# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Masahiko Maekawa' _publ_contact_author_address ; Research Institute for Science and Technology Kinki University 3-4-1, Kowakae Higashi-Osaka Osaka 577-8502 JAPAN ; _publ_contact_author_email MAEKAWA@RIST.KINDAI.AC.JP _publ_section_title ; Bowl-shaped Cu(I) metallamacrocyclic ethylene and carbonyl adducts as structural analogues of organic calixarenes ; loop_ _publ_author_name 'Masahiko Maekawa' 'Susumu Kitagawa' 'Hisashi Konaka' 'T. Kuroda-Sowa' 'Toshie Minematsu' ; M.Munakata ; #------------------------------------------------------------------------------ data_[Cu(pprd)(ethylene)](PF6)_Complex1-CCDC-659368 _database_code_depnum_ccdc_archive 'CCDC 659368' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C11 H11 Cu F6 N3 P ' _chemical_formula_moiety 'C11 H11 Cu N3, F6 P ' _chemical_formula_weight 393.74 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_Int_Tables_number 14 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 _cell_length_a 8.520(1) _cell_length_b 17.573(2) _cell_length_c 9.483(2) _cell_angle_alpha 90 _cell_angle_beta 102.185(9) _cell_angle_gamma 90 _cell_volume 1387.9(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 640 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 31.0 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784.00 _exptl_absorpt_coefficient_mu 1.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.711 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 27.91 _diffrn_reflns_number 13019 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.89 _diffrn_reflns_theta_full 30.89 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3913 _reflns_number_gt 3022 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1958 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3913 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0840P)^2^+3.0687P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.33 _refine_diff_density_min -0.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.26963(6) 0.64197(3) 0.22629(6) 0.0274(2) Uani 1.00 1 d . . . P(1) P -0.1295(2) 0.84886(7) 0.1428(1) 0.0321(3) Uani 1.00 1 d . . . F(1) F -0.3104(5) 0.8687(3) 0.0783(7) 0.102(2) Uani 1.00 1 d . . . F(2) F -0.1914(5) 0.7731(2) 0.2054(4) 0.065(1) Uani 1.00 1 d . . . F(3) F -0.1172(6) 0.8028(3) 0.0033(5) 0.083(2) Uani 1.00 1 d . . . F(4) F -0.0680(7) 0.9238(2) 0.0840(4) 0.085(2) Uani 1.00 1 d . . . F(5) F 0.0503(5) 0.8275(3) 0.2143(7) 0.098(2) Uani 1.00 1 d . . . F(6) F -0.1393(6) 0.8930(3) 0.2869(4) 0.082(2) Uani 1.00 1 d . . . N(1) N 0.3538(4) 0.6850(2) 0.0460(4) 0.0244(7) Uani 1.00 1 d . . . N(2) N 0.4626(4) 0.5689(2) 0.2190(4) 0.0254(7) Uani 1.00 1 d . . . N(3) N 0.3710(4) 0.7783(2) -0.1315(4) 0.0255(7) Uani 1.00 1 d . . . C(1) C 0.2976(5) 0.7441(2) -0.0366(5) 0.0262(8) Uani 1.00 1 d . . . C(2) C 0.5161(5) 0.7499(3) -0.1397(5) 0.0272(9) Uani 1.00 1 d . . . C(3) C 0.5823(5) 0.6873(3) -0.0614(5) 0.0268(8) Uani 1.00 1 d . . . C(4) C 0.6804(5) 0.5429(3) 0.1023(5) 0.0293(9) Uani 1.00 1 d . . . C(5) C 0.7249(6) 0.4795(3) 0.1898(6) 0.034(1) Uani 1.00 1 d . . . C(6) C 0.6343(6) 0.4612(3) 0.2916(5) 0.035(1) Uani 1.00 1 d . . . C(7) C 0.5027(6) 0.5065(3) 0.3018(5) 0.0312(9) Uani 1.00 1 d . . . C(8) C 0.4963(5) 0.6540(2) 0.0326(5) 0.0232(8) Uani 1.00 1 d . . . C(9) C 0.5500(5) 0.5866(2) 0.1204(5) 0.0253(8) Uani 1.00 1 d . . . C(10) C 0.0502(6) 0.6138(3) 0.2626(7) 0.046(1) Uani 1.00 1 d . . . C(11) C 0.0667(6) 0.5827(4) 0.1404(6) 0.048(1) Uani 1.00 1 d . . . H(1) H 0.4391 0.4928 0.3690 0.0380 Uiso 1.00 1 calc . . . H(2) H 0.6835 0.6676 -0.0710 0.0325 Uiso 1.00 1 calc . . . H(3) H 0.7384 0.5561 0.0306 0.0353 Uiso 1.00 1 calc . . . H(4) H 0.8147 0.4494 0.1803 0.0415 Uiso 1.00 1 calc . . . H(5) H 0.5749 0.7740 -0.2019 0.0332 Uiso 1.00 1 calc . . . H(6) H 0.1963 0.7638 -0.0275 0.0319 Uiso 1.00 1 calc . . . H(7) H 0.6624 0.4186 0.3535 0.0431 Uiso 1.00 1 calc . . . H(8) H 0.0008 0.6010 0.0536 0.0575 Uiso 1.00 1 calc . . . H(9) H 0.0738 0.5288 0.1363 0.0575 Uiso 1.00 1 calc . . . H(10) H 0.0460 0.5810 0.3414 0.0557 Uiso 1.00 1 calc . . . H(11) H -0.0270 0.6532 0.2586 0.0557 Uiso 1.00 1 calc . . . 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) 0.0225(3) 0.0357(3) 0.0251(3) -0.0047(2) 0.0077(2) -0.0052(2) P(1) 0.0306(6) 0.0386(7) 0.0283(6) -0.0064(5) 0.0087(5) -0.0036(5) F(1) 0.055(3) 0.072(3) 0.153(5) 0.019(2) -0.041(3) -0.046(3) F(2) 0.077(3) 0.063(2) 0.057(2) -0.031(2) 0.014(2) 0.009(2) F(3) 0.119(4) 0.077(3) 0.072(3) -0.050(3) 0.063(3) -0.041(2) F(4) 0.146(5) 0.054(2) 0.056(2) -0.045(3) 0.023(3) 0.001(2) F(5) 0.038(2) 0.069(3) 0.172(5) -0.004(2) -0.012(3) -0.016(3) F(6) 0.093(3) 0.108(4) 0.054(2) -0.055(3) 0.037(2) -0.044(2) N(1) 0.020(2) 0.030(2) 0.024(2) 0.001(1) 0.005(1) 0.000(1) N(2) 0.026(2) 0.025(2) 0.025(2) -0.001(1) 0.006(1) 0.000(1) N(3) 0.023(2) 0.030(2) 0.024(2) 0.003(1) 0.006(1) 0.005(1) C(1) 0.021(2) 0.029(2) 0.028(2) 0.001(2) 0.004(2) -0.003(2) C(2) 0.022(2) 0.037(2) 0.024(2) 0.000(2) 0.009(2) 0.004(2) C(3) 0.022(2) 0.033(2) 0.027(2) 0.003(2) 0.007(2) 0.002(2) C(4) 0.024(2) 0.028(2) 0.035(2) 0.001(2) 0.006(2) 0.000(2) C(5) 0.027(2) 0.029(2) 0.043(3) 0.007(2) -0.002(2) -0.002(2) C(6) 0.034(2) 0.032(2) 0.036(3) 0.000(2) -0.002(2) 0.005(2) C(7) 0.035(2) 0.034(2) 0.024(2) -0.004(2) 0.003(2) 0.005(2) C(8) 0.018(2) 0.027(2) 0.023(2) -0.003(1) 0.001(1) -0.003(1) C(9) 0.020(2) 0.027(2) 0.029(2) -0.002(1) 0.005(2) -0.004(2) C(10) 0.030(2) 0.055(3) 0.059(4) -0.017(2) 0.020(2) -0.018(3) C(11) 0.028(2) 0.068(4) 0.047(3) -0.026(2) 0.007(2) -0.019(3) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cu(1) N(1) 2.128(4) . . yes Cu(1) N(2) 2.099(4) . . yes Cu(1) N(3) 2.009(3) . 4_565 yes Cu(1) C(10) 2.033(6) . . yes Cu(1) C(11) 2.036(5) . . yes P(1) F(1) 1.572(5) . . yes P(1) F(2) 1.593(4) . . yes P(1) F(3) 1.573(5) . . yes P(1) F(4) 1.563(5) . . yes P(1) F(5) 1.584(4) . . yes P(1) F(6) 1.589(5) . . yes N(1) C(1) 1.328(5) . . yes N(1) C(8) 1.360(6) . . yes N(2) C(7) 1.350(6) . . yes N(2) C(9) 1.349(6) . . yes N(3) C(1) 1.342(6) . . yes N(3) C(2) 1.350(6) . . yes C(1) H(6) 0.951 . . no C(2) C(3) 1.378(6) . . yes C(2) H(5) 0.951 . . no C(3) C(8) 1.396(7) . . yes C(3) H(2) 0.952 . . no C(4) C(5) 1.393(7) . . yes C(4) C(9) 1.390(6) . . yes C(4) H(3) 0.949 . . no C(5) C(6) 1.395(8) . . yes C(5) H(4) 0.950 . . no C(6) C(7) 1.395(7) . . yes C(6) H(7) 0.949 . . no C(7) H(1) 0.950 . . no C(8) C(9) 1.465(6) . . yes C(10) C(11) 1.314(9) . . yes C(10) H(10) 0.950 . . no C(10) H(11) 0.950 . . no C(11) H(8) 0.950 . . no C(11) H(9) 0.950 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(2) 78.0(1) . . . yes N(1) Cu(1) N(3) 97.0(1) . . 4_565 yes N(1) Cu(1) C(10) 134.5(2) . . . yes N(1) Cu(1) C(11) 105.2(2) . . . yes N(2) Cu(1) N(3) 102.7(1) . . 4_565 yes N(2) Cu(1) C(10) 127.7(2) . . . yes N(2) Cu(1) C(11) 106.2(2) . . . yes N(3) Cu(1) C(10) 109.7(2) 4_565 . . yes N(3) Cu(1) C(11) 146.5(2) 4_565 . . yes C(10) Cu(1) C(11) 37.7(2) . . . yes F(1) P(1) F(2) 87.5(2) . . . yes F(1) P(1) F(3) 91.2(3) . . . yes F(1) P(1) F(4) 92.9(3) . . . yes F(1) P(1) F(5) 177.4(3) . . . yes F(1) P(1) F(6) 90.1(3) . . . yes F(2) P(1) F(3) 88.2(2) . . . yes F(2) P(1) F(4) 179.0(2) . . . yes F(2) P(1) F(5) 90.5(2) . . . yes F(2) P(1) F(6) 90.4(2) . . . yes F(3) P(1) F(4) 92.7(2) . . . yes F(3) P(1) F(5) 90.5(3) . . . yes F(3) P(1) F(6) 178.1(2) . . . yes F(4) P(1) F(5) 89.1(3) . . . yes F(4) P(1) F(6) 88.7(3) . . . yes F(5) P(1) F(6) 88.2(3) . . . yes Cu(1) N(1) C(1) 127.7(3) . . . yes Cu(1) N(1) C(8) 113.1(3) . . . yes C(1) N(1) C(8) 118.4(4) . . . yes Cu(1) N(2) C(7) 125.6(3) . . . yes Cu(1) N(2) C(9) 115.6(3) . . . yes C(7) N(2) C(9) 118.8(4) . . . yes Cu(1) N(3) C(1) 124.6(3) 4_564 . . yes Cu(1) N(3) C(2) 119.3(3) 4_564 . . yes C(1) N(3) C(2) 115.7(4) . . . yes N(1) C(1) N(3) 125.8(4) . . . yes N(1) C(1) H(6) 117.0 . . . no N(3) C(1) H(6) 117.2 . . . no N(3) C(2) C(3) 122.7(4) . . . yes N(3) C(2) H(5) 118.6 . . . no C(3) C(2) H(5) 118.7 . . . no C(2) C(3) C(8) 117.9(4) . . . yes C(2) C(3) H(2) 121.0 . . . no C(8) C(3) H(2) 121.1 . . . no C(5) C(4) C(9) 119.4(5) . . . yes C(5) C(4) H(3) 120.3 . . . no C(9) C(4) H(3) 120.2 . . . no C(4) C(5) C(6) 118.5(4) . . . yes C(4) C(5) H(4) 120.8 . . . no C(6) C(5) H(4) 120.8 . . . no C(5) C(6) C(7) 119.1(4) . . . yes C(5) C(6) H(7) 120.4 . . . no C(7) C(6) H(7) 120.5 . . . no N(2) C(7) C(6) 122.1(5) . . . yes N(2) C(7) H(1) 119.0 . . . no C(6) C(7) H(1) 118.9 . . . no N(1) C(8) C(3) 119.4(4) . . . yes N(1) C(8) C(9) 116.7(4) . . . yes C(3) C(8) C(9) 124.0(4) . . . yes N(2) C(9) C(4) 122.1(4) . . . yes N(2) C(9) C(8) 115.4(4) . . . yes C(4) C(9) C(8) 122.6(4) . . . yes Cu(1) C(10) C(11) 71.3(4) . . . yes Cu(1) C(10) H(10) 118.0 . . . no Cu(1) C(10) H(11) 118.0 . . . no C(11) C(10) H(10) 118.0 . . . no C(11) C(10) H(11) 118.0 . . . no H(10) C(10) H(11) 109.4 . . . no Cu(1) C(11) C(10) 71.0(3) . . . yes Cu(1) C(11) H(8) 118.1 . . . no Cu(1) C(11) H(9) 118.1 . . . no C(10) C(11) H(8) 118.0 . . . no C(10) C(11) H(9) 118.0 . . . no H(8) C(11) H(9) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(2) 3.086(7) . 1_455 ? F(1) C(7) 3.260(7) . 2_555 ? F(1) N(3) 3.401(6) . 1_455 ? F(1) C(3) 3.497(7) . 1_455 ? F(1) C(7) 3.530(7) . 4_464 ? F(2) C(2) 3.175(7) . 4_465 ? F(2) C(3) 3.214(6) . 1_455 ? F(2) C(3) 3.301(7) . 4_465 ? F(2) C(8) 3.508(5) . 1_455 ? F(3) C(3) 3.222(6) . 1_455 ? F(3) C(2) 3.267(6) . 1_455 ? F(3) C(10) 3.282(8) . 4_564 ? F(4) C(5) 3.385(6) . 2_655 ? F(4) F(4) 3.441(9) . 3_575 ? F(4) C(10) 3.470(8) . 4_564 ? F(5) C(5) 3.301(6) . 2_655 ? F(5) C(6) 3.578(7) . 2_655 ? F(6) C(3) 3.336(7) . 4_465 ? F(6) C(11) 3.433(8) . 2_555 ? N(3) C(10) 3.304(6) . 4_564 ? C(1) C(10) 3.552(7) . 4_564 ? C(2) C(8) 3.510(6) . 4_564 ? C(4) C(11) 3.309(7) . 1_655 ? C(4) C(9) 3.426(6) . 3_665 ? C(4) C(10) 3.430(7) . 1_655 ? C(5) C(8) 3.439(6) . 3_665 ? C(5) C(11) 3.544(8) . 1_655 ? C(5) C(9) 3.547(6) . 3_665 ? C(5) C(10) 3.593(7) . 1_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ ### END #------------------------------------------------------------------------------ data_[Cu4(pprd)4(C2H4)4](PF6)4_Complex2-CCDC-659369 _database_code_depnum_ccdc_archive 'CCDC 659369' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C44 H44 Cu4 F24 N12 P4 ' _chemical_formula_moiety 'C44 H44 Cu4 N12 4+, 4(P F6 -) ' _chemical_formula_weight 1574.95 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'i b a 2 ' _symmetry_space_group_name_Hall 'i 2 -2c ' _symmetry_Int_Tables_number 45 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -x,y,1/2+z x,-y,1/2+z 1/2+x,1/2+y,1/2+z 1/2-x,1/2-y,1/2+z 1/2-x,1/2+y,z 1/2+x,1/2-y,z _cell_length_a 14.6057(9) _cell_length_b 28.370(2) _cell_length_c 14.0685(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5829(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8840 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136.00 _exptl_absorpt_coefficient_mu 1.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.778 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 22491 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5905 _reflns_number_gt 5454 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0964 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5905 _refine_ls_number_parameters 417 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0493P)^2^+7.2415P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0040 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack(1983), 2413 Friedel pairs' _refine_ls_abs_structure_Flack 0.02(1) _chemical_absolute_configuration syn _refine_diff_density_max 0.60 _refine_diff_density_min -0.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.69911(3) 0.38843(1) 0.47894(4) 0.0231(1) Uani 1.00 1 d . . . Cu(2) Cu 0.71696(3) 0.60167(1) 0.47802(4) 0.0239(1) Uani 1.00 1 d . . . P(1) P 0.5000 0.5000 0.2177(2) 0.0350(3) Uani 1.00 2 d S . . P(2) P 1.0000 0.5000 0.5359(1) 0.0350(4) Uani 1.00 2 d S . . P(3) P 0.50626(7) 0.24251(4) 0.54202(9) 0.0246(2) Uani 1.00 1 d . . . F(1) F 0.5000 0.5000 0.3299(5) 0.130(3) Uani 1.00 2 d S . . F(2) F 0.5000 0.5000 0.1078(5) 0.106(3) Uani 1.00 2 d S . . F(3) F 0.5022(3) 0.4444(1) 0.2179(5) 0.088(1) Uani 1.00 1 d . . . F(4) F 0.6074(2) 0.5016(1) 0.2182(5) 0.089(1) Uani 1.00 1 d . . . F(5) F 0.8993(2) 0.4793(1) 0.5367(2) 0.0663(9) Uani 1.00 1 d . . . F(6) F 0.9899(7) 0.5197(4) 0.4305(6) 0.097(5) Uani 0.50 2 d P . . F(7) F 0.9571(6) 0.5443(3) 0.4994(9) 0.080(3) Uani 0.50 2 d P . . F(8) F 0.9726(6) 0.5530(3) 0.573(1) 0.100(4) Uani 0.50 2 d P . . F(9) F 0.9813(7) 0.5128(4) 0.6407(4) 0.076(5) Uani 0.50 2 d P . . F(10) F 0.5249(3) 0.18792(9) 0.5349(3) 0.071(1) Uani 1.00 1 d . . . F(11) F 0.4863(2) 0.29746(9) 0.5503(3) 0.0648(9) Uani 1.00 1 d . . . F(12) F 0.5238(2) 0.2420(1) 0.6535(2) 0.0552(8) Uani 1.00 1 d . . . F(13) F 0.4882(2) 0.2433(1) 0.4301(2) 0.0613(9) Uani 1.00 1 d . . . F(14) F 0.6102(2) 0.2533(1) 0.5228(3) 0.072(1) Uani 1.00 1 d . . . F(15) F 0.4014(2) 0.2325(1) 0.5632(3) 0.0664(10) Uani 1.00 1 d . . . N(1) N 0.4027(2) 0.3813(1) 0.4145(2) 0.0233(6) Uani 1.00 1 d . . . N(2) N 0.5645(2) 0.3762(1) 0.4228(2) 0.0210(6) Uani 1.00 1 d . . . N(3) N 0.7256(2) 0.3381(1) 0.3805(2) 0.0227(6) Uani 1.00 1 d . . . N(4) N 0.7333(2) 0.4496(1) 0.4144(2) 0.0229(6) Uani 1.00 1 d . . . N(5) N 0.7424(2) 0.5329(1) 0.4215(2) 0.0234(6) Uani 1.00 1 d . . . N(6) N 0.8127(2) 0.6169(1) 0.3781(2) 0.0233(7) Uani 1.00 1 d . . . C(1) C 0.4848(2) 0.3929(1) 0.4514(3) 0.0226(8) Uani 1.00 1 d . . . C(2) C 0.5653(2) 0.3459(1) 0.3488(2) 0.0193(6) Uani 1.00 1 d . . . C(3) C 0.4849(2) 0.3348(1) 0.3009(3) 0.0262(7) Uani 1.00 1 d . . . C(4) C 0.4054(3) 0.3533(1) 0.3376(3) 0.0277(8) Uani 1.00 1 d . . . C(5) C 0.6554(2) 0.3243(1) 0.3260(3) 0.0215(7) Uani 1.00 1 d . . . C(6) C 0.6662(3) 0.2914(1) 0.2547(3) 0.0290(8) Uani 1.00 1 d . . . C(7) C 0.7519(3) 0.2719(1) 0.2397(3) 0.0365(10) Uani 1.00 1 d . . . C(8) C 0.8232(3) 0.2853(1) 0.2970(3) 0.0348(9) Uani 1.00 1 d . . . C(9) C 0.8082(3) 0.3185(1) 0.3655(3) 0.0310(9) Uani 1.00 1 d . . . C(10) C 0.7176(3) 0.3545(2) 0.6063(4) 0.040(1) Uani 1.00 1 d . . . C(11) C 0.7124(3) 0.4022(1) 0.6183(3) 0.0279(8) Uani 1.00 1 d . . . C(12) C 0.7097(2) 0.4916(1) 0.4505(3) 0.0246(8) Uani 1.00 1 d . . . C(13) C 0.8031(2) 0.5334(1) 0.3497(3) 0.0212(7) Uani 1.00 1 d . . . C(14) C 0.8264(3) 0.4918(1) 0.3044(3) 0.0282(8) Uani 1.00 1 d . . . C(15) C 0.7908(3) 0.4509(1) 0.3399(3) 0.0296(8) Uani 1.00 1 d . . . C(16) C 0.8438(2) 0.5798(1) 0.3265(3) 0.0235(7) Uani 1.00 1 d . . . C(17) C 0.9095(3) 0.5859(2) 0.2572(3) 0.0331(9) Uani 1.00 1 d . . . C(18) C 0.9444(3) 0.6300(2) 0.2392(3) 0.039(1) Uani 1.00 1 d . . . C(19) C 0.9138(3) 0.6671(1) 0.2931(4) 0.0344(9) Uani 1.00 1 d . . . C(20) C 0.8482(3) 0.6593(1) 0.3606(3) 0.0285(8) Uani 1.00 1 d . . . C(21) C 0.7824(4) 0.6122(2) 0.6061(4) 0.049(1) Uani 1.00 1 d . . . C(22) C 0.6928(3) 0.6087(2) 0.6161(3) 0.036(1) Uani 1.00 1 d . . . H(1) H 0.4854 0.4133 0.4986 0.0270 Uiso 1.00 1 calc . . . H(2) H 0.4850 0.3169 0.2498 0.0315 Uiso 1.00 1 calc . . . H(3) H 0.3534 0.3464 0.3091 0.0332 Uiso 1.00 1 calc . . . H(4) H 0.6194 0.2829 0.2192 0.0348 Uiso 1.00 1 calc . . . H(5) H 0.7605 0.2512 0.1939 0.0438 Uiso 1.00 1 calc . . . H(6) H 0.8778 0.2727 0.2898 0.0417 Uiso 1.00 1 calc . . . H(7) H 0.8545 0.3275 0.4014 0.0371 Uiso 1.00 1 calc . . . H(8) H 0.6675 0.3373 0.6081 0.0481 Uiso 1.00 1 calc . . . H(9) H 0.7710 0.3410 0.5968 0.0481 Uiso 1.00 1 calc . . . H(10) H 0.6590 0.4158 0.6277 0.0335 Uiso 1.00 1 calc . . . H(11) H 0.7625 0.4195 0.6165 0.0335 Uiso 1.00 1 calc . . . H(12) H 0.6693 0.4918 0.4969 0.0294 Uiso 1.00 1 calc . . . H(13) H 0.8629 0.4916 0.2546 0.0339 Uiso 1.00 1 calc . . . H(14) H 0.8062 0.4241 0.3127 0.0355 Uiso 1.00 1 calc . . . H(15) H 0.9291 0.5614 0.2245 0.0397 Uiso 1.00 1 calc . . . H(16) H 0.9853 0.6344 0.1941 0.0467 Uiso 1.00 1 calc . . . H(17) H 0.9362 0.6956 0.2843 0.0412 Uiso 1.00 1 calc . . . H(18) H 0.8285 0.6835 0.3942 0.0342 Uiso 1.00 1 calc . . . H(19) H 0.8169 0.5868 0.6094 0.0586 Uiso 1.00 1 calc . . . H(20) H 0.8078 0.6399 0.5962 0.0586 Uiso 1.00 1 calc . . . H(21) H 0.6675 0.5810 0.6260 0.0434 Uiso 1.00 1 calc . . . H(22) H 0.6583 0.6341 0.6128 0.0434 Uiso 1.00 1 calc . . . 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) 0.0253(2) 0.0221(2) 0.0219(2) 0.0000(1) -0.0021(3) -0.0033(3) Cu(2) 0.0240(2) 0.0261(2) 0.0217(2) 0.0012(1) 0.0021(3) -0.0010(3) P(1) 0.0331(7) 0.0307(7) 0.041(1) -0.0012(8) 0.0000 0.0000 P(2) 0.0213(7) 0.059(1) 0.0254(8) 0.0052(7) 0.0000 0.0000 P(3) 0.0316(5) 0.0213(4) 0.0210(5) -0.0012(4) 0.0019(4) 0.0006(4) F(1) 0.171(8) 0.161(8) 0.056(5) -0.006(6) 0.0000 0.0000 F(2) 0.152(7) 0.129(6) 0.038(3) 0.005(5) 0.0000 0.0000 F(3) 0.056(2) 0.035(1) 0.174(5) -0.003(2) 0.007(2) 0.019(3) F(4) 0.035(1) 0.056(2) 0.176(4) 0.000(2) -0.007(3) 0.010(2) F(5) 0.034(2) 0.114(3) 0.051(2) -0.020(2) -0.006(1) 0.005(2) F(6) 0.068(7) 0.17(1) 0.050(5) -0.046(9) -0.036(6) 0.056(6) F(7) 0.065(5) 0.073(5) 0.104(8) 0.003(4) -0.025(5) 0.043(6) F(8) 0.079(6) 0.064(5) 0.16(1) 0.038(4) -0.036(7) -0.038(6) F(9) 0.058(8) 0.14(1) 0.030(3) -0.053(7) 0.017(3) -0.032(5) F(10) 0.126(3) 0.026(1) 0.060(2) 0.016(2) 0.044(2) 0.002(1) F(11) 0.107(3) 0.025(1) 0.061(2) 0.011(1) 0.020(2) 0.006(1) F(12) 0.067(2) 0.074(2) 0.025(1) 0.021(2) -0.006(1) -0.001(1) F(13) 0.088(2) 0.073(2) 0.023(2) 0.000(2) -0.009(1) 0.003(1) F(14) 0.039(2) 0.097(3) 0.079(2) -0.020(2) 0.021(1) -0.036(2) F(15) 0.039(2) 0.091(2) 0.070(2) -0.023(2) 0.012(2) -0.031(2) N(1) 0.021(1) 0.024(1) 0.025(2) 0.003(1) -0.001(1) 0.002(1) N(2) 0.021(1) 0.018(1) 0.023(2) -0.001(1) -0.001(1) -0.003(1) N(3) 0.021(1) 0.020(1) 0.027(2) 0.004(1) 0.004(1) 0.001(1) N(4) 0.024(1) 0.022(1) 0.023(2) -0.002(1) -0.003(1) -0.003(1) N(5) 0.021(1) 0.021(1) 0.028(2) 0.001(1) -0.002(1) 0.000(1) N(6) 0.025(2) 0.023(1) 0.023(2) -0.005(1) -0.003(1) 0.002(1) C(1) 0.021(2) 0.022(2) 0.024(2) 0.002(1) -0.004(1) -0.004(1) C(2) 0.023(2) 0.015(1) 0.020(2) 0.000(1) -0.001(1) -0.001(1) C(3) 0.026(2) 0.029(2) 0.024(2) 0.000(1) -0.003(2) -0.007(2) C(4) 0.026(2) 0.030(2) 0.027(2) 0.001(1) -0.009(2) -0.002(2) C(5) 0.025(2) 0.017(1) 0.023(2) -0.002(1) 0.001(1) 0.003(1) C(6) 0.029(2) 0.028(2) 0.030(2) -0.002(2) 0.003(2) -0.007(2) C(7) 0.039(2) 0.027(2) 0.043(3) 0.003(2) 0.008(2) -0.014(2) C(8) 0.028(2) 0.036(2) 0.040(2) 0.012(2) 0.001(2) -0.006(2) C(9) 0.022(2) 0.034(2) 0.036(2) 0.004(2) -0.001(2) -0.005(2) C(10) 0.053(3) 0.036(2) 0.032(2) 0.002(2) -0.005(2) 0.005(2) C(11) 0.045(2) 0.024(2) 0.015(2) 0.001(2) -0.013(2) -0.002(1) C(12) 0.021(2) 0.026(2) 0.027(2) 0.001(1) 0.002(1) -0.002(1) C(13) 0.021(2) 0.024(2) 0.018(2) 0.001(1) -0.001(1) -0.001(1) C(14) 0.029(2) 0.033(2) 0.023(2) 0.000(2) 0.008(2) -0.006(2) C(15) 0.035(2) 0.026(2) 0.028(2) -0.004(2) 0.001(2) -0.009(2) C(16) 0.019(2) 0.026(2) 0.026(2) 0.001(1) -0.002(1) 0.001(1) C(17) 0.033(2) 0.037(2) 0.030(2) -0.002(2) 0.007(2) 0.000(2) C(18) 0.029(2) 0.047(3) 0.041(3) -0.004(2) 0.008(2) 0.007(2) C(19) 0.033(2) 0.029(2) 0.041(2) -0.010(2) 0.003(2) 0.007(2) C(20) 0.027(2) 0.025(2) 0.034(2) -0.005(1) -0.004(2) 0.002(2) C(21) 0.044(3) 0.070(4) 0.032(3) -0.003(2) -0.010(2) -0.005(2) C(22) 0.025(2) 0.057(3) 0.026(2) 0.001(2) 0.002(2) -0.023(2) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cu(1) N(2) 2.146(3) . . yes Cu(1) N(3) 2.025(3) . . yes Cu(1) N(4) 2.022(3) . . yes Cu(1) C(10) 2.051(5) . . yes Cu(1) C(11) 2.008(4) . . yes Cu(2) N(1) 2.021(3) . 2_665 yes Cu(2) N(5) 2.138(3) . . yes Cu(2) N(6) 2.029(3) . . yes Cu(2) C(21) 2.062(6) . . yes Cu(2) C(22) 1.984(5) . . yes P(1) F(1) 1.579(8) . . yes P(1) F(2) 1.546(7) . . yes P(1) F(3) 1.577(3) . . yes P(1) F(3) 1.577(3) . 2_665 yes P(1) F(4) 1.569(3) . . yes P(1) F(4) 1.569(3) . 2_665 yes P(2) F(5) 1.584(3) . . yes P(2) F(5) 1.584(3) . 2_765 yes P(2) F(6) 1.590(9) . . yes P(2) F(6) 1.590(9) . 2_765 yes P(2) F(7) 1.494(9) . . yes P(2) F(7) 1.494(9) . 2_765 yes P(2) F(8) 1.639(9) . . yes P(2) F(8) 1.639(9) . 2_765 yes P(2) F(9) 1.544(7) . . yes P(2) F(9) 1.544(7) . 2_765 yes P(3) F(10) 1.576(3) . . yes P(3) F(11) 1.590(3) . . yes P(3) F(12) 1.589(3) . . yes P(3) F(13) 1.597(4) . . yes P(3) F(14) 1.571(3) . . yes P(3) F(15) 1.586(3) . . yes N(1) C(1) 1.348(4) . . yes N(1) C(4) 1.344(5) . . yes N(2) C(1) 1.319(4) . . yes N(2) C(2) 1.350(4) . . yes N(3) C(5) 1.340(5) . . yes N(3) C(9) 1.345(5) . . yes N(4) C(12) 1.340(4) . . yes N(4) C(15) 1.342(5) . . yes N(5) C(12) 1.330(4) . . yes N(5) C(13) 1.344(5) . . yes N(6) C(16) 1.357(5) . . yes N(6) C(20) 1.333(5) . . yes C(2) C(3) 1.391(5) . . yes C(2) C(5) 1.486(5) . . yes C(3) C(4) 1.375(5) . . yes C(5) C(6) 1.380(5) . . yes C(6) C(7) 1.383(6) . . yes C(7) C(8) 1.372(6) . . yes C(8) C(9) 1.366(6) . . yes C(10) C(11) 1.366(6) . . yes C(13) C(14) 1.385(5) . . yes C(13) C(16) 1.481(5) . . yes C(14) C(15) 1.365(5) . . yes C(16) C(17) 1.378(6) . . yes C(17) C(18) 1.376(6) . . yes C(18) C(19) 1.371(6) . . yes C(19) C(20) 1.367(6) . . yes C(21) C(22) 1.320(7) . . yes C(1) H(1) 0.881 . . no C(3) H(2) 0.881 . . no C(4) H(3) 0.881 . . no C(6) H(4) 0.880 . . no C(7) H(5) 0.881 . . no C(8) H(6) 0.881 . . no C(9) H(7) 0.881 . . no C(10) H(8) 0.880 . . no C(10) H(9) 0.881 . . no C(11) H(10) 0.880 . . no C(11) H(11) 0.880 . . no C(12) H(12) 0.881 . . no C(14) H(13) 0.881 . . no C(15) H(14) 0.880 . . no C(17) H(15) 0.881 . . no C(18) H(16) 0.881 . . no C(19) H(17) 0.881 . . no C(20) H(18) 0.881 . . no C(21) H(19) 0.881 . . no C(21) H(20) 0.880 . . no C(22) H(21) 0.881 . . no C(22) H(22) 0.880 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(2) Cu(1) N(3) 79.0(1) . . . yes N(2) Cu(1) N(4) 101.5(1) . . . yes N(2) Cu(1) C(10) 111.5(2) . . . yes N(2) Cu(1) C(11) 118.6(1) . . . yes N(3) Cu(1) N(4) 104.5(1) . . . yes N(3) Cu(1) C(10) 104.0(2) . . . yes N(3) Cu(1) C(11) 141.8(1) . . . yes N(4) Cu(1) C(10) 139.7(2) . . . yes N(4) Cu(1) C(11) 104.3(1) . . . yes C(10) Cu(1) C(11) 39.3(2) . . . yes N(1) Cu(2) N(5) 101.8(1) 2_665 . . yes N(1) Cu(2) N(6) 103.8(1) 2_665 . . yes N(1) Cu(2) C(21) 138.8(2) 2_665 . . yes N(1) Cu(2) C(22) 104.8(2) 2_665 . . yes N(5) Cu(2) N(6) 79.5(1) . . . yes N(5) Cu(2) C(21) 112.1(2) . . . yes N(5) Cu(2) C(22) 119.1(2) . . . yes N(6) Cu(2) C(21) 104.8(2) . . . yes N(6) Cu(2) C(22) 141.2(2) . . . yes C(21) Cu(2) C(22) 38.0(2) . . . yes F(1) P(1) F(2) 180.0000(1) . . . yes F(1) P(1) F(3) 89.9(3) . . . yes F(1) P(1) F(3) 89.9(3) . . 2_665 yes F(1) P(1) F(4) 89.8(3) . . . yes F(1) P(1) F(4) 89.8(3) . . 2_665 yes F(2) P(1) F(3) 90.1(3) . . . yes F(2) P(1) F(3) 90.1(3) . . 2_665 yes F(2) P(1) F(4) 90.2(3) . . . yes F(2) P(1) F(4) 90.2(3) . . 2_665 yes F(3) P(1) F(3) 179.8(5) . . 2_665 yes F(3) P(1) F(4) 90.5(2) . . . yes F(3) P(1) F(4) 89.5(2) . . 2_665 yes F(3) P(1) F(4) 89.5(2) 2_665 . . yes F(3) P(1) F(4) 90.5(2) 2_665 . 2_665 yes F(4) P(1) F(4) 179.5(5) . . 2_665 yes F(5) P(2) F(5) 179.2(3) . . 2_765 yes F(5) P(2) F(6) 92.9(4) . . . yes F(5) P(2) F(6) 87.9(4) . . 2_765 yes F(5) P(2) F(7) 85.7(3) . . . yes F(5) P(2) F(7) 94.6(3) . . 2_765 yes F(5) P(2) F(8) 96.4(3) . . . yes F(5) P(2) F(8) 83.3(3) . . 2_765 yes F(5) P(2) F(9) 85.2(4) . . . yes F(5) P(2) F(9) 94.0(4) . . 2_765 yes F(5) P(2) F(6) 87.9(4) 2_765 . . yes F(5) P(2) F(6) 92.9(4) 2_765 . 2_765 yes F(5) P(2) F(7) 94.6(3) 2_765 . . yes F(5) P(2) F(7) 85.7(3) 2_765 . 2_765 yes F(5) P(2) F(8) 83.3(3) 2_765 . . yes F(5) P(2) F(8) 96.4(3) 2_765 . 2_765 yes F(5) P(2) F(9) 94.0(4) 2_765 . . yes F(5) P(2) F(9) 85.2(4) 2_765 . 2_765 yes F(6) P(2) F(7) 90.8(6) . . 2_765 yes F(6) P(2) F(8) 87.2(6) . . . yes F(6) P(2) F(9) 171.7(6) . . 2_765 yes F(6) P(2) F(7) 90.8(6) 2_765 . . yes F(6) P(2) F(8) 87.2(6) 2_765 . 2_765 yes F(6) P(2) F(9) 171.7(6) 2_765 . . yes F(7) P(2) F(8) 168.9(4) . . 2_765 yes F(7) P(2) F(9) 93.2(6) . . . yes F(7) P(2) F(8) 168.9(4) 2_765 . . yes F(7) P(2) F(9) 93.2(6) 2_765 . 2_765 yes F(8) P(2) F(9) 87.5(7) . . 2_765 yes F(8) P(2) F(9) 87.5(7) 2_765 . . yes F(10) P(3) F(11) 179.2(2) . . . yes F(10) P(3) F(12) 91.5(2) . . . yes F(10) P(3) F(13) 88.9(2) . . . yes F(10) P(3) F(14) 90.8(2) . . . yes F(10) P(3) F(15) 90.2(2) . . . yes F(11) P(3) F(12) 88.1(2) . . . yes F(11) P(3) F(13) 91.6(2) . . . yes F(11) P(3) F(14) 89.9(2) . . . yes F(11) P(3) F(15) 89.1(2) . . . yes F(12) P(3) F(13) 179.6(2) . . . yes F(12) P(3) F(14) 90.9(2) . . . yes F(12) P(3) F(15) 88.2(2) . . . yes F(13) P(3) F(14) 89.2(2) . . . yes F(13) P(3) F(15) 91.7(2) . . . yes F(14) P(3) F(15) 178.7(2) . . . yes Cu(2) N(1) C(1) 122.8(3) 2_665 . . yes Cu(2) N(1) C(4) 121.5(2) 2_665 . . yes C(1) N(1) C(4) 115.3(3) . . . yes Cu(1) N(2) C(1) 129.7(2) . . . yes Cu(1) N(2) C(2) 112.2(2) . . . yes C(1) N(2) C(2) 118.1(3) . . . yes Cu(1) N(3) C(5) 116.9(2) . . . yes Cu(1) N(3) C(9) 124.8(3) . . . yes C(5) N(3) C(9) 118.4(3) . . . yes Cu(1) N(4) C(12) 122.0(3) . . . yes Cu(1) N(4) C(15) 122.0(2) . . . yes C(12) N(4) C(15) 115.6(3) . . . yes Cu(2) N(5) C(12) 128.9(3) . . . yes Cu(2) N(5) C(13) 112.6(2) . . . yes C(12) N(5) C(13) 118.4(3) . . . yes Cu(2) N(6) C(16) 115.8(2) . . . yes Cu(2) N(6) C(20) 126.1(3) . . . yes C(16) N(6) C(20) 118.1(3) . . . yes N(1) C(1) N(2) 125.6(3) . . . yes N(2) C(2) C(3) 120.7(3) . . . yes N(2) C(2) C(5) 115.9(3) . . . yes C(3) C(2) C(5) 123.3(3) . . . yes C(2) C(3) C(4) 116.4(4) . . . yes N(1) C(4) C(3) 123.5(3) . . . yes N(3) C(5) C(2) 115.6(3) . . . yes N(3) C(5) C(6) 121.8(3) . . . yes C(2) C(5) C(6) 122.6(3) . . . yes C(5) C(6) C(7) 119.0(4) . . . yes C(6) C(7) C(8) 119.1(4) . . . yes C(7) C(8) C(9) 119.0(4) . . . yes N(3) C(9) C(8) 122.7(4) . . . yes Cu(1) C(10) C(11) 68.6(3) . . . yes Cu(1) C(11) C(10) 72.0(3) . . . yes N(4) C(12) N(5) 125.2(3) . . . yes N(5) C(13) C(14) 120.0(3) . . . yes N(5) C(13) C(16) 116.0(3) . . . yes C(14) C(13) C(16) 123.9(3) . . . yes C(13) C(14) C(15) 117.5(4) . . . yes N(4) C(15) C(14) 123.2(4) . . . yes N(6) C(16) C(13) 115.9(3) . . . yes N(6) C(16) C(17) 121.0(3) . . . yes C(13) C(16) C(17) 123.1(3) . . . yes C(16) C(17) C(18) 120.1(4) . . . yes C(17) C(18) C(19) 118.4(4) . . . yes C(18) C(19) C(20) 119.2(4) . . . yes N(6) C(20) C(19) 123.1(4) . . . yes Cu(2) C(21) C(22) 67.8(3) . . . yes Cu(2) C(22) C(21) 74.2(3) . . . yes N(1) C(1) H(1) 117.2 . . . no N(2) C(1) H(1) 117.2 . . . no C(2) C(3) H(2) 121.8 . . . no C(4) C(3) H(2) 121.8 . . . no N(1) C(4) H(3) 118.2 . . . no C(3) C(4) H(3) 118.2 . . . no C(5) C(6) H(4) 120.5 . . . no C(7) C(6) H(4) 120.5 . . . no C(6) C(7) H(5) 120.4 . . . no C(8) C(7) H(5) 120.5 . . . no C(7) C(8) H(6) 120.5 . . . no C(9) C(8) H(6) 120.5 . . . no N(3) C(9) H(7) 118.6 . . . no C(8) C(9) H(7) 118.7 . . . no Cu(1) C(10) H(8) 100.1 . . . no Cu(1) C(10) H(9) 100.9 . . . no C(11) C(10) H(8) 120.1 . . . no C(11) C(10) H(9) 120.0 . . . no H(8) C(10) H(9) 119.9 . . . no Cu(1) C(11) H(10) 98.5 . . . no Cu(1) C(11) H(11) 99.3 . . . no C(10) C(11) H(10) 120.0 . . . no C(10) C(11) H(11) 120.0 . . . no H(10) C(11) H(11) 120.0 . . . no N(4) C(12) H(12) 117.4 . . . no N(5) C(12) H(12) 117.4 . . . no C(13) C(14) H(13) 121.2 . . . no C(15) C(14) H(13) 121.3 . . . no N(4) C(15) H(14) 118.4 . . . no C(14) C(15) H(14) 118.4 . . . no C(16) C(17) H(15) 120.0 . . . no C(18) C(17) H(15) 120.0 . . . no C(17) C(18) H(16) 120.8 . . . no C(19) C(18) H(16) 120.8 . . . no C(18) C(19) H(17) 120.4 . . . no C(20) C(19) H(17) 120.4 . . . no N(6) C(20) H(18) 118.4 . . . no C(19) C(20) H(18) 118.4 . . . no Cu(2) C(21) H(19) 101.1 . . . no Cu(2) C(21) H(20) 100.8 . . . no C(22) C(21) H(19) 120.0 . . . no C(22) C(21) H(20) 120.1 . . . no H(19) C(21) H(20) 119.9 . . . no Cu(2) C(22) H(21) 98.0 . . . no Cu(2) C(22) H(22) 97.7 . . . no C(21) C(22) H(21) 120.0 . . . no C(21) C(22) H(22) 120.0 . . . no H(21) C(22) H(22) 119.9 . . . 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 F(3) C(22) 3.474(6) . 4_564 ? F(4) C(11) 3.431(6) . 4_564 ? F(8) C(17) 3.25(1) . 3_755 ? F(8) C(18) 3.42(1) . 3_755 ? F(9) C(17) 3.09(1) . 3_755 ? F(9) C(14) 3.231(9) . 4_565 ? F(9) C(17) 3.41(1) . 4_565 ? F(10) C(20) 3.179(5) . 7_645 ? F(10) C(18) 3.513(6) . 5_445 ? F(10) C(19) 3.567(6) . 7_645 ? F(12) C(8) 3.109(5) . 6_655 ? F(12) C(19) 3.310(5) . 5_445 ? F(12) C(3) 3.354(5) . 3_655 ? F(12) C(6) 3.420(5) . 3_655 ? F(12) C(7) 3.516(5) . 6_655 ? F(12) C(18) 3.591(6) . 5_445 ? F(13) C(8) 3.159(5) . 8_455 ? F(13) C(19) 3.230(6) . 7_645 ? F(13) C(9) 3.290(5) . 8_455 ? F(13) C(20) 3.512(5) . 7_645 ? F(14) C(20) 3.561(5) . 7_645 ? F(15) C(6) 3.319(5) . 3_655 ? F(15) C(9) 3.419(5) . 8_455 ? F(15) C(7) 3.524(6) . 3_655 ? C(5) C(22) 3.555(6) . 4_564 ? C(6) C(22) 3.462(6) . 4_564 ? C(11) C(17) 3.495(6) . 4_565 ? C(11) C(16) 3.539(5) . 4_565 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ ### END #------------------------------------------------------------------------------ data_[Cu4(pprd)4(CO)4](PF6)4_Complex3-CCDC-659370 _database_code_depnum_ccdc_archive 'CCDC 659370' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H28 Cu4 F24 N12 O4 P4 ' _chemical_formula_moiety 'C40 H28 Cu4 N12 O4, 4(F6 P)' _chemical_formula_weight 1574.78 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n ' _symmetry_space_group_name_Hall '-P 4a ' _symmetry_Int_Tables_number 85 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,z 1/2-y,x,z y,1/2-x,z -x,-y,-z 1/2+x,1/2+y,-z 1/2+y,-x,-z -y,1/2+x,-z _cell_length_a 14.8455(8) _cell_length_b 14.8455(8) _cell_length_c 12.2984(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2710.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6379 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour L _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552.00 _exptl_absorpt_coefficient_mu 1.803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.965 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 15811 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3102 _reflns_number_gt 2732 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.0928 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3102 _refine_ls_number_parameters 204 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0291P)^2^+4.0002P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.54 _refine_diff_density_min -0.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.37827(2) -0.00077(2) 0.61783(3) 0.0191(1) Uani 1.00 1 d . . . P(1) P 0.7500 0.2500 1.0000 0.0221(3) Uani 1.00 4 d S . . P(2) P 0.7500 0.2500 0.5000 0.0226(3) Uani 1.00 4 d S . . P(3) P 0.2500 0.2500 0.8802(1) 0.0261(4) Uani 1.00 4 d S . . P(4) P 0.2500 0.2500 0.3925(2) 0.0293(4) Uani 1.00 4 d S . . F(1) F 0.7500 0.2500 0.8703(2) 0.0320(6) Uani 1.00 2 d S . . F(2) F 0.8519(1) 0.2131(1) 0.9995(2) 0.0315(4) Uani 1.00 1 d . . . F(3) F 0.7500 0.2500 0.6281(3) 0.073(1) Uani 1.00 2 d S . . F(4) F 0.7143(1) 0.3516(1) 0.5005(2) 0.0492(6) Uani 1.00 1 d . . . F(5) F 0.2500 0.2500 1.0100(3) 0.0342(9) Uani 1.00 4 d S . . F(6) F 0.2045(2) 0.3471(2) 0.8813(2) 0.0594(7) Uani 1.00 1 d . . . F(7) F 0.2500 0.2500 0.7511(4) 0.065(1) Uani 1.00 4 d S . . F(8) F 0.2500 0.2500 0.5240(4) 0.066(2) Uani 1.00 4 d S . . F(9) F 0.3456(2) 0.2032(2) 0.3971(3) 0.084(1) Uani 1.00 1 d . . . F(10) F 0.2500 0.2500 0.2682(5) 0.106(3) Uani 1.00 4 d S . . O(1) O 0.3566(2) -0.0205(2) 0.3819(2) 0.0343(6) Uani 1.00 1 d . . . N(1) N 0.4462(2) 0.1053(2) 0.6865(2) 0.0180(5) Uani 1.00 1 d . . . N(2) N 0.4537(2) -0.0681(2) 0.7312(2) 0.0213(5) Uani 1.00 1 d . . . N(3) N 0.4963(2) 0.2561(2) 0.6951(2) 0.0185(5) Uani 1.00 1 d . . . C(1) C 0.4464(2) 0.1899(2) 0.6527(2) 0.0197(6) Uani 1.00 1 d . . . C(2) C 0.5467(2) 0.2342(2) 0.7808(3) 0.0257(7) Uani 1.00 1 d . . . C(3) C 0.5492(2) 0.1483(2) 0.8229(3) 0.0268(7) Uani 1.00 1 d . . . C(4) C 0.5525(2) -0.0492(2) 0.8827(3) 0.0248(6) Uani 1.00 1 d . . . C(5) C 0.5563(2) -0.1418(2) 0.8973(3) 0.0317(8) Uani 1.00 1 d . . . C(6) C 0.5080(3) -0.1961(2) 0.8281(3) 0.0355(8) Uani 1.00 1 d . . . C(7) C 0.4570(2) -0.1572(2) 0.7467(3) 0.0298(7) Uani 1.00 1 d . . . C(8) C 0.4987(2) 0.0830(2) 0.7716(2) 0.0177(6) Uani 1.00 1 d . . . C(9) C 0.5013(2) -0.0144(2) 0.7984(2) 0.0189(6) Uani 1.00 1 d . . . C(10) C 0.3681(2) -0.0144(2) 0.4717(3) 0.0229(7) Uani 1.00 1 d . . . H(1) H 0.5847 -0.0101 0.9300 0.0298 Uiso 1.00 1 calc . . . H(2) H 0.5917 -0.1671 0.9540 0.0380 Uiso 1.00 1 calc . . . H(3) H 0.5097 -0.2597 0.8362 0.0426 Uiso 1.00 1 calc . . . H(4) H 0.5845 0.1345 0.8851 0.0321 Uiso 1.00 1 calc . . . H(5) H 0.4080 0.2048 0.5936 0.0237 Uiso 1.00 1 calc . . . H(6) H 0.4230 -0.1951 0.6999 0.0358 Uiso 1.00 1 calc . . . H(7) H 0.5824 0.2797 0.8141 0.0308 Uiso 1.00 1 calc . . . 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) 0.0175(2) 0.0187(2) 0.0211(2) -0.0003(1) -0.0030(2) -0.0004(2) P(1) 0.0253(5) 0.0253(5) 0.0157(8) 0.0000 0.0000 0.0000 P(2) 0.0207(5) 0.0207(5) 0.0264(9) 0.0000 0.0000 0.0000 P(3) 0.0298(5) 0.0298(5) 0.0186(8) 0.0000 0.0000 0.0000 P(4) 0.0327(6) 0.0327(6) 0.0225(9) 0.0000 0.0000 0.0000 F(1) 0.039(2) 0.042(2) 0.015(1) 0.008(1) 0.0000 0.0000 F(2) 0.027(1) 0.037(1) 0.030(1) 0.0047(8) -0.0018(8) 0.0049(9) F(3) 0.097(3) 0.096(3) 0.026(2) 0.002(3) 0.0000 0.0000 F(4) 0.029(1) 0.023(1) 0.096(2) 0.0029(8) 0.000(1) -0.001(1) F(5) 0.042(1) 0.042(1) 0.018(2) 0.0000 0.0000 0.0000 F(6) 0.081(2) 0.042(1) 0.055(2) 0.024(1) 0.010(1) 0.019(1) F(7) 0.087(2) 0.087(2) 0.021(2) 0.0000 0.0000 0.0000 F(8) 0.082(2) 0.082(2) 0.034(3) 0.0000 0.0000 0.0000 F(9) 0.059(2) 0.096(2) 0.096(3) 0.032(2) 0.009(2) -0.002(2) F(10) 0.149(4) 0.149(4) 0.021(3) 0.0000 0.0000 0.0000 O(1) 0.031(1) 0.049(2) 0.023(1) -0.002(1) 0.003(1) -0.004(1) N(1) 0.016(1) 0.019(1) 0.019(1) -0.0001(9) -0.0014(10) -0.0018(10) N(2) 0.019(1) 0.018(1) 0.028(1) 0.0023(9) -0.001(1) 0.002(1) N(3) 0.018(1) 0.018(1) 0.019(1) 0.0001(9) -0.0003(10) -0.0013(10) C(1) 0.016(1) 0.023(1) 0.020(1) 0.002(1) -0.003(1) 0.001(1) C(2) 0.029(2) 0.022(2) 0.026(2) -0.004(1) -0.008(1) -0.002(1) C(3) 0.031(2) 0.028(2) 0.022(2) -0.001(1) -0.011(1) 0.001(1) C(4) 0.020(2) 0.033(2) 0.022(2) 0.003(1) -0.001(1) 0.004(1) C(5) 0.029(2) 0.034(2) 0.032(2) 0.010(1) -0.002(1) 0.012(2) C(6) 0.037(2) 0.024(2) 0.045(2) 0.009(1) -0.001(2) 0.013(2) C(7) 0.030(2) 0.020(2) 0.040(2) 0.002(1) -0.003(2) 0.001(1) C(8) 0.013(1) 0.022(1) 0.018(1) 0.002(1) 0.002(1) 0.000(1) C(9) 0.014(1) 0.021(2) 0.022(1) 0.003(1) 0.004(1) 0.001(1) C(10) 0.016(1) 0.025(2) 0.028(2) -0.003(1) 0.003(1) -0.001(1) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cu(1) N(1) 2.051(2) . . yes Cu(1) N(2) 2.048(3) . . yes Cu(1) N(3) 2.048(2) . 4_555 yes Cu(1) C(10) 1.815(3) . . yes P(1) F(1) 1.596(3) . . yes P(1) F(1) 1.596(3) . 7_567 yes P(1) F(2) 1.610(2) . . yes P(1) F(2) 1.610(2) . 7_567 yes P(1) F(2) 1.610(2) . 8_647 yes P(1) F(2) 1.610(2) . 2_655 yes P(2) F(3) 1.575(3) . . yes P(2) F(3) 1.575(3) . 7_566 yes P(2) F(4) 1.598(2) . . yes P(2) F(4) 1.598(2) . 7_566 yes P(2) F(4) 1.598(2) . 8_646 yes P(2) F(4) 1.598(2) . 2_655 yes P(3) F(5) 1.596(4) . . yes P(3) F(6) 1.592(3) . . yes P(3) F(6) 1.592(3) . 2_555 yes P(3) F(6) 1.592(3) . 3_555 yes P(3) F(6) 1.592(3) . 4_555 yes P(3) F(7) 1.587(5) . . yes P(4) F(8) 1.618(5) . . yes P(4) F(9) 1.581(3) . . yes P(4) F(9) 1.581(3) . 2_555 yes P(4) F(9) 1.581(3) . 3_555 yes P(4) F(9) 1.581(3) . 4_555 yes P(4) F(10) 1.529(6) . . yes O(1) C(10) 1.121(4) . . yes N(1) C(1) 1.323(4) . . yes N(1) C(8) 1.346(4) . . yes N(2) C(7) 1.337(4) . . yes N(2) C(9) 1.349(4) . . yes N(3) C(1) 1.337(4) . . yes N(3) C(2) 1.334(4) . . yes C(1) H(5) 0.950 . . no C(2) C(3) 1.378(4) . . yes C(2) H(7) 0.950 . . no C(3) C(8) 1.379(4) . . yes C(3) H(4) 0.950 . . no C(4) C(5) 1.387(5) . . yes C(4) C(9) 1.385(4) . . yes C(4) H(1) 0.950 . . no C(5) C(6) 1.374(5) . . yes C(5) H(2) 0.950 . . no C(6) C(7) 1.383(5) . . yes C(6) H(3) 0.950 . . no C(7) H(6) 0.950 . . no C(8) C(9) 1.483(4) . . 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 N(1) Cu(1) N(2) 79.96(10) . . . yes N(1) Cu(1) N(3) 102.67(10) . . 4_555 yes N(1) Cu(1) C(10) 122.3(1) . . . yes N(2) Cu(1) N(3) 100.60(10) . . 4_555 yes N(2) Cu(1) C(10) 131.7(1) . . . yes N(3) Cu(1) C(10) 112.9(1) 4_555 . . yes F(1) P(1) F(1) 180.0 . . 7_567 yes F(1) P(1) F(2) 89.80(7) . . . yes F(1) P(1) F(2) 90.20(7) . . 7_567 yes F(1) P(1) F(2) 90.20(7) . . 8_647 yes F(1) P(1) F(2) 89.80(7) . . 2_655 yes F(1) P(1) F(2) 90.20(7) 7_567 . . yes F(1) P(1) F(2) 89.80(7) 7_567 . 7_567 yes F(1) P(1) F(2) 89.80(7) 7_567 . 8_647 yes F(1) P(1) F(2) 90.20(7) 7_567 . 2_655 yes F(2) P(1) F(2) 90.001(2) . . 7_567 yes F(2) P(1) F(2) 90.001(2) . . 8_647 yes F(2) P(1) F(2) 179.6(1) . . 2_655 yes F(2) P(1) F(2) 179.6(1) 7_567 . 8_647 yes F(2) P(1) F(2) 90.001(2) 7_567 . 2_655 yes F(2) P(1) F(2) 90.001(2) 8_647 . 2_655 yes F(3) P(2) F(3) 180.0 . . 7_566 yes F(3) P(2) F(4) 89.76(10) . . . yes F(3) P(2) F(4) 90.24(10) . . 7_566 yes F(3) P(2) F(4) 90.24(10) . . 8_646 yes F(3) P(2) F(4) 89.76(10) . . 2_655 yes F(3) P(2) F(4) 90.24(10) 7_566 . . yes F(3) P(2) F(4) 89.76(10) 7_566 . 7_566 yes F(3) P(2) F(4) 89.76(10) 7_566 . 8_646 yes F(3) P(2) F(4) 90.24(10) 7_566 . 2_655 yes F(4) P(2) F(4) 90.001(2) . . 7_566 yes F(4) P(2) F(4) 90.001(2) . . 8_646 yes F(4) P(2) F(4) 179.5(2) . . 2_655 yes F(4) P(2) F(4) 179.5(2) 7_566 . 8_646 yes F(4) P(2) F(4) 90.001(2) 7_566 . 2_655 yes F(4) P(2) F(4) 90.001(2) 8_646 . 2_655 yes F(5) P(3) F(6) 89.5(1) . . . yes F(5) P(3) F(6) 89.5(1) . . 2_555 yes F(5) P(3) F(6) 89.5(1) . . 3_555 yes F(5) P(3) F(6) 89.5(1) . . 4_555 yes F(5) P(3) F(7) 180.0 . . . yes F(6) P(3) F(6) 179.0(2) . . 2_555 yes F(6) P(3) F(6) 89.996(3) . . 3_555 yes F(6) P(3) F(6) 89.996(3) . . 4_555 yes F(6) P(3) F(7) 90.5(1) . . . yes F(6) P(3) F(6) 89.996(3) 2_555 . 3_555 yes F(6) P(3) F(6) 89.996(3) 2_555 . 4_555 yes F(6) P(3) F(7) 90.5(1) 2_555 . . yes F(6) P(3) F(6) 179.0(2) 3_555 . 4_555 yes F(6) P(3) F(7) 90.5(1) 3_555 . . yes F(6) P(3) F(7) 90.5(1) 4_555 . . yes F(8) P(4) F(9) 87.9(1) . . . yes F(8) P(4) F(9) 87.9(1) . . 2_555 yes F(8) P(4) F(9) 87.9(1) . . 3_555 yes F(8) P(4) F(9) 87.9(1) . . 4_555 yes F(8) P(4) F(10) 180.0 . . . yes F(9) P(4) F(9) 175.9(3) . . 2_555 yes F(9) P(4) F(9) 89.93(1) . . 3_555 yes F(9) P(4) F(9) 89.93(1) . . 4_555 yes F(9) P(4) F(10) 92.1(1) . . . yes F(9) P(4) F(9) 89.93(1) 2_555 . 3_555 yes F(9) P(4) F(9) 89.93(1) 2_555 . 4_555 yes F(9) P(4) F(10) 92.1(1) 2_555 . . yes F(9) P(4) F(9) 175.9(3) 3_555 . 4_555 yes F(9) P(4) F(10) 92.1(1) 3_555 . . yes F(9) P(4) F(10) 92.1(1) 4_555 . . yes Cu(1) N(1) C(1) 126.9(2) . . . yes Cu(1) N(1) C(8) 114.6(2) . . . yes C(1) N(1) C(8) 118.4(3) . . . yes Cu(1) N(2) C(7) 126.8(2) . . . yes Cu(1) N(2) C(9) 114.5(2) . . . yes C(7) N(2) C(9) 118.6(3) . . . yes Cu(1) N(3) C(1) 119.3(2) 3_555 . . yes Cu(1) N(3) C(2) 124.3(2) 3_555 . . yes C(1) N(3) C(2) 116.1(3) . . . yes N(1) C(1) N(3) 125.3(3) . . . yes N(1) C(1) H(5) 117.4 . . . no N(3) C(1) H(5) 117.4 . . . no N(3) C(2) C(3) 122.5(3) . . . yes N(3) C(2) H(7) 118.7 . . . no C(3) C(2) H(7) 118.7 . . . no C(2) C(3) C(8) 117.7(3) . . . yes C(2) C(3) H(4) 121.1 . . . no C(8) C(3) H(4) 121.1 . . . no C(5) C(4) C(9) 119.3(3) . . . yes C(5) C(4) H(1) 120.4 . . . no C(9) C(4) H(1) 120.4 . . . no C(4) C(5) C(6) 118.7(3) . . . yes C(4) C(5) H(2) 120.7 . . . no C(6) C(5) H(2) 120.7 . . . no C(5) C(6) C(7) 119.3(3) . . . yes C(5) C(6) H(3) 120.3 . . . no C(7) C(6) H(3) 120.3 . . . no N(2) C(7) C(6) 122.4(3) . . . yes N(2) C(7) H(6) 118.8 . . . no C(6) C(7) H(6) 118.8 . . . no N(1) C(8) C(3) 119.8(3) . . . yes N(1) C(8) C(9) 115.4(2) . . . yes C(3) C(8) C(9) 124.7(3) . . . yes N(2) C(9) C(4) 121.7(3) . . . yes N(2) C(9) C(8) 115.2(3) . . . yes C(4) C(9) C(8) 123.0(3) . . . yes Cu(1) C(10) O(1) 175.6(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 Cu(1) F(4) 3.585(2) . 6_446 ? F(2) C(6) 3.418(4) . 6_557 ? F(4) C(10) 3.048(4) . 6_556 ? F(4) O(1) 3.187(3) . 6_556 ? F(5) F(10) 3.175(7) . 1_556 ? F(5) C(5) 3.485(4) . 5_657 ? F(5) C(5) 3.485(4) . 6_457 ? F(5) C(5) 3.485(4) . 8_547 ? F(6) C(5) 3.504(4) . 6_457 ? F(9) C(7) 3.491(5) . 5_656 ? F(9) C(6) 3.522(5) . 5_656 ? O(1) C(8) 3.007(4) . 5_656 ? O(1) C(9) 3.105(4) . 5_656 ? O(1) N(1) 3.296(3) . 5_656 ? O(1) C(7) 3.373(4) . 8_546 ? O(1) N(2) 3.406(3) . 5_656 ? O(1) C(3) 3.450(4) . 5_656 ? O(1) C(6) 3.540(4) . 8_546 ? C(4) C(4) 3.590(6) . 5_657 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_[Cu3(pprd)3(C2H4)3]3(ClO4)9_Complex4-CCDC-659371 _database_code_depnum_ccdc_archive 'CCDC 659371' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C33 H33 Cl3 Cu3 N9 O12 ' _chemical_formula_moiety 'C33 H33 Cu3 N9, 3(Cl O4)' _chemical_formula_weight 1044.67 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall 'P 2c -2n ' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,z _cell_length_a 14.4419(7) _cell_length_b 38.607(2) _cell_length_c 21.448(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11958(1) _cell_formula_units_Z 12 _cell_measurement_reflns_used 30713 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6336.00 _exptl_absorpt_coefficient_mu 1.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.757 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 93735 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min 12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 23226 _reflns_number_gt 19520 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1168 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 23226 _refine_ls_number_parameters 1621 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0428P)^2^+17.0296P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0030 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack(1983), 9136 Friedel pairs' _refine_ls_abs_structure_Flack 0.113(9) _refine_diff_density_max 0.74 _refine_diff_density_min -0.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.95063(5) 0.73116(2) 0.49296(3) 0.0229(2) Uani 1.00 1 d . . . Cu(2) Cu 0.94750(5) 0.67411(2) 0.22608(4) 0.0217(1) Uani 1.00 1 d . . . Cu(3) Cu 0.93941(5) 0.82656(2) 0.27808(4) 0.0221(2) Uani 1.00 1 d . . . Cu(4) Cu 0.45817(5) 0.42954(2) 0.16549(3) 0.0223(2) Uani 1.00 1 d . . . Cu(5) Cu 0.45734(5) 0.49842(2) 0.41993(4) 0.0244(2) Uani 1.00 1 d . . . Cu(6) Cu 0.45204(5) 0.34224(2) 0.39664(4) 0.0247(2) Uani 1.00 1 d . . . Cu(7) Cu 0.94409(5) 0.37420(2) 0.18059(3) 0.0217(2) Uani 1.00 1 d . . . Cu(8) Cu 0.95727(5) 0.35394(2) 0.46386(3) 0.0226(2) Uani 1.00 1 d . . . Cu(9) Cu 0.95506(5) 0.49613(2) 0.34655(4) 0.0244(2) Uani 1.00 1 d . . . Cl(1) Cl 0.6820(1) 0.73882(4) 0.33091(8) 0.0286(3) Uani 1.00 1 d . . . Cl(2) Cl 0.19495(9) 0.42439(4) 0.32239(7) 0.0231(3) Uani 1.00 1 d . . . Cl(3) Cl 0.6985(1) 0.41257(4) 0.33325(8) 0.0292(3) Uani 1.00 1 d . . . Cl(4) Cl 0.9930(1) 0.60698(4) 0.48183(8) 0.0352(4) Uani 1.00 1 d . . . Cl(5) Cl 0.9906(1) 0.55194(5) 0.13541(9) 0.0405(4) Uani 1.00 1 d . . . Cl(6) Cl 0.4977(1) 0.55928(5) 0.1237(1) 0.0430(4) Uani 1.00 1 d . . . Cl(7) Cl 0.4987(1) 0.62003(5) 0.4681(1) 0.0459(5) Uani 1.00 1 d . . . Cl(8) Cl 0.4753(1) 0.25307(5) 0.22929(9) 0.0385(4) Uani 1.00 1 d . . . Cl(9) Cl 0.4951(1) 0.25098(4) 0.54807(8) 0.0299(3) Uani 1.00 1 d . . . O(1) O 0.6537(4) 0.7193(2) 0.3837(3) 0.059(2) Uani 1.00 1 d . . . O(2) O 0.6502(4) 0.7208(2) 0.2754(3) 0.061(2) Uani 1.00 1 d . . . O(3) O 0.6419(4) 0.7728(1) 0.3321(3) 0.056(2) Uani 1.00 1 d . . . O(4) O 0.7807(3) 0.7416(1) 0.3298(2) 0.028(1) Uani 1.00 1 d . . . O(5) O 0.1709(4) 0.4392(1) 0.2629(2) 0.046(1) Uani 1.00 1 d . . . O(6) O 0.1633(4) 0.4462(2) 0.3716(3) 0.049(1) Uani 1.00 1 d . . . O(7) O 0.1505(3) 0.3913(1) 0.3273(3) 0.047(1) Uani 1.00 1 d . . . O(8) O 0.2920(3) 0.4202(1) 0.3271(2) 0.030(1) Uani 1.00 1 d . . . O(9) O 0.6668(4) 0.3842(2) 0.2955(3) 0.060(2) Uani 1.00 1 d . . . O(10) O 0.6645(4) 0.4095(2) 0.3957(3) 0.061(2) Uani 1.00 1 d . . . O(11) O 0.6639(4) 0.4443(2) 0.3075(3) 0.063(2) Uani 1.00 1 d . . . O(12) O 0.7969(3) 0.4130(1) 0.3346(3) 0.044(1) Uani 1.00 1 d . . . O(13) O 1.0742(4) 0.6264(2) 0.4940(3) 0.080(2) Uani 1.00 1 d . . . O(14) O 1.0009(5) 0.5736(2) 0.5044(5) 0.128(4) Uani 1.00 1 d . . . O(15) O 0.9828(4) 0.6057(2) 0.4158(3) 0.074(2) Uani 1.00 1 d . . . O(16) O 0.9134(4) 0.6237(1) 0.5079(2) 0.045(1) Uani 1.00 1 d . . . O(17) O 1.0855(4) 0.5610(2) 0.1381(4) 0.079(2) Uani 1.00 1 d . . . O(18) O 0.9814(4) 0.5154(2) 0.1334(4) 0.074(2) Uani 1.00 1 d . . . O(19) O 0.9494(5) 0.5686(2) 0.0835(4) 0.092(3) Uani 1.00 1 d . . . O(20) O 0.9460(6) 0.5646(2) 0.1903(3) 0.099(3) Uani 1.00 1 d . . . O(21) O 0.5821(4) 0.5414(2) 0.1143(3) 0.070(2) Uani 1.00 1 d . . . O(22) O 0.4222(4) 0.5409(2) 0.0978(4) 0.072(2) Uani 1.00 1 d . . . O(23) O 0.5076(5) 0.5918(2) 0.0926(5) 0.097(3) Uani 1.00 1 d . . . O(24) O 0.4834(6) 0.5644(3) 0.1883(4) 0.133(4) Uani 1.00 1 d . . . O(25) O 0.5852(4) 0.6121(2) 0.4410(3) 0.055(2) Uani 1.00 1 d . . . O(26) O 0.4235(4) 0.6105(2) 0.4282(4) 0.088(3) Uani 1.00 1 d . . . O(27) O 0.4925(4) 0.6563(2) 0.4797(3) 0.065(2) Uani 1.00 1 d . . . O(28) O 0.4922(6) 0.6017(3) 0.5243(4) 0.136(4) Uani 1.00 1 d . . . O(29) O 0.5652(5) 0.2426(2) 0.2153(5) 0.106(3) Uani 1.00 1 d . . . O(30) O 0.4077(6) 0.2335(2) 0.1995(3) 0.095(3) Uani 1.00 1 d . . . O(31) O 0.4653(5) 0.2880(2) 0.2196(5) 0.090(3) Uani 1.00 1 d . . . O(32) O 0.4645(6) 0.2458(3) 0.2946(4) 0.124(4) Uani 1.00 1 d . . . O(33) O 0.5908(3) 0.2441(2) 0.5577(3) 0.049(1) Uani 1.00 1 d . . . O(34) O 0.4414(4) 0.2367(2) 0.5987(3) 0.048(1) Uani 1.00 1 d . . . O(35) O 0.4651(4) 0.2358(2) 0.4913(3) 0.051(1) Uani 1.00 1 d . . . O(36) O 0.4807(4) 0.2877(1) 0.5449(3) 0.052(1) Uani 1.00 1 d . . . N(1) N 0.9090(3) 0.6950(1) 0.4210(2) 0.021(1) Uani 1.00 1 d . . . N(2) N 0.9046(3) 0.6708(1) 0.3183(2) 0.022(1) Uani 1.00 1 d . . . N(3) N 0.8370(3) 0.7102(1) 0.5322(2) 0.024(1) Uani 1.00 1 d . . . N(4) N 0.8997(3) 0.7255(1) 0.2098(2) 0.018(1) Uani 1.00 1 d . . . N(5) N 0.8919(3) 0.7859(1) 0.2265(2) 0.020(1) Uani 1.00 1 d . . . N(6) N 0.8299(3) 0.6636(1) 0.1783(2) 0.020(1) Uani 1.00 1 d . . . N(7) N 0.8923(3) 0.8108(1) 0.3632(2) 0.022(1) Uani 1.00 1 d . . . N(8) N 0.8934(3) 0.7732(1) 0.4504(2) 0.020(1) Uani 1.00 1 d . . . N(9) N 0.8176(3) 0.8582(1) 0.2873(3) 0.025(1) Uani 1.00 1 d . . . N(10) N 0.4142(3) 0.4687(1) 0.2323(2) 0.022(1) Uani 1.00 1 d . . . N(11) N 0.4138(3) 0.4990(1) 0.3287(2) 0.025(1) Uani 1.00 1 d . . . N(12) N 0.3414(3) 0.4487(1) 0.1244(2) 0.024(1) Uani 1.00 1 d . . . N(13) N 0.4104(3) 0.4466(1) 0.4449(2) 0.019(1) Uani 1.00 1 d . . . N(14) N 0.4052(3) 0.3855(1) 0.4391(2) 0.020(1) Uani 1.00 1 d . . . N(15) N 0.3375(3) 0.5094(1) 0.4651(2) 0.020(1) Uani 1.00 1 d . . . N(16) N 0.4093(3) 0.3540(1) 0.3041(2) 0.018(1) Uani 1.00 1 d . . . N(17) N 0.4080(3) 0.3877(1) 0.2108(2) 0.022(1) Uani 1.00 1 d . . . N(18) N 0.3327(3) 0.3117(1) 0.3878(2) 0.023(1) Uani 1.00 1 d . . . N(19) N 0.9042(3) 0.3505(1) 0.2698(2) 0.020(1) Uani 1.00 1 d . . . N(20) N 0.9136(3) 0.3375(1) 0.3782(2) 0.022(1) Uani 1.00 1 d . . . N(21) N 0.8235(3) 0.3498(1) 0.1583(2) 0.022(1) Uani 1.00 1 d . . . N(22) N 0.9144(3) 0.4089(1) 0.4579(2) 0.021(1) Uani 1.00 1 d . . . N(23) N 0.9137(4) 0.4663(1) 0.4185(3) 0.028(1) Uani 1.00 1 d . . . N(24) N 0.8383(3) 0.3539(1) 0.5137(2) 0.022(1) Uani 1.00 1 d . . . N(25) N 0.9074(3) 0.4704(1) 0.2680(2) 0.020(1) Uani 1.00 1 d . . . N(26) N 0.9057(3) 0.4236(1) 0.1975(2) 0.022(1) Uani 1.00 1 d . . . N(27) N 0.8356(3) 0.5268(1) 0.3223(2) 0.022(1) Uani 1.00 1 d . . . C(1) C 0.9432(4) 0.6895(2) 0.3636(3) 0.020(1) Uani 1.00 1 d . . . C(2) C 0.8246(4) 0.6550(2) 0.3340(3) 0.027(1) Uani 1.00 1 d . . . C(3) C 0.7848(4) 0.6583(2) 0.3918(3) 0.023(1) Uani 1.00 1 d . . . C(4) C 0.8275(4) 0.6798(1) 0.4352(3) 0.018(1) Uani 1.00 1 d . . . C(5) C 0.7887(4) 0.6873(2) 0.4967(3) 0.023(1) Uani 1.00 1 d . . . C(6) C 0.7068(4) 0.6730(2) 0.5186(3) 0.031(1) Uani 1.00 1 d . . . C(7) C 0.6725(5) 0.6835(2) 0.5755(4) 0.039(2) Uani 1.00 1 d . . . C(8) C 0.7191(5) 0.7069(2) 0.6110(3) 0.032(2) Uani 1.00 1 d . . . C(9) C 0.8030(5) 0.7193(2) 0.5879(3) 0.026(1) Uani 1.00 1 d . . . C(10) C 1.0672(5) 0.7148(2) 0.5390(4) 0.045(2) Uani 1.00 1 d . . . C(11) C 1.0879(5) 0.7395(2) 0.4992(4) 0.052(2) Uani 1.00 1 d . . . C(12) C 0.9345(4) 0.7553(2) 0.2301(3) 0.022(1) Uani 1.00 1 d . . . C(13) C 0.8079(4) 0.7863(2) 0.1999(3) 0.023(1) Uani 1.00 1 d . . . C(14) C 0.7688(4) 0.7566(2) 0.1751(3) 0.025(1) Uani 1.00 1 d . . . C(15) C 0.8167(4) 0.7260(2) 0.1806(3) 0.020(1) Uani 1.00 1 d . . . C(16) C 0.7819(4) 0.6918(2) 0.1600(3) 0.019(1) Uani 1.00 1 d . . . C(17) C 0.7027(4) 0.6884(2) 0.1235(3) 0.028(1) Uani 1.00 1 d . . . C(18) C 0.6710(4) 0.6559(2) 0.1076(3) 0.032(2) Uani 1.00 1 d . . . C(19) C 0.7194(5) 0.6274(2) 0.1285(3) 0.031(1) Uani 1.00 1 d . . . C(20) C 0.7984(4) 0.6324(2) 0.1627(3) 0.026(1) Uani 1.00 1 d . . . C(21) C 1.0588(5) 0.6570(2) 0.1744(4) 0.046(2) Uani 1.00 1 d . . . C(22) C 1.0884(5) 0.6758(2) 0.2207(4) 0.040(2) Uani 1.00 1 d . . . C(23) C 0.9292(4) 0.7864(2) 0.3985(3) 0.020(1) Uani 1.00 1 d . . . C(24) C 0.8121(4) 0.7874(2) 0.4680(3) 0.025(1) Uani 1.00 1 d . . . C(25) C 0.7699(4) 0.8137(2) 0.4365(3) 0.026(1) Uani 1.00 1 d . . . C(26) C 0.8110(4) 0.8248(1) 0.3825(3) 0.021(1) Uani 1.00 1 d . . . C(27) C 0.7708(4) 0.8526(2) 0.3410(3) 0.024(1) Uani 1.00 1 d . . . C(28) C 0.6927(5) 0.8705(2) 0.3565(4) 0.038(2) Uani 1.00 1 d . . . C(29) C 0.6581(5) 0.8948(2) 0.3170(4) 0.043(2) Uani 1.00 1 d . . . C(30) C 0.7052(5) 0.9007(2) 0.2603(4) 0.039(2) Uani 1.00 1 d . . . C(31) C 0.7851(5) 0.8827(2) 0.2487(3) 0.032(2) Uani 1.00 1 d . . . C(32) C 1.0497(5) 0.8583(2) 0.2955(4) 0.047(2) Uani 1.00 1 d . . . C(33) C 1.0515(5) 0.8496(2) 0.2366(4) 0.039(2) Uani 1.00 1 d . . . C(34) C 0.4491(4) 0.4764(2) 0.2879(3) 0.022(1) Uani 1.00 1 d . . . C(35) C 0.3396(5) 0.5173(2) 0.3082(3) 0.033(2) Uani 1.00 1 d . . . C(36) C 0.3004(5) 0.5110(2) 0.2513(3) 0.033(2) Uani 1.00 1 d . . . C(37) C 0.3365(4) 0.4856(2) 0.2145(3) 0.022(1) Uani 1.00 1 d . . . C(38) C 0.2941(4) 0.4734(2) 0.1547(3) 0.021(1) Uani 1.00 1 d . . . C(39) C 0.2091(5) 0.4852(2) 0.1344(3) 0.035(2) Uani 1.00 1 d . . . C(40) C 0.1697(5) 0.4706(2) 0.0829(3) 0.036(2) Uani 1.00 1 d . . . C(41) C 0.2169(4) 0.4455(2) 0.0502(3) 0.032(2) Uani 1.00 1 d . . . C(42) C 0.3039(5) 0.4357(2) 0.0717(3) 0.030(1) Uani 1.00 1 d . . . C(43) C 0.5698(5) 0.4515(2) 0.1229(4) 0.039(2) Uani 1.00 1 d . . . C(44) C 0.5972(5) 0.4236(2) 0.1536(4) 0.038(2) Uani 1.00 1 d . . . C(45) C 0.4464(4) 0.4161(2) 0.4299(3) 0.023(1) Uani 1.00 1 d . . . C(46) C 0.3217(4) 0.3860(2) 0.4690(3) 0.022(1) Uani 1.00 1 d . . . C(47) C 0.2821(4) 0.4166(2) 0.4872(3) 0.022(1) Uani 1.00 1 d . . . C(48) C 0.3268(4) 0.4471(2) 0.4740(3) 0.019(1) Uani 1.00 1 d . . . C(49) C 0.2880(4) 0.4821(2) 0.4863(3) 0.020(1) Uani 1.00 1 d . . . C(50) C 0.2034(4) 0.4867(2) 0.5167(3) 0.024(1) Uani 1.00 1 d . . . C(51) C 0.1688(4) 0.5200(2) 0.5238(3) 0.029(1) Uani 1.00 1 d . . . C(52) C 0.2188(4) 0.5479(2) 0.5020(3) 0.026(1) Uani 1.00 1 d . . . C(53) C 0.3040(4) 0.5413(2) 0.4740(3) 0.025(1) Uani 1.00 1 d . . . C(54) C 0.5688(5) 0.5144(2) 0.4711(4) 0.048(2) Uani 1.00 1 d . . . C(55) C 0.5989(5) 0.5032(3) 0.4189(4) 0.055(2) Uani 1.00 1 d . . . C(56) C 0.4457(4) 0.3767(2) 0.2643(3) 0.021(1) Uani 1.00 1 d . . . C(57) C 0.3275(4) 0.3728(2) 0.1953(3) 0.024(1) Uani 1.00 1 d . . . C(58) C 0.2852(4) 0.3482(2) 0.2318(3) 0.025(1) Uani 1.00 1 d . . . C(59) C 0.3275(4) 0.3389(2) 0.2879(3) 0.019(1) Uani 1.00 1 d . . . C(60) C 0.2878(4) 0.3142(1) 0.3333(3) 0.019(1) Uani 1.00 1 d . . . C(61) C 0.2089(4) 0.2949(2) 0.3204(4) 0.033(2) Uani 1.00 1 d . . . C(62) C 0.1754(5) 0.2727(2) 0.3642(4) 0.042(2) Uani 1.00 1 d . . . C(63) C 0.2204(5) 0.2699(2) 0.4196(4) 0.035(2) Uani 1.00 1 d . . . C(64) C 0.2999(4) 0.2893(2) 0.4304(3) 0.029(1) Uani 1.00 1 d . . . C(65) C 0.5555(6) 0.3067(2) 0.3861(5) 0.058(2) Uani 1.00 1 d . . . C(66) C 0.5829(5) 0.3290(2) 0.4258(4) 0.045(2) Uani 1.00 1 d . . . C(67) C 0.9437(4) 0.3525(2) 0.3262(3) 0.023(1) Uani 1.00 1 d . . . C(68) C 0.8415(5) 0.3157(2) 0.3718(3) 0.032(2) Uani 1.00 1 d . . . C(69) C 0.7984(5) 0.3113(2) 0.3152(3) 0.033(2) Uani 1.00 1 d . . . C(70) C 0.8282(4) 0.3302(2) 0.2647(3) 0.022(1) Uani 1.00 1 d . . . C(71) C 0.7811(4) 0.3312(2) 0.2038(3) 0.024(1) Uani 1.00 1 d . . . C(72) C 0.6949(4) 0.3160(2) 0.1946(3) 0.031(2) Uani 1.00 1 d . . . C(73) C 0.6497(5) 0.3210(2) 0.1383(4) 0.039(2) Uani 1.00 1 d . . . C(74) C 0.6920(5) 0.3404(2) 0.0917(3) 0.033(2) Uani 1.00 1 d . . . C(75) C 0.7799(5) 0.3535(2) 0.1042(3) 0.030(1) Uani 1.00 1 d . . . C(76) C 1.0553(4) 0.3455(2) 0.1495(3) 0.029(1) Uani 1.00 1 d . . . C(77) C 1.0828(4) 0.3774(2) 0.1644(3) 0.032(2) Uani 1.00 1 d . . . C(78) C 0.9505(4) 0.4347(2) 0.4254(3) 0.025(1) Uani 1.00 1 d . . . C(79) C 0.8369(5) 0.4727(2) 0.4527(3) 0.029(1) Uani 1.00 1 d . . . C(80) C 0.7969(5) 0.4481(2) 0.4904(3) 0.033(2) Uani 1.00 1 d . . . C(81) C 0.8365(4) 0.4153(2) 0.4904(3) 0.023(1) Uani 1.00 1 d . . . C(82) C 0.7938(4) 0.3848(2) 0.5214(3) 0.025(1) Uani 1.00 1 d . . . C(83) C 0.7089(4) 0.3866(2) 0.5511(3) 0.033(2) Uani 1.00 1 d . . . C(84) C 0.6679(5) 0.3564(2) 0.5724(3) 0.037(2) Uani 1.00 1 d . . . C(85) C 0.7118(5) 0.3256(2) 0.5638(3) 0.032(2) Uani 1.00 1 d . . . C(86) C 0.7978(4) 0.3249(2) 0.5352(3) 0.027(1) Uani 1.00 1 d . . . C(87) C 1.0711(4) 0.3507(2) 0.5220(3) 0.033(2) Uani 1.00 1 d . . . C(88) C 1.0969(4) 0.3490(2) 0.4629(4) 0.041(2) Uani 1.00 1 d . . . C(89) C 0.9404(4) 0.4414(2) 0.2454(3) 0.020(1) Uani 1.00 1 d . . . C(90) C 0.8333(4) 0.4386(2) 0.1684(3) 0.024(1) Uani 1.00 1 d . . . C(91) C 0.7977(4) 0.4696(2) 0.1865(3) 0.027(1) Uani 1.00 1 d . . . C(92) C 0.8332(4) 0.4852(2) 0.2396(3) 0.020(1) Uani 1.00 1 d . . . C(93) C 0.7937(4) 0.5164(1) 0.2689(3) 0.020(1) Uani 1.00 1 d . . . C(94) C 0.7177(5) 0.5333(2) 0.2447(4) 0.035(2) Uani 1.00 1 d . . . C(95) C 0.6806(5) 0.5611(2) 0.2761(4) 0.036(2) Uani 1.00 1 d . . . C(96) C 0.7215(5) 0.5719(2) 0.3309(4) 0.035(2) Uani 1.00 1 d . . . C(97) C 0.8002(5) 0.5546(2) 0.3516(3) 0.031(2) Uani 1.00 1 d . . . C(98) C 1.0672(5) 0.5209(2) 0.3082(4) 0.043(2) Uani 1.00 1 d . . . C(99) C 1.0757(5) 0.5224(2) 0.3701(3) 0.033(2) Uani 1.00 1 d . . . H(1) H 1.0011 0.7001 0.3543 0.0238 Uiso 1.00 1 calc . . . H(2) H 0.7947 0.6410 0.3037 0.0329 Uiso 1.00 1 calc . . . H(3) H 0.7295 0.6461 0.4019 0.0270 Uiso 1.00 1 calc . . . H(4) H 0.6747 0.6562 0.4945 0.0376 Uiso 1.00 1 calc . . . H(5) H 0.6155 0.6743 0.5901 0.0480 Uiso 1.00 1 calc . . . H(6) H 0.6956 0.7144 0.6501 0.0373 Uiso 1.00 1 calc . . . H(7) H 0.8377 0.7349 0.6129 0.0320 Uiso 1.00 1 calc . . . H(8) H 1.0679 0.6913 0.5260 0.0536 Uiso 1.00 1 calc . . . H(9) H 1.0505 0.7206 0.5805 0.0536 Uiso 1.00 1 calc . . . H(10) H 1.0874 0.7629 0.5121 0.0612 Uiso 1.00 1 calc . . . H(11) H 1.1048 0.7336 0.4576 0.0612 Uiso 1.00 1 calc . . . H(12) H 0.9942 0.7548 0.2488 0.0263 Uiso 1.00 1 calc . . . H(13) H 0.7743 0.8075 0.1981 0.0279 Uiso 1.00 1 calc . . . H(14) H 0.7106 0.7572 0.1547 0.0307 Uiso 1.00 1 calc . . . H(15) H 0.6706 0.7084 0.1095 0.0336 Uiso 1.00 1 calc . . . H(16) H 0.6169 0.6532 0.0828 0.0387 Uiso 1.00 1 calc . . . H(17) H 0.6985 0.6047 0.1191 0.0370 Uiso 1.00 1 calc . . . H(18) H 0.8319 0.6125 0.1761 0.0323 Uiso 1.00 1 calc . . . H(19) H 1.0444 0.6675 0.1357 0.0549 Uiso 1.00 1 calc . . . H(20) H 1.0517 0.6326 0.1795 0.0549 Uiso 1.00 1 calc . . . H(21) H 1.1028 0.6652 0.2596 0.0479 Uiso 1.00 1 calc . . . H(22) H 1.0955 0.7001 0.2157 0.0479 Uiso 1.00 1 calc . . . H(23) H 0.9871 0.7773 0.3853 0.0243 Uiso 1.00 1 calc . . . H(24) H 0.7825 0.7785 0.5041 0.0309 Uiso 1.00 1 calc . . . H(25) H 0.7142 0.8238 0.4516 0.0323 Uiso 1.00 1 calc . . . H(26) H 0.6625 0.8660 0.3950 0.0462 Uiso 1.00 1 calc . . . H(27) H 0.6037 0.9076 0.3276 0.0528 Uiso 1.00 1 calc . . . H(28) H 0.6822 0.9170 0.2310 0.0466 Uiso 1.00 1 calc . . . H(29) H 0.8190 0.8877 0.2117 0.0388 Uiso 1.00 1 calc . . . H(30) H 1.0169 0.8784 0.3086 0.0569 Uiso 1.00 1 calc . . . H(31) H 1.0815 0.8445 0.3254 0.0569 Uiso 1.00 1 calc . . . H(32) H 1.0840 0.8296 0.2233 0.0459 Uiso 1.00 1 calc . . . H(33) H 1.0194 0.8634 0.2066 0.0459 Uiso 1.00 1 calc . . . H(34) H 0.5041 0.4648 0.2999 0.0265 Uiso 1.00 1 calc . . . H(35) H 0.3141 0.5349 0.3338 0.0399 Uiso 1.00 1 calc . . . H(36) H 0.2489 0.5243 0.2375 0.0396 Uiso 1.00 1 calc . . . H(37) H 0.1787 0.5035 0.1558 0.0426 Uiso 1.00 1 calc . . . H(38) H 0.1098 0.4777 0.0696 0.0435 Uiso 1.00 1 calc . . . H(39) H 0.1907 0.4351 0.0141 0.0388 Uiso 1.00 1 calc . . . H(40) H 0.3384 0.4193 0.0483 0.0360 Uiso 1.00 1 calc . . . H(41) H 0.5692 0.4735 0.1430 0.0474 Uiso 1.00 1 calc . . . H(42) H 0.5509 0.4497 0.0806 0.0474 Uiso 1.00 1 calc . . . H(43) H 0.5978 0.4017 0.1337 0.0467 Uiso 1.00 1 calc . . . H(44) H 0.6160 0.4254 0.1962 0.0467 Uiso 1.00 1 calc . . . H(45) H 0.5062 0.4160 0.4111 0.0281 Uiso 1.00 1 calc . . . H(46) H 0.2906 0.3648 0.4774 0.0268 Uiso 1.00 1 calc . . . H(47) H 0.2244 0.4167 0.5086 0.0264 Uiso 1.00 1 calc . . . H(48) H 0.1703 0.4673 0.5323 0.0292 Uiso 1.00 1 calc . . . H(49) H 0.1107 0.5235 0.5436 0.0352 Uiso 1.00 1 calc . . . H(50) H 0.1958 0.5710 0.5058 0.0317 Uiso 1.00 1 calc . . . H(51) H 0.3403 0.5605 0.4606 0.0315 Uiso 1.00 1 calc . . . H(52) H 0.5623 0.4992 0.5053 0.0567 Uiso 1.00 1 calc . . . H(53) H 0.5528 0.5383 0.4753 0.0567 Uiso 1.00 1 calc . . . H(54) H 0.6053 0.5185 0.3845 0.0673 Uiso 1.00 1 calc . . . H(55) H 0.6149 0.4795 0.4145 0.0673 Uiso 1.00 1 calc . . . H(56) H 0.5047 0.3860 0.2749 0.0258 Uiso 1.00 1 calc . . . H(57) H 0.2984 0.3795 0.1573 0.0293 Uiso 1.00 1 calc . . . H(58) H 0.2282 0.3379 0.2193 0.0303 Uiso 1.00 1 calc . . . H(59) H 0.1788 0.2973 0.2811 0.0402 Uiso 1.00 1 calc . . . H(60) H 0.1218 0.2593 0.3558 0.0511 Uiso 1.00 1 calc . . . H(61) H 0.1970 0.2548 0.4509 0.0423 Uiso 1.00 1 calc . . . H(62) H 0.3321 0.2866 0.4688 0.0351 Uiso 1.00 1 calc . . . H(63) H 0.5669 0.3099 0.3430 0.0704 Uiso 1.00 1 calc . . . H(64) H 0.5229 0.2865 0.3999 0.0704 Uiso 1.00 1 calc . . . H(65) H 0.5709 0.3256 0.4688 0.0541 Uiso 1.00 1 calc . . . H(66) H 0.6149 0.3490 0.4119 0.0541 Uiso 1.00 1 calc . . . H(67) H 0.9986 0.3661 0.3296 0.0275 Uiso 1.00 1 calc . . . H(68) H 0.8209 0.3029 0.4069 0.0393 Uiso 1.00 1 calc . . . H(69) H 0.7482 0.2954 0.3110 0.0401 Uiso 1.00 1 calc . . . H(70) H 0.6674 0.3022 0.2264 0.0378 Uiso 1.00 1 calc . . . H(71) H 0.5901 0.3113 0.1314 0.0477 Uiso 1.00 1 calc . . . H(72) H 0.6623 0.3446 0.0527 0.0405 Uiso 1.00 1 calc . . . H(73) H 0.8106 0.3658 0.0722 0.0367 Uiso 1.00 1 calc . . . H(74) H 1.0556 0.3277 0.1802 0.0354 Uiso 1.00 1 calc . . . H(75) H 1.0356 0.3405 0.1083 0.0354 Uiso 1.00 1 calc . . . H(76) H 1.0825 0.3951 0.1338 0.0388 Uiso 1.00 1 calc . . . H(77) H 1.1025 0.3823 0.2058 0.0388 Uiso 1.00 1 calc . . . H(78) H 1.0078 0.4304 0.4050 0.0299 Uiso 1.00 1 calc . . . H(79) H 0.8095 0.4951 0.4507 0.0354 Uiso 1.00 1 calc . . . H(80) H 0.7440 0.4533 0.5150 0.0409 Uiso 1.00 1 calc . . . H(81) H 0.6790 0.4083 0.5569 0.0403 Uiso 1.00 1 calc . . . H(82) H 0.6094 0.3571 0.5927 0.0456 Uiso 1.00 1 calc . . . H(83) H 0.6840 0.3047 0.5775 0.0383 Uiso 1.00 1 calc . . . H(84) H 0.8286 0.3033 0.5304 0.0326 Uiso 1.00 1 calc . . . H(85) H 1.0669 0.3724 0.5426 0.0404 Uiso 1.00 1 calc . . . H(86) H 1.0563 0.3300 0.5441 0.0404 Uiso 1.00 1 calc . . . H(87) H 1.1008 0.3273 0.4424 0.0495 Uiso 1.00 1 calc . . . H(88) H 1.1114 0.3697 0.4409 0.0495 Uiso 1.00 1 calc . . . H(89) H 0.9939 0.4321 0.2651 0.0245 Uiso 1.00 1 calc . . . H(90) H 0.8059 0.4270 0.1338 0.0290 Uiso 1.00 1 calc . . . H(91) H 0.7497 0.4804 0.1633 0.0329 Uiso 1.00 1 calc . . . H(92) H 0.6906 0.5256 0.2068 0.0422 Uiso 1.00 1 calc . . . H(93) H 0.6277 0.5727 0.2602 0.0438 Uiso 1.00 1 calc . . . H(94) H 0.6964 0.5908 0.3536 0.0424 Uiso 1.00 1 calc . . . H(95) H 0.8301 0.5627 0.3884 0.0378 Uiso 1.00 1 calc . . . H(96) H 1.0361 0.5389 0.2863 0.0509 Uiso 1.00 1 calc . . . H(97) H 1.0930 0.5019 0.2858 0.0509 Uiso 1.00 1 calc . . . H(98) H 1.1070 0.5045 0.3920 0.0393 Uiso 1.00 1 calc . . . H(99) H 1.0500 0.5414 0.3925 0.0393 Uiso 1.00 1 calc . . . 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) 0.0218(4) 0.0268(4) 0.0202(4) -0.0029(3) -0.0003(3) 0.0011(3) Cu(2) 0.0181(3) 0.0232(4) 0.0237(4) 0.0002(3) -0.0003(3) -0.0040(3) Cu(3) 0.0230(4) 0.0198(4) 0.0234(4) -0.0027(3) 0.0049(3) 0.0009(3) Cu(4) 0.0184(4) 0.0256(4) 0.0228(4) 0.0025(3) 0.0020(3) -0.0007(3) Cu(5) 0.0199(4) 0.0252(4) 0.0282(4) -0.0053(3) 0.0051(3) -0.0084(3) Cu(6) 0.0213(4) 0.0227(4) 0.0302(4) 0.0050(3) -0.0079(3) -0.0049(3) Cu(7) 0.0191(3) 0.0237(4) 0.0223(4) 0.0008(3) 0.0001(3) -0.0036(3) Cu(8) 0.0179(3) 0.0290(4) 0.0208(4) 0.0007(3) -0.0009(3) 0.0024(3) Cu(9) 0.0277(4) 0.0211(4) 0.0244(4) -0.0025(3) -0.0056(3) 0.0001(3) Cl(1) 0.0177(7) 0.0396(9) 0.0285(8) 0.0018(6) 0.0003(6) 0.0061(7) Cl(2) 0.0177(7) 0.0277(7) 0.0238(8) -0.0004(6) 0.0009(6) 0.0006(6) Cl(3) 0.0166(7) 0.0402(9) 0.0308(9) 0.0029(6) -0.0016(6) -0.0006(7) Cl(4) 0.0289(8) 0.0353(9) 0.041(1) 0.0086(7) 0.0064(8) 0.0058(7) Cl(5) 0.0333(9) 0.049(1) 0.039(1) -0.0045(8) -0.0016(8) 0.0039(8) Cl(6) 0.0358(9) 0.0370(9) 0.056(1) -0.0007(8) -0.0099(9) -0.0087(9) Cl(7) 0.0267(9) 0.049(1) 0.062(1) 0.0050(8) 0.0081(9) 0.0283(10) Cl(8) 0.0317(8) 0.0412(10) 0.043(1) 0.0014(7) -0.0042(8) -0.0067(8) Cl(9) 0.0227(7) 0.0365(9) 0.0304(8) -0.0001(7) 0.0029(7) 0.0034(7) O(1) 0.038(3) 0.088(4) 0.052(4) 0.008(3) 0.017(3) 0.033(3) O(2) 0.048(3) 0.087(5) 0.049(4) -0.023(3) -0.013(3) -0.021(3) O(3) 0.047(3) 0.049(3) 0.072(4) 0.025(3) 0.005(3) 0.000(3) O(4) 0.013(2) 0.040(3) 0.032(3) 0.004(2) -0.001(2) 0.003(2) O(5) 0.052(3) 0.049(3) 0.037(3) -0.009(3) -0.023(3) 0.016(2) O(6) 0.040(3) 0.064(4) 0.044(3) 0.021(3) 0.004(3) -0.022(3) O(7) 0.046(3) 0.043(3) 0.052(3) -0.027(2) 0.007(3) 0.005(3) O(8) 0.015(2) 0.043(3) 0.033(3) 0.004(2) -0.001(2) -0.001(2) O(9) 0.044(3) 0.052(4) 0.086(5) -0.002(3) -0.030(3) -0.020(3) O(10) 0.039(3) 0.111(5) 0.034(3) -0.013(3) 0.014(3) 0.003(3) O(11) 0.079(4) 0.058(4) 0.050(4) 0.038(3) -0.008(3) -0.002(3) O(12) 0.016(2) 0.067(4) 0.049(3) -0.006(2) 0.002(2) -0.012(3) O(13) 0.051(4) 0.111(6) 0.077(5) -0.018(4) -0.004(4) -0.033(4) O(14) 0.086(5) 0.087(5) 0.21(1) 0.057(4) 0.096(6) 0.105(6) O(15) 0.049(4) 0.121(6) 0.051(4) -0.002(4) 0.003(3) -0.037(4) O(16) 0.045(3) 0.053(3) 0.038(3) 0.029(3) 0.013(3) 0.012(2) O(17) 0.044(3) 0.064(4) 0.130(7) -0.014(3) 0.003(4) -0.025(4) O(18) 0.063(4) 0.046(4) 0.114(6) -0.012(3) 0.000(4) 0.008(4) O(19) 0.120(6) 0.079(5) 0.076(5) -0.033(4) -0.053(5) 0.032(4) O(20) 0.124(6) 0.115(6) 0.057(5) 0.075(5) 0.045(4) 0.029(4) O(21) 0.053(4) 0.068(4) 0.089(5) 0.019(3) 0.004(4) 0.010(4) O(22) 0.061(4) 0.052(4) 0.103(6) -0.025(3) -0.029(4) -0.002(4) O(23) 0.058(4) 0.045(4) 0.188(9) -0.004(3) -0.032(5) 0.036(5) O(24) 0.088(6) 0.22(1) 0.091(7) -0.050(7) 0.029(5) -0.086(7) O(25) 0.039(3) 0.061(4) 0.064(4) -0.005(3) 0.014(3) -0.014(3) O(26) 0.038(3) 0.060(4) 0.165(8) -0.021(3) -0.041(4) 0.037(5) O(27) 0.056(4) 0.055(4) 0.084(5) 0.014(3) -0.010(3) -0.006(3) O(28) 0.104(6) 0.190(10) 0.114(7) 0.067(6) 0.056(6) 0.123(7) O(29) 0.061(4) 0.083(5) 0.175(9) 0.025(4) 0.039(5) 0.025(6) O(30) 0.120(6) 0.091(5) 0.074(5) -0.065(5) -0.048(5) 0.022(4) O(31) 0.061(4) 0.052(4) 0.157(8) 0.003(3) 0.013(5) -0.013(5) O(32) 0.109(7) 0.21(1) 0.052(5) -0.062(7) -0.002(5) 0.000(6) O(33) 0.024(2) 0.076(4) 0.047(3) 0.003(3) 0.006(2) 0.003(3) O(34) 0.043(3) 0.063(4) 0.040(3) -0.009(3) 0.016(3) 0.018(3) O(35) 0.056(3) 0.065(4) 0.031(3) -0.005(3) -0.014(3) -0.005(3) O(36) 0.052(3) 0.028(3) 0.075(4) 0.000(2) 0.022(3) 0.005(3) N(1) 0.017(2) 0.021(3) 0.024(3) 0.002(2) -0.002(2) 0.004(2) N(2) 0.020(2) 0.027(3) 0.019(3) -0.003(2) 0.002(2) 0.002(2) N(3) 0.024(3) 0.024(3) 0.023(3) 0.002(2) 0.005(2) 0.005(2) N(4) 0.016(2) 0.018(2) 0.021(3) 0.001(2) 0.003(2) -0.001(2) N(5) 0.019(2) 0.024(3) 0.017(2) -0.003(2) 0.002(2) 0.002(2) N(6) 0.020(2) 0.026(3) 0.014(2) -0.004(2) 0.001(2) -0.001(2) N(7) 0.024(3) 0.019(2) 0.023(3) -0.001(2) 0.000(2) -0.001(2) N(8) 0.023(3) 0.022(2) 0.015(2) -0.005(2) 0.001(2) 0.001(2) N(9) 0.025(3) 0.019(3) 0.029(3) 0.001(2) -0.002(2) 0.003(2) N(10) 0.022(3) 0.025(3) 0.020(3) 0.005(2) 0.001(2) 0.000(2) N(11) 0.024(3) 0.028(3) 0.023(3) 0.000(2) 0.009(2) -0.006(2) N(12) 0.023(3) 0.029(3) 0.019(3) 0.002(2) 0.001(2) 0.002(2) N(13) 0.013(2) 0.019(2) 0.025(3) -0.003(2) 0.002(2) 0.000(2) N(14) 0.020(2) 0.015(2) 0.024(3) 0.002(2) -0.003(2) -0.003(2) N(15) 0.019(2) 0.021(2) 0.020(3) -0.001(2) -0.001(2) 0.001(2) N(16) 0.016(2) 0.019(2) 0.021(3) 0.000(2) -0.001(2) -0.002(2) N(17) 0.020(2) 0.024(3) 0.021(3) -0.001(2) 0.002(2) -0.004(2) N(18) 0.026(3) 0.015(2) 0.029(3) 0.002(2) -0.001(2) -0.002(2) N(19) 0.017(2) 0.026(3) 0.018(3) -0.002(2) 0.001(2) -0.002(2) N(20) 0.020(2) 0.024(3) 0.023(3) -0.002(2) 0.002(2) 0.000(2) N(21) 0.023(3) 0.018(2) 0.024(3) 0.004(2) -0.002(2) -0.004(2) N(22) 0.015(2) 0.027(3) 0.021(3) -0.001(2) 0.000(2) 0.002(2) N(23) 0.033(3) 0.028(3) 0.022(3) -0.007(2) -0.006(2) 0.001(2) N(24) 0.018(2) 0.029(3) 0.019(3) 0.002(2) 0.000(2) -0.001(2) N(25) 0.022(2) 0.018(2) 0.018(3) -0.003(2) -0.002(2) 0.001(2) N(26) 0.019(2) 0.024(3) 0.022(3) -0.001(2) 0.002(2) -0.001(2) N(27) 0.023(3) 0.015(2) 0.029(3) -0.001(2) 0.001(2) 0.004(2) C(1) 0.021(3) 0.020(3) 0.018(3) 0.007(2) 0.004(2) 0.002(2) C(2) 0.025(3) 0.025(3) 0.031(4) -0.007(3) 0.002(3) 0.005(3) C(3) 0.023(3) 0.027(3) 0.018(3) -0.008(3) 0.000(3) 0.001(3) C(4) 0.019(3) 0.017(3) 0.019(3) -0.001(2) 0.001(2) 0.002(2) C(5) 0.026(3) 0.019(3) 0.025(3) 0.003(2) 0.002(3) 0.005(2) C(6) 0.023(3) 0.038(4) 0.032(4) -0.008(3) 0.008(3) -0.002(3) C(7) 0.025(3) 0.054(5) 0.040(4) -0.002(3) 0.011(3) 0.009(4) C(8) 0.032(4) 0.044(4) 0.019(3) 0.009(3) 0.008(3) 0.009(3) C(9) 0.033(3) 0.023(3) 0.022(3) 0.005(3) 0.005(3) 0.007(2) C(10) 0.031(4) 0.064(5) 0.039(5) 0.011(4) -0.006(3) 0.002(4) C(11) 0.030(4) 0.074(6) 0.052(5) -0.011(4) -0.009(4) 0.000(5) C(12) 0.022(3) 0.024(3) 0.018(3) -0.003(2) 0.003(3) 0.000(2) C(13) 0.022(3) 0.018(3) 0.028(3) 0.001(2) -0.003(3) 0.005(2) C(14) 0.024(3) 0.034(3) 0.017(3) 0.003(3) -0.008(3) 0.002(3) C(15) 0.019(3) 0.029(3) 0.013(3) -0.003(2) 0.002(2) 0.000(2) C(16) 0.020(3) 0.025(3) 0.013(3) 0.001(2) 0.004(2) -0.007(2) C(17) 0.028(3) 0.033(4) 0.022(3) 0.007(3) -0.009(3) -0.001(3) C(18) 0.022(3) 0.044(4) 0.031(4) -0.003(3) -0.007(3) -0.004(3) C(19) 0.033(4) 0.033(4) 0.026(3) -0.012(3) 0.005(3) -0.008(3) C(20) 0.034(3) 0.024(3) 0.020(3) -0.005(3) 0.002(3) 0.000(3) C(21) 0.024(3) 0.069(5) 0.044(5) 0.019(4) 0.006(3) -0.001(4) C(22) 0.027(3) 0.043(4) 0.049(5) 0.006(3) 0.000(4) 0.000(4) C(23) 0.017(3) 0.022(3) 0.020(3) -0.001(2) 0.002(2) 0.000(2) C(24) 0.030(3) 0.029(3) 0.017(3) -0.003(3) 0.008(3) -0.003(3) C(25) 0.024(3) 0.025(3) 0.030(4) 0.004(3) 0.007(3) -0.005(3) C(26) 0.023(3) 0.016(3) 0.022(3) 0.000(2) -0.003(2) -0.001(2) C(27) 0.023(3) 0.023(3) 0.026(3) -0.002(2) 0.001(3) -0.002(3) C(28) 0.040(4) 0.024(3) 0.049(5) 0.008(3) 0.005(3) -0.002(3) C(29) 0.046(4) 0.025(4) 0.059(5) 0.015(3) 0.007(4) -0.003(3) C(30) 0.041(4) 0.020(3) 0.055(5) 0.006(3) -0.005(4) 0.006(3) C(31) 0.041(4) 0.022(3) 0.033(4) -0.007(3) 0.007(3) 0.006(3) C(32) 0.039(4) 0.043(4) 0.058(5) -0.019(4) -0.002(4) 0.004(4) C(33) 0.035(4) 0.032(4) 0.049(5) -0.007(3) 0.018(4) 0.009(3) C(34) 0.017(3) 0.025(3) 0.025(3) 0.008(2) -0.003(2) -0.005(2) C(35) 0.034(4) 0.036(4) 0.029(4) 0.015(3) 0.005(3) -0.012(3) C(36) 0.033(4) 0.035(4) 0.031(4) 0.015(3) 0.000(3) -0.002(3) C(37) 0.018(3) 0.026(3) 0.021(3) 0.006(2) 0.004(2) 0.004(2) C(38) 0.016(3) 0.027(3) 0.021(3) 0.002(2) 0.003(2) 0.003(3) C(39) 0.025(3) 0.042(4) 0.037(4) 0.005(3) 0.001(3) 0.008(3) C(40) 0.027(4) 0.050(5) 0.032(4) 0.008(3) -0.004(3) 0.014(3) C(41) 0.024(3) 0.050(4) 0.021(3) -0.003(3) -0.006(3) 0.012(3) C(42) 0.035(4) 0.034(4) 0.020(3) -0.004(3) -0.004(3) 0.003(3) C(43) 0.030(4) 0.040(4) 0.046(5) -0.005(3) 0.016(3) 0.007(3) C(44) 0.025(3) 0.043(4) 0.047(5) 0.002(3) 0.005(3) 0.006(3) C(45) 0.015(3) 0.025(3) 0.029(3) 0.000(2) -0.002(3) -0.006(3) C(46) 0.023(3) 0.023(3) 0.018(3) 0.000(2) -0.003(2) 0.004(2) C(47) 0.023(3) 0.024(3) 0.019(3) 0.000(2) 0.001(2) 0.003(2) C(48) 0.022(3) 0.022(3) 0.015(3) -0.001(2) -0.001(2) 0.001(2) C(49) 0.013(3) 0.031(3) 0.017(3) 0.002(2) -0.005(2) -0.002(2) C(50) 0.021(3) 0.030(3) 0.022(3) -0.001(3) -0.001(3) 0.000(3) C(51) 0.021(3) 0.036(4) 0.029(4) 0.005(3) 0.004(3) -0.008(3) C(52) 0.030(3) 0.026(3) 0.022(3) 0.001(3) -0.003(3) -0.007(3) C(53) 0.026(3) 0.023(3) 0.027(3) 0.003(3) 0.001(3) -0.007(2) C(54) 0.037(4) 0.063(5) 0.044(5) -0.003(4) -0.007(4) -0.012(4) C(55) 0.018(3) 0.086(7) 0.061(6) -0.019(4) 0.001(4) -0.013(5) C(56) 0.017(3) 0.026(3) 0.021(3) 0.003(2) -0.002(2) -0.006(2) C(57) 0.025(3) 0.023(3) 0.023(3) 0.003(3) -0.002(3) -0.001(2) C(58) 0.023(3) 0.027(3) 0.024(3) 0.000(3) -0.008(3) -0.007(3) C(59) 0.013(3) 0.019(3) 0.025(3) -0.001(2) -0.005(2) 0.001(2) C(60) 0.017(3) 0.017(3) 0.022(3) -0.001(2) -0.003(2) -0.005(2) C(61) 0.026(3) 0.033(4) 0.039(4) -0.007(3) -0.006(3) 0.005(3) C(62) 0.032(4) 0.033(4) 0.062(5) -0.012(3) -0.001(4) 0.005(4) C(63) 0.033(4) 0.025(3) 0.046(4) -0.007(3) 0.001(3) 0.006(3) C(64) 0.029(3) 0.020(3) 0.038(4) -0.002(3) 0.000(3) 0.008(3) C(65) 0.045(5) 0.051(5) 0.077(7) 0.027(4) -0.013(5) -0.006(5) C(66) 0.030(4) 0.051(5) 0.054(5) 0.006(3) -0.012(4) 0.005(4) C(67) 0.017(3) 0.028(3) 0.024(3) 0.003(2) 0.004(3) 0.003(3) C(68) 0.036(4) 0.030(3) 0.030(4) -0.015(3) 0.002(3) -0.007(3) C(69) 0.031(4) 0.037(4) 0.031(4) -0.012(3) 0.001(3) -0.003(3) C(70) 0.015(3) 0.029(3) 0.024(3) -0.003(2) 0.004(2) -0.005(3) C(71) 0.020(3) 0.027(3) 0.025(3) -0.002(3) -0.001(3) -0.007(3) C(72) 0.025(3) 0.037(4) 0.032(4) -0.005(3) -0.005(3) -0.007(3) C(73) 0.030(4) 0.045(4) 0.043(4) -0.003(3) -0.006(3) -0.017(4) C(74) 0.027(3) 0.043(4) 0.030(4) 0.007(3) -0.013(3) -0.015(3) C(75) 0.028(3) 0.031(4) 0.031(4) 0.011(3) -0.003(3) -0.005(3) C(76) 0.022(3) 0.031(3) 0.033(4) 0.010(3) -0.002(3) -0.009(3) C(77) 0.018(3) 0.045(4) 0.033(4) 0.008(3) -0.004(3) -0.004(3) C(78) 0.026(3) 0.025(3) 0.024(3) 0.004(3) -0.003(3) -0.001(2) C(79) 0.039(4) 0.022(3) 0.026(3) 0.002(3) 0.001(3) -0.006(3) C(80) 0.034(4) 0.037(4) 0.027(4) 0.008(3) 0.007(3) 0.001(3) C(81) 0.022(3) 0.030(3) 0.017(3) -0.001(3) 0.000(3) 0.000(2) C(82) 0.029(3) 0.030(3) 0.015(3) -0.003(3) -0.002(3) 0.003(2) C(83) 0.027(3) 0.039(4) 0.034(4) 0.008(3) 0.005(3) 0.001(3) C(84) 0.025(3) 0.054(5) 0.033(4) 0.001(3) 0.009(3) 0.004(3) C(85) 0.035(4) 0.038(4) 0.023(3) -0.009(3) -0.004(3) 0.009(3) C(86) 0.029(3) 0.027(3) 0.026(3) 0.000(3) -0.001(3) 0.006(3) C(87) 0.025(3) 0.050(4) 0.026(4) -0.002(3) -0.013(3) 0.007(3) C(88) 0.017(3) 0.060(5) 0.045(5) 0.006(3) -0.003(3) 0.000(4) C(89) 0.020(3) 0.018(3) 0.023(3) 0.001(2) -0.002(2) -0.002(2) C(90) 0.023(3) 0.031(3) 0.018(3) -0.003(3) -0.008(3) -0.003(3) C(91) 0.026(3) 0.025(3) 0.029(3) 0.002(3) -0.006(3) 0.005(3) C(92) 0.018(3) 0.022(3) 0.020(3) -0.004(2) -0.006(2) 0.005(2) C(93) 0.021(3) 0.016(3) 0.022(3) 0.001(2) -0.001(2) -0.003(2) C(94) 0.029(4) 0.028(4) 0.049(5) 0.005(3) -0.015(3) -0.006(3) C(95) 0.032(4) 0.025(3) 0.051(5) 0.008(3) -0.012(4) -0.004(3) C(96) 0.035(4) 0.019(3) 0.053(5) 0.002(3) 0.005(4) -0.009(3) C(97) 0.035(4) 0.026(3) 0.033(4) -0.006(3) 0.003(3) -0.005(3) C(98) 0.051(5) 0.034(4) 0.043(5) -0.017(3) 0.000(4) 0.004(3) C(99) 0.036(4) 0.023(3) 0.040(4) -0.004(3) -0.009(3) -0.005(3) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cu(1) N(1) 2.167(5) . . yes Cu(1) N(3) 2.014(5) . . yes Cu(1) N(8) 2.038(5) . . yes Cu(1) C(10) 2.051(8) . . yes Cu(1) C(11) 2.014(8) . . yes Cu(2) N(2) 2.076(5) . . yes Cu(2) N(4) 2.131(5) . . yes Cu(2) N(6) 2.025(5) . . yes Cu(2) C(21) 2.061(8) . . yes Cu(2) C(22) 2.039(7) . . yes Cu(3) N(5) 2.038(5) . . yes Cu(3) N(7) 2.042(5) . . yes Cu(3) N(9) 2.150(5) . . yes Cu(3) C(32) 2.045(8) . . yes Cu(3) C(33) 2.050(7) . . yes Cu(4) N(10) 2.177(5) . . yes Cu(4) N(12) 2.041(5) . . yes Cu(4) N(17) 2.020(5) . . yes Cu(4) C(43) 2.037(7) . . yes Cu(4) C(44) 2.037(7) . . yes Cu(5) N(11) 2.056(5) . . yes Cu(5) N(13) 2.180(5) . . yes Cu(5) N(15) 2.029(5) . . yes Cu(5) C(54) 2.043(8) . . yes Cu(5) C(55) 2.053(7) . . yes Cu(6) N(14) 2.020(5) . . yes Cu(6) N(16) 2.127(5) . . yes Cu(6) N(18) 2.096(5) . . yes Cu(6) C(65) 2.043(8) . . yes Cu(6) C(66) 2.056(8) . . yes Cu(7) N(19) 2.197(5) . . yes Cu(7) N(21) 2.037(5) . . yes Cu(7) N(26) 2.020(5) . . yes Cu(7) C(76) 2.062(6) . . yes Cu(7) C(77) 2.037(6) . . yes Cu(8) N(20) 2.043(5) . . yes Cu(8) N(22) 2.214(5) . . yes Cu(8) N(24) 2.024(5) . . yes Cu(8) C(87) 2.068(7) . . yes Cu(8) C(88) 2.025(6) . . yes Cu(9) N(23) 2.018(5) . . yes Cu(9) N(25) 2.074(5) . . yes Cu(9) N(27) 2.157(5) . . yes Cu(9) C(98) 2.053(8) . . yes Cu(9) C(99) 2.079(7) . . yes Cl(1) O(1) 1.421(6) . . yes Cl(1) O(2) 1.452(6) . . yes Cl(1) O(3) 1.434(6) . . yes Cl(1) O(4) 1.431(4) . . yes Cl(2) O(5) 1.440(5) . . yes Cl(2) O(6) 1.424(6) . . yes Cl(2) O(7) 1.436(5) . . yes Cl(2) O(8) 1.415(4) . . yes Cl(3) O(9) 1.436(6) . . yes Cl(3) O(10) 1.431(6) . . yes Cl(3) O(11) 1.433(6) . . yes Cl(3) O(12) 1.421(5) . . yes Cl(4) O(13) 1.416(7) . . yes Cl(4) O(14) 1.381(8) . . yes Cl(4) O(15) 1.425(7) . . yes Cl(4) O(16) 1.432(5) . . yes Cl(5) O(17) 1.415(6) . . yes Cl(5) O(18) 1.418(6) . . yes Cl(5) O(19) 1.418(8) . . yes Cl(5) O(20) 1.428(8) . . yes Cl(6) O(21) 1.416(6) . . yes Cl(6) O(22) 1.416(7) . . yes Cl(6) O(23) 1.430(7) . . yes Cl(6) O(24) 1.413(9) . . yes Cl(7) O(25) 1.411(6) . . yes Cl(7) O(26) 1.431(7) . . yes Cl(7) O(27) 1.425(6) . . yes Cl(7) O(28) 1.402(10) . . yes Cl(8) O(29) 1.392(8) . . yes Cl(8) O(30) 1.389(8) . . yes Cl(8) O(31) 1.371(7) . . yes Cl(8) O(32) 1.438(8) . . yes Cl(9) O(33) 1.422(5) . . yes Cl(9) O(34) 1.445(6) . . yes Cl(9) O(35) 1.420(6) . . yes Cl(9) O(36) 1.435(5) . . yes N(1) C(1) 1.342(8) . . yes N(1) C(4) 1.350(7) . . yes N(2) C(1) 1.333(8) . . yes N(2) C(2) 1.350(8) . . yes N(3) C(5) 1.357(8) . . yes N(3) C(9) 1.338(8) . . yes N(4) C(12) 1.327(7) . . yes N(4) C(15) 1.352(7) . . yes N(5) C(12) 1.337(7) . . yes N(5) C(13) 1.340(8) . . yes N(6) C(16) 1.350(7) . . yes N(6) C(20) 1.330(8) . . yes N(7) C(23) 1.321(8) . . yes N(7) C(26) 1.358(8) . . yes N(8) C(23) 1.327(8) . . yes N(8) C(24) 1.349(8) . . yes N(9) C(27) 1.355(8) . . yes N(9) C(31) 1.342(8) . . yes N(10) C(34) 1.329(8) . . yes N(10) C(37) 1.354(7) . . yes N(11) C(34) 1.337(8) . . yes N(11) C(35) 1.356(8) . . yes N(12) C(38) 1.342(8) . . yes N(12) C(42) 1.349(8) . . yes N(13) C(45) 1.326(7) . . yes N(13) C(48) 1.359(7) . . yes N(14) C(45) 1.337(7) . . yes N(14) C(46) 1.366(8) . . yes N(15) C(49) 1.352(8) . . yes N(15) C(53) 1.336(8) . . yes N(16) C(56) 1.329(8) . . yes N(16) C(59) 1.363(7) . . yes N(17) C(56) 1.341(8) . . yes N(17) C(57) 1.338(8) . . yes N(18) C(60) 1.341(8) . . yes N(18) C(64) 1.345(8) . . yes N(19) C(67) 1.340(8) . . yes N(19) C(70) 1.353(7) . . yes N(20) C(67) 1.331(8) . . yes N(20) C(68) 1.346(8) . . yes N(21) C(71) 1.359(8) . . yes N(21) C(75) 1.326(8) . . yes N(22) C(78) 1.323(8) . . yes N(22) C(81) 1.346(7) . . yes N(23) C(78) 1.338(8) . . yes N(23) C(79) 1.353(9) . . yes N(24) C(82) 1.364(8) . . yes N(24) C(86) 1.347(8) . . yes N(25) C(89) 1.309(7) . . yes N(25) C(92) 1.358(7) . . yes N(26) C(89) 1.334(8) . . yes N(26) C(90) 1.347(8) . . yes N(27) C(93) 1.354(8) . . yes N(27) C(97) 1.344(8) . . yes C(1) H(1) 0.951 . . no C(2) C(3) 1.372(9) . . yes C(2) H(2) 0.950 . . no C(3) C(4) 1.391(8) . . yes C(3) H(3) 0.953 . . no C(4) C(5) 1.463(8) . . yes C(5) C(6) 1.387(9) . . yes C(6) C(7) 1.38(1) . . yes C(6) H(4) 0.951 . . no C(7) C(8) 1.36(1) . . yes C(7) H(5) 0.950 . . no C(8) C(9) 1.393(9) . . yes C(8) H(6) 0.950 . . no C(9) H(7) 0.950 . . no C(10) C(11) 1.32(1) . . yes C(10) H(8) 0.950 . . no C(10) H(9) 0.949 . . no C(11) H(10) 0.945 . . no C(11) H(11) 0.951 . . no C(12) H(12) 0.951 . . no C(13) C(14) 1.387(9) . . yes C(13) H(13) 0.951 . . no C(14) C(15) 1.373(8) . . yes C(14) H(14) 0.948 . . no C(15) C(16) 1.481(8) . . yes C(16) C(17) 1.391(8) . . yes C(17) C(18) 1.378(10) . . yes C(17) H(15) 0.952 . . no C(18) C(19) 1.379(10) . . yes C(18) H(16) 0.951 . . no C(19) C(20) 1.370(9) . . yes C(19) H(17) 0.948 . . no C(20) H(18) 0.950 . . no C(21) C(22) 1.30(1) . . yes C(21) H(19) 0.948 . . no C(21) H(20) 0.952 . . no C(22) H(21) 0.953 . . no C(22) H(22) 0.950 . . no C(23) H(23) 0.950 . . no C(24) C(25) 1.362(9) . . yes C(24) H(24) 0.950 . . no C(25) C(26) 1.372(9) . . yes C(25) H(25) 0.951 . . no C(26) C(27) 1.508(8) . . yes C(27) C(28) 1.364(9) . . yes C(28) C(29) 1.36(1) . . yes C(28) H(26) 0.951 . . no C(29) C(30) 1.41(1) . . yes C(29) H(27) 0.956 . . no C(30) C(31) 1.371(10) . . yes C(30) H(28) 0.949 . . no C(31) H(29) 0.951 . . no C(32) C(33) 1.31(1) . . yes C(32) H(30) 0.950 . . no C(32) H(31) 0.951 . . no C(33) H(32) 0.948 . . no C(33) H(33) 0.956 . . no C(34) H(34) 0.949 . . no C(35) C(36) 1.366(10) . . yes C(35) H(35) 0.949 . . no C(36) C(37) 1.365(9) . . yes C(36) H(36) 0.949 . . no C(37) C(38) 1.497(8) . . yes C(38) C(39) 1.380(9) . . yes C(39) C(40) 1.37(1) . . yes C(39) H(37) 0.950 . . no C(40) C(41) 1.377(10) . . yes C(40) H(38) 0.951 . . no C(41) C(42) 1.390(9) . . yes C(41) H(39) 0.951 . . no C(42) H(40) 0.951 . . no C(43) C(44) 1.32(1) . . yes C(43) H(41) 0.954 . . no C(43) H(42) 0.949 . . no C(44) H(43) 0.948 . . no C(44) H(44) 0.955 . . no C(45) H(45) 0.953 . . no C(46) C(47) 1.368(8) . . yes C(46) H(46) 0.950 . . no C(47) C(48) 1.372(8) . . yes C(47) H(47) 0.952 . . no C(48) C(49) 1.489(8) . . yes C(49) C(50) 1.395(8) . . yes C(50) C(51) 1.388(9) . . yes C(50) H(48) 0.949 . . no C(51) C(52) 1.381(9) . . yes C(51) H(49) 0.950 . . no C(52) C(53) 1.393(9) . . yes C(52) H(50) 0.954 . . no C(53) H(51) 0.951 . . no C(54) C(55) 1.28(1) . . yes C(54) H(52) 0.945 . . no C(54) H(53) 0.954 . . no C(55) H(54) 0.951 . . no C(55) H(55) 0.948 . . no C(56) H(56) 0.952 . . no C(57) C(58) 1.374(9) . . yes C(57) H(57) 0.952 . . no C(58) C(59) 1.397(9) . . yes C(58) H(58) 0.953 . . no C(59) C(60) 1.478(8) . . yes C(60) C(61) 1.388(8) . . yes C(61) C(62) 1.36(1) . . yes C(61) H(59) 0.953 . . no C(62) C(63) 1.36(1) . . yes C(62) H(60) 0.950 . . no C(63) C(64) 1.391(9) . . yes C(63) H(61) 0.951 . . no C(64) H(62) 0.952 . . no C(65) C(66) 1.27(1) . . yes C(65) H(63) 0.947 . . no C(65) H(64) 0.956 . . no C(66) H(65) 0.947 . . no C(66) H(66) 0.950 . . no C(67) H(67) 0.952 . . no C(68) C(69) 1.374(10) . . yes C(68) H(68) 0.951 . . no C(69) C(70) 1.375(9) . . yes C(69) H(69) 0.955 . . no C(70) C(71) 1.472(9) . . yes C(71) C(72) 1.391(9) . . yes C(72) C(73) 1.39(1) . . yes C(72) H(70) 0.951 . . no C(73) C(74) 1.39(1) . . yes C(73) H(71) 0.950 . . no C(74) C(75) 1.393(9) . . yes C(74) H(72) 0.954 . . no C(75) H(73) 0.947 . . no C(76) C(77) 1.332(10) . . yes C(76) H(74) 0.951 . . no C(76) H(75) 0.949 . . no C(77) H(76) 0.947 . . no C(77) H(77) 0.950 . . no C(78) H(78) 0.951 . . no C(79) C(80) 1.372(9) . . yes C(79) H(79) 0.951 . . no C(80) C(81) 1.390(9) . . yes C(80) H(80) 0.950 . . no C(81) C(82) 1.486(9) . . yes C(82) C(83) 1.384(9) . . yes C(83) C(84) 1.38(1) . . yes C(83) H(81) 0.951 . . no C(84) C(85) 1.36(1) . . yes C(84) H(82) 0.950 . . no C(85) C(86) 1.386(9) . . yes C(85) H(83) 0.948 . . no C(86) H(84) 0.951 . . no C(87) C(88) 1.32(1) . . yes C(87) H(85) 0.949 . . no C(87) H(86) 0.953 . . no C(88) H(87) 0.949 . . no C(88) H(88) 0.952 . . no C(89) H(89) 0.951 . . no C(90) C(91) 1.360(9) . . yes C(90) H(90) 0.951 . . no C(91) C(92) 1.388(9) . . yes C(91) H(91) 0.949 . . no C(92) C(93) 1.474(8) . . yes C(93) C(94) 1.377(9) . . yes C(94) C(95) 1.377(10) . . yes C(94) H(92) 0.950 . . no C(95) C(96) 1.38(1) . . yes C(95) H(93) 0.949 . . no C(96) C(97) 1.391(9) . . yes C(96) H(94) 0.948 . . no C(97) H(95) 0.952 . . no C(98) C(99) 1.34(1) . . yes C(98) H(96) 0.949 . . no C(98) H(97) 0.953 . . no C(99) H(98) 0.950 . . no C(99) H(99) 0.953 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(3) 79.2(2) . . . yes N(1) Cu(1) N(8) 94.7(2) . . . yes N(1) Cu(1) C(10) 111.8(3) . . . yes N(1) Cu(1) C(11) 115.1(3) . . . yes N(3) Cu(1) N(8) 100.2(2) . . . yes N(3) Cu(1) C(10) 110.1(3) . . . yes N(3) Cu(1) C(11) 147.1(3) . . . yes N(8) Cu(1) C(10) 142.5(3) . . . yes N(8) Cu(1) C(11) 107.5(3) . . . yes C(10) Cu(1) C(11) 37.7(3) . . . yes N(2) Cu(2) N(4) 96.7(2) . . . yes N(2) Cu(2) N(6) 102.6(2) . . . yes N(2) Cu(2) C(21) 136.4(3) . . . yes N(2) Cu(2) C(22) 110.7(3) . . . yes N(4) Cu(2) N(6) 80.4(2) . . . yes N(4) Cu(2) C(21) 117.6(3) . . . yes N(4) Cu(2) C(22) 106.5(2) . . . yes N(6) Cu(2) C(21) 108.5(3) . . . yes N(6) Cu(2) C(22) 144.5(3) . . . yes C(21) Cu(2) C(22) 37.0(3) . . . yes N(5) Cu(3) N(7) 98.2(2) . . . yes N(5) Cu(3) N(9) 102.2(2) . . . yes N(5) Cu(3) C(32) 145.4(3) . . . yes N(5) Cu(3) C(33) 111.4(3) . . . yes N(7) Cu(3) N(9) 79.3(2) . . . yes N(7) Cu(3) C(32) 106.0(3) . . . yes N(7) Cu(3) C(33) 141.4(3) . . . yes N(9) Cu(3) C(32) 106.3(3) . . . yes N(9) Cu(3) C(33) 116.1(2) . . . yes C(32) Cu(3) C(33) 37.3(3) . . . yes N(10) Cu(4) N(12) 78.0(2) . . . yes N(10) Cu(4) N(17) 97.7(2) . . . yes N(10) Cu(4) C(43) 103.7(2) . . . yes N(10) Cu(4) C(44) 116.6(3) . . . yes N(12) Cu(4) N(17) 101.6(2) . . . yes N(12) Cu(4) C(43) 108.0(3) . . . yes N(12) Cu(4) C(44) 143.3(3) . . . yes N(17) Cu(4) C(43) 146.3(2) . . . yes N(17) Cu(4) C(44) 108.9(3) . . . yes C(43) Cu(4) C(44) 37.9(3) . . . yes N(11) Cu(5) N(13) 98.6(2) . . . yes N(11) Cu(5) N(15) 101.0(2) . . . yes N(11) Cu(5) C(54) 138.5(3) . . . yes N(11) Cu(5) C(55) 107.1(3) . . . yes N(13) Cu(5) N(15) 79.0(2) . . . yes N(13) Cu(5) C(54) 113.0(3) . . . yes N(13) Cu(5) C(55) 113.3(3) . . . yes N(15) Cu(5) C(54) 110.6(3) . . . yes N(15) Cu(5) C(55) 146.7(3) . . . yes C(54) Cu(5) C(55) 36.3(4) . . . yes N(14) Cu(6) N(16) 98.4(2) . . . yes N(14) Cu(6) N(18) 103.3(2) . . . yes N(14) Cu(6) C(65) 148.4(3) . . . yes N(14) Cu(6) C(66) 112.2(3) . . . yes N(16) Cu(6) N(18) 78.3(2) . . . yes N(16) Cu(6) C(65) 104.7(3) . . . yes N(16) Cu(6) C(66) 127.2(3) . . . yes N(18) Cu(6) C(65) 102.3(3) . . . yes N(18) Cu(6) C(66) 130.0(3) . . . yes C(65) Cu(6) C(66) 36.2(3) . . . yes N(19) Cu(7) N(21) 77.8(2) . . . yes N(19) Cu(7) N(26) 99.5(2) . . . yes N(19) Cu(7) C(76) 105.2(2) . . . yes N(19) Cu(7) C(77) 115.5(2) . . . yes N(21) Cu(7) N(26) 104.1(2) . . . yes N(21) Cu(7) C(76) 110.0(2) . . . yes N(21) Cu(7) C(77) 146.0(2) . . . yes N(26) Cu(7) C(76) 141.2(2) . . . yes N(26) Cu(7) C(77) 104.1(2) . . . yes C(76) Cu(7) C(77) 37.9(3) . . . yes N(20) Cu(8) N(22) 99.2(2) . . . yes N(20) Cu(8) N(24) 102.3(2) . . . yes N(20) Cu(8) C(87) 140.3(2) . . . yes N(20) Cu(8) C(88) 105.6(3) . . . yes N(22) Cu(8) N(24) 78.0(2) . . . yes N(22) Cu(8) C(87) 108.4(2) . . . yes N(22) Cu(8) C(88) 111.6(2) . . . yes N(24) Cu(8) C(87) 110.8(2) . . . yes N(24) Cu(8) C(88) 148.2(3) . . . yes C(87) Cu(8) C(88) 37.7(3) . . . yes N(23) Cu(9) N(25) 104.4(2) . . . yes N(23) Cu(9) N(27) 105.2(2) . . . yes N(23) Cu(9) C(98) 143.8(3) . . . yes N(23) Cu(9) C(99) 110.0(3) . . . yes N(25) Cu(9) N(27) 78.6(2) . . . yes N(25) Cu(9) C(98) 99.2(3) . . . yes N(25) Cu(9) C(99) 135.2(2) . . . yes N(27) Cu(9) C(98) 106.1(2) . . . yes N(27) Cu(9) C(99) 117.5(2) . . . yes C(98) Cu(9) C(99) 37.7(3) . . . yes O(1) Cl(1) O(2) 108.0(4) . . . yes O(1) Cl(1) O(3) 110.9(4) . . . yes O(1) Cl(1) O(4) 109.8(3) . . . yes O(2) Cl(1) O(3) 108.9(4) . . . yes O(2) Cl(1) O(4) 109.6(3) . . . yes O(3) Cl(1) O(4) 109.5(3) . . . yes O(5) Cl(2) O(6) 110.1(3) . . . yes O(5) Cl(2) O(7) 108.1(3) . . . yes O(5) Cl(2) O(8) 110.3(3) . . . yes O(6) Cl(2) O(7) 109.2(3) . . . yes O(6) Cl(2) O(8) 109.4(3) . . . yes O(7) Cl(2) O(8) 109.6(3) . . . yes O(9) Cl(3) O(10) 110.8(4) . . . yes O(9) Cl(3) O(11) 108.8(4) . . . yes O(9) Cl(3) O(12) 109.8(3) . . . yes O(10) Cl(3) O(11) 108.2(4) . . . yes O(10) Cl(3) O(12) 108.9(3) . . . yes O(11) Cl(3) O(12) 110.4(3) . . . yes O(13) Cl(4) O(14) 111.2(5) . . . yes O(13) Cl(4) O(15) 106.7(4) . . . yes O(13) Cl(4) O(16) 110.8(4) . . . yes O(14) Cl(4) O(15) 108.9(5) . . . yes O(14) Cl(4) O(16) 110.5(4) . . . yes O(15) Cl(4) O(16) 108.7(3) . . . yes O(17) Cl(5) O(18) 109.7(4) . . . yes O(17) Cl(5) O(19) 109.0(5) . . . yes O(17) Cl(5) O(20) 108.7(5) . . . yes O(18) Cl(5) O(19) 112.9(4) . . . yes O(18) Cl(5) O(20) 108.8(5) . . . yes O(19) Cl(5) O(20) 107.6(5) . . . yes O(21) Cl(6) O(22) 111.2(4) . . . yes O(21) Cl(6) O(23) 106.1(4) . . . yes O(21) Cl(6) O(24) 109.5(5) . . . yes O(22) Cl(6) O(23) 109.5(4) . . . yes O(22) Cl(6) O(24) 110.0(5) . . . yes O(23) Cl(6) O(24) 110.5(6) . . . yes O(25) Cl(7) O(26) 111.6(4) . . . yes O(25) Cl(7) O(27) 109.9(4) . . . yes O(25) Cl(7) O(28) 107.7(4) . . . yes O(26) Cl(7) O(27) 108.1(4) . . . yes O(26) Cl(7) O(28) 109.5(5) . . . yes O(27) Cl(7) O(28) 110.0(5) . . . yes O(29) Cl(8) O(30) 113.5(5) . . . yes O(29) Cl(8) O(31) 110.5(5) . . . yes O(29) Cl(8) O(32) 104.8(6) . . . yes O(30) Cl(8) O(31) 112.9(5) . . . yes O(30) Cl(8) O(32) 105.5(5) . . . yes O(31) Cl(8) O(32) 109.1(6) . . . yes O(33) Cl(9) O(34) 109.9(3) . . . yes O(33) Cl(9) O(35) 110.1(3) . . . yes O(33) Cl(9) O(36) 109.5(3) . . . yes O(34) Cl(9) O(35) 108.8(3) . . . yes O(34) Cl(9) O(36) 109.6(3) . . . yes O(35) Cl(9) O(36) 108.9(4) . . . yes Cu(1) N(1) C(1) 130.7(4) . . . yes Cu(1) N(1) C(4) 111.1(4) . . . yes C(1) N(1) C(4) 117.4(5) . . . yes Cu(2) N(2) C(1) 122.4(4) . . . yes Cu(2) N(2) C(2) 121.4(4) . . . yes C(1) N(2) C(2) 114.9(5) . . . yes Cu(1) N(3) C(5) 116.5(4) . . . yes Cu(1) N(3) C(9) 124.5(4) . . . yes C(5) N(3) C(9) 118.8(5) . . . yes Cu(2) N(4) C(12) 129.0(4) . . . yes Cu(2) N(4) C(15) 112.1(4) . . . yes C(12) N(4) C(15) 118.5(5) . . . yes Cu(3) N(5) C(12) 119.6(4) . . . yes Cu(3) N(5) C(13) 121.8(4) . . . yes C(12) N(5) C(13) 116.8(5) . . . yes Cu(2) N(6) C(16) 114.6(4) . . . yes Cu(2) N(6) C(20) 126.6(4) . . . yes C(16) N(6) C(20) 118.8(5) . . . yes Cu(3) N(7) C(23) 126.2(4) . . . yes Cu(3) N(7) C(26) 116.2(4) . . . yes C(23) N(7) C(26) 117.4(5) . . . yes Cu(1) N(8) C(23) 121.5(4) . . . yes Cu(1) N(8) C(24) 123.4(4) . . . yes C(23) N(8) C(24) 114.7(5) . . . yes Cu(3) N(9) C(27) 113.3(4) . . . yes Cu(3) N(9) C(31) 129.1(4) . . . yes C(27) N(9) C(31) 117.6(5) . . . yes Cu(4) N(10) C(34) 129.5(4) . . . yes Cu(4) N(10) C(37) 113.0(4) . . . yes C(34) N(10) C(37) 117.3(5) . . . yes Cu(5) N(11) C(34) 119.9(4) . . . yes Cu(5) N(11) C(35) 123.8(4) . . . yes C(34) N(11) C(35) 115.4(5) . . . yes Cu(4) N(12) C(38) 118.0(4) . . . yes Cu(4) N(12) C(42) 123.9(4) . . . yes C(38) N(12) C(42) 117.8(5) . . . yes Cu(5) N(13) C(45) 129.2(4) . . . yes Cu(5) N(13) C(48) 112.1(4) . . . yes C(45) N(13) C(48) 118.2(5) . . . yes Cu(6) N(14) C(45) 121.0(4) . . . yes Cu(6) N(14) C(46) 121.2(4) . . . yes C(45) N(14) C(46) 116.8(5) . . . yes Cu(5) N(15) C(49) 116.7(4) . . . yes Cu(5) N(15) C(53) 124.8(4) . . . yes C(49) N(15) C(53) 118.6(5) . . . yes Cu(6) N(16) C(56) 128.6(4) . . . yes Cu(6) N(16) C(59) 113.4(4) . . . yes C(56) N(16) C(59) 117.5(5) . . . yes Cu(4) N(17) C(56) 121.3(4) . . . yes Cu(4) N(17) C(57) 122.4(4) . . . yes C(56) N(17) C(57) 115.4(5) . . . yes Cu(6) N(18) C(60) 115.9(4) . . . yes Cu(6) N(18) C(64) 126.2(4) . . . yes C(60) N(18) C(64) 117.9(5) . . . yes Cu(7) N(19) C(67) 130.6(4) . . . yes Cu(7) N(19) C(70) 112.5(4) . . . yes C(67) N(19) C(70) 116.9(5) . . . yes Cu(8) N(20) C(67) 121.2(4) . . . yes Cu(8) N(20) C(68) 121.7(4) . . . yes C(67) N(20) C(68) 116.1(5) . . . yes Cu(7) N(21) C(71) 117.4(4) . . . yes Cu(7) N(21) C(75) 124.2(4) . . . yes C(71) N(21) C(75) 118.1(5) . . . yes Cu(8) N(22) C(78) 129.9(4) . . . yes Cu(8) N(22) C(81) 112.4(4) . . . yes C(78) N(22) C(81) 117.6(5) . . . yes Cu(9) N(23) C(78) 119.2(4) . . . yes Cu(9) N(23) C(79) 123.5(4) . . . yes C(78) N(23) C(79) 115.7(5) . . . yes Cu(8) N(24) C(82) 117.6(4) . . . yes Cu(8) N(24) C(86) 123.3(4) . . . yes C(82) N(24) C(86) 118.8(5) . . . yes Cu(9) N(25) C(89) 126.1(4) . . . yes Cu(9) N(25) C(92) 115.1(4) . . . yes C(89) N(25) C(92) 118.8(5) . . . yes Cu(7) N(26) C(89) 121.4(4) . . . yes Cu(7) N(26) C(90) 122.4(4) . . . yes C(89) N(26) C(90) 115.3(5) . . . yes Cu(9) N(27) C(93) 113.4(4) . . . yes Cu(9) N(27) C(97) 129.0(4) . . . yes C(93) N(27) C(97) 117.5(5) . . . yes N(1) C(1) N(2) 126.9(5) . . . yes N(1) C(1) H(1) 116.6 . . . no N(2) C(1) H(1) 116.5 . . . no N(2) C(2) C(3) 122.8(6) . . . yes N(2) C(2) H(2) 118.4 . . . no C(3) C(2) H(2) 118.8 . . . no C(2) C(3) C(4) 118.3(5) . . . yes C(2) C(3) H(3) 120.7 . . . no C(4) C(3) H(3) 121.0 . . . no N(1) C(4) C(3) 119.6(5) . . . yes N(1) C(4) C(5) 116.9(5) . . . yes C(3) C(4) C(5) 123.5(5) . . . yes N(3) C(5) C(4) 115.9(5) . . . yes N(3) C(5) C(6) 120.5(6) . . . yes C(4) C(5) C(6) 123.5(6) . . . yes C(5) C(6) C(7) 119.3(6) . . . yes C(5) C(6) H(4) 120.3 . . . no C(7) C(6) H(4) 120.4 . . . no C(6) C(7) C(8) 120.8(6) . . . yes C(6) C(7) H(5) 119.7 . . . no C(8) C(7) H(5) 119.6 . . . no C(7) C(8) C(9) 117.4(6) . . . yes C(7) C(8) H(6) 121.3 . . . no C(9) C(8) H(6) 121.4 . . . no N(3) C(9) C(8) 123.1(6) . . . yes N(3) C(9) H(7) 118.5 . . . no C(8) C(9) H(7) 118.4 . . . no Cu(1) C(10) C(11) 69.6(5) . . . yes Cu(1) C(10) H(8) 99.3 . . . no Cu(1) C(10) H(9) 99.8 . . . no C(11) C(10) H(8) 120.1 . . . no C(11) C(10) H(9) 119.8 . . . no H(8) C(10) H(9) 120.1 . . . no Cu(1) C(11) C(10) 72.7(5) . . . yes Cu(1) C(11) H(10) 99.5 . . . no Cu(1) C(11) H(11) 98.8 . . . no C(10) C(11) H(10) 120.0 . . . no C(10) C(11) H(11) 119.5 . . . no H(10) C(11) H(11) 120.4 . . . no N(4) C(12) N(5) 124.9(5) . . . yes N(4) C(12) H(12) 117.8 . . . no N(5) C(12) H(12) 117.3 . . . no N(5) C(13) C(14) 121.5(5) . . . yes N(5) C(13) H(13) 119.3 . . . no C(14) C(13) H(13) 119.1 . . . no C(13) C(14) C(15) 118.2(5) . . . yes C(13) C(14) H(14) 121.1 . . . no C(15) C(14) H(14) 120.6 . . . no N(4) C(15) C(14) 119.9(5) . . . yes N(4) C(15) C(16) 115.3(5) . . . yes C(14) C(15) C(16) 124.7(5) . . . yes N(6) C(16) C(15) 117.3(5) . . . yes N(6) C(16) C(17) 120.6(5) . . . yes C(15) C(16) C(17) 122.1(5) . . . yes C(16) C(17) C(18) 119.9(6) . . . yes C(16) C(17) H(15) 120.0 . . . no C(18) C(17) H(15) 120.0 . . . no C(17) C(18) C(19) 118.5(6) . . . yes C(17) C(18) H(16) 120.7 . . . no C(19) C(18) H(16) 120.8 . . . no C(18) C(19) C(20) 119.0(6) . . . yes C(18) C(19) H(17) 120.5 . . . no C(20) C(19) H(17) 120.5 . . . no N(6) C(20) C(19) 123.1(6) . . . yes N(6) C(20) H(18) 118.6 . . . no C(19) C(20) H(18) 118.2 . . . no Cu(2) C(21) C(22) 70.6(5) . . . yes Cu(2) C(21) H(19) 99.4 . . . no Cu(2) C(21) H(20) 99.9 . . . no C(22) C(21) H(19) 120.1 . . . no C(22) C(21) H(20) 120.0 . . . no H(19) C(21) H(20) 120.0 . . . no Cu(2) C(22) C(21) 72.4(4) . . . yes Cu(2) C(22) H(21) 99.0 . . . no Cu(2) C(22) H(22) 98.4 . . . no C(21) C(22) H(21) 120.1 . . . no C(21) C(22) H(22) 120.2 . . . no H(21) C(22) H(22) 119.7 . . . no N(7) C(23) N(8) 126.6(5) . . . yes N(7) C(23) H(23) 116.6 . . . no N(8) C(23) H(23) 116.8 . . . no N(8) C(24) C(25) 123.6(6) . . . yes N(8) C(24) H(24) 118.2 . . . no C(25) C(24) H(24) 118.2 . . . no C(24) C(25) C(26) 117.3(6) . . . yes C(24) C(25) H(25) 121.2 . . . no C(26) C(25) H(25) 121.5 . . . no N(7) C(26) C(25) 120.4(5) . . . yes N(7) C(26) C(27) 115.9(5) . . . yes C(25) C(26) C(27) 123.7(5) . . . yes N(9) C(27) C(26) 115.0(5) . . . yes N(9) C(27) C(28) 122.5(6) . . . yes C(26) C(27) C(28) 122.4(6) . . . yes C(27) C(28) C(29) 120.3(7) . . . yes C(27) C(28) H(26) 119.7 . . . no C(29) C(28) H(26) 120.1 . . . no C(28) C(29) C(30) 118.1(7) . . . yes C(28) C(29) H(27) 120.7 . . . no C(30) C(29) H(27) 121.1 . . . no C(29) C(30) C(31) 118.7(7) . . . yes C(29) C(30) H(28) 120.6 . . . no C(31) C(30) H(28) 120.7 . . . no N(9) C(31) C(30) 122.7(6) . . . yes N(9) C(31) H(29) 118.4 . . . no C(30) C(31) H(29) 118.9 . . . no Cu(3) C(32) C(33) 71.6(5) . . . yes Cu(3) C(32) H(30) 98.8 . . . no Cu(3) C(32) H(31) 99.4 . . . no C(33) C(32) H(30) 120.3 . . . no C(33) C(32) H(31) 119.8 . . . no H(30) C(32) H(31) 119.9 . . . no Cu(3) C(33) C(32) 71.2(5) . . . yes Cu(3) C(33) H(32) 99.7 . . . no Cu(3) C(33) H(33) 98.8 . . . no C(32) C(33) H(32) 120.6 . . . no C(32) C(33) H(33) 119.8 . . . no H(32) C(33) H(33) 119.5 . . . no N(10) C(34) N(11) 126.1(5) . . . yes N(10) C(34) H(34) 117.1 . . . no N(11) C(34) H(34) 116.8 . . . no N(11) C(35) C(36) 121.7(6) . . . yes N(11) C(35) H(35) 119.4 . . . no C(36) C(35) H(35) 118.9 . . . no C(35) C(36) C(37) 119.0(6) . . . yes C(35) C(36) H(36) 120.7 . . . no C(37) C(36) H(36) 120.3 . . . no N(10) C(37) C(36) 120.1(6) . . . yes N(10) C(37) C(38) 115.4(5) . . . yes C(36) C(37) C(38) 124.5(5) . . . yes N(12) C(38) C(37) 115.5(5) . . . yes N(12) C(38) C(39) 122.3(6) . . . yes C(37) C(38) C(39) 122.0(6) . . . yes C(38) C(39) C(40) 119.3(6) . . . yes C(38) C(39) H(37) 120.3 . . . no C(40) C(39) H(37) 120.4 . . . no C(39) C(40) C(41) 119.8(6) . . . yes C(39) C(40) H(38) 120.1 . . . no C(41) C(40) H(38) 120.2 . . . no C(40) C(41) C(42) 118.1(6) . . . yes C(40) C(41) H(39) 121.0 . . . no C(42) C(41) H(39) 121.0 . . . no N(12) C(42) C(41) 122.6(6) . . . yes N(12) C(42) H(40) 118.7 . . . no C(41) C(42) H(40) 118.7 . . . no Cu(4) C(43) C(44) 71.0(4) . . . yes Cu(4) C(43) H(41) 99.2 . . . no Cu(4) C(43) H(42) 99.9 . . . no C(44) C(43) H(41) 120.1 . . . no C(44) C(43) H(42) 120.2 . . . no H(41) C(43) H(42) 119.7 . . . no Cu(4) C(44) C(43) 71.0(4) . . . yes Cu(4) C(44) H(43) 99.5 . . . no Cu(4) C(44) H(44) 98.8 . . . no C(43) C(44) H(43) 120.3 . . . no C(43) C(44) H(44) 120.0 . . . no H(43) C(44) H(44) 119.7 . . . no N(13) C(45) N(14) 124.9(5) . . . yes N(13) C(45) H(45) 117.5 . . . no N(14) C(45) H(45) 117.6 . . . no N(14) C(46) C(47) 121.0(5) . . . yes N(14) C(46) H(46) 119.6 . . . no C(47) C(46) H(46) 119.4 . . . no C(46) C(47) C(48) 119.0(5) . . . yes C(46) C(47) H(47) 120.5 . . . no C(48) C(47) H(47) 120.5 . . . no N(13) C(48) C(47) 120.0(5) . . . yes N(13) C(48) C(49) 115.4(5) . . . yes C(47) C(48) C(49) 124.6(5) . . . yes N(15) C(49) C(48) 116.7(5) . . . yes N(15) C(49) C(50) 121.5(5) . . . yes C(48) C(49) C(50) 121.7(5) . . . yes C(49) C(50) C(51) 118.9(6) . . . yes C(49) C(50) H(48) 120.5 . . . no C(51) C(50) H(48) 120.6 . . . no C(50) C(51) C(52) 119.9(6) . . . yes C(50) C(51) H(49) 120.1 . . . no C(52) C(51) H(49) 120.0 . . . no C(51) C(52) C(53) 117.6(6) . . . yes C(51) C(52) H(50) 121.2 . . . no C(53) C(52) H(50) 121.2 . . . no N(15) C(53) C(52) 123.5(6) . . . yes N(15) C(53) H(51) 118.3 . . . no C(52) C(53) H(51) 118.3 . . . no Cu(5) C(54) C(55) 72.2(5) . . . yes Cu(5) C(54) H(52) 98.8 . . . no Cu(5) C(54) H(53) 98.8 . . . no C(55) C(54) H(52) 120.3 . . . no C(55) C(54) H(53) 119.6 . . . no H(52) C(54) H(53) 120.1 . . . no Cu(5) C(55) C(54) 71.4(5) . . . yes Cu(5) C(55) H(54) 99.3 . . . no Cu(5) C(55) H(55) 99.0 . . . no C(54) C(55) H(54) 120.1 . . . no C(54) C(55) H(55) 119.8 . . . no H(54) C(55) H(55) 120.1 . . . no N(16) C(56) N(17) 126.7(5) . . . yes N(16) C(56) H(56) 116.7 . . . no N(17) C(56) H(56) 116.6 . . . no N(17) C(57) C(58) 122.8(6) . . . yes N(17) C(57) H(57) 118.6 . . . no C(58) C(57) H(57) 118.6 . . . no C(57) C(58) C(59) 118.4(5) . . . yes C(57) C(58) H(58) 120.8 . . . no C(59) C(58) H(58) 120.8 . . . no N(16) C(59) C(58) 119.2(5) . . . yes N(16) C(59) C(60) 116.4(5) . . . yes C(58) C(59) C(60) 124.3(5) . . . yes N(18) C(60) C(59) 115.6(5) . . . yes N(18) C(60) C(61) 122.2(6) . . . yes C(59) C(60) C(61) 122.3(6) . . . yes C(60) C(61) C(62) 119.5(7) . . . yes C(60) C(61) H(59) 120.0 . . . no C(62) C(61) H(59) 120.6 . . . no C(61) C(62) C(63) 119.0(7) . . . yes C(61) C(62) H(60) 120.2 . . . no C(63) C(62) H(60) 120.7 . . . no C(62) C(63) C(64) 119.7(7) . . . yes C(62) C(63) H(61) 119.8 . . . no C(64) C(63) H(61) 120.5 . . . no N(18) C(64) C(63) 121.7(6) . . . yes N(18) C(64) H(62) 119.1 . . . no C(63) C(64) H(62) 119.2 . . . no Cu(6) C(65) C(66) 72.4(5) . . . yes Cu(6) C(65) H(63) 98.3 . . . no Cu(6) C(65) H(64) 98.7 . . . no C(66) C(65) H(63) 120.6 . . . no C(66) C(65) H(64) 119.7 . . . no H(63) C(65) H(64) 119.7 . . . no Cu(6) C(66) C(65) 71.3(5) . . . yes Cu(6) C(66) H(65) 99.3 . . . no Cu(6) C(66) H(66) 98.5 . . . no C(65) C(66) H(65) 120.2 . . . no C(65) C(66) H(66) 119.5 . . . no H(65) C(66) H(66) 120.3 . . . no N(19) C(67) N(20) 126.3(5) . . . yes N(19) C(67) H(67) 117.1 . . . no N(20) C(67) H(67) 116.6 . . . no N(20) C(68) C(69) 121.2(6) . . . yes N(20) C(68) H(68) 119.1 . . . no C(69) C(68) H(68) 119.7 . . . no C(68) C(69) C(70) 119.2(6) . . . yes C(68) C(69) H(69) 120.5 . . . no C(70) C(69) H(69) 120.3 . . . no N(19) C(70) C(69) 119.8(6) . . . yes N(19) C(70) C(71) 115.6(5) . . . yes C(69) C(70) C(71) 124.5(5) . . . yes N(21) C(71) C(70) 116.3(5) . . . yes N(21) C(71) C(72) 121.6(6) . . . yes C(70) C(71) C(72) 121.9(6) . . . yes C(71) C(72) C(73) 119.1(6) . . . yes C(71) C(72) H(70) 120.5 . . . no C(73) C(72) H(70) 120.4 . . . no C(72) C(73) C(74) 119.6(6) . . . yes C(72) C(73) H(71) 120.5 . . . no C(74) C(73) H(71) 119.9 . . . no C(73) C(74) C(75) 117.2(6) . . . yes C(73) C(74) H(72) 121.6 . . . no C(75) C(74) H(72) 121.1 . . . no N(21) C(75) C(74) 124.2(6) . . . yes N(21) C(75) H(73) 117.8 . . . no C(74) C(75) H(73) 118.0 . . . no Cu(7) C(76) C(77) 70.0(4) . . . yes Cu(7) C(76) H(74) 99.6 . . . no Cu(7) C(76) H(75) 100.1 . . . no C(77) C(76) H(74) 120.0 . . . no C(77) C(76) H(75) 120.0 . . . no H(74) C(76) H(75) 120.0 . . . no Cu(7) C(77) C(76) 72.1(4) . . . yes Cu(7) C(77) H(76) 99.0 . . . no Cu(7) C(77) H(77) 98.4 . . . no C(76) C(77) H(76) 119.9 . . . no C(76) C(77) H(77) 119.8 . . . no H(76) C(77) H(77) 120.3 . . . no N(22) C(78) N(23) 126.0(5) . . . yes N(22) C(78) H(78) 117.2 . . . no N(23) C(78) H(78) 116.9 . . . no N(23) C(79) C(80) 122.4(6) . . . yes N(23) C(79) H(79) 118.9 . . . no C(80) C(79) H(79) 118.7 . . . no C(79) C(80) C(81) 117.2(6) . . . yes C(79) C(80) H(80) 121.3 . . . no C(81) C(80) H(80) 121.4 . . . no N(22) C(81) C(80) 120.7(6) . . . yes N(22) C(81) C(82) 115.6(5) . . . yes C(80) C(81) C(82) 123.5(6) . . . yes N(24) C(82) C(81) 116.3(5) . . . yes N(24) C(82) C(83) 121.0(6) . . . yes C(81) C(82) C(83) 122.4(6) . . . yes C(82) C(83) C(84) 119.4(6) . . . yes C(82) C(83) H(81) 120.4 . . . no C(84) C(83) H(81) 120.3 . . . no C(83) C(84) C(85) 119.4(6) . . . yes C(83) C(84) H(82) 120.4 . . . no C(85) C(84) H(82) 120.2 . . . no C(84) C(85) C(86) 119.8(6) . . . yes C(84) C(85) H(83) 120.3 . . . no C(86) C(85) H(83) 120.0 . . . no N(24) C(86) C(85) 121.6(6) . . . yes N(24) C(86) H(84) 119.4 . . . no C(85) C(86) H(84) 119.0 . . . no Cu(8) C(87) C(88) 69.4(4) . . . yes Cu(8) C(87) H(85) 100.1 . . . no Cu(8) C(87) H(86) 100.0 . . . no C(88) C(87) H(85) 120.4 . . . no C(88) C(87) H(86) 119.9 . . . no H(85) C(87) H(86) 119.7 . . . no Cu(8) C(88) C(87) 72.9(4) . . . yes Cu(8) C(88) H(87) 98.5 . . . no Cu(8) C(88) H(88) 98.4 . . . no C(87) C(88) H(87) 120.3 . . . no C(87) C(88) H(88) 119.8 . . . no H(87) C(88) H(88) 119.9 . . . no N(25) C(89) N(26) 126.0(5) . . . yes N(25) C(89) H(89) 117.0 . . . no N(26) C(89) H(89) 117.0 . . . no N(26) C(90) C(91) 122.6(6) . . . yes N(26) C(90) H(90) 118.9 . . . no C(91) C(90) H(90) 118.5 . . . no C(90) C(91) C(92) 118.5(6) . . . yes C(90) C(91) H(91) 120.8 . . . no C(92) C(91) H(91) 120.6 . . . no N(25) C(92) C(91) 118.4(5) . . . yes N(25) C(92) C(93) 117.3(5) . . . yes C(91) C(92) C(93) 124.3(5) . . . yes N(27) C(93) C(92) 115.5(5) . . . yes N(27) C(93) C(94) 122.3(5) . . . yes C(92) C(93) C(94) 122.2(6) . . . yes C(93) C(94) C(95) 119.6(7) . . . yes C(93) C(94) H(92) 120.3 . . . no C(95) C(94) H(92) 120.1 . . . no C(94) C(95) C(96) 119.1(6) . . . yes C(94) C(95) H(93) 120.3 . . . no C(96) C(95) H(93) 120.6 . . . no C(95) C(96) C(97) 118.4(6) . . . yes C(95) C(96) H(94) 120.4 . . . no C(97) C(96) H(94) 121.2 . . . no N(27) C(97) C(96) 123.0(6) . . . yes N(27) C(97) H(95) 118.5 . . . no C(96) C(97) H(95) 118.5 . . . no Cu(9) C(98) C(99) 72.2(4) . . . yes Cu(9) C(98) H(96) 99.5 . . . no Cu(9) C(98) H(97) 98.7 . . . no C(99) C(98) H(96) 120.3 . . . no C(99) C(98) H(97) 119.8 . . . no H(96) C(98) H(97) 119.8 . . . no Cu(9) C(99) C(98) 70.1(4) . . . yes Cu(9) C(99) H(98) 99.4 . . . no Cu(9) C(99) H(99) 99.9 . . . no C(98) C(99) H(98) 120.4 . . . no C(98) C(99) H(99) 119.9 . . . no H(98) C(99) H(99) 119.7 . . . 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 Cu(3) O(2) 3.552(6) . 4_565 ? Cu(4) O(28) 3.336(9) . 2_664 ? Cu(8) O(35) 3.514(6) . 4_555 ? O(1) C(11) 3.09(1) . 4_465 ? O(1) C(23) 3.266(8) . 4_465 ? O(2) C(33) 3.181(10) . 4_465 ? O(2) C(12) 3.391(8) . 4_465 ? O(2) C(32) 3.41(1) . 4_465 ? O(3) C(22) 3.202(10) . 4_465 ? O(3) C(1) 3.287(8) . 4_465 ? O(5) C(89) 3.352(8) . 1_455 ? O(5) C(77) 3.432(9) . 1_455 ? O(6) C(99) 3.204(9) . 1_455 ? O(6) C(78) 3.313(8) . 1_455 ? O(6) C(98) 3.480(9) . 1_455 ? O(7) C(67) 3.339(8) . 1_455 ? O(7) C(88) 3.425(10) . 1_455 ? O(13) C(75) 3.260(10) . 2_765 ? O(13) C(28) 3.41(1) . 4_565 ? O(14) C(51) 3.22(1) . 1_655 ? O(14) C(52) 3.300(10) . 1_655 ? O(14) C(41) 3.38(1) . 2_665 ? O(14) C(40) 3.44(1) . 2_665 ? O(15) C(29) 3.30(1) . 4_565 ? O(15) C(28) 3.413(10) . 4_565 ? O(16) C(76) 3.293(9) . 2_765 ? O(16) C(77) 3.358(9) . 2_765 ? O(16) C(41) 3.391(9) . 2_665 ? O(17) C(39) 3.427(10) . 1_655 ? O(17) C(30) 3.47(1) . 4_565 ? O(17) C(81) 3.48(1) . 2_764 ? O(18) C(40) 3.400(9) . 1_655 ? O(18) C(51) 3.477(9) . 2_664 ? O(18) C(39) 3.489(9) . 1_655 ? O(19) C(50) 3.389(10) . 2_664 ? O(19) C(87) 3.40(1) . 2_764 ? O(19) N(22) 3.445(9) . 2_764 ? O(21) C(48) 3.315(9) . 2_664 ? O(21) C(49) 3.447(9) . 2_664 ? O(22) C(54) 3.46(1) . 2_664 ? O(22) C(83) 3.527(9) . 2_664 ? O(23) C(84) 3.257(10) . 2_664 ? O(23) C(83) 3.355(9) . 2_664 ? O(23) C(45) 3.56(1) . 2_664 ? O(25) C(32) 3.36(1) . 4_465 ? O(26) C(26) 3.138(9) . 4_465 ? O(26) C(27) 3.225(9) . 4_465 ? O(26) N(7) 3.376(8) . 4_465 ? O(26) C(32) 3.59(1) . 4_465 ? O(26) N(9) 3.598(10) . 4_465 ? O(27) C(23) 2.962(9) . 4_465 ? O(27) N(8) 3.138(8) . 4_465 ? O(27) N(7) 3.156(8) . 4_465 ? O(27) C(24) 3.402(8) . 4_465 ? O(27) C(26) 3.428(9) . 4_465 ? O(27) C(25) 3.541(9) . 4_465 ? O(27) C(74) 3.589(9) . 2_665 ? O(28) C(43) 3.08(1) . 2_665 ? O(28) C(44) 3.21(1) . 2_665 ? O(28) C(42) 3.43(1) . 2_665 ? O(29) C(61) 3.39(1) . 4_555 ? O(29) C(9) 3.45(1) . 3_644 ? O(30) C(70) 3.055(10) . 4_455 ? O(30) C(71) 3.099(10) . 4_455 ? O(30) C(69) 3.41(1) . 4_455 ? O(30) C(8) 3.50(1) . 2_664 ? O(30) C(10) 3.54(1) . 3_644 ? O(30) N(21) 3.553(9) . 4_455 ? O(30) N(19) 3.579(9) . 4_455 ? O(31) C(8) 3.54(1) . 2_664 ? O(32) C(69) 3.29(1) . 4_455 ? O(32) C(68) 3.40(1) . 4_455 ? O(32) C(62) 3.47(1) . 4_555 ? O(32) C(70) 3.59(1) . 4_455 ? O(33) C(15) 3.037(8) . 3_645 ? O(33) C(14) 3.269(8) . 3_645 ? O(33) N(4) 3.342(7) . 3_645 ? O(33) C(16) 3.503(8) . 3_645 ? O(33) C(63) 3.544(9) . 4_555 ? O(34) N(4) 3.334(7) . 3_645 ? O(34) C(12) 3.415(8) . 3_645 ? O(34) C(86) 3.436(8) . 4_455 ? O(34) C(14) 3.459(8) . 2_665 ? O(34) C(21) 3.48(1) . 3_645 ? O(34) C(22) 3.543(10) . 3_645 ? O(35) C(86) 3.493(8) . 4_455 ? O(36) C(17) 3.273(8) . 2_665 ? O(36) C(18) 3.368(9) . 2_665 ? C(7) C(57) 3.37(1) . 2_665 ? C(8) C(58) 3.356(9) . 2_665 ? C(9) C(76) 3.493(9) . 2_765 ? C(11) C(24) 3.466(10) . 4_565 ? C(11) C(25) 3.60(1) . 4_565 ? C(13) C(85) 3.302(9) . 3_654 ? C(13) C(22) 3.520(9) . 4_465 ? C(14) C(85) 3.589(9) . 3_654 ? C(17) C(33) 3.578(10) . 4_465 ? C(18) C(33) 3.27(1) . 4_465 ? C(18) C(46) 3.385(9) . 2_664 ? C(19) C(33) 3.47(1) . 4_465 ? C(19) C(47) 3.474(9) . 2_664 ? C(19) C(46) 3.510(9) . 2_664 ? C(21) C(30) 3.58(1) . 4_565 ? C(22) C(30) 3.51(1) . 4_565 ? C(22) C(29) 3.56(1) . 4_565 ? C(24) C(74) 3.353(9) . 3_655 ? C(25) C(74) 3.528(9) . 3_655 ? C(29) C(98) 3.51(1) . 4_465 ? C(29) C(99) 3.597(10) . 4_465 ? C(40) C(79) 3.549(10) . 2_664 ? C(42) C(54) 3.43(1) . 2_664 ? C(46) C(88) 3.549(9) . 1_455 ? C(51) C(90) 3.490(9) . 2_665 ? C(51) C(91) 3.547(9) . 2_665 ? C(51) C(99) 3.560(10) . 1_455 ? C(57) C(77) 3.599(8) . 1_455 ? C(58) C(77) 3.449(9) . 1_455 ? C(62) C(65) 3.55(1) . 4_455 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ ###END