 2.118(4) . ? Ni1 N32 2.143(4) . ? Ni1 N23 2.144(4) . ? Ni1 N24 2.164(4) . ? Ni1 N31 2.165(4) . ? Ni2 N11 2.087(4) . ? Ni2 N13 2.096(4) . ? Ni2 N14 2.113(4) . ? Ni2 N34 2.132(4) . ? Ni2 N12 2.147(4) . ? Ni2 N33 2.202(4) . ? N11 C12A 1.472(7) . ? N11 C13A 1.482(6) . ? N11 C14A 1.485(7) . ? N12 C12B 1.473(7) . ? N13 C13B 1.451(7) . ? N14 C14B 1.479(7) . ? C12A C12B 1.516(9) . ? C13A C13B 1.521(8) . ? C14A C14B 1.508(8) . ? N21 C23A 1.469(7) . ? N21 C24A 1.471(7) . ? N21 C22A 1.502(7) . ? N22 C22B 1.476(7) . ? N23 C23B 1.472(7) . ? N24 C24B 1.475(7) . ? C22A C22B 1.495(8) . ? C23A C23B 1.529(8) . ? C24A C24B 1.509(8) . ? N31 C32A 1.495(6) . ? N31 C34A 1.502(6) . ? N31 C33A 1.511(6) . ? N32 C32B 1.485(7) . ? N33 C33C 1.46(2) . ? N33 C33B 1.468(11) . ? N34 C34C 1.42(2) . ? N34 C34B 1.488(11) . ? C32A C32B 1.505(8) . ? C33A C33B 1.468(11) . ? C33A C33C 1.556(14) . ? C33B C34B 1.50(2) . ? C33C C34C 1.55(3) . ? C34A C34B 1.497(11) . ? C34A C34C 1.60(2) . ? Cl1 O14 1.392(6) . ? Cl1 O13 1.397(5) . ? Cl1 O12 1.411(5) . ? Cl1 O11 1.418(5) . ? Cl2 O24 1.402(5) . ? Cl2 O22 1.405(5) . ? Cl2 O23 1.412(5) . ? Cl2 O21 1.425(4) . ? Cl3 O33 1.385(9) . ? Cl3 O31' 1.39(2) . ? Cl3 O32 1.403(9) . ? Cl3 O32' 1.41(2) . ? Cl3 O34 1.447(11) . ? Cl3 O34' 1.47(2) . ? Cl3 O31 1.474(9) . ? Cl3 O33' 1.48(2) . ? Cl4 O44 1.361(6) . ? Cl4 O43 1.400(6) . ? Cl4 O41 1.416(5) . ? Cl4 O42 1.431(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 N21 Ni1 N22 83.3(2) . . ? N21 Ni1 N32 98.7(2) . . ? N22 Ni1 N32 177.4(2) . . ? N21 Ni1 N23 82.4(2) . . ? N22 Ni1 N23 93.4(2) . . ? N32 Ni1 N23 88.5(2) . . ? N21 Ni1 N24 81.2(2) . . ? N22 Ni1 N24 91.0(2) . . ? N32 Ni1 N24 87.7(2) . . ? N23 Ni1 N24 162.4(2) . . ? N21 Ni1 N31 177.3(2) . . ? N22 Ni1 N31 95.4(2) . . ? N32 Ni1 N31 82.7(2) . . ? N23 Ni1 N31 95.3(2) . . ? N24 Ni1 N31 101.2(2) . . ? N11 Ni2 N13 82.8(2) . . ? N11 Ni2 N14 83.8(2) . . ? N13 Ni2 N14 92.0(2) . . ? N11 Ni2 N34 177.3(2) . . ? N13 Ni2 N34 94.6(2) . . ? N14 Ni2 N34 95.5(2) . . ? N11 Ni2 N12 82.0(2) . . ? N13 Ni2 N12 92.6(2) . . ? N14 Ni2 N12 164.4(2) . . ? N34 Ni2 N12 99.0(2) . . ? N11 Ni2 N33 99.6(2) . . ? N13 Ni2 N33 177.6(2) . . ? N14 Ni2 N33 88.5(2) . . ? N34 Ni2 N33 83.01(15) . . ? N12 Ni2 N33 87.6(2) . . ? C12A N11 C13A 113.4(4) . . ? C12A N11 C14A 112.2(4) . . ? C13A N11 C14A 110.7(4) . . ? C12A N11 Ni2 104.8(3) . . ? C13A N11 Ni2 110.1(3) . . ? C14A N11 Ni2 105.0(3) . . ? C12B N12 Ni2 109.5(3) . . ? C13B N13 Ni2 108.4(3) . . ? C14B N14 Ni2 108.5(3) . . ? N11 C12A C12B 110.1(4) . . ? N12 C12B C12A 110.5(4) . . ? N11 C13A C13B 112.8(4) . . ? N13 C13B C13A 109.9(4) . . ? N11 C14A C14B 109.9(4) . . ? N14 C14B C14A 110.3(4) . . ? C23A N21 C24A 111.5(4) . . ? C23A N21 C22A 110.9(4) . . ? C24A N21 C22A 112.7(4) . . ? C23A N21 Ni1 106.3(3) . . ? C24A N21 Ni1 106.3(3) . . ? C22A N21 Ni1 108.8(3) . . ? C22B N22 Ni1 107.5(3) . . ? C23B N23 Ni1 109.6(3) . . ? C24B N24 Ni1 110.3(3) . . ? C22B C22A N21 113.1(4) . . ? N22 C22B C22A 110.1(4) . . ? N21 C23A C23B 110.4(4) . . ? N23 C23B C23A 110.9(4) . . ? N21 C24A C24B 111.2(4) . . ? N24 C24B C24A 110.9(4) . . ? C32A N31 C34A 109.9(4) . . ? C32A N31 C33A 109.8(4) . . ? C34A N31 C33A 105.8(4) . . ? C32A N31 Ni1 103.9(3) . . ? C34A N31 Ni1 115.2(3) . . ? C33A N31 Ni1 112.3(3) . . ? C32B N32 Ni1 107.8(3) . . ? C33C N33 Ni2 102.7(5) . . ? C33B N33 Ni2 104.9(4) . . ? C34C N34 Ni2 102.9(6) . . ? C34B N34 Ni2 107.2(4) . . ? N31 C32A C32B 109.5(4) . . ? N32 C32B C32A 108.8(5) . . ? C33B C33A N31 105.0(5) . . ? N31 C33A C33C 104.6(6) . . ? N33 C33B C33A 120.6(9) . . ? N33 C33B C34B 112.3(12) . . ? C33A C33B C34B 103.1(10) . . ? N33 C33C C34C 104.9(16) . . ? N33 C33C C33A 115.2(12) . . ? C34C C33C C33A 100.6(13) . . ? C34B C34A N31 103.7(5) . . ? N31 C34A C34C 106.7(6) . . ? N34 C34B C33B 110.7(11) . . ? N34 C34B C34A 119.6(9) . . ? C33B C34B C34A 101.0(10) . . ? N34 C34C C33C 109.2(16) . . ? N34 C34C C34A 117.2(13) . . ? C33C C34C C34A 97.8(14) . . ? O14 Cl1 O13 110.4(4) . . ? O14 Cl1 O12 107.5(5) . . ? O13 Cl1 O12 108.9(5) . . ? O14 Cl1 O11 111.7(4) . . ? O13 Cl1 O11 110.1(4) . . ? O12 Cl1 O11 108.1(4) . . ? O24 Cl2 O22 108.1(4) . . ? O24 Cl2 O23 112.5(4) . . ? O22 Cl2 O23 108.8(3) . . ? O24 Cl2 O21 109.6(3) . . ? O22 Cl2 O21 108.9(4) . . ? O23 Cl2 O21 109.0(3) . . ? O33 Cl3 O32 111.9(6) . . ? O31' Cl3 O32' 108.4(11) . . ? O33 Cl3 O34 112.4(6) . . ? O32 Cl3 O34 108.3(6) . . ? O31' Cl3 O34' 108.0(10) . . ? O32' Cl3 O34' 114.9(11) . . ? O33 Cl3 O31 110.7(5) . . ? O32 Cl3 O31 105.7(5) . . ? O34 Cl3 O31 107.4(6) . . ? O31' Cl3 O33' 114.8(10) . . ? O32' Cl3 O33' 103.0(10) . . ? O34' Cl3 O33' 107.9(10) . . ? O44 Cl4 O43 112.3(6) . . ? O44 Cl4 O41 110.0(5) . . ? O43 Cl4 O41 108.0(5) . . ? O44 Cl4 O42 110.4(4) . . ? O43 Cl4 O42 108.5(5) . . ? O41 Cl4 O42 107.5(3) . . ? _refine_diff_density_max 1.463 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.091 #===END