# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Dr Jack Lu' _publ_contact_author_address ; Department of Chemistry University of Houston-Clear Lake 2700 Bay Area Blvd. Houston TX 77586 UNITED STATES OF AMERICA ; _publ_contact_author_email LU@CL.UH.EDU _publ_section_title ; A novel two fold interpenetrating 3-D networks self-assembled from a 1-D coordination polymer ; loop_ _publ_author_name 'Jack Lu' 'Khalil A. Abboud' 'Wifredo A. Fernandez' 'Zhenghua Ge' data_{[Cu(BPY)2(H2O)2][Cu(BPY)2(H2O)(NO3)]}3NO3.12H2O _database_code_depnum_ccdc_archive 'CCDC 186585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C40 H36 Cu2 N8 O2, 4(N O3), 12(H2 O)' _chemical_formula_sum 'C40 H62 Cu2 N12 O27' _chemical_formula_weight 1270 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 14.3905(7) _cell_length_b 42.019(2) _cell_length_c 42.158(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25492(2) _cell_formula_units_Z 16 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10448 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type 'Empirical (SADABS, Blessing 1995)' _exptl_absorpt_correction_T_min 0.7794 _exptl_absorpt_correction_T_max 0.8769 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55326 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14615 _reflns_number_gt 12754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 1998)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1470P)^2^+148.2421P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.490(16) _refine_ls_number_reflns 14615 _refine_ls_number_parameters 778 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2233 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.118 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.61464(4) 0.126177(11) 0.089976(10) 0.01931(16) Uani 1 1 d . . . O1 O 0.4688(3) 0.14218(9) 0.11045(10) 0.0312(8) Uani 1 1 d . . . N1 N 0.5695(3) 0.12714(9) 0.04420(9) 0.0179(8) Uani 1 1 d . . . N2 N 0.5727(3) 0.08023(9) 0.09327(10) 0.0198(7) Uani 1 1 d . . . N3 N 0.6583(3) 0.17204(9) 0.08665(9) 0.0216(8) Uani 1 1 d . . . N4 N 0.4150(3) 0.12636(9) -0.11501(10) 0.0216(8) Uani 1 1 d . . . C1 C 0.5875(3) 0.10256(11) 0.02477(12) 0.0236(9) Uani 1 1 d . . . H1A H 0.6208 0.0848 0.0330 0.028 Uiso 1 1 calc R . . C2 C 0.5598(3) 0.10192(12) -0.00666(12) 0.0254(10) Uani 1 1 d . . . H2A H 0.5727 0.0839 -0.0196 0.031 Uiso 1 1 calc R . . C3 C 0.5132(4) 0.12787(12) -0.01881(12) 0.0230(10) Uani 1 1 d . . . C4 C 0.4945(4) 0.15365(13) 0.00108(12) 0.0267(10) Uani 1 1 d . . . H4A H 0.4627 0.1719 -0.0066 0.032 Uiso 1 1 calc R . . C5 C 0.5238(3) 0.15177(12) 0.03245(11) 0.0235(9) Uani 1 1 d . . . H5A H 0.5104 0.1691 0.0462 0.028 Uiso 1 1 calc R . . C6 C 0.4800(4) 0.12811(12) -0.05258(12) 0.0226(10) Uani 1 1 d . . . C7 C 0.5313(3) 0.11283(13) -0.07627(12) 0.0257(10) Uani 1 1 d . . . H7A H 0.5884 0.1026 -0.0714 0.031 Uiso 1 1 calc R . . C8 C 0.4971(3) 0.11288(12) -0.10698(11) 0.0243(10) Uani 1 1 d . . . H8A H 0.5329 0.1030 -0.1231 0.029 Uiso 1 1 calc R . . C9 C 0.3671(3) 0.14091(12) -0.09213(12) 0.0225(9) Uani 1 1 d . . . H9A H 0.3096 0.1506 -0.0975 0.027 Uiso 1 1 calc R . . C10 C 0.3968(3) 0.14263(12) -0.06088(12) 0.0255(10) Uani 1 1 d . . . H10A H 0.3609 0.1536 -0.0454 0.031 Uiso 1 1 calc R . . C11 C 0.6327(3) 0.05701(12) 0.10139(13) 0.0247(10) Uani 1 1 d . . . H11A H 0.6949 0.0624 0.1068 0.030 Uiso 1 1 calc R . . C12 C 0.6053(4) 0.02510(12) 0.10201(13) 0.0260(10) Uani 1 1 d . . . H12A H 0.6490 0.0090 0.1073 0.031 Uiso 1 1 calc R . . C13 C 0.5155(3) 0.01713(10) 0.09495(12) 0.0224(9) Uani 1 1 d . . . C14 C 0.4533(3) 0.04093(11) 0.08634(12) 0.0259(10) Uani 1 1 d . . . H14A H 0.3908 0.0360 0.0810 0.031 Uiso 1 1 calc R . . C15 C 0.4854(3) 0.07201(11) 0.08579(12) 0.0229(9) Uani 1 1 d . . . H15A H 0.4433 0.0884 0.0798 0.028 Uiso 1 1 calc R . . C16 C 0.7117(3) 0.18179(11) 0.06261(12) 0.0236(9) Uani 1 1 d . . . H16A H 0.7263 0.1670 0.0463 0.028 Uiso 1 1 calc R . . C17 C 0.7469(3) 0.21245(11) 0.06022(11) 0.0240(10) Uani 1 1 d . . . H17A H 0.7820 0.2187 0.0422 0.029 Uiso 1 1 calc R . . C18 C 0.7299(3) 0.23381(11) 0.08458(12) 0.0244(10) Uani 1 1 d . . . C19 C 0.6741(4) 0.22368(12) 0.11006(13) 0.0288(11) Uani 1 1 d . . . H19A H 0.6609 0.2376 0.1273 0.035 Uiso 1 1 calc R . . C20 C 0.6391(4) 0.19342(13) 0.10959(13) 0.0274(10) Uani 1 1 d . . . H20A H 0.5990 0.1871 0.1264 0.033 Uiso 1 1 calc R . . O2 O 0.7690(3) 0.10777(10) 0.07020(10) 0.0358(9) Uani 1 1 d . . . Cu2 Cu 0.36273(5) 0.123421(12) 0.265572(11) 0.02352(17) Uani 1 1 d . . . O3 O 0.2169(3) 0.10609(10) 0.28375(11) 0.0375(9) Uani 1 1 d . . . N5 N 0.4106(4) 0.12439(10) 0.31095(11) 0.0277(10) Uani 1 1 d . . . N6 N 0.4137(3) 0.07844(9) 0.26122(10) 0.0234(8) Uani 1 1 d . . . N7 N 0.3248(3) 0.17015(10) 0.26874(11) 0.0260(9) Uani 1 1 d . . . N8 N 0.5649(3) 0.12777(9) 0.47005(10) 0.0230(9) Uani 1 1 d . . . C21 C 0.3936(4) 0.10028(12) 0.33065(12) 0.0266(10) Uani 1 1 d . . . H21A H 0.3603 0.0824 0.3229 0.032 Uiso 1 1 calc R . . C22 C 0.4224(4) 0.10030(12) 0.36213(13) 0.0267(10) Uani 1 1 d . . . H22A H 0.4087 0.0826 0.3754 0.032 Uiso 1 1 calc R . . C23 C 0.4712(4) 0.12607(12) 0.37418(12) 0.0244(11) Uani 1 1 d . . . C24 C 0.4885(4) 0.15144(13) 0.35358(12) 0.0283(10) Uani 1 1 d . . . H24A H 0.5212 0.1697 0.3608 0.034 Uiso 1 1 calc R . . C25 C 0.4576(4) 0.14979(13) 0.32242(12) 0.0292(10) Uani 1 1 d . . . H25A H 0.4699 0.1672 0.3086 0.035 Uiso 1 1 calc R . . C26 C 0.5025(4) 0.12690(11) 0.40711(12) 0.0227(10) Uani 1 1 d . . . C27 C 0.4511(4) 0.11350(14) 0.43138(13) 0.0307(11) Uani 1 1 d . . . H27A H 0.3932 0.1037 0.4268 0.037 Uiso 1 1 calc R . . C28 C 0.4835(4) 0.11433(14) 0.46243(13) 0.0311(11) Uani 1 1 d . . . H28A H 0.4469 0.1051 0.4787 0.037 Uiso 1 1 calc R . . C29 C 0.6146(3) 0.14139(12) 0.44651(12) 0.0252(10) Uani 1 1 d . . . H29A H 0.6719 0.1513 0.4517 0.030 Uiso 1 1 calc R . . C30 C 0.5863(4) 0.14156(12) 0.41563(12) 0.0250(9) Uani 1 1 d . . . H30A H 0.6234 0.1516 0.3999 0.030 Uiso 1 1 calc R . . C31 C 0.3586(4) 0.05446(13) 0.25247(13) 0.0270(11) Uani 1 1 d . . . H31A H 0.2955 0.0588 0.2474 0.032 Uiso 1 1 calc R . . C32 C 0.3902(4) 0.02342(11) 0.25051(13) 0.0249(10) Uani 1 1 d . . . H32A H 0.3497 0.0070 0.2436 0.030 Uiso 1 1 calc R . . C33 C 0.4822(3) 0.01632(11) 0.25877(12) 0.0232(10) Uani 1 1 d . . . C34 C 0.5400(4) 0.04176(11) 0.26717(13) 0.0265(10) Uani 1 1 d . . . H34A H 0.6037 0.0382 0.2720 0.032 Uiso 1 1 calc R . . C35 C 0.5028(4) 0.07220(11) 0.26838(13) 0.0265(10) Uani 1 1 d . . . H35A H 0.5419 0.0893 0.2745 0.032 Uiso 1 1 calc R . . C36 C 0.2744(4) 0.18099(12) 0.29294(12) 0.0277(10) Uani 1 1 d . . . H36A H 0.2584 0.1667 0.3096 0.033 Uiso 1 1 calc R . . C37 C 0.2443(4) 0.21228(13) 0.29476(12) 0.0323(12) Uani 1 1 d . . . H37A H 0.2097 0.2195 0.3126 0.039 Uiso 1 1 calc R . . C38 C 0.2660(4) 0.23325(11) 0.26974(13) 0.0269(10) Uani 1 1 d . . . C39 C 0.3179(4) 0.22155(13) 0.24510(14) 0.0334(12) Uani 1 1 d . . . H39A H 0.3344 0.2352 0.2280 0.040 Uiso 1 1 calc R . . C40 C 0.3464(4) 0.19029(13) 0.24474(13) 0.0297(11) Uani 1 1 d . . . H40A H 0.3820 0.1827 0.2273 0.036 Uiso 1 1 calc R . . N9 N 0.2073(5) 0.1225(2) 0.36776(19) 0.075(2) Uani 1 1 d D . . O4 O 0.1893(7) 0.1477(2) 0.35782(18) 0.102(3) Uani 1 1 d D . . O5 O 0.1864(5) 0.1022(3) 0.35095(17) 0.154(6) Uani 1 1 d D . . O6 O 0.2403(5) 0.1183(2) 0.39507(16) 0.098(3) Uani 1 1 d D . . N10 N 0.2541(5) -0.00173(19) 0.8080(2) 0.072(2) Uani 1 1 d D . . O7 O 0.2619(5) 0.02141(15) 0.7910(2) 0.086(2) Uani 1 1 d D . . O8 O 0.2916(4) -0.02742(15) 0.8045(2) 0.091(2) Uani 1 1 d D . . O9 O 0.2049(6) 0.0000(2) 0.8324(2) 0.103(3) Uani 1 1 d D . . N11 N 0.5665(5) 0.16703(17) 0.24725(15) 0.0642(18) Uani 1 1 d D . . O10 O 0.5201(3) 0.14294(10) 0.24399(13) 0.0438(11) Uani 1 1 d D . . O11 O 0.5998(8) 0.1813(3) 0.2704(2) 0.156(5) Uani 1 1 d D . . O12 O 0.5821(7) 0.1826(2) 0.22160(18) 0.099(2) Uani 1 1 d D . . N12 N 0.0833(9) -0.0285(3) 0.6689(3) 0.021(3) Uiso 0.25 1 d PD A 1 O13 O 0.0289(13) -0.0498(4) 0.6656(6) 0.035(7) Uiso 0.25 1 d PD A 1 O14 O 0.0751(9) -0.0014(3) 0.6790(4) 0.027(3) Uiso 0.25 1 d PD A 1 O15 O 0.1619(9) -0.0348(4) 0.6570(4) 0.035(3) Uiso 0.25 1 d PD A 1 N13 N 0.2844(10) 0.0510(3) 0.5011(3) 0.019(3) Uiso 0.25 1 d PD B 2 O16 O 0.2984(19) 0.0733(4) 0.4852(5) 0.072(6) Uiso 0.25 1 d PD B 2 O17 O 0.2666(12) 0.0504(4) 0.5298(3) 0.041(4) Uiso 0.25 1 d PD B 2 O18 O 0.2907(13) 0.0248(4) 0.4881(4) 0.044(4) Uiso 0.25 1 d PD B 2 N14 N 0.2606(15) 0.0014(4) 0.5462(4) 0.044(5) Uiso 0.25 1 d PD C 3 O19 O 0.2721(10) -0.0199(3) 0.5657(4) 0.029(3) Uiso 0.25 1 d PD C 3 O20 O 0.2955(17) 0.0269(5) 0.5532(6) 0.074(6) Uiso 0.25 1 d PD C 3 O21 O 0.222(2) -0.0032(7) 0.5208(5) 0.097(10) Uiso 0.25 1 d PD C 3 N15 N 0.2814(15) 0.1220(3) 0.4863(4) 0.041(5) Uiso 0.25 1 d PD D 4 O22 O 0.2950(9) 0.0991(3) 0.5021(3) 0.022(3) Uiso 0.25 1 d PD D 4 O23 O 0.2962(8) 0.1462(3) 0.4992(3) 0.017(2) Uiso 0.25 1 d PD D 4 O24 O 0.2512(15) 0.1190(5) 0.4588(4) 0.049(5) Uiso 0.25 1 d PD D 4 O25 O 0.3800(5) 0.03054(18) 0.4231(2) 0.081(2) Uani 1 1 d . . . O26 O 0.3608(4) 0.19252(13) 0.09297(15) 0.0600(14) Uani 1 1 d . . . O27 O 0.4776(4) 0.17214(13) 0.16971(14) 0.0634(15) Uani 1 1 d . . . O28 O 0.3231(5) 0.21333(14) 0.16012(15) 0.0678(15) Uani 1 1 d . . . O29 O 0.6289(11) 0.2834(3) 0.1806(3) 0.160(5) Uani 1 1 d . . . O30 O 0.2392(8) 0.0421(3) 0.3801(2) 0.119(3) Uani 1 1 d . . . O31 O 0.3903(9) 0.0043(2) 0.7391(2) 0.124(4) Uani 1 1 d . . . O32 O 0.2312(10) 0.0342(3) 0.6946(4) 0.028(3) Uiso 0.25 1 d P E 5 O33 O 0.3568(15) -0.0444(5) 0.6641(5) 0.053(5) Uiso 0.25 1 d P F 5 O34 O 0.1708(11) 0.0279(4) 0.6887(4) 0.035(3) Uiso 0.25 1 d P E 5 O35 O 0.0206(15) -0.0502(4) 0.6722(6) 0.024(5) Uiso 0.25 1 d P G 6 O36 O 0.2264(10) -0.0320(3) 0.6577(4) 0.028(3) Uiso 0.25 1 d P H 6 O37 O 0.3484(11) 0.0432(4) 0.6914(4) 0.032(3) Uiso 0.25 1 d P I 6 O38 O 0.3284(17) -0.0128(6) 0.6049(6) 0.062(5) Uiso 0.25 1 d P J 7 O39 O 0.3391(9) -0.0540(3) 0.7059(3) 0.020(2) Uiso 0.25 1 d P . . O40 O 0.2426(9) 0.1621(3) 0.4455(3) 0.024(3) Uiso 0.25 1 d P . . O41 O 0.3403(13) 0.0538(4) 0.6406(5) 0.044(4) Uiso 0.25 1 d P . . O42 O 0.6991(13) 0.2324(4) 0.2097(4) 0.045(4) Uiso 0.25 1 d P . . O43 O 0.442(2) 0.0355(7) 0.6292(7) 0.077(7) Uiso 0.25 1 d P K 8 O44 O 0.3944(13) -0.0027(5) 0.6164(5) 0.046(4) Uiso 0.25 1 d P L 9 O45 O 0.2495(13) -0.0167(4) 0.5485(5) 0.043(4) Uiso 0.25 1 d P M 10 O46 O -0.0134(13) -0.0497(4) 0.6842(5) 0.034(4) Uiso 0.25 1 d P N 11 O47 O 0.2749(17) 0.0385(6) 0.4750(6) 0.064(6) Uiso 0.25 1 d P O 12 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 0.0299(3) 0.0148(3) 0.0132(3) 0.00176(18) -0.0071(2) -0.0079(2) O1 0.0356(19) 0.0281(19) 0.030(2) -0.0040(15) 0.0007(15) -0.0060(15) N1 0.0252(19) 0.0215(19) 0.0069(17) -0.0007(12) -0.0035(13) -0.0060(14) N2 0.0276(19) 0.0125(16) 0.0192(18) -0.0003(14) -0.0038(15) -0.0041(14) N3 0.0317(19) 0.0173(17) 0.0158(18) -0.0005(14) -0.0028(15) -0.0093(15) N4 0.026(2) 0.0210(19) 0.018(2) 0.0014(14) -0.0058(17) 0.0057(15) C1 0.030(2) 0.017(2) 0.024(2) 0.0001(17) -0.0067(18) -0.0040(18) C2 0.030(2) 0.028(2) 0.019(2) -0.0036(18) -0.0010(18) 0.0001(19) C3 0.023(2) 0.031(3) 0.015(2) -0.0026(17) -0.0038(18) -0.0006(18) C4 0.034(2) 0.027(2) 0.018(2) -0.0026(19) -0.0087(19) 0.0054(19) C5 0.032(2) 0.022(2) 0.016(2) -0.0002(17) -0.0010(17) 0.0005(18) C6 0.027(2) 0.027(2) 0.014(2) -0.0003(17) -0.0071(18) 0.0034(18) C7 0.024(2) 0.036(3) 0.017(2) 0.0013(19) -0.0058(17) 0.005(2) C8 0.028(2) 0.031(3) 0.014(2) -0.0017(18) -0.0016(17) 0.0087(19) C9 0.026(2) 0.025(2) 0.017(2) -0.0036(17) -0.0034(16) 0.0066(17) C10 0.028(2) 0.031(2) 0.018(2) -0.0027(18) 0.0004(18) 0.0078(19) C11 0.026(2) 0.019(2) 0.029(3) 0.0029(18) -0.0066(19) -0.0044(18) C12 0.031(2) 0.017(2) 0.030(3) 0.0032(18) -0.006(2) -0.0009(18) C13 0.031(2) 0.014(2) 0.022(2) -0.0015(16) 0.0017(18) -0.0045(17) C14 0.027(2) 0.023(2) 0.028(3) 0.0014(19) -0.0078(19) -0.0054(18) C15 0.028(2) 0.016(2) 0.024(2) 0.0013(17) -0.0040(18) -0.0020(17) C16 0.031(2) 0.020(2) 0.021(2) -0.0010(16) 0.0022(17) -0.0029(17) C17 0.031(2) 0.021(2) 0.020(2) 0.0046(17) 0.0028(17) -0.0054(18) C18 0.031(2) 0.017(2) 0.025(3) -0.0016(18) -0.0024(19) -0.0095(18) C19 0.043(3) 0.019(2) 0.024(2) -0.0058(18) 0.007(2) -0.007(2) C20 0.037(3) 0.023(2) 0.021(2) -0.0030(19) 0.004(2) -0.011(2) O2 0.039(2) 0.037(2) 0.032(2) -0.0019(17) -0.0036(16) -0.0049(17) Cu2 0.0379(4) 0.0159(3) 0.0167(3) -0.0022(2) -0.0036(2) 0.0095(2) O3 0.0319(19) 0.040(2) 0.041(2) 0.0038(18) 0.0024(17) 0.0015(17) N5 0.037(2) 0.021(2) 0.025(3) -0.0032(14) -0.0018(18) 0.0083(16) N6 0.032(2) 0.0164(18) 0.022(2) -0.0017(15) -0.0036(16) 0.0061(15) N7 0.039(2) 0.0168(18) 0.023(2) -0.0016(16) -0.0003(17) 0.0090(16) N8 0.032(2) 0.0213(19) 0.0157(19) 0.0034(14) 0.0011(17) -0.0055(16) C21 0.034(2) 0.024(2) 0.022(3) -0.0005(18) -0.0051(19) 0.0039(19) C22 0.033(2) 0.024(2) 0.023(2) 0.0023(18) -0.0060(19) 0.0056(19) C23 0.029(3) 0.029(3) 0.015(2) -0.0019(17) 0.0029(19) 0.0036(19) C24 0.039(3) 0.024(2) 0.022(2) -0.0032(19) -0.003(2) -0.002(2) C25 0.039(3) 0.028(2) 0.020(2) 0.0034(19) -0.003(2) 0.002(2) C26 0.027(2) 0.024(2) 0.017(2) 0.0010(17) -0.0004(19) 0.0040(17) C27 0.028(2) 0.036(3) 0.028(3) 0.000(2) -0.001(2) -0.005(2) C28 0.038(3) 0.029(3) 0.025(3) 0.002(2) -0.001(2) -0.010(2) C29 0.029(2) 0.028(2) 0.019(2) 0.0021(19) -0.0014(18) -0.0036(18) C30 0.028(2) 0.031(2) 0.016(2) 0.0029(18) 0.0023(18) -0.0014(19) C31 0.030(2) 0.025(2) 0.027(3) -0.001(2) -0.0001(19) 0.0019(19) C32 0.030(2) 0.016(2) 0.029(2) 0.0012(18) 0.0013(19) 0.0012(18) C33 0.028(2) 0.016(2) 0.025(3) -0.0002(17) -0.0005(18) 0.0024(18) C34 0.031(2) 0.015(2) 0.033(3) -0.0008(19) -0.002(2) 0.0058(18) C35 0.034(2) 0.014(2) 0.031(3) -0.0053(18) -0.008(2) 0.0045(18) C36 0.046(3) 0.020(2) 0.017(2) 0.0022(17) 0.0065(19) 0.007(2) C37 0.048(3) 0.028(3) 0.021(3) 0.0014(19) 0.009(2) 0.015(2) C38 0.036(2) 0.018(2) 0.027(3) -0.0020(19) -0.003(2) 0.0034(19) C39 0.046(3) 0.026(2) 0.028(3) 0.004(2) 0.007(2) 0.006(2) C40 0.042(3) 0.025(2) 0.023(2) 0.001(2) 0.009(2) 0.007(2) N9 0.052(4) 0.123(8) 0.049(4) 0.010(5) -0.001(3) 0.000(4) O4 0.121(7) 0.124(7) 0.061(4) 0.039(4) -0.008(4) -0.012(6) O5 0.039(3) 0.383(19) 0.040(3) -0.041(7) -0.004(3) 0.008(6) O6 0.072(4) 0.169(8) 0.052(4) -0.021(4) -0.024(3) 0.039(5) N10 0.041(3) 0.073(5) 0.103(6) -0.023(5) -0.017(4) 0.004(3) O7 0.079(4) 0.042(3) 0.138(7) 0.004(4) -0.041(4) -0.007(3) O8 0.058(3) 0.061(3) 0.155(7) -0.001(4) -0.014(4) 0.026(3) O9 0.094(6) 0.093(5) 0.122(7) -0.020(5) 0.012(5) 0.014(5) N11 0.072(4) 0.078(5) 0.043(3) -0.017(3) 0.001(3) 0.007(4) O10 0.042(2) 0.030(2) 0.059(3) -0.003(2) 0.012(2) 0.0000(18) O11 0.124(8) 0.250(14) 0.094(7) -0.080(8) -0.048(6) 0.027(9) O12 0.124(7) 0.095(5) 0.078(5) 0.017(4) -0.005(5) -0.029(5) O25 0.078(4) 0.071(4) 0.093(5) 0.007(4) 0.022(4) 0.007(3) O26 0.065(3) 0.053(3) 0.062(3) 0.015(3) -0.005(3) 0.008(2) O27 0.070(4) 0.047(3) 0.073(4) -0.013(2) 0.007(3) 0.005(3) O28 0.076(4) 0.063(3) 0.065(4) 0.001(3) 0.017(3) 0.003(3) O29 0.214(15) 0.126(10) 0.140(11) 0.002(8) -0.005(9) 0.035(9) O30 0.135(8) 0.144(8) 0.079(5) 0.000(5) -0.001(5) -0.051(7) O31 0.184(10) 0.123(7) 0.066(5) -0.005(5) 0.004(5) -0.061(7) _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 N2 2.028(4) . ? Cu1 N3 2.032(4) . ? Cu1 N4 2.034(4) 3 ? Cu1 N1 2.036(4) . ? Cu1 O1 2.367(4) . ? N1 C5 1.323(6) . ? N1 C1 1.343(6) . ? N2 C15 1.340(6) . ? N2 C11 1.348(6) . ? N3 C16 1.336(6) . ? N3 C20 1.349(6) . ? N4 C9 1.334(6) . ? N4 C8 1.353(6) . ? N4 Cu1 2.034(4) 11_454 ? C1 C2 1.384(7) . ? C1 H1A 0.9500 . ? C2 C3 1.379(7) . ? C2 H2A 0.9500 . ? C3 C4 1.396(7) . ? C3 C6 1.502(7) . ? C4 C5 1.391(7) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C10 1.388(7) . ? C6 C7 1.398(7) . ? C7 C8 1.385(7) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C10 1.387(7) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.398(7) . ? C11 H11A 0.9500 . ? C12 C13 1.367(7) . ? C12 H12A 0.9500 . ? C13 C14 1.391(7) . ? C13 C13 1.508(9) 2_655 ? C14 C15 1.385(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.388(6) . ? C16 H16A 0.9500 . ? C17 C18 1.385(7) . ? C17 H17A 0.9500 . ? C18 C19 1.408(7) . ? C18 C18 1.478(9) 14_655 ? C19 C20 1.368(7) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? Cu2 N5 2.034(5) . ? Cu2 N6 2.036(4) . ? Cu2 N8 2.040(4) 11_454 ? Cu2 N7 2.042(4) . ? Cu2 O3 2.350(4) . ? N5 C21 1.332(7) . ? N5 C25 1.353(7) . ? N6 C31 1.334(7) . ? N6 C35 1.343(7) . ? N7 C36 1.332(7) . ? N7 C40 1.355(7) . ? N8 C28 1.339(7) . ? N8 C29 1.350(7) . ? N8 Cu2 2.040(4) 3 ? C21 C22 1.391(7) . ? C21 H21A 0.9500 . ? C22 C23 1.387(7) . ? C22 H22A 0.9500 . ? C23 C24 1.397(7) . ? C23 C26 1.460(7) . ? C24 C25 1.389(7) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.382(7) . ? C26 C30 1.401(7) . ? C27 C28 1.390(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.364(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.384(7) . ? C31 H31A 0.9500 . ? C32 C33 1.401(7) . ? C32 H32A 0.9500 . ? C33 C34 1.399(7) . ? C33 C33 1.464(9) 2_655 ? C34 C35 1.387(6) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.386(7) . ? C36 H36A 0.9500 . ? C37 C38 1.409(7) . ? C37 H37A 0.9500 . ? C38 C39 1.371(8) . ? C38 C38 1.481(9) 14 ? C39 C40 1.376(7) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? N9 O5 1.148(11) . ? N9 O4 1.168(10) . ? N9 O6 1.258(9) . ? N10 O7 1.212(9) . ? N10 O8 1.215(9) . ? N10 O9 1.251(9) . ? N11 O10 1.220(8) . ? N11 O11 1.244(9) . ? N11 O12 1.284(9) . ? N12 O13 1.197(14) . ? N12 O14 1.222(13) . ? N12 O15 1.265(13) . ? N13 O16 1.173(14) . ? N13 O18 1.234(13) . ? N13 O17 1.237(13) . ? N14 O20 1.222(15) . ? N14 O19 1.225(14) . ? N14 O21 1.225(14) . ? N15 O23 1.171(14) . ? N15 O22 1.189(14) . ? N15 O24 1.246(14) . ? O32 O34 0.94(2) . ? O41 O43 1.72(3) . ? 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 N2 Cu1 N3 179.31(17) . . ? N2 Cu1 N4 89.55(16) . 3 ? N3 Cu1 N4 90.23(15) . 3 ? N2 Cu1 N1 89.37(15) . . ? N3 Cu1 N1 90.82(15) . . ? N4 Cu1 N1 177.02(18) 3 . ? N2 Cu1 O1 88.93(15) . . ? N3 Cu1 O1 91.72(16) . . ? N4 Cu1 O1 89.46(16) 3 . ? N1 Cu1 O1 93.29(16) . . ? C5 N1 C1 118.0(4) . . ? C5 N1 Cu1 121.9(3) . . ? C1 N1 Cu1 120.1(3) . . ? C15 N2 C11 118.3(4) . . ? C15 N2 Cu1 120.5(3) . . ? C11 N2 Cu1 121.1(3) . . ? C16 N3 C20 117.2(4) . . ? C16 N3 Cu1 121.4(3) . . ? C20 N3 Cu1 121.3(3) . . ? C9 N4 C8 117.5(4) . . ? C9 N4 Cu1 121.0(3) . 11_454 ? C8 N4 Cu1 121.5(3) . 11_454 ? N1 C1 C2 122.9(4) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 118.7(5) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 118.9(5) . . ? C2 C3 C6 120.8(4) . . ? C4 C3 C6 120.2(4) . . ? C5 C4 C3 118.0(5) . . ? C5 C4 H4A 121.0 . . ? C3 C4 H4A 121.0 . . ? N1 C5 C4 123.5(5) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C10 C6 C7 118.5(5) . . ? C10 C6 C3 121.1(5) . . ? C7 C6 C3 120.4(4) . . ? C8 C7 C6 118.7(4) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? N4 C8 C7 123.0(5) . . ? N4 C8 H8A 118.5 . . ? C7 C8 H8A 118.5 . . ? N4 C9 C10 123.4(4) . . ? N4 C9 H9A 118.3 . . ? C10 C9 H9A 118.3 . . ? C9 C10 C6 118.9(5) . . ? C9 C10 H10A 120.6 . . ? C6 C10 H10A 120.6 . . ? N2 C11 C12 121.2(4) . . ? N2 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 C13 120.9(5) . 2_655 ? C14 C13 C13 119.7(5) . 2_655 ? C15 C14 C13 117.9(4) . . ? C15 C14 H14A 121.1 . . ? C13 C14 H14A 121.1 . . ? N2 C15 C14 123.4(4) . . ? N2 C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? N3 C16 C17 123.3(4) . . ? N3 C16 H16A 118.3 . . ? C17 C16 H16A 118.3 . . ? C18 C17 C16 118.9(4) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 118.0(4) . . ? C17 C18 C18 121.8(4) . 14_655 ? C19 C18 C18 120.1(4) . 14_655 ? C20 C19 C18 118.7(5) . . ? C20 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? N3 C20 C19 123.7(5) . . ? N3 C20 H20A 118.2 . . ? C19 C20 H20A 118.2 . . ? N5 Cu2 N6 88.93(16) . . ? N5 Cu2 N8 179.73(16) . 11_454 ? N6 Cu2 N8 90.80(16) . 11_454 ? N5 Cu2 N7 90.55(17) . . ? N6 Cu2 N7 174.16(18) . . ? N8 Cu2 N7 89.72(17) 11_454 . ? N5 Cu2 O3 90.11(18) . . ? N6 Cu2 O3 93.64(17) . . ? N8 Cu2 O3 89.86(17) 11_454 . ? N7 Cu2 O3 92.18(17) . . ? C21 N5 C25 118.0(5) . . ? C21 N5 Cu2 120.6(4) . . ? C25 N5 Cu2 121.4(4) . . ? C31 N6 C35 118.8(4) . . ? C31 N6 Cu2 120.8(3) . . ? C35 N6 Cu2 120.3(3) . . ? C36 N7 C40 118.9(4) . . ? C36 N7 Cu2 121.6(3) . . ? C40 N7 Cu2 119.3(3) . . ? C28 N8 C29 117.8(5) . . ? C28 N8 Cu2 120.7(4) . 3 ? C29 N8 Cu2 121.5(4) . 3 ? N5 C21 C22 122.6(5) . . ? N5 C21 H21A 118.7 . . ? C22 C21 H21A 118.7 . . ? C23 C22 C21 120.1(5) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 117.3(5) . . ? C22 C23 C26 121.5(5) . . ? C24 C23 C26 121.2(5) . . ? C25 C24 C23 119.5(5) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? N5 C25 C24 122.5(5) . . ? N5 C25 H25A 118.7 . . ? C24 C25 H25A 118.7 . . ? C27 C26 C30 116.7(5) . . ? C27 C26 C23 122.0(5) . . ? C30 C26 C23 121.3(5) . . ? C26 C27 C28 120.5(5) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? N8 C28 C27 122.0(5) . . ? N8 C28 H28A 119.0 . . ? C27 C28 H28A 119.0 . . ? N8 C29 C30 123.1(5) . . ? N8 C29 H29A 118.5 . . ? C30 C29 H29A 118.5 . . ? C29 C30 C26 120.0(5) . . ? C29 C30 H30A 120.0 . . ? C26 C30 H30A 120.0 . . ? N6 C31 C32 122.2(5) . . ? N6 C31 H31A 118.9 . . ? C32 C31 H31A 118.9 . . ? C31 C32 C33 119.8(5) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C34 C33 C32 117.5(4) . . ? C34 C33 C33 120.6(5) . 2_655 ? C32 C33 C33 122.0(5) . 2_655 ? C35 C34 C33 119.0(5) . . ? C35 C34 H34A 120.5 . . ? C33 C34 H34A 120.5 . . ? N6 C35 C34 122.7(5) . . ? N6 C35 H35A 118.6 . . ? C34 C35 H35A 118.6 . . ? N7 C36 C37 122.5(5) . . ? N7 C36 H36A 118.8 . . ? C37 C36 H36A 118.8 . . ? C36 C37 C38 118.8(5) . . ? C36 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? C39 C38 C37 117.6(5) . . ? C39 C38 C38 120.7(4) . 14 ? C37 C38 C38 121.7(4) . 14 ? C38 C39 C40 120.9(5) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? N7 C40 C39 121.3(5) . . ? N7 C40 H40A 119.4 . . ? C39 C40 H40A 119.4 . . ? O5 N9 O4 113.2(9) . . ? O5 N9 O6 124.0(10) . . ? O4 N9 O6 122.6(10) . . ? O7 N10 O8 126.9(9) . . ? O7 N10 O9 119.4(8) . . ? O8 N10 O9 113.7(9) . . ? O10 N11 O11 134.4(10) . . ? O10 N11 O12 115.1(7) . . ? O11 N11 O12 110.4(10) . . ? O13 N12 O14 132.4(15) . . ? O13 N12 O15 112.5(15) . . ? O14 N12 O15 114.8(13) . . ? O16 N13 O18 116.5(16) . . ? O16 N13 O17 127.6(16) . . ? O18 N13 O17 115.8(14) . . ? O20 N14 O19 115.1(17) . . ? O20 N14 O21 122(2) . . ? O19 N14 O21 122.4(19) . . ? O23 N15 O22 114.3(14) . . ? O23 N15 O24 125.8(16) . . ? O22 N15 O24 119.8(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.368 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.165 data_CIF_file_of_[Cu(BPY)(NO3)2] _database_code_depnum_ccdc_archive 'CCDC 194213' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 N2 Cu 2+, 2 N O3 -' _chemical_formula_sum 'C10 H8 N4 O6 Cu' _chemical_formula_weight 343.74 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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 7.8122(8) _cell_length_b 7.8122(8) _cell_length_c 20.232(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1234.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3271 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 23.54 _exptl_crystal_description 'Prismatic block' _exptl_crystal_colour Purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 1.805 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4804 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 223(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' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 5724 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 23.54 _reflns_number_total 937 _reflns_number_gt 805 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^ > 4sigma(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^)+(0.0470P)^2^+0.0692P] 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 0.0038(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 917 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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 Cu Cu 0.80088(5) 0.80088(5) 0.0000 0.0205(2) Uani 1 2 d S . . O1 O 0.6503(3) 0.9500(3) 0.05324(10) 0.0233(5) Uani 1 1 d . . . O2 O 0.7944(3) 0.8010(3) 0.12401(11) 0.0345(6) Uani 1 1 d . . . O3 O 0.5866(4) 0.9657(4) 0.15680(12) 0.0442(7) Uani 1 1 d . . . N1 N 0.6204(3) 0.6204(3) 0.0000 0.0229(9) Uani 1 2 d S . . N2 N -0.0203(3) -0.0203(3) 0.0000 0.0201(8) Uani 1 2 d S . . N3 N 0.6766(4) 0.9050(4) 0.11363(13) 0.0273(7) Uani 1 1 d . . . C1 C 0.6283(5) 0.4863(4) 0.04069(18) 0.0272(9) Uani 1 1 d . . . H1 H 0.7221 0.4784 0.0696 0.033 Uiso 1 1 calc R . . C2 C 0.5070(5) 0.3592(5) 0.04263(18) 0.0273(9) Uani 1 1 d . . . H2 H 0.5185 0.2677 0.0725 0.033 Uiso 1 1 calc R . . C3 C 0.3662(4) 0.3662(4) 0.0000 0.0225(11) Uani 1 2 d S . . C4 C 0.2317(4) 0.2317(4) 0.0000 0.0199(11) Uani 1 2 d S . . C5 C 0.2674(4) 0.0644(5) 0.01785(16) 0.0267(8) Uani 1 1 d . . . H5 H 0.3787 0.0342 0.0312 0.032 Uiso 1 1 calc R . . C6 C 0.1422(4) -0.0564(4) 0.01623(16) 0.0241(8) Uani 1 1 d . . . H6 H 0.1707 -0.1699 0.0269 0.029 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 Cu 0.0181(2) 0.0181(2) 0.0252(3) -0.00154(19) 0.00154(19) -0.0064(3) O1 0.0225(13) 0.0265(13) 0.0209(12) 0.0018(11) 0.0013(10) -0.0008(10) O2 0.0329(17) 0.0355(17) 0.0350(13) 0.0049(13) -0.0017(12) 0.0028(14) O3 0.0436(17) 0.0548(18) 0.0342(14) -0.0164(13) 0.0101(13) 0.0014(16) N1 0.0212(13) 0.0212(13) 0.0263(19) -0.0006(15) 0.0006(15) -0.0074(18) N2 0.0210(13) 0.0210(13) 0.0183(18) -0.0013(12) 0.0013(12) 0.0000(16) N3 0.0263(17) 0.0289(17) 0.0267(15) -0.0095(13) 0.0057(14) -0.0096(16) C1 0.023(2) 0.027(2) 0.0317(19) -0.0020(17) -0.0047(16) -0.0063(16) C2 0.028(2) 0.022(2) 0.032(2) 0.0024(15) -0.0001(16) -0.0033(16) C3 0.0183(16) 0.0183(16) 0.031(2) -0.0033(17) 0.0033(17) -0.0020(19) C4 0.0189(16) 0.0189(16) 0.022(2) -0.0037(16) 0.0037(16) -0.007(2) C5 0.0159(17) 0.028(2) 0.036(2) 0.0039(15) -0.0031(14) -0.0022(16) C6 0.0245(19) 0.0182(17) 0.029(2) 0.0045(14) -0.0004(14) -0.0004(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 Cu O1 1.975(2) . ? Cu O1 1.975(2) 7 ? Cu N2 1.976(4) 1_665 ? Cu N1 1.994(4) . ? O1 N3 1.288(3) . ? O2 N3 1.245(4) . ? O3 N3 1.218(4) . ? N1 C1 1.334(4) 7 ? N1 C1 1.334(4) . ? N2 C6 1.341(4) . ? N2 C6 1.341(4) 7 ? N2 Cu 1.976(4) 1_445 ? C1 C2 1.374(5) . ? C2 C3 1.399(4) . ? C3 C2 1.399(4) 7 ? C3 C4 1.486(6) . ? C4 C5 1.384(4) 7 ? C4 C5 1.384(4) . ? C5 C6 1.360(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 O1 Cu O1 179.55(14) . 7 ? O1 Cu N2 90.22(7) . 1_665 ? O1 Cu N2 90.22(7) 7 1_665 ? O1 Cu N1 89.78(7) . . ? O1 Cu N1 89.77(7) 7 . ? N2 Cu N1 180.0 1_665 . ? N3 O1 Cu 105.13(19) . . ? C1 N1 C1 117.0(4) 7 . ? C1 N1 Cu 121.5(2) 7 . ? C1 N1 Cu 121.5(2) . . ? C6 N2 C6 117.2(4) . 7 ? C6 N2 Cu 121.4(2) . 1_445 ? C6 N2 Cu 121.4(2) 7 1_445 ? O3 N3 O2 124.1(3) . . ? O3 N3 O1 118.8(3) . . ? O2 N3 O1 117.2(2) . . ? N1 C1 C2 123.6(4) . . ? C1 C2 C3 119.8(4) . . ? C2 C3 C2 116.2(4) . 7 ? C2 C3 C4 121.9(2) . . ? C2 C3 C4 121.9(2) 7 . ? C5 C4 C5 116.6(4) 7 . ? C5 C4 C3 121.7(2) 7 . ? C5 C4 C3 121.7(2) . . ? C6 C5 C4 120.3(3) . . ? N2 C6 C5 122.8(3) . . ? 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 O1 Cu O1 N3 85.3(2) 7 . . . ? N2 Cu O1 N3 -94.72(19) 1_665 . . . ? N1 Cu O1 N3 85.28(19) . . . . ? O1 Cu N1 C1 79.4(2) . . . 7 ? O1 Cu N1 C1 -100.6(2) 7 . . 7 ? N2 Cu N1 C1 -133.62(19) 1_665 . . 7 ? O1 Cu N1 C1 -100.6(2) . . . . ? O1 Cu N1 C1 79.4(2) 7 . . . ? N2 Cu N1 C1 46.38(19) 1_665 . . . ? Cu O1 N3 O3 -172.8(2) . . . . ? Cu O1 N3 O2 7.3(3) . . . . ? C1 N1 C1 C2 -0.2(3) 7 . . . ? Cu N1 C1 C2 179.8(3) . . . . ? N1 C1 C2 C3 0.4(6) . . . . ? C1 C2 C3 C2 -0.2(3) . . . 7 ? C1 C2 C3 C4 179.8(3) . . . . ? C2 C3 C4 C5 151.3(2) . . . 7 ? C2 C3 C4 C5 -28.7(2) 7 . . 7 ? C2 C3 C4 C5 -28.7(2) . . . . ? C2 C3 C4 C5 151.3(2) 7 . . . ? C5 C4 C5 C6 1.2(2) 7 . . . ? C3 C4 C5 C6 -178.8(2) . . . . ? C6 N2 C6 C5 1.2(2) 7 . . . ? Cu N2 C6 C5 -178.8(2) 1_445 . . . ? C4 C5 C6 N2 -2.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.470 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.063