Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'L. Carlucci' 'G. Ciani' 'D.M. Proserpio' 'S. Rizzato' _publ_contact_author_name 'Prof G Ciani' _publ_contact_author_address ; Prof G Ciani Dipartimento di Chimica Strutturale e Stereochimica Inorganica and Centro CNR Via G. Venezian 21 20133 Milano Milano 20133 ITALY ; _publ_contact_author_email 'DAVIDE@CSMTBO.MI.CNR.IT' _publ_section_title ; Interlinked molecular squares with [Cu(2,2'-bipy)]2+ corners generating a three-dimensional network of unprecedented topological type ; data_2 _database_code_CSD 164240 _exptl_absorpt_correction_nazim 4.94 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 54 _chemical_formula_sum 'C44 H57 B3 Cl Cu2 F12 N8 O8.50' _chemical_formula_weight 1256.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-42d' #(122) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, -z+1/4' '-x, y+1/2, -z+1/4' 'y, x+1/2, z+1/4' '-y, -x+1/2, z+1/4' '-y, x, -z' 'y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1, -z+3/4' '-x+1/2, y+1, -z+3/4' 'y+1/2, x+1, z+3/4' '-y+1/2, -x+1, z+3/4' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 21.479(2) _cell_length_b 21.479(2) _cell_length_c 29.303(3) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 13519(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 917 _cell_measurement_theta_min 2. _cell_measurement_theta_max 24. _exptl_crystal_description 'cube-like' _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5144 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 2 _diffrn_reflns_number 25456 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2. _diffrn_reflns_theta_max 24. _reflns_number_total 5073 _reflns_number_observed 2933 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1617P)^2^+82.2720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(6) _refine_ls_number_reflns 5073 _refine_ls_number_parameters 343 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1790 _refine_ls_R_factor_obs 0.0982 _refine_ls_wR_factor_all 0.3268 _refine_ls_wR_factor_obs 0.2450 _refine_ls_goodness_of_fit_all 1.097 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.641 _refine_ls_shift/su_mean 0.032 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 O1S O 0.0539(10) 0.4798(10) 0.7986(7) 0.188(6) Uiso 1 1 d . . . O2S O -0.0311(17) 0.268(2) 0.6096(12) 0.188(6) Uiso 0.50 1 d P . . O3S O 0.102(2) 0.5660(19) 0.7492(14) 0.188(6) Uiso 0.50 1 d P . . O4S O 0.149(4) 0.574(4) 0.708(3) 0.188(6) Uiso 0.25 1 d P . . O5S O 0.025(3) 0.506(5) 0.901(2) 0.188(6) Uiso 0.25 1 d P . . O6S O 0.345(4) 0.900(4) 0.133(3) 0.188(6) Uiso 0.25 1 d P . . O7S O -0.030(4) 0.328(4) 0.600(3) 0.188(6) Uiso 0.25 1 d P . . O8S O 0.452(4) 0.282(3) 0.119(3) 0.188(6) Uiso 0.25 1 d P . . C12 C 0.1860(9) 0.0237(8) 0.8013(7) 0.106(6) Uani 1 1 d . . . H12 H 0.1476 0.0435 0.7991 0.128 Uiso 1 1 calc R . . C13 C 0.1897(17) -0.0421(11) 0.8106(9) 0.151(11) Uani 1 1 d . . . H13 H 0.1534 -0.0657 0.8109 0.181 Uiso 1 1 calc R . . C14 C 0.2410(17) -0.0682(10) 0.8184(9) 0.141(10) Uani 1 1 d . . . H14 H 0.2420 -0.1103 0.8257 0.169 Uiso 1 1 calc R . . C15 C 0.2986(13) -0.0333(9) 0.8163(8) 0.132(8) Uani 1 1 d . . . H15 H 0.3372 -0.0513 0.8218 0.159 Uiso 1 1 calc R . . C16 C 0.2919(8) 0.0268(7) 0.8056(6) 0.087(5) Uani 1 1 d . . . C17 C 0.3483(8) 0.0704(8) 0.8053(6) 0.098(5) Uani 1 1 d . . . C18 C 0.4087(10) 0.0535(13) 0.8147(11) 0.165(11) Uani 1 1 d . . . H18 H 0.4183 0.0118 0.8196 0.198 Uiso 1 1 calc R . . C19 C 0.4553(11) 0.0979(16) 0.8168(9) 0.151(10) Uani 1 1 d . . . H19 H 0.4940 0.0885 0.8294 0.181 Uiso 1 1 calc R . . N21 N 0.1538(5) 0.1599(5) 0.7793(5) 0.071(3) Uani 1 1 d D . . C22 C 0.1165(7) 0.1681(8) 0.8128(9) 0.129(8) Uani 1 1 d D . . H22 H 0.1331 0.1702 0.8421 0.154 Uiso 1 1 calc R . . C23 C 0.0523(10) 0.1740(10) 0.8078(10) 0.155(11) Uani 1 1 d D . . H23 H 0.0282 0.1801 0.8338 0.186 Uiso 1 1 calc R . . C24 C 0.0233(7) 0.1713(13) 0.7666(10) 0.147(10) Uani 1 1 d D . . C25 C 0.0657(10) 0.1643(13) 0.7291(10) 0.160(10) Uani 1 1 d D . . H25 H 0.0508 0.1655 0.6994 0.192 Uiso 1 1 calc R . . C26 C 0.1303(7) 0.1555(10) 0.7371(8) 0.118(7) Uani 1 1 d D . . H26 H 0.1566 0.1466 0.7127 0.142 Uiso 1 1 calc R . . C27 C -0.0478(8) 0.1708(7) 0.7613(8) 0.134(8) Uani 1 1 d D . . H27A H -0.0594 0.1571 0.7310 0.160 Uiso 1 1 calc R . . H27B H -0.0665 0.1431 0.7836 0.160 Uiso 1 1 calc R . . N31 N 0.2586(5) 0.2397(5) 0.7703(5) 0.078(3) Uani 1 1 d D . . C32 C 0.2669(6) 0.2563(7) 0.7274(6) 0.084(4) Uani 1 1 d D . . H32 H 0.2702 0.2251 0.7054 0.101 Uiso 1 1 calc R . . C33 C 0.2710(7) 0.3166(7) 0.7134(7) 0.097(5) Uani 1 1 d D . . H33 H 0.2793 0.3263 0.6831 0.117 Uiso 1 1 calc R . . C34 C 0.2625(13) 0.3629(7) 0.7452(7) 0.130(9) Uani 1 1 d D . . C35 C 0.2598(19) 0.3453(9) 0.7888(7) 0.219(18) Uani 1 1 d D . . H35 H 0.2599 0.3751 0.8119 0.263 Uiso 1 1 calc R . . C36 C 0.2570(16) 0.2815(8) 0.7999(7) 0.188(14) Uani 1 1 d D . . H36 H 0.2538 0.2701 0.8304 0.225 Uiso 1 1 calc R . . C37 C 0.2624(8) 0.4309(8) 0.7307(8) 0.148(9) Uani 1 1 d D . . H37A H 0.2335 0.4549 0.7490 0.177 Uiso 1 1 calc R . . H37B H 0.2510 0.4350 0.6988 0.177 Uiso 1 1 calc R . . C110 C 0.4434(9) 0.1544(15) 0.8004(8) 0.139(9) Uani 1 1 d . . . H110 H 0.4746 0.1838 0.7959 0.166 Uiso 1 1 calc R . . C111 C 0.3839(6) 0.1663(9) 0.7909(6) 0.101(6) Uani 1 1 d . . . H111 H 0.3748 0.2073 0.7832 0.121 Uiso 1 1 calc R . . N11 N 0.2389(5) 0.0558(4) 0.7960(4) 0.077(3) Uani 1 1 d . . . N112 N 0.3373(4) 0.1283(6) 0.7910(4) 0.074(3) Uani 1 1 d . . . B1 B 0.3059(7) 0.1082(6) 0.6644(5) 0.121(9) Uani 1 1 d D . . B2 B 0.5000 0.0000 0.5673(9) 0.19(3) Uani 1 2 d SD . . F11 F 0.2619(5) 0.1093(5) 0.6975(4) 0.128(4) Uani 1 1 d D . . F12 F 0.3611(6) 0.0952(6) 0.6856(5) 0.182(6) Uani 1 1 d D . . F13 F 0.3113(7) 0.1643(5) 0.6442(4) 0.177(6) Uani 1 1 d D . . F14 F 0.2916(6) 0.0649(5) 0.6330(4) 0.155(5) Uani 1 1 d D . . F21 F 0.5410(6) -0.0309(8) 0.5941(7) 0.237(9) Uani 1 1 d D . . F22 F 0.4693(8) -0.0409(6) 0.5408(7) 0.309(16) Uani 1 1 d D . . Cl Cl 0.2500 0.16475(18) 0.8750 0.0684(11) Uani 1 2 d S . . Cu Cu 0.24658(7) 0.14836(7) 0.78773(5) 0.0641(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C12 0.101(13) 0.070(11) 0.148(17) 0.008(10) -0.003(12) -0.041(9) C13 0.24(3) 0.069(14) 0.15(2) -0.010(14) 0.01(2) -0.051(18) C14 0.20(3) 0.056(11) 0.17(2) -0.005(12) 0.00(2) 0.012(17) C15 0.17(2) 0.065(12) 0.16(2) 0.006(12) 0.034(17) 0.043(14) C16 0.097(12) 0.047(8) 0.118(14) 0.006(8) 0.015(10) 0.018(8) C17 0.088(11) 0.088(11) 0.118(13) 0.015(9) 0.020(10) 0.038(10) C18 0.071(13) 0.15(2) 0.27(3) 0.05(2) 0.020(16) 0.072(15) C19 0.068(13) 0.22(3) 0.16(2) 0.04(2) 0.007(13) 0.045(17) N21 0.034(5) 0.077(7) 0.102(9) 0.000(7) -0.007(6) 0.001(5) C22 0.038(8) 0.17(2) 0.18(2) 0.015(17) -0.019(11) 0.027(11) C23 0.065(12) 0.24(3) 0.16(2) 0.05(2) 0.013(14) 0.029(16) C24 0.054(10) 0.22(3) 0.16(2) 0.039(19) -0.025(13) 0.029(13) C25 0.070(13) 0.23(3) 0.18(2) -0.01(2) -0.029(14) 0.030(16) C26 0.048(9) 0.160(19) 0.146(18) 0.000(15) -0.008(10) -0.012(11) C27 0.15(2) 0.076(12) 0.18(2) 0.009(12) -0.033(16) -0.014(12) N31 0.073(7) 0.039(6) 0.121(10) -0.004(6) -0.005(7) 0.007(5) C32 0.083(10) 0.060(8) 0.108(12) -0.001(9) 0.017(8) -0.002(8) C33 0.128(16) 0.069(10) 0.096(12) 0.011(9) -0.009(10) -0.004(9) C34 0.23(3) 0.067(11) 0.097(14) 0.013(10) 0.022(16) -0.038(15) C35 0.50(6) 0.071(12) 0.081(13) -0.017(11) 0.00(2) -0.08(3) C36 0.39(4) 0.050(10) 0.126(17) -0.005(10) 0.01(2) -0.07(2) C37 0.095(15) 0.15(2) 0.20(2) 0.052(17) 0.018(15) 0.020(14) C110 0.073(13) 0.19(3) 0.16(2) 0.046(19) -0.020(12) -0.002(15) C111 0.043(8) 0.129(15) 0.130(15) 0.021(12) -0.003(9) 0.009(9) N11 0.075(8) 0.037(5) 0.118(10) -0.009(5) -0.008(7) -0.004(5) N112 0.035(5) 0.082(8) 0.106(9) 0.003(7) -0.004(6) -0.005(5) B1 0.12(2) 0.049(11) 0.20(3) -0.049(15) -0.019(19) 0.007(11) B2 0.14(4) 0.12(3) 0.32(9) 0.000 0.000 -0.09(4) F11 0.110(8) 0.138(9) 0.135(8) -0.007(7) 0.012(7) -0.012(8) F12 0.136(12) 0.114(10) 0.30(2) -0.022(11) -0.005(12) -0.009(9) F13 0.260(19) 0.109(10) 0.163(12) 0.019(8) 0.002(11) -0.018(11) F14 0.209(14) 0.098(8) 0.158(11) -0.010(8) 0.008(10) 0.011(8) F21 0.159(16) 0.25(2) 0.30(3) -0.035(19) -0.010(15) -0.003(14) F22 0.44(4) 0.162(16) 0.32(3) 0.027(17) -0.18(3) -0.13(2) Cl 0.064(2) 0.057(2) 0.084(3) 0.000 -0.001(3) 0.000 Cu 0.0423(8) 0.0418(8) 0.1081(11) 0.0018(7) -0.0036(9) -0.0011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2S O2S 1.18(7) 3_556 ? O2S O7S 1.32(9) . ? O3S O4S 1.60(8) . ? O5S O5S 1.10(15) 2_565 ? O8S O8S 1.42(13) 3 ? C12 N11 1.338(19) . ? C12 C13 1.44(3) . ? C13 C14 1.26(4) . ? C14 C15 1.45(3) . ? C15 C16 1.34(2) . ? C16 N11 1.328(19) . ? C16 C17 1.53(2) . ? C17 N112 1.336(19) . ? C17 C18 1.37(2) . ? C18 C19 1.39(3) . ? C19 C110 1.33(3) . ? N21 C22 1.28(2) . ? N21 C26 1.34(2) . ? N21 Cu 2.023(11) . ? C22 C23 1.39(3) . ? C23 C24 1.36(3) . ? C24 C25 1.44(3) . ? C24 C27 1.533(10) . ? C25 C26 1.42(2) . ? C27 C37 1.524(10) 16_456 ? N31 C36 1.25(2) . ? N31 C32 1.321(17) . ? N31 Cu 2.043(11) . ? C32 C33 1.36(2) . ? C33 C34 1.37(2) . ? C34 C35 1.33(2) . ? C34 C37 1.522(10) . ? C35 C36 1.41(3) . ? C37 C27 1.524(10) 15_556 ? C110 C111 1.33(2) . ? C111 N112 1.290(18) . ? N11 Cu 2.009(10) . ? N112 Cu 1.998(10) . ? B1 F14 1.342(12) . ? B1 F13 1.348(13) . ? B1 F11 1.355(13) . ? B1 F12 1.369(13) . ? B2 F22 1.344(12) . ? B2 F22 1.344(12) 2_655 ? B2 F21 1.354(12) . ? B2 F21 1.354(12) 2_655 ? F11 Cu 2.794(10) . ? Cl Cu 2.5825(17) . ? Cl Cu 2.5825(17) 12_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2S O2S O7S 143(7) 3_556 . ? N11 C12 C13 119(2) . . ? C14 C13 C12 121(3) . . ? C13 C14 C15 121(2) . . ? C16 C15 C14 115(2) . . ? C15 C16 N11 126.6(19) . . ? C15 C16 C17 120.4(19) . . ? N11 C16 C17 113.0(12) . . ? N112 C17 C18 118(2) . . ? N112 C17 C16 115.6(14) . . ? C18 C17 C16 125.8(18) . . ? C19 C18 C17 121(2) . . ? C110 C19 C18 118(2) . . ? C22 N21 C26 118.8(14) . . ? C22 N21 Cu 122.7(12) . . ? C26 N21 Cu 118.4(11) . . ? N21 C22 C23 124(2) . . ? C22 C23 C24 123(2) . . ? C23 C24 C25 113.1(17) . . ? C23 C24 C27 123(2) . . ? C25 C24 C27 124(2) . . ? C26 C25 C24 121(2) . . ? N21 C26 C25 121(2) . . ? C37 C27 C24 106.1(15) 16_456 . ? C36 N31 C32 118.1(14) . . ? C36 N31 Cu 120.9(12) . . ? C32 N31 Cu 121.0(10) . . ? N31 C32 C33 123.5(15) . . ? C32 C33 C34 118.5(16) . . ? C35 C34 C33 116.7(15) . . ? C35 C34 C37 122.6(19) . . ? C33 C34 C37 120.4(18) . . ? C34 C35 C36 119.8(17) . . ? N31 C36 C35 122.6(19) . . ? C34 C37 C27 104.1(15) . 15_556 ? C111 C110 C19 116(2) . . ? N112 C111 C110 128(2) . . ? C12 N11 C16 117.4(13) . . ? C12 N11 Cu 126.4(12) . . ? C16 N11 Cu 114.8(10) . . ? C111 N112 C17 116.9(14) . . ? C111 N112 Cu 128.4(11) . . ? C17 N112 Cu 112.8(10) . . ? F14 B1 F13 109.7(11) . . ? F14 B1 F11 110.1(11) . . ? F13 B1 F11 111.1(10) . . ? F14 B1 F12 111.5(11) . . ? F13 B1 F12 107.9(11) . . ? F11 B1 F12 106.5(11) . . ? F22 B2 F22 109.5(15) . 2_655 ? F22 B2 F21 109.5(6) . . ? F22 B2 F21 109.6(6) 2_655 . ? F22 B2 F21 109.6(6) . 2_655 ? F22 B2 F21 109.5(6) 2_655 2_655 ? F21 B2 F21 109.1(15) . 2_655 ? B1 F11 Cu 139.9(8) . . ? Cu Cl Cu 164.33(18) . 12_546 ? N112 Cu N11 82.0(5) . . ? N112 Cu N21 173.2(5) . . ? N11 Cu N21 93.1(5) . . ? N112 Cu N31 95.5(5) . . ? N11 Cu N31 172.0(5) . . ? N21 Cu N31 88.7(5) . . ? N112 Cu Cl 87.4(4) . . ? N11 Cu Cl 91.0(4) . . ? N21 Cu Cl 97.6(4) . . ? N31 Cu Cl 96.5(4) . . ? N112 Cu F11 82.3(4) . . ? N11 Cu F11 80.0(4) . . ? N21 Cu F11 92.1(5) . . ? N31 Cu F11 92.1(4) . . ? Cl Cu F11 167.1(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.175 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.112 # * END data_3 _database_code_CSD 164241 _exptl_absorpt_correction_nazim 2.85 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C45 H43 B3 Cl3 Cu2 F12 N8 O2.50' _chemical_formula_weight 1229.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' #(15) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.457(5) _cell_length_b 40.814(17) _cell_length_c 14.502(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.424(9) _cell_angle_gamma 90.00 _cell_volume 6313(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 902 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.397 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 10 _diffrn_reflns_number 14189 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2. _diffrn_reflns_theta_max 24. _reflns_number_total 4937 _reflns_number_observed 3240 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1795P)^2^+6.1792P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4937 _refine_ls_number_parameters 373 _refine_ls_number_restraints 302 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_obs 0.0851 _refine_ls_wR_factor_all 0.2790 _refine_ls_wR_factor_obs 0.2436 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.004 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 Cu 0.56154(7) 0.105271(18) 0.11177(6) 0.0591(4) Uani 1 1 d . . . Cl Cl 0.5000 0.12656(6) 0.2500 0.0699(7) Uani 1 2 d S . . N1 N 0.5271(5) 0.05675(13) 0.1163(4) 0.0590(13) Uani 1 1 d . . . C11 C 0.6236(7) 0.03933(17) 0.1789(5) 0.0654(17) Uani 1 1 d . . . C12 C 0.6140(9) 0.00624(19) 0.1873(6) 0.081(2) Uani 1 1 d . . . H12 H 0.6820 -0.0057 0.2291 0.097 Uiso 1 1 calc R . . C13 C 0.5038(10) -0.0096(2) 0.1340(7) 0.090(3) Uani 1 1 d . . . H13 H 0.4959 -0.0321 0.1408 0.108 Uiso 1 1 calc R . . C14 C 0.4064(9) 0.0082(2) 0.0711(7) 0.085(2) Uani 1 1 d . . . H14 H 0.3314 -0.0019 0.0333 0.102 Uiso 1 1 calc R . . C15 C 0.4213(7) 0.04029(19) 0.0650(6) 0.075(2) Uani 1 1 d . . . H15 H 0.3541 0.0522 0.0223 0.090 Uiso 1 1 calc R . . N2 N 0.7269(5) 0.09110(15) 0.2130(4) 0.0622(14) Uani 1 1 d . . . C21 C 0.7317(6) 0.05895(18) 0.2358(5) 0.0649(17) Uani 1 1 d . . . C22 C 0.8327(8) 0.0458(2) 0.3132(7) 0.097(3) Uani 1 1 d . . . H22 H 0.8354 0.0236 0.3282 0.117 Uiso 1 1 calc R . . C23 C 0.9288(8) 0.0665(3) 0.3673(8) 0.113(3) Uani 1 1 d . . . H23 H 0.9963 0.0584 0.4204 0.135 Uiso 1 1 calc R . . C24 C 0.9241(8) 0.0987(3) 0.3423(8) 0.105(3) Uani 1 1 d . . . H24 H 0.9900 0.1127 0.3764 0.126 Uiso 1 1 calc R . . C25 C 0.8201(7) 0.1107(2) 0.2655(6) 0.083(2) Uani 1 1 d . . . H25 H 0.8156 0.1329 0.2505 0.099 Uiso 1 1 calc R . . N3 N 0.3982(5) 0.11325(14) -0.0013(4) 0.0620(14) Uani 1 1 d . . . C31 C 0.2925(7) 0.1204(2) 0.0135(6) 0.086(2) Uani 1 1 d . . . H31 H 0.2954 0.1233 0.0779 0.103 Uiso 1 1 calc R . . C32 C 0.1782(7) 0.1236(3) -0.0649(7) 0.096(3) Uani 1 1 d . . . H32 H 0.1054 0.1278 -0.0527 0.115 Uiso 1 1 calc R . . C33 C 0.1737(8) 0.1205(2) -0.1621(6) 0.085(2) Uani 1 1 d . . . C34 C 0.2842(7) 0.1135(2) -0.1746(6) 0.086(2) Uani 1 1 d . . . H34 H 0.2856 0.1112 -0.2379 0.103 Uiso 1 1 calc R . . C35 C 0.3911(7) 0.1100(2) -0.0945(6) 0.077(2) Uani 1 1 d . . . H35 H 0.4643 0.1051 -0.1053 0.092 Uiso 1 1 calc R . . C1A C 0.0576(7) 0.1226(2) -0.2508(6) 0.091(2) Uani 1 1 d . . . H1A1 H 0.0657 0.1240 -0.3122 0.109 Uiso 1 1 calc R . . C2A C 0.7634(15) 0.2365(2) -0.0021(10) 0.147(5) Uani 1 1 d . . . H2A1 H 0.8259 0.2332 -0.0278 0.176 Uiso 1 1 calc R . . N4 N 0.6267(6) 0.14784(14) 0.0792(5) 0.0755(17) Uani 1 1 d . . . C41 C 0.5746(11) 0.1761(2) 0.0894(8) 0.106(3) Uani 1 1 d . . . H41 H 0.5087 0.1763 0.1123 0.127 Uiso 1 1 calc R . . C42 C 0.6198(14) 0.2058(2) 0.0651(9) 0.129(4) Uani 1 1 d . . . H42 H 0.5858 0.2256 0.0749 0.154 Uiso 1 1 calc R . . C43 C 0.7140(12) 0.2058(3) 0.0270(9) 0.111(3) Uani 1 1 d . . . C45 C 0.7178(8) 0.1482(2) 0.0413(7) 0.090(2) Uani 1 1 d . . . H45 H 0.7536 0.1286 0.0328 0.108 Uiso 1 1 calc R . . C4 C 0.7587(10) 0.1769(3) 0.0151(9) 0.116(3) Uani 1 1 d . . . H4 H 0.8205 0.1761 -0.0121 0.139 Uiso 1 1 calc R . . O1W O 0.5000 0.1765(18) 0.7500 0.321(11) Uiso 0.50 2 d SP . . O2W O 0.566(4) 0.2087(10) 0.737(4) 0.321(11) Uiso 0.50 1 d P . . O3W O 0.716(4) 0.2049(9) 0.743(3) 0.321(11) Uiso 0.50 1 d P . . O4W O 0.927(4) 0.2096(9) 0.786(3) 0.321(11) Uiso 0.50 1 d P . . B2 B 0.873(2) 0.1974(6) 0.3770(19) 0.41(2) Uani 0.50 1 d PDU . . F21 F 0.904(3) 0.2282(5) 0.410(3) 0.49(2) Uani 0.50 1 d PDU . . F22 F 0.903(4) 0.1925(9) 0.297(2) 0.578(13) Uani 0.50 1 d PDU . . F23 F 0.939(2) 0.1768(6) 0.449(2) 0.319(15) Uani 0.50 1 d PDU . . F24 F 0.751(2) 0.1929(7) 0.356(3) 0.49(2) Uani 0.50 1 d PDU . . B1 B 0.7571(7) 0.0693(2) 0.9165(6) 0.088(2) Uani 1 1 d DU . . F11 F 0.8411(5) 0.09382(13) 0.9288(4) 0.1081(16) Uani 1 1 d DU A . F12 F 0.6459(7) 0.0774(3) 0.8455(8) 0.198(5) Uani 0.83 1 d PDU A 1 F13 F 0.7350(11) 0.0647(2) 1.0007(6) 0.157(3) Uani 0.83 1 d PDU A 1 F14 F 0.7965(10) 0.0422(2) 0.8874(11) 0.185(4) Uani 0.83 1 d PDU A 1 F12B F 0.657(2) 0.0804(7) 0.934(3) 0.150 Uiso 0.17 1 d PDU A 2 F14B F 0.811(3) 0.0450(6) 0.981(3) 0.150 Uiso 0.17 1 d PDU A 2 F13B F 0.721(4) 0.0571(8) 0.8251(16) 0.150 Uiso 0.17 1 d PDU A 2 Cl1W Cl 0.9132(5) 0.01692(17) 0.6500(6) 0.236(3) Uani 1 1 d DU . . C1W C 1.0000 0.0405(5) 0.7500 0.289(16) Uani 1 2 d SDU . . H1W1 H 1.0560 0.0544 0.7311 0.347 Uiso 0.50 1 calc PR . . H1W2 H 0.9440 0.0544 0.7689 0.347 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0439(5) 0.0571(5) 0.0622(6) 0.0057(3) 0.0025(4) -0.0064(3) Cl 0.0626(14) 0.0835(16) 0.0560(14) 0.000 0.0128(11) 0.000 N1 0.053(3) 0.060(3) 0.056(3) 0.000(2) 0.010(3) -0.008(2) C11 0.069(4) 0.070(4) 0.057(4) 0.004(3) 0.023(3) 0.005(3) C12 0.098(6) 0.065(5) 0.085(6) 0.013(4) 0.040(5) 0.014(4) C13 0.125(8) 0.063(5) 0.095(6) -0.004(4) 0.056(6) -0.018(5) C14 0.096(6) 0.069(5) 0.089(6) -0.005(4) 0.033(5) -0.026(4) C15 0.070(5) 0.080(5) 0.072(5) 0.000(4) 0.022(4) -0.009(4) N2 0.044(3) 0.081(4) 0.056(3) 0.005(3) 0.012(2) -0.002(3) C21 0.055(4) 0.078(4) 0.052(4) 0.002(3) 0.008(3) 0.013(3) C22 0.075(5) 0.100(6) 0.093(6) 0.015(5) 0.003(5) 0.022(5) C23 0.064(6) 0.135(9) 0.103(7) 0.006(6) -0.010(5) 0.033(6) C24 0.049(5) 0.139(9) 0.103(7) -0.021(6) 0.000(4) -0.013(5) C25 0.051(4) 0.099(6) 0.078(5) -0.006(4) 0.000(4) -0.009(4) N3 0.049(3) 0.072(3) 0.053(3) 0.004(3) 0.005(2) -0.002(2) C31 0.061(5) 0.127(7) 0.060(5) -0.004(4) 0.009(4) 0.014(5) C32 0.054(4) 0.135(8) 0.081(6) -0.009(5) 0.004(4) 0.020(5) C33 0.076(5) 0.091(5) 0.063(5) -0.015(4) -0.005(4) -0.009(4) C34 0.062(5) 0.128(7) 0.053(4) -0.006(4) 0.004(4) 0.005(4) C35 0.056(4) 0.105(6) 0.060(5) -0.007(4) 0.010(3) -0.005(4) C1A 0.076(5) 0.120(7) 0.062(5) 0.000(5) 0.006(4) 0.001(5) C2A 0.192(13) 0.096(7) 0.134(10) 0.026(8) 0.038(9) -0.050(10) N4 0.068(4) 0.062(4) 0.084(4) 0.003(3) 0.012(3) -0.013(3) C41 0.142(9) 0.062(5) 0.137(9) 0.008(5) 0.077(8) -0.006(5) C42 0.189(13) 0.073(6) 0.133(10) -0.002(6) 0.070(10) -0.009(7) C43 0.132(9) 0.087(7) 0.121(8) 0.004(6) 0.054(7) -0.042(6) C45 0.080(5) 0.085(5) 0.106(7) 0.013(5) 0.036(5) -0.015(4) C4 0.102(7) 0.107(8) 0.146(10) 0.010(7) 0.055(7) -0.034(6) B2 0.35(3) 0.32(3) 0.35(4) -0.08(4) -0.13(3) -0.12(6) F21 0.30(4) 0.22(2) 0.81(7) 0.00(3) 0.05(4) -0.13(2) F22 0.71(4) 0.56(3) 0.34(3) -0.03(3) 0.05(3) -0.521 F23 0.29(3) 0.27(2) 0.45(4) 0.07(3) 0.20(3) -0.07(2) F24 0.39(3) 0.29(3) 0.56(5) 0.11(3) -0.10(3) -0.20(2) B1 0.071(5) 0.097(5) 0.085(5) 0.005(5) 0.017(4) -0.020(4) F11 0.096(3) 0.108(3) 0.114(4) 0.004(3) 0.031(3) -0.037(3) F12 0.074(4) 0.288(12) 0.189(8) 0.114(9) -0.005(4) -0.041(5) F13 0.230(9) 0.152(7) 0.108(4) -0.024(4) 0.084(5) -0.099(6) F14 0.177(8) 0.138(5) 0.275(12) -0.093(7) 0.123(8) -0.053(5) Cl1W 0.136(4) 0.243(6) 0.302(8) 0.062(5) 0.048(4) 0.003(3) C1W 0.127(19) 0.17(2) 0.48(3) 0.000 0.01(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2 2.012(5) . ? Cu N3 2.014(5) . ? Cu N4 2.014(6) . ? Cu N1 2.025(5) . ? Cu Cl 2.5106(15) . ? Cl Cu 2.5106(15) 2_655 ? N1 C15 1.347(9) . ? N1 C11 1.349(9) . ? C11 C12 1.364(10) . ? C11 C21 1.452(10) . ? C12 C13 1.376(12) . ? C13 C14 1.366(13) . ? C14 C15 1.326(11) . ? N2 C25 1.329(9) . ? N2 C21 1.349(9) . ? C21 C22 1.393(10) . ? C22 C23 1.381(14) . ? C23 C24 1.362(15) . ? C24 C25 1.389(12) . ? N3 C35 1.332(10) . ? N3 C31 1.336(10) . ? C31 C32 1.391(11) . ? C32 C33 1.397(12) . ? C33 C34 1.373(12) . ? C33 C1A 1.477(11) . ? C34 C35 1.353(11) . ? C1A C1A 1.329(17) 2_554 ? C2A C2A 1.15(2) 7_655 ? C2A C43 1.499(13) . ? N4 C41 1.332(11) . ? N4 C45 1.345(11) . ? C41 C42 1.413(13) . ? C42 C43 1.381(16) . ? C43 C4 1.320(15) . ? C45 C4 1.365(13) . ? O1W O2W 1.56(5) . ? O1W O2W 1.56(5) 2_656 ? O2W O2W 1.68(9) 2_656 ? O2W O3W 1.70(5) . ? B2 F24 1.336(14) . ? B2 F23 1.341(14) . ? B2 F22 1.341(14) . ? B2 F21 1.342(14) . ? B1 F14 1.323(9) . ? B1 F13B 1.333(13) . ? B1 F12B 1.338(13) . ? B1 F13 1.349(9) . ? B1 F14B 1.352(13) . ? B1 F11 1.353(8) . ? B1 F12 1.354(9) . ? Cl1W C1W 1.721(9) . ? C1W Cl1W 1.721(9) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu N3 171.2(2) . . ? N2 Cu N4 95.1(2) . . ? N3 Cu N4 89.1(2) . . ? N2 Cu N1 80.7(2) . . ? N3 Cu N1 92.9(2) . . ? N4 Cu N1 160.8(3) . . ? N2 Cu Cl 88.90(17) . . ? N3 Cu Cl 98.36(18) . . ? N4 Cu Cl 97.2(2) . . ? N1 Cu Cl 101.40(17) . . ? Cu Cl Cu 139.51(12) 2_655 . ? C15 N1 C11 117.4(6) . . ? C15 N1 Cu 128.0(5) . . ? C11 N1 Cu 114.6(4) . . ? N1 C11 C12 120.6(7) . . ? N1 C11 C21 114.3(6) . . ? C12 C11 C21 125.1(7) . . ? C11 C12 C13 120.2(8) . . ? C14 C13 C12 118.8(8) . . ? C15 C14 C13 118.5(8) . . ? C14 C15 N1 124.5(8) . . ? C25 N2 C21 119.5(6) . . ? C25 N2 Cu 126.2(5) . . ? C21 N2 Cu 113.7(4) . . ? N2 C21 C22 121.3(7) . . ? N2 C21 C11 116.6(6) . . ? C22 C21 C11 122.0(7) . . ? C23 C22 C21 118.5(9) . . ? C24 C23 C22 119.6(8) . . ? C23 C24 C25 119.5(8) . . ? N2 C25 C24 121.5(8) . . ? C35 N3 C31 117.5(6) . . ? C35 N3 Cu 120.3(5) . . ? C31 N3 Cu 122.2(5) . . ? N3 C31 C32 121.8(8) . . ? C31 C32 C33 119.5(8) . . ? C34 C33 C32 117.1(7) . . ? C34 C33 C1A 118.6(8) . . ? C32 C33 C1A 124.3(8) . . ? C35 C34 C33 119.9(8) . . ? N3 C35 C34 124.1(8) . . ? C1A C1A C33 124.6(11) 2_554 . ? C2A C2A C43 131(2) 7_655 . ? C41 N4 C45 118.7(7) . . ? C41 N4 Cu 120.1(6) . . ? C45 N4 Cu 121.1(6) . . ? N4 C41 C42 119.7(10) . . ? C43 C42 C41 120.6(10) . . ? C4 C43 C42 116.9(9) . . ? C4 C43 C2A 120.3(12) . . ? C42 C43 C2A 122.8(12) . . ? N4 C45 C4 121.4(10) . . ? C43 C4 C45 122.6(11) . . ? O2W O1W O2W 65(4) . 2_656 ? O1W O2W O2W 57(2) . 2_656 ? O1W O2W O3W 116(3) . . ? O2W O2W O3W 164(6) 2_656 . ? F24 B2 F23 109.4(13) . . ? F24 B2 F22 111.3(13) . . ? F23 B2 F22 109.7(13) . . ? F24 B2 F21 109.1(13) . . ? F23 B2 F21 108.0(13) . . ? F22 B2 F21 109.3(13) . . ? F14 B1 F13B 52.1(17) . . ? F14 B1 F12B 139.3(13) . . ? F13B B1 F12B 110.0(12) . . ? F14 B1 F13 111.7(8) . . ? F13B B1 F13 139.1(13) . . ? F12B B1 F13 54.3(17) . . ? F14 B1 F14B 58.9(17) . . ? F13B B1 F14B 108.2(12) . . ? F12B B1 F14B 108.6(12) . . ? F13 B1 F14B 57.1(17) . . ? F14 B1 F11 110.6(7) . . ? F13B B1 F11 110.8(11) . . ? F12B B1 F11 110.0(11) . . ? F13 B1 F11 110.1(7) . . ? F14B B1 F11 109.2(11) . . ? F14 B1 F12 107.3(8) . . ? F13B B1 F12 58.2(18) . . ? F12B B1 F12 55.3(18) . . ? F13 B1 F12 106.7(8) . . ? F14B B1 F12 140.4(13) . . ? F11 B1 F12 110.3(7) . . ? Cl1W C1W Cl1W 112.1(11) 2_756 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.866 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.133 # * END