# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Hongjie Zhang' _publ_contact_author_name 'Dr Hongjie Zhang' _publ_contact_author_email hongjie@ciac.jl.cn data_tb _database_code_depnum_ccdc_archive 'CCDC 836983' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C25 H21 N5 Ni O5' _chemical_formula_sum 'C25.90 H23.10 N5.30 Ni O5.30' _chemical_formula_weight 552.11 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z' 'y+1/2, -x+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y, x, -z' '-y, -x, -z' _cell_length_a 22.3163(5) _cell_length_b 22.3163(5) _cell_length_c 12.7222(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6335.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 6259 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7899 _exptl_absorpt_correction_T_max 0.8753 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 35274 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6259 _reflns_number_gt 4912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 'ISOR' was used to restrain some abnormal thermal factors of atoms C3 and C4. ; _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^)+(0.0728P)^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 constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.52(2) _refine_ls_number_reflns 6259 _refine_ls_number_parameters 280 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _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 Ni1 Ni 0.260770(15) 0.747136(14) 0.24839(2) 0.03189(12) Uani 1 1 d . . . C1 C 0.35892(14) 0.72282(15) 0.1785(2) 0.0407(8) Uani 1 1 d . . . C2 C 0.41804(14) 0.71821(19) 0.1239(2) 0.0517(10) Uani 1 1 d . . . C3 C 0.47067(16) 0.7246(2) 0.1793(3) 0.0785(14) Uani 1 1 d U . . H3A H 0.4704 0.7274 0.2538 0.094 Uiso 1 1 calc R . . C4 C 0.52405(18) 0.7269(3) 0.1238(3) 0.0865(16) Uani 1 1 d U . . H4A H 0.5609 0.7326 0.1598 0.104 Uiso 1 1 calc R . . C5 C 0.52342(16) 0.7207(2) 0.0162(3) 0.0584(11) Uani 1 1 d . . . C6 C 0.42106(14) 0.70978(17) 0.0179(2) 0.0483(9) Uani 1 1 d . . . H6A H 0.3848 0.7028 -0.0194 0.058 Uiso 1 1 calc R . . C7 C 0.57908(16) 0.7268(2) -0.0466(2) 0.0550(10) Uani 1 1 d . . . C8 C 0.62729(16) 0.7585(2) -0.0084(3) 0.0625(12) Uani 1 1 d . . . H8A H 0.6258 0.7756 0.0599 0.075 Uiso 1 1 calc R . . C9 C 0.67809(15) 0.76536(19) -0.0701(3) 0.0561(10) Uani 1 1 d . . . H9A H 0.7110 0.7874 -0.0426 0.067 Uiso 1 1 calc R . . C10 C 0.63619(16) 0.71090(18) -0.2036(3) 0.0587(11) Uani 1 1 d . . . H10A H 0.6391 0.6933 -0.2714 0.070 Uiso 1 1 calc R . . C11 C 0.58379(17) 0.7032(2) -0.1459(3) 0.0639(11) Uani 1 1 d . . . H11A H 0.5512 0.6815 -0.1753 0.077 Uiso 1 1 calc R . . C12 C 0.23693(16) 0.34362(15) 0.6627(2) 0.0429(8) Uani 1 1 d . . . C13 C 0.23263(19) 0.40007(15) 0.6000(2) 0.0569(11) Uani 1 1 d . . . C14 C 0.2004(2) 0.44692(17) 0.6323(3) 0.0713(12) Uani 1 1 d . . . H14A H 0.1781 0.4444 0.6957 0.086 Uiso 1 1 calc R . . C15 C 0.1995(2) 0.49867(17) 0.5742(3) 0.0689(12) Uani 1 1 d . . . H15A H 0.1764 0.5319 0.5975 0.083 Uiso 1 1 calc R . . C16 C 0.2309(2) 0.50245(16) 0.4849(3) 0.0629(12) Uani 1 1 d . . . C17 C 0.2628(2) 0.40455(18) 0.5059(3) 0.0788(14) Uani 1 1 d . . . H17A H 0.2857 0.3715 0.4814 0.095 Uiso 1 1 calc R . . C18 C 0.23306(18) 0.55896(15) 0.4246(2) 0.0518(9) Uani 1 1 d . . . C19 C 0.2240(2) 0.61280(16) 0.4748(3) 0.0588(11) Uani 1 1 d . . . H19A H 0.2146 0.6138 0.5476 0.071 Uiso 1 1 calc R . . C20 C 0.22861(17) 0.66540(14) 0.4182(3) 0.0494(9) Uani 1 1 d . . . H20A H 0.2217 0.7023 0.4534 0.059 Uiso 1 1 calc R . . C21 C 0.25040(18) 0.61447(15) 0.2694(2) 0.0569(10) Uani 1 1 d . . . H21A H 0.2608 0.6145 0.1970 0.068 Uiso 1 1 calc R . . C22 C 0.2448(2) 0.56022(16) 0.3189(3) 0.0696(12) Uani 1 1 d . . . H22A H 0.2489 0.5240 0.2804 0.084 Uiso 1 1 calc R . . N1 N 0.47312(13) 0.71082(16) -0.0373(2) 0.0555(9) Uani 1 1 d . . . N2 N 0.68260(11) 0.74239(13) -0.16625(18) 0.0414(7) Uani 1 1 d . . . N3 N 0.2604(2) 0.45566(15) 0.4474(3) 0.0843(13) Uani 1 1 d . . . N4 N 0.24230(12) 0.66666(11) 0.31620(19) 0.0389(6) Uani 1 1 d . . . O1 O 0.31171(9) 0.71799(10) 0.12463(15) 0.0401(5) Uani 1 1 d . . . O2 O 0.35642(9) 0.73483(11) 0.27483(16) 0.0490(6) Uani 1 1 d . . . O3 O 0.21768(11) 0.34273(9) 0.75538(17) 0.0520(6) Uani 1 1 d . . . O4 O 0.26071(10) 0.29765(9) 0.62287(15) 0.0417(5) 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 Ni1 0.0372(2) 0.0367(2) 0.02180(19) -0.00043(18) -0.00125(18) 0.00246(14) C1 0.0392(19) 0.054(2) 0.0292(16) -0.0023(15) 0.0019(14) -0.0036(15) C2 0.0315(18) 0.089(3) 0.0347(18) -0.0038(18) -0.0037(14) 0.0031(18) C3 0.043(2) 0.158(4) 0.0342(18) -0.004(2) 0.0029(16) -0.012(2) C4 0.045(2) 0.174(5) 0.040(2) -0.007(3) -0.0039(17) -0.007(3) C5 0.040(2) 0.105(3) 0.0305(18) 0.0005(19) 0.0043(15) -0.007(2) C6 0.0329(18) 0.085(3) 0.0268(16) 0.0017(17) -0.0022(13) -0.0102(17) C7 0.037(2) 0.099(3) 0.0289(17) -0.0023(18) -0.0015(14) -0.003(2) C8 0.044(2) 0.110(4) 0.0333(18) -0.014(2) 0.0008(15) -0.012(2) C9 0.040(2) 0.093(3) 0.0349(18) -0.0174(19) 0.0002(14) -0.0066(19) C10 0.048(2) 0.089(3) 0.039(2) -0.017(2) 0.0065(16) -0.014(2) C11 0.056(2) 0.095(3) 0.041(2) -0.014(2) 0.0068(17) -0.026(2) C12 0.059(2) 0.0467(19) 0.0225(15) -0.0008(13) -0.0084(15) -0.0101(17) C13 0.098(3) 0.039(2) 0.0334(18) 0.0044(15) -0.0201(19) -0.015(2) C14 0.105(4) 0.044(2) 0.064(3) 0.009(2) -0.007(3) 0.003(2) C15 0.118(4) 0.033(2) 0.055(2) 0.0109(18) 0.003(3) 0.009(2) C16 0.103(3) 0.036(2) 0.050(2) 0.0003(17) -0.021(2) -0.010(2) C17 0.140(4) 0.046(2) 0.050(2) 0.0113(18) -0.003(3) -0.018(3) C18 0.082(3) 0.042(2) 0.0313(17) 0.0020(14) -0.0071(18) -0.0063(18) C19 0.100(3) 0.043(2) 0.0335(18) -0.0015(15) 0.0127(19) -0.004(2) C20 0.077(3) 0.0360(18) 0.0347(17) -0.0060(14) 0.0085(18) 0.0057(17) C21 0.100(3) 0.0430(18) 0.0282(16) 0.0002(14) 0.0099(19) 0.0043(19) C22 0.127(4) 0.041(2) 0.041(2) -0.0078(16) -0.003(2) -0.001(2) N1 0.0401(17) 0.098(3) 0.0279(14) -0.0076(16) -0.0027(12) -0.0068(17) N2 0.0389(14) 0.0625(18) 0.0228(13) -0.0017(13) 0.0011(10) -0.0050(14) N3 0.152(4) 0.053(2) 0.048(2) 0.0096(16) 0.003(2) -0.003(3) N4 0.0530(17) 0.0323(13) 0.0314(14) -0.0017(10) 0.0008(12) 0.0021(13) O1 0.0358(12) 0.0578(14) 0.0267(11) -0.0009(10) -0.0035(9) 0.0008(10) O2 0.0384(12) 0.0790(17) 0.0297(12) -0.0022(11) -0.0013(9) -0.0045(11) O3 0.0828(16) 0.0421(12) 0.0311(12) -0.0020(11) -0.0015(13) 0.0037(11) O4 0.0605(15) 0.0358(12) 0.0288(10) 0.0001(9) -0.0043(10) -0.0045(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 Ni1 N4 2.035(2) . ? Ni1 O4 2.045(2) 5_556 ? Ni1 N2 2.047(2) 6_465 ? Ni1 O1 2.048(2) . ? Ni1 O2 2.178(2) . ? Ni1 O3 2.187(2) 5_556 ? Ni1 C1 2.426(3) . ? Ni1 C12 2.433(3) 5_556 ? C1 O2 1.256(4) . ? C1 O1 1.261(4) . ? C1 C2 1.495(4) . ? C2 C6 1.363(4) . ? C2 C3 1.377(5) . ? C3 C4 1.386(5) . ? C4 C5 1.376(5) . ? C5 N1 1.332(4) . ? C5 C7 1.483(5) . ? C6 N1 1.358(4) . ? C7 C11 1.373(5) . ? C7 C8 1.376(5) . ? C8 C9 1.387(5) . ? C9 N2 1.330(4) . ? C10 N2 1.338(4) . ? C10 C11 1.391(5) . ? C12 O3 1.255(4) . ? C12 O4 1.261(4) . ? C12 C13 1.494(4) . ? C12 Ni1 2.433(3) 5_546 ? C13 C14 1.333(5) . ? C13 C17 1.378(5) . ? C14 C15 1.371(5) . ? C15 C16 1.338(5) . ? C16 N3 1.324(5) . ? C16 C18 1.477(5) . ? C17 N3 1.363(5) . ? C18 C22 1.370(5) . ? C18 C19 1.376(5) . ? C19 C20 1.381(5) . ? C20 N4 1.333(4) . ? C21 N4 1.320(4) . ? C21 C22 1.370(5) . ? N2 Ni1 2.047(2) 6_565 ? O3 Ni1 2.187(2) 5_546 ? O4 Ni1 2.045(2) 5_546 ? 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 N4 Ni1 O4 95.71(9) . 5_556 ? N4 Ni1 N2 98.32(11) . 6_465 ? O4 Ni1 N2 98.40(9) 5_556 6_465 ? N4 Ni1 O1 99.10(10) . . ? O4 Ni1 O1 157.04(10) 5_556 . ? N2 Ni1 O1 96.71(9) 6_465 . ? N4 Ni1 O2 91.25(10) . . ? O4 Ni1 O2 100.10(8) 5_556 . ? N2 Ni1 O2 158.19(9) 6_465 . ? O1 Ni1 O2 62.28(8) . . ? N4 Ni1 O3 156.16(9) . 5_556 ? O4 Ni1 O3 62.06(8) 5_556 5_556 ? N2 Ni1 O3 93.71(10) 6_465 5_556 ? O1 Ni1 O3 99.84(9) . 5_556 ? O2 Ni1 O3 84.89(9) . 5_556 ? N4 Ni1 C1 98.10(11) . . ? O4 Ni1 C1 128.94(10) 5_556 . ? N2 Ni1 C1 127.44(10) 6_465 . ? O1 Ni1 C1 31.33(9) . . ? O2 Ni1 C1 31.08(9) . . ? O3 Ni1 C1 90.67(10) 5_556 . ? N4 Ni1 C12 126.04(10) . 5_556 ? O4 Ni1 C12 31.21(9) 5_556 5_556 ? N2 Ni1 C12 98.88(11) 6_465 5_556 ? O1 Ni1 C12 128.82(10) . 5_556 ? O2 Ni1 C12 91.09(10) . 5_556 ? O3 Ni1 C12 30.95(9) 5_556 5_556 ? C1 Ni1 C12 110.46(12) . 5_556 ? O2 C1 O1 120.7(3) . . ? O2 C1 C2 120.5(3) . . ? O1 C1 C2 118.6(3) . . ? O2 C1 Ni1 63.53(16) . . ? O1 C1 Ni1 57.58(15) . . ? C2 C1 Ni1 169.4(3) . . ? C6 C2 C3 118.6(3) . . ? C6 C2 C1 120.9(3) . . ? C3 C2 C1 120.5(3) . . ? C2 C3 C4 118.4(3) . . ? C5 C4 C3 119.6(4) . . ? N1 C5 C4 122.3(3) . . ? N1 C5 C7 116.5(3) . . ? C4 C5 C7 121.2(3) . . ? N1 C6 C2 123.5(3) . . ? C11 C7 C8 117.5(3) . . ? C11 C7 C5 121.7(3) . . ? C8 C7 C5 120.8(3) . . ? C7 C8 C9 119.8(3) . . ? N2 C9 C8 122.6(3) . . ? N2 C10 C11 121.9(3) . . ? C7 C11 C10 120.1(3) . . ? O3 C12 O4 120.6(3) . . ? O3 C12 C13 119.5(3) . . ? O4 C12 C13 119.9(3) . . ? O3 C12 Ni1 63.66(16) . 5_546 ? O4 C12 Ni1 57.18(15) . 5_546 ? C13 C12 Ni1 174.8(2) . 5_546 ? C14 C13 C17 118.3(4) . . ? C14 C13 C12 122.1(4) . . ? C17 C13 C12 119.6(4) . . ? C13 C14 C15 120.2(4) . . ? C16 C15 C14 120.2(4) . . ? N3 C16 C15 121.2(4) . . ? N3 C16 C18 118.0(4) . . ? C15 C16 C18 120.8(4) . . ? N3 C17 C13 121.1(4) . . ? C22 C18 C19 117.8(3) . . ? C22 C18 C16 122.3(3) . . ? C19 C18 C16 120.0(3) . . ? C18 C19 C20 119.3(3) . . ? N4 C20 C19 122.9(3) . . ? N4 C21 C22 124.0(3) . . ? C18 C22 C21 119.1(3) . . ? C5 N1 C6 117.4(3) . . ? C9 N2 C10 118.0(3) . . ? C9 N2 Ni1 119.3(2) . 6_565 ? C10 N2 Ni1 122.6(2) . 6_565 ? C16 N3 C17 118.9(4) . . ? C21 N4 C20 116.8(3) . . ? C21 N4 Ni1 124.0(2) . . ? C20 N4 Ni1 118.5(2) . . ? C1 O1 Ni1 91.09(17) . . ? C1 O2 Ni1 85.40(18) . . ? C12 O3 Ni1 85.39(19) . 5_546 ? C12 O4 Ni1 91.61(18) . 5_546 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.599 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.060 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.015 701 84 ' ' 2 0.000 0.500 0.041 804 119 ' ' 3 0.500 0.000 -0.061 804 119 ' ' 4 0.500 0.500 -0.018 701 85 ' ' _platon_squeeze_details ; During the structure refinement, the atoms of the (DMF) solvent molecule were observed but could not be modeled satisfactorily. Therefore, the SQUEEZE routine in PLATON was used to modify the HKL file and the solvent equated to 1.3 DMF molecules per formula. ; # Attachment '- 2.cif' data_m1 _database_code_depnum_ccdc_archive 'CCDC 836984' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H36 N8 O9 Zn2' _chemical_formula_sum 'C39 H36 N8 O9 Zn2' _chemical_formula_weight 891.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c 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 6.1802(4) _cell_length_b 29.4218(18) _cell_length_c 23.3127(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.6630(10) _cell_angle_gamma 90.00 _cell_volume 4218.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 8320 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 26.05 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7458 _exptl_absorpt_correction_T_max 0.8501 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 23187 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.05 _reflns_number_total 8320 _reflns_number_gt 5599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For the disordered DMF molecules, Command 'DFIX' was used to restrain the bond length (C40-O10), and 'ISOR' was used in the refinement to restrain atoms (C35, C37, C41, C42, O10) with abnormal thermal factors. ; _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^)+(0.1101P)^2^+7.2052P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8320 _refine_ls_number_parameters 572 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1848 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.067 _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 Zn1 Zn 0.47547(11) 0.07625(2) 0.26923(3) 0.0218(2) Uani 1 1 d . . . Zn2 Zn 0.47972(11) -0.03910(2) 0.25274(3) 0.0215(2) Uani 1 1 d . . . C1 C 0.6064(10) 0.1611(2) 0.2654(2) 0.0253(13) Uani 1 1 d . . . C2 C 0.7426(10) 0.2024(2) 0.2600(3) 0.0280(13) Uani 1 1 d . . . C3 C 0.6671(11) 0.2451(2) 0.2750(3) 0.0364(16) Uani 1 1 d . . . H3A H 0.5296 0.2467 0.2899 0.044 Uiso 1 1 calc R . . C4 C 0.9659(10) 0.2807(2) 0.2479(3) 0.0289(14) Uani 1 1 d . . . C5 C 1.0549(11) 0.2405(2) 0.2325(3) 0.0356(16) Uani 1 1 d . . . H5A H 1.1920 0.2400 0.2173 0.043 Uiso 1 1 calc R . . C6 C 0.9427(10) 0.2009(2) 0.2393(3) 0.0337(15) Uani 1 1 d . . . H6A H 1.0035 0.1726 0.2298 0.040 Uiso 1 1 calc R . . C7 C 1.0799(10) 0.3248(2) 0.2428(3) 0.0293(14) Uani 1 1 d . . . C8 C 1.0092(10) 0.3648(2) 0.2680(3) 0.0304(14) Uani 1 1 d . . . H8A H 0.8778 0.3647 0.2859 0.036 Uiso 1 1 calc R . . C9 C 1.1301(9) 0.40415(19) 0.2667(2) 0.0244(12) Uani 1 1 d . . . H9A H 1.0816 0.4306 0.2850 0.029 Uiso 1 1 calc R . . C10 C 1.3755(11) 0.3690(2) 0.2134(3) 0.0313(14) Uani 1 1 d . . . H10A H 1.5006 0.3708 0.1929 0.038 Uiso 1 1 calc R . . C11 C 1.2679(10) 0.3282(2) 0.2135(3) 0.0340(15) Uani 1 1 d . . . H11A H 1.3196 0.3026 0.1941 0.041 Uiso 1 1 calc R . . C12 C 0.1563(9) -0.03650(19) 0.3319(2) 0.0227(12) Uani 1 1 d . . . C13 C 0.0769(9) -0.04929(19) 0.3887(2) 0.0244(13) Uani 1 1 d . . . C14 C -0.1295(10) -0.0370(2) 0.4013(2) 0.0297(14) Uani 1 1 d . . . H14A H -0.2233 -0.0229 0.3718 0.036 Uiso 1 1 calc R . . C15 C -0.0731(10) -0.0653(2) 0.4930(2) 0.0251(13) Uani 1 1 d . . . C16 C 0.1295(10) -0.0815(2) 0.4826(3) 0.0345(15) Uani 1 1 d . . . H16A H 0.2149 -0.0984 0.5112 0.041 Uiso 1 1 calc R . . C17 C 0.2055(10) -0.0728(2) 0.4303(3) 0.0346(15) Uani 1 1 d . . . H17A H 0.3460 -0.0829 0.4228 0.042 Uiso 1 1 calc R . . C18 C -0.1610(9) -0.0701(2) 0.5500(2) 0.0260(13) Uani 1 1 d . . . C19 C -0.3588(10) -0.0508(2) 0.5592(2) 0.0296(14) Uani 1 1 d . . . H19A H -0.4401 -0.0351 0.5286 0.036 Uiso 1 1 calc R . . C20 C -0.4386(10) -0.0540(2) 0.6114(2) 0.0283(13) Uani 1 1 d . . . H20A H -0.5731 -0.0397 0.6165 0.034 Uiso 1 1 calc R . . C21 C -0.1463(10) -0.0956(2) 0.6474(3) 0.0288(14) Uani 1 1 d . . . H21A H -0.0712 -0.1119 0.6784 0.035 Uiso 1 1 calc R . . C22 C -0.0533(10) -0.0932(2) 0.5959(2) 0.0293(14) Uani 1 1 d . . . H22A H 0.0831 -0.1072 0.5922 0.035 Uiso 1 1 calc R . . C23 C 0.3992(10) -0.0422(2) 0.1386(2) 0.0256(13) Uani 1 1 d . . . C24 C 0.2820(10) -0.0493(2) 0.0795(3) 0.0301(14) Uani 1 1 d . . . C25 C 0.0657(11) -0.0590(2) 0.0699(3) 0.0391(16) Uani 1 1 d . . . H25A H -0.0162 -0.0608 0.1022 0.047 Uiso 1 1 calc R . . C26 C 0.0772(10) -0.0620(2) -0.0285(3) 0.0315(14) Uani 1 1 d . . . C27 C 0.2923(12) -0.0539(4) -0.0220(3) 0.070(3) Uani 1 1 d . . . H27A H 0.3721 -0.0525 -0.0547 0.084 Uiso 1 1 calc R . . C28 C 0.3954(13) -0.0476(4) 0.0320(3) 0.074(3) Uani 1 1 d . . . H28A H 0.5475 -0.0420 0.0366 0.089 Uiso 1 1 calc R . . C29 C -0.0410(10) -0.0676(2) -0.0867(3) 0.0279(14) Uani 1 1 d . . . C30 C -0.2383(12) -0.0910(3) -0.0939(3) 0.0453(19) Uani 1 1 d . . . H30A H -0.2961 -0.1049 -0.0619 0.054 Uiso 1 1 calc R . . C31 C -0.3468(12) -0.0937(3) -0.1478(3) 0.0435(18) Uani 1 1 d . . . H31A H -0.4819 -0.1093 -0.1520 0.052 Uiso 1 1 calc R . . C32 C -0.0840(10) -0.0538(2) -0.1876(3) 0.0314(14) Uani 1 1 d . . . H32A H -0.0288 -0.0407 -0.2204 0.038 Uiso 1 1 calc R . . C33 C 0.0345(10) -0.0496(2) -0.1353(3) 0.0319(14) Uani 1 1 d . . . H33A H 0.1698 -0.0340 -0.1325 0.038 Uiso 1 1 calc R . . C34 C 0.718(2) 0.6885(5) -0.0016(5) 0.121(5) Uani 1 1 d . . . H34A H 0.5820 0.6758 -0.0201 0.182 Uiso 1 1 calc R . . H34B H 0.8370 0.6671 -0.0054 0.182 Uiso 1 1 calc R . . H34C H 0.7495 0.7173 -0.0203 0.182 Uiso 1 1 calc R . . C35 C 0.8755(18) 0.7165(4) 0.0952(6) 0.101(4) Uani 1 1 d U . . H35A H 0.8395 0.7196 0.1350 0.151 Uiso 1 1 calc R . . H35B H 0.9070 0.7465 0.0799 0.151 Uiso 1 1 calc R . . H35C H 1.0033 0.6969 0.0943 0.151 Uiso 1 1 calc R . . C36 C 0.5230(14) 0.6820(3) 0.0837(4) 0.054(2) Uani 1 1 d . . . H36A H 0.5239 0.6843 0.1244 0.065 Uiso 1 1 calc R . . C37 C 0.744(4) 0.3214(8) 0.4215(10) 0.088(6) Uani 0.50 1 d PU . . H37A H 0.7832 0.3195 0.3832 0.106 Uiso 0.50 1 calc PR . . C38 C 0.407(4) 0.3303(6) 0.4789(7) 0.077(6) Uani 0.50 1 d P . . H38A H 0.2512 0.3348 0.4680 0.116 Uiso 0.50 1 calc PR . . H38B H 0.4644 0.3560 0.5025 0.116 Uiso 0.50 1 calc PR . . H38C H 0.4291 0.3021 0.5010 0.116 Uiso 0.50 1 calc PR . . C39 C 0.421(3) 0.3380(6) 0.3761(7) 0.067(5) Uani 0.50 1 d P . . H39A H 0.5152 0.3349 0.3448 0.101 Uiso 0.50 1 calc PR . . H39B H 0.3716 0.3696 0.3780 0.101 Uiso 0.50 1 calc PR . . H39C H 0.2953 0.3179 0.3688 0.101 Uiso 0.50 1 calc PR . . C40 C 0.5690(19) 0.2746(4) 0.6173(4) 0.027(3) Uani 0.50 1 d PD . . H40 H 0.5412 0.3063 0.6195 0.080 Uiso 0.50 1 calc PR . . C41 C 0.817(3) 0.2179(7) 0.5926(6) 0.062(4) Uani 0.50 1 d PU . . H41A H 0.6938 0.1990 0.6012 0.092 Uiso 0.50 1 calc PR . . H41B H 0.9445 0.2104 0.6193 0.092 Uiso 0.50 1 calc PR . . H41C H 0.8495 0.2122 0.5529 0.092 Uiso 0.50 1 calc PR . . C42 C 0.926(4) 0.2968(9) 0.5856(10) 0.098(7) Uani 0.50 1 d PU . . H42A H 0.8678 0.3273 0.5909 0.148 Uiso 0.50 1 calc PR . . H42B H 0.9595 0.2932 0.5456 0.148 Uiso 0.50 1 calc PR . . H42C H 1.0596 0.2927 0.6116 0.148 Uiso 0.50 1 calc PR . . N1 N 0.7746(9) 0.28310(17) 0.2699(3) 0.0360(13) Uani 1 1 d . . . N2 N 1.3147(8) 0.40632(16) 0.2404(2) 0.0255(11) Uani 1 1 d . . . N3 N -0.2045(8) -0.04394(19) 0.4523(2) 0.0341(13) Uani 1 1 d . . . N4 N -0.3353(8) -0.07642(15) 0.6558(2) 0.0230(10) Uani 1 1 d . . . N5 N -0.0375(9) -0.0661(2) 0.0176(2) 0.0465(16) Uani 1 1 d . . . N6 N -0.2745(8) -0.07576(16) -0.1948(2) 0.0244(11) Uani 1 1 d . . . N7 N 0.6958(11) 0.6968(2) 0.0608(3) 0.0581(18) Uani 1 1 d . . . N8 N 0.5275(19) 0.3273(3) 0.4237(5) 0.035(3) Uani 0.50 1 d P . . N9 N 0.7653(17) 0.2628(5) 0.5987(5) 0.046(3) Uani 0.50 1 d P . . O1 O 0.6994(7) 0.12280(13) 0.26040(17) 0.0286(9) Uani 1 1 d . . . O2 O 0.4123(7) 0.16504(15) 0.2740(2) 0.0383(11) Uani 1 1 d . . . O3 O 0.0550(7) -0.00788(14) 0.30111(17) 0.0291(10) Uani 1 1 d . . . O4 O 0.3284(7) -0.05667(14) 0.32013(16) 0.0280(9) Uani 1 1 d . . . O5 O 0.2864(7) -0.04812(14) 0.18145(16) 0.0286(10) Uani 1 1 d . . . O6 O 0.5928(7) -0.03185(17) 0.14310(19) 0.0411(12) Uani 1 1 d . . . O7 O 0.6171(8) 0.01800(14) 0.2715(2) 0.0270(10) Uani 1 1 d . . . H7 H 0.723(14) 0.022(3) 0.284(4) 0.06(3) Uiso 1 1 d . . . O8 O 0.3621(11) 0.6656(2) 0.0573(3) 0.089(2) Uani 1 1 d . . . O9 O 0.903(3) 0.3179(7) 0.4587(8) 0.131(7) Uani 0.50 1 d P . . O10 O 0.4353(12) 0.2513(3) 0.6304(3) 0.0230(17) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0255(4) 0.0190(3) 0.0212(4) 0.0013(3) 0.0037(3) -0.0013(3) Zn2 0.0245(4) 0.0189(3) 0.0217(4) 0.0007(3) 0.0046(3) 0.0014(3) C1 0.027(3) 0.024(3) 0.025(3) 0.005(2) 0.001(2) -0.008(3) C2 0.030(3) 0.019(3) 0.034(3) 0.007(2) 0.000(3) -0.001(3) C3 0.034(4) 0.026(3) 0.052(4) 0.002(3) 0.020(3) -0.005(3) C4 0.027(3) 0.019(3) 0.042(4) 0.001(3) 0.005(3) -0.004(2) C5 0.032(4) 0.019(3) 0.058(4) 0.003(3) 0.012(3) 0.000(3) C6 0.030(3) 0.016(3) 0.056(4) 0.000(3) 0.008(3) 0.000(3) C7 0.027(3) 0.019(3) 0.042(4) 0.002(3) 0.004(3) -0.003(3) C8 0.024(3) 0.026(3) 0.043(4) 0.002(3) 0.012(3) -0.003(3) C9 0.028(3) 0.018(3) 0.028(3) 0.000(2) 0.006(2) 0.000(2) C10 0.037(4) 0.024(3) 0.037(4) -0.002(3) 0.019(3) 0.001(3) C11 0.033(4) 0.021(3) 0.051(4) -0.006(3) 0.015(3) -0.003(3) C12 0.027(3) 0.020(3) 0.021(3) 0.002(2) 0.003(2) -0.003(3) C13 0.025(3) 0.023(3) 0.025(3) 0.000(2) 0.005(2) 0.002(2) C14 0.026(3) 0.042(4) 0.021(3) 0.008(3) 0.004(2) 0.010(3) C15 0.028(3) 0.029(3) 0.019(3) 0.002(2) 0.006(2) 0.004(3) C16 0.031(4) 0.039(4) 0.035(4) 0.015(3) 0.007(3) 0.009(3) C17 0.027(3) 0.046(4) 0.032(4) 0.006(3) 0.012(3) 0.014(3) C18 0.023(3) 0.028(3) 0.027(3) 0.006(2) 0.002(2) 0.000(2) C19 0.030(3) 0.038(4) 0.021(3) 0.007(3) 0.002(3) 0.009(3) C20 0.031(3) 0.029(3) 0.026(3) 0.000(3) 0.004(3) 0.009(3) C21 0.024(3) 0.035(3) 0.028(3) 0.008(3) 0.003(3) 0.005(3) C22 0.028(3) 0.032(3) 0.028(3) 0.005(3) 0.007(3) 0.005(3) C23 0.028(3) 0.024(3) 0.024(3) -0.001(2) 0.000(3) 0.001(3) C24 0.031(3) 0.036(4) 0.022(3) 0.002(3) 0.000(3) 0.004(3) C25 0.038(4) 0.053(4) 0.026(3) 0.004(3) 0.001(3) -0.012(3) C26 0.034(4) 0.037(4) 0.024(3) 0.001(3) 0.003(3) 0.003(3) C27 0.032(4) 0.156(10) 0.022(4) 0.004(5) 0.008(3) 0.000(5) C28 0.030(4) 0.166(10) 0.025(4) 0.010(5) -0.001(3) -0.010(5) C29 0.031(3) 0.029(3) 0.024(3) 0.001(2) 0.004(3) 0.004(3) C30 0.047(4) 0.064(5) 0.025(3) 0.007(3) 0.004(3) -0.021(4) C31 0.043(4) 0.058(5) 0.029(4) 0.004(3) 0.003(3) -0.027(4) C32 0.033(3) 0.039(4) 0.023(3) 0.009(3) 0.005(3) -0.005(3) C33 0.030(3) 0.039(4) 0.026(3) 0.001(3) 0.002(3) -0.006(3) C34 0.137(11) 0.154(13) 0.082(8) 0.050(8) 0.054(8) 0.036(10) C35 0.081(6) 0.074(6) 0.142(8) 0.000(6) -0.016(6) -0.020(5) C36 0.059(5) 0.042(4) 0.063(5) -0.002(4) 0.012(4) -0.006(4) C37 0.100(10) 0.091(10) 0.073(9) -0.016(8) 0.003(8) 0.016(8) C38 0.122(17) 0.048(10) 0.060(11) -0.024(9) -0.001(11) -0.038(11) C39 0.101(15) 0.055(11) 0.042(9) -0.007(8) -0.014(9) 0.002(10) C40 0.037(7) 0.034(7) 0.010(5) 0.001(5) 0.001(5) 0.015(6) C41 0.058(8) 0.091(9) 0.035(7) -0.012(7) -0.001(6) 0.026(7) C42 0.076(10) 0.118(11) 0.104(10) 0.032(8) 0.022(8) -0.012(8) N1 0.035(3) 0.018(3) 0.057(4) -0.002(2) 0.018(3) -0.007(2) N2 0.028(3) 0.021(2) 0.029(3) 0.002(2) 0.006(2) 0.000(2) N3 0.031(3) 0.048(3) 0.024(3) 0.006(2) 0.006(2) 0.013(3) N4 0.027(3) 0.019(2) 0.023(2) 0.0013(19) 0.005(2) -0.002(2) N5 0.039(3) 0.073(5) 0.028(3) 0.005(3) 0.001(3) -0.010(3) N6 0.028(3) 0.025(3) 0.020(2) 0.001(2) 0.002(2) -0.002(2) N7 0.052(4) 0.054(4) 0.068(5) 0.022(4) 0.005(4) -0.001(3) N8 0.053(7) 0.013(5) 0.035(6) 0.004(4) -0.013(5) -0.007(5) N9 0.019(6) 0.091(10) 0.029(6) 0.021(6) 0.008(5) 0.000(6) O1 0.029(2) 0.019(2) 0.038(2) 0.0030(18) 0.0039(19) -0.0011(18) O2 0.029(2) 0.027(2) 0.060(3) 0.005(2) 0.010(2) -0.007(2) O3 0.031(2) 0.031(2) 0.026(2) 0.0075(18) 0.0054(18) 0.0052(19) O4 0.031(2) 0.031(2) 0.024(2) 0.0052(18) 0.0109(18) 0.0078(19) O5 0.027(2) 0.037(3) 0.021(2) 0.0001(17) 0.0034(17) -0.0038(19) O6 0.030(3) 0.062(3) 0.031(3) 0.003(2) 0.004(2) -0.014(2) O7 0.024(2) 0.021(2) 0.035(2) -0.0047(18) 0.000(2) -0.0013(19) O8 0.062(4) 0.079(5) 0.126(6) -0.021(4) 0.007(4) -0.025(4) O9 0.118(15) 0.154(18) 0.123(15) -0.002(13) 0.020(13) 0.012(14) O10 0.022(4) 0.030(4) 0.020(4) 0.005(3) 0.013(3) -0.009(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 Zn1 O7 1.923(4) . ? Zn1 O1 1.972(4) . ? Zn1 N4 2.026(5) 3_556 ? Zn1 N6 2.032(5) 3 ? Zn2 O7 1.913(4) . ? Zn2 O5 1.967(4) . ? Zn2 O4 1.975(4) . ? Zn2 N2 2.044(5) 2_745 ? C1 O2 1.241(7) . ? C1 O1 1.276(7) . ? C1 C2 1.490(8) . ? C2 C6 1.371(9) . ? C2 C3 1.396(9) . ? C3 N1 1.313(8) . ? C3 H3A 0.9500 . ? C4 N1 1.336(8) . ? C4 C5 1.368(9) . ? C4 C7 1.486(8) . ? C5 C6 1.373(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.403(8) . ? C7 C11 1.407(8) . ? C8 C9 1.380(8) . ? C8 H8A 0.9500 . ? C9 N2 1.349(7) . ? C9 H9A 0.9500 . ? C10 N2 1.338(7) . ? C10 C11 1.371(8) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 O3 1.236(7) . ? C12 O4 1.271(7) . ? C12 C13 1.505(8) . ? C13 C17 1.377(8) . ? C13 C14 1.384(8) . ? C14 N3 1.334(7) . ? C14 H14A 0.9500 . ? C15 N3 1.342(7) . ? C15 C16 1.384(8) . ? C15 C18 1.492(8) . ? C16 C17 1.374(9) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C22 1.382(8) . ? C18 C19 1.384(8) . ? C19 C20 1.362(8) . ? C19 H19A 0.9500 . ? C20 N4 1.335(7) . ? C20 H20A 0.9500 . ? C21 N4 1.329(7) . ? C21 C22 1.383(8) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 O6 1.229(7) . ? C23 O5 1.285(7) . ? C23 C24 1.507(8) . ? C24 C25 1.363(9) . ? C24 C28 1.369(9) . ? C25 N5 1.335(8) . ? C25 H25A 0.9500 . ? C26 C27 1.344(10) . ? C26 N5 1.349(8) . ? C26 C29 1.486(8) . ? C27 C28 1.366(10) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C33 1.374(8) . ? C29 C30 1.396(9) . ? C30 C31 1.367(9) . ? C30 H30A 0.9500 . ? C31 N6 1.332(8) . ? C31 H31A 0.9500 . ? C32 N6 1.338(8) . ? C32 C33 1.365(8) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 N7 1.495(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N7 1.427(12) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 O8 1.217(10) . ? C36 N7 1.315(10) . ? C36 H36A 0.9500 . ? C37 O9 1.25(3) . ? C37 N8 1.35(3) . ? C37 H37A 0.9500 . ? C38 N8 1.55(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 N8 1.272(17) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 O10 1.137(12) . ? C40 N9 1.373(16) . ? C40 H40 0.9500 . ? C41 N9 1.37(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 N9 1.47(2) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N2 Zn2 2.044(5) 2_755 ? N4 Zn1 2.026(5) 3_556 ? N6 Zn1 2.032(5) 3 ? O7 H7 0.70(8) . ? 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 O7 Zn1 O1 107.42(19) . . ? O7 Zn1 N4 102.20(19) . 3_556 ? O1 Zn1 N4 116.91(18) . 3_556 ? O7 Zn1 N6 104.77(19) . 3 ? O1 Zn1 N6 106.97(18) . 3 ? N4 Zn1 N6 117.36(19) 3_556 3 ? O7 Zn2 O5 122.01(19) . . ? O7 Zn2 O4 106.43(18) . . ? O5 Zn2 O4 109.95(17) . . ? O7 Zn2 N2 114.4(2) . 2_745 ? O5 Zn2 N2 106.31(18) . 2_745 ? O4 Zn2 N2 94.13(18) . 2_745 ? O2 C1 O1 123.3(5) . . ? O2 C1 C2 120.1(5) . . ? O1 C1 C2 116.7(5) . . ? C6 C2 C3 116.8(6) . . ? C6 C2 C1 122.7(6) . . ? C3 C2 C1 120.4(6) . . ? N1 C3 C2 124.0(6) . . ? N1 C3 H3A 118.0 . . ? C2 C3 H3A 118.0 . . ? N1 C4 C5 122.6(6) . . ? N1 C4 C7 115.5(5) . . ? C5 C4 C7 121.9(6) . . ? C4 C5 C6 118.9(6) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C2 C6 C5 119.9(6) . . ? C2 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C8 C7 C11 116.6(5) . . ? C8 C7 C4 121.9(6) . . ? C11 C7 C4 121.5(5) . . ? C9 C8 C7 120.2(5) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? N2 C9 C8 122.2(5) . . ? N2 C9 H9A 118.9 . . ? C8 C9 H9A 118.9 . . ? N2 C10 C11 123.9(6) . . ? N2 C10 H10A 118.0 . . ? C11 C10 H10A 118.0 . . ? C10 C11 C7 119.2(6) . . ? C10 C11 H11A 120.4 . . ? C7 C11 H11A 120.4 . . ? O3 C12 O4 125.4(5) . . ? O3 C12 C13 119.4(5) . . ? O4 C12 C13 115.2(5) . . ? C17 C13 C14 117.5(5) . . ? C17 C13 C12 121.9(5) . . ? C14 C13 C12 120.6(5) . . ? N3 C14 C13 123.9(6) . . ? N3 C14 H14A 118.1 . . ? C13 C14 H14A 118.1 . . ? N3 C15 C16 122.2(5) . . ? N3 C15 C18 115.2(5) . . ? C16 C15 C18 122.6(5) . . ? C17 C16 C15 119.1(6) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? C16 C17 C13 119.6(6) . . ? C16 C17 H17A 120.2 . . ? C13 C17 H17A 120.2 . . ? C22 C18 C19 116.7(5) . . ? C22 C18 C15 123.1(5) . . ? C19 C18 C15 120.2(5) . . ? C20 C19 C18 120.8(6) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? N4 C20 C19 122.6(6) . . ? N4 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? N4 C21 C22 123.5(6) . . ? N4 C21 H21A 118.2 . . ? C22 C21 H21A 118.2 . . ? C18 C22 C21 119.2(6) . . ? C18 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? O6 C23 O5 124.5(5) . . ? O6 C23 C24 119.2(5) . . ? O5 C23 C24 116.3(5) . . ? C25 C24 C28 116.5(6) . . ? C25 C24 C23 123.7(6) . . ? C28 C24 C23 119.7(6) . . ? N5 C25 C24 123.7(6) . . ? N5 C25 H25A 118.1 . . ? C24 C25 H25A 118.1 . . ? C27 C26 N5 121.2(6) . . ? C27 C26 C29 121.0(6) . . ? N5 C26 C29 117.9(6) . . ? C26 C27 C28 119.6(7) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C27 C28 C24 120.7(7) . . ? C27 C28 H28A 119.7 . . ? C24 C28 H28A 119.7 . . ? C33 C29 C30 117.1(6) . . ? C33 C29 C26 122.3(6) . . ? C30 C29 C26 120.6(5) . . ? C31 C30 C29 118.8(6) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? N6 C31 C30 124.0(6) . . ? N6 C31 H31A 118.0 . . ? C30 C31 H31A 118.0 . . ? N6 C32 C33 122.9(5) . . ? N6 C32 H32A 118.6 . . ? C33 C32 H32A 118.6 . . ? C32 C33 C29 120.4(6) . . ? C32 C33 H33A 119.8 . . ? C29 C33 H33A 119.8 . . ? N7 C34 H34A 109.5 . . ? N7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N7 C35 H35A 109.5 . . ? N7 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N7 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O8 C36 N7 125.7(9) . . ? O8 C36 H36A 117.2 . . ? N7 C36 H36A 117.2 . . ? O9 C37 N8 134(2) . . ? O9 C37 H37A 113.0 . . ? N8 C37 H37A 113.0 . . ? N8 C38 H38A 109.5 . . ? N8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N8 C39 H39A 109.5 . . ? N8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O10 C40 N9 128.3(12) . . ? O10 C40 H40 115.8 . . ? N9 C40 H40 115.8 . . ? N9 C41 H41A 109.5 . . ? N9 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N9 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N9 C42 H42A 109.5 . . ? N9 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N9 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C3 N1 C4 117.8(6) . . ? C10 N2 C9 117.7(5) . . ? C10 N2 Zn2 118.7(4) . 2_755 ? C9 N2 Zn2 123.3(4) . 2_755 ? C14 N3 C15 117.5(5) . . ? C21 N4 C20 117.2(5) . . ? C21 N4 Zn1 125.8(4) . 3_556 ? C20 N4 Zn1 117.0(4) . 3_556 ? C25 N5 C26 118.1(6) . . ? C31 N6 C32 116.8(5) . . ? C31 N6 Zn1 118.2(4) . 3 ? C32 N6 Zn1 124.4(4) . 3 ? C36 N7 C35 121.7(9) . . ? C36 N7 C34 119.8(9) . . ? C35 N7 C34 118.2(9) . . ? C39 N8 C37 115.1(16) . . ? C39 N8 C38 117.4(15) . . ? C37 N8 C38 126.6(15) . . ? C41 N9 C40 120.0(13) . . ? C41 N9 C42 117.9(15) . . ? C40 N9 C42 122.1(16) . . ? C1 O1 Zn1 106.1(4) . . ? C12 O4 Zn2 121.5(4) . . ? C23 O5 Zn2 107.9(4) . . ? Zn2 O7 Zn1 125.9(3) . . ? Zn2 O7 H7 129(7) . . ? Zn1 O7 H7 105(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.072 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.133 # Attachment '- 3.CIF' data_m2 _database_code_depnum_ccdc_archive 'CCDC 836985' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H35 Cd N7 O7' _chemical_formula_sum 'C31 H35 Cd N7 O7' _chemical_formula_weight 730.06 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c 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 8.1191(5) _cell_length_b 18.8297(11) _cell_length_c 18.7331(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.5740(10) _cell_angle_gamma 90.00 _cell_volume 2815.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5550 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 26.09 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8365 _exptl_absorpt_correction_T_max 0.8985 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15363 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.09 _reflns_number_total 5550 _reflns_number_gt 4119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5550 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.69288(3) 0.939848(11) 0.006551(12) 0.03387(11) Uani 1 1 d . . . C1 C 0.6778(5) 1.05338(17) -0.08661(18) 0.0358(8) Uani 1 1 d . . . C2 C 0.6635(5) 1.10830(17) -0.14448(18) 0.0371(9) Uani 1 1 d . . . C3 C 0.7503(6) 1.1062(2) -0.2014(2) 0.0579(12) Uani 1 1 d . . . H3A H 0.8322 1.0704 -0.2030 0.069 Uiso 1 1 calc R . . C4 C 0.7172(6) 1.1564(2) -0.2559(2) 0.0614(13) Uani 1 1 d . . . H4A H 0.7737 1.1546 -0.2960 0.074 Uiso 1 1 calc R . . C5 C 0.6028(6) 1.2088(2) -0.2519(2) 0.0467(10) Uani 1 1 d . . . C6 C 0.5522(5) 1.16408(17) -0.14430(19) 0.0426(9) Uani 1 1 d . . . H6A H 0.4936 1.1670 -0.1049 0.051 Uiso 1 1 calc R . . C7 C 0.5530(5) 1.26480(19) -0.30839(19) 0.0444(10) Uani 1 1 d . . . C8 C 0.6007(6) 1.2627(2) -0.3749(2) 0.0508(10) Uani 1 1 d . . . H8A H 0.6722 1.2261 -0.3862 0.061 Uiso 1 1 calc R . . C9 C 0.5426(5) 1.3150(2) -0.4252(2) 0.0482(10) Uani 1 1 d . . . H9A H 0.5771 1.3129 -0.4709 0.058 Uiso 1 1 calc R . . C10 C 0.4012(7) 1.3696(2) -0.3487(2) 0.0633(13) Uani 1 1 d . . . H10A H 0.3302 1.4069 -0.3385 0.076 Uiso 1 1 calc R . . C11 C 0.4562(7) 1.3203(2) -0.2946(2) 0.0710(15) Uani 1 1 d . . . H11A H 0.4264 1.3252 -0.2481 0.085 Uiso 1 1 calc R . . C12 C 1.0963(6) 1.3144(2) 0.4383(2) 0.0488(11) Uani 1 1 d . . . C13 C 1.0380(5) 1.2563(2) 0.3838(2) 0.0459(10) Uani 1 1 d . . . C14 C 0.9047(5) 1.2129(2) 0.3897(2) 0.0551(11) Uani 1 1 d . . . H14A H 0.8471 1.2186 0.4292 0.066 Uiso 1 1 calc R . . C15 C 0.8554(5) 1.1611(2) 0.3381(2) 0.0635(13) Uani 1 1 d . . . H15A H 0.7654 1.1300 0.3422 0.076 Uiso 1 1 calc R . . C16 C 0.9393(5) 1.1552(2) 0.2803(2) 0.0491(10) Uani 1 1 d . . . C17 C 1.1134(6) 1.2451(3) 0.3257(2) 0.0704(15) Uani 1 1 d . . . H17A H 1.2063 1.2744 0.3215 0.084 Uiso 1 1 calc R . . C18 C 0.8913(5) 1.1033(2) 0.2206(2) 0.0455(10) Uani 1 1 d . . . C19 C 0.7999(6) 1.0418(3) 0.2281(2) 0.0672(14) Uani 1 1 d . . . H19A H 0.7680 1.0305 0.2731 0.081 Uiso 1 1 calc R . . C20 C 0.7573(6) 0.9981(2) 0.1694(2) 0.0621(13) Uani 1 1 d . . . H20A H 0.6954 0.9564 0.1753 0.074 Uiso 1 1 calc R . . C21 C 0.8852(5) 1.0678(2) 0.0982(2) 0.0403(9) Uani 1 1 d . . . H21A H 0.9158 1.0774 0.0526 0.048 Uiso 1 1 calc R . . C22 C 0.9351(5) 1.1145(2) 0.1540(2) 0.0494(10) Uani 1 1 d . . . H22A H 1.0004 1.1548 0.1467 0.059 Uiso 1 1 calc R . . N1 N 0.5216(4) 1.21386(15) -0.19542(16) 0.0457(8) Uani 1 1 d . . . N2 N 0.4427(4) 1.36741(15) -0.41413(14) 0.0378(7) Uani 1 1 d . . . N3 N 1.0682(5) 1.1966(2) 0.27448(19) 0.0722(12) Uani 1 1 d . . . N4 N 0.7968(4) 1.01007(15) 0.10440(15) 0.0362(7) Uani 1 1 d . . . O1 O 0.5715(3) 1.05287(11) -0.04538(12) 0.0349(6) Uani 1 1 d . . . O2 O 0.7920(4) 1.00778(13) -0.08158(13) 0.0459(7) Uani 1 1 d . . . O3 O 1.2245(4) 1.34734(14) 0.42490(14) 0.0625(9) Uani 1 1 d . . . O4 O 1.0267(4) 1.32552(16) 0.48966(17) 0.0658(9) 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 Cd1 0.0604(2) 0.01993(14) 0.02108(14) 0.00014(9) 0.00687(11) 0.00866(12) C1 0.064(3) 0.0214(17) 0.0229(17) -0.0009(13) 0.0097(16) -0.0019(17) C2 0.061(3) 0.0237(17) 0.0279(18) 0.0022(14) 0.0123(17) -0.0027(17) C3 0.085(3) 0.053(3) 0.043(2) 0.0140(19) 0.032(2) 0.017(2) C4 0.103(4) 0.050(2) 0.039(2) 0.0177(19) 0.033(2) 0.013(3) C5 0.076(3) 0.036(2) 0.030(2) 0.0099(16) 0.0155(19) -0.006(2) C6 0.070(3) 0.0288(19) 0.0316(19) 0.0061(15) 0.0179(18) -0.0028(18) C7 0.071(3) 0.0318(19) 0.0300(19) 0.0099(15) 0.0084(18) -0.0032(19) C8 0.068(3) 0.052(2) 0.033(2) 0.0131(18) 0.0124(19) 0.007(2) C9 0.064(3) 0.055(2) 0.0263(19) 0.0085(18) 0.0105(18) -0.001(2) C10 0.122(4) 0.032(2) 0.041(2) 0.0114(17) 0.028(3) 0.008(2) C11 0.144(5) 0.035(2) 0.043(2) 0.0172(19) 0.043(3) 0.010(3) C12 0.061(3) 0.0312(19) 0.042(2) -0.0032(18) -0.023(2) 0.004(2) C13 0.041(2) 0.048(2) 0.041(2) -0.0126(17) -0.0145(18) -0.0004(19) C14 0.043(2) 0.065(3) 0.058(3) -0.032(2) 0.009(2) -0.003(2) C15 0.042(2) 0.077(3) 0.073(3) -0.048(3) 0.014(2) -0.019(2) C16 0.032(2) 0.062(3) 0.051(2) -0.026(2) 0.0022(18) -0.0092(19) C17 0.065(3) 0.093(4) 0.051(3) -0.030(3) 0.006(2) -0.041(3) C18 0.029(2) 0.059(3) 0.047(2) -0.0260(19) 0.0030(17) -0.0044(18) C19 0.074(3) 0.082(3) 0.052(3) -0.038(2) 0.031(2) -0.045(3) C20 0.085(3) 0.063(3) 0.044(2) -0.026(2) 0.026(2) -0.036(3) C21 0.032(2) 0.054(2) 0.033(2) -0.0091(17) 0.0016(15) -0.0032(18) C22 0.036(2) 0.063(3) 0.045(2) -0.014(2) -0.0019(18) -0.017(2) N1 0.077(2) 0.0283(15) 0.0343(17) 0.0122(13) 0.0169(16) 0.0017(16) N2 0.063(2) 0.0287(15) 0.0200(14) 0.0011(11) 0.0032(13) -0.0131(15) N3 0.061(2) 0.108(3) 0.049(2) -0.040(2) 0.0134(18) -0.047(2) N4 0.0361(17) 0.0387(17) 0.0329(16) -0.0110(13) 0.0042(13) -0.0045(14) O1 0.0573(16) 0.0234(12) 0.0249(12) 0.0042(9) 0.0099(11) 0.0028(11) O2 0.0711(19) 0.0363(14) 0.0347(14) 0.0059(11) 0.0213(13) 0.0107(14) O3 0.103(2) 0.0437(16) 0.0341(15) -0.0072(12) -0.0055(15) -0.0315(17) O4 0.069(2) 0.069(2) 0.0540(19) -0.0317(16) -0.0030(16) 0.0029(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.195(3) 2_745 ? Cd1 N4 2.292(3) . ? Cd1 N2 2.318(3) 2_644 ? Cd1 O2 2.345(2) . ? Cd1 O1 2.393(3) 3_675 ? Cd1 O1 2.469(2) . ? Cd1 C1 2.748(3) . ? C1 O2 1.254(4) . ? C1 O1 1.260(4) . ? C1 C2 1.487(4) . ? C2 C3 1.382(5) . ? C2 C6 1.386(5) . ? C3 C4 1.383(5) . ? C4 C5 1.365(6) . ? C5 N1 1.350(5) . ? C5 C7 1.496(5) . ? C6 N1 1.330(4) . ? C7 C11 1.360(6) . ? C7 C8 1.371(5) . ? C8 C9 1.385(5) . ? C9 N2 1.317(5) . ? C10 N2 1.331(5) . ? C10 C11 1.387(6) . ? C12 O4 1.220(5) . ? C12 O3 1.275(5) . ? C12 C13 1.511(5) . ? C13 C17 1.359(6) . ? C13 C14 1.377(6) . ? C14 C15 1.380(5) . ? C15 C16 1.385(5) . ? C16 N3 1.326(5) . ? C16 C18 1.483(5) . ? C17 N3 1.326(5) . ? C18 C22 1.376(5) . ? C18 C19 1.396(6) . ? C19 C20 1.365(5) . ? C20 N4 1.334(5) . ? C21 N4 1.319(4) . ? C21 C22 1.369(5) . ? N2 Cd1 2.318(3) 2_654 ? O1 Cd1 2.393(3) 3_675 ? O3 Cd1 2.195(3) 2_755 ? 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 O3 Cd1 N4 87.81(11) 2_745 . ? O3 Cd1 N2 91.28(10) 2_745 2_644 ? N4 Cd1 N2 172.66(11) . 2_644 ? O3 Cd1 O2 137.50(11) 2_745 . ? N4 Cd1 O2 97.17(10) . . ? N2 Cd1 O2 88.42(10) 2_644 . ? O3 Cd1 O1 93.59(11) 2_745 3_675 ? N4 Cd1 O1 86.73(9) . 3_675 ? N2 Cd1 O1 86.06(9) 2_644 3_675 ? O2 Cd1 O1 128.73(8) . 3_675 ? O3 Cd1 O1 166.35(10) 2_745 . ? N4 Cd1 O1 83.08(9) . . ? N2 Cd1 O1 96.46(9) 2_644 . ? O2 Cd1 O1 54.28(8) . . ? O1 Cd1 O1 75.81(8) 3_675 . ? O3 Cd1 C1 164.17(13) 2_745 . ? N4 Cd1 C1 91.49(10) . . ? N2 Cd1 C1 91.36(10) 2_644 . ? O2 Cd1 C1 27.06(10) . . ? O1 Cd1 C1 102.16(10) 3_675 . ? O1 Cd1 C1 27.28(10) . . ? O2 C1 O1 121.9(3) . . ? O2 C1 C2 119.2(3) . . ? O1 C1 C2 118.8(3) . . ? O2 C1 Cd1 58.25(16) . . ? O1 C1 Cd1 63.92(17) . . ? C2 C1 Cd1 172.8(2) . . ? C3 C2 C6 116.7(3) . . ? C3 C2 C1 124.0(3) . . ? C6 C2 C1 119.3(3) . . ? C2 C3 C4 119.5(4) . . ? C5 C4 C3 119.7(4) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C7 113.4(4) . . ? C4 C5 C7 124.6(3) . . ? N1 C6 C2 124.6(3) . . ? C11 C7 C8 117.6(3) . . ? C11 C7 C5 119.9(3) . . ? C8 C7 C5 122.5(4) . . ? C7 C8 C9 118.7(4) . . ? N2 C9 C8 124.6(3) . . ? N2 C10 C11 123.3(4) . . ? C7 C11 C10 119.7(4) . . ? O4 C12 O3 125.8(4) . . ? O4 C12 C13 121.6(4) . . ? O3 C12 C13 112.6(4) . . ? C17 C13 C14 116.6(4) . . ? C17 C13 C12 121.5(4) . . ? C14 C13 C12 121.9(4) . . ? C13 C14 C15 119.6(4) . . ? C14 C15 C16 118.9(4) . . ? N3 C16 C15 121.7(3) . . ? N3 C16 C18 115.3(3) . . ? C15 C16 C18 122.9(4) . . ? N3 C17 C13 125.5(4) . . ? C22 C18 C19 116.6(3) . . ? C22 C18 C16 120.5(4) . . ? C19 C18 C16 122.9(4) . . ? C20 C19 C18 118.7(4) . . ? N4 C20 C19 124.4(4) . . ? N4 C21 C22 123.5(4) . . ? C21 C22 C18 120.3(4) . . ? C6 N1 C5 117.4(3) . . ? C9 N2 C10 115.8(3) . . ? C9 N2 Cd1 123.0(2) . 2_654 ? C10 N2 Cd1 120.3(3) . 2_654 ? C16 N3 C17 117.5(4) . . ? C21 N4 C20 116.4(3) . . ? C21 N4 Cd1 122.1(2) . . ? C20 N4 Cd1 121.2(2) . . ? C1 O1 Cd1 160.0(2) . 3_675 ? C1 O1 Cd1 88.8(2) . . ? Cd1 O1 Cd1 104.19(8) 3_675 . ? C1 O2 Cd1 94.7(2) . . ? C12 O3 Cd1 116.3(3) . 2_755 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.601 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.096 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.027 0.500 0.000 531 300 ' ' 2 0.048 1.000 0.500 531 300 ' ' _platon_squeeze_details ; Attempts to refine peaks of residual electron density as guest atoms were unsuccessful, although the atoms of the (DMF) solvent molecule were observed but could not be modeled satisfactorily during the structure refinement. The data were corrected for disordered electron density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON C a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). A total solvent-accessible void volume of 1062.0 A^3^ with a total electron count of 600 (consistent with ca. three molecules of solvent DMF per formula characterized by elemental and thermo-gravimetric analysis) was found in the unit cell. ;