# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1229 # Constraining ferromagnetic coupling in dinuclear # mu-13-azido nickel(II) acetate cryptate compounds. # Crystal structure and magnetic behaviour of # [Ni2(L1)(N3)(H2O)](CF3SO3)3.2H2O.EtOH # # A. Escuer, C. harding, Y. Dussart, J. Nelson, # V. McKee and R. Vicente. # data_nir3bm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H66 F9 N11 Ni2 O13 S3' _chemical_formula_weight 1305.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5006(3) _cell_length_b 21.0205(4) _cell_length_c 16.4021(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.3410(10) _cell_angle_gamma 90.00 _cell_volume 5453.26(17) _cell_formula_units_Z 4 _cell_measurement_temperature 161(2) _cell_measurement_reflns_used 6022 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.9311 _exptl_special_details ; ? ; _diffrn_ambient_temperature 161(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with 0.3 degree frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27832 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8939 _reflns_number_gt 6786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 and SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8939 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.16468(5) 0.37242(3) 0.81396(5) 0.0194(2) Uani 1 d . . . Ni2 Ni -0.22953(5) 0.35484(4) 0.66721(5) 0.0223(2) Uani 1 d . . . N1 N 0.2939(3) 0.3827(2) 0.8523(3) 0.0215(11) Uani 1 d . . . C1A C 0.3196(4) 0.4361(3) 0.9174(4) 0.0245(14) Uani 1 d . . . H1A1 H 0.2955 0.4763 0.8852 0.029 Uiso 1 calc R . . H1A2 H 0.3820 0.4401 0.9457 0.029 Uiso 1 calc R . . C2A C 0.2893(4) 0.4252(3) 0.9891(4) 0.0248(14) Uani 1 d . . . H2A1 H 0.3229 0.3908 1.0298 0.030 Uiso 1 calc R . . H2A2 H 0.2977 0.4644 1.0254 0.030 Uiso 1 calc R . . N3A N 0.1981(3) 0.4074(2) 0.9484(3) 0.0215(11) Uani 1 d . . . C3A C 0.1447(4) 0.4592(3) 0.9592(4) 0.0270(14) Uani 1 d . . . H3A1 H 0.1339 0.4917 0.9119 0.032 Uiso 1 calc R . . H3A2 H 0.1757 0.4799 1.0185 0.032 Uiso 1 calc R . . C4A C 0.0619(4) 0.4346(3) 0.9527(4) 0.0226(13) Uani 1 d . . . C5A C 0.0598(4) 0.3882(3) 1.0118(4) 0.0295(15) Uani 1 d . . . H5A H 0.1112 0.3722 1.0572 0.035 Uiso 1 calc R . . C6A C -0.0160(4) 0.3654(3) 1.0050(4) 0.0318(16) Uani 1 d . . . H6A H -0.0165 0.3329 1.0451 0.038 Uiso 1 calc R . . C7A C -0.0913(4) 0.3885(3) 0.9414(4) 0.0297(15) Uani 1 d . . . H7A H -0.1433 0.3728 0.9385 0.036 Uiso 1 calc R . . C8A C -0.0912(4) 0.4354(3) 0.8808(4) 0.0237(14) Uani 1 d . . . C9A C -0.0142(4) 0.4574(3) 0.8879(4) 0.0238(14) Uani 1 d . . . H9A H -0.0134 0.4892 0.8472 0.029 Uiso 1 calc R . . C10A C -0.1718(4) 0.4623(3) 0.8107(4) 0.0272(14) Uani 1 d . . . H10A H -0.1932 0.4950 0.8390 0.033 Uiso 1 calc R . . H10B H -0.1597 0.4834 0.7636 0.033 Uiso 1 calc R . . N4A N -0.2389(3) 0.4136(2) 0.7672(3) 0.0258(12) Uani 1 d . . . C11A C -0.3223(4) 0.4452(3) 0.7174(4) 0.0290(15) Uani 1 d . . . H11A H -0.3206 0.4732 0.6697 0.035 Uiso 1 calc R . . H11B H -0.3364 0.4714 0.7592 0.035 Uiso 1 calc R . . C12A C -0.3875(4) 0.3941(3) 0.6762(4) 0.0311(15) Uani 1 d . . . H12A H -0.3930 0.3690 0.7246 0.037 Uiso 1 calc R . . H12B H -0.4430 0.4137 0.6389 0.037 Uiso 1 calc R . . N2 N -0.3626(3) 0.3515(2) 0.6195(3) 0.0256(12) Uani 1 d . . . C1B C 0.3383(4) 0.3225(3) 0.8939(4) 0.0263(14) Uani 1 d . . . H1B1 H 0.3925 0.3330 0.9456 0.032 Uiso 1 calc R . . H1B2 H 0.3515 0.2991 0.8491 0.032 Uiso 1 calc R . . C2B C 0.2873(4) 0.2801(3) 0.9261(4) 0.0249(14) Uani 1 d . . . H2B1 H 0.3111 0.2365 0.9359 0.030 Uiso 1 calc R . . H2B2 H 0.2911 0.2961 0.9844 0.030 Uiso 1 calc R . . N3B N 0.1984(3) 0.2780(2) 0.8604(3) 0.0207(11) Uani 1 d . . . C3B C 0.1489(4) 0.2431(3) 0.9016(4) 0.0267(14) Uani 1 d . . . H3B1 H 0.1831 0.2067 0.9368 0.032 Uiso 1 calc R . . H3B2 H 0.1394 0.2719 0.9440 0.032 Uiso 1 calc R . . C4B C 0.0654(4) 0.2187(3) 0.8346(4) 0.0241(14) Uani 1 d . . . C5B C 0.0603(4) 0.1714(3) 0.7734(4) 0.0275(14) Uani 1 d . . . H5B H 0.1105 0.1552 0.7722 0.033 Uiso 1 calc R . . C6B C -0.0172(4) 0.1477(3) 0.7144(5) 0.0332(16) Uani 1 d . . . H6B H -0.0202 0.1156 0.6724 0.040 Uiso 1 calc R . . C7B C -0.0910(4) 0.1707(3) 0.7163(4) 0.0312(15) Uani 1 d . . . H7B H -0.1442 0.1546 0.6749 0.037 Uiso 1 calc R . . C8B C -0.0876(4) 0.2168(3) 0.7779(4) 0.0264(14) Uani 1 d . . . C9B C -0.0091(4) 0.2404(3) 0.8370(4) 0.0253(14) Uani 1 d . . . H9B H -0.0061 0.2719 0.8799 0.030 Uiso 1 calc R . . C10B C -0.1651(4) 0.2367(3) 0.7885(4) 0.0309(15) Uani 1 d . . . H10C H -0.1865 0.1998 0.8100 0.037 Uiso 1 calc R . . H10D H -0.1491 0.2701 0.8355 0.037 Uiso 1 calc R . . N4B N -0.2344(3) 0.2613(2) 0.7047(3) 0.0275(12) Uani 1 d . . . C11B C -0.3172(4) 0.2549(3) 0.7089(4) 0.0318(15) Uani 1 d . . . H11C H -0.3145 0.2759 0.7641 0.038 Uiso 1 calc R . . H11D H -0.3300 0.2093 0.7117 0.038 Uiso 1 calc R . . C12B C -0.3858(4) 0.2847(3) 0.6273(4) 0.0321(16) Uani 1 d . . . H12C H -0.3930 0.2607 0.5725 0.039 Uiso 1 calc R . . H12D H -0.4399 0.2835 0.6328 0.039 Uiso 1 calc R . . C1C C 0.3039(4) 0.3979(3) 0.7692(4) 0.0291(15) Uani 1 d . . . H1C1 H 0.3638 0.3929 0.7803 0.035 Uiso 1 calc R . . H1C2 H 0.2869 0.4425 0.7512 0.035 Uiso 1 calc R . . C2C C 0.2488(4) 0.3531(3) 0.6943(4) 0.0310(15) Uani 1 d . . . H2C1 H 0.2517 0.3647 0.6372 0.037 Uiso 1 calc R . . H2C2 H 0.2692 0.3088 0.7098 0.037 Uiso 1 calc R . . N3C N 0.1609(3) 0.3582(2) 0.6834(3) 0.0248(12) Uani 1 d . . . C3C C 0.1057(4) 0.3096(3) 0.6188(4) 0.0313(15) Uani 1 d . . . H3C1 H 0.0979 0.2731 0.6527 0.038 Uiso 1 calc R . . H3C2 H 0.1331 0.2937 0.5811 0.038 Uiso 1 calc R . . C4C C 0.0208(4) 0.3376(3) 0.5591(4) 0.0238(14) Uani 1 d . . . C5C C 0.0146(4) 0.3892(3) 0.5045(4) 0.0293(15) Uani 1 d . . . H5C H 0.0645 0.4071 0.5046 0.035 Uiso 1 calc R . . C6C C -0.0627(4) 0.4150(3) 0.4501(4) 0.0350(17) Uani 1 d . . . H6C H -0.0658 0.4511 0.4140 0.042 Uiso 1 calc R . . C7C C -0.1356(4) 0.3887(3) 0.4477(4) 0.0282(15) Uani 1 d . . . H7C H -0.1890 0.4065 0.4098 0.034 Uiso 1 calc R . . C8C C -0.1311(4) 0.3363(3) 0.5008(4) 0.0270(14) Uani 1 d . . . C9C C -0.0532(4) 0.3112(3) 0.5564(4) 0.0246(14) Uani 1 d . . . H9C H -0.0501 0.2755 0.5933 0.030 Uiso 1 calc R . . C10C C -0.2107(4) 0.3058(3) 0.4960(5) 0.0317(16) Uani 1 d . . . H10E H -0.2469 0.2936 0.4328 0.038 Uiso 1 calc R . . H10F H -0.1958 0.2665 0.5329 0.038 Uiso 1 calc R . . N4C N -0.2592(3) 0.3490(2) 0.5291(3) 0.0232(11) Uani 1 d . . . C11C C -0.3514(4) 0.3409(3) 0.4768(4) 0.0298(15) Uani 1 d . . . H11E H -0.3653 0.2950 0.4692 0.036 Uiso 1 calc R . . H11F H -0.3694 0.3599 0.4161 0.036 Uiso 1 calc R . . C12C C -0.3978(4) 0.3723(3) 0.5244(4) 0.0308(15) Uani 1 d . . . H12E H -0.3927 0.4191 0.5218 0.037 Uiso 1 calc R . . H12F H -0.4585 0.3611 0.4939 0.037 Uiso 1 calc R . . N5 N 0.0375(3) 0.3616(2) 0.7697(3) 0.0253(12) Uani 1 d . . . N6 N -0.0351(4) 0.3671(2) 0.7355(3) 0.0197(11) Uani 1 d . . . N7 N -0.1086(3) 0.3740(3) 0.7001(4) 0.0284(12) Uani 1 d . . . S20 S -0.31779(11) 0.13611(8) 0.46624(13) 0.0326(4) Uani 1 d . . . O21 O -0.2862(6) 0.0752(3) 0.4896(12) 0.203(7) Uani 1 d . . . O22 O -0.3032(4) 0.1742(4) 0.5407(4) 0.080(2) Uani 1 d . . . O23 O -0.2998(4) 0.1657(4) 0.3998(4) 0.078(2) Uani 1 d . . . C20 C -0.4307(7) 0.1277(6) 0.4135(8) 0.080(3) Uani 1 d . . . F21 F -0.4658(4) 0.1842(5) 0.4028(8) 0.172(5) Uani 1 d . . . F22 F -0.4588(6) 0.1000(7) 0.3392(6) 0.228(7) Uani 1 d . . . F23 F -0.4567(4) 0.0956(4) 0.4646(5) 0.112(2) Uani 1 d . . . S30 S -0.25332(11) 0.53548(8) 0.50880(12) 0.0326(4) Uani 1 d . . . O31 O -0.2802(4) 0.5162(3) 0.4183(4) 0.079(2) Uani 1 d . . . O32 O -0.1883(3) 0.5822(3) 0.5372(4) 0.0603(17) Uani 1 d . . . O33 O -0.2408(3) 0.4849(2) 0.5719(4) 0.0427(13) Uani 1 d . . . C30 C -0.3439(5) 0.5779(3) 0.5076(5) 0.0421(19) Uani 1 d . . . F31 F -0.3291(4) 0.6015(3) 0.5854(4) 0.091(2) Uani 1 d . . . F32 F -0.4103(3) 0.5397(3) 0.4833(5) 0.093(2) Uani 1 d . . . F33 F -0.3663(3) 0.6253(2) 0.4487(4) 0.0664(14) Uani 1 d . . . S40 S 0.29551(11) 0.16602(8) 0.69682(11) 0.0325(4) Uani 1 d . . . O41 O 0.2720(3) 0.1941(2) 0.7623(3) 0.0460(13) Uani 1 d . . . O42 O 0.3055(4) 0.0986(2) 0.7006(4) 0.0595(16) Uani 1 d . . . O43 O 0.2508(3) 0.1904(2) 0.6080(3) 0.0366(11) Uani 1 d . . . C40 C 0.4016(5) 0.1961(4) 0.7289(6) 0.054(2) Uani 1 d . . . F41 F 0.4538(3) 0.1783(3) 0.8107(4) 0.103(2) Uani 1 d . . . F42 F 0.4041(3) 0.2593(2) 0.7267(4) 0.0698(16) Uani 1 d . . . F43 F 0.4331(3) 0.1752(3) 0.6726(4) 0.0765(17) Uani 1 d . . . O1W O 0.1341(3) 0.47097(19) 0.7605(3) 0.0288(10) Uani 1 d . . . O2W O -0.0362(3) 0.5041(2) 0.6718(3) 0.0417(12) Uani 1 d . . . O3W O 0.2421(3) 0.5734(2) 0.7930(3) 0.0425(12) Uani 1 d . . . O50 O 0.3557(4) 0.5695(3) 0.7183(4) 0.0541(15) Uani 1 d . . . C51 C 0.4376(16) 0.5496(16) 0.7557(17) 0.052(7) Uani 0.50 d P A 1 H51A H 0.4712 0.5747 0.7317 0.062 Uiso 0.50 calc PR A 1 H51B H 0.4409 0.5041 0.7417 0.062 Uiso 0.50 calc PR A 1 C52 C 0.4707(15) 0.5590(13) 0.8561(15) 0.082(8) Uani 0.50 d P A 1 H52A H 0.5292 0.5439 0.8859 0.122 Uiso 0.50 calc PR A 1 H52B H 0.4357 0.5350 0.8786 0.122 Uiso 0.50 calc PR A 1 H52C H 0.4687 0.6043 0.8691 0.122 Uiso 0.50 calc PR A 1 C51' C 0.4409(19) 0.5492(15) 0.796(2) 0.064(8) Uani 0.50 d P A 2 H51C H 0.4681 0.5854 0.8370 0.077 Uiso 0.50 calc PR A 2 H51D H 0.4325 0.5141 0.8319 0.077 Uiso 0.50 calc PR A 2 C52' C 0.4928(15) 0.5278(9) 0.7494(16) 0.075(6) Uani 0.50 d P A 2 H52D H 0.5490 0.5151 0.7942 0.112 Uiso 0.50 calc PR A 2 H52E H 0.4983 0.5627 0.7127 0.112 Uiso 0.50 calc PR A 2 H52F H 0.4652 0.4915 0.7104 0.112 Uiso 0.50 calc PR A 2 H3C H 0.1966 0.2623 0.8090 0.040 Uiso 1 d . . . H3D H 0.1899 0.3827 0.9878 0.040 Uiso 1 d . . . H3E H 0.1368 0.4020 0.6670 0.040 Uiso 1 d . . . H4A H -0.2369 0.3885 0.8188 0.040 Uiso 1 d . . . H4B H -0.2388 0.2426 0.6512 0.040 Uiso 1 d . . . H4C H -0.2413 0.3880 0.5190 0.040 Uiso 1 d . . . H1WA H 0.1670 0.5123 0.7747 0.040 Uiso 1 d . . . H1WB H -0.0490 0.5482 0.6601 0.040 Uiso 1 d . . . H2WA H -0.0800 0.4681 0.6503 0.040 Uiso 1 d . . . H2WB H 0.0720 0.4721 0.7345 0.040 Uiso 1 d . . . H3WA H 0.2698 0.5925 0.8503 0.040 Uiso 1 d . . . H3WB H 0.2891 0.5820 0.7741 0.040 Uiso 1 d . . . H50 H 0.3273 0.5421 0.6732 0.040 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0193(4) 0.0181(4) 0.0222(4) 0.0021(3) 0.0102(3) 0.0028(3) Ni2 0.0226(5) 0.0242(4) 0.0219(4) -0.0029(3) 0.0113(3) -0.0031(3) N1 0.018(3) 0.026(3) 0.023(3) 0.004(2) 0.011(2) 0.001(2) C1A 0.017(3) 0.019(3) 0.035(4) 0.005(3) 0.009(3) 0.001(3) C2A 0.018(3) 0.025(3) 0.028(3) -0.005(3) 0.007(3) -0.001(3) N3A 0.022(3) 0.020(3) 0.025(3) 0.000(2) 0.012(2) 0.002(2) C3A 0.028(4) 0.026(3) 0.026(3) 0.001(3) 0.012(3) 0.004(3) C4A 0.025(4) 0.025(3) 0.025(3) -0.008(3) 0.016(3) -0.003(3) C5A 0.024(4) 0.038(4) 0.021(3) 0.001(3) 0.004(3) 0.005(3) C6A 0.032(4) 0.040(4) 0.025(3) 0.006(3) 0.014(3) 0.001(3) C7A 0.027(4) 0.039(4) 0.030(4) -0.008(3) 0.019(3) -0.006(3) C8A 0.026(4) 0.030(3) 0.016(3) -0.005(3) 0.010(2) 0.003(3) C9A 0.028(4) 0.022(3) 0.023(3) -0.005(2) 0.013(3) -0.003(3) C10A 0.025(4) 0.031(4) 0.023(3) -0.008(3) 0.009(3) 0.001(3) N4A 0.023(3) 0.031(3) 0.024(3) -0.002(2) 0.011(2) 0.006(2) C11A 0.026(4) 0.032(4) 0.031(4) -0.003(3) 0.015(3) 0.007(3) C12A 0.021(4) 0.042(4) 0.030(4) 0.001(3) 0.010(3) 0.004(3) N2 0.024(3) 0.031(3) 0.020(3) -0.003(2) 0.008(2) -0.004(2) C1B 0.024(4) 0.029(4) 0.028(3) 0.006(3) 0.013(3) 0.010(3) C2B 0.027(4) 0.022(3) 0.027(3) 0.007(3) 0.014(3) 0.010(3) N3B 0.023(3) 0.018(3) 0.021(3) 0.001(2) 0.011(2) -0.001(2) C3B 0.036(4) 0.026(3) 0.022(3) 0.002(3) 0.016(3) 0.000(3) C4B 0.035(4) 0.013(3) 0.028(3) 0.005(2) 0.017(3) 0.000(3) C5B 0.036(4) 0.018(3) 0.036(4) 0.004(3) 0.022(3) 0.004(3) C6B 0.052(5) 0.012(3) 0.037(4) -0.004(3) 0.021(3) -0.004(3) C7B 0.036(4) 0.026(4) 0.029(4) 0.005(3) 0.011(3) -0.005(3) C8B 0.036(4) 0.021(3) 0.025(3) 0.007(3) 0.016(3) 0.001(3) C9B 0.038(4) 0.016(3) 0.025(3) 0.001(2) 0.016(3) -0.002(3) C10B 0.037(4) 0.030(4) 0.029(4) 0.007(3) 0.017(3) 0.003(3) N4B 0.032(3) 0.027(3) 0.025(3) 0.003(2) 0.014(2) 0.000(2) C11B 0.029(4) 0.036(4) 0.034(4) -0.001(3) 0.016(3) -0.007(3) C12B 0.026(4) 0.039(4) 0.032(4) -0.002(3) 0.013(3) -0.004(3) C1C 0.022(4) 0.037(4) 0.031(4) 0.011(3) 0.014(3) 0.008(3) C2C 0.030(4) 0.039(4) 0.032(4) 0.004(3) 0.020(3) 0.004(3) N3C 0.024(3) 0.023(3) 0.028(3) 0.005(2) 0.012(2) 0.007(2) C3C 0.037(4) 0.026(4) 0.032(4) -0.004(3) 0.016(3) 0.002(3) C4C 0.025(4) 0.027(3) 0.019(3) -0.005(2) 0.009(2) 0.002(3) C5C 0.030(4) 0.034(4) 0.026(3) 0.002(3) 0.014(3) -0.006(3) C6C 0.034(4) 0.040(4) 0.030(4) 0.015(3) 0.014(3) 0.002(3) C7C 0.027(4) 0.034(4) 0.021(3) 0.002(3) 0.008(3) 0.000(3) C8C 0.035(4) 0.027(3) 0.022(3) -0.011(3) 0.016(3) -0.004(3) C9C 0.037(4) 0.024(3) 0.018(3) -0.001(2) 0.018(3) 0.000(3) C10C 0.035(4) 0.032(4) 0.035(4) -0.014(3) 0.021(3) -0.009(3) N4C 0.025(3) 0.025(3) 0.020(3) -0.001(2) 0.010(2) -0.005(2) C11C 0.027(4) 0.032(4) 0.028(3) 0.002(3) 0.009(3) -0.006(3) C12C 0.025(4) 0.037(4) 0.029(4) 0.003(3) 0.009(3) -0.002(3) N5 0.017(3) 0.026(3) 0.031(3) 0.002(2) 0.009(2) 0.001(2) N6 0.027(4) 0.019(3) 0.018(3) -0.005(2) 0.014(2) -0.005(2) N7 0.024(3) 0.034(3) 0.028(3) -0.007(2) 0.011(2) -0.001(3) S20 0.0255(10) 0.0220(9) 0.0538(11) -0.0011(7) 0.0203(8) 0.0003(7) O21 0.107(7) 0.035(4) 0.49(2) 0.053(8) 0.155(11) 0.034(5) O22 0.072(4) 0.130(6) 0.045(4) -0.038(4) 0.033(3) -0.053(4) O23 0.059(4) 0.146(7) 0.041(3) -0.019(4) 0.031(3) -0.043(4) C20 0.067(8) 0.099(9) 0.091(9) -0.032(7) 0.050(6) -0.045(7) F21 0.041(4) 0.201(10) 0.230(11) 0.103(9) 0.017(5) 0.033(5) F22 0.156(8) 0.433(18) 0.117(7) -0.156(9) 0.080(6) -0.226(10) F23 0.067(4) 0.154(7) 0.136(6) 0.000(5) 0.064(4) -0.050(4) S30 0.0329(10) 0.0268(9) 0.0367(10) 0.0003(7) 0.0136(7) 0.0015(8) O31 0.093(5) 0.090(5) 0.044(4) -0.011(3) 0.019(3) 0.035(4) O32 0.038(3) 0.042(3) 0.097(5) 0.017(3) 0.026(3) -0.007(3) O33 0.041(3) 0.029(3) 0.058(3) 0.010(2) 0.021(2) 0.006(2) C30 0.042(5) 0.027(4) 0.055(5) 0.006(3) 0.018(4) 0.011(4) F31 0.121(5) 0.096(5) 0.076(4) -0.012(3) 0.060(4) 0.040(4) F32 0.043(3) 0.057(3) 0.173(7) 0.029(4) 0.042(4) 0.006(3) F33 0.062(3) 0.046(3) 0.087(4) 0.026(3) 0.027(3) 0.025(2) S40 0.0433(11) 0.0274(9) 0.0268(9) -0.0021(7) 0.0149(7) 0.0050(8) O41 0.067(4) 0.040(3) 0.039(3) -0.002(2) 0.030(3) 0.008(3) O42 0.100(5) 0.028(3) 0.061(4) 0.004(3) 0.044(3) 0.012(3) O43 0.040(3) 0.043(3) 0.027(3) -0.005(2) 0.015(2) 0.000(2) C40 0.043(5) 0.060(6) 0.053(5) -0.021(4) 0.014(4) 0.016(4) F41 0.060(4) 0.121(5) 0.071(4) -0.020(4) -0.027(3) 0.035(3) F42 0.044(3) 0.054(3) 0.111(4) -0.034(3) 0.033(3) -0.011(2) F43 0.043(3) 0.082(4) 0.112(5) -0.041(3) 0.040(3) 0.000(3) O1W 0.022(2) 0.019(2) 0.043(3) 0.0031(19) 0.0118(19) 0.0028(18) O2W 0.036(3) 0.030(3) 0.052(3) 0.011(2) 0.012(2) -0.002(2) O3W 0.039(3) 0.039(3) 0.046(3) -0.001(2) 0.014(2) 0.000(2) O50 0.050(4) 0.049(3) 0.066(4) 0.001(3) 0.026(3) 0.001(3) C51 0.032(12) 0.086(16) 0.039(15) 0.024(14) 0.016(11) -0.007(10) C52 0.082(17) 0.11(2) 0.041(12) 0.010(13) 0.015(12) -0.036(14) C51' 0.073(19) 0.074(15) 0.06(2) 0.01(2) 0.05(2) -0.016(13) C52' 0.068(15) 0.056(13) 0.115(19) -0.021(12) 0.053(13) -0.016(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.037(5) . y Ni1 N1 2.083(5) . y Ni1 N3B 2.117(5) . y Ni1 N3C 2.135(5) . y Ni1 N3A 2.154(5) . y Ni1 O1W 2.224(4) . y Ni2 N7 1.988(6) . y Ni2 N4B 2.072(5) . y Ni2 N4C 2.100(5) . y Ni2 N4A 2.115(5) . y Ni2 N2 2.118(5) . y N1 C1A 1.482(8) . ? N1 C1C 1.482(8) . ? N1 C1B 1.487(7) . ? C1A C2A 1.500(8) . ? C2A N3A 1.490(8) . ? N3A C3A 1.494(7) . ? C3A C4A 1.499(8) . ? C4A C9A 1.385(8) . ? C4A C5A 1.386(9) . ? C5A C6A 1.370(9) . ? C6A C7A 1.373(9) . ? C7A C8A 1.400(9) . ? C8A C9A 1.382(8) . ? C8A C10A 1.498(8) . ? C10A N4A 1.488(8) . ? N4A C11A 1.489(8) . ? C11A C12A 1.501(9) . ? C12A N2 1.484(8) . ? N2 C12C 1.477(8) . ? N2 C12B 1.482(8) . ? C1B C2B 1.509(8) . ? C2B N3B 1.466(8) . ? N3B C3B 1.498(7) . ? C3B C4B 1.493(9) . ? C4B C5B 1.389(8) . ? C4B C9B 1.398(9) . ? C5B C6B 1.378(9) . ? C6B C7B 1.392(9) . ? C7B C8B 1.382(9) . ? C8B C9B 1.390(9) . ? C8B C10B 1.500(9) . ? C10B N4B 1.484(8) . ? N4B C11B 1.485(8) . ? C11B C12B 1.500(9) . ? C1C C2C 1.519(9) . ? C2C N3C 1.474(8) . ? N3C C3C 1.492(8) . ? C3C C4C 1.505(9) . ? C4C C5C 1.382(9) . ? C4C C9C 1.392(9) . ? C5C C6C 1.374(9) . ? C6C C7C 1.375(9) . ? C7C C8C 1.386(9) . ? C8C C9C 1.379(9) . ? C8C C10C 1.505(9) . ? C10C N4C 1.495(8) . ? N4C C11C 1.477(8) . ? C11C C12C 1.500(9) . ? N5 N6 1.154(7) . y N6 N7 1.173(7) . y S20 O21 1.383(7) . ? S20 O22 1.390(6) . ? S20 O23 1.404(6) . ? S20 C20 1.795(11) . ? C20 F22 1.246(12) . ? C20 F23 1.300(12) . ? C20 F21 1.313(14) . ? S30 O31 1.411(6) . ? S30 O32 1.423(5) . ? S30 O33 1.433(5) . ? S30 C30 1.812(7) . ? C30 F31 1.288(9) . ? C30 F33 1.324(8) . ? C30 F32 1.326(9) . ? S40 O43 1.421(5) . ? S40 O42 1.425(5) . ? S40 O41 1.432(5) . ? S40 C40 1.814(9) . ? C40 F41 1.314(10) . ? C40 F42 1.329(10) . ? C40 F43 1.336(9) . ? O50 C51 1.36(3) . ? O50 C51' 1.55(3) . ? C51 C52 1.51(3) . ? C51' C52' 1.49(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 N5 Ni1 N1 177.0(2) . . y N5 Ni1 N3B 96.7(2) . . y N1 Ni1 N3B 83.63(19) . . y N5 Ni1 N3C 93.9(2) . . y N1 Ni1 N3C 83.14(19) . . y N3B Ni1 N3C 96.51(19) . . y N5 Ni1 N3A 100.3(2) . . y N1 Ni1 N3A 82.63(19) . . y N3B Ni1 N3A 92.33(18) . . y N3C Ni1 N3A 162.30(19) . . y N5 Ni1 O1W 85.52(18) . . y N1 Ni1 O1W 94.00(17) . . y N3B Ni1 O1W 176.45(17) . . y N3C Ni1 O1W 80.56(18) . . y N3A Ni1 O1W 89.98(17) . . y N7 Ni2 N4B 106.6(2) . . y N7 Ni2 N4C 92.7(2) . . y N4B Ni2 N4C 104.0(2) . . y N7 Ni2 N4A 95.6(2) . . y N4B Ni2 N4A 107.3(2) . . y N4C Ni2 N4A 143.6(2) . . y N7 Ni2 N2 169.0(2) . . y N4B Ni2 N2 84.2(2) . . y N4C Ni2 N2 82.79(19) . . y N4A Ni2 N2 82.41(19) . . y C1A N1 C1C 112.3(5) . . ? C1A N1 C1B 112.1(5) . . ? C1C N1 C1B 111.1(5) . . ? C1A N1 Ni1 104.6(3) . . ? C1C N1 Ni1 106.6(4) . . ? C1B N1 Ni1 109.7(4) . . ? N1 C1A C2A 110.4(5) . . ? N3A C2A C1A 111.0(5) . . ? C2A N3A C3A 111.6(5) . . ? C2A N3A Ni1 108.3(3) . . ? C3A N3A Ni1 117.4(4) . . ? N3A C3A C4A 112.0(5) . . ? C9A C4A C5A 118.4(6) . . ? C9A C4A C3A 121.2(6) . . ? C5A C4A C3A 120.4(6) . . ? C6A C5A C4A 120.2(6) . . ? C5A C6A C7A 121.3(6) . . ? C6A C7A C8A 119.7(6) . . ? C9A C8A C7A 118.2(6) . . ? C9A C8A C10A 120.2(6) . . ? C7A C8A C10A 121.6(6) . . ? C8A C9A C4A 122.1(6) . . ? N4A C10A C8A 113.5(5) . . ? C10A N4A C11A 110.1(5) . . ? C10A N4A Ni2 117.8(4) . . ? C11A N4A Ni2 102.6(3) . . ? N4A C11A C12A 107.8(5) . . ? N2 C12A C11A 110.1(5) . . ? C12C N2 C12B 111.4(5) . . ? C12C N2 C12A 112.5(5) . . ? C12B N2 C12A 110.7(5) . . ? C12C N2 Ni2 106.0(4) . . ? C12B N2 Ni2 107.3(4) . . ? C12A N2 Ni2 108.7(4) . . ? N1 C1B C2B 113.0(5) . . ? N3B C2B C1B 111.2(5) . . ? C2B N3B C3B 108.6(4) . . ? C2B N3B Ni1 106.3(3) . . ? C3B N3B Ni1 119.7(4) . . ? C4B C3B N3B 114.1(5) . . ? C5B C4B C9B 118.8(6) . . ? C5B C4B C3B 121.2(6) . . ? C9B C4B C3B 119.9(6) . . ? C6B C5B C4B 120.4(6) . . ? C5B C6B C7B 120.2(6) . . ? C8B C7B C6B 120.7(6) . . ? C7B C8B C9B 118.7(6) . . ? C7B C8B C10B 121.5(6) . . ? C9B C8B C10B 119.5(6) . . ? C8B C9B C4B 121.3(6) . . ? N4B C10B C8B 114.3(5) . . ? C10B N4B C11B 110.6(5) . . ? C10B N4B Ni2 119.0(4) . . ? C11B N4B Ni2 105.4(4) . . ? N4B C11B C12B 110.1(5) . . ? N2 C12B C11B 109.2(5) . . ? N1 C1C C2C 109.0(5) . . ? N3C C2C C1C 108.7(5) . . ? C2C N3C C3C 111.2(5) . . ? C2C N3C Ni1 107.8(4) . . ? C3C N3C Ni1 122.8(4) . . ? N3C C3C C4C 110.7(5) . . ? C5C C4C C9C 118.6(6) . . ? C5C C4C C3C 120.7(6) . . ? C9C C4C C3C 120.7(6) . . ? C6C C5C C4C 120.9(6) . . ? C5C C6C C7C 120.2(6) . . ? C6C C7C C8C 120.0(6) . . ? C9C C8C C7C 119.6(6) . . ? C9C C8C C10C 120.1(6) . . ? C7C C8C C10C 120.2(6) . . ? C8C C9C C4C 120.7(6) . . ? N4C C10C C8C 112.3(5) . . ? C11C N4C C10C 111.6(5) . . ? C11C N4C Ni2 109.7(4) . . ? C10C N4C Ni2 120.6(4) . . ? N4C C11C C12C 110.3(5) . . ? N2 C12C C11C 110.2(5) . . ? N6 N5 Ni1 165.8(5) . . y N5 N6 N7 178.6(6) . . y N6 N7 Ni2 157.6(5) . . y O21 S20 O22 112.9(8) . . ? O21 S20 O23 115.5(7) . . ? O22 S20 O23 114.1(4) . . ? O21 S20 C20 105.7(6) . . ? O22 S20 C20 103.3(4) . . ? O23 S20 C20 103.7(5) . . ? F22 C20 F23 106.7(9) . . ? F22 C20 F21 109.0(14) . . ? F23 C20 F21 106.6(10) . . ? F22 C20 S20 114.1(9) . . ? F23 C20 S20 110.9(10) . . ? F21 C20 S20 109.3(7) . . ? O31 S30 O32 113.7(4) . . ? O31 S30 O33 115.3(4) . . ? O32 S30 O33 115.0(3) . . ? O31 S30 C30 103.5(4) . . ? O32 S30 C30 103.7(4) . . ? O33 S30 C30 103.6(3) . . ? F31 C30 F33 107.7(6) . . ? F31 C30 F32 108.0(7) . . ? F33 C30 F32 106.8(6) . . ? F31 C30 S30 112.0(5) . . ? F33 C30 S30 111.3(6) . . ? F32 C30 S30 110.7(5) . . ? O43 S40 O42 114.0(3) . . ? O43 S40 O41 114.3(3) . . ? O42 S40 O41 116.5(3) . . ? O43 S40 C40 102.6(4) . . ? O42 S40 C40 104.1(4) . . ? O41 S40 C40 103.0(3) . . ? F41 C40 F42 107.3(7) . . ? F41 C40 F43 107.5(7) . . ? F42 C40 F43 106.4(8) . . ? F41 C40 S40 112.0(7) . . ? F42 C40 S40 112.4(5) . . ? F43 C40 S40 111.0(6) . . ? C51 O50 C51' 24.4(10) . . ? O50 C51 C52 107(2) . . ? C52' C51' O50 104(2) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.864 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.105