Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Akagi, Fumio' 'Fujinami, Shuhei' 'Shionoya, Mitsuhiko' 'Suzuki, Masatatsu' 'Suzuki, Shinnichiro' 'Yamaguchi, Kazuya' _publ_contact_author_name 'Dr Kazuya Yamaguchi' _publ_contact_author_address ; Dr Kazuya Yamaguchi Department of Chemistry Osaka University Graduate School of Science 1-16 Machikaneyama Toyonaka Osaka 560-0043 JAPAN ; _publ_requested_coeditor_name ? _publ_contact_author_phone 81-6-6850-5768 _publ_contact_author_fax 81-6-6850-5785 _publ_contact_author_email 'kazu@ch.wani.osaka-u.ac.jp' data_[Ni2(Me4tpdp)(CH3COO)(H2O)2](ClO4)2 _database_code_CSD 153180 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Nov 28 12:41:34 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku RAXIS-IV' _computing_cell_refinement 'Rigaku RAXIS-IV' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 939.06 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H46 Cl2 N6 O14 Ni2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 17.336(1) _cell_length_b 13.045(1) _cell_length_c 18.060(1) _cell_angle_alpha 90 _cell_angle_beta 100.938(5) _cell_angle_gamma 90 _cell_volume 4010.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153 _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 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 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 'brick' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1952.00 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 153 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISIV' _diffrn_measurement_method ? _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 6698 _reflns_number_total 6698 _reflns_number_observed 5724 _reflns_observed_criterion >3.0\s (I) _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_\s I/netI 0.027 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.70 _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 0 132 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 184 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 56 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 8 0.339 1.112 ;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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ni1 0.26019(4) 0.46490(5) 0.50716(3) 0.0348(2) Uani d . 1.00 . Ni2 0.30947(3) 0.19469(4) 0.51854(3) 0.0333(2) Uani d . 1.00 . Cl1 0.45806(9) 0.3014(1) 0.23657(8) 0.0564(4) Uani d . 1.00 . Cl2 0.08298(9) 0.2479(1) 0.20417(9) 0.0668(5) Uani d . 1.00 . O1 0.2660(2) 0.3243(2) 0.4679(2) 0.0332(8) Uani d . 1.00 . O2 0.3127(2) 0.4303(3) 0.6127(2) 0.0432(10) Uani d . 1.00 . O3 0.3237(2) 0.2596(3) 0.6236(2) 0.0405(9) Uani d . 1.00 . O4 0.3878(2) 0.4840(3) 0.4978(2) 0.047(1) Uani d . 1.00 . O5 0.4208(2) 0.2647(3) 0.5124(2) 0.0443(10) Uani d . 1.00 . O6 0.5001(4) 0.3131(4) 0.3117(3) 0.112(2) Uani d . 1.00 . O7 0.3887(3) 0.3650(5) 0.2323(3) 0.100(2) Uani d . 1.00 . O8 0.4877(7) 0.3327(9) 0.1786(6) 0.219(6) Uani d . 1.00 . O9 0.4303(5) 0.1988(4) 0.2303(4) 0.124(3) Uani d . 1.00 . O10 0.0966(4) 0.1392(6) 0.2235(4) 0.129(2) Uiso d . 1.00 . O11 0.1575(3) 0.2899(4) 0.1999(3) 0.082(1) Uiso d . 1.00 . O12 0.0567(5) 0.2758(7) 0.2740(5) 0.064(2) Uiso d . 0.50 . O13 0.040(1) 0.343(1) 0.207(1) 0.099(5) Uiso d . 0.33 . O14 0.0160(8) 0.273(1) 0.1502(8) 0.061(3) Uiso d . 0.33 . O15 0.0386(8) 0.2223(10) 0.1356(7) 0.081(3) Uiso d . 0.50 . O16 0.0634(9) 0.212(1) 0.1132(8) 0.060(4) Uiso d . 0.33 . O17 0.0205(2) -0.0073(3) 0.1132(2) 0.0453(10) Uani d . 1.00 . N1 0.2222(2) 0.4994(3) 0.3942(2) 0.037(1) Uani d . 1.00 . N2 0.2516(2) 0.6309(3) 0.5174(2) 0.043(1) Uani d . 1.00 . N3 0.1363(2) 0.4412(3) 0.5039(2) 0.043(1) Uani d . 1.00 . N4 0.3009(2) 0.1431(3) 0.4079(2) 0.038(1) Uani d . 1.00 . N5 0.3702(2) 0.0525(3) 0.5426(2) 0.044(1) Uani d . 1.00 . N6 0.1945(2) 0.1246(3) 0.5057(2) 0.038(1) Uani d . 1.00 . C1 0.2500(3) 0.6048(4) 0.3829(3) 0.044(1) Uani d . 1.00 . C2 0.2358(3) 0.6729(4) 0.4467(3) 0.044(1) Uani d . 1.00 . C3 0.2105(4) 0.7715(5) 0.4337(3) 0.059(2) Uani d . 1.00 . C4 0.2005(4) 0.8328(5) 0.4942(4) 0.061(2) Uani d . 1.00 . C5 0.2208(4) 0.7914(4) 0.5650(4) 0.056(2) Uani d . 1.00 . C6 0.2460(3) 0.6913(4) 0.5757(3) 0.046(2) Uani d . 1.00 . C7 0.2701(5) 0.6500(4) 0.6534(3) 0.069(2) Uani d . 1.00 . C8 0.1352(3) 0.4956(4) 0.3746(3) 0.045(1) Uani d . 1.00 . C9 0.0982(3) 0.4396(4) 0.4316(3) 0.043(1) Uani d . 1.00 . C10 0.0244(3) 0.3956(4) 0.4105(4) 0.057(2) Uani d . 1.00 . C11 -0.0124(3) 0.3557(5) 0.4645(5) 0.069(2) Uani d . 1.00 . C12 0.0242(4) 0.3618(4) 0.5384(5) 0.065(2) Uani d . 1.00 . C13 0.0990(3) 0.4037(5) 0.5574(4) 0.055(2) Uani d . 1.00 . C14 0.1379(4) 0.4122(6) 0.6376(4) 0.076(2) Uani d . 1.00 . C15 0.2572(3) 0.4202(4) 0.3540(2) 0.038(1) Uani d . 1.00 . C16 0.2466(3) 0.3163(4) 0.3890(2) 0.035(1) Uani d . 1.00 . C17 0.3007(3) 0.2371(4) 0.3624(2) 0.041(1) Uani d . 1.00 . C18 0.3709(3) 0.0774(5) 0.4096(3) 0.053(2) Uani d . 1.00 . C19 0.3838(3) 0.0091(4) 0.4778(3) 0.048(2) Uani d . 1.00 . C20 0.4106(4) -0.0889(5) 0.4732(4) 0.064(2) Uani d . 1.00 . C21 0.4243(4) -0.1478(5) 0.5388(5) 0.071(2) Uani d . 1.00 . C22 0.4139(3) -0.1040(4) 0.6060(4) 0.057(2) Uani d . 1.00 . C23 0.3869(3) -0.0044(5) 0.6058(3) 0.053(2) Uani d . 1.00 . C24 0.3760(5) 0.0420(5) 0.6792(4) 0.074(2) Uani d . 1.00 . C25 0.2285(3) 0.0815(4) 0.3848(3) 0.041(1) Uani d . 1.00 . C26 0.1681(3) 0.1014(4) 0.4323(3) 0.037(1) Uani d . 1.00 . C27 0.0891(3) 0.0875(4) 0.4026(3) 0.048(2) Uani d . 1.00 . C28 0.0357(3) 0.0959(4) 0.4489(4) 0.055(2) Uani d . 1.00 . C29 0.0619(3) 0.1144(5) 0.5241(4) 0.060(2) Uani d . 1.00 . C30 0.1418(3) 0.1276(4) 0.5526(3) 0.045(2) Uani d . 1.00 . C31 0.1703(4) 0.1386(6) 0.6343(4) 0.070(2) Uani d . 1.00 . C32 0.3327(3) 0.3492(4) 0.6486(3) 0.040(1) Uani d . 1.00 . C33 0.3697(4) 0.3617(4) 0.7304(3) 0.057(2) Uani d . 1.00 . H1 0.3048 0.6032 0.3822 0.0532 Uiso calc . 1.00 . H2 0.2224 0.6313 0.3364 0.0532 Uiso calc . 1.00 . H3 0.2000 0.7983 0.3839 0.0703 Uiso calc . 1.00 . H4 0.1805 0.9005 0.4869 0.0735 Uiso calc . 1.00 . H5 0.2170 0.8325 0.6076 0.0676 Uiso calc . 1.00 . H6 0.2381 0.5926 0.6595 0.0821 Uiso calc . 1.00 . H7 0.3235 0.6292 0.6610 0.0821 Uiso calc . 1.00 . H8 0.2639 0.7014 0.6889 0.0821 Uiso calc . 1.00 . H9 0.1157 0.5640 0.3707 0.0541 Uiso calc . 1.00 . H10 0.1205 0.4624 0.3272 0.0541 Uiso calc . 1.00 . H11 -0.0002 0.3931 0.3588 0.0680 Uiso calc . 1.00 . H12 -0.0626 0.3244 0.4510 0.0830 Uiso calc . 1.00 . H13 -0.0019 0.3373 0.5767 0.0775 Uiso calc . 1.00 . H14 0.1052 0.3825 0.6684 0.0907 Uiso calc . 1.00 . H15 0.1867 0.3772 0.6451 0.0907 Uiso calc . 1.00 . H16 0.1465 0.4824 0.6504 0.0907 Uiso calc . 1.00 . H17 0.2320 0.4199 0.3024 0.0460 Uiso calc . 1.00 . H18 0.3115 0.4338 0.3576 0.0460 Uiso calc . 1.00 . H19 0.1934 0.2947 0.3745 0.0422 Uiso calc . 1.00 . H20 0.3526 0.2640 0.3689 0.0492 Uiso calc . 1.00 . H21 0.2823 0.2217 0.3107 0.0492 Uiso calc . 1.00 . H22 0.3633 0.0365 0.3653 0.0629 Uiso calc . 1.00 . H23 0.4158 0.1198 0.4110 0.0629 Uiso calc . 1.00 . H24 0.4196 -0.1160 0.4267 0.0771 Uiso calc . 1.00 . H25 0.4410 -0.2171 0.5375 0.0853 Uiso calc . 1.00 . H26 0.4251 -0.1420 0.6518 0.0681 Uiso calc . 1.00 . H27 0.3911 -0.0062 0.7186 0.0891 Uiso calc . 1.00 . H28 0.4078 0.1016 0.6890 0.0891 Uiso calc . 1.00 . H29 0.3224 0.0601 0.6760 0.0891 Uiso calc . 1.00 . H30 0.2063 0.0975 0.3339 0.0494 Uiso calc . 1.00 . H31 0.2422 0.0109 0.3887 0.0494 Uiso calc . 1.00 . H32 0.0723 0.0723 0.3505 0.0580 Uiso calc . 1.00 . H33 -0.0190 0.0889 0.4293 0.0664 Uiso calc . 1.00 . H34 0.0252 0.1184 0.5570 0.0719 Uiso calc . 1.00 . H35 0.2038 0.0826 0.6520 0.0844 Uiso calc . 1.00 . H36 0.1989 0.2009 0.6440 0.0844 Uiso calc . 1.00 . H37 0.1270 0.1394 0.6594 0.0844 Uiso calc . 1.00 . H38 0.3827 0.2963 0.7523 0.0690 Uiso calc . 1.00 . H39 0.4162 0.4018 0.7345 0.0690 Uiso calc . 1.00 . H40 0.3340 0.3952 0.7562 0.0690 Uiso calc . 1.00 . H41 0.4138 0.4836 0.4610 0.0554 Uiso calc . 1.00 . H42 0.4151 0.4856 0.5385 0.0554 Uiso calc . 1.00 . H43 0.4084 0.3315 0.5154 0.0554 Uiso calc . 1.00 . H44 0.4499 0.2531 0.5514 0.0554 Uiso calc . 1.00 . 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 Ni1 0.0348(4) 0.0448(4) 0.0249(3) 0.0001(2) 0.0064(2) 0.0034(2) Ni2 0.0305(3) 0.0451(4) 0.0246(3) 0.0038(2) 0.0055(2) -0.0032(2) Cl1 0.0566(8) 0.0731(9) 0.0430(8) -0.0073(6) 0.0181(6) -0.0133(6) Cl2 0.0521(8) 0.086(1) 0.0534(9) -0.0150(7) -0.0117(7) 0.0061(7) O1 0.031(2) 0.052(2) 0.018(1) 0.001(1) 0.007(1) 0.000(1) O2 0.053(2) 0.047(2) 0.028(2) 0.006(2) 0.005(1) 0.004(1) O3 0.049(2) 0.048(2) 0.024(2) 0.007(1) 0.004(1) -0.002(1) O4 0.033(2) 0.080(2) 0.027(2) -0.011(2) 0.001(1) 0.001(2) O5 0.029(2) 0.067(2) 0.034(2) 0.003(1) 0.000(1) -0.005(2) O6 0.116(5) 0.079(4) 0.107(4) 0.035(3) -0.061(4) -0.047(3) O7 0.081(4) 0.129(5) 0.087(4) 0.031(3) 0.008(3) -0.025(3) O8 0.188(9) 0.33(2) 0.185(10) -0.010(10) 0.141(8) 0.052(9) O9 0.167(7) 0.065(4) 0.123(5) -0.018(3) -0.014(5) -0.033(3) O17 0.044(2) 0.058(2) 0.033(2) 0.005(2) 0.003(1) 0.000(1) N1 0.029(2) 0.049(2) 0.032(2) -0.007(2) 0.002(2) 0.007(2) N2 0.041(2) 0.051(2) 0.036(2) -0.004(2) 0.004(2) 0.006(2) N3 0.038(2) 0.047(2) 0.048(3) 0.005(2) 0.018(2) 0.009(2) N4 0.030(2) 0.055(2) 0.030(2) 0.003(2) 0.008(2) -0.010(2) N5 0.037(2) 0.051(2) 0.043(2) 0.011(2) 0.004(2) -0.006(2) N6 0.036(2) 0.041(2) 0.039(2) 0.001(2) 0.014(2) -0.001(2) C1 0.040(3) 0.055(3) 0.036(3) -0.014(2) 0.001(2) 0.009(2) C2 0.039(3) 0.041(3) 0.049(3) -0.011(2) 0.000(2) 0.014(2) C3 0.055(3) 0.061(4) 0.056(4) -0.009(3) -0.002(3) 0.017(3) C4 0.064(4) 0.045(3) 0.075(4) 0.000(3) 0.013(3) 0.020(3) C5 0.059(4) 0.048(3) 0.064(4) -0.004(2) 0.016(3) -0.005(3) C6 0.053(3) 0.043(3) 0.043(3) -0.002(2) 0.009(2) 0.000(2) C7 0.117(6) 0.045(3) 0.047(3) 0.013(3) 0.018(3) 0.001(2) C8 0.028(2) 0.056(3) 0.049(3) -0.005(2) 0.001(2) 0.015(2) C9 0.033(3) 0.038(3) 0.059(3) 0.002(2) 0.014(2) 0.004(2) C10 0.031(3) 0.048(3) 0.089(5) -0.004(2) 0.005(3) 0.004(3) C11 0.037(3) 0.053(4) 0.123(6) -0.005(2) 0.031(4) 0.013(4) C12 0.059(4) 0.049(3) 0.100(5) 0.008(3) 0.049(4) 0.015(3) C13 0.045(3) 0.061(3) 0.069(4) 0.016(2) 0.035(3) 0.022(3) C14 0.071(5) 0.109(6) 0.060(4) 0.021(4) 0.043(4) 0.026(4) C15 0.033(2) 0.055(3) 0.027(2) -0.009(2) 0.004(2) 0.004(2) C16 0.026(2) 0.059(3) 0.020(2) -0.007(2) 0.002(2) 0.002(2) C17 0.034(2) 0.068(3) 0.022(2) -0.009(2) 0.009(2) -0.010(2) C18 0.040(3) 0.075(4) 0.045(3) 0.010(3) 0.013(2) -0.021(3) C19 0.034(3) 0.060(3) 0.050(3) 0.011(2) 0.007(2) -0.012(2) C20 0.045(3) 0.070(4) 0.076(4) 0.016(3) 0.011(3) -0.026(3) C21 0.048(3) 0.052(4) 0.112(6) 0.018(3) 0.009(4) -0.014(4) C22 0.042(3) 0.050(3) 0.074(4) 0.012(2) 0.001(3) 0.002(3) C23 0.040(3) 0.062(3) 0.053(3) 0.016(2) 0.002(2) -0.001(3) C24 0.115(6) 0.058(4) 0.046(4) 0.034(4) 0.008(4) 0.008(3) C25 0.041(3) 0.052(3) 0.031(2) -0.005(2) 0.006(2) -0.009(2) C26 0.032(2) 0.042(3) 0.037(3) 0.000(2) 0.004(2) 0.002(2) C27 0.042(3) 0.046(3) 0.054(3) -0.009(2) 0.000(2) 0.009(2) C28 0.034(3) 0.057(3) 0.075(4) -0.007(2) 0.012(3) 0.008(3) C29 0.046(3) 0.052(3) 0.091(5) -0.006(2) 0.038(3) 0.000(3) C30 0.048(3) 0.039(3) 0.055(3) -0.002(2) 0.027(2) 0.004(2) C31 0.075(4) 0.089(5) 0.056(4) -0.012(3) 0.037(3) -0.015(3) C32 0.040(3) 0.056(3) 0.024(2) 0.002(2) 0.009(2) -0.005(2) C33 0.080(4) 0.059(3) 0.028(3) 0.005(3) -0.003(3) 0.000(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00185|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0056(9) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5724 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0599 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0957 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.895 _refine_ls_shift/esd_max 0.0080 _refine_ls_shift/esd_mean 0.0010 _refine_diff_density_min -1.00 _refine_diff_density_max 1.05 #------------------------------------------------------------------------------ _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 NI1 O1 1.977(3) 1_555 1_555 yes NI1 O2 2.002(3) 1_555 1_555 yes NI1 O4 2.265(4) 1_555 1_555 yes NI1 N1 2.071(4) 1_555 1_555 yes NI1 N2 2.181(4) 1_555 1_555 yes NI1 N3 2.159(4) 1_555 1_555 yes NI2 O1 2.000(3) 1_555 1_555 yes NI2 O3 2.050(3) 1_555 1_555 yes NI2 O5 2.156(3) 1_555 1_555 yes NI2 N4 2.087(4) 1_555 1_555 yes NI2 N5 2.137(4) 1_555 1_555 yes NI2 N6 2.165(4) 1_555 1_555 yes CL1 O6 1.421(5) 1_555 1_555 yes CL1 O7 1.451(5) 1_555 1_555 yes CL1 O8 1.315(8) 1_555 1_555 yes CL1 O9 1.420(6) 1_555 1_555 yes CL2 O10 1.469(8) 1_555 1_555 yes CL2 O11 1.418(6) 1_555 1_555 yes CL2 O12 1.466(9) 1_555 1_555 yes CL2 O13 1.45(2) 1_555 1_555 yes CL2 O14 1.40(1) 1_555 1_555 yes CL2 O15 1.37(1) 1_555 1_555 yes CL2 O16 1.68(1) 1_555 1_555 yes O1 C16 1.404(5) 1_555 1_555 yes O2 C32 1.254(6) 1_555 1_555 yes O3 C32 1.251(6) 1_555 1_555 yes O12 O13 1.49(2) 1_555 1_555 yes O13 O14 1.38(2) 1_555 1_555 yes O14 O15 0.83(1) 1_555 1_555 yes O14 O16 1.40(2) 1_555 1_555 yes O15 O16 0.66(2) 1_555 1_555 yes N1 C1 1.484(6) 1_555 1_555 yes N1 C8 1.484(6) 1_555 1_555 yes N1 C15 1.460(7) 1_555 1_555 yes N2 C2 1.368(6) 1_555 1_555 yes N2 C6 1.333(7) 1_555 1_555 yes N3 C9 1.348(7) 1_555 1_555 yes N3 C13 1.351(6) 1_555 1_555 yes N4 C17 1.475(7) 1_555 1_555 yes N4 C18 1.481(6) 1_555 1_555 yes N4 C25 1.482(6) 1_555 1_555 yes N5 C19 1.362(7) 1_555 1_555 yes N5 C23 1.345(7) 1_555 1_555 yes N6 C26 1.351(6) 1_555 1_555 yes N6 C30 1.359(6) 1_555 1_555 yes C1 C2 1.512(8) 1_555 1_555 yes C2 C3 1.365(8) 1_555 1_555 yes C3 C4 1.392(10) 1_555 1_555 yes C4 C5 1.371(9) 1_555 1_555 yes C5 C6 1.378(8) 1_555 1_555 yes C6 C7 1.487(8) 1_555 1_555 yes C8 C9 1.502(7) 1_555 1_555 yes C9 C10 1.388(7) 1_555 1_555 yes C10 C11 1.366(9) 1_555 1_555 yes C11 C12 1.37(1) 1_555 1_555 yes C12 C13 1.390(9) 1_555 1_555 yes C13 C14 1.481(9) 1_555 1_555 yes C15 C16 1.522(7) 1_555 1_555 yes C16 C17 1.534(7) 1_555 1_555 yes C18 C19 1.503(8) 1_555 1_555 yes C19 C20 1.368(8) 1_555 1_555 yes C20 C21 1.39(1) 1_555 1_555 yes C21 C22 1.385(10) 1_555 1_555 yes C22 C23 1.380(8) 1_555 1_555 yes C23 C24 1.501(9) 1_555 1_555 yes C25 C26 1.497(7) 1_555 1_555 yes C26 C27 1.384(7) 1_555 1_555 yes C27 C28 1.365(8) 1_555 1_555 yes C28 C29 1.370(9) 1_555 1_555 yes C29 C30 1.395(8) 1_555 1_555 yes C30 C31 1.470(9) 1_555 1_555 yes C32 C33 1.505(7) 1_555 1_555 yes #------------------------------------------------------------------------------ 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 NI1 O2 95.0(1) 1_555 1_555 1_555 yes O1 NI1 O4 87.6(1) 1_555 1_555 1_555 yes O1 NI1 N1 82.9(1) 1_555 1_555 1_555 yes O1 NI1 N2 164.0(1) 1_555 1_555 1_555 yes O1 NI1 N3 88.6(1) 1_555 1_555 1_555 yes O2 NI1 O4 79.7(1) 1_555 1_555 1_555 yes O2 NI1 N1 171.6(1) 1_555 1_555 1_555 yes O2 NI1 N2 99.8(1) 1_555 1_555 1_555 yes O2 NI1 N3 105.3(2) 1_555 1_555 1_555 yes O4 NI1 N1 92.0(1) 1_555 1_555 1_555 yes O4 NI1 N2 88.9(1) 1_555 1_555 1_555 yes O4 NI1 N3 174.0(1) 1_555 1_555 1_555 yes N1 NI1 N2 81.6(2) 1_555 1_555 1_555 yes N1 NI1 N3 82.9(2) 1_555 1_555 1_555 yes N2 NI1 N3 93.5(2) 1_555 1_555 1_555 yes O1 NI2 O3 92.4(1) 1_555 1_555 1_555 yes O1 NI2 O5 83.2(1) 1_555 1_555 1_555 yes O1 NI2 N4 83.2(1) 1_555 1_555 1_555 yes O1 NI2 N5 162.8(1) 1_555 1_555 1_555 yes O1 NI2 N6 92.8(1) 1_555 1_555 1_555 yes O3 NI2 O5 85.5(1) 1_555 1_555 1_555 yes O3 NI2 N4 173.7(2) 1_555 1_555 1_555 yes O3 NI2 N5 101.7(1) 1_555 1_555 1_555 yes O3 NI2 N6 102.7(1) 1_555 1_555 1_555 yes O5 NI2 N4 89.4(1) 1_555 1_555 1_555 yes O5 NI2 N5 88.1(2) 1_555 1_555 1_555 yes O5 NI2 N6 171.1(1) 1_555 1_555 1_555 yes N4 NI2 N5 81.8(2) 1_555 1_555 1_555 yes N4 NI2 N6 82.2(2) 1_555 1_555 1_555 yes N5 NI2 N6 93.6(2) 1_555 1_555 1_555 yes O6 CL1 O7 105.0(3) 1_555 1_555 1_555 yes O6 CL1 O8 121.2(7) 1_555 1_555 1_555 yes O6 CL1 O9 106.4(4) 1_555 1_555 1_555 yes O7 CL1 O8 103.0(6) 1_555 1_555 1_555 yes O7 CL1 O9 105.7(4) 1_555 1_555 1_555 yes O8 CL1 O9 114.0(7) 1_555 1_555 1_555 yes O10 CL2 O11 106.1(4) 1_555 1_555 1_555 yes O10 CL2 O12 95.6(5) 1_555 1_555 1_555 yes O10 CL2 O13 151.5(8) 1_555 1_555 1_555 yes O10 CL2 O14 117.5(7) 1_555 1_555 1_555 yes O10 CL2 O15 91.0(6) 1_555 1_555 1_555 yes O10 CL2 O16 87.4(6) 1_555 1_555 1_555 yes O11 CL2 O12 112.7(4) 1_555 1_555 1_555 yes O11 CL2 O13 98.5(8) 1_555 1_555 1_555 yes O11 CL2 O14 121.0(6) 1_555 1_555 1_555 yes O11 CL2 O15 114.0(6) 1_555 1_555 1_555 yes O11 CL2 O16 94.2(6) 1_555 1_555 1_555 yes O12 CL2 O13 61.2(8) 1_555 1_555 1_555 yes O12 CL2 O14 100.9(7) 1_555 1_555 1_555 yes O12 CL2 O15 128.7(7) 1_555 1_555 1_555 yes O12 CL2 O16 150.8(6) 1_555 1_555 1_555 yes O13 CL2 O14 57.6(9) 1_555 1_555 1_555 yes O13 CL2 O15 91.9(9) 1_555 1_555 1_555 yes O13 CL2 O16 105.1(9) 1_555 1_555 1_555 yes O14 CL2 O15 34.9(6) 1_555 1_555 1_555 yes O14 CL2 O16 53.1(8) 1_555 1_555 1_555 yes O15 CL2 O16 22.0(7) 1_555 1_555 1_555 yes NI1 O1 NI2 131.4(1) 1_555 1_555 1_555 yes NI1 O1 C16 114.5(3) 1_555 1_555 1_555 yes NI2 O1 C16 113.5(3) 1_555 1_555 1_555 yes NI1 O2 C32 135.5(3) 1_555 1_555 1_555 yes NI2 O3 C32 134.8(3) 1_555 1_555 1_555 yes NI1 O4 H41 135.3(3) 1_555 1_555 1_555 no NI1 O4 H42 110.5(3) 1_555 1_555 1_555 no H41 O4 H42 113.9(4) 1_555 1_555 1_555 no NI2 O5 H43 100.4(2) 1_555 1_555 1_555 no NI2 O5 H44 107.3(3) 1_555 1_555 1_555 no H43 O5 H44 104.4(4) 1_555 1_555 1_555 no CL2 O12 O13 59.1(8) 1_555 1_555 1_555 yes CL2 O13 O12 59.8(8) 1_555 1_555 1_555 yes CL2 O13 O14 59.4(9) 1_555 1_555 1_555 yes O12 O13 O14 101(1) 1_555 1_555 1_555 yes CL2 O14 O13 63.0(9) 1_555 1_555 1_555 yes CL2 O14 O15 70(1) 1_555 1_555 1_555 yes CL2 O14 O16 73.6(9) 1_555 1_555 1_555 yes O13 O14 O15 131(1) 1_555 1_555 1_555 yes O13 O14 O16 127(1) 1_555 1_555 1_555 yes O15 O14 O16 17(1) 1_555 1_555 1_555 yes CL2 O15 O14 74(1) 1_555 1_555 1_555 yes CL2 O15 O16 106(2) 1_555 1_555 1_555 yes O14 O15 O16 139(2) 1_555 1_555 1_555 yes CL2 O16 O14 53.3(7) 1_555 1_555 1_555 yes CL2 O16 O15 51(1) 1_555 1_555 1_555 yes O14 O16 O15 22(1) 1_555 1_555 1_555 yes NI1 N1 C1 106.6(3) 1_555 1_555 1_555 yes NI1 N1 C8 110.3(3) 1_555 1_555 1_555 yes NI1 N1 C15 104.6(3) 1_555 1_555 1_555 yes C1 N1 C8 109.9(4) 1_555 1_555 1_555 yes C1 N1 C15 114.3(4) 1_555 1_555 1_555 yes C8 N1 C15 110.9(4) 1_555 1_555 1_555 yes NI1 N2 C2 108.9(3) 1_555 1_555 1_555 yes NI1 N2 C6 132.1(3) 1_555 1_555 1_555 yes C2 N2 C6 117.9(5) 1_555 1_555 1_555 yes NI1 N3 C9 109.3(3) 1_555 1_555 1_555 yes NI1 N3 C13 129.8(4) 1_555 1_555 1_555 yes C9 N3 C13 118.3(5) 1_555 1_555 1_555 yes NI2 N4 C17 104.9(3) 1_555 1_555 1_555 yes NI2 N4 C18 104.9(3) 1_555 1_555 1_555 yes NI2 N4 C25 110.3(3) 1_555 1_555 1_555 yes C17 N4 C18 114.0(4) 1_555 1_555 1_555 yes C17 N4 C25 112.5(4) 1_555 1_555 1_555 yes C18 N4 C25 109.8(4) 1_555 1_555 1_555 yes NI2 N5 C19 110.2(3) 1_555 1_555 1_555 yes NI2 N5 C23 132.1(4) 1_555 1_555 1_555 yes C19 N5 C23 117.1(5) 1_555 1_555 1_555 yes NI2 N6 C26 109.5(3) 1_555 1_555 1_555 yes NI2 N6 C30 129.4(3) 1_555 1_555 1_555 yes C26 N6 C30 118.4(4) 1_555 1_555 1_555 yes N1 C1 C2 109.6(4) 1_555 1_555 1_555 yes N1 C1 H1 109.5(5) 1_555 1_555 1_555 no N1 C1 H2 109.6(4) 1_555 1_555 1_555 no C2 C1 H1 109.3(4) 1_555 1_555 1_555 no C2 C1 H2 109.4(5) 1_555 1_555 1_555 no H1 C1 H2 109.4(5) 1_555 1_555 1_555 no N2 C2 C1 116.3(5) 1_555 1_555 1_555 yes N2 C2 C3 122.6(6) 1_555 1_555 1_555 yes C1 C2 C3 121.1(5) 1_555 1_555 1_555 yes C2 C3 C4 119.3(6) 1_555 1_555 1_555 yes C2 C3 H3 120.5(7) 1_555 1_555 1_555 no C4 C3 H3 120.2(6) 1_555 1_555 1_555 no C3 C4 C5 117.2(6) 1_555 1_555 1_555 yes C3 C4 H4 121.5(6) 1_555 1_555 1_555 no C5 C4 H4 121.3(7) 1_555 1_555 1_555 no C4 C5 C6 121.5(6) 1_555 1_555 1_555 yes C4 C5 H5 119.2(6) 1_555 1_555 1_555 no C6 C5 H5 119.3(6) 1_555 1_555 1_555 no N2 C6 C5 121.2(5) 1_555 1_555 1_555 yes N2 C6 C7 118.8(5) 1_555 1_555 1_555 yes C5 C6 C7 120.0(5) 1_555 1_555 1_555 yes C6 C7 H6 109.3(6) 1_555 1_555 1_555 no C6 C7 H7 109.5(6) 1_555 1_555 1_555 no C6 C7 H8 109.6(5) 1_555 1_555 1_555 no H6 C7 H7 109.4(6) 1_555 1_555 1_555 no H6 C7 H8 109.5(7) 1_555 1_555 1_555 no H7 C7 H8 109.6(7) 1_555 1_555 1_555 no N1 C8 C9 113.5(4) 1_555 1_555 1_555 yes N1 C8 H9 108.4(4) 1_555 1_555 1_555 no N1 C8 H10 108.5(5) 1_555 1_555 1_555 no C9 C8 H9 108.4(5) 1_555 1_555 1_555 no C9 C8 H10 108.6(5) 1_555 1_555 1_555 no H9 C8 H10 109.4(5) 1_555 1_555 1_555 no N3 C9 C8 117.6(4) 1_555 1_555 1_555 yes N3 C9 C10 121.9(5) 1_555 1_555 1_555 yes C8 C9 C10 120.3(5) 1_555 1_555 1_555 yes C9 C10 C11 119.5(6) 1_555 1_555 1_555 yes C9 C10 H11 120.2(6) 1_555 1_555 1_555 no C11 C10 H11 120.3(6) 1_555 1_555 1_555 no C10 C11 C12 118.9(5) 1_555 1_555 1_555 yes C10 C11 H12 120.5(8) 1_555 1_555 1_555 no C12 C11 H12 120.5(7) 1_555 1_555 1_555 no C11 C12 C13 120.1(6) 1_555 1_555 1_555 yes C11 C12 H13 119.7(7) 1_555 1_555 1_555 no C13 C12 H13 120.3(8) 1_555 1_555 1_555 no N3 C13 C12 121.2(6) 1_555 1_555 1_555 yes N3 C13 C14 118.7(5) 1_555 1_555 1_555 yes C12 C13 C14 120.0(5) 1_555 1_555 1_555 yes C13 C14 H14 109.3(7) 1_555 1_555 1_555 no C13 C14 H15 109.4(6) 1_555 1_555 1_555 no C13 C14 H16 109.4(6) 1_555 1_555 1_555 no H14 C14 H15 109.6(7) 1_555 1_555 1_555 no H14 C14 H16 109.5(7) 1_555 1_555 1_555 no H15 C14 H16 109.6(8) 1_555 1_555 1_555 no N1 C15 C16 109.2(4) 1_555 1_555 1_555 yes N1 C15 H17 109.4(4) 1_555 1_555 1_555 no N1 C15 H18 109.6(4) 1_555 1_555 1_555 no C16 C15 H17 109.6(4) 1_555 1_555 1_555 no C16 C15 H18 109.5(4) 1_555 1_555 1_555 no H17 C15 H18 109.5(4) 1_555 1_555 1_555 no O1 C16 C15 109.4(4) 1_555 1_555 1_555 yes O1 C16 C17 108.9(4) 1_555 1_555 1_555 yes O1 C16 H19 109.6(4) 1_555 1_555 1_555 no C15 C16 C17 109.9(4) 1_555 1_555 1_555 yes C15 C16 H19 109.6(4) 1_555 1_555 1_555 no C17 C16 H19 109.4(4) 1_555 1_555 1_555 no N4 C17 C16 108.8(4) 1_555 1_555 1_555 yes N4 C17 H20 109.6(4) 1_555 1_555 1_555 no N4 C17 H21 109.7(5) 1_555 1_555 1_555 no C16 C17 H20 109.5(4) 1_555 1_555 1_555 no C16 C17 H21 109.8(4) 1_555 1_555 1_555 no H20 C17 H21 109.4(4) 1_555 1_555 1_555 no N4 C18 C19 110.7(4) 1_555 1_555 1_555 yes N4 C18 H22 109.1(5) 1_555 1_555 1_555 no N4 C18 H23 109.1(5) 1_555 1_555 1_555 no C19 C18 H22 109.4(6) 1_555 1_555 1_555 no C19 C18 H23 109.2(5) 1_555 1_555 1_555 no H22 C18 H23 109.3(5) 1_555 1_555 1_555 no N5 C19 C18 115.8(5) 1_555 1_555 1_555 yes N5 C19 C20 123.9(6) 1_555 1_555 1_555 yes C18 C19 C20 120.3(5) 1_555 1_555 1_555 yes C19 C20 C21 117.9(6) 1_555 1_555 1_555 yes C19 C20 H24 121.0(7) 1_555 1_555 1_555 no C21 C20 H24 121.0(6) 1_555 1_555 1_555 no C20 C21 C22 119.2(6) 1_555 1_555 1_555 yes C20 C21 H25 120.4(8) 1_555 1_555 1_555 no C22 C21 H25 120.4(8) 1_555 1_555 1_555 no C21 C22 C23 119.2(6) 1_555 1_555 1_555 yes C21 C22 H26 120.5(6) 1_555 1_555 1_555 no C23 C22 H26 120.4(6) 1_555 1_555 1_555 no N5 C23 C22 122.6(6) 1_555 1_555 1_555 yes N5 C23 C24 118.9(5) 1_555 1_555 1_555 yes C22 C23 C24 118.4(6) 1_555 1_555 1_555 yes C23 C24 H27 109.4(6) 1_555 1_555 1_555 no C23 C24 H28 109.2(7) 1_555 1_555 1_555 no C23 C24 H29 109.4(6) 1_555 1_555 1_555 no H27 C24 H28 109.6(7) 1_555 1_555 1_555 no H27 C24 H29 109.7(8) 1_555 1_555 1_555 no H28 C24 H29 109.5(6) 1_555 1_555 1_555 no N4 C25 C26 113.1(4) 1_555 1_555 1_555 yes N4 C25 H30 108.6(4) 1_555 1_555 1_555 no N4 C25 H31 108.6(5) 1_555 1_555 1_555 no C26 C25 H30 108.6(5) 1_555 1_555 1_555 no C26 C25 H31 108.6(4) 1_555 1_555 1_555 no H30 C25 H31 109.5(5) 1_555 1_555 1_555 no N6 C26 C25 117.2(4) 1_555 1_555 1_555 yes N6 C26 C27 122.4(5) 1_555 1_555 1_555 yes C25 C26 C27 120.2(4) 1_555 1_555 1_555 yes C26 C27 C28 119.2(5) 1_555 1_555 1_555 yes C26 C27 H32 120.4(6) 1_555 1_555 1_555 no C28 C27 H32 120.4(5) 1_555 1_555 1_555 no C27 C28 C29 119.1(5) 1_555 1_555 1_555 yes C27 C28 H33 120.6(6) 1_555 1_555 1_555 no C29 C28 H33 120.4(6) 1_555 1_555 1_555 no C28 C29 C30 120.4(5) 1_555 1_555 1_555 yes C28 C29 H34 119.7(6) 1_555 1_555 1_555 no C30 C29 H34 119.9(7) 1_555 1_555 1_555 no N6 C30 C29 120.3(5) 1_555 1_555 1_555 yes N6 C30 C31 119.3(5) 1_555 1_555 1_555 yes C29 C30 C31 120.2(5) 1_555 1_555 1_555 yes C30 C31 H35 109.3(6) 1_555 1_555 1_555 no C30 C31 H36 109.4(6) 1_555 1_555 1_555 no C30 C31 H37 109.6(6) 1_555 1_555 1_555 no H35 C31 H36 109.4(7) 1_555 1_555 1_555 no H35 C31 H37 109.6(7) 1_555 1_555 1_555 no H36 C31 H37 109.6(6) 1_555 1_555 1_555 no O2 C32 O3 126.7(4) 1_555 1_555 1_555 yes O2 C32 C33 116.1(4) 1_555 1_555 1_555 yes O3 C32 C33 117.2(4) 1_555 1_555 1_555 yes C32 C33 H38 109.5(5) 1_555 1_555 1_555 no C32 C33 H39 109.4(5) 1_555 1_555 1_555 no C32 C33 H40 109.6(5) 1_555 1_555 1_555 no H38 C33 H39 109.4(6) 1_555 1_555 1_555 no H38 C33 H40 109.6(6) 1_555 1_555 1_555 no H39 C33 H40 109.4(6) 1_555 1_555 1_555 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 O14 3.30(1) 1_555 4_555 ? O4 O17 2.787(5) 1_555 2_555 ? O4 O17 2.812(5) 1_555 4_555 ? O5 O15 2.72(1) 1_555 4_555 ? O5 O14 2.76(1) 1_555 4_555 ? O5 O16 2.80(1) 1_555 4_555 ? O5 C21 3.366(7) 1_555 3_656 ? O6 O17 2.763(6) 1_555 2_555 ? O6 C22 3.323(7) 1_555 3_656 ? O6 C21 3.510(10) 1_555 3_656 ? O7 O17 3.373(7) 1_555 2_555 ? O7 C3 3.387(8) 1_555 2_545 ? O7 C17 3.463(8) 1_555 1_555 ? O7 C15 3.528(7) 1_555 1_555 ? O8 C29 3.358(10) 1_555 4_554 ? O8 C31 3.43(1) 1_555 4_554 ? O9 C8 3.329(7) 1_555 2_545 ? O9 C3 3.589(9) 1_555 2_545 ? O10 O17 2.893(8) 1_555 1_555 ? O10 C27 3.331(10) 1_555 1_555 ? O10 C25 3.428(9) 1_555 1_555 ? O10 C1 3.591(9) 1_555 2_545 ? O11 C1 3.398(7) 1_555 2_545 ? O11 C15 3.434(7) 1_555 1_555 ? O11 C16 3.488(7) 1_555 1_555 ? O11 C20 3.503(8) 1_555 2_555 ? O11 C17 3.534(7) 1_555 1_555 ? O12 C10 3.06(1) 1_555 1_555 ? O12 C27 3.35(1) 1_555 1_555 ? O12 C9 3.52(1) 1_555 1_555 ? O12 C8 3.53(1) 1_555 1_555 ? O12 C16 3.582(10) 1_555 1_555 ? O13 C24 3.17(2) 1_555 4_454 ? O13 C23 3.60(2) 1_555 4_454 ? O14 C20 3.31(1) 1_555 2_555 ? O14 C24 3.53(2) 1_555 4_454 ? O14 C32 3.55(1) 1_555 4_454 ? O15 O17 3.03(1) 1_555 1_555 ? O15 C20 3.37(1) 1_555 2_555 ? O16 O17 2.95(1) 1_555 1_555 ? O16 C20 3.11(1) 1_555 2_555 ? O16 C21 3.34(2) 1_555 2_555 ? O16 C1 3.51(2) 1_555 2_545 ? N3 C11 3.524(7) 1_555 3_566 ? C5 C22 3.560(9) 1_555 1_565 ? C9 C12 3.457(7) 1_555 3_566 ? C10 C12 3.447(8) 1_555 3_566 ? C10 C13 3.499(8) 1_555 3_566 ? C11 C13 3.469(8) 1_555 3_566 ? C28 C29 3.306(8) 1_555 3_556 ? C28 C28 3.47(1) 1_555 3_556 ? #------------------------------------------------------------------------------ data_[Cu2(Me4tpdp)(CH3COO)](ClO4)2 _database_code_CSD 153181 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Nov 28 12:40:27 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection Rigaku RAXIS-IV _computing_cell_refinement Rigaku RAXIS-IV _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 968.83 _chemical_formula_analytical ? _chemical_formula_sum 'C37 H50 Cl2 Cu2 N6 O12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 17.577(3) _cell_length_b 17.387(2) _cell_length_c 14.257(2) _cell_angle_alpha 90 _cell_angle_beta 100.63(1) _cell_angle_gamma 90 _cell_volume 4282(1) _cell_formula_units_Z 4 _cell_measurement_temperature 153 _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 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _exptl_crystal_description 'spindle' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2008.00 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 153 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISIV' _diffrn_measurement_method ? _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 7300 _reflns_number_total 7300 _reflns_number_observed 6088 _reflns_observed_criterion >3.0\s(I) _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_\s I/netI 0.036 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.7 _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 Cu 0 8 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 148 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 200 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 24 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 48 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Cu1 0.77656(3) -0.03111(3) 0.82177(3) 0.0265(1) Uani d . 1.00 . Cu2 0.77543(3) -0.02730(3) 0.57316(3) 0.0266(1) Uani d . 1.00 . Cl1 0.55720(7) 0.24078(7) 0.89264(8) 0.0371(3) Uani d . 1.00 . Cl2 0.93747(7) 0.22841(9) 0.73579(9) 0.0482(4) Uani d . 1.00 . O1 0.7503(2) 0.0082(2) 0.6928(2) 0.0308(8) Uani d . 1.00 . O2 0.8169(2) -0.1261(2) 0.7825(2) 0.0427(9) Uani d . 1.00 . O3 0.8202(2) -0.1225(2) 0.6261(2) 0.0435(10) Uani d . 1.00 . O4 0.5234(2) 0.3158(2) 0.8846(3) 0.051(1) Uani d . 1.00 . O5 0.5297(3) 0.1978(2) 0.9644(3) 0.065(1) Uani d . 1.00 . O6 0.6409(2) 0.2471(2) 0.9169(3) 0.046(1) Uani d . 1.00 . O7 0.5376(2) 0.2016(2) 0.8031(3) 0.062(1) Uani d . 1.00 . O8 0.9702(4) 0.2345(3) 0.8321(4) 0.106(2) Uiso d . 1.00 . O9 0.8600(4) 0.2507(5) 0.7319(6) 0.045(2) Uiso d . 0.50 . O10 0.8621(5) 0.2530(5) 0.6923(7) 0.059(2) Uiso d . 0.50 . O11 0.9816(6) 0.3038(6) 0.7305(7) 0.087(3) Uiso d . 0.50 . O12 0.9775(4) 0.2451(5) 0.6622(5) 0.054(2) Uiso d . 0.50 . O13 0.9624(8) 0.1679(8) 0.7026(9) 0.113(4) Uiso d . 0.50 . O14 0.9328(4) 0.1384(4) 0.7333(5) 0.040(2) Uiso d . 0.50 . O15 0.6876(2) 0.0331(2) 1.1733(3) 0.047(1) Uani d . 1.00 . N1 0.7398(2) 0.0721(2) 0.8607(2) 0.0262(9) Uani d . 1.00 . N2 0.8544(2) -0.0165(2) 0.9511(2) 0.0311(10) Uani d . 1.00 . N3 0.6630(2) -0.0687(2) 0.8640(2) 0.0286(9) Uani d . 1.00 . N4 0.7381(2) 0.0766(2) 0.5223(2) 0.0288(9) Uani d . 1.00 . N5 0.6636(2) -0.0633(2) 0.4788(2) 0.0305(9) Uani d . 1.00 . N6 0.8526(2) -0.0076(2) 0.4779(2) 0.0318(10) Uani d . 1.00 . C1 0.7412(3) 0.0893(2) 0.6921(3) 0.028(1) Uani d . 1.00 . C2 0.6996(3) 0.1108(2) 0.7731(3) 0.030(1) Uani d . 1.00 . C3 0.6967(3) 0.1120(2) 0.5939(3) 0.031(1) Uani d . 1.00 . C4 0.8095(3) 0.1128(3) 0.9067(3) 0.033(1) Uani d . 1.00 . C5 0.8611(2) 0.0587(3) 0.9740(3) 0.033(1) Uani d . 1.00 . C6 0.9114(3) 0.0865(3) 1.0536(3) 0.042(1) Uani d . 1.00 . C7 0.9564(3) 0.0337(4) 1.1110(3) 0.053(2) Uani d . 1.00 . C8 0.9489(3) -0.0424(4) 1.0901(3) 0.049(2) Uani d . 1.00 . C9 0.8979(3) -0.0683(3) 1.0085(3) 0.039(1) Uani d . 1.00 . C10 0.8895(3) -0.1511(3) 0.9840(4) 0.053(2) Uani d . 1.00 . C11 0.6863(2) 0.0586(3) 0.9291(3) 0.029(1) Uani d . 1.00 . C12 0.6312(2) -0.0054(3) 0.8967(3) 0.027(1) Uani d . 1.00 . C13 0.5536(3) -0.0002(3) 0.9024(3) 0.035(1) Uani d . 1.00 . C14 0.5069(3) -0.0652(3) 0.8770(3) 0.038(1) Uani d . 1.00 . C15 0.5393(3) -0.1300(3) 0.8472(3) 0.037(1) Uani d . 1.00 . C16 0.6173(3) -0.1314(3) 0.8405(3) 0.032(1) Uani d . 1.00 . C17 0.6528(3) -0.2012(3) 0.8066(4) 0.046(1) Uani d . 1.00 . C18 0.6849(3) 0.0671(3) 0.4286(3) 0.031(1) Uani d . 1.00 . C19 0.6341(3) -0.0020(3) 0.4267(3) 0.032(1) Uani d . 1.00 . C20 0.5620(3) -0.0036(3) 0.3695(4) 0.047(1) Uani d . 1.00 . C21 0.5202(3) -0.0705(4) 0.3634(4) 0.062(2) Uani d . 1.00 . C22 0.5485(3) -0.1330(4) 0.4169(4) 0.053(2) Uani d . 1.00 . C23 0.6209(3) -0.1272(3) 0.4740(3) 0.038(1) Uani d . 1.00 . C24 0.6546(4) -0.1948(3) 0.5339(4) 0.058(2) Uani d . 1.00 . C25 0.8079(3) 0.1199(3) 0.5107(3) 0.036(1) Uani d . 1.00 . C26 0.8601(3) 0.0692(3) 0.4648(3) 0.034(1) Uani d . 1.00 . C27 0.9126(3) 0.0986(3) 0.4140(3) 0.046(1) Uani d . 1.00 . C28 0.9583(3) 0.0485(4) 0.3742(3) 0.053(2) Uani d . 1.00 . C29 0.9494(3) -0.0284(4) 0.3833(3) 0.051(2) Uani d . 1.00 . C30 0.8953(3) -0.0563(3) 0.4362(3) 0.041(1) Uani d . 1.00 . C31 0.8840(3) -0.1414(3) 0.4474(4) 0.054(2) Uani d . 1.00 . C32 0.8244(3) -0.1561(3) 0.7045(3) 0.035(1) Uani d . 1.00 . C33 0.8406(3) -0.2404(3) 0.7061(4) 0.047(1) Uani d . 1.00 . C34 0.7252(4) -0.0386(4) 1.1840(4) 0.064(2) Uani d . 1.00 . C35 0.6657(5) -0.1006(4) 1.1597(6) 0.082(2) Uani d . 1.00 . C36 0.7388(3) 0.0974(3) 1.1892(3) 0.043(1) Uani d . 1.00 . C37 0.6909(3) 0.1676(3) 1.1830(4) 0.049(2) Uani d . 1.00 . H1 0.7907 0.1130 0.7024 0.0340 Uiso calc . 1.00 . H2 0.6472 0.0941 0.7584 0.0359 Uiso calc . 1.00 . H3 0.7011 0.1649 0.7821 0.0359 Uiso calc . 1.00 . H4 0.6958 0.1664 0.5874 0.0375 Uiso calc . 1.00 . H5 0.6451 0.0932 0.5854 0.0375 Uiso calc . 1.00 . H6 0.8368 0.1308 0.8594 0.0395 Uiso calc . 1.00 . H7 0.7953 0.1553 0.9418 0.0395 Uiso calc . 1.00 . H8 0.9147 0.1399 1.0678 0.0509 Uiso calc . 1.00 . H9 0.9925 0.0506 1.1650 0.0642 Uiso calc . 1.00 . H10 0.9787 -0.0787 1.1312 0.0594 Uiso calc . 1.00 . H11 0.9234 -0.1802 1.0303 0.0634 Uiso calc . 1.00 . H12 0.8376 -0.1667 0.9833 0.0634 Uiso calc . 1.00 . H13 0.9022 -0.1593 0.9228 0.0634 Uiso calc . 1.00 . H14 0.7159 0.0459 0.9898 0.0343 Uiso calc . 1.00 . H15 0.6577 0.1043 0.9342 0.0343 Uiso calc . 1.00 . H16 0.5326 0.0459 0.9228 0.0421 Uiso calc . 1.00 . H17 0.4535 -0.0640 0.8805 0.0460 Uiso calc . 1.00 . H18 0.5084 -0.1746 0.8310 0.0445 Uiso calc . 1.00 . H19 0.6934 -0.2190 0.8551 0.0556 Uiso calc . 1.00 . H20 0.6146 -0.2402 0.7920 0.0556 Uiso calc . 1.00 . H21 0.6730 -0.1890 0.7510 0.0556 Uiso calc . 1.00 . H22 0.6531 0.1115 0.4166 0.0374 Uiso calc . 1.00 . H23 0.7149 0.0619 0.3801 0.0374 Uiso calc . 1.00 . H24 0.5416 0.0408 0.3349 0.0568 Uiso calc . 1.00 . H25 0.4713 -0.0734 0.3219 0.0739 Uiso calc . 1.00 . H26 0.5193 -0.1792 0.4147 0.0633 Uiso calc . 1.00 . H27 0.6644 -0.1806 0.5993 0.0692 Uiso calc . 1.00 . H28 0.6189 -0.2364 0.5244 0.0692 Uiso calc . 1.00 . H29 0.7016 -0.2101 0.5156 0.0692 Uiso calc . 1.00 . H30 0.7933 0.1636 0.4715 0.0431 Uiso calc . 1.00 . H31 0.8347 0.1362 0.5715 0.0431 Uiso calc . 1.00 . H32 0.9174 0.1526 0.4066 0.0554 Uiso calc . 1.00 . H33 0.9959 0.0677 0.3402 0.0634 Uiso calc . 1.00 . H34 0.9796 -0.0632 0.3542 0.0611 Uiso calc . 1.00 . H35 0.8958 -0.1546 0.5131 0.0646 Uiso calc . 1.00 . H36 0.8318 -0.1545 0.4223 0.0646 Uiso calc . 1.00 . H37 0.9174 -0.1688 0.4138 0.0646 Uiso calc . 1.00 . H38 0.8433 -0.2595 0.7691 0.0561 Uiso calc . 1.00 . H39 0.8002 -0.2660 0.6641 0.0561 Uiso calc . 1.00 . H40 0.8884 -0.2493 0.6861 0.0561 Uiso calc . 1.00 . H41 0.7615 -0.0415 1.1423 0.0764 Uiso calc . 1.00 . H42 0.7514 -0.0446 1.2481 0.0764 Uiso calc . 1.00 . H43 0.6905 -0.1493 1.1652 0.0981 Uiso calc . 1.00 . H44 0.6301 -0.0981 1.2023 0.0981 Uiso calc . 1.00 . H45 0.6388 -0.0936 1.0961 0.0981 Uiso calc . 1.00 . H46 0.7705 0.0938 1.2507 0.0514 Uiso calc . 1.00 . H47 0.7705 0.0987 1.1421 0.0514 Uiso calc . 1.00 . H48 0.6600 0.1712 1.1211 0.0590 Uiso calc . 1.00 . H49 0.6584 0.1653 1.2293 0.0590 Uiso calc . 1.00 . H50 0.7236 0.2114 1.1947 0.0590 Uiso calc . 1.00 . 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 Cu1 0.0289(3) 0.0289(3) 0.0218(3) 0.0031(2) 0.0048(2) 0.0013(2) Cu2 0.0314(3) 0.0265(3) 0.0222(3) 0.0023(2) 0.0058(2) 0.0002(2) Cl1 0.0417(7) 0.0309(6) 0.0397(6) 0.0020(5) 0.0101(5) -0.0008(5) Cl2 0.0356(7) 0.0633(9) 0.0450(6) 0.0010(6) 0.0053(5) 0.0000(6) O1 0.046(2) 0.019(1) 0.029(1) 0.004(1) 0.010(1) 0.000(1) O2 0.059(2) 0.039(2) 0.032(2) 0.017(2) 0.011(1) 0.006(1) O3 0.064(2) 0.040(2) 0.028(2) 0.016(2) 0.014(1) 0.002(1) O4 0.057(2) 0.031(2) 0.069(2) 0.011(2) 0.018(2) 0.005(2) O5 0.073(3) 0.053(2) 0.079(3) 0.008(2) 0.040(2) 0.028(2) O6 0.035(2) 0.038(2) 0.062(2) -0.004(1) 0.005(2) -0.007(2) O7 0.063(3) 0.065(3) 0.050(2) 0.004(2) -0.006(2) -0.024(2) O15 0.037(2) 0.045(2) 0.058(2) 0.005(2) 0.009(2) 0.005(2) N1 0.027(2) 0.028(2) 0.023(2) -0.001(1) 0.004(1) -0.001(1) N2 0.025(2) 0.043(2) 0.024(2) -0.002(2) 0.001(1) 0.002(2) N3 0.028(2) 0.031(2) 0.027(2) 0.000(2) 0.007(1) -0.001(2) N4 0.034(2) 0.029(2) 0.023(2) 0.000(2) 0.005(1) -0.002(1) N5 0.033(2) 0.033(2) 0.025(2) -0.002(2) 0.007(1) -0.003(2) N6 0.028(2) 0.041(2) 0.027(2) -0.005(2) 0.007(1) -0.007(2) C1 0.033(2) 0.027(2) 0.025(2) 0.001(2) 0.008(2) 0.001(2) C2 0.037(2) 0.028(2) 0.026(2) 0.002(2) 0.008(2) -0.002(2) C3 0.042(3) 0.030(2) 0.022(2) 0.004(2) 0.007(2) 0.004(2) C4 0.033(2) 0.035(2) 0.033(2) -0.010(2) 0.011(2) -0.004(2) C5 0.023(2) 0.052(3) 0.025(2) -0.005(2) 0.008(2) -0.003(2) C6 0.031(2) 0.064(3) 0.032(2) -0.007(2) 0.004(2) -0.012(2) C7 0.032(3) 0.100(5) 0.027(2) -0.008(3) -0.001(2) -0.011(3) C8 0.037(3) 0.082(4) 0.028(2) 0.002(3) 0.002(2) 0.012(3) C9 0.030(2) 0.058(3) 0.028(2) 0.002(2) 0.004(2) 0.011(2) C10 0.045(3) 0.055(4) 0.052(3) 0.001(3) -0.007(2) 0.025(3) C11 0.026(2) 0.036(2) 0.026(2) -0.001(2) 0.008(2) -0.004(2) C12 0.029(2) 0.033(2) 0.018(2) -0.001(2) 0.005(2) 0.003(2) C13 0.031(3) 0.041(3) 0.035(2) 0.001(2) 0.010(2) 0.002(2) C14 0.031(3) 0.044(3) 0.040(2) -0.006(2) 0.009(2) 0.000(2) C15 0.035(3) 0.040(3) 0.035(2) -0.012(2) 0.005(2) -0.001(2) C16 0.037(3) 0.034(2) 0.025(2) -0.007(2) 0.008(2) 0.000(2) C17 0.051(3) 0.036(3) 0.056(3) -0.005(2) 0.019(2) -0.005(2) C18 0.038(3) 0.033(2) 0.021(2) 0.004(2) 0.003(2) 0.005(2) C19 0.034(3) 0.040(2) 0.021(2) 0.003(2) 0.003(2) -0.002(2) C20 0.045(3) 0.054(3) 0.038(3) -0.002(3) -0.005(2) 0.003(2) C21 0.043(3) 0.084(5) 0.049(3) -0.014(3) -0.015(3) -0.008(3) C22 0.045(3) 0.065(4) 0.045(3) -0.019(3) 0.001(2) -0.006(3) C23 0.043(3) 0.040(3) 0.030(2) -0.013(2) 0.008(2) -0.006(2) C24 0.069(4) 0.042(3) 0.060(3) -0.016(3) 0.007(3) 0.010(3) C25 0.046(3) 0.034(2) 0.028(2) -0.013(2) 0.007(2) -0.001(2) C26 0.034(2) 0.043(3) 0.024(2) -0.009(2) 0.004(2) 0.000(2) C27 0.046(3) 0.067(4) 0.026(2) -0.016(3) 0.006(2) 0.005(2) C28 0.043(3) 0.086(5) 0.034(3) -0.014(3) 0.019(2) -0.001(3) C29 0.039(3) 0.086(5) 0.029(2) -0.004(3) 0.012(2) -0.008(3) C30 0.035(3) 0.059(3) 0.029(2) 0.000(2) 0.008(2) -0.014(2) C31 0.055(3) 0.050(3) 0.063(3) 0.003(3) 0.028(3) -0.020(3) C32 0.031(2) 0.036(2) 0.037(2) 0.006(2) 0.004(2) 0.001(2) C33 0.051(3) 0.036(3) 0.052(3) 0.014(2) 0.007(2) 0.003(2) C34 0.064(4) 0.070(4) 0.058(4) 0.023(3) 0.012(3) 0.009(3) C35 0.099(6) 0.042(4) 0.110(6) 0.015(4) 0.035(5) 0.015(4) C36 0.038(3) 0.064(3) 0.028(2) -0.010(3) 0.010(2) 0.002(2) C37 0.051(3) 0.050(3) 0.046(3) -0.015(3) 0.009(2) -0.002(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00168|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_metho 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0078(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6088 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0532 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0790 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.575 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -1.13 _refine_diff_density_max 1.09 #------------------------------------------------------------------------------ _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 CU1 O1 1.936(3) 1_555 1_555 yes CU1 O2 1.921(3) 1_555 1_555 yes CU1 N1 2.019(4) 1_555 1_555 yes CU1 N2 2.099(3) 1_555 1_555 yes CU1 N3 2.284(4) 1_555 1_555 yes CU2 O1 1.941(3) 1_555 1_555 yes CU2 O3 1.927(3) 1_555 1_555 yes CU2 N4 2.011(4) 1_555 1_555 yes CU2 N5 2.256(4) 1_555 1_555 yes CU2 N6 2.116(4) 1_555 1_555 yes CL1 O4 1.429(4) 1_555 1_555 yes CL1 O5 1.421(4) 1_555 1_555 yes CL1 O6 1.451(4) 1_555 1_555 yes CL1 O7 1.432(4) 1_555 1_555 yes CL2 O8 1.392(6) 1_555 1_555 yes CL2 O9 1.407(8) 1_555 1_555 yes CL2 O10 1.421(9) 1_555 1_555 yes CL2 O11 1.53(1) 1_555 1_555 yes CL2 O12 1.397(8) 1_555 1_555 yes CL2 O13 1.26(1) 1_555 1_555 yes CL2 O14 1.567(7) 1_555 1_555 yes O1 C1 1.419(5) 1_555 1_555 yes O2 C32 1.256(5) 1_555 1_555 yes O3 C32 1.251(5) 1_555 1_555 yes O9 O10 0.57(1) 1_555 1_555 yes O11 O12 1.40(1) 1_555 1_555 yes O12 O13 1.50(2) 1_555 1_555 yes O13 O14 0.90(1) 1_555 1_555 yes O15 C34 1.405(7) 1_555 1_555 yes O15 C36 1.428(6) 1_555 1_555 yes N1 C2 1.479(5) 1_555 1_555 yes N1 C4 1.462(5) 1_555 1_555 yes N1 C11 1.492(5) 1_555 1_555 yes N2 C5 1.347(6) 1_555 1_555 yes N2 C9 1.354(6) 1_555 1_555 yes N3 C12 1.355(6) 1_555 1_555 yes N3 C16 1.358(5) 1_555 1_555 yes N4 C3 1.493(5) 1_555 1_555 yes N4 C18 1.491(5) 1_555 1_555 yes N4 C25 1.475(6) 1_555 1_555 yes N5 C19 1.346(6) 1_555 1_555 yes N5 C23 1.336(6) 1_555 1_555 yes N6 C26 1.359(6) 1_555 1_555 yes N6 C30 1.341(6) 1_555 1_555 yes C1 C2 1.522(6) 1_555 1_555 yes C1 C3 1.524(5) 1_555 1_555 yes C4 C5 1.520(6) 1_555 1_555 yes C5 C6 1.390(6) 1_555 1_555 yes C6 C7 1.377(8) 1_555 1_555 yes C7 C8 1.357(8) 1_555 1_555 yes C8 C9 1.406(7) 1_555 1_555 yes C9 C10 1.482(8) 1_555 1_555 yes C11 C12 1.491(6) 1_555 1_555 yes C12 C13 1.384(6) 1_555 1_555 yes C13 C14 1.404(7) 1_555 1_555 yes C14 C15 1.366(7) 1_555 1_555 yes C15 C16 1.392(7) 1_555 1_555 yes C16 C17 1.485(7) 1_555 1_555 yes C18 C19 1.494(7) 1_555 1_555 yes C19 C20 1.374(7) 1_555 1_555 yes C20 C21 1.369(8) 1_555 1_555 yes C21 C22 1.369(8) 1_555 1_555 yes C22 C23 1.382(7) 1_555 1_555 yes C23 C24 1.508(7) 1_555 1_555 yes C25 C26 1.506(7) 1_555 1_555 yes C26 C27 1.373(7) 1_555 1_555 yes C27 C28 1.376(8) 1_555 1_555 yes C28 C29 1.354(8) 1_555 1_555 yes C29 C30 1.406(7) 1_555 1_555 yes C30 C31 1.505(8) 1_555 1_555 yes C32 C33 1.492(7) 1_555 1_555 yes C34 C35 1.50(1) 1_555 1_555 yes C36 C37 1.475(8) 1_555 1_555 yes #------------------------------------------------------------------------------ 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 CU1 O2 93.6(1) 1_555 1_555 1_555 yes O1 CU1 N1 85.1(1) 1_555 1_555 1_555 yes O1 CU1 N2 142.6(1) 1_555 1_555 1_555 yes O1 CU1 N3 106.5(1) 1_555 1_555 1_555 yes O2 CU1 N1 176.5(1) 1_555 1_555 1_555 yes O2 CU1 N2 98.3(1) 1_555 1_555 1_555 yes O2 CU1 N3 102.6(1) 1_555 1_555 1_555 yes N1 CU1 N2 80.8(1) 1_555 1_555 1_555 yes N1 CU1 N3 80.9(1) 1_555 1_555 1_555 yes N2 CU1 N3 105.3(1) 1_555 1_555 1_555 yes O1 CU2 O3 94.1(1) 1_555 1_555 1_555 yes O1 CU2 N4 85.4(1) 1_555 1_555 1_555 yes O1 CU2 N5 107.4(1) 1_555 1_555 1_555 yes O1 CU2 N6 142.1(1) 1_555 1_555 1_555 yes O3 CU2 N4 174.8(2) 1_555 1_555 1_555 yes O3 CU2 N5 104.1(1) 1_555 1_555 1_555 yes O3 CU2 N6 97.3(2) 1_555 1_555 1_555 yes N4 CU2 N5 81.0(1) 1_555 1_555 1_555 yes N4 CU2 N6 80.1(1) 1_555 1_555 1_555 yes N5 CU2 N6 104.7(1) 1_555 1_555 1_555 yes O4 CL1 O5 110.2(2) 1_555 1_555 1_555 yes O4 CL1 O6 109.7(2) 1_555 1_555 1_555 yes O4 CL1 O7 109.6(2) 1_555 1_555 1_555 yes O5 CL1 O6 109.4(2) 1_555 1_555 1_555 yes O5 CL1 O7 109.5(3) 1_555 1_555 1_555 yes O6 CL1 O7 108.4(2) 1_555 1_555 1_555 yes O8 CL2 O9 103.8(4) 1_555 1_555 1_555 yes O8 CL2 O10 126.2(5) 1_555 1_555 1_555 yes O8 CL2 O11 82.1(4) 1_555 1_555 1_555 yes O8 CL2 O12 123.5(4) 1_555 1_555 1_555 yes O8 CL2 O13 108.9(6) 1_555 1_555 1_555 yes O8 CL2 O14 96.3(4) 1_555 1_555 1_555 yes O9 CL2 O10 23.4(4) 1_555 1_555 1_555 yes O9 CL2 O11 104.9(5) 1_555 1_555 1_555 yes O9 CL2 O12 122.1(5) 1_555 1_555 1_555 yes O9 CL2 O13 127.9(7) 1_555 1_555 1_555 yes O9 CL2 O14 103.1(4) 1_555 1_555 1_555 yes O10 CL2 O11 99.2(6) 1_555 1_555 1_555 yes O10 CL2 O12 99.6(5) 1_555 1_555 1_555 yes O10 CL2 O13 116.6(7) 1_555 1_555 1_555 yes O10 CL2 O14 104.5(5) 1_555 1_555 1_555 yes O11 CL2 O12 57.0(5) 1_555 1_555 1_555 yes O11 CL2 O13 118.6(8) 1_555 1_555 1_555 yes O11 CL2 O14 151.5(5) 1_555 1_555 1_555 yes O12 CL2 O13 68.5(7) 1_555 1_555 1_555 yes O12 CL2 O14 102.8(4) 1_555 1_555 1_555 yes O13 CL2 O14 35.1(6) 1_555 1_555 1_555 yes CU1 O1 CU2 132.0(2) 1_555 1_555 1_555 yes CU1 O1 C1 111.4(2) 1_555 1_555 1_555 yes CU2 O1 C1 110.7(2) 1_555 1_555 1_555 yes CU1 O2 C32 136.0(3) 1_555 1_555 1_555 yes CU2 O3 C32 134.7(3) 1_555 1_555 1_555 yes CL2 O9 O10 79(1) 1_555 1_555 1_555 yes CL2 O10 O9 76(1) 1_555 1_555 1_555 yes CL2 O11 O12 56.6(5) 1_555 1_555 1_555 yes CL2 O12 O11 66.3(6) 1_555 1_555 1_555 yes CL2 O12 O13 51.6(6) 1_555 1_555 1_555 yes O11 O12 O13 111.9(8) 1_555 1_555 1_555 yes CL2 O13 O12 59.9(7) 1_555 1_555 1_555 yes CL2 O13 O14 91(1) 1_555 1_555 1_555 yes O12 O13 O14 148(1) 1_555 1_555 1_555 yes CL2 O14 O13 53(1) 1_555 1_555 1_555 yes C34 O15 C36 114.0(5) 1_555 1_555 1_555 yes CU1 N1 C2 107.4(2) 1_555 1_555 1_555 yes CU1 N1 C4 105.6(3) 1_555 1_555 1_555 yes CU1 N1 C11 108.2(3) 1_555 1_555 1_555 yes C2 N1 C4 112.8(3) 1_555 1_555 1_555 yes C2 N1 C11 111.3(3) 1_555 1_555 1_555 yes C4 N1 C11 111.1(3) 1_555 1_555 1_555 yes CU1 N2 C5 110.1(3) 1_555 1_555 1_555 yes CU1 N2 C9 130.9(3) 1_555 1_555 1_555 yes C5 N2 C9 118.9(4) 1_555 1_555 1_555 yes CU1 N3 C12 107.1(3) 1_555 1_555 1_555 yes CU1 N3 C16 132.0(3) 1_555 1_555 1_555 yes C12 N3 C16 118.3(4) 1_555 1_555 1_555 yes CU2 N4 C3 107.0(2) 1_555 1_555 1_555 yes CU2 N4 C18 109.4(3) 1_555 1_555 1_555 yes CU2 N4 C25 106.0(3) 1_555 1_555 1_555 yes C3 N4 C18 110.7(3) 1_555 1_555 1_555 yes C3 N4 C25 112.8(3) 1_555 1_555 1_555 yes C18 N4 C25 110.8(3) 1_555 1_555 1_555 yes CU2 N5 C19 108.3(3) 1_555 1_555 1_555 yes CU2 N5 C23 132.9(3) 1_555 1_555 1_555 yes C19 N5 C23 118.3(4) 1_555 1_555 1_555 yes CU2 N6 C26 109.7(3) 1_555 1_555 1_555 yes CU2 N6 C30 131.3(4) 1_555 1_555 1_555 yes C26 N6 C30 118.9(4) 1_555 1_555 1_555 yes O1 C1 C2 107.9(3) 1_555 1_555 1_555 yes O1 C1 C3 107.6(3) 1_555 1_555 1_555 yes O1 C1 H1 109.3(4) 1_555 1_555 1_555 no C2 C1 C3 113.3(4) 1_555 1_555 1_555 yes C2 C1 H1 109.3(4) 1_555 1_555 1_555 no C3 C1 H1 109.3(4) 1_555 1_555 1_555 no N1 C2 C1 108.0(3) 1_555 1_555 1_555 yes N1 C2 H2 109.8(4) 1_555 1_555 1_555 no N1 C2 H3 109.9(4) 1_555 1_555 1_555 no C1 C2 H2 109.9(4) 1_555 1_555 1_555 no C1 C2 H3 109.9(4) 1_555 1_555 1_555 no H2 C2 H3 109.5(4) 1_555 1_555 1_555 no N4 C3 C1 106.8(3) 1_555 1_555 1_555 yes N4 C3 H4 110.1(4) 1_555 1_555 1_555 no N4 C3 H5 110.1(4) 1_555 1_555 1_555 no C1 C3 H4 110.2(4) 1_555 1_555 1_555 no C1 C3 H5 110.2(4) 1_555 1_555 1_555 no H4 C3 H5 109.5(4) 1_555 1_555 1_555 no N1 C4 C5 109.7(3) 1_555 1_555 1_555 yes N1 C4 H6 109.4(4) 1_555 1_555 1_555 no N1 C4 H7 109.4(4) 1_555 1_555 1_555 no C5 C4 H6 109.4(4) 1_555 1_555 1_555 no C5 C4 H7 109.4(4) 1_555 1_555 1_555 no H6 C4 H7 109.5(4) 1_555 1_555 1_555 no N2 C5 C4 115.6(4) 1_555 1_555 1_555 yes N2 C5 C6 123.3(4) 1_555 1_555 1_555 yes C4 C5 C6 121.1(5) 1_555 1_555 1_555 yes C5 C6 C7 117.5(5) 1_555 1_555 1_555 yes C5 C6 H8 121.2(5) 1_555 1_555 1_555 no C7 C6 H8 121.2(5) 1_555 1_555 1_555 no C6 C7 C8 119.8(4) 1_555 1_555 1_555 yes C6 C7 H9 120.1(6) 1_555 1_555 1_555 no C8 C7 H9 120.1(6) 1_555 1_555 1_555 no C7 C8 C9 121.0(5) 1_555 1_555 1_555 yes C7 C8 H10 119.5(5) 1_555 1_555 1_555 no C9 C8 H10 119.5(6) 1_555 1_555 1_555 no N2 C9 C8 119.4(5) 1_555 1_555 1_555 yes N2 C9 C10 118.9(4) 1_555 1_555 1_555 yes C8 C9 C10 121.7(4) 1_555 1_555 1_555 yes C9 C10 H11 109.5(5) 1_555 1_555 1_555 no C9 C10 H12 109.4(5) 1_555 1_555 1_555 no C9 C10 H13 109.5(5) 1_555 1_555 1_555 no H11 C10 H12 109.5(5) 1_555 1_555 1_555 no H11 C10 H13 109.5(6) 1_555 1_555 1_555 no H12 C10 H13 109.5(5) 1_555 1_555 1_555 no N1 C11 C12 111.5(3) 1_555 1_555 1_555 yes N1 C11 H14 109.0(4) 1_555 1_555 1_555 no N1 C11 H15 109.0(4) 1_555 1_555 1_555 no C12 C11 H14 109.0(4) 1_555 1_555 1_555 no C12 C11 H15 109.0(4) 1_555 1_555 1_555 no H14 C11 H15 109.5(4) 1_555 1_555 1_555 no N3 C12 C11 115.3(4) 1_555 1_555 1_555 yes N3 C12 C13 123.1(4) 1_555 1_555 1_555 yes C11 C12 C13 121.6(4) 1_555 1_555 1_555 yes C12 C13 C14 117.9(4) 1_555 1_555 1_555 yes C12 C13 H16 121.1(5) 1_555 1_555 1_555 no C14 C13 H16 121.1(5) 1_555 1_555 1_555 no C13 C14 C15 119.2(4) 1_555 1_555 1_555 yes C13 C14 H17 120.4(5) 1_555 1_555 1_555 no C15 C14 H17 120.4(5) 1_555 1_555 1_555 no C14 C15 C16 120.5(4) 1_555 1_555 1_555 yes C14 C15 H18 119.8(5) 1_555 1_555 1_555 no C16 C15 H18 119.8(5) 1_555 1_555 1_555 no N3 C16 C15 120.9(4) 1_555 1_555 1_555 yes N3 C16 C17 118.2(4) 1_555 1_555 1_555 yes C15 C16 C17 120.9(4) 1_555 1_555 1_555 yes C16 C17 H19 109.5(4) 1_555 1_555 1_555 no C16 C17 H20 109.5(5) 1_555 1_555 1_555 no C16 C17 H21 109.5(5) 1_555 1_555 1_555 no H19 C17 H20 109.5(5) 1_555 1_555 1_555 no H19 C17 H21 109.5(5) 1_555 1_555 1_555 no H20 C17 H21 109.5(5) 1_555 1_555 1_555 no N4 C18 C19 112.4(3) 1_555 1_555 1_555 yes N4 C18 H22 108.7(4) 1_555 1_555 1_555 no N4 C18 H23 108.7(4) 1_555 1_555 1_555 no C19 C18 H22 108.7(4) 1_555 1_555 1_555 no C19 C18 H23 108.8(4) 1_555 1_555 1_555 no H22 C18 H23 109.5(4) 1_555 1_555 1_555 no N5 C19 C18 117.2(4) 1_555 1_555 1_555 yes N5 C19 C20 122.1(5) 1_555 1_555 1_555 yes C18 C19 C20 120.6(4) 1_555 1_555 1_555 yes C19 C20 C21 118.7(5) 1_555 1_555 1_555 yes C19 C20 H24 120.6(6) 1_555 1_555 1_555 no C21 C20 H24 120.7(5) 1_555 1_555 1_555 no C20 C21 C22 120.2(5) 1_555 1_555 1_555 yes C20 C21 H25 119.9(6) 1_555 1_555 1_555 no C22 C21 H25 119.9(6) 1_555 1_555 1_555 no C21 C22 C23 118.1(5) 1_555 1_555 1_555 yes C21 C22 H26 120.9(5) 1_555 1_555 1_555 no C23 C22 H26 120.9(6) 1_555 1_555 1_555 no N5 C23 C22 122.6(5) 1_555 1_555 1_555 yes N5 C23 C24 117.5(4) 1_555 1_555 1_555 yes C22 C23 C24 119.9(5) 1_555 1_555 1_555 yes C23 C24 H27 109.5(5) 1_555 1_555 1_555 no C23 C24 H28 109.5(5) 1_555 1_555 1_555 no C23 C24 H29 109.5(5) 1_555 1_555 1_555 no H27 C24 H28 109.5(6) 1_555 1_555 1_555 no H27 C24 H29 109.5(6) 1_555 1_555 1_555 no H28 C24 H29 109.5(6) 1_555 1_555 1_555 no N4 C25 C26 109.6(4) 1_555 1_555 1_555 yes N4 C25 H30 109.4(4) 1_555 1_555 1_555 no N4 C25 H31 109.4(4) 1_555 1_555 1_555 no C26 C25 H30 109.4(4) 1_555 1_555 1_555 no C26 C25 H31 109.5(4) 1_555 1_555 1_555 no H30 C25 H31 109.5(4) 1_555 1_555 1_555 no N6 C26 C25 115.7(4) 1_555 1_555 1_555 yes N6 C26 C27 122.1(5) 1_555 1_555 1_555 yes C25 C26 C27 122.3(5) 1_555 1_555 1_555 yes C26 C27 C28 118.8(5) 1_555 1_555 1_555 yes C26 C27 H32 120.6(6) 1_555 1_555 1_555 no C28 C27 H32 120.6(5) 1_555 1_555 1_555 no C27 C28 C29 119.9(5) 1_555 1_555 1_555 yes C27 C28 H33 120.0(6) 1_555 1_555 1_555 no C29 C28 H33 120.0(6) 1_555 1_555 1_555 no C28 C29 C30 119.6(5) 1_555 1_555 1_555 yes C28 C29 H34 120.2(6) 1_555 1_555 1_555 no C30 C29 H34 120.2(6) 1_555 1_555 1_555 no N6 C30 C29 120.6(5) 1_555 1_555 1_555 yes N6 C30 C31 118.6(5) 1_555 1_555 1_555 yes C29 C30 C31 120.8(5) 1_555 1_555 1_555 yes C30 C31 H35 109.5(5) 1_555 1_555 1_555 no C30 C31 H36 109.5(5) 1_555 1_555 1_555 no C30 C31 H37 109.5(5) 1_555 1_555 1_555 no H35 C31 H36 109.5(6) 1_555 1_555 1_555 no H35 C31 H37 109.5(6) 1_555 1_555 1_555 no H36 C31 H37 109.5(5) 1_555 1_555 1_555 no O2 C32 O3 126.8(4) 1_555 1_555 1_555 yes O2 C32 C33 116.4(4) 1_555 1_555 1_555 yes O3 C32 C33 116.8(4) 1_555 1_555 1_555 yes C32 C33 H38 109.5(5) 1_555 1_555 1_555 no C32 C33 H39 109.5(4) 1_555 1_555 1_555 no C32 C33 H40 109.5(5) 1_555 1_555 1_555 no H38 C33 H39 109.5(6) 1_555 1_555 1_555 no H38 C33 H40 109.5(5) 1_555 1_555 1_555 no H39 C33 H40 109.5(5) 1_555 1_555 1_555 no O15 C34 C35 108.6(5) 1_555 1_555 1_555 yes O15 C34 H41 109.7(6) 1_555 1_555 1_555 no O15 C34 H42 109.7(6) 1_555 1_555 1_555 no C35 C34 H41 109.7(6) 1_555 1_555 1_555 no C35 C34 H42 109.7(6) 1_555 1_555 1_555 no H41 C34 H42 109.4(6) 1_555 1_555 1_555 no C34 C35 H43 109.4(7) 1_555 1_555 1_555 no C34 C35 H44 109.4(7) 1_555 1_555 1_555 no C34 C35 H45 109.5(6) 1_555 1_555 1_555 no H43 C35 H44 109.5(7) 1_555 1_555 1_555 no H43 C35 H45 109.5(8) 1_555 1_555 1_555 no H44 C35 H45 109.5(8) 1_555 1_555 1_555 no O15 C36 C37 107.6(4) 1_555 1_555 1_555 yes O15 C36 H46 109.9(5) 1_555 1_555 1_555 no O15 C36 H47 109.9(5) 1_555 1_555 1_555 no C37 C36 H46 109.9(5) 1_555 1_555 1_555 no C37 C36 H47 109.9(5) 1_555 1_555 1_555 no H46 C36 H47 109.5(5) 1_555 1_555 1_555 no C36 C37 H48 109.4(5) 1_555 1_555 1_555 no C36 C37 H49 109.4(5) 1_555 1_555 1_555 no C36 C37 H50 109.4(5) 1_555 1_555 1_555 no H48 C37 H49 109.5(6) 1_555 1_555 1_555 no H48 C37 H50 109.5(5) 1_555 1_555 1_555 no H49 C37 H50 109.5(5) 1_555 1_555 1_555 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 O4 C20 3.351(7) 1_555 4_555 ? O4 C15 3.418(6) 1_555 2_656 ? O4 C22 3.424(7) 1_555 2_656 ? O4 C18 3.455(6) 1_555 4_555 ? O4 C24 3.537(8) 1_555 2_656 ? O5 C15 3.358(6) 1_555 3_657 ? O5 C14 3.374(6) 1_555 3_657 ? O5 C13 3.598(7) 1_555 1_555 ? O6 C18 3.319(6) 1_555 4_555 ? O6 C11 3.370(6) 1_555 1_555 ? O6 C2 3.417(5) 1_555 1_555 ? O6 C3 3.523(5) 1_555 4_555 ? O7 C21 3.312(7) 1_555 3_656 ? O7 C2 3.351(6) 1_555 1_555 ? O7 C22 3.434(6) 1_555 3_656 ? O8 C27 3.353(8) 1_555 4_555 ? O8 C33 3.496(8) 1_555 2_756 ? O8 C10 3.560(8) 1_555 3_757 ? O9 C37 3.252(9) 1_555 4_554 ? O9 C36 3.378(10) 1_555 4_554 ? O9 C1 3.480(9) 1_555 1_555 ? O10 C37 3.29(1) 1_555 4_554 ? O10 C36 3.38(1) 1_555 4_554 ? O10 C25 3.47(1) 1_555 1_555 ? O10 C1 3.55(1) 1_555 1_555 ? O11 C33 3.18(1) 1_555 2_756 ? O11 C6 3.22(1) 1_555 4_554 ? O11 C7 3.29(1) 1_555 4_554 ? O11 C28 3.36(1) 1_555 4_555 ? O11 C32 3.44(1) 1_555 2_756 ? O11 C27 3.52(1) 1_555 4_555 ? O12 C33 3.407(9) 1_555 2_756 ? O12 C6 3.415(9) 1_555 4_554 ? O13 C29 3.24(2) 1_555 3_756 ? O13 C25 3.58(1) 1_555 1_555 ? O14 C8 3.394(8) 1_555 3_757 ? O14 C1 3.418(9) 1_555 1_555 ? O14 C29 3.462(9) 1_555 3_756 ? O14 C25 3.524(8) 1_555 1_555 ? O15 C14 3.407(6) 1_555 3_657 ? O15 C11 3.506(5) 1_555 1_555 ? C6 C8 3.559(7) 1_555 3_757 ? C7 C9 3.382(7) 1_555 3_757 ? C7 C8 3.574(7) 1_555 3_757 ? C28 C30 3.374(7) 1_555 3_756 ? C28 C29 3.555(7) 1_555 3_756 ? #------------------------------------------------------------------------------ data_[Ni2(Me4tpdp)(DPP)(MeOH)2](ClO4)2 _database_code_CSD 153182 #============================================================================== _audit_creation_date '2000-10-31' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ? #============================================================================== _computing_data_collection Rigaku RAXIS-II _computing_cell_refinement Rigaku RAXIS-II _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 13.5091(4) _cell_length_b 20.927(1) _cell_length_c 18.0299(9) _cell_angle_alpha 90 _cell_angle_beta 96.4758(5) _cell_angle_gamma 90 _cell_volume 5064.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 138.2 _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 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1171.28 _chemical_formula_analytical ? _chemical_formula_sum 'C46 H59 Cl2 N6 O16 Ni2 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2440.00 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 138.2 _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 'unknown QUANTUM' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \\w _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 33186 _reflns_number_total 11459 _reflns_number_gt 8547 _reflns_threshold_expression I>3.00\\s(I) _diffrn_reflns_av_R_equivalents 0.02299 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.47 _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 0 236 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 184 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 64 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;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) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) 0.31933(3) 0.17451(2) 0.19624(2) 0.0151(1) 1.000 . Uani d ? Ni(2) 0.28688(3) 0.26633(2) 0.00982(2) 0.0157(1) 1.000 . Uani d ? Cl(1) 0.27080(8) -0.02765(4) -0.08021(5) 0.0317(2) 1.000 . Uani d ? Cl(2) 0.29848(8) 0.13181(6) -0.34375(6) 0.0442(3) 1.000 . Uani d ? P(1) 0.28711(6) 0.32629(4) 0.17759(5) 0.0162(2) 1.000 . Uani d ? O(1) 0.3243(2) 0.1952(1) 0.0860(1) 0.0170(6) 1.000 . Uani d ? O(2) 0.2831(2) 0.2650(1) 0.2187(1) 0.0195(6) 1.000 . Uani d ? O(3) 0.2804(2) 0.3292(1) 0.0952(1) 0.0198(6) 1.000 . Uani d ? O(4) 0.3860(2) 0.3604(1) 0.2145(1) 0.0222(6) 1.000 . Uani d ? O(5) 0.1978(2) 0.3712(1) 0.1973(1) 0.0202(6) 1.000 . Uani d ? O(6) 0.4730(2) 0.2086(1) 0.2204(1) 0.0237(6) 1.000 . Uani d ? O(7) 0.4427(2) 0.2915(1) 0.0167(1) 0.0263(7) 1.000 . Uani d ? O(8) 0.2261(3) 0.0025(2) -0.0220(2) 0.064(1) 1.000 . Uani d ? O(9) 0.3758(3) -0.0220(2) -0.0634(3) 0.078(2) 1.000 . Uani d ? O(10) 0.2391(4) -0.0925(2) -0.0831(2) 0.066(1) 1.000 . Uani d ? O(11) 0.2372(3) 0.0027(2) -0.1486(2) 0.061(1) 1.000 . Uani d ? O(12) 0.2146(4) 0.1328(2) -0.3964(3) 0.081(1) 1.000 . Uiso d ? O(13) 0.3607(4) 0.0796(3) -0.3708(4) 0.041(1) 0.600 S Uiso d ? O(14) 0.346(1) 0.0690(9) -0.338(1) 0.125(6) 0.400 S Uiso d ? O(15) 0.3547(5) 0.1880(3) -0.3484(4) 0.038(2) 0.600 S Uiso d ? O(16) 0.3660(7) 0.1832(4) -0.3242(6) 0.041(2) 0.400 S Uiso d ? O(17) 0.2831(5) 0.1115(4) -0.2689(4) 0.044(2) 0.500 S Uiso d ? O(18) 0.254(1) 0.1360(7) -0.2761(8) 0.038(3) 0.250 S Uiso d ? O(19) 0.210(1) 0.1599(6) -0.2991(8) 0.042(3) 0.250 S Uiso d ? O(20) 0.0923(3) 0.2391(2) -0.3764(2) 0.053(1) 1.000 . Uani d ? N(1) 0.3732(2) 0.0862(1) 0.1696(2) 0.0177(7) 1.000 . Uani d ? N(2) 0.3502(2) 0.1298(1) 0.3074(2) 0.0213(7) 1.000 . Uani d ? N(3) 0.1777(2) 0.1277(1) 0.1796(2) 0.0179(7) 1.000 . Uani d ? N(4) 0.3103(2) 0.1966(1) -0.0681(2) 0.0184(7) 1.000 . Uani d ? N(5) 0.2761(2) 0.3252(1) -0.0902(2) 0.0201(7) 1.000 . Uani d ? N(6) 0.1332(2) 0.2354(1) -0.0164(2) 0.0201(7) 1.000 . Uani d ? C(1) 0.3377(2) 0.1370(1) 0.0485(2) 0.0171(8) 1.000 . Uani d ? C(2) 0.4112(2) 0.0952(2) 0.0964(2) 0.0193(8) 1.000 . Uani d ? C(3) 0.3778(2) 0.1504(2) -0.0254(2) 0.0184(8) 1.000 . Uani d ? C(4) 0.4514(3) 0.0686(2) 0.2301(2) 0.0220(8) 1.000 . Uani d ? C(5) 0.4128(3) 0.0790(2) 0.3037(2) 0.0231(9) 1.000 . Uani d ? C(6) 0.4387(3) 0.0388(2) 0.3640(2) 0.030(1) 1.000 . Uani d ? C(7) 0.3992(3) 0.0512(2) 0.4304(2) 0.037(1) 1.000 . Uani d ? C(8) 0.3361(3) 0.1024(2) 0.4348(2) 0.033(1) 1.000 . Uani d ? C(9) 0.3131(3) 0.1413(2) 0.3723(2) 0.0261(9) 1.000 . Uani d ? C(10) 0.2441(4) 0.1968(2) 0.3758(2) 0.039(1) 1.000 . Uani d ? C(11) 0.2916(3) 0.0384(2) 0.1647(2) 0.0224(9) 1.000 . Uani d ? C(12) 0.1883(3) 0.0663(2) 0.1586(2) 0.0207(8) 1.000 . Uani d ? C(13) 0.1096(3) 0.0269(2) 0.1355(3) 0.035(1) 1.000 . Uani d ? C(14) 0.0135(3) 0.0495(2) 0.1363(3) 0.045(1) 1.000 . Uani d ? C(15) 0.0014(3) 0.1114(2) 0.1596(3) 0.035(1) 1.000 . Uani d ? C(16) 0.0830(3) 0.1497(2) 0.1806(2) 0.0236(9) 1.000 . Uani d ? C(17) 0.0682(3) 0.2173(2) 0.2050(3) 0.036(1) 1.000 . Uani d ? C(18) 0.3566(3) 0.2287(2) -0.1285(2) 0.0223(9) 1.000 . Uani d ? C(19) 0.3041(3) 0.2909(2) -0.1483(2) 0.0221(9) 1.000 . Uani d ? C(20) 0.2910(3) 0.3124(2) -0.2207(2) 0.027(1) 1.000 . Uani d ? C(21) 0.2481(3) 0.3719(2) -0.2364(2) 0.031(1) 1.000 . Uani d ? C(22) 0.2227(3) 0.4081(2) -0.1774(2) 0.0262(9) 1.000 . Uani d ? C(23) 0.2375(3) 0.3841(2) -0.1048(2) 0.0236(9) 1.000 . Uani d ? C(24) 0.2138(4) 0.4254(2) -0.0414(2) 0.038(1) 1.000 . Uani d ? C(25) 0.2163(3) 0.1656(2) -0.0982(2) 0.0220(9) 1.000 . Uani d ? C(26) 0.1311(3) 0.1793(2) -0.0530(2) 0.0219(8) 1.000 . Uani d ? C(27) 0.0513(3) 0.1373(2) -0.0568(2) 0.034(1) 1.000 . Uani d ? C(28) -0.0320(3) 0.1553(3) -0.0236(3) 0.044(1) 1.000 . Uani d ? C(29) -0.0331(3) 0.2146(2) 0.0088(2) 0.037(1) 1.000 . Uani d ? C(30) 0.0487(3) 0.2541(2) 0.0124(2) 0.0276(9) 1.000 . Uani d ? C(31) 0.0456(3) 0.3201(2) 0.0431(3) 0.037(1) 1.000 . Uani d ? C(32) 0.4236(3) 0.4194(2) 0.1950(2) 0.0209(8) 1.000 . Uani d ? C(33) 0.3655(3) 0.4670(2) 0.1600(2) 0.031(1) 1.000 . Uani d ? C(34) 0.4109(3) 0.5248(2) 0.1439(3) 0.041(1) 1.000 . Uani d ? C(35) 0.5112(4) 0.5340(2) 0.1642(3) 0.048(1) 1.000 . Uani d ? C(36) 0.5682(3) 0.4858(2) 0.2000(3) 0.044(1) 1.000 . Uani d ? C(37) 0.5244(3) 0.4279(2) 0.2150(2) 0.030(1) 1.000 . Uani d ? C(38) 0.1652(3) 0.3759(1) 0.2679(2) 0.0179(8) 1.000 . Uani d ? C(39) 0.2274(3) 0.3677(2) 0.3334(2) 0.0222(9) 1.000 . Uani d ? C(40) 0.1885(3) 0.3774(2) 0.4007(2) 0.0259(9) 1.000 . Uani d ? C(41) 0.0902(3) 0.3957(2) 0.4018(2) 0.029(1) 1.000 . Uani d ? C(42) 0.0283(3) 0.4024(2) 0.3357(2) 0.028(1) 1.000 . Uani d ? C(43) 0.0658(3) 0.3920(2) 0.2680(2) 0.0220(8) 1.000 . Uani d ? C(44) 0.5142(3) 0.2361(2) 0.2891(2) 0.031(1) 1.000 . Uani d ? C(45) 0.4778(4) 0.3563(2) 0.0083(3) 0.045(1) 1.000 . Uani d ? C(46) 0.1416(5) 0.2835(3) -0.4119(4) 0.073(2) 1.000 . Uani d ? H(1) 0.2756 0.1155 0.0394 0.021 1.000 . Uiso c ? H(2) 0.4170 0.0550 0.0730 0.023 1.000 . Uiso c ? H(3) 0.4745 0.1154 0.1033 0.023 1.000 . Uiso c ? H(4) 0.3802 0.1118 -0.0529 0.022 1.000 . Uiso c ? H(5) 0.4429 0.1680 -0.0165 0.022 1.000 . Uiso c ? H(6) 0.4686 0.0249 0.2252 0.026 1.000 . Uiso c ? H(7) 0.5087 0.0944 0.2270 0.026 1.000 . Uiso c ? H(8) 0.4822 0.0036 0.3600 0.036 1.000 . Uiso c ? H(9) 0.4158 0.0245 0.4726 0.044 1.000 . Uiso c ? H(10) 0.3084 0.1112 0.4799 0.039 1.000 . Uiso c ? H(11) 0.2232 0.1993 0.4243 0.046 1.000 . Uiso c ? H(12) 0.2776 0.2351 0.3653 0.046 1.000 . Uiso c ? H(13) 0.1876 0.1912 0.3399 0.046 1.000 . Uiso c ? H(14) 0.2967 0.0126 0.1219 0.027 1.000 . Uiso c ? H(15) 0.3005 0.0124 0.2082 0.027 1.000 . Uiso c ? H(16) 0.1210 -0.0153 0.1191 0.042 1.000 . Uiso c ? H(17) -0.0424 0.0231 0.1213 0.054 1.000 . Uiso c ? H(18) -0.0638 0.1279 0.1613 0.042 1.000 . Uiso c ? H(19) -0.0011 0.2262 0.2021 0.044 1.000 . Uiso c ? H(20) 0.0986 0.2457 0.1734 0.044 1.000 . Uiso c ? H(21) 0.0976 0.2226 0.2550 0.044 1.000 . Uiso c ? H(22) 0.4248 0.2369 -0.1123 0.027 1.000 . Uiso c ? H(23) 0.3517 0.2019 -0.1712 0.027 1.000 . Uiso c ? H(24) 0.3111 0.2867 -0.2598 0.033 1.000 . Uiso c ? H(25) 0.2367 0.3872 -0.2862 0.037 1.000 . Uiso c ? H(26) 0.1949 0.4495 -0.1863 0.031 1.000 . Uiso c ? H(27) 0.1872 0.4650 -0.0603 0.045 1.000 . Uiso c ? H(28) 0.2728 0.4330 -0.0087 0.045 1.000 . Uiso c ? H(29) 0.1662 0.4045 -0.0149 0.045 1.000 . Uiso c ? H(30) 0.1985 0.1805 -0.1477 0.026 1.000 . Uiso c ? H(31) 0.2267 0.1207 -0.0990 0.026 1.000 . Uiso c ? H(32) 0.0536 0.0974 -0.0815 0.041 1.000 . Uiso c ? H(33) -0.0872 0.1272 -0.0233 0.053 1.000 . Uiso c ? H(34) -0.0913 0.2286 0.0290 0.045 1.000 . Uiso c ? H(35) -0.0170 0.3271 0.0609 0.045 1.000 . Uiso c ? H(36) 0.0973 0.3250 0.0831 0.045 1.000 . Uiso c ? H(37) 0.0547 0.3502 0.0050 0.045 1.000 . Uiso c ? H(38) 0.2961 0.4608 0.1470 0.037 1.000 . Uiso c ? H(39) 0.3722 0.5578 0.1189 0.049 1.000 . Uiso c ? H(40) 0.5413 0.5734 0.1536 0.057 1.000 . Uiso c ? H(41) 0.6373 0.4924 0.2144 0.053 1.000 . Uiso c ? H(42) 0.5635 0.3945 0.2388 0.036 1.000 . Uiso c ? H(43) 0.2951 0.3558 0.3325 0.027 1.000 . Uiso c ? H(44) 0.2299 0.3714 0.4463 0.031 1.000 . Uiso c ? H(45) 0.0652 0.4037 0.4481 0.035 1.000 . Uiso c ? H(46) -0.0395 0.4141 0.3366 0.033 1.000 . Uiso c ? H(47) 0.0237 0.3958 0.2223 0.026 1.000 . Uiso c ? H(48) 0.5011 0.2228 0.1830 0.013 1.000 . Uiso c ? H(49) 0.5831 0.2262 0.2976 0.037 1.000 . Uiso c ? H(50) 0.5058 0.2812 0.2869 0.037 1.000 . Uiso c ? H(51) 0.4811 0.2194 0.3286 0.037 1.000 . Uiso c ? H(52) 0.4730 0.2899 0.0652 0.013 1.000 . Uiso c ? H(53) 0.4561 0.3712 -0.0407 0.054 1.000 . Uiso c ? H(54) 0.5486 0.3570 0.0160 0.054 1.000 . Uiso c ? H(55) 0.4519 0.3833 0.0438 0.054 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(1) 0.0192(2) 0.0127(2) 0.0133(2) 0.0005(1) 0.0021(2) -0.0002(1) Ni(2) 0.0176(2) 0.0170(2) 0.0130(2) 0.0022(2) 0.0041(2) -0.0002(1) Cl(1) 0.0422(5) 0.0300(5) 0.0225(5) -0.0000(4) 0.0015(4) -0.0056(3) Cl(2) 0.0319(5) 0.0727(8) 0.0290(5) -0.0182(5) 0.0082(4) -0.0124(5) P(1) 0.0195(4) 0.0139(4) 0.0157(4) 0.0012(3) 0.0040(3) -0.0017(3) O(1) 0.021(1) 0.016(1) 0.014(1) 0.0036(9) 0.0036(9) -0.0018(8) O(2) 0.028(1) 0.014(1) 0.017(1) 0.0010(9) 0.006(1) -0.0012(8) O(3) 0.025(1) 0.017(1) 0.017(1) 0.0011(9) 0.006(1) -0.0021(9) O(4) 0.021(1) 0.018(1) 0.026(1) -0.0020(9) -0.000(1) 0.0034(9) O(5) 0.025(1) 0.020(1) 0.016(1) 0.0060(9) 0.004(1) -0.0010(9) O(6) 0.024(1) 0.024(1) 0.022(1) -0.003(1) 0.002(1) -0.002(1) O(7) 0.021(1) 0.033(1) 0.026(1) -0.006(1) 0.003(1) -0.002(1) O(8) 0.082(3) 0.066(2) 0.044(2) 0.009(2) 0.016(2) -0.025(2) O(9) 0.045(2) 0.088(3) 0.103(4) 0.019(2) 0.015(2) 0.038(3) O(10) 0.137(4) 0.033(2) 0.027(2) -0.026(2) 0.000(2) -0.002(1) O(11) 0.105(3) 0.042(2) 0.031(2) -0.003(2) -0.016(2) 0.003(1) O(20) 0.041(2) 0.067(2) 0.051(2) 0.001(2) 0.004(2) -0.009(2) N(1) 0.022(1) 0.013(1) 0.018(1) 0.003(1) -0.000(1) 0.000(1) N(2) 0.026(2) 0.020(1) 0.018(1) -0.003(1) 0.001(1) 0.002(1) N(3) 0.022(1) 0.016(1) 0.016(1) -0.000(1) 0.005(1) -0.000(1) N(4) 0.018(1) 0.023(1) 0.014(1) 0.003(1) 0.004(1) -0.001(1) N(5) 0.024(1) 0.021(1) 0.016(1) 0.001(1) 0.005(1) 0.001(1) N(6) 0.017(1) 0.027(1) 0.017(1) 0.005(1) 0.001(1) 0.001(1) C(1) 0.020(2) 0.015(1) 0.016(2) 0.004(1) 0.002(1) -0.002(1) C(2) 0.020(2) 0.019(2) 0.019(2) 0.004(1) 0.003(1) -0.002(1) C(3) 0.019(2) 0.019(2) 0.018(2) 0.004(1) 0.005(1) -0.002(1) C(4) 0.025(2) 0.015(1) 0.024(2) 0.003(1) -0.004(1) 0.001(1) C(5) 0.026(2) 0.019(2) 0.023(2) -0.004(1) -0.004(1) 0.003(1) C(6) 0.031(2) 0.027(2) 0.031(2) -0.003(1) -0.006(2) 0.007(2) C(7) 0.040(2) 0.041(2) 0.027(2) -0.008(2) -0.010(2) 0.018(2) C(8) 0.031(2) 0.048(2) 0.018(2) -0.010(2) -0.001(2) 0.005(2) C(9) 0.029(2) 0.030(2) 0.019(2) -0.009(1) 0.000(1) 0.003(1) C(10) 0.052(3) 0.043(2) 0.023(2) 0.010(2) 0.013(2) 0.001(2) C(11) 0.027(2) 0.014(1) 0.026(2) 0.001(1) 0.002(1) -0.002(1) C(12) 0.026(2) 0.017(2) 0.020(2) -0.002(1) 0.005(1) -0.000(1) C(13) 0.030(2) 0.023(2) 0.053(3) -0.003(2) 0.006(2) -0.009(2) C(14) 0.026(2) 0.036(2) 0.073(4) -0.009(2) 0.008(2) -0.013(2) C(15) 0.022(2) 0.034(2) 0.050(3) -0.000(2) 0.012(2) -0.004(2) C(16) 0.025(2) 0.023(2) 0.024(2) 0.004(1) 0.007(1) 0.000(1) C(17) 0.030(2) 0.030(2) 0.049(3) 0.007(2) 0.004(2) -0.011(2) C(18) 0.025(2) 0.029(2) 0.016(2) 0.002(1) 0.010(1) -0.001(1) C(19) 0.019(2) 0.029(2) 0.019(2) -0.003(1) 0.006(1) -0.001(1) C(20) 0.034(2) 0.031(2) 0.020(2) -0.004(2) 0.010(2) -0.000(1) C(21) 0.040(2) 0.035(2) 0.018(2) -0.004(2) 0.005(2) 0.009(1) C(22) 0.026(2) 0.023(2) 0.029(2) -0.002(1) 0.002(2) 0.010(1) C(23) 0.026(2) 0.021(2) 0.025(2) -0.002(1) 0.006(1) 0.004(1) C(24) 0.056(3) 0.031(2) 0.027(2) 0.014(2) 0.010(2) 0.001(2) C(25) 0.025(2) 0.022(2) 0.019(2) 0.001(1) 0.001(1) -0.002(1) C(26) 0.020(2) 0.029(2) 0.016(2) 0.000(1) 0.000(1) 0.003(1) C(27) 0.031(2) 0.039(2) 0.033(2) -0.011(2) 0.003(2) -0.004(2) C(28) 0.026(2) 0.066(3) 0.041(3) -0.013(2) 0.006(2) -0.004(2) C(29) 0.016(2) 0.063(3) 0.034(2) -0.001(2) 0.006(2) -0.004(2) C(30) 0.019(2) 0.043(2) 0.021(2) 0.008(2) 0.002(1) 0.002(2) C(31) 0.028(2) 0.043(2) 0.041(3) 0.015(2) 0.005(2) -0.003(2) C(32) 0.024(2) 0.016(1) 0.024(2) -0.001(1) 0.004(1) -0.000(1) C(33) 0.027(2) 0.023(2) 0.042(2) -0.001(1) 0.000(2) 0.005(2) C(34) 0.039(2) 0.024(2) 0.058(3) -0.002(2) -0.003(2) 0.012(2) C(35) 0.044(3) 0.031(2) 0.067(3) -0.016(2) 0.003(2) 0.012(2) C(36) 0.026(2) 0.043(2) 0.060(3) -0.015(2) -0.003(2) 0.013(2) C(37) 0.024(2) 0.029(2) 0.038(2) -0.001(1) 0.002(2) 0.006(2) C(38) 0.027(2) 0.010(1) 0.017(2) -0.000(1) 0.009(1) -0.001(1) C(39) 0.027(2) 0.021(2) 0.020(2) 0.001(1) 0.006(1) -0.003(1) C(40) 0.035(2) 0.024(2) 0.019(2) -0.007(1) 0.006(1) -0.002(1) C(41) 0.031(2) 0.031(2) 0.026(2) -0.012(2) 0.016(2) -0.003(1) C(42) 0.025(2) 0.028(2) 0.032(2) -0.006(1) 0.015(2) -0.003(1) C(43) 0.026(2) 0.016(2) 0.024(2) -0.004(1) 0.006(1) 0.000(1) C(44) 0.031(2) 0.028(2) 0.032(2) -0.003(2) -0.007(2) -0.004(2) C(45) 0.040(3) 0.041(2) 0.056(3) -0.015(2) 0.013(2) -0.000(2) C(46) 0.098(5) 0.038(3) 0.071(4) -0.020(3) -0.041(4) 0.015(3) #============================================================================== # REFINEMENT DATA _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) + 0.00189|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 8547 _refine_ls_number_parameters 654 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_all 0.0776 _refine_ls_wR_factor_ref 0.0776 _refine_ls_goodness_of_fit_all 1.498 _refine_ls_goodness_of_fit_ref 1.498 _refine_ls_shift/su_max 0.0007 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.58 _refine_diff_density_max 2.20 #============================================================================== # MOLECULAR GEOMETRY _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ 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 # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ 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 ? ? ? ? ? ? # -- ENTER NON-BONDED CONTACTS HERE, ONE PER LINE -- # e.g. O1 N1 2.841(1) . . yes #------------------------------------------------------------------------------ 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 #------------------------------------------------------------------------------ #============================================================================== data__[Cu2(Me4tpdp)(BNP)](ClO4)2 _database_code_CSD 153183 #============================================================================== _audit_creation_date '2000-10-31' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ? #============================================================================== _computing_data_collection Rigaku RAXIS-IV _computing_cell_refinement Rigaku RAXIS-IV _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS86' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 22.941(4) _cell_length_b 36.360(4) _cell_length_c 14.160(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11812(2) _cell_formula_units_Z 8 _cell_measurement_temperature 288.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'spindle' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1296.52 _chemical_formula_analytical ? _chemical_formula_sum 'C48 H59.50 Cl2 Cu2 N8.50 O19.50 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 5360.00 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 288.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _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 7732 _reflns_number_total 7732 _reflns_number_gt 4691 _reflns_threshold_expression I>3.00\\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 25.69 _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 Cu 0 16 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 384 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 476 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 68 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 156 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cu(1) 0.22943(4) 0.61865(3) -0.00304(8) 0.0334(3) 1.000 . Uani d ? Cu(2) 0.20207(4) 0.61562(3) 0.25999(7) 0.0333(3) 1.000 . Uani d ? Cl(1) 0.0367(1) 0.51054(8) 0.6661(2) 0.067(1) 1.000 . Uani d ? Cl(2) 0.1018(2) 0.7500 0.1335(3) 0.050(1) 0.500 ST Uani d ? Cl(3) 0.4900(3) 0.2500 0.1557(4) 0.119(2) 0.500 ST Uani d ? P(1) 0.1523(1) 0.56518(6) 0.1060(2) 0.0345(8) 1.000 . Uani d ? O(1) 0.2284(2) 0.6346(1) 0.1328(4) 0.029(2) 1.000 . Uani d ? O(2) 0.1976(2) 0.5711(1) 0.0286(4) 0.038(2) 1.000 . Uani d ? O(3) 0.1703(2) 0.5720(1) 0.2052(4) 0.033(2) 1.000 . Uani d ? O(4) 0.1259(2) 0.5244(1) 0.0981(4) 0.031(2) 1.000 . Uani d ? O(5) 0.0984(2) 0.5890(1) 0.0787(4) 0.040(2) 1.000 . Uani d ? O(6) 0.2819(3) 0.3868(2) 0.0828(5) 0.058(2) 1.000 . Uani d ? O(7) 0.2239(4) 0.3680(2) 0.1895(5) 0.103(3) 1.000 . Uani d ? O(8) -0.1077(3) 0.6160(2) 0.3609(6) 0.089(3) 1.000 . Uani d ? O(9) -0.0865(3) 0.6725(2) 0.3244(7) 0.100(4) 1.000 . Uani d ? O(10) -0.0220(2) 0.5051(2) 0.6942(5) 0.078(2) 1.000 . Uani d ? O(11) 0.0497(3) 0.5459(2) 0.6311(5) 0.086(2) 1.000 . Uani d ? O(12) 0.0501(4) 0.4815(2) 0.5920(6) 0.184(4) 1.000 . Uani d ? O(13) 0.0727(3) 0.5015(2) 0.7417(7) 0.134(4) 1.000 . Uani d ? O(14) 0.0876(3) 0.7185(2) 0.0851(7) 0.101(3) 1.000 . Uani d ? O(15) 0.1655(3) 0.7500 0.1516(7) 0.065(3) 0.500 ST Uani d ? O(16) 0.0721(5) 0.7500 0.2186(9) 0.141(7) 0.500 ST Uani d ? O(17) 0.460(1) 0.2500 0.094(2) 0.35(2) 0.500 ST Uani d ? O(18) 0.4564(6) 0.2500 0.2437(9) 0.136(5) 0.500 ST Uani d ? O(19) 0.5121(4) 0.2179(2) 0.1326(8) 0.173(5) 1.000 . Uani d ? O(20) 1.0088 0.1110 0.0945 0.197 1.000 . Uiso c ? O(21) 1.1013(8) 0.2285(6) -0.025(2) 0.16(1) 0.500 S Uiso d ? O(22) 1.123(1) 0.2500 -0.142(2) 0.17(1) 0.300 S Uiso d ? O(23) 0.771(2) 0.2500 0.462(3) 0.06(2) 0.200 S Uiso d ? O(24) 0.2294(6) 0.2500 0.254(1) 0.143(5) 0.500 S Uiso d ? N(1) 0.2539(3) 0.6697(2) -0.0286(5) 0.032(2) 1.000 . Uani d ? N(2) 0.3178(3) 0.6084(2) -0.0599(5) 0.027(2) 1.000 . Uani d ? N(3) 0.1817(3) 0.6288(2) -0.1245(5) 0.040(3) 1.000 . Uani d ? N(4) 0.2261(3) 0.6640(2) 0.3083(5) 0.036(2) 1.000 . Uani d ? N(5) 0.2821(3) 0.6013(2) 0.3377(5) 0.037(2) 1.000 . Uani d ? N(6) 0.1378(3) 0.6224(2) 0.3635(5) 0.028(2) 1.000 . Uani d ? N(7) 0.2399(4) 0.3916(2) 0.1356(6) 0.056(3) 1.000 . Uani d ? N(8) -0.0782(4) 0.6403(3) 0.3229(6) 0.058(3) 1.000 . Uani d ? N(9) 0.0490(8) 0.2500 0.603(1) 0.078(7) 0.500 S Uiso d ? C(1) 0.2355(3) 0.6730(2) 0.1385(6) 0.029(3) 1.000 . Uani d ? C(2) 0.2759(4) 0.6856(2) 0.0576(6) 0.034(3) 1.000 . Uani d ? C(3) 0.2610(4) 0.6842(2) 0.2344(6) 0.036(3) 1.000 . Uani d ? C(4) 0.3002(4) 0.6715(2) -0.1024(5) 0.035(3) 1.000 . Uani d ? C(5) 0.3401(4) 0.6384(3) -0.0957(6) 0.045(3) 1.000 . Uani d ? C(6) 0.3948(4) 0.6431(3) -0.1315(6) 0.034(3) 1.000 . Uani d ? C(7) 0.4287(4) 0.6120(3) -0.1261(7) 0.051(4) 1.000 . Uani d ? C(8) 0.4075(4) 0.5800(3) -0.0902(7) 0.048(3) 1.000 . Uani d ? C(9) 0.3516(4) 0.5796(3) -0.0549(6) 0.039(3) 1.000 . Uani d ? C(10) 0.3266(4) 0.5438(2) -0.0168(7) 0.046(3) 1.000 . Uani d ? C(11) 0.2027(4) 0.6899(2) -0.0620(6) 0.048(3) 1.000 . Uani d ? C(12) 0.1709(4) 0.6640(3) -0.1315(7) 0.040(3) 1.000 . Uani d ? C(13) 0.1362(5) 0.6775(3) -0.2006(8) 0.057(4) 1.000 . Uani d ? C(14) 0.1108(5) 0.6537(3) -0.2674(9) 0.081(5) 1.000 . Uani d ? C(15) 0.1189(5) 0.6168(3) -0.2563(8) 0.081(4) 1.000 . Uani d ? C(16) 0.1594(4) 0.6031(3) -0.1850(7) 0.047(3) 1.000 . Uani d ? C(17) 0.1741(4) 0.5637(3) -0.1817(7) 0.056(3) 1.000 . Uani d ? C(18) 0.2605(4) 0.6593(2) 0.3994(6) 0.040(3) 1.000 . Uani d ? C(19) 0.3032(4) 0.6275(3) 0.3946(6) 0.038(3) 1.000 . Uani d ? C(20) 0.3520(4) 0.6284(3) 0.4375(7) 0.055(3) 1.000 . Uani d ? C(21) 0.3856(4) 0.6015(3) 0.4324(8) 0.070(4) 1.000 . Uani d ? C(22) 0.3694(4) 0.5687(3) 0.3807(7) 0.041(4) 1.000 . Uani d ? C(23) 0.3149(4) 0.5701(3) 0.3320(7) 0.041(4) 1.000 . Uani d ? C(24) 0.2901(4) 0.5379(3) 0.2706(8) 0.061(4) 1.000 . Uani d ? C(25) 0.1727(4) 0.6847(2) 0.3288(6) 0.039(3) 1.000 . Uani d ? C(26) 0.1308(4) 0.6577(2) 0.3789(6) 0.033(3) 1.000 . Uani d ? C(27) 0.0842(4) 0.6700(2) 0.4361(7) 0.035(3) 1.000 . Uani d ? C(28) 0.0457(4) 0.6450(3) 0.4796(6) 0.046(3) 1.000 . Uani d ? C(29) 0.0581(4) 0.6087(3) 0.4658(6) 0.048(3) 1.000 . Uani d ? C(30) 0.1064(4) 0.5961(2) 0.4104(6) 0.034(3) 1.000 . Uani d ? C(31) 0.1205(4) 0.5563(2) 0.4018(6) 0.042(3) 1.000 . Uani d ? C(32) 0.1573(4) 0.4940(2) 0.1072(6) 0.023(3) 1.000 . Uani d ? C(33) 0.2047(4) 0.4868(2) 0.0543(6) 0.045(3) 1.000 . Uani d ? C(34) 0.2343(4) 0.4527(2) 0.0636(7) 0.041(3) 1.000 . Uani d ? C(35) 0.2150(4) 0.4285(2) 0.1270(6) 0.043(3) 1.000 . Uani d ? C(36) 0.1683(4) 0.4349(3) 0.1822(7) 0.047(4) 1.000 . Uani d ? C(37) 0.1402(4) 0.4667(3) 0.1714(7) 0.044(3) 1.000 . Uani d ? C(38) 0.0554(4) 0.6013(2) 0.1440(6) 0.042(3) 1.000 . Uani d ? C(39) 0.0446(4) 0.6387(3) 0.1475(7) 0.047(3) 1.000 . Uani d ? C(40) -0.0036(4) 0.6504(2) 0.2102(7) 0.043(3) 1.000 . Uani d ? C(41) -0.0326(4) 0.6255(2) 0.2651(7) 0.043(3) 1.000 . Uani d ? C(42) -0.0196(4) 0.5902(2) 0.2588(7) 0.036(3) 1.000 . Uani d ? C(43) 0.0235(3) 0.5760(2) 0.2002(6) 0.041(3) 1.000 . Uani d ? C(44) 1.0246 0.1919 0.0639 0.288 1.000 . Uiso c ? C(45) 1.0278 0.1578 0.1134 0.214 1.000 . Uiso c ? C(46) 0.9983 0.0318 0.0556 0.169 1.000 . Uiso c ? C(47) 0.9921 0.0700 0.1163 0.190 1.000 . Uiso c ? C(48) 0.141(1) 0.2500 0.491(2) 0.144(9) 0.500 S Uiso d ? C(49) 0.105(1) 0.2500 0.530(3) 0.29(2) 0.500 S Uiso d ? H(1) 0.1961 0.6852 0.1331 0.045 1.000 . Uiso c ? H(2) 0.3131 0.6775 0.0714 0.052 1.000 . Uiso c ? H(3) 0.2755 0.7125 0.0567 0.052 1.000 . Uiso c ? H(4) 0.2624 0.7089 0.2455 0.052 1.000 . Uiso c ? H(5) 0.3008 0.6739 0.2380 0.052 1.000 . Uiso c ? H(6) 0.2788 0.6718 -0.1658 0.050 1.000 . Uiso c ? H(7) 0.3183 0.6952 -0.1003 0.050 1.000 . Uiso c ? H(8) 0.4101 0.6656 -0.1586 0.063 1.000 . Uiso c ? H(9) 0.4726 0.6120 -0.1483 0.073 1.000 . Uiso c ? H(10) 0.4341 0.5584 -0.0899 0.067 1.000 . Uiso c ? H(11) 0.3157 0.5462 0.0491 0.074 1.000 . Uiso c ? H(12) 0.2967 0.5349 -0.0520 0.074 1.000 . Uiso c ? H(13) 0.3582 0.5245 -0.0153 0.074 1.000 . Uiso c ? H(14) 0.1741 0.6946 -0.0120 0.058 1.000 . Uiso c ? H(15) 0.2093 0.7122 -0.0939 0.058 1.000 . Uiso c ? H(16) 0.1259 0.7047 -0.2117 0.088 1.000 . Uiso c ? H(17) 0.0785 0.6623 -0.3175 0.104 1.000 . Uiso c ? H(18) 0.1026 0.5992 -0.3055 0.090 1.000 . Uiso c ? H(19) 0.1594 0.5551 -0.1234 0.068 1.000 . Uiso c ? H(20) 0.1527 0.5506 -0.2318 0.068 1.000 . Uiso c ? H(21) 0.2126 0.5613 -0.1892 0.068 1.000 . Uiso c ? H(22) 0.2805 0.6816 0.4134 0.055 1.000 . Uiso c ? H(23) 0.2324 0.6555 0.4513 0.055 1.000 . Uiso c ? H(24) 0.3636 0.6482 0.4772 0.062 1.000 . Uiso c ? H(25) 0.4248 0.5955 0.4649 0.079 1.000 . Uiso c ? H(26) 0.3922 0.5450 0.3756 0.074 1.000 . Uiso c ? H(27) 0.2560 0.5293 0.2941 0.080 1.000 . Uiso c ? H(28) 0.2861 0.5463 0.2062 0.080 1.000 . Uiso c ? H(29) 0.3197 0.5186 0.2691 0.080 1.000 . Uiso c ? H(30) 0.1752 0.7065 0.3646 0.055 1.000 . Uiso c ? H(31) 0.1503 0.6926 0.2691 0.055 1.000 . Uiso c ? H(32) 0.0809 0.6974 0.4504 0.056 1.000 . Uiso c ? H(33) 0.0146 0.6536 0.5183 0.057 1.000 . Uiso c ? H(34) 0.0332 0.5915 0.4981 0.053 1.000 . Uiso c ? H(35) 0.0919 0.5432 0.4378 0.048 1.000 . Uiso c ? H(36) 0.1165 0.5504 0.3374 0.048 1.000 . Uiso c ? H(37) 0.1573 0.5528 0.4245 0.048 1.000 . Uiso c ? H(38) 0.2153 0.5034 0.0032 0.060 1.000 . Uiso c ? H(39) 0.2691 0.4479 0.0262 0.059 1.000 . Uiso c ? H(40) 0.1542 0.4162 0.2266 0.072 1.000 . Uiso c ? H(41) 0.1059 0.4726 0.2167 0.066 1.000 . Uiso c ? H(42) 0.0657 0.6559 0.1079 0.063 1.000 . Uiso c ? H(43) -0.0105 0.6773 0.2052 0.061 1.000 . Uiso c ? H(44) -0.0404 0.5729 0.2975 0.050 1.000 . Uiso c ? H(45) 0.0341 0.5495 0.1930 0.049 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 Cu(1) 0.0266(6) 0.0358(6) 0.0378(6) -0.0022(6) 0.0020(6) -0.0009(6) Cu(2) 0.0285(6) 0.0355(6) 0.0358(6) -0.0003(6) 0.0009(6) 0.0009(6) Cl(1) 0.042(2) 0.076(2) 0.085(2) -0.002(1) -0.003(2) 0.030(2) Cl(2) 0.045(2) 0.040(2) 0.066(3) 0.0000 0.007(2) 0.0000 Cl(3) 0.206(7) 0.066(3) 0.084(5) 0.0000 0.005(5) 0.0000 P(1) 0.027(2) 0.035(1) 0.042(2) -0.001(1) 0.001(1) -0.000(1) O(1) 0.027(4) 0.025(3) 0.034(4) -0.011(3) 0.007(3) -0.015(3) O(2) 0.026(3) 0.055(4) 0.031(4) -0.005(3) 0.013(3) -0.012(3) O(3) 0.017(3) 0.047(4) 0.036(3) -0.001(3) 0.006(3) -0.009(3) O(4) 0.008(3) 0.042(3) 0.043(4) -0.002(3) 0.004(3) -0.009(3) O(5) 0.030(4) 0.050(4) 0.039(4) 0.000(3) -0.000(3) 0.006(4) O(6) 0.050(5) 0.069(5) 0.055(5) 0.021(4) -0.023(4) -0.015(5) O(7) 0.115(7) 0.118(6) 0.076(6) 0.028(5) 0.046(5) 0.061(5) O(8) 0.069(6) 0.128(7) 0.070(6) 0.015(6) 0.048(5) 0.003(6) O(9) 0.059(6) 0.085(6) 0.16(1) 0.011(5) 0.023(6) -0.056(7) O(10) 0.026(4) 0.114(5) 0.092(6) 0.001(4) 0.020(4) 0.028(5) O(11) 0.095(5) 0.075(5) 0.088(5) -0.033(4) -0.003(5) 0.019(4) O(12) 0.27(1) 0.163(7) 0.120(8) 0.033(8) 0.074(8) -0.046(7) O(13) 0.086(6) 0.113(6) 0.203(9) -0.030(5) -0.098(7) 0.065(7) O(14) 0.054(5) 0.023(4) 0.23(1) -0.009(4) -0.029(6) -0.035(6) O(15) 0.025(6) 0.050(6) 0.121(8) 0.0000 -0.030(6) 0.0000 O(16) 0.060(9) 0.30(2) 0.07(1) 0.0000 0.022(8) 0.0000 O(17) 0.77(3) 0.24(2) 0.04(4) 0.0000 0.04(3) 0.0000 O(18) 0.24(1) 0.086(9) 0.079(9) 0.0000 0.07(1) 0.0000 O(19) 0.30(1) -0.002(6) 0.22(1) 0.062(7) 0.10(1) 0.024(7) N(1) 0.029(5) 0.031(4) 0.037(5) 0.014(4) -0.009(4) -0.000(4) N(2) 0.028(5) -0.004(5) 0.056(5) 0.005(4) 0.000(4) 0.006(4) N(3) 0.034(5) 0.051(5) 0.034(5) 0.004(4) -0.002(4) 0.007(5) N(4) 0.026(5) 0.052(4) 0.029(4) 0.009(4) 0.003(4) -0.007(4) N(5) 0.020(5) 0.048(5) 0.044(5) 0.020(4) 0.016(4) 0.009(4) N(6) 0.032(4) 0.027(5) 0.026(5) 0.008(4) -0.001(4) -0.006(4) N(7) 0.037(7) 0.095(7) 0.035(5) 0.035(6) 0.013(5) -0.016(5) N(8) -0.000(6) 0.092(7) 0.083(7) 0.020(5) 0.021(5) -0.034(6) C(1) 0.015(6) 0.023(5) 0.050(6) -0.006(5) -0.008(5) -0.000(5) C(2) 0.034(6) 0.047(6) 0.021(6) 0.001(5) -0.003(5) -0.005(5) C(3) 0.032(6) 0.053(5) 0.023(6) -0.012(5) -0.007(5) 0.002(5) C(4) 0.054(7) 0.033(5) 0.019(5) -0.021(5) -0.017(5) 0.004(5) C(5) 0.021(6) 0.084(6) 0.029(6) -0.005(5) -0.013(5) -0.026(5) C(6) 0.034(7) 0.022(8) 0.045(6) 0.007(6) -0.002(5) 0.003(6) C(7) 0.030(7) 0.084(8) 0.040(6) -0.031(7) -0.008(6) 0.001(7) C(8) 0.031(7) 0.052(7) 0.059(7) 0.023(6) 0.005(6) -0.033(6) C(9) 0.019(6) 0.058(7) 0.040(6) 0.003(6) -0.001(5) -0.010(6) C(10) 0.023(6) 0.030(5) 0.084(8) 0.000(5) 0.009(6) 0.014(6) C(11) 0.036(6) 0.077(6) 0.032(6) 0.002(5) 0.018(6) -0.016(6) C(12) 0.016(7) 0.072(7) 0.031(7) 0.017(5) -0.009(6) 0.024(6) C(13) 0.074(9) 0.048(7) 0.048(8) 0.036(7) 0.009(8) -0.012(7) C(14) 0.103(9) 0.088(9) 0.05(1) -0.001(8) -0.055(8) 0.013(9) C(15) 0.073(8) 0.091(9) 0.079(7) -0.049(8) -0.008(7) -0.014(8) C(16) 0.028(7) 0.084(7) 0.030(7) -0.007(6) -0.027(6) 0.015(6) C(17) 0.069(7) 0.025(6) 0.073(7) -0.017(6) -0.021(6) -0.005(6) C(18) 0.052(6) 0.041(6) 0.028(6) -0.022(5) -0.021(5) 0.008(5) C(19) 0.056(6) 0.030(7) 0.028(6) 0.006(6) 0.012(6) -0.010(5) C(20) 0.009(6) 0.095(7) 0.061(7) 0.025(6) -0.036(6) -0.007(6) C(21) 0.041(7) 0.108(9) 0.061(7) -0.052(7) -0.036(6) 0.021(8) C(22) -0.006(7) 0.080(8) 0.048(8) 0.030(6) 0.009(6) 0.061(7) C(23) 0.028(6) 0.070(9) 0.026(7) -0.006(6) 0.023(5) 0.003(7) C(24) 0.042(7) 0.099(6) 0.040(9) 0.043(6) 0.020(7) 0.006(7) C(25) 0.031(6) 0.038(5) 0.049(6) 0.012(5) 0.003(5) 0.007(5) C(26) 0.042(6) 0.037(6) 0.021(6) 0.014(5) -0.000(5) -0.006(5) C(27) 0.059(7) 0.002(6) 0.043(6) 0.018(5) -0.031(6) -0.011(5) C(28) 0.016(6) 0.095(7) 0.026(6) -0.023(6) 0.013(5) -0.004(6) C(29) 0.045(6) 0.054(7) 0.046(6) -0.013(5) -0.000(5) 0.008(5) C(30) 0.033(6) 0.047(6) 0.023(5) 0.010(5) -0.012(5) -0.002(5) C(31) 0.034(6) 0.054(6) 0.039(6) 0.000(5) 0.009(5) -0.015(5) C(32) 0.028(6) -0.005(6) 0.047(6) -0.011(5) -0.000(5) -0.007(5) C(33) 0.043(7) 0.036(5) 0.056(7) -0.003(5) 0.022(6) 0.007(5) C(34) 0.061(7) 0.025(6) 0.037(7) -0.013(6) 0.010(6) 0.000(6) C(35) 0.052(7) 0.047(6) 0.029(5) 0.017(6) -0.010(5) -0.008(6) C(36) 0.037(8) 0.055(8) 0.049(7) 0.020(7) 0.007(6) 0.026(7) C(37) 0.022(7) 0.071(7) 0.039(7) 0.014(6) 0.008(6) -0.005(6) C(38) 0.018(6) 0.066(6) 0.040(6) 0.007(5) -0.021(5) -0.020(6) C(39) 0.037(6) 0.051(7) 0.053(7) -0.007(6) -0.021(6) 0.008(6) C(40) 0.035(7) 0.037(6) 0.056(7) 0.018(6) -0.019(6) -0.014(6) C(41) 0.036(6) 0.039(7) 0.052(6) -0.023(5) -0.018(5) 0.005(6) C(42) 0.024(5) 0.066(6) 0.019(6) -0.005(5) 0.005(5) -0.000(6) C(43) 0.021(5) 0.064(6) 0.038(6) -0.009(5) -0.020(5) -0.000(5) #============================================================================== # REFINEMENT DATA _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) + 0.00240|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000044(1) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4691 _refine_ls_number_parameters 690 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.1120 _refine_ls_wR_factor_all 0.0580 _refine_ls_wR_factor_ref 0.0580 _refine_ls_goodness_of_fit_all 4.255 _refine_ls_goodness_of_fit_ref 4.260 _refine_ls_shift/su_max 24.9300 _refine_ls_shift/su_mean 2.7738 _refine_diff_density_min -0.70 _refine_diff_density_max 1.18 #============================================================================== # MOLECULAR GEOMETRY _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 CU1 O1 2.01(1) . . ? CU1 O2 1.93(1) . . ? CU1 N1 1.97(1) . . ? CU1 N2 2.21(1) . . ? CU1 N3 2.07(2) . . ? CU2 O1 2.02(1) . . ? CU2 O3 1.91(1) . . ? CU2 N4 1.96(1) . . ? CU2 N5 2.20(1) . . ? CU2 N6 2.09(1) . . ? CL1 O10 1.42(1) . . ? CL1 O11 1.41(1) . . ? CL1 O12 1.52(2) . . ? CL1 O13 1.39(2) . . ? CL2 O14 1.37(1) . . ? CL2 O14 1.37(1) . . ? CL2 O15 1.48(2) . . ? CL2 O16 1.38(2) . . ? CL3 O17 1.11(5) . . ? CL3 O18 1.47(3) . . ? CL3 O19 1.31(2) . . ? CL3 O19 1.31(2) . . ? P1 O2 1.52(1) . . ? P1 O3 1.49(1) . . ? P1 O4 1.60(1) . . ? P1 O5 1.56(1) . . ? O1 C1 1.41(2) . . ? O4 C32 1.33(2) . . ? O5 C38 1.42(2) . . ? O6 N7 1.23(2) . . ? O7 N7 1.21(2) . . ? O8 N8 1.24(2) . . ? O9 N8 1.19(2) . . ? O20 C45 1.7762(2) . . ? O20 C47 1.5714(2) . . ? O21 O21 1.56(9) . . ? N1 C2 1.44(2) . . ? N1 C4 1.49(2) . . ? N1 C11 1.46(2) . . ? N2 C5 1.31(2) . . ? N2 C9 1.31(2) . . ? N3 C12 1.31(2) . . ? N3 C16 1.37(2) . . ? N4 C3 1.51(2) . . ? N4 C18 1.52(2) . . ? N4 C25 1.47(2) . . ? N5 C19 1.34(2) . . ? N5 C23 1.36(2) . . ? N6 C26 1.31(2) . . ? N6 C30 1.37(2) . . ? N7 C35 1.46(2) . . ? N8 C41 1.43(2) . . ? N9 C49 1.65(8) . . ? C1 C2 1.54(2) . . ? C1 C3 1.53(2) . . ? C1 H1 1.01 . . no C2 H2 0.92 . . no C2 H3 0.98 . . no C3 H4 0.91 . . no C3 H5 0.99 . . no C4 C5 1.52(2) . . ? C4 H6 1.02 . . no C4 H7 0.96 . . no C5 C6 1.36(2) . . ? C6 C7 1.37(3) . . ? C6 H8 0.97 . . no C7 C8 1.36(3) . . ? C7 H9 1.05 . . no C8 C9 1.38(2) . . ? C8 H10 0.99 . . no C9 C10 1.52(2) . . ? C10 H11 0.97 . . no C10 H12 0.91 . . no C10 H13 1.01 . . no C11 C12 1.55(2) . . ? C11 H14 0.98 . . no C11 H15 0.94 . . no C12 C13 1.35(3) . . ? C13 C14 1.41(3) . . ? C13 H16 1.03 . . no C14 C15 1.37(3) . . ? C14 H17 1.07 . . no C15 C16 1.46(3) . . ? C15 H18 1.02 . . no C16 C17 1.47(3) . . ? C17 H19 0.94 . . no C17 H20 0.99 . . no C17 H21 0.89 . . no C18 C19 1.52(2) . . ? C18 H22 0.95 . . no C18 H23 0.99 . . no C19 C20 1.27(2) . . ? C20 C21 1.25(3) . . ? C20 H24 0.95 . . no C21 C22 1.45(3) . . ? C21 H25 1.03 . . no C22 C23 1.43(2) . . ? C22 H26 1.01 . . no C23 C24 1.57(3) . . ? C24 H27 0.90 . . no C24 H28 0.97 . . no C24 H29 0.98 . . no C25 C26 1.55(2) . . ? C25 H30 0.94 . . no C25 H31 1.03 . . no C26 C27 1.41(2) . . ? C27 C28 1.41(2) . . ? C27 H32 1.02 . . no C28 C29 1.36(2) . . ? C28 H33 0.95 . . no C29 C30 1.43(2) . . ? C29 H34 0.96 . . no C30 C31 1.49(2) . . ? C31 H35 0.96 . . no C31 H36 0.94 . . no C31 H37 0.91 . . no C32 C33 1.35(2) . . ? C32 C37 1.40(2) . . ? C33 C34 1.42(2) . . ? C33 H38 0.97 . . no C34 C35 1.33(2) . . ? C34 H39 0.97 . . no C35 C36 1.35(2) . . ? C36 C37 1.33(3) . . ? C36 H40 0.98 . . no C37 H41 1.04 . . no C38 C39 1.38(2) . . ? C38 C43 1.42(2) . . ? C39 C40 1.48(2) . . ? C39 H42 0.97 . . no C40 C41 1.37(2) . . ? C40 H43 1.00 . . no C41 C42 1.32(2) . . ? C42 C43 1.39(2) . . ? C42 H44 0.96 . . no C43 H45 1.00 . . no C44 C45 1.4275(1) . . ? C46 C47 1.6385(2) . . ? C48 C49 0.99(8) . . ? #------------------------------------------------------------------------------ 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 CU1 O2 91.8(4) . . . ? O1 CU1 N1 84.7(5) . . . ? O1 CU1 N2 114.0(5) . . . ? O1 CU1 N3 137.5(5) . . . ? O2 CU1 N1 173.4(5) . . . ? O2 CU1 N2 106.3(5) . . . ? O2 CU1 N3 98.7(5) . . . ? N1 CU1 N2 80.2(5) . . . ? N1 CU1 N3 80.3(6) . . . ? N2 CU1 N3 102.2(6) . . . ? O1 CU2 O3 92.0(4) . . . ? O1 CU2 N4 85.5(5) . . . ? O1 CU2 N5 106.0(5) . . . ? O1 CU2 N6 142.7(5) . . . ? O3 CU2 N4 172.3(5) . . . ? O3 CU2 N5 108.9(5) . . . ? O3 CU2 N6 96.5(5) . . . ? N4 CU2 N5 78.7(6) . . . ? N4 CU2 N6 81.3(6) . . . ? N5 CU2 N6 105.4(5) . . . ? O10 CL1 O11 115.3(9) . . . ? O10 CL1 O12 107(1) . . . ? O10 CL1 O13 108(1) . . . ? O11 CL1 O12 110(1) . . . ? O11 CL1 O13 111(1) . . . ? O12 CL1 O13 104(1) . . . ? O14 CL2 O14 113(2) . . . ? O14 CL2 O15 108.5(8) . . . ? O14 CL2 O16 109(1) . . . ? O14 CL2 O15 108.5(8) 7_565 7_565 7_565 ? O14 CL2 O16 109(1) 7_565 7_565 7_565 ? O15 CL2 O16 110(2) . . . ? O17 CL3 O18 110(3) . . . ? O17 CL3 O19 93(2) . . . ? O17 CL3 O19 93(2) . . . ? O18 CL3 O19 114(1) . . . ? O18 CL3 O19 114(1) . . . ? O19 CL3 O19 125(2) . . . ? O2 P1 O3 117.9(7) . . . ? O2 P1 O4 109.8(6) . . . ? O2 P1 O5 106.5(7) . . . ? O3 P1 O4 108.9(7) . . . ? O3 P1 O5 111.2(7) . . . ? O4 P1 O5 101.3(6) . . . ? CU1 O1 CU2 139.4(5) . . . ? CU1 O1 C1 110(1) . . . ? CU2 O1 C1 109(1) . . . ? CU1 O2 P1 123.5(7) . . . ? CU2 O3 P1 128.9(7) . . . ? P1 O4 C32 124(1) . . . ? P1 O5 C38 124(1) . . . ? C45 O20 C47 160.012(3) . . . ? CU1 N1 C2 109(1) . . . ? CU1 N1 C4 112(1) . . . ? CU1 N1 C11 108(1) . . . ? C2 N1 C4 109(1) . . . ? C2 N1 C11 111(1) . . . ? C4 N1 C11 109(1) . . . ? CU1 N2 C5 111(1) . . . ? CU1 N2 C9 131(1) . . . ? C5 N2 C9 117(2) . . . ? CU1 N3 C12 110(1) . . . ? CU1 N3 C16 127(1) . . . ? C12 N3 C16 123(2) . . . ? CU2 N4 C3 110(1) . . . ? CU2 N4 C18 110(1) . . . ? CU2 N4 C25 107(1) . . . ? C3 N4 C18 111(1) . . . ? C3 N4 C25 109(1) . . . ? C18 N4 C25 109(1) . . . ? CU2 N5 C19 116(1) . . . ? CU2 N5 C23 129(1) . . . ? C19 N5 C23 115(2) . . . ? CU2 N6 C26 108(1) . . . ? CU2 N6 C30 129(1) . . . ? C26 N6 C30 123(2) . . . ? O6 N7 O7 122(2) . . . ? O6 N7 C35 113(2) . . . ? O7 N7 C35 126(2) . . . ? O8 N8 O9 128(2) . . . ? O8 N8 C41 112(2) . . . ? O9 N8 C41 120(2) . . . ? O1 C1 C2 109(1) . . . ? O1 C1 C3 111(1) . . . ? O1 C1 H1 109.1 . . . no C2 C1 C3 111(1) . . . ? C2 C1 H1 110.6 . . . no C3 C1 H1 107.0 . . . no N1 C2 C1 108(1) . . . ? N1 C2 H2 112.1 . . . no N1 C2 H3 112.7 . . . no C1 C2 H2 107.8 . . . no C1 C2 H3 107.5 . . . no H2 C2 H3 109.1 . . . no N4 C3 C1 106(1) . . . ? N4 C3 H4 112.2 . . . no N4 C3 H5 105.7 . . . no C1 C3 H4 115.2 . . . no C1 C3 H5 107.4 . . . no H4 C3 H5 109.4 . . . no N1 C4 C5 111(1) . . . ? N1 C4 H6 105.8 . . . no N1 C4 H7 109.1 . . . no C5 C4 H6 110.5 . . . no C5 C4 H7 116.9 . . . no H6 C4 H7 103.2 . . . no N2 C5 C4 117(2) . . . ? N2 C5 C6 128(2) . . . ? C4 C5 C6 116(2) . . . ? C5 C6 C7 113(2) . . . ? C5 C6 H8 126.0 . . . no C7 C6 H8 120.7 . . . no C6 C7 C8 122(2) . . . ? C6 C7 H9 121.6 . . . no C8 C7 H9 116.9 . . . no C7 C8 C9 119(2) . . . ? C7 C8 H10 117.2 . . . no C9 C8 H10 124.2 . . . no N2 C9 C8 122(2) . . . ? N2 C9 C10 119(2) . . . ? C8 C9 C10 119(2) . . . ? C9 C10 H11 111.4 . . . no C9 C10 H12 113.4 . . . no C9 C10 H13 109.4 . . . no H11 C10 H12 111.3 . . . no H11 C10 H13 103.1 . . . no H12 C10 H13 107.7 . . . no N1 C11 C12 106(1) . . . ? N1 C11 H14 113.0 . . . no N1 C11 H15 117.4 . . . no C12 C11 H14 104.4 . . . no C12 C11 H15 107.2 . . . no H14 C11 H15 107.7 . . . no N3 C12 C11 117(2) . . . ? N3 C12 C13 121(2) . . . ? C11 C12 C13 121(2) . . . ? C12 C13 C14 120(2) . . . ? C12 C13 H16 126.4 . . . no C14 C13 H16 113.1 . . . no C13 C14 C15 118(2) . . . ? C13 C14 H17 123.6 . . . no C15 C14 H17 117.0 . . . no C14 C15 C16 120(2) . . . ? C14 C15 H18 119.3 . . . no C16 C15 H18 119.7 . . . no N3 C16 C15 116(2) . . . ? N3 C16 C17 124(2) . . . ? C15 C16 C17 120(2) . . . ? C16 C17 H19 105.6 . . . no C16 C17 H20 109.5 . . . no C16 C17 H21 108.5 . . . no H19 C17 H20 106.9 . . . no H19 C17 H21 115.1 . . . no H20 C17 H21 111.0 . . . no N4 C18 C19 112(2) . . . ? N4 C18 H22 109.4 . . . no N4 C18 H23 108.0 . . . no C19 C18 H22 110.2 . . . no C19 C18 H23 110.4 . . . no H22 C18 H23 106.2 . . . no N5 C19 C18 110(2) . . . ? N5 C19 C20 129(2) . . . ? C18 C19 C20 122(2) . . . ? C19 C20 C21 120(2) . . . ? C19 C20 H24 123.1 . . . no C21 C20 H24 117.1 . . . no C20 C21 C22 121(2) . . . ? C20 C21 H25 132.8 . . . no C22 C21 H25 105.8 . . . no C21 C22 C23 116(2) . . . ? C21 C22 H26 127.4 . . . no C23 C22 H26 116.6 . . . no N5 C23 C22 119(2) . . . ? N5 C23 C24 117(2) . . . ? C22 C23 C24 124(2) . . . ? C23 C24 H27 111.5 . . . no C23 C24 H28 108.8 . . . no C23 C24 H29 107.2 . . . no H27 C24 H28 112.1 . . . no H27 C24 H29 111.0 . . . no H28 C24 H29 105.9 . . . no N4 C25 C26 106(1) . . . ? N4 C25 H30 119.2 . . . no N4 C25 H31 113.3 . . . no C26 C25 H30 108.9 . . . no C26 C25 H31 104.2 . . . no H30 C25 H31 103.9 . . . no N6 C26 C25 118(2) . . . ? N6 C26 C27 120(2) . . . ? C25 C26 C27 122(2) . . . ? C26 C27 C28 121(2) . . . ? C26 C27 H32 118.7 . . . no C28 C27 H32 119.8 . . . no C27 C28 C29 116(2) . . . ? C27 C28 H33 120.5 . . . no C29 C28 H33 124.0 . . . no C28 C29 C30 123(2) . . . ? C28 C29 H34 115.8 . . . no C30 C29 H34 120.8 . . . no N6 C30 C29 117(2) . . . ? N6 C30 C31 122(2) . . . ? C29 C30 C31 122(2) . . . ? C30 C31 H35 107.0 . . . no C30 C31 H36 106.3 . . . no C30 C31 H37 108.0 . . . no H35 C31 H36 109.5 . . . no H35 C31 H37 112.1 . . . no H36 C31 H37 113.6 . . . no O4 C32 C33 123(2) . . . ? O4 C32 C37 120(2) . . . ? C33 C32 C37 117(2) . . . ? C32 C33 C34 120(2) . . . ? C32 C33 H38 119.8 . . . no C34 C33 H38 119.4 . . . no C33 C34 C35 119(2) . . . ? C33 C34 H39 120.0 . . . no C35 C34 H39 121.2 . . . no N7 C35 C34 122(2) . . . ? N7 C35 C36 115(2) . . . ? C34 C35 C36 123(2) . . . ? C35 C36 C37 118(2) . . . ? C35 C36 H40 121.1 . . . no C37 C36 H40 120.9 . . . no C32 C37 C36 124(2) . . . ? C32 C37 H41 117.8 . . . no C36 C37 H41 118.5 . . . no O5 C38 C39 117(2) . . . ? O5 C38 C43 121(2) . . . ? C39 C38 C43 122(2) . . . ? C38 C39 C40 116(2) . . . ? C38 C39 H42 121.6 . . . no C40 C39 H42 122.3 . . . no C39 C40 C41 121(2) . . . ? C39 C40 H43 111.1 . . . no C41 C40 H43 127.9 . . . no N8 C41 C40 116(2) . . . ? N8 C41 C42 125(2) . . . ? C40 C41 C42 120(2) . . . ? C41 C42 C43 124(2) . . . ? C41 C42 H44 119.0 . . . no C43 C42 H44 116.9 . . . no C38 C43 C42 118(2) . . . ? C38 C43 H45 116.3 . . . no C42 C43 H45 126.2 . . . no O20 C45 C44 138.260(6) . . . ? O20 C47 C46 132.838(6) . . . ? N9 C49 C48 175(9) . . . ? #------------------------------------------------------------------------------ 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 O4 C46 3.60(1) . 3_655 no O5 C47 3.52(1) . 3_655 no O5 O20 3.56(1) . 3_655 no O5 C46 3.58(1) . 3_655 no O6 C15 3.22(3) . 4_565 no O6 C18 3.24(2) . 4_564 no O6 C19 3.35(2) . 4_564 no O6 C14 3.57(3) . 4_565 no O6 C16 3.57(2) . 4_565 no O6 C30 3.59(2) . 4_564 no O7 C4 3.33(2) . 4_565 no O7 C16 3.38(3) . 4_565 no O7 C5 3.38(2) . 4_565 no O7 N3 3.41(2) . 4_565 no O8 C9 3.19(2) . 8_455 no O8 N2 3.31(2) . 8_455 no O8 C8 3.52(3) . 8_455 no O9 N9 3.12(2) . 3_556 no O9 C49 3.52(5) . 3_556 no O10 C43 3.31(2) . 5_566 no O10 C31 3.46(2) . 5_566 no O10 C37 3.47(2) . 5_566 no O10 C8 3.49(2) . 8_455 no O11 C29 3.28(2) . . no O11 C15 3.42(3) . 1_556 no O11 C8 3.54(2) . 8_455 no O12 C10 3.35(3) . 4_565 no O12 C42 3.43(3) . 5_566 no O12 C8 3.55(3) . 4_565 no O13 C17 3.42(2) . 1_556 no O13 C46 3.48(2) . 3_656 no O13 C24 3.48(2) . 4_565 no O13 C22 3.49(3) . 4_565 no O13 C47 3.53(2) . 3_656 no O13 C42 3.55(2) . 5_566 no O14 C39 3.19(2) . . no O14 C44 3.47(2) . 3_655 no O14 C11 3.52(2) . . no O15 C1 3.23(2) . . no O15 C1 3.23(2) . 7_565 no O15 C3 3.45(2) . . no O15 C3 3.45(2) . 7_565 no O15 C25 3.46(2) . . no O15 C25 3.46(2) . 7_565 no O17 N9 3.46(7) . 2 no O18 C13 3.48(3) . 4_565 no O18 C13 3.48(3) . 6_545 no O19 C49 3.35(7) . 2 no O19 C6 3.46(3) . 3_645 no O20 C21 3.36(2) . 6_644 no O21 O22 1.90(7) . . no O21 C44 2.54(5) . . no O23 O24 3.2(1) . 2 no O24 C4 3.57(3) . 4_565 no O24 C4 3.57(3) . 6_545 no N7 C16 3.44(3) . 4_565 no N7 C20 3.58(3) . 4_564 no N7 C15 3.60(3) . 4_565 no C2 C48 3.17(4) . 4_564 no C4 C48 3.42(3) . 4_564 no C7 C28 3.60(3) . 8 no C21 C41 3.48(3) . 8 no C21 C42 3.50(3) . 8 no C22 C42 3.32(3) . 8 no C23 C34 3.57(3) . 4_565 no C46 C46 2.7992(3) . 5_755 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 #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================