# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Ross Forgan' _publ_contact_author_email FORGANROSS@GMAIL.COM _publ_section_title ; Transport of Metal Salts by Zwitterionic Ligands; Simple but Highly Efficient Salicylaldoxime Extractants ; loop_ _publ_author_name 'Ross Forgan' 'James Davidson' 'Stuart G Galbraith' 'David K Henderson' 'Simon Parsons' ; P.Tasker ; 'Fraser White' # Attachment 'revised Cu(L2)Cl2.cif' data_dhpbcn _database_code_depnum_ccdc_archive 'CCDC 612042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C5H10NHCH2)((CH3)3C)(C6H2)O(CHNOH)CuCl2]' _chemical_formula_sum 'C17 H26 Cl2 Cu1 N2 O2' _chemical_formula_weight 566.45 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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.542(2) _cell_length_b 24.736(3) _cell_length_c 10.4427(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4272.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27848 _cell_measurement_theta_min 5 _cell_measurement_theta_max 52 _exptl_crystal_description lath _exptl_crystal_colour Green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.92804 _exptl_absorpt_correction_T_max 0.248576 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26073 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4372 _reflns_number_gt 3185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0869P)^2^+0.0000P] 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_extinction_coef ? _refine_ls_number_reflns 4372 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.05193(2) 0.341820(15) 0.38880(4) 0.03031(16) Uani 1 1 d . . . Cl1 Cl 0.18501(5) 0.36239(4) 0.40868(9) 0.0388(2) Uani 1 1 d . . . Cl2 Cl 0.07223(5) 0.25323(3) 0.43468(10) 0.0389(2) Uani 1 1 d . . . O1 O -0.06124(12) 0.32867(9) 0.3549(2) 0.0292(5) Uani 1 1 d . . . C1 C -0.12313(18) 0.35787(12) 0.3968(3) 0.0240(7) Uani 1 1 d . . . C2 C -0.11930(18) 0.41369(12) 0.4221(3) 0.0252(7) Uani 1 1 d . . . C3 C -0.18947(18) 0.44200(12) 0.4581(3) 0.0272(7) Uani 1 1 d . . . H3 H -0.1861 0.4800 0.4706 0.033 Uiso 1 1 calc R . . C4 C -0.26275(18) 0.41679(12) 0.4757(3) 0.0272(7) Uani 1 1 d . . . C5 C -0.26543(18) 0.36080(12) 0.4524(3) 0.0256(7) Uani 1 1 d . . . H5 H -0.3151 0.3422 0.4646 0.031 Uiso 1 1 calc R . . C6 C -0.19864(19) 0.33178(12) 0.4123(3) 0.0253(7) Uani 1 1 d . . . C21 C -0.04464(19) 0.44361(13) 0.4079(3) 0.0284(7) Uani 1 1 d . . . H21 H -0.0473 0.4820 0.4091 0.034 Uiso 1 1 calc R . . N22 N 0.02465(15) 0.42144(10) 0.3938(3) 0.0269(6) Uani 1 1 d . . . O23 O 0.08639(14) 0.45976(9) 0.3794(3) 0.0355(6) Uani 1 1 d . . . H23 H 0.1315 0.4442 0.3831 0.053 Uiso 1 1 calc R . . C41 C -0.33980(18) 0.44700(12) 0.5171(3) 0.0290(7) Uani 1 1 d . . . C42 C -0.3730(2) 0.42125(14) 0.6399(4) 0.0412(9) Uani 1 1 d . . . H42A H -0.4222 0.4403 0.6664 0.062 Uiso 1 1 calc R . . H42B H -0.3324 0.4238 0.7079 0.062 Uiso 1 1 calc R . . H42C H -0.3857 0.3831 0.6239 0.062 Uiso 1 1 calc R . . C43 C -0.4034(2) 0.44257(15) 0.4105(4) 0.0422(9) Uani 1 1 d . . . H43A H -0.4525 0.4618 0.4364 0.063 Uiso 1 1 calc R . . H43B H -0.4161 0.4044 0.3953 0.063 Uiso 1 1 calc R . . H43C H -0.3820 0.4587 0.3317 0.063 Uiso 1 1 calc R . . C44 C -0.3232(2) 0.50693(13) 0.5440(4) 0.0434(10) Uani 1 1 d . . . H44A H -0.3736 0.5248 0.5697 0.065 Uiso 1 1 calc R . . H44B H -0.3021 0.5242 0.4664 0.065 Uiso 1 1 calc R . . H44C H -0.2834 0.5101 0.6130 0.065 Uiso 1 1 calc R . . C61 C -0.20366(18) 0.27288(12) 0.3763(3) 0.0265(7) Uani 1 1 d . . . H61A H -0.1951 0.2691 0.2829 0.032 Uiso 1 1 calc R . . H61B H -0.2584 0.2592 0.3964 0.032 Uiso 1 1 calc R . . N62 N -0.14182(16) 0.23919(10) 0.4463(3) 0.0252(6) Uani 1 1 d . . . H62 H -0.103(3) 0.2569(14) 0.427(4) 0.039(11) Uiso 1 1 d . . . C63 C -0.1563(2) 0.24022(13) 0.5879(3) 0.0313(8) Uani 1 1 d . . . H63A H -0.2109 0.2259 0.6065 0.038 Uiso 1 1 calc R . . H63B H -0.1540 0.2780 0.6190 0.038 Uiso 1 1 calc R . . C64 C -0.0937(2) 0.20660(14) 0.6576(4) 0.0362(8) Uani 1 1 d . . . H64A H -0.1055 0.2067 0.7505 0.043 Uiso 1 1 calc R . . H64B H -0.0395 0.2227 0.6449 0.043 Uiso 1 1 calc R . . C65 C -0.0936(2) 0.14798(14) 0.6080(4) 0.0408(9) Uani 1 1 d . . . H65A H -0.0501 0.1273 0.6508 0.049 Uiso 1 1 calc R . . H65B H -0.1459 0.1306 0.6286 0.049 Uiso 1 1 calc R . . C66 C -0.0803(2) 0.14729(13) 0.4636(4) 0.0360(9) Uani 1 1 d . . . H66A H -0.0849 0.1097 0.4320 0.043 Uiso 1 1 calc R . . H66B H -0.0250 0.1603 0.4444 0.043 Uiso 1 1 calc R . . C67 C -0.1414(2) 0.18271(12) 0.3936(3) 0.0307(7) Uani 1 1 d . . . H67A H -0.1278 0.1838 0.3013 0.037 Uiso 1 1 calc R . . H67B H -0.1960 0.1668 0.4024 0.037 Uiso 1 1 calc R . . 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 Cu1 0.0058(2) 0.0382(2) 0.0469(3) -0.00077(18) -0.00070(17) 0.00019(15) Cl1 0.0073(4) 0.0525(5) 0.0566(6) -0.0049(4) -0.0038(4) -0.0004(3) Cl2 0.0178(4) 0.0444(4) 0.0544(6) 0.0116(4) 0.0017(4) 0.0036(3) O1 0.0079(11) 0.0380(11) 0.0415(15) -0.0061(10) 0.0006(10) 0.0028(9) C1 0.0099(15) 0.0352(14) 0.0268(18) 0.0001(13) -0.0002(13) 0.0004(12) C2 0.0086(15) 0.0369(15) 0.0301(19) -0.0029(13) -0.0003(13) -0.0016(12) C3 0.0128(15) 0.0348(15) 0.034(2) -0.0022(13) 0.0028(14) 0.0006(12) C4 0.0100(15) 0.0401(16) 0.031(2) -0.0034(14) 0.0037(14) 0.0012(13) C5 0.0079(14) 0.0384(15) 0.0304(19) -0.0019(14) 0.0003(13) -0.0012(12) C6 0.0113(15) 0.0337(15) 0.0308(19) 0.0015(13) 0.0002(13) -0.0009(12) C21 0.0135(16) 0.0361(16) 0.036(2) -0.0038(14) -0.0001(14) -0.0024(13) N22 0.0069(12) 0.0374(13) 0.0363(17) -0.0038(12) 0.0011(11) -0.0054(11) O23 0.0083(11) 0.0416(12) 0.0565(18) -0.0042(11) 0.0034(11) -0.0078(9) C41 0.0100(15) 0.0366(15) 0.041(2) -0.0026(14) 0.0045(14) 0.0028(12) C42 0.0210(19) 0.051(2) 0.051(3) -0.0025(17) 0.0124(17) 0.0026(16) C43 0.0178(18) 0.056(2) 0.053(3) -0.0007(18) -0.0006(17) 0.0114(16) C44 0.0176(17) 0.0404(18) 0.072(3) -0.0018(18) 0.0130(19) 0.0068(15) C61 0.0079(14) 0.0366(16) 0.035(2) 0.0028(14) -0.0027(13) -0.0018(12) N62 0.0082(13) 0.0332(13) 0.0343(17) 0.0009(11) -0.0002(12) -0.0026(11) C63 0.0196(17) 0.0445(17) 0.030(2) 0.0000(14) 0.0012(15) -0.0005(14) C64 0.0187(17) 0.056(2) 0.034(2) 0.0097(16) -0.0035(16) -0.0009(16) C65 0.0150(17) 0.053(2) 0.055(3) 0.0170(18) 0.0003(17) 0.0052(16) C66 0.0156(17) 0.0351(16) 0.057(3) 0.0053(16) 0.0046(17) 0.0012(13) C67 0.0197(17) 0.0354(15) 0.037(2) 0.0002(14) 0.0032(15) 0.0009(14) _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 Cu1 O1 1.933(2) . ? Cu1 N22 2.021(3) . ? Cu1 Cl2 2.2682(9) . ? Cu1 Cl1 2.2689(9) . ? O1 C1 1.327(4) . ? C1 C2 1.407(4) . ? C1 C6 1.415(4) . ? C2 C3 1.407(4) . ? C2 C21 1.447(4) . ? C3 C4 1.376(4) . ? C4 C5 1.407(4) . ? C4 C41 1.539(4) . ? C5 C6 1.383(4) . ? C6 C61 1.507(4) . ? C21 N22 1.279(4) . ? N22 O23 1.402(3) . ? C41 C44 1.533(4) . ? C41 C42 1.534(5) . ? C41 C43 1.536(5) . ? C61 N62 1.508(4) . ? N62 C63 1.498(4) . ? N62 C67 1.502(4) . ? C63 C64 1.515(4) . ? C64 C65 1.540(5) . ? C65 C66 1.524(5) . ? C66 C67 1.524(5) . ? 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 O1 Cu1 N22 87.27(10) . . ? O1 Cu1 Cl2 91.12(7) . . ? N22 Cu1 Cl2 165.69(9) . . ? O1 Cu1 Cl1 173.84(8) . . ? N22 Cu1 Cl1 89.76(8) . . ? Cl2 Cu1 Cl1 93.08(3) . . ? C1 O1 Cu1 126.5(2) . . ? O1 C1 C2 124.1(3) . . ? O1 C1 C6 118.0(3) . . ? C2 C1 C6 117.8(3) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 C21 118.5(3) . . ? C1 C2 C21 121.4(3) . . ? C4 C3 C2 122.5(3) . . ? C3 C4 C5 116.8(3) . . ? C3 C4 C41 123.2(3) . . ? C5 C4 C41 120.0(3) . . ? C6 C5 C4 122.6(3) . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C61 122.2(3) . . ? C1 C6 C61 117.5(3) . . ? N22 C21 C2 123.9(3) . . ? C21 N22 O23 112.0(3) . . ? C21 N22 Cu1 128.4(2) . . ? O23 N22 Cu1 119.57(19) . . ? C44 C41 C42 108.2(3) . . ? C44 C41 C43 108.9(3) . . ? C42 C41 C43 109.4(3) . . ? C44 C41 C4 111.9(2) . . ? C42 C41 C4 109.2(3) . . ? C43 C41 C4 109.2(3) . . ? C6 C61 N62 112.1(3) . . ? C63 N62 C67 112.2(3) . . ? C63 N62 C61 111.1(2) . . ? C67 N62 C61 109.8(2) . . ? N62 C63 C64 110.8(3) . . ? C63 C64 C65 110.8(3) . . ? C66 C65 C64 110.1(3) . . ? C65 C66 C67 111.9(3) . . ? N62 C67 C66 111.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.285 _refine_diff_density_min -1.774 _refine_diff_density_rms 0.125 # Attachment 'Zn2(L2)2Cl4.cif' data_dhzntb _database_code_depnum_ccdc_archive 'CCDC 660775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H52 Cl4 N4 O4 Zn2, 4(C H Cl3)' _chemical_formula_sum 'C38 H56 Cl16 N4 O4 Zn2' _chemical_formula_weight 1330.81 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1922(16) _cell_length_b 15.2573(17) _cell_length_c 15.8100(17) _cell_angle_alpha 90.166(2) _cell_angle_beta 107.680(2) _cell_angle_gamma 117.492(2) _cell_volume 2851.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6609 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.74 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.564 _exptl_absorpt_correction_T_max 0.680 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25571 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.82 _reflns_number_total 13277 _reflns_number_gt 11425 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart32 _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'DIRDIF 99' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material PLATON _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. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 431_ALERT_2_A Short Inter HL..A Contact Cl6S .. Cl6S .. 2.95 Ang. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1S 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C2S 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1V 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1T 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1U 302_ALERT_4_C Anion/Solvent Disorder ......................... 30.00 Perc. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 20.70 Deg. CL3V -C1V -CL6V 1.555 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 24.60 Deg. CL5V -C1V -CL2V 1.555 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 23.00 Deg. CL4V -C1V -CL1V 1.555 1.555 1.555 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 11.20 Deg. H1V -C1V -H1V' 1.555 1.555 1.555 The solvent molecules are chloroform. There is a short contact which is alleviated by disorder. The chloroform is rotationally disordered which accounts for anomolies in ADP's 912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1554 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 89 The data collection strategy used was to collect fully complete data to 2TH= 53deg. Some higher angle data were collected in the process and these have been included in the refinement. Please refer to the completeness statistics below #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 5963 5960 3 23.01 0.550 0.997 7954 7932 22 25.24 0.600 0.991 10322 10233 89 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.974 13139 12795 344 28.82 0.678 0.890 14920 13277 1643 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.35 Ratio 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.48 Ratio 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C41A 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C41B These are tBu groups 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.80 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? 154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. Values obtained from cell refinement checked. No issues found. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 30 Confirmed ; _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^)+(0.0559P)^2^+3.7785P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13277 _refine_ls_number_parameters 627 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Zn1 Zn 0.13767(2) 0.33325(2) 0.133565(19) 0.02196(8) Uani 1 1 d . . . Zn2 Zn 0.16448(2) 0.37036(2) 0.338436(19) 0.02233(8) Uani 1 1 d . . . Cl1 Cl -0.02641(5) 0.27281(5) 0.00292(4) 0.02816(14) Uani 1 1 d . . . Cl2 Cl 0.27464(6) 0.46341(5) 0.09804(5) 0.03191(15) Uani 1 1 d . . . Cl3 Cl 0.22124(6) 0.53211(5) 0.39345(4) 0.03080(14) Uani 1 1 d . . . Cl4 Cl 0.24803(5) 0.32211(5) 0.46978(4) 0.02952(14) Uani 1 1 d . . . O1A O 0.07388(14) 0.38026(13) 0.21152(11) 0.0234(4) Uani 1 1 d . . . C1A C -0.0318(2) 0.36645(18) 0.18790(16) 0.0216(5) Uani 1 1 d . . . C2A C -0.1158(2) 0.29039(19) 0.21409(17) 0.0241(5) Uani 1 1 d . . . C3A C -0.2267(2) 0.2761(2) 0.18290(17) 0.0263(5) Uani 1 1 d . . . H3A H -0.2829 0.2235 0.2005 0.032 Uiso 1 1 calc R . . C4A C -0.2571(2) 0.3360(2) 0.12738(17) 0.0252(5) Uani 1 1 d . . . C5A C -0.1706(2) 0.41426(19) 0.10529(17) 0.0246(5) Uani 1 1 d . . . H5A H -0.1880 0.4577 0.0687 0.030 Uiso 1 1 calc R . . C6A C -0.0605(2) 0.43025(19) 0.13523(16) 0.0226(5) Uani 1 1 d . . . C21A C -0.0930(2) 0.2255(2) 0.27453(19) 0.0301(6) Uani 1 1 d . . . H21A H -0.1557 0.1663 0.2785 0.036 Uiso 1 1 calc R . . N22A N 0.00641(19) 0.24322(17) 0.32271(16) 0.0301(5) Uani 1 1 d . . . O23A O 0.00420(18) 0.16976(17) 0.37588(16) 0.0454(6) Uani 1 1 d . . . H23A H 0.0701 0.1871 0.4107 0.068 Uiso 1 1 calc R . . C41A C -0.3784(2) 0.3201(2) 0.09063(19) 0.0317(6) Uani 1 1 d . . . C42A C -0.3773(3) 0.4195(3) 0.1062(3) 0.0505(9) Uani 1 1 d . . . H42A H -0.3275 0.4690 0.0784 0.076 Uiso 1 1 calc R . . H42B H -0.3495 0.4436 0.1711 0.076 Uiso 1 1 calc R . . H42C H -0.4542 0.4096 0.0792 0.076 Uiso 1 1 calc R . . C43A C -0.4261(3) 0.2843(3) -0.0115(2) 0.0489(9) Uani 1 1 d . . . H43A H -0.3765 0.3335 -0.0396 0.073 Uiso 1 1 calc R . . H43B H -0.5020 0.2772 -0.0360 0.073 Uiso 1 1 calc R . . H43C H -0.4302 0.2195 -0.0240 0.073 Uiso 1 1 calc R . . C44A C -0.4550(3) 0.2434(4) 0.1342(3) 0.0752(16) Uani 1 1 d . . . H44A H -0.5312 0.2353 0.1091 0.113 Uiso 1 1 calc R . . H44B H -0.4251 0.2664 0.1994 0.113 Uiso 1 1 calc R . . H44C H -0.4580 0.1789 0.1221 0.113 Uiso 1 1 calc R . . C61A C 0.0318(2) 0.51618(19) 0.11375(16) 0.0237(5) Uani 1 1 d . . . H61A H -0.0017 0.5466 0.0670 0.028 Uiso 1 1 calc R . . H61B H 0.0732 0.4913 0.0894 0.028 Uiso 1 1 calc R . . N62A N 0.11357(17) 0.59493(16) 0.19660(14) 0.0233(4) Uani 1 1 d . . . H62A H 0.1366 0.5635 0.2424 0.028 Uiso 1 1 calc R . . C63A C 0.0575(2) 0.6452(2) 0.22763(19) 0.0283(5) Uani 1 1 d . . . H63A H -0.0057 0.5948 0.2447 0.034 Uiso 1 1 calc R . . H63B H 0.0256 0.6732 0.1774 0.034 Uiso 1 1 calc R . . C64A C 0.1401(3) 0.7287(2) 0.3075(2) 0.0334(6) Uani 1 1 d . . . H64A H 0.1663 0.7000 0.3598 0.040 Uiso 1 1 calc R . . H64B H 0.1015 0.7624 0.3240 0.040 Uiso 1 1 calc R . . C65A C 0.2415(3) 0.8051(2) 0.2848(2) 0.0368(7) Uani 1 1 d . . . H65A H 0.2163 0.8376 0.2354 0.044 Uiso 1 1 calc R . . H65B H 0.2960 0.8577 0.3382 0.044 Uiso 1 1 calc R . . C66A C 0.2982(2) 0.7526(2) 0.2564(2) 0.0339(6) Uani 1 1 d . . . H66A H 0.3631 0.8020 0.2404 0.041 Uiso 1 1 calc R . . H66B H 0.3277 0.7241 0.3074 0.041 Uiso 1 1 calc R . . C67A C 0.2164(2) 0.6696(2) 0.17648(19) 0.0281(5) Uani 1 1 d . . . H67A H 0.1924 0.6989 0.1237 0.034 Uiso 1 1 calc R . . H67B H 0.2547 0.6348 0.1612 0.034 Uiso 1 1 calc R . . O1B O 0.25165(15) 0.35617(13) 0.26414(12) 0.0237(4) Uani 1 1 d . . . C1B C 0.3196(2) 0.31548(19) 0.28889(17) 0.0231(5) Uani 1 1 d . . . C2B C 0.2866(2) 0.2174(2) 0.25363(18) 0.0267(5) Uani 1 1 d . . . C3B C 0.3565(2) 0.1754(2) 0.28913(19) 0.0291(6) Uani 1 1 d . . . H3B H 0.3311 0.1077 0.2662 0.035 Uiso 1 1 calc R . . C4B C 0.4613(2) 0.2289(2) 0.35653(18) 0.0270(5) Uani 1 1 d . . . C5B C 0.4967(2) 0.3291(2) 0.38552(17) 0.0253(5) Uani 1 1 d . . . H5B H 0.5697 0.3689 0.4293 0.030 Uiso 1 1 calc R . . C6B C 0.4289(2) 0.37240(19) 0.35249(16) 0.0233(5) Uani 1 1 d . . . C21B C 0.1825(2) 0.1554(2) 0.17882(19) 0.0304(6) Uani 1 1 d . . . H21B H 0.1594 0.0862 0.1663 0.036 Uiso 1 1 calc R . . N22B N 0.12003(18) 0.18764(17) 0.12874(15) 0.0281(5) Uani 1 1 d . . . O23B O 0.02969(18) 0.11095(15) 0.05906(15) 0.0390(5) Uani 1 1 d . . . H23B H -0.0083 0.1343 0.0253 0.058 Uiso 1 1 calc R . . C41B C 0.5327(2) 0.1799(2) 0.4011(2) 0.0345(6) Uani 1 1 d . . . C42B C 0.6560(3) 0.2446(3) 0.4084(2) 0.0437(8) Uani 1 1 d . . . H42D H 0.6997 0.2118 0.4374 0.066 Uiso 1 1 calc R . . H42E H 0.6872 0.3104 0.4445 0.066 Uiso 1 1 calc R . . H42F H 0.6602 0.2532 0.3480 0.066 Uiso 1 1 calc R . . C43B C 0.4896(3) 0.0774(3) 0.3489(3) 0.0698(14) Uani 1 1 d . . . H43D H 0.5371 0.0487 0.3796 0.105 Uiso 1 1 calc R . . H43E H 0.4923 0.0842 0.2879 0.105 Uiso 1 1 calc R . . H43F H 0.4114 0.0333 0.3454 0.105 Uiso 1 1 calc R . . C44B C 0.5293(4) 0.1720(4) 0.4971(3) 0.0667(12) Uani 1 1 d . . . H44D H 0.5743 0.1410 0.5278 0.100 Uiso 1 1 calc R . . H44E H 0.4508 0.1308 0.4943 0.100 Uiso 1 1 calc R . . H44F H 0.5604 0.2392 0.5304 0.100 Uiso 1 1 calc R . . C61B C 0.4675(2) 0.47995(19) 0.38348(16) 0.0235(5) Uani 1 1 d . . . H61C H 0.5409 0.5087 0.4336 0.028 Uiso 1 1 calc R . . H61D H 0.4120 0.4842 0.4065 0.028 Uiso 1 1 calc R . . N62B N 0.48072(17) 0.54068(15) 0.30816(14) 0.0218(4) Uani 1 1 d . . . H62B H 0.4136 0.5090 0.2592 0.026 Uiso 1 1 calc R . . C63B C 0.5747(2) 0.5464(2) 0.27907(19) 0.0281(5) Uani 1 1 d . . . H63C H 0.5556 0.4780 0.2549 0.034 Uiso 1 1 calc R . . H63D H 0.6453 0.5735 0.3320 0.034 Uiso 1 1 calc R . . C64B C 0.5943(2) 0.6124(2) 0.2076(2) 0.0321(6) Uani 1 1 d . . . H64C H 0.6590 0.6171 0.1923 0.039 Uiso 1 1 calc R . . H64D H 0.5265 0.5817 0.1523 0.039 Uiso 1 1 calc R . . C65B C 0.6186(2) 0.7166(2) 0.2404(2) 0.0321(6) Uani 1 1 d . . . H65C H 0.6276 0.7575 0.1920 0.038 Uiso 1 1 calc R . . H65D H 0.6899 0.7498 0.2927 0.038 Uiso 1 1 calc R . . C66B C 0.5215(2) 0.7093(2) 0.26758(19) 0.0297(6) Uani 1 1 d . . . H66C H 0.5390 0.7773 0.2912 0.036 Uiso 1 1 calc R . . H66D H 0.4518 0.6814 0.2139 0.036 Uiso 1 1 calc R . . C67B C 0.5013(2) 0.64332(19) 0.33865(18) 0.0260(5) Uani 1 1 d . . . H67C H 0.5680 0.6751 0.3947 0.031 Uiso 1 1 calc R . . H67D H 0.4351 0.6372 0.3523 0.031 Uiso 1 1 calc R . . C1S C 0.1935(7) 0.9907(6) 0.5583(6) 0.0471(18) Uani 0.60 1 d P A 1 H1S H 0.1168 0.9505 0.5630 0.056 Uiso 0.60 1 calc PR A 1 Cl1S Cl 0.2977(2) 1.01020(15) 0.66201(15) 0.0608(5) Uani 0.60 1 d P A 1 Cl2S Cl 0.21130(18) 1.10710(12) 0.52936(13) 0.0682(5) Uani 0.60 1 d P A 1 Cl3S Cl 0.2073(2) 0.92603(18) 0.47459(18) 0.0946(8) Uani 0.60 1 d P A 1 C2S C 0.1479(13) 0.9807(11) 0.5247(9) 0.059(3) Uani 0.40 1 d P B 2 H2S H 0.0839 0.9138 0.5233 0.071 Uiso 0.40 1 calc PR B 2 Cl4S Cl 0.1594(6) 0.9850(4) 0.4199(3) 0.149(2) Uani 0.40 1 d P B 2 Cl5S Cl 0.2708(4) 0.9955(4) 0.6080(5) 0.1125(18) Uani 0.40 1 d P B 2 Cl6S Cl 0.1183(3) 1.0722(2) 0.5541(2) 0.0798(9) Uani 0.40 1 d P B 2 C1T C -0.1051(3) 0.6047(3) 0.4245(2) 0.0491(9) Uani 1 1 d . . . H1T H -0.1557 0.5912 0.4607 0.059 Uiso 1 1 calc R . . Cl1T Cl 0.03153(8) 0.63967(9) 0.49803(7) 0.0627(3) Uani 1 1 d . . . Cl2T Cl -0.15772(9) 0.49508(9) 0.34879(7) 0.0681(3) Uani 1 1 d . . . Cl3T Cl -0.10498(9) 0.70207(10) 0.36487(8) 0.0655(3) Uani 1 1 d . . . C1U C -0.0912(3) 0.8931(3) 0.1346(3) 0.0509(9) Uani 1 1 d . . . H1U H -0.0754 0.9367 0.0880 0.061 Uiso 1 1 calc R . . Cl1U Cl -0.12130(16) 0.95005(13) 0.21030(11) 0.1004(5) Uani 1 1 d . . . Cl2U Cl -0.20539(11) 0.77538(10) 0.07932(10) 0.0854(4) Uani 1 1 d . . . Cl3U Cl 0.02996(11) 0.88155(9) 0.18804(9) 0.0716(3) Uani 1 1 d . . . C1V C 0.2825(3) 0.9377(3) 0.0067(3) 0.0519(9) Uani 1 1 d D . . H1V H 0.2127 0.8719 -0.0217 0.062 Uiso 0.85 1 calc PR C 1 H1V' H 0.2209 0.8664 -0.0132 0.062 Uiso 0.15 1 calc PR C 2 Cl1V Cl 0.37248(15) 0.91992(13) 0.10089(12) 0.0782(4) Uani 0.85 1 d PD D 1 Cl2V Cl 0.35067(12) 0.98198(10) -0.07182(9) 0.0609(3) Uani 0.85 1 d PD D 1 Cl3V Cl 0.24394(10) 1.02135(11) 0.04120(11) 0.0591(3) Uani 0.85 1 d PD D 1 Cl4V Cl 0.4051(9) 0.9403(10) 0.0737(8) 0.096(4) Uiso 0.15 1 d PD D 2 Cl5V Cl 0.3015(9) 0.9910(8) -0.0877(6) 0.081(3) Uiso 0.15 1 d PD D 2 Cl6V Cl 0.2481(9) 1.0001(8) 0.0751(6) 0.067(3) Uiso 0.15 1 d PD D 2 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 Zn1 0.01799(14) 0.02201(14) 0.02073(14) 0.00513(10) 0.00261(11) 0.00813(11) Zn2 0.01804(14) 0.02421(15) 0.01960(14) 0.00589(11) 0.00303(11) 0.00831(11) Cl1 0.0251(3) 0.0286(3) 0.0229(3) 0.0036(2) -0.0009(2) 0.0125(3) Cl2 0.0249(3) 0.0313(3) 0.0300(3) 0.0101(3) 0.0088(3) 0.0065(3) Cl3 0.0336(3) 0.0271(3) 0.0269(3) 0.0031(2) 0.0049(3) 0.0143(3) Cl4 0.0232(3) 0.0351(3) 0.0237(3) 0.0111(2) 0.0031(2) 0.0120(3) O1A 0.0180(8) 0.0287(9) 0.0197(8) 0.0060(7) 0.0027(7) 0.0105(7) C1A 0.0172(11) 0.0238(12) 0.0178(11) 0.0028(9) 0.0020(9) 0.0077(9) C2A 0.0208(12) 0.0251(12) 0.0211(12) 0.0054(9) 0.0026(9) 0.0099(10) C3A 0.0199(12) 0.0281(13) 0.0231(12) 0.0052(10) 0.0049(10) 0.0071(10) C4A 0.0194(12) 0.0285(13) 0.0224(12) 0.0016(10) 0.0033(9) 0.0100(10) C5A 0.0232(12) 0.0263(12) 0.0211(12) 0.0033(9) 0.0035(10) 0.0119(10) C6A 0.0208(12) 0.0235(12) 0.0183(11) 0.0034(9) 0.0032(9) 0.0089(10) C21A 0.0217(13) 0.0274(13) 0.0313(14) 0.0119(11) 0.0056(11) 0.0064(11) N22A 0.0260(11) 0.0272(11) 0.0294(12) 0.0132(9) 0.0041(9) 0.0102(9) O23A 0.0280(11) 0.0391(12) 0.0501(14) 0.0287(10) 0.0000(10) 0.0095(9) C41A 0.0198(12) 0.0413(16) 0.0300(14) 0.0086(12) 0.0039(10) 0.0144(12) C42A 0.0348(17) 0.062(2) 0.058(2) -0.0038(18) 0.0084(15) 0.0310(17) C43A 0.0312(16) 0.060(2) 0.0391(18) -0.0067(15) -0.0073(13) 0.0214(16) C44A 0.0241(17) 0.114(4) 0.089(3) 0.067(3) 0.0238(19) 0.032(2) C61A 0.0222(12) 0.0251(12) 0.0197(11) 0.0056(9) 0.0052(9) 0.0095(10) N62A 0.0205(10) 0.0217(10) 0.0236(10) 0.0076(8) 0.0058(8) 0.0081(8) C63A 0.0242(13) 0.0270(13) 0.0315(14) 0.0055(10) 0.0104(11) 0.0101(11) C64A 0.0361(15) 0.0277(14) 0.0321(14) 0.0024(11) 0.0084(12) 0.0141(12) C65A 0.0283(14) 0.0237(13) 0.0471(17) 0.0021(12) 0.0038(13) 0.0093(11) C66A 0.0203(13) 0.0265(13) 0.0450(17) 0.0080(12) 0.0040(11) 0.0081(11) C67A 0.0196(12) 0.0277(13) 0.0346(14) 0.0098(11) 0.0097(11) 0.0092(10) O1B 0.0210(8) 0.0277(9) 0.0208(8) 0.0061(7) 0.0031(7) 0.0131(7) C1B 0.0214(12) 0.0263(12) 0.0210(11) 0.0087(9) 0.0065(9) 0.0116(10) C2B 0.0219(12) 0.0261(13) 0.0263(13) 0.0065(10) 0.0037(10) 0.0099(10) C3B 0.0260(13) 0.0249(13) 0.0297(13) 0.0047(10) 0.0023(11) 0.0114(11) C4B 0.0214(12) 0.0301(13) 0.0278(13) 0.0103(10) 0.0047(10) 0.0134(11) C5B 0.0172(11) 0.0304(13) 0.0231(12) 0.0075(10) 0.0038(9) 0.0092(10) C6B 0.0223(12) 0.0248(12) 0.0208(12) 0.0069(9) 0.0067(9) 0.0102(10) C21B 0.0252(13) 0.0228(12) 0.0349(15) 0.0033(10) 0.0026(11) 0.0099(11) N22B 0.0207(11) 0.0259(11) 0.0268(11) 0.0009(9) 0.0000(9) 0.0077(9) O23B 0.0310(11) 0.0268(10) 0.0385(12) -0.0043(8) -0.0106(9) 0.0116(9) C41B 0.0269(14) 0.0340(15) 0.0384(16) 0.0092(12) 0.0010(12) 0.0177(12) C42B 0.0297(15) 0.0430(18) 0.055(2) 0.0020(15) 0.0037(14) 0.0213(14) C43B 0.045(2) 0.0346(18) 0.101(3) -0.0048(19) -0.021(2) 0.0252(17) C44B 0.070(3) 0.099(3) 0.058(2) 0.046(2) 0.023(2) 0.061(3) C61B 0.0205(12) 0.0275(13) 0.0178(11) 0.0040(9) 0.0039(9) 0.0096(10) N62B 0.0172(10) 0.0235(10) 0.0207(10) 0.0033(8) 0.0040(8) 0.0081(8) C63B 0.0249(13) 0.0316(14) 0.0322(14) 0.0079(11) 0.0133(11) 0.0151(11) C64B 0.0284(14) 0.0361(15) 0.0318(14) 0.0077(11) 0.0145(11) 0.0132(12) C65B 0.0244(13) 0.0293(14) 0.0369(15) 0.0110(11) 0.0108(11) 0.0086(11) C66B 0.0234(13) 0.0285(13) 0.0346(14) 0.0083(11) 0.0072(11) 0.0121(11) C67B 0.0214(12) 0.0249(12) 0.0281(13) 0.0031(10) 0.0055(10) 0.0104(10) C1S 0.042(5) 0.034(3) 0.058(5) 0.014(3) 0.010(3) 0.016(3) Cl1S 0.0587(12) 0.0377(8) 0.0718(12) 0.0219(9) 0.0184(11) 0.0147(8) Cl2S 0.0831(13) 0.0380(8) 0.0698(11) 0.0116(7) 0.0080(10) 0.0296(8) Cl3S 0.119(2) 0.0664(13) 0.0864(15) -0.0211(11) 0.0159(14) 0.0473(13) C2S 0.063(9) 0.052(7) 0.054(8) 0.021(6) 0.023(6) 0.019(7) Cl4S 0.198(6) 0.136(4) 0.095(3) 0.000(3) 0.093(4) 0.042(4) Cl5S 0.064(3) 0.111(4) 0.163(5) 0.065(4) 0.042(3) 0.041(3) Cl6S 0.109(3) 0.0689(18) 0.0618(17) 0.0182(14) 0.0172(17) 0.0506(19) C1T 0.0335(17) 0.074(3) 0.0408(18) 0.0170(17) 0.0155(14) 0.0247(17) Cl1T 0.0440(5) 0.0844(7) 0.0477(5) 0.0101(5) 0.0026(4) 0.0297(5) Cl2T 0.0568(6) 0.0752(7) 0.0475(5) 0.0062(5) 0.0134(4) 0.0152(5) Cl3T 0.0464(5) 0.0931(8) 0.0759(7) 0.0404(6) 0.0315(5) 0.0420(5) C1U 0.055(2) 0.051(2) 0.055(2) 0.0165(17) 0.0274(18) 0.0272(18) Cl1U 0.1281(13) 0.1195(12) 0.0967(10) 0.0110(9) 0.0625(10) 0.0795(11) Cl2U 0.0721(8) 0.0619(7) 0.0975(10) 0.0125(6) 0.0407(7) 0.0061(6) Cl3U 0.0763(7) 0.0601(6) 0.0902(8) 0.0239(6) 0.0233(6) 0.0457(6) C1V 0.0381(18) 0.0413(18) 0.068(2) -0.0009(17) 0.0260(17) 0.0079(15) Cl1V 0.0883(11) 0.0916(11) 0.0883(11) 0.0470(9) 0.0487(9) 0.0587(9) Cl2V 0.0560(7) 0.0571(7) 0.0595(7) 0.0031(5) 0.0288(6) 0.0140(6) Cl3V 0.0398(6) 0.0605(8) 0.0704(9) -0.0106(7) 0.0105(6) 0.0243(6) _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 Zn1 O1A 2.0310(18) . ? Zn1 O1B 2.1085(17) . ? Zn1 N22B 2.116(2) . ? Zn1 Cl2 2.2679(7) . ? Zn1 Cl1 2.3715(7) . ? Zn2 O1B 2.0213(18) . ? Zn2 O1A 2.0775(17) . ? Zn2 N22A 2.121(2) . ? Zn2 Cl3 2.2853(8) . ? Zn2 Cl4 2.3620(7) . ? O1A C1A 1.342(3) . ? C1A C2A 1.402(4) . ? C1A C6A 1.404(3) . ? C2A C3A 1.407(4) . ? C2A C21A 1.454(4) . ? C3A C4A 1.389(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.402(4) . ? C4A C41A 1.537(4) . ? C5A C6A 1.387(3) . ? C5A H5A 0.9500 . ? C6A C61A 1.496(3) . ? C21A N22A 1.280(3) . ? C21A H21A 0.9500 . ? N22A O23A 1.397(3) . ? O23A H23A 0.8400 . ? C41A C44A 1.520(5) . ? C41A C42A 1.528(5) . ? C41A C43A 1.533(4) . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C61A N62A 1.512(3) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? N62A C63A 1.503(3) . ? N62A C67A 1.509(3) . ? N62A H62A 0.9300 . ? C63A C64A 1.517(4) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A C65A 1.525(4) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? C65A C66A 1.519(4) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C66A C67A 1.513(4) . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C67A H67A 0.9900 . ? C67A H67B 0.9900 . ? O1B C1B 1.339(3) . ? C1B C2B 1.400(4) . ? C1B C6B 1.405(3) . ? C2B C3B 1.400(4) . ? C2B C21B 1.456(4) . ? C3B C4B 1.388(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.395(4) . ? C4B C41B 1.533(4) . ? C5B C6B 1.386(4) . ? C5B H5B 0.9500 . ? C6B C61B 1.495(4) . ? C21B N22B 1.278(4) . ? C21B H21B 0.9500 . ? N22B O23B 1.406(3) . ? O23B H23B 0.8400 . ? C41B C43B 1.518(5) . ? C41B C42B 1.527(4) . ? C41B C44B 1.536(5) . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C61B N62B 1.514(3) . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? N62B C67B 1.502(3) . ? N62B C63B 1.505(3) . ? N62B H62B 0.9300 . ? C63B C64B 1.520(4) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B C65B 1.516(4) . ? C64B H64C 0.9900 . ? C64B H64D 0.9900 . ? C65B C66B 1.521(4) . ? C65B H65C 0.9900 . ? C65B H65D 0.9900 . ? C66B C67B 1.515(4) . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C67B H67C 0.9900 . ? C67B H67D 0.9900 . ? C1S Cl1S 1.756(8) . ? C1S Cl2S 1.757(8) . ? C1S Cl3S 1.758(10) . ? C1S H1S 1.0000 . ? C2S Cl4S 1.712(15) . ? C2S Cl6S 1.731(16) . ? C2S Cl5S 1.752(14) . ? C2S H2S 1.0000 . ? C1T Cl1T 1.752(3) . ? C1T Cl2T 1.755(4) . ? C1T Cl3T 1.762(4) . ? C1T H1T 1.0000 . ? C1U Cl1U 1.738(4) . ? C1U Cl2U 1.749(4) . ? C1U Cl3U 1.760(4) . ? C1U H1U 1.0000 . ? C1V Cl4V 1.723(10) . ? C1V Cl5V 1.735(9) . ? C1V Cl3V 1.745(4) . ? C1V Cl6V 1.748(9) . ? C1V Cl2V 1.751(4) . ? C1V Cl1V 1.758(4) . ? C1V H1V 1.0000 . ? C1V H1V' 1.0000 . ? 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 O1A Zn1 O1B 77.90(7) . . ? O1A Zn1 N22B 121.18(8) . . ? O1B Zn1 N22B 82.69(8) . . ? O1A Zn1 Cl2 112.05(6) . . ? O1B Zn1 Cl2 90.85(5) . . ? N22B Zn1 Cl2 123.28(7) . . ? O1A Zn1 Cl1 94.79(5) . . ? O1B Zn1 Cl1 163.99(5) . . ? N22B Zn1 Cl1 89.20(6) . . ? Cl2 Zn1 Cl1 105.12(3) . . ? O1B Zn2 O1A 78.83(7) . . ? O1B Zn2 N22A 116.21(9) . . ? O1A Zn2 N22A 81.91(8) . . ? O1B Zn2 Cl3 114.54(6) . . ? O1A Zn2 Cl3 91.87(5) . . ? N22A Zn2 Cl3 126.36(7) . . ? O1B Zn2 Cl4 97.61(5) . . ? O1A Zn2 Cl4 167.66(5) . . ? N22A Zn2 Cl4 89.24(6) . . ? Cl3 Zn2 Cl4 100.32(3) . . ? C1A O1A Zn1 126.34(15) . . ? C1A O1A Zn2 124.14(15) . . ? Zn1 O1A Zn2 100.63(8) . . ? O1A C1A C2A 122.5(2) . . ? O1A C1A C6A 119.5(2) . . ? C2A C1A C6A 118.0(2) . . ? C1A C2A C3A 119.8(2) . . ? C1A C2A C21A 122.6(2) . . ? C3A C2A C21A 117.6(2) . . ? C4A C3A C2A 122.5(2) . . ? C4A C3A H3A 118.8 . . ? C2A C3A H3A 118.8 . . ? C3A C4A C5A 116.7(2) . . ? C3A C4A C41A 123.4(2) . . ? C5A C4A C41A 120.0(2) . . ? C6A C5A C4A 122.1(2) . . ? C6A C5A H5A 119.0 . . ? C4A C5A H5A 119.0 . . ? C5A C6A C1A 120.8(2) . . ? C5A C6A C61A 121.5(2) . . ? C1A C6A C61A 117.7(2) . . ? N22A C21A C2A 123.9(2) . . ? N22A C21A H21A 118.0 . . ? C2A C21A H21A 118.0 . . ? C21A N22A O23A 112.2(2) . . ? C21A N22A Zn2 128.96(19) . . ? O23A N22A Zn2 118.65(16) . . ? N22A O23A H23A 109.5 . . ? C44A C41A C42A 109.5(3) . . ? C44A C41A C43A 109.3(3) . . ? C42A C41A C43A 107.2(3) . . ? C44A C41A C4A 111.9(2) . . ? C42A C41A C4A 110.0(2) . . ? C43A C41A C4A 108.8(2) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41A C43A H43A 109.5 . . ? C41A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C41A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C41A C44A H44A 109.5 . . ? C41A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C41A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C6A C61A N62A 111.2(2) . . ? C6A C61A H61A 109.4 . . ? N62A C61A H61A 109.4 . . ? C6A C61A H61B 109.4 . . ? N62A C61A H61B 109.4 . . ? H61A C61A H61B 108.0 . . ? C63A N62A C67A 111.6(2) . . ? C63A N62A C61A 110.89(19) . . ? C67A N62A C61A 109.3(2) . . ? C63A N62A H62A 108.3 . . ? C67A N62A H62A 108.3 . . ? C61A N62A H62A 108.3 . . ? N62A C63A C64A 111.7(2) . . ? N62A C63A H63A 109.3 . . ? C64A C63A H63A 109.3 . . ? N62A C63A H63B 109.3 . . ? C64A C63A H63B 109.3 . . ? H63A C63A H63B 107.9 . . ? C63A C64A C65A 110.6(2) . . ? C63A C64A H64A 109.5 . . ? C65A C64A H64A 109.5 . . ? C63A C64A H64B 109.5 . . ? C65A C64A H64B 109.5 . . ? H64A C64A H64B 108.1 . . ? C66A C65A C64A 109.4(2) . . ? C66A C65A H65A 109.8 . . ? C64A C65A H65A 109.8 . . ? C66A C65A H65B 109.8 . . ? C64A C65A H65B 109.8 . . ? H65A C65A H65B 108.2 . . ? C67A C66A C65A 111.3(2) . . ? C67A C66A H66A 109.4 . . ? C65A C66A H66A 109.4 . . ? C67A C66A H66B 109.4 . . ? C65A C66A H66B 109.4 . . ? H66A C66A H66B 108.0 . . ? N62A C67A C66A 111.1(2) . . ? N62A C67A H67A 109.4 . . ? C66A C67A H67A 109.4 . . ? N62A C67A H67B 109.4 . . ? C66A C67A H67B 109.4 . . ? H67A C67A H67B 108.0 . . ? C1B O1B Zn2 124.00(15) . . ? C1B O1B Zn1 126.13(16) . . ? Zn2 O1B Zn1 99.91(7) . . ? O1B C1B C2B 122.6(2) . . ? O1B C1B C6B 119.6(2) . . ? C2B C1B C6B 117.7(2) . . ? C1B C2B C3B 119.9(2) . . ? C1B C2B C21B 123.2(2) . . ? C3B C2B C21B 116.8(2) . . ? C4B C3B C2B 122.5(3) . . ? C4B C3B H3B 118.8 . . ? C2B C3B H3B 118.8 . . ? C3B C4B C5B 116.7(2) . . ? C3B C4B C41B 122.2(3) . . ? C5B C4B C41B 121.0(2) . . ? C6B C5B C4B 122.1(2) . . ? C6B C5B H5B 118.9 . . ? C4B C5B H5B 118.9 . . ? C5B C6B C1B 120.6(2) . . ? C5B C6B C61B 121.9(2) . . ? C1B C6B C61B 117.5(2) . . ? N22B C21B C2B 124.6(3) . . ? N22B C21B H21B 117.7 . . ? C2B C21B H21B 117.7 . . ? C21B N22B O23B 110.9(2) . . ? C21B N22B Zn1 130.28(19) . . ? O23B N22B Zn1 118.80(16) . . ? N22B O23B H23B 109.5 . . ? C43B C41B C42B 107.7(3) . . ? C43B C41B C4B 112.0(2) . . ? C42B C41B C4B 111.2(2) . . ? C43B C41B C44B 110.8(3) . . ? C42B C41B C44B 107.9(3) . . ? C4B C41B C44B 107.2(3) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C6B C61B N62B 111.7(2) . . ? C6B C61B H61C 109.3 . . ? N62B C61B H61C 109.3 . . ? C6B C61B H61D 109.3 . . ? N62B C61B H61D 109.3 . . ? H61C C61B H61D 107.9 . . ? C67B N62B C63B 111.4(2) . . ? C67B N62B C61B 109.35(19) . . ? C63B N62B C61B 110.79(19) . . ? C67B N62B H62B 108.4 . . ? C63B N62B H62B 108.4 . . ? C61B N62B H62B 108.4 . . ? N62B C63B C64B 111.7(2) . . ? N62B C63B H63C 109.3 . . ? C64B C63B H63C 109.3 . . ? N62B C63B H63D 109.3 . . ? C64B C63B H63D 109.3 . . ? H63C C63B H63D 107.9 . . ? C65B C64B C63B 111.0(2) . . ? C65B C64B H64C 109.4 . . ? C63B C64B H64C 109.4 . . ? C65B C64B H64D 109.4 . . ? C63B C64B H64D 109.4 . . ? H64C C64B H64D 108.0 . . ? C64B C65B C66B 109.6(2) . . ? C64B C65B H65C 109.8 . . ? C66B C65B H65C 109.8 . . ? C64B C65B H65D 109.8 . . ? C66B C65B H65D 109.8 . . ? H65C C65B H65D 108.2 . . ? C67B C66B C65B 111.4(2) . . ? C67B C66B H66C 109.3 . . ? C65B C66B H66C 109.3 . . ? C67B C66B H66D 109.3 . . ? C65B C66B H66D 109.3 . . ? H66C C66B H66D 108.0 . . ? N62B C67B C66B 111.6(2) . . ? N62B C67B H67C 109.3 . . ? C66B C67B H67C 109.3 . . ? N62B C67B H67D 109.3 . . ? C66B C67B H67D 109.3 . . ? H67C C67B H67D 108.0 . . ? Cl1S C1S Cl2S 109.4(4) . . ? Cl1S C1S Cl3S 109.4(5) . . ? Cl2S C1S Cl3S 109.1(5) . . ? Cl1S C1S H1S 109.7 . . ? Cl2S C1S H1S 109.7 . . ? Cl3S C1S H1S 109.7 . . ? Cl4S C2S Cl6S 111.2(8) . . ? Cl4S C2S Cl5S 112.3(10) . . ? Cl6S C2S Cl5S 108.6(8) . . ? Cl4S C2S H2S 108.2 . . ? Cl6S C2S H2S 108.2 . . ? Cl5S C2S H2S 108.2 . . ? Cl1T C1T Cl2T 110.5(2) . . ? Cl1T C1T Cl3T 110.5(2) . . ? Cl2T C1T Cl3T 110.0(2) . . ? Cl1T C1T H1T 108.6 . . ? Cl2T C1T H1T 108.6 . . ? Cl3T C1T H1T 108.6 . . ? Cl1U C1U Cl2U 111.9(2) . . ? Cl1U C1U Cl3U 111.4(2) . . ? Cl2U C1U Cl3U 109.7(2) . . ? Cl1U C1U H1U 107.9 . . ? Cl2U C1U H1U 107.9 . . ? Cl3U C1U H1U 107.9 . . ? Cl4V C1V Cl5V 110.3(6) . . ? Cl4V C1V Cl3V 119.0(5) . . ? Cl5V C1V Cl3V 93.1(4) . . ? Cl4V C1V Cl6V 106.2(6) . . ? Cl5V C1V Cl6V 113.6(5) . . ? Cl3V C1V Cl6V 20.7(3) . . ? Cl4V C1V Cl2V 86.6(5) . . ? Cl5V C1V Cl2V 24.6(3) . . ? Cl3V C1V Cl2V 111.2(2) . . ? Cl6V C1V Cl2V 129.5(4) . . ? Cl4V C1V Cl1V 23.0(4) . . ? Cl5V C1V Cl1V 133.3(4) . . ? Cl3V C1V Cl1V 109.5(2) . . ? Cl6V C1V Cl1V 91.8(4) . . ? Cl2V C1V Cl1V 109.6(2) . . ? Cl4V C1V H1V 119.7 . . ? Cl5V C1V H1V 101.0 . . ? Cl3V C1V H1V 108.8 . . ? Cl6V C1V H1V 106.2 . . ? Cl2V C1V H1V 108.8 . . ? Cl1V C1V H1V 108.8 . . ? Cl4V C1V H1V' 108.9 . . ? Cl5V C1V H1V' 108.9 . . ? Cl3V C1V H1V' 115.3 . . ? Cl6V C1V H1V' 108.9 . . ? Cl2V C1V H1V' 112.6 . . ? Cl1V C1V H1V' 97.7 . . ? H1V C1V H1V' 11.2 . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.175 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.084 # Attachment 'Cu(L2)2(NO3)2.cif' data_rf0005 _database_code_depnum_ccdc_archive 'CCDC 683051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Ross Forgan' _exptl_crystal_recrystallization_method 'MeOH/Et2O diffusion' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H52 Cu N6 O10' _chemical_formula_sum 'C34 H52 Cu N6 O10' _chemical_formula_weight 768.36 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' N N 0.0061 0.0033 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8940(6) _cell_length_b 11.1620(6) _cell_length_c 14.8410(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.682(3) _cell_angle_gamma 90.00 _cell_volume 1817.92(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7043 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.47 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6668 _exptl_absorpt_correction_T_max 0.8500 _exptl_absorpt_process_details 'SADABS 2004/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28245 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.50 _reflns_number_total 5192 _reflns_number_gt 4429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _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. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 241_ALERT_2_B Check High Ueq as Compared to Neighbors for O3S 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.22 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.06 Ratio 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1S 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cu1 This is probably due to disorder in the NO3 group which is coordinated to Cu1 Attempts to model it in parts produced a poorer quality solution. 420_ALERT_2_B D-H Without Acceptor O2 - H2 ... ? There is a hydrogen bond between O2-H2...O1 which is at 1.919 ang. The Angle is not ideal but an interaction clearly exists. 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 362 The data collection strategy used was to collect fully complete data to 2TH= 53deg. Some higher angle data were collected in the process and these have been included in the refinement. Please refer to the completeness statistics below #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1904 1904 0 23.01 0.550 1.000 2542 2542 0 25.24 0.600 1.000 3295 3295 0 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 1.000 4191 4191 0 29.84 0.700 0.963 5229 5035 194 30.50 0.714 0.935 5554 5192 362 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.71 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 These are the values output by saint. 794_ALERT_5_G Check Predicted Bond Valency for Cu1 (2) 2.25 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2 Confirmed ; _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^)+(0.0694P)^2^+0.6647P] 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_extinction_coef ? _refine_ls_number_reflns 5192 _refine_ls_number_parameters 237 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.0000 0.5000 0.0000 0.02162(9) Uani 1 2 d S . . O1 O 0.07220(9) 0.62547(10) 0.09198(8) 0.0243(2) Uani 1 1 d . . . C1 C 0.01859(13) 0.70043(13) 0.13144(10) 0.0207(3) Uani 1 1 d . . . C2 C -0.10763(13) 0.69821(13) 0.11221(10) 0.0219(3) Uani 1 1 d . . . C3 C -0.15654(13) 0.77697(13) 0.16201(11) 0.0240(3) Uani 1 1 d . . . H3 H -0.2414 0.7734 0.1481 0.029 Uiso 1 1 calc R . . C4 C -0.08640(13) 0.85894(13) 0.23004(11) 0.0242(3) Uani 1 1 d . . . C5 C 0.03771(13) 0.86347(13) 0.24535(10) 0.0244(3) Uani 1 1 d . . . H5 H 0.0884 0.9196 0.2912 0.029 Uiso 1 1 calc R . . C6 C 0.08963(12) 0.78979(13) 0.19669(10) 0.0214(3) Uani 1 1 d . . . C21 C -0.19277(13) 0.61931(13) 0.04161(10) 0.0232(3) Uani 1 1 d . . . H21 H -0.2766 0.6263 0.0309 0.028 Uiso 1 1 calc R . . N22 N -0.16244(11) 0.54053(12) -0.00754(9) 0.0227(2) Uani 1 1 d . . . O2 O -0.26099(10) 0.47714(11) -0.07356(9) 0.0299(3) Uani 1 1 d D . . H2 H -0.2238(7) 0.4244(10) -0.0865(3) 0.045 Uiso 1 1 d RD . . C41 C -0.13672(14) 0.93751(15) 0.29013(12) 0.0285(3) Uani 1 1 d . . . C42 C -0.0916(2) 1.06694(17) 0.29316(18) 0.0461(5) Uani 1 1 d . . . H42A H -0.0025 1.0686 0.3249 0.069 Uiso 1 1 calc R . . H42B H -0.1265 1.1170 0.3301 0.069 Uiso 1 1 calc R . . H42C H -0.1169 1.0978 0.2264 0.069 Uiso 1 1 calc R . . C43 C -0.09068(17) 0.8868(2) 0.39468(13) 0.0414(4) Uani 1 1 d . . . H43A H -0.1199 0.8044 0.3929 0.062 Uiso 1 1 calc R . . H43B H -0.1214 0.9363 0.4348 0.062 Uiso 1 1 calc R . . H43C H -0.0014 0.8874 0.4229 0.062 Uiso 1 1 calc R . . C44 C -0.27637(15) 0.93840(19) 0.24823(14) 0.0402(4) Uani 1 1 d . . . H44A H -0.3069 0.9654 0.1802 0.060 Uiso 1 1 calc R . . H44B H -0.3050 0.9930 0.2865 0.060 Uiso 1 1 calc R . . H44C H -0.3065 0.8574 0.2512 0.060 Uiso 1 1 calc R . . C61 C 0.22198(12) 0.80238(13) 0.21300(10) 0.0220(3) Uani 1 1 d . . . H61A H 0.2564 0.7219 0.2117 0.026 Uiso 1 1 calc R . . H61B H 0.2667 0.8372 0.2785 0.026 Uiso 1 1 calc R . . N62 N 0.24122(11) 0.88089(11) 0.13677(9) 0.0224(2) Uani 1 1 d D . . H62 H 0.1915(8) 0.8626(3) 0.0795(10) 0.027 Uiso 1 1 d RD . . C63 C 0.36525(14) 0.86014(16) 0.13528(12) 0.0302(3) Uani 1 1 d . . . H63A H 0.3731 0.7750 0.1199 0.036 Uiso 1 1 calc R . . H63B H 0.4282 0.8774 0.2007 0.036 Uiso 1 1 calc R . . C64 C 0.38634(16) 0.93931(17) 0.05987(13) 0.0347(4) Uani 1 1 d . . . H64A H 0.3286 0.9164 -0.0063 0.042 Uiso 1 1 calc R . . H64B H 0.4701 0.9265 0.0629 0.042 Uiso 1 1 calc R . . C65 C 0.36903(18) 1.07131(18) 0.07746(15) 0.0405(4) Uani 1 1 d . . . H65A H 0.4322 1.0969 0.1405 0.049 Uiso 1 1 calc R . . H65B H 0.3778 1.1204 0.0250 0.049 Uiso 1 1 calc R . . C66 C 0.24334(18) 1.09024(17) 0.07899(15) 0.0399(4) Uani 1 1 d . . . H66A H 0.1806 1.0720 0.0137 0.048 Uiso 1 1 calc R . . H66B H 0.2341 1.1752 0.0939 0.048 Uiso 1 1 calc R . . C67 C 0.22366(18) 1.01057(14) 0.15491(14) 0.0326(4) Uani 1 1 d . . . H67A H 0.2819 1.0334 0.2209 0.039 Uiso 1 1 calc R . . H67B H 0.1401 1.0227 0.1526 0.039 Uiso 1 1 calc R . . N1S N -0.06480(13) 0.24607(15) 0.07897(10) 0.0354(3) Uani 1 1 d . . . O2S O -0.17292(13) 0.26797(14) 0.05745(12) 0.0495(4) Uani 1 1 d . . . O3S O 0.01408(16) 0.3192(2) 0.12689(11) 0.0743(6) Uani 1 1 d . . . O4S O -0.04092(15) 0.14945(16) 0.04425(11) 0.0547(4) 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 Cu1 0.01765(14) 0.02413(14) 0.02305(14) -0.00519(8) 0.00782(10) -0.00224(8) O1 0.0194(5) 0.0269(5) 0.0278(5) -0.0077(4) 0.0104(4) -0.0022(4) C1 0.0207(6) 0.0220(6) 0.0211(6) -0.0017(5) 0.0100(5) -0.0022(5) C2 0.0208(6) 0.0231(6) 0.0237(6) -0.0010(5) 0.0107(5) -0.0023(5) C3 0.0207(6) 0.0266(7) 0.0278(7) -0.0013(5) 0.0127(5) -0.0016(5) C4 0.0241(7) 0.0257(7) 0.0264(7) -0.0020(5) 0.0137(5) -0.0009(5) C5 0.0239(7) 0.0257(7) 0.0249(7) -0.0043(5) 0.0110(5) -0.0040(5) C6 0.0183(6) 0.0245(6) 0.0226(6) -0.0018(5) 0.0091(5) -0.0028(5) C21 0.0180(6) 0.0264(7) 0.0260(7) -0.0003(5) 0.0093(5) -0.0023(5) N22 0.0172(5) 0.0240(6) 0.0243(6) -0.0028(5) 0.0050(4) -0.0037(5) O2 0.0193(5) 0.0287(5) 0.0344(6) -0.0092(4) 0.0023(4) -0.0023(4) C41 0.0251(7) 0.0317(8) 0.0320(8) -0.0080(6) 0.0148(6) -0.0012(6) C42 0.0490(11) 0.0310(9) 0.0707(14) -0.0131(9) 0.0370(10) -0.0025(8) C43 0.0394(9) 0.0582(12) 0.0315(8) -0.0066(8) 0.0190(7) 0.0062(8) C44 0.0273(8) 0.0534(11) 0.0420(9) -0.0147(8) 0.0159(7) 0.0040(8) C61 0.0196(6) 0.0253(7) 0.0216(6) -0.0012(5) 0.0086(5) -0.0031(5) N62 0.0193(5) 0.0266(6) 0.0222(6) -0.0012(4) 0.0090(4) -0.0019(5) C63 0.0212(7) 0.0388(8) 0.0347(8) 0.0030(6) 0.0155(6) 0.0015(6) C64 0.0291(8) 0.0464(10) 0.0353(8) 0.0036(7) 0.0198(7) -0.0014(7) C65 0.0416(10) 0.0417(10) 0.0443(10) 0.0049(8) 0.0234(8) -0.0103(8) C66 0.0458(10) 0.0323(9) 0.0493(11) 0.0084(7) 0.0269(9) -0.0001(8) C67 0.0386(9) 0.0263(8) 0.0415(9) 0.0021(6) 0.0249(8) 0.0015(6) N1S 0.0309(7) 0.0493(9) 0.0259(7) 0.0009(6) 0.0109(5) 0.0000(6) O2S 0.0322(7) 0.0517(8) 0.0662(9) 0.0070(7) 0.0208(6) -0.0006(6) O3S 0.0542(10) 0.1208(18) 0.0355(8) -0.0178(9) 0.0037(7) -0.0391(11) O4S 0.0566(9) 0.0587(9) 0.0515(9) 0.0068(7) 0.0237(7) 0.0195(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 Cu1 O1 1.9126(10) 3_565 ? Cu1 O1 1.9126(10) . ? Cu1 N22 1.9451(12) 3_565 ? Cu1 N22 1.9451(12) . ? O1 C1 1.3182(17) . ? C1 C2 1.4161(19) . ? C1 C6 1.4198(19) . ? C2 C3 1.4103(19) . ? C2 C21 1.4424(19) . ? C3 C4 1.379(2) . ? C3 H3 0.9500 . ? C4 C5 1.405(2) . ? C4 C41 1.528(2) . ? C5 C6 1.3868(19) . ? C5 H5 0.9500 . ? C6 C61 1.5042(19) . ? C21 N22 1.2800(19) . ? C21 H21 0.9500 . ? N22 O2 1.3960(15) . ? O2 H2 0.8027 . ? C41 C44 1.533(2) . ? C41 C42 1.536(3) . ? C41 C43 1.540(2) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C61 N62 1.5165(18) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? N62 C67 1.501(2) . ? N62 C63 1.5018(18) . ? N62 H62 0.8523 . ? C63 C64 1.521(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.524(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.519(3) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.523(2) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? N1S O2S 1.224(2) . ? N1S O3S 1.240(2) . ? N1S O4S 1.274(2) . ? 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 O1 Cu1 O1 180.00(6) 3_565 . ? O1 Cu1 N22 91.91(5) 3_565 3_565 ? O1 Cu1 N22 88.09(5) . 3_565 ? O1 Cu1 N22 88.09(5) 3_565 . ? O1 Cu1 N22 91.91(5) . . ? N22 Cu1 N22 180.00(7) 3_565 . ? C1 O1 Cu1 128.38(9) . . ? O1 C1 C2 123.79(13) . . ? O1 C1 C6 119.10(12) . . ? C2 C1 C6 117.10(12) . . ? C3 C2 C1 120.19(13) . . ? C3 C2 C21 116.44(13) . . ? C1 C2 C21 123.35(13) . . ? C4 C3 C2 122.80(13) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 116.32(13) . . ? C3 C4 C41 123.06(13) . . ? C5 C4 C41 120.56(13) . . ? C6 C5 C4 123.05(13) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C1 120.29(13) . . ? C5 C6 C61 120.62(12) . . ? C1 C6 C61 119.08(12) . . ? N22 C21 C2 124.07(13) . . ? N22 C21 H21 118.0 . . ? C2 C21 H21 118.0 . . ? C21 N22 O2 113.79(12) . . ? C21 N22 Cu1 128.24(10) . . ? O2 N22 Cu1 117.97(9) . . ? N22 O2 H2 98.6 . . ? C4 C41 C44 111.96(13) . . ? C4 C41 C42 110.23(13) . . ? C44 C41 C42 108.53(16) . . ? C4 C41 C43 108.05(14) . . ? C44 C41 C43 108.65(14) . . ? C42 C41 C43 109.38(15) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C6 C61 N62 112.56(11) . . ? C6 C61 H61A 109.1 . . ? N62 C61 H61A 109.1 . . ? C6 C61 H61B 109.1 . . ? N62 C61 H61B 109.1 . . ? H61A C61 H61B 107.8 . . ? C67 N62 C63 110.90(13) . . ? C67 N62 C61 110.60(11) . . ? C63 N62 C61 110.70(11) . . ? C67 N62 H62 108.6 . . ? C63 N62 H62 104.8 . . ? C61 N62 H62 111.0 . . ? N62 C63 C64 111.28(13) . . ? N62 C63 H63A 109.4 . . ? C64 C63 H63A 109.4 . . ? N62 C63 H63B 109.4 . . ? C64 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? C63 C64 C65 111.36(14) . . ? C63 C64 H64A 109.4 . . ? C65 C64 H64A 109.4 . . ? C63 C64 H64B 109.4 . . ? C65 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? C66 C65 C64 109.62(15) . . ? C66 C65 H65A 109.7 . . ? C64 C65 H65A 109.7 . . ? C66 C65 H65B 109.7 . . ? C64 C65 H65B 109.7 . . ? H65A C65 H65B 108.2 . . ? C65 C66 C67 111.28(16) . . ? C65 C66 H66A 109.4 . . ? C67 C66 H66A 109.4 . . ? C65 C66 H66B 109.4 . . ? C67 C66 H66B 109.4 . . ? H66A C66 H66B 108.0 . . ? N62 C67 C66 111.01(14) . . ? N62 C67 H67A 109.4 . . ? C66 C67 H67A 109.4 . . ? N62 C67 H67B 109.4 . . ? C66 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? O2S N1S O3S 120.29(19) . . ? O2S N1S O4S 116.05(16) . . ? O3S N1S O4S 123.51(18) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.917 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.094