Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_cudppa _database_code_CSD 182082 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Steed, Jonathan' 'Belcher, Warwick J.' 'Longstaff, Chritopher A.' 'Neckenig, Marcus R.' _publ_contact_author_name 'Dr Jonathan Steed' _publ_contact_author_address ; Chemistry King's College London Strand London WC2R 2LS UNITED KINGDOM ; _publ_contact_author_email 'JON.STEED@KCL.AC.UK' _publ_section_title ; Channel-containing 1D coordination polymers based on a linear dimetallic spacer ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 Cu2 N2 O11' _chemical_formula_weight 657.64 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 orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.9409(5) _cell_length_b 28.2648(5) _cell_length_c 8.7103(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3186.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.388 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6808 _exptl_absorpt_correction_T_max 0.8737 _exptl_absorpt_process_details 'Otwinowski and Minor, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13795 _diffrn_reflns_av_R_equivalents 0.1291 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3113 _reflns_number_gt 1860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _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^)+(0.0813P)^2^+0.6299P] 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 0.0037(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3113 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.009 _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 C2S C 1.1980(13) 0.3033(8) 0.127(3) 0.141(10) Uani 0.50 1 d P . . H2S1 H 1.1829 0.3352 0.0897 0.211 Uiso 0.50 1 calc PR . . H2S2 H 1.2578 0.2905 0.0723 0.211 Uiso 0.50 1 calc PR . . H2S3 H 1.2133 0.3046 0.2375 0.211 Uiso 0.50 1 calc PR . . O2S O 1.1156(8) 0.2753(4) 0.1036(11) 0.078(3) Uani 0.50 1 d P . . C1S C 1.0293(8) 0.3306(3) -0.2028(13) 0.113(4) Uani 1 1 d . . . H1S1 H 0.9585 0.3374 -0.1693 0.170 Uiso 1 1 calc R . . H1S2 H 1.0357 0.3371 -0.3129 0.170 Uiso 1 1 calc R . . H1S3 H 1.0777 0.3507 -0.1458 0.170 Uiso 1 1 calc R . . O1S O 1.0520(6) 0.2834(3) -0.1751(9) 0.139(3) Uani 1 1 d . . . H1S H 1.0620 0.2794 -0.0807 0.166 Uiso 1 1 d R . . C12 C 1.2877(4) 0.4434(2) 0.0051(8) 0.0478(16) Uani 1 1 d . . . H12A H 1.2844 0.4095 0.0287 0.072 Uiso 1 1 calc R . . H12B H 1.3278 0.4597 0.0846 0.072 Uiso 1 1 calc R . . H12C H 1.3209 0.4480 -0.0948 0.072 Uiso 1 1 calc R . . C4 C 0.9286(5) 0.32763(19) 0.3243(6) 0.0408(14) Uani 1 1 d . . . H4 H 0.9720 0.3011 0.3421 0.049 Uiso 1 1 calc R . . C8 C 0.7500 0.2500 0.3977(8) 0.0368(19) Uani 1 2 d S . . H8A H 0.8055 0.2376 0.3307 0.044 Uiso 0.50 1 calc PR . . H8B H 0.6945 0.2624 0.3307 0.044 Uiso 0.50 1 calc PR . . C1 C 0.8104(4) 0.40507(19) 0.2694(5) 0.0301(12) Uani 1 1 d . . . H1 H 0.7688 0.4322 0.2519 0.036 Uiso 1 1 calc R . . C7 C 0.7931(4) 0.29036(19) 0.4947(6) 0.0388(14) Uani 1 1 d . . . H7A H 0.7387 0.3021 0.5649 0.047 Uiso 1 1 calc R . . H7B H 0.8512 0.2785 0.5579 0.047 Uiso 1 1 calc R . . C2 C 0.7729(4) 0.37030(19) 0.3624(6) 0.0314(13) Uani 1 1 d . . . H2 H 0.7061 0.3735 0.4063 0.038 Uiso 1 1 calc R . . C5 C 0.9602(4) 0.36409(19) 0.2301(6) 0.0387(14) Uani 1 1 d . . . H5 H 1.0262 0.3616 0.1829 0.046 Uiso 1 1 calc R . . C6 C 0.8306(4) 0.33068(18) 0.3932(5) 0.0321(13) Uani 1 1 d . . . N1 N 0.9038(3) 0.40276(14) 0.2011(4) 0.0265(10) Uani 1 1 d . . . C11 C 1.1798(4) 0.4634(2) 0.0004(6) 0.0313(12) Uani 1 1 d . . . O4 O 0.9407(3) 0.43698(14) -0.1376(4) 0.0443(11) Uani 1 1 d . . . O1 O 0.9997(3) 0.49858(14) 0.2553(3) 0.0370(9) Uani 1 1 d . . . O3 O 0.8316(3) 0.49603(14) 0.0584(4) 0.0402(10) Uani 1 1 d . . . O2 O 1.1083(3) 0.43951(13) 0.0591(4) 0.0390(9) Uani 1 1 d . . . C9 C 1.0392(4) 0.53874(19) 0.2559(6) 0.0287(12) Uani 1 1 d . . . Cu1 Cu 0.96435(4) 0.46221(2) 0.07028(6) 0.0248(3) Uani 1 1 d . . . C10 C 1.0659(4) 0.5598(2) 0.4093(6) 0.0385(14) Uani 1 1 d . . . H10A H 1.0174 0.5481 0.4870 0.058 Uiso 1 1 calc R . . H10B H 1.0612 0.5943 0.4034 0.058 Uiso 1 1 calc R . . H10C H 1.1364 0.5506 0.4376 0.058 Uiso 1 1 calc R . . H2S H 1.0946 0.2570 0.1756 0.046 Uiso 0.50 1 d 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 C2S 0.065(12) 0.14(2) 0.22(3) 0.097(19) 0.019(14) 0.044(13) O2S 0.080(7) 0.076(7) 0.079(7) 0.034(5) 0.022(6) -0.021(6) C1S 0.147(9) 0.047(5) 0.146(10) 0.018(5) -0.035(7) 0.012(6) O1S 0.190(8) 0.095(6) 0.131(7) -0.001(5) 0.019(5) -0.001(5) C12 0.031(3) 0.051(4) 0.062(4) 0.010(3) 0.005(3) 0.001(3) C4 0.061(4) 0.028(3) 0.033(3) 0.002(3) 0.007(3) 0.000(3) C8 0.059(5) 0.034(4) 0.017(4) 0.000 0.000 -0.010(4) C1 0.033(3) 0.038(3) 0.019(3) 0.000(2) -0.006(2) -0.009(2) C7 0.072(4) 0.029(3) 0.015(3) -0.002(2) 0.001(3) -0.017(3) C2 0.039(3) 0.038(3) 0.017(3) 0.001(2) -0.001(2) -0.010(3) C5 0.049(3) 0.034(3) 0.032(3) 0.005(2) 0.015(3) -0.001(3) C6 0.057(4) 0.027(3) 0.012(3) -0.006(2) 0.002(2) -0.013(3) N1 0.034(2) 0.028(2) 0.018(2) 0.0008(17) -0.006(2) -0.006(2) C11 0.031(3) 0.039(3) 0.023(3) -0.004(3) -0.004(2) -0.004(3) O4 0.072(3) 0.040(2) 0.021(2) 0.0006(18) -0.0041(19) -0.022(2) O1 0.052(2) 0.041(3) 0.0173(18) -0.0007(16) 0.0020(18) -0.0130(19) O3 0.0280(19) 0.039(2) 0.053(3) 0.0209(19) -0.0019(17) -0.0075(17) O2 0.031(2) 0.043(2) 0.043(2) 0.0098(18) 0.0103(18) -0.0014(19) C9 0.026(3) 0.034(3) 0.026(3) -0.005(2) -0.004(2) -0.006(3) Cu1 0.0299(4) 0.0278(4) 0.0169(4) 0.0015(3) -0.0018(3) -0.0053(3) C10 0.041(3) 0.051(4) 0.024(3) -0.004(3) 0.000(2) -0.013(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 C2S O2S 1.34(2) . ? C1S O1S 1.386(10) . ? C12 C11 1.506(7) . ? C4 C5 1.379(7) . ? C4 C6 1.406(7) . ? C8 C7 1.525(6) . ? C8 C7 1.525(6) 2_655 ? C1 N1 1.349(6) . ? C1 C2 1.363(7) . ? C7 C6 1.522(7) . ? C2 C6 1.373(7) . ? C5 N1 1.338(7) . ? N1 Cu1 2.176(4) . ? C11 O2 1.255(6) . ? C11 O3 1.264(6) 5_765 ? O4 C9 1.265(6) 5_765 ? O4 Cu1 1.970(4) . ? O1 C9 1.245(6) . ? O1 Cu1 1.966(3) . ? O3 C11 1.264(6) 5_765 ? O3 Cu1 1.969(4) . ? O2 Cu1 1.972(4) . ? C9 O4 1.265(6) 5_765 ? C9 C10 1.503(7) . ? Cu1 Cu1 2.6294(11) 5_765 ? 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 C5 C4 C6 118.4(5) . . ? C7 C8 C7 112.7(6) . 2_655 ? N1 C1 C2 123.1(5) . . ? C6 C7 C8 110.8(4) . . ? C1 C2 C6 120.7(5) . . ? N1 C5 C4 124.1(5) . . ? C2 C6 C4 117.2(5) . . ? C2 C6 C7 123.5(5) . . ? C4 C6 C7 119.3(5) . . ? C5 N1 C1 116.4(4) . . ? C5 N1 Cu1 122.2(3) . . ? C1 N1 Cu1 121.1(3) . . ? O2 C11 O3 124.6(5) . 5_765 ? O2 C11 C12 118.0(5) . . ? O3 C11 C12 117.4(5) 5_765 . ? C9 O4 Cu1 121.3(3) 5_765 . ? C9 O1 Cu1 125.2(3) . . ? C11 O3 Cu1 124.3(3) 5_765 . ? C11 O2 Cu1 122.8(3) . . ? O1 C9 O4 125.2(5) . 5_765 ? O1 C9 C10 117.3(5) . . ? O4 C9 C10 117.5(5) 5_765 . ? O1 Cu1 O3 89.57(16) . . ? O1 Cu1 O4 168.27(15) . . ? O3 Cu1 O4 89.52(16) . . ? O1 Cu1 O2 89.46(16) . . ? O3 Cu1 O2 168.35(14) . . ? O4 Cu1 O2 89.08(16) . . ? O1 Cu1 N1 93.34(14) . . ? O3 Cu1 N1 95.07(15) . . ? O4 Cu1 N1 98.39(15) . . ? O2 Cu1 N1 96.57(15) . . ? O1 Cu1 Cu1 82.83(11) . 5_765 ? O3 Cu1 Cu1 83.53(10) . 5_765 ? O4 Cu1 Cu1 85.45(11) . 5_765 ? O2 Cu1 Cu1 84.83(11) . 5_765 ? N1 Cu1 Cu1 175.91(11) . 5_765 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C8 C7 C6 -177.4(5) 2_655 . . . ? N1 C1 C2 C6 1.0(8) . . . . ? C6 C4 C5 N1 0.8(8) . . . . ? C1 C2 C6 C4 -0.4(7) . . . . ? C1 C2 C6 C7 -179.5(5) . . . . ? C5 C4 C6 C2 -0.4(7) . . . . ? C5 C4 C6 C7 178.7(5) . . . . ? C8 C7 C6 C2 97.9(5) . . . . ? C8 C7 C6 C4 -81.1(6) . . . . ? C4 C5 N1 C1 -0.3(8) . . . . ? C4 C5 N1 Cu1 173.7(4) . . . . ? C2 C1 N1 C5 -0.6(7) . . . . ? C2 C1 N1 Cu1 -174.6(4) . . . . ? O3 C11 O2 Cu1 -0.5(7) 5_765 . . . ? C12 C11 O2 Cu1 177.2(4) . . . . ? Cu1 O1 C9 O4 2.6(8) . . . 5_765 ? Cu1 O1 C9 C10 -176.8(3) . . . . ? C9 O1 Cu1 O3 -84.4(4) . . . . ? C9 O1 Cu1 O4 1.2(10) . . . . ? C9 O1 Cu1 O2 84.0(4) . . . . ? C9 O1 Cu1 N1 -179.4(4) . . . . ? C9 O1 Cu1 Cu1 -0.8(4) . . . 5_765 ? C11 O3 Cu1 O1 82.3(4) 5_765 . . . ? C11 O3 Cu1 O4 -86.0(4) 5_765 . . . ? C11 O3 Cu1 O2 -2.9(10) 5_765 . . . ? C11 O3 Cu1 N1 175.6(4) 5_765 . . . ? C11 O3 Cu1 Cu1 -0.5(4) 5_765 . . 5_765 ? C9 O4 Cu1 O1 -3.8(10) 5_765 . . . ? C9 O4 Cu1 O3 81.8(4) 5_765 . . . ? C9 O4 Cu1 O2 -86.7(4) 5_765 . . . ? C9 O4 Cu1 N1 176.8(4) 5_765 . . . ? C9 O4 Cu1 Cu1 -1.8(4) 5_765 . . 5_765 ? C11 O2 Cu1 O1 -82.2(4) . . . . ? C11 O2 Cu1 O3 3.0(10) . . . . ? C11 O2 Cu1 O4 86.2(4) . . . . ? C11 O2 Cu1 N1 -175.5(4) . . . . ? C11 O2 Cu1 Cu1 0.7(4) . . . 5_765 ? C5 N1 Cu1 O1 -97.8(4) . . . . ? C1 N1 Cu1 O1 75.9(3) . . . . ? C5 N1 Cu1 O3 172.4(4) . . . . ? C1 N1 Cu1 O3 -14.0(4) . . . . ? C5 N1 Cu1 O4 82.1(4) . . . . ? C1 N1 Cu1 O4 -104.2(3) . . . . ? C5 N1 Cu1 O2 -7.9(4) . . . . ? C1 N1 Cu1 O2 165.7(3) . . . . ? C5 N1 Cu1 Cu1 -117.9(15) . . . 5_765 ? C1 N1 Cu1 Cu1 55.8(17) . . . 5_765 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S O2S 0.84 1.75 2.574(13) 165.1 . O2S H2S O1S 0.86 1.82 2.674(11) 178.0 8_566 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.587 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.122