# ja983772s.cif data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H28 Br2 N2 Ni' _chemical_formula_weight 623.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.456(2) _cell_length_b 12.088(3) _cell_length_c 13.020(3) _cell_angle_alpha 78.44(2) _cell_angle_beta 72.55(2) _cell_angle_gamma 69.80(2) _cell_volume 1324.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 59 _cell_measurement_theta_min 3.64 _cell_measurement_theta_max 12.59 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method ? _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 3.769 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.94 _diffrn_reflns_number 8884 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7623 _reflns_number_observed 4977 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7620 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_obs 0.0760 _refine_ls_wR_factor_all 0.2179 _refine_ls_wR_factor_obs 0.1830 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.121 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.121 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.15196(7) 0.83359(5) 0.25855(5) 0.0219(2) Uani 1 d . . Br1 Br 0.51762(11) 0.81796(6) -0.29304(5) 0.0587(2) Uani 1 d . . Br2 Br 0.01205(8) 0.63052(7) 0.82977(5) 0.0550(2) Uani 1 d . . N1 N 0.4450(5) 0.6502(3) 0.1847(3) 0.0242(8) Uani 1 d . . N2 N 0.3648(4) 0.6272(3) 0.3569(3) 0.0207(7) Uani 1 d . . C1 C 0.3244(5) 0.6975(4) 0.2666(3) 0.0200(8) Uani 1 d . . C2 C 0.5561(6) 0.5536(5) 0.2210(4) 0.0300(10) Uani 1 d . . H2 H 0.6482(6) 0.5082(5) 0.1789(4) 0.033(16) Uiso 1 calc R . C3 C 0.5047(6) 0.5390(4) 0.3280(4) 0.0288(10) Uani 1 d . . H3 H 0.5537(6) 0.4801(4) 0.3751(4) 0.040(17) Uiso 1 calc R . C4 C 0.4600(6) 0.6903(4) 0.0713(4) 0.0246(9) Uani 1 d . . C5 C 0.3674(6) 0.6687(5) 0.0181(4) 0.0289(10) Uani 1 d . . C6 C 0.3839(7) 0.7087(5) -0.0912(4) 0.0337(11) Uani 1 d . . H6 H 0.3216(7) 0.6972(5) -0.1289(4) 0.036(17) Uiso 1 calc R . C7 C 0.4930(7) 0.7653(5) -0.1429(4) 0.0332(12) Uani 1 d . . C8 C 0.5901(7) 0.7835(5) -0.0915(4) 0.0321(11) Uani 1 d . . H8 H 0.6650(7) 0.8202(5) -0.1298(4) 0.028(15) Uiso 1 calc R . C9 C 0.5740(6) 0.7459(5) 0.0186(4) 0.0276(10) Uani 1 d . . C10 C 0.2513(7) 0.6024(6) 0.0759(5) 0.0375(12) Uani 1 d . . H10A H 0.3057(8) 0.5200(9) 0.0901(37) 0.078(28) Uiso 1 calc R . H10B H 0.1830(38) 0.6110(38) 0.0313(18) 0.054(21) Uiso 1 calc R . H10C H 0.1915(41) 0.6343(30) 0.1431(20) 0.072(26) Uiso 1 calc R . C11 C 0.6779(8) 0.7669(7) 0.0756(5) 0.046(2) Uani 1 d . . H11A H 0.7431(46) 0.8103(44) 0.0259(13) 0.049(20) Uiso 1 calc R . H11B H 0.7418(47) 0.6921(7) 0.1018(40) 0.104(37) Uiso 1 calc R . H11C H 0.6152(8) 0.8116(44) 0.1355(28) 0.102(36) Uiso 1 calc R . C12 C 0.2747(5) 0.6335(4) 0.4664(4) 0.0206(8) Uani 1 d . . C13 C 0.2677(6) 0.7212(4) 0.5246(4) 0.0231(9) Uani 1 d . . C14 C 0.1865(6) 0.7207(5) 0.6333(4) 0.0317(11) Uani 1 d . . H14 H 0.1784(6) 0.7793(5) 0.6733(4) 0.032(16) Uiso 1 calc R . C15 C 0.1182(6) 0.6325(5) 0.6813(4) 0.0306(11) Uani 1 d . . C16 C 0.1274(6) 0.5441(5) 0.6236(4) 0.0301(10) Uani 1 d . . H16 H 0.0797(6) 0.4861(5) 0.6575(4) 0.047(19) Uiso 1 calc R . C17 C 0.2079(6) 0.5427(4) 0.5157(4) 0.0251(9) Uani 1 d . . C18 C 0.3502(7) 0.8123(5) 0.4741(4) 0.0353(12) Uani 1 d . . H18A H 0.2953(36) 0.8691(28) 0.4253(34) 0.099(34) Uiso 1 calc R . H18B H 0.4543(22) 0.7742(7) 0.4349(37) 0.067(25) Uiso 1 calc R . H18C H 0.3537(57) 0.8521(34) 0.5297(6) 0.086(30) Uiso 1 calc R . C19 C 0.2231(7) 0.4438(5) 0.4543(5) 0.0357(12) Uani 1 d . . H19A H 0.3193(34) 0.3822(25) 0.4563(42) 0.122(40) Uiso 1 calc R . H19B H 0.2219(71) 0.4741(13) 0.3804(13) 0.082(29) Uiso 1 calc R . H19C H 0.1377(39) 0.4122(36) 0.4872(30) 0.075(27) Uiso 1 calc R . C21 C -0.0100(6) 0.7525(4) 0.3408(4) 0.0279(10) Uani 1 d . . H21 H 0.0370(6) 0.6674(4) 0.3584(4) 0.059(22) Uiso 1 calc R . C22 C -0.1004(6) 0.8123(4) 0.4384(4) 0.0299(10) Uani 1 d . . H22 H -0.0630(6) 0.8113(4) 0.4971(4) 0.030(15) Uiso 1 calc R . C23 C -0.2483(7) 0.8696(5) 0.4284(5) 0.0359(12) Uani 1 d . . H23 H -0.3278(7) 0.9158(5) 0.4785(5) 0.069(26) Uiso 1 calc R . C24 C -0.2621(6) 0.8472(5) 0.3281(5) 0.0375(12) Uani 1 d . . H24 H -0.3515(6) 0.8765(5) 0.3026(5) 0.038(17) Uiso 1 calc R . C25 C -0.1231(7) 0.7761(5) 0.2769(5) 0.0343(11) Uani 1 d . . H25 H -0.1027(7) 0.7469(5) 0.2114(5) 0.018(13) Uiso 1 calc R . C31 C -0.0048(7) 1.0030(4) 0.2450(5) 0.0343(12) Uani 1 d . . H31 H -0.1084(7) 1.0168(4) 0.2836(5) 0.071(26) Uiso 1 calc R . C32 C 0.0572(9) 0.9707(5) 0.1380(5) 0.048(2) Uani 1 d . . H32 H 0.0017(9) 0.9636(5) 0.0928(5) 0.057(23) Uiso 1 calc R . C33 C 0.2169(9) 0.9518(6) 0.1132(6) 0.057(2) Uani 1 d . . H33 H 0.2877(9) 0.9295(6) 0.0482(6) 0.069(26) Uiso 1 calc R . C34 C 0.2532(8) 0.9726(5) 0.2054(8) 0.063(2) Uani 1 d . . H34 H 0.3525(8) 0.9622(5) 0.2118(8) 0.052(21) Uiso 1 calc R . C35 C 0.1147(8) 1.0109(5) 0.2839(6) 0.0454(15) Uani 1 d . . H35 H 0.1035(8) 1.0367(5) 0.3494(6) 0.082(30) Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0255(3) 0.0148(3) 0.0237(3) 0.0028(2) -0.0095(2) -0.0041(2) Br1 0.1016(6) 0.0514(4) 0.0218(3) 0.0059(2) -0.0205(3) -0.0229(4) Br2 0.0381(3) 0.0834(5) 0.0243(3) -0.0045(3) 0.0017(2) -0.0039(3) N1 0.027(2) 0.022(2) 0.019(2) 0.0018(14) -0.0083(15) -0.002(2) N2 0.022(2) 0.018(2) 0.019(2) 0.0007(13) -0.0088(14) -0.0011(14) C1 0.023(2) 0.016(2) 0.022(2) 0.0028(15) -0.010(2) -0.006(2) C2 0.024(2) 0.028(2) 0.027(2) -0.004(2) -0.006(2) 0.004(2) C3 0.028(2) 0.024(2) 0.026(2) 0.002(2) -0.010(2) 0.003(2) C4 0.028(2) 0.025(2) 0.018(2) -0.002(2) -0.005(2) -0.006(2) C5 0.034(3) 0.029(2) 0.024(2) -0.006(2) -0.008(2) -0.008(2) C6 0.050(3) 0.030(3) 0.024(2) -0.004(2) -0.014(2) -0.011(2) C7 0.052(3) 0.027(2) 0.018(2) -0.004(2) -0.009(2) -0.008(2) C8 0.039(3) 0.033(3) 0.023(2) 0.001(2) -0.004(2) -0.013(2) C9 0.030(2) 0.030(2) 0.022(2) -0.003(2) -0.006(2) -0.009(2) C10 0.040(3) 0.043(3) 0.038(3) -0.002(2) -0.012(2) -0.020(3) C11 0.048(4) 0.067(4) 0.038(3) 0.006(3) -0.019(3) -0.034(3) C12 0.023(2) 0.016(2) 0.020(2) 0.0001(15) -0.009(2) -0.002(2) C13 0.028(2) 0.017(2) 0.024(2) 0.001(2) -0.012(2) -0.003(2) C14 0.035(3) 0.033(3) 0.024(2) -0.007(2) -0.013(2) 0.000(2) C15 0.023(2) 0.039(3) 0.022(2) -0.001(2) -0.005(2) -0.002(2) C16 0.026(2) 0.031(2) 0.030(2) 0.006(2) -0.008(2) -0.010(2) C17 0.027(2) 0.023(2) 0.026(2) 0.001(2) -0.013(2) -0.007(2) C18 0.056(4) 0.024(2) 0.034(3) 0.001(2) -0.018(3) -0.019(2) C19 0.051(3) 0.024(2) 0.041(3) -0.001(2) -0.021(3) -0.016(2) C21 0.027(2) 0.022(2) 0.035(2) 0.003(2) -0.012(2) -0.007(2) C22 0.038(3) 0.026(2) 0.029(2) 0.002(2) -0.011(2) -0.014(2) C23 0.033(3) 0.029(3) 0.038(3) -0.002(2) 0.001(2) -0.010(2) C24 0.023(2) 0.039(3) 0.051(3) 0.003(2) -0.017(2) -0.007(2) C25 0.037(3) 0.035(3) 0.039(3) -0.004(2) -0.018(2) -0.013(2) C31 0.035(3) 0.014(2) 0.046(3) 0.002(2) -0.013(2) 0.001(2) C32 0.067(4) 0.025(3) 0.037(3) 0.010(2) -0.022(3) 0.003(3) C33 0.063(4) 0.029(3) 0.046(4) 0.015(3) 0.008(3) -0.002(3) C34 0.042(4) 0.022(3) 0.117(7) 0.024(3) -0.022(4) -0.017(3) C35 0.063(4) 0.020(2) 0.060(4) 0.003(2) -0.032(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.885(4) . ? Ni1 C21 2.021(5) . ? Ni1 C31 2.083(5) . ? Ni1 C34 2.113(6) . ? Ni1 C35 2.126(6) . ? Ni1 C32 2.189(6) . ? Ni1 C33 2.196(6) . ? Br1 C7 1.901(5) . ? Br2 C15 1.892(5) . ? N1 C1 1.352(6) . ? N1 C2 1.386(6) . ? N1 C4 1.439(6) . ? N2 C1 1.377(5) . ? N2 C3 1.384(6) . ? N2 C12 1.426(6) . ? C2 C3 1.328(7) . ? C4 C5 1.381(7) . ? C4 C9 1.399(7) . ? C5 C6 1.388(7) . ? C5 C10 1.510(7) . ? C6 C7 1.368(8) . ? C7 C8 1.379(8) . ? C8 C9 1.393(7) . ? C9 C11 1.505(7) . ? C12 C13 1.396(6) . ? C12 C17 1.403(6) . ? C13 C14 1.393(7) . ? C13 C18 1.500(7) . ? C14 C15 1.382(8) . ? C15 C16 1.390(8) . ? C16 C17 1.383(7) . ? C17 C19 1.512(7) . ? C21 C25 1.465(7) . ? C21 C22 1.468(7) . ? C22 C23 1.362(8) . ? C23 C24 1.436(9) . ? C24 C25 1.354(8) . ? C31 C35 1.407(9) . ? C31 C32 1.417(9) . ? C32 C33 1.391(11) . ? C33 C34 1.431(12) . ? C34 C35 1.394(11) . ? 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 C1 Ni1 C21 95.3(2) . . ? C1 Ni1 C31 167.9(2) . . ? C21 Ni1 C31 95.8(2) . . ? C1 Ni1 C34 103.3(2) . . ? C21 Ni1 C34 157.5(3) . . ? C31 Ni1 C34 64.8(2) . . ? C1 Ni1 C35 129.9(2) . . ? C21 Ni1 C35 119.1(3) . . ? C31 Ni1 C35 39.1(2) . . ? C34 Ni1 C35 38.4(3) . . ? C1 Ni1 C32 139.8(2) . . ? C21 Ni1 C32 108.6(3) . . ? C31 Ni1 C32 38.6(2) . . ? C34 Ni1 C32 64.1(3) . . ? C35 Ni1 C32 64.6(3) . . ? C1 Ni1 C33 108.9(2) . . ? C21 Ni1 C33 143.9(3) . . ? C31 Ni1 C33 63.6(2) . . ? C34 Ni1 C33 38.7(3) . . ? C35 Ni1 C33 64.0(3) . . ? C32 Ni1 C33 37.0(3) . . ? C1 N1 C2 112.4(4) . . ? C1 N1 C4 125.8(4) . . ? C2 N1 C4 121.8(4) . . ? C1 N2 C3 110.8(4) . . ? C1 N2 C12 127.1(4) . . ? C3 N2 C12 121.9(4) . . ? N1 C1 N2 102.9(4) . . ? N1 C1 Ni1 128.1(3) . . ? N2 C1 Ni1 128.9(3) . . ? C3 C2 N1 106.2(4) . . ? C2 C3 N2 107.6(4) . . ? C5 C4 C9 122.8(4) . . ? C5 C4 N1 119.6(4) . . ? C9 C4 N1 117.6(4) . . ? C4 C5 C6 118.3(5) . . ? C4 C5 C10 121.6(5) . . ? C6 C5 C10 120.1(5) . . ? C7 C6 C5 119.2(5) . . ? C6 C7 C8 122.9(5) . . ? C6 C7 Br1 119.1(4) . . ? C8 C7 Br1 117.9(4) . . ? C7 C8 C9 118.9(5) . . ? C8 C9 C4 117.7(5) . . ? C8 C9 C11 119.3(5) . . ? C4 C9 C11 123.0(5) . . ? C13 C12 C17 121.7(4) . . ? C13 C12 N2 120.0(4) . . ? C17 C12 N2 118.0(4) . . ? C14 C13 C12 118.7(4) . . ? C14 C13 C18 119.7(5) . . ? C12 C13 C18 121.6(4) . . ? C15 C14 C13 119.6(5) . . ? C14 C15 C16 121.6(5) . . ? C14 C15 Br2 119.3(4) . . ? C16 C15 Br2 119.0(4) . . ? C17 C16 C15 119.7(5) . . ? C16 C17 C12 118.6(4) . . ? C16 C17 C19 119.6(5) . . ? C12 C17 C19 121.7(4) . . ? C25 C21 C22 104.3(4) . . ? C25 C21 Ni1 108.5(4) . . ? C22 C21 Ni1 108.0(3) . . ? C23 C22 C21 108.5(5) . . ? C22 C23 C24 109.2(5) . . ? C25 C24 C23 108.6(5) . . ? C24 C25 C21 109.4(5) . . ? C35 C31 C32 109.4(6) . . ? C35 C31 Ni1 72.1(3) . . ? C32 C31 Ni1 74.7(3) . . ? C33 C32 C31 107.0(7) . . ? C33 C32 Ni1 71.8(4) . . ? C31 C32 Ni1 66.6(3) . . ? C32 C33 C34 108.1(6) . . ? C32 C33 Ni1 71.2(3) . . ? C34 C33 Ni1 67.5(3) . . ? C35 C34 C33 108.4(6) . . ? C35 C34 Ni1 71.3(4) . . ? C33 C34 Ni1 73.8(4) . . ? C34 C35 C31 106.8(6) . . ? C34 C35 Ni1 70.3(4) . . ? C31 C35 Ni1 68.8(3) . . ? _refine_diff_density_max 2.029 _refine_diff_density_min -2.293 _refine_diff_density_rms 0.189 data_6(THF) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H34 N4 Ni O' _chemical_formula_weight 453.26 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.165(3) _cell_length_b 9.693(2) _cell_length_c 23.201(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.82(2) _cell_angle_gamma 90.00 _cell_volume 2497.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 4.58 _cell_measurement_theta_max 12.51 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method ? _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 112.67 _diffrn_reflns_number 7800 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5726 _reflns_number_observed 4461 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1959P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5709 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_obs 0.0550 _refine_ls_wR_factor_all 0.2675 _refine_ls_wR_factor_obs 0.1736 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 0.843 _refine_ls_restrained_S_all 1.144 _refine_ls_restrained_S_obs 0.843 _refine_ls_shift/esd_max 0.311 _refine_ls_shift/esd_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.91727(4) 0.49131(4) 0.18919(2) 0.0263(2) Uani 1 d . . N11 N 0.8702(3) 0.2142(3) 0.14392(11) 0.0315(6) Uani 1 d . . N1 N 1.0529(2) 0.6124(3) 0.10124(12) 0.0306(6) Uani 1 d . . N2 N 0.8653(2) 0.6002(3) 0.07133(11) 0.0305(6) Uani 1 d . . C1 C 0.9456(3) 0.5695(3) 0.11754(13) 0.0276(6) Uani 1 d . . C11 C 0.9483(3) 0.3068(3) 0.17007(13) 0.0297(6) Uani 1 d . . C2 C 1.0403(3) 0.6671(3) 0.04523(14) 0.0331(7) Uani 1 d . . C4 C 1.1673(3) 0.6065(4) 0.1375(2) 0.0374(8) Uani 1 d . . H4A H 1.2067(14) 0.6944(11) 0.1370(11) 0.062(14) Uiso 1 calc R . H4B H 1.2175(12) 0.5370(24) 0.1229(9) 0.074(17) Uiso 1 calc R . H4C H 1.1529(4) 0.5842(33) 0.1765(3) 0.055(13) Uiso 1 calc R . C12 C 0.9265(4) 0.0873(4) 0.13764(15) 0.0396(8) Uani 1 d . . C3 C 0.9220(3) 0.6602(4) 0.02689(14) 0.0335(7) Uani 1 d . . C14 C 0.7423(3) 0.2385(4) 0.12944(15) 0.0382(7) Uani 1 d . . H14A H 0.6973(3) 0.1652(17) 0.1448(11) 0.076(17) Uiso 1 calc R . H14B H 0.7247(6) 0.2417(32) 0.0881(2) 0.062(14) Uiso 1 calc R . H14C H 0.7204(6) 0.3248(15) 0.1458(11) 0.047(12) Uiso 1 calc R . C23 C 0.9098(5) 0.6723(4) 0.2385(2) 0.0535(11) Uani 1 d . . H23 H 0.9420(5) 0.7552(4) 0.2271(2) 0.095(21) Uiso 1 calc R . C7 C 0.7359(3) 0.5843(5) 0.0691(2) 0.0451(9) Uani 1 d . . H7A H 0.7087(5) 0.5218(25) 0.0384(8) 0.121(31) Uiso 1 calc R . H7B H 0.6979(4) 0.6723(7) 0.0620(13) 0.057(14) Uiso 1 calc R . H7C H 0.7153(4) 0.5481(29) 0.1053(5) 0.029(9) Uiso 1 calc R . C21 C 0.8895(5) 0.4605(5) 0.2757(2) 0.0493(10) Uani 1 d . . H21 H 0.9061(5) 0.3754(5) 0.2933(2) 0.085(19) Uiso 1 calc R . C13 C 1.0413(4) 0.1007(4) 0.1596(2) 0.0461(9) Uani 1 d . . C15 C 0.8598(5) -0.0344(5) 0.1106(2) 0.0565(12) Uani 1 d . . H15A H 0.8296(22) -0.0123(11) 0.0714(5) 0.019(9) Uiso 1 calc R . H15B H 0.7938(16) -0.0568(19) 0.1323(8) 0.068(16) Uiso 1 calc R . H15C H 0.9133(9) -0.1119(9) 0.1105(11) 0.072(17) Uiso 1 calc R . C17 C 1.1640(4) 0.2900(5) 0.2105(2) 0.0561(11) Uani 1 d . . H17A H 1.2279(8) 0.2868(31) 0.1858(5) 0.054(13) Uiso 1 calc R . H17B H 1.1853(16) 0.2349(21) 0.2444(8) 0.084(18) Uiso 1 calc R . H17C H 1.1513(9) 0.3837(12) 0.2218(12) 0.072(17) Uiso 1 calc R . C16 C 1.1419(6) 0.0004(5) 0.1660(3) 0.070(2) Uani 1 d . . H16A H 1.1669(24) -0.0135(31) 0.2064(3) 0.090(25) Uiso 1 calc R . H16B H 1.2082(14) 0.0356(18) 0.1471(15) 0.081(20) Uiso 1 calc R . H16C H 1.1158(12) -0.0857(13) 0.1486(15) 0.091(21) Uiso 1 calc R . C24 C 0.7936(4) 0.6287(5) 0.2236(2) 0.0523(10) Uani 1 d . . H24 H 0.7349(4) 0.6788(5) 0.2013(2) 0.077(18) Uiso 1 calc R . C6 C 0.8546(4) 0.7077(5) -0.0285(2) 0.0509(10) Uani 1 d . . H6A H 0.8159(26) 0.7941(18) -0.0222(4) 0.062(15) Uiso 1 calc R . H6B H 0.7949(22) 0.6402(17) -0.0415(8) 0.074(17) Uiso 1 calc R . H6C H 0.9096(6) 0.7193(35) -0.0574(5) 0.106(24) Uiso 1 calc R . C22 C 0.9730(4) 0.5718(6) 0.2739(2) 0.0551(12) Uani 1 d . . H22 H 1.0512(4) 0.5770(6) 0.2918(2) 0.032(9) Uiso 1 calc R . C5 C 1.1427(4) 0.7241(5) 0.0166(2) 0.0514(11) Uani 1 d . . H5A H 1.2063(11) 0.6572(13) 0.0180(12) 0.065(16) Uiso 1 calc R . H5B H 1.1717(18) 0.8065(18) 0.0363(8) 0.062(15) Uiso 1 calc R . H5C H 1.1163(8) 0.7456(29) -0.0231(4) 0.048(12) Uiso 1 calc R . C34 C 0.4457(4) 0.4551(8) 0.0892(3) 0.0682(14) Uani 1 d . . H34 H 0.4389(4) 0.3876(8) 0.0606(3) 0.089(22) Uiso 1 calc R . C32 C 0.4609(4) 0.6563(7) 0.1295(3) 0.069(2) Uani 1 d . . H32 H 0.4661(4) 0.7517(7) 0.1331(3) 0.144(35) Uiso 1 calc R . C33 C 0.4443(5) 0.5898(8) 0.0790(3) 0.071(2) Uani 1 d . . H33 H 0.4335(5) 0.6310(8) 0.0427(3) 0.203(49) Uiso 1 calc R . C35 C 0.4580(5) 0.4294(9) 0.1455(4) 0.096(3) Uani 1 d . . H35 H 0.4593(5) 0.3431(9) 0.1631(4) 0.156(38) Uiso 1 calc R . C31 C 0.4694(5) 0.5661(13) 0.1754(3) 0.114(4) Uani 1 d . . H31 H 0.4796(5) 0.5851(13) 0.2149(3) 0.195(43) Uiso 1 calc R . N12 N 1.0541(3) 0.2363(3) 0.17948(13) 0.0371(6) Uani 1 d . . C25 C 0.7769(4) 0.5011(4) 0.2464(2) 0.0491(11) Uani 1 d . . H25 H 0.7058(4) 0.4505(4) 0.2433(2) 0.089(20) Uiso 1 calc R . C51 C 0.6424(12) 0.0090(20) 0.0075(9) 0.098(6) Uani 0.50 d P . C52 C 0.5418(17) -0.0286(27) 0.0474(9) 0.109(8) Uani 0.50 d P . O54 O 0.5054(43) -0.0315(44) -0.0404(27) 0.420(41) Uani 0.50 d P . C53 C 0.4425(40) -0.0459(57) 0.0045(16) 0.223(25) Uani 0.50 d P . C55 C 0.6028(17) 0.0117(17) -0.0495(11) 0.104(6) Uani 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0275(3) 0.0274(3) 0.0242(3) -0.00065(13) 0.0037(2) 0.00064(14) N11 0.041(2) 0.0290(13) 0.0257(12) -0.0010(10) 0.0072(11) -0.0001(11) N1 0.0289(13) 0.0332(13) 0.0298(13) 0.0005(10) 0.0034(10) 0.0010(11) N2 0.0327(14) 0.0311(13) 0.0266(12) -0.0001(10) -0.0019(11) 0.0004(11) C1 0.0246(14) 0.0268(14) 0.0306(14) -0.0020(11) -0.0003(11) 0.0027(11) C11 0.032(2) 0.0326(15) 0.0248(13) 0.0014(11) 0.0028(12) 0.0022(12) C2 0.039(2) 0.033(2) 0.0289(15) -0.0006(12) 0.0100(13) 0.0032(13) C4 0.0240(15) 0.047(2) 0.042(2) 0.0054(15) 0.0058(13) 0.0027(14) C12 0.061(2) 0.030(2) 0.030(2) -0.0022(12) 0.013(2) 0.004(2) C3 0.037(2) 0.035(2) 0.0290(15) -0.0010(12) 0.0069(13) 0.0017(13) C14 0.039(2) 0.043(2) 0.033(2) -0.0025(14) 0.0039(14) -0.0073(15) C23 0.085(3) 0.035(2) 0.045(2) -0.010(2) 0.028(2) -0.006(2) C7 0.038(2) 0.055(2) 0.040(2) 0.010(2) -0.007(2) -0.005(2) C21 0.075(3) 0.046(2) 0.030(2) 0.003(2) 0.019(2) 0.014(2) C13 0.062(3) 0.036(2) 0.041(2) 0.0002(15) 0.008(2) 0.014(2) C15 0.084(4) 0.036(2) 0.050(2) -0.009(2) 0.006(2) -0.003(2) C17 0.044(2) 0.053(2) 0.068(3) 0.007(2) -0.010(2) 0.011(2) C16 0.073(4) 0.051(3) 0.086(5) 0.002(2) 0.006(3) 0.030(2) C24 0.064(3) 0.054(2) 0.039(2) -0.009(2) 0.006(2) 0.020(2) C6 0.058(3) 0.060(3) 0.033(2) 0.006(2) -0.005(2) 0.000(2) C22 0.047(2) 0.084(3) 0.033(2) -0.024(2) 0.000(2) 0.001(2) C5 0.044(2) 0.070(3) 0.044(2) 0.013(2) 0.020(2) -0.003(2) C34 0.030(2) 0.102(4) 0.072(3) -0.009(3) 0.007(2) 0.001(3) C32 0.027(2) 0.096(4) 0.084(4) -0.022(3) 0.008(2) -0.011(2) C33 0.045(3) 0.108(5) 0.061(3) 0.001(3) -0.002(2) -0.007(3) C35 0.051(3) 0.119(6) 0.121(6) 0.055(5) 0.022(3) 0.030(4) C31 0.033(2) 0.264(11) 0.044(3) -0.036(5) -0.007(2) 0.033(4) N12 0.038(2) 0.0344(14) 0.0383(15) 0.0034(12) 0.0036(12) 0.0090(12) C25 0.045(2) 0.062(3) 0.044(2) -0.013(2) 0.019(2) -0.010(2) C51 0.036(6) 0.142(16) 0.108(13) 0.028(9) -0.019(7) -0.015(7) C52 0.065(10) 0.170(18) 0.083(11) 0.026(12) -0.033(10) -0.043(11) O54 0.360(51) 0.327(45) 0.656(94) -0.181(45) 0.450(66) -0.147(34) C53 0.224(43) 0.322(57) 0.131(23) -0.037(29) 0.062(27) -0.186(45) C55 0.069(10) 0.115(14) 0.128(16) -0.016(10) 0.013(10) 0.004(8) _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 C1 1.883(3) . ? Ni1 C11 1.883(3) . ? Ni1 C21 2.084(4) . ? Ni1 C23 2.101(4) . ? Ni1 C24 2.131(4) . ? Ni1 C22 2.147(4) . ? Ni1 C25 2.156(4) . ? N11 C11 1.351(4) . ? N11 C12 1.395(4) . ? N11 C14 1.453(5) . ? N1 C1 1.357(4) . ? N1 C2 1.398(4) . ? N1 C4 1.457(4) . ? N2 C1 1.359(4) . ? N2 C3 1.391(4) . ? N2 C7 1.449(5) . ? C11 N12 1.364(4) . ? C2 C3 1.347(5) . ? C2 C5 1.486(5) . ? C12 C13 1.336(6) . ? C12 C15 1.499(6) . ? C3 C6 1.495(5) . ? C23 C24 1.375(7) . ? C23 C22 1.414(7) . ? C21 C25 1.423(7) . ? C21 C22 1.430(7) . ? C13 N12 1.396(5) . ? C13 C16 1.482(6) . ? C17 N12 1.454(5) . ? C24 C25 1.365(6) . ? C34 C35 1.322(10) . ? C34 C33 1.327(10) . ? C32 C33 1.333(8) . ? C32 C31 1.375(11) . ? C35 C31 1.495(14) . ? C51 C53 1.03(6) 3_655 ? C51 C55 1.35(3) . ? C51 C52 1.57(3) . ? C51 O54 1.90(3) 3_655 ? C51 O54 1.84(7) . ? C52 O54 0.79(6) 3_655 ? C52 C53 1.43(5) 3_655 ? C52 C53 1.42(4) . ? C52 C55 1.63(3) 3_655 ? O54 C52 0.79(6) 3_655 ? O54 C55 1.20(4) . ? O54 C53 1.22(5) 3_655 ? O54 C53 1.32(4) . ? O54 C51 1.90(3) 3_655 ? C53 C51 1.03(6) 3_655 ? C53 C55 1.25(4) 3_655 ? C53 O54 1.22(5) 3_655 ? C53 C52 1.43(5) 3_655 ? C53 C53 1.59(5) 3_655 ? C55 C53 1.25(4) 3_655 ? C55 C52 1.63(3) 3_655 ? 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 C1 Ni1 C11 97.07(13) . . ? C1 Ni1 C21 164.4(2) . . ? C11 Ni1 C21 98.0(2) . . ? C1 Ni1 C23 99.48(15) . . ? C11 Ni1 C23 160.0(2) . . ? C21 Ni1 C23 64.9(2) . . ? C1 Ni1 C24 104.6(2) . . ? C11 Ni1 C24 145.4(2) . . ? C21 Ni1 C24 64.1(2) . . ? C23 Ni1 C24 37.9(2) . . ? C1 Ni1 C22 127.1(2) . . ? C11 Ni1 C22 121.2(2) . . ? C21 Ni1 C22 39.5(2) . . ? C23 Ni1 C22 38.9(2) . . ? C24 Ni1 C22 64.4(2) . . ? C1 Ni1 C25 136.4(2) . . ? C11 Ni1 C25 110.44(15) . . ? C21 Ni1 C25 39.2(2) . . ? C23 Ni1 C25 63.7(2) . . ? C24 Ni1 C25 37.1(2) . . ? C22 Ni1 C25 65.3(2) . . ? C11 N11 C12 110.8(3) . . ? C11 N11 C14 124.7(3) . . ? C12 N11 C14 124.2(3) . . ? C1 N1 C2 111.5(3) . . ? C1 N1 C4 125.0(3) . . ? C2 N1 C4 123.5(3) . . ? C1 N2 C3 111.3(3) . . ? C1 N2 C7 125.5(3) . . ? C3 N2 C7 123.0(3) . . ? N1 C1 N2 104.1(3) . . ? N1 C1 Ni1 127.0(2) . . ? N2 C1 Ni1 128.9(2) . . ? N11 C11 N12 104.3(3) . . ? N11 C11 Ni1 127.7(2) . . ? N12 C11 Ni1 128.0(3) . . ? C3 C2 N1 106.1(3) . . ? C3 C2 C5 130.6(3) . . ? N1 C2 C5 123.2(3) . . ? C13 C12 N11 107.4(3) . . ? C13 C12 C15 130.8(4) . . ? N11 C12 C15 121.8(4) . . ? C2 C3 N2 107.0(3) . . ? C2 C3 C6 130.4(3) . . ? N2 C3 C6 122.6(3) . . ? C24 C23 C22 109.7(4) . . ? C24 C23 Ni1 72.2(2) . . ? C22 C23 Ni1 72.3(2) . . ? C25 C21 C22 108.9(4) . . ? C25 C21 Ni1 73.1(2) . . ? C22 C21 Ni1 72.6(2) . . ? C12 C13 N12 106.3(3) . . ? C12 C13 C16 131.5(4) . . ? N12 C13 C16 122.2(4) . . ? C25 C24 C23 110.1(4) . . ? C25 C24 Ni1 72.4(2) . . ? C23 C24 Ni1 69.9(2) . . ? C23 C22 C21 104.4(4) . . ? C23 C22 Ni1 68.8(2) . . ? C21 C22 Ni1 67.9(2) . . ? C35 C34 C33 111.1(7) . . ? C33 C32 C31 111.4(7) . . ? C34 C33 C32 108.7(6) . . ? C34 C35 C31 106.6(7) . . ? C32 C31 C35 102.0(5) . . ? C11 N12 C13 111.1(3) . . ? C11 N12 C17 125.0(3) . . ? C13 N12 C17 123.6(3) . . ? C24 C25 C21 106.7(4) . . ? C24 C25 Ni1 70.5(2) . . ? C21 C25 Ni1 67.7(2) . . ? C53 C51 C55 61.7(23) 3_655 . ? C53 C51 C52 62.8(25) 3_655 . ? C55 C51 C52 113.5(13) . . ? C53 C51 O54 41.5(30) 3_655 3_655 ? C55 C51 O54 100.3(24) . 3_655 ? C52 C51 O54 24.0(19) . 3_655 ? C53 C51 O54 38.9(29) 3_655 . ? C55 C51 O54 40.8(15) . . ? C52 C51 O54 72.9(12) . . ? O54 C51 O54 64.2(28) 3_655 . ? O54 C52 C53 65.9(43) 3_655 3_655 ? O54 C52 C53 59.2(45) 3_655 . ? C53 C52 C53 67.9(19) 3_655 . ? O54 C52 C51 102.1(34) 3_655 . ? C53 C52 C51 39.6(22) 3_655 . ? C53 C52 C51 99.6(19) . . ? O54 C52 C55 44.8(28) 3_655 3_655 ? C53 C52 C55 100.4(25) 3_655 3_655 ? C53 C52 C55 47.8(18) . 3_655 ? C51 C52 C55 139.9(15) . 3_655 ? C52 O54 C55 107.6(48) 3_655 . ? C52 O54 C53 87.0(53) 3_655 3_655 ? C55 O54 C53 62.0(32) . 3_655 ? C52 O54 C53 81.0(36) 3_655 . ? C55 O54 C53 137.4(63) . . ? C53 O54 C53 77.4(40) 3_655 . ? C52 O54 C51 53.8(24) 3_655 3_655 ? C55 O54 C51 150.1(34) . 3_655 ? C53 O54 C51 91.6(31) 3_655 3_655 ? C53 O54 C51 31.0(25) . 3_655 ? C52 O54 C51 117.5(50) 3_655 . ? C55 O54 C51 47.2(27) . . ? C53 O54 C51 31.7(39) 3_655 . ? C53 O54 C51 91.3(43) . . ? C51 O54 C51 115.8(28) 3_655 . ? C51 C53 C55 72.1(35) 3_655 3_655 ? C51 C53 O54 109.4(64) 3_655 3_655 ? C55 C53 O54 58.2(24) 3_655 3_655 ? C51 C53 O54 107.5(47) 3_655 . ? C55 C53 O54 157.3(45) 3_655 . ? O54 C53 O54 102.6(40) 3_655 . ? C51 C53 C52 77.6(39) 3_655 3_655 ? C55 C53 C52 131.5(51) 3_655 3_655 ? O54 C53 C52 100.0(40) 3_655 3_655 ? O54 C53 C52 33.2(24) . 3_655 ? C51 C53 C52 141.4(49) 3_655 . ? C55 C53 C52 74.7(24) 3_655 . ? O54 C53 C52 33.7(30) 3_655 . ? O54 C53 C52 95.8(37) . . ? C52 C53 C52 112.1(19) 3_655 . ? C51 C53 C53 120.3(70) 3_655 3_655 ? C55 C53 C53 111.1(39) 3_655 3_655 ? O54 C53 C53 54.0(23) 3_655 3_655 ? O54 C53 C53 48.6(28) . 3_655 ? C52 C53 C53 55.9(25) 3_655 3_655 ? C52 C53 C53 56.2(27) . 3_655 ? C53 C55 O54 59.9(26) 3_655 . ? C53 C55 C51 46.2(28) 3_655 . ? O54 C55 C51 92.0(37) . . ? C53 C55 C52 57.5(23) 3_655 3_655 ? O54 C55 C52 27.6(28) . 3_655 ? C51 C55 C52 101.6(17) . 3_655 ? _refine_diff_density_max 1.131 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.160 data_7(THF)0.5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H76 Cr2 N8 O' _chemical_formula_weight 933.21 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(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 25.839(5) _cell_length_b 9.501(2) _cell_length_c 21.716(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.064(12) _cell_angle_gamma 90.00 _cell_volume 5096.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 5.88 _cell_measurement_theta_max 12.80 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method ? _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 99.97 _diffrn_reflns_number 14019 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11642 _reflns_number_observed 8213 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11638 _refine_ls_number_parameters 714 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_obs 0.0469 _refine_ls_wR_factor_all 0.1399 _refine_ls_wR_factor_obs 0.1177 _refine_ls_goodness_of_fit_all 1.112 _refine_ls_goodness_of_fit_obs 1.150 _refine_ls_restrained_S_all 1.135 _refine_ls_restrained_S_obs 1.150 _refine_ls_shift/esd_max 7.552 _refine_ls_shift/esd_mean 0.029 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 0.064821(14) 0.57826(4) 0.37461(2) 0.02348(10) Uani 1 d . . N1 N 0.15836(8) 0.6809(2) 0.49289(9) 0.0263(4) Uani 1 d . . N2 N 0.18544(8) 0.6796(2) 0.40940(9) 0.0270(4) Uani 1 d . . N11 N 0.10591(8) 0.2848(2) 0.34655(9) 0.0265(4) Uani 1 d . . N12 N 0.07764(8) 0.2715(2) 0.42891(9) 0.0279(4) Uani 1 d . . C1 C 0.14127(9) 0.6522(2) 0.42905(10) 0.0244(5) Uani 1 d . . C2 C 0.21190(9) 0.7242(3) 0.51271(12) 0.0305(5) Uani 1 d . . C3 C 0.22912(9) 0.7235(3) 0.45993(12) 0.0300(5) Uani 1 d . . C4 C 0.12463(10) 0.6677(3) 0.53597(12) 0.0340(6) Uani 1 d . . H4A H 0.1267(6) 0.7529(8) 0.5603(7) 0.058(10) Uiso 1 calc R . H4B H 0.1372(5) 0.5902(13) 0.5649(6) 0.060(10) Uiso 1 calc R . H4C H 0.0878(2) 0.6512(20) 0.51107(13) 0.035(7) Uiso 1 calc R . C5 C 0.24056(11) 0.7616(4) 0.58109(14) 0.0451(7) Uani 1 d . . H5A H 0.2422(8) 0.6804(7) 0.6079(2) 0.095(15) Uiso 1 calc R . H5B H 0.2213(5) 0.8357(17) 0.5949(4) 0.076(12) Uiso 1 calc R . H5C H 0.2766(3) 0.7925(23) 0.5843(2) 0.063(11) Uiso 1 calc R . C6 C 0.28282(11) 0.7589(3) 0.4514(2) 0.0453(7) Uani 1 d . . H6A H 0.2785(2) 0.8320(15) 0.4198(7) 0.054(10) Uiso 1 calc R . H6B H 0.2978(4) 0.6768(6) 0.4373(9) 0.050(9) Uiso 1 calc R . H6C H 0.3068(3) 0.7906(20) 0.4917(3) 0.063(11) Uiso 1 calc R . C7 C 0.18713(11) 0.6651(3) 0.34312(12) 0.0350(6) Uani 1 d . . H7A H 0.2078(6) 0.5832(11) 0.3396(2) 0.041(8) Uiso 1 calc R . H7B H 0.2037(7) 0.7471(9) 0.3313(3) 0.064(11) Uiso 1 calc R . H7C H 0.15096(12) 0.6555(20) 0.3149(2) 0.043(8) Uiso 1 calc R . C11 C 0.08274(9) 0.3633(3) 0.38318(11) 0.0249(5) Uani 1 d . . C12 C 0.11555(10) 0.1473(3) 0.36878(13) 0.0316(5) Uani 1 d . . C13 C 0.09749(10) 0.1391(3) 0.42134(13) 0.0336(6) Uani 1 d . . C14 C 0.11667(11) 0.3352(3) 0.28777(12) 0.0354(6) Uani 1 d . . H14A H 0.0995(6) 0.2737(11) 0.2526(2) 0.043(8) Uiso 1 calc R . H14B H 0.15501(11) 0.3361(18) 0.2940(3) 0.038(8) Uiso 1 calc R . H14C H 0.1025(7) 0.4287(8) 0.2782(5) 0.063(11) Uiso 1 calc R . C15 C 0.14283(11) 0.0416(3) 0.3385(2) 0.0449(7) Uani 1 d . . H15A H 0.1792(3) 0.0718(11) 0.3427(9) 0.058(10) Uiso 1 calc R . H15B H 0.1233(5) 0.0323(16) 0.2937(3) 0.050(9) Uiso 1 calc R . H15C H 0.1437(7) -0.0475(6) 0.3596(6) 0.065(11) Uiso 1 calc R . C16 C 0.0975(2) 0.0200(3) 0.4654(2) 0.0560(9) Uani 1 d . . H16A H 0.0609(2) -0.0018(18) 0.4642(10) 0.093(15) Uiso 1 calc R . H16B H 0.1178(9) 0.0456(11) 0.5085(3) 0.085(13) Uiso 1 calc R . H16C H 0.1138(10) -0.0608(9) 0.4521(8) 0.098(16) Uiso 1 calc R . C17 C 0.05151(12) 0.3055(3) 0.47801(13) 0.0409(7) Uani 1 d . . H17A H 0.0742(4) 0.2756(20) 0.5194(2) 0.051(9) Uiso 1 calc R . H17B H 0.0173(4) 0.2580(18) 0.4684(6) 0.061(10) Uiso 1 calc R . H17C H 0.0459(8) 0.4053(4) 0.4786(7) 0.093(15) Uiso 1 calc R . C21 C -0.00410(11) 0.7351(3) 0.37539(14) 0.0407(6) Uani 1 d . . H21 H -0.00484(11) 0.7857(3) 0.41177(14) 0.062(11) Uiso 1 calc R . C22 C -0.02703(10) 0.6037(3) 0.35787(14) 0.0389(6) Uani 1 d . . H22 H -0.04565(10) 0.5509(3) 0.38055(14) 0.067(11) Uiso 1 calc R . C23 C -0.01728(10) 0.5641(3) 0.29992(14) 0.0429(7) Uani 1 d . . H23 H -0.02759(10) 0.4797(3) 0.27806(14) 0.053(10) Uiso 1 calc R . C24 C 0.01081(11) 0.6747(4) 0.28078(13) 0.0484(8) Uani 1 d . . H24 H 0.02121(11) 0.6786(4) 0.24329(13) 0.063(10) Uiso 1 calc R . C25 C 0.02020(11) 0.7783(3) 0.32935(15) 0.0436(7) Uani 1 d . . H25 H 0.03940(11) 0.8615(3) 0.33037(15) 0.070(12) Uiso 1 calc R . Cr2 Cr 0.392133(15) 0.51409(4) 0.72800(2) 0.02515(10) Uani 1 d . . N101 N 0.27338(8) 0.4113(2) 0.70167(9) 0.0247(4) Uani 1 d . . N102 N 0.29489(7) 0.4103(2) 0.61394(9) 0.0239(4) Uani 1 d . . N111 N 0.39211(8) 0.8003(2) 0.65658(10) 0.0348(5) Uani 1 d . . N112 N 0.34605(8) 0.8177(2) 0.72270(11) 0.0346(5) Uani 1 d . . C101 C 0.31516(9) 0.4392(2) 0.67783(11) 0.0233(4) Uani 1 d . . C102 C 0.22783(9) 0.3685(3) 0.65377(12) 0.0281(5) Uani 1 d . . C103 C 0.24112(9) 0.3678(3) 0.59818(12) 0.0276(5) Uani 1 d . . C104 C 0.27636(11) 0.4189(3) 0.76976(12) 0.0339(6) Uani 1 d . . H10A H 0.2668(7) 0.3292(6) 0.7837(3) 0.050(9) Uiso 1 calc R . H10B H 0.2517(6) 0.4893(14) 0.7758(2) 0.051(9) Uiso 1 calc R . H10C H 0.3125(2) 0.4430(19) 0.7946(2) 0.049(9) Uiso 1 calc R . C105 C 0.17586(11) 0.3329(4) 0.66717(15) 0.0438(7) Uani 1 d . . H10D H 0.1622(5) 0.4148(7) 0.6831(10) 0.076(13) Uiso 1 calc R . H10E H 0.1821(2) 0.2595(16) 0.6989(8) 0.052(9) Uiso 1 calc R . H10F H 0.1499(3) 0.3015(22) 0.6282(3) 0.068(11) Uiso 1 calc R . C106 C 0.20892(11) 0.3285(3) 0.53172(13) 0.0408(7) Uani 1 d . . H10G H 0.2263(5) 0.2517(17) 0.5169(4) 0.077(12) Uiso 1 calc R . H10H H 0.2065(8) 0.4079(8) 0.5036(3) 0.073(12) Uiso 1 calc R . H10I H 0.1732(3) 0.3006(24) 0.5317(2) 0.076(12) Uiso 1 calc R . C107 C 0.32512(10) 0.4291(3) 0.56706(12) 0.0342(6) Uani 1 d . . H10J H 0.3147(6) 0.5164(10) 0.5445(7) 0.068(11) Uiso 1 calc R . H10K H 0.3172(6) 0.3527(11) 0.5368(6) 0.049(9) Uiso 1 calc R . H10L H 0.36321(11) 0.4306(21) 0.5891(2) 0.039(8) Uiso 1 calc R . C111 C 0.37650(9) 0.7250(3) 0.70060(12) 0.0289(5) Uani 1 d . . C112 C 0.37149(11) 0.9375(3) 0.65130(15) 0.0432(7) Uani 1 d . . C113 C 0.34261(11) 0.9480(3) 0.6930(2) 0.0423(7) Uani 1 d . . C114 C 0.42686(11) 0.7443(4) 0.62019(14) 0.0452(7) Uani 1 d . . H11A H 0.4603(4) 0.7959(16) 0.6310(8) 0.058(10) Uiso 1 calc R . H11B H 0.4089(4) 0.7534(22) 0.57491(14) 0.088(13) Uiso 1 calc R . H11C H 0.4342(7) 0.6468(7) 0.6307(8) 0.061(11) Uiso 1 calc R . C115 C 0.3816(2) 1.0416(4) 0.6046(2) 0.0682(12) Uani 1 d . . H11D H 0.3580(8) 1.0220(18) 0.5623(3) 0.074(12) Uiso 1 calc R . H11E H 0.4186(3) 1.0348(21) 0.6042(10) 0.092(15) Uiso 1 calc R . H11F H 0.3747(11) 1.1349(5) 0.6172(8) 0.151(24) Uiso 1 calc R . C116 C 0.30978(15) 1.0665(3) 0.7065(2) 0.0646(11) Uani 1 d . . H11G H 0.3218(7) 1.0886(17) 0.7516(3) 0.082(14) Uiso 1 calc R . H11H H 0.2723(2) 1.0397(9) 0.6946(11) 0.078(13) Uiso 1 calc R . H11I H 0.3140(7) 1.1476(8) 0.6821(9) 0.069(12) Uiso 1 calc R . C117 C 0.31895(13) 0.7839(4) 0.7705(2) 0.0509(8) Uani 1 d . . H11J H 0.2808(2) 0.7735(26) 0.7499(2) 0.074(12) Uiso 1 calc R . H11K H 0.3248(8) 0.8583(13) 0.8017(7) 0.092(14) Uiso 1 calc R . H11L H 0.3332(7) 0.6975(14) 0.7916(8) 0.068(11) Uiso 1 calc R . C121 C 0.47090(11) 0.5279(3) 0.81096(15) 0.0444(7) Uani 1 d . . H121 H 0.48202(11) 0.6138(3) 0.83107(15) 0.074(12) Uiso 1 calc R . C122 C 0.48415(11) 0.4771(3) 0.7576(2) 0.0457(7) Uani 1 d . . H122 H 0.50605(11) 0.5218(3) 0.7364(2) 0.045(9) Uiso 1 calc R . C123 C 0.45883(12) 0.3471(4) 0.7414(2) 0.0517(8) Uani 1 d . . H123 H 0.46086(12) 0.2893(4) 0.7076(2) 0.066(11) Uiso 1 calc R . C124 C 0.42944(11) 0.3192(3) 0.7857(2) 0.0528(9) Uani 1 d . . H124 H 0.40795(11) 0.2406(3) 0.7856(2) 0.091(14) Uiso 1 calc R . C125 C 0.43841(11) 0.4303(4) 0.82954(14) 0.0467(7) Uani 1 d . . H125 H 0.42505(11) 0.4377(4) 0.86478(14) 0.077(13) Uiso 1 calc R . C201 C 0.26544(12) 0.2018(3) 0.90079(13) 0.0422(7) Uani 1 d . . H201 H 0.22988(12) 0.1716(3) 0.89308(13) 0.062(11) Uiso 1 calc R . C202 C 0.28615(13) 0.3304(3) 0.92723(13) 0.0432(7) Uani 1 d . . H202 H 0.26689(13) 0.4007(3) 0.94067(13) 0.066(11) Uiso 1 calc R . C203 C 0.34027(13) 0.3360(4) 0.93017(14) 0.0515(8) Uani 1 d . . H203 H 0.36367(13) 0.4109(4) 0.94552(14) 0.085(14) Uiso 1 calc R . C204 C 0.35350(14) 0.2101(4) 0.9062(2) 0.0555(9) Uani 1 d . . H204 H 0.38740(14) 0.1855(4) 0.9028(2) 0.080(13) Uiso 1 calc R . C205 C 0.3069(2) 0.1266(4) 0.88792(14) 0.0522(8) Uani 1 d . . H205 H 0.3043(2) 0.0367(4) 0.87031(14) 0.070(12) Uiso 1 calc R . C401 C 0.1040(6) 0.9588(10) 0.6459(6) 0.070(5) Uani 0.61(3) d PG 1 H401 H 0.0910(6) 1.0464(10) 0.6293(6) 0.131(48) Uiso 0.69(14) calc PR 1 C402 C 0.1577(5) 0.9214(12) 0.6702(6) 0.088(6) Uani 0.68(3) d PG 1 H402 H 0.1873(8) 0.9794(18) 0.6729(9) 0.089(43) Uiso 0.55(13) calc PR 1 C403 C 0.1599(4) 0.7830(15) 0.6899(3) 0.061(4) Uani 0.56(3) d PG 1 H403 H 0.1911(6) 0.7312(24) 0.7081(5) 0.139(42) Uiso 0.82(13) calc PR 1 C404 C 0.1075(5) 0.7348(10) 0.6777(4) 0.058(5) Uani 0.54(3) d PG 1 H404 H 0.0972(9) 0.6448(13) 0.6863(8) 0.080(36) Uiso 0.57(11) calc PR 1 C405 C 0.0729(3) 0.8435(14) 0.6505(4) 0.065(8) Uani 0.57(4) d PG 1 H405 H 0.0353(4) 0.8396(22) 0.6376(6) 0.159(61) Uiso 0.67(15) calc PR 1 C411 C 0.0696(6) 0.7739(11) 0.6516(7) 0.050(4) Uani 0.44(3) d PG 2 H411 H 0.0409(6) 0.7116(11) 0.6470(7) 0.027(32) Uiso 0.34(9) calc PR 2 C412 C 0.0666(4) 0.9064(10) 0.6232(9) 0.066(5) Uani 0.44(3) d PG 2 H412 H 0.0356(7) 0.9480(18) 0.5963(13) 0.026(40) Uiso 0.27(9) calc PR 2 C413 C 0.1183(6) 0.9655(12) 0.6422(6) 0.051(7) Uani 0.35(3) d PG 2 H413 H 0.1278(10) 1.0534(18) 0.6301(8) 0.021(76) Uiso 0.13(9) calc PR 2 C414 C 0.1532(4) 0.8695(17) 0.6824(5) 0.056(6) Uani 0.44(3) d PG 2 H414 H 0.1900(6) 0.8823(26) 0.7019(8) 2.000(1354) Uiso 1.00(52) calc R 2 C415 C 0.1231(7) 0.7511(10) 0.6882(5) 0.054(6) Uani 0.45(3) d PG 2 H415 H 0.1363(10) 0.6710(15) 0.7123(7) 0.048(39) Uiso 0.38(10) calc PR 2 O501 O 0.4910(2) 0.3768(6) 0.6029(2) 0.159(2) Uani 1 d . . C502 C 0.4680(2) 0.1700(7) 1.0458(2) 0.092(2) Uani 1 d . . H50A H 0.4400(2) 0.2370(7) 1.0470(2) 0.258(43) Uiso 1 calc R . H50B H 0.4513(2) 0.0929(7) 1.0177(2) 0.284(52) Uiso 1 calc R . C503 C 0.4914(2) 0.7614(8) 0.9792(3) 0.114(2) Uani 1 d . . H50C H 0.4950(2) 0.7918(8) 1.0229(3) 0.138(22) Uiso 1 calc R . H50D H 0.4951(2) 0.6598(8) 0.9789(3) 0.109(21) Uiso 1 calc R . C504 C 0.4369(2) 0.8078(7) 0.9335(3) 0.099(2) Uani 1 d . . H50E H 0.4153(2) 0.7274(7) 0.9136(3) 0.125(21) Uiso 1 calc R . H50F H 0.4166(2) 0.8636(7) 0.9558(3) 0.151(24) Uiso 1 calc R . C505 C 0.4535(2) 0.8943(7) 0.8847(2) 0.094(2) Uani 1 d . . H50G H 0.4347(2) 0.8626(7) 0.8415(2) 0.088(14) Uiso 1 calc R . H50H H 0.4449(2) 0.9927(7) 0.8885(2) 0.199(35) Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0217(2) 0.0252(2) 0.0216(2) -0.0013(2) 0.00337(13) 0.00169(15) N1 0.0253(9) 0.0265(10) 0.0244(9) -0.0030(8) 0.0033(8) 0.0006(8) N2 0.0277(10) 0.0253(10) 0.0266(10) -0.0010(8) 0.0059(8) 0.0003(8) N11 0.0253(9) 0.0267(10) 0.0272(10) -0.0041(8) 0.0072(8) -0.0014(8) N12 0.0305(10) 0.0279(11) 0.0233(9) -0.0010(8) 0.0049(8) -0.0026(8) C1 0.0268(11) 0.0227(11) 0.0224(11) 0.0000(9) 0.0053(9) 0.0031(9) C2 0.0268(11) 0.0300(13) 0.0304(12) -0.0063(10) 0.0015(10) -0.0004(10) C3 0.0245(11) 0.0265(12) 0.0356(13) -0.0027(10) 0.0037(10) 0.0003(9) C4 0.0373(13) 0.0406(15) 0.0241(11) -0.0045(11) 0.0089(10) -0.0023(12) C5 0.0346(14) 0.055(2) 0.0371(15) -0.0183(15) -0.0032(12) -0.0001(13) C6 0.0306(14) 0.047(2) 0.059(2) -0.008(2) 0.0141(13) -0.0067(13) C7 0.0381(13) 0.0382(15) 0.0307(13) -0.0008(11) 0.0130(11) 0.0001(12) C11 0.0219(10) 0.0265(12) 0.0237(11) -0.0030(9) 0.0024(8) -0.0031(9) C12 0.0266(11) 0.0255(12) 0.0378(13) -0.0050(11) 0.0017(10) 0.0002(10) C13 0.0364(13) 0.0243(12) 0.0341(13) -0.0007(11) 0.0012(11) -0.0016(10) C14 0.0378(14) 0.040(2) 0.0327(13) -0.0073(12) 0.0173(11) -0.0058(12) C15 0.0360(15) 0.033(2) 0.063(2) -0.0141(14) 0.0103(14) 0.0043(12) C16 0.083(3) 0.032(2) 0.047(2) 0.0081(14) 0.009(2) -0.004(2) C17 0.051(2) 0.045(2) 0.0311(13) -0.0030(12) 0.0187(12) -0.0078(14) C21 0.0360(14) 0.040(2) 0.044(2) -0.0030(13) 0.0101(12) 0.0135(12) C22 0.0240(12) 0.046(2) 0.047(2) 0.0048(13) 0.0100(11) 0.0051(11) C23 0.0286(13) 0.047(2) 0.0411(15) -0.0101(14) -0.0080(11) 0.0038(12) C24 0.0383(14) 0.078(2) 0.0265(13) 0.0153(15) 0.0066(11) 0.019(2) C25 0.0331(13) 0.037(2) 0.053(2) 0.0153(14) 0.0008(12) 0.0040(12) Cr2 0.0215(2) 0.0218(2) 0.0299(2) 0.0011(2) 0.00392(14) 0.00132(15) N101 0.0261(9) 0.0240(10) 0.0246(9) 0.0019(8) 0.0084(8) -0.0002(8) N102 0.0236(9) 0.0229(10) 0.0246(9) 0.0009(8) 0.0061(7) 0.0001(8) N111 0.0296(10) 0.0317(12) 0.0355(11) 0.0041(10) -0.0019(9) -0.0071(9) N112 0.0320(11) 0.0226(10) 0.0439(12) -0.0003(9) 0.0031(9) 0.0027(9) C101 0.0250(10) 0.0192(11) 0.0251(11) 0.0027(9) 0.0065(9) 0.0016(9) C102 0.0232(11) 0.0264(12) 0.0347(12) 0.0019(10) 0.0087(9) -0.0017(9) C103 0.0238(11) 0.0268(12) 0.0302(12) -0.0019(10) 0.0050(9) -0.0018(9) C104 0.0388(13) 0.0383(14) 0.0275(12) 0.0018(11) 0.0141(10) 0.0013(12) C105 0.0308(13) 0.052(2) 0.052(2) -0.003(2) 0.0172(13) -0.0104(13) C106 0.0306(13) 0.051(2) 0.0368(14) -0.0107(14) 0.0041(11) -0.0029(13) C107 0.0348(13) 0.0404(15) 0.0312(12) 0.0009(12) 0.0154(11) -0.0018(12) C111 0.0248(11) 0.0251(12) 0.0313(12) -0.0001(10) -0.0003(9) -0.0031(9) C112 0.0354(14) 0.0287(14) 0.050(2) 0.0106(13) -0.0122(12) -0.0084(11) C113 0.0355(14) 0.0233(13) 0.055(2) 0.0001(12) -0.0071(13) -0.0007(11) C114 0.040(2) 0.054(2) 0.040(2) 0.0022(14) 0.0089(13) -0.0157(14) C115 0.061(2) 0.056(2) 0.069(2) 0.032(2) -0.011(2) -0.017(2) C116 0.059(2) 0.028(2) 0.092(3) -0.003(2) 0.000(2) 0.0078(15) C117 0.051(2) 0.042(2) 0.064(2) -0.007(2) 0.024(2) 0.0064(15) C121 0.0297(13) 0.042(2) 0.050(2) -0.0042(14) -0.0058(12) 0.0006(12) C122 0.0234(12) 0.053(2) 0.058(2) 0.014(2) 0.0087(12) 0.0052(13) C123 0.044(2) 0.049(2) 0.053(2) -0.008(2) 0.0003(14) 0.0248(15) C124 0.0310(14) 0.037(2) 0.078(2) 0.024(2) -0.0041(15) -0.0004(12) C125 0.0335(14) 0.065(2) 0.0373(15) 0.015(2) 0.0043(12) 0.0116(14) C201 0.046(2) 0.050(2) 0.0291(13) 0.0056(13) 0.0097(12) -0.0074(14) C202 0.054(2) 0.043(2) 0.0316(13) 0.0027(13) 0.0124(13) 0.0030(14) C203 0.055(2) 0.062(2) 0.0337(15) -0.0024(15) 0.0060(13) -0.018(2) C204 0.049(2) 0.072(2) 0.048(2) 0.015(2) 0.0174(15) 0.012(2) C205 0.084(2) 0.040(2) 0.038(2) 0.0032(14) 0.026(2) 0.005(2) C401 0.086(10) 0.066(7) 0.077(8) -0.008(5) 0.054(7) 0.007(6) C402 0.088(8) 0.097(10) 0.103(10) -0.070(8) 0.066(8) -0.053(7) C403 0.060(7) 0.095(9) 0.027(3) -0.018(5) 0.012(3) -0.021(6) C404 0.055(8) 0.094(8) 0.027(5) -0.013(4) 0.015(5) -0.044(6) C405 0.041(5) 0.121(20) 0.040(5) -0.020(9) 0.022(4) -0.020(7) C411 0.062(8) 0.059(7) 0.041(6) -0.019(5) 0.034(6) -0.027(6) C412 0.065(8) 0.055(8) 0.069(10) -0.024(6) 0.009(6) 0.017(6) C413 0.077(17) 0.041(8) 0.031(6) -0.010(5) 0.007(7) -0.035(7) C414 0.048(6) 0.077(15) 0.035(5) -0.015(7) -0.002(4) -0.026(7) C415 0.068(14) 0.061(7) 0.020(4) 0.003(4) -0.007(5) -0.014(6) O501 0.085(3) 0.289(7) 0.087(3) -0.048(4) 0.001(2) 0.046(3) C502 0.076(3) 0.135(5) 0.067(3) -0.006(3) 0.023(2) 0.017(3) C503 0.103(4) 0.155(7) 0.075(4) 0.022(4) 0.013(3) -0.011(4) C504 0.066(3) 0.134(5) 0.101(4) -0.017(4) 0.029(3) -0.006(3) C505 0.077(3) 0.119(5) 0.075(3) -0.008(3) 0.007(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C11 2.091(2) . ? Cr1 C1 2.103(2) . ? Cr1 C23 2.265(3) . ? Cr1 C25 2.290(3) . ? Cr1 C24 2.296(3) . ? Cr1 C22 2.306(2) . ? Cr1 C21 2.326(3) . ? N1 C1 1.354(3) . ? N1 C2 1.385(3) . ? N1 C4 1.459(3) . ? N2 C1 1.356(3) . ? N2 C3 1.388(3) . ? N2 C7 1.459(3) . ? N11 C11 1.351(3) . ? N11 C12 1.390(3) . ? N11 C14 1.464(3) . ? N12 C11 1.357(3) . ? N12 C13 1.386(3) . ? N12 C17 1.456(3) . ? C2 C3 1.346(3) . ? C2 C5 1.495(3) . ? C3 C6 1.491(3) . ? C12 C13 1.356(4) . ? C12 C15 1.486(4) . ? C13 C16 1.482(4) . ? C21 C22 1.386(4) . ? C21 C25 1.389(4) . ? C22 C23 1.405(4) . ? C23 C24 1.407(5) . ? C24 C25 1.411(4) . ? Cr2 C101 2.092(2) . ? Cr2 C111 2.096(3) . ? Cr2 C124 2.285(3) . ? Cr2 C121 2.292(3) . ? Cr2 C123 2.297(3) . ? Cr2 C122 2.301(3) . ? Cr2 C125 2.319(3) . ? N101 C101 1.353(3) . ? N101 C102 1.384(3) . ? N101 C104 1.460(3) . ? N102 C101 1.359(3) . ? N102 C103 1.390(3) . ? N102 C107 1.465(3) . ? N111 C111 1.347(3) . ? N111 C112 1.400(4) . ? N111 C114 1.460(4) . ? N112 C111 1.359(3) . ? N112 C113 1.386(3) . ? N112 C117 1.449(4) . ? C102 C103 1.349(3) . ? C102 C105 1.494(3) . ? C103 C106 1.486(3) . ? C112 C113 1.336(5) . ? C112 C115 1.494(4) . ? C113 C116 1.490(4) . ? C121 C125 1.388(4) . ? C121 C122 1.388(4) . ? C122 C123 1.393(5) . ? C123 C124 1.415(5) . ? C124 C125 1.395(5) . ? C201 C205 1.383(4) . ? C201 C202 1.388(4) . ? C202 C203 1.382(4) . ? C203 C204 1.388(5) . ? C204 C205 1.398(5) . ? C401 C402 1.379(6) . ? C401 C405 1.379(6) . ? C402 C403 1.379(6) . ? C403 C404 1.379(6) . ? C404 C405 1.379(6) . ? C411 C415 1.394(8) . ? C411 C412 1.394(8) . ? C412 C413 1.395(8) . ? C413 C414 1.394(8) . ? C414 C415 1.394(8) . ? O501 C502 1.287(6) 4_565 ? O501 C505 1.388(6) 2_646 ? C502 O501 1.287(5) 4_566 ? C502 C503 1.467(7) 3_667 ? C503 C502 1.467(7) 3_667 ? C503 C504 1.530(7) . ? C504 C505 1.500(7) . ? C505 O501 1.388(6) 2_656 ? 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 C11 Cr1 C1 97.42(9) . . ? C11 Cr1 C23 98.18(10) . . ? C1 Cr1 C23 161.86(11) . . ? C11 Cr1 C25 156.88(10) . . ? C1 Cr1 C25 103.64(10) . . ? C23 Cr1 C25 59.60(11) . . ? C11 Cr1 C24 122.00(11) . . ? C1 Cr1 C24 126.29(11) . . ? C23 Cr1 C24 35.93(11) . . ? C25 Cr1 C24 35.84(11) . . ? C11 Cr1 C22 107.90(10) . . ? C1 Cr1 C22 143.83(10) . . ? C23 Cr1 C22 35.79(10) . . ? C25 Cr1 C22 58.66(11) . . ? C24 Cr1 C22 59.24(10) . . ? C11 Cr1 C21 140.85(10) . . ? C1 Cr1 C21 112.14(10) . . ? C23 Cr1 C21 59.00(11) . . ? C25 Cr1 C21 35.03(10) . . ? C24 Cr1 C21 58.90(11) . . ? C22 Cr1 C21 34.83(10) . . ? C1 N1 C2 112.0(2) . . ? C1 N1 C4 124.2(2) . . ? C2 N1 C4 123.8(2) . . ? C1 N2 C3 111.9(2) . . ? C1 N2 C7 124.3(2) . . ? C3 N2 C7 123.7(2) . . ? C11 N11 C12 112.3(2) . . ? C11 N11 C14 124.3(2) . . ? C12 N11 C14 123.3(2) . . ? C11 N12 C13 112.2(2) . . ? C11 N12 C17 124.0(2) . . ? C13 N12 C17 123.7(2) . . ? N1 C1 N2 103.4(2) . . ? N1 C1 Cr1 127.8(2) . . ? N2 C1 Cr1 128.8(2) . . ? C3 C2 N1 106.5(2) . . ? C3 C2 C5 131.0(2) . . ? N1 C2 C5 122.5(2) . . ? C2 C3 N2 106.2(2) . . ? C2 C3 C6 131.0(2) . . ? N2 C3 C6 122.7(2) . . ? N11 C11 N12 103.4(2) . . ? N11 C11 Cr1 127.7(2) . . ? N12 C11 Cr1 128.8(2) . . ? C13 C12 N11 106.0(2) . . ? C13 C12 C15 131.2(3) . . ? N11 C12 C15 122.8(3) . . ? C12 C13 N12 106.2(2) . . ? C12 C13 C16 130.7(3) . . ? N12 C13 C16 123.1(3) . . ? C22 C21 C25 108.4(3) . . ? C22 C21 Cr1 71.8(2) . . ? C25 C21 Cr1 71.1(2) . . ? C21 C22 C23 108.2(3) . . ? C21 C22 Cr1 73.37(15) . . ? C23 C22 Cr1 70.52(14) . . ? C22 C23 C24 108.0(3) . . ? C22 C23 Cr1 73.69(15) . . ? C24 C23 Cr1 73.2(2) . . ? C23 C24 C25 106.9(3) . . ? C23 C24 Cr1 70.9(2) . . ? C25 C24 Cr1 71.9(2) . . ? C21 C25 C24 108.5(3) . . ? C21 C25 Cr1 73.9(2) . . ? C24 C25 Cr1 72.3(2) . . ? C101 Cr2 C111 95.91(9) . . ? C101 Cr2 C124 101.15(10) . . ? C111 Cr2 C124 161.07(11) . . ? C101 Cr2 C121 156.63(10) . . ? C111 Cr2 C121 102.76(10) . . ? C124 Cr2 C121 58.74(11) . . ? C101 Cr2 C123 113.20(11) . . ? C111 Cr2 C123 140.46(12) . . ? C124 Cr2 C123 35.99(12) . . ? C121 Cr2 C123 58.68(11) . . ? C101 Cr2 C122 147.13(11) . . ? C111 Cr2 C122 108.83(11) . . ? C124 Cr2 C122 59.19(11) . . ? C121 Cr2 C122 35.19(11) . . ? C123 Cr2 C122 35.28(12) . . ? C101 Cr2 C125 121.63(10) . . ? C111 Cr2 C125 126.92(11) . . ? C124 Cr2 C125 35.26(12) . . ? C121 Cr2 C125 35.03(11) . . ? C123 Cr2 C125 58.97(12) . . ? C122 Cr2 C125 58.65(11) . . ? C101 N101 C102 111.6(2) . . ? C101 N101 C104 124.5(2) . . ? C102 N101 C104 123.8(2) . . ? C101 N102 C103 111.6(2) . . ? C101 N102 C107 124.1(2) . . ? C103 N102 C107 124.2(2) . . ? C111 N111 C112 111.5(2) . . ? C111 N111 C114 123.4(2) . . ? C112 N111 C114 125.1(3) . . ? C111 N112 C113 112.3(2) . . ? C111 N112 C117 124.1(2) . . ? C113 N112 C117 123.6(2) . . ? N101 C101 N102 103.9(2) . . ? N101 C101 Cr2 127.6(2) . . ? N102 C101 Cr2 128.5(2) . . ? C103 C102 N101 106.9(2) . . ? C103 C102 C105 130.8(2) . . ? N101 C102 C105 122.3(2) . . ? C102 C103 N102 106.1(2) . . ? C102 C103 C106 130.8(2) . . ? N102 C103 C106 123.1(2) . . ? N111 C111 N112 103.4(2) . . ? N111 C111 Cr2 129.5(2) . . ? N112 C111 Cr2 127.1(2) . . ? C113 C112 N111 106.8(2) . . ? C113 C112 C115 130.9(3) . . ? N111 C112 C115 122.3(3) . . ? C112 C113 N112 106.0(2) . . ? C112 C113 C116 130.8(3) . . ? N112 C113 C116 123.1(3) . . ? C125 C121 C122 109.2(3) . . ? C125 C121 Cr2 73.5(2) . . ? C122 C121 Cr2 72.7(2) . . ? C121 C122 C123 107.9(3) . . ? C121 C122 Cr2 72.1(2) . . ? C123 C122 Cr2 72.2(2) . . ? C122 C123 C124 107.5(3) . . ? C122 C123 Cr2 72.5(2) . . ? C124 C123 Cr2 71.5(2) . . ? C125 C124 C123 107.9(3) . . ? C125 C124 Cr2 73.7(2) . . ? C123 C124 Cr2 72.5(2) . . ? C121 C125 C124 107.5(3) . . ? C121 C125 Cr2 71.4(2) . . ? C124 C125 Cr2 71.0(2) . . ? C205 C201 C202 108.1(3) . . ? C203 C202 C201 108.4(3) . . ? C202 C203 C204 107.9(3) . . ? C203 C204 C205 108.0(3) . . ? C201 C205 C204 107.7(3) . . ? C402 C401 C405 108.0 . . ? C401 C402 C403 108.0 . . ? C402 C403 C404 108.0 . . ? C403 C404 C405 108.0 . . ? C401 C405 C404 108.0 . . ? C415 C411 C412 108.0 . . ? C411 C412 C413 108.0 . . ? C414 C413 C412 108.0 . . ? C413 C414 C415 108.0 . . ? C411 C415 C414 108.0 . . ? C502 O501 C505 112.8(4) 4_565 2_646 ? O501 C502 C503 109.4(5) 4_566 3_667 ? C502 C503 C504 104.7(5) 3_667 . ? C505 C504 C503 102.5(4) . . ? O501 C505 C504 106.8(4) 2_656 . ? _refine_diff_density_max 0.627 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.063