Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal SOciety Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_contact_author_name 'Olof Kristiansson' _publ_contact_author_address ; Department of Chemistry SLU Box 7015, S-75007 Uppsala, Sweden ; _publ_contact_author_email olof.kristiansson@kemi.slu.se _publ_contact_author_fax '+18673476' _publ_contact_author_phone '+18672216' _publ_section_title ; Structure and Host-Guest Properties of the Nanoporous Tetrakis(p-nitrobenzoato)diaquacopper(II) Framework ; _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name _publ_author_address 'Kristiansson, Olof' ; Department of Chemistry SLU Box 7015 S-75007 Uppsala Sweden ; 'Tergenius, Lars-Erik' ; ? ; data_tetrakis(p-nitrobenzoato)diaquacopper(II)acetonesolvate _database_code_CSD 157260 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(4-nitrobenzoato)diaquacopper(II) acetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H26 Cu2 N4 O19' _chemical_formula_weight 885.64 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7335(9) _cell_length_b 11.9248(15) _cell_length_c 12.4536(16) _cell_angle_alpha 101.657(2) _cell_angle_beta 104.520(2) _cell_angle_gamma 97.283(2) _cell_volume 931.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2523 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6733 _exptl_absorpt_correction_T_max 0.7490 _exptl_absorpt_process_details 'Sadabs' _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_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ; Neglible as determined from a repetition of the first 50 frames at the end of the experiment ; _diffrn_reflns_number 5556 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3957 _reflns_number_gt 2523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998)' _computing_cell_refinement 'Bruker SMART and SAINT (1998)' _computing_data_reduction 'Bruker SAINT (1998)' _computing_structure_solution 'Bruker SHELXTL (1998)' _computing_structure_refinement 'Bruker SHELXTL (1998)' _computing_molecular_graphics 'Bruker SHELXTL (1998)' _computing_publication_material 'Bruker SHELXTL (1998)' _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^)+(0.0616P)^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 SHELXL _refine_ls_extinction_coef 0.0033(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3957 _refine_ls_number_parameters 282 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.918 _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 Cu1 Cu -0.16511(8) -0.06221(5) 0.01006(5) 0.02889(19) Uani 1 1 d . . . O11 O 0.1065(5) 0.1855(3) 0.1014(3) 0.0426(8) Uani 1 1 d . . . O12 O -0.1794(5) 0.0808(3) 0.1168(3) 0.0430(8) Uani 1 1 d . . . O13 O -0.0805(8) 0.6721(4) 0.4309(5) 0.1004(18) Uani 1 1 d . . . O14 O -0.3691(9) 0.5772(4) 0.4296(5) 0.113(2) Uani 1 1 d . . . N11 N -0.2043(9) 0.5826(4) 0.4071(5) 0.0676(14) Uani 1 1 d . . . C11 C -0.0468(7) 0.1734(4) 0.1413(4) 0.0337(10) Uani 1 1 d . . . C12 C -0.0789(7) 0.2775(4) 0.2196(4) 0.0366(11) Uani 1 1 d . . . C13 C 0.0630(8) 0.3808(4) 0.2509(4) 0.0488(13) Uani 1 1 d . . . H13 H 0.1844 0.3835 0.2280 0.059 Uiso 1 1 calc R . . C14 C 0.0270(9) 0.4800(5) 0.3155(5) 0.0539(14) Uani 1 1 d . . . H14 H 0.1237 0.5493 0.3378 0.065 Uiso 1 1 calc R . . C15 C -0.1562(9) 0.4740(4) 0.3463(5) 0.0472(13) Uani 1 1 d . . . C16 C -0.2945(9) 0.3729(4) 0.3217(5) 0.0522(14) Uani 1 1 d . . . H16 H -0.4136 0.3705 0.3468 0.063 Uiso 1 1 calc R . . C17 C -0.2544(8) 0.2734(4) 0.2583(4) 0.0445(13) Uani 1 1 d . . . H17 H -0.3465 0.2031 0.2414 0.053 Uiso 1 1 calc R . . O21 O 0.3100(5) -0.0002(3) 0.1167(3) 0.0424(8) Uani 1 1 d . . . O22 O 0.0269(5) -0.1036(3) 0.1363(3) 0.0442(8) Uani 1 1 d . . . O23 O 0.9105(6) -0.1095(3) 0.6012(3) 0.0612(10) Uani 1 1 d . . . O24 O 0.6401(7) -0.2004(3) 0.6288(3) 0.0625(11) Uani 1 1 d . . . N21 N 0.7245(7) -0.1500(3) 0.5725(3) 0.0424(10) Uani 1 1 d . . . C21 C 0.2182(7) -0.0637(4) 0.1661(4) 0.0344(10) Uani 1 1 d . . . C22 C 0.3510(7) -0.0932(4) 0.2683(4) 0.0315(10) Uani 1 1 d . . . C23 C 0.5668(7) -0.0601(4) 0.2991(4) 0.0386(11) Uani 1 1 d . . . H23 H 0.6290 -0.0238 0.2532 0.046 Uiso 1 1 calc R . . C24 C 0.6896(8) -0.0806(4) 0.3971(4) 0.0406(12) Uani 1 1 d . . . H24 H 0.8339 -0.0572 0.4184 0.049 Uiso 1 1 calc R . . C25 C 0.5951(7) -0.1361(4) 0.4627(4) 0.0362(11) Uani 1 1 d . . . C26 C 0.3818(8) -0.1718(4) 0.4331(4) 0.0417(12) Uani 1 1 d . . . H26 H 0.3207 -0.2093 0.4787 0.050 Uiso 1 1 calc R . . C27 C 0.2605(7) -0.1510(4) 0.3351(4) 0.0391(11) Uani 1 1 d . . . H27 H 0.1165 -0.1761 0.3134 0.047 Uiso 1 1 calc R . . O31 O -0.4432(6) -0.1652(4) 0.0180(4) 0.0505(9) Uani 1 1 d D . . H31A H -0.447(13) -0.211(5) -0.040(4) 0.14(4) Uiso 1 1 d D . . H31B H -0.561(5) -0.159(7) 0.016(7) 0.12(3) Uiso 1 1 d D . . O41 O 0.521(3) 0.4164(12) 0.0676(17) 0.239(13) Uani 0.50 1 d PD . . C43 C 0.359(3) 0.4527(16) 0.0643(16) 0.194(18) Uani 0.50 1 d PD . . C41 C 0.181(3) 0.4125(14) -0.0466(18) 0.232(16) Uani 0.50 1 d PD . . H41A H 0.2043 0.3437 -0.0933 0.347 Uiso 0.50 1 calc PR . . H41B H 0.1760 0.4731 -0.0870 0.347 Uiso 0.50 1 calc PR . . H41C H 0.0512 0.3955 -0.0292 0.347 Uiso 0.50 1 calc PR . . C42 C 0.382(5) 0.5866(13) 0.111(2) 0.32(2) Uani 0.50 1 d PD . . H42A H 0.5237 0.6193 0.1542 0.476 Uiso 0.50 1 calc PR . . H42B H 0.2918 0.6009 0.1590 0.476 Uiso 0.50 1 calc PR . . H42C H 0.3429 0.6222 0.0479 0.476 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 Cu1 0.0266(3) 0.0340(3) 0.0271(3) 0.0082(2) 0.0071(2) 0.0091(2) O11 0.0438(19) 0.0397(18) 0.045(2) 0.0027(16) 0.0184(18) 0.0103(15) O12 0.0433(19) 0.0438(19) 0.040(2) -0.0014(16) 0.0177(17) 0.0094(16) O13 0.108(4) 0.039(2) 0.146(5) -0.013(3) 0.051(4) 0.011(3) O14 0.136(5) 0.071(3) 0.160(6) 0.005(3) 0.098(5) 0.041(3) N11 0.088(4) 0.052(3) 0.073(4) 0.009(3) 0.037(3) 0.033(3) C11 0.035(2) 0.039(3) 0.026(2) 0.006(2) 0.003(2) 0.016(2) C12 0.042(3) 0.035(3) 0.031(3) 0.003(2) 0.010(2) 0.014(2) C13 0.046(3) 0.049(3) 0.048(3) -0.002(3) 0.017(3) 0.013(3) C14 0.056(3) 0.040(3) 0.059(4) 0.001(3) 0.015(3) 0.005(3) C15 0.065(3) 0.035(3) 0.046(3) 0.004(2) 0.022(3) 0.021(3) C16 0.061(4) 0.047(3) 0.059(4) 0.011(3) 0.031(3) 0.023(3) C17 0.055(3) 0.036(3) 0.049(3) 0.008(2) 0.025(3) 0.012(2) O21 0.0370(18) 0.063(2) 0.0356(19) 0.0241(17) 0.0110(16) 0.0190(16) O22 0.0374(19) 0.053(2) 0.040(2) 0.0211(17) 0.0002(16) 0.0068(16) O23 0.056(3) 0.062(2) 0.052(2) 0.017(2) -0.011(2) 0.012(2) O24 0.078(3) 0.078(3) 0.042(2) 0.034(2) 0.014(2) 0.027(2) N21 0.057(3) 0.037(2) 0.029(2) 0.0065(19) 0.002(2) 0.021(2) C21 0.042(3) 0.035(2) 0.031(2) 0.006(2) 0.013(2) 0.021(2) C22 0.036(2) 0.032(2) 0.026(2) 0.0065(19) 0.006(2) 0.013(2) C23 0.039(3) 0.048(3) 0.034(3) 0.017(2) 0.010(2) 0.013(2) C24 0.037(3) 0.046(3) 0.036(3) 0.011(2) 0.004(2) 0.011(2) C25 0.047(3) 0.036(2) 0.026(2) 0.005(2) 0.006(2) 0.020(2) C26 0.050(3) 0.046(3) 0.033(3) 0.016(2) 0.010(2) 0.012(2) C27 0.035(3) 0.047(3) 0.036(3) 0.014(2) 0.007(2) 0.009(2) O31 0.040(2) 0.055(2) 0.058(3) 0.013(2) 0.021(2) 0.0040(18) O41 0.35(3) 0.072(9) 0.180(18) 0.010(10) -0.103(19) 0.030(14) C43 0.24(3) 0.18(3) 0.108(18) -0.048(17) 0.13(2) -0.15(2) C41 0.47(5) 0.081(14) 0.19(3) 0.092(17) 0.09(3) 0.09(2) C42 0.57(7) 0.081(16) 0.24(3) 0.10(2) 0.01(4) -0.02(3) _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 O11 1.960(3) 2 ? Cu1 O22 1.960(3) . ? Cu1 O12 1.969(3) . ? Cu1 O21 1.970(3) 2 ? Cu1 O31 2.141(4) . ? Cu1 Cu1 2.6080(11) 2 ? O11 C11 1.258(5) . ? O11 Cu1 1.960(3) 2 ? O12 C11 1.259(5) . ? O13 N11 1.201(6) . ? O14 N11 1.208(6) . ? N11 C15 1.479(6) . ? C11 C12 1.490(6) . ? C12 C13 1.380(6) . ? C12 C17 1.382(6) . ? C13 C14 1.375(6) . ? C14 C15 1.379(7) . ? C15 C16 1.355(7) . ? C16 C17 1.383(6) . ? O21 C21 1.263(5) . ? O21 Cu1 1.970(3) 2 ? O22 C21 1.247(5) . ? O23 N21 1.218(5) . ? O24 N21 1.209(5) . ? N21 C25 1.478(6) . ? C21 C22 1.495(6) . ? C22 C27 1.385(6) . ? C22 C23 1.388(6) . ? C23 C24 1.377(6) . ? C24 C25 1.372(6) . ? C25 C26 1.377(7) . ? C26 C27 1.375(6) . ? O41 C43 1.219(16) . ? C43 C41 1.526(17) . ? C43 C42 1.559(16) . ? 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 O11 Cu1 O22 90.87(14) 2 . ? O11 Cu1 O12 168.89(13) 2 . ? O22 Cu1 O12 89.48(14) . . ? O11 Cu1 O21 89.25(14) 2 2 ? O22 Cu1 O21 168.88(13) . 2 ? O12 Cu1 O21 88.28(14) . 2 ? O11 Cu1 O31 94.58(16) 2 . ? O22 Cu1 O31 96.42(15) . . ? O12 Cu1 O31 96.42(15) . . ? O21 Cu1 O31 94.65(15) 2 . ? O11 Cu1 Cu1 84.10(9) 2 2 ? O22 Cu1 Cu1 86.03(10) . 2 ? O12 Cu1 Cu1 84.84(10) . 2 ? O21 Cu1 Cu1 82.92(10) 2 2 ? O31 Cu1 Cu1 177.25(13) . 2 ? C11 O11 Cu1 123.8(3) . 2 ? C11 O12 Cu1 122.5(3) . . ? O13 N11 O14 122.8(5) . . ? O13 N11 C15 119.3(5) . . ? O14 N11 C15 117.9(5) . . ? O11 C11 O12 124.7(4) . . ? O11 C11 C12 117.6(4) . . ? O12 C11 C12 117.6(4) . . ? C13 C12 C17 119.0(4) . . ? C13 C12 C11 120.2(4) . . ? C17 C12 C11 120.7(4) . . ? C14 C13 C12 120.8(5) . . ? C13 C14 C15 118.3(5) . . ? C16 C15 C14 122.5(5) . . ? C16 C15 N11 119.0(5) . . ? C14 C15 N11 118.5(5) . . ? C15 C16 C17 118.4(5) . . ? C12 C17 C16 120.8(5) . . ? C21 O21 Cu1 124.1(3) . 2 ? C21 O22 Cu1 121.4(3) . . ? O24 N21 O23 123.6(4) . . ? O24 N21 C25 118.4(4) . . ? O23 N21 C25 118.0(4) . . ? O22 C21 O21 125.3(4) . . ? O22 C21 C22 117.8(4) . . ? O21 C21 C22 116.8(4) . . ? C27 C22 C23 119.2(4) . . ? C27 C22 C21 120.5(4) . . ? C23 C22 C21 120.3(4) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 118.8(4) . . ? C24 C25 C26 121.8(4) . . ? C24 C25 N21 119.0(4) . . ? C26 C25 N21 119.1(4) . . ? C27 C26 C25 119.0(4) . . ? C26 C27 C22 120.5(4) . . ? O41 C43 C41 118.4(16) . . ? O41 C43 C42 116.1(16) . . ? C41 C43 C42 108.8(15) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.563 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.096 data_tetrakis(p-nitrobenzoato)diethanolcopper(II) _database_code_CSD 157261 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(4-nitrobenzoato)diethanolcopper(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Cu2 N4 O18' _chemical_formula_weight 881.65 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6724(8) _cell_length_b 11.1582(14) _cell_length_c 12.5549(16) _cell_angle_alpha 93.982(2) _cell_angle_beta 103.863(2) _cell_angle_gamma 94.956(2) _cell_volume 900.18(19) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2226 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7024 _exptl_absorpt_correction_T_max 0.8327 _exptl_absorpt_process_details 'Sadabs' _diffrn_ambient_temperature 295(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 CCD diffractometer' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ; Neglible as determined from a repetition of the first 50 frames at the end of the experiment ; _diffrn_reflns_number 5247 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3762 _reflns_number_gt 2226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998)' _computing_cell_refinement 'Bruker SMART and SAINT (1998)' _computing_data_reduction 'Bruker SAINT (1998)' _computing_structure_solution 'Bruker SHELXTL (1998)' _computing_structure_refinement 'Bruker SHELXTL (1998)' _computing_molecular_graphics 'Bruker SHELXTL (1998)' _computing_publication_material 'Bruker SHELXTL (1998)' _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^)+(0.0732P)^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 3762 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 Cu1 Cu 0.15815(9) 0.06314(6) -0.02008(5) 0.0327(2) Uani 1 1 d . . . O12 O 0.1969(6) -0.0870(4) -0.0997(3) 0.0522(11) Uani 1 1 d . . . O11 O -0.0761(6) -0.1942(4) -0.0675(3) 0.0539(11) Uani 1 1 d . . . O13 O 0.0486(11) -0.6545(5) -0.4330(5) 0.110(2) Uani 1 1 d . . . O14 O 0.3459(11) -0.5726(6) -0.4275(6) 0.128(3) Uani 1 1 d . . . O22 O 0.3123(5) 0.0055(4) 0.1165(3) 0.0494(11) Uani 1 1 d . . . O21 O 0.0413(5) -0.0997(4) 0.1529(3) 0.0535(11) Uani 1 1 d . . . O23 O 0.6664(7) -0.2115(5) 0.6490(4) 0.0727(15) Uani 1 1 d . . . O24 O 0.9290(7) -0.1249(4) 0.6050(4) 0.0696(14) Uani 1 1 d . . . O31 O 0.4161(5) 0.1745(3) -0.0488(3) 0.0426(9) Uani 1 1 d . . . N11 N 0.1855(12) -0.5754(5) -0.3992(5) 0.0735(18) Uani 1 1 d . . . N21 N 0.7465(7) -0.1611(4) 0.5845(4) 0.0446(12) Uani 1 1 d . . . C11 C 0.0731(8) -0.1817(5) -0.1116(4) 0.0377(13) Uani 1 1 d . . . C12 C 0.1075(8) -0.2873(5) -0.1834(4) 0.0351(12) Uani 1 1 d . . . C13 C -0.0385(9) -0.3854(6) -0.2114(5) 0.0521(16) Uani 1 1 d . . . H23 H -0.1549 -0.3880 -0.1827 0.063 Uiso 1 1 calc R . . C14 C -0.0143(10) -0.4805(6) -0.2820(6) 0.0607(18) Uani 1 1 d . . . H24 H -0.1141 -0.5470 -0.3017 0.073 Uiso 1 1 calc R . . C15 C 0.1609(10) -0.4755(6) -0.3230(5) 0.0515(15) Uani 1 1 d . . . C16 C 0.3094(10) -0.3781(5) -0.2942(5) 0.0510(16) Uani 1 1 d . . . H26 H 0.4276 -0.3765 -0.3213 0.061 Uiso 1 1 calc R . . C17 C 0.2830(8) -0.2830(5) -0.2254(5) 0.0450(14) Uani 1 1 d . . . H17 H 0.3817 -0.2159 -0.2068 0.054 Uiso 1 1 calc R . . C21 C 0.2292(8) -0.0582(5) 0.1755(4) 0.0336(12) Uani 1 1 d . . . C22 C 0.3650(7) -0.0882(5) 0.2813(4) 0.0336(12) Uani 1 1 d . . . C23 C 0.5771(8) -0.0518(5) 0.3067(4) 0.0389(13) Uani 1 1 d . . . H43 H 0.6349 -0.0095 0.2581 0.047 Uiso 1 1 calc R . . C24 C 0.7013(8) -0.0795(5) 0.4055(4) 0.0422(14) Uani 1 1 d . . . H44 H 0.8437 -0.0573 0.4230 0.051 Uiso 1 1 calc R . . C25 C 0.6137(8) -0.1391(5) 0.4765(4) 0.0361(12) Uani 1 1 d . . . C26 C 0.4047(8) -0.1773(6) 0.4539(5) 0.0445(14) Uani 1 1 d . . . H46 H 0.3483 -0.2192 0.5032 0.053 Uiso 1 1 calc R . . C27 C 0.2817(8) -0.1505(5) 0.3539(4) 0.0416(14) Uani 1 1 d . . . H47 H 0.1400 -0.1753 0.3360 0.050 Uiso 1 1 calc R . . C31 C 0.4007(14) 0.2930(8) -0.0820(9) 0.112(4) Uani 1 1 d . . . H53A H 0.2914 0.2874 -0.1494 0.135 Uiso 1 1 calc R . . H53B H 0.3544 0.3401 -0.0263 0.135 Uiso 1 1 calc R . . C32 C 0.5747(16) 0.3593(8) -0.1006(9) 0.126(4) Uani 1 1 d . . . H54A H 0.5388 0.4369 -0.1227 0.189 Uiso 1 1 calc R . . H54B H 0.6209 0.3166 -0.1578 0.189 Uiso 1 1 calc R . . H54C H 0.6838 0.3699 -0.0341 0.189 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 0.0225(3) 0.0440(4) 0.0308(3) 0.0023(3) 0.0054(2) 0.0033(2) O12 0.037(2) 0.058(3) 0.060(3) -0.019(2) 0.0196(19) -0.004(2) O11 0.050(3) 0.049(3) 0.071(3) -0.007(2) 0.038(2) 0.001(2) O13 0.118(5) 0.077(4) 0.130(6) -0.053(4) 0.053(4) -0.021(4) O14 0.139(6) 0.090(5) 0.178(7) -0.049(5) 0.105(6) 0.001(4) O22 0.030(2) 0.081(3) 0.037(2) 0.022(2) 0.0038(16) 0.0047(19) O21 0.029(2) 0.075(3) 0.049(2) 0.024(2) -0.0074(17) -0.005(2) O23 0.063(3) 0.108(4) 0.048(3) 0.038(3) 0.006(2) 0.009(3) O24 0.042(3) 0.095(4) 0.057(3) 0.019(3) -0.017(2) -0.005(2) O31 0.033(2) 0.042(2) 0.054(2) 0.0090(19) 0.0132(17) 0.0026(17) N11 0.099(5) 0.050(4) 0.083(5) -0.006(3) 0.045(4) 0.015(4) N21 0.045(3) 0.049(3) 0.035(3) 0.006(2) -0.003(2) 0.012(2) C11 0.029(3) 0.050(4) 0.031(3) 0.006(3) -0.001(2) 0.011(3) C12 0.030(3) 0.040(3) 0.032(3) 0.001(2) -0.001(2) 0.009(2) C13 0.042(3) 0.058(4) 0.061(4) -0.006(3) 0.024(3) 0.003(3) C14 0.060(4) 0.048(4) 0.072(5) -0.015(3) 0.023(4) -0.007(3) C15 0.062(4) 0.049(4) 0.048(4) 0.000(3) 0.018(3) 0.016(3) C16 0.056(4) 0.049(4) 0.058(4) 0.002(3) 0.032(3) 0.008(3) C17 0.035(3) 0.047(4) 0.052(4) -0.008(3) 0.015(3) -0.001(3) C21 0.029(3) 0.038(3) 0.030(3) 0.000(2) 0.001(2) 0.012(2) C22 0.029(3) 0.043(3) 0.026(3) 0.003(2) 0.001(2) 0.008(2) C23 0.035(3) 0.048(3) 0.032(3) 0.005(3) 0.004(2) 0.005(2) C24 0.026(3) 0.055(4) 0.038(3) 0.001(3) -0.004(2) 0.004(3) C25 0.035(3) 0.040(3) 0.028(3) 0.005(2) -0.003(2) 0.010(2) C26 0.034(3) 0.060(4) 0.038(3) 0.009(3) 0.006(2) 0.001(3) C27 0.029(3) 0.051(4) 0.040(3) 0.003(3) 0.001(2) 0.002(3) C31 0.087(7) 0.084(7) 0.191(11) 0.049(7) 0.075(7) 0.009(5) C32 0.130(9) 0.081(7) 0.177(11) 0.025(7) 0.062(8) -0.007(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 Cu1 O22 1.958(4) . ? Cu1 O12 1.959(4) . ? Cu1 O21 1.960(4) 2 ? Cu1 O11 1.963(4) 2 ? Cu1 O31 2.151(3) . ? Cu1 Cu1 2.6055(12) 2 ? O12 C11 1.261(6) . ? O11 C11 1.252(6) . ? O11 Cu1 1.963(4) 2 ? O13 N11 1.190(8) . ? O14 N11 1.204(8) . ? O22 C21 1.251(6) . ? O21 C21 1.256(6) . ? O21 Cu1 1.960(4) 2 ? O23 N21 1.215(6) . ? O24 N21 1.210(6) . ? O31 C31 1.418(8) . ? N11 C15 1.464(8) . ? N21 C25 1.481(6) . ? C11 C12 1.501(7) . ? C12 C13 1.367(7) . ? C12 C17 1.393(7) . ? C13 C14 1.381(8) . ? C14 C15 1.384(8) . ? C15 C16 1.371(8) . ? C16 C17 1.372(8) . ? C21 C22 1.494(6) . ? C22 C27 1.375(7) . ? C22 C23 1.391(7) . ? C23 C24 1.388(7) . ? C24 C25 1.357(7) . ? C25 C26 1.377(7) . ? C26 C27 1.392(7) . ? C31 C32 1.398(11) . ? 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 O22 Cu1 O12 88.70(18) . . ? O22 Cu1 O21 168.85(15) . 2 ? O12 Cu1 O21 89.14(18) . 2 ? O22 Cu1 O11 89.26(18) . 2 ? O12 Cu1 O11 168.87(15) . 2 ? O21 Cu1 O11 90.75(19) 2 2 ? O22 Cu1 O31 96.03(15) . . ? O12 Cu1 O31 97.86(15) . . ? O21 Cu1 O31 95.09(15) 2 . ? O11 Cu1 O31 93.23(15) 2 . ? O22 Cu1 Cu1 83.92(11) . 2 ? O12 Cu1 Cu1 84.82(11) . 2 ? O21 Cu1 Cu1 84.99(11) 2 2 ? O11 Cu1 Cu1 84.08(11) 2 2 ? O31 Cu1 Cu1 177.31(12) . 2 ? C11 O12 Cu1 122.6(4) . . ? C11 O11 Cu1 123.5(4) . 2 ? C21 O22 Cu1 123.5(3) . . ? C21 O21 Cu1 122.1(3) . 2 ? C31 O31 Cu1 123.0(4) . . ? O13 N11 O14 122.0(7) . . ? O13 N11 C15 120.4(7) . . ? O14 N11 C15 117.6(7) . . ? O24 N21 O23 123.4(5) . . ? O24 N21 C25 117.9(5) . . ? O23 N21 C25 118.7(5) . . ? O11 C11 O12 124.7(5) . . ? O11 C11 C12 117.6(5) . . ? O12 C11 C12 117.7(5) . . ? C13 C12 C17 120.2(5) . . ? C13 C12 C11 119.7(5) . . ? C17 C12 C11 120.1(5) . . ? C12 C13 C14 120.4(5) . . ? C13 C14 C15 119.0(6) . . ? C16 C15 C14 121.0(6) . . ? C16 C15 N11 119.9(6) . . ? C14 C15 N11 119.1(6) . . ? C15 C16 C17 119.8(6) . . ? C16 C17 C12 119.7(5) . . ? O22 C21 O21 125.3(5) . . ? O22 C21 C22 117.3(4) . . ? O21 C21 C22 117.4(4) . . ? C27 C22 C23 119.8(5) . . ? C27 C22 C21 120.5(5) . . ? C23 C22 C21 119.7(4) . . ? C24 C23 C22 119.1(5) . . ? C25 C24 C23 119.7(5) . . ? C24 C25 C26 122.9(5) . . ? C24 C25 N21 118.9(5) . . ? C26 C25 N21 118.2(5) . . ? C25 C26 C27 117.1(5) . . ? C22 C27 C26 121.4(5) . . ? C32 C31 O31 119.7(7) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.699 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.104