# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1428 #============================================================================ data_global #============================================================================ _audit_creation_method 'form.cif (version 2.0)' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof.Fun Hoong Kun' _publ_contact_author_address ; X-ray Crystallography Unit School of Physics Universiti Sains Malaysia 11800 USM, Penang MALAYSIA ; _publ_contact_author_email 'hkfun@usm.my' _publ_contact_author_fax '6 04 6579150' _publ_contact_author_phone '6 04 6577888 Ext. 3690' _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ? #============================================================================ # TITLE AND AUTHOR LIST _publ_section_title ; The First Structurally Characterized 3,4'-Bipyridine Copper(I) Coordination Polymer with an Approximate Rectangular Molecular Box ; loop_ _publ_author_name _publ_author_address 'Hoong-Kun Fun' ; X-ray Crystallography Unit School of Physics Universiti Sains Malaysia 11800 USM, Penang Malaysia ; 'S.Shanmuga Sundara Raj' ; X-ray Crystallography Unit School of Physics Universiti Sains Malaysia 11800 USM, Penang Malaysia ; 'Ren-Gen Xiong' ; Coordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 P.R.China ; 'Jing-Lin Zuo' ; Coordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 P.R.China ; 'Zhi Yu' ; Coordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 P.R.China ; 'Xiao-Lei Zhu' ; Coordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 P.R.China ; 'Xiao-Zeng You' ; Coordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 P.R.China ; #============================================================================ _publ_section_references ; Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Siemens (1996a). SMART Software Reference Manual, Siemens Analytical X-Ray Systems, Inc., Siemens (1996b). SAINT v4 Software Reference Manual, Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; The data collection was covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating thirty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #============================================================================ data_9/02054C _audit_creation_method SHELXL-97 _chemical_name_systematic ; The First Structurally Characterized 3,4'-Bipyridine Copper(I) Coordination Polymer with an Approximate Rectangular Molecular Box ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Br2 Cu2 N4' _chemical_formula_weight 599.27 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' 'Br' 'Br' -0.2901 2.4595 '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 ' 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 9.4944(1) _cell_length_b 12.9445(2) _cell_length_c 16.9514(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.924(1) _cell_angle_gamma 90.00 _cell_volume 2083.06(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 33.20 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 5.891 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.131 _exptl_absorpt_correction_T_max 0.309 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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 ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13331 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4759 _reflns_number_gt 3873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996a)' _computing_cell_refinement 'SAINT (Siemens, 1996b)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and PARST (Nardelli, 1995)' _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^)+(0.0286P)^2^+1.2680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4759 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.044 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.075 _refine_ls_wR_factor_gt 0.070 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.25159(4) 0.24438(3) 0.19109(2) 0.04946(11) Uani 1 1 d . . . Cu2 Cu 0.44587(4) 0.20036(3) 0.07333(2) 0.05122(11) Uani 1 1 d . . . Br1 Br 0.25947(3) 0.07340(2) 0.114132(17) 0.04636(9) Uani 1 1 d . . . Br2 Br 0.43126(3) 0.37660(2) 0.147345(19) 0.04886(9) Uani 1 1 d . . . N1 N 0.3035(3) 0.21115(19) 0.30249(13) 0.0408(5) Uani 1 1 d . . . N2 N 0.5742(3) 0.18433(19) 0.65353(13) 0.0393(5) Uani 1 1 d . . . N3 N 0.6307(3) 0.1499(2) 0.11836(13) 0.0407(5) Uani 1 1 d . . . N4 N 0.8999(3) 0.2560(2) 0.46283(14) 0.0439(6) Uani 1 1 d . . . C1 C 0.2902(3) 0.1167(2) 0.33367(17) 0.0435(7) Uani 1 1 d . . . C2 C 0.3249(3) 0.0935(2) 0.41133(17) 0.0427(7) Uani 1 1 d . . . C3 C 0.3766(3) 0.1706(2) 0.46085(15) 0.0359(6) Uani 1 1 d . . . C4 C 0.3905(4) 0.2680(2) 0.42865(17) 0.0468(7) Uani 1 1 d . . . C5 C 0.3532(4) 0.2861(2) 0.35097(17) 0.0494(8) Uani 1 1 d . . . C6 C 0.4159(3) 0.1489(2) 0.54403(15) 0.0357(6) Uani 1 1 d . . . C7 C 0.3428(4) 0.0803(3) 0.5906(2) 0.0543(8) Uani 1 1 d . . . C8 C 0.3873(4) 0.0643(3) 0.6674(2) 0.0617(10) Uani 1 1 d . . . H8A H 0.3394 0.0181 0.6993 0.074 Uiso 1 1 calc R . . C9 C 0.5023(3) 0.1166(3) 0.69666(17) 0.0456(7) Uani 1 1 d . . . C10 C 0.5301(3) 0.1990(2) 0.57865(15) 0.0387(6) Uani 1 1 d . . . C11 C 0.6699(3) 0.1793(2) 0.19181(15) 0.0401(6) Uani 1 1 d . . . C12 C 0.7961(3) 0.1526(2) 0.22799(14) 0.0325(5) Uani 1 1 d . . . C13 C 0.8878(3) 0.0916(2) 0.18543(18) 0.0410(6) Uani 1 1 d . . . C14 C 0.8482(3) 0.0603(3) 0.11031(19) 0.0484(7) Uani 1 1 d . . . C15 C 0.7208(3) 0.0906(2) 0.07924(17) 0.0439(7) Uani 1 1 d . . . C16 C 0.8308(3) 0.1893(2) 0.30898(14) 0.0337(6) Uani 1 1 d . . . C17 C 0.7735(4) 0.2781(3) 0.34026(17) 0.0501(8) Uani 1 1 d . . . C18 C 0.8102(4) 0.3084(3) 0.41605(18) 0.0532(8) Uani 1 1 d . . . C19 C 0.9522(4) 0.1694(3) 0.43297(19) 0.0544(9) Uani 1 1 d . . . C20 C 0.9215(4) 0.1343(3) 0.35763(18) 0.0500(8) Uani 1 1 d . . . H1 H 0.263(3) 0.064(3) 0.2990(19) 0.051(9) Uiso 1 1 d . . . H2 H 0.316(4) 0.025(3) 0.427(2) 0.065(11) Uiso 1 1 d . . . H4 H 0.419(4) 0.332(3) 0.460(2) 0.072(11) Uiso 1 1 d . . . H5 H 0.364(4) 0.354(3) 0.325(2) 0.059(10) Uiso 1 1 d . . . H7 H 0.267(4) 0.047(3) 0.568(2) 0.067(11) Uiso 1 1 d . . . H9 H 0.538(3) 0.110(3) 0.751(2) 0.051(9) Uiso 1 1 d . . . H10 H 0.585(4) 0.248(3) 0.550(2) 0.058(10) Uiso 1 1 d . . . H11 H 0.602(3) 0.225(3) 0.2191(19) 0.051(9) Uiso 1 1 d . . . H13 H 0.965(4) 0.072(3) 0.206(2) 0.051(10) Uiso 1 1 d . . . H14 H 0.913(4) 0.018(3) 0.079(2) 0.061(10) Uiso 1 1 d . . . H15 H 0.689(3) 0.070(2) 0.0295(19) 0.045(8) Uiso 1 1 d . . . H17 H 0.712(4) 0.321(3) 0.310(2) 0.065(11) Uiso 1 1 d . . . H18 H 0.771(3) 0.370(3) 0.4373(19) 0.053(9) Uiso 1 1 d . . . H19 H 1.012(4) 0.137(3) 0.467(2) 0.064(11) Uiso 1 1 d . . . H20 H 0.960(4) 0.070(3) 0.338(2) 0.070(11) Uiso 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 0.0578(2) 0.0554(2) 0.03467(19) 0.00157(16) -0.01662(16) 0.00242(18) Cu2 0.0583(2) 0.0600(3) 0.03476(19) 0.00328(17) -0.01592(16) -0.0006(2) Br1 0.05880(19) 0.03946(16) 0.04093(16) -0.00750(12) 0.00438(13) -0.00738(14) Br2 0.05548(19) 0.03414(15) 0.05684(19) -0.00196(13) -0.00329(14) -0.00379(13) N1 0.0498(14) 0.0412(13) 0.0310(11) -0.0031(10) -0.0098(10) 0.0035(11) N2 0.0452(13) 0.0445(13) 0.0281(11) 0.0005(10) -0.0041(9) -0.0004(11) N3 0.0462(14) 0.0459(14) 0.0299(11) -0.0031(10) -0.0045(10) 0.0001(11) N4 0.0496(14) 0.0490(15) 0.0329(12) -0.0028(10) -0.0109(10) 0.0091(12) C1 0.0550(18) 0.0398(16) 0.0352(15) -0.0073(12) -0.0143(13) -0.0022(13) C2 0.0507(18) 0.0370(16) 0.0398(15) 0.0017(12) -0.0142(13) -0.0054(13) C3 0.0394(14) 0.0396(15) 0.0286(12) 0.0005(11) -0.0064(10) -0.0006(12) C4 0.071(2) 0.0382(16) 0.0309(14) -0.0044(12) -0.0113(13) -0.0065(15) C5 0.080(2) 0.0365(16) 0.0315(14) 0.0015(12) -0.0120(14) -0.0046(15) C6 0.0400(14) 0.0366(14) 0.0302(13) 0.0017(11) -0.0048(10) -0.0014(12) C7 0.056(2) 0.062(2) 0.0445(17) 0.0093(15) -0.0083(15) -0.0215(17) C8 0.067(2) 0.073(2) 0.0449(18) 0.0212(17) -0.0014(15) -0.0238(19) C9 0.0565(18) 0.0525(18) 0.0276(14) 0.0083(12) -0.0047(12) 0.0012(15) C10 0.0451(16) 0.0446(16) 0.0264(12) 0.0037(11) -0.0033(11) -0.0072(13) C11 0.0440(16) 0.0484(17) 0.0279(13) -0.0026(12) -0.0030(11) 0.0089(13) C12 0.0380(14) 0.0319(13) 0.0276(12) -0.0004(10) -0.0013(10) -0.0018(11) C13 0.0367(16) 0.0437(16) 0.0427(16) -0.0084(12) -0.0017(12) 0.0020(13) C14 0.0465(17) 0.0515(19) 0.0474(17) -0.0184(14) 0.0070(13) 0.0027(15) C15 0.0542(18) 0.0440(16) 0.0336(15) -0.0094(12) 0.0006(13) -0.0071(14) C16 0.0349(14) 0.0368(14) 0.0292(12) -0.0003(10) -0.0039(10) 0.0035(11) C17 0.070(2) 0.0480(18) 0.0317(14) -0.0035(13) -0.0146(14) 0.0241(16) C18 0.078(2) 0.0471(18) 0.0344(15) -0.0073(13) -0.0122(15) 0.0246(17) C19 0.0557(19) 0.066(2) 0.0406(16) -0.0072(15) -0.0186(14) 0.0252(17) C20 0.0567(19) 0.0506(19) 0.0422(16) -0.0105(14) -0.0118(13) 0.0242(16) _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 N1 1.991(2) . ? Cu1 N2 2.015(2) 4_565 ? Cu1 Br2 2.5357(5) . ? Cu1 Br1 2.5708(5) . ? Cu1 Cu2 2.7983(6) . ? Cu2 N4 1.998(2) 4_565 ? Cu2 N3 2.012(2) . ? Cu2 Br1 2.5201(5) . ? Cu2 Br2 2.6084(5) . ? N1 C1 1.339(4) . ? N1 C5 1.351(4) . ? N2 C9 1.336(4) . ? N2 C10 1.344(3) . ? N2 Cu1 2.015(2) 4_666 ? N3 C15 1.333(4) . ? N3 C11 1.349(3) . ? N4 C19 1.330(4) . ? N4 C18 1.339(4) . ? N4 Cu2 1.998(2) 4_666 ? C1 C2 1.385(4) . ? C2 C3 1.389(4) . ? C3 C4 1.380(4) . ? C3 C6 1.480(3) . ? C4 C5 1.378(4) . ? C6 C7 1.383(4) . ? C6 C10 1.386(4) . ? C7 C8 1.377(5) . ? C8 C9 1.371(5) . ? C11 C12 1.381(4) . ? C12 C13 1.386(4) . ? C12 C16 1.485(3) . ? C13 C14 1.383(4) . ? C14 C15 1.369(5) . ? C16 C20 1.381(4) . ? C16 C17 1.382(4) . ? C17 C18 1.382(4) . ? C19 C20 1.382(4) . ? 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 Cu1 N2 126.27(10) . 4_565 ? N1 Cu1 Br2 105.41(8) . . ? N2 Cu1 Br2 99.28(7) 4_565 . ? N1 Cu1 Br1 106.65(7) . . ? N2 Cu1 Br1 105.37(7) 4_565 . ? Br2 Cu1 Br1 114.048(18) . . ? N1 Cu1 Cu2 118.47(7) . . ? N2 Cu1 Cu2 115.16(6) 4_565 . ? Br2 Cu1 Cu2 58.302(14) . . ? Br1 Cu1 Cu2 55.792(14) . . ? N4 Cu2 N3 128.59(10) 4_565 . ? N4 Cu2 Br1 107.32(7) 4_565 . ? N3 Cu2 Br1 107.23(7) . . ? N4 Cu2 Br2 101.03(8) 4_565 . ? N3 Cu2 Br2 98.89(7) . . ? Br1 Cu2 Br2 113.287(18) . . ? N4 Cu2 Cu1 118.33(8) 4_565 . ? N3 Cu2 Cu1 112.12(7) . . ? Br1 Cu2 Cu1 57.528(14) . . ? Br2 Cu2 Cu1 55.805(14) . . ? Cu2 Br1 Cu1 66.680(15) . . ? Cu1 Br2 Cu2 65.893(15) . . ? C1 N1 C5 116.7(2) . . ? C1 N1 Cu1 123.25(19) . . ? C5 N1 Cu1 120.0(2) . . ? C9 N2 C10 117.1(3) . . ? C9 N2 Cu1 124.02(19) . 4_666 ? C10 N2 Cu1 118.68(19) . 4_666 ? C15 N3 C11 116.9(3) . . ? C15 N3 Cu2 124.10(19) . . ? C11 N3 Cu2 118.97(19) . . ? C19 N4 C18 116.1(3) . . ? C19 N4 Cu2 121.2(2) . 4_666 ? C18 N4 Cu2 122.7(2) . 4_666 ? N1 C1 C2 123.4(3) . . ? C1 C2 C3 119.7(3) . . ? C4 C3 C2 116.9(2) . . ? C4 C3 C6 121.7(2) . . ? C2 C3 C6 121.4(3) . . ? C5 C4 C3 120.5(3) . . ? N1 C5 C4 122.8(3) . . ? C7 C6 C10 117.1(3) . . ? C7 C6 C3 123.1(3) . . ? C10 C6 C3 119.9(2) . . ? C8 C7 C6 119.1(3) . . ? C9 C8 C7 119.9(3) . . ? N2 C9 C8 122.5(3) . . ? N2 C10 C6 124.3(3) . . ? N3 C11 C12 124.3(3) . . ? C11 C12 C13 117.3(2) . . ? C11 C12 C16 120.5(2) . . ? C13 C12 C16 122.1(2) . . ? C14 C13 C12 118.8(3) . . ? C15 C14 C13 119.7(3) . . ? N3 C15 C14 122.9(3) . . ? C20 C16 C17 116.5(3) . . ? C20 C16 C12 120.9(3) . . ? C17 C16 C12 122.6(2) . . ? C16 C17 C18 119.8(3) . . ? N4 C18 C17 123.8(3) . . ? N4 C19 C20 123.7(3) . . ? C16 C20 C19 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.50 _refine_diff_density_min -0.65 _refine_diff_density_rms 0.09 #============================================================================ # END OF CIF