Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'L. Lindoy' 'Cameron Kepert' 'Yanyan Mulyana' 'Andrew Parkin' 'Peter Turner' _publ_contact_author_name 'Prof Leonard F. Lindoy' _publ_contact_author_address ; School of Chemistry, F11 University of Sydney Sydney NSW 2006. AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New cobalt(II) and zinc(II) coordination frameworks incorporating a pyridyl-pyrazole ditopic ligand ; data_lfl98 _database_code_depnum_ccdc_archive 'CCDC 258483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H26 Co N10 O17' _chemical_formula_sum 'C16 H26 Co N10 O17' _chemical_formula_weight 689.40 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5821(3) _cell_length_b 11.9066(4) _cell_length_c 12.7124(5) _cell_angle_alpha 105.859(2) _cell_angle_beta 105.380(2) _cell_angle_gamma 95.207(2) _cell_volume 1324.19(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4975 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.8 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.74 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _diffrn_crystal_treatment ; Attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(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 1000' _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 15544 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.76 _reflns_number_total 6218 _reflns_number_gt 5460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0615P)^2^+1.0015P] 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 0 _refine_ls_number_reflns 6218 _refine_ls_number_parameters 440 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Co1A Co 0.5000 0.0000 0.0000 0.01766(9) Uani 1 2 d S . . O1WA O 0.58972(16) -0.07571(13) 0.12422(12) 0.0267(3) Uani 1 1 d D . . H1A1 H 0.660(2) -0.112(2) 0.126(2) 0.036(7) Uiso 1 1 d D . . H1A2 H 0.584(3) -0.056(2) 0.1906(17) 0.044(8) Uiso 1 1 d D . . O2WA O 0.69001(15) 0.13280(11) 0.05140(12) 0.0234(3) Uani 1 1 d D . . H2A1 H 0.676(3) 0.1994(18) 0.049(3) 0.049(8) Uiso 1 1 d D . . H2A2 H 0.751(3) 0.149(2) 0.1171(16) 0.041(7) Uiso 1 1 d D . . C1A C 0.44467(19) 0.21891(15) 0.17920(15) 0.0195(3) Uani 1 1 d . . . H1A H 0.5343 0.2672 0.1883 0.023 Uiso 1 1 calc R . . N2A N 0.40037(17) 0.10744(13) 0.11161(13) 0.0200(3) Uani 1 1 d . . . N3A N 0.26791(16) 0.07250(13) 0.12376(13) 0.0198(3) Uani 1 1 d . . . H3A H 0.2140 0.0016 0.0875 0.024 Uiso 1 1 calc R . . C4A C 0.22910(19) 0.15813(15) 0.19700(15) 0.0202(3) Uani 1 1 d . . . H4A H 0.1417 0.1531 0.2186 0.024 Uiso 1 1 calc R . . C5A C 0.34085(18) 0.25602(14) 0.23559(14) 0.0175(3) Uani 1 1 d . . . C6A C 0.34489(18) 0.37188(14) 0.31391(14) 0.0176(3) Uani 1 1 d . . . C7A C 0.2396(2) 0.38951(16) 0.37254(16) 0.0237(4) Uani 1 1 d . . . H7A H 0.1687 0.3242 0.3647 0.028 Uiso 1 1 calc R . . C8A C 0.2384(2) 0.50033(17) 0.44114(16) 0.0275(4) Uani 1 1 d . . . H8A H 0.1664 0.5117 0.4802 0.033 Uiso 1 1 calc R . . N9A N 0.33914(18) 0.59285(13) 0.45298(13) 0.0249(3) Uani 1 1 d . . . H9A H 0.3355 0.6639 0.4955 0.030 Uiso 1 1 calc R . . C10A C 0.4450(2) 0.58000(16) 0.40188(15) 0.0246(4) Uani 1 1 d . . . H10A H 0.5162 0.6468 0.4136 0.030 Uiso 1 1 calc R . . C11A C 0.4512(2) 0.47045(15) 0.33249(15) 0.0220(3) Uani 1 1 d . . . H11A H 0.5271 0.4615 0.2972 0.026 Uiso 1 1 calc R . . Co1B Co 0.0000 0.0000 0.5000 0.01822(9) Uani 1 2 d S . . O1WB O -0.15557(15) 0.01565(12) 0.36092(11) 0.0245(3) Uani 1 1 d D . . H1B1 H -0.206(3) 0.0699(19) 0.372(2) 0.036(7) Uiso 1 1 d D . . H1B2 H -0.133(3) 0.016(2) 0.3018(18) 0.040(7) Uiso 1 1 d D . . O2WB O -0.13956(16) -0.14919(12) 0.50266(13) 0.0274(3) Uani 1 1 d D . . H2B1 H -0.209(3) -0.187(3) 0.443(2) 0.054(9) Uiso 1 1 d D . . H2B2 H -0.088(3) -0.196(2) 0.523(3) 0.061(10) Uiso 1 1 d D . . C1B C 0.04787(19) -0.22273(15) 0.33173(15) 0.0207(3) Uani 1 1 d . . . H1B H -0.0409 -0.2662 0.3308 0.025 Uiso 1 1 calc R . . N2B N 0.09691(17) -0.10882(13) 0.38871(13) 0.0205(3) Uani 1 1 d . . . N3B N 0.22567(16) -0.08260(13) 0.36746(13) 0.0200(3) Uani 1 1 d . . . H3B H 0.2814 -0.0119 0.3955 0.024 Uiso 1 1 calc R . . C4B C 0.2574(2) -0.17690(15) 0.29889(15) 0.0214(3) Uani 1 1 d . . . H4B H 0.3416 -0.1793 0.2728 0.026 Uiso 1 1 calc R . . C5B C 0.14406(19) -0.27084(14) 0.27289(14) 0.0183(3) Uani 1 1 d . . . C6B C 0.1255(2) -0.39254(15) 0.20138(15) 0.0221(3) Uani 1 1 d . . . C7B C 0.2210(3) -0.42771(19) 0.13747(17) 0.0332(5) Uani 1 1 d . . . H7B H 0.3008 -0.3723 0.1404 0.040 Uiso 1 1 calc R . . C8B C 0.1971(4) -0.5449(2) 0.06973(19) 0.0488(7) Uani 1 1 d . . . H8B H 0.2605 -0.5699 0.0251 0.059 Uiso 1 1 calc R . . N9B N 0.0860(3) -0.62284(16) 0.06671(16) 0.0496(6) Uani 1 1 d . . . H9B H 0.0736 -0.6968 0.0234 0.060 Uiso 1 1 calc R . . C10B C -0.0070(3) -0.59292(18) 0.1269(2) 0.0446(6) Uani 1 1 d . . . H10B H -0.0848 -0.6510 0.1227 0.054 Uiso 1 1 calc R . . C11B C 0.0097(2) -0.47836(17) 0.19484(19) 0.0334(4) Uani 1 1 d . . . H11B H -0.0567 -0.4568 0.2375 0.040 Uiso 1 1 calc R . . N1 N 0.35953(19) 0.34649(15) -0.23091(16) 0.0308(4) Uani 1 1 d . . . O11 O 0.2681(2) 0.3810(2) -0.2997(2) 0.0751(8) Uani 1 1 d . . . O12 O 0.4012(3) 0.25527(16) -0.2693(2) 0.0677(7) Uani 1 1 d . . . O13 O 0.4046(3) 0.40508(17) -0.12918(16) 0.0594(5) Uani 1 1 d . . . N2 N 0.88404(17) 0.29847(13) 0.34184(13) 0.0221(3) Uani 1 1 d . . . O21 O 0.90846(15) 0.21569(12) 0.26616(12) 0.0281(3) Uani 1 1 d . . . O22 O 0.79209(17) 0.36008(13) 0.31387(13) 0.0328(3) Uani 1 1 d . . . O23 O 0.95506(15) 0.31741(12) 0.44537(11) 0.0267(3) Uani 1 1 d . . . N3 N -0.06539(17) -0.11169(13) 0.10515(13) 0.0216(3) Uani 1 1 d . . . O31 O -0.05509(17) -0.00906(12) 0.16695(13) 0.0340(3) Uani 1 1 d . . . O32 O -0.17219(15) -0.19020(11) 0.09027(12) 0.0261(3) Uani 1 1 d . . . O33 O 0.03016(15) -0.13863(12) 0.05592(12) 0.0274(3) Uani 1 1 d . . . N4 N 0.46352(16) 0.89208(13) 0.60098(12) 0.0196(3) Uani 1 1 d . . . O41 O 0.49071(16) 0.99322(12) 0.67062(13) 0.0306(3) Uani 1 1 d . . . O42 O 0.55106(15) 0.85709(12) 0.54782(12) 0.0274(3) Uani 1 1 d . . . O43 O 0.34427(14) 0.82395(11) 0.58447(12) 0.0235(3) Uani 1 1 d . . . O1W O 0.6206(2) 0.34810(15) 0.03838(18) 0.0452(4) Uani 1 1 d D . . H1W1 H 0.650(4) 0.413(2) 0.090(3) 0.082(12) Uiso 1 1 d D . . H1W2 H 0.560(8) 0.347(8) -0.024(4) 0.26(4) Uiso 1 1 d 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 Co1A 0.01788(17) 0.01459(16) 0.01976(16) 0.00187(12) 0.00778(12) 0.00356(12) O1WA 0.0285(7) 0.0319(7) 0.0246(6) 0.0097(5) 0.0121(6) 0.0137(6) O2WA 0.0216(6) 0.0193(6) 0.0267(7) 0.0031(5) 0.0078(5) 0.0013(5) C1A 0.0193(8) 0.0169(7) 0.0223(8) 0.0035(6) 0.0091(6) 0.0035(6) N2A 0.0187(7) 0.0184(7) 0.0227(7) 0.0037(5) 0.0089(6) 0.0034(5) N3A 0.0183(7) 0.0156(6) 0.0232(7) 0.0017(5) 0.0075(6) 0.0012(5) C4A 0.0183(8) 0.0183(8) 0.0236(8) 0.0034(6) 0.0088(6) 0.0030(6) C5A 0.0166(8) 0.0172(7) 0.0188(7) 0.0044(6) 0.0064(6) 0.0042(6) C6A 0.0172(8) 0.0177(7) 0.0167(7) 0.0035(6) 0.0041(6) 0.0059(6) C7A 0.0179(8) 0.0239(9) 0.0252(8) 0.0006(7) 0.0072(7) 0.0027(7) C8A 0.0210(9) 0.0301(10) 0.0261(9) -0.0016(7) 0.0078(7) 0.0080(7) N9A 0.0289(8) 0.0188(7) 0.0202(7) -0.0010(6) 0.0021(6) 0.0088(6) C10A 0.0302(10) 0.0180(8) 0.0220(8) 0.0048(6) 0.0044(7) 0.0015(7) C11A 0.0249(9) 0.0192(8) 0.0220(8) 0.0050(6) 0.0089(7) 0.0029(7) Co1B 0.01737(17) 0.01487(16) 0.02260(17) 0.00304(12) 0.00873(13) 0.00421(12) O1WB 0.0227(7) 0.0268(7) 0.0254(6) 0.0060(5) 0.0105(5) 0.0087(5) O2WB 0.0258(7) 0.0207(6) 0.0366(8) 0.0056(6) 0.0147(6) 0.0027(5) C1B 0.0172(8) 0.0185(8) 0.0253(8) 0.0040(6) 0.0078(7) 0.0021(6) N2B 0.0189(7) 0.0176(7) 0.0248(7) 0.0035(6) 0.0093(6) 0.0033(5) N3B 0.0185(7) 0.0152(6) 0.0261(7) 0.0035(5) 0.0101(6) 0.0006(5) C4B 0.0208(8) 0.0188(8) 0.0250(8) 0.0043(6) 0.0103(7) 0.0036(6) C5B 0.0184(8) 0.0162(7) 0.0197(7) 0.0036(6) 0.0062(6) 0.0043(6) C6B 0.0275(9) 0.0173(8) 0.0177(7) 0.0032(6) 0.0021(7) 0.0071(7) C7B 0.0467(13) 0.0308(10) 0.0253(9) 0.0061(8) 0.0147(9) 0.0185(9) C8B 0.082(2) 0.0453(14) 0.0233(10) 0.0078(9) 0.0162(11) 0.0423(14) N9B 0.0857(17) 0.0178(8) 0.0254(9) -0.0015(7) -0.0099(10) 0.0161(10) C10B 0.0551(15) 0.0179(9) 0.0401(12) 0.0032(8) -0.0111(11) -0.0011(9) C11B 0.0357(11) 0.0197(9) 0.0357(10) 0.0050(8) 0.0011(9) 0.0005(8) N1 0.0267(8) 0.0234(8) 0.0419(10) 0.0089(7) 0.0128(7) -0.0008(6) O11 0.0244(9) 0.1126(19) 0.1022(18) 0.0777(16) 0.0018(10) -0.0054(10) O12 0.1084(19) 0.0307(9) 0.0892(16) 0.0169(10) 0.0699(15) 0.0218(10) O13 0.0755(14) 0.0461(10) 0.0416(10) -0.0062(8) 0.0179(10) -0.0020(10) N2 0.0215(7) 0.0177(7) 0.0258(7) 0.0028(6) 0.0099(6) 0.0011(6) O21 0.0293(7) 0.0231(6) 0.0272(7) -0.0019(5) 0.0105(6) 0.0058(5) O22 0.0332(8) 0.0293(7) 0.0361(8) 0.0080(6) 0.0099(6) 0.0141(6) O23 0.0270(7) 0.0265(6) 0.0239(6) 0.0038(5) 0.0077(5) 0.0043(5) N3 0.0232(7) 0.0174(7) 0.0214(7) 0.0024(5) 0.0061(6) 0.0027(6) O31 0.0396(8) 0.0179(6) 0.0400(8) -0.0059(6) 0.0224(7) -0.0021(6) O32 0.0230(7) 0.0174(6) 0.0339(7) 0.0008(5) 0.0102(6) 0.0005(5) O33 0.0267(7) 0.0219(6) 0.0313(7) -0.0002(5) 0.0144(6) 0.0024(5) N4 0.0191(7) 0.0185(7) 0.0206(7) 0.0049(5) 0.0066(5) 0.0026(5) O41 0.0325(8) 0.0188(6) 0.0356(7) -0.0039(5) 0.0180(6) -0.0043(5) O42 0.0247(7) 0.0253(7) 0.0324(7) 0.0024(5) 0.0160(6) 0.0033(5) O43 0.0182(6) 0.0183(6) 0.0314(7) 0.0022(5) 0.0099(5) -0.0001(5) O1W 0.0601(12) 0.0274(8) 0.0567(11) 0.0143(8) 0.0295(9) 0.0096(8) _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 Co1A O1WA 2.0601(14) . ? Co1A O1WA 2.0601(14) 2_655 ? Co1A N2A 2.1234(14) 2_655 ? Co1A N2A 2.1235(14) . ? Co1A O2WA 2.1269(13) 2_655 ? Co1A O2WA 2.1269(13) . ? C1A N2A 1.327(2) . ? C1A C5A 1.408(2) . ? N2A N3A 1.361(2) . ? N3A C4A 1.333(2) . ? C4A C5A 1.389(2) . ? C5A C6A 1.454(2) . ? C6A C7A 1.403(2) . ? C6A C11A 1.405(2) . ? C7A C8A 1.372(2) . ? C8A N9A 1.344(3) . ? N9A C10A 1.341(3) . ? C10A C11A 1.377(2) . ? Co1B O1WB 2.0531(14) 2_556 ? Co1B O1WB 2.0531(14) . ? Co1B N2B 2.1109(14) 2_556 ? Co1B N2B 2.1109(14) . ? Co1B O2WB 2.1379(14) . ? Co1B O2WB 2.1379(14) 2_556 ? C1B N2B 1.324(2) . ? C1B C5B 1.402(2) . ? N2B N3B 1.359(2) . ? N3B C4B 1.335(2) . ? C4B C5B 1.388(2) . ? C5B C6B 1.451(2) . ? C6B C7B 1.397(3) . ? C6B C11B 1.407(3) . ? C7B C8B 1.387(3) . ? C8B N9B 1.332(4) . ? N9B C10B 1.333(4) . ? C10B C11B 1.369(3) . ? N1 O12 1.212(2) . ? N1 O13 1.225(3) . ? N1 O11 1.247(3) . ? N2 O22 1.239(2) . ? N2 O23 1.257(2) . ? N2 O21 1.2629(19) . ? N3 O31 1.2380(19) . ? N3 O33 1.257(2) . ? N3 O32 1.259(2) . ? N4 O41 1.2409(19) . ? N4 O42 1.2426(19) . ? N4 O43 1.2726(19) . ? 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 O1WA Co1A O1WA 180.00(7) . 2_655 ? O1WA Co1A N2A 89.51(6) . 2_655 ? O1WA Co1A N2A 90.49(6) 2_655 2_655 ? O1WA Co1A N2A 90.49(6) . . ? O1WA Co1A N2A 89.51(6) 2_655 . ? N2A Co1A N2A 180.00(7) 2_655 . ? O1WA Co1A O2WA 86.92(6) . 2_655 ? O1WA Co1A O2WA 93.08(6) 2_655 2_655 ? N2A Co1A O2WA 92.84(5) 2_655 2_655 ? N2A Co1A O2WA 87.16(5) . 2_655 ? O1WA Co1A O2WA 93.08(6) . . ? O1WA Co1A O2WA 86.92(6) 2_655 . ? N2A Co1A O2WA 87.16(5) 2_655 . ? N2A Co1A O2WA 92.84(5) . . ? O2WA Co1A O2WA 180.0 2_655 . ? N2A C1A C5A 110.84(15) . . ? C1A N2A N3A 105.28(14) . . ? C1A N2A Co1A 130.23(12) . . ? N3A N2A Co1A 124.45(11) . . ? C4A N3A N2A 112.24(14) . . ? N3A C4A C5A 106.89(15) . . ? C4A C5A C1A 104.75(14) . . ? C4A C5A C6A 126.80(15) . . ? C1A C5A C6A 128.41(16) . . ? C7A C6A C11A 117.40(15) . . ? C7A C6A C5A 120.61(16) . . ? C11A C6A C5A 121.99(15) . . ? C8A C7A C6A 120.51(18) . . ? N9A C8A C7A 119.89(17) . . ? C10A N9A C8A 121.91(15) . . ? N9A C10A C11A 120.32(17) . . ? C10A C11A C6A 119.88(17) . . ? O1WB Co1B O1WB 180.0 2_556 . ? O1WB Co1B N2B 89.91(5) 2_556 2_556 ? O1WB Co1B N2B 90.09(5) . 2_556 ? O1WB Co1B N2B 90.09(5) 2_556 . ? O1WB Co1B N2B 89.91(5) . . ? N2B Co1B N2B 180.0 2_556 . ? O1WB Co1B O2WB 88.84(6) 2_556 . ? O1WB Co1B O2WB 91.16(6) . . ? N2B Co1B O2WB 87.71(5) 2_556 . ? N2B Co1B O2WB 92.29(5) . . ? O1WB Co1B O2WB 91.16(6) 2_556 2_556 ? O1WB Co1B O2WB 88.84(6) . 2_556 ? N2B Co1B O2WB 92.29(5) 2_556 2_556 ? N2B Co1B O2WB 87.71(5) . 2_556 ? O2WB Co1B O2WB 180.00(9) . 2_556 ? N2B C1B C5B 111.10(15) . . ? C1B N2B N3B 105.39(14) . . ? C1B N2B Co1B 125.59(12) . . ? N3B N2B Co1B 128.79(11) . . ? C4B N3B N2B 111.89(14) . . ? N3B C4B C5B 106.99(15) . . ? C4B C5B C1B 104.63(14) . . ? C4B C5B C6B 129.00(16) . . ? C1B C5B C6B 126.37(16) . . ? C7B C6B C11B 118.30(18) . . ? C7B C6B C5B 121.28(18) . . ? C11B C6B C5B 120.43(17) . . ? C8B C7B C6B 118.8(2) . . ? N9B C8B C7B 120.5(2) . . ? C8B N9B C10B 122.46(19) . . ? N9B C10B C11B 119.9(2) . . ? C10B C11B C6B 120.0(2) . . ? O12 N1 O13 122.7(2) . . ? O12 N1 O11 117.4(2) . . ? O13 N1 O11 119.9(2) . . ? O22 N2 O23 120.89(15) . . ? O22 N2 O21 120.21(16) . . ? O23 N2 O21 118.90(15) . . ? O31 N3 O33 120.44(15) . . ? O31 N3 O32 120.38(15) . . ? O33 N3 O32 119.18(14) . . ? O41 N4 O42 120.84(15) . . ? O41 N4 O43 119.11(14) . . ? O42 N4 O43 120.06(14) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.794 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.077 data_lfl77 _database_code_depnum_ccdc_archive 'CCDC 258484' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Cl2 N6 O2 Zn2' _chemical_formula_weight 582.09 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' Cl Cl 0.1484 0.1585 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 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 8.864(2) _cell_length_b 16.191(4) _cell_length_c 10.443(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.688(4) _cell_angle_gamma 90.00 _cell_volume 1361.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 107 _cell_measurement_theta_min 2.516 _cell_measurement_theta_max 28.017 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.204 _exptl_crystal_size_mid 0.118 _exptl_crystal_size_min 0.102 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 1.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 138 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 12736 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.24 _reflns_number_total 3175 _reflns_number_gt 2750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3175 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 Zn1 Zn 0.18318(6) 0.44319(3) 0.52227(6) 0.01970(16) Uani 1 1 d . . . Cl1 Cl 0.43133(14) 0.46810(8) 0.70613(14) 0.0316(3) Uani 1 1 d . . . N1 N 0.1124(4) 0.5492(2) 0.4156(4) 0.0206(7) Uani 1 1 d . . . N2 N -0.0164(4) 0.5975(2) 0.4121(4) 0.0209(8) Uani 1 1 d . . . C1 C 0.1952(6) 0.5913(3) 0.3551(5) 0.0259(10) Uani 1 1 d . . . H1 H 0.2911 0.5718 0.3456 0.031 Uiso 1 1 calc R . . C2 C 0.1203(5) 0.6685(3) 0.3075(5) 0.0228(9) Uani 1 1 d . . . C3 C -0.0127(6) 0.6683(3) 0.3467(6) 0.0296(11) Uani 1 1 d . . . H3 H -0.0897 0.7123 0.3293 0.036 Uiso 1 1 calc R . . N3 N 0.2666(5) 0.8563(2) 0.0944(4) 0.0251(8) Uani 1 1 d . . . C4 C 0.1713(6) 0.7331(3) 0.2357(5) 0.0253(10) Uani 1 1 d . . . C5 C 0.0720(7) 0.8012(4) 0.1777(7) 0.0459(16) Uani 1 1 d . . . H5 H -0.0302 0.8073 0.1859 0.055 Uiso 1 1 calc R . . C6 C 0.1221(7) 0.8607(3) 0.1072(7) 0.0416(15) Uani 1 1 d . . . H6 H 0.0509 0.9064 0.0663 0.050 Uiso 1 1 calc R . . C7 C 0.3671(6) 0.7930(3) 0.1588(6) 0.0346(12) Uani 1 1 d . . . H7 H 0.4733 0.7908 0.1569 0.042 Uiso 1 1 calc R . . C8 C 0.3241(6) 0.7307(3) 0.2279(6) 0.0365(13) Uani 1 1 d . . . H8 H 0.3988 0.6865 0.2699 0.044 Uiso 1 1 calc R . . O1 O 0.2491(7) 0.6309(3) 0.7717(5) 0.0657(14) Uani 1 1 d . . . H1O H 0.3086 0.5961 0.7546 0.099 Uiso 1 1 calc R . . C9 C 0.2612(13) 0.6186(7) 0.9088(11) 0.095(3) Uani 1 1 d . . . H9A H 0.2199 0.6689 0.9375 0.114 Uiso 1 1 calc R . . H9B H 0.3801 0.6127 0.9731 0.114 Uiso 1 1 calc R . . C10 C 0.1688(14) 0.5449(8) 0.9301(11) 0.121(5) Uani 1 1 d . . . H10A H 0.2164 0.4939 0.9123 0.182 Uiso 1 1 calc R . . H10B H 0.0514 0.5485 0.8646 0.182 Uiso 1 1 calc R . . H10C H 0.1789 0.5448 1.0272 0.182 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 Zn1 0.0224(3) 0.0149(2) 0.0318(3) 0.0034(2) 0.0212(2) 0.00333(19) Cl1 0.0226(5) 0.0371(6) 0.0388(7) -0.0024(5) 0.0164(5) 0.0016(5) N1 0.0225(17) 0.0156(16) 0.033(2) 0.0048(15) 0.0212(16) 0.0026(14) N2 0.0218(18) 0.0172(17) 0.032(2) 0.0040(15) 0.0199(17) 0.0033(14) C1 0.025(2) 0.023(2) 0.039(3) 0.009(2) 0.023(2) 0.0041(18) C2 0.022(2) 0.023(2) 0.031(2) 0.0043(19) 0.0176(19) 0.0007(17) C3 0.032(2) 0.021(2) 0.051(3) 0.013(2) 0.032(2) 0.0069(19) N3 0.026(2) 0.0205(18) 0.039(2) 0.0035(16) 0.0238(19) 0.0009(15) C4 0.026(2) 0.024(2) 0.037(3) 0.004(2) 0.024(2) -0.0011(18) C5 0.041(3) 0.041(3) 0.080(5) 0.033(3) 0.050(3) 0.018(2) C6 0.040(3) 0.034(3) 0.071(4) 0.028(3) 0.043(3) 0.017(2) C7 0.025(2) 0.032(3) 0.057(3) 0.013(2) 0.027(2) 0.004(2) C8 0.026(2) 0.031(3) 0.062(4) 0.022(2) 0.028(3) 0.010(2) O1 0.072(3) 0.078(4) 0.061(3) 0.007(3) 0.041(3) 0.031(3) C9 0.094(7) 0.114(8) 0.080(7) -0.019(6) 0.038(6) -0.011(6) C10 0.113(9) 0.186(13) 0.072(6) -0.006(8) 0.046(6) -0.058(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 Zn1 N2 1.984(3) 3_566 ? Zn1 N1 1.999(4) . ? Zn1 N3 2.029(4) 2_545 ? Zn1 Cl1 2.2715(14) . ? N1 C1 1.338(5) . ? N1 N2 1.371(5) . ? N2 C3 1.343(6) . ? N2 Zn1 1.984(3) 3_566 ? C1 C2 1.405(6) . ? C1 H1 0.9500 . ? C2 C3 1.400(6) . ? C2 C4 1.464(6) . ? C3 H3 0.9500 . ? N3 C7 1.341(6) . ? N3 C6 1.344(6) . ? N3 Zn1 2.029(4) 2 ? C4 C5 1.383(7) . ? C4 C8 1.392(6) . ? C5 C6 1.394(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.382(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? O1 C9 1.405(11) . ? O1 H1O 0.8400 . ? C9 C10 1.515(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 Zn1 N1 111.82(14) 3_566 . ? N2 Zn1 N3 111.07(15) 3_566 2_545 ? N1 Zn1 N3 110.94(16) . 2_545 ? N2 Zn1 Cl1 111.43(12) 3_566 . ? N1 Zn1 Cl1 106.63(12) . . ? N3 Zn1 Cl1 104.65(12) 2_545 . ? C1 N1 N2 108.2(3) . . ? C1 N1 Zn1 126.5(3) . . ? N2 N1 Zn1 124.6(3) . . ? C3 N2 N1 107.6(3) . . ? C3 N2 Zn1 129.8(3) . 3_566 ? N1 N2 Zn1 122.3(3) . 3_566 ? N1 C1 C2 110.4(4) . . ? N1 C1 H1 124.8 . . ? C2 C1 H1 124.8 . . ? C3 C2 C1 103.1(4) . . ? C3 C2 C4 129.0(4) . . ? C1 C2 C4 128.0(4) . . ? N2 C3 C2 110.7(4) . . ? N2 C3 H3 124.7 . . ? C2 C3 H3 124.7 . . ? C7 N3 C6 116.9(4) . . ? C7 N3 Zn1 124.4(3) . 2 ? C6 N3 Zn1 118.7(3) . 2 ? C5 C4 C8 117.0(4) . . ? C5 C4 C2 121.2(4) . . ? C8 C4 C2 121.8(4) . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N3 C6 C5 122.9(5) . . ? N3 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? N3 C7 C8 123.3(4) . . ? N3 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C4 119.9(4) . . ? C7 C8 H8 120.1 . . ? C4 C8 H8 120.1 . . ? C9 O1 H1O 109.5 . . ? O1 C9 C10 116.5(8) . . ? O1 C9 H9A 108.2 . . ? C10 C9 H9A 108.2 . . ? O1 C9 H9B 108.2 . . ? C10 C9 H9B 108.2 . . ? H9A C9 H9B 107.3 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 N2 Zn1 N1 C1 -178.3(4) 3_566 . . . ? N3 Zn1 N1 C1 -53.7(4) 2_545 . . . ? Cl1 Zn1 N1 C1 59.6(4) . . . . ? N2 Zn1 N1 N2 12.8(5) 3_566 . . . ? N3 Zn1 N1 N2 137.3(3) 2_545 . . . ? Cl1 Zn1 N1 N2 -109.3(3) . . . . ? C1 N1 N2 C3 1.2(5) . . . . ? Zn1 N1 N2 C3 171.8(3) . . . . ? C1 N1 N2 Zn1 175.4(3) . . . 3_566 ? Zn1 N1 N2 Zn1 -14.0(5) . . . 3_566 ? N2 N1 C1 C2 -1.1(5) . . . . ? Zn1 N1 C1 C2 -171.5(3) . . . . ? N1 C1 C2 C3 0.6(6) . . . . ? N1 C1 C2 C4 -179.9(5) . . . . ? N1 N2 C3 C2 -0.8(6) . . . . ? Zn1 N2 C3 C2 -174.4(3) 3_566 . . . ? C1 C2 C3 N2 0.2(6) . . . . ? C4 C2 C3 N2 -179.3(5) . . . . ? C3 C2 C4 C5 -9.7(9) . . . . ? C1 C2 C4 C5 170.9(6) . . . . ? C3 C2 C4 C8 167.5(6) . . . . ? C1 C2 C4 C8 -11.9(8) . . . . ? C8 C4 C5 C6 4.2(9) . . . . ? C2 C4 C5 C6 -178.5(6) . . . . ? C7 N3 C6 C5 -2.9(9) . . . . ? Zn1 N3 C6 C5 175.9(5) 2 . . . ? C4 C5 C6 N3 -1.3(11) . . . . ? C6 N3 C7 C8 4.4(9) . . . . ? Zn1 N3 C7 C8 -174.4(5) 2 . . . ? N3 C7 C8 C4 -1.6(9) . . . . ? C5 C4 C8 C7 -2.8(9) . . . . ? C2 C4 C8 C7 179.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O Cl1 0.84 2.49 3.309(5) 165.5 . _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.814 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.113 data_lfl105 _database_code_depnum_ccdc_archive 'CCDC 258485' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co(NO3)4(C8N6H8)2 _chemical_formula_sum 'C16 H16 Co N10 O12' _chemical_formula_weight 599.32 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_Int_Tables_number ? 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 13.0784(12) _cell_length_b 11.1055(9) _cell_length_c 15.9865(13) _cell_angle_alpha 90.00 _cell_angle_beta 108.225(4) _cell_angle_gamma 90.00 _cell_volume 2205.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6306 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.9 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.94 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _diffrn_crystal_treatment ; Attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 1000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7995 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 28.83 _reflns_number_total 2609 _reflns_number_gt 2134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0907P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 2609 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.0000 0.5000 0.0000 0.01747(17) Uani 1 2 d S . . C1 C 0.08910(17) 0.29390(18) 0.14094(14) 0.0200(4) Uani 1 1 d . . . H1 H 0.0767 0.2325 0.0994 0.024 Uiso 1 1 calc R . . N2 N 0.07715(14) 0.41123(14) 0.12137(12) 0.0207(4) Uani 1 1 d . . . N3 N 0.10361(15) 0.46796(15) 0.20064(12) 0.0194(4) Uani 1 1 d . . . H3 H 0.1029 0.5449 0.2066 0.023 Uiso 1 1 calc R . . C4 C 0.13080(16) 0.39115(17) 0.26798(14) 0.0198(4) Uani 1 1 d . . . H4 H 0.1513 0.4108 0.3275 0.024 Uiso 1 1 calc R . . C5 C 0.12276(15) 0.27564(17) 0.23232(14) 0.0184(4) Uani 1 1 d . . . C6 C 0.13673(15) 0.16091(17) 0.27928(14) 0.0181(4) Uani 1 1 d . . . C7 C 0.14945(17) 0.15633(17) 0.37001(14) 0.0209(4) Uani 1 1 d . . . H7 H 0.1522 0.2271 0.4017 0.025 Uiso 1 1 calc R . . C8 C 0.15777(18) 0.04693(19) 0.41134(15) 0.0237(5) Uani 1 1 d . . . H8 H 0.1672 0.0437 0.4714 0.028 Uiso 1 1 calc R . . N9 N 0.15247(15) -0.05560(15) 0.36576(12) 0.0232(4) Uani 1 1 d . . . H9 H 0.1565 -0.1233 0.3927 0.028 Uiso 1 1 calc R . . C10 C 0.14107(17) -0.05553(18) 0.27940(15) 0.0229(5) Uani 1 1 d . . . H10 H 0.1383 -0.1280 0.2496 0.027 Uiso 1 1 calc R . . C11 C 0.13342(17) 0.05149(18) 0.23498(14) 0.0212(4) Uani 1 1 d . . . H11 H 0.1260 0.0514 0.1752 0.025 Uiso 1 1 calc R . . N1N N 0.10028(15) 0.73829(14) 0.09143(12) 0.0225(4) Uani 1 1 d . . . O1N1 O 0.09405(12) 0.66055(12) 0.03151(10) 0.0235(4) Uani 1 1 d . . . O1N2 O 0.08506(14) 0.70893(13) 0.16181(11) 0.0276(4) Uani 1 1 d . . . O1N3 O 0.12343(18) 0.84344(14) 0.07918(12) 0.0405(5) Uani 1 1 d . . . N2N N -0.14430(14) 0.65030(14) 0.07996(12) 0.0212(4) Uani 1 1 d . . . O2N1 O -0.11957(13) 0.54521(12) 0.05854(10) 0.0231(3) Uani 1 1 d . . . O2N2 O -0.18238(16) 0.65982(14) 0.14088(12) 0.0336(4) Uani 1 1 d . . . O2N3 O -0.12989(13) 0.74057(12) 0.03844(10) 0.0257(4) Uani 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 0.0201(2) 0.0114(2) 0.0203(3) 0.00048(13) 0.00546(17) 0.00077(12) C1 0.0206(10) 0.0139(9) 0.0255(11) 0.0004(8) 0.0073(8) 0.0010(7) N2 0.0219(9) 0.0151(8) 0.0247(9) -0.0003(7) 0.0066(7) 0.0009(6) N3 0.0201(8) 0.0140(7) 0.0224(9) -0.0018(7) 0.0045(7) -0.0010(6) C4 0.0196(9) 0.0142(8) 0.0245(10) 0.0007(8) 0.0052(8) 0.0002(7) C5 0.0164(9) 0.0148(8) 0.0235(10) -0.0012(7) 0.0057(8) 0.0006(7) C6 0.0125(9) 0.0164(8) 0.0247(10) 0.0006(8) 0.0048(7) 0.0006(7) C7 0.0217(10) 0.0161(9) 0.0242(10) -0.0017(8) 0.0064(8) 0.0012(7) C8 0.0268(11) 0.0201(10) 0.0230(10) 0.0009(8) 0.0060(8) 0.0008(8) N9 0.0246(9) 0.0143(7) 0.0295(10) 0.0037(7) 0.0069(7) 0.0011(6) C10 0.0225(10) 0.0157(9) 0.0305(11) -0.0039(8) 0.0086(9) 0.0005(7) C11 0.0219(10) 0.0190(9) 0.0227(10) -0.0015(8) 0.0069(8) 0.0012(7) N1N 0.0248(9) 0.0144(7) 0.0253(9) 0.0000(7) 0.0035(7) -0.0026(7) O1N1 0.0252(8) 0.0171(7) 0.0275(8) -0.0051(6) 0.0074(6) -0.0041(6) O1N2 0.0417(10) 0.0145(7) 0.0251(8) 0.0002(6) 0.0082(7) -0.0036(6) O1N3 0.0710(14) 0.0163(7) 0.0377(10) -0.0019(7) 0.0222(9) -0.0128(8) N2N 0.0215(9) 0.0175(8) 0.0241(9) 0.0000(7) 0.0063(7) 0.0023(6) O2N1 0.0281(8) 0.0140(7) 0.0297(8) -0.0022(6) 0.0127(6) 0.0016(6) O2N2 0.0483(11) 0.0263(8) 0.0348(9) 0.0027(7) 0.0256(8) 0.0092(7) O2N3 0.0319(8) 0.0157(7) 0.0313(8) 0.0030(6) 0.0125(7) 0.0024(6) _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 O2N1 2.1186(16) 5_565 ? Co1 O2N1 2.1186(16) . ? Co1 N2 2.1284(17) . ? Co1 N2 2.1284(17) 5_565 ? Co1 O1N1 2.1349(14) 5_565 ? Co1 O1N1 2.1349(14) . ? C1 N2 1.338(2) . ? C1 C5 1.402(3) . ? N2 N3 1.360(2) . ? N3 C4 1.332(3) . ? C4 C5 1.394(3) . ? C5 C6 1.461(3) . ? C6 C11 1.400(3) . ? C6 C7 1.408(3) . ? C7 C8 1.371(3) . ? C8 N9 1.342(3) . ? N9 C10 1.341(3) . ? C10 C11 1.372(3) . ? N1N O1N3 1.237(2) . ? N1N O1N2 1.246(3) . ? N1N O1N1 1.273(2) . ? N2N O2N2 1.229(3) . ? N2N O2N3 1.249(2) . ? N2N O2N1 1.286(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2N1 Co1 O2N1 180.00(7) 5_565 . ? O2N1 Co1 N2 95.04(7) 5_565 . ? O2N1 Co1 N2 84.96(7) . . ? O2N1 Co1 N2 84.96(7) 5_565 5_565 ? O2N1 Co1 N2 95.04(7) . 5_565 ? N2 Co1 N2 180.0 . 5_565 ? O2N1 Co1 O1N1 98.52(6) 5_565 5_565 ? O2N1 Co1 O1N1 81.48(6) . 5_565 ? N2 Co1 O1N1 84.39(6) . 5_565 ? N2 Co1 O1N1 95.61(6) 5_565 5_565 ? O2N1 Co1 O1N1 81.48(6) 5_565 . ? O2N1 Co1 O1N1 98.52(6) . . ? N2 Co1 O1N1 95.61(6) . . ? N2 Co1 O1N1 84.39(6) 5_565 . ? O1N1 Co1 O1N1 180.00(4) 5_565 . ? N2 C1 C5 111.11(18) . . ? C1 N2 N3 104.85(16) . . ? C1 N2 Co1 130.68(14) . . ? N3 N2 Co1 123.02(12) . . ? C4 N3 N2 112.48(16) . . ? N3 C4 C5 106.97(18) . . ? C4 C5 C1 104.59(17) . . ? C4 C5 C6 127.66(19) . . ? C1 C5 C6 127.55(18) . . ? C11 C6 C7 117.68(18) . . ? C11 C6 C5 121.18(19) . . ? C7 C6 C5 121.08(18) . . ? C8 C7 C6 119.63(19) . . ? N9 C8 C7 120.5(2) . . ? C10 N9 C8 121.91(19) . . ? N9 C10 C11 119.99(19) . . ? C10 C11 C6 120.3(2) . . ? O1N3 N1N O1N2 120.40(18) . . ? O1N3 N1N O1N1 118.83(19) . . ? O1N2 N1N O1N1 120.76(16) . . ? N1N O1N1 Co1 129.83(14) . . ? O2N2 N2N O2N3 121.20(17) . . ? O2N2 N2N O2N1 119.14(17) . . ? O2N3 N2N O2N1 119.66(18) . . ? N2N O2N1 Co1 127.93(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O1N2 0.88 1.93 2.741(2) 153.1 . N3 H3 O2N2 0.88 2.65 3.223(2) 124.0 2 N9 H9 O2N3 0.88 1.94 2.800(2) 163.5 2_545 N9 H9 O2N2 0.88 2.50 3.191(2) 135.9 2_545 _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 1.284 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.108