Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal SOciety of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Zhan Shi' _publ_contact_author_email ZSHI@MAIL.JLU.EDU.CN _publ_section_title ; Towards Rational Design of Metal-Organic Frameworks with Helical Units in Mixed Ligand System ; loop_ _publ_author_name 'Zhan Shi.' 'Minghui Bi.' 'Shouhua Feng.' 'Lu Gao.' 'Yawei Hu.' 'Guanghua Li.' ; Xiaomin Liu ; # Attachment 'compound1.CIF' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 672250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C27 H22 Co N2 O5' _chemical_formula_sum 'C27 H22 Co N2 O5' _chemical_formula_weight 513.40 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' 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 P2(1)/n _symmetry_space_group_name_Hall -P2yn 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 9.7103(11) _cell_length_b 10.0679(11) _cell_length_c 24.245(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.852(2) _cell_angle_gamma 90.00 _cell_volume 2370.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5859 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8143 _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 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16582 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5859 _reflns_number_gt 3686 _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 SHELXP-97 _computing_publication_material 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^)+(0.0527P)^2^+2.5431P] 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 5859 _refine_ls_number_parameters 316 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.030 _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 -0.07733(4) 0.61379(4) 0.505582(16) 0.03090(14) Uani 1 1 d . . . O1 O -0.1504(2) 0.3135(3) 0.82510(9) 0.0499(7) Uani 1 1 d . . . O2 O -0.1056(2) 0.5408(3) 0.58340(8) 0.0414(6) Uani 1 1 d . . . O3 O 0.0208(3) 0.3569(3) 0.57389(9) 0.0446(6) Uani 1 1 d . . . O4 O 0.3825(2) 0.1611(3) 0.96608(9) 0.0446(6) Uani 1 1 d . . . O5 O 0.2502(2) -0.0178(3) 0.97870(10) 0.0462(6) Uani 1 1 d . . . N1 N -0.1505(3) 0.8017(3) 0.52019(10) 0.0360(6) Uani 1 1 d . . . N2 N -0.6426(5) 1.4105(5) 0.7821(2) 0.0934(14) Uani 1 1 d U . . C1 C -0.1206(3) 0.3399(4) 0.77043(12) 0.0394(8) Uani 1 1 d . . . C2 C -0.1778(4) 0.4535(4) 0.74808(13) 0.0465(9) Uani 1 1 d . . . H2 H -0.2308 0.5094 0.7697 0.080 Uiso 1 1 calc . . . C3 C -0.1556(4) 0.4837(4) 0.69339(13) 0.0433(9) Uani 1 1 d . . . H3 H -0.1931 0.5608 0.6783 0.080 Uiso 1 1 calc . . . C4 C -0.0774(3) 0.3994(3) 0.66052(12) 0.0344(7) Uani 1 1 d . . . C5 C -0.0241(4) 0.2845(4) 0.68369(13) 0.0419(8) Uani 1 1 d . . . H5 H 0.0271 0.2269 0.6621 0.080 Uiso 1 1 calc . . . C6 C -0.0458(4) 0.2539(4) 0.73852(14) 0.0469(9) Uani 1 1 d . . . H6 H -0.0102 0.1760 0.7536 0.080 Uiso 1 1 calc . . . C7 C -0.0519(3) 0.4350(4) 0.60163(12) 0.0352(7) Uani 1 1 d . . . C8 C -0.0447(3) 0.2657(4) 0.85916(12) 0.0368(8) Uani 1 1 d . . . C9 C -0.0802(3) 0.1744(4) 0.89856(12) 0.0359(7) Uani 1 1 d . . . H9 H -0.1713 0.1477 0.9023 0.080 Uiso 1 1 calc . . . C10 C 0.0224(3) 0.1228(3) 0.93260(12) 0.0345(7) Uani 1 1 d . . . H10 H -0.0003 0.0602 0.9592 0.080 Uiso 1 1 calc . . . C11 C 0.1578(3) 0.1626(3) 0.92781(12) 0.0316(7) Uani 1 1 d . . . C12 C 0.1894(3) 0.2599(4) 0.88965(13) 0.0398(8) Uani 1 1 d . . . H12 H 0.2794 0.2907 0.8873 0.080 Uiso 1 1 calc . . . C13 C 0.0883(4) 0.3119(4) 0.85486(14) 0.0424(8) Uani 1 1 d . . . H13 H 0.1099 0.3768 0.8291 0.080 Uiso 1 1 calc . . . C14 C 0.2711(3) 0.0977(4) 0.96048(12) 0.0356(7) Uani 1 1 d . . . C15 C -0.2456(5) 0.8570(4) 0.48835(16) 0.0581(11) Uani 1 1 d . . . H15 H -0.2737 0.8118 0.4567 0.080 Uiso 1 1 calc . . . C16 C -0.3053(5) 0.9773(5) 0.49914(17) 0.0644(13) Uani 1 1 d . . . H16 H -0.3716 1.0113 0.4749 0.080 Uiso 1 1 calc . . . C17 C -0.2681(4) 1.0482(4) 0.54558(14) 0.0460(9) Uani 1 1 d . . . C18 C -0.1680(5) 0.9906(5) 0.57830(18) 0.0657(13) Uani 1 1 d . . . H18 H -0.1374 1.0342 0.6100 0.080 Uiso 1 1 calc . . . C19 C -0.1127(4) 0.8699(4) 0.56493(17) 0.0595(12) Uani 1 1 d . . . H19 H -0.0456 0.8339 0.5882 0.080 Uiso 1 1 calc . . . C20 C -0.3345(5) 1.1781(4) 0.55962(16) 0.0548(10) Uani 1 1 d . . . H20A H -0.4027 1.1989 0.5313 0.080 Uiso 1 1 calc . . . H20B H -0.2650 1.2472 0.5590 0.080 Uiso 1 1 calc . . . C21 C -0.4042(5) 1.1806(4) 0.61566(17) 0.0569(11) Uani 1 1 d . . . H21A H -0.4716 1.1096 0.6174 0.080 Uiso 1 1 calc . . . H21B H -0.3359 1.1658 0.6446 0.080 Uiso 1 1 calc . . . C22 C -0.4745(5) 1.3122(4) 0.62488(17) 0.0596(11) Uani 1 1 d . . . H22A H -0.4076 1.3818 0.6185 0.080 Uiso 1 1 calc . . . H22B H -0.5465 1.3216 0.5970 0.080 Uiso 1 1 calc . . . C23 C -0.6931(7) 1.4530(7) 0.7372(3) 0.0991(18) Uani 1 1 d U . . H23 H -0.7669 1.5116 0.7394 0.080 Uiso 1 1 calc . . . C24 C -0.6481(6) 1.4198(6) 0.6849(2) 0.0874(16) Uani 1 1 d U . . H24 H -0.6927 1.4534 0.6537 0.080 Uiso 1 1 calc . . . C25 C -0.5372(4) 1.3367(4) 0.67990(18) 0.0563(10) Uani 1 1 d . . . C26 C -0.4852(6) 1.2869(6) 0.7283(2) 0.0863(16) Uani 1 1 d U . . H26 H -0.4128 1.2264 0.7280 0.080 Uiso 1 1 calc . . . C27 C -0.5411(7) 1.3272(7) 0.7781(3) 0.106(2) Uani 1 1 d U . . H27 H -0.5035 1.2924 0.8105 0.080 Uiso 1 1 calc . . . 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 0.0306(2) 0.0402(3) 0.0218(2) -0.00150(19) -0.00316(15) 0.0056(2) O1 0.0355(13) 0.089(2) 0.0253(11) 0.0197(12) 0.0026(9) 0.0147(13) O2 0.0422(14) 0.0561(16) 0.0259(11) 0.0086(11) 0.0013(9) 0.0100(12) O3 0.0528(15) 0.0579(16) 0.0230(11) 0.0023(11) 0.0050(10) 0.0100(13) O4 0.0311(13) 0.0611(16) 0.0412(13) 0.0018(12) -0.0111(10) -0.0013(12) O5 0.0413(14) 0.0560(17) 0.0412(13) 0.0143(12) -0.0063(10) 0.0022(12) N1 0.0382(16) 0.0400(16) 0.0298(13) 0.0000(12) -0.0026(11) 0.0045(13) N2 0.0926(16) 0.0945(16) 0.0931(16) -0.0035(10) 0.0068(10) -0.0003(10) C1 0.0340(17) 0.062(2) 0.0224(14) 0.0095(15) -0.0023(13) 0.0047(16) C2 0.051(2) 0.062(2) 0.0271(16) 0.0040(16) 0.0030(15) 0.0183(19) C3 0.053(2) 0.050(2) 0.0263(15) 0.0062(15) -0.0013(14) 0.0142(18) C4 0.0342(17) 0.047(2) 0.0214(14) 0.0017(14) -0.0040(12) 0.0023(15) C5 0.045(2) 0.050(2) 0.0305(16) 0.0019(15) 0.0002(14) 0.0095(17) C6 0.054(2) 0.054(2) 0.0329(17) 0.0131(17) -0.0005(16) 0.0153(19) C7 0.0334(17) 0.049(2) 0.0230(14) 0.0010(14) -0.0028(13) -0.0012(15) C8 0.0336(17) 0.054(2) 0.0228(14) 0.0084(14) -0.0017(12) 0.0039(16) C9 0.0274(16) 0.052(2) 0.0280(15) 0.0044(15) 0.0002(12) -0.0033(15) C10 0.0343(17) 0.0443(19) 0.0247(14) 0.0067(14) -0.0026(12) -0.0030(15) C11 0.0312(16) 0.0403(18) 0.0231(14) 0.0011(13) -0.0042(12) 0.0003(14) C12 0.0304(17) 0.054(2) 0.0352(17) 0.0093(16) -0.0018(13) -0.0074(16) C13 0.0395(19) 0.053(2) 0.0346(17) 0.0166(16) 0.0009(14) -0.0033(17) C14 0.0309(17) 0.052(2) 0.0241(14) 0.0000(15) -0.0021(12) 0.0021(15) C15 0.070(3) 0.061(3) 0.043(2) -0.0131(19) -0.0221(19) 0.020(2) C16 0.081(3) 0.062(3) 0.049(2) -0.004(2) -0.022(2) 0.031(2) C17 0.055(2) 0.044(2) 0.0388(19) 0.0029(16) 0.0056(16) 0.0054(18) C18 0.071(3) 0.063(3) 0.063(3) -0.025(2) -0.023(2) 0.019(2) C19 0.059(3) 0.065(3) 0.054(2) -0.017(2) -0.0244(19) 0.021(2) C20 0.076(3) 0.039(2) 0.049(2) 0.0025(18) 0.008(2) 0.014(2) C21 0.072(3) 0.044(2) 0.055(2) 0.0039(19) 0.005(2) 0.012(2) C22 0.070(3) 0.051(2) 0.058(2) -0.007(2) -0.004(2) 0.013(2) C23 0.098(2) 0.099(2) 0.100(2) 0.0014(10) 0.0068(10) 0.0023(10) C24 0.0875(18) 0.0874(18) 0.0874(18) 0.0027(10) 0.0042(10) 0.0030(10) C25 0.052(2) 0.051(2) 0.067(3) -0.005(2) 0.003(2) 0.004(2) C26 0.0857(18) 0.0886(18) 0.0847(18) -0.0016(10) 0.0017(10) 0.0042(10) C27 0.106(2) 0.108(2) 0.104(2) -0.0002(10) 0.0013(10) 0.0018(10) _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 2.032(2) 4_565 ? Co1 O3 2.033(2) 3_566 ? Co1 O2 2.047(2) . ? Co1 N1 2.053(3) . ? Co1 O4 2.059(2) 2_556 ? Co1 Co1 2.7550(9) 3_566 ? O1 C1 1.387(4) . ? O1 C8 1.393(4) . ? O2 C7 1.263(4) . ? O3 C7 1.258(4) . ? O3 Co1 2.033(2) 3_566 ? O4 C14 1.261(4) . ? O4 Co1 2.059(2) 2_546 ? O5 C14 1.262(4) . ? O5 Co1 2.032(2) 4_666 ? N1 C15 1.318(4) . ? N1 C19 1.331(4) . ? N2 C23 1.262(7) . ? N2 C27 1.299(8) . ? C1 C6 1.375(5) . ? C1 C2 1.379(5) . ? C2 C3 1.380(4) . ? C2 H2 0.9300 . ? C3 C4 1.397(5) . ? C3 H3 0.9300 . ? C4 C5 1.383(5) . ? C4 C7 1.496(4) . ? C5 C6 1.384(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.373(4) . ? C8 C13 1.378(5) . ? C9 C10 1.385(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 C12 1.385(5) . ? C11 C14 1.496(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.369(6) . ? C15 H15 0.9300 . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 C18 1.373(5) . ? C17 C20 1.500(5) . ? C18 C19 1.369(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.527(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.508(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C25 1.495(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.389(8) . ? C23 H23 0.9300 . ? C24 C25 1.371(7) . ? C24 H24 0.9300 . ? C25 C26 1.366(7) . ? C26 C27 1.392(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? 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 89.88(10) 4_565 3_566 ? O5 Co1 O2 90.21(10) 4_565 . ? O3 Co1 O2 165.36(10) 3_566 . ? O5 Co1 N1 101.98(11) 4_565 . ? O3 Co1 N1 97.41(10) 3_566 . ? O2 Co1 N1 96.89(10) . . ? O5 Co1 O4 164.93(11) 4_565 2_556 ? O3 Co1 O4 91.31(10) 3_566 2_556 ? O2 Co1 O4 84.88(10) . 2_556 ? N1 Co1 O4 92.76(11) . 2_556 ? O5 Co1 Co1 91.19(8) 4_565 3_566 ? O3 Co1 Co1 82.66(7) 3_566 3_566 ? O2 Co1 Co1 82.70(7) . 3_566 ? N1 Co1 Co1 166.82(8) . 3_566 ? O4 Co1 Co1 74.07(8) 2_556 3_566 ? C1 O1 C8 118.1(2) . . ? C7 O2 Co1 124.4(2) . . ? C7 O3 Co1 125.3(2) . 3_566 ? C14 O4 Co1 134.5(2) . 2_546 ? C14 O5 Co1 114.5(2) . 4_666 ? C15 N1 C19 116.2(3) . . ? C15 N1 Co1 122.0(2) . . ? C19 N1 Co1 121.6(2) . . ? C23 N2 C27 116.2(6) . . ? C6 C1 C2 120.9(3) . . ? C6 C1 O1 122.4(3) . . ? C2 C1 O1 116.5(3) . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 C7 121.4(3) . . ? C3 C4 C7 119.9(3) . . ? C4 C5 C6 121.0(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.3(3) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O3 C7 O2 124.9(3) . . ? O3 C7 C4 117.6(3) . . ? O2 C7 C4 117.6(3) . . ? C9 C8 C13 121.6(3) . . ? C9 C8 O1 116.9(3) . . ? C13 C8 O1 121.4(3) . . ? C8 C9 C10 118.6(3) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 C14 121.5(3) . . ? C12 C11 C14 119.6(3) . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C8 C13 C12 118.8(3) . . ? C8 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? O4 C14 O5 124.8(3) . . ? O4 C14 C11 117.3(3) . . ? O5 C14 C11 117.9(3) . . ? N1 C15 C16 123.9(3) . . ? N1 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C15 C16 C17 120.5(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 115.4(4) . . ? C18 C17 C20 122.7(4) . . ? C16 C17 C20 121.9(4) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? N1 C19 C18 123.1(4) . . ? N1 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C17 C20 C21 114.5(3) . . ? C17 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? C17 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C20 110.7(3) . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C25 C22 C21 117.9(4) . . ? C25 C22 H22A 107.8 . . ? C21 C22 H22A 107.8 . . ? C25 C22 H22B 107.8 . . ? C21 C22 H22B 107.8 . . ? H22A C22 H22B 107.2 . . ? N2 C23 C24 125.6(6) . . ? N2 C23 H23 117.2 . . ? C24 C23 H23 117.2 . . ? C25 C24 C23 119.1(6) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C24 115.4(5) . . ? C26 C25 C22 123.8(4) . . ? C24 C25 C22 120.7(4) . . ? C25 C26 C27 119.7(5) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N2 C27 C26 123.9(6) . . ? N2 C27 H27 118.0 . . ? C26 C27 H27 118.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.772 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.076 # Attachment 'compound2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 672251' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C27 H24 Co N2 O6' _chemical_formula_sum 'C27 H24 Co N2 O6' _chemical_formula_weight 531.41 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 Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 13.979(3) _cell_length_b 19.700(5) _cell_length_c 36.094(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9940(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2186 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.19 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4400 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8042 _exptl_absorpt_correction_T_max 0.8511 _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 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13070 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.19 _reflns_number_total 2186 _reflns_number_gt 1342 _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 SHELXP-97 _computing_publication_material 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^)+(0.1630P)^2^+87.1822P] 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 2186 _refine_ls_number_parameters 143 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1499 _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.3002 _refine_ls_wR_factor_gt 0.2565 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.050 _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 0.6250 0.6250 0.41717(4) 0.0572(6) Uani 1 2 d S . . O1 O 0.1250 0.6250 0.5321(2) 0.086(3) Uani 1 2 d S . . O2 O 0.4917(4) 0.6681(3) 0.43038(17) 0.0733(15) Uani 1 1 d . . . O3 O 0.5356(4) 0.5773(3) 0.46072(16) 0.0748(15) Uani 1 1 d . . . O1W O 0.3750 0.7426(8) 0.3750 0.153(5) Uani 1 2 d S . . N1 N 0.5781(5) 0.5550(3) 0.37786(19) 0.0634(16) Uani 1 1 d . . . C1 C 0.2100(5) 0.6245(5) 0.5112(2) 0.070(2) Uani 1 1 d . . . C2 C 0.2268(6) 0.6704(5) 0.4844(3) 0.074(2) Uani 1 1 d . . . H2 H 0.1797 0.7016 0.4779 0.140 Uiso 1 1 calc . . . C3 C 0.3137(6) 0.6712(4) 0.4665(3) 0.072(2) Uani 1 1 d . . . H3 H 0.3255 0.7033 0.4482 0.140 Uiso 1 1 calc . . . C4 C 0.3839(5) 0.6243(4) 0.4756(2) 0.0626(18) Uani 1 1 d . . . C5 C 0.3647(5) 0.5769(4) 0.5031(2) 0.0671(19) Uani 1 1 d . . . H5 H 0.4107 0.5448 0.5093 0.140 Uiso 1 1 calc . . . C6 C 0.2785(6) 0.5769(5) 0.5212(2) 0.076(2) Uani 1 1 d . . . H6 H 0.2660 0.5456 0.5398 0.140 Uiso 1 1 calc . . . C7 C 0.4751(5) 0.6229(4) 0.4549(2) 0.0608(18) Uani 1 1 d . . . C8 C 0.6197(10) 0.5020(8) 0.3670(5) 0.137(4) Uani 1 1 d . . . H8 H 0.6784 0.4910 0.3775 0.140 Uiso 1 1 calc . . . C9 C 0.5826(8) 0.4592(6) 0.3403(4) 0.111(3) Uani 1 1 d U . . H9 H 0.6223 0.4258 0.3305 0.140 Uiso 1 1 calc . . . C10 C 0.4955(8) 0.4631(7) 0.3282(4) 0.111(3) Uani 1 1 d U . . C11 C 0.4509(9) 0.5169(7) 0.3387(5) 0.137(4) Uani 1 1 d . . . H11 H 0.3886 0.5253 0.3309 0.140 Uiso 1 1 calc . . . C12 C 0.4988(13) 0.5626(6) 0.3622(4) 0.133(3) Uani 1 1 d . . . H12 H 0.4678 0.6036 0.3666 0.140 Uiso 1 1 calc . . . C13 C 0.4512(11) 0.4163(6) 0.3000(4) 0.133(3) Uani 1 1 d . . . H13A H 0.4992 0.3864 0.2895 0.140 Uiso 1 1 calc . . . H13B H 0.4221 0.4422 0.2801 0.140 Uiso 1 1 calc . . . C14 C 0.3750 0.3750 0.3209(6) 0.133(3) Uani 1 2 d S . . H14A H 0.3412 0.4064 0.3369 0.140 Uiso 0.50 1 calc P . . H14B H 0.4088 0.3436 0.3369 0.140 Uiso 0.50 1 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0445(8) 0.0608(9) 0.0665(10) 0.000 0.000 -0.0053(6) O1 0.046(4) 0.152(8) 0.059(4) 0.000 0.000 -0.010(5) O2 0.059(3) 0.073(3) 0.088(4) 0.009(3) 0.012(3) -0.001(3) O3 0.055(3) 0.088(4) 0.082(4) 0.014(3) 0.004(3) 0.009(3) O1W 0.152(12) 0.136(10) 0.172(13) 0.000 -0.034(10) 0.000 N1 0.054(3) 0.065(4) 0.071(4) 0.001(3) -0.011(3) -0.012(3) C1 0.051(4) 0.096(6) 0.064(5) -0.002(5) -0.002(4) -0.011(4) C2 0.057(5) 0.080(5) 0.085(6) 0.007(5) -0.008(4) -0.002(4) C3 0.059(5) 0.073(5) 0.082(5) 0.006(4) 0.009(4) -0.005(4) C4 0.052(4) 0.065(4) 0.072(5) -0.001(4) 0.000(3) -0.008(4) C5 0.056(4) 0.079(5) 0.066(4) 0.004(4) 0.000(4) -0.004(4) C6 0.058(5) 0.103(6) 0.066(5) 0.009(5) -0.006(4) -0.016(4) C7 0.058(4) 0.063(4) 0.062(4) 0.004(4) 0.001(3) -0.005(4) C8 0.101(6) 0.135(7) 0.174(10) -0.055(7) -0.061(6) 0.005(6) C9 0.083(4) 0.125(5) 0.125(5) -0.050(4) 0.008(4) -0.013(4) C10 0.083(4) 0.125(5) 0.125(5) -0.050(4) 0.008(4) -0.013(4) C11 0.101(6) 0.135(7) 0.174(10) -0.055(7) -0.061(6) 0.005(6) C12 0.168(9) 0.092(5) 0.138(7) -0.012(5) -0.051(7) -0.032(5) C13 0.168(9) 0.092(5) 0.138(7) -0.012(5) -0.051(7) -0.032(5) C14 0.168(9) 0.092(5) 0.138(7) -0.012(5) -0.051(7) -0.032(5) _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 N1 2.084(6) . ? Co1 N1 2.084(6) 14 ? Co1 O2 2.102(5) 14 ? Co1 O2 2.102(5) . ? Co1 O3 2.218(6) 14 ? Co1 O3 2.218(6) . ? Co1 C7 2.500(8) 14 ? Co1 C7 2.500(8) . ? O1 C1 1.408(9) . ? O1 C1 1.408(9) 14_455 ? O2 C7 1.277(9) . ? O3 C7 1.252(9) . ? N1 C12 1.254(16) . ? N1 C8 1.258(15) . ? C1 C2 1.346(12) . ? C1 C6 1.387(13) . ? C2 C3 1.376(12) . ? C2 H2 0.9300 . ? C3 C4 1.387(12) . ? C3 H3 0.9300 . ? C4 C5 1.390(11) . ? C4 C7 1.479(11) . ? C5 C6 1.370(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.382(16) . ? C8 H8 0.9300 . ? C9 C10 1.296(16) . ? C9 H9 0.9300 . ? C10 C11 1.286(17) . ? C10 C13 1.507(16) . ? C11 C12 1.406(17) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.536(19) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C13 1.536(19) 2 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 N1 Co1 N1 94.2(4) . 14 ? N1 Co1 O2 99.6(2) . 14 ? N1 Co1 O2 98.2(3) 14 14 ? N1 Co1 O2 98.2(3) . . ? N1 Co1 O2 99.6(2) 14 . ? O2 Co1 O2 153.8(3) 14 . ? N1 Co1 O3 160.1(2) . 14 ? N1 Co1 O3 91.4(2) 14 14 ? O2 Co1 O3 60.7(2) 14 14 ? O2 Co1 O3 99.6(2) . 14 ? N1 Co1 O3 91.4(2) . . ? N1 Co1 O3 160.1(2) 14 . ? O2 Co1 O3 99.6(2) 14 . ? O2 Co1 O3 60.7(2) . . ? O3 Co1 O3 89.7(3) 14 . ? N1 Co1 C7 130.2(3) . 14 ? N1 Co1 C7 95.5(3) 14 14 ? O2 Co1 C7 30.7(2) 14 14 ? O2 Co1 C7 127.8(3) . 14 ? O3 Co1 C7 30.0(2) 14 14 ? O3 Co1 C7 95.4(2) . 14 ? N1 Co1 C7 95.5(3) . . ? N1 Co1 C7 130.2(3) 14 . ? O2 Co1 C7 127.8(3) 14 . ? O2 Co1 C7 30.7(2) . . ? O3 Co1 C7 95.4(2) 14 . ? O3 Co1 C7 30.0(2) . . ? C7 Co1 C7 114.0(4) 14 . ? C1 O1 C1 115.0(8) . 14_455 ? C7 O2 Co1 92.1(5) . . ? C7 O3 Co1 87.6(5) . . ? C12 N1 C8 111.5(10) . . ? C12 N1 Co1 120.4(8) . . ? C8 N1 Co1 128.0(7) . . ? C2 C1 C6 121.3(8) . . ? C2 C1 O1 122.0(8) . . ? C6 C1 O1 116.6(7) . . ? C1 C2 C3 119.9(8) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.4(8) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 118.8(7) . . ? C3 C4 C7 120.1(7) . . ? C5 C4 C7 121.0(7) . . ? C6 C5 C4 120.6(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.0(8) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? O3 C7 O2 119.6(7) . . ? O3 C7 C4 120.8(7) . . ? O2 C7 C4 119.7(7) . . ? O3 C7 Co1 62.4(4) . . ? O2 C7 Co1 57.2(4) . . ? C4 C7 Co1 176.7(6) . . ? N1 C8 C9 123.4(11) . . ? N1 C8 H8 118.3 . . ? C9 C8 H8 118.3 . . ? C10 C9 C8 123.4(12) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C11 C10 C9 113.9(11) . . ? C11 C10 C13 120.3(12) . . ? C9 C10 C13 125.2(12) . . ? C10 C11 C12 118.3(12) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N1 C12 C11 128.1(14) . . ? N1 C12 H12 116.0 . . ? C11 C12 H12 116.0 . . ? C10 C13 C14 106.2(13) . . ? C10 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? C10 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? C13 C14 C13 121.4(17) . 2 ? C13 C14 H14A 107.0 . . ? C13 C14 H14A 107.0 2 . ? C13 C14 H14B 107.0 . . ? C13 C14 H14B 107.0 2 . ? H14A C14 H14B 106.7 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.849 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.101 #===========================================END