# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_paper _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author ; Prof Mir Wais Hosseini Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, F-67000 Strasbourg, France ; _publ_contact_author_email hosseini@chimie.u-strasbg.fr _publ_contact_author_fax '33 3 90 24 13 23' _publ_contact_author_phone '33 3 90 24 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; D.Salazar-Mendoza ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_section_title ; Combination of primary amide and dipyrrin for the elaboration of extended architectures built upon both coordination and hydrogen bonding ; _publ_contact_author_name 'Prof Mir Wais Hosseini' ###Material relevant to compound 1 at 173K ## data_compound1 _database_code_depnum_ccdc_archive 'CCDC 716997' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H13 N3 O' _chemical_formula_sum 'C16 H13 N3 O' _chemical_formula_weight 263.29 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.3670(16) _cell_length_b 9.2645(3) _cell_length_c 16.8012(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.829(2) _cell_angle_gamma 90.00 _cell_volume 5325.1(4) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3778 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.26 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9667 _exptl_absorpt_correction_T_max 0.9899 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 21337 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6119 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0526P)^2^+5.2363P] 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 SHELXL _refine_ls_extinction_coef 0.00074(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6119 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C1 C 0.02985(8) 0.6214(3) 0.56504(16) 0.0547(7) Uani 1 1 d . . . H1A H 0.0127 0.5486 0.5676 0.066 Uiso 1 1 calc R . . C2 C 0.06302(8) 0.6015(3) 0.54361(15) 0.0485(6) Uani 1 1 d . . . H2 H 0.0718 0.5149 0.5285 0.058 Uiso 1 1 calc R . . C3 C 0.08051(7) 0.7354(2) 0.54909(14) 0.0398(5) Uani 1 1 d . . . H3 H 0.1035 0.7552 0.5387 0.048 Uiso 1 1 calc R . . C4 C 0.05743(6) 0.8358(2) 0.57307(13) 0.0353(5) Uani 1 1 d . . . C5 C 0.06318(6) 0.9862(2) 0.59025(13) 0.0322(5) Uani 1 1 d . . . C6 C 0.03814(6) 1.0736(2) 0.61462(14) 0.0378(5) Uani 1 1 d . . . C7 C 0.04242(8) 1.2226(3) 0.63726(16) 0.0481(6) Uani 1 1 d . . . H7 H 0.0631 1.2825 0.6385 0.058 Uiso 1 1 calc R . . C8 C 0.01021(9) 1.2601(3) 0.65674(19) 0.0601(8) Uani 1 1 d . . . H8 H 0.0046 1.3506 0.6736 0.072 Uiso 1 1 calc R . . C9 C -0.01292(8) 1.1341(3) 0.64615(16) 0.0588(8) Uani 1 1 d . . . H9 H -0.0367 1.1305 0.6553 0.071 Uiso 1 1 calc R . . C10 C 0.09881(6) 1.0489(2) 0.57934(13) 0.0315(5) Uani 1 1 d . . . C11 C 0.13582(6) 1.0053(2) 0.63076(14) 0.0385(5) Uani 1 1 d . . . H11 H 0.1384 0.9425 0.6755 0.046 Uiso 1 1 calc R . . C12 C 0.16882(6) 1.0541(2) 0.61609(14) 0.0369(5) Uani 1 1 d . . . H12 H 0.1934 1.0235 0.6508 0.044 Uiso 1 1 calc R . . C13 C 0.16561(6) 1.1485(2) 0.54984(13) 0.0297(4) Uani 1 1 d . . . C14 C 0.12891(6) 1.1970(2) 0.50062(13) 0.0326(5) Uani 1 1 d . . . H14 H 0.1265 1.2630 0.4574 0.039 Uiso 1 1 calc R . . C15 C 0.09572(6) 1.1483(2) 0.51504(13) 0.0336(5) Uani 1 1 d . . . H15 H 0.0713 1.1819 0.4817 0.040 Uiso 1 1 calc R . . C16 C 0.20049(6) 1.1963(2) 0.52903(13) 0.0308(5) Uani 1 1 d . . . N1 N 0.02608(6) 0.7612(2) 0.58159(12) 0.0453(5) Uani 1 1 d . . . H1 H 0.0073 0.7981 0.5952 0.054 Uiso 1 1 calc R . . N2 N 0.00307(6) 1.0223(2) 0.62188(12) 0.0487(5) Uani 1 1 d . . . N3 N 0.23231(5) 1.1163(2) 0.55757(13) 0.0427(5) Uani 1 1 d . . . H3A H 0.2529 1.1400 0.5466 0.051 Uiso 1 1 calc R . . H3B H 0.2324 1.0405 0.5872 0.051 Uiso 1 1 calc R . . O1 O 0.19906(4) 1.30699(15) 0.48593(10) 0.0371(4) Uani 1 1 d . . . C17 C 0.13276(10) 0.1393(3) 0.89269(19) 0.0642(8) Uani 1 1 d . . . H17 H 0.1233 0.0735 0.9229 0.077 Uiso 1 1 calc R . . C18 C 0.16430(9) 0.1128(3) 0.86431(18) 0.0620(8) Uani 1 1 d . . . H18 H 0.1790 0.0286 0.8718 0.074 Uiso 1 1 calc R . . C19 C 0.16911(8) 0.2351(3) 0.82353(16) 0.0490(6) Uani 1 1 d . . . H19 H 0.1879 0.2504 0.7981 0.059 Uiso 1 1 calc R . . C20 C 0.14004(7) 0.3347(2) 0.82726(14) 0.0400(5) Uani 1 1 d . . . C21 C 0.13293(6) 0.4756(2) 0.79577(13) 0.0373(5) Uani 1 1 d . . . C22 C 0.10335(6) 0.5658(3) 0.80463(13) 0.0375(5) Uani 1 1 d . . . C23 C 0.09193(7) 0.7037(3) 0.77236(14) 0.0452(6) Uani 1 1 d . . . H23 H 0.1040 0.7596 0.7424 0.054 Uiso 1 1 calc R . . C24 C 0.05964(8) 0.7426(3) 0.79256(15) 0.0526(7) Uani 1 1 d . . . H24 H 0.0458 0.8288 0.7790 0.063 Uiso 1 1 calc R . . C25 C 0.05188(7) 0.6269(3) 0.83743(16) 0.0511(7) Uani 1 1 d . . . H25 H 0.0314 0.6238 0.8586 0.061 Uiso 1 1 calc R . . C26 C 0.15639(6) 0.5311(2) 0.74454(13) 0.0349(5) Uani 1 1 d . . . C27 C 0.15257(7) 0.4640(2) 0.66812(15) 0.0399(5) Uani 1 1 d . . . H27 H 0.1367 0.3829 0.6516 0.048 Uiso 1 1 calc R . . C28 C 0.17217(7) 0.5169(2) 0.61629(15) 0.0398(5) Uani 1 1 d . . . H28 H 0.1686 0.4727 0.5645 0.048 Uiso 1 1 calc R . . C29 C 0.19691(6) 0.6347(2) 0.64077(14) 0.0343(5) Uani 1 1 d . . . C30 C 0.20139(7) 0.6996(2) 0.71810(14) 0.0388(5) Uani 1 1 d . . . H30 H 0.2183 0.7775 0.7360 0.047 Uiso 1 1 calc R . . C31 C 0.18102(7) 0.6498(2) 0.76885(14) 0.0387(5) Uani 1 1 d . . . H31 H 0.1839 0.6962 0.8197 0.046 Uiso 1 1 calc R . . C32 C 0.21859(7) 0.6943(2) 0.58598(15) 0.0372(5) Uani 1 1 d . . . N4 N 0.11826(7) 0.2698(2) 0.87092(13) 0.0523(6) Uani 1 1 d . . . H4 H 0.0989 0.3076 0.8818 0.063 Uiso 1 1 calc R . . N5 N 0.07791(6) 0.5206(2) 0.84594(13) 0.0462(5) Uani 1 1 d . . . N6 N 0.21900(7) 0.6132(2) 0.52127(14) 0.0520(6) Uani 1 1 d . . . H6A H 0.2313 0.6422 0.4885 0.062 Uiso 1 1 calc R . . H6B H 0.2070 0.5316 0.5120 0.062 Uiso 1 1 calc R . . O2 O 0.23540(5) 0.81211(16) 0.60163(11) 0.0439(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 C1 0.0645(18) 0.0586(17) 0.0464(14) -0.0154(12) 0.0258(13) -0.0333(14) C2 0.0601(17) 0.0461(14) 0.0443(14) -0.0091(11) 0.0245(13) -0.0121(12) C3 0.0418(13) 0.0439(13) 0.0390(12) 0.0000(10) 0.0208(10) -0.0033(10) C4 0.0329(12) 0.0437(13) 0.0305(11) 0.0035(9) 0.0123(9) -0.0087(9) C5 0.0273(11) 0.0405(12) 0.0302(10) 0.0089(9) 0.0117(8) 0.0005(9) C6 0.0303(11) 0.0489(14) 0.0373(12) 0.0099(10) 0.0156(9) 0.0018(10) C7 0.0527(16) 0.0432(14) 0.0578(15) 0.0113(12) 0.0311(13) 0.0056(11) C8 0.069(2) 0.0560(17) 0.0711(18) 0.0183(14) 0.0442(16) 0.0238(14) C9 0.0403(15) 0.092(2) 0.0502(15) 0.0183(15) 0.0236(12) 0.0167(15) C10 0.0323(11) 0.0314(11) 0.0345(11) 0.0031(9) 0.0161(9) -0.0014(9) C11 0.0337(12) 0.0443(13) 0.0409(12) 0.0155(10) 0.0170(10) -0.0008(10) C12 0.0292(11) 0.0418(13) 0.0401(12) 0.0096(10) 0.0123(9) -0.0004(9) C13 0.0329(11) 0.0260(10) 0.0362(11) -0.0015(8) 0.0194(9) -0.0033(8) C14 0.0363(12) 0.0305(11) 0.0363(11) 0.0059(9) 0.0192(9) -0.0014(9) C15 0.0288(11) 0.0361(12) 0.0386(11) 0.0072(9) 0.0151(9) 0.0016(9) C16 0.0332(11) 0.0284(11) 0.0357(11) -0.0025(9) 0.0180(9) -0.0045(9) N1 0.0435(12) 0.0581(13) 0.0398(11) -0.0049(9) 0.0214(9) -0.0195(10) N2 0.0295(10) 0.0798(15) 0.0416(11) 0.0052(10) 0.0184(9) 0.0043(10) N3 0.0344(11) 0.0376(10) 0.0649(13) 0.0141(9) 0.0284(10) 0.0009(8) O1 0.0396(9) 0.0315(8) 0.0498(9) 0.0062(7) 0.0278(7) -0.0017(6) C17 0.089(2) 0.0477(16) 0.0711(19) 0.0215(14) 0.0470(18) 0.0066(15) C18 0.081(2) 0.0489(16) 0.0624(18) 0.0146(13) 0.0333(16) 0.0122(15) C19 0.0524(16) 0.0516(15) 0.0485(14) 0.0082(12) 0.0243(12) 0.0047(12) C20 0.0437(13) 0.0443(13) 0.0376(12) 0.0049(10) 0.0213(10) -0.0006(10) C21 0.0354(12) 0.0496(13) 0.0305(11) 0.0000(10) 0.0158(9) -0.0043(10) C22 0.0356(12) 0.0495(14) 0.0327(11) 0.0011(10) 0.0185(10) -0.0012(10) C23 0.0456(14) 0.0605(16) 0.0341(12) 0.0060(11) 0.0197(11) 0.0106(12) C24 0.0477(15) 0.0682(18) 0.0410(14) -0.0025(12) 0.0137(12) 0.0183(13) C25 0.0411(14) 0.0670(17) 0.0529(15) -0.0122(13) 0.0260(12) 0.0011(12) C26 0.0339(12) 0.0392(12) 0.0361(11) 0.0043(9) 0.0179(9) 0.0028(9) C27 0.0426(13) 0.0387(12) 0.0463(13) -0.0028(10) 0.0256(11) -0.0070(10) C28 0.0469(14) 0.0397(13) 0.0438(13) -0.0027(10) 0.0298(11) -0.0037(10) C29 0.0361(12) 0.0304(11) 0.0436(12) 0.0057(9) 0.0228(10) 0.0039(9) C30 0.0416(13) 0.0338(12) 0.0452(13) 0.0012(10) 0.0200(11) -0.0042(10) C31 0.0436(13) 0.0407(13) 0.0360(12) 0.0002(10) 0.0191(10) -0.0003(10) C32 0.0419(13) 0.0300(11) 0.0485(13) 0.0077(10) 0.0267(11) 0.0056(10) N4 0.0589(14) 0.0533(13) 0.0594(14) 0.0152(10) 0.0393(12) 0.0029(11) N5 0.0433(12) 0.0553(13) 0.0509(12) -0.0063(10) 0.0303(10) -0.0053(10) N6 0.0763(16) 0.0370(11) 0.0654(14) -0.0035(10) 0.0536(13) -0.0116(10) O2 0.0503(10) 0.0309(8) 0.0612(10) 0.0018(7) 0.0328(9) -0.0034(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 C1 N1 1.341(3) . ? C1 C2 1.383(4) . ? C1 H1A 0.9300 . ? C2 C3 1.383(3) . ? C2 H2 0.9300 . ? C3 C4 1.401(3) . ? C3 H3 0.9300 . ? C4 N1 1.382(3) . ? C4 C5 1.424(3) . ? C5 C6 1.380(3) . ? C5 C10 1.487(3) . ? C6 N2 1.405(3) . ? C6 C7 1.426(3) . ? C7 C8 1.363(3) . ? C7 H7 0.9300 . ? C8 C9 1.414(4) . ? C8 H8 0.9300 . ? C9 N2 1.319(3) . ? C9 H9 0.9300 . ? C10 C11 1.390(3) . ? C10 C15 1.394(3) . ? C11 C12 1.381(3) . ? C11 H11 0.9300 . ? C12 C13 1.389(3) . ? C12 H12 0.9300 . ? C13 C14 1.385(3) . ? C13 C16 1.492(3) . ? C14 C15 1.385(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.247(2) . ? C16 N3 1.320(3) . ? N1 H1 0.8600 . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C17 N4 1.320(3) . ? C17 C18 1.405(4) . ? C17 H17 0.9300 . ? C18 C19 1.366(3) . ? C18 H18 0.9300 . ? C19 C20 1.420(3) . ? C19 H19 0.9300 . ? C20 N4 1.386(3) . ? C20 C21 1.399(3) . ? C21 C22 1.410(3) . ? C21 C26 1.494(3) . ? C22 C23 1.395(3) . ? C22 N5 1.396(3) . ? C23 C24 1.376(3) . ? C23 H23 0.9300 . ? C24 C25 1.394(4) . ? C24 H24 0.9300 . ? C25 N5 1.339(3) . ? C25 H25 0.9300 . ? C26 C31 1.390(3) . ? C26 C27 1.390(3) . ? C27 C28 1.388(3) . ? C27 H27 0.9300 . ? C28 C29 1.385(3) . ? C28 H28 0.9300 . ? C29 C30 1.390(3) . ? C29 C32 1.505(3) . ? C30 C31 1.384(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O2 1.235(3) . ? C32 N6 1.326(3) . ? N4 H4 0.8600 . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? 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 C1 C2 110.0(2) . . ? N1 C1 H1A 125.0 . . ? C2 C1 H1A 125.0 . . ? C3 C2 C1 106.5(2) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 107.9(2) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? N1 C4 C3 107.07(19) . . ? N1 C4 C5 122.6(2) . . ? C3 C4 C5 130.3(2) . . ? C6 C5 C4 124.6(2) . . ? C6 C5 C10 119.85(19) . . ? C4 C5 C10 115.55(18) . . ? C5 C6 N2 122.5(2) . . ? C5 C6 C7 128.6(2) . . ? N2 C6 C7 108.9(2) . . ? C8 C7 C6 106.6(2) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? C7 C8 C9 106.4(2) . . ? C7 C8 H8 126.8 . . ? C9 C8 H8 126.8 . . ? N2 C9 C8 112.4(2) . . ? N2 C9 H9 123.8 . . ? C8 C9 H9 123.8 . . ? C11 C10 C15 118.70(19) . . ? C11 C10 C5 120.67(18) . . ? C15 C10 C5 120.58(19) . . ? C12 C11 C10 120.71(19) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 118.99(18) . . ? C14 C13 C16 119.18(18) . . ? C12 C13 C16 121.82(19) . . ? C15 C14 C13 120.69(19) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C10 120.3(2) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? O1 C16 N3 122.11(19) . . ? O1 C16 C13 120.57(19) . . ? N3 C16 C13 117.31(18) . . ? C1 N1 C4 108.4(2) . . ? C1 N1 H1 125.8 . . ? C4 N1 H1 125.8 . . ? C9 N2 C6 105.6(2) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N4 C17 C18 111.2(2) . . ? N4 C17 H17 124.4 . . ? C18 C17 H17 124.4 . . ? C19 C18 C17 106.4(2) . . ? C19 C18 H18 126.8 . . ? C17 C18 H18 126.8 . . ? C18 C19 C20 107.0(2) . . ? C18 C19 H19 126.5 . . ? C20 C19 H19 126.5 . . ? N4 C20 C21 122.6(2) . . ? N4 C20 C19 108.0(2) . . ? C21 C20 C19 129.4(2) . . ? C20 C21 C22 124.3(2) . . ? C20 C21 C26 118.1(2) . . ? C22 C21 C26 117.5(2) . . ? C23 C22 N5 107.9(2) . . ? C23 C22 C21 129.7(2) . . ? N5 C22 C21 122.2(2) . . ? C24 C23 C22 108.1(2) . . ? C24 C23 H23 126.0 . . ? C22 C23 H23 126.0 . . ? C23 C24 C25 106.2(2) . . ? C23 C24 H24 126.9 . . ? C25 C24 H24 126.9 . . ? N5 C25 C24 111.0(2) . . ? N5 C25 H25 124.5 . . ? C24 C25 H25 124.5 . . ? C31 C26 C27 118.52(19) . . ? C31 C26 C21 122.7(2) . . ? C27 C26 C21 118.7(2) . . ? C28 C27 C26 120.7(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 120.8(2) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 118.45(19) . . ? C28 C29 C32 122.0(2) . . ? C30 C29 C32 119.6(2) . . ? C31 C30 C29 120.9(2) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C26 120.6(2) . . ? C30 C31 H31 119.7 . . ? C26 C31 H31 119.7 . . ? O2 C32 N6 122.2(2) . . ? O2 C32 C29 121.2(2) . . ? N6 C32 C29 116.6(2) . . ? C17 N4 C20 107.3(2) . . ? C17 N4 H4 126.3 . . ? C20 N4 H4 126.3 . . ? C25 N5 C22 106.9(2) . . ? C32 N6 H6A 120.0 . . ? C32 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.244 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.051 #===END ###Material relevant to compound 2 at 173K ######## data_compound2 _database_code_depnum_ccdc_archive 'CCDC 716998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 N3 O' _chemical_formula_sum 'C16 H15 N3 O' _chemical_formula_weight 265.31 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3130(3) _cell_length_b 9.5783(3) _cell_length_c 9.8020(3) _cell_angle_alpha 80.064(2) _cell_angle_beta 65.596(2) _cell_angle_gamma 74.133(2) _cell_volume 682.08(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2747 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.52 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9698 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 7482 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.93 _reflns_number_total 2865 _reflns_number_gt 2277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0689P)^2^+0.2063P] 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 ? _refine_ls_number_reflns 2865 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 C1 C -0.0388(3) 0.78913(19) 0.30586(19) 0.0309(4) Uani 1 1 d . . . H1A H -0.1560 0.8409 0.3193 0.037 Uiso 1 1 calc R . . C2 C 0.0089(3) 0.64926(19) 0.3590(2) 0.0324(4) Uani 1 1 d . . . H2A H -0.0693 0.5886 0.4153 0.039 Uiso 1 1 calc R . . C3 C 0.2001(2) 0.61385(17) 0.31228(18) 0.0269(4) Uani 1 1 d . . . H3 H 0.2705 0.5252 0.3318 0.032 Uiso 1 1 calc R . . C4 C 0.2626(2) 0.73396(16) 0.23310(17) 0.0228(4) Uani 1 1 d . . . C5 C 0.4522(2) 0.75857(16) 0.15494(17) 0.0224(4) Uani 1 1 d . . . H5 H 0.4752 0.7813 0.0480 0.027 Uiso 1 1 calc R . . C6 C 0.4725(2) 0.88685(16) 0.21271(17) 0.0234(4) Uani 1 1 d . . . C7 C 0.3753(2) 0.95596(18) 0.34331(18) 0.0282(4) Uani 1 1 d . . . H7 H 0.2718 0.9342 0.4208 0.034 Uiso 1 1 calc R . . C8 C 0.4615(3) 1.06711(19) 0.3389(2) 0.0332(4) Uani 1 1 d . . . H8 H 0.4242 1.1319 0.4125 0.040 Uiso 1 1 calc R . . C9 C 0.6092(3) 1.06103(18) 0.2067(2) 0.0334(4) Uani 1 1 d . . . H9 H 0.6913 1.1208 0.1740 0.040 Uiso 1 1 calc R . . C10 C 0.5906(2) 0.62043(16) 0.16864(17) 0.0227(4) Uani 1 1 d . . . C11 C 0.6935(2) 0.53358(17) 0.04876(18) 0.0275(4) Uani 1 1 d . . . H11 H 0.6782 0.5599 -0.0417 0.033 Uiso 1 1 calc R . . C12 C 0.8192(3) 0.40768(17) 0.06211(19) 0.0283(4) Uani 1 1 d . . . H12 H 0.8881 0.3508 -0.0194 0.034 Uiso 1 1 calc R . . C13 C 0.8420(2) 0.36679(16) 0.19743(18) 0.0253(4) Uani 1 1 d . . . C14 C 0.7364(3) 0.45186(18) 0.31855(19) 0.0287(4) Uani 1 1 d . . . H14 H 0.7484 0.4238 0.4102 0.034 Uiso 1 1 calc R . . C15 C 0.6133(2) 0.57799(18) 0.30408(18) 0.0277(4) Uani 1 1 d . . . H15 H 0.5451 0.6351 0.3855 0.033 Uiso 1 1 calc R . . C16 C 0.9847(3) 0.23535(18) 0.2062(2) 0.0307(4) Uani 1 1 d . . . N1 N 0.1148(2) 0.83967(14) 0.22987(15) 0.0273(3) Uani 1 1 d . . . H1 H 0.1186 0.9253 0.1862 0.033 Uiso 1 1 calc R . . N2 N 0.6149(2) 0.95132(15) 0.13087(16) 0.0289(3) Uani 1 1 d . . . H2 H 0.6961 0.9265 0.0444 0.035 Uiso 1 1 calc R . . N3 N 1.0396(3) 0.22106(19) 0.3185(2) 0.0564(6) Uani 1 1 d . . . H3A H 1.1216 0.1466 0.3268 0.068 Uiso 1 1 calc R . . H3B H 0.9932 0.2863 0.3828 0.068 Uiso 1 1 calc R . . O1 O 1.04958(18) 0.14298(12) 0.11243(14) 0.0342(3) 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 C1 0.0231(10) 0.0353(9) 0.0341(9) -0.0004(7) -0.0134(8) -0.0037(8) C2 0.0324(11) 0.0338(9) 0.0352(9) 0.0081(7) -0.0166(8) -0.0146(8) C3 0.0302(10) 0.0233(7) 0.0298(8) 0.0038(6) -0.0163(7) -0.0057(7) C4 0.0236(9) 0.0213(7) 0.0239(7) -0.0020(6) -0.0114(7) -0.0018(7) C5 0.0226(9) 0.0204(7) 0.0221(7) 0.0004(6) -0.0096(7) -0.0012(6) C6 0.0221(9) 0.0204(7) 0.0265(7) 0.0024(6) -0.0115(7) -0.0022(6) C7 0.0250(10) 0.0270(8) 0.0292(8) -0.0023(7) -0.0100(7) -0.0013(7) C8 0.0382(12) 0.0272(8) 0.0388(9) -0.0056(7) -0.0214(9) -0.0020(8) C9 0.0352(11) 0.0262(8) 0.0463(10) 0.0034(8) -0.0240(9) -0.0091(8) C10 0.0202(9) 0.0203(7) 0.0261(8) 0.0000(6) -0.0085(7) -0.0036(6) C11 0.0309(11) 0.0257(8) 0.0259(8) -0.0022(6) -0.0128(7) -0.0032(7) C12 0.0297(10) 0.0224(8) 0.0308(8) -0.0065(6) -0.0111(7) -0.0009(7) C13 0.0223(9) 0.0200(7) 0.0343(8) -0.0002(6) -0.0123(7) -0.0048(7) C14 0.0322(11) 0.0271(8) 0.0293(8) -0.0001(7) -0.0166(8) -0.0038(7) C15 0.0280(10) 0.0265(8) 0.0253(8) -0.0044(6) -0.0101(7) 0.0002(7) C16 0.0292(10) 0.0218(8) 0.0417(10) -0.0006(7) -0.0161(8) -0.0038(7) N1 0.0264(9) 0.0214(6) 0.0331(7) 0.0028(6) -0.0140(6) -0.0023(6) N2 0.0270(9) 0.0282(7) 0.0296(7) 0.0020(6) -0.0098(6) -0.0078(6) N3 0.0629(14) 0.0413(10) 0.0763(13) -0.0225(9) -0.0524(12) 0.0227(9) O1 0.0332(8) 0.0233(6) 0.0382(7) -0.0032(5) -0.0102(6) 0.0008(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 C1 N1 1.359(2) . ? C1 C2 1.365(2) . ? C1 H1A 0.9300 . ? C2 C3 1.417(3) . ? C2 H2A 0.9300 . ? C3 C4 1.372(2) . ? C3 H3 0.9300 . ? C4 N1 1.370(2) . ? C4 C5 1.507(2) . ? C5 C6 1.514(2) . ? C5 C10 1.525(2) . ? C5 H5 0.9800 . ? C6 N2 1.367(2) . ? C6 C7 1.369(2) . ? C7 C8 1.423(2) . ? C7 H7 0.9300 . ? C8 C9 1.365(3) . ? C8 H8 0.9300 . ? C9 N2 1.368(2) . ? C9 H9 0.9300 . ? C10 C11 1.386(2) . ? C10 C15 1.394(2) . ? C11 C12 1.390(2) . ? C11 H11 0.9300 . ? C12 C13 1.392(2) . ? C12 H12 0.9300 . ? C13 C14 1.388(2) . ? C13 C16 1.493(2) . ? C14 C15 1.382(2) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.237(2) . ? C16 N3 1.330(2) . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? 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 C1 C2 108.13(16) . . ? N1 C1 H1A 125.9 . . ? C2 C1 H1A 125.9 . . ? C1 C2 C3 107.13(16) . . ? C1 C2 H2A 126.4 . . ? C3 C2 H2A 126.4 . . ? C4 C3 C2 107.65(14) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? N1 C4 C3 107.13(15) . . ? N1 C4 C5 121.67(13) . . ? C3 C4 C5 131.17(15) . . ? C4 C5 C6 111.57(13) . . ? C4 C5 C10 110.54(12) . . ? C6 C5 C10 111.67(13) . . ? C4 C5 H5 107.6 . . ? C6 C5 H5 107.6 . . ? C10 C5 H5 107.6 . . ? N2 C6 C7 107.35(15) . . ? N2 C6 C5 120.22(14) . . ? C7 C6 C5 132.38(15) . . ? C6 C7 C8 107.58(16) . . ? C6 C7 H7 126.2 . . ? C8 C7 H7 126.2 . . ? C9 C8 C7 107.27(16) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? C8 C9 N2 107.74(16) . . ? C8 C9 H9 126.1 . . ? N2 C9 H9 126.1 . . ? C11 C10 C15 118.74(15) . . ? C11 C10 C5 121.15(13) . . ? C15 C10 C5 120.11(14) . . ? C10 C11 C12 120.84(14) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 120.01(15) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 119.24(15) . . ? C14 C13 C16 121.87(15) . . ? C12 C13 C16 118.85(15) . . ? C15 C14 C13 120.50(15) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C10 120.65(15) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? O1 C16 N3 121.12(17) . . ? O1 C16 C13 121.22(16) . . ? N3 C16 C13 117.66(16) . . ? C1 N1 C4 109.96(14) . . ? C1 N1 H1 125.0 . . ? C4 N1 H1 125.0 . . ? C6 N2 C9 110.06(15) . . ? C6 N2 H2 125.0 . . ? C9 N2 H2 125.0 . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.93 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.207 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.067 #===END ###Material relevant to compound 4THF at 173K ## data_compound4THF _database_code_depnum_ccdc_archive 'CCDC 716999' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 Cu N6 O2, 2(C4 H8 O)' _chemical_formula_sum 'C40 H40 Cu N6 O4' _chemical_formula_weight 732.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.9322(12) _cell_length_b 15.8716(8) _cell_length_c 10.2807(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.4940(10) _cell_angle_gamma 90.00 _cell_volume 3605.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3052 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.03 _exptl_crystal_description rod _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7981 _exptl_absorpt_correction_T_max 0.8967 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 10737 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4095 _reflns_number_gt 3423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0827P)^2^+8.7717P] 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 ? _refine_ls_number_reflns 4095 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 C1 C 0.06073(13) 0.73801(17) 0.1854(3) 0.0232(6) Uani 1 1 d . . . H1 H 0.0243 0.7099 0.1509 0.028 Uiso 1 1 calc R . . C2 C 0.11711(13) 0.70862(18) 0.1747(3) 0.0246(6) Uani 1 1 d . . . H2 H 0.1244 0.6592 0.1331 0.030 Uiso 1 1 calc R . . C3 C 0.15935(12) 0.76750(18) 0.2379(3) 0.0228(6) Uani 1 1 d . . . H3 H 0.2008 0.7652 0.2473 0.027 Uiso 1 1 calc R . . C4 C 0.12781(11) 0.83220(17) 0.2859(3) 0.0192(5) Uani 1 1 d . . . C5 C 0.15177(12) 0.90837(18) 0.3472(3) 0.0200(5) Uani 1 1 d . . . C6 C 0.11840(12) 0.97406(17) 0.3817(3) 0.0216(6) Uani 1 1 d . . . C7 C 0.14044(13) 1.04902(18) 0.4549(3) 0.0262(6) Uani 1 1 d . . . H7 H 0.1808 1.0649 0.4872 0.031 Uiso 1 1 calc R . . C8 C 0.09115(14) 1.09338(19) 0.4690(3) 0.0281(6) Uani 1 1 d . . . H8 H 0.0914 1.1445 0.5132 0.034 Uiso 1 1 calc R . . C9 C 0.03987(13) 1.04552(18) 0.4026(3) 0.0251(6) Uani 1 1 d . . . H9 H 0.0001 1.0616 0.3955 0.030 Uiso 1 1 calc R . . C10 C 0.21827(12) 0.92262(18) 0.3757(3) 0.0210(5) Uani 1 1 d . . . C11 C 0.23945(13) 0.98313(19) 0.3005(3) 0.0268(6) Uani 1 1 d . . . H11 H 0.2122 1.0124 0.2322 0.032 Uiso 1 1 calc R . . C12 C 0.30070(13) 0.99948(19) 0.3272(3) 0.0257(6) Uani 1 1 d . . . H12 H 0.3145 1.0384 0.2747 0.031 Uiso 1 1 calc R . . C13 C 0.34174(12) 0.95844(18) 0.4318(3) 0.0209(5) Uani 1 1 d . . . C14 C 0.32077(12) 0.89813(18) 0.5069(3) 0.0240(6) Uani 1 1 d . . . H14 H 0.3480 0.8699 0.5766 0.029 Uiso 1 1 calc R . . C15 C 0.25950(13) 0.88002(19) 0.4781(3) 0.0245(6) Uani 1 1 d . . . H15 H 0.2459 0.8391 0.5278 0.029 Uiso 1 1 calc R . . C16 C 0.40772(12) 0.97869(18) 0.4589(3) 0.0220(6) Uani 1 1 d . . . N1 N 0.06612(10) 0.81162(14) 0.2518(2) 0.0196(5) Uani 1 1 d . . . N2 N 0.05556(10) 0.97428(15) 0.3513(2) 0.0219(5) Uani 1 1 d . . . N3 N 0.44148(11) 0.97134(19) 0.5852(3) 0.0324(6) Uani 1 1 d . . . H3A H 0.4795 0.9828 0.6047 0.039 Uiso 1 1 calc R . . H3B H 0.4253 0.9551 0.6474 0.039 Uiso 1 1 calc R . . O1 O 0.42877(9) 1.00185(14) 0.3654(2) 0.0263(5) Uani 1 1 d . . . Cu1 Cu 0.0000 0.89034(3) 0.2500 0.01997(17) Uani 1 2 d S . . C17 C 0.1733(3) 0.2736(4) 0.3222(7) 0.0885(8) Uani 1 1 d . . . H17A H 0.1982 0.3231 0.3225 0.106 Uiso 1 1 calc R . . H17B H 0.1864 0.2472 0.4103 0.106 Uiso 1 1 calc R . . C18 C 0.1087(3) 0.2986(4) 0.2943(7) 0.0885(8) Uani 1 1 d . . . H18A H 0.1043 0.3593 0.2849 0.106 Uiso 1 1 calc R . . H18B H 0.0916 0.2801 0.3662 0.106 Uiso 1 1 calc R . . C19 C 0.0783(3) 0.2548(4) 0.1631(7) 0.0885(8) Uani 1 1 d . . . H19A H 0.0404 0.2292 0.1671 0.106 Uiso 1 1 calc R . . H19B H 0.0706 0.2938 0.0878 0.106 Uiso 1 1 calc R . . C20 C 0.1235(3) 0.1894(4) 0.1514(7) 0.0885(8) Uani 1 1 d . . . H20A H 0.1143 0.1362 0.1878 0.106 Uiso 1 1 calc R . . H20B H 0.1228 0.1811 0.0575 0.106 Uiso 1 1 calc R . . O2 O 0.1799(2) 0.2182(3) 0.2242(4) 0.0885(8) 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 C1 0.0221(13) 0.0212(13) 0.0246(14) 0.0019(11) 0.0037(11) -0.0013(10) C2 0.0275(14) 0.0209(13) 0.0255(15) 0.0029(11) 0.0073(12) 0.0063(11) C3 0.0192(12) 0.0243(13) 0.0239(14) 0.0052(11) 0.0044(11) 0.0050(10) C4 0.0152(12) 0.0226(13) 0.0192(13) 0.0050(10) 0.0035(10) 0.0014(9) C5 0.0151(12) 0.0261(13) 0.0177(13) 0.0038(11) 0.0024(10) -0.0002(10) C6 0.0168(12) 0.0234(13) 0.0235(14) 0.0008(11) 0.0033(11) -0.0035(10) C7 0.0245(14) 0.0276(14) 0.0239(15) -0.0026(12) 0.0020(12) -0.0064(11) C8 0.0334(16) 0.0266(14) 0.0242(15) -0.0060(12) 0.0078(13) -0.0028(12) C9 0.0258(14) 0.0247(14) 0.0260(16) -0.0029(11) 0.0091(12) 0.0013(11) C10 0.0152(12) 0.0245(13) 0.0225(14) -0.0001(11) 0.0033(10) -0.0020(10) C11 0.0187(13) 0.0321(15) 0.0257(16) 0.0093(12) -0.0006(11) -0.0018(11) C12 0.0210(13) 0.0292(14) 0.0260(15) 0.0069(12) 0.0046(11) -0.0051(11) C13 0.0156(12) 0.0260(13) 0.0204(14) -0.0019(11) 0.0035(10) -0.0011(10) C14 0.0161(12) 0.0341(15) 0.0198(14) 0.0070(12) 0.0015(11) 0.0008(10) C15 0.0187(13) 0.0292(14) 0.0254(15) 0.0065(12) 0.0056(11) -0.0027(10) C16 0.0159(12) 0.0271(14) 0.0221(14) -0.0022(11) 0.0036(11) -0.0018(10) N1 0.0161(11) 0.0189(10) 0.0236(12) 0.0014(9) 0.0051(9) -0.0010(8) N2 0.0165(11) 0.0232(11) 0.0261(13) -0.0016(10) 0.0058(9) -0.0001(9) N3 0.0149(11) 0.0596(18) 0.0215(13) 0.0036(12) 0.0030(10) -0.0078(11) O1 0.0169(9) 0.0406(12) 0.0217(11) 0.0024(9) 0.0059(8) -0.0030(8) Cu1 0.0126(2) 0.0196(3) 0.0268(3) 0.000 0.00376(19) 0.000 C17 0.0941(19) 0.0881(18) 0.0921(19) 0.0056(14) 0.0404(16) 0.0049(14) C18 0.0941(19) 0.0881(18) 0.0921(19) 0.0056(14) 0.0404(16) 0.0049(14) C19 0.0941(19) 0.0881(18) 0.0921(19) 0.0056(14) 0.0404(16) 0.0049(14) C20 0.0941(19) 0.0881(18) 0.0921(19) 0.0056(14) 0.0404(16) 0.0049(14) O2 0.0941(19) 0.0881(18) 0.0921(19) 0.0056(14) 0.0404(16) 0.0049(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(4) . ? C1 C2 1.406(4) . ? C1 H1 0.9300 . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C3 C4 1.418(4) . ? C3 H3 0.9300 . ? C4 N1 1.402(3) . ? C4 C5 1.406(4) . ? C5 C6 1.394(4) . ? C5 C10 1.491(4) . ? C6 N2 1.390(3) . ? C6 C7 1.427(4) . ? C7 C8 1.372(4) . ? C7 H7 0.9300 . ? C8 C9 1.413(4) . ? C8 H8 0.9300 . ? C9 N2 1.337(4) . ? C9 H9 0.9300 . ? C10 C15 1.388(4) . ? C10 C11 1.399(4) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 C13 1.387(4) . ? C12 H12 0.9300 . ? C13 C14 1.394(4) . ? C13 C16 1.499(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.241(3) . ? C16 N3 1.327(4) . ? N1 Cu1 1.961(2) . ? N2 Cu1 1.943(2) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? Cu1 N2 1.943(2) 2 ? Cu1 N1 1.961(2) 2 ? C17 O2 1.377(7) . ? C17 C18 1.485(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.512(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.495(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O2 1.388(8) . ? C20 H20A 0.9700 . ? C20 H20B 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 C1 C2 111.5(2) . . ? N1 C1 H1 124.2 . . ? C2 C1 H1 124.2 . . ? C3 C2 C1 106.5(2) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.2(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 124.1(2) . . ? N1 C4 C3 108.6(2) . . ? C5 C4 C3 127.2(2) . . ? C6 C5 C4 125.6(2) . . ? C6 C5 C10 116.0(2) . . ? C4 C5 C10 118.4(2) . . ? N2 C6 C5 123.5(2) . . ? N2 C6 C7 108.4(2) . . ? C5 C6 C7 128.1(3) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.0(3) . . ? C7 C8 H8 127.0 . . ? C9 C8 H8 127.0 . . ? N2 C9 C8 111.6(3) . . ? N2 C9 H9 124.2 . . ? C8 C9 H9 124.2 . . ? C15 C10 C11 119.1(2) . . ? C15 C10 C5 121.9(2) . . ? C11 C10 C5 118.9(3) . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 119.2(3) . . ? C12 C13 C16 119.1(2) . . ? C14 C13 C16 121.7(3) . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 120.4(3) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? O1 C16 N3 122.5(3) . . ? O1 C16 C13 120.1(3) . . ? N3 C16 C13 117.3(2) . . ? C1 N1 C4 106.3(2) . . ? C1 N1 Cu1 125.73(19) . . ? C4 N1 Cu1 125.44(18) . . ? C9 N2 C6 106.6(2) . . ? C9 N2 Cu1 125.8(2) . . ? C6 N2 Cu1 127.62(19) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N2 Cu1 N2 93.42(14) . 2 ? N2 Cu1 N1 146.79(10) . 2 ? N2 Cu1 N1 92.13(9) 2 2 ? N2 Cu1 N1 92.13(9) . . ? N2 Cu1 N1 146.79(10) 2 . ? N1 Cu1 N1 100.85(13) 2 . ? O2 C17 C18 109.2(6) . . ? O2 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O2 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? C17 C18 C19 104.4(5) . . ? C17 C18 H18A 110.9 . . ? C19 C18 H18A 110.9 . . ? C17 C18 H18B 110.9 . . ? C19 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? C20 C19 C18 103.1(6) . . ? C20 C19 H19A 111.1 . . ? C18 C19 H19A 111.1 . . ? C20 C19 H19B 111.1 . . ? C18 C19 H19B 111.1 . . ? H19A C19 H19B 109.1 . . ? O2 C20 C19 107.2(6) . . ? O2 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? O2 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C17 O2 C20 109.6(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.214 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.116 #===END ###Material relevant to compound 4CHCl3 at 173K ## data_compound4CHCl3 _database_code_depnum_ccdc_archive 'CCDC 717000' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 Cu N6 O2, C2 H2 Cl6' _chemical_formula_sum 'C34 H26 Cl6 Cu N6 O2' _chemical_formula_weight 826.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.9849(16) _cell_length_b 16.1578(13) _cell_length_c 10.2185(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.103(3) _cell_angle_gamma 90.00 _cell_volume 3646.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1156 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 21.02 _exptl_crystal_description rod _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7378 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details sadabs _exptl_special_details ; The chloroform solvate molecule is disordered over two positions which have been modeled accordingly ; _diffrn_ambient_temperature 173(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 13056 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1071 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4151 _reflns_number_gt 2249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1073P)^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 SHELXL _refine_ls_extinction_coef 0.0031(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4151 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.2011 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 C1 C 0.06144(19) 0.7413(3) 0.1865(4) 0.0305(10) Uani 1 1 d . . . H1 H 0.0253 0.7130 0.1511 0.037 Uiso 1 1 calc R . . C2 C 0.1178(2) 0.7144(3) 0.1758(5) 0.0354(11) Uani 1 1 d . . . H2 H 0.1255 0.6664 0.1332 0.042 Uiso 1 1 calc R . . C3 C 0.15909(19) 0.7719(3) 0.2395(4) 0.0322(10) Uani 1 1 d . . . H3 H 0.2004 0.7707 0.2482 0.039 Uiso 1 1 calc R . . C4 C 0.12787(18) 0.8338(3) 0.2900(4) 0.0265(9) Uani 1 1 d . . . C5 C 0.15168(19) 0.9080(3) 0.3532(4) 0.0301(10) Uani 1 1 d . . . C6 C 0.11810(19) 0.9725(3) 0.3885(4) 0.0293(10) Uani 1 1 d . . . C7 C 0.1396(2) 1.0459(3) 0.4636(4) 0.0352(11) Uani 1 1 d . . . H7 H 0.1799 1.0614 0.4986 0.042 Uiso 1 1 calc R . . C8 C 0.0900(2) 1.0895(3) 0.4748(5) 0.0379(11) Uani 1 1 d . . . H8 H 0.0901 1.1395 0.5200 0.045 Uiso 1 1 calc R . . C9 C 0.0387(2) 1.0432(3) 0.4040(4) 0.0336(11) Uani 1 1 d . . . H9 H -0.0011 1.0594 0.3936 0.040 Uiso 1 1 calc R . . C10 C 0.21825(18) 0.9247(3) 0.3815(4) 0.0280(10) Uani 1 1 d . . . C11 C 0.2381(2) 0.9865(3) 0.3098(5) 0.0347(11) Uani 1 1 d . . . H11 H 0.2100 1.0164 0.2437 0.042 Uiso 1 1 calc R . . C12 C 0.2987(2) 1.0043(3) 0.3353(5) 0.0340(11) Uani 1 1 d . . . H12 H 0.3113 1.0448 0.2846 0.041 Uiso 1 1 calc R . . C13 C 0.34122(18) 0.9618(3) 0.4364(4) 0.0284(10) Uani 1 1 d . . . C14 C 0.32174(19) 0.8988(3) 0.5079(4) 0.0338(11) Uani 1 1 d . . . H14 H 0.3498 0.8690 0.5743 0.041 Uiso 1 1 calc R . . C15 C 0.26078(19) 0.8810(3) 0.4797(5) 0.0347(11) Uani 1 1 d . . . H15 H 0.2481 0.8389 0.5275 0.042 Uiso 1 1 calc R . . C16 C 0.40718(18) 0.9832(3) 0.4625(4) 0.0295(10) Uani 1 1 d . . . N1 N 0.06632(15) 0.8135(2) 0.2548(3) 0.0273(8) Uani 1 1 d . . . N2 N 0.05503(15) 0.9724(2) 0.3533(4) 0.0295(8) Uani 1 1 d . . . N3 N 0.44262(16) 0.9713(3) 0.5882(4) 0.0448(11) Uani 1 1 d . . . H3A H 0.4807 0.9820 0.6071 0.054 Uiso 1 1 calc R . . H3B H 0.4274 0.9529 0.6506 0.054 Uiso 1 1 calc R . . O1 O 0.42660(13) 1.0096(2) 0.3686(3) 0.0355(8) Uani 1 1 d . . . Cu1 Cu 0.0000 0.89011(5) 0.2500 0.0300(3) Uani 1 2 d S . . C17 C 0.1189(4) 0.7582(5) 0.7693(9) 0.106(3) Uani 1 1 d . . . H17 H 0.1188 0.8018 0.8358 0.127 Uiso 1 1 calc R A 1 Cl1A Cl 0.1309(8) 0.7996(6) 0.6359(14) 0.208(7) Uani 0.502(7) 1 d P B 1 Cl2A Cl 0.1722(3) 0.6901(5) 0.8397(5) 0.153(4) Uani 0.502(7) 1 d P B 1 Cl3A Cl 0.0484(4) 0.7053(4) 0.7307(11) 0.213(4) Uani 0.502(7) 1 d P . 1 Cl1B Cl 0.1035(6) 0.7983(9) 0.6094(12) 0.197(6) Uani 0.498(7) 1 d P B 2 Cl2B Cl 0.2006(3) 0.7699(5) 0.8577(8) 0.167(3) Uani 0.498(7) 1 d P B 2 Cl3B Cl 0.1034(3) 0.6605(3) 0.7867(5) 0.111(3) Uani 0.498(7) 1 d P B 2 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 C1 0.024(2) 0.025(2) 0.041(3) 0.000(2) 0.0076(19) -0.0034(19) C2 0.035(3) 0.028(3) 0.045(3) 0.005(2) 0.015(2) 0.006(2) C3 0.027(2) 0.034(3) 0.036(3) 0.009(2) 0.0085(19) 0.006(2) C4 0.019(2) 0.030(2) 0.030(2) 0.0032(19) 0.0043(17) -0.0015(18) C5 0.024(2) 0.039(3) 0.028(2) 0.0081(19) 0.0091(18) 0.002(2) C6 0.025(2) 0.036(3) 0.027(2) 0.0043(19) 0.0071(18) -0.004(2) C7 0.033(2) 0.038(3) 0.033(3) 0.000(2) 0.006(2) -0.009(2) C8 0.045(3) 0.037(3) 0.033(3) -0.006(2) 0.014(2) -0.006(2) C9 0.033(2) 0.034(3) 0.037(3) -0.001(2) 0.015(2) 0.002(2) C10 0.022(2) 0.031(2) 0.028(2) 0.0005(19) 0.0020(17) -0.0030(19) C11 0.027(2) 0.038(3) 0.034(3) 0.008(2) 0.0008(19) -0.002(2) C12 0.028(2) 0.035(3) 0.038(3) 0.009(2) 0.008(2) -0.005(2) C13 0.024(2) 0.037(3) 0.025(2) -0.0005(19) 0.0086(18) -0.0039(19) C14 0.023(2) 0.044(3) 0.033(2) 0.009(2) 0.0054(18) 0.003(2) C15 0.025(2) 0.043(3) 0.036(3) 0.010(2) 0.0082(19) 0.001(2) C16 0.022(2) 0.034(3) 0.031(2) -0.002(2) 0.0050(18) -0.0011(19) N1 0.0214(18) 0.027(2) 0.032(2) 0.0007(16) 0.0058(15) -0.0020(16) N2 0.0248(18) 0.030(2) 0.035(2) 0.0011(16) 0.0098(16) 0.0020(17) N3 0.0178(18) 0.085(4) 0.028(2) 0.005(2) 0.0011(16) -0.005(2) O1 0.0252(16) 0.051(2) 0.0308(17) 0.0028(15) 0.0088(13) -0.0047(15) Cu1 0.0223(4) 0.0304(5) 0.0373(5) 0.000 0.0083(3) 0.000 C17 0.149(8) 0.071(5) 0.134(7) -0.016(5) 0.100(7) -0.013(6) Cl1A 0.383(19) 0.097(5) 0.239(14) 0.043(6) 0.248(14) 0.018(8) Cl2A 0.169(7) 0.205(9) 0.088(4) -0.010(4) 0.039(4) 0.055(7) Cl3A 0.155(7) 0.107(5) 0.381(13) 0.018(7) 0.079(8) -0.011(5) Cl1B 0.252(11) 0.262(12) 0.101(5) 0.097(6) 0.088(6) 0.160(10) Cl2B 0.104(4) 0.153(6) 0.271(9) -0.088(6) 0.094(5) 0.003(4) Cl3B 0.175(7) 0.060(3) 0.121(4) -0.012(3) 0.079(4) -0.017(3) _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 C1 N1 1.349(5) . ? C1 C2 1.398(6) . ? C1 H1 0.9300 . ? C2 C3 1.359(6) . ? C2 H2 0.9300 . ? C3 C4 1.409(6) . ? C3 H3 0.9300 . ? C4 N1 1.398(5) . ? C4 C5 1.399(6) . ? C5 C6 1.402(6) . ? C5 C10 1.501(6) . ? C6 N2 1.393(5) . ? C6 C7 1.424(6) . ? C7 C8 1.371(6) . ? C7 H7 0.9300 . ? C8 C9 1.415(6) . ? C8 H8 0.9300 . ? C9 N2 1.350(5) . ? C9 H9 0.9300 . ? C10 C15 1.384(6) . ? C10 C11 1.389(6) . ? C11 C12 1.375(6) . ? C11 H11 0.9300 . ? C12 C13 1.391(6) . ? C12 H12 0.9300 . ? C13 C14 1.397(6) . ? C13 C16 1.505(6) . ? C14 C15 1.380(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.240(5) . ? C16 N3 1.331(5) . ? N1 Cu1 1.953(3) . ? N2 Cu1 1.934(4) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? Cu1 N2 1.934(4) 2 ? Cu1 N1 1.953(3) 2 ? C17 Cl1A 1.609(12) . ? C17 Cl3B 1.638(9) . ? C17 Cl2A 1.655(10) . ? C17 Cl1B 1.701(13) . ? C17 Cl3A 1.776(10) . ? C17 Cl2B 1.854(12) . ? C17 H17 0.9800 . ? Cl3A Cl3A 2.365(16) 2_556 ? 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 C1 C2 111.3(4) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 106.8(4) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 107.5(4) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N1 C4 C5 123.9(4) . . ? N1 C4 C3 108.8(4) . . ? C5 C4 C3 127.1(4) . . ? C4 C5 C6 125.7(4) . . ? C4 C5 C10 119.4(4) . . ? C6 C5 C10 114.9(4) . . ? N2 C6 C5 122.7(4) . . ? N2 C6 C7 108.7(4) . . ? C5 C6 C7 128.6(4) . . ? C8 C7 C6 107.5(4) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.2(4) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 111.3(4) . . ? N2 C9 H9 124.3 . . ? C8 C9 H9 124.3 . . ? C15 C10 C11 118.7(4) . . ? C15 C10 C5 121.7(4) . . ? C11 C10 C5 119.6(4) . . ? C12 C11 C10 120.9(4) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 119.2(4) . . ? C12 C13 C16 118.9(4) . . ? C14 C13 C16 121.9(4) . . ? C15 C14 C13 119.8(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 121.1(4) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O1 C16 N3 122.8(4) . . ? O1 C16 C13 120.2(4) . . ? N3 C16 C13 117.0(4) . . ? C1 N1 C4 105.6(3) . . ? C1 N1 Cu1 125.6(3) . . ? C4 N1 Cu1 125.8(3) . . ? C9 N2 C6 106.2(4) . . ? C9 N2 Cu1 125.6(3) . . ? C6 N2 Cu1 128.1(3) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N2 Cu1 N2 93.1(2) . 2 ? N2 Cu1 N1 146.79(14) . 2 ? N2 Cu1 N1 91.95(14) 2 2 ? N2 Cu1 N1 91.95(14) . . ? N2 Cu1 N1 146.79(14) 2 . ? N1 Cu1 N1 101.4(2) 2 . ? Cl1A C17 Cl3B 125.9(7) . . ? Cl1A C17 Cl2A 111.4(7) . . ? Cl3B C17 Cl2A 58.0(5) . . ? Cl1A C17 Cl1B 21.1(9) . . ? Cl3B C17 Cl1B 118.5(8) . . ? Cl2A C17 Cl1B 127.1(6) . . ? Cl1A C17 Cl3A 111.8(9) . . ? Cl3B C17 Cl3A 49.3(4) . . ? Cl2A C17 Cl3A 107.2(6) . . ? Cl1B C17 Cl3A 92.1(8) . . ? Cl1A C17 Cl2B 89.0(8) . . ? Cl3B C17 Cl2B 105.5(7) . . ? Cl2A C17 Cl2B 47.8(4) . . ? Cl1B C17 Cl2B 110.0(7) . . ? Cl3A C17 Cl2B 153.6(7) . . ? Cl1A C17 H17 108.8 . . ? Cl3B C17 H17 125.1 . . ? Cl2A C17 H17 108.8 . . ? Cl1B C17 H17 110.6 . . ? Cl3A C17 H17 108.8 . . ? Cl2B C17 H17 77.6 . . ? C17 Cl3A Cl3A 143.7(6) . 2_556 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.673 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.131 #===END ###Material relevant to compound 5 at 173K ## data_compound5 _database_code_depnum_ccdc_archive 'CCDC 717001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 N6 O2 Zn, 2(C4 H8 O2)' _chemical_formula_sum 'C40 H40 N6 O6 Zn' _chemical_formula_weight 766.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2840 1.4300 '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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9609(3) _cell_length_b 13.6458(3) _cell_length_c 14.1783(3) _cell_angle_alpha 103.3150(10) _cell_angle_beta 97.276(2) _cell_angle_gamma 95.440(2) _cell_volume 1844.86(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4338 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8632 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 19542 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8216 _reflns_number_gt 6104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0656P)^2^+3.5041P] 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 ? _refine_ls_number_reflns 8216 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1781 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 C1 C 0.5008(4) 0.1719(3) 0.2269(3) 0.0444(10) Uani 1 1 d . . . H1 H 0.5424 0.2254 0.2060 0.053 Uiso 1 1 calc R . . C2 C 0.5633(4) 0.0861(4) 0.2387(3) 0.0454(10) Uani 1 1 d . . . H2 H 0.6497 0.0725 0.2257 0.055 Uiso 1 1 calc R . . C3 C 0.4719(4) 0.0271(3) 0.2727(3) 0.0362(9) Uani 1 1 d . . . H3 H 0.4847 -0.0342 0.2885 0.043 Uiso 1 1 calc R . . C4 C 0.3534(4) 0.0772(3) 0.2797(2) 0.0273(7) Uani 1 1 d . . . C5 C 0.2322(4) 0.0438(2) 0.3097(2) 0.0252(7) Uani 1 1 d . . . C6 C 0.1116(4) 0.0891(3) 0.3093(2) 0.0278(7) Uani 1 1 d . . . C7 C -0.0038(4) 0.0643(3) 0.3525(3) 0.0350(8) Uani 1 1 d . . . H7 H -0.0172 0.0106 0.3819 0.042 Uiso 1 1 calc R . . C8 C -0.0919(5) 0.1341(4) 0.3429(3) 0.0452(10) Uani 1 1 d . . . H8 H -0.1759 0.1373 0.3649 0.054 Uiso 1 1 calc R . . C9 C -0.0304(5) 0.1993(3) 0.2937(3) 0.0445(10) Uani 1 1 d . . . H9 H -0.0691 0.2537 0.2773 0.053 Uiso 1 1 calc R . . C10 C 0.2342(4) -0.0476(2) 0.3507(2) 0.0255(7) Uani 1 1 d . . . C11 C 0.3190(4) -0.0422(3) 0.4379(2) 0.0275(7) Uani 1 1 d . . . H11 H 0.3743 0.0181 0.4698 0.033 Uiso 1 1 calc R . . C12 C 0.3222(4) -0.1255(3) 0.4777(2) 0.0279(7) Uani 1 1 d . . . H12 H 0.3804 -0.1212 0.5357 0.034 Uiso 1 1 calc R . . C13 C 0.2382(4) -0.2162(2) 0.4311(2) 0.0248(7) Uani 1 1 d . . . C14 C 0.1523(4) -0.2211(3) 0.3451(3) 0.0316(8) Uani 1 1 d . . . H14 H 0.0949 -0.2807 0.3140 0.038 Uiso 1 1 calc R . . C15 C 0.1509(4) -0.1380(3) 0.3049(3) 0.0331(8) Uani 1 1 d . . . H15 H 0.0937 -0.1426 0.2464 0.040 Uiso 1 1 calc R . . C16 C 0.2370(4) -0.3056(3) 0.4759(2) 0.0296(8) Uani 1 1 d . . . C17 C 0.2796(5) 0.4588(3) 0.2775(3) 0.0406(9) Uani 1 1 d . . . H17 H 0.2895 0.4562 0.3429 0.049 Uiso 1 1 calc R . . C18 C 0.2978(5) 0.5484(3) 0.2460(3) 0.0416(10) Uani 1 1 d . . . H18 H 0.3205 0.6140 0.2855 0.050 Uiso 1 1 calc R . . C19 C 0.2754(4) 0.5207(3) 0.1456(3) 0.0365(9) Uani 1 1 d . . . H19 H 0.2809 0.5640 0.1039 0.044 Uiso 1 1 calc R . . C20 C 0.2422(4) 0.4137(2) 0.1171(2) 0.0291(8) Uani 1 1 d . . . C21 C 0.2098(4) 0.3528(3) 0.0212(3) 0.0293(7) Uani 1 1 d . . . C22 C 0.1789(4) 0.2476(3) -0.0084(2) 0.0286(7) Uani 1 1 d . . . C23 C 0.1483(4) 0.1853(3) -0.1055(3) 0.0347(8) Uani 1 1 d . . . H23 H 0.1415 0.2076 -0.1630 0.042 Uiso 1 1 calc R . . C24 C 0.1306(5) 0.0862(3) -0.0991(3) 0.0407(9) Uani 1 1 d . . . H24 H 0.1097 0.0284 -0.1508 0.049 Uiso 1 1 calc R . . C25 C 0.1507(5) 0.0899(3) 0.0016(3) 0.0394(9) Uani 1 1 d . . . H25 H 0.1452 0.0328 0.0269 0.047 Uiso 1 1 calc R . . C26 C 0.2106(4) 0.4060(3) -0.0609(2) 0.0294(8) Uani 1 1 d . . . C27 C 0.3326(4) 0.4342(3) -0.0909(3) 0.0359(9) Uani 1 1 d . . . H27 H 0.4147 0.4235 -0.0581 0.043 Uiso 1 1 calc R . . C28 C 0.3323(4) 0.4784(3) -0.1698(3) 0.0361(9) Uani 1 1 d . . . H28 H 0.4145 0.4973 -0.1894 0.043 Uiso 1 1 calc R . . C29 C 0.2107(4) 0.4947(3) -0.2195(2) 0.0296(8) Uani 1 1 d . . . C30 C 0.0895(4) 0.4683(3) -0.1886(3) 0.0354(9) Uani 1 1 d . . . H30 H 0.0076 0.4798 -0.2211 0.042 Uiso 1 1 calc R . . C31 C 0.0890(4) 0.4249(3) -0.1092(3) 0.0368(9) Uani 1 1 d . . . H31 H 0.0069 0.4082 -0.0883 0.044 Uiso 1 1 calc R . . N1 N 0.3757(3) 0.1672(2) 0.2494(2) 0.0334(7) Uani 1 1 d . . . N2 N 0.0909(3) 0.1741(2) 0.2729(2) 0.0333(7) Uani 1 1 d . . . N3 N 0.3518(3) -0.3139(3) 0.5300(2) 0.0403(8) Uani 1 1 d . . . H3A H 0.3557 -0.3630 0.5585 0.048 Uiso 1 1 calc R . . H3B H 0.4226 -0.2701 0.5367 0.048 Uiso 1 1 calc R . . N4 N 0.2466(4) 0.3775(2) 0.2021(2) 0.0352(7) Uani 1 1 d . . . N5 N 0.1783(3) 0.1844(2) 0.0564(2) 0.0329(7) Uani 1 1 d . . . N6 N 0.1066(4) 0.5258(3) -0.3730(2) 0.0407(8) Uani 1 1 d . . . H6A H 0.1077 0.5510 -0.4232 0.049 Uiso 1 1 calc R . . H6B H 0.0333 0.4915 -0.3656 0.049 Uiso 1 1 calc R . . O1 O 0.1317(3) -0.36662(19) 0.46357(19) 0.0361(6) Uani 1 1 d . . . O2 O 0.3257(3) 0.5883(3) -0.3137(2) 0.0556(9) Uani 1 1 d . . . Zn1 Zn 0.22148(5) 0.23329(3) 0.20131(3) 0.03549(15) Uani 1 1 d . . . C32 C 0.2185(4) 0.5399(3) -0.3064(3) 0.0351(9) Uani 1 1 d . . . C33 C 0.6853(5) 0.8185(5) 0.3136(4) 0.0605(14) Uani 1 1 d . . . H33A H 0.6615 0.8162 0.2446 0.073 Uiso 1 1 calc R . . H33B H 0.7032 0.8892 0.3497 0.073 Uiso 1 1 calc R . . C34 C 0.5691(5) 0.7665(4) 0.3480(4) 0.0571(13) Uani 1 1 d . . . H34A H 0.4881 0.7989 0.3364 0.069 Uiso 1 1 calc R . . H34B H 0.5501 0.6961 0.3110 0.069 Uiso 1 1 calc R . . C35 C 0.7203(6) 0.7242(4) 0.4665(4) 0.0604(13) Uani 1 1 d . . . H35A H 0.7024 0.6525 0.4337 0.072 Uiso 1 1 calc R . . H35B H 0.7447 0.7302 0.5362 0.072 Uiso 1 1 calc R . . C36 C 0.8371(5) 0.7727(5) 0.4289(4) 0.0601(13) Uani 1 1 d . . . H36A H 0.8609 0.8426 0.4664 0.072 Uiso 1 1 calc R . . H36B H 0.9158 0.7374 0.4384 0.072 Uiso 1 1 calc R . . O3 O 0.6001(3) 0.7707(2) 0.4499(2) 0.0487(7) Uani 1 1 d . . . O4 O 0.8048(3) 0.7705(3) 0.3278(2) 0.0571(9) Uani 1 1 d . . . C37 C 0.7575(9) 0.2773(8) -0.0283(8) 0.1313(18) Uani 1 1 d . . . H37A H 0.7503 0.3337 0.0260 0.158 Uiso 1 1 calc R . . H37B H 0.8211 0.3009 -0.0672 0.158 Uiso 1 1 calc R . . C38 C 0.8090(9) 0.1940(8) 0.0100(8) 0.1313(18) Uani 1 1 d . . . H38A H 0.8440 0.1486 -0.0419 0.158 Uiso 1 1 calc R . . H38B H 0.8844 0.2222 0.0626 0.158 Uiso 1 1 calc R . . C39 C 0.5888(9) 0.1191(9) -0.0084(8) 0.1313(18) Uani 1 1 d . . . H39A H 0.5217 0.0921 0.0261 0.158 Uiso 1 1 calc R . . H39B H 0.5925 0.0674 -0.0675 0.158 Uiso 1 1 calc R . . C40 C 0.5456(9) 0.2014(8) -0.0348(8) 0.1313(18) Uani 1 1 d . . . H40A H 0.5342 0.2512 0.0237 0.158 Uiso 1 1 calc R . . H40B H 0.4572 0.1814 -0.0759 0.158 Uiso 1 1 calc R . . O5 O 0.7068(8) 0.1355(5) 0.0465(4) 0.122(2) Uani 1 1 d . . . O6 O 0.6335(8) 0.2452(6) -0.0842(5) 0.153(3) 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 C1 0.038(2) 0.060(3) 0.038(2) 0.0260(19) 0.0020(18) -0.014(2) C2 0.031(2) 0.071(3) 0.037(2) 0.021(2) 0.0046(17) 0.001(2) C3 0.034(2) 0.046(2) 0.0314(18) 0.0155(16) 0.0019(16) 0.0054(17) C4 0.032(2) 0.0291(17) 0.0220(15) 0.0112(13) 0.0019(14) 0.0019(14) C5 0.0320(19) 0.0228(15) 0.0207(14) 0.0088(12) 0.0006(13) -0.0004(13) C6 0.032(2) 0.0301(17) 0.0231(15) 0.0110(13) 0.0034(14) 0.0047(15) C7 0.034(2) 0.044(2) 0.0271(17) 0.0104(15) 0.0050(15) 0.0022(17) C8 0.038(2) 0.064(3) 0.033(2) 0.0056(19) 0.0067(18) 0.014(2) C9 0.049(3) 0.049(2) 0.039(2) 0.0123(18) 0.0059(19) 0.024(2) C10 0.0283(19) 0.0252(16) 0.0248(15) 0.0110(13) 0.0031(14) 0.0024(14) C11 0.032(2) 0.0248(16) 0.0240(16) 0.0087(13) -0.0014(14) -0.0040(14) C12 0.032(2) 0.0289(17) 0.0237(16) 0.0119(13) 0.0023(14) -0.0017(14) C13 0.0293(19) 0.0234(15) 0.0249(15) 0.0108(12) 0.0075(14) 0.0040(13) C14 0.037(2) 0.0258(17) 0.0300(17) 0.0089(14) -0.0012(15) -0.0023(15) C15 0.037(2) 0.0309(18) 0.0290(17) 0.0122(14) -0.0068(15) -0.0023(15) C16 0.038(2) 0.0277(17) 0.0266(16) 0.0121(13) 0.0080(15) 0.0032(15) C17 0.056(3) 0.035(2) 0.0295(18) 0.0067(15) 0.0084(18) 0.0006(18) C18 0.047(3) 0.0258(18) 0.050(2) 0.0045(16) 0.013(2) 0.0024(17) C19 0.041(2) 0.0279(18) 0.046(2) 0.0167(16) 0.0133(18) 0.0060(16) C20 0.037(2) 0.0235(16) 0.0293(17) 0.0115(13) 0.0041(15) 0.0042(14) C21 0.031(2) 0.0306(17) 0.0316(17) 0.0173(14) 0.0056(15) 0.0043(15) C22 0.030(2) 0.0303(17) 0.0268(16) 0.0125(14) -0.0002(14) 0.0036(14) C23 0.037(2) 0.040(2) 0.0258(17) 0.0100(15) -0.0009(15) 0.0035(17) C24 0.048(3) 0.037(2) 0.0321(19) 0.0020(16) 0.0007(18) 0.0052(18) C25 0.052(3) 0.0253(17) 0.040(2) 0.0118(15) 0.0017(19) 0.0009(17) C26 0.038(2) 0.0271(16) 0.0265(16) 0.0130(13) 0.0047(15) 0.0040(15) C27 0.031(2) 0.042(2) 0.041(2) 0.0246(17) 0.0040(17) 0.0042(17) C28 0.034(2) 0.041(2) 0.039(2) 0.0223(17) 0.0036(17) -0.0001(17) C29 0.036(2) 0.0246(16) 0.0290(17) 0.0116(13) 0.0036(15) 0.0001(14) C30 0.034(2) 0.042(2) 0.0368(19) 0.0227(16) 0.0035(16) 0.0051(17) C31 0.033(2) 0.045(2) 0.041(2) 0.0258(18) 0.0064(17) 0.0072(17) N1 0.0350(18) 0.0349(16) 0.0326(15) 0.0176(13) 0.0036(13) -0.0054(13) N2 0.0402(19) 0.0338(16) 0.0300(15) 0.0141(13) 0.0046(14) 0.0111(14) N3 0.0363(19) 0.0424(18) 0.050(2) 0.0325(16) 0.0018(15) -0.0026(15) N4 0.054(2) 0.0254(14) 0.0270(14) 0.0107(12) 0.0036(14) 0.0039(14) N5 0.046(2) 0.0260(14) 0.0276(15) 0.0119(12) 0.0020(14) 0.0011(13) N6 0.043(2) 0.0475(19) 0.0359(17) 0.0264(15) -0.0005(15) -0.0069(16) O1 0.0417(16) 0.0293(13) 0.0384(14) 0.0173(11) 0.0016(12) -0.0060(12) O2 0.051(2) 0.067(2) 0.0519(18) 0.0413(16) -0.0072(15) -0.0223(16) Zn1 0.0536(3) 0.0277(2) 0.0277(2) 0.01471(17) 0.00268(19) 0.00291(19) C32 0.048(2) 0.0299(18) 0.0292(18) 0.0153(14) 0.0008(17) 0.0011(17) C33 0.045(3) 0.097(4) 0.047(3) 0.026(3) 0.015(2) 0.020(3) C34 0.040(3) 0.072(3) 0.051(3) 0.001(2) 0.004(2) 0.006(2) C35 0.060(3) 0.059(3) 0.072(3) 0.027(3) 0.019(3) 0.022(3) C36 0.044(3) 0.084(4) 0.050(3) 0.011(3) 0.005(2) 0.013(3) O3 0.0438(19) 0.0522(18) 0.0569(19) 0.0187(15) 0.0199(15) 0.0114(14) O4 0.0402(19) 0.090(3) 0.0400(16) 0.0089(16) 0.0101(14) 0.0135(17) C37 0.083(3) 0.169(5) 0.159(4) 0.075(4) 0.022(3) 0.008(3) C38 0.083(3) 0.169(5) 0.159(4) 0.075(4) 0.022(3) 0.008(3) C39 0.083(3) 0.169(5) 0.159(4) 0.075(4) 0.022(3) 0.008(3) C40 0.083(3) 0.169(5) 0.159(4) 0.075(4) 0.022(3) 0.008(3) O5 0.168(6) 0.122(4) 0.126(4) 0.084(4) 0.073(4) 0.063(4) O6 0.140(6) 0.194(7) 0.186(7) 0.149(6) 0.038(5) 0.055(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 C1 N1 1.324(5) . ? C1 C2 1.410(6) . ? C1 H1 0.9300 . ? C2 C3 1.365(6) . ? C2 H2 0.9300 . ? C3 C4 1.421(5) . ? C3 H3 0.9300 . ? C4 N1 1.399(4) . ? C4 C5 1.400(5) . ? C5 C6 1.402(5) . ? C5 C10 1.494(4) . ? C6 N2 1.396(4) . ? C6 C7 1.418(5) . ? C7 C8 1.373(6) . ? C7 H7 0.9300 . ? C8 C9 1.395(6) . ? C8 H8 0.9300 . ? C9 N2 1.337(5) . ? C9 H9 0.9300 . ? C10 C11 1.389(4) . ? C10 C15 1.390(5) . ? C11 C12 1.381(4) . ? C11 H11 0.9300 . ? C12 C13 1.399(5) . ? C12 H12 0.9300 . ? C13 C14 1.382(5) . ? C13 C16 1.500(4) . ? C14 C15 1.381(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.243(4) . ? C16 N3 1.323(5) . ? C17 N4 1.333(5) . ? C17 C18 1.400(5) . ? C17 H17 0.9300 . ? C18 C19 1.368(6) . ? C18 H18 0.9300 . ? C19 C20 1.417(5) . ? C19 H19 0.9300 . ? C20 C21 1.401(5) . ? C20 N4 1.401(4) . ? C21 C22 1.393(5) . ? C21 C26 1.508(4) . ? C22 N5 1.397(4) . ? C22 C23 1.420(5) . ? C23 C24 1.373(5) . ? C23 H23 0.9300 . ? C24 C25 1.405(5) . ? C24 H24 0.9300 . ? C25 N5 1.326(5) . ? C25 H25 0.9300 . ? C26 C27 1.387(5) . ? C26 C31 1.390(5) . ? C27 C28 1.387(5) . ? C27 H27 0.9300 . ? C28 C29 1.386(5) . ? C28 H28 0.9300 . ? C29 C30 1.380(5) . ? C29 C32 1.506(4) . ? C30 C31 1.388(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? N1 Zn1 1.979(3) . ? N2 Zn1 1.972(3) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 Zn1 1.957(3) . ? N5 Zn1 1.985(3) . ? N6 C32 1.334(5) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O2 C32 1.231(5) . ? C33 O4 1.426(6) . ? C33 C34 1.492(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O3 1.425(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 O3 1.426(6) . ? C35 C36 1.499(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O4 1.421(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O6 1.355(10) . ? C37 C38 1.475(12) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O5 1.453(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 O5 1.295(10) . ? C39 C40 1.353(12) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 O6 1.366(10) . ? C40 H40A 0.9700 . ? C40 H40B 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 C1 C2 111.8(4) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C3 C2 C1 106.5(4) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.0(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 124.3(3) . . ? N1 C4 C3 108.5(3) . . ? C5 C4 C3 127.2(3) . . ? C4 C5 C6 127.2(3) . . ? C4 C5 C10 116.1(3) . . ? C6 C5 C10 116.6(3) . . ? N2 C6 C5 124.5(3) . . ? N2 C6 C7 108.1(3) . . ? C5 C6 C7 127.2(3) . . ? C8 C7 C6 107.4(4) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.3(4) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 111.8(4) . . ? N2 C9 H9 124.1 . . ? C8 C9 H9 124.1 . . ? C11 C10 C15 118.8(3) . . ? C11 C10 C5 119.6(3) . . ? C15 C10 C5 121.7(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 C16 120.4(3) . . ? C12 C13 C16 120.5(3) . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 120.8(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? O1 C16 N3 122.8(3) . . ? O1 C16 C13 120.7(3) . . ? N3 C16 C13 116.5(3) . . ? N4 C17 C18 111.7(3) . . ? N4 C17 H17 124.1 . . ? C18 C17 H17 124.1 . . ? C19 C18 C17 106.6(3) . . ? C19 C18 H18 126.7 . . ? C17 C18 H18 126.7 . . ? C18 C19 C20 107.2(3) . . ? C18 C19 H19 126.4 . . ? C20 C19 H19 126.4 . . ? C21 C20 N4 124.8(3) . . ? C21 C20 C19 126.9(3) . . ? N4 C20 C19 108.3(3) . . ? C22 C21 C20 127.8(3) . . ? C22 C21 C26 115.2(3) . . ? C20 C21 C26 117.0(3) . . ? C21 C22 N5 123.9(3) . . ? C21 C22 C23 128.0(3) . . ? N5 C22 C23 108.1(3) . . ? C24 C23 C22 107.5(3) . . ? C24 C23 H23 126.2 . . ? C22 C23 H23 126.2 . . ? C23 C24 C25 105.8(3) . . ? C23 C24 H24 127.1 . . ? C25 C24 H24 127.1 . . ? N5 C25 C24 112.2(3) . . ? N5 C25 H25 123.9 . . ? C24 C25 H25 123.9 . . ? C27 C26 C31 119.2(3) . . ? C27 C26 C21 120.3(3) . . ? C31 C26 C21 120.5(3) . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 119.3(3) . . ? C30 C29 C32 123.2(3) . . ? C28 C29 C32 117.5(3) . . ? C29 C30 C31 120.4(4) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 120.3(4) . . ? C30 C31 H31 119.8 . . ? C26 C31 H31 119.9 . . ? C1 N1 C4 106.3(3) . . ? C1 N1 Zn1 128.0(2) . . ? C4 N1 Zn1 121.2(3) . . ? C9 N2 C6 106.4(3) . . ? C9 N2 Zn1 130.8(3) . . ? C6 N2 Zn1 122.8(3) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C17 N4 C20 106.2(3) . . ? C17 N4 Zn1 129.8(3) . . ? C20 N4 Zn1 123.9(2) . . ? C25 N5 C22 106.5(3) . . ? C25 N5 Zn1 129.1(2) . . ? C22 N5 Zn1 124.3(2) . . ? C32 N6 H6A 120.0 . . ? C32 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N4 Zn1 N2 123.50(14) . . ? N4 Zn1 N1 120.70(14) . . ? N2 Zn1 N1 94.70(12) . . ? N4 Zn1 N5 95.15(12) . . ? N2 Zn1 N5 114.30(13) . . ? N1 Zn1 N5 109.08(13) . . ? O2 C32 N6 122.4(3) . . ? O2 C32 C29 119.8(3) . . ? N6 C32 C29 117.9(3) . . ? O4 C33 C34 110.5(4) . . ? O4 C33 H33A 109.6 . . ? C34 C33 H33A 109.6 . . ? O4 C33 H33B 109.6 . . ? C34 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? O3 C34 C33 110.8(4) . . ? O3 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? O3 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? O3 C35 C36 111.2(4) . . ? O3 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? O3 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? O4 C36 C35 112.0(4) . . ? O4 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? O4 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C34 O3 C35 109.1(4) . . ? C36 O4 C33 109.0(4) . . ? O6 C37 C38 110.3(8) . . ? O6 C37 H37A 109.6 . . ? C38 C37 H37A 109.6 . . ? O6 C37 H37B 109.6 . . ? C38 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? O5 C38 C37 113.8(7) . . ? O5 C38 H38A 108.8 . . ? C37 C38 H38A 108.8 . . ? O5 C38 H38B 108.8 . . ? C37 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? O5 C39 C40 115.2(10) . . ? O5 C39 H39A 108.5 . . ? C40 C39 H39A 108.5 . . ? O5 C39 H39B 108.5 . . ? C40 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C39 C40 O6 113.0(9) . . ? C39 C40 H40A 109.0 . . ? O6 C40 H40A 109.0 . . ? C39 C40 H40B 109.0 . . ? O6 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C39 O5 C38 112.6(7) . . ? C37 O6 C40 111.0(8) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.786 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.087 #===END ###Material relevant to compound 6 at 173K ## data_compound6 _database_code_depnum_ccdc_archive 'CCDC 717002' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H38 Cu2 N6 O6, 1.5(C4 H8 O2)' _chemical_formula_sum 'C48 H50 Cu2 N6 O9' _chemical_formula_weight 982.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3200 1.2650 '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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5360(8) _cell_length_b 13.8314(4) _cell_length_c 14.2718(4) _cell_angle_alpha 111.8430(10) _cell_angle_beta 102.397(2) _cell_angle_gamma 104.374(2) _cell_volume 2258.09(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8214 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.53 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7326 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 36519 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.53 _reflns_number_total 10304 _reflns_number_gt 7866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0653P)^2^+1.0032P] 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 ? _refine_ls_number_reflns 10304 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1431 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 C1 C 0.2578(2) 0.3602(3) 0.6815(2) 0.0318(7) Uani 1 1 d . . . H1 H 0.2666 0.4353 0.7060 0.038 Uiso 1 1 calc R . . C2 C 0.1604(3) 0.2719(3) 0.6112(3) 0.0384(8) Uani 1 1 d . . . H2 H 0.0952 0.2776 0.5814 0.046 Uiso 1 1 calc R . . C3 C 0.1798(2) 0.1755(3) 0.5950(2) 0.0320(7) Uani 1 1 d . . . H3 H 0.1301 0.1029 0.5523 0.038 Uiso 1 1 calc R . . C4 C 0.2904(2) 0.2074(2) 0.6559(2) 0.0243(6) Uani 1 1 d . . . C5 C 0.3492(2) 0.1369(2) 0.6581(2) 0.0230(6) Uani 1 1 d . . . C6 C 0.4614(2) 0.1732(2) 0.7090(2) 0.0223(6) Uani 1 1 d . . . C7 C 0.5273(2) 0.1081(2) 0.7068(2) 0.0265(6) Uani 1 1 d . . . H7 H 0.5033 0.0304 0.6755 0.032 Uiso 1 1 calc R . . C8 C 0.6335(2) 0.1804(3) 0.7594(2) 0.0291(6) Uani 1 1 d . . . H8 H 0.6950 0.1616 0.7694 0.035 Uiso 1 1 calc R . . C9 C 0.6300(2) 0.2879(2) 0.7949(2) 0.0273(6) Uani 1 1 d . . . H9 H 0.6910 0.3531 0.8338 0.033 Uiso 1 1 calc R . . C10 C 0.2887(2) 0.0141(2) 0.5981(2) 0.0237(6) Uani 1 1 d . . . C11 C 0.3136(2) -0.0521(2) 0.5121(2) 0.0271(6) Uani 1 1 d . . . H11 H 0.3681 -0.0191 0.4915 0.033 Uiso 1 1 calc R . . C12 C 0.2578(2) -0.1663(2) 0.4574(2) 0.0285(6) Uani 1 1 d . . . H12 H 0.2750 -0.2095 0.4001 0.034 Uiso 1 1 calc R . . C13 C 0.1767(2) -0.2170(2) 0.4870(2) 0.0260(6) Uani 1 1 d . . . C14 C 0.1501(2) -0.1521(2) 0.5711(2) 0.0279(6) Uani 1 1 d . . . H14 H 0.0952 -0.1856 0.5910 0.033 Uiso 1 1 calc R . . C15 C 0.2052(2) -0.0368(2) 0.6259(2) 0.0269(6) Uani 1 1 d . . . H15 H 0.1861 0.0063 0.6815 0.032 Uiso 1 1 calc R . . C16 C 0.1177(2) -0.3407(2) 0.4230(2) 0.0301(7) Uani 1 1 d . . . C17 C 0.4197(3) 0.7067(3) 0.9664(3) 0.0490(9) Uani 1 1 d . . . H17A H 0.4062 0.7297 0.9107 0.074 Uiso 1 1 calc R . . H17B H 0.4599 0.7714 1.0343 0.074 Uiso 1 1 calc R . . H17C H 0.3519 0.6669 0.9687 0.074 Uiso 1 1 calc R . . C18 C 0.4843(3) 0.6319(3) 0.9439(3) 0.0360(7) Uani 1 1 d . . . C19 C 0.5837(3) 0.6601(3) 1.0190(3) 0.0381(8) Uani 1 1 d . . . H19 H 0.6076 0.7247 1.0834 0.046 Uiso 1 1 calc R . . C20 C 0.6500(3) 0.5968(3) 1.0035(2) 0.0339(7) Uani 1 1 d . . . C21 C 0.7615(3) 0.6405(3) 1.0855(3) 0.0471(9) Uani 1 1 d . . . H21A H 0.7707 0.5839 1.1062 0.071 Uiso 1 1 calc R . . H21B H 0.7693 0.7055 1.1474 0.071 Uiso 1 1 calc R . . H21C H 0.8154 0.6600 1.0549 0.071 Uiso 1 1 calc R . . C22 C 0.3907(2) 0.7543(3) 0.7197(2) 0.0341(7) Uani 1 1 d . . . H22 H 0.3292 0.6971 0.6648 0.041 Uiso 1 1 calc R . . C23 C 0.3952(3) 0.8628(3) 0.7807(3) 0.0387(8) Uani 1 1 d . . . H23 H 0.3389 0.8896 0.7731 0.046 Uiso 1 1 calc R . . C24 C 0.4980(2) 0.9213(3) 0.8531(3) 0.0341(7) Uani 1 1 d . . . H24 H 0.5247 0.9953 0.9051 0.041 Uiso 1 1 calc R . . C25 C 0.5567(2) 0.8478(2) 0.8344(2) 0.0265(6) Uani 1 1 d . . . C26 C 0.6650(2) 0.8707(2) 0.8894(2) 0.0258(6) Uani 1 1 d . . . C27 C 0.7171(2) 0.7927(2) 0.8715(2) 0.0264(6) Uani 1 1 d . . . C28 C 0.8274(2) 0.8125(3) 0.9192(2) 0.0312(7) Uani 1 1 d . . . H28 H 0.8807 0.8811 0.9691 0.037 Uiso 1 1 calc R . . C29 C 0.8414(3) 0.7127(3) 0.8790(3) 0.0366(7) Uani 1 1 d . . . H29 H 0.9056 0.6999 0.8965 0.044 Uiso 1 1 calc R . . C30 C 0.7403(2) 0.6335(3) 0.8064(2) 0.0323(7) Uani 1 1 d . . . H30 H 0.7271 0.5580 0.7675 0.039 Uiso 1 1 calc R . . C31 C 0.7309(2) 0.9871(2) 0.9748(2) 0.0270(6) Uani 1 1 d . . . C32 C 0.7411(2) 1.0772(2) 0.9510(2) 0.0313(7) Uani 1 1 d . . . H32 H 0.7070 1.0646 0.8814 0.038 Uiso 1 1 calc R . . C33 C 0.8011(2) 1.1846(2) 1.0293(2) 0.0315(7) Uani 1 1 d . . . H33 H 0.8069 1.2438 1.0118 0.038 Uiso 1 1 calc R . . C34 C 0.8529(2) 1.2062(2) 1.1338(2) 0.0265(6) Uani 1 1 d . . . C35 C 0.8444(2) 1.1163(2) 1.1574(2) 0.0306(7) Uani 1 1 d . . . H35 H 0.8796 1.1290 1.2267 0.037 Uiso 1 1 calc R . . C36 C 0.7844(2) 1.0085(2) 1.0794(2) 0.0306(7) Uani 1 1 d . . . H36 H 0.7796 0.9494 1.0967 0.037 Uiso 1 1 calc R . . C37 C 0.9179(2) 1.3223(2) 1.2219(2) 0.0310(7) Uani 1 1 d . . . C38 C 0.2231(3) 0.4106(3) 0.4338(3) 0.0473(9) Uani 1 1 d . . . H38A H 0.1721 0.4031 0.4705 0.071 Uiso 1 1 calc R . . H38B H 0.2035 0.3413 0.3712 0.071 Uiso 1 1 calc R . . H38C H 0.2223 0.4688 0.4127 0.071 Uiso 1 1 calc R . . C39 C 0.3345(3) 0.4394(3) 0.5072(2) 0.0338(7) Uani 1 1 d . . . C40 C 0.3884(3) 0.3647(3) 0.4847(2) 0.0359(7) Uani 1 1 d . . . H40 H 0.3577 0.3016 0.4185 0.043 Uiso 1 1 calc R . . C41 C 0.4851(3) 0.3783(3) 0.5550(2) 0.0332(7) Uani 1 1 d . . . C42 C 0.5333(3) 0.2892(3) 0.5263(3) 0.0431(8) Uani 1 1 d . . . H42A H 0.6087 0.3225 0.5372 0.065 Uiso 1 1 calc R . . H42B H 0.4957 0.2357 0.4523 0.065 Uiso 1 1 calc R . . H42C H 0.5265 0.2522 0.5710 0.065 Uiso 1 1 calc R . . N1 N 0.33625(19) 0.3236(2) 0.70882(19) 0.0257(5) Uani 1 1 d . . . N2 N 0.52833(18) 0.28587(19) 0.76628(17) 0.0230(5) Uani 1 1 d . . . N3 N 0.0666(2) -0.3953(2) 0.4683(2) 0.0371(6) Uani 1 1 d . . . H3A H 0.0313 -0.4662 0.4328 0.045 Uiso 1 1 calc R . . H3B H 0.0687 -0.3599 0.5330 0.045 Uiso 1 1 calc R . . N4 N 0.48679(19) 0.7438(2) 0.75116(19) 0.0271(5) Uani 1 1 d . . . N5 N 0.66459(19) 0.67944(19) 0.79974(18) 0.0253(5) Uani 1 1 d . . . N6 N 0.9490(2) 1.4012(2) 1.1910(2) 0.0440(7) Uani 1 1 d . . . H6A H 0.9871 1.4690 1.2382 0.053 Uiso 1 1 calc R . . H6B H 0.9311 1.3844 1.1237 0.053 Uiso 1 1 calc R . . O1 O 0.44033(18) 0.54375(18) 0.85348(18) 0.0377(5) Uani 1 1 d . . . O2 O 0.62441(16) 0.50191(17) 0.92388(16) 0.0330(5) Uani 1 1 d . . . O3 O 0.1166(2) -0.38826(18) 0.33077(17) 0.0491(7) Uani 1 1 d . . . O4 O 0.37310(17) 0.53446(17) 0.58910(17) 0.0345(5) Uani 1 1 d . . . O5 O 0.53859(17) 0.46390(17) 0.64665(16) 0.0331(5) Uani 1 1 d . . . O6 O 0.94178(19) 1.34272(18) 1.31758(16) 0.0416(6) Uani 1 1 d . . . Cu1 Cu 0.48389(3) 0.41513(3) 0.81153(3) 0.02626(11) Uani 1 1 d . . . Cu2 Cu 0.51557(3) 0.60465(3) 0.69748(3) 0.02675(11) Uani 1 1 d . . . C43 C -0.0161(3) -0.0951(4) 0.2429(4) 0.0624(11) Uani 1 1 d . . . H43A H -0.0354 -0.1322 0.1655 0.075 Uiso 1 1 calc R . . H43B H -0.0768 -0.1275 0.2612 0.075 Uiso 1 1 calc R . . C44 C 0.0801(4) -0.1129(4) 0.2936(4) 0.0628(11) Uani 1 1 d . . . H44A H 0.0985 -0.0776 0.3710 0.075 Uiso 1 1 calc R . . H44B H 0.0644 -0.1923 0.2695 0.075 Uiso 1 1 calc R . . C45 C 0.1894(3) 0.0470(4) 0.2984(4) 0.0720(14) Uani 1 1 d . . . H45A H 0.2477 0.0780 0.2766 0.086 Uiso 1 1 calc R . . H45B H 0.2120 0.0861 0.3761 0.086 Uiso 1 1 calc R . . C46 C 0.0922(4) 0.0640(4) 0.2509(5) 0.0938(19) Uani 1 1 d . . . H46A H 0.1076 0.1434 0.2760 0.113 Uiso 1 1 calc R . . H46B H 0.0733 0.0299 0.1735 0.113 Uiso 1 1 calc R . . O7 O 0.0040(2) 0.0182(3) 0.2771(3) 0.0757(10) Uani 1 1 d . . . O8 O 0.1697(2) -0.0668(3) 0.2660(2) 0.0679(8) Uani 1 1 d . . . C47 C -0.0522(3) 0.3993(3) -0.0920(2) 0.0390(8) Uani 1 1 d . . . H47A H -0.1124 0.3284 -0.1347 0.047 Uiso 1 1 calc R . . H47B H -0.0047 0.4058 -0.1332 0.047 Uiso 1 1 calc R . . C48 C 0.0939(3) 0.5086(3) 0.0692(3) 0.0414(8) Uani 1 1 d . . . H48A H 0.1442 0.5172 0.0311 0.050 Uiso 1 1 calc R . . H48B H 0.1329 0.5114 0.1363 0.050 Uiso 1 1 calc R . . O9 O 0.00587(18) 0.40159(19) 0.00510(18) 0.0433(6) 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 C1 0.0362(16) 0.0282(17) 0.0398(17) 0.0196(14) 0.0156(14) 0.0166(14) C2 0.0326(16) 0.040(2) 0.0435(19) 0.0211(16) 0.0076(14) 0.0162(15) C3 0.0265(15) 0.0313(17) 0.0324(16) 0.0134(14) 0.0057(12) 0.0065(13) C4 0.0268(14) 0.0195(14) 0.0224(13) 0.0079(12) 0.0074(11) 0.0053(12) C5 0.0277(14) 0.0212(14) 0.0196(13) 0.0095(11) 0.0101(11) 0.0059(11) C6 0.0248(13) 0.0164(14) 0.0216(13) 0.0067(11) 0.0083(11) 0.0038(11) C7 0.0278(14) 0.0211(15) 0.0290(15) 0.0110(12) 0.0093(12) 0.0073(12) C8 0.0261(14) 0.0330(17) 0.0300(15) 0.0144(13) 0.0094(12) 0.0132(13) C9 0.0238(13) 0.0273(16) 0.0264(14) 0.0112(13) 0.0068(11) 0.0051(12) C10 0.0237(13) 0.0192(14) 0.0228(13) 0.0080(11) 0.0046(11) 0.0044(11) C11 0.0259(14) 0.0247(15) 0.0282(14) 0.0113(12) 0.0111(12) 0.0043(12) C12 0.0325(15) 0.0220(15) 0.0255(14) 0.0062(12) 0.0104(12) 0.0074(12) C13 0.0280(14) 0.0208(15) 0.0211(13) 0.0084(12) 0.0013(11) 0.0035(12) C14 0.0280(14) 0.0250(16) 0.0259(14) 0.0110(12) 0.0095(12) 0.0025(12) C15 0.0293(14) 0.0222(15) 0.0228(14) 0.0055(12) 0.0080(12) 0.0071(12) C16 0.0340(16) 0.0203(15) 0.0249(14) 0.0071(12) 0.0074(12) -0.0006(12) C17 0.083(3) 0.035(2) 0.045(2) 0.0195(17) 0.036(2) 0.032(2) C18 0.060(2) 0.0185(16) 0.0373(17) 0.0130(14) 0.0309(16) 0.0141(15) C19 0.052(2) 0.0208(16) 0.0305(16) 0.0029(13) 0.0208(15) 0.0036(15) C20 0.0388(17) 0.0252(16) 0.0274(15) 0.0063(13) 0.0176(13) -0.0017(14) C21 0.0373(18) 0.044(2) 0.0338(18) -0.0006(16) 0.0181(15) -0.0041(16) C22 0.0289(15) 0.0303(17) 0.0340(16) 0.0095(14) 0.0044(13) 0.0095(13) C23 0.0390(17) 0.0336(19) 0.0429(18) 0.0125(15) 0.0126(15) 0.0207(15) C24 0.0371(17) 0.0234(16) 0.0357(17) 0.0085(13) 0.0092(14) 0.0115(14) C25 0.0328(15) 0.0191(15) 0.0248(14) 0.0080(12) 0.0089(12) 0.0086(12) C26 0.0308(14) 0.0231(15) 0.0225(13) 0.0114(12) 0.0083(12) 0.0073(12) C27 0.0303(15) 0.0216(15) 0.0236(14) 0.0109(12) 0.0056(12) 0.0055(12) C28 0.0306(15) 0.0294(17) 0.0303(15) 0.0148(14) 0.0059(12) 0.0076(13) C29 0.0336(16) 0.0391(19) 0.0419(18) 0.0218(16) 0.0120(14) 0.0162(15) C30 0.0393(17) 0.0281(17) 0.0332(16) 0.0152(14) 0.0132(14) 0.0152(14) C31 0.0289(14) 0.0232(15) 0.0245(14) 0.0086(12) 0.0071(12) 0.0077(12) C32 0.0394(16) 0.0247(16) 0.0227(14) 0.0112(13) 0.0022(12) 0.0065(13) C33 0.0403(17) 0.0215(15) 0.0305(15) 0.0139(13) 0.0088(13) 0.0070(13) C34 0.0302(14) 0.0187(14) 0.0242(14) 0.0066(12) 0.0093(12) 0.0034(12) C35 0.0369(16) 0.0294(17) 0.0209(14) 0.0112(13) 0.0060(12) 0.0084(13) C36 0.0402(16) 0.0225(15) 0.0275(15) 0.0117(13) 0.0107(13) 0.0088(13) C37 0.0347(16) 0.0238(16) 0.0263(15) 0.0059(13) 0.0118(13) 0.0049(13) C38 0.0411(19) 0.042(2) 0.0362(18) 0.0079(16) 0.0005(15) 0.0051(16) C39 0.0380(17) 0.0268(17) 0.0274(15) 0.0106(13) 0.0074(13) 0.0028(14) C40 0.0466(18) 0.0216(16) 0.0256(15) 0.0053(13) 0.0080(14) 0.0023(14) C41 0.0480(19) 0.0226(16) 0.0304(16) 0.0133(13) 0.0170(14) 0.0098(14) C42 0.066(2) 0.0321(19) 0.0380(18) 0.0166(16) 0.0226(17) 0.0220(17) N1 0.0290(12) 0.0212(13) 0.0289(12) 0.0123(10) 0.0114(10) 0.0093(10) N2 0.0237(11) 0.0198(12) 0.0213(11) 0.0073(10) 0.0071(9) 0.0046(10) N3 0.0545(17) 0.0178(13) 0.0266(13) 0.0068(11) 0.0122(12) -0.0002(12) N4 0.0296(12) 0.0217(13) 0.0265(12) 0.0100(10) 0.0069(10) 0.0073(10) N5 0.0321(12) 0.0201(12) 0.0252(12) 0.0112(10) 0.0101(10) 0.0097(10) N6 0.0606(18) 0.0218(14) 0.0277(14) 0.0048(12) 0.0085(13) -0.0045(13) O1 0.0488(13) 0.0220(12) 0.0391(12) 0.0103(10) 0.0141(11) 0.0138(10) O2 0.0326(11) 0.0213(11) 0.0298(11) 0.0025(9) 0.0098(9) 0.0003(9) O3 0.0653(16) 0.0258(13) 0.0291(12) 0.0007(10) 0.0166(11) -0.0092(11) O4 0.0342(11) 0.0253(12) 0.0315(11) 0.0058(9) 0.0050(9) 0.0070(9) O5 0.0416(12) 0.0186(11) 0.0306(11) 0.0076(9) 0.0070(9) 0.0075(9) O6 0.0540(14) 0.0315(13) 0.0234(11) 0.0068(10) 0.0118(10) 0.0001(11) Cu1 0.0288(2) 0.01663(19) 0.02796(19) 0.00709(15) 0.00856(15) 0.00521(15) Cu2 0.0302(2) 0.0187(2) 0.02589(19) 0.00814(15) 0.00574(15) 0.00645(15) C43 0.047(2) 0.061(3) 0.063(3) 0.026(2) 0.013(2) 0.000(2) C44 0.080(3) 0.056(3) 0.073(3) 0.036(2) 0.035(2) 0.038(2) C45 0.050(2) 0.074(3) 0.068(3) 0.017(3) 0.031(2) 0.000(2) C46 0.081(3) 0.076(4) 0.179(6) 0.095(4) 0.067(4) 0.037(3) O7 0.0607(19) 0.075(2) 0.146(3) 0.079(2) 0.059(2) 0.0449(17) O8 0.0637(18) 0.084(2) 0.083(2) 0.0402(19) 0.0444(17) 0.0480(18) C47 0.0425(18) 0.0305(18) 0.0300(16) 0.0099(14) 0.0042(14) 0.0040(15) C48 0.0317(16) 0.038(2) 0.0387(18) 0.0122(16) 0.0020(14) 0.0045(15) O9 0.0448(13) 0.0307(13) 0.0407(13) 0.0137(11) 0.0033(11) 0.0050(11) _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 C1 N1 1.331(4) . ? C1 C2 1.399(4) . ? C1 H1 0.9300 . ? C2 C3 1.368(4) . ? C2 H2 0.9300 . ? C3 C4 1.421(4) . ? C3 H3 0.9300 . ? C4 N1 1.393(4) . ? C4 C5 1.407(4) . ? C5 C6 1.400(4) . ? C5 C10 1.489(4) . ? C6 N2 1.397(3) . ? C6 C7 1.415(4) . ? C7 C8 1.376(4) . ? C7 H7 0.9300 . ? C8 C9 1.399(4) . ? C8 H8 0.9300 . ? C9 N2 1.338(3) . ? C9 H9 0.9300 . ? C10 C15 1.391(4) . ? C10 C11 1.399(4) . ? C11 C12 1.383(4) . ? C11 H11 0.9300 . ? C12 C13 1.384(4) . ? C12 H12 0.9300 . ? C13 C14 1.386(4) . ? C13 C16 1.498(4) . ? C14 C15 1.393(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O3 1.228(3) . ? C16 N3 1.328(4) . ? C17 C18 1.504(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O1 1.282(4) . ? C18 C19 1.387(5) . ? C19 C20 1.397(5) . ? C19 H19 0.9300 . ? C20 O2 1.276(3) . ? C20 C21 1.508(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.344(4) . ? C22 C23 1.405(4) . ? C22 H22 0.9300 . ? C23 C24 1.364(4) . ? C23 H23 0.9300 . ? C24 C25 1.423(4) . ? C24 H24 0.9300 . ? C25 N4 1.395(4) . ? C25 C26 1.399(4) . ? C26 C27 1.406(4) . ? C26 C31 1.494(4) . ? C27 N5 1.395(4) . ? C27 C28 1.410(4) . ? C28 C29 1.364(4) . ? C28 H28 0.9300 . ? C29 C30 1.396(4) . ? C29 H29 0.9300 . ? C30 N5 1.337(4) . ? C30 H30 0.9300 . ? C31 C32 1.392(4) . ? C31 C36 1.393(4) . ? C32 C33 1.376(4) . ? C32 H32 0.9300 . ? C33 C34 1.387(4) . ? C33 H33 0.9300 . ? C34 C35 1.389(4) . ? C34 C37 1.502(4) . ? C35 C36 1.377(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 O6 1.236(3) . ? C37 N6 1.332(4) . ? C38 C39 1.498(4) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O4 1.273(4) . ? C39 C40 1.390(5) . ? C40 C41 1.388(4) . ? C40 H40 0.9300 . ? C41 O5 1.286(4) . ? C41 C42 1.501(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N1 Cu1 1.962(2) . ? N2 Cu1 1.954(2) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 Cu2 1.962(2) . ? N5 Cu2 1.961(2) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O1 Cu1 1.937(2) . ? O2 Cu1 1.938(2) . ? O4 Cu2 1.930(2) . ? O5 Cu2 1.939(2) . ? C43 O7 1.390(5) . ? C43 C44 1.473(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O8 1.428(5) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 O8 1.401(5) . ? C45 C46 1.460(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 O7 1.400(5) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 O9 1.423(4) . ? C47 C48 1.475(5) 2_565 ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O9 1.447(4) . ? C48 C47 1.475(5) 2_565 ? C48 H48A 0.9700 . ? C48 H48B 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 C1 C2 111.7(3) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C3 C2 C1 106.6(3) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 106.9(3) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 124.0(2) . . ? N1 C4 C3 108.4(2) . . ? C5 C4 C3 127.4(3) . . ? C6 C5 C4 125.1(3) . . ? C6 C5 C10 117.1(2) . . ? C4 C5 C10 117.7(2) . . ? N2 C6 C5 123.2(2) . . ? N2 C6 C7 108.3(2) . . ? C5 C6 C7 128.3(3) . . ? C8 C7 C6 107.5(3) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 106.0(2) . . ? C7 C8 H8 127.0 . . ? C9 C8 H8 127.0 . . ? N2 C9 C8 112.0(3) . . ? N2 C9 H9 124.0 . . ? C8 C9 H9 124.0 . . ? C15 C10 C11 118.7(3) . . ? C15 C10 C5 120.5(2) . . ? C11 C10 C5 120.7(2) . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 119.5(3) . . ? C12 C13 C16 118.0(3) . . ? C14 C13 C16 122.5(3) . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 120.5(3) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O3 C16 N3 122.0(3) . . ? O3 C16 C13 119.7(3) . . ? N3 C16 C13 118.2(3) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C18 C19 124.7(3) . . ? O1 C18 C17 115.4(3) . . ? C19 C18 C17 119.9(3) . . ? C18 C19 C20 123.6(3) . . ? C18 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? O2 C20 C19 125.3(3) . . ? O2 C20 C21 115.2(3) . . ? C19 C20 C21 119.4(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C23 111.2(3) . . ? N4 C22 H22 124.4 . . ? C23 C22 H22 124.4 . . ? C24 C23 C22 106.9(3) . . ? C24 C23 H23 126.6 . . ? C22 C23 H23 126.6 . . ? C23 C24 C25 107.2(3) . . ? C23 C24 H24 126.4 . . ? C25 C24 H24 126.4 . . ? N4 C25 C26 123.7(3) . . ? N4 C25 C24 108.4(2) . . ? C26 C25 C24 127.8(3) . . ? C25 C26 C27 125.3(3) . . ? C25 C26 C31 117.6(3) . . ? C27 C26 C31 117.1(2) . . ? N5 C27 C26 123.8(3) . . ? N5 C27 C28 108.5(3) . . ? C26 C27 C28 127.7(3) . . ? C29 C28 C27 107.5(3) . . ? C29 C28 H28 126.3 . . ? C27 C28 H28 126.3 . . ? C28 C29 C30 106.3(3) . . ? C28 C29 H29 126.8 . . ? C30 C29 H29 126.8 . . ? N5 C30 C29 111.8(3) . . ? N5 C30 H30 124.1 . . ? C29 C30 H30 124.1 . . ? C32 C31 C36 118.3(3) . . ? C32 C31 C26 120.4(2) . . ? C36 C31 C26 121.3(3) . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 121.0(3) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C35 118.3(3) . . ? C33 C34 C37 122.7(3) . . ? C35 C34 C37 119.0(3) . . ? C36 C35 C34 120.9(3) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C31 120.7(3) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? O6 C37 N6 122.2(3) . . ? O6 C37 C34 121.5(3) . . ? N6 C37 C34 116.2(3) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C39 C40 124.3(3) . . ? O4 C39 C38 115.2(3) . . ? C40 C39 C38 120.5(3) . . ? C41 C40 C39 124.1(3) . . ? C41 C40 H40 118.0 . . ? C39 C40 H40 118.0 . . ? O5 C41 C40 124.4(3) . . ? O5 C41 C42 115.5(3) . . ? C40 C41 C42 120.1(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C1 N1 C4 106.3(2) . . ? C1 N1 Cu1 126.7(2) . . ? C4 N1 Cu1 126.78(18) . . ? C9 N2 C6 106.2(2) . . ? C9 N2 Cu1 125.97(19) . . ? C6 N2 Cu1 127.47(18) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C22 N4 C25 106.3(2) . . ? C22 N4 Cu2 125.6(2) . . ? C25 N4 Cu2 127.87(19) . . ? C30 N5 C27 105.8(2) . . ? C30 N5 Cu2 126.2(2) . . ? C27 N5 Cu2 127.62(19) . . ? C37 N6 H6A 120.0 . . ? C37 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C18 O1 Cu1 126.2(2) . . ? C20 O2 Cu1 126.2(2) . . ? C39 O4 Cu2 127.6(2) . . ? C41 O5 Cu2 126.3(2) . . ? O1 Cu1 O2 90.93(9) . . ? O1 Cu1 N2 178.64(9) . . ? O2 Cu1 N2 89.40(9) . . ? O1 Cu1 N1 88.94(10) . . ? O2 Cu1 N1 174.04(9) . . ? N2 Cu1 N1 90.87(10) . . ? O4 Cu2 O5 90.38(9) . . ? O4 Cu2 N5 175.50(9) . . ? O5 Cu2 N5 89.94(9) . . ? O4 Cu2 N4 88.52(9) . . ? O5 Cu2 N4 177.23(9) . . ? N5 Cu2 N4 91.35(10) . . ? O7 C43 C44 110.8(3) . . ? O7 C43 H43A 109.5 . . ? C44 C43 H43A 109.5 . . ? O7 C43 H43B 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 108.1 . . ? O8 C44 C43 110.0(3) . . ? O8 C44 H44A 109.7 . . ? C43 C44 H44A 109.7 . . ? O8 C44 H44B 109.7 . . ? C43 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? O8 C45 C46 110.9(4) . . ? O8 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? O8 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.0 . . ? O7 C46 C45 112.2(4) . . ? O7 C46 H46A 109.2 . . ? C45 C46 H46A 109.2 . . ? O7 C46 H46B 109.2 . . ? C45 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C43 O7 C46 108.8(4) . . ? C45 O8 C44 109.0(3) . . ? O9 C47 C48 110.8(3) . 2_565 ? O9 C47 H47A 109.5 . . ? C48 C47 H47A 109.5 2_565 . ? O9 C47 H47B 109.5 . . ? C48 C47 H47B 109.5 2_565 . ? H47A C47 H47B 108.1 . . ? O9 C48 C47 110.8(3) . 2_565 ? O9 C48 H48A 109.5 . . ? C47 C48 H48A 109.5 2_565 . ? O9 C48 H48B 109.5 . . ? C47 C48 H48B 109.5 2_565 . ? H48A C48 H48B 108.1 . . ? C47 O9 C48 109.0(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.894 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.164 #===END ###Material relevant to compound 7(CHCl3) at 173K ## data_compound7CHCl3 _database_code_depnum_ccdc_archive 'CCDC 717003' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C32 H26 Co N5 O3, C H Cl3' _chemical_formula_sum 'C33 H27 Cl3 Co N5 O3' _chemical_formula_weight 706.88 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' Cl Cl 0.1484 0.1585 '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)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4382(5) _cell_length_b 21.1339(8) _cell_length_c 12.3217(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.3580(10) _cell_angle_gamma 90.00 _cell_volume 3187.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6566 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.25 _exptl_crystal_description prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7650 _exptl_absorpt_correction_T_max 0.8923 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 30856 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7325 _reflns_number_gt 4826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1751P)^2^+6.2311P] 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 SHELXL _refine_ls_extinction_coef 0.027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7325 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1305 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2930 _refine_ls_wR_factor_gt 0.2598 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 C1 C 0.6808(5) 0.2897(2) 0.2424(5) 0.0350(11) Uani 1 1 d . . . H1 H 0.6284 0.3119 0.1797 0.042 Uiso 1 1 calc R . . C2 C 0.7884(5) 0.3109(3) 0.3088(5) 0.0393(12) Uani 1 1 d . . . H2 H 0.8189 0.3488 0.2991 0.047 Uiso 1 1 calc R . . C3 C 0.8389(4) 0.2644(3) 0.3902(5) 0.0373(12) Uani 1 1 d . . . H3 H 0.9115 0.2647 0.4450 0.045 Uiso 1 1 calc R . . C4 C 0.7631(4) 0.2162(2) 0.3776(4) 0.0310(11) Uani 1 1 d . . . C5 C 0.7698(4) 0.1648(2) 0.4518(5) 0.0314(11) Uani 1 1 d . . . C6 C 0.6789(4) 0.1289(2) 0.4428(4) 0.0309(11) Uani 1 1 d . . . C7 C 0.6676(5) 0.0901(3) 0.5327(5) 0.0383(12) Uani 1 1 d . . . H7 H 0.7235 0.0756 0.6025 0.046 Uiso 1 1 calc R . . C8 C 0.5592(5) 0.0787(3) 0.4958(5) 0.0389(12) Uani 1 1 d . . . H8 H 0.5264 0.0561 0.5369 0.047 Uiso 1 1 calc R . . C9 C 0.5050(5) 0.1079(2) 0.3825(5) 0.0352(11) Uani 1 1 d . . . H9 H 0.4300 0.1066 0.3369 0.042 Uiso 1 1 calc R . . C10 C 0.8760(4) 0.1504(3) 0.5532(5) 0.0349(11) Uani 1 1 d . . . C11 C 0.9298(4) 0.1941(3) 0.6406(5) 0.0341(11) Uani 1 1 d . . . H11 H 0.9018 0.2348 0.6342 0.041 Uiso 1 1 calc R . . C12 C 1.0256(4) 0.1784(3) 0.7387(5) 0.0362(12) Uani 1 1 d . . . H12 H 1.0613 0.2086 0.7968 0.043 Uiso 1 1 calc R . . C13 C 1.0674(4) 0.1177(3) 0.7490(5) 0.0371(12) Uani 1 1 d . . . C14 C 1.0150(5) 0.0735(3) 0.6612(5) 0.0457(14) Uani 1 1 d . . . H14 H 1.0442 0.0331 0.6671 0.055 Uiso 1 1 calc R . . C15 C 0.9191(5) 0.0891(3) 0.5642(5) 0.0447(14) Uani 1 1 d . . . H15 H 0.8834 0.0589 0.5064 0.054 Uiso 1 1 calc R . . C16 C 1.1700(4) 0.0963(3) 0.8544(5) 0.0419(13) Uani 1 1 d . . . C17 C 0.3683(5) 0.2584(3) 0.1280(5) 0.0394(12) Uani 1 1 d . . . C18 C 0.2792(5) 0.2848(4) 0.1466(6) 0.0556(17) Uani 1 1 d . . . H18 H 0.2756 0.2790 0.2197 0.067 Uiso 1 1 calc R . . C19 C 0.1980(7) 0.3187(5) 0.0589(8) 0.081(3) Uani 1 1 d . . . H19 H 0.1392 0.3336 0.0728 0.097 Uiso 1 1 calc R . . C20 C 0.2021(7) 0.3312(5) -0.0499(8) 0.084(3) Uani 1 1 d . . . H20 H 0.1480 0.3553 -0.1074 0.100 Uiso 1 1 calc R . . C21 C 0.2884(6) 0.3069(4) -0.0708(6) 0.0583(18) Uani 1 1 d . . . H21 H 0.2915 0.3147 -0.1436 0.070 Uiso 1 1 calc R . . C22 C 0.3725(5) 0.2703(3) 0.0168(5) 0.0403(13) Uani 1 1 d . . . C23 C 0.4565(5) 0.2472(3) -0.0139(5) 0.0374(12) Uani 1 1 d . . . H23 H 0.4567 0.2607 -0.0857 0.045 Uiso 1 1 calc R . . C24 C 0.6145(5) 0.1898(3) 0.0064(6) 0.0455(14) Uani 1 1 d . . . H24A H 0.6430 0.2266 -0.0182 0.055 Uiso 1 1 calc R . . H24B H 0.5818 0.1618 -0.0616 0.055 Uiso 1 1 calc R . . C25 C 0.7062(5) 0.1557(3) 0.1075(6) 0.0438(14) Uani 1 1 d . . . H25A H 0.7449 0.1271 0.0767 0.053 Uiso 1 1 calc R . . H25B H 0.7578 0.1857 0.1610 0.053 Uiso 1 1 calc R . . C26 C 0.6475(5) 0.0597(3) 0.1669(5) 0.0423(13) Uani 1 1 d . . . H26 H 0.7013 0.0380 0.1530 0.051 Uiso 1 1 calc R . . C27 C 0.5653(5) 0.0238(3) 0.1861(5) 0.0408(13) Uani 1 1 d . . . C28 C 0.5853(6) -0.0394(3) 0.2242(6) 0.0515(15) Uani 1 1 d . . . H28 H 0.6548 -0.0564 0.2462 0.062 Uiso 1 1 calc R . . C29 C 0.5031(7) -0.0764(3) 0.2294(6) 0.0591(19) Uani 1 1 d . . . H29 H 0.5174 -0.1175 0.2588 0.071 Uiso 1 1 calc R . . C30 C 0.3988(6) -0.0514(3) 0.1900(6) 0.0507(16) Uani 1 1 d . . . H30 H 0.3422 -0.0769 0.1896 0.061 Uiso 1 1 calc R . . C31 C 0.3768(5) 0.0105(3) 0.1512(5) 0.0459(14) Uani 1 1 d . . . H31 H 0.3057 0.0258 0.1243 0.055 Uiso 1 1 calc R . . C32 C 0.4606(4) 0.0508(3) 0.1519(5) 0.0355(12) Uani 1 1 d . . . N1 N 0.6637(3) 0.23306(19) 0.2814(4) 0.0291(9) Uani 1 1 d . . . N2 N 0.5757(3) 0.13718(19) 0.3507(4) 0.0293(9) Uani 1 1 d . . . N3 N 1.2335(4) 0.1394(3) 0.9252(5) 0.0623(17) Uani 1 1 d . . . H3A H 1.2911 0.1283 0.9863 0.075 Uiso 1 1 calc R . . H3B H 1.2177 0.1788 0.9109 0.075 Uiso 1 1 calc R . . N4 N 0.5322(4) 0.2091(2) 0.0498(4) 0.0347(10) Uani 1 1 d . . . N5 N 0.6496(3) 0.1207(2) 0.1681(4) 0.0349(10) Uani 1 1 d . . . O1 O 1.1889(4) 0.0391(2) 0.8708(5) 0.0656(14) Uani 1 1 d . . . O2 O 0.4399(3) 0.22553(17) 0.2143(3) 0.0329(8) Uani 1 1 d . . . O3 O 0.4389(3) 0.11081(17) 0.1217(3) 0.0342(8) Uani 1 1 d . . . Co1 Co 0.54894(5) 0.17357(3) 0.19834(6) 0.0276(3) Uani 1 1 d . . . C33 C 1.0044(18) 0.4478(9) 0.642(2) 0.226(12) Uani 1 1 d . . . H33 H 0.9599 0.4862 0.6175 0.272 Uiso 1 1 calc R . . Cl1 Cl 1.1385(4) 0.4701(3) 0.7333(6) 0.201(2) Uani 1 1 d . . . Cl2 Cl 0.9609(5) 0.4016(4) 0.7501(10) 0.316(6) Uani 1 1 d . . . Cl3 Cl 0.9857(10) 0.4104(7) 0.5311(12) 0.406(8) 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 C1 0.042(3) 0.030(3) 0.032(3) 0.001(2) 0.014(2) 0.002(2) C2 0.041(3) 0.034(3) 0.040(3) 0.001(2) 0.015(3) -0.006(2) C3 0.029(3) 0.042(3) 0.036(3) 0.002(2) 0.009(2) -0.005(2) C4 0.027(2) 0.034(3) 0.027(2) 0.001(2) 0.006(2) 0.001(2) C5 0.032(3) 0.030(2) 0.030(3) -0.0039(19) 0.011(2) 0.0003(19) C6 0.032(3) 0.031(2) 0.023(2) 0.0009(19) 0.005(2) 0.000(2) C7 0.045(3) 0.035(3) 0.027(3) 0.003(2) 0.007(2) -0.003(2) C8 0.049(3) 0.039(3) 0.028(3) 0.003(2) 0.016(2) -0.009(2) C9 0.040(3) 0.035(3) 0.030(3) -0.006(2) 0.014(2) -0.006(2) C10 0.029(3) 0.041(3) 0.030(3) 0.003(2) 0.008(2) 0.003(2) C11 0.031(3) 0.032(3) 0.036(3) -0.002(2) 0.010(2) 0.000(2) C12 0.028(3) 0.042(3) 0.032(3) -0.007(2) 0.006(2) -0.002(2) C13 0.026(2) 0.049(3) 0.033(3) 0.001(2) 0.008(2) 0.003(2) C14 0.045(3) 0.038(3) 0.044(3) -0.001(3) 0.008(3) 0.012(3) C15 0.038(3) 0.039(3) 0.042(3) -0.010(2) 0.002(3) 0.003(2) C16 0.025(3) 0.055(4) 0.039(3) 0.003(3) 0.006(2) 0.007(2) C17 0.040(3) 0.041(3) 0.033(3) -0.001(2) 0.011(2) 0.001(2) C18 0.046(3) 0.084(5) 0.039(3) 0.008(3) 0.020(3) 0.016(3) C19 0.074(5) 0.111(7) 0.066(5) 0.024(5) 0.038(5) 0.048(5) C20 0.070(5) 0.114(7) 0.066(5) 0.046(5) 0.028(4) 0.050(5) C21 0.059(4) 0.071(4) 0.043(4) 0.024(3) 0.019(3) 0.015(3) C22 0.045(3) 0.041(3) 0.030(3) 0.005(2) 0.010(2) 0.003(2) C23 0.044(3) 0.042(3) 0.025(3) -0.001(2) 0.013(2) -0.009(2) C24 0.054(4) 0.055(4) 0.039(3) -0.003(3) 0.031(3) -0.002(3) C25 0.046(3) 0.046(3) 0.051(4) -0.011(3) 0.032(3) -0.004(3) C26 0.040(3) 0.041(3) 0.045(3) -0.007(3) 0.017(3) 0.004(2) C27 0.048(3) 0.035(3) 0.036(3) -0.005(2) 0.014(3) -0.001(2) C28 0.066(4) 0.033(3) 0.054(4) 0.000(3) 0.024(3) 0.007(3) C29 0.090(6) 0.034(3) 0.050(4) 0.000(3) 0.026(4) -0.004(3) C30 0.063(4) 0.044(3) 0.038(3) -0.001(3) 0.014(3) -0.018(3) C31 0.047(3) 0.048(3) 0.035(3) -0.002(3) 0.010(3) -0.012(3) C32 0.040(3) 0.037(3) 0.023(2) -0.002(2) 0.007(2) -0.007(2) N1 0.030(2) 0.032(2) 0.024(2) 0.0023(17) 0.0109(17) 0.0011(17) N2 0.028(2) 0.030(2) 0.026(2) -0.0019(17) 0.0083(17) -0.0030(16) N3 0.043(3) 0.054(3) 0.057(4) 0.009(3) -0.013(3) -0.003(3) N4 0.036(2) 0.041(2) 0.029(2) -0.0059(19) 0.0148(19) -0.0079(19) N5 0.030(2) 0.036(2) 0.039(3) -0.0062(19) 0.015(2) -0.0049(18) O1 0.043(3) 0.054(3) 0.068(3) -0.001(2) -0.009(2) 0.013(2) O2 0.0330(19) 0.042(2) 0.0227(17) 0.0022(15) 0.0101(15) 0.0037(15) O3 0.0304(18) 0.039(2) 0.0267(18) -0.0005(15) 0.0054(15) -0.0034(15) Co1 0.0279(4) 0.0321(4) 0.0221(4) -0.0007(3) 0.0094(3) -0.0015(3) C33 0.21(2) 0.128(14) 0.25(2) -0.050(15) 0.009(18) -0.084(15) Cl1 0.135(4) 0.195(5) 0.265(7) -0.045(5) 0.076(4) -0.039(3) Cl2 0.159(5) 0.248(8) 0.418(13) 0.144(8) -0.004(6) -0.042(5) Cl3 0.398(14) 0.430(15) 0.402(16) -0.265(14) 0.177(12) -0.192(13) _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 C1 N1 1.344(7) . ? C1 C2 1.410(8) . ? C1 H1 0.9300 . ? C2 C3 1.368(8) . ? C2 H2 0.9300 . ? C3 C4 1.404(7) . ? C3 H3 0.9300 . ? C4 C5 1.397(7) . ? C4 N1 1.418(6) . ? C5 C6 1.403(7) . ? C5 C10 1.491(7) . ? C6 N2 1.394(6) . ? C6 C7 1.436(7) . ? C7 C8 1.356(8) . ? C7 H7 0.9300 . ? C8 C9 1.422(8) . ? C8 H8 0.9300 . ? C9 N2 1.321(7) . ? C9 H9 0.9300 . ? C10 C11 1.375(8) . ? C10 C15 1.402(8) . ? C11 C12 1.394(7) . ? C11 H11 0.9300 . ? C12 C13 1.386(8) . ? C12 H12 0.9300 . ? C13 C14 1.382(8) . ? C13 C16 1.522(7) . ? C14 C15 1.388(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.235(8) . ? C16 N3 1.306(8) . ? C17 O2 1.301(7) . ? C17 C22 1.417(8) . ? C17 C18 1.423(9) . ? C18 C19 1.379(10) . ? C18 H18 0.9300 . ? C19 C20 1.388(12) . ? C19 H19 0.9300 . ? C20 C21 1.386(11) . ? C20 H20 0.9300 . ? C21 C22 1.427(8) . ? C21 H21 0.9300 . ? C22 C23 1.417(8) . ? C23 N4 1.281(7) . ? C23 H23 0.9300 . ? C24 N4 1.471(7) . ? C24 C25 1.524(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N5 1.467(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N5 1.290(7) . ? C26 C27 1.438(8) . ? C26 H26 0.9300 . ? C27 C28 1.405(8) . ? C27 C32 1.411(8) . ? C28 C29 1.377(10) . ? C28 H28 0.9300 . ? C29 C30 1.385(10) . ? C29 H29 0.9300 . ? C30 C31 1.384(9) . ? C30 H30 0.9300 . ? C31 C32 1.409(8) . ? C31 H31 0.9300 . ? C32 O3 1.320(6) . ? N1 Co1 1.925(4) . ? N2 Co1 1.921(4) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 Co1 1.903(4) . ? N5 Co1 1.906(4) . ? O2 Co1 1.904(4) . ? O3 Co1 1.920(4) . ? C33 Cl3 1.50(2) . ? C33 Cl1 1.752(19) . ? C33 Cl2 1.93(3) . ? C33 H33 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 N1 C1 C2 111.2(5) . . ? N1 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 106.1(5) . . ? C3 C2 H2 127.0 . . ? C1 C2 H2 127.0 . . ? C2 C3 C4 108.8(5) . . ? C2 C3 H3 125.6 . . ? C4 C3 H3 125.6 . . ? C5 C4 C3 130.0(5) . . ? C5 C4 N1 121.8(4) . . ? C3 C4 N1 107.5(4) . . ? C4 C5 C6 123.3(5) . . ? C4 C5 C10 119.2(5) . . ? C6 C5 C10 117.2(5) . . ? N2 C6 C5 122.5(4) . . ? N2 C6 C7 108.2(4) . . ? C5 C6 C7 127.9(5) . . ? C8 C7 C6 106.4(5) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? C7 C8 C9 107.3(5) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? N2 C9 C8 110.7(5) . . ? N2 C9 H9 124.6 . . ? C8 C9 H9 124.6 . . ? C11 C10 C15 118.8(5) . . ? C11 C10 C5 122.1(5) . . ? C15 C10 C5 119.0(5) . . ? C10 C11 C12 121.3(5) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 119.9(5) . . ? C14 C13 C16 117.2(5) . . ? C12 C13 C16 122.9(5) . . ? C13 C14 C15 120.3(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 120.2(5) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? O1 C16 N3 122.7(5) . . ? O1 C16 C13 118.9(5) . . ? N3 C16 C13 118.4(5) . . ? O2 C17 C22 125.0(5) . . ? O2 C17 C18 117.8(5) . . ? C22 C17 C18 117.3(5) . . ? C19 C18 C17 121.6(6) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 121.5(7) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 118.6(7) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 121.5(6) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C17 123.5(5) . . ? C23 C22 C21 117.1(5) . . ? C17 C22 C21 119.5(6) . . ? N4 C23 C22 124.8(5) . . ? N4 C23 H23 117.6 . . ? C22 C23 H23 117.6 . . ? N4 C24 C25 108.1(5) . . ? N4 C24 H24A 110.1 . . ? C25 C24 H24A 110.1 . . ? N4 C24 H24B 110.1 . . ? C25 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? N5 C25 C24 103.8(5) . . ? N5 C25 H25A 111.0 . . ? C24 C25 H25A 111.0 . . ? N5 C25 H25B 111.0 . . ? C24 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? N5 C26 C27 122.7(5) . . ? N5 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C28 C27 C32 120.9(6) . . ? C28 C27 C26 120.1(6) . . ? C32 C27 C26 118.5(5) . . ? C29 C28 C27 120.6(7) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 118.9(6) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 121.5(6) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C30 C31 C32 120.9(6) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? O3 C32 C31 119.7(5) . . ? O3 C32 C27 123.3(5) . . ? C31 C32 C27 117.0(5) . . ? C1 N1 C4 106.4(4) . . ? C1 N1 Co1 127.5(4) . . ? C4 N1 Co1 123.5(3) . . ? C9 N2 C6 107.2(4) . . ? C9 N2 Co1 127.5(4) . . ? C6 N2 Co1 124.6(3) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C23 N4 C24 118.5(5) . . ? C23 N4 Co1 126.0(4) . . ? C24 N4 Co1 115.5(4) . . ? C26 N5 C25 120.8(5) . . ? C26 N5 Co1 125.0(4) . . ? C25 N5 Co1 111.3(3) . . ? C17 O2 Co1 124.4(3) . . ? C32 O3 Co1 119.3(3) . . ? N4 Co1 O2 94.60(17) . . ? N4 Co1 N5 81.7(2) . . ? O2 Co1 N5 174.99(17) . . ? N4 Co1 O3 92.16(17) . . ? O2 Co1 O3 88.87(16) . . ? N5 Co1 O3 87.91(17) . . ? N4 Co1 N2 176.33(18) . . ? O2 Co1 N2 88.40(16) . . ? N5 Co1 N2 95.44(19) . . ? O3 Co1 N2 90.01(16) . . ? N4 Co1 N1 90.28(18) . . ? O2 Co1 N1 92.87(17) . . ? N5 Co1 N1 90.52(18) . . ? O3 Co1 N1 176.88(16) . . ? N2 Co1 N1 87.45(17) . . ? Cl3 C33 Cl1 118.0(18) . . ? Cl3 C33 Cl2 112.2(12) . . ? Cl1 C33 Cl2 102.4(13) . . ? Cl3 C33 H33 108.0 . . ? Cl1 C33 H33 108.0 . . ? Cl2 C33 H33 108.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.393 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.248 #===END ###Material relevant to compound 7(acetone) at 173K ## data_7(acetone) _database_code_depnum_ccdc_archive 'CCDC 717004' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C32 H26 Co N5 O3), 3(C3 H6 O)' _chemical_formula_sum 'C73 H70 Co2 N10 O9' _chemical_formula_weight 1349.25 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 'Pbcn ' _symmetry_space_group_name_Hall '-P 2n 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.4552(4) _cell_length_b 17.1577(3) _cell_length_c 17.1153(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6887.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9428 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.21 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9424 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70305 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.55 _reflns_number_total 7937 _reflns_number_gt 5846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1066P)^2^+7.7569P] 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 7937 _refine_ls_number_parameters 403 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.096 _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 C1 C 0.20176(15) 0.0645(2) 0.8259(2) 0.0327(8) Uani 1 1 d . . . H1 H 0.1777 0.0230 0.8143 0.039 Uiso 1 1 calc R . . C2 C 0.24659(16) 0.0613(2) 0.8801(2) 0.0396(9) Uani 1 1 d . . . H2 H 0.2576 0.0184 0.9098 0.047 Uiso 1 1 calc R . . C3 C 0.27105(16) 0.1341(2) 0.8805(2) 0.0373(8) Uani 1 1 d . . . H3 H 0.3014 0.1501 0.9116 0.045 Uiso 1 1 calc R . . C4 C 0.24178(14) 0.1801(2) 0.82531(18) 0.0289(7) Uani 1 1 d . . . C5 C 0.25772(15) 0.2534(2) 0.79634(19) 0.0297(7) Uani 1 1 d . . . C6 C 0.23608(15) 0.2852(2) 0.72746(19) 0.0312(8) Uani 1 1 d . . . C7 C 0.25579(17) 0.3511(2) 0.6845(2) 0.0400(9) Uani 1 1 d . . . H7 H 0.2820 0.3880 0.7015 0.048 Uiso 1 1 calc R . . C8 C 0.22885(18) 0.3497(2) 0.6136(2) 0.0434(10) Uani 1 1 d . . . H8 H 0.2337 0.3850 0.5728 0.052 Uiso 1 1 calc R . . C9 C 0.19234(15) 0.2845(2) 0.6143(2) 0.0334(8) Uani 1 1 d . . . H9 H 0.1691 0.2701 0.5727 0.040 Uiso 1 1 calc R . . C10 C 0.30483(15) 0.2945(2) 0.83777(19) 0.0303(7) Uani 1 1 d . . . C11 C 0.29983(15) 0.3127(2) 0.9170(2) 0.0326(8) Uani 1 1 d . . . H11 H 0.2668 0.2995 0.9439 0.039 Uiso 1 1 calc R . . C12 C 0.34402(14) 0.3506(2) 0.95617(19) 0.0288(7) Uani 1 1 d . . . H12 H 0.3406 0.3615 1.0092 0.035 Uiso 1 1 calc R . . C13 C 0.39298(14) 0.37214(18) 0.91633(18) 0.0251(6) Uani 1 1 d . . . C14 C 0.39811(15) 0.3524(2) 0.83792(19) 0.0314(7) Uani 1 1 d . . . H14 H 0.4312 0.3658 0.8111 0.038 Uiso 1 1 calc R . . C15 C 0.35512(16) 0.3132(2) 0.7988(2) 0.0337(8) Uani 1 1 d . . . H15 H 0.3598 0.2995 0.7466 0.040 Uiso 1 1 calc R . . C16 C 0.43927(13) 0.42095(18) 0.95206(18) 0.0226(6) Uani 1 1 d . . . C17 C 0.14579(13) 0.02902(19) 0.63257(18) 0.0238(6) Uani 1 1 d . . . C18 C 0.16769(15) -0.0151(2) 0.56998(19) 0.0304(7) Uani 1 1 d . . . H18 H 0.1989 0.0038 0.5423 0.037 Uiso 1 1 calc R . . C19 C 0.14428(16) -0.0851(2) 0.5488(2) 0.0381(9) Uani 1 1 d . . . H19 H 0.1591 -0.1120 0.5062 0.046 Uiso 1 1 calc R . . C20 C 0.09833(17) -0.1166(2) 0.5903(2) 0.0388(9) Uani 1 1 d . . . H20 H 0.0822 -0.1639 0.5753 0.047 Uiso 1 1 calc R . . C21 C 0.07772(15) -0.0770(2) 0.6528(2) 0.0317(8) Uani 1 1 d . . . H21 H 0.0480 -0.0985 0.6815 0.038 Uiso 1 1 calc R . . C22 C 0.10004(13) -0.00401(19) 0.67572(18) 0.0249(6) Uani 1 1 d . . . C23 C 0.07557(13) 0.03379(19) 0.74292(19) 0.0257(7) Uani 1 1 d . . . H23 H 0.0481 0.0063 0.7708 0.031 Uiso 1 1 calc R . . C24 C 0.06162(16) 0.1321(2) 0.8402(2) 0.0331(8) Uani 1 1 d . . . H24A H 0.0621 0.0925 0.8806 0.040 Uiso 1 1 calc R . . H24B H 0.0224 0.1468 0.8303 0.040 Uiso 1 1 calc R . . C25 C 0.09617(17) 0.2032(2) 0.8662(2) 0.0344(8) Uani 1 1 d . . . H25A H 0.0740 0.2366 0.9005 0.041 Uiso 1 1 calc R . . H25B H 0.1309 0.1877 0.8927 0.041 Uiso 1 1 calc R . . C26 C 0.08280(17) 0.3060(2) 0.7749(2) 0.0367(8) Uani 1 1 d . . . H26 H 0.0704 0.3374 0.8157 0.044 Uiso 1 1 calc R . . C27 C 0.07173(18) 0.3318(2) 0.6959(2) 0.0399(9) Uani 1 1 d . . . C28 C 0.0548(2) 0.4086(3) 0.6819(3) 0.0616(13) Uani 1 1 d . . . H28 H 0.0572 0.4450 0.7221 0.074 Uiso 1 1 calc R . . C29 C 0.0347(3) 0.4315(3) 0.6100(3) 0.0757(17) Uani 1 1 d . . . H29 H 0.0242 0.4830 0.6009 0.091 Uiso 1 1 calc R . . C30 C 0.0305(3) 0.3759(3) 0.5513(3) 0.0693(15) Uani 1 1 d . . . H30 H 0.0164 0.3906 0.5027 0.083 Uiso 1 1 calc R . . C31 C 0.04666(19) 0.2997(3) 0.5628(3) 0.0484(10) Uani 1 1 d . . . H31 H 0.0427 0.2638 0.5224 0.058 Uiso 1 1 calc R . . C32 C 0.06910(15) 0.2756(2) 0.6352(2) 0.0330(8) Uani 1 1 d . . . N1 N 0.19817(12) 0.13525(17) 0.79285(15) 0.0261(6) Uani 1 1 d . . . N2 N 0.19517(12) 0.24624(17) 0.68157(16) 0.0285(6) Uani 1 1 d . . . N3 N 0.45259(11) 0.41087(16) 1.02640(15) 0.0255(6) Uani 1 1 d . . . H3A H 0.4790 0.4386 1.0474 0.031 Uiso 1 1 calc R . . H3B H 0.4348 0.3766 1.0538 0.031 Uiso 1 1 calc R . . N4 N 0.08841(11) 0.10169(16) 0.76743(15) 0.0246(6) Uani 1 1 d . . . N5 N 0.10872(12) 0.24231(17) 0.79198(16) 0.0297(6) Uani 1 1 d . . . O1 O 0.46383(10) 0.46972(13) 0.91056(13) 0.0278(5) Uani 1 1 d . . . O2 O 0.16831(9) 0.09778(13) 0.64545(12) 0.0264(5) Uani 1 1 d . . . O3 O 0.08589(9) 0.20287(13) 0.64385(13) 0.0275(5) Uani 1 1 d . . . Co1 Co 0.141627(18) 0.17058(2) 0.71998(2) 0.02277(15) Uani 1 1 d . . . C33 C 0.6770(6) 0.0725(10) 0.8230(8) 0.215(4) Uani 1 1 d . . . H33A H 0.6577 0.0644 0.7742 0.322 Uiso 1 1 calc R . . H33B H 0.6787 0.0242 0.8512 0.322 Uiso 1 1 calc R . . H33C H 0.7150 0.0909 0.8132 0.322 Uiso 1 1 calc R . . C34 C 0.6465(8) 0.1293(12) 0.8684(9) 0.215(4) Uani 1 1 d D . . C35 C 0.6719(6) 0.1475(10) 0.9402(8) 0.215(4) Uani 1 1 d D . . H35A H 0.6493 0.1859 0.9668 0.322 Uiso 1 1 calc R . . H35B H 0.7095 0.1678 0.9314 0.322 Uiso 1 1 calc R . . H35C H 0.6743 0.1013 0.9717 0.322 Uiso 1 1 calc R . . O4 O 0.5972(7) 0.1465(12) 0.8746(16) 0.481(16) Uani 1 1 d . . . C36 C 0.5000 0.1774(16) 0.7500 0.405(11) Uani 1 2 d SD . . C37 C 0.4651(9) 0.1291(13) 0.8044(13) 0.405(11) Uani 1 1 d D . . H37A H 0.4437 0.1626 0.8384 0.607 Uiso 1 1 calc R . . H37B H 0.4898 0.0966 0.8350 0.607 Uiso 1 1 calc R . . H37C H 0.4394 0.0971 0.7748 0.607 Uiso 1 1 calc R . . O5 O 0.5000 0.2517(15) 0.7500 0.405(11) Uani 1 2 d SD . . 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 C1 0.0366(18) 0.0346(19) 0.0269(17) 0.0043(14) -0.0033(14) -0.0075(15) C2 0.043(2) 0.043(2) 0.0331(19) 0.0112(17) -0.0081(16) -0.0057(17) C3 0.040(2) 0.049(2) 0.0231(17) 0.0045(16) -0.0085(14) -0.0117(17) C4 0.0299(17) 0.0377(19) 0.0190(15) 0.0001(13) -0.0020(13) -0.0095(14) C5 0.0324(18) 0.0369(18) 0.0197(16) -0.0025(13) -0.0010(13) -0.0108(14) C6 0.0354(18) 0.0350(19) 0.0232(16) 0.0015(14) -0.0037(13) -0.0125(15) C7 0.045(2) 0.042(2) 0.0329(19) 0.0086(16) -0.0095(16) -0.0227(17) C8 0.046(2) 0.050(2) 0.033(2) 0.0148(18) -0.0091(17) -0.0246(19) C9 0.0360(18) 0.041(2) 0.0233(16) 0.0067(15) -0.0047(14) -0.0134(15) C10 0.0329(17) 0.0345(18) 0.0234(16) 0.0000(14) -0.0059(13) -0.0103(14) C11 0.0309(17) 0.044(2) 0.0229(17) -0.0020(14) 0.0029(13) -0.0105(15) C12 0.0317(17) 0.0356(18) 0.0190(15) -0.0045(13) -0.0004(13) -0.0064(14) C13 0.0289(16) 0.0253(15) 0.0211(15) -0.0012(12) -0.0022(12) -0.0034(13) C14 0.0296(17) 0.0421(19) 0.0224(16) -0.0006(14) 0.0028(13) -0.0138(15) C15 0.042(2) 0.042(2) 0.0166(15) -0.0026(14) -0.0004(14) -0.0148(16) C16 0.0203(14) 0.0258(15) 0.0218(15) -0.0014(12) -0.0009(11) 0.0001(12) C17 0.0231(15) 0.0283(16) 0.0201(15) 0.0006(12) -0.0051(12) 0.0010(12) C18 0.0316(17) 0.0350(18) 0.0247(17) -0.0022(14) -0.0059(13) 0.0085(14) C19 0.044(2) 0.038(2) 0.0325(19) -0.0095(16) -0.0095(16) 0.0096(16) C20 0.048(2) 0.0308(18) 0.038(2) -0.0049(16) -0.0170(17) 0.0000(16) C21 0.0339(18) 0.0310(18) 0.0302(18) 0.0038(14) -0.0117(14) -0.0052(14) C22 0.0251(15) 0.0255(15) 0.0240(16) 0.0029(12) -0.0085(12) -0.0004(12) C23 0.0225(15) 0.0280(16) 0.0266(16) 0.0053(13) -0.0024(12) -0.0067(12) C24 0.0380(19) 0.0321(18) 0.0292(18) 0.0000(15) 0.0124(14) -0.0027(15) C25 0.046(2) 0.0349(19) 0.0222(17) -0.0018(14) 0.0072(15) -0.0014(16) C26 0.046(2) 0.0285(17) 0.036(2) -0.0051(15) 0.0063(16) -0.0043(16) C27 0.048(2) 0.0291(18) 0.043(2) 0.0066(16) 0.0055(18) -0.0007(16) C28 0.090(4) 0.034(2) 0.061(3) 0.005(2) 0.011(3) 0.005(2) C29 0.120(5) 0.040(3) 0.068(3) 0.020(3) 0.011(3) 0.020(3) C30 0.090(4) 0.063(3) 0.055(3) 0.028(3) -0.005(3) 0.016(3) C31 0.057(3) 0.048(2) 0.040(2) 0.0078(19) -0.007(2) 0.004(2) C32 0.0317(18) 0.0326(18) 0.0347(19) 0.0080(15) -0.0005(14) -0.0039(14) N1 0.0282(14) 0.0310(15) 0.0191(13) 0.0020(11) -0.0022(10) -0.0090(11) N2 0.0305(14) 0.0346(15) 0.0204(13) 0.0031(12) -0.0039(11) -0.0112(12) N3 0.0264(13) 0.0310(14) 0.0192(13) 0.0012(11) -0.0014(10) -0.0084(11) N4 0.0252(13) 0.0264(14) 0.0221(13) 0.0011(10) 0.0037(10) -0.0019(11) N5 0.0358(16) 0.0297(15) 0.0237(14) -0.0032(11) 0.0029(11) -0.0096(12) O1 0.0289(12) 0.0313(12) 0.0232(11) 0.0032(9) -0.0053(9) -0.0087(9) O2 0.0270(11) 0.0309(12) 0.0213(11) -0.0012(9) 0.0016(9) -0.0052(9) O3 0.0286(12) 0.0278(12) 0.0263(12) 0.0003(9) -0.0041(9) -0.0047(9) Co1 0.0260(2) 0.0247(2) 0.0176(2) 0.00023(16) -0.00059(16) -0.00694(16) C33 0.184(9) 0.288(12) 0.173(9) -0.044(8) -0.008(7) -0.018(8) C34 0.184(9) 0.288(12) 0.173(9) -0.044(8) -0.008(7) -0.018(8) C35 0.184(9) 0.288(12) 0.173(9) -0.044(8) -0.008(7) -0.018(8) O4 0.179(13) 0.47(3) 0.79(5) -0.13(3) -0.12(2) 0.093(15) C36 0.216(14) 0.38(3) 0.62(3) 0.000 -0.094(16) 0.000 C37 0.216(14) 0.38(3) 0.62(3) 0.000 -0.094(16) 0.000 O5 0.216(14) 0.38(3) 0.62(3) 0.000 -0.094(16) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(4) . ? C1 C2 1.404(5) . ? C1 H1 0.9300 . ? C2 C3 1.375(5) . ? C2 H2 0.9300 . ? C3 C4 1.410(5) . ? C3 H3 0.9300 . ? C4 N1 1.396(4) . ? C4 C5 1.402(5) . ? C5 C6 1.395(5) . ? C5 C10 1.490(4) . ? C6 N2 1.409(4) . ? C6 C7 1.426(5) . ? C7 C8 1.369(5) . ? C7 H7 0.9300 . ? C8 C9 1.409(5) . ? C8 H8 0.9300 . ? C9 N2 1.327(4) . ? C9 H9 0.9300 . ? C10 C15 1.393(5) . ? C10 C11 1.396(5) . ? C11 C12 1.396(5) . ? C11 H11 0.9300 . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C13 C14 1.389(4) . ? C13 C16 1.501(4) . ? C14 C15 1.384(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O1 1.240(4) . ? C16 N3 1.321(4) . ? C17 O2 1.311(4) . ? C17 C18 1.409(5) . ? C17 C22 1.421(4) . ? C18 C19 1.369(5) . ? C18 H18 0.9300 . ? C19 C20 1.400(6) . ? C19 H19 0.9300 . ? C20 C21 1.357(5) . ? C20 H20 0.9300 . ? C21 C22 1.412(5) . ? C21 H21 0.9300 . ? C22 C23 1.440(5) . ? C23 N4 1.274(4) . ? C23 H23 0.9300 . ? C24 N4 1.490(4) . ? C24 C25 1.531(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N5 1.467(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N5 1.284(5) . ? C26 C27 1.445(6) . ? C26 H26 0.9300 . ? C27 C28 1.397(6) . ? C27 C32 1.419(5) . ? C28 C29 1.376(7) . ? C28 H28 0.9300 . ? C29 C30 1.390(8) . ? C29 H29 0.9300 . ? C30 C31 1.375(7) . ? C30 H30 0.9300 . ? C31 C32 1.409(5) . ? C31 H31 0.9300 . ? C32 O3 1.317(4) . ? N1 Co1 1.919(3) . ? N2 Co1 1.922(3) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 Co1 1.901(3) . ? N5 Co1 1.905(3) . ? O2 Co1 1.892(2) . ? O3 Co1 1.927(2) . ? C33 C34 1.44(2) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O4 1.20(2) . ? C34 C35 1.402(9) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O5 1.275(10) . ? C36 C37 1.491(9) . ? C36 C37 1.491(9) 3_656 ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 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 N1 C1 C2 111.2(3) . . ? N1 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 106.3(3) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 107.6(3) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N1 C4 C5 123.3(3) . . ? N1 C4 C3 108.3(3) . . ? C5 C4 C3 127.5(3) . . ? C6 C5 C4 123.6(3) . . ? C6 C5 C10 119.1(3) . . ? C4 C5 C10 117.0(3) . . ? C5 C6 N2 122.2(3) . . ? C5 C6 C7 128.9(3) . . ? N2 C6 C7 108.0(3) . . ? C8 C7 C6 107.1(3) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 106.6(3) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C8 111.7(3) . . ? N2 C9 H9 124.1 . . ? C8 C9 H9 124.1 . . ? C15 C10 C11 119.0(3) . . ? C15 C10 C5 120.6(3) . . ? C11 C10 C5 120.4(3) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 118.8(3) . . ? C12 C13 C16 123.2(3) . . ? C14 C13 C16 117.8(3) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C10 119.8(3) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? O1 C16 N3 122.0(3) . . ? O1 C16 C13 118.6(3) . . ? N3 C16 C13 119.4(3) . . ? O2 C17 C18 117.7(3) . . ? O2 C17 C22 125.2(3) . . ? C18 C17 C22 117.2(3) . . ? C19 C18 C17 121.8(3) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 120.9(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 118.7(3) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 122.1(4) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C17 119.3(3) . . ? C21 C22 C23 118.2(3) . . ? C17 C22 C23 122.5(3) . . ? N4 C23 C22 125.5(3) . . ? N4 C23 H23 117.3 . . ? C22 C23 H23 117.3 . . ? N4 C24 C25 107.4(3) . . ? N4 C24 H24A 110.2 . . ? C25 C24 H24A 110.2 . . ? N4 C24 H24B 110.2 . . ? C25 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? N5 C25 C24 102.6(3) . . ? N5 C25 H25A 111.2 . . ? C24 C25 H25A 111.2 . . ? N5 C25 H25B 111.2 . . ? C24 C25 H25B 111.2 . . ? H25A C25 H25B 109.2 . . ? N5 C26 C27 124.0(3) . . ? N5 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? C28 C27 C32 120.2(4) . . ? C28 C27 C26 120.0(4) . . ? C32 C27 C26 119.0(3) . . ? C29 C28 C27 121.3(5) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 118.4(4) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C31 C30 C29 122.0(5) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 120.5(4) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? O3 C32 C31 119.3(4) . . ? O3 C32 C27 123.2(3) . . ? C31 C32 C27 117.5(4) . . ? C1 N1 C4 106.6(3) . . ? C1 N1 Co1 127.1(2) . . ? C4 N1 Co1 126.2(2) . . ? C9 N2 C6 106.4(3) . . ? C9 N2 Co1 126.7(2) . . ? C6 N2 Co1 125.1(2) . . ? C16 N3 H3A 120.0 . . ? C16 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C23 N4 C24 119.7(3) . . ? C23 N4 Co1 125.7(2) . . ? C24 N4 Co1 114.6(2) . . ? C26 N5 C25 119.4(3) . . ? C26 N5 Co1 126.4(3) . . ? C25 N5 Co1 110.3(2) . . ? C17 O2 Co1 125.0(2) . . ? C32 O3 Co1 123.5(2) . . ? O2 Co1 N4 95.44(11) . . ? O2 Co1 N5 175.39(11) . . ? N4 Co1 N5 81.91(12) . . ? O2 Co1 N1 90.06(11) . . ? N4 Co1 N1 88.84(12) . . ? N5 Co1 N1 93.65(12) . . ? O2 Co1 N2 89.95(11) . . ? N4 Co1 N2 174.22(12) . . ? N5 Co1 N2 92.84(12) . . ? N1 Co1 N2 89.09(12) . . ? O2 Co1 O3 87.61(10) . . ? N4 Co1 O3 91.27(11) . . ? N5 Co1 O3 88.67(11) . . ? N1 Co1 O3 177.67(11) . . ? N2 Co1 O3 91.02(11) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O4 C34 C35 106(2) . . ? O4 C34 C33 134.1(19) . . ? C35 C34 C33 114.4(18) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O5 C36 C37 123.8(11) . . ? O5 C36 C37 123.8(11) . 3_656 ? C37 C36 C37 112(2) . 3_656 ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.381 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.174 #===END