# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Wei Sun' _publ_contact_author_email WSUN@LZB.AC.CN _publ_section_title ; Unexpected formation of a novel organometallic hetero-cation crystal with a rare coordination mode ; loop_ _publ_author_name 'Wei Sun.' 'Fanguo Deng.' 'Bin Hu.' 'Chun-Gu Xia.' # Attachment 'Revised_[bmim]K[Co_CO_4]2.cif' data_c _database_code_depnum_ccdc_archive 'CCDC 654275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H15 Co2 K N2 O8' _chemical_formula_weight 520.26 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' K K 0.2009 0.2494 '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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.579(5) _cell_length_b 8.392(4) _cell_length_c 13.423(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.594(4) _cell_angle_gamma 90.00 _cell_volume 1167.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3433 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 26.19 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 1.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5503 _exptl_absorpt_correction_T_max 0.6725 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8345 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2321 _reflns_number_gt 1933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0462P)^2^+0.1801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2321 _refine_ls_number_parameters 195 _refine_ls_number_restraints 152 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.239 _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 0.71668(4) 0.2500 0.43731(3) 0.05821(15) Uani 1 2 d S . 4 Co2 Co -0.25399(4) 0.2500 -0.03341(3) 0.06001(15) Uani 1 2 d S . 4 K1 K 0.17695(7) 0.2500 0.28233(5) 0.0582(2) Uani 1 2 d SU . 4 C1 C 0.7436(3) 0.0792(4) 0.5128(2) 0.0866(9) Uani 1 1 d U . 4 C2 C 0.8345(4) 0.2500 0.3623(3) 0.0769(11) Uani 1 2 d SU . 4 C3 C 0.5569(4) 0.2500 0.3711(3) 0.0801(11) Uani 1 2 d SU . 4 C4 C -0.1080(4) 0.2500 0.0540(3) 0.0905(14) Uani 1 2 d SU . 4 C5 C -0.3845(4) 0.2500 0.0292(3) 0.0806(11) Uani 1 2 d SU . 4 C6 C -0.2597(3) 0.0809(4) -0.1100(2) 0.0901(9) Uani 1 1 d U . 4 O1 O 0.7613(3) -0.0331(4) 0.5625(2) 0.1400(11) Uani 1 1 d U . 4 O2 O 0.9166(4) 0.2500 0.3180(3) 0.1284(13) Uani 1 2 d SU . 4 O3 O 0.4498(3) 0.2500 0.3303(3) 0.1183(12) Uani 1 2 d SU . 4 O4 O -0.0091(3) 0.2500 0.1086(3) 0.1354(15) Uani 1 2 d SU . 4 O5 O -0.4689(4) 0.2500 0.0707(3) 0.1440(16) Uani 1 2 d SU . 4 O6 O -0.2605(3) -0.0286(4) -0.1616(2) 0.1410(11) Uani 1 1 d U . 4 N1 N 0.5621(3) 0.7303(10) 0.2703(2) 0.0718(13) Uani 0.50 1 d PDU A -1 N2 N 0.6879(3) 0.7650(10) 0.1654(2) 0.0713(11) Uani 0.50 1 d PDU A -1 C7 C 0.6308(4) 0.8367(7) 0.2317(4) 0.0791(15) Uani 0.50 1 d PDU A -1 H7 H 0.6378 0.9443 0.2486 0.095 Uiso 0.50 1 calc PR A -1 C8 C 0.5787(5) 0.5883(7) 0.2254(4) 0.0818(16) Uani 0.50 1 d PDU A -1 H8 H 0.5416 0.4920 0.2384 0.098 Uiso 0.50 1 calc PR A -1 C9 C 0.6552(5) 0.6093(7) 0.1608(4) 0.0807(14) Uani 0.50 1 d PDU A -1 H9 H 0.6819 0.5319 0.1199 0.097 Uiso 0.50 1 calc PR A -1 C10 C 0.4846(5) 0.769(3) 0.3468(4) 0.125(3) Uani 0.50 1 d PDU A -1 H10A H 0.5210 0.7179 0.4099 0.187 Uiso 0.50 1 calc PR A -1 H10B H 0.3976 0.7331 0.3235 0.187 Uiso 0.50 1 calc PR A -1 H10C H 0.4847 0.8827 0.3568 0.187 Uiso 0.50 1 calc PR A -1 C11 C 0.7738(6) 0.8414(9) 0.1069(5) 0.128(2) Uani 0.50 1 d PDU A -1 H11A H 0.7480 0.8106 0.0360 0.154 Uiso 0.50 1 calc PR A -1 H11B H 0.7647 0.9561 0.1108 0.154 Uiso 0.50 1 calc PR A -1 C12 C 0.9088(7) 0.7985(15) 0.1434(6) 0.168(3) Uani 0.50 1 d PDU A -1 H12A H 0.9163 0.6879 0.1245 0.202 Uiso 0.50 1 calc PR A -1 H12B H 0.9574 0.8599 0.1028 0.202 Uiso 0.50 1 calc PR A -1 C13 C 0.9787(8) 0.8119(13) 0.2472(7) 0.164(4) Uani 0.50 1 d PDU A -1 H13A H 0.9683 0.9202 0.2696 0.196 Uiso 0.50 1 calc PR A -1 H13B H 1.0697 0.7974 0.2470 0.196 Uiso 0.50 1 calc PR A -1 C14 C 0.9437(9) 0.6988(17) 0.3273(8) 0.205(6) Uani 0.50 1 d PDU A -1 H14A H 0.8763 0.7454 0.3561 0.307 Uiso 0.5 1 calc pR A -1 H14B H 1.0183 0.6812 0.3801 0.307 Uiso 0.50 1 calc PR A -1 H14C H 0.9146 0.5990 0.2959 0.307 Uiso 0.50 1 calc PR A -1 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 0.0484(3) 0.0764(3) 0.0491(2) 0.000 0.00812(19) 0.000 Co2 0.0543(3) 0.0752(3) 0.0481(2) 0.000 0.00439(19) 0.000 K1 0.0540(4) 0.0690(5) 0.0488(4) 0.000 0.0033(3) 0.000 C1 0.0796(18) 0.109(2) 0.0695(16) 0.0180(17) 0.0114(14) -0.0011(17) C2 0.074(2) 0.084(3) 0.078(2) 0.000 0.028(2) 0.000 C3 0.057(2) 0.103(3) 0.076(2) 0.000 0.0032(19) 0.000 C4 0.069(2) 0.140(4) 0.056(2) 0.000 -0.0005(19) 0.000 C5 0.082(3) 0.090(3) 0.074(2) 0.000 0.024(2) 0.000 C6 0.0766(17) 0.114(3) 0.0751(17) -0.0222(18) 0.0056(14) 0.0181(18) O1 0.158(2) 0.132(2) 0.126(2) 0.0676(19) 0.0192(19) 0.0038(19) O2 0.113(3) 0.158(3) 0.137(3) 0.000 0.081(2) 0.000 O3 0.0595(17) 0.155(3) 0.127(3) 0.000 -0.0130(18) 0.000 O4 0.082(2) 0.222(4) 0.084(2) 0.000 -0.0251(18) 0.000 O5 0.120(3) 0.195(4) 0.137(3) 0.000 0.074(3) 0.000 O6 0.137(2) 0.152(2) 0.129(2) -0.076(2) 0.0139(17) 0.0258(19) N1 0.0585(18) 0.096(4) 0.0621(18) 0.000(3) 0.0149(15) 0.004(3) N2 0.081(2) 0.070(3) 0.0680(18) 0.013(3) 0.0268(16) 0.007(4) C7 0.076(4) 0.070(3) 0.090(4) -0.005(3) 0.014(3) 0.011(3) C8 0.068(3) 0.075(4) 0.099(4) 0.017(3) 0.009(3) -0.005(3) C9 0.078(3) 0.076(3) 0.089(4) -0.013(3) 0.019(3) -0.002(3) C10 0.088(3) 0.203(10) 0.094(3) 0.001(9) 0.043(3) -0.003(10) C11 0.136(4) 0.138(5) 0.131(5) 0.028(4) 0.072(4) -0.018(4) C12 0.139(5) 0.192(9) 0.202(6) 0.022(6) 0.105(5) -0.016(6) C13 0.117(5) 0.203(10) 0.194(7) -0.022(6) 0.086(5) -0.013(6) C14 0.104(6) 0.222(16) 0.262(9) 0.073(9) -0.027(7) -0.015(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C3 1.744(4) . ? Co1 C1 1.745(3) . ? Co1 C1 1.745(3) 4_565 ? Co1 C2 1.753(4) . ? Co2 C4 1.742(4) . ? Co2 C6 1.747(3) 4_565 ? Co2 C6 1.747(3) . ? Co2 C5 1.755(4) . ? K1 O6 2.727(3) 2 ? K1 O6 2.727(3) 3 ? K1 O4 2.732(3) . ? K1 O1 2.745(3) 2_656 ? K1 O1 2.745(3) 3_656 ? K1 O3 2.828(3) . ? K1 O2 2.889(4) 1_455 ? C1 O1 1.148(4) . ? C2 O2 1.147(5) . ? C3 O3 1.156(5) . ? C4 O4 1.150(5) . ? C5 O5 1.143(5) . ? C6 O6 1.149(4) . ? O1 K1 2.744(3) 3_656 ? O2 K1 2.889(4) 1_655 ? O6 K1 2.727(3) 3 ? N1 C7 1.322(7) . ? N1 C8 1.362(8) . ? N1 C10 1.473(7) . ? N2 C7 1.317(7) . ? N2 C9 1.350(9) . ? N2 C11 1.463(7) . ? C7 H7 0.9300 . ? C8 C9 1.311(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.459(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.444(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.535(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 C3 Co1 C1 108.91(12) . . ? C3 Co1 C1 108.91(12) . 4_565 ? C1 Co1 C1 110.4(2) . 4_565 ? C3 Co1 C2 115.8(2) . . ? C1 Co1 C2 106.38(13) . . ? C1 Co1 C2 106.38(13) 4_565 . ? C4 Co2 C6 108.53(12) . 4_565 ? C4 Co2 C6 108.53(12) . . ? C6 Co2 C6 108.7(2) 4_565 . ? C4 Co2 C5 110.7(2) . . ? C6 Co2 C5 110.18(13) 4_565 . ? C6 Co2 C5 110.18(13) . . ? O6 K1 O6 85.90(15) 2 3 ? O6 K1 O4 75.91(9) 2 . ? O6 K1 O4 75.91(9) 3 . ? O6 K1 O1 86.75(10) 2 2_656 ? O6 K1 O1 147.88(9) 3 2_656 ? O4 K1 O1 131.95(8) . 2_656 ? O6 K1 O1 147.88(9) 2 3_656 ? O6 K1 O1 86.75(10) 3 3_656 ? O4 K1 O1 131.95(8) . 3_656 ? O1 K1 O1 83.09(15) 2_656 3_656 ? O6 K1 O3 72.40(9) 2 . ? O6 K1 O3 72.40(9) 3 . ? O4 K1 O3 136.18(12) . . ? O1 K1 O3 75.57(9) 2_656 . ? O1 K1 O3 75.57(9) 3_656 . ? O6 K1 O2 122.15(9) 2 1_455 ? O6 K1 O2 122.15(9) 3 1_455 ? O4 K1 O2 66.07(12) . 1_455 ? O1 K1 O2 87.91(9) 2_656 1_455 ? O1 K1 O2 87.91(9) 3_656 1_455 ? O3 K1 O2 157.76(12) . 1_455 ? O1 C1 Co1 180.0(5) . . ? O2 C2 Co1 176.2(4) . . ? O3 C3 Co1 177.7(4) . . ? O4 C4 Co2 177.3(4) . . ? O5 C5 Co2 179.5(4) . . ? O6 C6 Co2 178.0(3) . . ? C1 O1 K1 166.3(3) . 3_656 ? C2 O2 K1 158.9(4) . 1_655 ? C3 O3 K1 165.2(4) . . ? C4 O4 K1 161.9(4) . . ? C6 O6 K1 159.8(3) . 3 ? C7 N1 C8 106.7(5) . . ? C7 N1 C10 123.3(10) . . ? C8 N1 C10 130.0(10) . . ? C7 N2 C9 109.0(5) . . ? C7 N2 C11 125.5(8) . . ? C9 N2 C11 125.5(6) . . ? N2 C7 N1 108.6(6) . . ? N2 C7 H7 125.7 . . ? N1 C7 H7 125.7 . . ? C9 C8 N1 109.1(5) . . ? C9 C8 H8 125.5 . . ? N1 C8 H8 125.5 . . ? C8 C9 N2 106.6(5) . . ? C8 C9 H9 126.7 . . ? N2 C9 H9 126.7 . . ? C12 C11 N2 112.5(5) . . ? C12 C11 H11A 109.1 . . ? N2 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? N2 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 125.6(8) . . ? C13 C12 H12A 105.9 . . ? C11 C12 H12A 105.9 . . ? C13 C12 H12B 105.9 . . ? C11 C12 H12B 105.9 . . ? H12A C12 H12B 106.2 . . ? C12 C13 C14 118.6(9) . . ? C12 C13 H13A 107.7 . . ? C14 C13 H13A 107.7 . . ? C12 C13 H13B 107.7 . . ? C14 C13 H13B 107.7 . . ? H13A C13 H13B 107.1 . . ? 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 C3 Co1 C1 O1 -171(100) . . . . ? C1 Co1 C1 O1 -52(100) 4_565 . . . ? C2 Co1 C1 O1 63(100) . . . . ? C3 Co1 C2 O2 180.000(11) . . . . ? C1 Co1 C2 O2 -58.86(12) . . . . ? C1 Co1 C2 O2 58.86(12) 4_565 . . . ? C1 Co1 C3 O3 60.23(12) . . . . ? C1 Co1 C3 O3 -60.23(12) 4_565 . . . ? C2 Co1 C3 O3 180.000(13) . . . . ? C6 Co2 C4 O4 -58.97(13) 4_565 . . . ? C6 Co2 C4 O4 58.97(13) . . . . ? C5 Co2 C4 O4 180.000(3) . . . . ? C4 Co2 C5 O5 0.002(13) . . . . ? C6 Co2 C5 O5 -120.04(12) 4_565 . . . ? C6 Co2 C5 O5 120.04(12) . . . . ? C4 Co2 C6 O6 -65(9) . . . . ? C6 Co2 C6 O6 53(9) 4_565 . . . ? C5 Co2 C6 O6 173(9) . . . . ? Co1 C1 O1 K1 46(100) . . . 3_656 ? Co1 C2 O2 K1 0.001(12) . . . 1_655 ? Co1 C3 O3 K1 0.000(15) . . . . ? O6 K1 O3 C3 134.37(8) 2 . . . ? O6 K1 O3 C3 -134.37(8) 3 . . . ? O4 K1 O3 C3 180.000(2) . . . . ? O1 K1 O3 C3 43.22(8) 2_656 . . . ? O1 K1 O3 C3 -43.22(8) 3_656 . . . ? O2 K1 O3 C3 -0.001(2) 1_455 . . . ? Co2 C4 O4 K1 180.000(3) . . . . ? O6 K1 O4 C4 -135.37(8) 2 . . . ? O6 K1 O4 C4 135.37(8) 3 . . . ? O1 K1 O4 C4 -63.09(12) 2_656 . . . ? O1 K1 O4 C4 63.09(12) 3_656 . . . ? O3 K1 O4 C4 180.0 . . . . ? O2 K1 O4 C4 0.0 1_455 . . . ? Co2 C6 O6 K1 20(10) . . . 3 ? C9 N2 C7 N1 0.1(3) . . . . ? C11 N2 C7 N1 -179.4(3) . . . . ? C8 N1 C7 N2 0.1(3) . . . . ? C10 N1 C7 N2 -179.6(3) . . . . ? C7 N1 C8 C9 -0.3(4) . . . . ? C10 N1 C8 C9 179.4(4) . . . . ? N1 C8 C9 N2 0.4(5) . . . . ? C7 N2 C9 C8 -0.3(4) . . . . ? C11 N2 C9 C8 179.2(4) . . . . ? C7 N2 C11 C12 106.5(8) . . . . ? C9 N2 C11 C12 -72.9(8) . . . . ? N2 C11 C12 C13 -52.8(15) . . . . ? C11 C12 C13 C14 69.6(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.232 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.059 # Attachment 'Revised_[C4Py]K[Co_CO_4]2.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 692197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Co4 K2 N2 O16' _chemical_formula_weight 1034.50 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' K K 0.2009 0.2494 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.318(7) _cell_length_b 8.633(6) _cell_length_c 13.110(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.219(8) _cell_angle_gamma 90.00 _cell_volume 1155.8(14) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2082 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6934 _exptl_absorpt_correction_T_max 0.7574 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8890 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2303 _reflns_number_gt 1624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0722P)^2^+0.5666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2303 _refine_ls_number_parameters 172 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.110 _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 1.21945(8) 0.2500 0.45348(6) 0.0610(3) Uani 1 2 d S . 1 Co2 Co 0.24354(8) 0.2500 -0.02374(6) 0.0668(3) Uani 1 2 d S . 1 K3 K 0.68429(13) 0.2500 0.27736(10) 0.0637(4) Uani 1 2 d SU . 1 O1 O 1.2664(6) -0.0261(7) 0.5782(4) 0.161(2) Uani 1 1 d . . 1 O2 O 0.9539(6) 0.2500 0.3438(6) 0.132(2) Uani 1 2 d SU . 1 O3 O 1.4258(7) 0.2500 0.3260(6) 0.146(3) Uani 1 2 d S . 1 O4 O 0.4928(6) 0.2500 0.1092(5) 0.157(3) Uani 1 2 d SU . 1 O5 O 0.0177(8) 0.2500 0.0814(6) 0.147(3) Uani 1 2 d S . 1 O6 O 0.2404(5) -0.0230(6) -0.1531(4) 0.1407(19) Uani 1 1 d . . 1 C1 C 1.2458(5) 0.0839(9) 0.5287(4) 0.0987(19) Uani 1 1 d . . 1 C2 C 1.0601(7) 0.2500 0.3874(6) 0.085(2) Uani 1 2 d SU . 1 C3 C 1.3410(8) 0.2500 0.3734(6) 0.081(2) Uani 1 2 d S . 1 C4 C 0.3902(8) 0.2500 0.0597(6) 0.100(3) Uani 1 2 d SU . 1 C5 C 0.1083(8) 0.2500 0.0416(6) 0.0780(19) Uani 1 2 d S . 1 C6 C 0.2409(5) 0.0854(8) -0.1015(4) 0.0943(17) Uani 1 1 d . . 1 C7 C 0.8732(6) 0.3745(8) 0.7566(5) 0.099(3) Uani 0.50 1 d PGU A -1 H7 H 0.8507 0.4788 0.7565 0.119 Uiso 0.50 1 calc PR A -1 C8 C 0.9535(6) 0.3207(12) 0.6905(5) 0.107(3) Uani 0.50 1 d PGU A -1 H8 H 0.9859 0.3884 0.6451 0.129 Uiso 0.50 1 calc PR A -1 C9 C 0.9860(6) 0.1686(13) 0.6907(5) 0.109(3) Uani 0.50 1 d PGU A -1 H9 H 1.0406 0.1320 0.6454 0.131 Uiso 0.50 1 calc PR A -1 C10 C 0.9388(6) 0.0693(10) 0.7573(5) 0.093(3) Uani 0.50 1 d PGU A -1 H10 H 0.9611 -0.0351 0.7575 0.112 Uiso 0.50 1 calc PR A -1 C11 C 0.8591(5) 0.1229(7) 0.8234(4) 0.077(3) Uani 0.50 1 d PGU A -1 H11 H 0.8270 0.0553 0.8690 0.093 Uiso 0.50 1 calc PR A -1 C12 C 0.7410(7) 0.3311(9) 0.8922(5) 0.124(3) Uani 0.50 1 d PGU A -1 H12A H 0.7590 0.4401 0.9056 0.149 Uiso 0.50 1 calc PR A -1 H12B H 0.7595 0.2761 0.9571 0.149 Uiso 0.50 1 calc PR A -1 C13 C 0.6001(7) 0.3118(10) 0.8505(6) 0.152(4) Uani 0.50 1 d PGU A -1 H13A H 0.5695 0.4139 0.8275 0.182 Uiso 0.50 1 calc PR A -1 H13B H 0.5567 0.2875 0.9095 0.182 Uiso 0.50 1 calc PR A -1 C14 C 0.5429(6) 0.2007(11) 0.7658(7) 0.158(5) Uani 0.50 1 d PGU A -1 H14A H 0.5614 0.0974 0.7932 0.190 Uiso 0.50 1 calc PR A -1 H14B H 0.4486 0.2134 0.7591 0.190 Uiso 0.50 1 calc PR A -1 C15 C 0.5752(6) 0.1978(13) 0.6590(7) 0.178(8) Uani 0.50 1 d PGU A -1 H15A H 0.5350 0.2849 0.6213 0.267 Uiso 0.50 1 calc PR A -1 H15B H 0.5429 0.1036 0.6256 0.267 Uiso 0.50 1 calc PR A -1 H15C H 0.6684 0.2031 0.6609 0.267 Uiso 0.50 1 calc PR A -1 N1 N 0.8264(4) 0.2745(7) 0.8228(3) 0.080(2) Uani 0.50 1 d PGU A -1 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 0.0488(5) 0.0803(6) 0.0531(5) 0.000 0.0047(4) 0.000 Co2 0.0570(5) 0.0909(7) 0.0497(5) 0.000 -0.0018(4) 0.000 K3 0.0564(8) 0.0800(10) 0.0519(7) 0.000 -0.0016(6) 0.000 O1 0.169(5) 0.156(5) 0.156(5) 0.093(4) 0.014(4) 0.001(4) O2 0.062(3) 0.156(6) 0.165(6) 0.000 -0.027(4) 0.000 O3 0.115(5) 0.208(8) 0.134(5) 0.000 0.078(5) 0.000 O4 0.085(4) 0.279(10) 0.094(4) 0.000 -0.033(3) 0.000 O5 0.126(6) 0.167(7) 0.164(7) 0.000 0.079(5) 0.000 O6 0.129(4) 0.158(5) 0.132(4) -0.073(4) 0.009(3) 0.020(3) C1 0.078(4) 0.131(5) 0.086(4) 0.027(4) 0.008(3) -0.010(3) C2 0.062(4) 0.096(6) 0.094(5) 0.000 0.000(4) 0.000 C3 0.077(5) 0.086(5) 0.083(5) 0.000 0.019(4) 0.000 C4 0.083(5) 0.153(8) 0.058(4) 0.000 -0.009(4) 0.000 C5 0.078(5) 0.081(5) 0.079(5) 0.000 0.021(4) 0.000 C6 0.077(3) 0.129(5) 0.075(3) -0.022(4) 0.002(3) 0.010(3) C7 0.089(6) 0.089(6) 0.118(7) 0.008(6) 0.009(6) 0.000(5) C8 0.077(6) 0.126(7) 0.124(6) 0.026(7) 0.029(5) -0.008(6) C9 0.078(6) 0.138(7) 0.114(6) 0.002(8) 0.026(5) 0.014(6) C10 0.075(6) 0.106(7) 0.097(6) -0.003(6) 0.005(5) 0.010(5) C11 0.085(5) 0.077(6) 0.070(5) -0.004(5) 0.010(5) 0.010(5) C12 0.145(7) 0.125(7) 0.107(6) -0.028(6) 0.031(6) 0.032(6) C13 0.152(8) 0.168(10) 0.150(8) -0.046(6) 0.078(7) 0.003(7) C14 0.131(8) 0.187(12) 0.170(10) -0.038(8) 0.067(8) -0.024(8) C15 0.114(10) 0.188(19) 0.215(14) -0.026(13) -0.029(10) -0.018(10) N1 0.093(4) 0.077(5) 0.070(3) -0.013(4) 0.014(3) 0.010(4) _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 C1 1.740(7) 4_565 ? Co1 C1 1.740(7) . ? Co1 C2 1.745(7) . ? Co1 C3 1.747(8) . ? Co2 C4 1.736(8) . ? Co2 C5 1.739(8) . ? Co2 C6 1.746(7) . ? Co2 C6 1.746(7) 4_565 ? K3 O1 2.703(5) 2_756 ? K3 O1 2.703(5) 3_756 ? K3 O6 2.731(5) 3_655 ? K3 O6 2.731(5) 2_655 ? K3 O4 2.742(6) . ? K3 O2 2.794(6) . ? K3 O3 2.829(7) 1_455 ? O1 C1 1.153(7) . ? O1 K3 2.703(5) 3_756 ? O2 C2 1.161(8) . ? O3 C3 1.143(9) . ? O3 K3 2.829(7) 1_655 ? O4 C4 1.160(9) . ? O5 C5 1.133(9) . ? O6 C6 1.155(7) . ? O6 K3 2.731(5) 3_655 ? C7 N1 1.361(3) . ? C7 C8 1.363(3) . ? C7 H7 0.9300 . ? C8 C9 1.355(3) . ? C8 H8 0.9300 . ? C9 C10 1.362(3) . ? C9 H9 0.9300 . ? C10 C11 1.359(3) . ? C10 H10 0.9300 . ? C11 N1 1.351(3) . ? C11 H11 0.9300 . ? C12 N1 1.439(3) . ? C12 C13 1.487(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.522(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.486(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 C1 Co1 C1 111.1(4) 4_565 . ? C1 Co1 C2 109.9(2) 4_565 . ? C1 Co1 C2 109.9(2) . . ? C1 Co1 C3 105.8(2) 4_565 . ? C1 Co1 C3 105.8(2) . . ? C2 Co1 C3 114.1(4) . . ? C4 Co2 C5 112.2(4) . . ? C4 Co2 C6 107.9(2) . . ? C5 Co2 C6 109.9(2) . . ? C4 Co2 C6 107.9(2) . 4_565 ? C5 Co2 C6 109.9(2) . 4_565 ? C6 Co2 C6 108.9(4) . 4_565 ? O1 K3 O1 91.3(3) 2_756 3_756 ? O1 K3 O6 152.86(17) 2_756 3_655 ? O1 K3 O6 82.16(19) 3_756 3_655 ? O1 K3 O6 82.16(19) 2_756 2_655 ? O1 K3 O6 152.86(17) 3_756 2_655 ? O6 K3 O6 91.7(3) 3_655 2_655 ? O1 K3 O4 127.23(15) 2_756 . ? O1 K3 O4 127.23(15) 3_756 . ? O6 K3 O4 75.79(16) 3_655 . ? O6 K3 O4 75.79(16) 2_655 . ? O1 K3 O2 72.69(16) 2_756 . ? O1 K3 O2 72.69(16) 3_756 . ? O6 K3 O2 80.23(16) 3_655 . ? O6 K3 O2 80.23(16) 2_655 . ? O4 K3 O2 145.3(2) . . ? O1 K3 O3 86.04(17) 2_756 1_455 ? O1 K3 O3 86.04(17) 3_756 1_455 ? O6 K3 O3 119.49(15) 3_655 1_455 ? O6 K3 O3 119.49(15) 2_655 1_455 ? O4 K3 O3 65.6(2) . 1_455 ? O2 K3 O3 149.1(2) . 1_455 ? C1 O1 K3 170.0(6) . 3_756 ? C2 O2 K3 168.8(7) . . ? C3 O3 K3 160.4(7) . 1_655 ? C4 O4 K3 160.9(7) . . ? C6 O6 K3 162.4(5) . 3_655 ? O1 C1 Co1 178.3(6) . . ? O2 C2 Co1 179.8(8) . . ? O3 C3 Co1 176.0(8) . . ? O4 C4 Co2 175.0(8) . . ? O5 C5 Co2 177.8(8) . . ? O6 C6 Co2 179.3(6) . . ? N1 C7 C8 119.5 . . ? N1 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.1 . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.9 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? N1 C11 C10 120.0 . . ? N1 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? N1 C12 C13 112.6 . . ? N1 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 126.6 . . ? C12 C13 H13A 105.7 . . ? C14 C13 H13A 105.7 . . ? C12 C13 H13B 105.7 . . ? C14 C13 H13B 105.7 . . ? H13A C13 H13B 106.1 . . ? C15 C14 C13 125.6 . . ? C15 C14 H14A 105.9 . . ? C13 C14 H14A 105.9 . . ? C15 C14 H14B 105.9 . . ? C13 C14 H14B 105.9 . . ? H14A C14 H14B 106.2 . . ? C11 N1 C7 120.5 . . ? C11 N1 C12 120.0 . . ? C7 N1 C12 119.5 . . ? 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 O1 K3 O2 C2 48.51(15) 2_756 . . . ? O1 K3 O2 C2 -48.51(15) 3_756 . . . ? O6 K3 O2 C2 -133.27(13) 3_655 . . . ? O6 K3 O2 C2 133.27(13) 2_655 . . . ? O4 K3 O2 C2 180.000(5) . . . . ? O3 K3 O2 C2 0.000(5) 1_455 . . . ? O1 K3 O4 C4 -63.9(2) 2_756 . . . ? O1 K3 O4 C4 63.9(2) 3_756 . . . ? O6 K3 O4 C4 132.25(14) 3_655 . . . ? O6 K3 O4 C4 -132.25(14) 2_655 . . . ? O2 K3 O4 C4 180.0 . . . . ? O3 K3 O4 C4 0.0 1_455 . . . ? K3 O1 C1 Co1 100(22) 3_756 . . . ? C1 Co1 C1 O1 -89(23) 4_565 . . . ? C2 Co1 C1 O1 150(23) . . . . ? C3 Co1 C1 O1 26(23) . . . . ? K3 O2 C2 Co1 0(100) . . . . ? C1 Co1 C2 O2 -61(100) 4_565 . . . ? C1 Co1 C2 O2 61(100) . . . . ? C3 Co1 C2 O2 180(100) . . . . ? K3 O3 C3 Co1 0.000(16) 1_655 . . . ? C1 Co1 C3 O3 59.0(2) 4_565 . . . ? C1 Co1 C3 O3 -59.0(2) . . . . ? C2 Co1 C3 O3 180.000(18) . . . . ? K3 O4 C4 Co2 180.000(3) . . . . ? C5 Co2 C4 O4 180.000(3) . . . . ? C6 Co2 C4 O4 58.8(2) . . . . ? C6 Co2 C4 O4 -58.8(2) 4_565 . . . ? C4 Co2 C5 O5 180.000(9) . . . . ? C6 Co2 C5 O5 -59.9(2) . . . . ? C6 Co2 C5 O5 59.9(2) 4_565 . . . ? K3 O6 C6 Co2 8(55) 3_655 . . . ? C4 Co2 C6 O6 -53(54) . . . . ? C5 Co2 C6 O6 -175(100) . . . . ? C6 Co2 C6 O6 64(54) 4_565 . . . ? N1 C7 C8 C9 0.1 . . . . ? C7 C8 C9 C10 -0.1 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 N1 0.2 . . . . ? N1 C12 C13 C14 20.2 . . . . ? C12 C13 C14 C15 -58.8 . . . . ? C10 C11 N1 C7 -0.3 . . . . ? C10 C11 N1 C12 179.4 . . . . ? C8 C7 N1 C11 0.1 . . . . ? C8 C7 N1 C12 -179.6 . . . . ? C13 C12 N1 C11 -85.1 . . . . ? C13 C12 N1 C7 94.7 . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.574 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.064