#Supplementary Material (ESI) for Dalton Transactions #This journal is (C) The Royal Society of Chemistry 2001 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1226 data_global_for_complex [ZnTPAA](ClO4)2 1. _database_code_CSD 165086 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr. Aminou. Mohamadou' _publ_contact_author_address # Address of author for correspondence ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; _publ_contact_author_phone '(33) 03 26 91 33 34' _publ_contact_author_fax '(33) 03 26 91 33 34' _publ_contact_author_email aminou.mohamadou@univ-reims.fr _publ_requested_journal 'J. Chem. Soc. Dalton Trans' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in. 'J. Chem. Soc. Dalton Trans The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Equilibrium and structural studies of zinc(II) complexes of tripodal N7 ligands involving pyridine and amine or amide nitrogen donors. Crystal structure of zinc(II) complex. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address ' Aminou Mohamadou ' ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; ' Christian Gerard ' ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; #========= # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ? _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=========================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. Data for complex [ZnTPAA](ClO4)2 1. #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C24 H33 Cl2 N7 O8 Zn' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H33 Cl2 N7 O8 Zn' _chemical_formula_weight 683.85 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Zn ? 0.222 1.431 International_Tables_Vol_IV_Table_2.3.1 #=========================================================================== #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.9115(2) _cell_length_b 16.1184(3) _cell_length_c 19.2407(5) _cell_angle_alpha 90 _cell_angle_beta 103.543(5) _cell_angle_gamma 90 _cell_volume 2988.4(1) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=========================================================================== #========================================================================== == #======= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12287 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance == 35. mm. Scan angle == 2.0 deg 1 scans of 30 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta == 5.90 Omega == 0.00 Kappa == 0.00 90 frames Set 2 Theta == -5.90 Kappa == -164.00 Phi == 0.00 19 frames Friedel pairs were averaged. Internal R == 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12287 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7072 _reflns_number_gt 3876 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3876 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.085 _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_all 0.132 _refine_ls_wR_factor_ref 0.070 _refine_ls_goodness_of_fit_all 2.485 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.677 _refine_diff_density_min -0.505 #=========================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol ZN 0.24781(4) 0.22260(2) 0.62118(2) 0.0381(2) Uani ? ? Zn N1 0.3125(3) 0.3194(2) 0.5576(2) 0.051(2) Uani ? ? N C1 0.1922(5) 0.3765(2) 0.5382(3) 0.062(3) Uani ? ? C C2 0.1394(4) 0.3951(2) 0.6038(3) 0.057(2) Uani ? ? C N2 0.0956(3) 0.3172(2) 0.6338(2) 0.047(2) Uani ? ? N C3 0.0717(5) 0.3318(3) 0.7057(3) 0.070(3) Uani ? ? C C4 -0.0002(4) 0.2622(3) 0.7319(2) 0.059(2) Uani ? ? C N3 -0.0877(4) 0.2173(2) 0.6830(2) 0.062(2) Uani ? ? N C5 -0.1573(5) 0.1563(3) 0.7070(3) 0.079(3) Uani ? ? C C6 -0.1448(5) 0.1411(4) 0.7781(3) 0.103(4) Uani ? ? C C7 -0.0544(7) 0.1864(5) 0.8273(3) 0.110(4) Uani ? ? C C8 0.0193(6) 0.2491(4) 0.8039(3) 0.087(3) Uani ? ? C C9 0.4381(5) 0.3635(3) 0.5990(3) 0.067(3) Uani ? ? C C10 0.5190(4) 0.3121(3) 0.6628(3) 0.064(3) Uani ? ? C N4 0.4226(3) 0.2748(2) 0.7008(2) 0.048(2) Uani ? ? N C11 0.4830(5) 0.2095(3) 0.7521(3) 0.063(3) Uani ? ? C C12 0.3752(4) 0.1481(2) 0.7624(2) 0.050(2) Uani ? ? C N5 0.2630(3) 0.1395(2) 0.7085(2) 0.043(2) Uani ? ? N C13 0.1699(4) 0.0828(2) 0.7144(2) 0.055(2) Uani ? ? C C14 0.1850(5) 0.0324(3) 0.7741(3) 0.082(3) Uani ? ? C C15 0.2969(5) 0.0417(3) 0.8291(3) 0.077(3) Uani ? ? C C16 0.3941(5) 0.0998(3) 0.8234(2) 0.067(3) Uani ? ? C C17 0.3413(5) 0.2785(2) 0.4929(2) 0.069(3) Uani ? ? C C18 0.4330(5) 0.2042(3) 0.5133(3) 0.076(3) Uani ? ? C N6 0.3803(3) 0.1477(2) 0.5621(2) 0.049(2) Uani ? ? N C19 0.2937(4) 0.0795(2) 0.5240(2) 0.061(2) Uani ? ? C C20 0.1440(4) 0.1030(2) 0.4980(2) 0.046(2) Uani ? ? C N7 0.0895(3) 0.1536(2) 0.5391(2) 0.045(2) Uani ? ? N C21 -0.0477(4) 0.1701(2) 0.5186(2) 0.053(2) Uani ? ? C C22 -0.1316(5) 0.1388(2) 0.4580(2) 0.058(2) Uani ? ? C C23 -0.0760(5) 0.0887(3) 0.4151(2) 0.063(3) Uani ? ? C C24 0.0641(5) 0.0695(2) 0.4349(2) 0.056(2) Uani ? ? C CL1 0.5646(1) -0.04629(7) 0.67334(6) 0.0634(6) Uani ? ? Cl O1 0.5928(4) 0.0175(2) 0.6310(2) 0.116(3) Uani ? ? O O2 0.6353(6) -0.1177(3) 0.6619(3) 0.151(4) Uani ? ? O O3 0.4223(4) -0.0641(4) 0.6578(3) 0.159(4) Uani ? ? O O4 0.6097(5) -0.0305(3) 0.7473(2) 0.122(3) Uani ? ? O CL2 -0.2616(1) 0.37826(6) 0.48930(6) 0.0581(6) Uani ? ? Cl O5 -0.1444(4) 0.4022(3) 0.4665(2) 0.126(3) Uani ? ? O O6 -0.3248(5) 0.3081(2) 0.4537(3) 0.119(3) Uani ? ? O O7 -0.3640(4) 0.4409(2) 0.4824(2) 0.088(2) Uani ? ? O O8 -0.2188(4) 0.3581(4) 0.5620(2) 0.145(3) Uani ? ? O H1 0.1206 0.3511 0.5031 0.0864 Uiso calc C1 H H2 0.2200 0.4266 0.5196 0.0864 Uiso calc C1 H H3 0.0623 0.4317 0.5914 0.0810 Uiso calc C2 H H4 0.2112 0.4207 0.6387 0.0810 Uiso calc C2 H H5 0.0168 0.3804 0.7041 0.0911 Uiso calc C3 H H6 0.1589 0.3400 0.7382 0.0911 Uiso calc C3 H H7 -0.2177 0.1222 0.6730 0.1076 Uiso calc C5 H H8 -0.1992 0.0991 0.7930 0.1319 Uiso calc C6 H H9 -0.0419 0.1754 0.8769 0.1513 Uiso calc C7 H H10 0.0823 0.2824 0.8372 0.1149 Uiso calc C8 H H11 0.4098 0.4141 0.6166 0.0866 Uiso calc C9 H H12 0.4976 0.3750 0.5681 0.0866 Uiso calc C9 H H13 0.5820 0.3472 0.6944 0.0875 Uiso calc C10 H H14 0.5692 0.2695 0.6457 0.0875 Uiso calc C10 H H15 0.5237 0.2345 0.7968 0.0895 Uiso calc C11 H H16 0.5524 0.1811 0.7348 0.0895 Uiso calc C11 H H17 0.0899 0.0763 0.6764 0.0706 Uiso calc C13 H H18 0.1170 -0.0084 0.7764 0.1052 Uiso calc C14 H H19 0.3079 0.0085 0.8708 0.1020 Uiso calc C15 H H20 0.4743 0.1071 0.8611 0.0917 Uiso calc C16 H H21 0.3861 0.3170 0.4684 0.0893 Uiso calc C17 H H22 0.2561 0.2614 0.4624 0.0893 Uiso calc C17 H H23 0.5234 0.2224 0.5366 0.0945 Uiso calc C18 H H24 0.4372 0.1745 0.4712 0.0945 Uiso calc C18 H H25 0.2997 0.0337 0.5556 0.0811 Uiso calc C19 H H26 0.3288 0.0639 0.4840 0.0811 Uiso calc C19 H H27 -0.0876 0.2053 0.5479 0.0709 Uiso calc C21 H H28 -0.2278 0.1517 0.4459 0.0798 Uiso calc C22 H H29 -0.1325 0.0672 0.3721 0.0893 Uiso calc C23 H H30 0.1048 0.0341 0.4060 0.0770 Uiso calc C24 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol ZN 0.0393(2) 0.0380(2) 0.0369(2) -0.0031(2) 0.0050(2) 0.0011(2) Zn N1 0.053(2) 0.047(1) 0.054(2) -0.005(1) 0.011(2) 0.007(2) N C1 0.064(3) 0.045(2) 0.083(3) -0.003(2) 0.004(2) 0.019(2) C C2 0.055(2) 0.040(2) 0.086(3) 0.004(2) 0.004(2) 0.003(2) C N2 0.049(2) 0.041(1) 0.051(2) 0.004(1) 0.008(2) -0.006(1) N C3 0.067(3) 0.068(2) 0.074(3) 0.003(2) 0.015(2) -0.026(2) C C4 0.050(2) 0.072(2) 0.056(2) 0.006(2) 0.021(2) -0.016(2) C N3 0.050(2) 0.076(2) 0.064(2) -0.002(2) 0.012(2) -0.001(2) N C5 0.049(3) 0.091(3) 0.110(4) -0.009(2) 0.022(3) 0.003(3) C C6 0.079(3) 0.139(4) 0.100(3) 0.007(3) 0.049(2) 0.039(3) C C7 0.108(4) 0.181(6) 0.068(3) 0.016(5) 0.035(3) 0.009(4) C C8 0.086(3) 0.124(4) 0.061(3) -0.001(3) 0.029(2) -0.022(3) C C9 0.061(2) 0.059(2) 0.082(3) -0.017(2) 0.022(2) 0.005(2) C C10 0.043(2) 0.071(2) 0.084(3) -0.010(2) 0.008(2) -0.005(3) C N4 0.040(2) 0.056(2) 0.049(2) -0.008(1) -0.001(2) 0.000(2) N C11 0.046(2) 0.089(3) 0.059(3) -0.002(2) -0.012(2) 0.002(2) C C12 0.055(2) 0.055(2) 0.041(2) 0.015(2) 0.008(2) -0.001(2) C N5 0.046(2) 0.043(1) 0.039(2) 0.005(1) 0.008(1) 0.002(1) N C13 0.061(2) 0.046(2) 0.058(2) -0.002(2) 0.019(2) 0.004(2) C C14 0.103(3) 0.055(2) 0.097(3) 0.000(2) 0.049(2) 0.017(2) C C15 0.112(4) 0.070(2) 0.059(3) 0.018(3) 0.029(2) 0.023(2) C C16 0.084(3) 0.084(3) 0.041(2) 0.027(2) 0.012(2) 0.007(2) C C17 0.089(3) 0.069(3) 0.054(2) -0.010(2) 0.029(2) 0.010(2) C C18 0.081(3) 0.081(3) 0.067(3) -0.004(2) 0.039(2) -0.003(2) C N6 0.053(2) 0.053(2) 0.043(2) 0.000(1) 0.015(1) -0.001(1) N C19 0.070(3) 0.051(2) 0.065(3) 0.009(2) 0.013(2) -0.005(2) C C20 0.064(2) 0.036(2) 0.041(2) -0.001(2) 0.007(2) -0.002(2) C N7 0.054(2) 0.041(1) 0.041(2) 0.000(1) 0.004(1) -0.006(1) N C21 0.052(2) 0.047(2) 0.061(3) -0.005(2) 0.004(2) -0.012(2) C C22 0.058(3) 0.055(2) 0.060(3) -0.004(2) -0.008(2) -0.005(2) C C23 0.083(3) 0.059(2) 0.051(3) -0.010(2) -0.010(2) -0.013(2) C C24 0.077(3) 0.052(2) 0.045(2) -0.000(2) 0.006(2) -0.010(2) C CL1 0.0710(7) 0.0664(6) 0.0542(6) 0.0120(5) 0.0033(5) 0.0073(5) Cl O1 0.122(3) 0.109(2) 0.119(3) -0.013(2) -0.000(3) 0.049(2) O O2 0.249(5) 0.136(3) 0.101(3) 0.097(3) 0.031(3) 0.008(3) O O3 0.085(3) 0.248(5) 0.190(5) -0.053(3) -0.029(3) 0.088(4) O O4 0.164(4) 0.155(3) 0.071(3) 0.018(3) 0.005(3) -0.013(3) O CL2 0.0456(5) 0.0564(5) 0.0762(7) 0.0033(4) 0.0148(5) 0.0097(5) Cl O5 0.085(2) 0.170(3) 0.138(3) -0.025(2) 0.064(2) -0.021(3) O O6 0.100(3) 0.069(2) 0.248(5) -0.002(2) 0.018(3) -0.041(3) O O7 0.078(2) 0.069(2) 0.127(3) 0.014(2) 0.014(2) 0.016(2) O O8 0.103(3) 0.281(5) 0.105(3) 0.073(3) 0.033(2) 0.086(3) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ZN N1 2.171(3) . . ? ZN N2 2.198(3) . . ? ZN N4 2.194(3) . . ? ZN N5 2.126(3) . . ? ZN N6 2.274(3) . . ? ZN N7 2.243(3) . . ? N1 C1 1.482(6) . . ? N1 C9 1.492(6) . . ? N1 C17 1.494(6) . . ? C1 C2 1.506(7) . . ? C2 N2 1.490(6) . . ? N2 C3 1.476(6) . . ? C3 C4 1.479(7) . . ? C4 N3 1.334(6) . . ? C4 C8 1.371(8) . . ? N3 C5 1.343(7) . . ? C5 C6 1.368(9) . . ? C6 C7 1.35(1) . . ? C7 C8 1.38(1) . . ? C9 C10 1.540(7) . . ? C10 N4 1.463(6) . . ? N4 C11 1.471(6) . . ? C11 C12 1.504(7) . . ? C12 N5 1.339(5) . . ? C12 C16 1.383(6) . . ? N5 C13 1.322(5) . . ? C13 C14 1.387(7) . . ? C14 C15 1.349(8) . . ? C15 C16 1.366(8) . . ? C17 C18 1.499(7) . . ? C18 N6 1.488(6) . . ? N6 C19 1.479(6) . . ? C19 C20 1.499(6) . . ? C20 N7 1.335(5) . . ? C20 C24 1.394(6) . . ? N7 C21 1.351(5) . . ? C21 C22 1.360(6) . . ? C22 C23 1.360(7) . . ? C23 C24 1.386(7) . . ? CL1 O1 1.380(4) . . ? CL1 O2 1.392(5) . . ? CL1 O3 1.401(5) . . ? CL1 O4 1.411(5) . . ? CL2 O5 1.389(4) . . ? CL2 O6 1.392(4) . . ? CL2 O7 1.416(4) . . ? CL2 O8 1.402(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 ZN N2 82.2(1) . . . ? N1 ZN N4 80.2(1) . . . ? N1 ZN N5 157.3(1) . . . ? N1 ZN N6 79.5(1) . . . ? N1 ZN N7 102.1(1) . . . ? N2 ZN N4 96.1(1) . . . ? N2 ZN N5 105.8(1) . . . ? N2 ZN N6 156.2(1) . . . ? N2 ZN N7 92.1(1) . . . ? N4 ZN N5 78.0(1) . . . ? N4 ZN N6 95.7(1) . . . ? N4 ZN N7 171.7(1) . . . ? N5 ZN N6 96.8(1) . . . ? N5 ZN N7 98.7(1) . . . ? N6 ZN N7 77.0(1) . . . ? C1 N1 C9 111.1(3) . . . ? C1 N1 C17 111.3(4) . . . ? C9 N1 C17 111.0(4) . . . ? N1 C1 C2 109.3(4) . . . ? C1 C2 N2 110.3(3) . . . ? C2 N2 C3 110.7(4) . . . ? N2 C3 C4 113.2(4) . . . ? C3 C4 N3 117.2(5) . . . ? C3 C4 C8 119.8(5) . . . ? N3 C4 C8 122.9(5) . . . ? C4 N3 C5 117.2(5) . . . ? N3 C5 C6 122.7(6) . . . ? C5 C6 C7 119.5(7) . . . ? C6 C7 C8 118.7(7) . . . ? C4 C8 C7 118.9(6) . . . ? N1 C9 C10 112.5(3) . . . ? C9 C10 N4 109.9(4) . . . ? C10 N4 C11 114.8(4) . . . ? N4 C11 C12 111.7(4) . . . ? C11 C12 N5 116.9(4) . . . ? C11 C12 C16 121.5(5) . . . ? N5 C12 C16 121.5(4) . . . ? C12 N5 C13 118.3(4) . . . ? N5 C13 C14 122.3(5) . . . ? C13 C14 C15 119.6(5) . . . ? C14 C15 C16 118.6(5) . . . ? C12 C16 C15 119.7(5) . . . ? N1 C17 C18 111.0(4) . . . ? C17 C18 N6 111.9(4) . . . ? C18 N6 C19 113.0(4) . . . ? N6 C19 C20 113.1(3) . . . ? C19 C20 N7 117.6(4) . . . ? C19 C20 C24 120.6(4) . . . ? N7 C20 C24 121.8(4) . . . ? C20 N7 C21 117.8(4) . . . ? N7 C21 C22 123.3(4) . . . ? C21 C22 C23 119.1(5) . . . ? C22 C23 C24 119.3(4) . . . ? C20 C24 C23 118.7(4) . . . ? O1 CL1 O2 110.2(4) . . . ? O1 CL1 O3 111.1(3) . . . ? O1 CL1 O4 113.6(3) . . . ? O2 CL1 O3 108.4(5) . . . ? O2 CL1 O4 104.8(3) . . . ? O3 CL1 O4 108.5(4) . . . ? O5 CL2 O6 112.6(3) . . . ? O5 CL2 O7 114.0(3) . . . ? O5 CL2 O8 107.4(3) . . . ? O6 CL2 O7 107.7(3) . . . ? O6 CL2 O8 107.4(4) . . . ? O7 CL2 O8 107.6(3) . . . ? # == == ============================================================END data_global_for Protonated TRENPICAM [HTRENPICAM](ClO4). _database_code_CSD 165087 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr. Aminou. Mohamadou' _publ_contact_author_address # Address of author for correspondence ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; _publ_contact_author_phone '(33) 03 26 91 33 34' _publ_contact_author_fax '(33) 03 26 91 32 43' _publ_contact_author_email aminou.mohamadou@univ-reims.fr _publ_requested_journal 'J. Chem. Soc. Dalton Trans' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in. 'J. Chem. Soc. Dalton Trans The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Equilibrium and structural studies of zinc(II) complexes of tripodal N7 ligands involving pyridine and amine or amide nitrogen donors. Crystal structure of zinc(II) complex. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address ' Aminou Mohamadou ' ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; 'Christian Gerard ' ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; #========================================================================= # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ? _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=========================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #Data for compound [HTRENPICAM](ClO4) #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C24 H28 Cl N7 O7' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H28 Cl N7 O7' _chemical_formula_weight 561.99 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 7.3724(1) _cell_length_b 27.1686(6) _cell_length_c 13.3039(3) _cell_angle_alpha 90 _cell_angle_beta 100.696(5) _cell_angle_gamma 90 _cell_volume 2618.44(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 10162 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.43 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=========================================================================== #========================================================================== == #======= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 10162 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance == 36. mm. Scan angle == 2.0 deg 1 scans of 40 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta == 6.30 Omega == 0.00 Kappa == 0.00 151 frames Set 2 Theta == -6.10 Kappa == -141.00 Phi == 0.00 30 frames Friedel pairs were not averaged. Internal R == 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10162 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6140 _reflns_number_gt 2803 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=========================================================================== #========================================================================== == #======= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2803 _refine_ls_number_parameters 370 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.123 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_all 0.203 _refine_ls_wR_factor_ref 0.070 _refine_ls_goodness_of_fit_all 3.124 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_shift/su_max 0.006 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.951 _refine_diff_density_min -0.263 #=========================================================================== #========================================================================== == #======= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol N1 0.5939(4) 0.0590(1) 0.7846(2) 0.038(2) 1.000 Uani ? ? N C1 0.6040(6) 0.0102(1) 0.7316(3) 0.041(2) 1.000 Uani ? ? C C2 0.7777(6) 0.0029(1) 0.6874(3) 0.046(2) 1.000 Uani ? ? C N2 0.7760(5) 0.0255(1) 0.5871(2) 0.044(2) 1.000 Uani ? ? N C3 0.7875(5) 0.0742(1) 0.5772(3) 0.037(2) 1.000 Uani ? ? C O1 0.7819(4) 0.10365(9) 0.6480(2) 0.044(1) 1.000 Uani ? ? O C4 0.8134(5) 0.0925(1) 0.4741(3) 0.037(2) 1.000 Uani ? ? C N3 0.7888(5) 0.0595(1) 0.3977(2) 0.044(2) 1.000 Uani ? ? N C5 0.8160(6) 0.0758(2) 0.3071(3) 0.053(2) 1.000 Uani ? ? C C6 0.8700(6) 0.1231(2) 0.2904(3) 0.054(2) 1.000 Uani ? ? C C7 0.8944(6) 0.1562(2) 0.3694(3) 0.050(2) 1.000 Uani ? ? C C8 0.8641(5) 0.1406(1) 0.4638(3) 0.042(2) 1.000 Uani ? ? C C9 0.4032(6) 0.0683(2) 0.8051(3) 0.047(2) 1.000 Uani ? ? C C10 0.2564(5) 0.0742(2) 0.7104(3) 0.047(2) 1.000 Uani ? ? C N4 0.2993(5) 0.1128(1) 0.6431(3) 0.043(2) 1.000 Uani ? ? N C11 0.3188(5) 0.1038(1) 0.5465(3) 0.042(2) 1.000 Uani ? ? C O2 0.3116(5) 0.0628(1) 0.5092(2) 0.065(2) 1.000 Uani ? ? O C12 0.3501(5) 0.1477(1) 0.4854(3) 0.043(2) 1.000 Uani ? ? C N5 0.3373(6) 0.1915(1) 0.5283(3) 0.059(2) 1.000 Uani ? ? N C13 0.3631(9) 0.2315(2) 0.4726(5) 0.074(3) 1.000 Uani ? ? C C14 0.4030(8) 0.2283(2) 0.3764(4) 0.083(3) 1.000 Uani ? ? C C15 0.4135(7) 0.1833(2) 0.3327(4) 0.077(3) 1.000 Uani ? ? C C16 0.3863(6) 0.1418(2) 0.3882(4) 0.058(3) 1.000 Uani ? ? C C17 0.7324(6) 0.0609(2) 0.8837(3) 0.046(2) 1.000 Uani ? ? C C18 0.7616(6) 0.1118(2) 0.9310(3) 0.051(2) 1.000 Uani ? ? C N6 0.8400(5) 0.1471(1) 0.8683(3) 0.048(2) 1.000 Uani ? ? N C19 0.7277(6) 0.1753(1) 0.8002(3) 0.047(2) 1.000 Uani ? ? C O3 0.5577(4) 0.1737(1) 0.7883(2) 0.053(2) 1.000 Uani ? ? O C20 0.8205(6) 0.2096(1) 0.7370(3) 0.048(2) 1.000 Uani ? ? C N7 1.0032(5) 0.2056(1) 0.7456(3) 0.058(2) 1.000 Uani ? ? N C21 1.0812(7) 0.2356(2) 0.6851(4) 0.069(3) 1.000 Uani ? ? C C22 0.9860(8) 0.2686(2) 0.6185(4) 0.075(3) 1.000 Uani ? ? C C23 0.8011(8) 0.2722(2) 0.6115(4) 0.069(3) 1.000 Uani ? ? C C24 0.7150(6) 0.2419(2) 0.6721(4) 0.057(3) 1.000 Uani ? ? C CL 0.2877(2) 0.40288(5) 0.56016(9) 0.0687(7) 1.000 Uani ? ? Cl O4 0.4443(5) 0.4312(2) 0.5690(3) 0.100(2) 1.000 Uani ? ? O O5 0.190(1) 0.3935(4) 0.4687(6) 0.107(6) 0.500 Uani ? ? O O6 0.255(1) 0.3630(2) 0.4995(6) 0.080(5) 0.500 Uani ? ? O O7 0.1950(5) 0.4053(2) 0.6413(3) 0.105(3) 1.000 Uani ? ? O O5A 0.402(1) 0.3538(3) 0.5806(9) 0.142(7) 0.500 Uani ? ? O O6A 0.177(1) 0.4431(3) 0.4871(7) 0.108(6) 0.500 Uani ? ? O H01 0.6366 0.0863 0.7309 0.0489 1.000 Uiso ? ? H H1 0.5006 0.0078 0.6773 0.0570 1.000 Uiso calc C1 H H2 0.5982 -0.0153 0.7797 0.0570 1.000 Uiso calc C1 H H3 0.7961 -0.0315 0.6810 0.0616 1.000 Uiso calc C2 H H4 0.8783 0.0164 0.7343 0.0616 1.000 Uiso calc C2 H H5 0.7970 0.0536 0.2511 0.0700 1.000 Uiso calc C5 H H6 0.8902 0.1327 0.2247 0.0695 1.000 Uiso calc C6 H H7 0.9313 0.1890 0.3596 0.0648 1.000 Uiso calc C7 H H8 0.8780 0.1627 0.5201 0.0543 1.000 Uiso calc C8 H H9 0.4066 0.0976 0.8444 0.0597 1.000 Uiso calc C9 H H10 0.3697 0.0414 0.8434 0.0597 1.000 Uiso calc C9 H H11 0.1428 0.0820 0.7307 0.0593 1.000 Uiso calc C10 H H12 0.2444 0.0440 0.6739 0.0593 1.000 Uiso calc C10 H H13 0.3531 0.2632 0.5014 0.1110 1.000 Uiso calc C13 H H14 0.4233 0.2573 0.3402 0.1138 1.000 Uiso calc C14 H H15 0.4390 0.1805 0.2655 0.1017 1.000 Uiso calc C15 H H16 0.3924 0.1099 0.3598 0.0751 1.000 Uiso calc C16 H H17 0.8475 0.0493 0.8708 0.0624 1.000 Uiso calc C17 H H18 0.6906 0.0397 0.9315 0.0624 1.000 Uiso calc C17 H H19 0.8429 0.1090 0.9951 0.0682 1.000 Uiso calc C18 H H20 0.6457 0.1240 0.9413 0.0682 1.000 Uiso calc C18 H H21 1.2109 0.2335 0.6891 0.0886 1.000 Uiso calc C21 H H22 1.0484 0.2888 0.5776 0.0991 1.000 Uiso calc C22 H H23 0.7315 0.2951 0.5659 0.0928 1.000 Uiso calc C23 H H24 0.5853 0.2435 0.6687 0.0754 1.000 Uiso calc C24 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol N1 0.051(2) 0.034(2) 0.031(2) -0.004(1) 0.014(1) -0.002(1) N C1 0.068(3) 0.028(2) 0.036(2) -0.004(2) 0.012(2) -0.000(2) C C2 0.072(3) 0.032(2) 0.041(2) 0.006(2) 0.018(2) 0.002(2) C N2 0.066(2) 0.033(2) 0.038(2) 0.003(2) 0.020(1) 0.005(2) N C3 0.041(2) 0.034(2) 0.037(2) -0.001(2) 0.011(2) -0.002(2) C O1 0.065(2) 0.034(1) 0.040(1) -0.005(1) 0.020(1) -0.006(1) O C4 0.037(2) 0.035(2) 0.038(2) 0.002(2) 0.011(2) 0.001(2) C N3 0.061(2) 0.039(2) 0.036(2) 0.001(2) 0.019(1) -0.003(2) N C5 0.075(3) 0.050(3) 0.040(2) 0.001(2) 0.022(2) -0.002(2) C C6 0.064(2) 0.057(3) 0.044(2) 0.004(2) 0.023(2) 0.010(2) C C7 0.054(2) 0.041(2) 0.056(2) -0.002(2) 0.013(2) 0.011(2) C C8 0.044(2) 0.037(2) 0.044(2) -0.003(2) 0.009(2) 0.002(2) C C9 0.055(2) 0.046(2) 0.042(2) -0.009(2) 0.022(2) -0.003(2) C C10 0.047(2) 0.046(2) 0.048(2) -0.006(2) 0.019(2) -0.001(2) C N4 0.053(2) 0.036(2) 0.042(2) -0.002(2) 0.011(2) -0.000(2) N C11 0.045(2) 0.033(2) 0.051(2) -0.002(2) 0.012(2) 0.003(2) C O2 0.147(3) 0.032(2) 0.057(2) -0.010(2) 0.042(2) -0.009(2) O C12 0.037(2) 0.036(2) 0.057(2) 0.001(2) 0.004(2) 0.008(2) C N5 0.076(3) 0.036(2) 0.074(3) -0.007(2) -0.004(2) 0.010(2) N C13 0.106(4) 0.041(3) 0.095(4) -0.015(3) -0.018(3) 0.020(3) C C14 0.084(4) 0.075(3) 0.091(4) -0.031(3) -0.016(3) 0.046(3) C C15 0.063(3) 0.089(4) 0.082(3) -0.005(3) 0.013(3) 0.037(3) C C16 0.050(2) 0.063(3) 0.062(3) 0.006(2) 0.017(2) 0.019(2) C C17 0.062(3) 0.051(2) 0.031(2) -0.002(2) 0.008(2) -0.002(2) C C18 0.063(3) 0.055(3) 0.038(2) -0.002(2) 0.007(2) -0.010(2) C N6 0.061(2) 0.043(2) 0.041(2) -0.005(2) 0.009(2) -0.011(2) N C19 0.060(2) 0.036(2) 0.047(2) -0.004(2) 0.014(2) -0.020(2) C O3 0.052(2) 0.045(2) 0.064(2) -0.005(1) 0.015(1) -0.009(2) O C20 0.053(2) 0.037(2) 0.059(2) -0.011(2) 0.013(2) -0.021(2) C N7 0.058(2) 0.055(2) 0.061(2) -0.015(2) 0.009(2) -0.016(2) N C21 0.065(3) 0.065(3) 0.077(3) -0.027(2) 0.019(2) -0.016(3) C C22 0.090(3) 0.057(3) 0.084(4) -0.024(3) 0.020(3) -0.003(3) C C23 0.086(3) 0.048(3) 0.079(3) -0.010(3) 0.012(3) 0.003(3) C C24 0.064(3) 0.041(2) 0.070(3) -0.010(2) 0.014(2) -0.006(2) C CL 0.0852(7) 0.0785(8) 0.0485(6) -0.0324(6) 0.0284(5) -0.0207(6) Cl O4 0.094(2) 0.131(3) 0.082(2) -0.049(2) 0.041(2) -0.050(2) O O5 0.089(4) 0.27(1) 0.052(4) -0.095(5) 0.021(3) -0.051(5) O O6 0.145(6) 0.038(3) 0.093(5) -0.017(4) 0.040(4) -0.023(4) O O7 0.124(2) 0.134(3) 0.070(2) -0.033(3) 0.061(2) -0.024(2) O O5A 0.195(8) 0.070(5) 0.212(9) 0.050(5) 0.106(6) 0.034(6) O O6A 0.101(6) 0.115(6) 0.108(6) 0.010(5) 0.024(5) 0.029(5) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.510(5) . . ? N1 C9 1.503(5) . . ? N1 C17 1.511(5) . . ? N1 H01 1.1168 . . ? C1 C2 1.518(6) . . ? C1 H01 2.0839 . . ? C2 N2 1.468(5) . . ? N2 C3 1.334(5) . . ? C3 O1 1.242(5) . . ? C3 C4 1.504(5) . . ? O1 H01 1.7394 . . ? C4 N3 1.342(5) . . ? C4 C8 1.375(5) . . ? N3 C5 1.334(5) . . ? C5 C6 1.374(6) . . ? C6 C7 1.370(6) . . ? C7 C8 1.381(6) . . ? C9 C10 1.510(6) . . ? C9 H01 2.1921 . . ? C10 N4 1.452(5) . . ? N4 C11 1.342(5) . . ? C11 O2 1.217(5) . . ? C11 C12 1.485(6) . . ? C12 N5 1.331(6) . . ? C12 C16 1.377(6) . . ? N5 C13 1.349(7) . . ? C13 C14 1.369(9) . . ? C14 C15 1.363(9) . . ? C15 C16 1.382(7) . . ? C17 C18 1.520(6) . . ? C17 H01 2.1399 . . ? C18 N6 1.460(6) . . ? N6 C19 1.346(6) . . ? C19 O3 1.234(5) . . ? C19 C20 1.503(6) . . ? C20 N7 1.335(6) . . ? C20 C24 1.367(7) . . ? N7 C21 1.347(7) . . ? C21 C22 1.361(8) . . ? C22 C23 1.353(8) . . ? C23 C24 1.387(7) . . ? CL O4 1.374(4) . . ? CL O5 1.32(1) . . ? CL O6 1.35(1) . . ? CL O7 1.382(4) . . ? CL O5A 1.57(1) . . ? CL O6A 1.59(1) . . ? O4 O5A 2.13(1) . . ? O4 O6A 2.09(1) . . ? O5 O6 1.01(2) . . ? O5 O6A 1.38(2) . . ? O6 O5A 1.40(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C9 111.2(3) . . . ? C1 N1 C17 110.7(3) . . . ? C1 N1 H01 103.97 . . . ? C9 N1 C17 109.9(3) . . . ? C9 N1 H01 112.78 . . . ? C17 N1 H01 108.11 . . . ? N1 C1 C2 114.4(3) . . . ? N1 C1 H01 31.34 . . . ? C2 C1 H01 91.25 . . . ? C1 C2 N2 115.6(4) . . . ? C2 N2 C3 121.0(3) . . . ? N2 C3 O1 123.5(4) . . . ? N2 C3 C4 116.0(4) . . . ? O1 C3 C4 120.5(4) . . . ? C3 O1 H01 114.69 . . . ? C3 C4 N3 116.6(3) . . . ? C3 C4 C8 119.2(4) . . . ? N3 C4 C8 124.1(4) . . . ? C4 N3 C5 116.1(4) . . . ? N3 C5 C6 123.7(4) . . . ? C5 C6 C7 119.3(4) . . . ? C6 C7 C8 118.5(4) . . . ? C4 C8 C7 118.3(4) . . . ? N1 C9 C10 114.6(3) . . . ? N1 C9 H01 28.02 . . . ? C10 C9 H01 95.82 . . . ? C9 C10 N4 112.7(3) . . . ? C10 N4 C11 122.2(3) . . . ? N4 C11 O2 123.6(4) . . . ? N4 C11 C12 115.6(4) . . . ? O2 C11 C12 120.8(4) . . . ? C11 C12 N5 116.9(4) . . . ? C11 C12 C16 119.9(4) . . . ? N5 C12 C16 123.2(4) . . . ? C12 N5 C13 117.1(5) . . . ? N5 C13 C14 122.7(6) . . . ? C13 C14 C15 119.7(5) . . . ? C14 C15 C16 118.6(6) . . . ? C12 C16 C15 118.7(5) . . . ? N1 C17 C18 114.4(4) . . . ? N1 C17 H01 29.74 . . . ? C18 C17 H01 95.45 . . . ? C17 C18 N6 113.7(4) . . . ? C18 N6 C19 119.9(4) . . . ? N6 C19 O3 123.3(4) . . . ? N6 C19 C20 116.2(4) . . . ? O3 C19 C20 120.5(4) . . . ? C19 C20 N7 117.3(4) . . . ? C19 C20 C24 119.1(4) . . . ? N7 C20 C24 123.6(5) . . . ? C20 N7 C21 115.8(5) . . . ? N7 C21 C22 124.2(5) . . . ? C21 C22 C23 118.9(5) . . . ? C22 C23 C24 118.7(5) . . . ? C20 C24 C23 118.7(5) . . . ? O4 CL O5 119.5(6) . . . ? O4 CL O6 123.6(7) . . . ? O4 CL O7 115.8(3) . . . ? O4 CL O5A 92.5(6) . . . ? O4 CL O6A 89.8(5) . . . ? O5 CL O6 44.4(8) . . . ? O5 CL O7 117.9(5) . . . ? O5 CL O5A 100(1) . . . ? O5 CL O6A 55.7(9) . . . ? O6 CL O7 116.7(6) . . . ? O6 CL O5A 56.7(7) . . . ? O6 CL O6A 100.0(7) . . . ? O7 CL O5A 103.5(5) . . . ? O7 CL O6A 99.9(5) . . . ? O5A CL O6A 152.7(7) . . . ? CL O4 O5A 47.5(4) . . . ? CL O4 O6A 49.2(3) . . . ? O5A O4 O6A 93.2(5) . . . ? CL O5 O6 69(1) . . . ? CL O5 O6A 72.1(8) . . . ? O6 O5 O6A 141(1) . . . ? CL O6 O5 66.4(9) . . . ? CL O6 O5A 69.9(8) . . . ? O5 O6 O5A 134(1) . . . ? CL O5A O4 40.0(3) . . . ? CL O5A O6 53.4(5) . . . ? O4 O5A O6 82.6(6) . . . ? CL O6A O4 41.0(3) . . . ? CL O6A O5 52.2(6) . . . ? O4 O6A O5 81.3(7) . . . ? N1 H01 C1 44.69 . . . ? N1 H01 O1 149.99 . . . ? N1 H01 C9 39.20 . . . ? N1 H01 C17 42.15 . . . ? C1 H01 O1 110.87 . . . ? C1 H01 C9 71.06 . . . ? C1 H01 C17 72.09 . . . ? O1 H01 C9 166.79 . . . ? O1 H01 C17 123.81 . . . ? C9 H01 C17 69.39 . . . ? # ========================================================================= #=============================================================END