# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co4(N3)4(PTA)3(4-CV)2]n.2nH2O' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Co4(N3)4(PTA)3(4-CV)2]n.2nH2O' _chemical_formula_sum 'C60 H44 Co4 N18 O14' _chemical_formula_weight 1476.85 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.2796(5) _cell_length_b 16.9872(8) _cell_length_c 33.1264(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.110(4) _cell_angle_gamma 90.00 _cell_volume 6343.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6651 _cell_measurement_theta_min 2.1679 _cell_measurement_theta_max 27.4971 _exptl_crystal_description Prism _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.110 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 'Rigaku Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21902 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5884 _reflns_number_gt 5290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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^)+(0.1005P)^2^+6.8685P] 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 5884 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.65653(4) 0.70294(2) 0.027159(13) 0.03046(17) Uani 1 1 d . . . Co2 Co 0.45939(4) 0.61260(3) 0.086855(13) 0.02984(16) Uani 1 1 d . . . O1 O 0.4301(2) 0.66602(15) 0.14497(7) 0.0449(6) Uani 1 1 d . . . O2 O 0.5031(2) 0.54642(16) 0.14326(7) 0.0457(7) Uani 1 1 d . . . O3 O 0.3793(2) 0.70281(14) 0.05654(8) 0.0393(6) Uani 1 1 d . . . O4 O 0.5162(2) 0.76962(16) 0.02363(9) 0.0547(8) Uani 1 1 d . . . O5 O 0.0215(2) 1.03224(13) 0.04864(7) 0.0368(5) Uani 1 1 d . . . O6 O 0.1506(2) 1.09333(13) 0.00904(8) 0.0414(6) Uani 1 1 d . . . N1 N -0.3196(9) 0.0428(8) 0.2879(3) 0.228(6) Uani 1 1 d . . . N2 N -0.2510(3) 0.3884(2) 0.14449(10) 0.0451(8) Uani 1 1 d . . . N3 N 0.2910(3) 0.55299(17) 0.08702(9) 0.0373(7) Uani 1 1 d . . . N4 N 0.6347(3) 0.66739(19) 0.08783(9) 0.0424(7) Uani 1 1 d . . . N5 N 0.6725(3) 0.7037(2) 0.11575(10) 0.0499(8) Uani 1 1 d . . . N6 N 0.7034(5) 0.7432(3) 0.14307(14) 0.0908(16) Uani 1 1 d . . . N7 N 0.8117(3) 0.76082(18) 0.03549(9) 0.0404(7) Uani 1 1 d . . . N8 N 0.8873(3) 0.7539(2) 0.06122(10) 0.0459(8) Uani 1 1 d . . . N9 N 0.9627(4) 0.7485(3) 0.08537(14) 0.0869(16) Uani 1 1 d . . . C1 C -0.3252(8) 0.0987(8) 0.2682(3) 0.166(5) Uani 1 1 d . . . C2 C -0.3363(6) 0.1698(7) 0.2427(2) 0.118(3) Uani 1 1 d . . . C3 C -0.3764(7) 0.1562(5) 0.2044(2) 0.108(2) Uani 1 1 d . . . H3A H -0.3968 0.1055 0.1961 0.130 Uiso 1 1 calc R . . C4 C -0.3070(7) 0.2446(8) 0.2551(2) 0.132(4) Uani 1 1 d . . . H4A H -0.2809 0.2536 0.2816 0.158 Uiso 1 1 calc R . . C5 C -0.3161(6) 0.3061(5) 0.22847(19) 0.100(2) Uani 1 1 d . . . H5A H -0.2952 0.3566 0.2370 0.120 Uiso 1 1 calc R . . C6 C -0.3867(5) 0.2195(4) 0.17732(17) 0.0806(16) Uani 1 1 d . . . H6A H -0.4150 0.2104 0.1510 0.097 Uiso 1 1 calc R . . C7 C -0.3562(4) 0.2940(3) 0.18878(14) 0.0580(11) Uani 1 1 d . . . C8 C -0.3670(4) 0.3584(3) 0.15847(16) 0.0616(12) Uani 1 1 d . . . H8A H -0.4101 0.4017 0.1701 0.074 Uiso 1 1 calc R . . H8B H -0.4134 0.3394 0.1352 0.074 Uiso 1 1 calc R . . C9 C -0.1533(4) 0.3421(2) 0.14416(13) 0.0496(10) Uani 1 1 d . . . H9A H -0.1572 0.2905 0.1534 0.060 Uiso 1 1 calc R . . C10 C -0.2474(3) 0.4621(2) 0.13031(13) 0.0489(10) Uani 1 1 d . . . H10A H -0.3154 0.4931 0.1303 0.059 Uiso 1 1 calc R . . C11 C -0.0488(4) 0.3709(2) 0.13028(13) 0.0468(9) Uani 1 1 d . . . H11A H 0.0178 0.3386 0.1303 0.056 Uiso 1 1 calc R . . C12 C -0.1453(4) 0.4922(2) 0.11582(14) 0.0507(10) Uani 1 1 d . . . H12A H -0.1451 0.5432 0.1056 0.061 Uiso 1 1 calc R . . C13 C -0.0410(3) 0.4478(2) 0.11615(11) 0.0397(8) Uani 1 1 d . . . C14 C 0.0723(3) 0.4830(2) 0.10360(11) 0.0399(8) Uani 1 1 d . . . C15 C 0.0857(4) 0.5632(2) 0.09999(16) 0.0597(12) Uani 1 1 d . . . H15A H 0.0209 0.5961 0.1032 0.072 Uiso 1 1 calc R . . C16 C 0.1719(4) 0.4386(3) 0.09570(19) 0.0712(15) Uani 1 1 d . . . H16A H 0.1678 0.3840 0.0958 0.085 Uiso 1 1 calc R . . C17 C 0.2781(4) 0.4761(3) 0.08757(17) 0.0654(13) Uani 1 1 d . . . H17A H 0.3435 0.4450 0.0822 0.078 Uiso 1 1 calc R . . C18 C 0.1935(4) 0.5948(2) 0.09179(16) 0.0571(12) Uani 1 1 d . . . H18A H 0.1987 0.6492 0.0894 0.068 Uiso 1 1 calc R . . C19 C 0.4717(3) 0.6060(2) 0.16284(11) 0.0387(8) Uani 1 1 d . . . C20 C 0.4848(3) 0.6062(2) 0.20820(11) 0.0399(8) Uani 1 1 d . . . C21 C 0.4916(4) 0.6759(2) 0.22946(12) 0.0522(10) Uani 1 1 d . . . H21A H 0.4846 0.7235 0.2157 0.063 Uiso 1 1 calc R . . C22 C 0.4936(5) 0.5363(2) 0.22907(12) 0.0558(11) Uani 1 1 d . . . H22A H 0.4911 0.4888 0.2151 0.067 Uiso 1 1 calc R . . C23 C 0.4145(3) 0.7615(2) 0.03790(11) 0.0349(8) Uani 1 1 d . . . C24 C 0.3318(3) 0.82977(19) 0.03158(10) 0.0310(7) Uani 1 1 d . . . C25 C 0.3734(3) 0.8991(2) 0.01494(11) 0.0365(8) Uani 1 1 d . . . H25A H 0.4505 0.9017 0.0060 0.044 Uiso 1 1 calc R . . C26 C 0.2154(3) 0.82530(19) 0.04378(11) 0.0345(7) Uani 1 1 d . . . H26A H 0.1865 0.7783 0.0539 0.041 Uiso 1 1 calc R . . C27 C 0.1427(3) 0.89049(19) 0.04086(11) 0.0344(8) Uani 1 1 d . . . H27A H 0.0649 0.8873 0.0492 0.041 Uiso 1 1 calc R . . C28 C 0.3004(3) 0.9642(2) 0.01175(11) 0.0370(8) Uani 1 1 d . . . H28A H 0.3280 1.0104 0.0004 0.044 Uiso 1 1 calc R . . C29 C 0.1850(3) 0.96083(19) 0.02555(10) 0.0310(7) Uani 1 1 d . . . C30 C 0.1124(3) 1.03435(19) 0.02782(10) 0.0319(7) Uani 1 1 d . . . O1W O -0.658(3) 0.3772(17) 0.1771(9) 0.646(19) 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 Co1 0.0241(3) 0.0287(3) 0.0388(3) 0.00465(18) 0.0041(2) 0.00494(17) Co2 0.0316(3) 0.0301(3) 0.0281(3) 0.00366(17) 0.00466(19) 0.00906(18) O1 0.0517(16) 0.0481(15) 0.0351(14) 0.0042(11) 0.0051(12) 0.0108(12) O2 0.0522(16) 0.0537(16) 0.0313(13) -0.0011(11) 0.0042(12) 0.0190(13) O3 0.0360(13) 0.0338(13) 0.0479(15) 0.0115(11) 0.0009(11) 0.0089(10) O4 0.0415(15) 0.0491(16) 0.075(2) 0.0235(14) 0.0214(14) 0.0218(13) O5 0.0330(13) 0.0327(12) 0.0452(14) -0.0056(10) 0.0078(11) 0.0082(10) O6 0.0529(16) 0.0281(12) 0.0441(15) 0.0049(10) 0.0119(12) 0.0088(11) N1 0.173(9) 0.324(14) 0.186(9) 0.178(10) -0.004(7) -0.001(9) N2 0.0328(16) 0.057(2) 0.0461(19) -0.0064(15) 0.0037(14) 0.0002(14) N3 0.0359(16) 0.0356(15) 0.0409(17) 0.0026(12) 0.0076(13) 0.0047(12) N4 0.0403(17) 0.0534(19) 0.0335(17) 0.0025(14) 0.0027(14) -0.0064(14) N5 0.0435(19) 0.065(2) 0.041(2) 0.0016(17) 0.0025(16) -0.0057(16) N6 0.086(3) 0.120(4) 0.066(3) -0.028(3) -0.003(2) -0.023(3) N7 0.0342(16) 0.0462(18) 0.0405(17) 0.0131(13) 0.0000(14) -0.0013(13) N8 0.0343(17) 0.056(2) 0.0469(19) 0.0134(15) -0.0009(16) -0.0086(14) N9 0.056(3) 0.127(4) 0.076(3) 0.035(3) -0.025(2) -0.021(3) C1 0.090(5) 0.277(13) 0.133(7) 0.133(9) 0.018(5) 0.011(7) C2 0.062(4) 0.214(10) 0.077(5) 0.075(6) 0.004(3) 0.004(5) C3 0.105(5) 0.113(6) 0.106(5) 0.044(4) -0.012(4) -0.021(4) C4 0.092(6) 0.250(13) 0.053(4) 0.016(6) -0.007(4) -0.006(7) C5 0.083(4) 0.152(7) 0.065(4) -0.015(4) -0.003(3) -0.017(4) C6 0.091(4) 0.090(4) 0.060(3) 0.017(3) -0.008(3) -0.015(3) C7 0.035(2) 0.086(3) 0.053(3) 0.000(2) 0.0097(19) -0.005(2) C8 0.036(2) 0.070(3) 0.079(3) 0.001(2) 0.010(2) -0.002(2) C9 0.041(2) 0.046(2) 0.062(3) 0.0014(19) 0.0081(19) 0.0007(17) C10 0.036(2) 0.052(2) 0.059(3) -0.0036(19) 0.0015(18) 0.0062(17) C11 0.037(2) 0.050(2) 0.054(2) 0.0035(18) 0.0078(18) 0.0086(17) C12 0.039(2) 0.046(2) 0.067(3) 0.0000(19) 0.0028(19) 0.0057(17) C13 0.0352(19) 0.042(2) 0.042(2) -0.0051(15) 0.0044(16) 0.0042(15) C14 0.0363(19) 0.042(2) 0.042(2) -0.0024(15) 0.0018(16) 0.0047(15) C15 0.039(2) 0.043(2) 0.099(4) 0.008(2) 0.011(2) 0.0098(17) C16 0.051(3) 0.037(2) 0.128(5) -0.002(2) 0.033(3) 0.0034(19) C17 0.047(2) 0.043(2) 0.108(4) 0.003(2) 0.026(2) 0.0115(19) C18 0.041(2) 0.041(2) 0.090(3) 0.014(2) 0.012(2) 0.0049(17) C19 0.0337(18) 0.053(2) 0.0291(18) 0.0016(16) 0.0058(15) 0.0040(16) C20 0.041(2) 0.050(2) 0.0297(19) 0.0025(15) 0.0058(15) 0.0023(16) C21 0.076(3) 0.046(2) 0.036(2) 0.0046(17) 0.002(2) 0.002(2) C22 0.091(4) 0.044(2) 0.033(2) -0.0059(17) 0.008(2) 0.001(2) C23 0.0330(18) 0.0362(18) 0.0354(18) 0.0028(14) 0.0016(14) 0.0110(14) C24 0.0306(17) 0.0327(16) 0.0301(17) 0.0003(13) 0.0048(13) 0.0079(13) C25 0.0304(17) 0.0364(18) 0.043(2) 0.0064(15) 0.0097(15) 0.0083(14) C26 0.0324(17) 0.0263(16) 0.045(2) 0.0061(14) 0.0035(15) 0.0043(13) C27 0.0273(17) 0.0328(17) 0.043(2) 0.0025(14) 0.0050(15) 0.0060(13) C28 0.0354(18) 0.0326(17) 0.044(2) 0.0103(14) 0.0088(15) 0.0083(14) C29 0.0327(17) 0.0321(17) 0.0283(17) 0.0010(13) 0.0005(13) 0.0082(13) C30 0.0352(18) 0.0298(16) 0.0304(17) -0.0009(13) -0.0007(14) 0.0088(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 Co1 O4 1.946(2) . ? Co1 O6 1.957(2) 3_545 ? Co1 N7 2.018(3) . ? Co1 N4 2.121(3) . ? Co1 N7 2.207(3) 7_665 ? Co2 O5 2.005(2) 3_545 ? Co2 O3 2.026(2) . ? Co2 N3 2.152(3) . ? Co2 O1 2.165(3) . ? Co2 N4 2.185(3) . ? Co2 O2 2.220(3) . ? Co2 C19 2.518(4) . ? O1 C19 1.261(4) . ? O2 C19 1.260(4) . ? O3 C23 1.245(4) . ? O4 C23 1.264(4) . ? O5 C30 1.257(4) . ? O5 Co2 2.005(2) 3_455 ? O6 C30 1.263(4) . ? O6 Co1 1.957(2) 3_455 ? N1 C1 1.153(11) . ? N2 C10 1.338(5) . ? N2 C9 1.354(5) . ? N2 C8 1.494(5) . ? N3 C17 1.315(5) . ? N3 C18 1.324(5) . ? N4 N5 1.178(5) . ? N5 N6 1.170(5) . ? N7 N8 1.189(4) . ? N7 Co1 2.207(3) 7_665 ? N8 N9 1.149(5) . ? C1 C2 1.477(12) . ? C2 C3 1.353(11) . ? C2 C4 1.372(12) . ? C3 C6 1.401(8) . ? C4 C5 1.368(11) . ? C5 C7 1.390(8) . ? C6 C7 1.361(7) . ? C7 C8 1.487(7) . ? C9 C11 1.372(6) . ? C10 C12 1.364(6) . ? C11 C13 1.391(5) . ? C12 C13 1.398(5) . ? C13 C14 1.485(5) . ? C14 C15 1.376(5) . ? C14 C16 1.386(6) . ? C15 C18 1.365(6) . ? C16 C17 1.391(6) . ? C19 C20 1.504(5) . ? C20 C22 1.376(5) . ? C20 C21 1.378(5) . ? C21 C21 1.367(8) 2_655 ? C22 C22 1.389(8) 2_655 ? C23 C24 1.498(4) . ? C24 C25 1.390(5) . ? C24 C26 1.390(5) . ? C25 C28 1.380(5) . ? C26 C27 1.380(4) . ? C27 C29 1.390(5) . ? C28 C29 1.396(5) . ? C29 C30 1.497(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 O4 Co1 O6 121.12(13) . 3_545 ? O4 Co1 N7 115.09(13) . . ? O6 Co1 N7 121.70(12) 3_545 . ? O4 Co1 N4 95.76(12) . . ? O6 Co1 N4 90.90(12) 3_545 . ? N7 Co1 N4 98.01(12) . . ? O4 Co1 N7 86.61(12) . 7_665 ? O6 Co1 N7 88.96(11) 3_545 7_665 ? N7 Co1 N7 79.79(13) . 7_665 ? N4 Co1 N7 177.31(11) . 7_665 ? O5 Co2 O3 111.21(10) 3_545 . ? O5 Co2 N3 90.58(10) 3_545 . ? O3 Co2 N3 88.85(11) . . ? O5 Co2 O1 156.21(10) 3_545 . ? O3 Co2 O1 92.51(10) . . ? N3 Co2 O1 91.79(11) . . ? O5 Co2 N4 87.83(11) 3_545 . ? O3 Co2 N4 94.12(11) . . ? N3 Co2 N4 176.99(12) . . ? O1 Co2 N4 88.63(11) . . ? O5 Co2 O2 96.58(10) 3_545 . ? O3 Co2 O2 151.77(10) . . ? N3 Co2 O2 85.89(11) . . ? O1 Co2 O2 60.02(9) . . ? N4 Co2 O2 91.74(11) . . ? O5 Co2 C19 126.36(11) 3_545 . ? O3 Co2 C19 122.42(11) . . ? N3 Co2 C19 89.59(12) . . ? O1 Co2 C19 30.04(10) . . ? N4 Co2 C19 89.29(12) . . ? O2 Co2 C19 30.01(11) . . ? C19 O1 Co2 90.7(2) . . ? C19 O2 Co2 88.2(2) . . ? C23 O3 Co2 135.0(2) . . ? C23 O4 Co1 131.4(2) . . ? C30 O5 Co2 129.6(2) . 3_455 ? C30 O6 Co1 127.7(2) . 3_455 ? C10 N2 C9 120.4(4) . . ? C10 N2 C8 117.8(3) . . ? C9 N2 C8 121.7(4) . . ? C17 N3 C18 116.0(4) . . ? C17 N3 Co2 124.5(3) . . ? C18 N3 Co2 119.0(3) . . ? N5 N4 Co1 122.9(3) . . ? N5 N4 Co2 122.4(3) . . ? Co1 N4 Co2 104.11(13) . . ? N6 N5 N4 175.3(5) . . ? N8 N7 Co1 130.2(3) . . ? N8 N7 Co1 124.4(3) . 7_665 ? Co1 N7 Co1 100.21(13) . 7_665 ? N9 N8 N7 177.9(4) . . ? N1 C1 C2 178.2(11) . . ? C3 C2 C4 120.4(7) . . ? C3 C2 C1 114.6(11) . . ? C4 C2 C1 125.0(9) . . ? C2 C3 C6 119.1(8) . . ? C5 C4 C2 120.3(7) . . ? C4 C5 C7 120.7(7) . . ? C7 C6 C3 121.4(6) . . ? C6 C7 C5 118.2(6) . . ? C6 C7 C8 118.8(4) . . ? C5 C7 C8 123.0(5) . . ? C7 C8 N2 114.2(4) . . ? N2 C9 C11 120.4(4) . . ? N2 C10 C12 120.8(4) . . ? C9 C11 C13 120.9(4) . . ? C10 C12 C13 121.1(4) . . ? C11 C13 C12 116.5(4) . . ? C11 C13 C14 122.6(3) . . ? C12 C13 C14 120.8(3) . . ? C15 C14 C16 115.4(4) . . ? C15 C14 C13 121.5(3) . . ? C16 C14 C13 123.1(3) . . ? C18 C15 C14 120.5(4) . . ? C14 C16 C17 119.9(4) . . ? N3 C17 C16 123.6(4) . . ? N3 C18 C15 124.3(4) . . ? O2 C19 O1 121.0(3) . . ? O2 C19 C20 119.8(3) . . ? O1 C19 C20 119.2(3) . . ? O2 C19 Co2 61.79(18) . . ? O1 C19 Co2 59.26(18) . . ? C20 C19 Co2 176.4(3) . . ? C22 C20 C21 118.9(4) . . ? C22 C20 C19 120.2(3) . . ? C21 C20 C19 120.9(3) . . ? C21 C21 C20 120.8(2) 2_655 . ? C20 C22 C22 120.3(2) . 2_655 ? O3 C23 O4 125.7(3) . . ? O3 C23 C24 118.7(3) . . ? O4 C23 C24 115.6(3) . . ? C25 C24 C26 119.8(3) . . ? C25 C24 C23 119.6(3) . . ? C26 C24 C23 120.5(3) . . ? C28 C25 C24 120.0(3) . . ? C27 C26 C24 120.1(3) . . ? C26 C27 C29 120.3(3) . . ? C25 C28 C29 120.2(3) . . ? C27 C29 C28 119.5(3) . . ? C27 C29 C30 120.2(3) . . ? C28 C29 C30 120.0(3) . . ? O5 C30 O6 126.3(3) . . ? O5 C30 C29 117.5(3) . . ? O6 C30 C29 116.1(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.575 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.069 _database_code_depnum_ccdc_archive 'CCDC 967138' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co4(N3)4(PTA)3(3-CV)2]n.nH2O ' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Co4(N3)4(PTA)3(3-CV)2]n.nH2O ' _chemical_formula_sum 'C60 H42 Co4 N18 O13' _chemical_formula_weight 1458.84 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.2319(9) _cell_length_b 17.0040(13) _cell_length_c 33.097(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.524(6) _cell_angle_gamma 90.00 _cell_volume 6291.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6403 _cell_measurement_theta_min 2.1849 _cell_measurement_theta_max 27.5010 _exptl_crystal_description Prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.231 _exptl_crystal_size_min 0.195 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 'Rigaku Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17290 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5781 _reflns_number_gt 4882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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^)+(0.0401P)^2^+13.2178P] 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 5781 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Co1 Co 0.16011(4) 0.20226(3) 0.026136(14) 0.01975(15) Uani 1 1 d . . . Co2 Co -0.02878(4) 0.11357(3) 0.085987(14) 0.02016(15) Uani 1 1 d . . . O1 O -0.0552(2) 0.17075(16) 0.14295(7) 0.0265(6) Uani 1 1 d . . . O2 O 0.0217(2) 0.05165(16) 0.14374(7) 0.0251(6) Uani 1 1 d . . . O3 O 0.1472(2) 0.09312(15) 0.00745(7) 0.0239(6) Uani 1 1 d . . . O4 O 0.0265(2) 0.03147(15) 0.04812(7) 0.0232(6) Uani 1 1 d . . . O5 O 0.5206(2) -0.22848(16) 0.02305(8) 0.0317(7) Uani 1 1 d . . . O6 O 0.3862(2) -0.29747(16) 0.05452(7) 0.0253(6) Uani 1 1 d . . . N1 N -0.8624(7) -0.4686(4) 0.2186(2) 0.127(3) Uani 1 1 d . . . N2 N -0.7378(3) -0.1067(2) 0.14264(9) 0.0253(7) Uani 1 1 d . . . N3 N -0.1967(3) 0.05572(19) 0.08757(9) 0.0225(7) Uani 1 1 d . . . N4 N 0.1480(3) 0.1652(2) 0.08685(9) 0.0255(8) Uani 1 1 d . . . N5 N 0.1863(3) 0.2049(2) 0.11472(10) 0.0329(9) Uani 1 1 d . . . N6 N 0.2213(4) 0.2470(3) 0.14144(12) 0.0548(12) Uani 1 1 d . . . N7 N 0.3166(3) 0.26040(19) 0.03612(9) 0.0233(7) Uani 1 1 d . . . N8 N 0.3980(3) 0.25078(19) 0.06236(10) 0.0258(8) Uani 1 1 d . . . N9 N 0.4772(3) 0.2430(2) 0.08688(11) 0.0382(9) Uani 1 1 d . . . C1 C -0.8549(7) -0.4011(4) 0.2210(2) 0.083(2) Uani 1 1 d . . . C2 C -0.8422(5) -0.3161(4) 0.22411(16) 0.0580(15) Uani 1 1 d . . . C3 C -0.8558(4) -0.2686(3) 0.18940(14) 0.0452(13) Uani 1 1 d . . . H3A H -0.8754 -0.2919 0.1642 0.054 Uiso 1 1 calc R . . C4 C -0.8162(5) -0.2811(4) 0.26146(16) 0.0618(16) Uani 1 1 d . . . H4A H -0.8083 -0.3120 0.2848 0.074 Uiso 1 1 calc R . . C5 C -0.8019(5) -0.2010(4) 0.26459(15) 0.0619(16) Uani 1 1 d . . . H5A H -0.7843 -0.1781 0.2900 0.074 Uiso 1 1 calc R . . C6 C -0.8135(4) -0.1535(3) 0.22964(14) 0.0501(13) Uani 1 1 d . . . H6A H -0.8031 -0.0993 0.2317 0.060 Uiso 1 1 calc R . . C7 C -0.8411(4) -0.1888(3) 0.19155(12) 0.0343(10) Uani 1 1 d . . . C8 C -0.8547(4) -0.1390(3) 0.15336(12) 0.0304(10) Uani 1 1 d . . . H8A H -0.8901 -0.1706 0.1310 0.036 Uiso 1 1 calc R . . H8B H -0.9087 -0.0957 0.1572 0.036 Uiso 1 1 calc R . . C9 C -0.7347(4) -0.0324(3) 0.12893(12) 0.0319(10) Uani 1 1 d . . . H9A H -0.8033 -0.0015 0.1278 0.038 Uiso 1 1 calc R . . C10 C -0.6402(4) -0.1531(3) 0.14331(12) 0.0303(10) Uani 1 1 d . . . H10A H -0.6447 -0.2050 0.1518 0.036 Uiso 1 1 calc R . . C11 C -0.5341(4) -0.1245(2) 0.13165(11) 0.0282(9) Uani 1 1 d . . . H11A H -0.4671 -0.1568 0.1329 0.034 Uiso 1 1 calc R . . C12 C -0.6308(3) -0.0019(3) 0.11664(13) 0.0313(10) Uani 1 1 d . . . H12A H -0.6297 0.0497 0.1073 0.038 Uiso 1 1 calc R . . C13 C -0.5268(3) -0.0470(2) 0.11790(11) 0.0248(9) Uani 1 1 d . . . C14 C -0.4139(3) -0.0129(2) 0.10593(11) 0.0245(9) Uani 1 1 d . . . C15 C -0.3986(4) 0.0680(3) 0.10474(12) 0.0311(10) Uani 1 1 d . . . H15A H -0.4609 0.1012 0.1101 0.037 Uiso 1 1 calc R . . C16 C -0.3176(4) -0.0586(3) 0.09581(13) 0.0322(10) Uani 1 1 d . . . H16A H -0.3238 -0.1131 0.0949 0.039 Uiso 1 1 calc R . . C17 C -0.2131(4) -0.0223(3) 0.08718(12) 0.0326(10) Uani 1 1 d . . . H17A H -0.1502 -0.0539 0.0807 0.039 Uiso 1 1 calc R . . C18 C -0.2914(3) 0.0991(2) 0.09566(12) 0.0287(9) Uani 1 1 d . . . H18A H -0.2840 0.1536 0.0951 0.034 Uiso 1 1 calc R . . C19 C -0.0138(3) 0.1115(2) 0.16221(11) 0.0234(9) Uani 1 1 d . . . C20 C -0.0065(3) 0.1119(2) 0.20778(11) 0.0238(9) Uani 1 1 d . . . C21 C -0.0026(4) 0.0414(2) 0.22879(11) 0.0314(10) Uani 1 1 d . . . H21A H -0.0034 -0.0060 0.2147 0.038 Uiso 1 1 calc R . . C22 C -0.0046(4) 0.1827(2) 0.22894(11) 0.0286(9) Uani 1 1 d . . . H22A H -0.0095 0.2301 0.2148 0.034 Uiso 1 1 calc R . . C23 C 0.1139(3) 0.0337(2) 0.02680(10) 0.0218(8) Uani 1 1 d . . . C24 C 0.1867(3) -0.0388(2) 0.02484(10) 0.0209(8) Uani 1 1 d . . . C25 C 0.3000(3) -0.0348(2) 0.01102(11) 0.0235(9) Uani 1 1 d . . . H25A H 0.3257 0.0117 -0.0002 0.028 Uiso 1 1 calc R . . C26 C 0.1467(3) -0.1097(2) 0.04015(11) 0.0227(9) Uani 1 1 d . . . H26A H 0.0700 -0.1131 0.0484 0.027 Uiso 1 1 calc R . . C27 C 0.2206(3) -0.1745(2) 0.04298(11) 0.0236(9) Uani 1 1 d . . . H27A H 0.1937 -0.2217 0.0531 0.028 Uiso 1 1 calc R . . C28 C 0.3747(3) -0.1001(2) 0.01391(11) 0.0248(9) Uani 1 1 d . . . H28A H 0.4502 -0.0974 0.0047 0.030 Uiso 1 1 calc R . . C29 C 0.3359(3) -0.1695(2) 0.03070(10) 0.0214(8) Uani 1 1 d . . . C30 C 0.4200(3) -0.2376(2) 0.03665(11) 0.0222(9) Uani 1 1 d . . . O1W O 0.0000 0.3935(6) 0.2500 0.236(7) Uani 1 2 d S . . 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 Co1 0.0205(3) 0.0182(3) 0.0211(3) 0.0017(2) 0.0046(2) 0.0030(2) Co2 0.0248(3) 0.0194(3) 0.0169(3) 0.0024(2) 0.0056(2) 0.0059(2) O1 0.0353(16) 0.0264(17) 0.0183(13) 0.0034(12) 0.0060(11) 0.0082(13) O2 0.0308(15) 0.0264(16) 0.0186(13) -0.0011(11) 0.0058(11) 0.0066(12) O3 0.0321(15) 0.0206(16) 0.0200(13) 0.0025(11) 0.0075(11) 0.0049(12) O4 0.0239(14) 0.0213(15) 0.0253(14) -0.0021(11) 0.0073(11) 0.0032(11) O5 0.0301(16) 0.0265(17) 0.0404(16) 0.0118(13) 0.0136(13) 0.0123(13) O6 0.0272(15) 0.0228(16) 0.0257(14) 0.0057(12) 0.0013(11) 0.0069(12) N1 0.187(8) 0.079(5) 0.112(5) 0.014(4) 0.009(5) -0.051(5) N2 0.0243(18) 0.028(2) 0.0233(16) -0.0008(15) 0.0031(14) 0.0033(15) N3 0.0269(18) 0.022(2) 0.0192(15) 0.0041(13) 0.0056(13) 0.0040(14) N4 0.0280(19) 0.028(2) 0.0204(16) 0.0003(15) 0.0033(14) -0.0035(15) N5 0.032(2) 0.042(2) 0.0256(19) 0.0015(18) 0.0085(16) -0.0034(18) N6 0.059(3) 0.067(3) 0.039(2) -0.015(2) 0.003(2) -0.011(2) N7 0.0227(18) 0.025(2) 0.0213(16) 0.0070(14) -0.0011(14) -0.0020(14) N8 0.031(2) 0.021(2) 0.0267(18) 0.0025(14) 0.0091(17) -0.0024(15) N9 0.036(2) 0.040(3) 0.036(2) 0.0059(17) -0.0099(18) -0.0004(18) C1 0.108(6) 0.066(5) 0.077(5) 0.029(4) 0.013(4) -0.028(4) C2 0.058(3) 0.069(4) 0.049(3) 0.020(3) 0.010(3) -0.015(3) C3 0.045(3) 0.057(4) 0.034(2) 0.013(2) 0.007(2) -0.015(2) C4 0.056(4) 0.083(5) 0.047(3) 0.022(3) 0.008(3) -0.008(3) C5 0.067(4) 0.089(5) 0.029(3) -0.001(3) 0.003(2) 0.002(3) C6 0.051(3) 0.061(4) 0.038(3) -0.005(2) 0.004(2) 0.002(3) C7 0.027(2) 0.048(3) 0.028(2) 0.000(2) 0.0080(18) -0.004(2) C8 0.028(2) 0.038(3) 0.026(2) -0.0028(18) 0.0042(17) -0.0029(19) C9 0.032(2) 0.027(3) 0.036(2) 0.0010(19) 0.0006(19) 0.0089(19) C10 0.033(2) 0.029(3) 0.029(2) 0.0047(18) 0.0033(18) 0.0008(19) C11 0.028(2) 0.030(3) 0.028(2) 0.0015(18) 0.0082(17) 0.0047(18) C12 0.028(2) 0.024(2) 0.042(2) 0.0049(19) 0.0050(19) 0.0041(19) C13 0.027(2) 0.026(2) 0.0221(19) -0.0036(16) 0.0030(16) 0.0033(17) C14 0.024(2) 0.029(3) 0.0204(19) 0.0041(17) 0.0033(16) 0.0057(18) C15 0.026(2) 0.028(3) 0.040(2) 0.0074(19) 0.0114(19) 0.0115(19) C16 0.034(2) 0.022(2) 0.042(2) -0.0001(19) 0.014(2) 0.0018(19) C17 0.030(2) 0.032(3) 0.037(2) 0.002(2) 0.0098(19) 0.008(2) C18 0.028(2) 0.021(2) 0.039(2) 0.0036(18) 0.0077(18) 0.0040(18) C19 0.024(2) 0.027(2) 0.0196(19) 0.0042(17) 0.0058(16) 0.0011(18) C20 0.025(2) 0.027(2) 0.0198(18) 0.0022(17) 0.0040(16) 0.0031(17) C21 0.048(3) 0.023(2) 0.023(2) -0.0063(17) 0.0048(18) 0.001(2) C22 0.040(2) 0.024(2) 0.0219(19) 0.0031(17) 0.0036(17) 0.0015(19) C23 0.027(2) 0.021(2) 0.0172(18) -0.0010(16) -0.0006(16) 0.0038(17) C24 0.028(2) 0.021(2) 0.0136(17) 0.0007(15) 0.0026(15) 0.0052(17) C25 0.028(2) 0.021(2) 0.0227(19) 0.0033(16) 0.0045(16) 0.0010(17) C26 0.024(2) 0.026(2) 0.0186(18) -0.0003(16) 0.0040(15) 0.0037(17) C27 0.032(2) 0.018(2) 0.0209(18) 0.0020(16) 0.0058(16) 0.0013(17) C28 0.024(2) 0.027(2) 0.0241(19) 0.0017(17) 0.0072(16) 0.0036(17) C29 0.026(2) 0.020(2) 0.0186(18) 0.0005(15) 0.0036(15) 0.0075(17) C30 0.027(2) 0.022(2) 0.0180(18) -0.0039(16) 0.0040(16) 0.0036(17) O1W 0.232(13) 0.102(8) 0.40(2) 0.000 0.178(14) 0.000 _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 Co1 O5 1.955(3) 3_455 ? Co1 O3 1.957(3) . ? Co1 N7 2.016(3) . ? Co1 N4 2.123(3) . ? Co1 N7 2.196(3) 7 ? Co2 O4 2.014(2) . ? Co2 O6 2.023(3) 3_455 ? Co2 N3 2.132(3) . ? Co2 O1 2.167(2) . ? Co2 N4 2.169(3) . ? Co2 O2 2.208(3) . ? Co2 C19 2.512(4) . ? O1 C19 1.257(4) . ? O2 C19 1.271(5) . ? O3 C23 1.272(4) . ? O4 C23 1.264(4) . ? O5 C30 1.266(4) . ? O5 Co1 1.955(3) 3_545 ? O6 C30 1.254(4) . ? O6 Co2 2.023(3) 3_545 ? N1 C1 1.154(9) . ? N2 C9 1.343(5) . ? N2 C10 1.349(5) . ? N2 C8 1.497(5) . ? N3 C17 1.339(5) . ? N3 C18 1.343(5) . ? N4 N5 1.189(5) . ? N5 N6 1.176(5) . ? N7 N8 1.210(4) . ? N7 Co1 2.196(3) 7 ? N8 N9 1.153(4) . ? C1 C2 1.455(9) . ? C2 C4 1.378(8) . ? C2 C3 1.400(7) . ? C3 C7 1.368(6) . ? C4 C5 1.375(8) . ? C5 C6 1.406(7) . ? C6 C7 1.404(6) . ? C7 C8 1.517(6) . ? C9 C12 1.375(6) . ? C10 C11 1.376(5) . ? C11 C13 1.399(6) . ? C12 C13 1.395(5) . ? C13 C14 1.482(5) . ? C14 C15 1.388(6) . ? C14 C16 1.399(5) . ? C15 C18 1.375(5) . ? C16 C17 1.380(6) . ? C19 C20 1.503(5) . ? C20 C21 1.384(5) . ? C20 C22 1.392(5) . ? C21 C21 1.400(7) 2 ? C22 C22 1.388(7) 2 ? C23 C24 1.483(5) . ? C24 C25 1.396(5) . ? C24 C26 1.399(5) . ? C25 C28 1.389(5) . ? C26 C27 1.378(5) . ? C27 C29 1.397(5) . ? C28 C29 1.393(5) . ? C29 C30 1.494(5) . ? 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 O5 Co1 O3 121.35(12) 3_455 . ? O5 Co1 N7 113.24(13) 3_455 . ? O3 Co1 N7 123.63(12) . . ? O5 Co1 N4 95.99(12) 3_455 . ? O3 Co1 N4 90.48(12) . . ? N7 Co1 N4 97.16(12) . . ? O5 Co1 N7 86.80(11) 3_455 7 ? O3 Co1 N7 89.39(11) . 7 ? N7 Co1 N7 80.28(13) . 7 ? N4 Co1 N7 176.81(12) . 7 ? O4 Co2 O6 110.88(10) . 3_455 ? O4 Co2 N3 91.26(11) . . ? O6 Co2 N3 89.02(11) 3_455 . ? O4 Co2 O1 158.26(10) . . ? O6 Co2 O1 90.86(10) 3_455 . ? N3 Co2 O1 89.42(11) . . ? O4 Co2 N4 87.25(11) . . ? O6 Co2 N4 95.17(12) 3_455 . ? N3 Co2 N4 175.81(12) . . ? O1 Co2 N4 90.51(11) . . ? O4 Co2 O2 98.01(10) . . ? O6 Co2 O2 150.62(10) 3_455 . ? N3 Co2 O2 85.00(11) . . ? O1 Co2 O2 60.40(10) . . ? N4 Co2 O2 91.32(11) . . ? O4 Co2 C19 128.35(12) . . ? O6 Co2 C19 120.66(12) 3_455 . ? N3 Co2 C19 86.73(12) . . ? O1 Co2 C19 30.02(11) . . ? N4 Co2 C19 91.12(12) . . ? O2 Co2 C19 30.38(11) . . ? C19 O1 Co2 90.4(2) . . ? C19 O2 Co2 88.2(2) . . ? C23 O3 Co1 127.6(2) . . ? C23 O4 Co2 129.0(2) . . ? C30 O5 Co1 130.3(3) . 3_545 ? C30 O6 Co2 134.5(2) . 3_545 ? C9 N2 C10 120.6(3) . . ? C9 N2 C8 118.4(3) . . ? C10 N2 C8 120.8(3) . . ? C17 N3 C18 115.8(3) . . ? C17 N3 Co2 125.3(3) . . ? C18 N3 Co2 118.1(3) . . ? N5 N4 Co1 121.0(3) . . ? N5 N4 Co2 120.1(3) . . ? Co1 N4 Co2 104.46(13) . . ? N6 N5 N4 176.9(5) . . ? N8 N7 Co1 129.6(3) . . ? N8 N7 Co1 124.2(2) . 7 ? Co1 N7 Co1 99.72(13) . 7 ? N9 N8 N7 178.3(4) . . ? N1 C1 C2 178.6(9) . . ? C4 C2 C3 119.0(6) . . ? C4 C2 C1 120.1(5) . . ? C3 C2 C1 120.9(5) . . ? C7 C3 C2 121.7(5) . . ? C5 C4 C2 120.6(5) . . ? C4 C5 C6 120.4(5) . . ? C7 C6 C5 119.2(5) . . ? C3 C7 C6 119.1(4) . . ? C3 C7 C8 120.6(4) . . ? C6 C7 C8 120.3(4) . . ? N2 C8 C7 112.5(3) . . ? N2 C9 C12 120.3(4) . . ? N2 C10 C11 120.9(4) . . ? C10 C11 C13 120.3(4) . . ? C9 C12 C13 121.1(4) . . ? C12 C13 C11 116.9(4) . . ? C12 C13 C14 120.8(4) . . ? C11 C13 C14 122.3(3) . . ? C15 C14 C16 116.2(4) . . ? C15 C14 C13 120.5(3) . . ? C16 C14 C13 123.3(4) . . ? C18 C15 C14 120.2(4) . . ? C17 C16 C14 119.6(4) . . ? N3 C17 C16 124.1(4) . . ? N3 C18 C15 124.0(4) . . ? O1 C19 O2 121.0(3) . . ? O1 C19 C20 119.2(3) . . ? O2 C19 C20 119.8(3) . . ? O1 C19 Co2 59.60(18) . . ? O2 C19 Co2 61.45(18) . . ? C20 C19 Co2 178.8(3) . . ? C21 C20 C22 119.9(3) . . ? C21 C20 C19 119.8(3) . . ? C22 C20 C19 120.3(3) . . ? C20 C21 C21 120.0(2) . 2 ? C22 C22 C20 120.1(2) 2 . ? O4 C23 O3 125.9(4) . . ? O4 C23 C24 117.4(3) . . ? O3 C23 C24 116.6(3) . . ? C25 C24 C26 119.7(3) . . ? C25 C24 C23 119.9(3) . . ? C26 C24 C23 120.2(3) . . ? C28 C25 C24 120.1(4) . . ? C27 C26 C24 120.1(3) . . ? C26 C27 C29 120.1(4) . . ? C25 C28 C29 119.7(3) . . ? C28 C29 C27 120.1(3) . . ? C28 C29 C30 119.5(3) . . ? C27 C29 C30 120.4(3) . . ? O6 C30 O5 126.0(4) . . ? O6 C30 C29 118.3(3) . . ? O5 C30 C29 115.6(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.614 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 967139' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cu6(N3)14(4-CV)2]n' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Cu6(N3)14(4-CV)2]n' _chemical_formula_sum 'C36 H28 Cu6 N48' _chemical_formula_weight 1514.30 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' 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 P2(1)/n _symmetry_space_group_name_hall '-P 2yn' 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 8.6131(9) _cell_length_b 13.4894(13) _cell_length_c 22.967(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.547(7) _cell_angle_gamma 90.00 _cell_volume 2645.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7413 _cell_measurement_theta_min 2.3409 _cell_measurement_theta_max 27.5554 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 2.454 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 'Rigaku Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19773 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4927 _reflns_number_gt 4308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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^)+(0.0876P)^2^+4.3685P] 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 4927 _refine_ls_number_parameters 406 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _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 0.36318(6) 0.59591(4) 0.00932(2) 0.01897(13) Uani 1 1 d . . . Cu2 Cu 0.50240(6) 0.81859(4) -0.00367(2) 0.01928(13) Uani 1 1 d . . . Cu3 Cu 0.25244(6) 0.37737(4) -0.00595(2) 0.02013(13) Uani 1 1 d . . . N1 N -0.9168(5) 1.3293(3) 0.2208(2) 0.0479(13) Uani 1 1 d . . . N2 N -0.2081(4) 0.9773(3) 0.23971(15) 0.0214(9) Uani 1 1 d . . . N3 N 0.3359(4) 0.8680(2) 0.04623(16) 0.0195(8) Uani 1 1 d . . . N4 N 0.6757(4) 0.7467(3) -0.04160(16) 0.0243(9) Uani 1 1 d U . . N5 N 0.7761(4) 0.7968(3) -0.06075(15) 0.0249(9) Uani 1 1 d U . . N6 N 0.8686(5) 0.8422(3) -0.07991(17) 0.0311(10) Uani 1 1 d . . . N7 N 0.3465(4) 0.7167(3) -0.04030(15) 0.0211(9) Uani 1 1 d . . . N8 N 0.3015(4) 0.7168(3) -0.09292(16) 0.0258(9) Uani 1 1 d . . . N9 N 0.2555(6) 0.7185(3) -0.14165(18) 0.0493(13) Uani 1 1 d . . . N10 N 0.6619(4) 0.9123(3) 0.03306(17) 0.0257(9) Uani 1 1 d . . . N11 N 0.6366(4) 0.9893(3) 0.05676(16) 0.0238(9) Uani 1 1 d . . . N12 N 0.6162(5) 1.0631(3) 0.08081(16) 0.0292(10) Uani 1 1 d . . . N13 N 0.5418(4) 0.6640(3) 0.05885(16) 0.0234(9) Uani 1 1 d . . . N14 N 0.5578(4) 0.6771(2) 0.11049(16) 0.0205(9) Uani 1 1 d . . . N15 N 0.5767(5) 0.6942(3) 0.15966(17) 0.0346(11) Uani 1 1 d . . . N16 N 0.1780(4) 0.6472(3) 0.06945(16) 0.0260(9) Uani 1 1 d . . . N17 N 0.0450(4) 0.6662(2) 0.06248(15) 0.0220(9) Uani 1 1 d . . . N18 N -0.0884(4) 0.6904(3) 0.05973(17) 0.0261(9) Uani 1 1 d . . . N19 N 0.4007(4) 0.4627(2) 0.04837(15) 0.0194(8) Uani 1 1 d . . . N20 N 0.4143(4) 0.4542(3) 0.10131(17) 0.0256(9) Uani 1 1 d . . . N21 N 0.4302(6) 0.4464(3) 0.15100(18) 0.0439(13) Uani 1 1 d . . . N22 N 0.2115(4) 0.5141(3) -0.04600(15) 0.0209(9) Uani 1 1 d . . . N23 N 0.0818(4) 0.5503(3) -0.05769(15) 0.0223(9) Uani 1 1 d . . . N24 N -0.0401(4) 0.5846(3) -0.06994(17) 0.0276(10) Uani 1 1 d . . . C1 C -0.8126(6) 1.2753(4) 0.2275(2) 0.0368(13) Uani 1 1 d . . . C2 C -0.6851(5) 1.2048(3) 0.2404(2) 0.0283(12) Uani 1 1 d . . . C3 C -0.5726(6) 1.1964(4) 0.2036(2) 0.0309(12) Uani 1 1 d . . . H3A H -0.5777 1.2357 0.1701 0.037 Uiso 1 1 calc R . . C4 C -0.6813(6) 1.1454(4) 0.2892(2) 0.0343(13) Uani 1 1 d . . . H4A H -0.7595 1.1505 0.3134 0.041 Uiso 1 1 calc R . . C5 C -0.5597(6) 1.0776(4) 0.3022(2) 0.0314(12) Uani 1 1 d . . . H5A H -0.5570 1.0371 0.3351 0.038 Uiso 1 1 calc R . . C6 C -0.4510(6) 1.1290(3) 0.2166(2) 0.0289(12) Uani 1 1 d . . . H6A H -0.3748 1.1234 0.1916 0.035 Uiso 1 1 calc R . . C7 C -0.4419(5) 1.0701(3) 0.26626(18) 0.0236(11) Uani 1 1 d . . . C8 C -0.3103(5) 0.9981(3) 0.28581(18) 0.0223(10) Uani 1 1 d . . . H8A H -0.2465 1.0249 0.3201 0.027 Uiso 1 1 calc R . . H8B H -0.3550 0.9362 0.2972 0.027 Uiso 1 1 calc R . . C9 C -0.2254(5) 0.8932(3) 0.20784(19) 0.0240(11) Uani 1 1 d . . . H9A H -0.3035 0.8483 0.2139 0.029 Uiso 1 1 calc R . . C10 C -0.0969(5) 1.0447(3) 0.2305(2) 0.0287(11) Uani 1 1 d . . . H10A H -0.0884 1.1034 0.2520 0.034 Uiso 1 1 calc R . . C11 C 0.0026(6) 1.0270(4) 0.1900(2) 0.0325(12) Uani 1 1 d . . . H11A H 0.0786 1.0736 0.1841 0.039 Uiso 1 1 calc R . . C12 C -0.1273(5) 0.8735(3) 0.1660(2) 0.0267(11) Uani 1 1 d . . . H12A H -0.1408 0.8158 0.1437 0.032 Uiso 1 1 calc R . . C13 C -0.0090(5) 0.9395(3) 0.15744(18) 0.0235(11) Uani 1 1 d . . . C14 C 0.1085(5) 0.9175(3) 0.11710(19) 0.0220(10) Uani 1 1 d . . . C15 C 0.0679(5) 0.8981(3) 0.0581(2) 0.0221(10) Uani 1 1 d . . . H15A H -0.0361 0.9015 0.0412 0.027 Uiso 1 1 calc R . . C16 C 0.2665(5) 0.9143(3) 0.14004(19) 0.0230(11) Uani 1 1 d . . . H16A H 0.2979 0.9285 0.1794 0.028 Uiso 1 1 calc R . . C17 C 0.3755(5) 0.8898(3) 0.10367(19) 0.0217(10) Uani 1 1 d . . . H17A H 0.4807 0.8881 0.1193 0.026 Uiso 1 1 calc R . . C18 C 0.1848(5) 0.8733(3) 0.02442(18) 0.0208(10) Uani 1 1 d . . . H18A H 0.1564 0.8598 -0.0153 0.025 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 Cu1 0.0217(2) 0.0112(2) 0.0233(3) 0.00001(19) 0.0004(2) -0.00122(19) Cu2 0.0203(2) 0.0135(3) 0.0236(3) -0.0025(2) 0.0015(2) -0.00065(19) Cu3 0.0214(2) 0.0130(2) 0.0256(3) -0.0016(2) 0.0016(2) -0.00131(19) N1 0.048(3) 0.043(3) 0.049(3) -0.005(2) -0.008(2) 0.013(2) N2 0.0241(17) 0.0203(18) 0.0190(17) -0.0004(14) -0.0003(14) 0.0003(15) N3 0.0168(15) 0.0098(16) 0.0306(19) 0.0013(14) -0.0017(14) 0.0031(13) N4 0.0259(17) 0.0185(18) 0.0279(19) 0.0025(15) 0.0016(15) -0.0017(15) N5 0.036(2) 0.0183(18) 0.0191(18) -0.0029(15) 0.0000(15) 0.0057(16) N6 0.0320(19) 0.025(2) 0.038(2) 0.0036(18) 0.0104(17) -0.0106(17) N7 0.0188(16) 0.0156(17) 0.0286(19) -0.0017(15) 0.0016(14) -0.0010(14) N8 0.0267(18) 0.0181(18) 0.032(2) 0.0006(16) 0.0004(16) -0.0066(15) N9 0.077(3) 0.040(2) 0.027(2) 0.0070(19) -0.009(2) -0.032(2) N10 0.0256(18) 0.0139(18) 0.038(2) -0.0092(16) 0.0065(16) 0.0017(15) N11 0.0257(17) 0.0173(18) 0.0262(19) 0.0068(15) -0.0048(15) -0.0084(15) N12 0.042(2) 0.0149(19) 0.031(2) -0.0026(16) 0.0046(17) -0.0009(17) N13 0.0198(16) 0.0204(18) 0.0295(19) -0.0008(16) 0.0013(15) 0.0005(15) N14 0.0223(17) 0.0099(16) 0.0288(19) 0.0081(14) 0.0012(15) -0.0001(13) N15 0.052(2) 0.024(2) 0.026(2) 0.0034(17) -0.0028(19) -0.0066(19) N16 0.0221(17) 0.027(2) 0.029(2) -0.0040(16) 0.0053(15) 0.0043(16) N17 0.0318(19) 0.0112(17) 0.0239(18) -0.0034(14) 0.0074(15) -0.0054(15) N18 0.0225(18) 0.0196(19) 0.037(2) -0.0055(16) 0.0055(16) 0.0027(15) N19 0.0193(16) 0.0133(17) 0.0241(18) -0.0009(14) -0.0021(14) -0.0015(14) N20 0.0293(18) 0.0104(17) 0.035(2) -0.0039(15) -0.0041(16) -0.0007(15) N21 0.067(3) 0.039(3) 0.022(2) 0.0027(19) -0.004(2) -0.012(2) N22 0.0262(17) 0.0156(17) 0.0208(17) -0.0013(14) 0.0028(14) 0.0030(14) N23 0.0285(18) 0.0173(18) 0.0226(18) -0.0043(15) 0.0086(15) -0.0051(15) N24 0.0249(19) 0.027(2) 0.030(2) -0.0015(17) 0.0011(16) -0.0005(16) C1 0.042(3) 0.029(3) 0.036(3) 0.000(2) -0.006(2) 0.002(2) C2 0.033(2) 0.020(2) 0.030(2) -0.0047(19) -0.0051(19) 0.0045(19) C3 0.042(3) 0.028(2) 0.023(2) 0.0077(19) 0.004(2) 0.002(2) C4 0.037(2) 0.039(3) 0.029(2) 0.002(2) 0.010(2) 0.011(2) C5 0.039(3) 0.035(3) 0.021(2) 0.006(2) 0.0068(19) 0.008(2) C6 0.038(2) 0.016(2) 0.034(3) 0.0015(19) 0.010(2) -0.0042(19) C7 0.030(2) 0.020(2) 0.019(2) -0.0017(17) 0.0009(18) 0.0008(18) C8 0.028(2) 0.017(2) 0.023(2) 0.0006(17) 0.0096(17) 0.0012(17) C9 0.024(2) 0.019(2) 0.028(2) 0.0009(18) 0.0007(18) -0.0057(17) C10 0.037(2) 0.017(2) 0.034(2) -0.0075(19) 0.011(2) -0.0099(19) C11 0.039(2) 0.026(2) 0.035(3) -0.005(2) 0.012(2) -0.011(2) C12 0.034(2) 0.018(2) 0.027(2) -0.0028(18) 0.0016(19) 0.0036(19) C13 0.032(2) 0.019(2) 0.020(2) 0.0010(18) 0.0039(18) -0.0041(18) C14 0.026(2) 0.013(2) 0.028(2) -0.0029(17) 0.0086(18) 0.0028(17) C15 0.0187(19) 0.014(2) 0.033(2) 0.0026(18) 0.0035(17) -0.0009(16) C16 0.026(2) 0.023(2) 0.019(2) -0.0008(17) 0.0001(17) -0.0055(18) C17 0.023(2) 0.018(2) 0.023(2) 0.0032(17) -0.0004(17) 0.0021(17) C18 0.028(2) 0.016(2) 0.019(2) -0.0051(16) 0.0041(17) -0.0048(17) _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 N7 1.982(4) . ? Cu1 N13 2.011(3) . ? Cu1 N19 2.015(3) . ? Cu1 N22 2.025(3) . ? Cu1 N16 2.347(4) . ? Cu2 N10 1.973(4) . ? Cu2 N7 2.026(3) . ? Cu2 N3 2.060(4) . ? Cu2 N4 2.067(4) . ? Cu3 N18 1.975(4) 3_565 ? Cu3 N19 2.023(3) . ? Cu3 N4 2.049(3) 3_665 ? Cu3 N22 2.071(3) . ? Cu3 N13 2.344(4) 3_665 ? N1 C1 1.151(7) . ? N2 C9 1.347(6) . ? N2 C10 1.357(6) . ? N2 C8 1.490(6) . ? N3 C18 1.334(5) . ? N3 C17 1.351(5) . ? N4 N5 1.223(5) . ? N4 Cu3 2.049(3) 3_665 ? N5 N6 1.138(5) . ? N7 N8 1.220(5) . ? N8 N9 1.137(5) . ? N10 N11 1.206(5) . ? N11 N12 1.163(5) . ? N13 N14 1.189(5) . ? N13 Cu3 2.344(4) 3_665 ? N14 N15 1.143(5) . ? N16 N17 1.165(5) . ? N17 N18 1.188(5) . ? N18 Cu3 1.975(4) 3_565 ? N19 N20 1.211(5) . ? N20 N21 1.136(5) . ? N22 N23 1.216(5) . ? N23 N24 1.148(5) . ? C1 C2 1.454(7) . ? C2 C3 1.372(7) . ? C2 C4 1.374(7) . ? C3 C6 1.389(7) . ? C4 C5 1.394(7) . ? C5 C7 1.394(7) . ? C6 C7 1.383(6) . ? C7 C8 1.516(6) . ? C9 C12 1.386(7) . ? C10 C11 1.367(7) . ? C11 C13 1.393(6) . ? C12 C13 1.387(6) . ? C13 C14 1.489(6) . ? C14 C15 1.379(6) . ? C14 C16 1.394(6) . ? C15 C18 1.389(6) . ? C16 C17 1.376(6) . ? 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 N7 Cu1 N13 86.68(14) . . ? N7 Cu1 N19 169.66(15) . . ? N13 Cu1 N19 95.14(14) . . ? N7 Cu1 N22 95.45(14) . . ? N13 Cu1 N22 170.43(15) . . ? N19 Cu1 N22 81.14(13) . . ? N7 Cu1 N16 95.31(14) . . ? N13 Cu1 N16 93.49(14) . . ? N19 Cu1 N16 94.74(14) . . ? N22 Cu1 N16 95.59(14) . . ? N10 Cu2 N7 177.08(14) . . ? N10 Cu2 N3 92.94(14) . . ? N7 Cu2 N3 88.78(14) . . ? N10 Cu2 N4 88.85(15) . . ? N7 Cu2 N4 89.00(14) . . ? N3 Cu2 N4 168.64(14) . . ? N18 Cu3 N19 172.26(14) 3_565 . ? N18 Cu3 N4 95.52(14) 3_565 3_665 ? N19 Cu3 N4 90.82(13) . 3_665 ? N18 Cu3 N22 93.94(14) 3_565 . ? N19 Cu3 N22 79.85(13) . . ? N4 Cu3 N22 170.47(13) 3_665 . ? N18 Cu3 N13 95.34(14) 3_565 3_665 ? N19 Cu3 N13 89.78(13) . 3_665 ? N4 Cu3 N13 83.45(14) 3_665 3_665 ? N22 Cu3 N13 94.48(13) . 3_665 ? C9 N2 C10 120.6(4) . . ? C9 N2 C8 120.7(4) . . ? C10 N2 C8 118.6(4) . . ? C18 N3 C17 117.6(4) . . ? C18 N3 Cu2 121.6(3) . . ? C17 N3 Cu2 120.6(3) . . ? N5 N4 Cu3 117.7(3) . 3_665 ? N5 N4 Cu2 118.5(3) . . ? Cu3 N4 Cu2 110.05(17) 3_665 . ? N6 N5 N4 178.3(4) . . ? N8 N7 Cu1 124.1(3) . . ? N8 N7 Cu2 121.2(3) . . ? Cu1 N7 Cu2 108.96(15) . . ? N9 N8 N7 177.9(5) . . ? N11 N10 Cu2 126.0(3) . . ? N12 N11 N10 178.0(4) . . ? N14 N13 Cu1 127.8(3) . . ? N14 N13 Cu3 123.8(3) . 3_665 ? Cu1 N13 Cu3 99.92(15) . 3_665 ? N15 N14 N13 176.5(4) . . ? N17 N16 Cu1 135.7(3) . . ? N16 N17 N18 174.2(4) . . ? N17 N18 Cu3 120.8(3) . 3_565 ? N20 N19 Cu1 121.3(3) . . ? N20 N19 Cu3 122.4(3) . . ? Cu1 N19 Cu3 100.47(14) . . ? N21 N20 N19 178.7(5) . . ? N23 N22 Cu1 114.7(3) . . ? N23 N22 Cu3 123.6(3) . . ? Cu1 N22 Cu3 98.53(14) . . ? N24 N23 N22 178.6(4) . . ? N1 C1 C2 175.4(6) . . ? C3 C2 C4 120.8(4) . . ? C3 C2 C1 120.2(4) . . ? C4 C2 C1 118.9(5) . . ? C2 C3 C6 119.6(4) . . ? C2 C4 C5 119.6(5) . . ? C4 C5 C7 120.4(4) . . ? C7 C6 C3 120.9(5) . . ? C6 C7 C5 118.7(4) . . ? C6 C7 C8 124.9(4) . . ? C5 C7 C8 116.4(4) . . ? N2 C8 C7 113.5(3) . . ? N2 C9 C12 120.3(4) . . ? N2 C10 C11 120.4(4) . . ? C10 C11 C13 120.5(4) . . ? C9 C12 C13 120.1(4) . . ? C12 C13 C11 118.0(4) . . ? C12 C13 C14 122.1(4) . . ? C11 C13 C14 119.8(4) . . ? C15 C14 C16 118.3(4) . . ? C15 C14 C13 123.0(4) . . ? C16 C14 C13 118.7(4) . . ? C14 C15 C18 119.0(4) . . ? C17 C16 C14 119.2(4) . . ? N3 C17 C16 122.7(4) . . ? N3 C18 C15 123.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.621 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.125 _database_code_depnum_ccdc_archive 'CCDC 967140'