Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_jk1-148a _database_code_CSD 187373 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Catena-((\m-1,3-bis(4-pyridyl)propane)Copper(I)-tetrafluoroborate) ; _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Jin, Kun' ; Department of Chemistry and Chemical Biology Rutgers University 610 Taylor Road Piscataway, NJ 08854 USA ; 'Huang, Xiaoying' ; Department of Chemistry and Chemical Biology Rutgers University 610 Taylor Road Piscataway, NJ 08854 USA ; 'Pang, Long' ; Department of Chemistry and Chemical Biology Rutgers University 610 Taylor Road Piscataway, NJ 08854 USA ; 'Li, Jing' ; Department of Chemistry and Chemical Biology Rutgers University 610 Taylor Road Piscataway, NJ 08854 USA ; 'Appel, Aaron' ; Department of Chemistry Washington State University Pullman Washington 99164 USA ; 'Wherland, Scot' ; Department of Chemistry Washington State University Pullman Washington 99164 USA ; _publ_contact_author_name 'Dr Jing Li' _publ_contact_author_address ; Department of Chemistry Rutgers University Camden New Jersey 08102 UNITED STATES OF AMERICA ; _publ_contact_author_phone 856-225-6160 _publ_contact_author_fax 856-225-6506 _publ_contact_author_email jingli@rutchem.rutgers.edu _publ_requested_journal 'Chem. Comm.' _publ_requested_coeditor_name ? _publ_section_title ; [Cu(bpp)]BF4: the first extended coordination network prepared solvothermally using an ionic liquid as a reactive solvent ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cu(bpp)(BF4) _chemical_formula_sum 'C13 H14 B Cu F4 N2' _chemical_formula_weight 348.61 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' 'F' 'F' 0.0171 0.0103 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.451(2) _cell_length_b 8.557(2) _cell_length_c 16.569(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.50(3) _cell_angle_gamma 90.00 _cell_volume 1474.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6038 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD area detector' _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method 'Phi oscillations' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -90.0000 - 90.0000 Image width: 0.5000 Exp time: 75.0000 Rotation axis: Phi Omega: 0.0000 Chi: 0.0000 Phi: 0.0000 XTD: 35.3075 2theta: -10.2724 scan: Number of images: 80 Slice: -20.0000 - 20.0000 Image width: 0.5000 Exp time: 75.0000 Rotation axis: Omega Omega: 0.0000 Chi: -90.0000 Phi: 0.0000 XTD: 35.3075 2theta: -10.2724 ; _diffrn_measurement_device_details ; AFC7: Eulerian 3-circle ; _diffrn_reflns_number 8887 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2699 _reflns_number_gt 2049 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0100P)^2^+7.0000P] 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 2699 _refine_ls_number_parameters 226 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.004 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.05186(7) 0.14378(8) 0.04353(5) 0.0507(3) Uani 1 1 d . . . N1 N -0.0733(4) 0.2793(5) -0.0072(3) 0.0410(11) Uani 1 1 d . . . N2 N -0.8265(4) 0.4639(5) -0.3857(3) 0.0410(11) Uani 1 1 d . . . C1 C -0.0635(5) 0.3452(7) -0.0800(4) 0.0475(14) Uani 1 1 d . . . H1A H 0.0061 0.3184 -0.1082 0.057 Uiso 1 1 calc R A . C2 C -0.1519(5) 0.4508(6) -0.1148(3) 0.0458(14) Uani 1 1 d . . . H2B H -0.1424 0.4913 -0.1659 0.055 Uiso 1 1 calc R . . C3 C -0.2546(5) 0.4965(6) -0.0737(3) 0.0387(13) Uani 1 1 d . . . C4 C -0.2644(5) 0.4268(7) 0.0005(3) 0.0494(14) Uani 1 1 d . . . H4A H -0.3326 0.4517 0.0303 0.059 Uiso 1 1 calc R . . C5 C -0.1734(6) 0.3205(7) 0.0304(3) 0.0504(15) Uani 1 1 d . . . H5A H -0.1831 0.2749 0.0804 0.060 Uiso 1 1 calc R A . C6 C -0.3527(5) 0.6119(6) -0.1095(4) 0.0460(14) Uani 1 1 d . . . H6A H -0.3093 0.6935 -0.1369 0.055 Uiso 1 1 calc R . . H6B H -0.3946 0.6602 -0.0660 0.055 Uiso 1 1 calc R . . C7 C -0.4540(5) 0.5377(5) -0.1690(3) 0.0355(12) Uani 1 1 d . . . H7A H -0.5050 0.4651 -0.1406 0.043 Uiso 1 1 calc R A . H7B H -0.4125 0.4797 -0.2095 0.043 Uiso 1 1 calc R . . C8 C -0.5415(5) 0.6623(6) -0.2106(3) 0.0482(14) Uani 1 1 d . . . H8A H -0.5834 0.7187 -0.1697 0.058 Uiso 1 1 calc R . . H8B H -0.4893 0.7363 -0.2373 0.058 Uiso 1 1 calc R . . C9 C -0.6424(5) 0.5973(6) -0.2720(3) 0.0402(13) Uani 1 1 d . . . C10 C -0.6217(5) 0.5830(6) -0.3535(4) 0.0440(14) Uani 1 1 d . . . H10A H -0.5450 0.6179 -0.3713 0.053 Uiso 1 1 calc R . . C11 C -0.7141(5) 0.5176(6) -0.4073(3) 0.0425(13) Uani 1 1 d . . . H11A H -0.6981 0.5100 -0.4614 0.051 Uiso 1 1 calc R A . C12 C -0.8469(6) 0.4788(7) -0.3081(4) 0.0528(15) Uani 1 1 d . . . H12A H -0.9250 0.4446 -0.2920 0.063 Uiso 1 1 calc R A . C13 C -0.7582(6) 0.5424(7) -0.2505(4) 0.0551(16) Uani 1 1 d . . . H13A H -0.7767 0.5482 -0.1968 0.066 Uiso 1 1 calc R . . B B 0.2278(5) 0.1019(6) -0.1412(3) 0.0586(19) Uani 1 1 d D . . F1A F 0.1748(12) 0.1663(19) -0.2122(6) 0.136(6) Uani 0.70 1 d PDU A 1 F2A F 0.3106(8) -0.0214(7) -0.1426(6) 0.128(3) Uani 0.70 1 d PDU A 1 F3A F 0.3050(9) 0.2149(9) -0.1038(6) 0.130(3) Uani 0.70 1 d PDU A 1 F4A F 0.1392(5) 0.0591(9) -0.0897(4) 0.0806(19) Uani 0.70 1 d PDU A 1 F1B F 0.1314(16) 0.143(4) -0.1992(12) 0.087(7) Uani 0.30 1 d PDU A 2 F2B F 0.201(2) -0.0465(10) -0.1688(11) 0.133(7) Uani 0.30 1 d PDU A 2 F3B F 0.3198(17) 0.188(2) -0.1742(17) 0.146(8) Uani 0.30 1 d PDU A 2 F4B F 0.2008(19) 0.174(2) -0.0711(6) 0.096(5) Uani 0.30 1 d PDU A 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 Cu 0.0468(4) 0.0404(4) 0.0600(5) -0.0024(3) -0.0204(3) 0.0050(3) N1 0.038(3) 0.037(2) 0.045(3) -0.004(2) -0.010(2) 0.0058(19) N2 0.037(3) 0.035(2) 0.048(3) 0.004(2) -0.014(2) 0.0010(19) C1 0.036(3) 0.048(3) 0.059(4) 0.005(3) 0.006(3) 0.005(3) C2 0.050(3) 0.043(3) 0.044(3) 0.004(3) 0.001(3) 0.002(3) C3 0.040(3) 0.030(3) 0.043(3) -0.008(2) -0.013(2) 0.000(2) C4 0.048(3) 0.059(4) 0.041(3) -0.004(3) 0.003(3) 0.013(3) C5 0.058(4) 0.057(4) 0.034(3) -0.001(3) -0.003(3) 0.016(3) C6 0.046(3) 0.037(3) 0.051(3) -0.006(3) -0.013(3) 0.006(2) C7 0.038(3) 0.028(2) 0.039(3) -0.002(2) -0.005(2) 0.002(2) C8 0.051(3) 0.034(3) 0.055(3) -0.001(3) -0.017(3) 0.004(2) C9 0.044(3) 0.028(3) 0.045(3) 0.004(2) -0.013(2) 0.006(2) C10 0.036(3) 0.037(3) 0.057(4) 0.003(3) -0.008(3) 0.000(2) C11 0.043(3) 0.042(3) 0.041(3) 0.001(2) -0.005(2) 0.004(2) C12 0.041(3) 0.063(4) 0.053(4) 0.007(3) -0.001(3) -0.005(3) C13 0.057(4) 0.059(4) 0.048(4) -0.002(3) -0.002(3) -0.003(3) B 0.055(5) 0.064(5) 0.059(5) 0.001(4) 0.016(4) 0.001(4) F1A 0.241(14) 0.103(7) 0.065(6) 0.033(5) 0.025(8) -0.032(9) F2A 0.114(6) 0.070(4) 0.220(9) 0.009(5) 0.114(6) 0.031(4) F3A 0.135(7) 0.116(6) 0.137(7) -0.022(6) -0.004(6) -0.025(5) F4A 0.057(4) 0.099(5) 0.091(5) 0.031(4) 0.035(3) 0.019(3) F1B 0.091(10) 0.115(17) 0.058(11) 0.002(10) 0.022(9) -0.006(10) F2B 0.196(16) 0.108(12) 0.091(11) 0.031(10) -0.006(12) 0.016(13) F3B 0.113(13) 0.187(17) 0.147(15) 0.035(14) 0.060(13) 0.022(12) F4B 0.094(11) 0.145(14) 0.054(8) 0.004(9) 0.029(8) 0.056(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 1.884(4) . ? Cu N2 1.885(4) 4_666 ? Cu F4A 2.573(6) . ? Cu F4B 2.581(16) . ? Cu Cu 3.0018(15) 3 ? N1 C5 1.317(7) . ? N1 C1 1.344(7) . ? N2 C12 1.329(7) . ? N2 C11 1.341(7) . ? N2 Cu 1.885(4) 4_465 ? C1 C2 1.378(7) . ? C1 H1A 0.9300 . ? C2 C3 1.381(8) . ? C2 H2B 0.9300 . ? C3 C4 1.379(8) . ? C3 C6 1.504(7) . ? C4 C5 1.373(7) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.515(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.526(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.499(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C13 1.376(8) . ? C9 C10 1.393(8) . ? C10 C11 1.370(7) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.377(8) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? B F2A 1.366(2) . ? B F1A 1.368(2) . ? B F4B 1.368(2) . ? B F4A 1.368(2) . ? B F3B 1.368(2) . ? B F2B 1.369(2) . ? B F3A 1.370(2) . ? B F1B 1.370(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 N1 Cu N2 167.43(19) . 4_666 ? N1 Cu F4A 94.5(2) . . ? N2 Cu F4A 97.0(2) 4_666 . ? N1 Cu F4B 93.0(4) . . ? N2 Cu F4B 95.0(4) 4_666 . ? N1 Cu Cu 94.99(13) . 3 ? N2 Cu Cu 95.11(13) 4_666 3 ? F4A Cu Cu 59.87(16) . 3 ? F4B Cu Cu 86.8(4) . 3 ? C5 N1 C1 116.4(4) . . ? C5 N1 Cu 120.2(4) . . ? C1 N1 Cu 123.3(4) . . ? C12 N2 C11 116.8(5) . . ? C12 N2 Cu 119.1(4) . 4_465 ? C11 N2 Cu 123.9(4) . 4_465 ? N1 C1 C2 123.0(5) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 120.1(5) . . ? C1 C2 H2B 120.0 . . ? C3 C2 H2B 120.0 . . ? C4 C3 C2 116.4(5) . . ? C4 C3 C6 122.0(5) . . ? C2 C3 C6 121.6(5) . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C5 C4 124.1(5) . . ? N1 C5 H5A 117.9 . . ? C4 C5 H5A 117.9 . . ? C3 C6 C7 112.9(4) . . ? C3 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C3 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 C8 110.7(4) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C7 113.6(4) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C13 C9 C10 116.3(5) . . ? C13 C9 C8 122.0(5) . . ? C10 C9 C8 121.7(5) . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? N2 C11 C10 123.2(5) . . ? N2 C11 H11A 118.4 . . ? C10 C11 H11A 118.4 . . ? N2 C12 C13 123.2(6) . . ? N2 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C9 C13 C12 120.4(6) . . ? C9 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? F2A B F1A 120.1(10) . . ? F2A B F4A 105.8(5) . . ? F1A B F4A 113.7(7) . . ? F2A B F3A 101.9(7) . . ? F1A B F3A 106.1(8) . . ? F4A B F3A 108.2(6) . . ? F4B B F3B 107.8(15) . . ? F4B B F2B 130.3(14) . . ? F3B B F2B 120.0(16) . . ? F4B B F1B 106.4(15) . . ? F3B B F1B 94.5(15) . . ? F2B B F1B 83.7(17) . . ? B F4A Cu 141.0(5) . . ? B F4B Cu 140.2(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.649 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.092