# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global # always start the CIF with a "data_global" section _journal_name_full Chem.Commun. #============================================================================= # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 #============================================================================= _audit_creation_date '16. februar 2001' _audit_creation_method 'from SHELXL97 CIF and IUCr SHELXL97-template' _audit_update_record ; ? ; _publ_contact_author_name 'Finn K. Larsen' _publ_contact_author_address ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 Aarhus C Denmark ; _publ_contact_author_phone '45 8942 3897' _publ_contact_author_fax '45 8619 6199' _publ_contact_author_email kre@chem.au.dk _publ_section_title ; Theoretical studies on bi and tetranuclear Ni pivalate complexes ; _publ_section_references ; Sheldrick, G. M. (1997). SHelxs97. University of Gottigen, Germany. Siemens (1995) SMART and SAINT Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc. Madison, Winsconsin, USA ; _publ_section_figure_captions ; ? ; loop_ _publ_author_name 'R. Winpenny' 'F. P. Booy' 'Kirsten Christensen' 'Finn Larsen' 'Gopalan Rajaraman' ; G.A.Timco ; # e.g. Fig. 1. A view of (1). Displacement ellipsoids are drawn here # at the 30% probability level. # No Figures or Figure legends are required for Electronic-Paper # submissions. data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 268277' _chemical_name_systematic ; ? ; _chemical_name_common (Ni2(m-H2O)(O2CCMe3)4(HO2CCMe3)4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H78 Ni2 O17' _chemical_formula_weight 948.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.088(5) _cell_length_b 19.348(5) _cell_length_c 48.185(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 11269(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14374 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.3 _exptl_crystal_description sphere _exptl_crystal_colour 'light green' _exptl_crystal_size_rad '0.30 mm' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type 'multi-scan, SADABS, Sheldrick, 1996' _exptl_absorpt_correction_T_min 0.728017 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; Crystal source: Grigore Timco, The University of Manchester ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 76750 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -65 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 29.33 _reflns_number_total 14374 _reflns_number_gt 7325 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+12.4183P] 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 SHELXL _refine_ls_extinction_coef 0.00029(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14374 _refine_ls_number_parameters 631 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 3.761 _refine_ls_shift/su_mean 0.062 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 0.08011(3) 0.11226(2) 0.092353(9) 0.04586(13) Uani 1 1 d . . . Ni2 Ni 0.16549(4) 0.11013(2) 0.159246(8) 0.04298(13) Uani 1 1 d . . . O3 O 0.1353(2) 0.05227(11) 0.12455(5) 0.0409(5) Uani 1 1 d . . . H3A H 0.093(3) 0.017(2) 0.1299(8) 0.078(14) Uiso 1 1 d . . . H3B H 0.192(4) 0.031(2) 0.1185(9) 0.092(16) Uiso 1 1 d . . . O10 O 0.0370(2) 0.17641(12) 0.15552(5) 0.0563(6) Uani 1 1 d . . . O11 O -0.04834(19) 0.14911(12) 0.11571(5) 0.0572(6) Uani 1 1 d . . . O21 O 0.2706(2) 0.17429(11) 0.13811(5) 0.0549(6) Uani 1 1 d . . . O20 O 0.1737(2) 0.19760(12) 0.09976(5) 0.0572(6) Uani 1 1 d . . . O30 O 0.06846(18) 0.04623(11) 0.18350(4) 0.0465(5) Uani 1 1 d . . . O31 O 0.0047(2) -0.02742(13) 0.15166(5) 0.0644(7) Uani 1 1 d . . . O40 O 0.20106(18) 0.07481(12) 0.06607(5) 0.0520(6) Uani 1 1 d . A . O41 O 0.2939(2) 0.00794(14) 0.09561(5) 0.0637(7) Uani 1 1 d . A . O50 O 0.2103(2) 0.16681(12) 0.19454(5) 0.0576(6) Uani 1 1 d . . . O51 O 0.1001(3) 0.12144(15) 0.22646(6) 0.0784(9) Uani 1 1 d . . . H51 H 0.0873 0.0936 0.2140 0.118 Uiso 1 1 calc R . . O60 O 0.0095(2) 0.16752(14) 0.05971(6) 0.0654(7) Uani 1 1 d . . . O61 O 0.1321(3) 0.1524(2) 0.02648(6) 0.1018(12) Uani 1 1 d . . . H61 H 0.1492 0.1184 0.0357 0.153 Uiso 1 1 calc R . . O70 O -0.01851(19) 0.02827(13) 0.08033(5) 0.0564(6) Uani 1 1 d . . . O71 O -0.1855(2) 0.06395(18) 0.09319(9) 0.0989(12) Uani 1 1 d . . . H71 H -0.1524 0.1003 0.0959 0.148 Uiso 1 1 calc R . . O80 O 0.29917(18) 0.04550(11) 0.16850(5) 0.0488(6) Uani 1 1 d . . . O81 O 0.4424(2) 0.11448(14) 0.15901(7) 0.0786(9) Uani 1 1 d . . . H81 H 0.3940 0.1381 0.1518 0.118 Uiso 1 1 calc R . . C10 C -0.0435(3) 0.17934(17) 0.13924(8) 0.0509(9) Uani 1 1 d . . . C11 C -0.1434(3) 0.22316(19) 0.14751(8) 0.0682(11) Uani 1 1 d D . . C12 C -0.2360(4) 0.1730(3) 0.15560(11) 0.115(2) Uani 1 1 d D . . H12A H -0.2534 0.1439 0.1401 0.172 Uiso 1 1 calc R . . H12B H -0.3006 0.1987 0.1609 0.172 Uiso 1 1 calc R . . H12C H -0.2122 0.1450 0.1709 0.172 Uiso 1 1 calc R . . C13 C -0.1149(4) 0.2684(2) 0.17301(10) 0.0998(17) Uani 1 1 d D . . H13A H -0.0994 0.2393 0.1886 0.150 Uiso 1 1 calc R . . H13B H -0.1764 0.2979 0.1773 0.150 Uiso 1 1 calc R . . H13C H -0.0511 0.2962 0.1689 0.150 Uiso 1 1 calc R . . C14 C -0.1771(6) 0.2682(3) 0.12322(11) 0.211(5) Uani 1 1 d D . . H14A H -0.1156 0.2965 0.1177 0.316 Uiso 1 1 calc R . . H14B H -0.2378 0.2973 0.1286 0.316 Uiso 1 1 calc R . . H14C H -0.1992 0.2395 0.1080 0.316 Uiso 1 1 calc R . . C20 C 0.2456(3) 0.21261(17) 0.11715(8) 0.0512(8) Uani 1 1 d . . . C21 C 0.3029(4) 0.2833(2) 0.11523(9) 0.0850(14) Uani 1 1 d D . . C22 C 0.2262(7) 0.3338(3) 0.13152(16) 0.235(6) Uani 1 1 d D . . H22A H 0.2135 0.3160 0.1498 0.352 Uiso 1 1 calc R . . H22B H 0.1569 0.3382 0.1220 0.352 Uiso 1 1 calc R . . H22C H 0.2611 0.3782 0.1328 0.352 Uiso 1 1 calc R . . C23 C 0.3096(5) 0.3082(3) 0.08550(10) 0.117(2) Uani 1 1 d D . . H23A H 0.3434 0.3531 0.0850 0.176 Uiso 1 1 calc R . . H23B H 0.2365 0.3109 0.0778 0.176 Uiso 1 1 calc R . . H23C H 0.3532 0.2764 0.0748 0.176 Uiso 1 1 calc R . . C24 C 0.4148(5) 0.2830(3) 0.12906(13) 0.164(4) Uani 1 1 d D . . H24A H 0.4073 0.2677 0.1479 0.246 Uiso 1 1 calc R . . H24B H 0.4451 0.3289 0.1288 0.246 Uiso 1 1 calc R . . H24C H 0.4634 0.2523 0.1192 0.246 Uiso 1 1 calc R . . C30 C 0.0116(3) -0.00643(16) 0.17630(8) 0.0477(8) Uani 1 1 d . . . C31 C -0.0472(3) -0.04687(19) 0.19943(8) 0.0599(10) Uani 1 1 d . . . C32 C 0.0403(4) -0.0768(3) 0.21889(12) 0.113(2) Uani 1 1 d . . . H32A H 0.0046 -0.1013 0.2337 0.169 Uiso 1 1 calc R . . H32B H 0.0842 -0.0399 0.2264 0.169 Uiso 1 1 calc R . . H32C H 0.0870 -0.1080 0.2088 0.169 Uiso 1 1 calc R . . C33 C -0.1182(4) 0.0035(3) 0.21660(10) 0.0988(16) Uani 1 1 d . . . H33A H -0.1667 0.0286 0.2045 0.148 Uiso 1 1 calc R . . H33B H -0.0709 0.0354 0.2262 0.148 Uiso 1 1 calc R . . H33C H -0.1613 -0.0220 0.2298 0.148 Uiso 1 1 calc R . . C34 C -0.1209(5) -0.1030(3) 0.18667(11) 0.121(2) Uani 1 1 d . . . H34A H -0.0755 -0.1396 0.1795 0.182 Uiso 1 1 calc R . . H34B H -0.1638 -0.0834 0.1719 0.182 Uiso 1 1 calc R . . H34C H -0.1697 -0.1210 0.2006 0.182 Uiso 1 1 calc R . . C40 C 0.2794(3) 0.03377(19) 0.07193(8) 0.0573(9) Uani 1 1 d D . . C41 C 0.3475(4) 0.0060(3) 0.04662(10) 0.0496(15) Uiso 0.664(8) 1 d PD A 1 C42 C 0.2746(6) -0.0375(4) 0.02791(13) 0.086(3) Uani 0.664(8) 1 d PD A 1 H42A H 0.2165 -0.0093 0.0204 0.129 Uiso 0.664(8) 1 calc PR A 1 H42B H 0.2430 -0.0747 0.0384 0.129 Uiso 0.664(8) 1 calc PR A 1 H42C H 0.3182 -0.0560 0.0130 0.129 Uiso 0.664(8) 1 calc PR A 1 C43 C 0.3931(9) 0.0672(4) 0.0303(2) 0.120(5) Uani 0.664(8) 1 d PD A 1 H43A H 0.3337 0.0900 0.0208 0.180 Uiso 0.664(8) 1 calc PR A 1 H43B H 0.4464 0.0510 0.0170 0.180 Uiso 0.664(8) 1 calc PR A 1 H43C H 0.4280 0.0990 0.0428 0.180 Uiso 0.664(8) 1 calc PR A 1 C44 C 0.4433(11) -0.0383(5) 0.0569(5) 0.107(6) Uani 0.664(8) 1 d PD A 1 H44A H 0.4914 -0.0491 0.0417 0.161 Uiso 0.664(8) 1 calc PR A 1 H44B H 0.4149 -0.0803 0.0648 0.161 Uiso 0.664(8) 1 calc PR A 1 H44C H 0.4839 -0.0133 0.0708 0.161 Uiso 0.664(8) 1 calc PR A 1 C4T C 0.3840(7) 0.0323(6) 0.0532(2) 0.056(3) Uiso 0.336(8) 1 d PD A 2 C45 C 0.4761(11) 0.0803(7) 0.0628(4) 0.128(9) Uani 0.336(8) 1 d PD A 2 H45A H 0.4473 0.1262 0.0650 0.192 Uiso 0.336(8) 1 calc PR A 2 H45B H 0.5342 0.0808 0.0492 0.192 Uiso 0.336(8) 1 calc PR A 2 H45C H 0.5050 0.0643 0.0802 0.192 Uiso 0.336(8) 1 calc PR A 2 C46 C 0.421(2) -0.0430(6) 0.0545(8) 0.082(9) Uani 0.336(8) 1 d PD A 2 H46A H 0.4825 -0.0498 0.0423 0.123 Uiso 0.336(8) 1 calc PR A 2 H46B H 0.3607 -0.0723 0.0488 0.123 Uiso 0.336(8) 1 calc PR A 2 H46C H 0.4419 -0.0543 0.0731 0.123 Uiso 0.336(8) 1 calc PR A 2 C47 C 0.3456(17) 0.0510(14) 0.0241(3) 0.26(3) Uani 0.336(8) 1 d PD A 2 H47A H 0.3851 0.0911 0.0177 0.395 Uiso 0.336(8) 1 calc PR A 2 H47B H 0.2678 0.0607 0.0243 0.395 Uiso 0.336(8) 1 calc PR A 2 H47C H 0.3598 0.0130 0.0117 0.395 Uiso 0.336(8) 1 calc PR A 2 C50 C 0.1749(3) 0.16626(16) 0.21795(8) 0.0472(8) Uani 1 1 d . B . C51 C 0.2140(3) 0.21845(18) 0.23952(7) 0.0571(9) Uani 1 1 d D . . C52 C 0.3394(4) 0.2217(4) 0.23935(13) 0.095(3) Uani 0.759(8) 1 d PD B 1 H52A H 0.3689 0.1787 0.2460 0.142 Uiso 0.759(8) 1 calc PR B 1 H52B H 0.3638 0.2586 0.2512 0.142 Uiso 0.759(8) 1 calc PR B 1 H52C H 0.3650 0.2298 0.2208 0.142 Uiso 0.759(8) 1 calc PR B 1 C53 C 0.1668(5) 0.2062(3) 0.26803(10) 0.083(2) Uani 0.759(8) 1 d PD B 1 H53A H 0.1950 0.1635 0.2753 0.125 Uiso 0.759(8) 1 calc PR B 1 H53B H 0.0876 0.2039 0.2669 0.125 Uiso 0.759(8) 1 calc PR B 1 H53C H 0.1878 0.2435 0.2801 0.125 Uiso 0.759(8) 1 calc PR B 1 C54 C 0.1715(6) 0.2913(2) 0.22958(12) 0.089(2) Uani 0.759(8) 1 d PD B 1 H54A H 0.0923 0.2928 0.2309 0.133 Uiso 0.759(8) 1 calc PR B 1 H54B H 0.1934 0.2987 0.2107 0.133 Uiso 0.759(8) 1 calc PR B 1 H54C H 0.2029 0.3266 0.2411 0.133 Uiso 0.759(8) 1 calc PR B 1 C55 C 0.2999(14) 0.1863(5) 0.2600(3) 0.130(11) Uiso 0.241(8) 1 d PD B 2 H55A H 0.3340 0.1468 0.2515 0.195 Uiso 0.241(8) 1 calc PR B 2 H55B H 0.2630 0.1723 0.2767 0.195 Uiso 0.241(8) 1 calc PR B 2 H55C H 0.3555 0.2200 0.2643 0.195 Uiso 0.241(8) 1 calc PR B 2 C56 C 0.2702(14) 0.2758(6) 0.22402(17) 0.085(7) Uiso 0.241(8) 1 d PD B 2 H56A H 0.3313 0.2574 0.2136 0.128 Uiso 0.241(8) 1 calc PR B 2 H56B H 0.2969 0.3096 0.2370 0.128 Uiso 0.241(8) 1 calc PR B 2 H56C H 0.2185 0.2971 0.2116 0.128 Uiso 0.241(8) 1 calc PR B 2 C57 C 0.1182(8) 0.2448(8) 0.2570(3) 0.119(10) Uiso 0.241(8) 1 d PD B 2 H57A H 0.0852 0.2069 0.2668 0.178 Uiso 0.241(8) 1 calc PR B 2 H57B H 0.0639 0.2658 0.2452 0.178 Uiso 0.241(8) 1 calc PR B 2 H57C H 0.1449 0.2784 0.2701 0.178 Uiso 0.241(8) 1 calc PR B 2 C60 C 0.0403(3) 0.17997(19) 0.03669(8) 0.0596(10) Uani 1 1 d . . . C61 C -0.0222(4) 0.2273(2) 0.01689(9) 0.0712(11) Uani 1 1 d . . . C62 C 0.0590(5) 0.2675(3) -0.00083(15) 0.154(3) Uani 1 1 d . . . H62A H 0.0990 0.2995 0.0106 0.232 Uiso 1 1 calc R . . H62B H 0.0195 0.2924 -0.0149 0.232 Uiso 1 1 calc R . . H62C H 0.1100 0.2360 -0.0094 0.232 Uiso 1 1 calc R . . C63 C -0.0979(5) 0.2751(3) 0.03301(11) 0.117(2) Uani 1 1 d . . . H63A H -0.1468 0.2481 0.0444 0.175 Uiso 1 1 calc R . . H63B H -0.1405 0.3025 0.0203 0.175 Uiso 1 1 calc R . . H63C H -0.0543 0.3049 0.0446 0.175 Uiso 1 1 calc R . . C64 C -0.0908(6) 0.1815(4) -0.00171(13) 0.145(3) Uani 1 1 d . . . H64A H -0.0433 0.1496 -0.0112 0.218 Uiso 1 1 calc R . . H64B H -0.1295 0.2094 -0.0150 0.218 Uiso 1 1 calc R . . H64C H -0.1432 0.1563 0.0093 0.218 Uiso 1 1 calc R . . C70 C -0.1172(3) 0.0184(2) 0.08189(8) 0.0630(10) Uani 1 1 d . C . C71 C -0.1731(3) -0.0465(2) 0.07114(8) 0.0736(12) Uani 1 1 d D . . C72 C -0.2763(5) -0.0649(3) 0.08922(15) 0.112(3) Uani 0.797(9) 1 d PD C 1 H72A H -0.3234 -0.0251 0.0908 0.168 Uiso 0.797(9) 1 calc PR C 1 H72B H -0.2525 -0.0789 0.1074 0.168 Uiso 0.797(9) 1 calc PR C 1 H72C H -0.3164 -0.1020 0.0806 0.168 Uiso 0.797(9) 1 calc PR C 1 C73 C -0.2128(8) -0.0309(4) 0.04232(12) 0.157(5) Uani 0.797(9) 1 d PD C 1 H73A H -0.1506 -0.0281 0.0300 0.236 Uiso 0.797(9) 1 calc PR C 1 H73B H -0.2516 0.0124 0.0423 0.236 Uiso 0.797(9) 1 calc PR C 1 H73C H -0.2617 -0.0670 0.0362 0.236 Uiso 0.797(9) 1 calc PR C 1 C74 C -0.0965(6) -0.1084(3) 0.07245(19) 0.134(4) Uani 0.797(9) 1 d PD C 1 H74A H -0.0338 -0.1007 0.0606 0.201 Uiso 0.797(9) 1 calc PR C 1 H74B H -0.1354 -0.1489 0.0664 0.201 Uiso 0.797(9) 1 calc PR C 1 H74C H -0.0716 -0.1149 0.0912 0.201 Uiso 0.797(9) 1 calc PR C 1 C75 C -0.1049(12) -0.0734(8) 0.0459(3) 0.074(7) Uiso 0.203(9) 1 d PD C 2 H75A H -0.0894 -0.0357 0.0336 0.111 Uiso 0.203(9) 1 calc PR C 2 H75B H -0.1467 -0.1081 0.0363 0.111 Uiso 0.203(9) 1 calc PR C 2 H75C H -0.0366 -0.0929 0.0524 0.111 Uiso 0.203(9) 1 calc PR C 2 C76 C -0.2872(10) -0.0264(5) 0.0605(5) 0.146(15) Uiso 0.203(9) 1 d PD C 2 H76A H -0.2816 0.0149 0.0495 0.218 Uiso 0.203(9) 1 calc PR C 2 H76B H -0.3357 -0.0183 0.0759 0.218 Uiso 0.203(9) 1 calc PR C 2 H76C H -0.3164 -0.0631 0.0492 0.218 Uiso 0.203(9) 1 calc PR C 2 C77 C -0.180(2) -0.1031(6) 0.0927(3) 0.21(2) Uiso 0.203(9) 1 d PD C 2 H77A H -0.2462 -0.0971 0.1035 0.315 Uiso 0.203(9) 1 calc PR C 2 H77B H -0.1167 -0.1009 0.1046 0.315 Uiso 0.203(9) 1 calc PR C 2 H77C H -0.1823 -0.1472 0.0836 0.315 Uiso 0.203(9) 1 calc PR C 2 C80 C 0.3984(3) 0.05558(18) 0.16826(8) 0.0536(9) Uani 1 1 d . . . C81 C 0.4822(3) 0.00371(18) 0.17859(8) 0.0592(10) Uani 1 1 d D . . C82 C 0.4240(3) -0.05751(19) 0.19194(9) 0.0772(12) Uani 1 1 d D . . H82A H 0.3799 -0.0417 0.2072 0.116 Uiso 1 1 calc R . . H82B H 0.4781 -0.0900 0.1985 0.116 Uiso 1 1 calc R . . H82C H 0.3772 -0.0795 0.1785 0.116 Uiso 1 1 calc R . . C83 C 0.5580(3) 0.0393(2) 0.19989(9) 0.0867(14) Uani 1 1 d D . . H83A H 0.5939 0.0781 0.1914 0.130 Uiso 1 1 calc R . . H83B H 0.6128 0.0070 0.2063 0.130 Uiso 1 1 calc R . . H83C H 0.5146 0.0549 0.2154 0.130 Uiso 1 1 calc R . . C84 C 0.5494(4) -0.0204(2) 0.15327(10) 0.0989(16) Uani 1 1 d D . . H84A H 0.5012 -0.0432 0.1404 0.148 Uiso 1 1 calc R . . H84B H 0.6060 -0.0519 0.1592 0.148 Uiso 1 1 calc R . . H84C H 0.5828 0.0189 0.1445 0.148 Uiso 1 1 calc 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 0.0453(2) 0.0511(2) 0.0412(2) 0.0022(2) 0.00238(19) 0.01149(19) Ni2 0.0539(2) 0.0364(2) 0.0386(2) 0.00263(18) 0.00486(19) -0.00463(19) O3 0.0429(12) 0.0390(12) 0.0407(13) 0.0001(10) 0.0050(10) 0.0020(11) O10 0.0650(16) 0.0499(14) 0.0541(16) 0.0018(12) 0.0094(13) 0.0123(12) O11 0.0507(14) 0.0613(15) 0.0595(16) -0.0090(13) 0.0034(12) 0.0133(12) O21 0.0641(15) 0.0459(13) 0.0547(15) 0.0118(12) 0.0092(12) -0.0103(11) O20 0.0687(16) 0.0516(14) 0.0513(15) 0.0113(12) 0.0078(13) 0.0013(12) O30 0.0524(13) 0.0449(12) 0.0422(13) 0.0003(10) 0.0062(10) -0.0125(10) O31 0.0803(18) 0.0578(15) 0.0549(16) -0.0072(13) 0.0037(14) -0.0236(13) O40 0.0480(13) 0.0655(15) 0.0424(13) 0.0055(12) 0.0064(11) 0.0187(12) O41 0.0628(16) 0.0746(17) 0.0538(16) 0.0149(14) 0.0121(13) 0.0252(14) O50 0.0753(17) 0.0490(13) 0.0484(15) -0.0015(12) 0.0069(13) -0.0188(12) O51 0.103(2) 0.082(2) 0.0508(16) -0.0108(14) 0.0180(16) -0.0429(17) O60 0.0650(16) 0.0793(18) 0.0519(16) 0.0115(14) -0.0009(13) 0.0229(14) O61 0.112(3) 0.134(3) 0.0594(19) 0.0272(19) 0.0231(18) 0.065(2) O70 0.0467(14) 0.0709(16) 0.0515(15) -0.0120(12) -0.0048(11) 0.0092(12) O71 0.0533(16) 0.100(2) 0.143(3) -0.052(2) 0.0075(18) 0.0083(16) O80 0.0466(13) 0.0481(13) 0.0519(14) 0.0061(11) -0.0067(11) -0.0097(11) O81 0.0564(16) 0.0620(17) 0.117(3) 0.0265(17) -0.0032(16) -0.0156(14) C10 0.059(2) 0.0399(17) 0.054(2) 0.0078(17) 0.0232(19) 0.0100(16) C11 0.075(3) 0.067(2) 0.062(3) 0.010(2) 0.021(2) 0.033(2) C12 0.064(3) 0.135(5) 0.146(5) -0.041(4) 0.043(3) -0.007(3) C13 0.095(3) 0.074(3) 0.131(5) -0.045(3) 0.044(3) 0.007(3) C14 0.293(10) 0.222(8) 0.117(5) 0.077(5) 0.079(6) 0.216(8) C20 0.060(2) 0.0417(18) 0.052(2) 0.0054(17) 0.0115(19) -0.0019(16) C21 0.113(4) 0.060(3) 0.082(3) 0.031(2) 0.002(3) -0.026(3) C22 0.371(14) 0.046(3) 0.287(11) -0.023(5) 0.182(11) -0.016(5) C23 0.135(5) 0.110(4) 0.107(4) 0.060(4) -0.006(4) -0.045(4) C24 0.178(6) 0.132(5) 0.182(7) 0.086(5) -0.082(6) -0.107(5) C30 0.0481(19) 0.0380(17) 0.057(2) 0.0057(17) -0.0001(17) -0.0027(15) C31 0.063(2) 0.057(2) 0.060(2) 0.0104(19) 0.0022(19) -0.0190(18) C32 0.112(4) 0.106(4) 0.120(5) 0.074(4) -0.006(4) -0.003(3) C33 0.085(3) 0.123(4) 0.089(4) -0.002(3) 0.034(3) -0.029(3) C34 0.162(5) 0.115(4) 0.087(4) 0.006(3) 0.015(4) -0.099(4) C40 0.049(2) 0.061(2) 0.062(3) 0.004(2) 0.0121(18) 0.0095(18) C42 0.121(6) 0.085(5) 0.051(4) -0.011(4) 0.017(4) 0.014(5) C43 0.128(10) 0.079(5) 0.153(12) 0.034(6) 0.082(8) -0.001(6) C44 0.063(7) 0.152(13) 0.106(11) -0.003(10) 0.015(7) 0.047(7) C45 0.109(14) 0.082(10) 0.19(2) 0.035(12) 0.097(15) 0.018(10) C46 0.072(13) 0.076(14) 0.10(2) 0.006(13) 0.053(12) 0.007(10) C47 0.15(2) 0.58(8) 0.061(12) 0.11(3) 0.071(14) 0.24(4) C50 0.0518(19) 0.0416(17) 0.048(2) 0.0000(16) -0.0025(17) 0.0015(15) C51 0.064(2) 0.059(2) 0.049(2) -0.0068(18) -0.0065(18) -0.0047(18) C52 0.071(4) 0.128(6) 0.084(5) -0.033(4) -0.014(3) -0.023(4) C53 0.122(5) 0.081(4) 0.047(3) -0.015(3) 0.000(3) -0.035(4) C54 0.149(7) 0.048(3) 0.068(4) -0.011(3) -0.008(4) 0.010(3) C60 0.071(3) 0.057(2) 0.050(2) -0.0036(19) -0.001(2) 0.0117(19) C61 0.080(3) 0.077(3) 0.056(3) 0.014(2) -0.010(2) 0.018(2) C62 0.127(5) 0.159(6) 0.176(7) 0.110(6) 0.026(5) 0.046(5) C63 0.145(5) 0.116(4) 0.090(4) 0.020(3) -0.001(4) 0.070(4) C64 0.150(6) 0.175(6) 0.111(5) -0.023(5) -0.068(4) 0.044(5) C70 0.058(2) 0.075(3) 0.056(2) -0.005(2) -0.0052(19) 0.009(2) C71 0.060(2) 0.084(3) 0.076(3) -0.021(2) -0.009(2) 0.000(2) C72 0.108(6) 0.091(5) 0.137(7) 0.014(4) 0.012(5) -0.015(4) C73 0.239(12) 0.162(8) 0.070(5) 0.034(5) -0.061(6) -0.104(8) C74 0.112(6) 0.090(5) 0.200(11) -0.046(6) -0.026(6) 0.029(4) C80 0.062(2) 0.0466(19) 0.052(2) -0.0007(17) 0.0050(18) -0.0081(17) C81 0.055(2) 0.051(2) 0.072(3) 0.0003(19) 0.0024(19) 0.0025(17) C82 0.079(3) 0.060(2) 0.092(3) 0.015(2) -0.010(2) 0.006(2) C83 0.073(3) 0.089(3) 0.098(4) 0.006(3) -0.022(3) -0.001(2) C84 0.103(4) 0.085(3) 0.109(4) 0.002(3) 0.033(3) 0.026(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 O20 2.033(3) . yes Ni1 O11 2.046(2) . yes Ni1 O3 2.049(2) . yes Ni1 O40 2.066(2) . yes Ni1 O60 2.085(2) . yes Ni1 O70 2.097(3) . yes Ni2 O10 2.022(3) . yes Ni2 O3 2.045(2) . yes Ni2 O21 2.048(2) . yes Ni2 O30 2.066(2) . yes Ni2 O80 2.091(2) . yes Ni2 O50 2.095(2) . yes O10 C10 1.250(4) . yes O11 C10 1.277(4) . yes O21 C20 1.289(4) . yes O20 C20 1.242(4) . yes O30 C30 1.277(4) . yes O31 C30 1.258(4) . yes O40 C40 1.267(4) . yes O41 C40 1.258(4) . yes O50 C50 1.206(4) . yes O51 C50 1.318(4) . yes O60 C60 1.195(4) . yes O61 C60 1.326(5) . yes O70 C70 1.211(4) . yes O71 C70 1.324(5) . yes O80 C80 1.215(4) . yes O81 C80 1.334(4) . yes C10 C11 1.529(5) . yes C11 C14 1.516(5) . yes C11 C12 1.532(5) . yes C11 C13 1.548(5) . yes C20 C21 1.535(5) . yes C21 C24 1.509(6) . yes C21 C23 1.514(5) . yes C21 C22 1.558(6) . yes C30 C31 1.536(5) . yes C31 C32 1.527(6) . yes C31 C34 1.533(6) . yes C31 C33 1.540(6) . yes C40 C4T 1.555(8) . yes C40 C41 1.567(6) . yes C41 C42 1.515(6) . yes C41 C44 1.523(7) . yes C41 C43 1.525(6) . yes C4T C47 1.520(8) . yes C4T C45 1.523(8) . yes C4T C46 1.524(8) . yes C50 C51 1.524(5) . yes C51 C53 1.506(5) . yes C51 C56 1.501(8) . yes C51 C52 1.518(5) . yes C51 C57 1.520(8) . yes C51 C55 1.561(8) . yes C51 C54 1.574(5) . yes C60 C61 1.523(5) . yes C61 C64 1.509(7) . yes C61 C62 1.516(7) . yes C61 C63 1.515(6) . yes C70 C71 1.517(6) . yes C71 C73 1.500(6) . yes C71 C74 1.516(6) . yes C71 C77 1.511(9) . yes C71 C76 1.523(9) . yes C71 C75 1.557(8) . yes C71 C72 1.563(6) . yes C80 C81 1.511(5) . yes C81 C82 1.521(4) . yes C81 C84 1.538(5) . yes C81 C83 1.538(5) . yes 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 O20 Ni1 O11 92.44(10) . . yes O20 Ni1 O3 98.39(10) . . yes O11 Ni1 O3 91.61(10) . . yes O20 Ni1 O40 89.93(10) . . yes O11 Ni1 O40 175.36(10) . . yes O3 Ni1 O40 91.99(9) . . yes O20 Ni1 O60 86.77(11) . . yes O11 Ni1 O60 85.73(10) . . yes O3 Ni1 O60 174.30(11) . . yes O40 Ni1 O60 90.42(10) . . yes O20 Ni1 O70 173.80(10) . . yes O11 Ni1 O70 89.46(10) . . yes O3 Ni1 O70 87.45(9) . . yes O40 Ni1 O70 87.77(10) . . yes O60 Ni1 O70 87.49(10) . . yes O10 Ni2 O3 97.92(10) . . yes O10 Ni2 O21 92.76(10) . . yes O3 Ni2 O21 92.06(10) . . yes O10 Ni2 O30 89.63(9) . . yes O3 Ni2 O30 91.93(9) . . yes O21 Ni2 O30 175.03(9) . . yes O10 Ni2 O80 172.56(10) . . yes O3 Ni2 O80 89.12(9) . . yes O21 Ni2 O80 89.37(10) . . yes O30 Ni2 O80 87.73(9) . . yes O10 Ni2 O50 86.49(10) . . yes O3 Ni2 O50 175.18(10) . . yes O21 Ni2 O50 85.75(9) . . yes O30 Ni2 O50 90.05(9) . . yes O80 Ni2 O50 86.56(10) . . yes Ni2 O3 Ni1 111.53(10) . . yes C10 O10 Ni2 133.0(2) . . yes C10 O11 Ni1 127.8(2) . . yes C20 O21 Ni2 126.4(2) . . yes C20 O20 Ni1 134.2(2) . . yes C30 O30 Ni2 129.0(2) . . yes C40 O40 Ni1 127.7(2) . . yes C50 O50 Ni2 131.5(2) . . yes C60 O60 Ni1 132.6(3) . . yes C70 O70 Ni1 131.7(3) . . yes C80 O80 Ni2 131.7(2) . . yes O10 C10 O11 124.9(3) . . yes O10 C10 C11 118.4(3) . . yes O11 C10 C11 116.7(4) . . yes C14 C11 C10 109.3(3) . . yes C14 C11 C12 111.4(4) . . yes C10 C11 C12 107.0(3) . . yes C14 C11 C13 110.3(4) . . yes C10 C11 C13 110.2(3) . . yes C12 C11 C13 108.6(3) . . yes O20 C20 O21 124.0(3) . . yes O20 C20 C21 118.9(3) . . yes O21 C20 C21 117.0(3) . . yes C24 C21 C23 111.8(4) . . yes C24 C21 C20 112.0(4) . . yes C23 C21 C20 111.4(4) . . yes C24 C21 C22 108.2(4) . . yes C23 C21 C22 108.0(4) . . yes C20 C21 C22 105.1(4) . . yes O31 C30 O30 123.3(3) . . yes O31 C30 C31 119.4(3) . . yes O30 C30 C31 117.3(3) . . yes C32 C31 C34 112.4(4) . . yes C32 C31 C30 108.6(3) . . yes C34 C31 C30 109.8(3) . . yes C32 C31 C33 107.2(4) . . yes C34 C31 C33 109.8(4) . . yes C30 C31 C33 109.0(3) . . yes O41 C40 O40 123.7(3) . . yes O41 C40 C4T 114.0(5) . . yes O40 C40 C4T 119.3(5) . . yes O41 C40 C41 119.8(3) . . yes O40 C40 C41 115.7(4) . . yes C4T C40 C41 27.6(4) . . yes C42 C41 C44 108.9(6) . . yes C42 C41 C43 109.6(5) . . yes C44 C41 C43 109.2(6) . . yes C42 C41 C40 110.4(4) . . yes C44 C41 C40 109.8(10) . . yes C43 C41 C40 108.9(5) . . yes C47 C4T C45 111.0(8) . . yes C47 C4T C46 110.8(8) . . yes C45 C4T C46 111.0(8) . . yes C47 C4T C40 106.5(10) . . yes C45 C4T C40 114.0(8) . . yes C46 C4T C40 103.3(17) . . yes O50 C50 O51 122.7(3) . . yes O50 C50 C51 121.5(3) . . yes O51 C50 C51 115.9(3) . . yes C53 C51 C56 137.9(4) . . yes C53 C51 C52 112.9(4) . . yes C56 C51 C52 60.9(7) . . yes C53 C51 C50 113.6(3) . . yes C56 C51 C50 106.9(3) . . yes C52 C51 C50 109.4(3) . . yes C53 C51 C57 42.2(7) . . yes C56 C51 C57 111.9(5) . . yes C52 C51 C57 138.6(4) . . yes C50 C51 C57 111.4(3) . . yes C53 C51 C55 67.2(7) . . yes C56 C51 C55 107.9(5) . . yes C52 C51 C55 49.9(7) . . yes C50 C51 C55 111.9(3) . . yes C57 C51 C55 106.9(5) . . yes C53 C51 C54 107.1(3) . . yes C56 C51 C54 48.3(7) . . yes C52 C51 C54 106.7(4) . . yes C50 C51 C54 106.5(3) . . yes C57 C51 C54 67.7(7) . . yes C55 C51 C54 140.0(4) . . yes O60 C60 O61 121.6(4) . . yes O60 C60 C61 123.3(4) . . yes O61 C60 C61 115.1(4) . . yes C64 C61 C62 108.8(5) . . yes C64 C61 C63 109.3(5) . . yes C62 C61 C63 111.6(4) . . yes C64 C61 C60 106.9(4) . . yes C62 C61 C60 109.9(4) . . yes C63 C61 C60 110.2(4) . . yes O70 C70 O71 122.3(4) . . yes O70 C70 C71 123.2(4) . . yes O71 C70 C71 114.5(3) . . yes C73 C71 C74 113.2(4) . . yes C73 C71 C77 139.7(5) . . yes C74 C71 C77 55.5(9) . . yes C73 C71 C70 107.0(4) . . yes C74 C71 C70 111.6(4) . . yes C77 C71 C70 113.0(4) . . yes C73 C71 C76 49.1(9) . . yes C74 C71 C76 140.3(5) . . yes C77 C71 C76 111.4(5) . . yes C70 C71 C76 107.9(4) . . yes C73 C71 C75 60.9(8) . . yes C74 C71 C75 56.3(8) . . yes C77 C71 C75 108.9(5) . . yes C70 C71 C75 107.9(4) . . yes C76 C71 C75 107.5(5) . . yes C73 C71 C72 107.8(4) . . yes C74 C71 C72 106.5(4) . . yes C77 C71 C72 53.6(10) . . yes C70 C71 C72 110.7(4) . . yes C76 C71 C72 61.5(9) . . yes C75 C71 C72 141.4(5) . . yes O80 C80 O81 122.3(3) . . yes O80 C80 C81 123.5(3) . . yes O81 C80 C81 114.2(3) . . yes C80 C81 C82 110.3(3) . . yes C80 C81 C84 107.1(3) . . yes C82 C81 C84 110.1(3) . . yes C80 C81 C83 108.8(3) . . yes C82 C81 C83 110.0(3) . . yes C84 C81 C83 110.5(3) . . yes _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 29.33 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.720 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.065