# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1153 data_shelxl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'compound 2a' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H51 B Co N6' _chemical_formula_weight 553.50 _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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.309(3) _cell_length_b 16.206(17) _cell_length_c 19.207(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.02(2) _cell_angle_gamma 90.00 _cell_volume 3159.7(36) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method ? _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK?Ga _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4201 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.62 _reflns_number_total 4201 _reflns_number_observed 3267 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[?Gs^2^(Fo^2^)+(0.1000P)^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 4201 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_obs 0.0825 _refine_ls_wR_factor_all 0.2235 _refine_ls_wR_factor_obs 0.2003 _refine_ls_goodness_of_fit_all 1.662 _refine_ls_goodness_of_fit_obs 1.793 _refine_ls_restrained_S_all 1.662 _refine_ls_restrained_S_obs 1.793 _refine_ls_shift/esd_max 0.074 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 1.07466(10) 0.73508(7) 0.76507(6) 0.0612(4) Uani 1 d . . N11 N 0.9200(7) 0.7365(4) 0.6821(4) 0.062(2) Uani 1 d . . N12 N 0.7985(6) 0.7337(4) 0.7024(3) 0.062(2) Uani 1 d . . N21 N 0.9880(7) 0.8231(4) 0.8154(3) 0.060(2) Uani 1 d . . N22 N 0.8599(7) 0.8107(4) 0.8166(3) 0.059(2) Uani 1 d . . N31 N 0.9900(6) 0.6442(4) 0.8140(3) 0.058(2) Uani 1 d . . N32 N 0.8606(6) 0.6540(4) 0.8137(3) 0.061(2) Uani 1 d . . C1 C 1.2644(10) 0.7356(6) 0.7522(5) 0.071(2) Uani 1 d . . C2 C 1.3618(19) 0.7337(10) 0.8100(14) 0.189(10) Uani 1 d . . H2A H 1.3544(60) 0.6841(29) 0.8364(31) 0.189 Uiso 1 calc R . H2B H 1.3539(60) 0.7808(32) 0.8393(29) 0.189 Uiso 1 calc R . H2C H 1.4460(19) 0.7349(62) 0.7951(14) 0.189 Uiso 1 calc R . C11 C 0.9034(9) 0.7414(5) 0.6125(4) 0.066(2) Uani 1 d . . C12 C 0.7719(9) 0.7415(5) 0.5844(5) 0.071(2) Uani 1 d . . C13 C 0.7051(9) 0.7374(5) 0.6419(5) 0.068(2) Uani 1 d . . C14 C 1.0230(9) 0.7452(5) 0.5770(5) 0.071(2) Uani 1 d . . C15 C 1.0842(11) 0.6596(6) 0.5742(6) 0.100(3) Uani 1 d . . H15A H 1.0971(48) 0.6352(14) 0.6205(8) 0.100 Uiso 1 calc R . H15B H 1.1675(25) 0.6644(7) 0.5587(27) 0.100 Uiso 1 calc R . H15C H 1.0264(25) 0.6254(11) 0.5418(21) 0.100 Uiso 1 calc R . C16 C 0.9943(13) 0.7772(7) 0.5024(6) 0.108(4) Uani 1 d . . H16A H 1.0740(17) 0.7777(38) 0.4830(13) 0.108 Uiso 1 calc R . H16B H 0.9597(59) 0.8322(15) 0.5023(7) 0.108 Uiso 1 calc R . H16C H 0.9308(47) 0.7420(22) 0.4743(10) 0.108 Uiso 1 calc R . C17 C 0.5596(9) 0.7337(6) 0.6417(5) 0.072(2) Uani 1 d . . C18 C 0.5160(10) 0.6442(6) 0.6426(7) 0.101(3) Uani 1 d . . H18A H 0.4251(18) 0.6419(6) 0.6476(30) 0.101 Uiso 1 calc R . H18B H 0.5687(37) 0.6160(10) 0.6815(18) 0.101 Uiso 1 calc R . H18C H 0.5266(51) 0.6180(11) 0.5991(13) 0.101 Uiso 1 calc R . C19 C 0.4837(11) 0.7816(7) 0.5799(6) 0.102(3) Uani 1 d . . H19A H 0.5182(39) 0.8366(13) 0.5801(19) 0.102 Uiso 1 calc R . H19B H 0.3924(14) 0.7838(32) 0.5842(18) 0.102 Uiso 1 calc R . H19C H 0.4926(50) 0.7547(21) 0.5365(7) 0.102 Uiso 1 calc R . C21 C 1.0237(9) 0.8943(5) 0.8485(4) 0.066(2) Uani 1 d . . C22 C 0.9136(9) 0.9256(5) 0.8727(5) 0.075(2) Uani 1 d . . C23 C 0.8101(8) 0.8715(4) 0.8531(4) 0.060(2) Uani 1 d . . C24 C 1.1606(9) 0.9261(6) 0.8546(5) 0.075(2) Uani 1 d . . C25 C 1.2385(12) 0.9135(12) 0.9239(7) 0.167(7) Uani 1 d . . H25A H 1.2298(73) 0.8573(17) 0.9381(21) 0.167 Uiso 1 calc R . H25B H 1.2082(62) 0.9497(39) 0.9572(12) 0.167 Uiso 1 calc R . H25C H 1.3293(18) 0.9250(60) 0.9224(14) 0.167 Uiso 1 calc R . C26 C 1.1638(13) 1.0128(7) 0.8354(8) 0.133(5) Uani 1 d . . H26A H 1.2534(14) 1.0297(13) 0.8365(37) 0.133 Uiso 1 calc R . H26B H 1.1256(63) 1.0453(8) 0.8684(22) 0.133 Uiso 1 calc R . H26C H 1.1145(58) 1.0207(10) 0.7886(16) 0.133 Uiso 1 calc R . C27 C 0.6721(9) 0.8787(5) 0.8646(5) 0.077(2) Uani 1 d . . C28 C 0.6587(10) 0.9274(7) 0.9296(5) 0.091(3) Uani 1 d . . H28A H 0.7118(42) 0.9027(19) 0.9702(6) 0.091 Uiso 1 calc R . H28B H 0.5682(13) 0.9277(29) 0.9355(17) 0.091 Uiso 1 calc R . H28C H 0.6876(50) 0.9831(10) 0.9244(13) 0.091 Uiso 1 calc R . C29 C 0.5850(10) 0.9185(7) 0.7992(5) 0.094(3) Uani 1 d . . H29A H 0.6281(26) 0.9667(20) 0.7853(18) 0.094 Uiso 1 calc R . H29B H 0.5015(22) 0.9338(31) 0.8110(10) 0.094 Uiso 1 calc R . H29C H 0.5715(46) 0.8796(13) 0.7609(11) 0.094 Uiso 1 calc R . C31 C 1.0275(8) 0.5729(5) 0.8468(4) 0.066(2) Uani 1 d . . C32 C 0.9169(9) 0.5358(5) 0.8687(4) 0.071(2) Uani 1 d . . C33 C 0.8135(9) 0.5884(5) 0.8477(4) 0.066(2) Uani 1 d . . C34 C 1.1691(9) 0.5438(5) 0.8571(5) 0.077(2) Uani 1 d . . C35 C 1.2350(11) 0.5585(8) 0.9321(6) 0.114(4) Uani 1 d . . H35A H 1.1842(36) 0.5332(34) 0.9637(6) 0.114 Uiso 1 calc R . H35B H 1.2413(57) 0.6167(8) 0.9411(11) 0.114 Uiso 1 calc R . H35C H 1.3218(27) 0.5349(36) 0.9395(11) 0.114 Uiso 1 calc R . C36 C 1.1743(11) 0.4538(7) 0.8384(7) 0.117(4) Uani 1 d . . H36A H 1.1397(56) 0.4214(8) 0.8728(19) 0.117 Uiso 1 calc R . H36B H 1.2639(13) 0.4381(12) 0.8380(32) 0.117 Uiso 1 calc R . H36C H 1.1225(49) 0.4446(10) 0.7925(15) 0.117 Uiso 1 calc R . C37 C 0.6727(9) 0.5812(6) 0.8557(5) 0.075(2) Uani 1 d . . C38 C 0.6460(10) 0.6278(6) 0.9220(6) 0.094(3) Uani 1 d . . H38A H 0.6899(47) 0.6001(20) 0.9637(6) 0.094 Uiso 1 calc R . H38B H 0.5530(11) 0.6290(32) 0.9221(17) 0.094 Uiso 1 calc R . H38C H 0.6787(52) 0.6832(12) 0.9214(16) 0.094 Uiso 1 calc R . C39 C 0.6321(10) 0.4916(6) 0.8611(6) 0.095(3) Uani 1 d . . H39A H 0.5378(10) 0.4881(7) 0.8545(29) 0.095 Uiso 1 calc R . H39B H 0.6693(44) 0.4705(11) 0.9069(11) 0.095 Uiso 1 calc R . H39C H 0.6636(46) 0.4598(9) 0.8253(18) 0.095 Uiso 1 calc R . B1 B 0.7880(8) 0.7327(5) 0.7788(4) 0.054(2) Uani 1 d . . H0 H 0.6984 0.7328 0.7838 0.065 Uiso 1 d . . H1A H 1.2793 0.6897 0.7238 0.088 Uiso 1 d . . H1B H 1.2795 0.7854 0.7272 0.088 Uiso 1 d . . H12 H 0.7344 0.7448 0.5347 0.082 Uiso 1 d . . H14 H 1.0823 0.7801 0.6057 0.090 Uiso 1 d . . H17 H 0.5444 0.7579 0.6847 0.086 Uiso 1 d . . H22 H 0.9130 0.9726 0.9028 0.091 Uiso 1 d . . H24 H 1.2012 0.8960 0.8186 0.100 Uiso 1 d . . H27 H 0.6392 0.8224 0.8699 0.089 Uiso 1 d . . H32 H 0.9160 0.4864 0.8949 0.088 Uiso 1 d . . H34 H 1.2164 0.5751 0.8282 0.109 Uiso 1 d . . H37 H 0.6231 0.6038 0.8158 0.097 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 Co1 0.0651(7) 0.0408(6) 0.0775(7) 0.0017(5) 0.0116(5) 0.0001(5) N11 0.073(4) 0.044(3) 0.072(4) -0.002(3) 0.017(3) 0.003(3) N12 0.059(4) 0.054(4) 0.071(4) 0.001(3) 0.005(3) 0.001(3) N21 0.064(5) 0.038(4) 0.077(4) 0.005(3) 0.008(3) -0.008(3) N22 0.071(5) 0.032(4) 0.070(4) -0.007(3) 0.005(3) -0.001(3) N31 0.063(5) 0.042(4) 0.070(4) -0.002(3) 0.012(3) 0.000(3) N32 0.063(4) 0.040(4) 0.075(4) -0.005(3) 0.000(3) -0.002(3) C1 0.080(6) 0.056(5) 0.084(5) 0.007(4) 0.032(4) 0.005(5) C2 0.149(16) 0.082(10) 0.364(34) 0.016(14) 0.121(19) -0.005(10) C11 0.086(6) 0.044(5) 0.068(5) -0.002(3) 0.012(4) 0.002(4) C12 0.080(6) 0.054(5) 0.076(5) 0.003(4) 0.004(4) -0.001(4) C13 0.083(6) 0.040(4) 0.078(5) 0.002(4) 0.001(4) 0.000(4) C14 0.083(6) 0.055(6) 0.073(5) 0.001(4) 0.007(4) 0.005(4) C15 0.102(9) 0.073(7) 0.125(8) 0.001(6) 0.021(7) 0.015(6) C16 0.106(9) 0.105(10) 0.115(8) 0.032(7) 0.021(6) 0.005(7) C17 0.075(6) 0.052(5) 0.084(6) -0.005(4) 0.001(4) -0.001(4) C18 0.075(7) 0.053(6) 0.174(10) 0.015(6) 0.021(6) -0.003(5) C19 0.088(7) 0.078(8) 0.131(9) -0.003(6) -0.009(6) 0.021(6) C21 0.087(6) 0.048(5) 0.062(4) 0.005(4) 0.006(4) -0.008(4) C22 0.088(7) 0.045(5) 0.094(6) -0.009(4) 0.023(5) 0.000(4) C23 0.075(6) 0.032(4) 0.072(5) -0.002(3) 0.010(4) 0.003(3) C24 0.075(6) 0.061(6) 0.087(6) -0.002(4) 0.004(5) -0.010(4) C25 0.087(9) 0.271(22) 0.134(10) 0.053(12) -0.006(8) -0.067(11) C26 0.115(11) 0.075(9) 0.201(14) 0.036(9) 0.009(9) -0.019(7) C27 0.079(6) 0.048(5) 0.101(6) -0.003(4) 0.009(5) 0.009(4) C28 0.082(7) 0.084(7) 0.110(7) -0.015(6) 0.025(5) 0.007(5) C29 0.071(7) 0.077(7) 0.130(7) -0.006(6) 0.005(6) 0.018(5) C31 0.069(6) 0.043(5) 0.083(5) 0.002(4) 0.008(4) -0.004(4) C32 0.089(7) 0.045(5) 0.077(5) 0.017(4) 0.011(4) 0.003(4) C33 0.087(7) 0.049(5) 0.061(4) -0.001(3) 0.010(4) -0.016(4) C34 0.082(7) 0.050(5) 0.097(6) 0.006(4) 0.005(5) 0.003(4) C35 0.090(8) 0.115(10) 0.124(8) -0.026(7) -0.016(7) 0.017(7) C36 0.086(8) 0.083(9) 0.181(11) -0.006(8) 0.025(7) 0.031(6) C37 0.088(7) 0.056(5) 0.084(6) 0.000(4) 0.023(5) -0.003(4) C38 0.088(8) 0.065(6) 0.130(8) -0.006(6) 0.022(6) -0.012(5) C39 0.092(8) 0.065(7) 0.124(8) 0.001(6) 0.005(6) -0.020(5) B1 0.059(5) 0.035(4) 0.068(5) -0.004(4) 0.009(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 2.014(9) . ? Co1 N21 2.017(7) . ? Co1 N31 2.025(6) . ? Co1 N11 2.049(7) . ? N11 C11 1.320(10) . ? N11 N12 1.376(9) . ? N12 C13 1.376(10) . ? N12 B1 1.489(10) . ? N21 N22 1.340(9) . ? N21 C21 1.338(10) . ? N22 C23 1.360(9) . ? N22 B1 1.578(10) . ? N31 C31 1.340(10) . ? N31 N32 1.342(9) . ? N32 C33 1.379(10) . ? N32 B1 1.569(11) . ? C1 C2 1.36(2) . ? C11 C12 1.369(12) . ? C11 C14 1.511(13) . ? C12 C13 1.400(12) . ? C13 C17 1.500(13) . ? C14 C16 1.502(14) . ? C14 C15 1.529(12) . ? C17 C18 1.519(13) . ? C17 C19 1.516(13) . ? C21 C22 1.395(11) . ? C21 C24 1.488(12) . ? C22 C23 1.381(12) . ? C23 C27 1.481(11) . ? C24 C25 1.444(14) . ? C24 C26 1.454(14) . ? C27 C28 1.504(12) . ? C27 C29 1.551(12) . ? C31 C32 1.415(11) . ? C31 C34 1.515(12) . ? C32 C33 1.370(12) . ? C33 C37 1.490(12) . ? C34 C36 1.504(14) . ? C34 C35 1.501(13) . ? C37 C39 1.519(13) . ? C37 C38 1.546(13) . ? 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 Co1 N21 125.2(3) . . ? C1 Co1 N31 124.5(3) . . ? N21 Co1 N31 91.7(2) . . ? C1 Co1 N11 123.1(3) . . ? N21 Co1 N11 90.9(3) . . ? N31 Co1 N11 91.7(3) . . ? C11 N11 N12 109.0(7) . . ? C11 N11 Co1 137.3(6) . . ? N12 N11 Co1 113.7(5) . . ? N11 N12 C13 107.2(6) . . ? N11 N12 B1 120.4(6) . . ? C13 N12 B1 132.3(7) . . ? N22 N21 C21 108.1(6) . . ? N22 N21 Co1 115.0(4) . . ? C21 N21 Co1 136.8(6) . . ? N21 N22 C23 111.2(6) . . ? N21 N22 B1 119.8(6) . . ? C23 N22 B1 129.0(7) . . ? C31 N31 N32 108.0(6) . . ? C31 N31 Co1 137.2(6) . . ? N32 N31 Co1 114.8(5) . . ? N31 N32 C33 109.8(6) . . ? N31 N32 B1 119.9(6) . . ? C33 N32 B1 130.4(7) . . ? C2 C1 Co1 119.7(10) . . ? N11 C11 C12 110.1(8) . . ? N11 C11 C14 119.2(8) . . ? C12 C11 C14 130.7(7) . . ? C11 C12 C13 106.2(7) . . ? N12 C13 C12 107.5(7) . . ? N12 C13 C17 123.5(8) . . ? C12 C13 C17 128.9(8) . . ? C16 C14 C11 113.8(8) . . ? C16 C14 C15 107.1(8) . . ? C11 C14 C15 110.6(8) . . ? C13 C17 C18 109.6(7) . . ? C13 C17 C19 111.2(9) . . ? C18 C17 C19 112.6(8) . . ? N21 C21 C22 107.4(7) . . ? N21 C21 C24 121.0(7) . . ? C22 C21 C24 131.6(8) . . ? C23 C22 C21 108.3(8) . . ? N22 C23 C22 104.9(7) . . ? N22 C23 C27 126.2(7) . . ? C22 C23 C27 128.8(8) . . ? C25 C24 C26 109.7(11) . . ? C25 C24 C21 113.0(8) . . ? C26 C24 C21 112.2(9) . . ? C23 C27 C28 113.2(8) . . ? C23 C27 C29 110.4(8) . . ? C28 C27 C29 109.2(8) . . ? N31 C31 C32 109.0(7) . . ? N31 C31 C34 121.5(7) . . ? C32 C31 C34 129.6(8) . . ? C33 C32 C31 105.9(7) . . ? C32 C33 N32 107.4(8) . . ? C32 C33 C37 130.0(8) . . ? N32 C33 C37 122.6(8) . . ? C36 C34 C35 110.8(9) . . ? C36 C34 C31 110.1(8) . . ? C35 C34 C31 109.9(8) . . ? C33 C37 C39 111.5(8) . . ? C33 C37 C38 111.3(8) . . ? C39 C37 C38 108.7(8) . . ? N12 B1 N32 108.6(6) . . ? N12 B1 N22 109.6(6) . . ? N32 B1 N22 107.7(6) . . ? _refine_diff_density_max 1.001 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.099 #=END data_shelxl2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'compound 3c ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H51 B N6 Ni O2' _chemical_formula_weight 609.30 _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.968(5) _cell_length_b 15.820(2) _cell_length_c 21.570(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.02(2) _cell_angle_gamma 90.00 _cell_volume 3376.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method ? _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK?Ga _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6368 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.57 _reflns_number_total 6368 _reflns_number_observed 5974 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[?Gs^2^(Fo^2^)+(0.1000P)^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 6368 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_obs 0.0844 _refine_ls_wR_factor_all 0.2375 _refine_ls_wR_factor_obs 0.2337 _refine_ls_goodness_of_fit_all 1.990 _refine_ls_goodness_of_fit_obs 2.025 _refine_ls_restrained_S_all 1.990 _refine_ls_restrained_S_obs 2.025 _refine_ls_shift/esd_max 0.080 _refine_ls_shift/esd_mean 0.003 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 0.15665(4) 0.16045(3) 0.82390(2) 0.0352(2) Uani 1 d . . O1 O -0.0250(3) 0.2906(2) 0.7863(2) 0.0820(12) Uani 1 d . . O2 O -0.1219(4) 0.1231(3) 0.8382(3) 0.095(2) Uani 1 d . . N11 N 0.2551(3) 0.0537(2) 0.85991(15) 0.0406(7) Uani 1 d . . N12 N 0.3934(3) 0.0571(2) 0.86301(14) 0.0382(6) Uani 1 d . . N21 N 0.2616(3) 0.1431(2) 0.75063(14) 0.0364(6) Uani 1 d . . N22 N 0.3991(3) 0.1378(2) 0.7646(2) 0.0391(7) Uani 1 d . . N31 N 0.2969(3) 0.2275(2) 0.88015(14) 0.0390(6) Uani 1 d . . N32 N 0.4271(3) 0.2138(2) 0.86837(15) 0.0392(6) Uani 1 d . . C1 C 0.0893(4) 0.2677(2) 0.7883(2) 0.0450(8) Uani 1 d . . C2 C 0.1935(4) 0.3233(2) 0.7616(2) 0.0468(9) Uani 1 d . . C3 C 0.1690(6) 0.4166(3) 0.7718(2) 0.0643(12) Uani 1 d . . H3A H 0.1688(29) 0.4273(4) 0.8156(3) 0.064 Uiso 1 calc R . H3B H 0.0832(14) 0.4326(5) 0.7497(11) 0.064 Uiso 1 calc R . H3C H 0.2394(16) 0.4491(3) 0.7565(12) 0.064 Uiso 1 calc R . C4 C -0.0124(5) 0.1358(3) 0.8336(2) 0.0560(11) Uani 1 d . . C11 C 0.2248(4) -0.0208(2) 0.8838(2) 0.0468(9) Uani 1 d . . C12 C 0.3429(5) -0.0650(3) 0.9030(2) 0.0540(10) Uani 1 d . . C13 C 0.4478(4) -0.0145(3) 0.8899(2) 0.0497(9) Uani 1 d . . C14 C 0.0807(5) -0.0480(3) 0.8853(3) 0.0672(14) Uani 1 d . . C15 C 0.0692(7) -0.1293(5) 0.9140(6) 0.152(5) Uani 1 d . . H15A H -0.0238(11) -0.1401(19) 0.9187(29) 0.152 Uiso 1 calc R . H15B H 0.1221(53) -0.1298(14) 0.9543(13) 0.152 Uiso 1 calc R . H15C H 0.1017(61) -0.1722(6) 0.8881(15) 0.152 Uiso 1 calc R . C16 C 0.0184(8) -0.0742(6) 0.8152(4) 0.122(3) Uani 1 d . . H16A H 0.0552(38) -0.0382(20) 0.7857(4) 0.122 Uiso 1 calc R . H16B H -0.0781(9) -0.0681(30) 0.8108(8) 0.122 Uiso 1 calc R . H16C H 0.0411(42) -0.1320(11) 0.8076(9) 0.122 Uiso 1 calc R . C17 C 0.5978(5) -0.0311(3) 0.9010(3) 0.0665(13) Uani 1 d . . C18 C 0.6306(7) -0.0890(5) 0.9599(3) 0.095(2) Uani 1 d . . H18A H 0.6019(38) -0.1457(7) 0.9496(6) 0.095 Uiso 1 calc R . H18B H 0.5838(33) -0.0682(16) 0.9931(7) 0.095 Uiso 1 calc R . H18C H 0.7262(9) -0.0884(21) 0.9729(12) 0.095 Uiso 1 calc R . C19 C 0.6507(7) -0.0667(6) 0.8506(4) 0.112(3) Uani 1 d . . H19A H 0.6089(35) -0.0413(22) 0.8126(4) 0.112 Uiso 1 calc R . H19B H 0.6334(41) -0.1264(8) 0.8496(13) 0.112 Uiso 1 calc R . H19C H 0.7464(11) -0.0569(25) 0.8546(12) 0.112 Uiso 1 calc R . C21 C 0.2305(4) 0.1366(2) 0.6893(2) 0.0404(8) Uani 1 d . . C22 C 0.3487(5) 0.1282(3) 0.6613(2) 0.0511(10) Uani 1 d . . C23 C 0.4532(4) 0.1287(3) 0.7091(2) 0.0478(9) Uani 1 d . . C24 C 0.0856(5) 0.1355(3) 0.6594(2) 0.0518(10) Uani 1 d . . C25 C 0.0454(16) 0.0460(8) 0.6297(8) 0.102(6) Uani 0.51 d P . C25A C 0.0397(22) 0.0489(16) 0.6671(13) 0.117(9) Uani 0.49 d P . C26 C 0.0438(14) 0.2042(7) 0.6132(6) 0.072(3) Uani 0.51 d P . C26A C 0.0889(16) 0.1732(10) 0.5909(6) 0.077(4) Uani 0.49 d P . C27 C 0.6029(5) 0.1203(3) 0.7077(3) 0.0612(12) Uani 1 d . . C28 C 0.6157(18) 0.0591(11) 0.6453(9) 0.103(5) Uani 0.57 d P . C28A C 0.6456(22) 0.0388(11) 0.6818(12) 0.096(7) Uani 0.43 d P . C29 C 0.6581(13) 0.2027(11) 0.6987(7) 0.067(3) Uani 0.57 d P . C29A C 0.6720(23) 0.1975(14) 0.6770(11) 0.087(7) Uani 0.43 d P . C31 C 0.2975(4) 0.2948(2) 0.9165(2) 0.0402(8) Uani 1 d . . C32 C 0.4290(4) 0.3258(2) 0.9289(2) 0.0487(9) Uani 1 d . . C33 C 0.5085(4) 0.2737(2) 0.8981(2) 0.0462(9) Uani 1 d . . C34 C 0.1707(4) 0.3256(3) 0.9409(2) 0.0465(9) Uani 1 d . . C35 C 0.1838(6) 0.4150(3) 0.9640(3) 0.0745(15) Uani 1 d . . H35A H 0.2446(26) 0.4168(4) 1.0021(9) 0.075 Uiso 1 calc R . H35B H 0.0967(8) 0.4356(8) 0.9716(15) 0.075 Uiso 1 calc R . H35C H 0.2185(32) 0.4497(5) 0.9331(7) 0.075 Uiso 1 calc R . C36 C 0.1318(5) 0.2654(3) 0.9911(2) 0.0660(13) Uani 1 d . . H36A H 0.2024(15) 0.2645(15) 1.0256(7) 0.066 Uiso 1 calc R . H36B H 0.1191(30) 0.2096(5) 0.9740(5) 0.066 Uiso 1 calc R . H36C H 0.0493(17) 0.2844(12) 1.0053(10) 0.066 Uiso 1 calc R . C37 C 0.6564(4) 0.2778(3) 0.8921(3) 0.0618(12) Uani 1 d . . C38 C 0.7140(12) 0.3622(7) 0.8908(12) 0.131(8) Uani 0.58 d P . C38A C 0.6674(13) 0.3222(12) 0.8322(8) 0.090(5) Uani 0.42 d P . C39 C 0.7331(9) 0.2232(9) 0.9492(5) 0.086(3) Uani 0.58 d P . C39A C 0.7253(17) 0.3311(19) 0.9566(12) 0.141(10) Uani 0.42 d P . B1 B 0.4600(4) 0.1326(3) 0.8336(2) 0.0403(9) Uani 1 d . . H0 H 0.5693 0.1200 0.8370 0.091 Uiso 1 d . . H2A H 0.1907 0.3122 0.7180 0.058 Uiso 1 d . . H2B H 0.2817 0.3087 0.7817 0.058 Uiso 1 d . . H12 H 0.3504 -0.1196 0.9221 0.064 Uiso 1 d . . H14 H 0.0277 -0.0061 0.9032 0.081 Uiso 1 d . . H17 H 0.6417 0.0218 0.9106 0.081 Uiso 1 d . . H22 H 0.3552 0.1235 0.6174 0.062 Uiso 1 d . . H32 H 0.4578 0.3742 0.9536 0.058 Uiso 1 d . . H34 H 0.1011 0.3248 0.9068 0.056 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 0.0249(3) 0.0302(3) 0.0508(3) -0.0002(2) 0.0059(2) 0.0010(2) O1 0.040(2) 0.061(2) 0.143(4) 0.031(2) 0.006(2) 0.018(2) O2 0.032(2) 0.082(3) 0.173(4) 0.045(3) 0.022(2) 0.005(2) N11 0.0274(15) 0.0338(15) 0.061(2) 0.0026(12) 0.0085(13) 0.0010(12) N12 0.0284(15) 0.0300(14) 0.056(2) 0.0017(12) 0.0059(12) 0.0017(11) N21 0.0301(15) 0.0338(14) 0.046(2) -0.0009(11) 0.0088(12) 0.0019(11) N22 0.0250(14) 0.0331(14) 0.061(2) -0.0008(13) 0.0137(13) 0.0046(11) N31 0.0286(15) 0.0312(14) 0.056(2) 0.0005(12) 0.0020(12) 0.0018(11) N32 0.0249(14) 0.0318(14) 0.060(2) 0.0006(12) 0.0019(12) 0.0004(11) C1 0.038(2) 0.035(2) 0.060(2) 0.0017(15) 0.002(2) 0.0066(15) C2 0.048(2) 0.033(2) 0.059(2) 0.0046(15) 0.003(2) 0.000(2) C3 0.078(3) 0.034(2) 0.079(3) 0.003(2) 0.002(2) -0.002(2) C4 0.048(3) 0.044(2) 0.076(3) 0.014(2) 0.007(2) -0.001(2) C11 0.038(2) 0.037(2) 0.067(2) 0.005(2) 0.013(2) 0.001(2) C12 0.052(3) 0.032(2) 0.078(3) 0.013(2) 0.008(2) 0.004(2) C13 0.038(2) 0.037(2) 0.071(3) 0.004(2) -0.002(2) 0.006(2) C14 0.046(3) 0.045(2) 0.116(4) 0.014(2) 0.030(3) -0.003(2) C15 0.057(4) 0.094(5) 0.307(14) 0.097(7) 0.025(6) -0.010(4) C16 0.083(5) 0.103(6) 0.180(8) -0.039(6) 0.021(5) -0.020(4) C17 0.040(2) 0.046(2) 0.109(4) 0.010(2) -0.007(2) 0.007(2) C18 0.083(4) 0.091(5) 0.103(4) 0.005(4) -0.016(3) 0.026(4) C19 0.063(4) 0.140(7) 0.134(6) 0.007(5) 0.014(4) 0.042(4) C21 0.043(2) 0.032(2) 0.047(2) -0.0009(13) 0.0110(15) 0.0045(15) C22 0.059(3) 0.047(2) 0.051(2) 0.003(2) 0.018(2) 0.009(2) C23 0.046(2) 0.040(2) 0.061(2) 0.008(2) 0.023(2) 0.006(2) C24 0.050(3) 0.047(2) 0.057(2) -0.005(2) -0.003(2) 0.008(2) C25 0.084(8) 0.050(5) 0.162(14) -0.018(7) -0.029(10) -0.013(5) C25A 0.058(9) 0.117(15) 0.171(21) -0.049(16) -0.009(13) -0.016(8) C26 0.083(9) 0.051(6) 0.074(7) 0.014(5) -0.025(6) 0.002(5) C26A 0.085(10) 0.083(10) 0.060(7) -0.003(6) -0.007(6) 0.007(7) C27 0.046(2) 0.059(3) 0.087(3) 0.012(2) 0.037(2) 0.015(2) C28 0.086(10) 0.081(11) 0.153(15) -0.007(9) 0.066(11) 0.022(8) C28A 0.083(12) 0.046(7) 0.172(22) 0.016(10) 0.072(15) 0.021(7) C29 0.033(5) 0.089(8) 0.085(9) 0.006(7) 0.033(5) -0.012(5) C29A 0.081(11) 0.063(8) 0.137(18) 0.025(10) 0.094(12) 0.006(7) C31 0.036(2) 0.034(2) 0.049(2) 0.0002(14) 0.0004(14) 0.0039(14) C32 0.045(2) 0.036(2) 0.063(2) -0.006(2) -0.004(2) 0.000(2) C33 0.036(2) 0.031(2) 0.069(2) 0.003(2) -0.005(2) -0.0020(14) C34 0.046(2) 0.045(2) 0.047(2) -0.0022(15) 0.001(2) 0.009(2) C35 0.087(4) 0.052(3) 0.090(4) -0.010(2) 0.034(3) 0.010(3) C36 0.058(3) 0.069(3) 0.075(3) 0.014(2) 0.025(2) 0.010(2) C37 0.035(2) 0.047(2) 0.102(3) -0.003(2) 0.001(2) -0.008(2) C38 0.046(6) 0.057(6) 0.299(25) -0.023(10) 0.056(10) -0.020(5) C38A 0.039(7) 0.110(13) 0.127(14) -0.006(10) 0.031(8) -0.013(7) C39 0.041(5) 0.117(9) 0.092(7) -0.002(6) -0.022(4) 0.009(5) C39A 0.037(8) 0.230(30) 0.148(18) -0.040(17) -0.026(10) -0.038(12) B1 0.023(2) 0.033(2) 0.065(2) -0.001(2) 0.005(2) 0.0015(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 Ni1 C4 1.767(5) . ? Ni1 C1 1.947(4) . ? Ni1 N21 2.018(3) . ? Ni1 N31 2.034(3) . ? Ni1 N11 2.058(3) . ? O1 C1 1.192(5) . ? O2 C4 1.126(6) . ? N11 C11 1.335(5) . ? N11 N12 1.373(4) . ? N12 C13 1.355(5) . ? N12 B1 1.541(5) . ? N21 C21 1.324(5) . ? N21 N22 1.370(4) . ? N22 C23 1.380(5) . ? N22 B1 1.537(6) . ? N31 C31 1.323(5) . ? N31 N32 1.370(4) . ? N32 C33 1.358(5) . ? N32 B1 1.543(5) . ? C1 C2 1.527(6) . ? C2 C3 1.517(6) . ? C11 C12 1.389(6) . ? C11 C14 1.504(6) . ? C12 C13 1.373(6) . ? C13 C17 1.508(6) . ? C14 C15 1.438(8) . ? C14 C16 1.617(10) . ? C17 C19 1.385(8) . ? C17 C18 1.567(8) . ? C21 C22 1.395(5) . ? C21 C24 1.509(6) . ? C22 C23 1.374(6) . ? C23 C27 1.503(6) . ? C24 C25A 1.46(3) . ? C24 C26 1.498(11) . ? C24 C26A 1.596(15) . ? C24 C25 1.585(12) . ? C25 C25A 0.82(3) . ? C26 C26A 0.85(2) . ? C27 C29 1.44(2) . ? C27 C28A 1.49(2) . ? C27 C29A 1.59(2) . ? C27 C28 1.68(2) . ? C28 C28A 0.87(3) . ? C29 C29A 0.51(2) . ? C31 C32 1.395(6) . ? C31 C34 1.508(5) . ? C32 C33 1.369(6) . ? C33 C37 1.497(6) . ? C34 C35 1.499(6) . ? C34 C36 1.527(6) . ? C37 C38A 1.49(2) . ? C37 C38 1.455(11) . ? C37 C39 1.617(11) . ? C37 C39A 1.70(2) . ? C38 C39A 1.49(3) . ? C38 C38A 1.44(3) . ? C39 C39A 1.72(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 C4 Ni1 C1 87.2(2) . . ? C4 Ni1 N21 131.0(2) . . ? C1 Ni1 N21 89.80(14) . . ? C4 Ni1 N31 129.8(2) . . ? C1 Ni1 N31 87.71(14) . . ? N21 Ni1 N31 98.86(13) . . ? C4 Ni1 N11 101.1(2) . . ? C1 Ni1 N11 171.74(15) . . ? N21 Ni1 N11 85.12(12) . . ? N31 Ni1 N11 86.64(12) . . ? C11 N11 N12 106.8(3) . . ? C11 N11 Ni1 138.6(3) . . ? N12 N11 Ni1 114.6(2) . . ? C13 N12 N11 109.6(3) . . ? C13 N12 B1 130.9(3) . . ? N11 N12 B1 119.4(3) . . ? C21 N21 N22 108.7(3) . . ? C21 N21 Ni1 135.4(3) . . ? N22 N21 Ni1 115.9(2) . . ? N21 N22 C23 107.5(3) . . ? N21 N22 B1 118.9(3) . . ? C23 N22 B1 133.1(3) . . ? C31 N31 N32 107.6(3) . . ? C31 N31 Ni1 136.6(3) . . ? N32 N31 Ni1 113.9(2) . . ? C33 N32 N31 109.1(3) . . ? C33 N32 B1 131.4(3) . . ? N31 N32 B1 119.0(3) . . ? O1 C1 C2 120.1(4) . . ? O1 C1 Ni1 124.2(3) . . ? C2 C1 Ni1 115.7(3) . . ? C1 C2 C3 112.2(4) . . ? O2 C4 Ni1 177.0(4) . . ? N11 C11 C12 109.7(4) . . ? N11 C11 C14 121.5(4) . . ? C12 C11 C14 128.8(4) . . ? C13 C12 C11 106.5(3) . . ? N12 C13 C12 107.5(3) . . ? N12 C13 C17 123.4(4) . . ? C12 C13 C17 129.1(4) . . ? C15 C14 C11 113.1(5) . . ? C15 C14 C16 97.5(7) . . ? C11 C14 C16 108.2(4) . . ? C19 C17 C13 114.3(5) . . ? C19 C17 C18 109.7(5) . . ? C13 C17 C18 109.6(5) . . ? N21 C21 C22 109.5(4) . . ? N21 C21 C24 121.5(3) . . ? C22 C21 C24 128.9(4) . . ? C23 C22 C21 106.0(4) . . ? N22 C23 C22 108.2(3) . . ? N22 C23 C27 121.4(4) . . ? C22 C23 C27 130.4(4) . . ? C25A C24 C21 105.0(10) . . ? C25A C24 C26 133.7(11) . . ? C21 C24 C26 116.8(6) . . ? C25A C24 C26A 119.9(12) . . ? C21 C24 C26A 105.4(7) . . ? C26 C24 C26A 31.8(6) . . ? C25A C24 C25 30.8(10) . . ? C21 C24 C25 111.4(6) . . ? C26 C24 C25 110.1(8) . . ? C26A C24 C25 89.6(9) . . ? C25A C25 C24 66.1(22) . . ? C25 C25A C24 83.1(28) . . ? C26A C26 C24 80.4(14) . . ? C26 C26A C24 67.8(13) . . ? C29 C27 C23 108.7(6) . . ? C29 C27 C28A 127.1(9) . . ? C23 C27 C28A 114.5(10) . . ? C29 C27 C29A 18.6(10) . . ? C23 C27 C29A 115.0(9) . . ? C28A C27 C29A 110.7(10) . . ? C29 C27 C28 110.3(9) . . ? C23 C27 C28 103.9(7) . . ? C28A C27 C28 31.2(9) . . ? C29A C27 C28 91.7(10) . . ? C28A C28 C27 62.4(20) . . ? C28 C28A C27 86.4(19) . . ? C29A C29 C27 97.5(43) . . ? C29 C29A C27 64.0(36) . . ? N31 C31 C32 109.4(3) . . ? N31 C31 C34 121.6(3) . . ? C32 C31 C34 128.9(3) . . ? C33 C32 C31 106.4(3) . . ? N32 C33 C32 107.6(4) . . ? N32 C33 C37 121.8(4) . . ? C32 C33 C37 130.6(4) . . ? C31 C34 C35 112.2(4) . . ? C31 C34 C36 110.0(3) . . ? C35 C34 C36 111.8(4) . . ? C38A C37 C38 58.6(11) . . ? C38A C37 C33 105.9(6) . . ? C38 C37 C33 115.9(6) . . ? C38A C37 C39 146.7(7) . . ? C38 C37 C39 110.7(10) . . ? C33 C37 C39 106.9(5) . . ? C38A C37 C39A 114.4(13) . . ? C38 C37 C39A 55.9(12) . . ? C33 C37 C39A 104.7(8) . . ? C39 C37 C39A 62.3(11) . . ? C39A C38 C38A 131.9(15) . . ? C39A C38 C37 70.3(11) . . ? C38A C38 C37 61.8(9) . . ? C37 C38A C38 59.6(9) . . ? C37 C39 C39A 61.2(9) . . ? C38 C39A C37 53.8(8) . . ? C38 C39A C39 103.8(15) . . ? C37 C39A C39 56.5(9) . . ? N22 B1 N12 107.5(3) . . ? N22 B1 N32 110.1(3) . . ? N12 B1 N32 108.4(3) . . ? _refine_diff_density_max 1.209 _refine_diff_density_min -1.406 _refine_diff_density_rms 0.135 #END