Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Christian Limberg' _publ_contact_author_email CHRISTIAN.LIMBERG@CHEMIE.HU-BERLIN.DE _publ_section_title ; A low-coordinate nickel(II) hydride complex and its reactivity ; loop_ _publ_author_name 'Christian Limberg' 'Stefan Pfirrmann' 'Burkhard Ziemer' # Attachment 'Pfirr13f.cif' data_pfirr13 _database_code_depnum_ccdc_archive 'CCDC 694380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (N,N'-Bis(2,6-di-isopropylphenyl)-pentan-2,4-di-iminato-N,N') -(4-dimethylaminopyridine-N)-nickel(I) ; _chemical_name_common ; (N,N'-Bis(2,6-di-isopropylphenyl)-pentan-2,4-di-iminato-N,N') -(4-dimethylaminopyridine-N)-nickel(i) ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H51 N4 Ni' _chemical_formula_sum 'C36 H51 N4 Ni' _chemical_formula_weight 598.52 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' 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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.6270(5) _cell_length_b 22.8973(13) _cell_length_c 16.9475(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.210(5) _cell_angle_gamma 90.00 _cell_volume 3347.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method none _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7425 _exptl_absorpt_correction_T_max 0.9305 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,201 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26845 _diffrn_reflns_av_R_equivalents 0.1074 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.25 _reflns_number_total 11309 _reflns_number_gt 8731 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (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. Although trying SIMU, C16, C65 and C67 could not refind anisotropicially. An explanation for this may be the bad crystal quality (multiple twinned), Which also holds for the low C-C bond precision and the low data completness. The large carbon atom Ueq(max)/Ueq(min) ratio may be results from rather anisotropic forces in crystal packing. ; _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^)+(0.1762P)^2^+3.6848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881. SHELXL97 set here the Flack parameter to 0.0 without su. It may be because our crystal was twice twinned and 3 BASF parameters had to be calculated. So the parameter becoms meaningless. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 11309 _refine_ls_number_parameters 729 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2655 _refine_ls_wR_factor_gt 0.2435 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1799(14) 0.1525(5) 0.1078(7) 0.029(2) Uani 1 1 d . . . C2 C 0.2515(14) 0.1403(4) 0.1830(6) 0.026(2) Uani 1 1 d . . . C3 C 0.1626(16) 0.1083(5) 0.2372(7) 0.035(3) Uani 1 1 d . . . H3 H 0.2106 0.0968 0.2857 0.042 Uiso 1 1 calc R . . C4 C 0.0127(19) 0.0931(6) 0.2237(8) 0.043(4) Uani 1 1 d . . . H4 H -0.0444 0.0734 0.2629 0.052 Uiso 1 1 calc R . . C5 C -0.0563(14) 0.1072(4) 0.1503(8) 0.033(3) Uani 1 1 d . . . H5 H -0.1620 0.0975 0.1406 0.040 Uiso 1 1 calc R . . C6 C 0.0260(15) 0.1350(4) 0.0915(6) 0.030(3) Uani 1 1 d . . . C7 C 0.4121(17) 0.1590(5) 0.2041(6) 0.038(3) Uani 1 1 d . . . H7 H 0.4563 0.1777 0.1562 0.046 Uiso 1 1 calc R . . C8 C 0.4137(18) 0.2053(7) 0.2703(10) 0.056(4) Uani 1 1 d . . . H8A H 0.3512 0.1913 0.3141 0.067 Uiso 1 1 d R . . H8B H 0.3689 0.2415 0.2493 0.067 Uiso 1 1 d R . . H8C H 0.5200 0.2126 0.2893 0.067 Uiso 1 1 d R . . C9 C 0.521(2) 0.1063(8) 0.2274(9) 0.062(5) Uani 1 1 d . . . H9A H 0.6288 0.1193 0.2262 0.075 Uiso 1 1 d R . . H9B H 0.5045 0.0746 0.1893 0.075 Uiso 1 1 d R . . H9C H 0.4971 0.0924 0.2805 0.075 Uiso 1 1 d R . . C10 C -0.0505(16) 0.1467(5) 0.0096(7) 0.037(3) Uani 1 1 d . . . H10 H 0.0326 0.1583 -0.0275 0.044 Uiso 1 1 calc R . . C11 C -0.129(2) 0.0926(7) -0.0228(10) 0.057(4) Uani 1 1 d . . . H11A H -0.1985 0.0749 0.0155 0.068 Uiso 1 1 d R . . H11B H -0.0482 0.0646 -0.0365 0.068 Uiso 1 1 d R . . H11C H -0.1888 0.1033 -0.0705 0.068 Uiso 1 1 d R . . C12 C -0.168(2) 0.1941(9) 0.0106(11) 0.070(5) Uani 1 1 d . . . H12A H -0.1910 0.2055 -0.0442 0.084 Uiso 1 1 d R . . H12B H -0.1275 0.2279 0.0399 0.084 Uiso 1 1 d R . . H12C H -0.2636 0.1805 0.0351 0.084 Uiso 1 1 d R . . C13 C 0.3501(14) 0.1614(5) -0.0003(7) 0.029(3) Uani 1 1 d . . . C14 C 0.4257(12) 0.1906(4) -0.0585(6) 0.021(2) Uani 1 1 d . . . H14 H 0.4962 0.1682 -0.0884 0.026 Uiso 1 1 calc R . . C15 C 0.4116(12) 0.2496(4) -0.0794(6) 0.021(2) Uani 1 1 d . . . C16 C 0.3755(14) 0.0955(5) 0.0048(6) 0.027(2) Uiso 1 1 d . . . H16A H 0.4415 0.0870 0.0511 0.032 Uiso 1 1 d R . . H16B H 0.4283 0.0830 -0.0430 0.032 Uiso 1 1 d R . . H16C H 0.2772 0.0744 0.0089 0.032 Uiso 1 1 d R . . C17 C 0.4942(13) 0.2701(5) -0.1525(6) 0.031(2) Uani 1 1 d . . . H17A H 0.4980 0.3129 -0.1526 0.037 Uiso 1 1 d R . . H17B H 0.4391 0.2565 -0.2002 0.037 Uiso 1 1 d R . . H17C H 0.6000 0.2545 -0.1515 0.037 Uiso 1 1 d R . . C18 C 0.2945(15) 0.3446(4) -0.0727(5) 0.025(2) Uani 1 1 d . . . C19 C 0.1893(14) 0.3523(4) -0.1358(6) 0.029(2) Uani 1 1 d . . . C20 C 0.1486(17) 0.4086(5) -0.1596(7) 0.038(3) Uani 1 1 d . . . H20 H 0.0757 0.4145 -0.2016 0.046 Uiso 1 1 calc R . . C21 C 0.2166(18) 0.4561(5) -0.1208(7) 0.043(3) Uani 1 1 d . . . H21 H 0.1889 0.4946 -0.1367 0.052 Uiso 1 1 calc R . . C22 C 0.3234(17) 0.4485(4) -0.0598(7) 0.042(3) Uani 1 1 d . . . H22 H 0.3690 0.4817 -0.0352 0.050 Uiso 1 1 calc R . . C23 C 0.3650(15) 0.3933(5) -0.0340(6) 0.031(3) Uani 1 1 d . . . C24 C 0.1075(15) 0.3008(5) -0.1766(6) 0.034(3) Uani 1 1 d . . . H24A H 0.1665 0.2646 -0.1621 0.040 Uiso 1 1 calc R . . C25 C -0.053(2) 0.2936(8) -0.1477(11) 0.078(6) Uani 1 1 d . . . H25A H -0.1043 0.2671 -0.1854 0.093 Uiso 1 1 d R . . H25B H -0.1074 0.3312 -0.1478 0.093 Uiso 1 1 d R . . H25C H -0.0552 0.2765 -0.0947 0.093 Uiso 1 1 d R . . C26 C 0.114(2) 0.3077(6) -0.2668(6) 0.050(4) Uani 1 1 d . . . H26A H 0.0936 0.2699 -0.2918 0.060 Uiso 1 1 d R . . H26B H 0.2181 0.3212 -0.2808 0.060 Uiso 1 1 d R . . H26C H 0.0370 0.3362 -0.2851 0.060 Uiso 1 1 d R . . C27 C 0.4854(16) 0.3835(4) 0.0346(6) 0.031(3) Uani 1 1 d . . . H27 H 0.4544 0.3476 0.0640 0.037 Uiso 1 1 calc R . . C28 C 0.643(2) 0.3723(8) -0.0007(10) 0.064(4) Uani 1 1 d . . . H28A H 0.6890 0.4093 -0.0172 0.076 Uiso 1 1 d R . . H28B H 0.6297 0.3465 -0.0466 0.076 Uiso 1 1 d R . . H28C H 0.7106 0.3535 0.0388 0.076 Uiso 1 1 d R . . C29 C 0.481(2) 0.4343(5) 0.0909(8) 0.059(5) Uani 1 1 d . . . H29A H 0.3752 0.4435 0.1075 0.070 Uiso 1 1 d R . . H29B H 0.5242 0.4681 0.0636 0.070 Uiso 1 1 d R . . H29C H 0.5454 0.4251 0.1374 0.070 Uiso 1 1 d R . . C30 C 0.0509(15) 0.3795(4) 0.0650(7) 0.031(3) Uani 1 1 d . . . H30 H 0.0339 0.3748 0.0098 0.037 Uiso 1 1 calc R . . C31 C -0.0127(14) 0.4286(4) 0.1002(7) 0.028(2) Uani 1 1 d . . . H31 H -0.0659 0.4573 0.0694 0.033 Uiso 1 1 calc R . . C32 C 0.0038(18) 0.4347(5) 0.1817(8) 0.043(3) Uani 1 1 d . . . C33 C 0.093(3) 0.3933(6) 0.2208(8) 0.077(6) Uani 1 1 d . . . H33 H 0.1126 0.3968 0.2759 0.093 Uiso 1 1 calc R . . C34 C 0.153(2) 0.3477(5) 0.1801(7) 0.063(5) Uani 1 1 d . . . H34 H 0.2128 0.3202 0.2093 0.076 Uiso 1 1 calc R . . C35 C -0.154(2) 0.5238(7) 0.1784(10) 0.058(4) Uani 1 1 d . . . H35A H -0.2379 0.5045 0.1486 0.070 Uiso 1 1 d R . . H35B H -0.0883 0.5454 0.1420 0.070 Uiso 1 1 d R . . H35C H -0.1980 0.5509 0.2166 0.070 Uiso 1 1 d R . . C36 C -0.044(2) 0.4848(7) 0.3062(7) 0.070(5) Uani 1 1 d . . . H36A H -0.1055 0.5180 0.3244 0.084 Uiso 1 1 d R . . H36B H 0.0654 0.4913 0.3196 0.084 Uiso 1 1 d R . . H36C H -0.0797 0.4490 0.3321 0.084 Uiso 1 1 d R . . C37 C 0.5812(13) 0.5951(4) 0.4034(6) 0.021(2) Uani 1 1 d . . . C38 C 0.5122(14) 0.6080(4) 0.3286(6) 0.029(2) Uani 1 1 d . . . C39 C 0.6021(15) 0.6370(5) 0.2746(6) 0.034(3) Uani 1 1 d . . . H39 H 0.5590 0.6451 0.2237 0.040 Uiso 1 1 calc R . . C40 C 0.7506(14) 0.6542(4) 0.2917(6) 0.023(2) Uani 1 1 d . . . H40 H 0.8093 0.6734 0.2525 0.028 Uiso 1 1 calc R . . C41 C 0.8163(15) 0.6440(4) 0.3658(6) 0.029(3) Uani 1 1 d . . . H41 H 0.9171 0.6582 0.3786 0.035 Uiso 1 1 calc R . . C42 C 0.7320(13) 0.6122(4) 0.4222(6) 0.026(2) Uani 1 1 d . . . C43 C 0.3481(15) 0.5875(5) 0.3074(7) 0.036(3) Uani 1 1 d . . . H43 H 0.3025 0.5664 0.3531 0.043 Uiso 1 1 calc R . . C44 C 0.358(2) 0.5459(6) 0.2345(9) 0.053(4) Uani 1 1 d . . . H44A H 0.4334 0.5150 0.2456 0.064 Uiso 1 1 calc R . . H44B H 0.3895 0.5683 0.1883 0.064 Uiso 1 1 calc R . . H44C H 0.2556 0.5284 0.2238 0.064 Uiso 1 1 calc R . . C45 C 0.2441(15) 0.6408(6) 0.2837(9) 0.039(3) Uani 1 1 d . . . H45A H 0.1378 0.6273 0.2730 0.047 Uiso 1 1 calc R . . H45B H 0.2848 0.6592 0.2362 0.047 Uiso 1 1 calc R . . H45C H 0.2443 0.6692 0.3269 0.047 Uiso 1 1 calc R . . C46 C 0.8107(15) 0.5981(5) 0.5027(7) 0.033(3) Uani 1 1 d . . . H46 H 0.7285 0.5854 0.5397 0.040 Uiso 1 1 calc R . . C47 C 0.8941(18) 0.6513(5) 0.5395(8) 0.044(3) Uani 1 1 d . . . H47A H 0.8222 0.6840 0.5457 0.053 Uiso 1 1 d R . . H47B H 0.9797 0.6634 0.5060 0.053 Uiso 1 1 d R . . H47C H 0.9354 0.6395 0.5914 0.053 Uiso 1 1 d R . . C48 C 0.9241(19) 0.5488(5) 0.4944(7) 0.045(4) Uani 1 1 d . . . H48A H 0.9767 0.5418 0.5454 0.054 Uiso 1 1 d R . . H48B H 1.0007 0.5596 0.4551 0.054 Uiso 1 1 d R . . H48C H 0.8699 0.5132 0.4774 0.054 Uiso 1 1 d R . . C49 C 0.4104(14) 0.5893(4) 0.5121(6) 0.024(2) Uani 1 1 d . . . C50 C 0.3367(14) 0.5587(4) 0.5714(5) 0.026(2) Uani 1 1 d . . . H50 H 0.2698 0.5814 0.6030 0.031 Uiso 1 1 calc R . . C51 C 0.3467(13) 0.4986(4) 0.5916(6) 0.023(2) Uani 1 1 d . . . C52 C 0.3991(17) 0.6542(5) 0.5120(7) 0.034(3) Uani 1 1 d . . . H52A H 0.5032 0.6713 0.5141 0.041 Uiso 1 1 d R . . H52B H 0.3409 0.6673 0.5578 0.041 Uiso 1 1 d R . . H52C H 0.3450 0.6666 0.4634 0.041 Uiso 1 1 d R . . C53 C 0.2566(14) 0.4810(5) 0.6644(6) 0.030(2) Uani 1 1 d . . . H53A H 0.2646 0.4386 0.6716 0.036 Uiso 1 1 d R . . H53B H 0.1474 0.4919 0.6571 0.036 Uiso 1 1 d R . . H53C H 0.2999 0.5008 0.7111 0.036 Uiso 1 1 d R . . C54 C 0.4499(13) 0.4036(4) 0.5806(7) 0.025(2) Uani 1 1 d . . . C55 C 0.5574(13) 0.3936(4) 0.6424(6) 0.027(2) Uani 1 1 d . . . C56 C 0.5869(14) 0.3349(4) 0.6645(6) 0.027(2) Uani 1 1 d . . . H56 H 0.6592 0.3273 0.7064 0.032 Uiso 1 1 calc R . . C57 C 0.5164(15) 0.2893(5) 0.6284(6) 0.034(3) Uani 1 1 d . . . H57 H 0.5382 0.2506 0.6457 0.040 Uiso 1 1 calc R . . C58 C 0.4113(14) 0.2986(4) 0.5658(6) 0.029(2) Uani 1 1 d . . . H58 H 0.3639 0.2664 0.5395 0.034 Uiso 1 1 calc R . . C59 C 0.3758(13) 0.3566(4) 0.5417(6) 0.025(2) Uani 1 1 d . . . C60 C 0.6421(13) 0.4426(4) 0.6847(6) 0.026(2) Uani 1 1 d . . . H60 H 0.5891 0.4798 0.6691 0.032 Uiso 1 1 calc R . . C61 C 0.8079(14) 0.4468(6) 0.6569(8) 0.038(3) Uani 1 1 d . . . H61A H 0.8079 0.4647 0.6044 0.045 Uiso 1 1 d R . . H61B H 0.8536 0.4077 0.6542 0.045 Uiso 1 1 d R . . H61C H 0.8689 0.4709 0.6938 0.045 Uiso 1 1 d R . . C62 C 0.6385(17) 0.4388(6) 0.7745(8) 0.044(3) Uani 1 1 d . . . H62A H 0.7090 0.4679 0.7980 0.053 Uiso 1 1 d R . . H62B H 0.6714 0.3996 0.7909 0.053 Uiso 1 1 d R . . H62C H 0.5329 0.4461 0.7923 0.053 Uiso 1 1 d R . . C63 C 0.2564(18) 0.3674(5) 0.4759(7) 0.039(3) Uani 1 1 d . . . H63 H 0.2899 0.4038 0.4483 0.047 Uiso 1 1 calc R . . C64 C 0.102(2) 0.3787(8) 0.5033(11) 0.064(4) Uani 1 1 d . . . H64A H 0.1028 0.4119 0.5398 0.076 Uiso 1 1 d R . . H64B H 0.0611 0.3442 0.5300 0.076 Uiso 1 1 d R . . H64C H 0.0358 0.3879 0.4572 0.076 Uiso 1 1 d R . . C65 C 0.249(2) 0.3203(7) 0.4140(9) 0.050(3) Uiso 1 1 d . . . H65A H 0.2240 0.2822 0.4367 0.059 Uiso 1 1 d R . . H65B H 0.3512 0.3186 0.3901 0.059 Uiso 1 1 d R . . H65C H 0.1706 0.3305 0.3735 0.059 Uiso 1 1 d R . . C66 C 0.6918(13) 0.3675(4) 0.4409(7) 0.025(2) Uani 1 1 d . . . H66 H 0.7065 0.3691 0.4966 0.030 Uiso 1 1 calc R . . C67 C 0.7546(15) 0.3222(5) 0.3997(6) 0.026(2) Uiso 1 1 d . . . H67 H 0.8081 0.2924 0.4282 0.032 Uiso 1 1 calc R . . C68 C 0.7434(15) 0.3179(4) 0.3178(6) 0.030(3) Uani 1 1 d . . . C69 C 0.651(3) 0.3611(6) 0.2817(7) 0.071(6) Uani 1 1 d . . . H69 H 0.6293 0.3593 0.2266 0.085 Uiso 1 1 calc R . . C70 C 0.591(3) 0.4056(6) 0.3249(8) 0.065(5) Uani 1 1 d . . . H70 H 0.5328 0.4348 0.2976 0.078 Uiso 1 1 calc R . . C71 C 0.9010(15) 0.2299(5) 0.3146(8) 0.039(3) Uani 1 1 d . . . H71A H 0.8350 0.2000 0.3380 0.046 Uiso 1 1 d R . . H71B H 0.9659 0.2479 0.3561 0.046 Uiso 1 1 d R . . H71C H 0.9672 0.2119 0.2751 0.046 Uiso 1 1 d R . . C72 C 0.792(2) 0.2717(7) 0.1899(7) 0.060(4) Uani 1 1 d . . . H72A H 0.8323 0.3084 0.1688 0.072 Uiso 1 1 d R . . H72B H 0.6823 0.2677 0.1749 0.072 Uiso 1 1 d R . . H72C H 0.8506 0.2389 0.1683 0.072 Uiso 1 1 d R . . N1 N 0.2592(12) 0.1873(4) 0.0507(5) 0.028(2) Uani 1 1 d . . . N2 N 0.3258(11) 0.2870(3) -0.0407(5) 0.026(2) Uani 1 1 d . . . N3 N 0.1344(13) 0.3381(4) 0.1027(5) 0.033(2) Uani 1 1 d . . . N4 N -0.0626(14) 0.4791(5) 0.2208(5) 0.045(3) Uani 1 1 d . . . N5 N 0.4988(11) 0.5604(4) 0.4594(5) 0.0224(18) Uani 1 1 d . . . N6 N 0.4265(10) 0.4608(3) 0.5505(5) 0.0247(19) Uani 1 1 d . . . N7 N 0.6075(13) 0.4108(4) 0.4033(6) 0.033(2) Uani 1 1 d . . . N8 N 0.8049(14) 0.2737(4) 0.2758(6) 0.045(3) Uani 1 1 d . . . Ni1 Ni 0.53259(16) 0.48062(4) 0.45587(7) 0.0247(3) Uani 1 1 d . . . Ni2 Ni 0.21838(16) 0.26776(5) 0.05424(7) 0.0253(3) Uani 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 C1 0.026(6) 0.030(5) 0.032(6) -0.001(4) 0.013(5) -0.001(4) C2 0.041(7) 0.016(4) 0.022(5) 0.003(4) 0.012(5) -0.008(4) C3 0.054(9) 0.024(5) 0.027(5) 0.009(4) 0.007(5) 0.001(5) C4 0.052(10) 0.032(6) 0.045(7) 0.012(5) 0.022(7) -0.005(6) C5 0.027(7) 0.013(5) 0.059(8) -0.007(5) 0.007(6) -0.001(4) C6 0.042(8) 0.019(5) 0.028(5) -0.002(4) 0.009(5) -0.004(4) C7 0.055(9) 0.041(6) 0.018(5) 0.001(4) 0.008(5) -0.001(6) C8 0.033(9) 0.063(9) 0.072(10) -0.016(7) -0.024(7) 0.005(6) C9 0.076(13) 0.066(10) 0.046(8) 0.008(7) 0.007(8) -0.002(9) C10 0.041(8) 0.027(5) 0.044(6) 0.004(5) 0.003(6) 0.000(5) C11 0.069(12) 0.044(8) 0.057(9) -0.012(7) -0.020(8) -0.011(8) C12 0.051(11) 0.078(12) 0.079(12) 0.017(9) -0.025(9) 0.016(9) C13 0.024(7) 0.035(6) 0.028(6) -0.006(4) 0.003(5) -0.011(5) C14 0.019(6) 0.020(4) 0.025(5) -0.005(4) -0.003(4) -0.001(4) C15 0.009(5) 0.031(5) 0.022(5) -0.005(4) -0.008(4) 0.001(4) C17 0.023(6) 0.027(5) 0.043(6) 0.007(5) 0.012(5) 0.011(5) C18 0.045(7) 0.017(4) 0.013(4) -0.002(3) 0.009(5) 0.010(4) C19 0.037(7) 0.024(5) 0.025(5) 0.007(4) 0.007(5) 0.002(4) C20 0.052(9) 0.026(6) 0.037(6) 0.004(4) 0.005(6) 0.010(5) C21 0.080(10) 0.013(4) 0.037(6) 0.007(4) 0.008(7) 0.006(5) C22 0.075(10) 0.015(5) 0.036(6) -0.002(4) 0.016(6) -0.004(5) C23 0.045(8) 0.026(5) 0.021(5) 0.004(4) 0.000(5) -0.006(5) C24 0.043(8) 0.036(6) 0.022(5) -0.018(4) -0.003(5) 0.008(5) C25 0.095(16) 0.074(11) 0.064(10) -0.019(8) -0.011(10) -0.050(11) C26 0.094(13) 0.045(7) 0.011(5) 0.000(4) -0.011(6) 0.021(7) C27 0.048(8) 0.017(5) 0.028(5) -0.007(4) 0.007(5) -0.014(5) C28 0.055(11) 0.074(11) 0.061(9) 0.010(8) -0.013(8) -0.026(8) C29 0.126(15) 0.010(5) 0.039(7) -0.005(4) -0.030(8) -0.007(6) C30 0.043(8) 0.015(5) 0.034(6) -0.001(4) 0.009(6) -0.004(5) C31 0.036(7) 0.009(4) 0.040(6) -0.001(4) 0.012(5) 0.004(4) C32 0.070(10) 0.015(5) 0.044(7) 0.002(4) 0.014(7) 0.010(5) C33 0.17(2) 0.038(7) 0.025(6) 0.004(5) -0.003(9) 0.039(10) C34 0.145(17) 0.023(6) 0.021(6) 0.011(5) -0.006(7) 0.032(8) C35 0.047(9) 0.056(9) 0.071(10) -0.009(7) 0.001(8) 0.023(7) C36 0.142(16) 0.042(7) 0.026(6) -0.008(6) 0.027(8) 0.018(9) C37 0.032(6) 0.008(4) 0.023(5) 0.001(3) 0.000(4) 0.004(4) C38 0.033(7) 0.023(5) 0.030(5) -0.004(4) -0.002(5) 0.005(4) C39 0.054(9) 0.029(5) 0.018(5) 0.010(4) 0.015(5) 0.018(5) C40 0.020(6) 0.019(5) 0.031(5) 0.012(4) 0.008(5) 0.002(4) C41 0.038(7) 0.025(5) 0.026(5) 0.008(4) 0.009(5) 0.000(4) C42 0.024(6) 0.019(5) 0.035(6) 0.007(4) 0.005(5) 0.005(4) C43 0.036(8) 0.032(6) 0.040(7) 0.009(5) 0.001(6) -0.006(5) C44 0.057(10) 0.039(7) 0.062(9) -0.016(6) -0.024(7) 0.007(6) C45 0.010(6) 0.048(8) 0.059(8) -0.005(6) -0.003(6) 0.002(5) C46 0.030(7) 0.036(6) 0.034(6) 0.001(5) -0.003(5) -0.014(5) C47 0.057(9) 0.031(6) 0.045(7) -0.001(5) -0.003(7) -0.008(6) C48 0.081(11) 0.031(6) 0.022(5) -0.011(4) -0.014(6) 0.016(6) C49 0.043(7) 0.009(4) 0.018(5) -0.002(3) 0.010(5) 0.003(4) C50 0.047(7) 0.015(4) 0.015(4) 0.002(4) 0.003(5) 0.013(4) C51 0.029(6) 0.012(4) 0.029(5) 0.005(3) 0.000(5) 0.002(4) C52 0.047(8) 0.012(5) 0.044(7) 0.001(4) 0.011(6) 0.007(5) C53 0.041(7) 0.025(5) 0.023(5) -0.001(4) 0.004(4) -0.013(5) C54 0.015(6) 0.016(4) 0.044(6) 0.000(4) 0.009(5) 0.002(4) C55 0.025(6) 0.025(5) 0.029(5) -0.006(4) -0.002(5) 0.011(4) C56 0.032(7) 0.025(5) 0.025(5) 0.003(4) 0.000(5) 0.008(4) C57 0.051(8) 0.020(5) 0.030(6) 0.006(4) 0.011(5) 0.000(5) C58 0.036(7) 0.020(5) 0.030(6) 0.009(4) 0.000(5) 0.005(4) C59 0.032(6) 0.016(5) 0.027(5) 0.000(4) 0.000(5) 0.001(4) C60 0.024(6) 0.019(5) 0.036(6) 0.010(4) -0.009(5) 0.000(4) C61 0.021(7) 0.046(7) 0.046(7) -0.015(5) 0.000(5) -0.002(5) C62 0.045(9) 0.039(7) 0.048(7) -0.013(5) -0.011(6) -0.002(6) C63 0.056(10) 0.024(5) 0.037(6) 0.006(4) -0.005(6) -0.008(5) C64 0.041(10) 0.077(11) 0.073(10) 0.011(8) -0.014(8) -0.016(8) C66 0.021(6) 0.022(5) 0.034(6) -0.001(4) 0.002(5) 0.004(4) C68 0.055(8) 0.022(5) 0.014(5) -0.002(4) 0.018(5) 0.005(5) C69 0.157(18) 0.034(7) 0.022(6) 0.007(5) 0.013(8) 0.048(9) C70 0.132(17) 0.026(6) 0.036(7) 0.000(5) -0.004(8) 0.037(8) C71 0.027(7) 0.021(5) 0.068(8) -0.011(5) -0.002(6) 0.000(4) C72 0.116(13) 0.039(6) 0.026(6) -0.006(5) 0.014(7) 0.009(8) N1 0.031(6) 0.022(4) 0.032(5) 0.003(3) 0.001(4) 0.005(4) N2 0.032(6) 0.012(3) 0.033(5) 0.005(3) -0.001(4) 0.000(3) N3 0.052(7) 0.021(4) 0.028(5) -0.004(3) 0.003(4) -0.003(4) N4 0.085(8) 0.021(4) 0.030(4) -0.008(4) 0.014(5) 0.015(5) N5 0.018(5) 0.019(4) 0.031(5) -0.005(3) 0.002(4) -0.003(3) N6 0.026(5) 0.022(4) 0.026(4) 0.003(3) -0.004(4) 0.002(3) N7 0.045(7) 0.019(4) 0.035(5) 0.002(4) 0.006(5) 0.011(4) N8 0.065(8) 0.023(5) 0.048(6) -0.002(4) 0.009(5) 0.007(5) Ni1 0.0358(8) 0.0161(5) 0.0224(6) 0.0003(5) 0.0056(5) 0.0008(5) Ni2 0.0373(8) 0.0160(5) 0.0227(6) 0.0000(5) 0.0042(5) 0.0019(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 C1 C6 1.408(18) . ? C1 C2 1.432(17) . ? C1 N1 1.438(14) . ? C2 C3 1.413(14) . ? C2 C7 1.486(19) . ? C3 C4 1.35(2) . ? C3 H3 0.9500 . ? C4 C5 1.41(2) . ? C4 H4 0.9500 . ? C5 C6 1.390(15) . ? C5 H5 0.9500 . ? C6 C10 1.548(17) . ? C7 C8 1.544(18) . ? C7 C9 1.57(2) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.49(2) . ? C10 C11 1.510(19) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.319(15) . ? C13 C14 1.369(15) . ? C13 C16 1.526(16) . ? C14 C15 1.400(14) . ? C14 H14 0.9500 . ? C15 N2 1.317(13) . ? C15 C17 1.517(14) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.399(17) . ? C18 C23 1.423(15) . ? C18 N2 1.448(12) . ? C19 C20 1.394(15) . ? C19 C24 1.531(16) . ? C20 C21 1.394(19) . ? C20 H20 0.9500 . ? C21 C22 1.38(2) . ? C21 H21 0.9500 . ? C22 C23 1.382(16) . ? C22 H22 0.9500 . ? C23 C27 1.560(18) . ? C24 C25 1.49(2) . ? C24 C26 1.539(14) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.506(15) . ? C27 C28 1.52(2) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N3 1.345(16) . ? C30 C31 1.392(14) . ? C30 H30 0.9500 . ? C31 C32 1.393(17) . ? C31 H31 0.9500 . ? C32 N4 1.349(15) . ? C32 C33 1.38(2) . ? C33 C34 1.359(19) . ? C33 H33 0.9500 . ? C34 N3 1.335(16) . ? C34 H34 0.9500 . ? C35 N4 1.469(18) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N4 1.458(15) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.389(16) . ? C37 C38 1.419(15) . ? C37 N5 1.437(13) . ? C38 C39 1.382(15) . ? C38 C43 1.527(18) . ? C39 C40 1.366(18) . ? C39 H39 0.9500 . ? C40 C41 1.388(16) . ? C40 H40 0.9500 . ? C41 C42 1.414(14) . ? C41 H41 0.9500 . ? C42 C46 1.545(16) . ? C43 C45 1.561(18) . ? C43 C44 1.565(18) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.503(18) . ? C46 C47 1.539(16) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N5 1.359(13) . ? C49 C50 1.389(14) . ? C49 C52 1.488(13) . ? C50 C51 1.421(13) . ? C50 H50 0.9500 . ? C51 N6 1.314(13) . ? C51 C53 1.527(14) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.403(17) . ? C54 C59 1.408(15) . ? C54 N6 1.420(13) . ? C55 C56 1.417(14) . ? C55 C60 1.512(15) . ? C56 C57 1.349(17) . ? C56 H56 0.9500 . ? C57 C58 1.398(17) . ? C57 H57 0.9500 . ? C58 C59 1.420(14) . ? C58 H58 0.9500 . ? C59 C63 1.522(18) . ? C60 C61 1.518(16) . ? C60 C62 1.525(17) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.44(2) . ? C63 C65 1.505(19) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.369(15) . ? C66 N7 1.378(14) . ? C66 H66 0.9500 . ? C67 C68 1.392(15) . ? C67 H67 0.9500 . ? C68 N8 1.352(14) . ? C68 C69 1.405(18) . ? C69 C70 1.362(18) . ? C69 H69 0.9500 . ? C70 N7 1.338(17) . ? C70 H70 0.9500 . ? C71 N8 1.450(17) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 N8 1.459(15) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N1 Ni2 1.878(9) . ? N2 Ni2 1.925(8) . ? N3 Ni2 1.954(9) . ? N5 Ni1 1.851(8) . ? N6 Ni1 1.918(9) . ? N7 Ni1 1.947(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 120.4(9) . . ? C6 C1 N1 119.1(10) . . ? C2 C1 N1 120.3(10) . . ? C3 C2 C1 116.7(11) . . ? C3 C2 C7 120.6(11) . . ? C1 C2 C7 122.7(9) . . ? C4 C3 C2 123.6(12) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 118.4(10) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 121.8(12) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 118.9(11) . . ? C5 C6 C10 120.5(11) . . ? C1 C6 C10 120.6(9) . . ? C2 C7 C8 111.5(11) . . ? C2 C7 C9 112.8(11) . . ? C8 C7 C9 110.4(12) . . ? C2 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C9 C7 H7 107.3 . . ? C7 C8 H8A 109.3 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 110.4 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 108.9 . . ? C7 C9 H9B 109.2 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 110.3 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 107.5(14) . . ? C12 C10 C6 113.2(12) . . ? C11 C10 C6 111.4(10) . . ? C12 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C6 C10 H10 108.2 . . ? C10 C11 H11A 112.0 . . ? C10 C11 H11B 107.8 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 108.6 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 107.7 . . ? C10 C12 H12B 110.1 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 110.6 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 123.4(11) . . ? N1 C13 C16 119.6(9) . . ? C14 C13 C16 117.0(10) . . ? C13 C14 C15 127.9(10) . . ? C13 C14 H14 116.1 . . ? C15 C14 H14 116.1 . . ? N2 C15 C14 123.3(9) . . ? N2 C15 C17 118.9(9) . . ? C14 C15 C17 117.8(9) . . ? C13 C16 H16A 108.7 . . ? C13 C16 H16B 108.1 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 111.6 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.2 . . ? C15 C17 H17B 110.3 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.0 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.2(9) . . ? C19 C18 N2 120.9(10) . . ? C23 C18 N2 117.8(10) . . ? C20 C19 C18 119.5(11) . . ? C20 C19 C24 118.1(11) . . ? C18 C19 C24 122.2(9) . . ? C19 C20 C21 119.0(12) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 121.4(10) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 121.1(11) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 117.7(11) . . ? C22 C23 C27 122.1(10) . . ? C18 C23 C27 120.2(9) . . ? C25 C24 C19 111.1(10) . . ? C25 C24 C26 113.2(13) . . ? C19 C24 C26 110.0(10) . . ? C25 C24 H24A 107.4 . . ? C19 C24 H24A 107.4 . . ? C26 C24 H24A 107.4 . . ? C24 C25 H25A 105.3 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 112.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.2 . . ? C24 C26 H26B 109.2 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 110.1 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 114.7(13) . . ? C29 C27 C23 109.6(11) . . ? C28 C27 C23 108.5(10) . . ? C29 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C23 C27 H27 108.0 . . ? C27 C28 H28A 109.9 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.4 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 112.7 . . ? C27 C29 H29B 107.1 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 108.6 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 125.3(11) . . ? N3 C30 H30 117.3 . . ? C31 C30 H30 117.3 . . ? C30 C31 C32 118.2(11) . . ? C30 C31 H31 120.9 . . ? C32 C31 H31 120.9 . . ? N4 C32 C33 121.3(12) . . ? N4 C32 C31 121.8(11) . . ? C33 C32 C31 116.9(11) . . ? C34 C33 C32 119.8(13) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? N3 C34 C33 126.0(13) . . ? N3 C34 H34 117.0 . . ? C33 C34 H34 117.0 . . ? N4 C35 H35A 108.8 . . ? N4 C35 H35B 110.4 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.2 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.4 . . ? N4 C36 H36B 109.1 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.9 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 121.3(9) . . ? C42 C37 N5 118.5(9) . . ? C38 C37 N5 120.0(10) . . ? C39 C38 C37 117.4(11) . . ? C39 C38 C43 121.4(11) . . ? C37 C38 C43 121.1(10) . . ? C40 C39 C38 122.3(10) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C39 C40 C41 120.4(9) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C42 119.5(11) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C37 C42 C41 118.8(10) . . ? C37 C42 C46 122.4(9) . . ? C41 C42 C46 118.7(10) . . ? C38 C43 C45 110.3(10) . . ? C38 C43 C44 108.0(10) . . ? C45 C43 C44 108.1(11) . . ? C38 C43 H43 110.1 . . ? C45 C43 H43 110.1 . . ? C44 C43 H43 110.1 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C47 109.4(11) . . ? C48 C46 C42 110.4(9) . . ? C47 C46 C42 112.7(10) . . ? C48 C46 H46 108.0 . . ? C47 C46 H46 108.0 . . ? C42 C46 H46 108.0 . . ? C46 C47 H47A 110.9 . . ? C46 C47 H47B 109.9 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 107.6 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.3 . . ? C46 C48 H48B 108.9 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 110.2 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N5 C49 C50 120.1(8) . . ? N5 C49 C52 121.5(9) . . ? C50 C49 C52 118.2(9) . . ? C49 C50 C51 129.5(9) . . ? C49 C50 H50 115.2 . . ? C51 C50 H50 115.2 . . ? N6 C51 C50 122.7(9) . . ? N6 C51 C53 122.4(8) . . ? C50 C51 C53 114.9(9) . . ? C49 C52 H52A 109.9 . . ? C49 C52 H52B 109.8 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 108.7 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.1 . . ? C51 C53 H53B 109.6 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.8 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C59 120.8(9) . . ? C55 C54 N6 120.4(10) . . ? C59 C54 N6 118.5(10) . . ? C54 C55 C56 117.7(10) . . ? C54 C55 C60 122.6(9) . . ? C56 C55 C60 119.8(10) . . ? C57 C56 C55 122.5(11) . . ? C57 C56 H56 118.7 . . ? C55 C56 H56 118.7 . . ? C56 C57 C58 120.3(10) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C57 C58 C59 119.6(10) . . ? C57 C58 H58 120.2 . . ? C59 C58 H58 120.2 . . ? C54 C59 C58 119.1(11) . . ? C54 C59 C63 120.8(9) . . ? C58 C59 C63 120.1(10) . . ? C55 C60 C61 110.3(9) . . ? C55 C60 C62 114.3(9) . . ? C61 C60 C62 110.7(11) . . ? C55 C60 H60 107.1 . . ? C61 C60 H60 107.1 . . ? C62 C60 H60 107.1 . . ? C60 C61 H61A 109.1 . . ? C60 C61 H61B 109.9 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.9 . . ? C60 C62 H62B 108.8 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.6 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C65 109.0(13) . . ? C64 C63 C59 114.1(12) . . ? C65 C63 C59 114.4(11) . . ? C64 C63 H63 106.2 . . ? C65 C63 H63 106.2 . . ? C59 C63 H63 106.2 . . ? C63 C64 H64A 110.3 . . ? C63 C64 H64B 110.3 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 107.8 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 111.8 . . ? C63 C65 H65B 106.9 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.7 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 N7 121.3(10) . . ? C67 C66 H66 119.3 . . ? N7 C66 H66 119.3 . . ? C66 C67 C68 122.9(11) . . ? C66 C67 H67 118.6 . . ? C68 C67 H67 118.6 . . ? N8 C68 C67 123.9(11) . . ? N8 C68 C69 121.6(10) . . ? C67 C68 C69 114.3(10) . . ? C70 C69 C68 120.8(12) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? N7 C70 C69 124.4(12) . . ? N7 C70 H70 117.8 . . ? C69 C70 H70 117.8 . . ? N8 C71 H71A 109.7 . . ? N8 C71 H71B 110.3 . . ? H71A C71 H71B 109.5 . . ? N8 C71 H71C 108.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N8 C72 H72A 108.4 . . ? N8 C72 H72B 108.3 . . ? H72A C72 H72B 109.5 . . ? N8 C72 H72C 111.7 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C13 N1 C1 119.3(9) . . ? C13 N1 Ni2 125.2(8) . . ? C1 N1 Ni2 115.5(7) . . ? C15 N2 C18 120.5(8) . . ? C15 N2 Ni2 123.6(6) . . ? C18 N2 Ni2 115.6(6) . . ? C34 N3 C30 113.7(10) . . ? C34 N3 Ni2 120.8(8) . . ? C30 N3 Ni2 125.5(7) . . ? C32 N4 C36 121.1(12) . . ? C32 N4 C35 120.8(11) . . ? C36 N4 C35 118.0(11) . . ? C49 N5 C37 117.2(8) . . ? C49 N5 Ni1 126.3(7) . . ? C37 N5 Ni1 116.4(6) . . ? C51 N6 C54 119.3(8) . . ? C51 N6 Ni1 123.5(6) . . ? C54 N6 Ni1 116.9(7) . . ? C70 N7 C66 116.1(10) . . ? C70 N7 Ni1 119.8(8) . . ? C66 N7 Ni1 123.8(8) . . ? C68 N8 C71 120.4(10) . . ? C68 N8 C72 121.9(11) . . ? C71 N8 C72 117.4(11) . . ? N5 Ni1 N6 97.4(4) . . ? N5 Ni1 N7 151.5(4) . . ? N6 Ni1 N7 111.0(4) . . ? N1 Ni2 N2 96.0(4) . . ? N1 Ni2 N3 153.4(4) . . ? N2 Ni2 N3 110.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.6(15) . . . . ? N1 C1 C2 C3 176.9(9) . . . . ? C6 C1 C2 C7 -178.5(10) . . . . ? N1 C1 C2 C7 -4.2(16) . . . . ? C1 C2 C3 C4 -5.3(17) . . . . ? C7 C2 C3 C4 175.8(11) . . . . ? C2 C3 C4 C5 3.4(19) . . . . ? C3 C4 C5 C6 1.3(18) . . . . ? C4 C5 C6 C1 -3.7(16) . . . . ? C4 C5 C6 C10 176.4(10) . . . . ? C2 C1 C6 C5 1.7(15) . . . . ? N1 C1 C6 C5 -172.7(9) . . . . ? C2 C1 C6 C10 -178.5(10) . . . . ? N1 C1 C6 C10 7.2(15) . . . . ? C3 C2 C7 C8 -67.5(14) . . . . ? C1 C2 C7 C8 113.6(12) . . . . ? C3 C2 C7 C9 57.3(14) . . . . ? C1 C2 C7 C9 -121.7(12) . . . . ? C5 C6 C10 C12 72.9(15) . . . . ? C1 C6 C10 C12 -107.0(14) . . . . ? C5 C6 C10 C11 -48.4(16) . . . . ? C1 C6 C10 C11 131.7(13) . . . . ? N1 C13 C14 C15 -6.1(19) . . . . ? C16 C13 C14 C15 174.2(10) . . . . ? C13 C14 C15 N2 4.1(17) . . . . ? C13 C14 C15 C17 -173.1(11) . . . . ? C23 C18 C19 C20 -2.2(16) . . . . ? N2 C18 C19 C20 172.9(10) . . . . ? C23 C18 C19 C24 -177.8(10) . . . . ? N2 C18 C19 C24 -2.7(15) . . . . ? C18 C19 C20 C21 1.4(17) . . . . ? C24 C19 C20 C21 177.1(11) . . . . ? C19 C20 C21 C22 0.3(19) . . . . ? C20 C21 C22 C23 -1.1(19) . . . . ? C21 C22 C23 C18 0.2(17) . . . . ? C21 C22 C23 C27 179.9(11) . . . . ? C19 C18 C23 C22 1.4(16) . . . . ? N2 C18 C23 C22 -173.8(10) . . . . ? C19 C18 C23 C27 -178.3(10) . . . . ? N2 C18 C23 C27 6.5(15) . . . . ? C20 C19 C24 C25 -75.7(15) . . . . ? C18 C19 C24 C25 99.9(15) . . . . ? C20 C19 C24 C26 50.4(15) . . . . ? C18 C19 C24 C26 -134.0(11) . . . . ? C22 C23 C27 C29 29.4(16) . . . . ? C18 C23 C27 C29 -150.9(12) . . . . ? C22 C23 C27 C28 -96.4(13) . . . . ? C18 C23 C27 C28 83.2(13) . . . . ? N3 C30 C31 C32 -3.3(19) . . . . ? C30 C31 C32 N4 -175.9(13) . . . . ? C30 C31 C32 C33 5(2) . . . . ? N4 C32 C33 C34 177.2(18) . . . . ? C31 C32 C33 C34 -4(3) . . . . ? C32 C33 C34 N3 0(3) . . . . ? C42 C37 C38 C39 1.5(14) . . . . ? N5 C37 C38 C39 -174.2(9) . . . . ? C42 C37 C38 C43 178.2(9) . . . . ? N5 C37 C38 C43 2.4(14) . . . . ? C37 C38 C39 C40 -1.6(15) . . . . ? C43 C38 C39 C40 -178.2(10) . . . . ? C38 C39 C40 C41 -1.2(16) . . . . ? C39 C40 C41 C42 4.0(16) . . . . ? C38 C37 C42 C41 1.2(14) . . . . ? N5 C37 C42 C41 177.0(9) . . . . ? C38 C37 C42 C46 -179.3(9) . . . . ? N5 C37 C42 C46 -3.5(14) . . . . ? C40 C41 C42 C37 -4.0(15) . . . . ? C40 C41 C42 C46 176.5(10) . . . . ? C39 C38 C43 C45 -60.1(14) . . . . ? C37 C38 C43 C45 123.3(11) . . . . ? C39 C38 C43 C44 57.8(14) . . . . ? C37 C38 C43 C44 -118.7(11) . . . . ? C37 C42 C46 C48 103.8(12) . . . . ? C41 C42 C46 C48 -76.7(13) . . . . ? C37 C42 C46 C47 -133.5(11) . . . . ? C41 C42 C46 C47 46.0(14) . . . . ? N5 C49 C50 C51 5.3(19) . . . . ? C52 C49 C50 C51 -170.2(12) . . . . ? C49 C50 C51 N6 -4(2) . . . . ? C49 C50 C51 C53 176.1(11) . . . . ? C59 C54 C55 C56 -0.7(15) . . . . ? N6 C54 C55 C56 -173.8(9) . . . . ? C59 C54 C55 C60 178.7(10) . . . . ? N6 C54 C55 C60 5.6(15) . . . . ? C54 C55 C56 C57 0.2(16) . . . . ? C60 C55 C56 C57 -179.3(10) . . . . ? C55 C56 C57 C58 1.0(17) . . . . ? C56 C57 C58 C59 -1.7(16) . . . . ? C55 C54 C59 C58 0.0(15) . . . . ? N6 C54 C59 C58 173.2(9) . . . . ? C55 C54 C59 C63 178.6(10) . . . . ? N6 C54 C59 C63 -8.2(15) . . . . ? C57 C58 C59 C54 1.2(15) . . . . ? C57 C58 C59 C63 -177.4(10) . . . . ? C54 C55 C60 C61 -103.4(12) . . . . ? C56 C55 C60 C61 76.0(13) . . . . ? C54 C55 C60 C62 131.2(11) . . . . ? C56 C55 C60 C62 -49.4(14) . . . . ? C54 C59 C63 C64 -83.9(14) . . . . ? C58 C59 C63 C64 94.7(14) . . . . ? C54 C59 C63 C65 149.7(11) . . . . ? C58 C59 C63 C65 -31.8(16) . . . . ? N7 C66 C67 C68 2.6(18) . . . . ? C66 C67 C68 N8 179.8(12) . . . . ? C66 C67 C68 C69 -5(2) . . . . ? N8 C68 C69 C70 -179.5(17) . . . . ? C67 C68 C69 C70 6(3) . . . . ? C68 C69 C70 N7 -3(3) . . . . ? C14 C13 N1 C1 177.5(11) . . . . ? C16 C13 N1 C1 -2.9(17) . . . . ? C14 C13 N1 Ni2 -0.9(17) . . . . ? C16 C13 N1 Ni2 178.7(8) . . . . ? C6 C1 N1 C13 -95.8(13) . . . . ? C2 C1 N1 C13 89.8(13) . . . . ? C6 C1 N1 Ni2 82.7(11) . . . . ? C2 C1 N1 Ni2 -91.7(11) . . . . ? C14 C15 N2 C18 -169.3(10) . . . . ? C17 C15 N2 C18 7.9(15) . . . . ? C14 C15 N2 Ni2 4.4(14) . . . . ? C17 C15 N2 Ni2 -178.5(7) . . . . ? C19 C18 N2 C15 74.5(14) . . . . ? C23 C18 N2 C15 -110.2(11) . . . . ? C19 C18 N2 Ni2 -99.7(9) . . . . ? C23 C18 N2 Ni2 75.6(11) . . . . ? C33 C34 N3 C30 1(3) . . . . ? C33 C34 N3 Ni2 -176.5(17) . . . . ? C31 C30 N3 C34 0.1(19) . . . . ? C31 C30 N3 Ni2 178.0(9) . . . . ? C33 C32 N4 C36 -1(2) . . . . ? C31 C32 N4 C36 179.9(15) . . . . ? C33 C32 N4 C35 178.4(17) . . . . ? C31 C32 N4 C35 -1(2) . . . . ? C50 C49 N5 C37 -175.4(10) . . . . ? C52 C49 N5 C37 0.0(17) . . . . ? C50 C49 N5 Ni1 1.0(16) . . . . ? C52 C49 N5 Ni1 176.4(9) . . . . ? C42 C37 N5 C49 92.2(12) . . . . ? C38 C37 N5 C49 -92.0(12) . . . . ? C42 C37 N5 Ni1 -84.6(9) . . . . ? C38 C37 N5 Ni1 91.3(10) . . . . ? C50 C51 N6 C54 170.8(11) . . . . ? C53 C51 N6 C54 -9.7(16) . . . . ? C50 C51 N6 Ni1 -2.7(16) . . . . ? C53 C51 N6 Ni1 176.8(8) . . . . ? C55 C54 N6 C51 -75.3(13) . . . . ? C59 C54 N6 C51 111.4(12) . . . . ? C55 C54 N6 Ni1 98.6(10) . . . . ? C59 C54 N6 Ni1 -74.7(11) . . . . ? C69 C70 N7 C66 0(3) . . . . ? C69 C70 N7 Ni1 174.1(17) . . . . ? C67 C66 N7 C70 0.4(19) . . . . ? C67 C66 N7 Ni1 -173.5(9) . . . . ? C67 C68 N8 C71 -5.9(19) . . . . ? C69 C68 N8 C71 179.7(14) . . . . ? C67 C68 N8 C72 -179.0(13) . . . . ? C69 C68 N8 C72 7(2) . . . . ? C49 N5 Ni1 N6 -5.5(10) . . . . ? C37 N5 Ni1 N6 170.9(7) . . . . ? C49 N5 Ni1 N7 168.3(10) . . . . ? C37 N5 Ni1 N7 -15.4(13) . . . . ? C51 N6 Ni1 N5 6.3(10) . . . . ? C54 N6 Ni1 N5 -167.3(8) . . . . ? C51 N6 Ni1 N7 -170.5(9) . . . . ? C54 N6 Ni1 N7 15.9(9) . . . . ? C70 N7 Ni1 N5 -37.0(18) . . . . ? C66 N7 Ni1 N5 136.7(9) . . . . ? C70 N7 Ni1 N6 136.4(13) . . . . ? C66 N7 Ni1 N6 -49.9(11) . . . . ? C13 N1 Ni2 N2 6.5(11) . . . . ? C1 N1 Ni2 N2 -172.0(8) . . . . ? C13 N1 Ni2 N3 -170.2(10) . . . . ? C1 N1 Ni2 N3 11.4(15) . . . . ? C15 N2 Ni2 N1 -8.1(9) . . . . ? C18 N2 Ni2 N1 165.9(8) . . . . ? C15 N2 Ni2 N3 170.3(8) . . . . ? C18 N2 Ni2 N3 -15.7(9) . . . . ? C34 N3 Ni2 N1 42.9(18) . . . . ? C30 N3 Ni2 N1 -134.7(10) . . . . ? C34 N3 Ni2 N2 -133.5(12) . . . . ? C30 N3 Ni2 N2 48.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 2.500 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.116 data_pfirr14 _database_code_depnum_ccdc_archive 'CCDC 694381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(\m~2~-hydrido)-(N,N'-bis(2,6-di-isopropylphenyl) -pentan-2,4-di-iminato-N,N')-nickel(II) ; _chemical_name_common ; Bis(mu!2$-hydrido)-(N,N'-bis(2,6-di-isopropylphenyl) -pentan- 2,4-di-iminato-N,N')-nickel(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H84 N4 Ni2, C4 H10 O' _chemical_formula_sum 'C62 H94 N4 Ni2 O' _chemical_formula_weight 1028.83 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5933(13) _cell_length_b 18.187(2) _cell_length_c 28.265(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.742(15) _cell_angle_gamma 90.00 _cell_volume 5890.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method none _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6856 _exptl_absorpt_correction_T_max 0.8759 _exptl_absorpt_process_details ; The program XSHAPE1.02 (Stoe, 1997) was used for crystal optimisation before the numerical absorption correction basing on a Gaussian algorithsm and implemented in XRED1.08 (Stoe, 1997) was applied. In XSHAPE 150 strong reflections with 4 symmetry equivalents in each case were used for that optimisation. XSHAPE bases on the program HABITUS (Herrendorf, W. (1993). PhD thesis. Universit\"at Karlsruhe, Germany). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a \f-axis diffractometer supplied with an area detector. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_measurement_device 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f-rotation,\f-incr.=1.4\%,157 exposures' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31426 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10624 _reflns_number_gt 6456 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'IPDS2.87 (Stoe & Cie, 1997)' _computing_cell_refinement 'IPDS2.87 (Stoe & Cie, 1997)' _computing_data_reduction 'IPDS2.87 (Stoe & Cie, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (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. The large carbon and hyrogen atom Ueq(max)/Ueq(min) ratio may be results from very anisotropic forces of packing the crystal structure. ; _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^)+(0.0345P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00054(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10624 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_S_all 0.811 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1030(2) 0.22726(15) 0.35134(8) 0.0307(6) Uani 1 1 d . . . C2 C -0.1453(3) 0.27949(16) 0.38079(9) 0.0336(7) Uani 1 1 d . . . C3 C -0.2154(3) 0.25534(18) 0.41365(9) 0.0423(7) Uani 1 1 d . . . H3 H -0.2449 0.2901 0.4338 0.051 Uiso 1 1 calc R . . C4 C -0.2427(3) 0.18213(19) 0.41745(11) 0.0489(8) Uani 1 1 d . . . H4 H -0.2913 0.1668 0.4398 0.050(9) Uiso 1 1 calc R . . C5 C -0.1992(3) 0.13124(18) 0.38864(11) 0.0474(8) Uani 1 1 d . . . H5 H -0.2170 0.0807 0.3919 0.057 Uiso 1 1 calc R . . C6 C -0.1302(3) 0.15223(16) 0.35513(10) 0.0378(7) Uani 1 1 d . . . C7 C -0.1140(3) 0.36046(16) 0.37991(10) 0.0399(7) Uani 1 1 d . . . H7 H -0.0725 0.3690 0.3519 0.035(8) Uiso 1 1 calc R . . C8 C -0.0299(3) 0.3797(2) 0.42541(12) 0.0556(9) Uani 1 1 d . . . H8A H -0.0061 0.4312 0.4241 0.067 Uiso 1 1 calc R . . H8B H 0.0391 0.3480 0.4278 0.067 Uiso 1 1 calc R . . H8C H -0.0690 0.3720 0.4534 0.067 Uiso 1 1 calc R . . C9 C -0.2216(3) 0.41143(18) 0.37454(11) 0.0497(9) Uani 1 1 d . . . H9A H -0.1966 0.4625 0.3717 0.060 Uiso 1 1 calc R . . H9B H -0.2609 0.4064 0.4027 0.060 Uiso 1 1 calc R . . H9C H -0.2755 0.3977 0.3458 0.060 Uiso 1 1 calc R . . C10 C -0.0860(3) 0.09440(18) 0.32371(12) 0.0517(9) Uani 1 1 d . . . H10 H -0.0275 0.1189 0.3064 0.062 Uiso 1 1 calc R . . C11 C -0.1824(6) 0.0681(5) 0.2868(3) 0.223(5) Uani 1 1 d . . . H11A H -0.2094 0.1086 0.2650 0.268 Uiso 1 1 calc R . . H11B H -0.2472 0.0508 0.3025 0.268 Uiso 1 1 calc R . . H11C H -0.1543 0.0278 0.2687 0.268 Uiso 1 1 calc R . . C12 C -0.0246(7) 0.0325(3) 0.35181(18) 0.143(3) Uani 1 1 d . . . H12A H -0.0794 0.0069 0.3693 0.171 Uiso 1 1 calc R . . H12B H 0.0404 0.0520 0.3746 0.171 Uiso 1 1 calc R . . H12C H 0.0055 -0.0019 0.3300 0.171 Uiso 1 1 calc R . . C13 C 0.1052(3) 0.28121(15) 0.23835(8) 0.0299(6) Uani 1 1 d . . . C14 C -0.0070(3) 0.30285(16) 0.24198(9) 0.0337(7) Uani 1 1 d . . . H14 H -0.0428 0.3359 0.2182 0.031(7) Uiso 1 1 calc R . . C15 C -0.0743(3) 0.28147(15) 0.27689(9) 0.0321(6) Uani 1 1 d . . . C16 C 0.1529(3) 0.30307(17) 0.19323(9) 0.0406(7) Uani 1 1 d . . . H16A H 0.1814 0.2592 0.1785 0.049 Uiso 1 1 calc R . . H16B H 0.2172 0.3380 0.2014 0.049 Uiso 1 1 calc R . . H16C H 0.0908 0.3261 0.1707 0.049 Uiso 1 1 calc R . . C17 C -0.2031(3) 0.2949(2) 0.26550(11) 0.0502(9) Uani 1 1 d . . . H17A H -0.2450 0.2486 0.2679 0.060 Uiso 1 1 calc R . . H17B H -0.2219 0.3144 0.2329 0.060 Uiso 1 1 calc R . . H17C H -0.2265 0.3306 0.2883 0.060 Uiso 1 1 calc R . . C18 C 0.2678(3) 0.20166(15) 0.25745(8) 0.0289(6) Uani 1 1 d . . . C19 C 0.3832(2) 0.22785(15) 0.26585(8) 0.0314(6) Uani 1 1 d . . . C20 C 0.4695(3) 0.18717(17) 0.24868(10) 0.0404(7) Uani 1 1 d . . . H20 H 0.5481 0.2038 0.2546 0.046(9) Uiso 1 1 calc R . . C21 C 0.4433(3) 0.12295(17) 0.22308(10) 0.0447(8) Uani 1 1 d . . . H21 H 0.5028 0.0969 0.2105 0.054(9) Uiso 1 1 calc R . . C22 C 0.3315(3) 0.09733(17) 0.21608(10) 0.0412(8) Uani 1 1 d . . . H22 H 0.3148 0.0528 0.1989 0.049(9) Uiso 1 1 calc R . . C23 C 0.2411(3) 0.13395(15) 0.23319(9) 0.0338(7) Uani 1 1 d . . . C24 C 0.4173(3) 0.29857(16) 0.29276(10) 0.0379(7) Uani 1 1 d . . . H24 H 0.3451 0.3206 0.3022 0.030(7) Uiso 1 1 calc R . . C25 C 0.5030(3) 0.28285(19) 0.33886(11) 0.0513(9) Uani 1 1 d . . . H25A H 0.5726 0.2582 0.3307 0.062 Uiso 1 1 calc R . . H25B H 0.4653 0.2511 0.3599 0.062 Uiso 1 1 calc R . . H25C H 0.5258 0.3293 0.3553 0.062 Uiso 1 1 calc R . . C26 C 0.4691(3) 0.35434(18) 0.26122(12) 0.0541(9) Uani 1 1 d . . . H26A H 0.4105 0.3671 0.2337 0.065 Uiso 1 1 calc R . . H26B H 0.5375 0.3328 0.2499 0.065 Uiso 1 1 calc R . . H26C H 0.4925 0.3988 0.2799 0.065 Uiso 1 1 calc R . . C27 C 0.1192(3) 0.10131(16) 0.22657(10) 0.0421(8) Uani 1 1 d . . . H27 H 0.0730 0.1283 0.2482 0.048(9) Uiso 1 1 calc R . . C28 C 0.0568(4) 0.1099(2) 0.17553(13) 0.0705(12) Uani 1 1 d . . . H28A H 0.1025 0.0859 0.1535 0.085 Uiso 1 1 calc R . . H28B H 0.0482 0.1622 0.1676 0.085 Uiso 1 1 calc R . . H28C H -0.0205 0.0870 0.1726 0.085 Uiso 1 1 calc R . . C29 C 0.1213(4) 0.01976(19) 0.24035(12) 0.0605(10) Uani 1 1 d . . . H29A H 0.1641 0.0137 0.2728 0.073 Uiso 1 1 calc R . . H29B H 0.1599 -0.0085 0.2177 0.073 Uiso 1 1 calc R . . H29C H 0.0412 0.0020 0.2393 0.073 Uiso 1 1 calc R . . C30 C 0.2811(2) 0.40209(13) 0.44933(9) 0.0261(6) Uani 1 1 d . . . C31 C 0.2603(3) 0.45216(13) 0.41129(9) 0.0310(6) Uani 1 1 d . . . C32 C 0.2036(3) 0.51824(15) 0.41859(10) 0.0379(7) Uani 1 1 d . . . H32 H 0.1882 0.5525 0.3930 0.055(10) Uiso 1 1 calc R . . C33 C 0.1698(3) 0.53459(15) 0.46170(10) 0.0406(8) Uani 1 1 d . . . H33 H 0.1330 0.5802 0.4662 0.049 Uiso 1 1 calc R . . C34 C 0.1894(3) 0.48479(16) 0.49838(10) 0.0378(7) Uani 1 1 d . . . H34 H 0.1646 0.4964 0.5280 0.038(8) Uiso 1 1 calc R . . C35 C 0.2443(3) 0.41798(15) 0.49365(9) 0.0308(6) Uani 1 1 d . . . C36 C 0.2962(3) 0.43758(15) 0.36304(9) 0.0366(7) Uani 1 1 d . . . H36 H 0.3381 0.3893 0.3648 0.027(7) Uiso 1 1 calc R . . C37 C 0.1897(3) 0.43171(19) 0.32407(10) 0.0527(9) Uani 1 1 d . . . H37A H 0.1470 0.4784 0.3217 0.063 Uiso 1 1 calc R . . H37B H 0.1386 0.3923 0.3322 0.063 Uiso 1 1 calc R . . H37C H 0.2152 0.4207 0.2933 0.063 Uiso 1 1 calc R . . C38 C 0.3792(4) 0.4963(2) 0.34968(14) 0.0778(14) Uani 1 1 d . . . H38A H 0.4492 0.4978 0.3740 0.093 Uiso 1 1 calc R . . H38B H 0.3404 0.5443 0.3480 0.093 Uiso 1 1 calc R . . H38C H 0.4016 0.4845 0.3185 0.093 Uiso 1 1 calc R . . C39 C 0.2611(3) 0.36509(17) 0.53565(9) 0.0417(8) Uani 1 1 d . . . H39 H 0.2975 0.3191 0.5253 0.051(9) Uiso 1 1 calc R . . C40 C 0.1451(4) 0.3449(2) 0.55072(12) 0.0641(11) Uani 1 1 d . . . H40A H 0.0923 0.3259 0.5230 0.077 Uiso 1 1 calc R . . H40B H 0.1105 0.3886 0.5632 0.077 Uiso 1 1 calc R . . H40C H 0.1574 0.3070 0.5757 0.077 Uiso 1 1 calc R . . C41 C 0.3436(4) 0.3977(2) 0.57832(11) 0.0677(12) Uani 1 1 d . . . H41C H 0.3503 0.3636 0.6054 0.081 Uiso 1 1 calc R . . H41B H 0.3122 0.4447 0.5876 0.081 Uiso 1 1 calc R . . H41A H 0.4208 0.4057 0.5691 0.081 Uiso 1 1 calc R . . C42 C 0.4497(3) 0.32753(14) 0.46688(9) 0.0281(6) Uani 1 1 d . . . C43 C 0.5038(2) 0.26104(15) 0.47995(8) 0.0295(6) Uani 1 1 d . . . H43 H 0.5847 0.2631 0.4922 0.034(7) Uiso 1 1 calc R . . C44 C 0.4526(3) 0.19124(15) 0.47717(9) 0.0285(6) Uani 1 1 d . . . C45 C 0.5217(3) 0.39647(16) 0.47888(11) 0.0443(8) Uani 1 1 d . . . H45A H 0.5261 0.4242 0.4495 0.053 Uiso 1 1 calc R . . H45B H 0.6006 0.3828 0.4939 0.053 Uiso 1 1 calc R . . H45C H 0.4850 0.4270 0.5010 0.053 Uiso 1 1 calc R . . C46 C 0.5204(3) 0.13126(16) 0.50604(10) 0.0422(8) Uani 1 1 d . . . H46A H 0.5879 0.1527 0.5264 0.051 Uiso 1 1 calc R . . H46B H 0.5471 0.0952 0.4843 0.051 Uiso 1 1 calc R . . H46C H 0.4700 0.1069 0.5261 0.051 Uiso 1 1 calc R . . C47 C 0.3019(3) 0.10415(14) 0.45153(10) 0.0335(7) Uani 1 1 d . . . C48 C 0.3387(3) 0.04999(16) 0.42280(10) 0.0406(7) Uani 1 1 d . . . C49 C 0.2880(3) -0.02000(17) 0.42401(13) 0.0547(9) Uani 1 1 d . . . H49 H 0.3103 -0.0578 0.4040 0.066 Uiso 1 1 calc R . . C50 C 0.2074(3) -0.03499(19) 0.45328(15) 0.0628(11) Uani 1 1 d . . . H50 H 0.1762 -0.0832 0.4541 0.075 Uiso 1 1 calc R . . C51 C 0.1717(3) 0.01855(18) 0.48117(13) 0.0576(10) Uani 1 1 d . . . H51 H 0.1151 0.0075 0.5011 0.069 Uiso 1 1 calc R . . C52 C 0.2170(3) 0.08980(16) 0.48107(11) 0.0422(8) Uani 1 1 d . . . C53 C 0.4263(3) 0.06432(17) 0.38949(11) 0.0529(9) Uani 1 1 d . . . H53 H 0.4554 0.1159 0.3947 0.057(10) Uiso 1 1 calc R . . C54 C 0.5341(4) 0.0109(2) 0.39895(14) 0.0677(11) Uani 1 1 d . . . H54A H 0.5067 -0.0401 0.3972 0.081 Uiso 1 1 calc R . . H54B H 0.5779 0.0205 0.4308 0.081 Uiso 1 1 calc R . . H54C H 0.5848 0.0191 0.3747 0.081 Uiso 1 1 calc R . . C55 C 0.3719(5) 0.0572(2) 0.33977(13) 0.0868(15) Uani 1 1 d . . . H55A H 0.4304 0.0659 0.3187 0.104 Uiso 1 1 calc R . . H55B H 0.3090 0.0934 0.3328 0.104 Uiso 1 1 calc R . . H55C H 0.3398 0.0075 0.3343 0.104 Uiso 1 1 calc R . . C56 C 0.1713(3) 0.14769(18) 0.51169(11) 0.0468(8) Uani 1 1 d . . . H56 H 0.2176 0.1936 0.5094 0.045(8) Uiso 1 1 calc R . . C57 C 0.0435(3) 0.1646(2) 0.49155(13) 0.0611(10) Uani 1 1 d . . . H57A H 0.0129 0.2010 0.5119 0.073 Uiso 1 1 calc R . . H57B H -0.0027 0.1193 0.4909 0.073 Uiso 1 1 calc R . . H57C H 0.0389 0.1841 0.4590 0.073 Uiso 1 1 calc R . . C58 C 0.1843(4) 0.1258(2) 0.56434(13) 0.0791(13) Uani 1 1 d . . . H58A H 0.1542 0.1652 0.5827 0.095 Uiso 1 1 calc R . . H58B H 0.2669 0.1174 0.5767 0.095 Uiso 1 1 calc R . . H58C H 0.1401 0.0805 0.5675 0.095 Uiso 1 1 calc R . . C59 C 0.4819(4) 0.2145(2) 0.62938(16) 0.0867(14) Uani 1 1 d . . . H59A H 0.4210 0.2389 0.6442 0.104 Uiso 1 1 calc R . . H59B H 0.5008 0.1669 0.6450 0.104 Uiso 1 1 calc R . . H59C H 0.4537 0.2067 0.5953 0.104 Uiso 1 1 calc R . . C60 C 0.5861(4) 0.2605(2) 0.63484(13) 0.0719(11) Uani 1 1 d . . . H60A H 0.5660 0.3095 0.6207 0.086 Uiso 1 1 calc R . . H60B H 0.6157 0.2673 0.6693 0.086 Uiso 1 1 calc R . . C61 C 0.7706(4) 0.2745(3) 0.61396(17) 0.0887(14) Uani 1 1 d . . . H61A H 0.8080 0.2810 0.6476 0.106 Uiso 1 1 calc R . . H61B H 0.7456 0.3235 0.6010 0.106 Uiso 1 1 calc R . . C62 C 0.8544(5) 0.2433(3) 0.58624(18) 0.1093(18) Uani 1 1 d . . . H62A H 0.8171 0.2365 0.5530 0.131 Uiso 1 1 calc R . . H62B H 0.8814 0.1957 0.5999 0.131 Uiso 1 1 calc R . . H62C H 0.9210 0.2767 0.5871 0.131 Uiso 1 1 calc R . . N1 N -0.02711(18) 0.24997(12) 0.31777(6) 0.0280(5) Uani 1 1 d . . . N2 N 0.17264(18) 0.24235(12) 0.27225(6) 0.0259(5) Uani 1 1 d . . . N3 N 0.3397(2) 0.33243(11) 0.44458(7) 0.0239(5) Uani 1 1 d . . . N4 N 0.3498(2) 0.17788(11) 0.45135(7) 0.0274(5) Uani 1 1 d . . . Ni1 Ni 0.13703(3) 0.235651(18) 0.335993(10) 0.02393(9) Uani 1 1 d . . . H1 H 0.119(2) 0.2235(13) 0.3899(8) 0.029 Uiso 1 1 d . . . Ni2 Ni 0.25950(3) 0.250459(17) 0.411581(10) 0.02280(9) Uani 1 1 d . . . H2 H 0.277(2) 0.2238(13) 0.3556(8) 0.027 Uiso 1 1 d . . . O1 O 0.6728(3) 0.22861(14) 0.61246(9) 0.0688(7) Uani 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 C1 0.0175(17) 0.0451(17) 0.0304(13) -0.0044(11) 0.0062(11) -0.0055(12) C2 0.0214(18) 0.0462(17) 0.0341(14) -0.0041(12) 0.0071(12) -0.0034(12) C3 0.0327(19) 0.057(2) 0.0410(14) -0.0042(15) 0.0175(12) -0.0020(16) C4 0.036(2) 0.064(2) 0.0526(19) 0.0013(16) 0.0252(16) -0.0074(17) C5 0.042(2) 0.047(2) 0.057(2) -0.0023(14) 0.0206(17) -0.0132(15) C6 0.031(2) 0.0428(18) 0.0414(16) -0.0059(13) 0.0120(13) -0.0060(13) C7 0.034(2) 0.0458(18) 0.0437(17) -0.0108(13) 0.0166(14) -0.0044(14) C8 0.037(2) 0.061(2) 0.069(2) -0.0290(17) 0.0088(17) -0.0043(16) C9 0.051(3) 0.0448(19) 0.0559(19) -0.0049(15) 0.0163(17) 0.0006(15) C10 0.056(3) 0.044(2) 0.060(2) -0.0144(15) 0.0243(17) -0.0121(16) C11 0.098(6) 0.327(11) 0.231(8) -0.244(8) -0.018(5) 0.022(6) C12 0.251(9) 0.084(4) 0.115(4) 0.022(3) 0.098(5) 0.088(5) C13 0.0244(18) 0.0383(16) 0.0272(13) -0.0031(11) 0.0050(11) -0.0013(12) C14 0.0256(19) 0.0458(17) 0.0282(14) 0.0069(12) -0.0009(12) 0.0051(13) C15 0.0211(18) 0.0460(17) 0.0291(14) -0.0078(11) 0.0030(11) 0.0011(12) C16 0.036(2) 0.055(2) 0.0315(15) 0.0102(13) 0.0086(13) 0.0007(14) C17 0.022(2) 0.086(3) 0.0404(17) -0.0036(15) 0.0004(13) 0.0060(16) C18 0.0264(19) 0.0382(16) 0.0243(13) 0.0009(11) 0.0108(11) 0.0021(12) C19 0.0238(18) 0.0423(17) 0.0288(13) -0.0030(11) 0.0059(11) 0.0017(12) C20 0.027(2) 0.053(2) 0.0438(17) -0.0038(14) 0.0149(13) 0.0024(14) C21 0.043(2) 0.0501(19) 0.0457(17) -0.0047(14) 0.0219(15) 0.0113(16) C22 0.047(2) 0.0415(18) 0.0386(16) -0.0103(13) 0.0177(14) 0.0013(15) C23 0.038(2) 0.0382(17) 0.0270(13) -0.0021(11) 0.0099(12) -0.0008(13) C24 0.0208(19) 0.0493(19) 0.0451(16) -0.0109(13) 0.0095(13) -0.0030(13) C25 0.031(2) 0.073(2) 0.0497(18) -0.0174(16) 0.0041(14) -0.0071(16) C26 0.041(2) 0.051(2) 0.073(2) -0.0096(17) 0.0163(17) -0.0089(16) C27 0.039(2) 0.0450(19) 0.0432(16) -0.0177(13) 0.0100(14) -0.0089(14) C28 0.065(3) 0.070(3) 0.067(2) 0.0006(19) -0.018(2) -0.018(2) C29 0.061(3) 0.058(2) 0.063(2) 0.0000(17) 0.0132(19) -0.0175(19) C30 0.0206(17) 0.0203(13) 0.0364(14) -0.0060(10) 0.0013(11) -0.0015(11) C31 0.0288(18) 0.0261(14) 0.0377(15) -0.0045(12) 0.0033(12) -0.0005(12) C32 0.041(2) 0.0270(15) 0.0443(16) 0.0042(12) 0.0026(14) 0.0031(13) C33 0.042(2) 0.0265(16) 0.0522(18) -0.0082(13) 0.0022(15) 0.0076(13) C34 0.038(2) 0.0372(17) 0.0386(16) -0.0128(13) 0.0062(13) 0.0037(13) C35 0.0282(19) 0.0315(15) 0.0320(14) -0.0063(11) 0.0021(12) 0.0023(12) C36 0.046(2) 0.0267(15) 0.0395(16) 0.0011(11) 0.0128(14) 0.0006(13) C37 0.068(3) 0.052(2) 0.0358(17) 0.0053(14) -0.0005(16) 0.0189(18) C38 0.107(4) 0.050(2) 0.088(3) -0.003(2) 0.054(3) -0.022(2) C39 0.054(2) 0.0422(18) 0.0301(15) -0.0035(12) 0.0098(14) 0.0126(15) C40 0.074(3) 0.074(3) 0.049(2) 0.0157(17) 0.0257(19) 0.005(2) C41 0.077(3) 0.078(3) 0.0427(19) 0.0006(17) -0.0086(18) 0.025(2) C42 0.0263(19) 0.0276(14) 0.0311(14) -0.0050(11) 0.0070(12) -0.0012(11) C43 0.0185(16) 0.0373(16) 0.0318(12) -0.0016(11) 0.0011(10) 0.0013(12) C44 0.0232(18) 0.0331(15) 0.0293(14) 0.0051(11) 0.0045(12) 0.0035(11) C45 0.028(2) 0.0350(17) 0.067(2) -0.0121(14) -0.0018(15) -0.0061(13) C46 0.037(2) 0.0438(19) 0.0438(17) 0.0097(13) 0.0006(14) 0.0057(14) C47 0.032(2) 0.0238(15) 0.0434(16) 0.0063(12) 0.0028(13) -0.0012(12) C48 0.043(2) 0.0266(16) 0.0517(18) 0.0024(13) 0.0062(15) 0.0007(13) C49 0.058(3) 0.0256(17) 0.078(2) 0.0000(15) 0.0044(19) 0.0024(15) C50 0.048(3) 0.0333(19) 0.109(3) 0.0057(19) 0.017(2) -0.0108(16) C51 0.044(3) 0.040(2) 0.092(3) 0.0133(18) 0.020(2) -0.0058(16) C52 0.033(2) 0.0331(17) 0.060(2) 0.0131(14) 0.0064(15) -0.0054(13) C53 0.082(3) 0.0286(18) 0.0524(19) -0.0057(14) 0.0234(18) 0.0023(16) C54 0.068(3) 0.053(2) 0.087(3) 0.0042(19) 0.029(2) -0.004(2) C55 0.132(5) 0.073(3) 0.055(2) 0.011(2) 0.015(2) 0.016(3) C56 0.044(2) 0.0441(19) 0.0559(19) 0.0092(14) 0.0200(16) -0.0045(15) C57 0.047(3) 0.064(2) 0.076(2) 0.0037(18) 0.0236(19) 0.0062(18) C58 0.089(4) 0.093(3) 0.057(2) 0.015(2) 0.016(2) 0.001(3) C59 0.087(4) 0.080(3) 0.100(3) -0.021(2) 0.038(3) -0.013(3) C60 0.073(3) 0.071(3) 0.073(2) -0.009(2) 0.014(2) 0.005(2) C61 0.081(4) 0.079(3) 0.109(3) -0.034(3) 0.025(3) -0.022(3) C62 0.085(4) 0.117(4) 0.134(4) -0.057(4) 0.044(3) -0.029(3) N1 0.0195(13) 0.0373(13) 0.0280(10) -0.0046(10) 0.0058(8) -0.0035(10) N2 0.0205(13) 0.0335(12) 0.0239(9) -0.0010(9) 0.0037(8) -0.0005(10) N3 0.0207(15) 0.0238(12) 0.0271(11) -0.0035(8) 0.0034(9) 0.0013(9) N4 0.0266(16) 0.0248(12) 0.0311(12) 0.0034(9) 0.0057(10) 0.0003(9) Ni1 0.0195(2) 0.03095(19) 0.02173(15) -0.00262(13) 0.00460(12) -0.00179(14) Ni2 0.0220(2) 0.02217(16) 0.02390(15) -0.00091(13) 0.00250(12) -0.00111(14) O1 0.071(2) 0.0634(17) 0.0753(17) -0.0198(12) 0.0211(14) -0.0073(14) _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 C1 C2 1.400(4) . ? C1 C6 1.408(4) . ? C1 N1 1.449(3) . ? C2 C3 1.395(4) . ? C2 C7 1.518(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 C10 1.515(4) . ? C7 C8 1.531(4) . ? C7 C9 1.542(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.487(6) . ? C10 C12 1.494(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.342(3) . ? C13 C14 1.378(4) . ? C13 C16 1.518(3) . ? C14 C15 1.402(4) . ? C14 H14 0.9500 . ? C15 N1 1.330(3) . ? C15 C17 1.499(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.406(4) . ? C18 C23 1.421(4) . ? C18 N2 1.442(3) . ? C19 C20 1.390(4) . ? C19 C24 1.516(4) . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.363(5) . ? C21 H21 0.9500 . ? C22 C23 1.389(4) . ? C22 H22 0.9500 . ? C23 C27 1.519(4) . ? C24 C26 1.532(4) . ? C24 C25 1.541(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.520(4) . ? C27 C29 1.533(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.402(4) . ? C30 C35 1.413(4) . ? C30 N3 1.454(3) . ? C31 C32 1.400(4) . ? C31 C36 1.509(4) . ? C32 C33 1.368(4) . ? C32 H32 0.9500 . ? C33 C34 1.369(4) . ? C33 H33 0.9500 . ? C34 C35 1.387(4) . ? C34 H34 0.9500 . ? C35 C39 1.517(4) . ? C36 C38 1.522(4) . ? C36 C37 1.528(4) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.517(5) . ? C39 C41 1.540(5) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41C 0.9800 . ? C41 H41B 0.9800 . ? C41 H41A 0.9800 . ? C42 N3 1.336(3) . ? C42 C43 1.386(4) . ? C42 C45 1.516(4) . ? C43 C44 1.398(4) . ? C43 H43 0.9500 . ? C44 N4 1.322(3) . ? C44 C46 1.509(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.384(4) . ? C47 C52 1.408(4) . ? C47 N4 1.452(3) . ? C48 C49 1.405(4) . ? C48 C53 1.509(4) . ? C49 C50 1.366(5) . ? C49 H49 0.9500 . ? C50 C51 1.356(5) . ? C50 H50 0.9500 . ? C51 C52 1.398(4) . ? C51 H51 0.9500 . ? C52 C56 1.509(4) . ? C53 C55 1.456(5) . ? C53 C54 1.573(5) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C58 1.526(4) . ? C56 C57 1.535(5) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.459(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 O1 1.393(4) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 O1 1.404(5) . ? C61 C62 1.452(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N1 Ni1 1.912(2) . ? N2 Ni1 1.9125(18) . ? N3 Ni2 1.922(2) . ? N4 Ni2 1.935(2) . ? Ni1 Ni2 2.3939(6) . ? Ni1 H1 1.58(2) . ? Ni1 H2 1.65(3) . ? Ni2 H1 1.72(3) . ? Ni2 H2 1.70(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.6(2) . . ? C2 C1 N1 119.9(2) . . ? C6 C1 N1 119.4(2) . . ? C3 C2 C1 118.3(3) . . ? C3 C2 C7 118.8(2) . . ? C1 C2 C7 122.9(2) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C10 119.5(3) . . ? C1 C6 C10 121.9(3) . . ? C2 C7 C8 109.3(3) . . ? C2 C7 C9 113.2(3) . . ? C8 C7 C9 110.3(2) . . ? C2 C7 H7 108.0 . . ? C8 C7 H7 108.0 . . ? C9 C7 H7 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 112.2(5) . . ? C11 C10 C6 110.4(4) . . ? C12 C10 C6 112.8(3) . . ? C11 C10 H10 107.0 . . ? C12 C10 H10 107.0 . . ? C6 C10 H10 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 123.5(2) . . ? N2 C13 C16 119.4(3) . . ? C14 C13 C16 117.1(2) . . ? C13 C14 C15 127.3(3) . . ? C13 C14 H14 116.4 . . ? C15 C14 H14 116.4 . . ? N1 C15 C14 122.1(3) . . ? N1 C15 C17 121.4(2) . . ? C14 C15 C17 116.5(2) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.5(2) . . ? C19 C18 N2 121.8(2) . . ? C23 C18 N2 117.7(2) . . ? C20 C19 C18 118.5(3) . . ? C20 C19 C24 118.7(3) . . ? C18 C19 C24 122.8(2) . . ? C21 C20 C19 121.3(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 122.4(3) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C22 C23 C18 117.6(3) . . ? C22 C23 C27 120.5(3) . . ? C18 C23 C27 121.9(3) . . ? C19 C24 C26 111.4(2) . . ? C19 C24 C25 110.6(3) . . ? C26 C24 C25 110.8(3) . . ? C19 C24 H24 107.9 . . ? C26 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 112.1(3) . . ? C23 C27 C29 111.6(3) . . ? C28 C27 C29 109.1(3) . . ? C23 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C29 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 120.5(2) . . ? C31 C30 N3 121.6(2) . . ? C35 C30 N3 117.9(2) . . ? C32 C31 C30 118.3(2) . . ? C32 C31 C36 119.0(2) . . ? C30 C31 C36 122.7(2) . . ? C33 C32 C31 121.5(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C33 C34 C35 122.1(3) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C30 118.0(2) . . ? C34 C35 C39 119.1(2) . . ? C30 C35 C39 122.9(2) . . ? C31 C36 C38 111.9(2) . . ? C31 C36 C37 111.1(3) . . ? C38 C36 C37 110.0(3) . . ? C31 C36 H36 107.9 . . ? C38 C36 H36 107.9 . . ? C37 C36 H36 107.9 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C35 111.0(3) . . ? C40 C39 C41 110.2(3) . . ? C35 C39 C41 111.0(3) . . ? C40 C39 H39 108.1 . . ? C35 C39 H39 108.1 . . ? C41 C39 H39 108.1 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41C 109.5 . . ? C39 C41 H41B 109.5 . . ? H41C C41 H41B 109.5 . . ? C39 C41 H41A 109.5 . . ? H41C C41 H41A 109.5 . . ? H41B C41 H41A 109.5 . . ? N3 C42 C43 123.0(2) . . ? N3 C42 C45 120.3(2) . . ? C43 C42 C45 116.8(3) . . ? C42 C43 C44 127.3(3) . . ? C42 C43 H43 116.3 . . ? C44 C43 H43 116.3 . . ? N4 C44 C43 122.5(2) . . ? N4 C44 C46 121.1(3) . . ? C43 C44 C46 116.4(3) . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 121.4(3) . . ? C48 C47 N4 120.2(3) . . ? C52 C47 N4 118.4(2) . . ? C47 C48 C49 117.6(3) . . ? C47 C48 C53 122.7(3) . . ? C49 C48 C53 119.7(3) . . ? C50 C49 C48 121.5(3) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C51 C50 C49 120.4(3) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 121.1(3) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C51 C52 C47 118.0(3) . . ? C51 C52 C56 118.7(3) . . ? C47 C52 C56 123.3(3) . . ? C55 C53 C48 110.7(4) . . ? C55 C53 C54 109.0(3) . . ? C48 C53 C54 112.3(3) . . ? C55 C53 H53 108.2 . . ? C48 C53 H53 108.2 . . ? C54 C53 H53 108.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C56 C58 112.7(3) . . ? C52 C56 C57 109.3(3) . . ? C58 C56 C57 111.1(3) . . ? C52 C56 H56 107.8 . . ? C58 C56 H56 107.8 . . ? C57 C56 H56 107.8 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O1 C60 C59 110.9(3) . . ? O1 C60 H60A 109.5 . . ? C59 C60 H60A 109.5 . . ? O1 C60 H60B 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 108.1 . . ? O1 C61 C62 110.8(4) . . ? O1 C61 H61A 109.5 . . ? C62 C61 H61A 109.5 . . ? O1 C61 H61B 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 108.1 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C15 N1 C1 118.8(2) . . ? C15 N1 Ni1 123.60(18) . . ? C1 N1 Ni1 117.59(16) . . ? C13 N2 C18 116.84(19) . . ? C13 N2 Ni1 121.37(18) . . ? C18 N2 Ni1 121.64(15) . . ? C42 N3 C30 116.1(2) . . ? C42 N3 Ni2 122.27(17) . . ? C30 N3 Ni2 121.49(17) . . ? C44 N4 C47 118.7(2) . . ? C44 N4 Ni2 123.92(18) . . ? C47 N4 Ni2 117.31(18) . . ? N1 Ni1 N2 94.93(8) . . ? N1 Ni1 Ni2 131.00(6) . . ? N2 Ni1 Ni2 130.54(6) . . ? N1 Ni1 H1 90.5(10) . . ? N2 Ni1 H1 173.4(9) . . ? Ni2 Ni1 H1 45.8(9) . . ? N1 Ni1 H2 176.1(8) . . ? N2 Ni1 H2 88.9(8) . . ? Ni2 Ni1 H2 45.2(8) . . ? H1 Ni1 H2 85.6(12) . . ? N3 Ni2 N4 93.90(9) . . ? N3 Ni2 Ni1 134.27(6) . . ? N4 Ni2 Ni1 129.56(6) . . ? N3 Ni2 H1 139.1(8) . . ? N4 Ni2 H1 114.3(8) . . ? Ni1 Ni2 H1 41.4(7) . . ? N3 Ni2 H2 123.8(9) . . ? N4 Ni2 H2 102.4(8) . . ? Ni1 Ni2 H2 43.6(9) . . ? H1 Ni2 H2 80.1(12) . . ? C60 O1 C61 112.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.4(4) . . . . ? N1 C1 C2 C3 -178.2(2) . . . . ? C6 C1 C2 C7 177.0(3) . . . . ? N1 C1 C2 C7 -0.8(4) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C7 C2 C3 C4 -177.3(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C4 C5 C6 C1 1.1(5) . . . . ? C4 C5 C6 C10 -179.0(3) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? N1 C1 C6 C5 177.6(3) . . . . ? C2 C1 C6 C10 179.9(3) . . . . ? N1 C1 C6 C10 -2.3(4) . . . . ? C3 C2 C7 C8 69.8(4) . . . . ? C1 C2 C7 C8 -107.5(3) . . . . ? C3 C2 C7 C9 -53.6(4) . . . . ? C1 C2 C7 C9 129.1(3) . . . . ? C5 C6 C10 C11 73.5(6) . . . . ? C1 C6 C10 C11 -106.6(5) . . . . ? C5 C6 C10 C12 -52.8(5) . . . . ? C1 C6 C10 C12 127.0(4) . . . . ? N2 C13 C14 C15 -8.7(5) . . . . ? C16 C13 C14 C15 171.2(3) . . . . ? C13 C14 C15 N1 16.0(5) . . . . ? C13 C14 C15 C17 -163.1(3) . . . . ? C23 C18 C19 C20 1.9(4) . . . . ? N2 C18 C19 C20 -177.2(2) . . . . ? C23 C18 C19 C24 -178.2(2) . . . . ? N2 C18 C19 C24 2.7(4) . . . . ? C18 C19 C20 C21 1.2(4) . . . . ? C24 C19 C20 C21 -178.7(3) . . . . ? C19 C20 C21 C22 -2.6(5) . . . . ? C20 C21 C22 C23 1.0(5) . . . . ? C21 C22 C23 C18 2.0(4) . . . . ? C21 C22 C23 C27 -177.0(3) . . . . ? C19 C18 C23 C22 -3.4(4) . . . . ? N2 C18 C23 C22 175.7(2) . . . . ? C19 C18 C23 C27 175.6(2) . . . . ? N2 C18 C23 C27 -5.3(4) . . . . ? C20 C19 C24 C26 61.2(4) . . . . ? C18 C19 C24 C26 -118.7(3) . . . . ? C20 C19 C24 C25 -62.5(3) . . . . ? C18 C19 C24 C25 117.6(3) . . . . ? C22 C23 C27 C28 -75.7(4) . . . . ? C18 C23 C27 C28 105.3(3) . . . . ? C22 C23 C27 C29 47.0(4) . . . . ? C18 C23 C27 C29 -131.9(3) . . . . ? C35 C30 C31 C32 0.7(4) . . . . ? N3 C30 C31 C32 -179.9(3) . . . . ? C35 C30 C31 C36 -179.1(3) . . . . ? N3 C30 C31 C36 0.3(4) . . . . ? C30 C31 C32 C33 0.6(5) . . . . ? C36 C31 C32 C33 -179.5(3) . . . . ? C31 C32 C33 C34 -1.4(5) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C33 C34 C35 C30 0.4(5) . . . . ? C33 C34 C35 C39 -179.0(3) . . . . ? C31 C30 C35 C34 -1.2(4) . . . . ? N3 C30 C35 C34 179.3(3) . . . . ? C31 C30 C35 C39 178.2(3) . . . . ? N3 C30 C35 C39 -1.3(4) . . . . ? C32 C31 C36 C38 59.1(4) . . . . ? C30 C31 C36 C38 -121.0(3) . . . . ? C32 C31 C36 C37 -64.3(4) . . . . ? C30 C31 C36 C37 115.6(3) . . . . ? C34 C35 C39 C40 58.3(4) . . . . ? C30 C35 C39 C40 -121.1(3) . . . . ? C34 C35 C39 C41 -64.7(4) . . . . ? C30 C35 C39 C41 115.9(3) . . . . ? N3 C42 C43 C44 -7.2(4) . . . . ? C45 C42 C43 C44 173.1(3) . . . . ? C42 C43 C44 N4 15.8(4) . . . . ? C42 C43 C44 C46 -163.3(3) . . . . ? C52 C47 C48 C49 0.2(5) . . . . ? N4 C47 C48 C49 -179.1(3) . . . . ? C52 C47 C48 C53 177.8(3) . . . . ? N4 C47 C48 C53 -1.5(5) . . . . ? C47 C48 C49 C50 -1.6(5) . . . . ? C53 C48 C49 C50 -179.3(3) . . . . ? C48 C49 C50 C51 1.8(6) . . . . ? C49 C50 C51 C52 -0.6(6) . . . . ? C50 C51 C52 C47 -0.7(5) . . . . ? C50 C51 C52 C56 178.1(4) . . . . ? C48 C47 C52 C51 1.0(5) . . . . ? N4 C47 C52 C51 -179.7(3) . . . . ? C48 C47 C52 C56 -177.8(3) . . . . ? N4 C47 C52 C56 1.5(5) . . . . ? C47 C48 C53 C55 -113.4(4) . . . . ? C49 C48 C53 C55 64.2(4) . . . . ? C47 C48 C53 C54 124.6(3) . . . . ? C49 C48 C53 C54 -57.9(4) . . . . ? C51 C52 C56 C58 56.4(5) . . . . ? C47 C52 C56 C58 -124.8(3) . . . . ? C51 C52 C56 C57 -67.7(4) . . . . ? C47 C52 C56 C57 111.1(3) . . . . ? C14 C15 N1 C1 -178.0(2) . . . . ? C17 C15 N1 C1 1.1(4) . . . . ? C14 C15 N1 Ni1 4.2(4) . . . . ? C17 C15 N1 Ni1 -176.8(2) . . . . ? C2 C1 N1 C15 -78.6(3) . . . . ? C6 C1 N1 C15 103.6(3) . . . . ? C2 C1 N1 Ni1 99.4(3) . . . . ? C6 C1 N1 Ni1 -78.4(3) . . . . ? C14 C13 N2 C18 158.3(3) . . . . ? C16 C13 N2 C18 -21.5(4) . . . . ? C14 C13 N2 Ni1 -17.2(4) . . . . ? C16 C13 N2 Ni1 162.89(19) . . . . ? C19 C18 N2 C13 100.6(3) . . . . ? C23 C18 N2 C13 -78.4(3) . . . . ? C19 C18 N2 Ni1 -83.8(3) . . . . ? C23 C18 N2 Ni1 97.1(2) . . . . ? C43 C42 N3 C30 157.3(2) . . . . ? C45 C42 N3 C30 -23.0(4) . . . . ? C43 C42 N3 Ni2 -18.7(3) . . . . ? C45 C42 N3 Ni2 161.0(2) . . . . ? C31 C30 N3 C42 106.3(3) . . . . ? C35 C30 N3 C42 -74.2(3) . . . . ? C31 C30 N3 Ni2 -77.6(3) . . . . ? C35 C30 N3 Ni2 101.9(2) . . . . ? C43 C44 N4 C47 -178.4(2) . . . . ? C46 C44 N4 C47 0.6(4) . . . . ? C43 C44 N4 Ni2 3.2(4) . . . . ? C46 C44 N4 Ni2 -177.78(19) . . . . ? C48 C47 N4 C44 -80.9(3) . . . . ? C52 C47 N4 C44 99.8(3) . . . . ? C48 C47 N4 Ni2 97.6(3) . . . . ? C52 C47 N4 Ni2 -81.7(3) . . . . ? C15 N1 Ni1 N2 -21.1(2) . . . . ? C1 N1 Ni1 N2 161.02(19) . . . . ? C15 N1 Ni1 Ni2 138.84(18) . . . . ? C1 N1 Ni1 Ni2 -39.0(2) . . . . ? C13 N2 Ni1 N1 27.2(2) . . . . ? C18 N2 Ni1 N1 -148.2(2) . . . . ? C13 N2 Ni1 Ni2 -132.90(18) . . . . ? C18 N2 Ni1 Ni2 51.7(2) . . . . ? C42 N3 Ni2 N4 27.4(2) . . . . ? C30 N3 Ni2 N4 -148.4(2) . . . . ? C42 N3 Ni2 Ni1 -135.87(17) . . . . ? C30 N3 Ni2 Ni1 48.3(2) . . . . ? C44 N4 Ni2 N3 -20.1(2) . . . . ? C47 N4 Ni2 N3 161.5(2) . . . . ? C44 N4 Ni2 Ni1 144.46(18) . . . . ? C47 N4 Ni2 Ni1 -34.0(2) . . . . ? N1 Ni1 Ni2 N3 -85.28(13) . . . . ? N2 Ni1 Ni2 N3 68.02(13) . . . . ? N1 Ni1 Ni2 N4 116.55(13) . . . . ? N2 Ni1 Ni2 N4 -90.15(12) . . . . ? C59 C60 O1 C61 175.3(4) . . . . ? C62 C61 O1 C60 -174.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.334 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.050 data_pfirr19 _database_code_depnum_ccdc_archive 'CCDC 694382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (N,N'-Bis(2,6-di-isopropylphenyl)-pentan-2,4-di-iminato -N,N')-(propionitrile-N)-nickel(I) ; _chemical_name_common ; (N,N'-Bis(2,6-di-isopropylphenyl)-pentan-2,4-di-iminato - N,N')-(propionitrile-N)-nickel(i) ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H46 N3 Ni' _chemical_formula_sum 'C32 H46 N3 Ni' _chemical_formula_weight 531.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 8.812(2) _cell_length_b 9.1249(16) _cell_length_c 19.980(4) _cell_angle_alpha 87.59(2) _cell_angle_beta 80.83(3) _cell_angle_gamma 73.63(3) _cell_volume 1521.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method none _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.9017 _exptl_absorpt_correction_T_max 0.9491 _exptl_absorpt_process_details ; The correction was carried out by ABSCOR (Stoe, 1997), a modification of DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166. In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones. ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a \f-axis diffractometer supplied with an area detector. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_measurement_device 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f-oscill.,\f-incr.=1.2\%,220 exposures' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15879 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5185 _reflns_number_gt 4278 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'IPDS2.87 (Stoe & Cie, 1997)' _computing_cell_refinement 'IPDS2.87 (Stoe & Cie, 1997)' _computing_data_reduction 'IPDS2.87 (Stoe & Cie, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (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^)+(0.1037P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5185 _refine_ls_number_parameters 336 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2803(3) 0.5677(3) 0.70743(13) 0.0341(6) Uani 1 1 d . . . C2 C 0.2804(3) 0.5513(3) 0.77771(13) 0.0363(6) Uani 1 1 d . . . H2 H 0.3586 0.5858 0.7950 0.044 Uiso 1 1 calc R . . C3 C 0.1805(3) 0.4907(3) 0.82545(13) 0.0357(6) Uani 1 1 d . . . C4 C 0.3962(4) 0.6440(4) 0.66738(15) 0.0456(7) Uani 1 1 d . . . H4A H 0.4606 0.5770 0.6300 0.055 Uiso 1 1 calc R . . H4B H 0.4668 0.6641 0.6970 0.055 Uiso 1 1 calc R . . H4C H 0.3369 0.7407 0.6490 0.055 Uiso 1 1 calc R . . C5 C 0.2045(4) 0.4924(5) 0.89887(15) 0.0541(9) Uani 1 1 d . . . H5A H 0.1080 0.5584 0.9254 0.065 Uiso 1 1 calc R . . H5B H 0.2960 0.5317 0.9016 0.065 Uiso 1 1 calc R . . H5C H 0.2250 0.3884 0.9170 0.065 Uiso 1 1 calc R . . C6 C 0.1803(3) 0.5445(3) 0.60426(12) 0.0311(5) Uani 1 1 d . . . C7 C 0.2756(3) 0.4313(3) 0.55713(13) 0.0342(6) Uani 1 1 d . . . C8 C 0.2598(4) 0.4546(4) 0.48898(13) 0.0409(7) Uani 1 1 d . . . H8 H 0.3233 0.3801 0.4565 0.049 Uiso 1 1 calc R . . C9 C 0.1532(4) 0.5844(4) 0.46728(13) 0.0440(7) Uani 1 1 d . . . H9 H 0.1428 0.5969 0.4206 0.053 Uiso 1 1 calc R . . C10 C 0.0628(4) 0.6950(4) 0.51363(14) 0.0409(7) Uani 1 1 d . . . H10 H -0.0082 0.7843 0.4983 0.049 Uiso 1 1 calc R . . C11 C 0.0733(3) 0.6782(3) 0.58298(13) 0.0343(6) Uani 1 1 d . . . C12 C 0.3893(4) 0.2860(4) 0.58047(15) 0.0429(7) Uani 1 1 d . . . H12 H 0.4284 0.3126 0.6214 0.051 Uiso 1 1 calc R . . C13 C 0.3025(5) 0.1661(4) 0.6013(2) 0.0596(9) Uani 1 1 d . . . H13A H 0.3757 0.0767 0.6192 0.072 Uiso 1 1 calc R . . H13B H 0.2649 0.1358 0.5619 0.072 Uiso 1 1 calc R . . H13C H 0.2107 0.2080 0.6365 0.072 Uiso 1 1 calc R . . C14 C 0.5364(4) 0.2192(4) 0.5272(2) 0.0565(9) Uani 1 1 d . . . H14A H 0.6132 0.1373 0.5476 0.068 Uiso 1 1 calc R . . H14B H 0.5867 0.2997 0.5107 0.068 Uiso 1 1 calc R . . H14C H 0.5033 0.1780 0.4892 0.068 Uiso 1 1 calc R . . C15 C -0.0290(4) 0.8015(4) 0.63314(15) 0.0414(7) Uani 1 1 d . . . H15 H 0.0105 0.7785 0.6777 0.050 Uiso 1 1 calc R . . C16 C -0.2044(4) 0.7991(5) 0.6435(2) 0.0590(9) Uani 1 1 d . . . H16A H -0.2678 0.8774 0.6767 0.071 Uiso 1 1 calc R . . H16B H -0.2119 0.6984 0.6601 0.071 Uiso 1 1 calc R . . H16C H -0.2455 0.8198 0.6003 0.071 Uiso 1 1 calc R . . C17 C -0.0157(5) 0.9603(4) 0.6111(2) 0.0640(10) Uani 1 1 d . . . H17A H -0.0609 0.9886 0.5691 0.077 Uiso 1 1 calc R . . H17B H 0.0972 0.9596 0.6034 0.077 Uiso 1 1 calc R . . H17C H -0.0748 1.0346 0.6467 0.077 Uiso 1 1 calc R . . C18 C -0.0370(3) 0.3825(3) 0.86133(12) 0.0348(6) Uani 1 1 d . . . C19 C -0.1794(3) 0.4897(3) 0.89027(13) 0.0365(6) Uani 1 1 d . . . C20 C -0.2879(4) 0.4369(4) 0.93697(14) 0.0456(7) Uani 1 1 d . . . H20 H -0.3850 0.5070 0.9568 0.055 Uiso 1 1 calc R . . C21 C -0.2565(4) 0.2846(4) 0.95483(16) 0.0537(8) Uani 1 1 d . . . H21 H -0.3316 0.2509 0.9867 0.064 Uiso 1 1 calc R . . C22 C -0.1150(5) 0.1808(4) 0.92617(15) 0.0508(8) Uani 1 1 d . . . H22 H -0.0936 0.0764 0.9390 0.061 Uiso 1 1 calc R . . C23 C -0.0040(4) 0.2278(4) 0.87891(13) 0.0423(7) Uani 1 1 d . . . C24 C -0.2206(4) 0.6567(4) 0.87060(14) 0.0432(7) Uani 1 1 d . . . H24 H -0.1259 0.6735 0.8397 0.052 Uiso 1 1 calc R . . C25 C -0.3619(5) 0.6963(4) 0.8310(2) 0.0618(10) Uani 1 1 d . . . H25A H -0.3805 0.8018 0.8149 0.074 Uiso 1 1 calc R . . H25B H -0.4580 0.6853 0.8606 0.074 Uiso 1 1 calc R . . H25C H -0.3376 0.6270 0.7921 0.074 Uiso 1 1 calc R . . C26 C -0.2551(5) 0.7641(5) 0.93144(18) 0.0604(9) Uani 1 1 d . . . H26A H -0.2767 0.8701 0.9156 0.072 Uiso 1 1 calc R . . H26B H -0.1621 0.7397 0.9552 0.072 Uiso 1 1 calc R . . H26C H -0.3486 0.7513 0.9624 0.072 Uiso 1 1 calc R . . C27 C 0.1481(5) 0.1103(4) 0.84733(16) 0.0561(9) Uani 1 1 d . . . H27 H 0.2194 0.1673 0.8209 0.067 Uiso 1 1 calc R . . C28 C 0.1144(8) 0.0056(6) 0.7986(3) 0.102(2) Uani 1 1 d . . . H28A H 0.2156 -0.0635 0.7772 0.122 Uiso 1 1 calc R . . H28B H 0.0587 0.0666 0.7637 0.122 Uiso 1 1 calc R . . H28C H 0.0472 -0.0543 0.8233 0.122 Uiso 1 1 calc R . . C29 C 0.2381(7) 0.0179(7) 0.9011(2) 0.0929(18) Uani 1 1 d . . . H29A H 0.3337 -0.0579 0.8791 0.112 Uiso 1 1 calc R . . H29B H 0.1686 -0.0343 0.9298 0.112 Uiso 1 1 calc R . . H29C H 0.2700 0.0864 0.9291 0.112 Uiso 1 1 calc R . . C30 C -0.2540(4) 0.2968(4) 0.73261(17) 0.0462(7) Uani 1 1 d . . . C31 C -0.3860(4) 0.2286(5) 0.7424(3) 0.0671(11) Uani 1 1 d D . . H31A H -0.4879 0.3106 0.7444 0.081 Uiso 1 1 calc R . . H31B H -0.3764 0.1628 0.7029 0.081 Uiso 1 1 calc R . . C32 C -0.3905(9) 0.1400(10) 0.8023(4) 0.130(3) Uani 1 1 d D . . H32A H -0.4811 0.0962 0.8064 0.156 Uiso 1 1 calc R . . H32B H -0.4029 0.2051 0.8417 0.156 Uiso 1 1 calc R . . H32C H -0.2906 0.0575 0.8002 0.156 Uiso 1 1 calc R . . N1 N 0.1820(3) 0.5182(3) 0.67573(10) 0.0309(5) Uani 1 1 d . . . N2 N 0.0679(3) 0.4332(3) 0.80915(10) 0.0315(5) Uani 1 1 d . . . N3 N -0.1483(3) 0.3492(3) 0.72548(11) 0.0407(6) Uani 1 1 d . . . Ni1 Ni 0.02463(4) 0.43047(4) 0.717676(15) 0.03245(14) Uani 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 C1 0.0342(13) 0.0327(15) 0.0331(12) -0.0008(10) -0.0037(10) -0.0060(11) C2 0.0347(14) 0.0433(17) 0.0347(12) -0.0021(11) -0.0090(10) -0.0149(12) C3 0.0370(14) 0.0370(16) 0.0310(12) 0.0007(10) -0.0059(10) -0.0067(12) C4 0.0468(17) 0.057(2) 0.0396(14) 0.0012(13) -0.0061(12) -0.0261(15) C5 0.0563(19) 0.078(3) 0.0340(14) 0.0060(14) -0.0145(13) -0.0251(18) C6 0.0366(13) 0.0320(15) 0.0278(11) 0.0010(10) -0.0040(10) -0.0154(11) C7 0.0331(13) 0.0375(17) 0.0345(12) -0.0042(10) 0.0003(10) -0.0166(11) C8 0.0420(15) 0.053(2) 0.0319(12) -0.0086(12) 0.0026(11) -0.0229(14) C9 0.0515(17) 0.060(2) 0.0288(12) 0.0065(12) -0.0087(11) -0.0289(15) C10 0.0464(16) 0.0439(18) 0.0380(14) 0.0106(12) -0.0109(12) -0.0205(13) C11 0.0382(14) 0.0333(16) 0.0347(12) 0.0038(10) -0.0057(10) -0.0158(12) C12 0.0438(16) 0.0386(18) 0.0441(14) -0.0072(12) -0.0055(12) -0.0079(13) C13 0.053(2) 0.042(2) 0.072(2) 0.0037(15) 0.0097(16) -0.0049(16) C14 0.0425(17) 0.047(2) 0.075(2) -0.0114(16) 0.0035(15) -0.0101(15) C15 0.0464(16) 0.0319(17) 0.0453(14) -0.0001(11) -0.0081(12) -0.0097(13) C16 0.0506(19) 0.047(2) 0.076(2) -0.0128(17) 0.0092(16) -0.0160(16) C17 0.065(2) 0.037(2) 0.089(3) -0.0048(17) -0.002(2) -0.0178(18) C18 0.0384(14) 0.0375(16) 0.0260(11) 0.0007(10) -0.0018(10) -0.0087(12) C19 0.0377(14) 0.0379(16) 0.0311(11) -0.0006(10) -0.0032(10) -0.0069(12) C20 0.0435(16) 0.047(2) 0.0398(14) 0.0003(12) 0.0063(12) -0.0100(14) C21 0.058(2) 0.056(2) 0.0457(16) 0.0059(14) 0.0086(14) -0.0220(17) C22 0.065(2) 0.0379(19) 0.0441(15) 0.0058(12) 0.0033(14) -0.0126(16) C23 0.0529(17) 0.0355(17) 0.0323(12) 0.0044(11) -0.0012(12) -0.0058(14) C24 0.0414(15) 0.0395(18) 0.0401(14) 0.0000(12) 0.0002(11) -0.0012(13) C25 0.064(2) 0.048(2) 0.065(2) -0.0012(16) -0.0204(17) 0.0052(18) C26 0.078(3) 0.045(2) 0.0565(19) -0.0053(15) -0.0069(17) -0.0164(18) C27 0.067(2) 0.0363(19) 0.0477(16) 0.0050(13) 0.0106(15) 0.0020(16) C28 0.119(5) 0.069(3) 0.089(3) -0.033(3) -0.011(3) 0.019(3) C29 0.083(3) 0.091(4) 0.068(2) 0.004(2) -0.006(2) 0.031(3) C30 0.0417(16) 0.0373(18) 0.0593(17) -0.0056(13) -0.0046(13) -0.0115(14) C31 0.0381(18) 0.046(2) 0.115(3) -0.009(2) -0.0062(19) -0.0103(16) C32 0.106(5) 0.159(8) 0.149(6) 0.059(5) -0.042(4) -0.073(5) N1 0.0339(11) 0.0317(13) 0.0273(10) -0.0014(8) -0.0054(8) -0.0089(9) N2 0.0333(11) 0.0297(12) 0.0293(10) 0.0022(8) -0.0017(8) -0.0072(9) N3 0.0470(14) 0.0394(15) 0.0349(11) -0.0017(9) -0.0057(10) -0.0110(11) Ni1 0.0373(2) 0.0348(2) 0.02662(18) 0.00067(12) -0.00333(12) -0.01321(15) _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 C1 N1 1.333(4) . ? C1 C2 1.406(4) . ? C1 C4 1.504(4) . ? C2 C3 1.397(4) . ? C2 H2 0.9500 . ? C3 N2 1.332(4) . ? C3 C5 1.516(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.412(4) . ? C6 C7 1.414(4) . ? C6 N1 1.440(3) . ? C7 C8 1.392(4) . ? C7 C12 1.525(4) . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C9 C10 1.378(5) . ? C9 H9 0.9500 . ? C10 C11 1.402(4) . ? C10 H10 0.9500 . ? C11 C15 1.523(4) . ? C12 C13 1.512(5) . ? C12 C14 1.535(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.527(5) . ? C15 C16 1.533(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.400(4) . ? C18 C19 1.411(4) . ? C18 N2 1.432(3) . ? C19 C20 1.398(4) . ? C19 C24 1.514(4) . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C21 C22 1.390(5) . ? C21 H21 0.9500 . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C23 C27 1.523(4) . ? C24 C25 1.531(5) . ? C24 C26 1.531(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.510(7) . ? C27 C29 1.521(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N3 1.149(4) . ? C30 C31 1.450(5) . ? C31 C32 1.418(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1 Ni1 1.861(2) . ? N2 Ni1 1.928(2) . ? N3 Ni1 1.857(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.3(3) . . ? N1 C1 C4 119.6(2) . . ? C2 C1 C4 118.1(2) . . ? C3 C2 C1 128.5(3) . . ? C3 C2 H2 115.7 . . ? C1 C2 H2 115.7 . . ? N2 C3 C2 123.2(2) . . ? N2 C3 C5 119.9(3) . . ? C2 C3 C5 116.9(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.2(2) . . ? C11 C6 N1 118.9(2) . . ? C7 C6 N1 119.7(2) . . ? C8 C7 C6 118.0(3) . . ? C8 C7 C12 121.0(3) . . ? C6 C7 C12 121.0(2) . . ? C9 C8 C7 121.6(3) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.4(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.0(3) . . ? C10 C11 C15 120.3(3) . . ? C6 C11 C15 121.7(2) . . ? C13 C12 C7 110.9(3) . . ? C13 C12 C14 109.7(3) . . ? C7 C12 C14 113.3(3) . . ? C13 C12 H12 107.6 . . ? C7 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.1(3) . . ? C11 C15 C16 110.7(3) . . ? C17 C15 C16 110.3(3) . . ? C11 C15 H15 107.9 . . ? C17 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? 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 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.3(3) . . ? C23 C18 N2 120.2(2) . . ? C19 C18 N2 118.3(3) . . ? C20 C19 C18 118.0(3) . . ? C20 C19 C24 119.5(3) . . ? C18 C19 C24 122.5(3) . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 118.6(3) . . ? C22 C23 C27 119.5(3) . . ? C18 C23 C27 121.9(3) . . ? C19 C24 C25 110.4(3) . . ? C19 C24 C26 113.0(3) . . ? C25 C24 C26 110.5(3) . . ? C19 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C26 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 110.4(4) . . ? C28 C27 C23 112.0(4) . . ? C29 C27 C23 111.6(3) . . ? C28 C27 H27 107.5 . . ? C29 C27 H27 107.5 . . ? C23 C27 H27 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 179.0(4) . . ? C32 C31 C30 112.7(4) . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? C30 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 N1 C6 120.4(2) . . ? C1 N1 Ni1 125.32(18) . . ? C6 N1 Ni1 113.98(17) . . ? C3 N2 C18 120.0(2) . . ? C3 N2 Ni1 123.01(19) . . ? C18 N2 Ni1 116.80(17) . . ? C30 N3 Ni1 177.5(3) . . ? N3 Ni1 N1 157.86(10) . . ? N3 Ni1 N2 104.50(10) . . ? N1 Ni1 N2 97.58(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -3.0(5) . . . . ? C4 C1 C2 C3 177.1(3) . . . . ? C1 C2 C3 N2 2.0(5) . . . . ? C1 C2 C3 C5 -177.9(3) . . . . ? C11 C6 C7 C8 -0.7(4) . . . . ? N1 C6 C7 C8 174.2(2) . . . . ? C11 C6 C7 C12 -179.1(3) . . . . ? N1 C6 C7 C12 -4.3(4) . . . . ? C6 C7 C8 C9 -0.4(4) . . . . ? C12 C7 C8 C9 178.1(3) . . . . ? C7 C8 C9 C10 1.4(5) . . . . ? C8 C9 C10 C11 -1.3(5) . . . . ? C9 C10 C11 C6 0.2(4) . . . . ? C9 C10 C11 C15 -179.5(3) . . . . ? C7 C6 C11 C10 0.7(4) . . . . ? N1 C6 C11 C10 -174.1(3) . . . . ? C7 C6 C11 C15 -179.5(3) . . . . ? N1 C6 C11 C15 5.6(4) . . . . ? C8 C7 C12 C13 -93.0(3) . . . . ? C6 C7 C12 C13 85.4(3) . . . . ? C8 C7 C12 C14 30.9(4) . . . . ? C6 C7 C12 C14 -150.7(3) . . . . ? C10 C11 C15 C17 -50.7(4) . . . . ? C6 C11 C15 C17 129.6(3) . . . . ? C10 C11 C15 C16 72.9(4) . . . . ? C6 C11 C15 C16 -106.8(3) . . . . ? C23 C18 C19 C20 -0.4(4) . . . . ? N2 C18 C19 C20 174.6(2) . . . . ? C23 C18 C19 C24 -178.0(3) . . . . ? N2 C18 C19 C24 -3.1(4) . . . . ? C18 C19 C20 C21 0.5(4) . . . . ? C24 C19 C20 C21 178.3(3) . . . . ? C19 C20 C21 C22 -0.1(5) . . . . ? C20 C21 C22 C23 -0.6(5) . . . . ? C21 C22 C23 C18 0.7(5) . . . . ? C21 C22 C23 C27 -178.6(3) . . . . ? C19 C18 C23 C22 -0.2(4) . . . . ? N2 C18 C23 C22 -175.1(3) . . . . ? C19 C18 C23 C27 179.1(3) . . . . ? N2 C18 C23 C27 4.2(4) . . . . ? C20 C19 C24 C25 -67.0(4) . . . . ? C18 C19 C24 C25 110.7(3) . . . . ? C20 C19 C24 C26 57.4(4) . . . . ? C18 C19 C24 C26 -125.0(3) . . . . ? C22 C23 C27 C28 71.0(5) . . . . ? C18 C23 C27 C28 -108.4(4) . . . . ? C22 C23 C27 C29 -53.5(5) . . . . ? C18 C23 C27 C29 127.2(4) . . . . ? C2 C1 N1 C6 176.8(2) . . . . ? C4 C1 N1 C6 -3.3(4) . . . . ? C2 C1 N1 Ni1 3.4(4) . . . . ? C4 C1 N1 Ni1 -176.7(2) . . . . ? C11 C6 N1 C1 -91.0(3) . . . . ? C7 C6 N1 C1 94.0(3) . . . . ? C11 C6 N1 Ni1 83.1(3) . . . . ? C7 C6 N1 Ni1 -91.8(3) . . . . ? C2 C3 N2 C18 -175.8(3) . . . . ? C5 C3 N2 C18 4.1(4) . . . . ? C2 C3 N2 Ni1 -1.5(4) . . . . ? C5 C3 N2 Ni1 178.4(2) . . . . ? C23 C18 N2 C3 -96.6(3) . . . . ? C19 C18 N2 C3 88.4(3) . . . . ? C23 C18 N2 Ni1 88.7(3) . . . . ? C19 C18 N2 Ni1 -86.3(3) . . . . ? C1 N1 Ni1 N3 173.5(3) . . . . ? C6 N1 Ni1 N3 -0.4(4) . . . . ? C1 N1 Ni1 N2 -2.5(2) . . . . ? C6 N1 Ni1 N2 -176.28(18) . . . . ? C3 N2 Ni1 N3 -176.9(2) . . . . ? C18 N2 Ni1 N3 -2.4(2) . . . . ? C3 N2 Ni1 N1 1.5(2) . . . . ? C18 N2 Ni1 N1 176.04(19) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.710 _refine_diff_density_min -1.149 _refine_diff_density_rms 0.078 # start Validation Reply Form _vrf_PLAT029_II ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94 RESPONSE: A large cusp of data is missing, because our image plate system has only one rotation axis. With remounting the crystal for measuring a second data set it got lost. Unfortunately, the quality of further crystals checked was bad. ; # end Validation Reply Form