# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Thomas Fabrice' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; 'Carlos Perez Del Valle' '' '' 'Olivier Jarjayes' '' '' 'Christian Philouze' '' '' 'Olaf Rotthaus' '' '' _publ_contact_author_name 'Thomas Fabrice' _publ_contact_author_email FABRICE.THOMAS@UJF-GRENOBLE.FR _publ_section_title ; Oxidized nickel(II) complexes of bis and tetra(salicylidene) phenylenediamine Schiff bases: What about the influence of the phenylene substituents? ; _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? # Attachment '692330.CIF' data_Mono_C_ _database_code_depnum_ccdc_archive 'CCDC 692329' #------------------------------------------------------------------------------ _audit_creation_date 2008-06-16 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'Enraf-Nonius Kappa CCD' _computing_cell_refinement 'Enraf-Nonius Kappa CCD ' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 29.792(4) _cell_length_b 19.255(2) _cell_length_c 13.8064(6) _cell_angle_alpha 90 _cell_angle_beta 117.44(1) _cell_angle_gamma 90 _cell_volume 7029(1) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 657.52 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H50 N2 O4 Ni ' _chemical_formula_moiety 'C38 H50 N2 O4 Ni ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2816.00 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type CCD _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 16775 _reflns_number_total 6350 _reflns_number_gt 3429 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.105 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H 0 400 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 304 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 32 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 8 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni 0.04106(2) 0.08124(2) 0.41036(3) 0.0176(1) 1.000 . Uani d ? O(1) 0.10873(9) 0.0855(1) 0.4460(2) 0.0226(6) 1.000 . Uani d ? O(2) 0.04500(9) 0.1768(1) 0.4234(2) 0.0225(6) 1.000 . Uani d ? O(3) -0.0952(1) -0.1938(1) 0.2619(2) 0.0306(7) 1.000 . Uani d ? O(4) -0.1613(1) -0.1010(1) 0.2366(2) 0.0287(7) 1.000 . Uani d ? N(1) 0.0382(1) -0.0154(1) 0.4032(2) 0.0163(6) 1.000 . Uani d ? N(2) -0.0273(1) 0.0771(2) 0.3707(2) 0.0177(6) 1.000 . Uani d ? C(1) 0.1419(1) 0.0357(2) 0.4782(3) 0.0184(8) 1.000 . Uani d ? C(2) 0.1944(1) 0.0504(2) 0.5116(3) 0.0220(8) 1.000 . Uani d ? C(3) 0.2282(1) -0.0027(2) 0.5570(3) 0.029(1) 1.000 . Uani d ? C(4) 0.2162(1) -0.0723(2) 0.5695(3) 0.0326(9) 1.000 D Uani d ? C(5) 0.1660(1) -0.0865(2) 0.5283(3) 0.0248(9) 1.000 . Uani d ? C(6) 0.1284(1) -0.0346(2) 0.4825(3) 0.0195(8) 1.000 . Uani d ? C(7) 0.0772(1) -0.0559(2) 0.4400(3) 0.0183(8) 1.000 . Uani d ? C(8) -0.0117(1) -0.0411(2) 0.3608(2) 0.0149(8) 1.000 . Uani d ? C(9) -0.0260(1) -0.1103(2) 0.3361(3) 0.0207(8) 1.000 . Uani d ? C(10) -0.0767(1) -0.1283(2) 0.2934(3) 0.0216(8) 1.000 . Uani d ? C(11) -0.1133(1) -0.0769(2) 0.2782(3) 0.0202(8) 1.000 . Uani d ? C(12) -0.0989(1) -0.0087(2) 0.3013(3) 0.0190(8) 1.000 . Uani d ? C(13) -0.0477(1) 0.0092(2) 0.3428(2) 0.0164(8) 1.000 . Uani d ? C(14) -0.0553(1) 0.1293(2) 0.3719(3) 0.0197(9) 1.000 . Uani d ? C(15) -0.0387(1) 0.1990(2) 0.3984(3) 0.0207(8) 1.000 . Uani d ? C(16) -0.0738(1) 0.2473(2) 0.4005(3) 0.0224(9) 1.000 . Uani d ? C(17) -0.0620(1) 0.3161(2) 0.4222(3) 0.0269(9) 1.000 . Uani d ? C(18) -0.0135(1) 0.3360(2) 0.4387(3) 0.0254(9) 1.000 . Uani d ? C(19) 0.0223(1) 0.2929(2) 0.4350(3) 0.0233(9) 1.000 . Uani d ? C(20) 0.0104(1) 0.2196(2) 0.4181(3) 0.0190(8) 1.000 . Uani d ? C(21) 0.2119(1) 0.1233(2) 0.5011(3) 0.0316(9) 1.000 . Uani d ? C(22) 0.2674(2) 0.1248(3) 0.5257(3) 0.048(1) 1.000 . Uani d ? C(23) 0.1811(2) 0.1507(2) 0.3833(3) 0.034(1) 1.000 . Uani d ? C(24) 0.2051(2) 0.1713(2) 0.5809(3) 0.047(1) 1.000 . Uani d ? C(25) 0.2613(2) -0.1164(4) 0.6467(5) 0.043(2) 0.600 D Uiso d ? C(25') 0.2524(3) -0.1344(3) 0.6049(7) 0.013(2) 0.400 D Uiso d ? C(26) 0.2446(2) -0.1812(3) 0.6769(5) 0.097(2) 1.000 . Uani d ? C(27) 0.2997(3) -0.1205(4) 0.6129(6) 0.084(2) 0.800 . Uiso d ? C(28') 0.2445(5) -0.1917(7) 0.523(1) 0.091(4) 0.500 . Uiso d ? C(28) 0.2909(4) -0.0839(4) 0.7546(7) 0.105(3) 0.700 . Uani d ? C(29) -0.0610(2) -0.2455(2) 0.2674(3) 0.039(1) 1.000 . Uani d ? C(30) -0.1994(1) -0.0507(2) 0.2173(3) 0.031(1) 1.000 . Uani d ? C(31) -0.0980(2) 0.3707(2) 0.4285(4) 0.041(1) 1.000 . Uani d ? C(32) -0.0754(2) 0.4018(2) 0.5430(4) 0.057(1) 1.000 . Uani d ? C(33) -0.1054(2) 0.4291(2) 0.3463(4) 0.053(1) 1.000 . Uani d ? C(34) -0.1491(2) 0.3393(3) 0.4018(5) 0.067(2) 1.000 . Uani d ? C(35) 0.0736(1) 0.3203(2) 0.4508(3) 0.0315(9) 1.000 . Uani d ? C(36) 0.0847(1) 0.2949(2) 0.3591(3) 0.034(1) 1.000 . Uani d ? C(37) 0.1146(2) 0.2947(3) 0.5605(3) 0.057(1) 1.000 . Uani d ? C(38) 0.0752(2) 0.3993(2) 0.4499(4) 0.061(1) 1.000 . Uani d ? H(1) 0.2630 0.0080 0.5824 0.035 1.000 . Uiso c ? H(2) 0.1558 -0.1330 0.5303 0.030 1.000 . Uiso c ? H(3) 0.0710 -0.1045 0.4380 0.021 1.000 . Uiso c ? H(4) -0.0013 -0.1449 0.3483 0.025 1.000 . Uiso c ? H(5) -0.1235 0.0262 0.2892 0.023 1.000 . Uiso c ? H(6) -0.0896 0.1197 0.3534 0.024 1.000 . Uiso c ? H(7) -0.1065 0.2316 0.3865 0.027 1.000 . Uiso c ? H(8) -0.0048 0.3837 0.4536 0.030 1.000 . Uiso c ? H(9) 0.2719 0.0963 0.4747 0.057 1.000 . Uiso c ? H(10) 0.2878 0.1079 0.5974 0.057 1.000 . Uiso c ? H(11) 0.2769 0.1711 0.5201 0.057 1.000 . Uiso c ? H(12) 0.1866 0.1216 0.3342 0.041 1.000 . Uiso c ? H(13) 0.1916 0.1967 0.3787 0.041 1.000 . Uiso c ? H(14) 0.1461 0.1509 0.3644 0.041 1.000 . Uiso c ? H(15) 0.2247 0.1547 0.6532 0.057 1.000 . Uiso c ? H(16) 0.2158 0.2168 0.5748 0.057 1.000 . Uiso c ? H(17) 0.1704 0.1723 0.5644 0.057 1.000 . Uiso c ? H(18) 0.2264 -0.2086 0.6134 0.116 1.000 . Uiso c ? H(19) 0.2732 -0.2063 0.7276 0.116 1.000 . Uiso c ? H(20) 0.2233 -0.1705 0.7091 0.116 1.000 . Uiso c ? H(21) 0.2867 -0.1431 0.5442 0.101 0.800 . Uiso d ? H(22) 0.3276 -0.1460 0.6653 0.101 0.800 . Uiso d ? H(23) 0.3105 -0.0749 0.6068 0.101 0.800 . Uiso d ? H(24) 0.3194 -0.1121 0.7974 0.125 0.700 . Uiso d ? H(24') 0.2381 -0.2342 0.5496 0.110 0.500 . Uiso d ? H(25) 0.3021 -0.0393 0.7455 0.125 0.700 . Uiso d ? H(25') 0.2165 -0.1804 0.4554 0.110 0.500 . Uiso d ? H(26) 0.2704 -0.0794 0.7903 0.125 0.700 . Uiso d ? H(26') 0.2740 -0.1963 0.5140 0.110 0.500 . Uiso d ? H(27) -0.0784 -0.2884 0.2437 0.047 1.000 . Uiso c ? H(28) -0.0352 -0.2499 0.3405 0.047 1.000 . Uiso c ? H(29) -0.0463 -0.2332 0.2217 0.047 1.000 . Uiso c ? H(30) -0.2314 -0.0730 0.1885 0.037 1.000 . Uiso c ? H(31) -0.1926 -0.0284 0.2840 0.037 1.000 . Uiso c ? H(32) -0.1996 -0.0173 0.1666 0.037 1.000 . Uiso c ? H(33) -0.0706 0.3661 0.5944 0.069 1.000 . Uiso c ? H(34) -0.0437 0.4227 0.5597 0.069 1.000 . Uiso c ? H(35) -0.0977 0.4359 0.5461 0.069 1.000 . Uiso c ? H(36) -0.1186 0.4101 0.2750 0.063 1.000 . Uiso c ? H(37) -0.0738 0.4507 0.3649 0.063 1.000 . Uiso c ? H(38) -0.1284 0.4626 0.3485 0.063 1.000 . Uiso c ? H(39) -0.1447 0.3029 0.4518 0.081 1.000 . Uiso c ? H(40) -0.1705 0.3740 0.4072 0.081 1.000 . Uiso c ? H(41) -0.1640 0.3212 0.3296 0.081 1.000 . Uiso c ? H(42) 0.0607 0.3143 0.2917 0.040 1.000 . Uiso c ? H(43) 0.0825 0.2457 0.3550 0.040 1.000 . Uiso c ? H(44) 0.1178 0.3090 0.3737 0.040 1.000 . Uiso c ? H(45) 0.1142 0.2454 0.5622 0.069 1.000 . Uiso c ? H(46) 0.1467 0.3102 0.5703 0.069 1.000 . Uiso c ? H(47) 0.1085 0.3126 0.6175 0.069 1.000 . Uiso c ? H(48) 0.0499 0.4160 0.3817 0.073 1.000 . Uiso c ? H(49) 0.1075 0.4142 0.4604 0.073 1.000 . Uiso c ? H(50) 0.0690 0.4170 0.5069 0.073 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0173(2) 0.0188(2) 0.0157(2) -0.0028(2) 0.0067(2) -0.0010(2) O(1) 0.019(1) 0.020(1) 0.027(1) -0.005(1) 0.009(1) -0.003(1) O(2) 0.020(1) 0.021(1) 0.025(1) -0.004(1) 0.008(1) -0.001(1) O(3) 0.029(1) 0.023(1) 0.041(1) -0.010(1) 0.018(1) -0.009(1) O(4) 0.022(1) 0.034(2) 0.028(1) -0.010(1) 0.010(1) -0.006(1) N(1) 0.019(1) 0.022(1) 0.009(1) -0.002(1) 0.007(1) 0.001(1) N(2) 0.016(1) 0.023(1) 0.013(1) -0.006(1) 0.006(1) -0.003(1) C(1) 0.023(2) 0.025(2) 0.010(2) 0.000(1) 0.010(1) 0.002(1) C(2) 0.018(2) 0.037(2) 0.009(2) -0.005(1) 0.004(1) 0.002(2) C(3) 0.017(2) 0.049(2) 0.017(2) 0.002(2) 0.005(2) 0.011(2) C(4) 0.023(2) 0.047(2) 0.027(2) 0.008(2) 0.011(2) 0.018(2) C(5) 0.024(2) 0.031(2) 0.023(2) 0.005(2) 0.014(1) 0.010(2) C(6) 0.022(2) 0.027(2) 0.015(2) -0.001(1) 0.013(1) 0.002(2) C(7) 0.022(1) 0.023(2) 0.013(2) -0.002(1) 0.011(1) 0.001(1) C(8) 0.018(1) 0.020(2) 0.009(2) 0.000(1) 0.008(1) 0.000(1) C(9) 0.024(2) 0.020(2) 0.018(2) -0.001(2) 0.009(2) 0.001(2) C(10) 0.027(2) 0.023(2) 0.016(2) -0.007(1) 0.011(2) -0.002(1) C(11) 0.021(2) 0.029(2) 0.012(2) -0.006(1) 0.008(1) -0.004(2) C(12) 0.017(2) 0.027(2) 0.013(2) -0.003(2) 0.007(1) -0.005(2) C(13) 0.017(2) 0.021(2) 0.009(2) -0.002(1) 0.004(1) -0.005(1) C(14) 0.014(2) 0.028(2) 0.014(2) -0.002(1) 0.004(1) -0.001(2) C(15) 0.019(2) 0.029(2) 0.018(2) -0.002(1) 0.012(1) -0.003(2) C(16) 0.024(2) 0.024(2) 0.027(2) 0.000(2) 0.019(2) 0.000(2) C(17) 0.035(2) 0.025(2) 0.028(2) -0.003(2) 0.020(2) -0.006(2) C(18) 0.035(2) 0.016(2) 0.027(2) -0.004(2) 0.016(2) -0.001(2) C(19) 0.027(2) 0.022(2) 0.017(2) -0.006(1) 0.008(2) 0.000(2) C(20) 0.021(2) 0.021(2) 0.015(2) 0.000(1) 0.007(1) 0.002(2) C(21) 0.019(2) 0.044(2) 0.031(2) -0.017(2) 0.012(2) 0.007(2) C(22) 0.021(2) 0.064(3) 0.054(3) -0.006(2) 0.013(2) 0.030(2) C(23) 0.031(2) 0.031(2) 0.037(2) -0.005(2) 0.013(2) 0.009(2) C(24) 0.069(3) 0.040(3) 0.049(2) -0.025(2) 0.040(2) -0.019(2) C(26) 0.084(4) 0.069(4) 0.165(5) 0.045(3) 0.080(3) 0.073(3) C(28) 0.067(6) 0.074(6) 0.095(6) 0.001(5) -0.030(5) 0.049(5) C(29) 0.043(2) 0.025(2) 0.056(2) -0.004(2) 0.029(2) -0.016(2) C(30) 0.021(2) 0.041(2) 0.026(2) -0.007(2) 0.006(2) -0.004(2) C(31) 0.046(2) 0.023(2) 0.063(2) 0.008(2) 0.034(2) -0.004(2) C(32) 0.096(4) 0.026(3) 0.069(2) 0.004(2) 0.055(2) -0.010(2) C(33) 0.055(3) 0.036(3) 0.061(3) 0.018(2) 0.022(2) 0.008(2) C(34) 0.044(2) 0.047(3) 0.125(4) 0.005(2) 0.051(3) -0.014(3) C(35) 0.031(2) 0.031(2) 0.033(2) -0.015(2) 0.015(2) -0.008(2) C(36) 0.026(2) 0.041(3) 0.036(2) -0.011(2) 0.016(2) -0.004(2) C(37) 0.031(3) 0.093(4) 0.034(2) -0.028(3) 0.002(2) 0.002(2) C(38) 0.071(3) 0.031(2) 0.101(4) -0.021(2) 0.056(3) -0.016(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00160|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3429 _refine_ls_number_parameters 404 _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_all 0.0751 _refine_ls_wR_factor_ref 0.0751 _refine_ls_goodness_of_fit_all 1.310 _refine_ls_goodness_of_fit_ref 1.310 _refine_ls_shift/su_max 0.0206 _refine_ls_shift/su_mean 0.2820 _refine_diff_density_min -0.46 _refine_diff_density_max 1.20 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag NI O1 1.844(3) . . yes NI O2 1.848(3) . . yes NI N1 1.862(3) . . yes NI N2 1.850(3) . . yes O1 C1 1.299(5) . . yes O2 C20 1.296(5) . . yes O3 C10 1.365(5) . . yes O3 C29 1.402(6) . . yes O4 C11 1.352(5) . . yes O4 C30 1.420(6) . . yes N1 C7 1.294(5) . . yes N1 C8 1.414(5) . . yes N2 C13 1.418(5) . . yes N2 C14 1.313(5) . . yes C1 C2 1.440(6) . . yes C1 C6 1.421(6) . . yes C2 C3 1.368(6) . . yes C2 C21 1.528(6) . . yes C3 C4 1.418(6) . . yes C3 H1 0.95 . . no C4 C5 1.361(6) . . yes C4 C25 1.530(2) . . yes C4 C25' 1.531(1) . . yes C5 C6 1.413(6) . . yes C5 H2 0.95 . . no C6 C7 1.419(6) . . yes C7 H3 0.95 . . no C8 C9 1.391(6) . . yes C8 C13 1.381(6) . . yes C9 C10 1.387(6) . . yes C9 H4 0.95 . . no C10 C11 1.415(6) . . yes C11 C12 1.374(6) . . yes C12 C13 1.404(6) . . yes C12 H5 0.95 . . no C14 C15 1.419(6) . . yes C14 H6 0.95 . . no C15 C16 1.409(6) . . yes C15 C20 1.414(6) . . yes C16 C17 1.368(6) . . yes C16 H7 0.95 . . no C17 C18 1.408(6) . . yes C17 C31 1.534(7) . . yes C18 C19 1.370(6) . . yes C18 H8 0.95 . . no C19 C20 1.447(6) . . yes C19 C35 1.535(6) . . yes C21 C22 1.526(7) . . yes C21 C23 1.546(6) . . yes C21 C24 1.523(7) . . yes C22 H9 0.95 . . no C22 H10 0.95 . . no C22 H11 0.95 . . no C23 H12 0.95 . . no C23 H13 0.95 . . no C23 H14 0.95 . . no C24 H15 0.95 . . no C24 H16 0.95 . . no C24 H17 0.95 . . no C25 C25' 0.62(1) . . yes C25 C26 1.47(1) . . yes C25 C27 1.42(1) . . yes C25 C28 1.48(1) . . yes C25' C26 1.44(1) . . yes C25' C27 1.39(1) . . yes C25' C28' 1.52(2) . . yes C25' H18 1.66 . . no C25' H21 1.60 . . no C26 H18 0.95 . . no C26 H19 0.95 . . no C26 H20 0.95 . . no C27 H21 0.95 . . no C27 H22 0.95 . . no C27 H23 0.95 . . no C28' H18 1.60 . . no C28' H21 1.49 . . no C28' H24' 0.95 . . no C28' H25' 0.95 . . no C28' H26' 0.95 . . no C28 H24 0.95 . . no C28 H25 0.95 . . no C28 H26 0.95 . . no C29 H27 0.95 . . no C29 H28 0.95 . . no C29 H29 0.95 . . no C30 H30 0.95 . . no C30 H31 0.95 . . no C30 H32 0.95 . . no C31 C32 1.526(7) . . yes C31 C33 1.539(7) . . yes C31 C34 1.515(7) . . yes C32 H33 0.95 . . no C32 H34 0.95 . . no C32 H35 0.95 . . no C33 H36 0.95 . . no C33 H37 0.95 . . no C33 H38 0.95 . . no C34 H39 0.95 . . no C34 H40 0.95 . . no C34 H41 0.95 . . no C35 C36 1.528(7) . . yes C35 C37 1.525(6) . . yes C35 C38 1.523(7) . . yes C36 H42 0.95 . . no C36 H43 0.95 . . no C36 H44 0.95 . . no C37 H45 0.95 . . no C37 H46 0.95 . . no C37 H47 0.95 . . no C38 H48 0.95 . . no C38 H49 0.95 . . no C38 H50 0.95 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 NI O2 85.3(1) . . . yes O1 NI N1 94.3(1) . . . yes O1 NI N2 178.5(1) . . . yes O2 NI N1 177.7(1) . . . yes O2 NI N2 94.8(1) . . . yes N1 NI N2 85.7(2) . . . yes NI O1 C1 128.6(3) . . . yes NI O2 C20 127.9(3) . . . yes C10 O3 C29 117.5(4) . . . yes C11 O4 C30 116.3(3) . . . yes NI N1 C7 124.8(3) . . . yes NI N1 C8 112.7(3) . . . yes C7 N1 C8 122.3(4) . . . yes NI N2 C13 113.4(3) . . . yes NI N2 C14 125.7(3) . . . yes C13 N2 C14 120.9(4) . . . yes O1 C1 C2 120.5(4) . . . yes O1 C1 C6 122.2(4) . . . yes C2 C1 C6 117.3(4) . . . yes C1 C2 C3 117.6(4) . . . yes C1 C2 C21 121.2(4) . . . yes C3 C2 C21 121.2(4) . . . yes C2 C3 C4 125.9(4) . . . yes C2 C3 H1 117.0 . . . no C4 C3 H1 117.0 . . . no C3 C4 C5 115.5(4) . . . yes C3 C4 C25 114.8(5) . . . yes C3 C4 C25' 126.6(5) . . . yes C5 C4 C25 128.5(5) . . . yes C5 C4 C25' 117.0(5) . . . yes C4 C5 C6 122.4(4) . . . yes C4 C5 H2 118.8 . . . no C6 C5 H2 118.8 . . . no C1 C6 C5 120.8(4) . . . yes C1 C6 C7 121.9(4) . . . yes C5 C6 C7 117.3(4) . . . yes N1 C7 C6 126.0(4) . . . yes N1 C7 H3 116.9 . . . no C6 C7 H3 117.1 . . . no N1 C8 C9 125.6(4) . . . yes N1 C8 C13 114.2(4) . . . yes C9 C8 C13 120.2(4) . . . yes C8 C9 C10 119.6(4) . . . yes C8 C9 H4 120.2 . . . no C10 C9 H4 120.2 . . . no O3 C10 C9 124.6(4) . . . yes O3 C10 C11 115.3(4) . . . yes C9 C10 C11 120.2(4) . . . yes O4 C11 C10 114.6(4) . . . yes O4 C11 C12 125.6(4) . . . yes C10 C11 C12 119.8(4) . . . yes C11 C12 C13 119.6(4) . . . yes C11 C12 H5 120.2 . . . no C13 C12 H5 120.2 . . . no N2 C13 C8 113.4(4) . . . yes N2 C13 C12 126.0(4) . . . yes C8 C13 C12 120.6(4) . . . yes N2 C14 C15 125.4(4) . . . yes N2 C14 H6 117.3 . . . no C15 C14 H6 117.3 . . . no C14 C15 C16 117.0(4) . . . yes C14 C15 C20 121.5(4) . . . yes C16 C15 C20 121.5(4) . . . yes C15 C16 C17 121.6(4) . . . yes C15 C16 H7 119.2 . . . no C17 C16 H7 119.2 . . . no C16 C17 C18 116.1(4) . . . yes C16 C17 C31 124.1(4) . . . yes C18 C17 C31 119.8(4) . . . yes C17 C18 C19 125.9(4) . . . yes C17 C18 H8 117.1 . . . no C19 C18 H8 117.1 . . . no C18 C19 C20 117.4(4) . . . yes C18 C19 C35 121.8(4) . . . yes C20 C19 C35 120.7(4) . . . yes O2 C20 C15 124.0(4) . . . yes O2 C20 C19 118.8(4) . . . yes C15 C20 C19 117.3(4) . . . yes C2 C21 C22 112.2(4) . . . yes C2 C21 C23 110.5(3) . . . yes C2 C21 C24 108.8(4) . . . yes C22 C21 C23 106.6(4) . . . yes C22 C21 C24 108.7(4) . . . yes C23 C21 C24 109.9(4) . . . yes C21 C22 H9 109.5 . . . no C21 C22 H10 109.5 . . . no C21 C22 H11 109.5 . . . no H9 C22 H10 109.5 . . . no H9 C22 H11 109.5 . . . no H10 C22 H11 109.5 . . . no C21 C23 H12 109.5 . . . no C21 C23 H13 109.5 . . . no C21 C23 H14 109.5 . . . no H12 C23 H13 109.5 . . . no H12 C23 H14 109.5 . . . no H13 C23 H14 109.5 . . . no C21 C24 H15 109.5 . . . no C21 C24 H16 109.5 . . . no C21 C24 H17 109.5 . . . no H15 C24 H16 109.5 . . . no H15 C24 H17 109.5 . . . no H16 C24 H17 109.5 . . . no C4 C25 C25' 78.5(3) . . . yes C4 C25 C26 111.4(6) . . . yes C4 C25 C27 112.5(7) . . . yes C4 C25 C28 113.2(7) . . . yes C25' C25 C26 75(1) . . . yes C25' C25 C27 74(1) . . . yes C25' C25 C28 168.3(7) . . . yes C26 C25 C27 118.2(7) . . . yes C26 C25 C28 101.4(7) . . . yes C27 C25 C28 99.0(8) . . . yes C4 C25' C25 78.2(3) . . . yes C4 C25' C26 113.3(7) . . . yes C4 C25' C27 114.5(7) . . . yes C4 C25' C28' 119.1(8) . . . yes C4 C25' H18 114.4 . . . no C4 C25' H21 116.1 . . . no C25 C25' C26 81(2) . . . yes C25 C25' C27 81(1) . . . yes C25 C25' C28' 162.6(8) . . . yes C25 C25' H18 115.5 . . . no C25 C25' H21 116.5 . . . no C26 C25' C27 123.2(6) . . . yes C26 C25' C28' 92.2(8) . . . yes C26 C25' H18 34.9 . . . no C26 C25' H21 129.9 . . . no C27 C25' C28' 90.2(9) . . . yes C27 C25' H18 130.7 . . . no C27 C25' H21 36.1 . . . no C28' C25' H18 60.4 . . . no C28' C25' H21 56.8 . . . no H18 C25' H21 112.2 . . . no C25 C26 C25' 24.5(5) . . . yes C25 C26 H18 109.5 . . . no C25 C26 H19 109.5 . . . no C25 C26 H20 109.5 . . . no C25' C26 H18 85.2 . . . no C25' C26 H19 116.8 . . . no C25' C26 H20 122.9 . . . no H18 C26 H19 109.5 . . . no H18 C26 H20 109.5 . . . no H19 C26 H20 109.5 . . . no C25 C27 C25' 25.4(5) . . . yes C25 C27 H21 109.5 . . . no C25 C27 H22 109.5 . . . no C25 C27 H23 109.5 . . . no C25' C27 H21 84.3 . . . no C25' C27 H22 117.5 . . . no C25' C27 H23 122.8 . . . no H21 C27 H22 109.5 . . . no H21 C27 H23 109.5 . . . no H22 C27 H23 109.5 . . . no C25' C28' H24' 109.5 . . . no C25' C28' H25' 109.5 . . . no C25' C28' H26' 109.5 . . . no H18 C28' H21 122.5 . . . no H18 C28' H25' 110.9 . . . no H21 C28' H25' 109.1 . . . no H24' C28' H25' 109.5 . . . no H24' C28' H26' 109.5 . . . no H25' C28' H26' 109.5 . . . no C25 C28 H24 109.5 . . . no C25 C28 H25 109.5 . . . no C25 C28 H26 109.5 . . . no H24 C28 H25 109.5 . . . no H24 C28 H26 109.5 . . . no H25 C28 H26 109.5 . . . no O3 C29 H27 109.5 . . . no O3 C29 H28 109.5 . . . no O3 C29 H29 109.5 . . . no H27 C29 H28 109.5 . . . no H27 C29 H29 109.5 . . . no H28 C29 H29 109.5 . . . no O4 C30 H30 109.5 . . . no O4 C30 H31 109.5 . . . no O4 C30 H32 109.5 . . . no H30 C30 H31 109.5 . . . no H30 C30 H32 109.5 . . . no H31 C30 H32 109.5 . . . no C17 C31 C32 109.9(4) . . . yes C17 C31 C33 109.0(4) . . . yes C17 C31 C34 111.2(4) . . . yes C32 C31 C33 108.8(4) . . . yes C32 C31 C34 108.9(5) . . . yes C33 C31 C34 109.0(4) . . . yes C31 C32 H33 109.5 . . . no C31 C32 H34 109.5 . . . no C31 C32 H35 109.5 . . . no H33 C32 H34 109.5 . . . no H33 C32 H35 109.5 . . . no H34 C32 H35 109.5 . . . no C31 C33 H36 109.5 . . . no C31 C33 H37 109.5 . . . no C31 C33 H38 109.5 . . . no H36 C33 H37 109.5 . . . no H36 C33 H38 109.5 . . . no H37 C33 H38 109.5 . . . no C31 C34 H39 109.5 . . . no C31 C34 H40 109.5 . . . no C31 C34 H41 109.5 . . . no H39 C34 H40 109.5 . . . no H39 C34 H41 109.5 . . . no H40 C34 H41 109.5 . . . no C19 C35 C36 110.8(3) . . . yes C19 C35 C37 108.7(4) . . . yes C19 C35 C38 112.0(4) . . . yes C36 C35 C37 109.8(4) . . . yes C36 C35 C38 107.0(4) . . . yes C37 C35 C38 108.5(4) . . . yes C35 C36 H42 109.5 . . . no C35 C36 H43 109.5 . . . no C35 C36 H44 109.5 . . . no H42 C36 H43 109.5 . . . no H42 C36 H44 109.5 . . . no H43 C36 H44 109.5 . . . no C35 C37 H45 109.5 . . . no C35 C37 H46 109.5 . . . no C35 C37 H47 109.5 . . . no H45 C37 H46 109.5 . . . no H45 C37 H47 109.5 . . . no H46 C37 H47 109.5 . . . no C35 C38 H48 109.5 . . . no C35 C38 H49 109.5 . . . no C35 C38 H50 109.5 . . . no H48 C38 H49 109.5 . . . no H48 C38 H50 109.5 . . . no H49 C38 H50 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O3 C37 3.381(7) . 3_556 no O4 C24 3.594(6) . 3_556 no N1 C13 3.388(5) . 3_556 no N1 C8 3.391(4) . 2 no N1 N2 3.493(5) . 3_556 no N1 C13 3.567(5) . 2 no N2 C8 3.406(5) . 3_556 no N2 C7 3.577(5) . 3_556 no C1 C12 3.565(5) . 2 no C3 C30 3.597(6) . 2 no C6 C11 3.511(5) . 2 no C6 C12 3.577(6) . 3_556 no C7 C14 3.276(6) . 3_556 no C7 C10 3.504(6) . 2 no C7 C9 3.549(5) . 2 no C7 C12 3.549(5) . 3_556 no C8 C8 3.438(8) . 2 no C9 C9 3.384(9) . 2 no C16 C36 3.567(6) . 2 no C28' C28' 2.40(3) . 7_546 no C29 C37 3.548(8) . 3_556 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ # Attachment '692329.cif' data_Cristal_pose_dans_la_grais _database_code_depnum_ccdc_archive 'CCDC 692330' _computing_data_collection 'Enraf-Nonius Kappa CCD' _computing_cell_refinement 'Enraf-Nonius Kappa CC' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.029(6) _cell_length_b 12.317(4) _cell_length_c 13.16(1) _cell_angle_alpha 99.11(4) _cell_angle_beta 102.79(4) _cell_angle_gamma 100.68(3) _cell_volume 1828(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293.0 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 719.51 _chemical_formula_analytical ? _chemical_formula_sum 'C37 H48 N4 O7 Ni ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 764.00 _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Quantum CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 37746 _reflns_number_total 8323 _reflns_number_gt 3882 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.12387 _diffrn_reflns_av_sigmaI/netI 0.220 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 74 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 2 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 14 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni -0.04771(5) -0.08708(5) 0.29184(5) 0.0357(1) 1.000 . Uani d ? O(1) -0.1483(3) -0.0864(3) 0.1645(3) 0.0449(9) 1.000 . Uani d ? O(2) -0.1552(3) -0.2133(3) 0.2957(2) 0.0412(8) 1.000 . Uani d ? O(3) 0.4997(6) 0.2546(8) 0.4045(5) 0.261(3) 1.000 . Uani d ? O(4) 0.4996(5) 0.3135(6) 0.5493(7) 0.203(3) 1.000 . Uani d ? O(5) 0.5550(4) 0.1156(7) 0.6011(5) 0.143(2) 1.000 . Uani d ? O(6) 0.4540(4) 0.0476(5) 0.6940(4) 0.117(2) 1.000 . Uani d ? O(7) 0.2260(7) -0.1419(7) 0.7103(5) 0.184(3) 1.000 . Uani d ? N(1) 0.0620(3) 0.0377(3) 0.2871(3) 0.039(1) 1.000 . Uani d ? N(2) 0.0553(3) -0.0894(3) 0.4199(3) 0.0333(9) 1.000 . Uani d ? N(3) 0.4629(4) 0.2440(5) 0.4705(4) 0.081(2) 1.000 . Uani d ? N(4) 0.4633(4) 0.0823(4) 0.6167(4) 0.057(1) 1.000 . Uani d ? C(1) -0.1403(4) -0.0141(4) 0.1016(4) 0.040(1) 1.000 . Uani d ? C(2) -0.2307(4) -0.0275(4) 0.0062(4) 0.040(1) 1.000 . Uani d ? C(3) -0.2268(4) 0.0578(4) -0.0494(4) 0.043(1) 1.000 . Uani d ? C(4) -0.1373(4) 0.1580(4) -0.0217(4) 0.044(1) 1.000 . Uani d ? C(5) -0.0465(4) 0.1643(4) 0.0616(4) 0.049(1) 1.000 . Uani d ? C(6) -0.0452(4) 0.0816(4) 0.1262(4) 0.046(1) 1.000 . Uani d ? C(7) 0.0513(4) 0.1008(4) 0.2149(4) 0.044(1) 1.000 . Uani d ? C(8) 0.1659(4) 0.0627(4) 0.3700(4) 0.037(1) 1.000 . Uani d ? C(9) 0.2666(4) 0.1448(4) 0.3828(4) 0.044(1) 1.000 . Uani d ? C(10) 0.3615(4) 0.1543(4) 0.4634(4) 0.044(1) 1.000 . Uani d ? C(11) 0.3592(4) 0.0822(4) 0.5368(4) 0.043(1) 1.000 . Uani d ? C(12) 0.2590(4) 0.0017(4) 0.5261(4) 0.046(1) 1.000 . Uani d ? C(13) 0.1606(4) -0.0091(4) 0.4422(3) 0.035(1) 1.000 . Uani d ? C(14) 0.0346(4) -0.1568(4) 0.4848(4) 0.037(1) 1.000 . Uani d ? C(15) -0.0649(4) -0.2446(4) 0.4655(3) 0.035(1) 1.000 . Uani d ? C(16) -0.0682(4) -0.3117(4) 0.5446(4) 0.044(1) 1.000 . Uani d ? C(17) -0.1562(4) -0.4034(4) 0.5310(4) 0.044(1) 1.000 . Uani d ? C(18) -0.2439(4) -0.4310(4) 0.4344(4) 0.046(1) 1.000 . Uani d ? C(19) -0.2466(4) -0.3728(4) 0.3524(4) 0.042(1) 1.000 . Uani d ? C(20) -0.1547(4) -0.2736(4) 0.3691(4) 0.040(1) 1.000 . Uani d ? C(21) -0.3330(4) -0.1337(4) -0.0303(4) 0.045(1) 1.000 . Uani d ? C(22) -0.2849(5) -0.2402(5) -0.0349(5) 0.070(2) 1.000 . Uani d ? C(23) -0.4098(5) -0.1315(6) 0.0472(5) 0.070(2) 1.000 . Uani d ? C(24) -0.4104(5) -0.1373(5) -0.1422(5) 0.074(2) 1.000 . Uani d ? C(25) -0.1491(5) 0.2525(4) -0.0843(4) 0.052(1) 1.000 . Uani d ? C(26) -0.0342(9) 0.3379(7) -0.0591(8) 0.176(3) 1.000 . Uani d ? C(27) -0.1823(9) 0.2085(6) -0.2012(5) 0.109(3) 1.000 . Uani d ? C(28) -0.244(1) 0.3039(8) -0.0589(9) 0.211(4) 1.000 . Uani d ? C(31) -0.1618(5) -0.4794(4) 0.6136(4) 0.054(1) 1.000 . Uani d ? C(32) -0.1860(6) -0.6030(5) 0.5574(5) 0.076(2) 1.000 . Uani d ? C(33) -0.0461(7) -0.4541(6) 0.6972(6) 0.107(2) 1.000 . Uani d ? C(34) -0.2598(7) -0.4636(6) 0.6643(5) 0.094(2) 1.000 . Uani d ? C(35) -0.3380(4) -0.4171(4) 0.2455(4) 0.048(1) 1.000 . Uani d ? C(36) -0.2760(7) -0.4450(6) 0.1590(6) 0.086(2) 1.000 . Uani d ? C(37) -0.4087(5) -0.3299(5) 0.2180(5) 0.077(2) 1.000 . Uani d ? C(38) -0.4256(6) -0.5232(5) 0.2465(5) 0.084(2) 1.000 . Uani d ? C(39) 0.2625(8) -0.2102(9) 0.7647(8) 0.123(3) 1.000 . Uani d ? H(1) -0.2375 -0.2396 0.0334 0.084 1.000 . Uiso c ? H(2) -0.2887 0.0489 -0.1112 0.052 1.000 . Uiso c ? H(3) 0.0193 0.2262 0.0779 0.059 1.000 . Uiso c ? H(4) 0.1214 0.1716 0.2229 0.054 1.000 . Uiso c ? H(5) 0.2688 0.1945 0.3346 0.053 1.000 . Uiso c ? H(6) 0.2566 -0.0465 0.5757 0.055 1.000 . Uiso c ? H(7) 0.1031 -0.1492 0.5539 0.054 1.000 . Uiso c ? H(8) -0.0070 -0.2914 0.6085 0.053 1.000 . Uiso c ? H(9) -0.3063 -0.4946 0.4246 0.055 1.000 . Uiso c ? H(10) -0.3480 -0.3049 -0.0558 0.084 1.000 . Uiso c ? H(11) -0.2391 -0.2422 -0.0852 0.084 1.000 . Uiso c ? H(12) -0.4410 -0.0660 0.0484 0.085 1.000 . Uiso c ? H(13) -0.3643 -0.1302 0.1165 0.085 1.000 . Uiso c ? H(14) -0.4722 -0.1971 0.0251 0.085 1.000 . Uiso c ? H(15) -0.4430 -0.0727 -0.1402 0.089 1.000 . Uiso c ? H(16) -0.3640 -0.1378 -0.1920 0.089 1.000 . Uiso c ? H(17) -0.4717 -0.2037 -0.1630 0.089 1.000 . Uiso c ? H(18) -0.0104 0.3703 0.0149 0.211 1.000 . Uiso c ? H(19) -0.0434 0.3956 -0.0982 0.211 1.000 . Uiso c ? H(20) 0.0236 0.3017 -0.0782 0.211 1.000 . Uiso c ? H(21) -0.1854 0.2696 -0.2368 0.131 1.000 . Uiso c ? H(22) -0.1259 0.1700 -0.2199 0.131 1.000 . Uiso c ? H(23) -0.2570 0.1577 -0.2216 0.131 1.000 . Uiso c ? H(24) -0.2245 0.3362 0.0151 0.254 1.000 . Uiso c ? H(25) -0.2547 0.3611 -0.0985 0.254 1.000 . Uiso c ? H(26) -0.3151 0.2474 -0.0770 0.254 1.000 . Uiso c ? H(27) -0.1925 -0.6500 0.6075 0.091 1.000 . Uiso c ? H(28) -0.1235 -0.6146 0.5269 0.091 1.000 . Uiso c ? H(29) -0.2570 -0.6213 0.5028 0.091 1.000 . Uiso c ? H(30) 0.0137 -0.4686 0.6639 0.128 1.000 . Uiso c ? H(31) -0.0271 -0.3770 0.7325 0.128 1.000 . Uiso c ? H(32) -0.0523 -0.5008 0.7475 0.128 1.000 . Uiso c ? H(33) -0.2452 -0.3872 0.7005 0.113 1.000 . Uiso c ? H(34) -0.3317 -0.4818 0.6107 0.113 1.000 . Uiso c ? H(35) -0.2645 -0.5118 0.7136 0.113 1.000 . Uiso c ? H(36) -0.2232 -0.3788 0.1557 0.104 1.000 . Uiso c ? H(37) -0.3323 -0.4729 0.0922 0.104 1.000 . Uiso c ? H(38) -0.2339 -0.5009 0.1750 0.104 1.000 . Uiso c ? H(39) -0.3571 -0.2618 0.2171 0.093 1.000 . Uiso c ? H(40) -0.4622 -0.3582 0.1499 0.093 1.000 . Uiso c ? H(41) -0.4507 -0.3154 0.2699 0.093 1.000 . Uiso c ? H(42) -0.4663 -0.5065 0.2991 0.101 1.000 . Uiso c ? H(43) -0.3853 -0.5803 0.2624 0.101 1.000 . Uiso c ? H(44) -0.4801 -0.5490 0.1786 0.101 1.000 . Uiso c ? H(45) 0.3293 -0.1708 0.8206 0.147 1.000 . Uiso c ? H(46) 0.2831 -0.2676 0.7202 0.147 1.000 . Uiso c ? H(47) 0.2025 -0.2435 0.7941 0.147 1.000 . Uiso c ? H(48) 0.2860 -0.1085 0.6809 0.220 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0330(3) 0.0302(3) 0.0403(3) -0.0017(2) 0.0055(2) 0.0130(2) O(1) 0.039(2) 0.040(2) 0.049(2) -0.004(1) 0.001(1) 0.020(1) O(2) 0.039(2) 0.034(2) 0.044(2) -0.004(1) 0.002(1) 0.016(1) O(3) 0.156(4) 0.414(9) 0.087(4) -0.204(4) 0.025(3) 0.012(5) O(4) 0.108(4) 0.130(5) 0.301(9) -0.070(4) 0.085(5) -0.086(5) O(5) 0.040(2) 0.248(7) 0.133(4) 0.008(3) -0.003(3) 0.083(4) O(6) 0.078(3) 0.153(4) 0.100(3) -0.014(3) -0.026(3) 0.082(3) O(7) 0.186(7) 0.212(7) 0.112(4) -0.039(6) -0.017(5) 0.093(4) N(1) 0.035(2) 0.037(2) 0.041(2) -0.004(2) 0.006(2) 0.015(2) N(2) 0.030(2) 0.030(2) 0.037(2) 0.001(1) 0.004(1) 0.012(2) N(3) 0.039(2) 0.099(4) 0.075(3) -0.030(2) -0.005(2) 0.015(3) N(4) 0.044(2) 0.062(3) 0.054(3) 0.001(2) 0.000(2) 0.012(2) C(1) 0.043(2) 0.038(2) 0.038(2) 0.007(2) 0.008(2) 0.012(2) C(2) 0.038(2) 0.039(2) 0.042(3) 0.009(2) 0.008(2) 0.009(2) C(3) 0.048(3) 0.040(3) 0.039(3) 0.006(2) 0.007(2) 0.014(2) C(4) 0.048(3) 0.044(3) 0.041(3) 0.010(2) 0.012(2) 0.016(2) C(5) 0.044(3) 0.044(3) 0.054(3) -0.004(2) 0.004(2) 0.023(2) C(6) 0.041(2) 0.042(3) 0.052(3) 0.002(2) 0.008(2) 0.019(2) C(7) 0.042(2) 0.038(3) 0.046(3) -0.007(2) 0.006(2) 0.017(2) C(8) 0.034(2) 0.034(2) 0.039(2) -0.002(2) 0.005(2) 0.009(2) C(9) 0.042(2) 0.039(3) 0.048(3) -0.002(2) 0.009(2) 0.015(2) C(10) 0.036(2) 0.040(3) 0.050(3) -0.004(2) 0.008(2) 0.007(2) C(11) 0.037(2) 0.037(3) 0.044(3) -0.001(2) -0.002(2) 0.003(2) C(12) 0.046(3) 0.044(3) 0.045(3) 0.006(2) 0.009(2) 0.013(2) C(13) 0.033(2) 0.036(2) 0.033(2) 0.005(2) 0.005(2) 0.004(2) C(14) 0.040(2) 0.030(2) 0.042(2) 0.006(2) 0.008(2) 0.012(2) C(15) 0.041(2) 0.029(2) 0.035(2) 0.002(2) 0.008(2) 0.012(2) C(16) 0.045(3) 0.043(3) 0.043(3) 0.001(2) 0.011(2) 0.017(2) C(17) 0.050(3) 0.041(3) 0.046(3) 0.005(2) 0.018(2) 0.019(2) C(18) 0.042(2) 0.033(2) 0.063(3) -0.001(2) 0.016(2) 0.018(2) C(19) 0.040(2) 0.033(2) 0.052(3) 0.002(2) 0.012(2) 0.011(2) C(20) 0.045(2) 0.033(2) 0.048(3) 0.009(2) 0.017(2) 0.018(2) C(21) 0.036(2) 0.043(3) 0.048(3) 0.000(2) -0.002(2) 0.013(2) C(22) 0.062(3) 0.043(3) 0.086(4) -0.002(3) 0.000(3) 0.004(3) C(23) 0.047(3) 0.083(4) 0.076(4) -0.001(3) 0.013(3) 0.025(3) C(24) 0.065(4) 0.065(4) 0.067(4) -0.014(3) -0.016(3) 0.022(3) C(25) 0.066(3) 0.042(3) 0.050(3) 0.014(2) 0.011(2) 0.023(2) C(26) 0.164(8) 0.128(5) 0.177(6) -0.059(5) -0.071(6) 0.130(4) C(27) 0.211(9) 0.065(4) 0.057(4) 0.032(5) 0.028(5) 0.037(3) C(28) 0.367(8) 0.181(5) 0.286(8) 0.229(5) 0.258(6) 0.185(5) C(31) 0.059(3) 0.044(3) 0.060(3) -0.003(2) 0.015(2) 0.030(2) C(32) 0.100(4) 0.058(3) 0.086(4) 0.025(3) 0.031(3) 0.045(3) C(33) 0.107(5) 0.102(5) 0.094(5) -0.023(4) -0.004(4) 0.070(3) C(34) 0.139(5) 0.080(4) 0.091(4) 0.021(4) 0.074(3) 0.042(3) C(35) 0.052(3) 0.031(2) 0.051(3) -0.009(2) 0.001(2) 0.013(2) C(36) 0.103(5) 0.066(4) 0.068(4) -0.004(4) 0.008(4) 0.000(3) C(37) 0.058(3) 0.066(4) 0.090(5) -0.007(3) -0.008(3) 0.027(3) C(38) 0.080(4) 0.058(4) 0.084(4) -0.032(3) -0.007(3) 0.025(3) C(39) 0.108(6) 0.160(8) 0.106(6) 0.044(6) 0.015(5) 0.045(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3882 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_all 0.0899 _refine_ls_wR_factor_ref 0.0899 _refine_ls_goodness_of_fit_all 1.170 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_shift/su_max 0.0061 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_min -0.53 _refine_diff_density_max 0.80 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag NI O1 1.840(3) . . yes NI O2 1.844(3) . . yes NI N1 1.850(4) . . yes NI N2 1.866(4) . . yes O1 C1 1.313(6) . . yes O2 C20 1.308(6) . . yes O3 N3 1.074(7) . . yes O4 N3 1.174(8) . . yes O5 N4 1.178(6) . . yes O6 N4 1.184(6) . . yes O7 C39 1.27(1) . . yes O7 H48 0.95 . . no N1 C7 1.320(6) . . yes N1 C8 1.413(5) . . yes N2 C13 1.396(5) . . yes N2 C14 1.314(6) . . yes N3 C10 1.461(6) . . yes N4 C11 1.446(6) . . yes C1 C2 1.432(6) . . yes C1 C6 1.421(6) . . yes C2 C3 1.372(7) . . yes C2 C21 1.549(6) . . yes C3 C4 1.416(6) . . yes C3 H2 0.95 . . no C4 C5 1.347(7) . . yes C4 C25 1.539(7) . . yes C5 C6 1.426(7) . . yes C5 H3 0.95 . . no C6 C7 1.406(6) . . yes C7 H4 1.07 . . no C8 C9 1.385(6) . . yes C8 C13 1.400(7) . . yes C9 C10 1.348(6) . . yes C9 H5 0.95 . . no C10 C11 1.413(7) . . yes C11 C12 1.377(6) . . yes C12 C13 1.398(6) . . yes C12 H6 0.95 . . no C14 C15 1.401(6) . . yes C14 H7 1.06 . . no C15 C16 1.431(7) . . yes C15 C20 1.418(6) . . yes C16 C17 1.355(6) . . yes C16 H8 0.95 . . no C17 C18 1.408(7) . . yes C17 C31 1.547(7) . . yes C18 C19 1.384(7) . . yes C18 H9 0.95 . . no C19 C20 1.439(6) . . yes C19 C35 1.528(6) . . yes C21 C22 1.526(8) . . yes C21 C23 1.521(8) . . yes C21 C24 1.548(7) . . yes C22 H1 0.95 . . no C22 H10 0.95 . . no C22 H11 0.95 . . no C23 H12 0.95 . . no C23 H13 0.95 . . no C23 H14 0.95 . . no C24 H15 0.95 . . no C24 H16 0.95 . . no C24 H17 0.95 . . no C25 C26 1.51(1) . . yes C25 C27 1.484(8) . . yes C25 C28 1.48(1) . . yes C26 H18 0.95 . . no C26 H19 0.95 . . no C26 H20 0.95 . . no C27 H21 0.95 . . no C27 H22 0.95 . . no C27 H23 0.95 . . no C28 H24 0.95 . . no C28 H25 0.95 . . no C28 H26 0.95 . . no C31 C32 1.528(8) . . yes C31 C33 1.515(8) . . yes C31 C34 1.506(9) . . yes C32 H27 0.95 . . no C32 H28 0.95 . . no C32 H29 0.95 . . no C33 H30 0.95 . . no C33 H31 0.95 . . no C33 H32 0.95 . . no C34 H33 0.95 . . no C34 H34 0.95 . . no C34 H35 0.95 . . no C35 C36 1.524(9) . . yes C35 C37 1.527(9) . . yes C35 C38 1.523(7) . . yes C36 H36 0.95 . . no C36 H37 0.95 . . no C36 H38 0.95 . . no C37 H39 0.95 . . no C37 H40 0.95 . . no C37 H41 0.95 . . no C38 H42 0.95 . . no C38 H43 0.95 . . no C38 H44 0.95 . . no C39 H45 0.95 . . no C39 H46 0.95 . . no C39 H47 0.95 . . no H1 H10 1.55 . . no H1 H11 1.55 . . no H6 H48 1.69 . . no H10 H11 1.55 . . no H12 H13 1.55 . . no H12 H14 1.55 . . no H13 H14 1.55 . . no H15 H16 1.55 . . no H15 H17 1.55 . . no H16 H17 1.55 . . no H18 H19 1.55 . . no H18 H20 1.55 . . no H19 H20 1.55 . . no H21 H22 1.55 . . no H21 H23 1.55 . . no H22 H23 1.55 . . no H24 H25 1.55 . . no H24 H26 1.55 . . no H25 H26 1.55 . . no H27 H28 1.55 . . no H27 H29 1.55 . . no H28 H29 1.55 . . no H30 H31 1.55 . . no H30 H32 1.55 . . no H31 H32 1.55 . . no H33 H34 1.55 . . no H33 H35 1.55 . . no H34 H35 1.55 . . no H36 H37 1.55 . . no H36 H38 1.55 . . no H37 H38 1.55 . . no H39 H40 1.55 . . no H39 H41 1.55 . . no H40 H41 1.55 . . no H42 H43 1.55 . . no H42 H44 1.55 . . no H43 H44 1.55 . . no H45 H46 1.55 . . no H45 H47 1.55 . . no H46 H47 1.55 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 NI O2 86.0(1) . . . yes O1 NI N1 94.3(1) . . . yes O1 NI N2 179.1(2) . . . yes O2 NI N1 178.9(2) . . . yes O2 NI N2 94.0(1) . . . yes N1 NI N2 85.8(2) . . . yes NI O1 C1 129.3(3) . . . yes NI O2 C20 129.7(3) . . . yes C39 O7 H48 109.5 . . . no H45 O7 H48 93.3 . . . no H46 O7 H48 93.4 . . . no H47 O7 H48 139.0 . . . no NI N1 C7 126.3(3) . . . yes NI N1 C8 113.9(3) . . . yes C7 N1 C8 119.7(4) . . . yes NI N2 C13 112.6(3) . . . yes NI N2 C14 125.7(3) . . . yes C13 N2 C14 121.7(4) . . . yes O3 N3 O4 118.1(7) . . . yes O3 N3 C10 123.2(6) . . . yes O4 N3 C10 118.3(6) . . . yes O5 N4 O6 122.4(5) . . . yes O5 N4 C11 118.1(5) . . . yes O6 N4 C11 119.6(5) . . . yes O1 C1 C2 120.5(4) . . . yes O1 C1 C6 122.2(4) . . . yes C2 C1 C6 117.3(4) . . . yes C1 C2 C3 118.4(4) . . . yes C1 C2 C21 120.5(4) . . . yes C3 C2 C21 121.1(4) . . . yes C2 C3 C4 124.9(4) . . . yes C2 C3 H2 117.5 . . . no C4 C3 H2 117.5 . . . no C3 C4 C5 116.1(4) . . . yes C3 C4 C25 119.9(4) . . . yes C5 C4 C25 124.0(4) . . . yes C4 C5 C6 122.5(4) . . . yes C4 C5 H3 118.7 . . . no C6 C5 H3 118.7 . . . no C1 C6 C5 120.1(4) . . . yes C1 C6 C7 122.4(4) . . . yes C5 C6 C7 117.4(4) . . . yes N1 C7 C6 125.1(4) . . . yes N1 C7 H4 118.3 . . . no C6 C7 H4 116.6 . . . no N1 C8 C9 127.2(4) . . . yes N1 C8 C13 112.3(4) . . . yes C9 C8 C13 120.4(4) . . . yes C8 C9 C10 120.2(5) . . . yes C8 C9 H5 119.9 . . . no C10 C9 H5 119.9 . . . no N3 C10 C9 116.0(5) . . . yes N3 C10 C11 123.4(4) . . . yes C9 C10 C11 120.6(4) . . . yes N4 C11 C10 121.7(4) . . . yes N4 C11 C12 118.3(5) . . . yes C10 C11 C12 119.7(4) . . . yes C11 C12 C13 119.8(5) . . . yes C11 C12 H6 120.1 . . . no C13 C12 H6 120.1 . . . no N2 C13 C8 115.1(4) . . . yes N2 C13 C12 125.7(4) . . . yes C8 C13 C12 119.2(4) . . . yes N2 C14 C15 125.5(4) . . . yes N2 C14 H7 116.7 . . . no C15 C14 H7 117.5 . . . no C14 C15 C16 116.8(4) . . . yes C14 C15 C20 122.8(4) . . . yes C16 C15 C20 120.2(4) . . . yes C15 C16 C17 121.9(4) . . . yes C15 C16 H8 119.1 . . . no C17 C16 H8 119.1 . . . no C16 C17 C18 116.9(4) . . . yes C16 C17 C31 123.4(4) . . . yes C18 C17 C31 119.6(4) . . . yes C17 C18 C19 125.3(4) . . . yes C17 C18 H9 117.4 . . . no C19 C18 H9 117.4 . . . no C18 C19 C20 117.3(4) . . . yes C18 C19 C35 121.3(4) . . . yes C20 C19 C35 121.2(4) . . . yes O2 C20 C15 121.8(4) . . . yes O2 C20 C19 119.8(4) . . . yes C15 C20 C19 118.4(4) . . . yes C2 C21 C22 110.0(4) . . . yes C2 C21 C23 109.5(4) . . . yes C2 C21 C24 111.2(4) . . . yes C22 C21 C23 109.9(5) . . . yes C22 C21 C24 108.4(4) . . . yes C23 C21 C24 107.9(4) . . . yes C21 C22 H1 109.5 . . . no C21 C22 H10 109.5 . . . no C21 C22 H11 109.5 . . . no H1 C22 H10 109.5 . . . no H1 C22 H11 109.5 . . . no H10 C22 H11 109.5 . . . no C21 C23 H12 109.5 . . . no C21 C23 H13 109.5 . . . no C21 C23 H14 109.5 . . . no H12 C23 H13 109.5 . . . no H12 C23 H14 109.5 . . . no H13 C23 H14 109.5 . . . no C21 C24 H15 109.5 . . . no C21 C24 H16 109.5 . . . no C21 C24 H17 109.5 . . . no H15 C24 H16 109.5 . . . no H15 C24 H17 109.5 . . . no H16 C24 H17 109.5 . . . no C4 C25 C26 110.8(5) . . . yes C4 C25 C27 112.0(5) . . . yes C4 C25 C28 108.1(5) . . . yes C26 C25 C27 106.4(6) . . . yes C26 C25 C28 112.4(7) . . . yes C27 C25 C28 107.0(7) . . . yes C25 C26 H18 109.5 . . . no C25 C26 H19 109.5 . . . no C25 C26 H20 109.5 . . . no H18 C26 H19 109.5 . . . no H18 C26 H20 109.5 . . . no H19 C26 H20 109.5 . . . no C25 C27 H21 109.5 . . . no C25 C27 H22 109.5 . . . no C25 C27 H23 109.5 . . . no H21 C27 H22 109.5 . . . no H21 C27 H23 109.5 . . . no H22 C27 H23 109.5 . . . no C25 C28 H24 109.5 . . . no C25 C28 H25 109.5 . . . no C25 C28 H26 109.5 . . . no H24 C28 H25 109.5 . . . no H24 C28 H26 109.5 . . . no H25 C28 H26 109.5 . . . no C17 C31 C32 109.3(4) . . . yes C17 C31 C33 111.2(4) . . . yes C17 C31 C34 109.5(5) . . . yes C32 C31 C33 107.2(5) . . . yes C32 C31 C34 108.6(5) . . . yes C33 C31 C34 110.9(6) . . . yes C31 C32 H27 109.5 . . . no C31 C32 H28 109.5 . . . no C31 C32 H29 109.5 . . . no H27 C32 H28 109.5 . . . no H27 C32 H29 109.5 . . . no H28 C32 H29 109.5 . . . no C31 C33 H30 109.5 . . . no C31 C33 H31 109.5 . . . no C31 C33 H32 109.5 . . . no H30 C33 H31 109.5 . . . no H30 C33 H32 109.5 . . . no H31 C33 H32 109.5 . . . no C31 C34 H33 109.5 . . . no C31 C34 H34 109.5 . . . no C31 C34 H35 109.5 . . . no H33 C34 H34 109.5 . . . no H33 C34 H35 109.5 . . . no H34 C34 H35 109.5 . . . no C19 C35 C36 108.9(4) . . . yes C19 C35 C37 111.3(4) . . . yes C19 C35 C38 111.8(4) . . . yes C36 C35 C37 109.4(5) . . . yes C36 C35 C38 108.6(5) . . . yes C37 C35 C38 106.7(5) . . . yes C35 C36 H36 109.5 . . . no C35 C36 H37 109.5 . . . no C35 C36 H38 109.5 . . . no H36 C36 H37 109.5 . . . no H36 C36 H38 109.5 . . . no H37 C36 H38 109.5 . . . no C35 C37 H39 109.5 . . . no C35 C37 H40 109.5 . . . no C35 C37 H41 109.5 . . . no H39 C37 H40 109.5 . . . no H39 C37 H41 109.5 . . . no H40 C37 H41 109.5 . . . no C35 C38 H42 109.5 . . . no C35 C38 H43 109.5 . . . no C35 C38 H44 109.5 . . . no H42 C38 H43 109.5 . . . no H42 C38 H44 109.5 . . . no H43 C38 H44 109.5 . . . no O7 C39 H45 109.5 . . . no O7 C39 H46 109.5 . . . no O7 C39 H47 109.5 . . . no H45 C39 H46 109.5 . . . no H45 C39 H47 109.5 . . . no H45 C39 H48 93.3 . . . no H46 C39 H47 109.5 . . . no H46 C39 H48 93.3 . . . no H47 C39 H48 139.0 . . . no H1 H10 H11 60.0 . . . no H1 H11 H10 60.0 . . . no H13 H12 H14 60.0 . . . no H12 H13 H14 60.0 . . . no H12 H14 H13 60.0 . . . no H16 H15 H17 60.0 . . . no H15 H16 H17 60.0 . . . no H15 H17 H16 60.0 . . . no H19 H18 H20 60.0 . . . no H18 H19 H20 60.0 . . . no H18 H20 H19 60.0 . . . no H22 H21 H23 60.0 . . . no H21 H22 H23 60.0 . . . no H21 H23 H22 60.0 . . . no H25 H24 H26 60.0 . . . no H24 H25 H26 60.0 . . . no H24 H26 H25 60.0 . . . no H28 H27 H29 60.0 . . . no H27 H28 H29 60.0 . . . no H27 H29 H28 60.0 . . . no H31 H30 H32 60.0 . . . no H30 H31 H32 60.0 . . . no H30 H32 H31 60.0 . . . no H34 H33 H35 60.0 . . . no H33 H34 H35 60.0 . . . no H33 H35 H34 60.0 . . . no H37 H36 H38 60.0 . . . no H36 H37 H38 60.0 . . . no H36 H38 H37 60.0 . . . no H40 H39 H41 60.0 . . . no H39 H40 H41 60.0 . . . no H39 H41 H40 60.0 . . . no H43 H42 H44 60.0 . . . no H42 H43 H44 60.0 . . . no H42 H44 H43 60.0 . . . no H46 H45 H47 60.0 . . . no H45 H46 H47 60.0 . . . no H45 H47 H46 60.0 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 O7 3.42(1) . 2_556 no O3 C24 3.372(9) . 2 no O4 C37 3.46(1) . 2_556 no O4 C34 3.464(9) . 1_665 no O5 C11 3.264(9) . 2_656 no O5 N4 3.394(9) . 2_656 no O5 O5 3.40(1) . 2_656 no O5 C12 3.462(9) . 2_656 no O5 C27 3.48(1) . 1_656 no O6 O7 3.326(9) . . no O6 C23 3.584(9) . 2_556 no O7 C12 3.269(9) . . no O7 C14 3.285(8) . . no O7 C1 3.35(1) . 2_556 no O7 C6 3.48(1) . 2_556 no N2 N2 3.453(7) . 2_556 no N2 C14 3.543(6) . 2_556 no C8 C15 3.439(7) . 2_556 no C8 C16 3.589(7) . 2_556 no C13 C14 3.574(7) . 2_556 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O7 H48 O6 0.95 2.472 3.326(9) 149.42 .