Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Jorge A. R. Navarro' _publ_contact_author_address ; Department of Inorganic Chemistry University of Granada Av. fuentenueva S/N Granada 18071 SPAIN ; _publ_contact_author_email JARN@UGR.ES _publ_section_title ; Heteroleptic Pyrimidine-2-olate and 4,4'-bipyridine Copper(II) Layered Metal-organic Frameworks with Swelling Properties ; loop_ _publ_author_name 'Jorge A. R. Navarro' 'Elisa Barea' 'Miguel Quiros' 'Juan M. Salas' data_cuel _database_code_depnum_ccdc_archive 'CCDC 232901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cu3Cl2(OH)3(2-pymo)(4,4'-bpy)1.5)n(NO3)n.6.25nH2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H41.50 Cl2 Cu3 N9 O12.25' _chemical_formula_weight 1033.78 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' Cl Cl 0.1484 0.1585 '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 orthorrombic _symmetry_space_group_name_H-M 'P n n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.076(3) _cell_length_b 19.341(3) _cell_length_c 13.481(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4452.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2098 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.7 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2110 _exptl_absorpt_coefficient_mu 1.607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6260 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details ? _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27660 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.44 _reflns_number_total 8792 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+15.0000P] 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 constr _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 0.38(3) _refine_ls_number_reflns 8792 _refine_ls_number_parameters 532 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.2176 _refine_ls_wR_factor_gt 0.2010 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.001 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 0.74340(8) 0.39747(6) 0.5000 0.0191(3) Uani 1 1 d . . . Cu2 Cu 0.78112(7) 0.53035(6) 0.63488(15) 0.0193(3) Uani 1 1 d . . . Cu3 Cu 0.70975(7) 0.26090(6) 0.36270(15) 0.0178(3) Uani 1 1 d . . . Cl2 Cl 0.59672(18) 0.33689(14) 0.4426(2) 0.0335(7) Uani 1 1 d . . . Cl3 Cl 0.88731(15) 0.44800(12) 0.5623(2) 0.0218(5) Uani 1 1 d . . . O2 O 0.6993(4) 0.4752(4) 0.5766(6) 0.0242(17) Uani 1 1 d . . . O3 O 0.7847(4) 0.3205(4) 0.4245(5) 0.0206(16) Uani 1 1 d . . . N1P N 0.6363(5) 0.1969(4) 0.2968(6) 0.0200(19) Uani 1 1 d . . . C2P C 0.6795(6) 0.1463(6) 0.2496(8) 0.021(2) Uani 1 1 d . . . O2P O 0.7518(4) 0.1468(4) 0.2498(6) 0.0212(14) Uani 1 1 d . . . N3P N 0.6392(5) 0.0939(4) 0.1974(7) 0.0214(19) Uani 1 1 d . . . C4P C 0.5631(7) 0.0941(5) 0.1939(10) 0.031(3) Uani 1 1 d . . . H4P H 0.5368 0.0591 0.1574 0.037 Uiso 1 1 d R . . C5P C 0.5198(7) 0.1449(7) 0.2394(11) 0.038(3) Uani 1 1 d . . . H5P H 0.4642 0.1450 0.2375 0.045 Uiso 1 1 d R . . C6P C 0.5602(6) 0.1964(5) 0.2919(9) 0.026(2) Uani 1 1 d . . . H6P H 0.5315 0.2319 0.3243 0.032 Uiso 1 1 d R . . N11 N 0.7471(5) 0.4572(4) 0.3744(7) 0.0207(19) Uani 1 1 d . . . C12 C 0.6874(6) 0.4976(5) 0.3478(8) 0.021(2) Uani 1 1 d . . . H12 H 0.6409 0.4968 0.3865 0.025 Uiso 1 1 d R . . C13 C 0.6906(6) 0.5401(5) 0.2672(8) 0.020(2) Uani 1 1 d . . . H13 H 0.6471 0.5683 0.2504 0.024 Uiso 1 1 d R . . C14 C 0.7563(7) 0.5422(5) 0.2103(8) 0.023(2) Uani 1 1 d . . . C15 C 0.8195(6) 0.4990(5) 0.2360(8) 0.019(2) Uani 1 1 d . . . H15 H 0.8656 0.4977 0.1966 0.023 Uiso 1 1 d R . . C16 C 0.8120(6) 0.4577(5) 0.3201(8) 0.022(2) Uani 1 1 d . . . H16 H 0.8547 0.4292 0.3392 0.026 Uiso 1 1 d R . . N21 N 0.7385(5) 0.3365(4) 0.6230(7) 0.024(2) Uani 1 1 d . . . C22 C 0.6760(7) 0.3323(5) 0.6818(8) 0.023(2) Uani 1 1 d . . . H22 H 0.6324 0.3610 0.6670 0.027 Uiso 1 1 d R . . C23 C 0.6703(7) 0.2885(5) 0.7618(8) 0.026(2) Uani 1 1 d . . . H23 H 0.6227 0.2852 0.7979 0.032 Uiso 1 1 d R . . C24 C 0.7351(7) 0.2494(5) 0.7895(8) 0.020(2) Uani 1 1 d . . . C25 C 0.8011(7) 0.2537(5) 0.7295(10) 0.028(3) Uani 1 1 d . . . H25 H 0.8456 0.2260 0.7440 0.033 Uiso 1 1 d R . . C26 C 0.8027(7) 0.2973(5) 0.6480(9) 0.024(2) Uani 1 1 d . . . H26 H 0.8488 0.3003 0.6088 0.029 Uiso 1 1 d R . . N31 N 0.7741(5) 0.6000(4) 0.5212(6) 0.022(2) Uani 1 1 d . . . C32 C 0.8356(7) 0.6145(5) 0.4675(9) 0.032(3) Uani 1 1 d . . . H32 H 0.8832 0.5912 0.4819 0.038 Uiso 1 1 d R . . C33 C 0.8357(7) 0.6626(6) 0.3919(8) 0.030(3) Uani 1 1 d . . . H33 H 0.8812 0.6698 0.3527 0.037 Uiso 1 1 d R . . C34 C 0.7690(7) 0.7000(5) 0.3729(9) 0.025(2) Uani 1 1 d . . . C35 C 0.7032(7) 0.6840(5) 0.4311(8) 0.026(2) Uani 1 1 d . . . H35 H 0.6546 0.7065 0.4194 0.031 Uiso 1 1 d R . . C36 C 0.7090(6) 0.6359(5) 0.5044(9) 0.022(2) Uani 1 1 d . . . H36 H 0.6647 0.6272 0.5452 0.027 Uiso 1 1 d R . . N41 N 0.7659(5) 0.4832(4) 0.7689(7) 0.0213(19) Uani 1 1 d . . . C42 C 0.6987(7) 0.4784(6) 0.8123(9) 0.033(3) Uani 1 1 d . . . H42 H 0.6550 0.4985 0.7797 0.040 Uiso 1 1 d R . . C43 C 0.6855(8) 0.4468(6) 0.9038(9) 0.037(3) Uani 1 1 d . . . H43 H 0.6343 0.4446 0.9311 0.045 Uiso 1 1 d R . . C44 C 0.7482(7) 0.4177(5) 0.9528(8) 0.022(2) Uani 1 1 d . . . C45 C 0.8220(8) 0.4248(7) 0.9093(10) 0.040(3) Uani 1 1 d . . . H45 H 0.8676 0.4090 0.9426 0.048 Uiso 1 1 d R . . C46 C 0.8278(8) 0.4565(7) 0.8195(9) 0.039(3) Uani 1 1 d . . . H46 H 0.8782 0.4593 0.7898 0.046 Uiso 1 1 d R . . N51 N 0.7218(5) 0.1893(4) 0.4736(6) 0.0184(19) Uani 1 1 d . . . C52 C 0.6616(7) 0.1740(5) 0.5324(8) 0.025(2) Uani 1 1 d . . . H52 H 0.6138 0.1982 0.5227 0.030 Uiso 1 1 d R . . C53 C 0.6646(6) 0.1256(5) 0.6076(8) 0.025(2) Uani 1 1 d . . . H53 H 0.6197 0.1155 0.6467 0.030 Uiso 1 1 d R . . C54 C 0.7361(6) 0.0916(5) 0.6246(8) 0.019(2) Uani 1 1 d . . . C55 C 0.7971(6) 0.1053(5) 0.5625(9) 0.026(2) Uani 1 1 d . . . H55 H 0.8449 0.0808 0.5701 0.032 Uiso 1 1 d R . . C56 C 0.7898(6) 0.1547(5) 0.4869(8) 0.020(2) Uani 1 1 d . . . H56 H 0.8334 0.1642 0.4453 0.024 Uiso 1 1 d R . . N61 N 0.7206(5) 0.3130(4) 0.2303(7) 0.0197(18) Uani 1 1 d . . . C62 C 0.7841(8) 0.3073(7) 0.1773(10) 0.040(3) Uani 1 1 d . . . H62 H 0.8250 0.2790 0.2023 0.048 Uiso 1 1 d R . . C63 C 0.7957(8) 0.3385(6) 0.0885(10) 0.040(3) Uani 1 1 d . . . H63 H 0.8432 0.3313 0.0535 0.048 Uiso 1 1 d R . . C64 C 0.7393(7) 0.3818(5) 0.0488(9) 0.024(2) Uani 1 1 d . . . C65 C 0.6712(7) 0.3871(7) 0.1064(9) 0.037(3) Uani 1 1 d . . . H65 H 0.6296 0.4159 0.0844 0.044 Uiso 1 1 d R . . C66 C 0.6643(7) 0.3524(6) 0.1931(9) 0.037(3) Uani 1 1 d . . . H66 H 0.6172 0.3566 0.2300 0.044 Uiso 1 1 d R . . N1N N 0.996(2) 0.4504(9) 0.0161(15) 0.122(14) Uiso 0.50 1 d PD . . O1N O 1.003(2) 0.4866(12) -0.0568(12) 0.071(7) Uiso 0.50 1 d PD . . O2N O 0.988(3) 0.3879(9) 0.007(2) 0.175(18) Uiso 0.50 1 d PD . . O3N O 0.9832(17) 0.4764(11) 0.0971(13) 0.099(9) Uiso 0.50 1 d PD . . N2N N 0.493(2) 0.3580(14) 0.0239(19) 0.119(14) Uiso 0.50 1 d PD . . O4N O 0.4780(16) 0.3393(12) 0.108(2) 0.089(8) Uiso 0.50 1 d PD . . O5N O 0.487(3) 0.4194(17) 0.001(3) 0.179(17) Uiso 0.50 1 d PD . . O6N O 0.498(7) 0.315(2) -0.042(3) 0.57(8) Uiso 0.50 1 d PD . . O1W O 1.0000 0.5000 0.3946(10) 0.048(3) Uani 1 2 d S . . O2W O 0.4637(7) 0.2677(6) 0.5684(11) 0.085(4) Uani 1 1 d . . . O3W O 0.9099(7) 0.1581(10) 0.2336(10) 0.114(6) Uani 1 1 d . . . O4W O 0.9986(8) 0.3807(9) 0.2488(14) 0.129(7) Uani 1 1 d . . . O5W O 0.5000 0.5000 0.163(2) 0.089(8) Uiso 0.70 2 d SP . . O6W O 0.9410(13) 0.2833(12) 0.3806(18) 0.117(8) Uiso 0.70 1 d P . . O7W O 0.4887(15) 0.4352(13) 0.337(2) 0.138(9) Uiso 0.70 1 d P . . O8W O 0.9713(14) 0.3666(12) 0.066(2) 0.071(6) Uiso 0.50 1 d P . . O9W O 0.525(7) 0.512(6) 0.603(5) 0.36(5) Uiso 0.50 1 d P . . 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 0.0320(7) 0.0170(5) 0.0082(5) 0.0050(4) -0.0006(5) -0.0020(4) Cu2 0.0326(7) 0.0160(6) 0.0094(6) 0.0041(5) 0.0018(6) 0.0000(5) Cu3 0.0296(7) 0.0152(5) 0.0086(6) 0.0033(5) -0.0015(5) -0.0025(5) Cl2 0.0436(18) 0.0342(15) 0.0226(16) 0.0043(12) 0.0041(12) -0.0026(11) Cl3 0.0306(14) 0.0198(11) 0.0151(13) 0.0014(10) 0.0002(10) 0.0006(9) O2 0.031(5) 0.026(4) 0.015(4) 0.004(3) 0.000(3) -0.001(3) O3 0.033(4) 0.021(4) 0.008(4) 0.000(3) -0.005(3) -0.004(3) N1P 0.034(5) 0.011(4) 0.015(5) 0.006(3) 0.003(4) 0.000(3) C2P 0.048(7) 0.012(4) 0.002(4) 0.011(3) -0.005(5) -0.010(5) O2P 0.025(4) 0.024(3) 0.014(3) 0.000(2) -0.003(3) -0.001(3) N3P 0.032(5) 0.013(4) 0.019(5) 0.010(4) -0.003(4) -0.003(3) C4P 0.030(6) 0.020(5) 0.044(8) 0.003(5) -0.008(5) 0.000(4) C5P 0.044(7) 0.028(5) 0.041(8) -0.009(5) 0.004(6) 0.002(5) C6P 0.025(6) 0.022(5) 0.032(7) 0.002(5) 0.004(5) 0.004(4) N11 0.031(5) 0.018(4) 0.014(5) 0.003(4) 0.003(4) -0.001(3) C12 0.027(6) 0.023(5) 0.013(6) 0.007(4) 0.000(4) -0.001(4) C13 0.024(5) 0.021(5) 0.014(6) 0.003(4) 0.001(4) -0.004(4) C14 0.043(7) 0.017(5) 0.010(6) 0.006(4) -0.012(5) -0.009(4) C15 0.026(5) 0.014(5) 0.019(6) 0.004(4) 0.000(4) 0.002(4) C16 0.030(6) 0.022(5) 0.014(5) 0.006(4) 0.000(4) -0.002(4) N21 0.042(6) 0.018(4) 0.011(5) 0.006(4) -0.009(4) -0.003(4) C22 0.038(6) 0.014(5) 0.016(5) 0.009(4) -0.001(5) -0.002(4) C23 0.039(7) 0.026(6) 0.014(6) 0.011(4) 0.005(5) 0.000(5) C24 0.035(6) 0.015(5) 0.011(6) 0.001(4) -0.003(5) 0.002(4) C25 0.043(7) 0.016(5) 0.024(7) 0.002(5) -0.009(6) 0.005(5) C26 0.037(6) 0.019(5) 0.016(6) 0.004(4) -0.004(5) -0.002(4) N31 0.036(5) 0.022(4) 0.009(5) 0.006(4) 0.004(4) 0.005(4) C32 0.047(8) 0.022(6) 0.027(7) 0.010(5) 0.001(5) 0.005(5) C33 0.038(7) 0.037(6) 0.016(6) 0.014(5) 0.006(5) 0.004(5) C34 0.050(7) 0.012(5) 0.014(6) 0.005(4) 0.011(5) 0.004(4) C35 0.044(7) 0.022(5) 0.013(5) 0.009(4) -0.003(5) 0.009(5) C36 0.022(5) 0.030(6) 0.015(5) 0.002(5) -0.003(5) -0.006(4) N41 0.031(5) 0.016(4) 0.016(5) -0.003(4) 0.002(4) 0.001(4) C42 0.027(6) 0.048(8) 0.024(7) 0.017(6) 0.004(5) 0.014(5) C43 0.044(8) 0.045(7) 0.022(7) 0.025(6) 0.009(5) 0.005(6) C44 0.043(7) 0.011(4) 0.012(5) 0.005(4) 0.006(5) -0.003(4) C45 0.038(7) 0.057(8) 0.026(7) 0.029(6) 0.001(6) 0.009(6) C46 0.053(8) 0.050(8) 0.013(6) 0.014(6) 0.005(6) 0.008(6) N51 0.032(5) 0.020(4) 0.003(4) 0.001(3) -0.001(3) -0.008(3) C52 0.028(6) 0.026(6) 0.021(6) 0.010(4) 0.000(4) 0.001(4) C53 0.020(6) 0.027(5) 0.027(7) 0.009(5) 0.001(4) -0.002(4) C54 0.031(6) 0.019(5) 0.007(5) 0.005(4) 0.000(4) -0.002(4) C55 0.024(6) 0.025(5) 0.030(7) 0.012(5) -0.001(5) -0.002(4) C56 0.028(6) 0.015(5) 0.017(6) 0.008(4) -0.002(4) -0.001(4) N61 0.026(5) 0.027(5) 0.006(4) 0.003(4) 0.002(4) -0.004(4) C62 0.040(7) 0.043(7) 0.037(8) 0.023(6) 0.010(6) 0.005(6) C63 0.058(9) 0.039(7) 0.024(7) 0.017(6) 0.019(6) 0.009(6) C64 0.037(7) 0.017(5) 0.017(6) -0.002(4) -0.005(5) -0.003(4) C65 0.035(7) 0.056(8) 0.019(7) 0.020(6) 0.002(5) -0.004(6) C66 0.034(7) 0.049(7) 0.027(7) 0.016(6) 0.004(5) 0.005(5) O1W 0.057(9) 0.056(8) 0.032(7) 0.000 0.000 -0.015(6) O2W 0.076(9) 0.082(8) 0.098(11) 0.018(8) 0.024(8) 0.013(7) O3W 0.053(7) 0.227(18) 0.061(9) 0.052(10) 0.004(7) -0.015(9) O4W 0.066(9) 0.169(15) 0.152(15) 0.079(13) 0.020(10) 0.032(9) _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 O3 1.936(7) . ? Cu1 O2 1.973(8) . ? Cu1 N21 2.037(9) . ? Cu1 N11 2.051(9) . ? Cu1 Cl3 2.775(3) . ? Cu1 Cl2 2.872(3) . ? Cu2 O2 1.925(8) . ? Cu2 N3P 2.018(9) 4_655 ? Cu2 N41 2.040(9) . ? Cu2 N31 2.044(8) . ? Cu2 Cl3 2.604(3) . ? Cu3 O3 1.913(7) . ? Cu3 N1P 1.973(9) . ? Cu3 N51 2.049(8) . ? Cu3 N61 2.059(9) . ? Cu3 Cl2 2.654(3) . ? N1P C6P 1.302(14) . ? N1P C2P 1.381(14) . ? C2P O2P 1.235(11) . ? C2P N3P 1.412(14) . ? N3P C4P 1.301(14) . ? N3P Cu2 2.018(9) 4_644 ? C4P C5P 1.374(16) . ? C5P C6P 1.403(16) . ? N11 C16 1.328(13) . ? N11 C12 1.333(13) . ? C12 C13 1.363(14) . ? C13 C14 1.359(15) . ? C14 C15 1.409(14) . ? C14 C54 1.505(14) 4_654 ? C15 C16 1.394(14) . ? N21 C22 1.332(14) . ? N21 C26 1.375(14) . ? C22 C23 1.374(13) . ? C23 C24 1.392(15) . ? C24 C25 1.390(16) . ? C24 C34 1.477(13) 4_645 ? C25 C26 1.384(16) . ? N31 C32 1.305(15) . ? N31 C36 1.331(13) . ? C32 C33 1.380(15) . ? C33 C34 1.373(15) . ? C34 C35 1.405(15) . ? C34 C24 1.477(13) 4_654 ? C35 C36 1.361(15) . ? N41 C42 1.292(14) . ? N41 C46 1.361(15) . ? C42 C43 1.394(15) . ? C43 C44 1.378(16) . ? C44 C45 1.397(16) . ? C44 C64 1.477(12) 1_556 ? C45 C46 1.360(15) . ? N51 C52 1.332(13) . ? N51 C56 1.351(13) . ? C52 C53 1.381(14) . ? C53 C54 1.406(14) . ? C54 C55 1.361(15) . ? C54 C14 1.505(14) 4_645 ? C55 C56 1.403(14) . ? N61 C62 1.303(15) . ? N61 C66 1.324(14) . ? C62 C63 1.354(16) . ? C63 C64 1.383(17) . ? C64 C65 1.402(17) . ? C64 C44 1.477(12) 1_554 ? C65 C66 1.354(15) . ? N1N O1N 1.214(9) . ? N1N O3N 1.221(9) . ? N1N O2N 1.222(9) . ? N1N O8W 1.80(3) . ? O2N O8W 0.94(4) . ? N2N O4N 1.219(9) . ? N2N O6N 1.223(9) . ? N2N O5N 1.230(9) . ? O9W O9W 1.0(2) 2_665 ? 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 O3 Cu1 O2 178.9(3) . . ? O3 Cu1 N21 89.9(3) . . ? O2 Cu1 N21 90.0(3) . . ? O3 Cu1 N11 89.3(3) . . ? O2 Cu1 N11 90.8(3) . . ? N21 Cu1 N11 178.8(4) . . ? O3 Cu1 Cl3 96.2(2) . . ? O2 Cu1 Cl3 84.9(2) . . ? N21 Cu1 Cl3 89.6(3) . . ? N11 Cu1 Cl3 91.4(3) . . ? O3 Cu1 Cl2 82.1(2) . . ? O2 Cu1 Cl2 96.8(2) . . ? N21 Cu1 Cl2 87.0(3) . . ? N11 Cu1 Cl2 92.0(3) . . ? Cl3 Cu1 Cl2 176.20(9) . . ? O2 Cu2 N3P 175.6(3) . 4_655 ? O2 Cu2 N41 91.2(3) . . ? N3P Cu2 N41 89.3(3) 4_655 . ? O2 Cu2 N31 91.0(3) . . ? N3P Cu2 N31 87.2(3) 4_655 . ? N41 Cu2 N31 162.0(3) . . ? O2 Cu2 Cl3 90.7(2) . . ? N3P Cu2 Cl3 93.4(3) 4_655 . ? N41 Cu2 Cl3 98.5(3) . . ? N31 Cu2 Cl3 99.3(3) . . ? O3 Cu3 N1P 177.5(4) . . ? O3 Cu3 N51 91.3(3) . . ? N1P Cu3 N51 88.2(3) . . ? O3 Cu3 N61 91.3(3) . . ? N1P Cu3 N61 88.5(3) . . ? N51 Cu3 N61 162.7(3) . . ? O3 Cu3 Cl2 88.6(2) . . ? N1P Cu3 Cl2 93.9(3) . . ? N51 Cu3 Cl2 98.7(3) . . ? N61 Cu3 Cl2 98.4(3) . . ? Cu3 Cl2 Cu1 72.61(9) . . ? Cu2 Cl3 Cu1 73.29(8) . . ? Cu2 O2 Cu1 111.0(4) . . ? Cu3 O3 Cu1 116.7(4) . . ? C6P N1P C2P 120.3(9) . . ? C6P N1P Cu3 131.5(7) . . ? C2P N1P Cu3 108.2(7) . . ? O2P C2P N1P 121.8(10) . . ? O2P C2P N3P 119.6(11) . . ? N1P C2P N3P 118.6(9) . . ? C4P N3P C2P 120.1(10) . . ? C4P N3P Cu2 131.3(8) . 4_644 ? C2P N3P Cu2 108.5(7) . 4_644 ? N3P C4P C5P 121.6(11) . . ? C4P C5P C6P 117.9(11) . . ? N1P C6P C5P 121.5(10) . . ? C16 N11 C12 119.1(9) . . ? C16 N11 Cu1 118.9(7) . . ? C12 N11 Cu1 121.9(7) . . ? N11 C12 C13 122.5(10) . . ? C14 C13 C12 120.1(10) . . ? C13 C14 C15 118.4(10) . . ? C13 C14 C54 121.6(10) . 4_654 ? C15 C14 C54 120.0(10) . 4_654 ? C16 C15 C14 118.0(10) . . ? N11 C16 C15 121.9(10) . . ? C22 N21 C26 117.4(9) . . ? C22 N21 Cu1 123.5(7) . . ? C26 N21 Cu1 119.1(8) . . ? N21 C22 C23 124.1(10) . . ? C22 C23 C24 119.3(11) . . ? C25 C24 C23 117.1(10) . . ? C25 C24 C34 121.4(10) . 4_645 ? C23 C24 C34 121.2(10) . 4_645 ? C26 C25 C24 121.0(10) . . ? N21 C26 C25 120.9(11) . . ? C32 N31 C36 117.7(9) . . ? C32 N31 Cu2 120.7(7) . . ? C36 N31 Cu2 121.3(7) . . ? N31 C32 C33 123.8(11) . . ? C34 C33 C32 119.4(11) . . ? C33 C34 C35 116.3(9) . . ? C33 C34 C24 121.4(10) . 4_654 ? C35 C34 C24 122.0(10) . 4_654 ? C36 C35 C34 119.9(10) . . ? N31 C36 C35 122.7(10) . . ? C42 N41 C46 115.8(10) . . ? C42 N41 Cu2 123.2(8) . . ? C46 N41 Cu2 121.0(8) . . ? N41 C42 C43 125.2(11) . . ? C44 C43 C42 118.5(11) . . ? C43 C44 C45 117.3(10) . . ? C43 C44 C64 122.2(10) . 1_556 ? C45 C44 C64 120.5(10) . 1_556 ? C46 C45 C44 119.0(12) . . ? C45 C46 N41 124.1(13) . . ? C52 N51 C56 118.3(9) . . ? C52 N51 Cu3 120.4(7) . . ? C56 N51 Cu3 121.2(7) . . ? N51 C52 C53 124.0(10) . . ? C52 C53 C54 118.0(10) . . ? C55 C54 C53 118.3(9) . . ? C55 C54 C14 122.0(9) . 4_645 ? C53 C54 C14 119.8(9) . 4_645 ? C54 C55 C56 120.7(10) . . ? N51 C56 C55 120.7(10) . . ? C62 N61 C66 116.4(10) . . ? C62 N61 Cu3 120.6(8) . . ? C66 N61 Cu3 123.0(8) . . ? N61 C62 C63 124.7(12) . . ? C62 C63 C64 120.6(12) . . ? C63 C64 C65 114.1(11) . . ? C63 C64 C44 123.5(10) . 1_554 ? C65 C64 C44 122.4(10) . 1_554 ? C66 C65 C64 120.9(12) . . ? N61 C66 C65 123.3(12) . . ? O1N N1N O3N 120.3(11) . . ? O1N N1N O2N 120.0(11) . . ? O3N N1N O2N 118.7(11) . . ? O1N N1N O8W 148(2) . . ? O3N N1N O8W 89.9(15) . . ? O2N N1N O8W 28.8(15) . . ? O8W O2N N1N 112(2) . . ? O4N N2N O6N 119.4(13) . . ? O4N N2N O5N 120.1(13) . . ? O6N N2N O5N 118.9(13) . . ? O2N O8W N1N 38.8(13) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.381 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.177