# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1378 data_dbmva _audit_creation_date 98-01-27 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common [(thptach)Cr(CO)3] #ActaC _chemical_formula_analytical C15_H27_Cr_N3_O6 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural [(C12H27N3O3)Cr(CO)3] #ActaC _chemical_formula_sum C15_H27_Cr_N3_O6 #ActaC _chemical_formula_weight 397.39 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf NONIUS software' #ActaC _computing_cell_refinement 'Enraf NONIUS software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 12.582(4) #ActaC _cell_length_b 12.186(3) #ActaC _cell_length_c 12.849(2) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 107.56(2) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 1878.3(8) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 10 #ActaC _cell_measurement_theta_min 20.4 #ActaC _cell_measurement_theta_max 23.9 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21/n_1 #ActaC _symmetry_space_group_name_Hall -p_2yn #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour orange #ActaC _exptl_crystal_size_max 1.30 #ActaC _exptl_crystal_size_mid 0.85 #ActaC _exptl_crystal_size_min 0.25 #ActaC _exptl_crystal_density_diffrn 1.405 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 840 #ActaC _exptl_absorpt_process_details 'XTAL ABSORB software' _exptl_absorpt_coefficient_mu 0.64 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.62 #ActaC _exptl_absorpt_correction_T_max 0.78 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/omega #ActaC _diffrn_standards_number 10 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 6 7 6 6 -7 6 -6 7 -6 -6 -7 -6 9 7 -8 -9 7 8 -9 -7 8 9 -7 -8 0 0 14 0 0 -14 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 5770 #ActaC _diffrn_reflns_av_R_equivalents .033 #ActaC _diffrn_reflns_av_sigmaI/netI .034 #ActaC _diffrn_reflns_limit_h_min -16 #ActaC _diffrn_reflns_limit_h_max 16 #ActaC _diffrn_reflns_limit_k_min -15 #ActaC _diffrn_reflns_limit_k_max 0 #ActaC _diffrn_reflns_limit_l_min -16 #ActaC _diffrn_reflns_limit_l_max 3 #ActaC _diffrn_reflns_theta_min 1.99 #ActaC _diffrn_reflns_theta_max 27.47 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 60 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 108 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 12 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 24 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cr ? 0 4 .284 .624 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Cr .21296(3) .25888(3) .35438(3) .0311(2) Uani ? ? N11 .33437(15) .15675(15) .47457(14) .0320(8) Uani ? ? C111 .3451(2) .03794(19) .4993(2) .0377(11) Uani ? ? C112 .2364(2) -.0139(2) .5011(2) .0434(12) Uani ? ? C113 .2545(2) -.1289(2) .5465(2) .0490(13) Uani ? ? O113 .3264(2) -.12199(19) .65588(18) .0628(12) Uani ? ? C12 .42821(18) .1992(2) .4411(2) .0356(10) Uani ? ? N13 .38941(15) .30855(15) .39675(15) .0335(8) Uani ? ? C131 .4605(2) .3580(2) .3366(2) .0430(12) Uani ? ? C132 .4471(2) .3051(3) .2273(2) .0470(13) Uani ? ? C133 .5307(2) .3523(3) .1752(3) .0527(15) Uani ? ? O133 .63769(18) .31128(19) .2323(2) .0584(12) Uani ? ? C14 .3786(2) .3803(2) .4855(2) .0379(11) Uani ? ? N15 .28754(16) .32985(16) .51764(15) .0360(9) Uani ? ? C151 .2444(3) .3962(2) .5926(2) .0492(13) Uani ? ? C152 .1952(3) .5050(3) .5473(2) .0519(14) Uani ? ? C153 .1235(3) .5494(3) .6144(3) .0589(16) Uani ? ? O153 .18577(18) .5607(2) .72769(17) .0537(11) Uani ? ? C16 .3236(2) .2225(2) .5664(2) .0383(11) Uani ? ? C01 .1378(2) .3749(2) .2777(2) .0410(11) Uani ? ? O01 .08613(18) .4466(2) .22750(19) .0696(12) Uani ? ? C02 .0790(2) .2067(2) .3570(2) .0458(12) Uani ? ? O02 -.00893(17) .1720(2) .3531(2) .0772(14) Uani ? ? C03 .1879(2) .1869(2) .2259(2) .0423(12) Uani ? ? O03 .1660(2) .1428(2) .14125(17) .0681(12) Uani ? ? H111a .406(2) .026(2) .572(2) .034(6) Uiso ? ? H111b .372(2) .003(2) .445(2) .045(7) Uiso ? ? H112a .179(2) -.012(2) .422(2) .053(8) Uiso ? ? H112b .196(2) .030(2) .542(2) .052(8) Uiso ? ? H113a .292(2) -.174(2) .506(2) .055(8) Uiso ? ? H113b .187(3) -.159(3) .553(2) .062(9) Uiso ? ? H113 .332(3) -.174(3) .681(3) .081(14) Uiso ? ? H12a .437(2) .152(2) .378(2) .036(6) Uiso ? ? H12b .503(2) .205(2) .505(2) .038(6) Uiso ? ? H131a .535(2) .355(2) .378(2) .044(7) Uiso ? ? H131b .443(2) .433(3) .326(2) .050(8) Uiso ? ? H132a .374(2) .318(2) .184(2) .045(7) Uiso ? ? H132b .459(2) .228(2) .232(2) .040(7) Uiso ? ? H133a .534(2) .432(2) .176(2) .047(8) Uiso ? ? H133b .515(3) .326(3) .101(3) .064(9) Uiso ? ? H133 .679(3) .353(3) .243(3) .065(12) Uiso ? ? H14a .357(2) .449(2) .454(2) .032(6) Uiso ? ? H14b .452(3) .381(2) .548(3) .060(9) Uiso ? ? H151a .300(2) .409(2) .663(2) .055(8) Uiso ? ? H151b .158(3) .381(2) .591(2) .058(8) Uiso ? ? H152a .143(3) .499(4) .456(4) .102(13) Uiso ? ? H152b .265(4) .565(4) .540(4) .137(18) Uiso ? ? H153a .067(3) .495(3) .623(3) .071(10) Uiso ? ? H153b .094(3) .621(3) .589(3) .082(12) Uiso ? ? H153 .184(3) .506(3) .755(2) .042(9) Uiso ? ? H16a .271(2) .192(2) .594(2) .047(8) Uiso ? ? H16b .384(3) .223(2) .628(2) .048(8) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Cr .0267(2) .0371(2) .0260(2) .00064(13) .00281(14) .00085(14) N11 .0307(9) .0357(9) .0275(9) .0022(7) .0057(7) .0026(7) C111 .0399(12) .0355(12) .0364(12) .0040(9) .0096(10) .0052(10) C112 .0356(12) .0426(13) .0441(14) -.0020(10) -.0000(11) .0067(11) C113 .0463(14) .0422(14) .0531(17) -.0046(11) .0067(13) .0067(12) O113 .0794(15) .0473(12) .0497(12) -.0021(11) .0015(10) .0175(10) C12 .0296(11) .0375(12) .0375(12) .0032(9) .0069(9) .0030(10) N13 .0307(9) .0339(10) .0342(10) .0003(7) .0073(8) .0023(8) C131 .0404(13) .0405(13) .0495(15) -.0048(10) .0156(12) .0040(11) C132 .0375(13) .0637(18) .0389(14) -.0015(12) .0101(11) .0095(12) C133 .0447(14) .0665(19) .0498(17) .0086(13) .0186(13) .0191(14) O133 .0418(11) .0554(13) .0795(16) .0055(10) .0204(11) .0248(11) C14 .0358(12) .0370(12) .0369(13) -.0008(9) .0048(10) -.0040(10) N15 .0375(10) .0394(10) .0280(10) .0043(8) .0056(8) -.0023(8) C151 .0576(17) .0513(15) .0374(14) .0136(12) .0126(12) -.0067(11) C152 .0543(16) .0570(16) .0434(15) .0117(13) .0132(13) -.0005(13) C153 .0511(17) .071(2) .0513(17) .0177(15) .0109(14) -.0120(15) O153 .0640(13) .0544(13) .0428(11) -.0057(10) .0162(9) -.0129(10) C16 .0427(13) .0422(13) .0283(12) .0046(10) .0080(11) .0003(9) C01 .0338(11) .0551(14) .0296(12) .0008(10) .0029(9) .0045(10) O01 .0599(13) .0735(15) .0650(14) .0193(11) .0032(11) .0287(12) C02 .0376(13) .0528(14) .0436(14) .0028(11) .0071(11) .0054(12) O02 .0366(11) .0940(18) .1007(19) -.0134(11) .0203(12) .0103(15) C03 .0353(12) .0475(14) .0389(13) -.0019(10) .0033(10) -.0051(11) O03 .0697(14) .0809(15) .0445(12) -.0026(12) .0033(10) -.0234(11) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 3020(964) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 3703 #ActaC _refine_ls_number_parameters 335 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .057 #ActaC _refine_ls_R_factor_obs .049 #ActaC _refine_ls_wR_factor_all .066 #ActaC _refine_ls_wR_factor_obs .064 #ActaC _refine_ls_goodness_of_fit_all 1.796 #ActaC _refine_ls_goodness_of_fit_obs 1.892 #ActaC _refine_ls_shift/esd_max .088 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -.673 #ActaC _refine_diff_density_max .577 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Cr N11 2.2008(17) . . ? Cr N13 2.205(2) . . ? Cr N15 2.2002(18) . . ? Cr C01 1.817(2) . . ? Cr C02 1.811(3) . . ? Cr C03 1.811(3) . . ? N11 C111 1.480(3) . . ? N11 C12 1.467(3) . . ? N11 C16 1.467(3) . . ? C111 C112 1.514(4) . . ? C111 H111a 1.02(2) . . ? C111 H111b .96(3) . . ? C112 C113 1.509(4) . . ? C112 H112a 1.05(3) . . ? C112 H112b .99(3) . . ? C113 O113 1.426(3) . . ? C113 H113a .98(3) . . ? C113 H113b .96(4) . . ? O113 H113 .70(4) . . ? C12 N13 1.473(3) . . ? C12 H12a 1.02(3) . . ? C12 H12b 1.05(2) . . ? N13 C131 1.476(4) . . ? N13 C14 1.475(3) . . ? C131 C132 1.507(4) . . ? C131 H131a .93(3) . . ? C131 H131b .94(3) . . ? C132 C133 1.520(5) . . ? C132 H132a .94(3) . . ? C132 H132b .96(3) . . ? C133 O133 1.416(3) . . ? C133 H133a .97(3) . . ? C133 H133b .97(3) . . ? O133 H133 .72(4) . . ? C14 N15 1.465(4) . . ? C14 H14a .93(2) . . ? C14 H14b 1.03(3) . . ? N15 C151 1.481(4) . . ? N15 C16 1.462(3) . . ? C151 C152 1.505(4) . . ? C151 H151a .98(3) . . ? C151 H151b 1.10(3) . . ? C152 C153 1.524(5) . . ? C152 H152a 1.16(4) . . ? C152 H152b 1.17(5) . . ? C153 O153 1.436(4) . . ? C153 H153a 1.00(4) . . ? C153 H153b .96(4) . . ? O153 H153 .75(3) . . ? C16 H16a .92(3) . . ? C16 H16b .92(3) . . ? C01 O01 1.162(3) . . ? C02 O02 1.171(4) . . ? C03 O03 1.170(3) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Cr C111 3.408(2) . . ? Cr C12 2.699(2) . . ? Cr C131 3.413(3) . . ? Cr C14 2.693(2) . . ? Cr C151 3.405(3) . . ? Cr C16 2.696(2) . . ? Cr O01 2.978(2) . . ? Cr O02 2.981(3) . . ? Cr O03 2.979(2) . . ? Cr H12a 3.04(3) . . ? Cr H14a 2.98(2) . . ? Cr H16a 3.05(3) . . ? N11 C112 2.493(3) . . ? N11 N13 2.306(3) . . ? N11 C14 2.775(3) . . ? N11 N15 2.302(3) . . ? N11 H111a 2.05(2) . . ? N11 H111b 2.00(3) . . ? N11 H112a 2.78(3) . . ? N11 H112b 2.65(3) . . ? N11 H12a 2.04(3) . . ? N11 H12b 2.12(3) . . ? N11 H16a 1.98(3) . . ? N11 H16b 2.05(3) . . ? C111 C113 2.494(4) . . ? C111 O113 2.862(4) . . ? C111 C12 2.446(4) . . ? C111 C16 2.454(4) . . ? C111 H112a 2.11(3) . . ? C111 H112b 2.10(3) . . ? C111 H113a 2.68(3) . . ? C111 H12a 2.60(3) . . ? C111 H16a 2.57(3) . . ? C112 O113 2.369(3) . . ? C112 H111a 2.11(2) . . ? C112 H111b 2.06(3) . . ? C112 H113a 2.07(3) . . ? C112 H113b 2.05(3) . . ? C113 H111a 2.63(3) . . ? C113 H112a 2.14(3) . . ? C113 H112b 2.07(3) . . ? C113 H113 1.80(4) . . ? O113 O133 2.683(3) . 3_656 ? O113 O153 2.713(3) . 2_546 ? O113 H111a 2.47(3) . . ? O113 H112b 2.61(3) . . ? O113 H113a 1.95(3) . . ? O113 H113b 1.90(3) . . ? O113 H153 1.97(3) . 2_546 ? C12 C131 2.458(4) . . ? C12 C14 2.408(4) . . ? C12 N15 2.772(3) . . ? C12 C16 2.385(4) . . ? C12 H111b 2.50(3) . . ? C12 H131a 2.59(3) . . ? C12 H14b 2.58(3) . . ? C12 H16b 2.64(4) . . ? N13 C132 2.494(4) . . ? N13 N15 2.307(3) . . ? N13 C16 2.762(4) . . ? N13 H12a 2.04(3) . . ? N13 H12b 2.09(2) . . ? N13 H131a 1.99(3) . . ? N13 H131b 1.99(3) . . ? N13 H132a 2.69(3) . . ? N13 H132b 2.72(3) . . ? N13 H14a 1.95(3) . . ? N13 H14b 2.07(3) . . ? C131 C133 2.488(5) . . ? C131 O133 2.982(4) . . ? C131 C14 2.448(4) . . ? C131 H12a 2.60(3) . . ? C131 H132a 2.00(3) . . ? C131 H132b 2.08(3) . . ? C131 H133a 2.66(3) . . ? C131 H14a 2.53(3) . . ? C132 O133 2.380(4) . . ? C132 H131a 2.01(2) . . ? C132 H131b 2.02(3) . . ? C132 H133a 2.11(3) . . ? C132 H133b 2.07(4) . . ? C133 H131a 2.60(3) . . ? C133 H131b 2.69(3) . . ? C133 H132a 2.06(3) . . ? C133 H132b 2.01(3) . . ? C133 H133 1.81(3) . . ? O133 O153 2.635(3) . 3_666 ? O133 H113 1.99(4) . 3_656 ? O133 H131a 2.64(3) . . ? O133 H132b 2.46(3) . . ? O133 H133a 1.95(3) . . ? O133 H133b 1.92(3) . . ? O133 H16a 2.78(3) . 4_554 ? C14 C151 2.487(5) . . ? C14 C16 2.385(4) . . ? C14 H12b 2.61(3) . . ? C14 H131b 2.51(3) . . ? C14 H16b 2.64(3) . . ? N15 C152 2.513(4) . . ? N15 H14a 1.99(3) . . ? N15 H14b 2.09(3) . . ? N15 H151a 2.07(3) . . ? N15 H151b 2.21(4) . . ? N15 H152a 2.70(4) . . ? N15 H16a 1.99(3) . . ? N15 H16b 2.03(3) . . ? C151 C153 2.478(5) . . ? C151 O153 2.889(4) . . ? C151 C16 2.405(4) . . ? C151 H14a 2.67(3) . . ? C151 H152a 2.21(4) . . ? C151 H152b 2.21(5) . . ? C151 H153a 2.66(4) . . ? C151 H16a 2.51(3) . . ? C151 H16b 2.69(3) . . ? C152 O153 2.452(4) . . ? C152 H151a 2.03(3) . . ? C152 H151b 1.72(3) . . ? C152 H153a 2.12(4) . . ? C152 H153b 2.08(4) . . ? C153 H151b 2.13(3) . . ? C153 H152a 2.21(5) . . ? C153 H152b 2.27(6) . . ? C153 H153 1.81(3) . . ? O153 H133 1.93(4) . 3_666 ? O153 H151a 2.62(3) . . ? O153 H151b 2.76(3) . . ? O153 H153a 1.86(3) . . ? O153 H153b 1.95(3) . . ? O153 H16a 2.71(3) . 2_556 ? C16 H111a 2.60(2) . . ? C16 H12b 2.61(3) . . ? C16 H14b 2.58(3) . . ? C16 H151a 2.65(3) . . ? C01 C02 2.497(4) . . ? C01 C03 2.518(4) . . ? O01 H111a 2.55(2) . 4_454 ? O01 H111b 2.52(3) . 2 ? C02 C03 2.482(4) . . ? O03 H14a 2.63(3) . 2_545 ? O03 H14b 2.61(3) . 4_454 ? H111a H111b 1.58(4) . . ? H111b H112a 2.37(4) . . ? H111b H12a 2.27(4) . . ? H112a H112b 1.57(4) . . ? H112b H113b 2.32(4) . . ? H112b H16a 2.20(4) . . ? H113a H113b 1.63(5) . . ? H113a H113 2.16(5) . . ? H113b H113 2.06(5) . . ? H113 H153 2.37(5) . 2_546 ? H12a H12b 1.72(3) . . ? H12a H132b 2.19(4) . . ? H12b H14b 2.35(4) . . ? H131a H131b 1.49(4) . . ? H131b H132a 2.26(4) . . ? H131b H14a 2.24(4) . . ? H132a H132b 1.54(4) . . ? H132a H133b 2.33(5) . . ? H132b H133b 2.34(5) . . ? H133a H133b 1.58(4) . . ? H133a H133 2.01(4) . . ? H133b H133 2.34(4) . . ? H14a H14b 1.65(4) . . ? H14a H152b 2.31(6) . . ? H151a H151b 1.78(4) . . ? H151b H152a 2.21(6) . . ? H151b H153a 1.92(5) . . ? H152a H152b 1.78(6) . . ? H153a H153b 1.66(5) . . ? H153a H153 1.88(4) . . ? H16a H16b 1.41(4) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC N11 Cr N13 63.13(7) . . . ? N11 Cr N15 63.08(7) . . . ? N11 Cr C01 163.33(9) . . . ? N11 Cr C02 103.98(10) . . . ? N11 Cr C03 105.00(9) . . . ? N13 Cr N15 63.17(8) . . . ? N13 Cr C01 103.94(10) . . . ? N13 Cr C02 164.82(10) . . . ? N13 Cr C03 104.10(10) . . . ? N15 Cr C01 102.34(9) . . . ? N15 Cr C02 104.59(11) . . . ? N15 Cr C03 165.09(9) . . . ? C01 Cr C02 87.01(12) . . . ? C01 Cr C03 87.92(11) . . . ? C02 Cr C03 86.54(12) . . . ? Cr N11 C111 134.67(13) . . . ? Cr N11 C12 92.54(12) . . . ? Cr N11 C16 92.44(13) . . . ? C111 N11 C12 112.22(19) . . . ? C111 N11 C16 112.8(2) . . . ? C12 N11 C16 108.73(18) . . . ? N11 C111 C112 112.8(2) . . . ? N11 C111 H111a 109.0(14) . . . ? N11 C111 H111b 108.1(17) . . . ? C112 C111 H111a 111.0(16) . . . ? C112 C111 H111b 110.1(16) . . . ? H111a C111 H111b 106(2) . . . ? C111 C112 C113 111.2(2) . . . ? C111 C112 H112a 109.7(19) . . . ? C111 C112 H112b 112.8(17) . . . ? C113 C112 H112a 111.8(16) . . . ? C113 C112 H112b 110.3(18) . . . ? H112a C112 H112b 101(2) . . . ? C112 C113 O113 107.6(2) . . . ? C112 C113 H113a 111.1(18) . . . ? C112 C113 H113b 110.9(18) . . . ? O113 C113 H113a 107.1(16) . . . ? O113 C113 H113b 104.4(18) . . . ? H113a C113 H113b 115(3) . . . ? C113 O113 H113 110(3) . . . ? N11 C12 N13 103.31(18) . . . ? N11 C12 H12a 108.8(15) . . . ? N11 C12 H12b 113.8(17) . . . ? N13 C12 H12a 107.9(14) . . . ? N13 C12 H12b 110.7(14) . . . ? H12a C12 H12b 112(2) . . . ? Cr N13 C12 92.21(13) . . . ? Cr N13 C131 134.99(14) . . . ? Cr N13 C14 91.86(14) . . . ? C12 N13 C131 112.9(2) . . . ? C12 N13 C14 109.51(19) . . . ? C131 N13 C14 112.04(19) . . . ? N13 C131 C132 113.5(2) . . . ? N13 C131 H131a 110.1(19) . . . ? N13 C131 H131b 109(2) . . . ? C132 C131 H131a 109.4(19) . . . ? C132 C131 H131b 108.9(18) . . . ? H131a C131 H131b 106(2) . . . ? C131 C132 C133 110.5(2) . . . ? C131 C132 H132a 107(2) . . . ? C131 C132 H132b 113.5(17) . . . ? C133 C132 H132a 111(2) . . . ? C133 C132 H132b 106(2) . . . ? H132a C132 H132b 108(2) . . . ? C132 C133 O133 108.3(3) . . . ? C132 C133 H133a 114(2) . . . ? C132 C133 H133b 110(2) . . . ? O133 C133 H133a 108.6(16) . . . ? O133 C133 H133b 106(2) . . . ? H133a C133 H133b 110(3) . . . ? C133 O133 H133 112(3) . . . ? N13 C14 N15 103.41(18) . . . ? N13 C14 H14a 106.3(16) . . . ? N13 C14 H14b 110(2) . . . ? N15 C14 H14a 110.5(16) . . . ? N15 C14 H14b 112(2) . . . ? H14a C14 H14b 114(2) . . . ? Cr N15 C14 92.35(14) . . . ? Cr N15 C151 134.46(15) . . . ? Cr N15 C16 92.59(13) . . . ? C14 N15 C151 115.2(2) . . . ? C14 N15 C16 109.2(2) . . . ? C151 N15 C16 109.6(2) . . . ? N15 C151 C152 114.7(2) . . . ? N15 C151 H151a 113(2) . . . ? N15 C151 H151b 116.8(16) . . . ? C152 C151 H151a 107.9(18) . . . ? C152 C151 H151b 81.1(15) . . . ? H151a C151 H151b 118(3) . . . ? C151 C152 C153 109.8(3) . . . ? C151 C152 H152a 112(2) . . . ? C151 C152 H152b 111(2) . . . ? C153 C152 H152a 110(2) . . . ? C153 C152 H152b 114(3) . . . ? H152a C152 H152b 100(3) . . . ? C152 C153 O153 111.9(2) . . . ? C152 C153 H153a 113(2) . . . ? C152 C153 H153b 111(3) . . . ? O153 C153 H153a 98.0(19) . . . ? O153 C153 H153b 107(2) . . . ? H153a C153 H153b 115(3) . . . ? C153 O153 H153 108(2) . . . ? N11 C16 N15 103.63(19) . . . ? N11 C16 H16a 110.2(18) . . . ? N11 C16 H16b 117(2) . . . ? N15 C16 H16a 111.0(18) . . . ? N15 C16 H16b 115.4(18) . . . ? H16a C16 H16b 100(3) . . . ? Cr C01 O01 177.4(2) . . . ? Cr C02 O02 176.6(3) . . . ? Cr C03 O03 176.4(2) . . . ? _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? data_dbmvb4 _audit_creation_date 98-06-25 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common [Cr(CO)3(thetach)] #ActaC _chemical_formula_analytical C12_H21_Cr_N3_O6 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural [(C9_H21_N3_O3)_Cr_(CO)3] #ActaC _chemical_formula_sum C12_H21_Cr_N3_O6 #ActaC _chemical_formula_weight 355.31 #ActaC _chemical_melting_point 130 #ActaC _computing_data_collection 'Bruker SMART software' #ActaC _computing_cell_refinement 'Bruker SAINT software' #ActaC _computing_data_reduction 'Bruker SAINT software' #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 12.8160(9) #ActaC _cell_length_b 15.0260(10) #ActaC _cell_length_c 16.4780(10) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 92.0870(10) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 3171.1(4) #ActaC _cell_formula_units_Z 8 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 4059 #ActaC _cell_measurement_theta_min 1 #ActaC _cell_measurement_theta_max 29 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21_1 #ActaC _symmetry_space_group_name_Hall p_2yb #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,1/2+y,-z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour orange #ActaC _exptl_crystal_size_max 0.18 #ActaC _exptl_crystal_size_mid 0.17 #ActaC _exptl_crystal_size_min 0.07 #ActaC _exptl_crystal_density_diffrn 1.488 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 1488 #ActaC _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_coefficient_mu 0.75 #ActaC _exptl_absorpt_correction_type 'multi scan' #ActaC _exptl_absorpt_correction_T_min 0.71 #ActaC _exptl_absorpt_correction_T_max 0.89 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'CCD area detector' #ActaC _diffrn_measurement_device 'Bruker CCD diffractometer' #ActaC _diffrn_measurement_method 'omega scans' #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 27676 #ActaC _diffrn_reflns_av_R_equivalents 0.0232 #ActaC _diffrn_reflns_av_sigmaI/netI .175 #ActaC _diffrn_reflns_limit_h_min -17 #ActaC _diffrn_reflns_limit_h_max 17 #ActaC _diffrn_reflns_limit_k_min -20 #ActaC _diffrn_reflns_limit_k_max 20 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 22 #ActaC _diffrn_reflns_theta_min 1.24 #ActaC _diffrn_reflns_theta_max 29.13 #ActaC _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 96 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 168 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cr ? 0 8 .284 .624 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 24 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 48 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Cr1 .20383(12) 1.00000 .62284(9) .0346(9) Uani ? ? Cr2 .26808(12) .52073(14) .64004(10) .0387(10) Uani ? ? Cr3 .75592(12) .50164(16) -.11208(9) .0348(9) Uani ? ? Cr4 .29955(12) .52901(13) .13392(9) .0304(8) Uani ? ? N11 .0987(7) 1.0850(6) .5499(5) .031(5) Uani ? ? C111 .0917(9) 1.1832(8) .5383(7) .044(7) Uani ? ? C112 .1828(9) 1.2254(8) .4974(8) .052(7) Uani ? ? O112 .1790(7) 1.2117(6) .4118(5) .065(6) Uani ? ? C12 .1121(8) 1.0336(8) .4761(6) .039(5) Uani ? ? N13 .1398(7) .9441(6) .5076(5) .040(5) Uani ? ? C131 .1821(10) .8834(8) .4458(7) .053(7) Uani ? ? C132 .2963(13) .8966(11) .4348(11) .099(12) Uani ? ? O132 .3220(12) .8340(10) .3763(10) .167(14) Uani ? ? C14 .0525(9) .9054(7) .5479(6) .040(6) Uani ? ? N15 .0385(7) .9618(6) .6185(5) .037(5) Uani ? ? C151 -.0330(9) .9263(7) .6782(7) .055(7) Uani ? ? C152 .0087(10) .8445(7) .7230(7) .052(7) Uani ? ? O152 -.0086(9) .7683(6) .6754(6) .077(7) Uani ? ? C16 .0068(8) 1.0524(7) .5909(7) .040(6) Uani ? ? C101 .2679(9) .9089(8) .6751(7) .044(7) Uani ? ? O101 .3126(7) .8526(7) .7121(6) .066(6) Uani ? ? C102 .2168(9) 1.0615(8) .7162(7) .047(7) Uani ? ? O102 .2320(9) 1.0984(7) .7780(6) .085(7) Uani ? ? C103 .3325(10) 1.0380(8) .5981(7) .048(7) Uani ? ? O103 .4181(7) 1.0627(7) .5876(6) .077(7) Uani ? ? N21 .3757(8) .4369(7) .7120(6) .045(6) Uani ? ? C211 .3846(12) .3378(9) .7232(10) .072(10) Uani ? ? C212 .3788(14) .2906(10) .6545(12) .095(12) Uani ? ? O212 .4800(11) .2928(9) .6174(8) .129(11) Uani ? ? C22 .4662(9) .4811(9) .6781(8) .055(8) Uani ? ? N23 .4266(7) .5698(6) .6588(6) .044(5) Uani ? ? C231 .4985(10) .6199(9) .6089(9) .066(9) Uani ? ? C232 .4495(12) .7025(12) .5717(10) .094(12) Uani ? ? O232 .5221(10) .7589(8) .5446(7) .106(9) Uani ? ? C24 .3997(11) .6157(8) .7354(8) .058(8) Uani ? ? N25 .3133(8) .5651(7) .7649(6) .054(7) Uani ? ? C251 .2570(14) .6095(13) .8319(9) .094(12) Uani ? ? C252 .1760(14) .6663(13) .8079(10) .095(12) Uani ? ? O252 .0951(7) .6340(6) .7620(5) .052(5) Uani ? ? C26 .3498(10) .4755(9) .7886(7) .054(8) Uani ? ? C201 .2012(9) .6142(9) .5914(7) .047(7) Uani ? ? O201 .1582(8) .6716(7) .5551(6) .076(7) Uani ? ? C202 .1479(10) .4582(8) .6476(6) .044(7) Uani ? ? O202 .0715(7) .4153(7) .6490(5) .071(6) Uani ? ? C203 .2684(10) .4758(8) .5383(8) .048(7) Uani ? ? O203 .2624(9) .4501(7) .4715(6) .077(7) Uani ? ? N31 .8134(6) .4555(6) .0093(5) .032(5) Uani ? ? C311 .7655(9) .4167(8) .0815(7) .044(7) Uani ? ? C312 .6790(9) .3498(7) .0590(7) .043(6) Uani ? ? O312 .5914(6) .3935(6) .0224(5) .048(5) Uani ? ? C32 .8906(9) .3980(8) -.0286(7) .041(6) Uani ? ? N33 .9085(7) .4413(6) -.1055(5) .039(5) Uani ? ? C331 .9489(9) .3850(8) -.1713(7) .054(7) Uani ? ? C332 1.0415(10) .3296(9) -.1507(8) .064(8) Uani ? ? O332 1.1237(7) .3820(6) -.1207(6) .076(6) Uani ? ? C34 .9606(8) .5277(8) -.0907(6) .044(6) Uani ? ? N35 .8793(7) .5810(6) -.0531(5) .039(5) Uani ? ? C351 .8996(11) .6770(8) -.0530(8) .055(7) Uani ? ? C352 .8032(9) .7361(6) -.0429(7) .050(7) Uani ? ? O352 .7719(6) .7339(5) .0371(5) .054(5) Uani ? ? C36 .8598(8) .5433(8) .0278(7) .041(6) Uani ? ? C301 .7528(9) .5457(8) -.2153(7) .050(7) Uani ? ? O301 .7438(9) .5717(7) -.2816(6) .085(7) Uani ? ? C302 .6341(9) .5606(8) -.0978(6) .042(7) Uani ? ? O302 .5556(7) .5991(7) -.0957(5) .074(6) Uani ? ? C303 .6803(9) .4099(8) -.1554(7) .043(7) Uani ? ? O303 .6335(8) .3532(6) -.1874(6) .069(6) Uani ? ? N41 .3299(7) .5755(6) .2603(5) .035(5) Uani ? ? C411 .2663(10) .6217(7) .3215(7) .046(6) Uani ? ? C412 .1892(11) .6869(8) .2838(8) .058(8) Uani ? ? O412 .1085(8) .6446(7) .2441(7) .084(7) Uani ? ? C42 .3638(8) .4858(7) .2880(6) .033(5) Uani ? ? N43 .4009(7) .4470(6) .2130(5) .033(5) Uani ? ? C431 .4188(9) .3481(8) .2154(7) .042(6) Uani ? ? C432 .3314(9) .2960(7) .2444(7) .050(7) Uani ? ? O432 .3338(7) .2977(5) .3321(5) .064(6) Uani ? ? C44 .4948(7) .4930(7) .1868(6) .035(5) Uani ? ? N45 .4551(6) .5821(5) .1635(5) .033(5) Uani ? ? C451 .5314(8) .6347(7) .1175(7) .045(6) Uani ? ? C452 .4794(8) .7039(7) .0651(7) .046(6) Uani ? ? O452 .5583(6) .7621(5) .0383(6) .065(5) Uani ? ? C46 .4209(9) .6284(7) .2362(6) .040(6) Uani ? ? C401 .3195(8) .4766(7) .0368(6) .042(6) Uani ? ? O401 .3283(7) .4410(6) -.0255(5) .068(6) Uani ? ? C402 .2332(8) .6174(7) .0776(7) .040(6) Uani ? ? O402 .1864(7) .6696(6) .0375(5) .062(6) Uani ? ? C403 .1733(8) .4739(7) .1302(6) .033(5) Uani ? ? O403 .0920(6) .4423(6) .1219(5) .055(5) Uani ? ? H111a .08448 1.21135 .59089 .05700 Uiso ? ? H111b .02855 1.19819 .50667 .05700 Uiso ? ? H112a .24575 1.20083 .51967 .06100 Uiso ? ? H112b .18409 1.28905 .50808 .06100 Uiso ? ? H12a .16645 1.05871 .44361 .05100 Uiso ? ? H12b .04937 1.03225 .44152 .05100 Uiso ? ? H131a .14692 .89483 .39389 .06800 Uiso ? ? H131b .17002 .82434 .46094 .06800 Uiso ? ? H132a .33316 .88691 .48623 .13700 Uiso ? ? H132b .31009 .95681 .41865 .13700 Uiso ? ? H14a .06559 .84540 .56241 .05100 Uiso ? ? H14b -.01027 .90586 .51179 .05100 Uiso ? ? H151a -.09954 .91227 .65084 .07300 Uiso ? ? H151b -.04931 .97390 .71692 .07300 Uiso ? ? H152a -.02204 .83735 .77391 .06500 Uiso ? ? H152b .08396 .85350 .73375 .06500 Uiso ? ? H152 .03531 .71895 .68849 .11000 Uiso ? ? H16a -.00685 1.09076 .63816 .05700 Uiso ? ? H16b -.05474 1.05260 .55763 .05700 Uiso ? ? H211a .32991 .32056 .75879 .08700 Uiso ? ? H211b .44991 .32636 .75053 .08700 Uiso ? ? H212a .32391 .31792 .62022 .11700 Uiso ? ? H212b .35809 .23244 .66681 .11700 Uiso ? ? H212 .50896 .26633 .56865 .19000 Uiso ? ? H22a .48824 .45169 .62958 .07200 Uiso ? ? H22b .52608 .48274 .71548 .07200 Uiso ? ? H231a .51961 .58125 .56484 .08200 Uiso ? ? H231b .56010 .63680 .63884 .08200 Uiso ? ? H232a .40904 .73453 .61011 .12600 Uiso ? ? H232b .40080 .68802 .52606 .12600 Uiso ? ? H232 .51429 .72087 .48529 .15600 Uiso ? ? H24a .38152 .67886 .72545 .06800 Uiso ? ? H24b .45837 .61782 .77451 .06800 Uiso ? ? H251a .30740 .64289 .86625 .11100 Uiso ? ? H251b .22759 .56526 .86615 .11100 Uiso ? ? H252a .20861 .71531 .77756 .11100 Uiso ? ? H252b .14862 .69454 .85543 .11100 Uiso ? ? H252 .11837 .60857 .72059 .07700 Uiso ? ? H26a .29313 .44253 .81404 .06700 Uiso ? ? H26b .40630 .47747 .82783 .06700 Uiso ? ? H311a .73710 .46543 .11280 .05800 Uiso ? ? H311b .82011 .39025 .11460 .05800 Uiso ? ? H312a .65789 .31811 .10588 .05900 Uiso ? ? H312b .70515 .30661 .02118 .05900 Uiso ? ? H312 .62815 .41582 -.02941 .07400 Uiso ? ? H32a .86255 .33896 -.03823 .05800 Uiso ? ? H32b .95280 .39186 .00451 .05800 Uiso ? ? H331a .96630 .42218 -.21624 .07300 Uiso ? ? H331b .89268 .34656 -.18943 .07300 Uiso ? ? H332a 1.06095 .29737 -.19706 .07900 Uiso ? ? H332b 1.02165 .28760 -.10955 .07900 Uiso ? ? H332 1.17369 .33120 -.08943 .11400 Uiso ? ? H34a .98421 .55530 -.13913 .05700 Uiso ? ? H34b 1.02183 .52224 -.05381 .05700 Uiso ? ? H351a .93048 .69394 -.10424 .06900 Uiso ? ? H351b .94979 .69313 -.01077 .06900 Uiso ? ? H352a .74670 .71556 -.07820 .06300 Uiso ? ? H352b .81669 .79753 -.05837 .06300 Uiso ? ? H352 .72830 .75788 .05996 .08000 Uiso ? ? H36a .81441 .58195 .05742 .04900 Uiso ? ? H36b .92466 .53921 .05932 .04900 Uiso ? ? H411a .31047 .65323 .36100 .06200 Uiso ? ? H411b .22680 .57907 .35092 .06200 Uiso ? ? H412a .22548 .72454 .24575 .07600 Uiso ? ? H412b .16317 .72724 .32470 .07600 Uiso ? ? H412 .03762 .63858 .26178 .10000 Uiso ? ? H42a .30584 .45429 .30931 .04500 Uiso ? ? H42b .41728 .48980 .33017 .04500 Uiso ? ? H431a .47725 .33709 .25279 .05100 Uiso ? ? H431b .43605 .32833 .16345 .05100 Uiso ? ? H432a .33496 .23722 .22457 .06500 Uiso ? ? H432b .26725 .32282 .22232 .06500 Uiso ? ? H432 .28017 .25772 .34236 .09700 Uiso ? ? H44a .52593 .46376 .14119 .04600 Uiso ? ? H44b .54902 .49549 .22960 .04600 Uiso ? ? H451a .56891 .59512 .08416 .05700 Uiso ? ? H451b .58029 .66401 .15406 .05700 Uiso ? ? H452a .42865 .73581 .09465 .05900 Uiso ? ? H452b .44413 .67636 .01905 .05900 Uiso ? ? H452 .51349 .82100 .02796 .09600 Uiso ? ? H46a .40146 .68950 .22431 .04700 Uiso ? ? H46b .47429 .62970 .27819 .04700 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Cr1 .0369(9) .0330(9) .0336(9) .0032(8) -.0040(7) -.0021(8) Cr2 .0392(10) .0386(11) .0376(9) .0047(9) -.0080(7) -.0020(8) Cr3 .0382(9) .0329(9) .0331(9) .0002(8) -.0028(6) .0017(8) Cr4 .0335(8) .0274(8) .0303(8) -.0018(7) -.0003(6) .0023(7) N11 .030(5) .023(4) .040(5) .001(3) .004(4) .002(4) C111 .050(7) .032(6) .050(7) .004(5) .000(5) .003(5) C112 .045(7) .040(7) .070(9) -.008(5) -.006(6) .000(6) O112 .074(6) .062(5) .059(6) .002(4) .021(4) .015(4) C12 .045(6) .042(6) .030(5) -.011(5) -.000(4) -.001(5) N13 .048(6) .034(5) .037(5) .002(4) .003(4) -.003(4) C131 .065(8) .050(7) .045(7) -.001(6) .011(6) -.012(5) C132 .089(12) .074(11) .136(15) .002(9) .056(11) -.057(10) O132 .152(14) .144(12) .211(16) -.030(10) .099(12) -.089(12) C14 .045(6) .037(6) .037(6) -.005(5) -.000(5) -.002(5) N15 .039(5) .031(4) .040(5) .003(4) .003(4) .002(4) C151 .061(8) .044(6) .061(8) .010(5) .024(6) .012(5) C152 .069(8) .040(6) .047(7) .003(5) .013(6) .007(5) O152 .114(9) .038(5) .076(7) .001(5) -.025(6) .007(5) C16 .039(6) .033(6) .050(7) .009(4) .007(5) .005(4) C101 .037(6) .049(7) .045(7) -.000(5) .001(5) .005(6) O101 .065(6) .060(6) .073(7) .009(5) -.014(5) .016(5) C102 .054(7) .047(7) .039(7) -.004(5) -.004(5) .002(5) O102 .113(9) .091(8) .050(6) -.009(6) -.016(5) -.026(5) C103 .063(8) .038(6) .042(6) -.002(6) -.014(5) -.002(5) O103 .047(6) .101(8) .082(7) -.014(5) -.008(5) .014(6) N21 .038(6) .048(6) .048(6) .001(4) -.011(4) .002(5) C211 .079(11) .033(7) .100(12) .012(7) -.030(8) .001(8) C212 .094(13) .065(10) .123(15) .013(9) -.027(11) .010(10) O212 .140(13) .127(11) .123(10) -.031(9) .040(9) -.052(8) C22 .037(7) .056(8) .073(9) .012(5) -.005(6) -.004(6) N23 .046(6) .034(5) .051(6) .004(4) -.007(4) .005(4) C231 .049(8) .060(8) .090(10) -.012(6) -.008(7) .020(7) C232 .069(10) .107(13) .107(13) -.014(9) -.004(9) .063(11) O232 .121(11) .091(8) .107(9) -.026(7) -.004(8) .019(7) C24 .069(9) .042(7) .060(8) .015(6) -.032(7) -.017(6) N25 .051(7) .065(7) .045(6) .004(5) -.013(5) -.009(5) C251 .113(14) .118(15) .050(9) .052(11) -.017(8) -.038(9) C252 .094(13) .118(15) .072(11) .030(11) .010(9) -.052(10) O252 .057(5) .053(5) .047(5) .009(4) .002(4) .002(4) C26 .050(8) .064(9) .046(7) .013(6) -.015(5) .004(6) C201 .043(7) .049(7) .050(7) -.003(5) -.003(5) -.000(6) O201 .077(7) .055(6) .093(7) .014(5) -.024(5) .028(5) C202 .051(8) .051(7) .029(6) .013(6) -.008(5) -.000(5) O202 .048(6) .098(8) .065(6) -.024(5) -.008(4) .012(5) C203 .062(8) .032(6) .049(8) -.007(5) -.003(6) .000(5) O203 .127(9) .065(6) .039(5) -.009(6) -.002(5) -.004(5) N31 .031(5) .035(5) .029(5) -.000(4) -.001(3) .003(4) C311 .047(7) .043(7) .041(7) .000(5) -.002(5) -.001(5) C312 .054(7) .024(5) .052(7) .004(4) .005(5) .003(5) O312 .039(4) .054(5) .053(5) -.006(4) .011(4) -.003(4) C32 .036(7) .043(6) .045(7) .001(5) -.005(5) .003(5) N33 .038(5) .036(5) .044(5) .001(4) .004(4) .001(4) C331 .054(7) .063(8) .047(7) -.006(6) .007(5) -.013(6) C332 .056(8) .068(9) .067(9) .008(6) .006(6) -.005(7) O332 .055(6) .078(6) .095(7) .003(5) -.008(5) .001(5) C34 .034(5) .058(7) .042(6) -.001(5) .006(4) .006(5) N35 .043(5) .035(5) .039(5) -.007(4) .005(4) .002(4) C351 .063(8) .034(6) .067(8) -.019(6) .013(6) -.008(6) C352 .065(8) .022(5) .063(8) .003(5) -.007(6) .008(5) O352 .060(5) .047(4) .056(5) .014(4) .007(4) .003(4) C36 .031(6) .050(7) .042(6) -.001(5) -.005(4) -.010(5) C301 .059(7) .040(7) .050(7) .003(5) -.002(5) .001(5) O301 .119(9) .089(8) .046(6) .014(6) .001(5) .028(5) C302 .046(7) .046(7) .033(6) .005(5) -.010(5) .001(5) O302 .055(6) .100(8) .066(6) .032(5) -.012(4) -.019(5) C303 .054(7) .040(7) .035(6) .001(5) -.006(5) .007(5) O303 .082(7) .058(6) .064(6) -.019(5) -.024(5) -.006(5) N41 .044(5) .029(4) .031(5) -.005(4) .003(4) .001(4) C411 .071(8) .031(6) .037(6) -.002(5) .017(6) -.009(5) C412 .065(8) .036(6) .076(9) .004(5) .020(7) .011(6) O412 .059(6) .082(7) .111(9) .007(5) .022(6) .008(6) C42 .043(6) .030(5) .026(5) .004(4) -.002(4) -.000(4) N43 .034(5) .036(5) .030(5) .002(4) .004(4) .004(4) C431 .043(7) .032(6) .051(7) .007(5) .010(5) .005(5) C432 .065(8) .032(6) .053(8) -.006(5) .007(6) .006(5) O432 .084(6) .049(5) .060(6) -.013(4) .017(5) .015(4) C44 .033(5) .030(5) .041(5) .006(4) -.000(4) .005(4) N45 .034(5) .032(4) .034(5) .004(3) .004(4) .003(4) C451 .038(6) .040(6) .056(7) .001(4) .010(5) .010(5) C452 .043(6) .046(6) .049(7) .003(5) .009(5) .011(5) O452 .039(5) .044(4) .112(7) -.000(3) .019(5) .040(5) C46 .052(7) .027(5) .041(6) -.001(5) -.003(5) -.005(4) C401 .046(6) .042(6) .039(6) -.002(5) .004(5) .004(5) O401 .092(7) .072(6) .041(5) .002(5) .002(5) -.013(4) C402 .039(6) .033(6) .048(7) -.003(5) -.002(5) .005(5) O402 .065(6) .049(5) .072(6) .015(4) -.008(5) .022(5) C403 .034(6) .033(5) .032(5) .001(4) .000(4) .003(4) O403 .045(5) .064(5) .058(5) -.014(4) -.002(4) -.000(4) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 3121(196) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details Flack_xabs_refined #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 4222.5 #ActaC _refine_ls_number_parameters 794 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .113 #ActaC _refine_ls_R_factor_obs .051 #ActaC _refine_ls_wR_factor_all .103 #ActaC _refine_ls_wR_factor_obs .053 #ActaC _refine_ls_goodness_of_fit_all 3.887 #ActaC _refine_ls_goodness_of_fit_obs 2.781 #ActaC _refine_ls_shift/esd_max .049 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -.402 #ActaC _refine_diff_density_max .737 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Cr1 N11 2.185(8) . . ? Cr1 N13 2.208(9) . . ? Cr1 N15 2.194(9) . . ? Cr1 C101 1.799(12) . . ? Cr1 C102 1.797(12) . . ? Cr1 C103 1.806(13) . . ? Cr2 N21 2.186(10) . . ? Cr2 N23 2.173(10) . . ? Cr2 N25 2.219(10) . . ? Cr2 C201 1.817(13) . . ? Cr2 C202 1.812(12) . . ? Cr2 C203 1.808(13) . . ? Cr3 N31 2.218(8) . . ? Cr3 N33 2.155(9) . . ? Cr3 N35 2.181(9) . . ? Cr3 C301 1.824(12) . . ? Cr3 C302 1.818(12) . . ? Cr3 C303 1.817(12) . . ? Cr4 N41 2.217(9) . . ? Cr4 N43 2.186(9) . . ? Cr4 N45 2.185(8) . . ? Cr4 C401 1.809(11) . . ? Cr4 C402 1.814(11) . . ? Cr4 C403 1.816(10) . . ? N11 C111 1.490(15) . . ? N11 C12 1.456(13) . . ? N11 C16 1.462(14) . . ? C111 C112 1.510(17) . . ? C111 H111a .972(12) . . ? C111 H111b .973(12) . . ? C112 O112 1.425(16) . . ? C112 H112a .949(12) . . ? C112 H112b .972(11) . . ? C12 N13 1.481(15) . . ? C12 H12a .970(10) . . ? C12 H12b .968(10) . . ? N13 C131 1.485(15) . . ? N13 C14 1.444(14) . . ? C131 C132 1.49(2) . . ? C131 H131a .967(12) . . ? C131 H131b .936(12) . . ? C132 O132 1.39(2) . . ? C132 H132a .966(18) . . ? C132 H132b .961(17) . . ? C14 N15 1.456(14) . . ? C14 H14a .947(11) . . ? C14 H14b .983(11) . . ? N15 C151 1.468(15) . . ? N15 C16 1.488(13) . . ? C151 C152 1.522(16) . . ? C151 H151a .973(12) . . ? C151 H151b .986(12) . . ? C152 O152 1.401(14) . . ? C152 H152a .945(12) . . ? C152 H152b .984(12) . . ? O152 H152 .951(10) . . ? C16 H16a .989(11) . . ? C16 H16b .944(11) . . ? C101 O101 1.178(15) . . ? C102 O102 1.169(16) . . ? C103 O103 1.177(16) . . ? N21 C211 1.503(18) . . ? N21 C22 1.465(16) . . ? N21 C26 1.440(16) . . ? C211 C212 1.34(2) . . ? C211 H211a .966(16) . . ? C211 H211b .952(16) . . ? C212 O212 1.45(2) . . ? C212 H212a .976(18) . . ? C212 H212b .938(16) . . ? O212 H212 .982(14) . . ? C22 N23 1.457(16) . . ? C22 H22a .965(13) . . ? C22 H22b .967(12) . . ? N23 C231 1.465(17) . . ? N23 C24 1.489(16) . . ? C231 C232 1.51(2) . . ? C231 H231a .975(14) . . ? C231 H231b .951(13) . . ? C232 O232 1.35(2) . . ? C232 H232a .962(17) . . ? C232 H232b .984(16) . . ? O232 H232 1.133(12) . . ? C24 N25 1.442(17) . . ? C24 H24a .990(13) . . ? C24 H24b .973(13) . . ? N25 C251 1.50(2) . . ? N25 C26 1.473(17) . . ? C251 C252 1.39(3) . . ? C251 H251a .981(17) . . ? C251 H251b .959(17) . . ? C252 O252 1.35(2) . . ? C252 H252a .991(18) . . ? C252 H252b .968(17) . . ? O252 H252 .845(8) . . ? C26 H26a .985(13) . . ? C26 H26b .954(12) . . ? C201 O201 1.175(16) . . ? C202 O202 1.173(16) . . ? C203 O203 1.166(16) . . ? N31 C311 1.478(14) . . ? N31 C32 1.470(14) . . ? N31 C36 1.475(15) . . ? C311 C312 1.531(16) . . ? C311 H311a .974(11) . . ? C311 H311b .958(11) . . ? C312 O312 1.417(13) . . ? C312 H312a .955(11) . . ? C312 H312b .968(11) . . ? O312 H312 1.046(8) . . ? C32 N33 1.451(15) . . ? C32 H32a .968(12) . . ? C32 H32b .954(11) . . ? N33 C331 1.483(15) . . ? N33 C34 1.477(15) . . ? C331 C332 1.479(18) . . ? C331 H331a .961(12) . . ? C331 H331b .963(12) . . ? C332 O332 1.392(16) . . ? C332 H332a .946(13) . . ? C332 H332b .967(13) . . ? O332 H332 1.111(9) . . ? C34 N35 1.469(14) . . ? C34 H34a .958(11) . . ? C34 H34b .978(10) . . ? N35 C351 1.466(16) . . ? N35 C36 1.478(14) . . ? C351 C352 1.536(17) . . ? C351 H351a .978(13) . . ? C351 H351b .961(13) . . ? C352 O352 1.391(15) . . ? C352 H352a .963(12) . . ? C352 H352b .975(10) . . ? O352 H352 .774(8) . . ? C36 H36a .966(11) . . ? C36 H36b .966(10) . . ? C301 O301 1.162(15) . . ? C302 O302 1.161(15) . . ? C303 O303 1.157(15) . . ? N41 C411 1.491(14) . . ? N41 C42 1.483(14) . . ? N41 C46 1.477(14) . . ? C411 C412 1.509(17) . . ? C411 H411a .971(11) . . ? C411 H411b .959(12) . . ? C412 O412 1.362(16) . . ? C412 H412a .975(13) . . ? C412 H412b .974(13) . . ? O412 H412 .968(10) . . ? C42 N43 1.461(13) . . ? C42 H42a .958(10) . . ? C42 H42b .960(10) . . ? N43 C431 1.504(15) . . ? N43 C44 1.466(13) . . ? C431 C432 1.461(17) . . ? C431 H431a .967(11) . . ? C431 H431b .940(12) . . ? C432 O432 1.445(15) . . ? C432 H432a .943(11) . . ? C432 H432b .974(12) . . ? O432 H432 .933(9) . . ? C44 N45 1.477(13) . . ? C44 H44a .969(10) . . ? C44 H44b .973(9) . . ? N45 C451 1.487(14) . . ? N45 C46 1.467(13) . . ? C451 C452 1.493(15) . . ? C451 H451a .952(11) . . ? C451 H451b .960(11) . . ? C452 O452 1.419(14) . . ? C452 H452a .955(11) . . ? C452 H452b .963(11) . . ? O452 H452 1.066(8) . . ? C46 H46a .969(10) . . ? C46 H46b .956(11) . . ? C401 O401 1.167(14) . . ? C402 O402 1.175(14) . . ? C403 O403 1.149(13) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Cr1 C111 3.382(12) . . ? Cr1 C12 2.698(10) . . ? Cr1 C131 3.406(12) . . ? Cr1 C14 2.671(11) . . ? Cr1 C151 3.387(12) . . ? Cr1 C16 2.679(11) . . ? Cr1 O101 2.976(10) . . ? Cr1 O102 2.964(10) . . ? Cr1 O103 2.980(9) . . ? Cr1 H12a 3.1028(15) . . ? Cr1 H14a 3.0657(10) . . ? Cr1 H16a 3.0436(14) . . ? Cr2 C211 3.393(15) . . ? Cr2 C22 2.661(12) . . ? Cr2 C231 3.363(13) . . ? Cr2 C24 2.675(13) . . ? Cr2 C251 3.439(15) . . ? Cr2 O252 3.489(9) . . ? Cr2 C26 2.714(12) . . ? Cr2 O201 2.990(10) . . ? Cr2 O202 2.984(10) . . ? Cr2 O203 2.971(10) . . ? Cr2 H212a 3.150(2) . . ? Cr2 H22a 3.0170(17) . . ? Cr2 H24a 3.0969(19) . . ? Cr2 H252 2.7149(17) . . ? Cr2 H26a 3.1044(17) . . ? Cr3 C311 3.434(11) . . ? Cr3 O312 3.513(8) . . ? Cr3 C32 2.669(11) . . ? Cr3 C331 3.212(13) . . ? Cr3 C34 2.663(10) . . ? Cr3 C351 3.340(13) . . ? Cr3 C36 2.694(11) . . ? Cr3 O301 2.984(10) . . ? Cr3 O302 2.976(10) . . ? Cr3 O303 2.973(10) . . ? Cr3 H312 2.5223(18) . . ? Cr3 H32a 3.034(2) . . ? Cr3 H34a 3.0829(17) . . ? Cr3 H36a 3.1091(17) . . ? Cr4 C411 3.430(11) . . ? Cr4 O412 3.555(10) . . ? Cr4 C42 2.719(10) . . ? Cr4 C431 3.372(12) . . ? Cr4 C44 2.675(9) . . ? Cr4 C451 3.389(11) . . ? Cr4 C46 2.702(11) . . ? Cr4 O401 2.976(8) . . ? Cr4 O402 2.987(9) . . ? Cr4 O403 2.962(8) . . ? Cr4 H42a 3.0989(15) . . ? Cr4 H44a 3.0607(16) . . ? Cr4 H46a 3.0981(17) . . ? N11 C112 2.537(14) . . ? N11 O112 3.168(12) . . ? N11 N13 2.296(12) . . ? N11 C14 2.762(13) . . ? N11 N15 2.316(12) . . ? N11 H111a 2.026(8) . . ? N11 H111b 2.040(8) . . ? N11 H112a 2.627(8) . . ? N11 H12a 2.022(9) . . ? N11 H12b 2.033(8) . . ? N11 H16a 2.023(9) . . ? N11 H16b 2.034(8) . . ? C111 O112 2.440(15) . . ? C111 C12 2.487(17) . . ? C111 C16 2.421(16) . . ? C111 O201 3.507(16) . 2_556 ? C111 H112a 2.027(12) . . ? C111 H112b 2.056(12) . . ? C111 H12a 2.638(12) . . ? C111 H16a 2.526(12) . . ? C112 O152 3.612(16) . 2_556 ? C112 O203 3.557(16) . 1_565 ? C112 O432 3.567(16) . 1_565 ? C112 H111a 2.037(13) . . ? C112 H111b 2.031(12) . . ? C112 H12a 2.663(12) . . ? O112 C12 3.014(15) . . ? O112 O152 2.707(14) . 2_556 ? O112 O232 3.936(16) . 2_656 ? O112 O203 3.856(14) . 1_565 ? O112 O301 3.187(14) . 2_655 ? O112 C432 3.663(15) . 1_565 ? O112 O432 2.742(13) . 1_565 ? O112 H111a 3.231(9) . . ? O112 H111b 2.535(9) . . ? O112 H112a 1.951(9) . . ? O112 H112b 1.966(9) . . ? O112 H12a 2.364(9) . . ? O112 H12b 3.214(9) . . ? O112 H151a 3.333(9) . 2_556 ? O112 H152 3.156(9) . 2_556 ? O112 H432 1.891(9) . 1_565 ? C12 C131 2.487(17) . . ? C12 C14 2.400(16) . . ? C12 N15 2.780(13) . . ? C12 C16 2.380(15) . . ? C12 O202 3.549(14) . 2_556 ? C12 H131a 2.535(11) . . ? C12 H14b 2.561(11) . . ? C12 H16b 2.582(10) . . ? N13 C132 2.48(2) . . ? N13 O132 3.638(18) . . ? N13 N15 2.296(12) . . ? N13 C16 2.759(14) . . ? N13 H12a 2.055(9) . . ? N13 H12b 2.047(9) . . ? N13 H131a 2.019(9) . . ? N13 H131b 2.000(9) . . ? N13 H132a 2.659(9) . . ? N13 H132b 2.680(9) . . ? N13 H14a 1.995(9) . . ? N13 H14b 2.010(9) . . ? C131 O132 2.29(2) . . ? C131 C14 2.431(16) . . ? C131 O201 3.675(16) . . ? C131 O202 3.587(15) . 2_556 ? C131 H12a 2.642(12) . . ? C131 H132a 2.025(12) . . ? C131 H132b 2.039(12) . . ? C131 H14a 2.542(12) . . ? C132 O212 3.40(2) . 2_656 ? C132 O301 3.67(2) . 2_655 ? C132 H131a 2.007(17) . . ? C132 H131b 2.008(17) . . ? O132 O212 2.61(2) . 2_656 ? O132 C22 3.64(2) . 2_656 ? O132 O232 3.87(2) . . ? O132 O301 3.977(19) . 2_655 ? O132 O303 3.20(2) . 2_655 ? O132 C411 3.386(19) . . ? O132 C412 3.15(2) . . ? O132 H131a 2.450(15) . . ? O132 H131b 2.441(16) . . ? O132 H132a 1.978(16) . . ? O132 H132b 1.980(15) . . ? O132 H212 2.531(15) . 2_656 ? O132 H22a 3.011(15) . 2_656 ? O132 H22b 3.360(16) . 2_656 ? O132 H411a 2.732(15) . . ? O132 H412a 2.945(16) . . ? O132 H412b 2.705(15) . . ? C14 C151 2.465(16) . . ? C14 O152 3.065(14) . . ? C14 C16 2.399(15) . . ? C14 O202 3.563(14) . 2_556 ? C14 H12b 2.588(11) . . ? C14 H131b 2.442(11) . . ? C14 H151a 2.631(11) . . ? C14 H16b 2.611(11) . . ? N15 C152 2.503(14) . . ? N15 O152 3.120(12) . . ? N15 H14a 2.014(8) . . ? N15 H14b 2.028(8) . . ? N15 H151a 2.009(9) . . ? N15 H151b 2.015(9) . . ? N15 H152b 2.551(8) . . ? N15 H16a 2.052(8) . . ? N15 H16b 2.052(8) . . ? C151 O152 2.395(14) . . ? C151 C16 2.444(16) . . ? C151 O412 3.664(15) . 2_556 ? C151 O403 3.416(15) . 2_556 ? C151 H14a 2.625(12) . . ? C151 H152a 2.069(12) . . ? C151 H152b 2.045(12) . . ? C151 H16a 2.582(11) . . ? C152 O252 3.404(14) . . ? C152 O403 3.255(14) . 2_556 ? C152 H151a 2.063(11) . . ? C152 H151b 2.083(11) . . ? C152 H152 2.003(11) . . ? O152 O101 4.329(15) . . ? O152 C252 3.51(2) . . ? O152 O252 2.781(13) . . ? O152 O201 3.305(15) . . ? O152 O432 4.188(14) . 2_556 ? O152 H111b 3.182(9) . 2_546 ? O152 H14a 2.418(10) . . ? O152 H151a 2.483(9) . . ? O152 H151b 3.211(9) . . ? O152 H152a 1.939(9) . . ? O152 H152b 1.972(10) . . ? O152 H252a 3.298(10) . . ? O152 H252 2.979(10) . . ? C16 O201 3.620(15) . 2_556 ? C16 O412 3.433(15) . 2_556 ? C16 H111a 2.587(10) . . ? C16 H111b 2.613(11) . . ? C16 H12b 2.559(11) . . ? C16 H14b 2.565(11) . . ? C16 H151b 2.516(11) . . ? C101 C102 2.485(17) . . ? C101 O102 3.354(16) . . ? C101 C103 2.477(17) . . ? C101 O103 3.366(15) . . ? O101 C102 3.371(16) . . ? O101 O102 3.996(15) . . ? O101 C103 3.374(15) . . ? O101 O103 4.024(14) . . ? O101 O232 4.164(16) . . ? O101 C252 3.69(2) . . ? O101 O201 4.198(14) . . ? O101 C431 3.603(15) . 2_656 ? O101 C44 3.608(13) . 2_656 ? O101 H152b 2.965(10) . . ? O101 H232a 2.766(10) . . ? O101 H24a 2.763(10) . . ? O101 H252a 2.703(10) . . ? O101 H312a 3.055(9) . 2_656 ? O101 H431a 2.744(9) . 2_656 ? O101 H44b 2.924(10) . 2_656 ? C102 C103 2.514(17) . . ? C102 O103 3.398(15) . . ? O102 C103 3.397(15) . . ? O102 O103 4.045(14) . . ? O102 C311 3.579(15) . 2_656 ? O102 O352 3.667(13) . 2_656 ? O102 C36 3.547(15) . 2_656 ? O102 C451 3.474(15) . 2_656 ? O102 H212b 3.200(11) . 1_565 ? O102 H311a 2.708(10) . 2_656 ? O102 H36a 2.809(10) . 2_656 ? O102 H44b 3.210(11) . 2_656 ? O102 H451a 3.354(10) . 2_656 ? O102 H451b 2.795(11) . 2_656 ? O103 C212 3.638(19) . 1_565 ? O103 O212 3.577(17) . 1_565 ? O103 C231 3.553(17) . 2_656 ? O103 O232 3.762(16) . 2_656 ? O103 C42 3.596(13) . 2_656 ? O103 C46 3.636(14) . 2_656 ? O103 H112a 3.204(10) . . ? O103 H132a 3.290(10) . . ? O103 H212b 2.979(10) . 1_565 ? O103 H212 3.293(10) . 1_565 ? O103 H231a 2.678(10) . 2_656 ? O103 H232 2.814(10) . 2_656 ? O103 H42b 2.697(9) . 2_656 ? O103 H44b 3.190(10) . 2_656 ? O103 H46b 2.753(9) . 2_656 ? N21 C212 2.39(2) . . ? N21 O212 3.009(17) . . ? N21 N23 2.286(14) . . ? N21 C24 2.730(17) . . ? N21 N25 2.272(15) . . ? N21 H211a 2.006(11) . . ? N21 H211b 2.005(10) . . ? N21 H212a 2.418(10) . . ? N21 H22a 2.029(10) . . ? N21 H22b 2.045(10) . . ? N21 H26a 2.021(10) . . ? N21 H26b 2.028(10) . . ? C211 O212 2.27(2) . . ? C211 C22 2.52(2) . . ? C211 C26 2.38(2) . . ? C211 O303 3.472(18) . 1_556 ? C211 H212a 1.865(16) . . ? C211 H212b 1.861(15) . . ? C211 H22a 2.687(16) . . ? C211 H26a 2.494(16) . . ? C212 O232 3.59(2) . 2_646 ? C212 H211a 1.90(2) . . ? C212 H211b 1.876(18) . . ? C212 H212 2.255(19) . . ? O212 C22 3.008(18) . . ? O212 C232 3.55(2) . 2_646 ? O212 O232 2.717(18) . 2_646 ? O212 O203 4.320(17) . . ? O212 O303 3.817(16) . 1_556 ? O212 C46 3.647(17) . 2_646 ? O212 H132a 3.309(14) . 2_646 ? O212 H211a 3.103(14) . . ? O212 H211b 2.297(13) . . ? O212 H212a 2.038(15) . . ? O212 H212b 2.005(14) . . ? O212 H22a 2.398(13) . . ? O212 H22b 3.322(13) . . ? O212 H232b 3.266(14) . 2_646 ? O212 H232 2.012(13) . 2_646 ? O212 H46a 3.351(13) . 2_646 ? O212 H46b 3.038(13) . 2_646 ? C22 C231 2.419(19) . . ? C22 C24 2.401(18) . . ? C22 N25 2.772(16) . . ? C22 C26 2.398(18) . . ? C22 O303 3.586(16) . 1_556 ? C22 H211b 2.625(13) . . ? C22 H231a 2.512(13) . . ? C22 H24b 2.601(13) . . ? C22 H26b 2.611(13) . . ? N23 C232 2.48(2) . . ? N23 O232 3.645(16) . . ? N23 N25 2.314(14) . . ? N23 C26 2.775(16) . . ? N23 H22a 2.008(9) . . ? N23 H22b 2.030(9) . . ? N23 H231a 1.996(10) . . ? N23 H231b 2.023(10) . . ? N23 H232a 2.609(9) . . ? N23 H24a 2.067(9) . . ? N23 H24b 2.065(9) . . ? C231 O232 2.368(18) . . ? C231 C24 2.48(2) . . ? C231 O301 3.641(17) . 1_556 ? C231 O432 3.544(15) . 2_656 ? C231 H22a 2.554(13) . . ? C231 H232a 2.070(13) . . ? C231 H232b 2.087(13) . . ? C231 H232 2.554(14) . . ? C231 H24a 2.632(14) . . ? C232 O432 3.457(18) . 2_656 ? C232 H212 2.577(17) . 2_656 ? C232 H231a 2.036(17) . . ? C232 H231b 2.023(16) . . ? C232 H232 1.697(17) . . ? O232 O203 4.000(17) . 2_656 ? O232 O432 2.758(15) . 2_656 ? O232 H112a 3.312(13) . 2_646 ? O232 H132a 3.212(13) . . ? O232 H212 1.897(12) . 2_656 ? O232 H231a 2.691(12) . . ? O232 H231b 2.442(12) . . ? O232 H232a 1.874(13) . . ? O232 H232b 1.900(13) . . ? O232 H432 3.091(12) . 2_656 ? C24 C251 2.47(2) . . ? C24 C26 2.378(19) . . ? C24 O302 3.376(16) . 1_556 ? C24 H22b 2.600(13) . . ? C24 H231b 2.664(14) . . ? C24 H251a 2.530(14) . . ? C24 H26b 2.575(13) . . ? N25 C252 2.45(2) . . ? N25 O252 2.980(13) . . ? N25 H24a 2.037(11) . . ? N25 H24b 2.022(11) . . ? N25 H251a 2.042(10) . . ? N25 H251b 2.031(10) . . ? N25 H252a 2.638(11) . . ? N25 H252 2.659(10) . . ? N25 H26a 2.032(11) . . ? N25 H26b 2.035(11) . . ? C251 O252 2.365(19) . . ? C251 C26 2.46(2) . . ? C251 O401 3.55(2) . 1_556 ? C251 O402 3.653(18) . 1_556 ? C251 H24a 2.629(17) . . ? C251 H252a 1.917(18) . . ? C251 H252b 1.937(18) . . ? C251 H252 2.507(16) . . ? C251 H26a 2.570(19) . . ? C252 H251a 1.941(17) . . ? C252 H251b 1.902(18) . . ? C252 H252 1.814(17) . . ? O252 C201 3.181(15) . . ? O252 O201 3.576(13) . . ? O252 C202 3.329(14) . . ? O252 O202 3.783(13) . . ? O252 O332 4.261(13) . 1_456 ? O252 C34 3.424(14) . 1_456 ? O252 H152b 3.333(8) . . ? O252 H152 1.901(8) . . ? O252 H251a 3.167(8) . . ? O252 H251b 2.585(8) . . ? O252 H252a 1.909(8) . . ? O252 H252b 1.895(8) . . ? O252 H34a 2.499(8) . 1_456 ? O252 H351a 3.235(8) . 1_456 ? C26 O332 3.593(16) . 1_456 ? C26 O401 3.129(14) . 1_556 ? C26 H211a 2.391(13) . . ? C26 H211b 2.669(13) . . ? C26 H22b 2.602(12) . . ? C26 H24b 2.566(13) . . ? C26 H251b 2.459(13) . . ? C201 C202 2.620(17) . . ? C201 O202 3.565(16) . . ? C201 C203 2.426(17) . . ? C201 O203 3.272(16) . . ? C201 H252 2.415(12) . . ? O201 C202 3.555(16) . . ? O201 O202 4.311(15) . . ? O201 C203 3.280(16) . . ? O201 O203 3.860(15) . . ? O201 H111b 2.598(10) . 2_546 ? O201 H12b 3.388(10) . 2_546 ? O201 H131b 2.777(10) . . ? O201 H14a 2.872(10) . . ? O201 H152 2.840(10) . . ? O201 H16b 2.869(10) . 2_546 ? O201 H232b 3.172(10) . . ? O201 H252 2.949(10) . . ? C202 C203 2.429(17) . . ? C202 O203 3.301(15) . . ? C202 H252 2.594(12) . . ? O202 C203 3.295(16) . . ? O202 O203 3.916(14) . . ? O202 C331 3.433(15) . 1_456 ? O202 C332 3.577(16) . 1_456 ? O202 O332 3.861(13) . 1_456 ? O202 H111a 3.217(11) . 1_545 ? O202 H112b 3.364(10) . 1_545 ? O202 H12b 2.746(10) . 2_546 ? O202 H131a 2.879(9) . 2_546 ? O202 H14b 2.740(9) . 2_546 ? O202 H252 3.183(10) . . ? O202 H331a 2.642(9) . 1_456 ? O202 H332a 3.102(10) . 1_456 ? O203 C411 3.574(15) . . ? O203 C42 3.378(14) . . ? O203 O432 3.393(13) . . ? O203 H112b 2.697(11) . 1_545 ? O203 H14b 3.321(12) . 2_546 ? O203 H151a 2.905(10) . 2_546 ? O203 H16b 3.098(11) . 2_546 ? O203 H212a 3.229(10) . . ? O203 H411b 2.801(10) . . ? O203 H42a 2.751(9) . . ? O203 H42b 3.171(11) . . ? N31 C312 2.502(14) . . ? N31 O312 3.009(11) . . ? N31 N33 2.299(12) . . ? N31 C34 2.772(13) . . ? N31 N35 2.322(13) . . ? N31 H311a 2.001(8) . . ? N31 H311b 1.991(8) . . ? N31 H312b 2.643(9) . . ? N31 H312 2.507(8) . . ? N31 H32a 2.028(9) . . ? N31 H32b 2.031(8) . . ? N31 H36a 2.059(9) . . ? N31 H36b 2.052(8) . . ? C311 O312 2.427(13) . . ? C311 C32 2.480(16) . . ? C311 C36 2.438(17) . . ? C311 H312a 2.073(11) . . ? C311 H312b 2.065(11) . . ? C311 H312 2.491(11) . . ? C311 H32a 2.643(11) . . ? C311 H36a 2.595(11) . . ? C312 O452 3.634(14) . 2_645 ? C312 O402 3.611(14) . 2_645 ? C312 H311a 2.076(11) . . ? C312 H311b 2.087(11) . . ? C312 H312 1.861(11) . . ? O312 C302 3.258(14) . . ? O312 O302 3.672(13) . . ? O312 C303 3.192(14) . . ? O312 O303 3.570(12) . . ? O312 C44 3.369(12) . . ? O312 C452 3.305(14) . 2_645 ? O312 O452 2.905(11) . 2_645 ? O312 O401 3.508(12) . . ? O312 H311a 2.583(8) . . ? O312 H311b 3.253(7) . . ? O312 H312a 1.953(8) . . ? O312 H312b 1.958(8) . . ? O312 H431b 3.265(8) . . ? O312 H44a 2.402(8) . . ? O312 H451a 3.213(9) . . ? O312 H452a 3.060(8) . 2_645 ? O312 H452b 3.360(9) . 2_645 ? O312 H452 1.897(8) . 2_645 ? C32 C331 2.501(17) . . ? C32 O332 3.410(15) . . ? C32 C34 2.392(17) . . ? C32 N35 2.782(15) . . ? C32 C36 2.411(17) . . ? C32 O402 3.573(15) . 2_645 ? C32 O403 3.576(14) . 1_655 ? C32 H311b 2.559(12) . . ? C32 H34b 2.557(12) . . ? C32 H36b 2.596(12) . . ? N33 C332 2.524(16) . . ? N33 O332 2.918(13) . . ? N33 N35 2.306(13) . . ? N33 C36 2.769(15) . . ? N33 H32a 1.997(9) . . ? N33 H32b 2.022(9) . . ? N33 H331a 2.014(9) . . ? N33 H331b 1.990(9) . . ? N33 H34a 2.055(9) . . ? N33 H34b 2.055(9) . . ? C331 O332 2.362(15) . . ? C331 C34 2.524(17) . . ? C331 H32a 2.586(12) . . ? C331 H332a 2.005(12) . . ? C331 H332b 1.993(12) . . ? C331 H34a 2.649(13) . . ? C332 O352 3.311(15) . 2_745 ? C332 O412 3.684(17) . 2_645 ? C332 H331a 1.989(13) . . ? C332 H331b 2.006(13) . . ? C332 H332 1.940(13) . . ? O332 C34 3.080(15) . . ? O332 C352 3.574(15) . 2_745 ? O332 O352 2.916(12) . 2_745 ? O332 O401 3.134(13) . 1_655 ? O332 O403 4.134(13) . 1_655 ? O332 H251b 3.069(10) . 1_654 ? O332 H26a 2.620(9) . 1_654 ? O332 H32b 3.067(9) . . ? O332 H331a 2.585(9) . . ? O332 H331b 3.177(9) . . ? O332 H332a 1.943(9) . . ? O332 H332b 1.943(9) . . ? O332 H34a 3.167(9) . . ? O332 H34b 2.732(10) . . ? O332 H352b 3.277(10) . 2_745 ? O332 H352 2.818(9) . 2_745 ? C34 C351 2.462(17) . . ? C34 C36 2.392(15) . . ? C34 H32b 2.579(12) . . ? C34 H331a 2.610(11) . . ? C34 H351a 2.536(12) . . ? C34 H36b 2.537(10) . . ? N35 C352 2.534(14) . . ? N35 O352 3.087(12) . . ? N35 H34a 2.026(9) . . ? N35 H34b 2.029(9) . . ? N35 H351a 2.015(9) . . ? N35 H351b 2.023(9) . . ? N35 H352a 2.664(9) . . ? N35 H36a 2.029(9) . . ? N35 H36b 2.020(9) . . ? C351 O352 2.407(16) . . ? C351 C36 2.474(18) . . ? C351 H34a 2.577(13) . . ? C351 H352a 2.071(13) . . ? C351 H352b 2.100(13) . . ? C351 H36a 2.587(13) . . ? C352 O452 3.478(15) . . ? C352 O403 3.637(13) . 2_655 ? C352 H332 2.615(11) . 2_755 ? C352 H351a 2.050(12) . . ? C352 H351b 2.038(12) . . ? C352 H352 2.005(12) . . ? O352 C36 3.083(14) . . ? O352 O302 4.016(12) . . ? O352 O452 2.770(11) . . ? O352 O401 3.369(12) . 2_655 ? O352 H332b 2.974(8) . 2_755 ? O352 H332 1.823(7) . 2_755 ? O352 H351a 3.203(8) . . ? O352 H351b 2.515(8) . . ? O352 H352a 1.935(8) . . ? O352 H352b 1.945(8) . . ? O352 H36a 2.369(7) . . ? O352 H451b 3.346(8) . . ? C36 O403 3.638(13) . 1_655 ? C36 H311a 2.442(11) . . ? C36 H32b 2.604(12) . . ? C36 H34b 2.535(11) . . ? C36 H351b 2.618(12) . . ? C301 C302 2.515(17) . . ? C301 O302 3.358(15) . . ? C301 C303 2.464(16) . . ? C301 O303 3.312(15) . . ? O301 C302 3.389(15) . . ? O301 O302 3.989(14) . . ? O301 C303 3.320(15) . . ? O301 O303 3.918(15) . . ? O301 C432 3.564(16) . 2_655 ? O301 O432 3.626(14) . 2_655 ? O301 H12a 2.952(10) . 2_645 ? O301 H132b 2.907(10) . 2_645 ? O301 H22b 3.093(11) . 1_554 ? O301 H231b 2.828(11) . 1_554 ? O301 H432a 2.855(11) . 2_655 ? O301 H432 2.981(11) . 2_655 ? C302 C303 2.535(16) . . ? C302 O303 3.449(15) . . ? C302 H312 2.453(11) . . ? O302 C303 3.424(15) . . ? O302 O303 4.129(14) . . ? O302 C451 3.578(14) . . ? O302 C452 3.262(15) . . ? O302 O452 3.295(13) . . ? O302 O401 3.964(14) . . ? O302 H24b 2.453(9) . 1_554 ? O302 H251a 3.287(9) . 1_554 ? O302 H26b 2.902(10) . 1_554 ? O302 H312 3.093(10) . . ? O302 H352a 3.014(10) . . ? O302 H432a 3.317(10) . 2_655 ? O302 H451a 2.962(9) . . ? O302 H452b 2.675(9) . . ? C303 H312 2.206(11) . . ? O303 C452 3.376(15) . 2_645 ? O303 O452 3.794(13) . 2_645 ? O303 C46 3.535(14) . 2_645 ? O303 O402 4.316(13) . 2_645 ? O303 H211b 2.563(10) . 1_554 ? O303 H22b 2.843(9) . 1_554 ? O303 H312 2.772(9) . . ? O303 H331b 3.325(10) . . ? O303 H412a 2.838(10) . 2_645 ? O303 H452a 2.484(10) . 2_645 ? O303 H452 3.323(10) . 2_645 ? O303 H46a 2.569(10) . 2_645 ? N41 C412 2.502(16) . . ? N41 O412 3.025(13) . . ? N41 N43 2.283(12) . . ? N41 C44 2.766(13) . . ? N41 N45 2.305(12) . . ? N41 H411a 2.052(9) . . ? N41 H411b 2.031(9) . . ? N41 H412a 2.616(9) . . ? N41 H42a 2.021(9) . . ? N41 H42b 2.036(9) . . ? N41 H46a 2.041(9) . . ? N41 H46b 2.033(9) . . ? C411 O412 2.376(15) . . ? C411 C42 2.467(16) . . ? C411 C46 2.472(17) . . ? C411 H412a 2.042(11) . . ? C411 H412b 2.066(12) . . ? C411 H42a 2.575(11) . . ? C411 H46a 2.609(12) . . ? C412 H411a 2.036(13) . . ? C412 H411b 2.011(12) . . ? C412 H412 2.094(13) . . ? O412 C402 3.252(16) . . ? O412 O402 3.602(14) . . ? O412 C403 3.303(14) . . ? O412 O403 3.649(13) . . ? O412 H151b 2.757(10) . 2_546 ? O412 H16a 2.509(11) . 2_546 ? O412 H331b 3.165(10) . 2_655 ? O412 H332a 3.234(10) . 2_655 ? O412 H411a 3.172(10) . . ? O412 H411b 2.484(10) . . ? O412 H412a 1.921(10) . . ? O412 H412b 1.931(10) . . ? C42 C431 2.503(16) . . ? C42 C432 2.966(15) . . ? C42 O432 2.947(13) . . ? C42 C44 2.411(14) . . ? C42 N45 2.800(13) . . ? C42 C46 2.429(15) . . ? C42 H411b 2.501(10) . . ? C42 H44b 2.598(10) . . ? C42 H46b 2.593(10) . . ? N43 C432 2.499(14) . . ? N43 O432 3.123(12) . . ? N43 N45 2.303(12) . . ? N43 C46 2.763(14) . . ? N43 H42a 2.039(8) . . ? N43 H42b 2.039(8) . . ? N43 H431a 2.017(9) . . ? N43 H431b 2.019(9) . . ? N43 H432b 2.541(9) . . ? N43 H44a 2.042(8) . . ? N43 H44b 2.043(9) . . ? C431 O432 2.369(15) . . ? C431 C44 2.438(16) . . ? C431 H42a 2.683(12) . . ? C431 H432a 1.992(12) . . ? C431 H432b 1.986(12) . . ? C431 H44a 2.554(12) . . ? C432 H42a 2.633(11) . . ? C432 H431a 1.969(12) . . ? C432 H431b 1.986(12) . . ? C432 H432 1.856(12) . . ? O432 H231b 2.807(8) . 2_646 ? O432 H42a 2.407(8) . . ? O432 H42b 3.079(8) . . ? O432 H431a 2.370(9) . . ? O432 H431b 3.149(9) . . ? O432 H432a 1.992(8) . . ? O432 H432b 2.007(8) . . ? C44 C451 2.468(15) . . ? C44 C46 2.399(14) . . ? C44 H42b 2.596(9) . . ? C44 H431a 2.596(10) . . ? C44 H431b 2.611(10) . . ? C44 H451a 2.497(10) . . ? C44 H46b 2.566(10) . . ? N45 C452 2.473(14) . . ? N45 O452 3.677(12) . . ? N45 H44a 2.036(8) . . ? N45 H44b 2.057(8) . . ? N45 H451a 2.004(8) . . ? N45 H451b 2.033(8) . . ? N45 H452a 2.591(8) . . ? N45 H46a 2.033(8) . . ? N45 H46b 2.027(8) . . ? C451 O452 2.350(13) . . ? C451 C46 2.458(16) . . ? C451 H44a 2.599(10) . . ? C451 H452a 2.037(10) . . ? C451 H452b 2.036(11) . . ? C451 H46a 2.600(11) . . ? C452 H451a 2.015(11) . . ? C452 H451b 2.010(11) . . ? C452 H452 1.919(11) . . ? O452 O401 3.068(12) . 2_655 ? O452 H312 3.324(8) . 2_655 ? O452 H352a 3.215(9) . . ? O452 H352 2.195(8) . . ? O452 H451a 2.622(8) . . ? O452 H451b 2.419(9) . . ? O452 H452a 1.973(8) . . ? O452 H452b 1.966(8) . . ? C46 H411a 2.565(11) . . ? C46 H42b 2.597(10) . . ? C46 H44b 2.591(11) . . ? C46 H451b 2.549(11) . . ? C401 C402 2.491(15) . . ? C401 O402 3.365(14) . . ? C401 C403 2.467(15) . . ? C401 O403 3.321(13) . . ? O401 C402 3.398(14) . . ? O401 O402 4.040(13) . . ? O401 C403 3.337(13) . . ? O401 O403 3.950(12) . . ? O401 H251b 2.858(9) . 1_554 ? O401 H26a 2.666(8) . 1_554 ? O401 H26b 2.705(8) . 1_554 ? O401 H332 2.758(9) . 1_455 ? O401 H352b 3.194(9) . 2_645 ? O401 H352 2.897(9) . 2_645 ? O401 H452 2.715(9) . 2_645 ? C402 C403 2.458(15) . . ? C402 O403 3.291(14) . . ? O402 C403 3.320(13) . . ? O402 O403 3.897(12) . . ? O402 H251a 3.294(9) . 1_554 ? O402 H251b 3.289(9) . 1_554 ? O402 H252b 3.045(9) . 1_554 ? O402 H312b 2.684(9) . 2_655 ? O402 H32a 2.621(9) . 2_655 ? O402 H34b 3.374(9) . 1_455 ? O402 H351b 3.127(9) . 1_455 ? O402 H452a 3.362(9) . . ? O402 H452b 3.330(9) . . ? O403 H151b 2.772(8) . 2_546 ? O403 H152a 2.520(8) . 2_546 ? O403 H32b 2.692(8) . 1_455 ? O403 H34b 3.232(8) . 1_455 ? O403 H352b 2.699(8) . 2_645 ? O403 H36b 2.761(8) . 1_455 ? O403 H432b 3.276(8) . . ? H111a H111b 1.55125(8) . . ? H111a H112b 2.23197(9) . . ? H111a H16a 2.30791(11) . . ? H112a H112b 1.55150(8) . . ? H12a H12b 1.55145(10) . . ? H12b H14b 2.36562(11) . . ? H12b H16b 2.39171(11) . . ? H131a H131b 1.55125(7) . . ? H131a H132b 2.31187(13) . . ? H131b H132a 2.31637(13) . . ? H131b H14a 2.20228(10) . . ? H132a H132b 1.55134(7) . . ? H14a H14b 1.55152(6) . . ? H151a H151b 1.55131(6) . . ? H151b H152a 2.27816(13) . . ? H151b H16a 2.26168(10) . . ? H152a H152b 1.55171(9) . . ? H152b H152 2.23575(12) . . ? H152 H252 2.03046(10) . . ? H16a H16b 1.55146(7) . . ? H16a H412 1.85410(9) . 2_556 ? H211a H211b 1.55131(11) . . ? H211a H212a 2.28220(14) . . ? H211a H212b 2.05444(9) . . ? H211a H26a 2.10741(11) . . ? H211b H212b 2.27184(9) . . ? H212a H212b 1.55129(7) . . ? H212 H232b 2.29981(9) . 2_646 ? H212 H232 1.15157(5) . 2_646 ? H22a H22b 1.55126(8) . . ? H22a H231a 2.26292(12) . . ? H231a H231b 1.55138(7) . . ? H231a H232b 2.28689(10) . . ? H232a H232b 1.55147(8) . . ? H232a H24a 2.11781(11) . . ? H232b H232 1.69755(9) . . ? H24a H24b 1.55139(6) . . ? H24b H26b 2.38902(13) . . ? H251a H251b 1.55137(8) . . ? H251a H252a 2.18819(8) . . ? H251a H252b 2.17913(13) . . ? H251b H252b 2.19455(12) . . ? H251b H26a 2.21274(11) . . ? H252a H252b 1.55139(7) . . ? H252a H252 2.17074(9) . . ? H26a H26b 1.55141(10) . . ? H311a H311b 1.55129(7) . . ? H311a H36a 2.22389(10) . . ? H311b H312a 2.34439(13) . . ? H312a H312b 1.55120(8) . . ? H312b H312 2.07405(9) . . ? H312b H32a 2.32545(13) . . ? H312 H452 2.30843(12) . 2_645 ? H32a H32b 1.55123(7) . . ? H32b H34b 2.36773(11) . . ? H331a H331b 1.55140(7) . . ? H331a H332a 2.24956(11) . . ? H331a H34a 2.37633(12) . . ? H331b H332a 2.28748(14) . . ? H331b H332b 2.25632(10) . . ? H332a H332b 1.55160(8) . . ? H332a H332 2.30322(10) . . ? H332b H332 2.07096(13) . . ? H332 H352 1.72711(8) . 2_745 ? H34a H34b 1.55126(8) . . ? H34a H351a 2.27448(13) . . ? H34b H36b 2.29348(11) . . ? H351a H351b 1.55108(9) . . ? H351a H352b 2.28060(10) . . ? H352a H352b 1.55147(7) . . ? H352a H352 2.38369(13) . . ? H352b H352 2.36664(11) . . ? H36a H36b 1.55134(9) . . ? H411a H411b 1.55119(7) . . ? H411a H412b 2.25300(12) . . ? H411b H42a 2.24994(11) . . ? H412a H412b 1.55160(7) . . ? H412a H46a 2.35515(15) . . ? H412b H412 2.30592(10) . . ? H42a H42b 1.55142(9) . . ? H42b H46b 2.39417(13) . . ? H431a H431b 1.55136(8) . . ? H431a H432a 2.39414(12) . . ? H431b H432a 2.15918(9) . . ? H431b H44a 2.37346(12) . . ? H432a H432b 1.55127(8) . . ? H432a H432 2.11056(11) . . ? H432b H432 2.20748(11) . . ? H44a H44b 1.55107(8) . . ? H44a H451a 2.26278(12) . . ? H44b H46b 2.38349(12) . . ? H451a H451b 1.55152(7) . . ? H451a H452b 2.25247(9) . . ? H452a H452b 1.55151(7) . . ? H452a H452 2.02866(8) . . ? H452a H46a 2.28575(12) . . ? H452b H452 2.35069(14) . . ? H46a H46b 1.55129(6) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC N11 Cr1 N13 63.0(3) . . . ? N11 Cr1 N15 63.9(3) . . . ? N11 Cr1 C101 165.8(4) . . . ? N11 Cr1 C102 101.9(4) . . . ? N11 Cr1 C103 104.0(4) . . . ? N13 Cr1 N15 62.9(3) . . . ? N13 Cr1 C101 105.7(4) . . . ? N13 Cr1 C102 162.2(5) . . . ? N13 Cr1 C103 103.9(4) . . . ? N15 Cr1 C101 103.8(4) . . . ? N15 Cr1 C102 102.8(4) . . . ? N15 Cr1 C103 164.7(4) . . . ? C101 Cr1 C102 87.4(5) . . . ? C101 Cr1 C103 86.8(5) . . . ? C102 Cr1 C103 88.5(5) . . . ? N21 Cr2 N23 63.3(4) . . . ? N21 Cr2 N25 62.1(4) . . . ? N21 Cr2 C201 164.5(5) . . . ? N21 Cr2 C202 100.7(5) . . . ? N21 Cr2 C203 105.4(5) . . . ? N23 Cr2 N25 63.6(4) . . . ? N23 Cr2 C201 103.0(5) . . . ? N23 Cr2 C202 163.5(5) . . . ? N23 Cr2 C203 103.0(5) . . . ? N25 Cr2 C201 106.3(5) . . . ? N25 Cr2 C202 106.6(4) . . . ? N25 Cr2 C203 164.3(5) . . . ? C201 Cr2 C202 92.5(5) . . . ? C201 Cr2 C203 84.0(5) . . . ? C202 Cr2 C203 84.3(5) . . . ? N31 Cr3 N33 63.4(3) . . . ? N31 Cr3 N35 63.7(3) . . . ? N31 Cr3 C301 161.8(4) . . . ? N31 Cr3 C302 107.1(4) . . . ? N31 Cr3 C303 105.8(4) . . . ? N33 Cr3 N35 64.3(3) . . . ? N33 Cr3 C301 100.9(5) . . . ? N33 Cr3 C302 168.8(4) . . . ? N33 Cr3 C303 99.8(5) . . . ? N35 Cr3 C301 102.0(5) . . . ? N35 Cr3 C302 106.8(4) . . . ? N35 Cr3 C303 163.3(5) . . . ? C301 Cr3 C302 87.3(5) . . . ? C301 Cr3 C303 85.2(5) . . . ? C302 Cr3 C303 88.4(5) . . . ? N41 Cr4 N43 62.5(3) . . . ? N41 Cr4 N45 63.1(3) . . . ? N41 Cr4 C401 160.3(4) . . . ? N41 Cr4 C402 108.2(4) . . . ? N41 Cr4 C403 107.5(4) . . . ? N43 Cr4 N45 63.6(3) . . . ? N43 Cr4 C401 100.5(4) . . . ? N43 Cr4 C402 167.1(4) . . . ? N43 Cr4 C403 105.8(4) . . . ? N45 Cr4 C401 101.5(4) . . . ? N45 Cr4 C402 104.7(4) . . . ? N45 Cr4 C403 167.9(4) . . . ? C401 Cr4 C402 86.9(5) . . . ? C401 Cr4 C403 85.7(5) . . . ? C402 Cr4 C403 85.2(5) . . . ? Cr1 N11 C111 133.0(7) . . . ? Cr1 N11 C12 93.5(6) . . . ? Cr1 N11 C16 92.4(6) . . . ? C111 N11 C12 115.2(9) . . . ? C111 N11 C16 110.2(8) . . . ? C12 N11 C16 109.3(8) . . . ? N11 C111 C112 115.5(10) . . . ? N11 C111 H111a 108.9(10) . . . ? N11 C111 H111b 110.1(10) . . . ? C112 C111 H111a 108.3(11) . . . ? C112 C111 H111b 107.8(11) . . . ? H111a C111 H111b 105.8(12) . . . ? C111 C112 O112 112.4(10) . . . ? C111 C112 H112a 108.9(11) . . . ? C111 C112 H112b 110.0(11) . . . ? O112 C112 H112a 108.9(11) . . . ? O112 C112 H112b 108.7(11) . . . ? H112a C112 H112b 107.8(11) . . . ? N11 C12 N13 102.9(8) . . . ? N11 C12 H12a 111.4(10) . . . ? N11 C12 H12b 112.5(9) . . . ? N13 C12 H12a 112.3(10) . . . ? N13 C12 H12b 111.7(10) . . . ? H12a C12 H12b 106.3(9) . . . ? Cr1 N13 C12 91.8(6) . . . ? Cr1 N13 C131 133.6(7) . . . ? Cr1 N13 C14 91.6(6) . . . ? C12 N13 C131 114.0(8) . . . ? C12 N13 C14 110.3(8) . . . ? C131 N13 C14 112.2(9) . . . ? N13 C131 C132 112.7(11) . . . ? N13 C131 H131a 109.1(10) . . . ? N13 C131 H131b 109.3(10) . . . ? C132 C131 H131a 107.3(12) . . . ? C132 C131 H131b 109.3(12) . . . ? H131a C131 H131b 109.1(12) . . . ? C131 C132 O132 104.5(13) . . . ? C131 C132 H132a 108.9(15) . . . ? C131 C132 H132b 110.4(14) . . . ? O132 C132 H132a 112.6(15) . . . ? O132 C132 H132b 113.1(17) . . . ? H132a C132 H132b 107.2(16) . . . ? N13 C14 N15 104.7(8) . . . ? N13 C14 H14a 111.5(10) . . . ? N13 C14 H14b 110.5(9) . . . ? N15 C14 H14a 112.2(9) . . . ? N15 C14 H14b 111.0(10) . . . ? H14a C14 H14b 107.0(10) . . . ? Cr1 N15 C14 91.8(6) . . . ? Cr1 N15 C151 134.4(7) . . . ? Cr1 N15 C16 91.3(6) . . . ? C14 N15 C151 115.0(8) . . . ? C14 N15 C16 109.1(8) . . . ? C151 N15 C16 111.5(8) . . . ? N15 C151 C152 113.7(10) . . . ? N15 C151 H151a 109.1(10) . . . ? N15 C151 H151b 108.8(10) . . . ? C152 C151 H151a 109.6(10) . . . ? C152 C151 H151b 110.5(10) . . . ? H151a C151 H151b 104.7(11) . . . ? C151 C152 O152 110.1(9) . . . ? C151 C152 H152a 111.9(11) . . . ? C151 C152 H152b 107.5(10) . . . ? O152 C152 H152a 110.0(10) . . . ? O152 C152 H152b 110.3(11) . . . ? H152a C152 H152b 107.1(11) . . . ? C152 O152 H152 115.5(10) . . . ? N11 C16 N15 103.4(8) . . . ? N11 C16 H16a 109.7(9) . . . ? N11 C16 H16b 113.6(10) . . . ? N15 C16 H16a 110.3(9) . . . ? N15 C16 H16b 113.2(9) . . . ? H16a C16 H16b 106.7(10) . . . ? Cr1 C101 O101 176.3(11) . . . ? Cr1 C102 O102 175.1(11) . . . ? Cr1 C103 O103 175.4(10) . . . ? Cr2 N21 C211 132.9(8) . . . ? Cr2 N21 C22 91.4(7) . . . ? Cr2 N21 C26 94.7(7) . . . ? C211 N21 C22 116.0(10) . . . ? C211 N21 C26 108.1(10) . . . ? C22 N21 C26 111.3(10) . . . ? N21 C211 C212 114.8(14) . . . ? N21 C211 H211a 106.7(13) . . . ? N21 C211 H211b 107.4(12) . . . ? C212 C211 H211a 110.7(15) . . . ? C212 C211 H211b 109.0(15) . . . ? H211a C211 H211b 108.0(16) . . . ? C211 C212 O212 108.7(14) . . . ? C211 C212 H212a 106.5(15) . . . ? C211 C212 H212b 108.6(18) . . . ? O212 C212 H212a 112.6(16) . . . ? O212 C212 H212b 112.1(15) . . . ? H212a C212 H212b 108.2(17) . . . ? C212 O212 H212 134.7(14) . . . ? N21 C22 N23 102.9(9) . . . ? N21 C22 H22a 111.6(11) . . . ? N21 C22 H22b 112.9(11) . . . ? N23 C22 H22a 110.4(11) . . . ? N23 C22 H22b 112.2(11) . . . ? H22a C22 H22b 106.9(11) . . . ? Cr2 N23 C22 92.1(6) . . . ? Cr2 N23 C231 134.3(8) . . . ? Cr2 N23 C24 91.9(7) . . . ? C22 N23 C231 111.8(9) . . . ? C22 N23 C24 109.2(9) . . . ? C231 N23 C24 114.0(10) . . . ? N23 C231 C232 112.9(11) . . . ? N23 C231 H231a 108.1(11) . . . ? N23 C231 H231b 111.9(12) . . . ? C232 C231 H231a 108.0(13) . . . ? C232 C231 H231b 108.4(12) . . . ? H231a C231 H231b 107.3(12) . . . ? C231 C232 O232 111.8(13) . . . ? C231 C232 H232a 111.7(15) . . . ? C231 C232 H232b 111.8(15) . . . ? O232 C232 H232a 107.4(16) . . . ? O232 C232 H232b 108.2(15) . . . ? H232a C232 H232b 105.7(15) . . . ? C232 O232 H232 85.9(11) . . . ? N23 C24 N25 104.2(10) . . . ? N23 C24 H24a 111.3(11) . . . ? N23 C24 H24b 112.3(12) . . . ? N25 C24 H24a 112.5(12) . . . ? N25 C24 H24b 112.3(12) . . . ? H24a C24 H24b 104.5(12) . . . ? Cr2 N25 C24 91.4(7) . . . ? Cr2 N25 C251 134.5(9) . . . ? Cr2 N25 C26 92.4(7) . . . ? C24 N25 C251 114.2(11) . . . ? C24 N25 C26 109.3(10) . . . ? C251 N25 C26 111.6(10) . . . ? N25 C251 C252 116.0(12) . . . ? N25 C251 H251a 109.2(15) . . . ? N25 C251 H251b 109.6(16) . . . ? C252 C251 H251a 108.6(17) . . . ? C252 C251 H251b 106.7(16) . . . ? H251a C251 H251b 106.2(14) . . . ? C251 C252 O252 119.2(16) . . . ? C251 C252 H252a 106.0(16) . . . ? C251 C252 H252b 109.2(15) . . . ? O252 C252 H252a 108.3(14) . . . ? O252 C252 H252b 108.5(15) . . . ? H252a C252 H252b 104.8(18) . . . ? C252 O252 H252 109.2(11) . . . ? N21 C26 N25 102.6(9) . . . ? N21 C26 H26a 111.5(11) . . . ? N21 C26 H26b 114.4(11) . . . ? N25 C26 H26a 110.0(11) . . . ? N25 C26 H26b 112.2(12) . . . ? H26a C26 H26b 106.3(12) . . . ? Cr2 C201 O201 175.6(11) . . . ? Cr2 C202 O202 176.6(10) . . . ? Cr2 C203 O203 175.3(11) . . . ? Cr3 N31 C311 135.7(7) . . . ? Cr3 N31 C32 90.4(6) . . . ? Cr3 N31 C36 91.4(6) . . . ? C311 N31 C32 114.6(9) . . . ? C311 N31 C36 111.3(8) . . . ? C32 N31 C36 109.9(8) . . . ? N31 C311 C312 112.5(9) . . . ? N31 C311 H311a 107.6(10) . . . ? N31 C311 H311b 107.8(10) . . . ? C312 C311 H311a 110.0(10) . . . ? C312 C311 H311b 111.9(10) . . . ? H311a C311 H311b 106.8(11) . . . ? C311 C312 O312 110.8(9) . . . ? C311 C312 H312a 110.8(10) . . . ? C311 C312 H312b 109.4(10) . . . ? O312 C312 H312a 109.4(10) . . . ? O312 C312 H312b 108.9(10) . . . ? H312a C312 H312b 107.5(10) . . . ? C312 O312 H312 97.0(7) . . . ? N31 C32 N33 103.8(9) . . . ? N31 C32 H32a 110.9(10) . . . ? N31 C32 H32b 112.1(10) . . . ? N33 C32 H32a 109.7(10) . . . ? N33 C32 H32b 112.8(10) . . . ? H32a C32 H32b 107.6(11) . . . ? Cr3 N33 C32 93.4(6) . . . ? Cr3 N33 C331 123.0(7) . . . ? Cr3 N33 C34 92.4(6) . . . ? C32 N33 C331 116.9(9) . . . ? C32 N33 C34 109.5(8) . . . ? C331 N33 C34 117.1(9) . . . ? N33 C331 C332 116.9(10) . . . ? N33 C331 H331a 109.1(11) . . . ? N33 C331 H331b 107.0(10) . . . ? C332 C331 H331a 107.3(11) . . . ? C332 C331 H331b 108.6(11) . . . ? H331a C331 H331b 107.5(11) . . . ? C331 C332 O332 110.7(11) . . . ? C331 C332 H332a 109.6(11) . . . ? C331 C332 H332b 107.4(11) . . . ? O332 C332 H332a 111.0(12) . . . ? O332 C332 H332b 109.6(11) . . . ? H332a C332 H332b 108.5(13) . . . ? C332 O332 H332 101.0(9) . . . ? N33 C34 N35 103.0(8) . . . ? N33 C34 H34a 113.4(10) . . . ? N33 C34 H34b 112.1(10) . . . ? N35 C34 H34a 111.5(10) . . . ? N35 C34 H34b 110.4(9) . . . ? H34a C34 H34b 106.5(9) . . . ? Cr3 N35 C34 91.6(6) . . . ? Cr3 N35 C351 131.6(8) . . . ? Cr3 N35 C36 92.8(6) . . . ? C34 N35 C351 114.0(9) . . . ? C34 N35 C36 108.6(9) . . . ? C351 N35 C36 114.4(9) . . . ? N35 C351 C352 115.1(10) . . . ? N35 C351 H351a 109.5(11) . . . ? N35 C351 H351b 111.2(11) . . . ? C352 C351 H351a 107.2(11) . . . ? C352 C351 H351b 107.1(11) . . . ? H351a C351 H351b 106.2(13) . . . ? C351 C352 O352 110.6(9) . . . ? C351 C352 H352a 109.9(10) . . . ? C351 C352 H352b 111.6(11) . . . ? O352 C352 H352a 109.2(10) . . . ? O352 C352 H352b 109.2(9) . . . ? H352a C352 H352b 106.3(11) . . . ? C352 O352 H352 133.5(9) . . . ? N31 C36 N35 103.7(8) . . . ? N31 C36 H36a 113.3(9) . . . ? N31 C36 H36b 112.7(11) . . . ? N35 C36 H36a 110.5(10) . . . ? N35 C36 H36b 109.8(9) . . . ? H36a C36 H36b 106.8(11) . . . ? Cr3 C301 O301 175.3(11) . . . ? Cr3 C302 O302 174.3(10) . . . ? Cr3 C303 O303 176.1(10) . . . ? Cr4 N41 C411 134.4(7) . . . ? Cr4 N41 C42 92.4(6) . . . ? Cr4 N41 C46 91.8(6) . . . ? C411 N41 C42 112.1(8) . . . ? C411 N41 C46 112.8(8) . . . ? C42 N41 C46 110.3(8) . . . ? N41 C411 C412 113.0(9) . . . ? N41 C411 H411a 111.1(11) . . . ? N41 C411 H411b 110.1(10) . . . ? C412 C411 H411a 108.4(10) . . . ? C412 C411 H411b 107.0(11) . . . ? H411a C411 H411b 107.0(10) . . . ? C411 C412 O412 111.6(10) . . . ? C411 C412 H412a 108.7(12) . . . ? C411 C412 H412b 110.8(12) . . . ? O412 C412 H412a 109.5(12) . . . ? O412 C412 H412b 110.4(12) . . . ? H412a C412 H412b 105.6(11) . . . ? C412 O412 H412 127.2(11) . . . ? N41 C42 N43 101.7(7) . . . ? N41 C42 H42a 109.9(9) . . . ? N41 C42 H42b 111.0(9) . . . ? N43 C42 H42a 113.2(9) . . . ? N43 C42 H42b 113.1(9) . . . ? H42a C42 H42b 107.9(9) . . . ? Cr4 N43 C42 94.3(6) . . . ? Cr4 N43 C431 131.3(7) . . . ? Cr4 N43 C44 92.0(6) . . . ? C42 N43 C431 115.2(8) . . . ? C42 N43 C44 110.9(8) . . . ? C431 N43 C44 110.3(8) . . . ? N43 C431 C432 114.9(9) . . . ? N43 C431 H431a 107.5(10) . . . ? N43 C431 H431b 109.2(10) . . . ? C432 C431 H431a 106.5(11) . . . ? C432 C431 H431b 109.7(11) . . . ? H431a C431 H431b 108.8(11) . . . ? C431 C432 O432 109.2(9) . . . ? C431 C432 H432a 109.9(11) . . . ? C431 C432 H432b 107.6(10) . . . ? O432 C432 H432a 111.3(10) . . . ? O432 C432 H432b 110.7(11) . . . ? H432a C432 H432b 108.0(11) . . . ? C432 O432 H432 100.4(8) . . . ? N43 C44 N45 103.0(7) . . . ? N43 C44 H44a 112.3(9) . . . ? N43 C44 H44b 112.2(8) . . . ? N45 C44 H44a 110.9(8) . . . ? N45 C44 H44b 112.6(9) . . . ? H44a C44 H44b 106.0(9) . . . ? Cr4 N45 C44 91.7(5) . . . ? Cr4 N45 C451 133.8(6) . . . ? Cr4 N45 C46 93.3(6) . . . ? C44 N45 C451 112.8(7) . . . ? C44 N45 C46 109.2(7) . . . ? C451 N45 C46 112.7(8) . . . ? N45 C451 C452 112.1(8) . . . ? N45 C451 H451a 108.5(9) . . . ? N45 C451 H451b 110.6(10) . . . ? C452 C451 H451a 109.0(10) . . . ? C452 C451 H451b 108.1(9) . . . ? H451a C451 H451b 108.5(10) . . . ? C451 C452 O452 107.5(8) . . . ? C451 C452 H452a 110.7(10) . . . ? C451 C452 H452b 110.1(10) . . . ? O452 C452 H452a 110.9(10) . . . ? O452 C452 H452b 109.8(10) . . . ? H452a C452 H452b 107.9(10) . . . ? C452 O452 H452 100.1(7) . . . ? N41 C46 N45 103.0(8) . . . ? N41 C46 H46a 111.4(10) . . . ? N41 C46 H46b 111.6(9) . . . ? N45 C46 H46a 111.5(9) . . . ? N45 C46 H46b 111.9(10) . . . ? H46a C46 H46b 107.4(10) . . . ? Cr4 C401 O401 177.1(10) . . . ? Cr4 C402 O402 174.7(10) . . . ? Cr4 C403 O403 174.5(9) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_total 8034 #ActaC _reflns_number_observed 4459 #ActaC _reflns_observed_criterion refl_observed_if_F____>4.000_sigma(F___) _reflns_d_resolution_high .73 _reflns_d_resolution_low 16.413 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? data_dbmvb _audit_creation_date 97-12-21 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common tohbtach #ActaC _chemical_formula_analytical C24_H27_N3_O3_0.25(EtOAc)._5/8(H2_O) #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum C50_H58_N6_O8.25 #ActaC _chemical_formula_weight 875.05 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-NONIUS software' #ActaC _computing_cell_refinement 'Enraf-NONIUS software' #ActaC _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 26.308(13) #ActaC _cell_length_b 14.650(7) #ActaC _cell_length_c 25.424(17) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 92.71(5) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 9788(9) #ActaC _cell_formula_units_Z 8 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 8 #ActaC _cell_measurement_theta_min 13.5 #ActaC _cell_measurement_theta_max 14.2 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M c_1_2/c_1 #ActaC _symmetry_space_group_name_Hall -c_2yc #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description needle #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour none #ActaC _exptl_crystal_size_max 0.90 #ActaC _exptl_crystal_size_mid 0.30 #ActaC _exptl_crystal_size_min 0.22 #ActaC _exptl_crystal_density_diffrn 1.191 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 3748 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 0.08 #ActaC _exptl_absorpt_correction_type ? #ActaC _exptl_absorpt_correction_T_min ? #ActaC _exptl_absorpt_correction_T_max ? #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'rotating-anode' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number 8 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 10 6 10 10 -6 10 -10 6 -10 -10 -6 -10 11 5 -10 -11 -5 10 -11 5 10 11 -5 -10 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 9320 #ActaC _diffrn_reflns_av_R_equivalents .007 #ActaC _diffrn_reflns_av_sigmaI/netI .034 #ActaC _diffrn_reflns_limit_h_min -31 #ActaC _diffrn_reflns_limit_h_max 31 #ActaC _diffrn_reflns_limit_k_min -17 #ActaC _diffrn_reflns_limit_k_max 0 #ActaC _diffrn_reflns_limit_l_min -30 #ActaC _diffrn_reflns_limit_l_max 1 #ActaC _diffrn_reflns_theta_min 1.55 #ActaC _diffrn_reflns_theta_max 24.99 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 400 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 484 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 48 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 66 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC N11 .67269(9) .40817(16) .16846(9) .0449(15) Uani ? ? C110 .69144(12) .3133(2) .17239(12) .055(2) Uani ? ? C111 .66730(11) .2532(2) .13014(12) .048(2) Uani ? ? C112 .65794(12) .2856(2) .07940(13) .053(2) Uani ? ? O112 .66803(9) .37443(15) .06645(8) .0699(16) Uani ? ? C113 .63795(14) .2297(2) .04016(14) .066(2) Uani ? ? C114 .62860(14) .1394(3) .05049(15) .076(3) Uani ? ? C115 .63795(14) .1052(2) .10005(16) .077(3) Uani ? ? C116 .65661(13) .1621(2) .13971(14) .063(2) Uani ? ? C12 .61919(11) .4148(2) .18137(12) .048(2) Uani ? ? N13 .60230(9) .50811(16) .17121(10) .0464(16) Uani ? ? C130 .54720(12) .5170(2) .17849(13) .057(2) Uani ? ? C131 .52328(11) .5961(2) .14902(13) .056(2) Uani ? ? C132 .53735(12) .6181(2) .09849(14) .063(2) Uani ? ? O132 .57564(9) .57385(19) .07517(9) .0831(19) Uani ? ? C133 .51175(15) .6856(3) .06985(16) .084(3) Uani ? ? C134 .47202(16) .7298(3) .0909(2) .103(3) Uani ? ? C135 .45722(15) .7102(3) .1398(2) .103(3) Uani ? ? C136 .48321(13) .6436(3) .16915(16) .079(3) Uani ? ? C14 .63204(11) .5707(2) .20574(13) .053(2) Uani ? ? N15 .68625(9) .56377(17) .19681(10) .0481(16) Uani ? ? C150 .70028(12) .6061(2) .14774(13) .056(2) Uani ? ? C151 .75697(11) .6186(2) .14360(12) .049(2) Uani ? ? C152 .78887(13) .6405(2) .18626(13) .062(2) Uani ? ? O152 .77221(9) .6484(2) .23617(10) .090(2) Uani ? ? C153 .84021(13) .6575(3) .17943(15) .078(3) Uani ? ? C154 .85929(13) .6530(3) .13109(16) .076(3) Uani ? ? C155 .82867(14) .6315(2) .08845(14) .070(3) Uani ? ? C156 .77783(13) .6142(2) .09521(14) .060(2) Uani ? ? C16 .70317(12) .4701(2) .20277(12) .049(2) Uani ? ? N21 .70100(9) .56439(16) .42354(9) .0447(15) Uani ? ? C210 .72124(12) .6575(2) .43260(12) .051(2) Uani ? ? C211 .69860(12) .7256(2) .39345(12) .048(2) Uani ? ? C212 .68845(12) .7024(2) .34117(12) .052(2) Uani ? ? O212 .69576(9) .61541(15) .32349(8) .0653(15) Uani ? ? C213 .67092(13) .7676(2) .30527(13) .064(2) Uani ? ? C214 .66330(14) .8558(2) .32143(15) .075(3) Uani ? ? C215 .67268(15) .8803(2) .37279(15) .076(3) Uani ? ? C216 .69046(13) .8153(2) .40870(14) .063(2) Uani ? ? C22 .64747(11) .5582(2) .43661(12) .048(2) Uani ? ? N23 .62891(9) .46769(16) .42063(9) .0453(16) Uani ? ? C230 .57390(12) .4592(2) .42873(13) .054(2) Uani ? ? C231 .54982(11) .3840(2) .39598(12) .050(2) Uani ? ? C232 .56343(12) .3694(2) .34460(13) .055(2) Uani ? ? O232 .60083(9) .41895(18) .32284(9) .0752(17) Uani ? ? C233 .53845(13) .3050(3) .31341(15) .072(3) Uani ? ? C234 .49974(15) .2550(3) .33354(18) .088(3) Uani ? ? C235 .48529(14) .2669(3) .38370(16) .084(3) Uani ? ? C236 .51048(13) .3325(3) .41486(14) .071(3) Uani ? ? C24 .65838(12) .3982(2) .45067(13) .053(2) Uani ? ? N25 .71247(9) .40454(16) .44115(10) .0483(16) Uani ? ? C250 .72514(12) .3737(2) .38839(13) .055(2) Uani ? ? C251 .78136(12) .3601(2) .38369(12) .050(2) Uani ? ? C252 .81099(12) .3171(2) .42352(13) .056(2) Uani ? ? O252 .79036(9) .28796(16) .46852(9) .0727(17) Uani ? ? C253 .86241(13) .3014(3) .41794(15) .072(3) Uani ? ? C254 .88400(14) .3274(3) .37251(15) .079(3) Uani ? ? C255 .85617(15) .3699(3) .33294(15) .084(3) Uani ? ? C256 .80473(13) .3862(3) .33896(14) .068(2) Uani ? ? C26 .73069(12) .4959(2) .45352(12) .046(2) Uani ? ? O01 1.00000 .50000 .50000 .41(3) Uani ? ? O02 1.0146(5) .5390(9) .5349(6) .318(16) Uani ? ? O03 .9554(5) .4335(11) .5306(7) .364(18) Uani ? ? C1 .9631(6) .4799(9) .7586(8) .37(3) Uani ? ? C2 .9886(5) .5280(9) .7150(4) .41(4) Uani ? ? O2 1.0152(5) .5850(11) .7255(5) .50(3) Uani ? ? O3 .9645(4) .5254(9) .6632(8) .71(4) Uani ? ? C4 .9994(5) .5035(12) .6255(9) .55(4) Uani ? ? C5 .9702(6) .4951(11) .5707(9) .35(3) Uani ? ? H110a .6859(9) .2914(17) .2064(10) .053(8) Uiso ? ? H110b .7307(11) .319(2) .1645(11) .080(10) Uiso ? ? H112 .6742(12) .402(2) .0990(12) .095(11) Uiso ? ? H113 .6281(12) .254(2) .0052(12) .092(11) Uiso ? ? H114 .6168(11) .098(2) .0242(11) .077(10) Uiso ? ? H115 .6305(13) .044(2) .1067(13) .105(12) Uiso ? ? H116 .6626(9) .1399(17) .1735(9) .050(8) Uiso ? ? H12a .6137(9) .3994(16) .2194(9) .043(7) Uiso ? ? H12b .5986(10) .3729(17) .1565(10) .059(9) Uiso ? ? H130a .5392(10) .5199(17) .2199(10) .054(8) Uiso ? ? H130b .5333(10) .4572(19) .1671(10) .066(9) Uiso ? ? H132 .5927(14) .535(2) .1078(14) .119(14) Uiso ? ? H133 .5240(12) .697(2) .0315(12) .093(11) Uiso ? ? H134 .4556(14) .770(3) .0686(14) .128(14) Uiso ? ? H135 .4322(13) .738(2) .1580(12) .106(12) Uiso ? ? H136 .4754(11) .629(2) .2059(11) .077(10) Uiso ? ? H14a .6262(11) .551(2) .2446(11) .079(10) Uiso ? ? H14b .6184(10) .6318(17) .1983(10) .054(8) Uiso ? ? H150a .6859(11) .662(2) .1439(11) .073(9) Uiso ? ? H150b .6890(11) .567(2) .1119(11) .078(10) Uiso ? ? H152 .7401(15) .623(3) .2340(15) .149(16) Uiso ? ? H153 .8582(11) .668(2) .2068(11) .071(9) Uiso ? ? H154 .8928(10) .6647(19) .1276(10) .068(9) Uiso ? ? H155 .8392(13) .629(2) .0521(13) .114(13) Uiso ? ? H156 .7550(12) .598(2) .0646(12) .088(11) Uiso ? ? H16a .7401(9) .4642(17) .1906(9) .050(8) Uiso ? ? H16b .6995(10) .4539(18) .2396(10) .059(9) Uiso ? ? H210a .7585(10) .6502(19) .4248(10) .065(9) Uiso ? ? H210b .7176(9) .6767(16) .4677(9) .041(7) Uiso ? ? H212 .7000(15) .569(3) .3657(15) .138(15) Uiso ? ? H213 .6638(10) .754(2) .2698(11) .071(9) Uiso ? ? H214 .6522(11) .905(2) .2969(11) .073(10) Uiso ? ? H215 .6706(12) .941(2) .3883(12) .101(12) Uiso ? ? H216 .6975(11) .833(2) .4467(11) .082(10) Uiso ? ? H22a .6272(9) .6014(17) .4175(9) .049(8) Uiso ? ? H22b .6443(9) .5682(17) .4781(9) .048(8) Uiso ? ? H230a .5610(11) .5136(19) .4197(10) .065(9) Uiso ? ? H230b .5689(10) .4504(18) .4701(10) .065(9) Uiso ? ? H232 .6181(16) .446(3) .3559(16) .158(17) Uiso ? ? H233 .5512(11) .295(2) .2766(11) .083(10) Uiso ? ? H234 .4855(10) .2146(18) .3126(10) .065(9) Uiso ? ? H235 .4609(15) .240(3) .4067(15) .137(15) Uiso ? ? H236 .5009(12) .348(2) .4544(12) .088(11) Uiso ? ? H24a .6455(9) .3401(17) .4407(10) .055(8) Uiso ? ? H24b .6512(11) .409(2) .4904(11) .077(10) Uiso ? ? H250a .7108(10) .4129(18) .3583(10) .058(9) Uiso ? ? H250b .7074(11) .317(2) .3805(11) .078(10) Uiso ? ? H252 .7561(18) .331(3) .4689(18) .20(2) Uiso ? ? H253 .8817(12) .272(2) .4483(12) .094(11) Uiso ? ? H254 .9197(11) .317(2) .3722(11) .086(11) Uiso ? ? H255 .8678(12) .392(2) .3016(12) .095(11) Uiso ? ? H256 .7824(11) .422(2) .3118(11) .074(10) Uiso ? ? H26a .7664(10) .5050(18) .4436(10) .063(9) Uiso ? ? H26b .7281(9) .5061(16) .4940(9) .040(7) Uiso ? ? H1a .93053 .49995 .75030 .55000 Uiso ? ? H1b .95736 .41189 .73214 .55000 Uiso ? ? H1c .97594 .46068 .78273 .55000 Uiso ? ? H4a 1.02946 .52116 .62145 .55000 Uiso ? ? H4b 1.00236 .43068 .63496 .55000 Uiso ? ? H5a .93270 .46769 .57060 .38000 Uiso ? ? H5b .95979 .55818 .55709 .38000 Uiso ? ? H5c .98364 .46526 .54208 .38000 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC N11 .0410(15) .0398(15) .0541(17) .0030(12) .0024(13) .0006(13) C110 .061(2) .052(2) .051(2) .0100(18) .0029(17) .0093(17) C111 .047(2) .043(2) .056(2) .0078(16) .0019(16) -.0003(17) C112 .056(2) .047(2) .055(2) .0004(17) .0066(17) -.0012(17) O112 .101(2) .0569(16) .0518(15) -.0064(14) -.0002(14) .0067(12) C113 .071(3) .063(3) .064(2) .003(2) -.002(2) -.010(2) C114 .072(3) .071(3) .084(3) -.001(2) -.003(2) -.025(2) C115 .079(3) .047(2) .104(3) -.008(2) .005(2) -.009(2) C116 .066(2) .050(2) .074(3) .0076(19) .002(2) .012(2) C12 .041(2) .051(2) .054(2) -.0039(16) .0044(16) -.0008(17) N13 .0356(16) .0455(16) .0580(17) -.0021(12) -.0002(13) -.0067(13) C130 .039(2) .059(2) .073(2) -.0038(17) .0071(18) -.004(2) C131 .041(2) .056(2) .072(2) -.0049(17) -.0041(17) -.011(2) C132 .047(2) .063(2) .077(3) -.0036(18) -.0066(19) -.008(2) O132 .0790(19) .106(2) .0645(17) .0112(16) .0075(14) -.0007(15) C133 .072(3) .089(3) .090(3) -.009(2) -.020(2) .006(3) C134 .082(3) .078(3) .144(4) .000(2) -.040(3) .010(3) C135 .055(3) .088(3) .165(5) .022(2) -.005(3) -.019(3) C136 .055(2) .085(3) .099(3) .012(2) .008(2) -.005(3) C14 .042(2) .054(2) .062(2) -.0027(17) .0022(17) -.0116(18) N15 .0410(16) .0496(17) .0536(17) -.0044(13) .0000(13) -.0046(14) C150 .046(2) .053(2) .068(2) -.0050(17) -.0037(18) .0076(19) C151 .048(2) .0381(19) .059(2) -.0060(15) -.0012(17) -.0017(16) C152 .052(2) .067(2) .068(2) -.0104(19) .0014(18) -.011(2) O152 .0646(17) .130(2) .0755(18) -.0346(17) -.0009(14) -.0360(17) C153 .052(2) .095(3) .085(3) -.016(2) -.011(2) -.011(2) C154 .046(2) .073(3) .109(3) -.008(2) .014(2) .001(2) C155 .071(3) .060(2) .079(3) -.001(2) .010(2) .006(2) C156 .059(2) .050(2) .071(2) -.0040(18) -.0026(19) .004(2) C16 .042(2) .057(2) .048(2) -.0021(16) -.0029(16) .0028(17) N21 .0444(15) .0378(15) .0513(16) -.0001(13) -.0032(13) -.0010(13) C210 .056(2) .045(2) .051(2) -.0088(17) -.0001(17) -.0044(17) C211 .046(2) .038(2) .059(2) -.0077(16) .0053(16) -.0010(16) C212 .048(2) .049(2) .058(2) -.0083(16) .0023(17) .0032(17) O212 .0883(18) .0534(15) .0538(14) -.0038(13) .0005(13) -.0088(12) C213 .062(2) .066(3) .065(2) -.011(2) -.005(2) .011(2) C214 .066(3) .059(2) .099(3) -.002(2) -.004(2) .025(2) C215 .085(3) .044(2) .099(3) .004(2) .014(2) .002(2) C216 .066(2) .047(2) .077(3) -.0049(18) .006(2) -.002(2) C22 .047(2) .042(2) .055(2) .0041(16) -.0004(16) -.0019(17) N23 .0410(16) .0404(16) .0544(17) .0010(12) .0012(13) -.0002(13) C230 .041(2) .060(2) .061(2) .0037(17) .0055(17) .0010(19) C231 .0369(18) .052(2) .059(2) .0003(16) -.0020(16) .0110(17) C232 .045(2) .056(2) .064(2) -.0008(17) -.0072(17) .0030(18) O232 .0634(16) .104(2) .0588(16) -.0188(15) .0079(13) -.0027(15) C233 .057(2) .075(3) .082(3) .001(2) -.015(2) -.012(2) C234 .072(3) .056(2) .132(4) -.004(2) -.039(3) -.005(3) C235 .062(3) .084(3) .105(3) -.019(2) -.007(2) .027(3) C236 .054(2) .080(3) .077(3) -.010(2) -.003(2) .016(2) C24 .048(2) .045(2) .065(2) -.0015(16) -.0014(17) .0066(18) N25 .0432(16) .0430(16) .0581(17) .0031(13) -.0030(13) .0004(13) C250 .049(2) .049(2) .065(2) .0042(17) -.0097(18) -.0077(18) C251 .051(2) .043(2) .057(2) .0002(16) -.0001(17) -.0092(17) C252 .049(2) .050(2) .068(2) .0048(17) -.0050(18) -.0053(18) O252 .0656(17) .0763(17) .0757(17) .0140(14) -.0011(13) .0170(14) C253 .055(2) .076(3) .084(3) .010(2) -.004(2) -.005(2) C254 .054(2) .086(3) .096(3) .001(2) .000(2) -.023(2) C255 .077(3) .103(3) .074(3) -.013(3) .018(2) -.012(3) C256 .058(2) .079(3) .066(2) .001(2) .001(2) -.004(2) C26 .045(2) .046(2) .048(2) -.0006(16) -.0039(15) .0023(16) O01 .23(2) .70(5) .28(2) -.15(2) -.087(17) -.02(3) O02 .238(14) .291(17) .42(2) -.007(11) -.046(14) -.082(14) O03 .228(13) .41(2) .46(2) -.013(13) .032(14) .193(17) C1 .29(2) .102(11) .71(4) .028(12) .05(3) .09(2) C2 .23(2) .25(2) .72(7) -.056(19) -.16(3) .09(3) O2 .222(19) .47(2) .82(5) -.004(16) .16(2) .31(3) O3 .172(12) .243(17) 1.69(9) .014(11) -.21(3) .20(3) C4 .137(14) .163(17) 1.33(10) .003(13) -.13(3) .18(3) C5 .28(2) .170(16) .58(4) -.124(16) -.01(2) -.04(2) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight_atomblock_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type atomblock #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment refined #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 8768(1324) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 4068 #ActaC _refine_ls_number_parameters 837 #ActaC _refine_ls_number_restraints 10 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .124 #ActaC _refine_ls_R_factor_obs .049 #ActaC _refine_ls_wR_factor_all .079 #ActaC _refine_ls_wR_factor_obs .058 #ActaC _refine_ls_goodness_of_fit_all 1.37 #ActaC _refine_ls_goodness_of_fit_obs 1.533 #ActaC _refine_ls_shift/esd_max .123 #ActaC _refine_ls_shift/esd_mean .01 #ActaC _refine_diff_density_min -.165 #ActaC _refine_diff_density_max .209 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC N11 C110 1.477(4) . . ? N11 C12 1.464(4) . . ? N11 C16 1.470(4) . . ? N11 H112 1.77(3) . . ? C110 C111 1.506(4) . . ? C110 H110a .94(2) . . ? C110 H110b 1.07(3) . . ? C111 C112 1.386(4) . . ? C111 C116 1.388(5) . . ? C112 O112 1.371(4) . . ? C112 C113 1.377(5) . . ? O112 H112 .93(3) . . ? C113 C114 1.372(5) . . ? C113 H113 .98(3) . . ? C114 C115 1.368(5) . . ? C114 H114 .95(3) . . ? C115 C116 1.380(5) . . ? C115 H115 .93(3) . . ? C116 H116 .92(2) . . ? C12 N13 1.457(4) . . ? C12 H12a 1.01(2) . . ? C12 H12b 1.02(2) . . ? N13 C130 1.476(4) . . ? N13 C14 1.469(4) . . ? N13 H132 1.67(3) . . ? C130 C131 1.502(5) . . ? C130 H130a 1.08(3) . . ? C130 H130b .99(3) . . ? C131 C132 1.391(5) . . ? C131 C136 1.382(5) . . ? C132 O132 1.357(4) . . ? C132 C133 1.384(5) . . ? O132 H132 1.09(3) . . ? C133 C134 1.360(6) . . ? C133 H133 1.06(3) . . ? C134 C135 1.352(7) . . ? C134 H134 .91(4) . . ? C135 C136 1.388(6) . . ? C135 H135 .92(3) . . ? C136 H136 .99(3) . . ? C14 N15 1.458(4) . . ? C14 H14a 1.05(3) . . ? C14 H14b .98(2) . . ? N15 C150 1.456(4) . . ? N15 C16 1.449(4) . . ? N15 H152 1.88(4) . . ? C150 C151 1.511(4) . . ? C150 H150a .91(3) . . ? C150 H150b 1.11(3) . . ? C151 C152 1.377(5) . . ? C151 C156 1.372(5) . . ? C152 O152 1.367(4) . . ? C152 C153 1.392(5) . . ? O152 H152 .92(4) . . ? C153 C154 1.351(6) . . ? C153 H153 .84(3) . . ? C154 C155 1.357(5) . . ? C154 H154 .91(3) . . ? C155 C156 1.380(5) . . ? C155 H155 .98(3) . . ? C156 H156 .99(3) . . ? C16 H16a 1.04(2) . . ? C16 H16b .98(3) . . ? N21 C210 1.478(4) . . ? N21 C22 1.465(4) . . ? N21 C26 1.464(4) . . ? N21 H212 1.47(4) . . ? C210 C211 1.511(4) . . ? C210 H210a 1.02(3) . . ? C210 H210b .94(2) . . ? C211 C212 1.386(4) . . ? C211 C216 1.391(4) . . ? C212 O212 1.367(4) . . ? C212 C213 1.385(5) . . ? O212 H212 1.27(4) . . ? C213 C214 1.373(5) . . ? C213 H213 .94(3) . . ? C214 C215 1.365(6) . . ? C214 H214 .98(3) . . ? C215 C216 1.384(5) . . ? C215 H215 .98(3) . . ? C216 H216 1.01(3) . . ? C22 N23 1.464(4) . . ? C22 H22a .95(2) . . ? C22 H22b 1.07(2) . . ? N23 C230 1.477(4) . . ? N23 C24 1.471(4) . . ? N23 H230a 1.91(3) . . ? N23 H232 1.69(4) . . ? C230 C231 1.504(4) . . ? C230 H230a .89(3) . . ? C230 H230b 1.07(3) . . ? C231 C232 1.387(5) . . ? C231 C236 1.385(5) . . ? C232 O232 1.361(4) . . ? C232 C233 1.380(5) . . ? O232 H232 1.02(4) . . ? C233 C234 1.372(5) . . ? C233 H233 1.02(3) . . ? C234 C235 1.359(6) . . ? C234 H234 .87(3) . . ? C235 C236 1.392(5) . . ? C235 H235 .97(4) . . ? C236 H236 1.07(3) . . ? C24 N25 1.458(4) . . ? C24 H24a .95(3) . . ? C24 H24b 1.05(3) . . ? N25 C250 1.469(4) . . ? N25 C26 1.451(4) . . ? N25 H252 1.70(5) . . ? C250 C251 1.503(4) . . ? C250 H250a 1.01(3) . . ? C250 H250b .96(3) . . ? C251 C252 1.399(4) . . ? C251 C256 1.372(5) . . ? C252 O252 1.358(4) . . ? C252 C253 1.386(5) . . ? O252 H252 1.10(5) . . ? C253 C254 1.365(5) . . ? C253 H253 1.00(3) . . ? C254 C255 1.366(5) . . ? C254 H254 .95(3) . . ? C255 C256 1.390(5) . . ? C255 H255 .92(3) . . ? C256 H256 1.03(3) . . ? C26 H26a .99(3) . . ? C26 H26b 1.05(2) . . ? O01 O02 1.108(14) . . ? O01 O03 1.737(15) . . ? O01 C5 2.00(2) . . ? O01 H5c 1.2776(6) . . ? O01 O02 1.108(14) . 3_766 ? O01 O03 1.737(15) . 3_766 ? O01 C5 2.00(2) . 3_766 ? O01 H5c 1.2776(6) . 3_766 ? O02 C5 1.64(2) . . ? O02 H5b 1.599(13) . . ? O02 H5c 1.370(13) . . ? O02 O03 1.92(2) . 3_766 ? O03 C5 1.40(3) . . ? O03 H5a 1.304(16) . . ? O03 H5c .913(14) . . ? C1 C2 1.50(2) . . ? C1 H1a .921(16) . . ? C1 H1b 1.207(16) . . ? C1 H1c .742(19) . . ? C1 C2 1.58(2) . 2_756 ? C1 O2 1.68(2) . 2_756 ? C2 O2 1.11(2) . . ? C2 O3 1.43(2) . . ? C2 C2 1.852(14) . 2_756 ? C2 O2 1.736(18) . 2_756 ? C2 H1c 1.358(13) . 2_756 ? O2 O2 1.51(2) . 2_756 ? O3 C4 1.40(3) . . ? C4 C5 1.56(3) . . ? C4 H4a .843(13) . . ? C4 H4b 1.096(18) . . ? C5 H5a 1.066(17) . . ? C5 H5b 1.020(17) . . ? C5 H5c .93(2) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC N11 C111 2.473(4) . . ? N11 C112 2.901(4) . . ? N11 O112 2.637(4) . . ? N11 N13 2.364(3) . . ? N11 C14 2.794(4) . . ? N11 N15 2.412(4) . . ? N11 C150 3.041(4) . . ? N11 H110a 1.99(2) . . ? N11 H110b 2.01(3) . . ? N11 H12a 2.07(2) . . ? N11 H12b 2.03(2) . . ? N11 H150b 2.78(3) . . ? N11 H16a 2.01(2) . . ? N11 H16b 2.02(3) . . ? C110 C112 2.516(5) . . ? C110 O112 2.877(4) . . ? C110 C116 2.523(5) . . ? C110 C12 2.433(5) . . ? C110 C16 2.438(5) . . ? C110 H112 2.30(3) . . ? C110 H116 2.65(2) . . ? C110 H12b 2.61(3) . . ? C110 H16a 2.59(2) . . ? C110 H16b 2.68(3) . . ? C111 O112 2.404(4) . . ? C111 C113 2.404(5) . . ? C111 C114 2.778(5) . . ? C111 C115 2.414(5) . . ? C111 H110a 2.05(2) . . ? C111 H110b 2.08(3) . . ? C111 H112 2.33(3) . . ? C111 H116 2.00(2) . . ? C111 H12b 2.63(3) . . ? C112 C114 2.381(5) . . ? C112 C115 2.751(5) . . ? C112 C116 2.374(5) . . ? C112 H112 1.82(3) . . ? C112 H113 2.06(3) . . ? O112 C113 2.350(4) . . ? O112 H113 2.54(3) . . ? O112 H22b 2.45(2) . 4_564 ? C113 C115 2.376(5) . . ? C113 C116 2.740(5) . . ? C113 H114 2.05(3) . . ? C114 C116 2.375(5) . . ? C114 H113 2.04(3) . . ? C114 H115 2.00(3) . . ? C115 H114 1.98(3) . . ? C115 H116 2.01(2) . . ? C116 H110a 2.63(2) . . ? C116 H115 2.03(3) . . ? C12 C130 2.413(4) . . ? C12 C14 2.386(5) . . ? C12 N15 2.822(4) . . ? C12 C16 2.391(4) . . ? C12 H110a 2.58(2) . . ? C12 H112 2.61(3) . . ? C12 H130b 2.35(3) . . ? C12 H132 2.64(3) . . ? C12 H14a 2.57(3) . . ? C12 H16b 2.59(3) . . ? N13 C131 2.488(4) . . ? N13 C132 2.939(4) . . ? N13 O132 2.687(4) . . ? N13 N15 2.415(3) . . ? N13 C150 3.034(4) . . ? N13 C16 2.792(4) . . ? N13 H12a 2.02(2) . . ? N13 H12b 2.02(3) . . ? N13 H130a 2.12(3) . . ? N13 H130b 1.96(3) . . ? N13 H14a 2.04(3) . . ? N13 H14b 1.98(2) . . ? C130 C132 2.519(5) . . ? C130 O132 2.888(4) . . ? C130 C136 2.509(5) . . ? C130 C14 2.436(4) . . ? C130 H12a 2.63(2) . . ? C130 H12b 2.58(3) . . ? C130 H132 2.22(4) . . ? C130 H136 2.62(3) . . ? C130 H14a 2.66(3) . . ? C130 H14b 2.55(3) . . ? C131 O132 2.403(4) . . ? C131 C133 2.409(5) . . ? C131 C134 2.766(5) . . ? C131 C135 2.415(5) . . ? C131 H130a 2.14(3) . . ? C131 H130b 2.10(3) . . ? C131 H132 2.33(4) . . ? C131 H136 2.02(3) . . ? C132 C134 2.374(5) . . ? C132 C135 2.753(6) . . ? C132 C136 2.374(5) . . ? C132 H132 1.90(4) . . ? C132 H133 2.08(3) . . ? O132 C133 2.345(5) . . ? O132 H133 2.49(3) . . ? O132 H230b 2.69(3) . 4_564 ? C133 C135 2.365(6) . . ? C133 C136 2.738(6) . . ? C133 H134 1.92(4) . . ? C134 C136 2.363(6) . . ? C134 H133 2.14(3) . . ? C134 H135 2.05(3) . . ? C135 H134 2.01(4) . . ? C135 H136 2.10(3) . . ? C136 H130a 2.63(3) . . ? C136 H135 1.94(3) . . ? C14 C150 2.432(5) . . ? C14 C16 2.386(4) . . ? C14 H12a 2.58(2) . . ? C14 H130a 2.60(3) . . ? C14 H150a 2.55(3) . . ? C14 H16b 2.58(3) . . ? N15 C151 2.485(4) . . ? N15 C152 2.948(4) . . ? N15 O152 2.728(4) . . ? N15 H14a 2.05(3) . . ? N15 H14b 2.05(3) . . ? N15 H150a 1.97(3) . . ? N15 H150b 2.16(3) . . ? N15 H16a 2.05(2) . . ? N15 H16b 1.97(3) . . ? C150 C152 2.536(5) . . ? C150 O152 2.936(4) . . ? C150 C156 2.494(5) . . ? C150 C16 2.434(5) . . ? C150 H14b 2.59(3) . . ? C150 H152 2.40(4) . . ? C150 H156 2.62(3) . . ? C150 H16a 2.55(2) . . ? C151 O152 2.409(4) . . ? C151 C153 2.400(5) . . ? C151 C154 2.771(5) . . ? C151 C155 2.410(5) . . ? C151 H150a 1.98(3) . . ? C151 H150b 2.07(3) . . ? C151 H152 2.36(4) . . ? C151 H156 2.03(3) . . ? C151 H16a 2.61(2) . . ? C152 C154 2.383(5) . . ? C152 C155 2.747(5) . . ? C152 C156 2.351(5) . . ? C152 H152 1.83(4) . . ? C152 H153 1.92(3) . . ? O152 C153 2.354(5) . . ? O152 O212 3.103(4) . . ? O152 H110a 2.75(2) . 6_655 ? O152 H153 2.43(3) . . ? C153 C155 2.350(5) . . ? C153 C156 2.711(5) . . ? C153 H154 1.96(3) . . ? C154 C156 2.359(5) . . ? C154 H153 1.94(3) . . ? C154 H155 2.08(3) . . ? C155 H154 1.98(3) . . ? C155 H156 2.06(3) . . ? C156 H150b 2.49(3) . . ? C156 H155 2.01(3) . . ? C16 H110a 2.66(3) . . ? C16 H110b 2.53(3) . . ? C16 H12a 2.62(2) . . ? C16 H14a 2.62(3) . . ? C16 H152 2.55(4) . . ? N21 C211 2.482(4) . . ? N21 C212 2.918(4) . . ? N21 O212 2.648(4) . . ? N21 N23 2.366(3) . . ? N21 C24 2.781(4) . . ? N21 N25 2.401(4) . . ? N21 C250 3.011(4) . . ? N21 H210a 1.97(3) . . ? N21 H210b 2.03(2) . . ? N21 H22a 2.02(2) . . ? N21 H22b 2.08(2) . . ? N21 H250a 2.79(3) . . ? N21 H26a 1.97(3) . . ? N21 H26b 2.08(2) . . ? C210 C212 2.528(5) . . ? C210 O212 2.889(4) . . ? C210 C216 2.515(5) . . ? C210 C22 2.432(4) . . ? C210 C26 2.437(4) . . ? C210 H212 2.19(4) . . ? C210 H216 2.67(3) . . ? C210 H22a 2.62(2) . . ? C210 H26a 2.54(3) . . ? C211 O212 2.400(4) . . ? C211 C213 2.404(5) . . ? C211 C214 2.774(5) . . ? C211 C215 2.417(5) . . ? C211 H210a 2.05(3) . . ? C211 H210b 2.06(2) . . ? C211 H212 2.40(4) . . ? C211 H216 2.07(3) . . ? C212 C214 2.389(5) . . ? C212 C215 2.765(5) . . ? C212 C216 2.384(5) . . ? C212 H212 2.06(4) . . ? C212 H213 2.04(3) . . ? O212 C213 2.363(4) . . ? O212 H152 2.61(4) . . ? O212 H213 2.57(3) . . ? C213 C215 2.381(5) . . ? C213 C216 2.746(5) . . ? C213 H214 2.08(3) . . ? C214 C216 2.374(5) . . ? C214 H213 1.99(3) . . ? C214 H215 2.11(3) . . ? C215 H214 2.01(3) . . ? C215 H216 2.08(3) . . ? C216 H210b 2.60(2) . . ? C216 H215 1.98(3) . . ? C22 C230 2.419(4) . . ? C22 C24 2.386(4) . . ? C22 N25 2.826(4) . . ? C22 C26 2.392(4) . . ? C22 H210b 2.63(2) . . ? C22 H212 2.33(4) . . ? C22 H230a 2.39(3) . . ? C22 H24b 2.58(3) . . ? C22 H26b 2.63(2) . . ? N23 C231 2.471(4) . . ? N23 C232 2.909(4) . . ? N23 O232 2.658(4) . . ? N23 N25 2.419(3) . . ? N23 C250 3.029(4) . . ? N23 C26 2.798(4) . . ? N23 H22a 1.96(2) . . ? N23 H22b 2.10(2) . . ? N23 H230b 2.08(3) . . ? N23 H24a 1.98(3) . . ? N23 H24b 2.03(3) . . ? C230 C232 2.515(5) . . ? C230 O232 2.877(4) . . ? C230 C236 2.510(5) . . ? C230 C24 2.436(4) . . ? C230 H22a 2.53(2) . . ? C230 H232 2.24(4) . . ? C230 H236 2.62(3) . . ? C230 H24a 2.58(3) . . ? C230 H24b 2.61(3) . . ? C231 O232 2.400(4) . . ? C231 C233 2.403(5) . . ? C231 C234 2.761(5) . . ? C231 C235 2.422(5) . . ? C231 H230a 2.01(3) . . ? C231 H230b 2.16(3) . . ? C231 H232 2.30(4) . . ? C231 H236 2.08(3) . . ? C232 C234 2.377(5) . . ? C232 C235 2.768(5) . . ? C232 C236 2.379(5) . . ? C232 H232 1.84(4) . . ? C232 H233 2.06(3) . . ? O232 C233 2.346(4) . . ? O232 H12a 2.68(2) . . ? O232 H233 2.50(3) . . ? C233 C235 2.387(6) . . ? C233 C236 2.745(5) . . ? C233 H234 1.92(3) . . ? C234 C236 2.363(6) . . ? C234 H233 2.11(3) . . ? C234 H235 2.17(4) . . ? C235 H234 1.96(3) . . ? C235 H236 2.18(3) . . ? C236 H230b 2.67(3) . . ? C236 H235 1.88(4) . . ? C24 C250 2.446(5) . . ? C24 C26 2.379(4) . . ? C24 H22b 2.62(2) . . ? C24 H230b 2.54(3) . . ? C24 H232 2.68(4) . . ? C24 H250b 2.54(3) . . ? C24 H26b 2.62(2) . . ? N25 C251 2.468(4) . . ? N25 C252 2.945(4) . . ? N25 O252 2.732(3) . . ? N25 H24a 2.00(3) . . ? N25 H24b 2.09(3) . . ? N25 H250a 2.11(3) . . ? N25 H250b 2.00(3) . . ? N25 H26a 2.04(3) . . ? N25 H26b 2.03(2) . . ? C250 C252 2.529(5) . . ? C250 O252 2.888(4) . . ? C250 C256 2.499(5) . . ? C250 C26 2.439(4) . . ? C250 H24a 2.58(3) . . ? C250 H252 2.26(5) . . ? C250 H256 2.61(3) . . ? C250 H26a 2.59(3) . . ? C251 O252 2.403(4) . . ? C251 C253 2.423(5) . . ? C251 C254 2.770(5) . . ? C251 C255 2.408(5) . . ? C251 H250a 2.08(3) . . ? C251 H250b 2.04(3) . . ? C251 H252 2.33(5) . . ? C251 H256 2.04(3) . . ? C251 H26a 2.65(3) . . ? C252 C254 2.373(5) . . ? C252 C255 2.752(5) . . ? C252 C256 2.375(5) . . ? C252 H252 1.90(5) . . ? C252 H253 2.05(3) . . ? O252 O252 2.938(4) . 7_656 ? O252 C253 2.349(4) . . ? O252 H155 2.72(3) . 4_565 ? O252 H252 2.69(5) . 7_656 ? O252 H253 2.49(3) . . ? C253 C255 2.381(6) . . ? C253 C256 2.755(5) . . ? C253 H254 1.96(3) . . ? C254 C256 2.377(5) . . ? C254 H253 2.10(3) . . ? C254 H255 2.06(3) . . ? C255 H254 2.06(3) . . ? C255 H256 2.13(3) . . ? C256 H250a 2.57(3) . . ? C256 H255 1.95(3) . . ? C26 H210a 2.50(3) . . ? C26 H210b 2.70(2) . . ? C26 H212 2.57(4) . . ? C26 H22b 2.61(2) . . ? C26 H24b 2.66(3) . . ? C26 H252 2.53(5) . . ? O01 H5a 2.6232(11) . 3_766 ? O01 H5a 2.6232(11) . . ? O01 H5b 2.0242(8) . . ? O01 H5b 2.0242(8) . 3_766 ? O02 O02 2.22(2) . 3_766 ? O02 O03 2.19(2) . . ? O02 C4 2.41(3) . . ? O02 C5 2.78(3) . 3_766 ? O02 H4a 2.233(15) . . ? O02 H5a 2.597(13) . . ? O02 H5c 1.960(15) . 3_766 ? O03 C4 2.82(3) . . ? O03 H5b 1.949(16) . . ? C1 C1 2.01(2) . 2_756 ? C1 O2 2.25(2) . . ? C1 O3 2.52(3) . . ? C1 O3 2.77(2) . 2_756 ? C1 H1b 2.320(16) . 2_756 ? C1 H1c 1.979(18) . 2_756 ? C2 C4 2.33(3) . . ? C2 H1a 2.302(12) . 2_756 ? C2 H1a 1.853(12) . . ? C2 H1b 2.558(12) . 2_756 ? C2 H1b 1.947(13) . . ? C2 H1c 2.026(11) . . ? C2 H4a 2.658(11) . . ? C2 H4b 2.525(11) . . ? O2 O3 2.20(2) . . ? O2 O3 2.99(2) . 2_756 ? O2 C4 2.82(3) . . ? O2 H1a 2.655(15) . . ? O2 H1a 1.971(15) . 2_756 ? O2 H1c 2.578(15) . . ? O2 H1c 1.849(16) . 2_756 ? O3 C5 2.41(3) . . ? O3 H1a 2.45(2) . . ? O3 H1b 2.430(18) . . ? O3 H1c 2.246(15) . 2_756 ? O3 H4a 2.056(14) . . ? O3 H4b 1.872(14) . . ? O3 H5a 2.60(2) . . ? O3 H5b 2.74(2) . . ? C4 H1c 2.47(2) . 2_756 ? C4 H5a 2.253(17) . . ? C4 H5b 2.14(2) . . ? C4 H5c 2.21(2) . . ? C5 H4a 2.012(19) . . ? C5 H4b 2.04(2) . . ? H110a H110b 1.68(4) . . ? H110b H16a 2.24(4) . . ? H113 H114 2.36(4) . . ? H114 H115 2.25(4) . . ? H115 H116 2.33(4) . . ? H12a H12b 1.68(3) . . ? H12a H14a 2.34(4) . . ? H12b H130b 2.14(4) . . ? H130a H130b 1.63(4) . . ? H130a H136 2.33(4) . . ? H130a H14a 2.39(4) . . ? H133 H134 2.33(5) . . ? H133 H236 2.13(4) . 4_564 ? H135 H136 2.29(4) . . ? H14a H14b 1.67(4) . . ? H14b H150a 2.34(4) . . ? H150a H150b 1.62(4) . . ? H150b H156 2.21(4) . . ? H153 H154 2.25(4) . . ? H154 H155 2.38(4) . . ? H155 H156 2.30(5) . . ? H16a H16b 1.69(4) . . ? H210a H210b 1.61(4) . . ? H210a H26a 2.19(4) . . ? H210b H216 2.40(4) . . ? H212 H250a 2.32(5) . . ? H213 H214 2.34(4) . . ? H215 H216 2.27(4) . . ? H22a H22b 1.66(3) . . ? H22a H230a 2.17(4) . . ? H22b H24b 2.36(4) . . ? H22b H26b 2.40(3) . . ? H230a H230b 1.59(4) . . ? H230b H236 2.35(4) . . ? H230b H24b 2.28(4) . . ? H233 H234 2.32(4) . . ? H235 H236 2.23(5) . . ? H24a H24b 1.62(4) . . ? H24a H250b 2.31(4) . . ? H250a H250b 1.51(4) . . ? H250a H256 2.27(4) . . ? H253 H254 2.32(4) . . ? H255 H256 2.32(4) . . ? H26a H26b 1.67(4) . . ? H1a H1b 1.5513(5) . . ? H1a H1c 1.5313(5) . . ? H1b H1b 2.3802(10) . 2_756 ? H1b H1c 1.5312(7) . . ? H1b H1c 1.9483(8) . 2_756 ? H1c H1c 2.1381(10) . 2_756 ? H1c H4b 2.1875(13) . 2_756 ? H4a H4b 1.5513(6) . . ? H5a H5b 1.5513(6) . . ? H5a H5c 1.5540(6) . . ? H5b H5c 1.5540(6) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC C110 N11 C12 111.7(2) . . . ? C110 N11 C16 111.7(2) . . . ? C110 N11 H112 89.8(10) . . . ? C12 N11 C16 109.2(2) . . . ? C12 N11 H112 107.1(10) . . . ? C16 N11 H112 125.8(10) . . . ? N11 C110 C111 112.0(2) . . . ? N11 C110 H110a 108.5(15) . . . ? N11 C110 H110b 103.5(16) . . . ? C111 C110 H110a 112.2(15) . . . ? C111 C110 H110b 107.0(16) . . . ? H110a C110 H110b 113(2) . . . ? C110 C111 C112 120.9(3) . . . ? C110 C111 C116 121.3(3) . . . ? C112 C111 C116 117.7(3) . . . ? C111 C112 O112 121.4(3) . . . ? C111 C112 C113 121.0(3) . . . ? O112 C112 C113 117.6(3) . . . ? C112 O112 H112 103(2) . . . ? C112 C113 C114 120.1(3) . . . ? C112 C113 H113 120.9(19) . . . ? C114 C113 H113 118.9(19) . . . ? C113 C114 C115 120.3(3) . . . ? C113 C114 H114 122.8(17) . . . ? C115 C114 H114 116.9(17) . . . ? C114 C115 C116 119.6(3) . . . ? C114 C115 H115 119(2) . . . ? C116 C115 H115 121(2) . . . ? C111 C116 C115 121.4(3) . . . ? C111 C116 H116 118.3(15) . . . ? C115 C116 H116 120.3(15) . . . ? N11 C12 N13 108.1(2) . . . ? N11 C12 H12a 112.5(14) . . . ? N11 C12 H12b 108.0(15) . . . ? N13 C12 H12a 108.8(14) . . . ? N13 C12 H12b 107.8(14) . . . ? H12a C12 H12b 111(2) . . . ? C12 N13 C130 110.7(2) . . . ? C12 N13 C14 109.3(2) . . . ? C12 N13 H132 115.1(12) . . . ? C130 N13 C14 111.6(2) . . . ? C130 N13 H132 89.7(13) . . . ? C14 N13 H132 118.9(12) . . . ? N13 C130 C131 113.4(3) . . . ? N13 C130 H130a 111.3(13) . . . ? N13 C130 H130b 103.7(16) . . . ? C131 C130 H130a 111.0(14) . . . ? C131 C130 H130b 113.5(15) . . . ? H130a C130 H130b 103(2) . . . ? C130 C131 C132 121.0(3) . . . ? C130 C131 C136 120.9(3) . . . ? C132 C131 C136 117.8(3) . . . ? C131 C132 O132 121.9(3) . . . ? C131 C132 C133 120.5(3) . . . ? O132 C132 C133 117.6(3) . . . ? C132 O132 H132 102(2) . . . ? C132 C133 C134 119.8(4) . . . ? C132 C133 H133 116.0(17) . . . ? C134 C133 H133 124.1(17) . . . ? C133 C134 C135 121.4(4) . . . ? C133 C134 H134 114(2) . . . ? C135 C134 H134 124(2) . . . ? C134 C135 C136 119.2(4) . . . ? C134 C135 H135 128(2) . . . ? C136 C135 H135 113(2) . . . ? C131 C136 C135 121.4(4) . . . ? C131 C136 H136 115.8(17) . . . ? C135 C136 H136 122.8(17) . . . ? N13 C14 N15 111.1(2) . . . ? N13 C14 H14a 107.4(16) . . . ? N13 C14 H14b 105.9(14) . . . ? N15 C14 H14a 108.4(16) . . . ? N15 C14 H14b 112.7(15) . . . ? H14a C14 H14b 111(2) . . . ? C14 N15 C150 113.1(2) . . . ? C14 N15 C16 110.3(2) . . . ? C14 N15 H152 127.6(13) . . . ? C150 N15 C16 113.8(2) . . . ? C150 N15 H152 91.1(12) . . . ? C16 N15 H152 99.3(12) . . . ? N15 C150 C151 113.7(3) . . . ? N15 C150 H150a 110.9(18) . . . ? N15 C150 H150b 114.5(15) . . . ? C151 C150 H150a 106.8(18) . . . ? C151 C150 H150b 103.6(15) . . . ? H150a C150 H150b 107(2) . . . ? C150 C151 C152 122.7(3) . . . ? C150 C151 C156 119.6(3) . . . ? C152 C151 C156 117.6(3) . . . ? C151 C152 O152 122.7(3) . . . ? C151 C152 C153 120.1(3) . . . ? O152 C152 C153 117.1(3) . . . ? C152 O152 H152 104(2) . . . ? C152 C153 C154 120.6(3) . . . ? C152 C153 H153 116(2) . . . ? C154 C153 H153 123(2) . . . ? C153 C154 C155 120.4(3) . . . ? C153 C154 H154 119.0(17) . . . ? C155 C154 H154 120.6(17) . . . ? C154 C155 C156 119.0(3) . . . ? C154 C155 H155 125(2) . . . ? C156 C155 H155 115(2) . . . ? C151 C156 C155 122.3(3) . . . ? C151 C156 H156 117.5(18) . . . ? C155 C156 H156 120.2(18) . . . ? N11 C16 N15 111.5(2) . . . ? N11 C16 H16a 105.4(13) . . . ? N11 C16 H16b 110.1(15) . . . ? N15 C16 H16a 109.5(14) . . . ? N15 C16 H16b 106.7(16) . . . ? H16a C16 H16b 114(2) . . . ? C210 N21 C22 111.4(2) . . . ? C210 N21 C26 111.8(2) . . . ? C210 N21 H212 95.7(15) . . . ? C22 N21 C26 109.5(2) . . . ? C22 N21 H212 105.0(15) . . . ? C26 N21 H212 122.6(15) . . . ? N21 C210 C211 112.2(2) . . . ? N21 C210 H210a 102.6(15) . . . ? N21 C210 H210b 111.7(14) . . . ? C211 C210 H210a 107.2(15) . . . ? C211 C210 H210b 111.8(14) . . . ? H210a C210 H210b 111(2) . . . ? C210 C211 C212 121.5(3) . . . ? C210 C211 C216 120.1(3) . . . ? C212 C211 C216 118.3(3) . . . ? C211 C212 O212 121.3(3) . . . ? C211 C212 C213 120.4(3) . . . ? O212 C212 C213 118.3(3) . . . ? C212 O212 H212 103.1(18) . . . ? C212 C213 C214 120.0(3) . . . ? C212 C213 H213 122.3(18) . . . ? C214 C213 H213 117.7(18) . . . ? C213 C214 C215 120.7(3) . . . ? C213 C214 H214 122.6(17) . . . ? C215 C214 H214 116.6(17) . . . ? C214 C215 C216 119.4(3) . . . ? C214 C215 H215 127.9(19) . . . ? C216 C215 H215 112.6(19) . . . ? C211 C216 C215 121.2(3) . . . ? C211 C216 H216 118.7(17) . . . ? C215 C216 H216 120.1(17) . . . ? N21 C22 N23 107.8(2) . . . ? N21 C22 H22a 111.5(15) . . . ? N21 C22 H22b 109.5(13) . . . ? N23 C22 H22a 106.9(15) . . . ? N23 C22 H22b 110.9(13) . . . ? H22a C22 H22b 110(2) . . . ? C22 N23 C230 110.7(2) . . . ? C22 N23 C24 108.8(2) . . . ? C22 N23 H230a 89.1(8) . . . ? C22 N23 H232 118.6(14) . . . ? C230 N23 C24 111.4(2) . . . ? C230 N23 H230a 26.9(8) . . . ? C230 N23 H232 90.0(15) . . . ? C24 N23 H230a 136.1(8) . . . ? C24 N23 H232 116.0(14) . . . ? H230a N23 H232 86.6(16) . . . ? N23 C230 C231 112.0(3) . . . ? N23 C230 H230a 104.6(18) . . . ? N23 C230 H230b 108.2(14) . . . ? C231 C230 H230a 111.6(17) . . . ? C231 C230 H230b 112.8(14) . . . ? H230a C230 H230b 107(2) . . . ? C230 C231 C232 120.9(3) . . . ? C230 C231 C236 120.7(3) . . . ? C232 C231 C236 118.2(3) . . . ? C231 C232 O232 121.7(3) . . . ? C231 C232 C233 120.6(3) . . . ? O232 C232 C233 117.7(3) . . . ? C232 O232 H232 100(2) . . . ? C232 C233 C234 119.5(4) . . . ? C232 C233 H233 117.3(17) . . . ? C234 C233 H233 123.1(17) . . . ? C233 C234 C235 121.8(4) . . . ? C233 C234 H234 116.2(18) . . . ? C235 C234 H234 122.0(18) . . . ? C234 C235 C236 118.4(4) . . . ? C234 C235 H235 137(2) . . . ? C236 C235 H235 104(2) . . . ? C231 C236 C235 121.5(3) . . . ? C231 C236 H236 114.7(17) . . . ? C235 C236 H236 123.8(17) . . . ? N23 C24 N25 111.4(2) . . . ? N23 C24 H24a 108.1(15) . . . ? N23 C24 H24b 106.3(16) . . . ? N25 C24 H24a 110.7(15) . . . ? N25 C24 H24b 111.8(15) . . . ? H24a C24 H24b 108(2) . . . ? C24 N25 C250 113.4(2) . . . ? C24 N25 C26 109.8(2) . . . ? C24 N25 H252 122.4(16) . . . ? C250 N25 C26 113.3(2) . . . ? C250 N25 H252 90.3(16) . . . ? C26 N25 H252 106.5(16) . . . ? N25 C250 C251 112.3(2) . . . ? N25 C250 H250a 114.9(15) . . . ? N25 C250 H250b 109.0(17) . . . ? C251 C250 H250a 110.3(15) . . . ? C251 C250 H250b 109.8(18) . . . ? H250a C250 H250b 100(2) . . . ? C250 C251 C252 121.3(3) . . . ? C250 C251 C256 120.7(3) . . . ? C252 C251 C256 118.0(3) . . . ? C251 C252 O252 121.4(3) . . . ? C251 C252 C253 120.9(3) . . . ? O252 C252 C253 117.7(3) . . . ? C252 O252 H252 101(2) . . . ? C252 C253 C254 119.2(3) . . . ? C252 C253 H253 117.0(19) . . . ? C254 C253 H253 123.9(19) . . . ? C253 C254 C255 121.4(3) . . . ? C253 C254 H254 114.5(18) . . . ? C255 C254 H254 124.0(18) . . . ? C254 C255 C256 119.2(4) . . . ? C254 C255 H255 127(2) . . . ? C256 C255 H255 114(2) . . . ? C251 C256 C255 121.3(3) . . . ? C251 C256 H256 115.7(16) . . . ? C255 C256 H256 122.9(16) . . . ? N21 C26 N25 110.9(2) . . . ? N21 C26 H26a 105.3(15) . . . ? N21 C26 H26b 110.9(13) . . . ? N25 C26 H26a 112.0(16) . . . ? N25 C26 H26b 108.0(13) . . . ? H26a C26 H26b 110(2) . . . ? O02 O01 O03 98.5(9) . . . ? O02 O01 C5 55.5(9) . . . ? O02 O01 H5c 69.7(7) . . . ? O02 O01 O02 180.0000 . . 3_766 ? O02 O01 O03 81.5(9) . . 3_766 ? O02 O01 C5 124.5(9) . . 3_766 ? O02 O01 H5c 110.3(7) . . 3_766 ? O03 O01 C5 43.5(7) . . . ? O03 O01 H5c 30.7(5) . . . ? O03 O01 O02 81.5(9) . . 3_766 ? O03 O01 O03 180.0000 . . 3_766 ? O03 O01 C5 136.5(7) . . 3_766 ? O03 O01 H5c 149.3(5) . . 3_766 ? C5 O01 H5c 21.5(5) . . . ? C5 O01 O02 124.5(9) . . 3_766 ? C5 O01 O03 136.5(7) . . 3_766 ? C5 O01 C5 180.0000 . . 3_766 ? C5 O01 H5c 158.5(5) . . 3_766 ? H5c O01 O02 110.3(7) . . 3_766 ? H5c O01 O03 149.3(5) . . 3_766 ? H5c O01 C5 158.5(5) . . 3_766 ? H5c O01 H5c 180.0000 . . 3_766 ? O02 O01 O03 98.5(9) 3_766 . 3_766 ? O02 O01 C5 55.5(9) 3_766 . 3_766 ? O02 O01 H5c 69.7(7) 3_766 . 3_766 ? O03 O01 C5 43.5(7) 3_766 . 3_766 ? O03 O01 H5c 30.7(5) 3_766 . 3_766 ? C5 O01 H5c 21.5(5) 3_766 . 3_766 ? O01 O02 C5 90.8(11) . . . ? O01 O02 H5b 95.1(8) . . . ? O01 O02 H5c 61.0(6) . . . ? O01 O02 O03 63.6(8) . . 3_766 ? C5 O02 H5b 36.6(7) . . . ? C5 O02 H5c 34.5(7) . . . ? C5 O02 O03 153.4(12) . . 3_766 ? H5b O02 H5c 62.6(5) . . . ? H5b O02 O03 133.2(9) . . 3_766 ? H5c O02 O03 123.6(10) . . 3_766 ? O01 O03 C5 78.1(11) . . . ? O01 O03 H5a 118.5(11) . . . ? O01 O03 H5c 45.6(7) . . . ? O01 O03 O02 34.8(5) . . 3_766 ? C5 O03 H5a 46.2(9) . . . ? C5 O03 H5c 41.0(10) . . . ? C5 O03 O02 112.5(13) . . 3_766 ? H5a O03 H5c 87.1(12) . . . ? H5a O03 O02 144.9(12) . . 3_766 ? H5c O03 O02 79.0(11) . . 3_766 ? C2 C1 H1a 97.1(15) . . . ? C2 C1 H1b 91.4(13) . . . ? C2 C1 H1c 126.0(17) . . . ? C2 C1 C2 74.0(9) . . 2_756 ? C2 C1 O2 65.8(9) . . 2_756 ? H1a C1 H1b 92.6(14) . . . ? H1a C1 H1c 134(2) . . . ? H1a C1 C2 132.7(14) . . 2_756 ? H1a C1 O2 93.7(11) . . 2_756 ? H1b C1 H1c 100.8(13) . . . ? H1b C1 C2 133.1(13) . . 2_756 ? H1b C1 O2 156.9(16) . . 2_756 ? H1c C1 C2 59.3(11) . . 2_756 ? H1c C1 O2 90.7(15) . . 2_756 ? C2 C1 O2 39.8(8) 2_756 . 2_756 ? C1 C2 O2 118.3(12) . . . ? C1 C2 O3 118.2(12) . . . ? C1 C2 C1 81.6(11) . . 2_756 ? C1 C2 C2 54.9(8) . . 2_756 ? C1 C2 O2 62.3(9) . . 2_756 ? C1 C2 H1c 87.6(9) . . 2_756 ? O2 C2 O3 119.0(13) . . . ? O2 C2 C1 75.3(11) . . 2_756 ? O2 C2 C2 66.3(10) . . 2_756 ? O2 C2 O2 59.5(10) . . 2_756 ? O2 C2 H1c 96.3(12) . . 2_756 ? O3 C2 C1 133.8(12) . . 2_756 ? O3 C2 C2 172.6(11) . . 2_756 ? O3 C2 O2 140.5(11) . . 2_756 ? O3 C2 H1c 107.1(9) . . 2_756 ? C1 C2 C2 51.1(9) 2_756 . 2_756 ? C1 C2 O2 85.5(10) 2_756 . 2_756 ? C1 C2 H1c 28.0(7) 2_756 . 2_756 ? C2 C2 O2 36.0(7) 2_756 . 2_756 ? C2 C2 H1c 76.5(6) 2_756 . 2_756 ? O2 C2 H1c 112.3(8) 2_756 . 2_756 ? C2 O2 C1 64.9(11) . . 2_756 ? C2 O2 C2 77.7(11) . . 2_756 ? C2 O2 O2 81.1(12) . . 2_756 ? C1 O2 C2 51.9(9) 2_756 . 2_756 ? C1 O2 O2 89.3(12) 2_756 . 2_756 ? C2 O2 O2 39.4(8) 2_756 . 2_756 ? C2 O3 C4 111.0(11) . . . ? O3 C4 C5 108.6(12) . . . ? O3 C4 H4a 132(2) . . . ? O3 C4 H4b 96.7(15) . . . ? C5 C4 H4a 110(2) . . . ? C5 C4 H4b 98.3(14) . . . ? H4a C4 H4b 105.6(14) . . . ? O01 C5 O02 33.7(7) . . . ? O01 C5 O03 58.4(10) . . . ? O01 C5 C4 127.1(11) . . . ? O01 C5 H5a 114.5(16) . . . ? O01 C5 H5b 76.9(13) . . . ? O01 C5 H5c 30.1(8) . . . ? O02 C5 O03 91.7(15) . . . ? O02 C5 C4 97.6(12) . . . ? O02 C5 H5a 146(2) . . . ? O02 C5 H5b 69.2(12) . . . ? O02 C5 H5c 56.4(11) . . . ? O03 C5 C4 143.8(16) . . . ? O03 C5 H5a 62.0(11) . . . ? O03 C5 H5b 106.0(18) . . . ? O03 C5 H5c 40.0(10) . . . ? C4 C5 H5a 116.6(18) . . . ? C4 C5 H5b 110.1(16) . . . ? C4 C5 H5c 123.0(16) . . . ? H5a C5 H5b 96.0(14) . . . ? H5a C5 H5c 101.9(17) . . . ? H5b C5 H5c 105(2) . . . ? N11 H112 O112 154(3) . . . ? N13 H132 O132 154(3) . . . ? N15 H152 O152 152(4) . . . ? N21 H212 O212 150(3) . . . ? N23 H230a C230 48.5(14) . . . ? N23 H232 O232 158(4) . . . ? N25 H252 O252 154(4) . . . ? C1 H1c C2 92.6(12) . . 2_756 ? O03 H5a C5 71.8(13) . . . ? O02 H5b C5 74.2(12) . . . ? O01 H5c O02 49.3(6) . . . ? O01 H5c O03 103.7(11) . . . ? O01 H5c C5 128.4(11) . . . ? O02 H5c O03 147.0(12) . . . ? O02 H5c C5 89.1(12) . . . ? O03 H5c C5 99.0(14) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min -30 _reflns_limit_l_max 30 _reflns_number_total 8607 #ActaC _reflns_number_observed 4068 #ActaC _reflns_observed_criterion refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .841 _reflns_d_resolution_low 13.139 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ?