Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr. Aminou Mohamadou' _publ_contact_author_address ; Dr. A. Mohamadou 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_ASTM ? _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 ; Structure effects of potentially hexadentate N4O2 N4S2 or N6 donor ligands involving pyridine, amine and ether or thioether donors. Crystal structure of Copper(II) and Zinc(II) complexes. ; # 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 ' Caroline Jubert ' ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; ' Aminou Mohamadou ' ; Universite de Reims Champagne-Ardenne GRECI, Moulin de la Housse BP 1039 51687 Reims cedex 2 France ; 'Marrot, Jerome' ; Institut Lavoisier, IREM, UMR CNRS C 8637 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; ' Jean-Pierre Barbier ' ; 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_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of G\"ottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #=========================================================================== data_complex [Cupydado](ClO4)2 (1) _database_code_CSD 142187 # 5. CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Cl2 Cu N4 O10' _chemical_formula_weight 592.87 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5178(2) _cell_length_b 13.9439(2) _cell_length_c 18.3494(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.1180(10) _cell_angle_gamma 90.00 _cell_volume 2431.64(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9307 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5904 _exptl_absorpt_correction_T_max 0.7188 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16933 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 29.76 _reflns_number_total 9516 _reflns_number_gt 7175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0619P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(11) _refine_ls_number_reflns 9516 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Cl1 Cl 0.98730(11) 0.81844(7) 0.34951(6) 0.0606(3) Uani 1 1 d . . . O1A O 0.9091(6) 0.7665(4) 0.2940(2) 0.1215(15) Uani 1 1 d . . . O1B O 0.9786(6) 0.7815(4) 0.4201(2) 0.1352(19) Uani 1 1 d . . . O1C O 1.1203(6) 0.8186(9) 0.3336(4) 0.225(5) Uani 1 1 d . . . O1D O 0.9467(10) 0.9139(4) 0.3483(4) 0.222(4) Uani 1 1 d . . . Cl2 Cl 0.54139(11) 0.19805(8) 0.75542(6) 0.0608(3) Uani 1 1 d . . . O2A O 0.6116(4) 0.2786(3) 0.7909(2) 0.0905(10) Uani 1 1 d . . . O2B O 0.6389(5) 0.1352(4) 0.7285(3) 0.1143(15) Uani 1 1 d . . . O2C O 0.4517(6) 0.2353(5) 0.6983(3) 0.158(2) Uani 1 1 d . . . O2D O 0.4616(7) 0.1506(4) 0.8063(3) 0.158(3) Uani 1 1 d . . . Cl3 Cl 0.54046(11) 0.18724(8) 0.11304(6) 0.0625(3) Uani 1 1 d . . . O3A O 0.5397(7) 0.0922(3) 0.0948(4) 0.159(3) Uani 1 1 d . . . O3B O 0.5584(6) 0.2367(4) 0.0450(3) 0.142(2) Uani 1 1 d . . . O3C O 0.4123(7) 0.2164(7) 0.1373(4) 0.200(4) Uani 1 1 d . . . O3D O 0.6527(6) 0.2108(5) 0.1598(3) 0.148(2) Uani 1 1 d . . . Cl4 Cl 0.98581(10) 0.79129(8) 0.69200(7) 0.0670(3) Uani 1 1 d . . . O4A O 1.1250(3) 0.7637(3) 0.7181(2) 0.0898(10) Uani 1 1 d . . . O4B O 0.8894(4) 0.7796(5) 0.7458(3) 0.133(2) Uani 1 1 d . . . O4C O 0.9843(5) 0.8866(4) 0.6712(4) 0.177(3) Uani 1 1 d . . . O4D O 0.9453(5) 0.7367(6) 0.6312(3) 0.173(3) Uani 1 1 d . . . Cu1 Cu 0.38292(5) 0.77610(3) 0.61520(2) 0.05067(13) Uani 1 1 d . . . O1 O 0.6183(3) 0.8424(2) 0.60038(15) 0.0584(7) Uani 1 1 d . . . O2 O 0.4703(4) 0.7528(2) 0.49322(16) 0.0701(8) Uani 1 1 d . . . N1 N 0.2895(3) 0.8972(3) 0.5824(2) 0.0565(8) Uani 1 1 d . . . N2 N 0.4316(4) 0.8567(3) 0.70976(19) 0.0629(9) Uani 1 1 d . . . H2N H 0.4141 0.8191 0.7488 0.076 Uiso 1 1 calc R . . N3 N 0.2370(4) 0.6816(3) 0.5618(3) 0.0755(12) Uani 1 1 d . . . H3N H 0.1504 0.7092 0.5620 0.091 Uiso 1 1 calc R . . N4 N 0.4721(4) 0.6504(2) 0.64547(18) 0.0542(8) Uani 1 1 d . . . C1 C 0.2349(5) 0.9157(3) 0.5153(3) 0.0688(12) Uani 1 1 d . . . H1 H 0.2440 0.8694 0.4794 0.083 Uiso 1 1 calc R . . C2 C 0.1664(5) 0.9992(4) 0.4965(4) 0.0866(16) Uani 1 1 d . . . H2 H 0.1281 1.0084 0.4492 0.104 Uiso 1 1 calc R . . C3 C 0.1551(5) 1.0692(4) 0.5487(4) 0.0859(17) Uani 1 1 d . . . H3 H 0.1087 1.1265 0.5375 0.103 Uiso 1 1 calc R . . C4 C 0.2142(5) 1.0527(3) 0.6184(4) 0.0775(15) Uani 1 1 d . . . H4 H 0.2107 1.0996 0.6543 0.093 Uiso 1 1 calc R . . C5 C 0.2787(4) 0.9651(3) 0.6339(3) 0.0607(11) Uani 1 1 d . . . C6 C 0.3324(5) 0.9375(3) 0.7095(3) 0.0725(14) Uani 1 1 d . . . H6A H 0.3788 0.9924 0.7327 0.087 Uiso 1 1 calc R . . H6B H 0.2533 0.9203 0.7380 0.087 Uiso 1 1 calc R . . C7 C 0.5809(5) 0.8886(4) 0.7187(2) 0.0704(12) Uani 1 1 d . . . H7A H 0.6389 0.8357 0.7369 0.084 Uiso 1 1 calc R . . H7B H 0.5887 0.9401 0.7543 0.084 Uiso 1 1 calc R . . C8 C 0.6328(4) 0.9228(3) 0.6478(3) 0.0606(11) Uani 1 1 d . . . H8A H 0.5767 0.9763 0.6289 0.073 Uiso 1 1 calc R . . H8B H 0.7303 0.9428 0.6536 0.073 Uiso 1 1 calc R . . C9 C 0.6560(5) 0.8571(4) 0.5277(2) 0.0696(12) Uani 1 1 d . . . H9A H 0.7560 0.8699 0.5264 0.084 Uiso 1 1 calc R . . H9B H 0.6046 0.9110 0.5061 0.084 Uiso 1 1 calc R . . C10 C 0.6191(5) 0.7679(4) 0.4881(2) 0.0760(13) Uani 1 1 d . . . H10A H 0.6417 0.7735 0.4373 0.091 Uiso 1 1 calc R . . H10B H 0.6714 0.7143 0.5096 0.091 Uiso 1 1 calc R . . C11 C 0.4202(7) 0.6607(4) 0.4715(3) 0.0837(16) Uani 1 1 d . . . H11A H 0.4685 0.6111 0.5003 0.100 Uiso 1 1 calc R . . H11B H 0.4357 0.6495 0.4204 0.100 Uiso 1 1 calc R . . C12 C 0.2671(7) 0.6599(4) 0.4840(3) 0.0914(18) Uani 1 1 d . . . H12A H 0.2288 0.5973 0.4710 0.110 Uiso 1 1 calc R . . H12B H 0.2200 0.7069 0.4523 0.110 Uiso 1 1 calc R . . C13 C 0.2378(5) 0.5965(4) 0.6117(4) 0.0834(16) Uani 1 1 d . . . H13A H 0.1822 0.6103 0.6533 0.100 Uiso 1 1 calc R . . H13B H 0.1964 0.5417 0.5861 0.100 Uiso 1 1 calc R . . C14 C 0.3845(5) 0.5743(3) 0.6372(2) 0.0603(11) Uani 1 1 d . . . C15 C 0.4343(6) 0.4823(3) 0.6507(3) 0.0702(13) Uani 1 1 d . . . H15 H 0.3732 0.4302 0.6469 0.084 Uiso 1 1 calc R . . C16 C 0.5766(7) 0.4680(4) 0.6702(3) 0.0796(15) Uani 1 1 d . . . H16 H 0.6123 0.4065 0.6778 0.095 Uiso 1 1 calc R . . C17 C 0.6624(6) 0.5465(4) 0.6777(3) 0.0736(13) Uani 1 1 d . . . H17 H 0.7575 0.5386 0.6908 0.088 Uiso 1 1 calc R . . C18 C 0.6084(5) 0.6368(3) 0.6658(2) 0.0620(11) Uani 1 1 d . . . H18 H 0.6674 0.6896 0.6719 0.074 Uiso 1 1 calc R . . Cu1' Cu 0.08871(4) 0.26375(3) 0.87690(2) 0.04880(12) Uani 1 1 d . . . O1' O 0.2073(3) 0.3168(2) 0.99250(16) 0.0636(7) Uani 1 1 d . . . O2' O -0.0524(3) 0.2437(2) 0.98892(17) 0.0699(8) Uani 1 1 d . . . N1' N 0.0005(4) 0.3895(2) 0.86041(17) 0.0527(8) Uani 1 1 d . . . N2' N 0.2695(3) 0.3385(3) 0.84876(19) 0.0590(8) Uani 1 1 d . . . H2N' H 0.3129 0.3023 0.8153 0.071 Uiso 1 1 calc R . . N3' N -0.0879(4) 0.1807(3) 0.8440(2) 0.0594(9) Uani 1 1 d . . . H3N' H -0.1393 0.2139 0.8091 0.071 Uiso 1 1 calc R . . N4' N 0.1722(3) 0.1324(2) 0.89240(18) 0.0517(7) Uani 1 1 d . . . C1' C -0.1344(5) 0.4119(4) 0.8759(3) 0.0682(12) Uani 1 1 d . . . H1' H -0.1878 0.3658 0.8985 0.082 Uiso 1 1 calc R . . C2' C -0.1951(6) 0.4999(4) 0.8595(3) 0.0780(14) Uani 1 1 d . . . H2' H -0.2879 0.5127 0.8698 0.094 Uiso 1 1 calc R . . C3' C -0.1142(7) 0.5675(4) 0.8277(3) 0.0786(15) Uani 1 1 d . . . H3' H -0.1526 0.6270 0.8155 0.094 Uiso 1 1 calc R . . C4' C 0.0209(7) 0.5486(3) 0.8138(2) 0.0755(15) Uani 1 1 d . . . H4' H 0.0761 0.5958 0.7938 0.091 Uiso 1 1 calc R . . C5' C 0.0778(5) 0.4577(3) 0.8298(2) 0.0575(10) Uani 1 1 d . . . C6' C 0.2203(5) 0.4287(4) 0.8113(2) 0.0687(12) Uani 1 1 d . . . H6'1 H 0.2855 0.4800 0.8246 0.082 Uiso 1 1 calc R . . H6'2 H 0.2214 0.4196 0.7589 0.082 Uiso 1 1 calc R . . C7' C 0.3733(5) 0.3559(4) 0.9106(3) 0.0691(12) Uani 1 1 d . . . H7'1 H 0.4407 0.4037 0.8965 0.083 Uiso 1 1 calc R . . H7'2 H 0.4242 0.2970 0.9220 0.083 Uiso 1 1 calc R . . C8' C 0.3035(5) 0.3895(4) 0.9765(3) 0.0686(12) Uani 1 1 d . . . H8'1 H 0.3720 0.3986 1.0170 0.082 Uiso 1 1 calc R . . H8'2 H 0.2549 0.4497 0.9668 0.082 Uiso 1 1 calc R . . C9' C 0.1229(5) 0.3352(4) 1.0523(2) 0.0735(13) Uani 1 1 d . . . H9'1 H 0.0690 0.3936 1.0443 0.088 Uiso 1 1 calc R . . H9'2 H 0.1809 0.3417 1.0971 0.088 Uiso 1 1 calc R . . C10' C 0.0280(6) 0.2513(4) 1.0563(2) 0.0735(13) Uani 1 1 d . . . H10C H 0.0828 0.1934 1.0651 0.088 Uiso 1 1 calc R . . H10D H -0.0339 0.2594 1.0961 0.088 Uiso 1 1 calc R . . C11' C -0.1164(5) 0.1520(4) 0.9762(3) 0.0783(14) Uani 1 1 d . . . H11C H -0.1861 0.1401 1.0117 0.094 Uiso 1 1 calc R . . H11D H -0.0458 0.1019 0.9806 0.094 Uiso 1 1 calc R . . C12' C -0.1831(5) 0.1525(4) 0.9022(3) 0.0759(13) Uani 1 1 d . . . H12C H -0.2622 0.1965 0.9011 0.091 Uiso 1 1 calc R . . H12D H -0.2199 0.0890 0.8913 0.091 Uiso 1 1 calc R . . C13' C -0.0251(5) 0.0971(3) 0.8090(3) 0.0663(11) Uani 1 1 d . . . H13C H 0.0047 0.1148 0.7611 0.080 Uiso 1 1 calc R . . H13D H -0.0942 0.0462 0.8031 0.080 Uiso 1 1 calc R . . C14' C 0.0992(5) 0.0628(3) 0.8558(2) 0.0566(10) Uani 1 1 d . . . C15' C 0.1416(5) -0.0315(3) 0.8634(2) 0.0683(13) Uani 1 1 d . . . H15' H 0.0930 -0.0796 0.8375 0.082 Uiso 1 1 calc R . . C16' C 0.2558(7) -0.0543(4) 0.9095(3) 0.0840(17) Uani 1 1 d . . . H16' H 0.2855 -0.1176 0.9148 0.101 Uiso 1 1 calc R . . C17' C 0.3235(6) 0.0164(4) 0.9465(3) 0.0751(14) Uani 1 1 d . . . H17' H 0.3990 0.0017 0.9789 0.090 Uiso 1 1 calc R . . C18' C 0.2827(5) 0.1093(3) 0.9371(2) 0.0603(10) Uani 1 1 d . . . H18' H 0.3325 0.1576 0.9621 0.072 Uiso 1 1 calc R . . 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 Cl1 0.0578(5) 0.0527(6) 0.0703(6) 0.0034(5) -0.0050(5) 0.0012(4) O1A 0.168(4) 0.082(3) 0.108(3) -0.023(3) -0.039(3) -0.012(3) O1B 0.170(4) 0.133(4) 0.102(3) 0.026(3) 0.002(3) -0.067(4) O1C 0.099(4) 0.384(15) 0.195(7) 0.017(8) 0.037(4) -0.025(6) O1D 0.372(11) 0.105(4) 0.172(5) -0.066(4) -0.150(6) 0.118(6) Cl2 0.0602(6) 0.0580(6) 0.0644(6) -0.0120(5) 0.0052(5) -0.0015(5) O2A 0.118(3) 0.059(2) 0.092(2) -0.007(2) -0.0202(19) -0.015(2) O2B 0.101(3) 0.098(3) 0.146(4) -0.041(3) 0.024(3) 0.023(3) O2C 0.154(5) 0.144(5) 0.166(5) -0.017(4) -0.093(4) 0.021(4) O2D 0.201(6) 0.129(5) 0.154(5) -0.029(4) 0.098(4) -0.075(4) Cl3 0.0573(5) 0.0558(6) 0.0731(6) -0.0085(5) -0.0081(5) -0.0024(5) O3A 0.189(6) 0.064(3) 0.218(7) -0.033(3) -0.039(5) -0.005(3) O3B 0.149(4) 0.162(6) 0.112(3) 0.035(3) -0.021(3) -0.025(4) O3C 0.136(5) 0.272(11) 0.194(6) -0.030(6) 0.027(4) 0.080(6) O3D 0.131(4) 0.173(6) 0.132(4) -0.015(4) -0.061(3) -0.023(4) Cl4 0.0465(5) 0.0639(7) 0.0903(7) 0.0143(5) 0.0007(5) -0.0008(4) O4A 0.0520(15) 0.083(2) 0.132(3) 0.007(2) -0.0176(17) 0.0119(19) O4B 0.090(3) 0.183(6) 0.130(3) 0.046(4) 0.037(3) 0.024(4) O4C 0.069(3) 0.112(4) 0.350(9) 0.118(5) 0.002(4) -0.003(3) O4D 0.087(3) 0.273(9) 0.155(4) -0.099(5) -0.034(3) 0.055(4) Cu1 0.0529(2) 0.0415(3) 0.0576(3) -0.0082(2) 0.00330(18) -0.0021(2) O1 0.0632(17) 0.0511(16) 0.0612(16) 0.0084(13) 0.0075(13) -0.0010(14) O2 0.098(2) 0.0529(18) 0.0593(16) -0.0111(13) 0.0002(15) 0.0188(17) N1 0.0479(18) 0.0485(19) 0.073(2) -0.0197(16) 0.0032(16) 0.0048(15) N2 0.085(3) 0.055(2) 0.0505(18) -0.0035(15) 0.0159(17) -0.0183(19) N3 0.0507(19) 0.054(2) 0.120(3) -0.026(2) -0.006(2) 0.0046(17) N4 0.062(2) 0.0417(18) 0.0588(19) 0.0009(15) 0.0061(16) -0.0014(15) C1 0.067(3) 0.056(3) 0.082(3) -0.010(2) -0.006(2) 0.010(2) C2 0.066(3) 0.062(3) 0.130(5) 0.006(3) -0.010(3) 0.018(2) C3 0.059(3) 0.055(3) 0.146(6) 0.008(3) 0.015(3) 0.004(2) C4 0.061(3) 0.048(3) 0.126(5) -0.021(3) 0.035(3) -0.003(2) C5 0.047(2) 0.046(2) 0.091(3) -0.016(2) 0.025(2) -0.0081(17) C6 0.079(3) 0.062(3) 0.080(3) -0.029(2) 0.032(2) -0.023(2) C7 0.089(3) 0.059(3) 0.061(3) -0.005(2) -0.017(2) -0.009(2) C8 0.047(2) 0.053(2) 0.081(3) 0.006(2) -0.004(2) -0.0071(19) C9 0.073(3) 0.062(3) 0.076(3) 0.015(2) 0.024(2) 0.004(2) C10 0.092(3) 0.070(3) 0.069(3) 0.010(3) 0.030(2) 0.028(3) C11 0.130(5) 0.061(3) 0.059(3) -0.011(2) -0.006(3) 0.023(3) C12 0.109(4) 0.063(3) 0.097(4) -0.025(3) -0.042(3) 0.007(3) C13 0.061(3) 0.058(3) 0.133(5) -0.022(3) 0.017(3) -0.012(2) C14 0.071(3) 0.041(2) 0.071(3) -0.0073(19) 0.022(2) -0.0032(19) C15 0.096(4) 0.047(2) 0.070(3) 0.000(2) 0.024(3) -0.008(2) C16 0.115(4) 0.062(3) 0.061(3) 0.009(2) 0.002(3) 0.017(3) C17 0.093(4) 0.062(3) 0.063(3) 0.011(2) -0.019(2) 0.008(3) C18 0.073(3) 0.058(3) 0.053(2) 0.0091(19) -0.012(2) -0.005(2) Cu1' 0.0439(2) 0.0406(3) 0.0618(3) 0.0035(2) 0.00170(17) 0.0004(2) O1' 0.0667(17) 0.0627(19) 0.0614(17) -0.0090(13) 0.0041(13) 0.0056(14) O2' 0.078(2) 0.0567(19) 0.0762(19) 0.0130(15) 0.0138(16) -0.0011(15) N1' 0.0590(19) 0.0439(18) 0.0544(18) 0.0062(14) -0.0037(15) 0.0015(15) N2' 0.0526(18) 0.059(2) 0.066(2) -0.0145(17) 0.0127(15) -0.0097(17) N3' 0.0512(18) 0.052(2) 0.074(2) 0.0105(17) -0.0059(16) -0.0071(16) N4' 0.0526(18) 0.0437(18) 0.0591(19) 0.0017(15) 0.0061(14) -0.0020(15) C1' 0.061(3) 0.063(3) 0.080(3) 0.011(2) -0.005(2) 0.015(2) C2' 0.090(4) 0.060(3) 0.082(3) -0.006(3) -0.020(3) 0.021(3) C3' 0.114(4) 0.050(3) 0.069(3) -0.005(2) -0.022(3) 0.021(3) C4' 0.128(5) 0.045(2) 0.052(2) 0.0023(18) -0.014(3) -0.016(3) C5' 0.082(3) 0.048(2) 0.042(2) 0.0002(16) -0.0042(19) -0.010(2) C6' 0.078(3) 0.071(3) 0.057(2) 0.001(2) 0.000(2) -0.028(2) C7' 0.053(2) 0.069(3) 0.084(3) -0.009(2) -0.004(2) -0.003(2) C8' 0.068(3) 0.065(3) 0.072(3) -0.015(2) -0.012(2) -0.007(2) C9' 0.092(3) 0.074(3) 0.055(2) -0.005(2) 0.003(2) 0.020(3) C10' 0.099(3) 0.071(3) 0.051(2) 0.008(2) 0.011(2) 0.012(3) C11' 0.075(3) 0.062(3) 0.100(4) 0.023(3) 0.029(3) 0.000(2) C12' 0.054(3) 0.077(3) 0.098(4) 0.004(3) 0.015(2) -0.013(2) C13' 0.076(3) 0.053(3) 0.069(3) 0.000(2) -0.004(2) -0.014(2) C14' 0.071(3) 0.048(2) 0.053(2) 0.0020(18) 0.023(2) 0.002(2) C15' 0.098(4) 0.046(2) 0.064(3) 0.0006(19) 0.032(3) 0.003(2) C16' 0.111(4) 0.053(3) 0.092(4) 0.013(3) 0.039(3) 0.028(3) C17' 0.077(3) 0.070(3) 0.079(3) 0.016(3) 0.011(3) 0.026(3) C18' 0.053(2) 0.059(3) 0.069(3) 0.003(2) 0.007(2) 0.015(2) _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 Cl1 O1C 1.315(6) . ? Cl1 O1D 1.386(5) . ? Cl1 O1B 1.402(4) . ? Cl1 O1A 1.427(4) . ? Cl2 O2B 1.387(4) . ? Cl2 O2D 1.401(5) . ? Cl2 O2C 1.415(5) . ? Cl2 O2A 1.443(4) . ? Cl3 O3A 1.367(5) . ? Cl3 O3D 1.373(4) . ? Cl3 O3C 1.383(6) . ? Cl3 O3B 1.444(5) . ? Cl4 O4C 1.382(5) . ? Cl4 O4D 1.388(5) . ? Cl4 O4B 1.394(4) . ? Cl4 O4A 1.436(3) . ? Cu1 N1 1.987(4) . ? Cu1 N4 2.013(4) . ? Cu1 N2 2.098(3) . ? Cu1 N3 2.115(4) . ? O1 C9 1.414(5) . ? O1 C8 1.420(5) . ? O2 C11 1.420(6) . ? O2 C10 1.440(6) . ? N1 C1 1.336(6) . ? N1 C5 1.345(5) . ? N2 C6 1.469(6) . ? N2 C7 1.490(6) . ? N2 H2 0.9100 . ? N3 C13 1.499(7) . ? N3 C12 1.503(7) . ? N3 H3 0.9100 . ? N4 C18 1.343(6) . ? N4 C14 1.353(6) . ? C1 C2 1.370(7) . ? C1 H1 0.9300 . ? C2 C3 1.376(9) . ? C2 H2 0.9300 . ? C3 C4 1.389(8) . ? C3 H3 0.9300 . ? C4 C5 1.389(7) . ? C4 H4 0.9300 . ? C5 C6 1.502(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.495(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.475(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.488(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.481(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.385(7) . ? C15 C16 1.396(8) . ? C15 H15 0.9300 . ? C16 C17 1.368(7) . ? C16 H16 0.9300 . ? C17 C18 1.373(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? Cu1' N1' 1.960(3) . ? Cu1' N4' 2.010(3) . ? Cu1' N2' 2.100(3) . ? Cu1' N3' 2.102(3) . ? O1' C8' 1.407(6) . ? O1' C9' 1.418(5) . ? O2' C10' 1.422(6) . ? O2' C11' 1.429(6) . ? N1' C5' 1.344(5) . ? N1' C1' 1.366(6) . ? N2' C7' 1.483(6) . ? N2' C6' 1.497(6) . ? N2' H2' 0.9100 . ? N3' C13' 1.473(6) . ? N3' C12' 1.492(6) . ? N3' H3' 0.9100 . ? N4' C18' 1.337(5) . ? N4' C14' 1.351(6) . ? C1' C2' 1.383(7) . ? C1' H1' 0.9300 . ? C2' C3' 1.368(8) . ? C2' H2' 0.9300 . ? C3' C4' 1.350(8) . ? C3' H3' 0.9300 . ? C4' C5' 1.404(7) . ? C4' H4' 0.9300 . ? C5' C6' 1.472(7) . ? C6' H6'1 0.9700 . ? C6' H6'2 0.9700 . ? C7' C8' 1.487(6) . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C9' C10' 1.482(7) . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11' C12' 1.466(8) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? C13' C14' 1.502(7) . ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' C15' 1.380(6) . ? C15' C16' 1.377(8) . ? C15' H15' 0.9300 . ? C16' C17' 1.342(8) . ? C16' H16' 0.9300 . ? C17' C18' 1.362(6) . ? C17' H17' 0.9300 . ? C18' H18' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1C Cl1 O1D 105.4(7) . . ? O1C Cl1 O1B 108.2(4) . . ? O1D Cl1 O1B 109.8(4) . . ? O1C Cl1 O1A 108.2(5) . . ? O1D Cl1 O1A 110.0(3) . . ? O1B Cl1 O1A 114.8(3) . . ? O2B Cl2 O2D 109.7(4) . . ? O2B Cl2 O2C 110.9(4) . . ? O2D Cl2 O2C 109.9(4) . . ? O2B Cl2 O2A 110.5(3) . . ? O2D Cl2 O2A 108.8(3) . . ? O2C Cl2 O2A 107.1(3) . . ? O3A Cl3 O3D 112.2(4) . . ? O3A Cl3 O3C 111.8(5) . . ? O3D Cl3 O3C 113.5(4) . . ? O3A Cl3 O3B 104.6(4) . . ? O3D Cl3 O3B 107.5(4) . . ? O3C Cl3 O3B 106.6(5) . . ? O4C Cl4 O4D 107.9(5) . . ? O4C Cl4 O4B 108.1(4) . . ? O4D Cl4 O4B 109.9(4) . . ? O4C Cl4 O4A 110.2(3) . . ? O4D Cl4 O4A 109.4(3) . . ? O4B Cl4 O4A 111.3(3) . . ? N1 Cu1 N4 177.60(14) . . ? N1 Cu1 N2 82.53(15) . . ? N4 Cu1 N2 99.66(15) . . ? N1 Cu1 N3 96.75(16) . . ? N4 Cu1 N3 80.90(15) . . ? N2 Cu1 N3 145.73(16) . . ? C9 O1 C8 116.2(3) . . ? C11 O2 C10 115.5(4) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Cu1 126.0(3) . . ? C5 N1 Cu1 115.8(3) . . ? C6 N2 C7 112.4(4) . . ? C6 N2 Cu1 107.2(3) . . ? C7 N2 Cu1 114.7(3) . . ? C6 N2 H2 107.4 . . ? C7 N2 H2 107.4 . . ? Cu1 N2 H2 107.4 . . ? C13 N3 C12 115.2(4) . . ? C13 N3 Cu1 103.2(3) . . ? C12 N3 Cu1 114.3(3) . . ? C13 N3 H3 107.9 . . ? C12 N3 H3 107.9 . . ? Cu1 N3 H3 107.9 . . ? C18 N4 C14 120.0(4) . . ? C18 N4 Cu1 125.9(3) . . ? C14 N4 Cu1 113.8(3) . . ? N1 C1 C2 123.5(5) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.8(6) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 118.7(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 121.7(5) . . ? N1 C5 C6 115.6(4) . . ? C4 C5 C6 122.6(4) . . ? N2 C6 C5 112.7(3) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 110.9(3) . . ? N2 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? O1 C8 C7 104.8(4) . . ? O1 C8 H8A 110.8 . . ? C7 C8 H8A 110.8 . . ? O1 C8 H8B 110.8 . . ? C7 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? O1 C9 C10 106.1(4) . . ? O1 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O1 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O2 C10 C9 107.4(3) . . ? O2 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O2 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O2 C11 C12 106.3(4) . . ? O2 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? O2 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? C11 C12 N3 112.6(4) . . ? C11 C12 H12A 109.1 . . ? N3 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? N3 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C14 C13 N3 109.4(4) . . ? C14 C13 H13A 109.8 . . ? N3 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? N3 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? N4 C14 C15 120.2(5) . . ? N4 C14 C13 115.8(4) . . ? C15 C14 C13 123.9(5) . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 118.5(5) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? N4 C18 C17 121.4(5) . . ? N4 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? N1' Cu1' N4' 177.80(14) . . ? N1' Cu1' N2' 82.42(15) . . ? N4' Cu1' N2' 99.43(14) . . ? N1' Cu1' N3' 96.84(15) . . ? N4' Cu1' N3' 80.96(14) . . ? N2' Cu1' N3' 148.81(14) . . ? C8' O1' C9' 115.7(4) . . ? C10' O2' C11' 114.4(4) . . ? C5' N1' C1' 117.8(4) . . ? C5' N1' Cu1' 117.3(3) . . ? C1' N1' Cu1' 124.9(3) . . ? C7' N2' C6' 113.1(4) . . ? C7' N2' Cu1' 114.4(3) . . ? C6' N2' Cu1' 106.9(3) . . ? C7' N2' H2' 107.4 . . ? C6' N2' H2' 107.4 . . ? Cu1' N2' H2' 107.4 . . ? C13' N3' C12' 112.4(4) . . ? C13' N3' Cu1' 102.9(3) . . ? C12' N3' Cu1' 116.5(3) . . ? C13' N3' H3' 108.2 . . ? C12' N3' H3' 108.2 . . ? Cu1' N3' H3' 108.2 . . ? C18' N4' C14' 119.8(4) . . ? C18' N4' Cu1' 126.7(3) . . ? C14' N4' Cu1' 113.3(3) . . ? N1' C1' C2' 123.0(5) . . ? N1' C1' H1' 118.5 . . ? C2' C1' H1' 118.5 . . ? C3' C2' C1' 117.7(5) . . ? C3' C2' H2' 121.1 . . ? C1' C2' H2' 121.1 . . ? C4' C3' C2' 120.7(5) . . ? C4' C3' H3' 119.6 . . ? C2' C3' H3' 119.6 . . ? C3' C4' C5' 119.8(5) . . ? C3' C4' H4' 120.1 . . ? C5' C4' H4' 120.1 . . ? N1' C5' C4' 120.9(5) . . ? N1' C5' C6' 115.7(4) . . ? C4' C5' C6' 123.3(4) . . ? C5' C6' N2' 113.2(3) . . ? C5' C6' H6'1 108.9 . . ? N2' C6' H6'1 108.9 . . ? C5' C6' H6'2 108.9 . . ? N2' C6' H6'2 108.9 . . ? H6'1 C6' H6'2 107.8 . . ? N2' C7' C8' 111.4(4) . . ? N2' C7' H7'1 109.3 . . ? C8' C7' H7'1 109.3 . . ? N2' C7' H7'2 109.3 . . ? C8' C7' H7'2 109.3 . . ? H7'1 C7' H7'2 108.0 . . ? O1' C8' C7' 105.5(4) . . ? O1' C8' H8'1 110.6 . . ? C7' C8' H8'1 110.6 . . ? O1' C8' H8'2 110.6 . . ? C7' C8' H8'2 110.6 . . ? H8'1 C8' H8'2 108.8 . . ? O1' C9' C10' 105.5(4) . . ? O1' C9' H9'1 110.6 . . ? C10' C9' H9'1 110.6 . . ? O1' C9' H9'2 110.6 . . ? C10' C9' H9'2 110.6 . . ? H9'1 C9' H9'2 108.8 . . ? O2' C10' C9' 108.5(4) . . ? O2' C10' H10C 110.0 . . ? C9' C10' H10C 110.0 . . ? O2' C10' H10D 110.0 . . ? C9' C10' H10D 110.0 . . ? H10C C10' H10D 108.4 . . ? O2' C11' C12' 107.9(4) . . ? O2' C11' H11C 110.1 . . ? C12' C11' H11C 110.1 . . ? O2' C11' H11D 110.1 . . ? C12' C11' H11D 110.1 . . ? H11C C11' H11D 108.4 . . ? C11' C12' N3' 114.5(4) . . ? C11' C12' H12C 108.6 . . ? N3' C12' H12C 108.6 . . ? C11' C12' H12D 108.6 . . ? N3' C12' H12D 108.6 . . ? H12C C12' H12D 107.6 . . ? N3' C13' C14' 109.2(4) . . ? N3' C13' H13C 109.8 . . ? C14' C13' H13C 109.8 . . ? N3' C13' H13D 109.8 . . ? C14' C13' H13D 109.8 . . ? H13C C13' H13D 108.3 . . ? N4' C14' C15' 119.7(5) . . ? N4' C14' C13' 115.0(4) . . ? C15' C14' C13' 125.3(4) . . ? C16' C15' C14' 119.9(5) . . ? C16' C15' H15' 120.0 . . ? C14' C15' H15' 120.0 . . ? C17' C16' C15' 118.9(5) . . ? C17' C16' H16' 120.6 . . ? C15' C16' H16' 120.6 . . ? C16' C17' C18' 120.6(5) . . ? C16' C17' H17' 119.7 . . ? C18' C17' H17' 119.7 . . ? N4' C18' C17' 121.1(5) . . ? N4' C18' H18' 119.4 . . ? C17' C18' H18' 119.4 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 29.76 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.547 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.052 #===========================END data_complex_4_[Znpydadt](ClO4)2 (4) _database_code_CSD 155152 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H26 Cl2 N4 O8 S2 Zn' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H26 Cl2 N4 O8 S2 Zn' _chemical_formula_weight 626.83 _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 S ? 0.110 0.124 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 13.5168(9) _cell_length_b 9.8812(3) _cell_length_c 19.824(1) _cell_angle_alpha 90 _cell_angle_beta 109.594(5) _cell_angle_gamma 90 _cell_volume 2494.5(5) _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 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.67 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.418 _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 ; 10397 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 20 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 == -4.10 Kappa == 114.00 Phi == 0.00 18 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 10397 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.44 _reflns_number_total 5945 _reflns_number_gt 2346 _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 2346 _refine_ls_number_parameters 334 _refine_ls_number_restraints 8 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.122 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_all 0.246 _refine_ls_wR_factor_ref 0.064 _refine_ls_goodness_of_fit_all 6.763 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.300 _refine_diff_density_min -0.399 #=========================================================================== # 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 ZN 0.77577(5) 0.00250(6) 0.05338(3) 0.0343(3) 1.000 Uani ? ? Zn N1 0.9252(3) 0.0325(4) 0.1315(2) 0.035(2) 1.000 Uani ? ? N C1 0.9866(4) -0.0638(6) 0.1741(3) 0.043(3) 1.000 Uani ? ? C C2 1.0783(5) -0.0351(7) 0.2274(3) 0.047(4) 1.000 Uani ? ? C C3 1.1084(5) 0.0976(7) 0.2387(3) 0.050(4) 1.000 Uani ? ? C C4 1.0484(4) 0.1966(6) 0.1967(3) 0.051(3) 1.000 Uani ? ? C C5 0.9570(4) 0.1615(6) 0.1427(3) 0.042(3) 1.000 Uani ? ? C C6 0.8891(5) 0.2644(6) 0.0918(3) 0.052(4) 1.000 Uani ? ? C N2 0.7787(3) 0.2195(4) 0.0611(2) 0.041(3) 1.000 Uani ? ? N C7 0.7239(5) 0.2892(6) -0.0067(4) 0.052(4) 1.000 Uani ? ? C C8 0.6133(5) 0.2385(6) -0.0396(4) 0.061(4) 1.000 Uani ? ? C S1 0.5985(1) 0.0566(2) -0.04888(8) 0.0436(8) 1.000 Uani ? ? S C9 0.6248(5) 0.0210(6) -0.1304(3) 0.052(4) 1.000 Uani ? ? C C10 0.7369(5) 0.0396(6) -0.1302(3) 0.052(4) 1.000 Uani ? ? C S2 0.8444(1) -0.0164(1) -0.05470(8) 0.0442(8) 1.000 Uani ? ? S C11 0.8348(5) -0.1992(6) -0.0595(4) 0.058(4) 1.000 Uani ? ? C C12 0.7528(5) -0.2610(6) -0.0328(3) 0.049(3) 1.000 Uani ? ? C N3 0.7658(3) -0.2143(4) 0.0402(2) 0.035(2) 1.000 Uani ? ? N C13 0.6784(5) -0.2612(5) 0.0634(3) 0.048(3) 1.000 Uani ? ? C C14 0.6749(4) -0.1838(5) 0.1276(3) 0.036(3) 1.000 Uani ? ? C N4 0.7092(3) -0.0555(4) 0.1331(2) 0.038(2) 1.000 Uani ? ? N C15 0.7054(5) 0.0172(6) 0.1885(3) 0.050(4) 1.000 Uani ? ? C C16 0.6691(5) -0.0335(7) 0.2405(3) 0.062(4) 1.000 Uani ? ? C C17 0.6347(5) -0.1628(7) 0.2349(3) 0.061(4) 1.000 Uani ? ? C C18 0.6383(4) -0.2415(6) 0.1786(3) 0.048(3) 1.000 Uani ? ? C CL1 1.0562(1) -0.3963(1) 0.11899(9) 0.0544(9) 1.000 Uani ? ? Cl O1 1.0921(4) -0.5210(5) 0.1045(4) 0.106(4) 1.000 Uani ? ? O O2 1.0745(4) -0.2924(5) 0.0765(3) 0.127(4) 1.000 Uani ? ? O O3 0.9456(3) -0.3993(4) 0.1054(3) 0.074(3) 1.000 Uani ? ? O O4 1.1062(5) -0.3581(7) 0.1916(3) 0.114(5) 1.000 Uani ? ? O CL2 0.5681(1) 0.3657(2) 0.1452(1) 0.071(1) 1.000 Uani ? ? Cl O5 0.6709(4) 0.3914(5) 0.1480(3) 0.105(4) 1.000 Uani ? ? O O6 0.549(1) 0.431(2) 0.2001(5) 0.17(1) 0.500 Uani ? ? O O7 0.5316(5) 0.2461(5) 0.1101(4) 0.105(4) 1.000 Uani ? ? O O8 0.512(1) 0.460(1) 0.0793(7) 0.110(9) 0.500 Uani ? ? O O9 0.589(1) 0.295(1) 0.2189(6) 0.125(8) 0.500 Uani ? ? O O10 0.5002(8) 0.459(1) 0.1441(7) 0.106(7) 0.500 Uani ? ? O H01 0.7155 0.2482 0.0832 0.0533 1.000 Uiso ? ? H H02 0.8425 -0.2487 0.0780 0.0455 1.000 Uiso ? ? H H1 0.9646 -0.1555 0.1665 0.0576 1.000 Uiso calc C1 H H2 1.1202 -0.1050 0.2558 0.0669 1.000 Uiso calc C2 H H3 1.1714 0.1207 0.2760 0.0728 1.000 Uiso calc C3 H H4 1.0693 0.2887 0.2045 0.0650 1.000 Uiso calc C4 H H5 0.9161 0.2788 0.0538 0.0674 1.000 Uiso calc C6 H H6 0.8913 0.3468 0.1169 0.0674 1.000 Uiso calc C6 H H7 0.7609 0.2739 -0.0391 0.0717 1.000 Uiso calc C7 H H8 0.7222 0.3835 0.0022 0.0717 1.000 Uiso calc C7 H H9 0.5848 0.2772 -0.0860 0.0810 1.000 Uiso calc C8 H H10 0.5743 0.2685 -0.0106 0.0810 1.000 Uiso calc C8 H H11 0.5811 0.0787 -0.1665 0.0684 1.000 Uiso calc C9 H H12 0.6060 -0.0706 -0.1426 0.0684 1.000 Uiso calc C9 H H13 0.7466 0.1338 -0.1353 0.0685 1.000 Uiso calc C10 H H14 0.7418 -0.0071 -0.1708 0.0685 1.000 Uiso calc C10 H H15 0.9012 -0.2353 -0.0318 0.0735 1.000 Uiso calc C11 H H16 0.8191 -0.2248 -0.1081 0.0735 1.000 Uiso calc C11 H H17 0.7594 -0.3568 -0.0325 0.0633 1.000 Uiso calc C12 H H18 0.6851 -0.2358 -0.0639 0.0633 1.000 Uiso calc C12 H H19 0.6877 -0.3546 0.0751 0.0626 1.000 Uiso calc C13 H H20 0.6140 -0.2485 0.0253 0.0626 1.000 Uiso calc C13 H H21 0.7287 0.1084 0.1923 0.0652 1.000 Uiso calc C15 H H22 0.6682 0.0215 0.2796 0.0795 1.000 Uiso calc C16 H H23 0.6081 -0.1992 0.2698 0.0760 1.000 Uiso calc C17 H H24 0.6163 -0.3333 0.1746 0.0623 1.000 Uiso calc C18 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 0.0328(3) 0.0304(3) 0.0407(3) -0.0035(3) 0.0133(2) -0.0008(3) Zn N1 0.031(2) 0.041(3) 0.033(2) -0.008(2) 0.012(2) -0.004(2) N C1 0.043(3) 0.048(3) 0.040(3) 0.000(3) 0.010(3) -0.000(3) C C2 0.038(3) 0.071(4) 0.040(3) 0.001(3) 0.005(3) 0.002(3) C C3 0.033(3) 0.092(5) 0.040(4) -0.012(3) 0.008(3) -0.011(3) C C4 0.043(3) 0.056(3) 0.055(4) -0.022(3) 0.021(3) -0.019(3) C C5 0.039(3) 0.045(3) 0.043(3) -0.009(3) 0.020(2) -0.008(3) C C6 0.054(4) 0.043(3) 0.061(4) -0.014(3) 0.022(3) 0.000(3) C N2 0.037(2) 0.033(2) 0.056(3) -0.002(2) 0.021(2) 0.001(2) N C7 0.059(4) 0.034(3) 0.069(4) 0.008(3) 0.018(3) 0.011(3) C C8 0.053(4) 0.053(4) 0.081(5) 0.015(3) 0.021(3) 0.008(4) C S1 0.0326(8) 0.0529(8) 0.0481(9) 0.0034(7) 0.0152(6) 0.0062(8) S C9 0.047(3) 0.067(4) 0.045(3) 0.003(3) 0.016(3) 0.007(3) C C10 0.050(4) 0.066(4) 0.043(3) 0.008(3) 0.017(3) 0.011(3) C S2 0.0366(8) 0.0507(9) 0.0466(8) 0.0016(7) 0.0200(6) 0.0030(7) S C11 0.065(4) 0.044(3) 0.067(4) 0.010(3) 0.030(3) -0.005(3) C C12 0.063(4) 0.036(3) 0.052(4) -0.004(3) 0.025(3) -0.004(3) C N3 0.032(2) 0.037(2) 0.036(3) -0.003(2) 0.011(2) -0.003(2) N C13 0.051(3) 0.039(3) 0.056(4) -0.015(3) 0.020(3) -0.002(3) C C14 0.028(3) 0.040(3) 0.043(3) 0.004(2) 0.011(2) 0.009(3) C N4 0.035(3) 0.038(2) 0.039(3) -0.000(2) 0.009(2) 0.002(2) N C15 0.048(4) 0.052(4) 0.050(3) -0.001(3) 0.015(3) -0.007(3) C C16 0.065(4) 0.081(5) 0.046(3) 0.011(3) 0.030(3) -0.002(3) C C17 0.052(4) 0.076(4) 0.057(4) 0.010(3) 0.031(3) 0.020(3) C C18 0.037(3) 0.055(4) 0.056(4) 0.003(3) 0.020(2) 0.020(3) C CL1 0.0523(9) 0.0442(8) 0.070(1) 0.0019(7) 0.0254(7) 0.0038(8) Cl O1 0.089(4) 0.064(3) 0.209(6) 0.020(3) 0.049(4) -0.035(3) O O2 0.148(4) 0.094(4) 0.146(4) -0.022(3) 0.098(3) 0.022(3) O O3 0.050(3) 0.064(3) 0.125(4) 0.005(2) 0.028(2) 0.009(3) O O4 0.111(5) 0.172(5) 0.078(4) 0.053(4) -0.013(4) -0.026(4) O CL2 0.055(1) 0.066(1) 0.098(1) -0.0143(9) 0.0310(8) -0.0284(9) Cl O5 0.062(3) 0.104(4) 0.180(5) -0.028(3) 0.063(3) -0.049(3) O O6 0.189(9) 0.31(2) 0.090(6) -0.07(1) 0.113(5) -0.078(9) O O7 0.110(5) 0.065(3) 0.161(6) -0.029(3) -0.006(4) -0.010(4) O O8 0.13(1) 0.084(7) 0.12(1) 0.005(8) -0.022(9) 0.037(7) O O9 0.165(9) 0.109(8) 0.110(8) 0.047(7) 0.069(6) 0.003(7) O O10 0.095(6) 0.061(6) 0.207(9) 0.020(5) 0.094(5) 0.007(7) 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 2.114(5) . . ? ZN N2 2.149(5) . . ? ZN S1 2.623(2) . . ? ZN S2 2.611(2) . . ? ZN N3 2.157(5) . . ? ZN N4 2.142(5) . . ? ZN H01 2.6889 . . ? ZN H02 2.6303 . . ? N1 C1 1.355(8) . . ? N1 C5 1.340(7) . . ? C1 C2 1.362(9) . . ? C2 C3 1.37(1) . . ? C3 C4 1.36(1) . . ? C4 C5 1.380(9) . . ? C5 C6 1.508(9) . . ? C6 N2 1.478(9) . . ? N2 C7 1.471(9) . . ? N2 H01 1.1190 . . ? C7 C8 1.50(1) . . ? C7 H01 1.8680 . . ? C8 S1 1.810(7) . . ? S1 C9 1.803(7) . . ? C9 C10 1.52(1) . . ? C10 S2 1.788(7) . . ? S2 C11 1.811(7) . . ? C11 C12 1.508(9) . . ? C12 N3 1.472(8) . . ? N3 C13 1.478(8) . . ? N3 H02 1.1103 . . ? C13 C14 1.499(9) . . ? C14 N4 1.342(8) . . ? C14 C18 1.389(9) . . ? N4 C15 1.327(8) . . ? C15 C16 1.38(1) . . ? C16 C17 1.35(1) . . ? C17 C18 1.38(1) . . ? CL1 O1 1.389(5) . . ? CL1 O2 1.400(6) . . ? CL1 O3 1.428(5) . . ? CL1 O4 1.421(7) . . ? O3 H02 1.9855 . . ? CL2 O5 1.395(6) . . ? CL2 O6 1.36(2) . . ? CL2 O7 1.377(6) . . ? CL2 O8 1.58(2) . . ? CL2 O9 1.56(2) . . ? CL2 O10 1.29(1) . . ? O6 O9 1.45(3) . . ? O6 O10 1.12(3) . . ? O8 O10 1.34(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 N1 ZN N2 79.5(2) . . . ? N1 ZN S1 159.8(1) . . . ? N1 ZN S2 95.5(1) . . . ? N1 ZN N3 103.5(2) . . . ? N1 ZN N4 91.8(2) . . . ? N1 ZN H01 89.87 . . . ? N1 ZN H02 79.18 . . . ? N2 ZN S1 80.9(2) . . . ? N2 ZN S2 97.3(1) . . . ? N2 ZN N3 176.9(2) . . . ? N2 ZN N4 102.5(2) . . . ? N2 ZN H01 23.53 . . . ? N2 ZN H02 158.65 . . . ? S1 ZN S2 82.19(6) . . . ? S1 ZN N3 96.0(1) . . . ? S1 ZN N4 97.1(1) . . . ? S1 ZN H01 73.75 . . . ? S1 ZN H02 120.24 . . . ? S2 ZN N3 81.6(1) . . . ? S2 ZN N4 159.9(1) . . . ? S2 ZN H01 117.52 . . . ? S2 ZN H02 83.73 . . . ? N3 ZN N4 78.4(2) . . . ? N3 ZN H01 155.81 . . . ? N3 ZN H02 24.34 . . . ? N4 ZN H01 81.15 . . . ? N4 ZN H02 79.24 . . . ? H01 ZN H02 157.16 . . . ? C1 N1 C5 118.0(6) . . . ? N1 C1 C2 123.0(6) . . . ? C1 C2 C3 118.0(7) . . . ? C2 C3 C4 120.4(7) . . . ? C3 C4 C5 119.2(6) . . . ? N1 C5 C4 121.5(6) . . . ? N1 C5 C6 116.1(6) . . . ? C4 C5 C6 122.4(6) . . . ? C5 C6 N2 112.2(5) . . . ? C6 N2 C7 111.4(5) . . . ? C6 N2 H01 124.12 . . . ? C7 N2 H01 91.30 . . . ? N2 C7 C8 111.3(6) . . . ? N2 C7 H01 36.79 . . . ? C8 C7 H01 88.39 . . . ? C7 C8 S1 115.8(5) . . . ? C8 S1 C9 103.7(3) . . . ? S1 C9 C10 117.9(5) . . . ? C9 C10 S2 119.5(5) . . . ? C10 S2 C11 104.0(4) . . . ? S2 C11 C12 115.7(5) . . . ? C11 C12 N3 111.0(6) . . . ? C12 N3 C13 111.3(5) . . . ? C12 N3 H02 110.14 . . . ? C13 N3 H02 110.91 . . . ? N3 C13 C14 111.1(5) . . . ? C13 C14 N4 116.3(6) . . . ? C13 C14 C18 122.0(6) . . . ? N4 C14 C18 121.8(6) . . . ? C14 N4 C15 118.1(6) . . . ? N4 C15 C16 123.1(7) . . . ? C15 C16 C17 118.8(7) . . . ? C16 C17 C18 119.7(7) . . . ? C14 C18 C17 118.6(7) . . . ? O1 CL1 O2 112.5(5) . . . ? O1 CL1 O3 111.0(4) . . . ? O1 CL1 O4 111.4(5) . . . ? O2 CL1 O3 106.7(4) . . . ? O2 CL1 O4 107.2(5) . . . ? O3 CL1 O4 108.0(4) . . . ? CL1 O3 H02 129.05 . . . ? O5 CL2 O6 109(1) . . . ? O5 CL2 O7 111.1(4) . . . ? O5 CL2 O8 97.0(8) . . . ? O5 CL2 O9 100.3(8) . . . ? O5 CL2 O10 124.2(8) . . . ? O6 CL2 O7 132(1) . . . ? O6 CL2 O8 102(1) . . . ? O6 CL2 O9 59(1) . . . ? O6 CL2 O10 49(1) . . . ? O7 CL2 O8 95.6(7) . . . ? O7 CL2 O9 90.6(7) . . . ? O7 CL2 O10 118(1) . . . ? O8 CL2 O9 158(1) . . . ? O8 CL2 O10 54(1) . . . ? O9 CL2 O10 103(1) . . . ? CL2 O6 O9 67(1) . . . ? CL2 O6 O10 61(1) . . . ? O9 O6 O10 121(2) . . . ? CL2 O8 O10 51.8(8) . . . ? CL2 O9 O6 53.7(9) . . . ? CL2 O10 O6 68(1) . . . ? CL2 O10 O8 73(1) . . . ? O6 O10 O8 136(2) . . . ? N2 H01 C7 51.91 . . . ? N3 H02 O3 145.60 . . . ? #============================================================END data_complex_3_[Znpydado](ClO4)2 H2O (3) _database_code_CSD 155153 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H28 Cl2 N4 O11 Zn' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H28 Cl2 N4 O11 Zn' _chemical_formula_weight 612.72 _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 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 9.3266(5) _cell_length_b 11.6770(5) _cell_length_c 12.2295(5) _cell_angle_alpha 94.039(5) _cell_angle_beta 99.520(5) _cell_angle_gamma 107.008(5) _cell_volume 1246.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _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 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.63 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=========================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _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 ; 8342 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 30 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta == 6.40 Omega == 0.00 Kappa == 0.00 91 frames Set 2 Theta == -6.40 Kappa == -174.00 Phi == 0.00 22 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 8342 _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 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5674 _reflns_number_gt 3514 _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 3514 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_all 0.824 _refine_ls_wR_factor_ref 0.080 _refine_ls_goodness_of_fit_all 14.957 _refine_ls_goodness_of_fit_ref 1.332 _refine_ls_shift/su_max 0.005 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.363 _refine_diff_density_min -0.249 #=========================================================================== # 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 0.46262(6) 0.26770(4) 0.25331(4) 0.0264(2) Uani ? ? Zn N1 0.6166(4) 0.2876(3) 0.1398(3) 0.031(2) Uani ? ? N C1 0.5852(5) 0.2406(4) 0.0301(4) 0.033(2) Uani ? ? C C2 0.6889(6) 0.2687(4) -0.0373(4) 0.038(2) Uani ? ? C C3 0.8339(6) 0.3454(4) 0.0072(4) 0.044(2) Uani ? ? C C4 0.8684(6) 0.3953(4) 0.1178(4) 0.038(2) Uani ? ? C C5 0.7555(5) 0.3638(4) 0.1804(4) 0.029(2) Uani ? ? C C6 0.7855(6) 0.4168(5) 0.3021(4) 0.036(3) Uani ? ? C N2 0.6410(4) 0.4203(3) 0.3372(3) 0.032(2) Uani ? ? N C7 0.5993(6) 0.5293(4) 0.3138(4) 0.042(3) Uani ? ? C C8 0.5089(6) 0.5173(4) 0.1989(4) 0.039(2) Uani ? ? C O1 0.3791(4) 0.4103(3) 0.1865(3) 0.034(2) Uani ? ? O C9 0.2840(6) 0.3751(5) 0.0796(4) 0.044(3) Uani ? ? C C10 0.1766(6) 0.2504(5) 0.0820(4) 0.044(3) Uani ? ? C O2 0.2733(4) 0.1774(3) 0.1144(3) 0.035(2) Uani ? ? O C11 0.1960(6) 0.0605(4) 0.1408(4) 0.040(3) Uani ? ? C C12 0.3197(7) 0.0086(4) 0.1864(4) 0.046(3) Uani ? ? C N3 0.4349(4) 0.0883(3) 0.2824(3) 0.037(2) Uani ? ? N C13 0.3896(6) 0.0733(4) 0.3919(4) 0.039(2) Uani ? ? C C14 0.2916(6) 0.1489(4) 0.4163(4) 0.030(2) Uani ? ? C N4 0.3099(4) 0.2491(3) 0.3683(3) 0.029(2) Uani ? ? N C15 0.2244(5) 0.3218(4) 0.3882(4) 0.036(2) Uani ? ? C C16 0.1219(6) 0.2962(4) 0.4577(4) 0.040(3) Uani ? ? C C17 0.1054(6) 0.1920(5) 0.5100(4) 0.041(3) Uani ? ? C C18 0.1916(6) 0.1169(4) 0.4895(4) 0.038(3) Uani ? ? C CL1 0.7616(1) 0.3308(1) 0.6315(1) 0.0429(6) Uani ? ? Cl O3 0.6147(6) 0.3111(6) 0.5787(5) 0.114(4) Uani ? ? O O4 0.8611(7) 0.4103(4) 0.5684(4) 0.092(3) Uani ? ? O O5 0.8110(7) 0.2315(4) 0.6402(7) 0.134(4) Uani ? ? O O6 0.7908(6) 0.4020(5) 0.7367(3) 0.076(3) Uani ? ? O CL2 0.7772(2) 0.0107(1) 0.2180(1) 0.0577(8) Uani ? ? Cl O7 0.6380(7) -0.0677(7) 0.1823(6) 0.143(5) Uani ? ? O O8 0.8231(8) 0.0699(6) 0.1311(5) 0.241(4) Uani ? ? O O9 0.8894(5) -0.0442(4) 0.2589(4) 0.083(2) Uani ? ? O O10 0.7630(6) 0.0880(5) 0.3066(4) 0.091(3) Uani ? ? O O11 1.1074(6) 0.2889(4) 0.8126(4) 0.077(3) Uani ? ? O H1 0.4866 0.1858 -0.0004 0.0419 Uiso calc C1 H H2 0.6622 0.2360 -0.1139 0.0467 Uiso calc C2 H H3 0.9093 0.3637 -0.0379 0.0506 Uiso calc C3 H H4 0.9667 0.4496 0.1499 0.0495 Uiso calc C4 H H5 0.8541 0.4966 0.3116 0.0534 Uiso calc C6 H H6 0.8300 0.3685 0.3474 0.0534 Uiso calc C6 H H7 0.6903 0.5953 0.3221 0.0590 Uiso calc C7 H H8 0.5403 0.5447 0.3661 0.0590 Uiso calc C7 H H9 0.5693 0.5094 0.1452 0.0509 Uiso calc C8 H H10 0.4756 0.5861 0.1895 0.0509 Uiso calc C8 H H11 0.3438 0.3730 0.0241 0.0567 Uiso calc C9 H H12 0.2276 0.4300 0.0642 0.0567 Uiso calc C9 H H13 0.1147 0.2190 0.0102 0.0608 Uiso calc C10 H H14 0.1131 0.2529 0.1348 0.0608 Uiso calc C10 H H15 0.1320 0.0110 0.0755 0.0564 Uiso calc C11 H H16 0.1361 0.0672 0.1952 0.0564 Uiso calc C11 H H17 0.3713 -0.0042 0.1281 0.0624 Uiso calc C12 H H18 0.2736 -0.0665 0.2108 0.0624 Uiso calc C12 H H19 0.4793 0.0958 0.4485 0.0520 Uiso calc C13 H H20 0.3344 -0.0091 0.3922 0.0520 Uiso calc C13 H H21 0.2364 0.3928 0.3525 0.0451 Uiso calc C15 H H22 0.0630 0.3482 0.4702 0.0531 Uiso calc C16 H H23 0.0356 0.1726 0.5594 0.0620 Uiso calc C17 H H24 0.1825 0.0457 0.5245 0.0535 Uiso calc C18 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 0.0241(2) 0.0274(2) 0.0279(2) 0.0085(2) 0.0081(2) 0.0061(2) Zn N1 0.029(2) 0.034(2) 0.029(2) 0.008(1) 0.009(2) -0.001(2) N C1 0.036(2) 0.031(2) 0.033(2) 0.013(2) 0.010(2) 0.002(2) C C2 0.052(2) 0.033(2) 0.031(2) 0.022(2) 0.016(2) 0.006(2) C C3 0.045(2) 0.040(2) 0.046(2) 0.022(2) 0.027(2) 0.018(2) C C4 0.027(2) 0.038(2) 0.053(3) 0.010(2) 0.014(2) 0.013(2) C C5 0.023(2) 0.034(2) 0.031(2) 0.010(2) 0.006(2) 0.006(2) C C6 0.027(2) 0.059(3) 0.030(2) 0.006(2) -0.001(2) 0.007(2) C N2 0.031(2) 0.035(2) 0.030(2) 0.004(2) 0.009(2) 0.002(2) N C7 0.048(3) 0.032(2) 0.050(3) 0.005(2) 0.011(2) -0.007(2) C C8 0.042(3) 0.029(2) 0.049(3) 0.010(2) 0.014(2) 0.015(2) C O1 0.037(2) 0.033(1) 0.034(2) 0.013(1) 0.009(1) 0.014(1) O C9 0.041(3) 0.051(3) 0.040(3) 0.017(2) 0.002(2) 0.017(2) C C10 0.032(3) 0.065(3) 0.040(3) 0.013(2) -0.003(2) 0.019(2) C O2 0.029(2) 0.037(2) 0.040(2) 0.004(1) 0.007(1) 0.004(1) O C11 0.042(3) 0.034(2) 0.043(3) -0.006(2) 0.013(2) -0.001(2) C C12 0.061(3) 0.029(2) 0.054(3) 0.008(2) 0.024(2) -0.000(2) C N3 0.038(2) 0.030(2) 0.043(2) 0.014(1) 0.015(2) 0.013(2) N C13 0.044(3) 0.028(2) 0.050(3) 0.012(2) 0.009(2) 0.012(2) C C14 0.030(2) 0.033(2) 0.028(2) 0.004(2) 0.003(2) 0.005(2) C N4 0.026(2) 0.031(2) 0.030(2) 0.010(1) 0.009(2) 0.010(1) N C15 0.036(2) 0.044(2) 0.030(2) 0.019(2) 0.010(2) 0.002(2) C C16 0.034(2) 0.054(3) 0.033(2) 0.015(2) 0.005(2) -0.002(2) C C17 0.035(3) 0.068(3) 0.028(2) -0.001(2) 0.011(2) -0.008(2) C C18 0.046(3) 0.036(2) 0.034(2) -0.001(2) 0.011(2) 0.009(2) C CL1 0.0425(6) 0.0465(6) 0.0400(6) 0.0187(5) 0.0060(5) 0.0037(5) Cl O3 0.051(3) 0.212(5) 0.137(4) 0.040(3) -0.018(3) -0.085(4) O O4 0.118(4) 0.081(3) 0.082(3) 0.023(3) 0.041(3) 0.024(2) O O5 0.135(4) 0.062(2) 0.289(8) 0.059(2) 0.074(5) 0.047(4) O O6 0.091(4) 0.106(3) 0.046(2) 0.016(3) 0.006(2) -0.009(2) O CL2 0.0418(7) 0.1024(9) 0.0449(7) 0.0336(6) 0.0115(6) 0.0136(7) Cl O7 0.057(4) 0.257(6) 0.198(6) 0.004(4) -0.017(4) -0.148(4) O O8 0.256(5) 0.338(5) 0.163(3) 0.231(3) 0.151(3) 0.192(3) O O9 0.078(2) 0.084(2) 0.086(3) 0.047(2) 0.034(2) 0.038(2) O O10 0.076(3) 0.132(3) 0.077(3) 0.055(2) -0.007(3) -0.017(3) O O11 0.105(4) 0.076(3) 0.058(3) 0.028(2) 0.000(3) 0.004(2) 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 2.133(4) . . ? ZN N2 2.107(4) . . ? ZN O1 2.188(3) . . ? ZN O2 2.186(4) . . ? ZN N3 2.098(4) . . ? ZN N4 2.140(4) . . ? N1 C1 1.364(6) . . ? N1 C5 1.329(6) . . ? C1 C2 1.355(7) . . ? C2 C3 1.381(8) . . ? C3 C4 1.381(8) . . ? C4 C5 1.382(7) . . ? C5 C6 1.519(7) . . ? C6 N2 1.491(7) . . ? N2 C7 1.469(7) . . ? C7 C8 1.488(8) . . ? C8 O1 1.441(6) . . ? O1 C9 1.412(6) . . ? C9 C10 1.513(8) . . ? C10 O2 1.441(7) . . ? O2 C11 1.432(6) . . ? C11 C12 1.501(9) . . ? C12 N3 1.498(7) . . ? N3 C13 1.476(7) . . ? C13 C14 1.493(7) . . ? C14 N4 1.326(6) . . ? C14 C18 1.389(7) . . ? N4 C15 1.359(6) . . ? C15 C16 1.366(7) . . ? C16 C17 1.394(9) . . ? C17 C18 1.388(8) . . ? CL1 O3 1.359(6) . . ? CL1 O4 1.467(6) . . ? CL1 O5 1.371(6) . . ? CL1 O6 1.422(5) . . ? CL2 O7 1.332(7) . . ? CL2 O8 1.368(7) . . ? CL2 O9 1.421(5) . . ? CL2 O10 1.410(5) . . ? O7 O8 2.20(1) . . ? O7 O10 2.181(8) . . ? 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 79.6(2) . . . ? N1 ZN O1 90.7(1) . . . ? N1 ZN O2 89.2(1) . . . ? N1 ZN N3 100.4(2) . . . ? N1 ZN N4 179.4(2) . . . ? N2 ZN O1 80.4(2) . . . ? N2 ZN O2 152.0(2) . . . ? N2 ZN N3 125.9(2) . . . ? N2 ZN N4 99.9(2) . . . ? O1 ZN O2 74.1(1) . . . ? O1 ZN N3 152.8(2) . . . ? O1 ZN N4 89.3(1) . . . ? O2 ZN N3 81.2(2) . . . ? O2 ZN N4 91.3(1) . . . ? N3 ZN N4 79.8(2) . . . ? ZN N1 C1 127.8(4) . . . ? ZN N1 C5 114.5(3) . . . ? C1 N1 C5 117.4(4) . . . ? N1 C1 C2 122.7(5) . . . ? C1 C2 C3 119.0(5) . . . ? C2 C3 C4 119.5(5) . . . ? C3 C4 C5 118.0(5) . . . ? N1 C5 C4 123.4(4) . . . ? N1 C5 C6 116.1(4) . . . ? C4 C5 C6 120.5(5) . . . ? C5 C6 N2 111.1(4) . . . ? ZN N2 C6 108.4(3) . . . ? ZN N2 C7 108.8(3) . . . ? C6 N2 C7 113.9(4) . . . ? N2 C7 C8 112.6(4) . . . ? C7 C8 O1 106.9(4) . . . ? ZN O1 C8 107.4(3) . . . ? ZN O1 C9 114.0(3) . . . ? C8 O1 C9 116.6(4) . . . ? O1 C9 C10 106.4(4) . . . ? C9 C10 O2 105.6(5) . . . ? ZN O2 C10 113.1(3) . . . ? ZN O2 C11 108.4(3) . . . ? C10 O2 C11 115.2(4) . . . ? O2 C11 C12 105.6(5) . . . ? C11 C12 N3 113.5(4) . . . ? ZN N3 C12 107.5(3) . . . ? ZN N3 C13 108.1(3) . . . ? C12 N3 C13 113.9(4) . . . ? N3 C13 C14 112.4(4) . . . ? C13 C14 N4 116.5(5) . . . ? C13 C14 C18 120.9(5) . . . ? N4 C14 C18 122.5(5) . . . ? ZN N4 C14 113.4(3) . . . ? ZN N4 C15 127.2(3) . . . ? C14 N4 C15 119.1(4) . . . ? N4 C15 C16 122.1(5) . . . ? C15 C16 C17 118.5(5) . . . ? C16 C17 C18 119.6(5) . . . ? C14 C18 C17 118.0(5) . . . ? O3 CL1 O4 107.4(5) . . . ? O3 CL1 O5 116.9(5) . . . ? O3 CL1 O6 110.1(4) . . . ? O4 CL1 O5 106.4(4) . . . ? O4 CL1 O6 103.0(3) . . . ? O5 CL1 O6 111.9(5) . . . ? O7 CL2 O8 109.0(7) . . . ? O7 CL2 O9 113.6(6) . . . ? O7 CL2 O10 105.4(4) . . . ? O8 CL2 O9 107.4(4) . . . ? O8 CL2 O10 113.0(6) . . . ? O9 CL2 O10 108.5(3) . . . ? CL2 O7 O8 36.1(4) . . . ? CL2 O7 O10 38.5(3) . . . ? O8 O7 O10 63.9(4) . . . ? CL2 O8 O7 35.0(4) . . . ? CL2 O10 O7 36.1(3) . . . ? # =============================================END data_complex_5_[Cupytrien](ClO4)2 H2O (5) _database_code_CSD 155154 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H30 Cl2 N6 O9 Zn' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H30 Cl2 N6 O9 Zn' _chemical_formula_weight 610.75 _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/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.5701(5) _cell_length_b 15.8048(9) _cell_length_c 15.2231(6) _cell_angle_alpha 90 _cell_angle_beta 98.749(5) _cell_angle_gamma 90 _cell_volume 2513.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 10613 _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 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.250 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=========================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _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 ; 10613 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 == 0.00 112 frames Set 2 Theta == -6.30 Kappa == 129.00 Phi == 0.00 18 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 10613 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5974 _reflns_number_gt 3488 _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 3488 _refine_ls_number_parameters 325 _refine_ls_number_restraints 16 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.084 _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_all 0.363 _refine_ls_wR_factor_ref 0.066 _refine_ls_goodness_of_fit_all 7.097 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.010 _refine_diff_density_min -0.385 #=========================================================================== # # 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 0.17807(4) 0.25557(2) 0.46011(2) 0.0261(2) Uani ? ? Zn N1 0.3447(3) 0.2116(2) 0.4095(2) 0.027(1) Uani ? ? N C1 0.4189(4) 0.2571(2) 0.3623(2) 0.032(2) Uani ? ? C C2 0.5243(4) 0.2239(3) 0.3321(2) 0.041(2) Uani ? ? C C3 0.5541(4) 0.1392(3) 0.3488(2) 0.046(2) Uani ? ? C C4 0.4780(4) 0.0926(3) 0.3952(2) 0.042(2) Uani ? ? C C5 0.3746(4) 0.1302(2) 0.4269(2) 0.031(2) Uani ? ? C C6 0.2988(4) 0.0835(2) 0.4866(2) 0.040(2) Uani ? ? C N2 0.1718(3) 0.1199(2) 0.4882(2) 0.034(2) Uani ? ? N C7 0.0678(4) 0.0832(3) 0.4229(3) 0.051(2) Uani ? ? C C8 0.0504(4) 0.1319(3) 0.3355(3) 0.047(2) Uani ? ? C N3 0.0302(3) 0.2232(2) 0.3514(2) 0.039(2) Uani ? ? N C9 -0.0963(4) 0.2432(3) 0.3771(3) 0.052(3) Uani ? ? C C10 -0.0861(4) 0.3132(3) 0.4463(3) 0.051(2) Uani ? ? C N4 0.0121(3) 0.2892(2) 0.5201(2) 0.040(2) Uani ? ? N C11 0.0544(4) 0.3563(3) 0.5858(2) 0.051(2) Uani ? ? C C12 0.1778(4) 0.3280(3) 0.6410(2) 0.043(2) Uani ? ? C N5 0.2756(3) 0.3077(2) 0.5850(2) 0.031(2) Uani ? ? N C13 0.3531(4) 0.3806(3) 0.5656(2) 0.037(2) Uani ? ? C C14 0.2932(3) 0.4288(2) 0.4842(2) 0.031(2) Uani ? ? C N6 0.2138(3) 0.3860(2) 0.4225(2) 0.027(1) Uani ? ? N C15 0.1672(3) 0.4259(2) 0.3460(2) 0.032(2) Uani ? ? C C16 0.1971(4) 0.5077(3) 0.3294(3) 0.043(2) Uani ? ? C C17 0.2775(4) 0.5526(3) 0.3930(3) 0.047(2) Uani ? ? C C18 0.3243(4) 0.5122(2) 0.4719(3) 0.040(2) Uani ? ? C CL1 0.1313(1) 0.29911(7) 0.12590(6) 0.0429(5) Uani ? ? Cl O1 0.1667(4) 0.3824(2) 0.1131(2) 0.075(2) Uani ? ? O O2 0.0038(3) 0.3034(3) 0.1568(2) 0.082(2) Uani ? ? O O3 0.2095(4) 0.2593(2) 0.1961(2) 0.065(2) Uani ? ? O O4 0.1173(4) 0.2505(2) 0.0472(2) 0.057(2) Uani ? ? O CL2 -0.2689(1) 0.44254(6) 0.23861(6) 0.0447(5) Uani ? ? Cl O5 -0.1608(4) 0.4667(2) 0.2999(3) 0.090(3) Uani ? ? O O6 -0.3773(4) 0.4376(3) 0.2838(2) 0.106(3) Uani ? ? O O7 -0.2921(3) 0.5042(2) 0.1703(2) 0.055(2) Uani ? ? O O8 -0.2581(5) 0.3627(2) 0.1992(2) 0.076(2) Uani ? ? O O9 -0.5497(3) 0.3644(3) 0.1220(2) 0.082(2) Uani ? ? O H01 0.1491 0.1080 0.5412 0.0452 Uiso ? ? H H02 0.0304 0.2524 0.2940 0.0537 Uiso ? ? H H03 -0.0219 0.2468 0.5571 0.0533 Uiso ? ? H H04 0.3313 0.2662 0.6182 0.0538 Uiso ? ? H H1 0.3972 0.3146 0.3494 0.0425 Uiso calc C1 H H2 0.5759 0.2582 0.3005 0.0547 Uiso calc C2 H H3 0.6260 0.1143 0.3283 0.0633 Uiso calc C3 H H4 0.4956 0.0342 0.4060 0.0558 Uiso calc C4 H H5 0.3448 0.0845 0.5453 0.0563 Uiso calc C6 H H6 0.2886 0.0266 0.4667 0.0563 Uiso calc C6 H H7 -0.0100 0.0852 0.4470 0.0704 Uiso calc C7 H H8 0.0882 0.0261 0.4118 0.0704 Uiso calc C7 H H9 -0.0218 0.1101 0.2974 0.0648 Uiso calc C8 H H10 0.1247 0.1252 0.3081 0.0648 Uiso calc C8 H H11 -0.1295 0.1938 0.4008 0.0766 Uiso calc C9 H H12 -0.1527 0.2610 0.3258 0.0766 Uiso calc C9 H H13 -0.1659 0.3200 0.4669 0.0690 Uiso calc C10 H H14 -0.0629 0.3648 0.4210 0.0690 Uiso calc C10 H H15 -0.0089 0.3650 0.6230 0.0649 Uiso calc C11 H H16 0.0679 0.4075 0.5559 0.0649 Uiso calc C11 H H17 0.1617 0.2791 0.6738 0.0570 Uiso calc C12 H H18 0.2089 0.3722 0.6809 0.0570 Uiso calc C12 H H19 0.4349 0.3609 0.5563 0.0490 Uiso calc C13 H H20 0.3625 0.4178 0.6152 0.0490 Uiso calc C13 H H21 0.1114 0.3958 0.3019 0.0420 Uiso calc C15 H H22 0.1629 0.5336 0.2747 0.0558 Uiso calc C16 H H23 0.3000 0.6096 0.3828 0.0656 Uiso calc C17 H H24 0.3777 0.5418 0.5176 0.0544 Uiso calc C18 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 0.0277(2) 0.0258(2) 0.0249(2) -0.0008(2) 0.0036(2) 0.0010(2) Zn N1 0.031(1) 0.027(1) 0.023(1) 0.003(1) 0.003(1) -0.003(1) N C1 0.036(2) 0.037(2) 0.025(2) -0.000(2) 0.005(2) -0.001(2) C C2 0.037(2) 0.059(3) 0.031(2) 0.004(2) 0.009(2) -0.002(2) C C3 0.041(2) 0.071(3) 0.034(2) 0.023(2) 0.007(2) -0.011(2) C C4 0.049(2) 0.042(2) 0.035(2) 0.021(2) -0.003(2) -0.007(2) C C5 0.045(2) 0.030(2) 0.022(2) 0.007(2) -0.004(2) -0.002(2) C C6 0.059(2) 0.028(2) 0.040(2) 0.005(2) -0.004(2) 0.000(2) C N2 0.043(2) 0.032(2) 0.030(1) -0.005(2) 0.001(1) 0.003(1) N C7 0.063(3) 0.039(2) 0.054(2) -0.026(2) -0.012(2) 0.007(2) C C8 0.059(2) 0.044(2) 0.041(2) -0.021(2) -0.010(2) -0.003(2) C N3 0.044(2) 0.045(2) 0.031(2) -0.013(2) -0.003(1) 0.012(2) N C9 0.029(2) 0.083(4) 0.059(3) -0.007(2) -0.012(2) 0.024(2) C C10 0.032(2) 0.072(3) 0.056(2) 0.007(2) 0.009(2) 0.015(2) C N4 0.033(2) 0.048(2) 0.040(2) 0.002(2) 0.013(1) 0.010(2) N C11 0.059(2) 0.053(3) 0.043(2) 0.018(2) 0.022(2) 0.003(2) C C12 0.059(2) 0.040(2) 0.035(2) 0.001(2) 0.013(2) -0.004(2) C N5 0.043(2) 0.028(2) 0.024(1) 0.006(1) 0.004(1) -0.001(1) N C13 0.039(2) 0.038(2) 0.033(2) -0.004(2) -0.002(2) -0.006(2) C C14 0.028(2) 0.026(2) 0.038(2) 0.003(2) 0.009(2) -0.007(2) C N6 0.032(1) 0.023(1) 0.027(1) 0.001(1) 0.007(1) 0.000(1) N C15 0.036(2) 0.029(2) 0.032(2) 0.005(2) 0.005(2) 0.004(2) C C16 0.045(2) 0.036(2) 0.049(2) 0.008(2) 0.010(2) 0.016(2) C C17 0.050(2) 0.028(2) 0.073(3) -0.005(2) 0.008(2) 0.007(2) C C18 0.041(2) 0.029(2) 0.054(2) -0.003(2) 0.004(2) -0.003(2) C CL1 0.0635(6) 0.0357(5) 0.0349(5) 0.0072(5) -0.0075(5) -0.0012(4) Cl O1 0.131(3) 0.039(2) 0.083(2) -0.022(2) 0.026(2) 0.012(2) O O2 0.050(2) 0.121(3) 0.093(2) -0.003(2) 0.020(2) -0.024(3) O O3 0.092(2) 0.069(2) 0.043(2) 0.017(2) -0.017(2) 0.002(2) O O4 0.091(2) 0.059(2) 0.035(2) 0.010(2) -0.004(2) -0.007(1) O CL2 0.0741(7) 0.0306(5) 0.0395(5) -0.0043(5) -0.0001(5) -0.0043(4) Cl O5 0.100(2) 0.066(2) 0.110(3) 0.003(2) -0.056(2) -0.001(2) O O6 0.135(3) 0.117(4) 0.076(2) -0.037(3) 0.057(2) -0.009(2) O O7 0.056(2) 0.049(2) 0.061(2) -0.004(2) 0.001(1) 0.016(2) O O8 0.189(4) 0.036(2) 0.064(2) 0.016(2) 0.024(2) -0.007(2) O O9 0.071(2) 0.077(3) 0.102(2) 0.000(2) 0.025(2) -0.014(2) 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 2.142(3) . . ? ZN N2 2.189(3) . . ? ZN N3 2.158(3) . . ? ZN N4 2.164(3) . . ? ZN N5 2.182(3) . . ? ZN N6 2.188(3) . . ? N1 C1 1.350(5) . . ? N1 C5 1.342(5) . . ? C1 C2 1.372(6) . . ? C2 C3 1.390(7) . . ? C3 C4 1.365(6) . . ? C4 C5 1.393(6) . . ? C5 C6 1.495(6) . . ? C6 N2 1.463(6) . . ? C6 H01 1.9347 . . ? N2 C7 1.484(5) . . ? N2 H01 0.8961 . . ? C7 C8 1.524(6) . . ? C7 H01 1.9138 . . ? C8 N3 1.484(6) . . ? C8 H02 2.0083 . . ? N3 C9 1.482(6) . . ? N3 H02 0.9894 . . ? C9 C10 1.520(7) . . ? C9 H02 1.9815 . . ? C10 N4 1.459(6) . . ? C10 H03 2.0144 . . ? N4 C11 1.480(6) . . ? N4 H03 0.9780 . . ? C11 C12 1.508(6) . . ? C11 H03 1.9307 . . ? C12 N5 1.472(5) . . ? C12 H04 1.9707 . . ? N5 C13 1.468(5) . . ? N5 H04 0.9710 . . ? C13 C14 1.510(6) . . ? C13 H04 2.0046 . . ? C14 N6 1.342(5) . . ? C14 C18 1.378(5) . . ? N6 C15 1.350(5) . . ? C15 C16 1.363(6) . . ? C16 C17 1.384(6) . . ? C17 C18 1.384(6) . . ? CL1 O1 1.390(4) . . ? CL1 O2 1.495(4) . . ? CL1 O3 1.397(3) . . ? CL1 O4 1.412(3) . . ? O2 H04 2.1332 . 4_454 ? CL2 O5 1.414(4) . . ? CL2 O6 1.425(5) . . ? CL2 O7 1.420(3) . . ? CL2 O8 1.410(4) . . ? O9 H03 2.0588 . 4_454 ? 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 78.7(1) . . . ? N1 ZN N3 100.8(1) . . . ? N1 ZN N4 174.3(1) . . . ? N1 ZN N5 97.5(1) . . . ? N1 ZN N6 91.6(1) . . . ? N2 ZN N3 83.0(1) . . . ? N2 ZN N4 96.2(1) . . . ? N2 ZN N5 102.9(1) . . . ? N2 ZN N6 170.2(1) . . . ? N3 ZN N4 80.9(1) . . . ? N3 ZN N5 161.6(1) . . . ? N3 ZN N6 99.0(1) . . . ? N4 ZN N5 81.1(1) . . . ? N4 ZN N6 93.6(1) . . . ? N5 ZN N6 78.1(1) . . . ? ZN N1 C1 126.5(3) . . . ? ZN N1 C5 115.0(3) . . . ? C1 N1 C5 118.5(3) . . . ? N1 C1 C2 122.8(4) . . . ? C1 C2 C3 118.7(4) . . . ? C2 C3 C4 118.7(4) . . . ? C3 C4 C5 120.2(4) . . . ? N1 C5 C4 121.0(4) . . . ? N1 C5 C6 117.4(4) . . . ? C4 C5 C6 121.4(4) . . . ? C5 C6 N2 113.2(3) . . . ? C5 C6 H01 135.41 . . . ? N2 C6 H01 26.18 . . . ? ZN N2 C6 109.1(2) . . . ? ZN N2 C7 107.0(2) . . . ? ZN N2 H01 113.72 . . . ? C6 N2 C7 115.1(4) . . . ? C6 N2 H01 107.74 . . . ? C7 N2 H01 104.33 . . . ? N2 C7 C8 111.5(3) . . . ? N2 C7 H01 26.98 . . . ? C8 C7 H01 134.10 . . . ? C7 C8 N3 110.4(4) . . . ? C7 C8 H02 138.26 . . . ? N3 C8 H02 28.13 . . . ? ZN N3 C8 104.5(2) . . . ? ZN N3 C9 108.9(3) . . . ? ZN N3 H02 117.88 . . . ? C8 N3 C9 114.1(4) . . . ? C8 N3 H02 106.89 . . . ? C9 N3 H02 104.81 . . . ? N3 C9 C10 111.5(4) . . . ? N3 C9 H02 28.86 . . . ? C10 C9 H02 113.92 . . . ? C9 C10 N4 108.2(4) . . . ? C9 C10 H03 100.44 . . . ? N4 C10 H03 27.15 . . . ? ZN N4 C10 105.4(3) . . . ? ZN N4 C11 106.3(2) . . . ? ZN N4 H03 117.83 . . . ? C10 N4 C11 116.2(4) . . . ? C10 N4 H03 109.96 . . . ? C11 N4 H03 101.60 . . . ? N4 C11 C12 108.1(4) . . . ? N4 C11 H03 29.75 . . . ? C12 C11 H03 99.01 . . . ? C11 C12 N5 111.5(3) . . . ? C11 C12 H04 135.61 . . . ? N5 C12 H04 28.32 . . . ? ZN N5 C12 107.9(2) . . . ? ZN N5 C13 109.0(2) . . . ? ZN N5 H04 111.49 . . . ? C12 N5 C13 114.0(3) . . . ? C12 N5 H04 105.68 . . . ? C13 N5 H04 108.81 . . . ? N5 C13 C14 112.6(3) . . . ? N5 C13 H04 27.29 . . . ? C14 C13 H04 136.35 . . . ? C13 C14 N6 117.4(3) . . . ? C13 C14 C18 121.0(4) . . . ? N6 C14 C18 121.6(4) . . . ? ZN N6 C14 113.9(2) . . . ? ZN N6 C15 127.6(3) . . . ? C14 N6 C15 118.4(3) . . . ? N6 C15 C16 122.5(4) . . . ? C15 C16 C17 119.5(4) . . . ? C16 C17 C18 118.1(4) . . . ? C14 C18 C17 119.9(4) . . . ? O1 CL1 O2 106.0(3) . . . ? O1 CL1 O3 113.1(2) . . . ? O1 CL1 O4 113.1(2) . . . ? O2 CL1 O3 103.7(3) . . . ? O2 CL1 O4 108.0(2) . . . ? O3 CL1 O4 112.2(2) . . . ? CL1 O2 H04 131.53 . . 4_454 ? O5 CL2 O6 109.0(3) . . . ? O5 CL2 O7 109.3(2) . . . ? O5 CL2 O8 114.4(3) . . . ? O6 CL2 O7 109.3(3) . . . ? O6 CL2 O8 106.2(3) . . . ? O7 CL2 O8 108.6(2) . . . ? C6 H01 N2 46.08 . . . ? C6 H01 C7 80.49 . . . ? N2 H01 C7 48.69 . . . ? C8 H02 N3 44.99 . . . ? C8 H02 C9 77.22 . . . ? N3 H02 C9 46.33 . . . ? C10 H03 N4 42.89 . . . ? C10 H03 C11 78.39 . . . ? C10 H03 O9 142.34 . . 4_555 ? N4 H03 C11 48.65 . . . ? N4 H03 O9 162.31 . . 4_555 ? C11 H03 O9 137.88 . . 4_555 ? C12 H04 N5 46.00 . . . ? C12 H04 C13 76.70 . . . ? C12 H04 O2 154.04 . . 4_555 ? N5 H04 C13 43.90 . . . ? N5 H04 O2 156.54 . . 4_555 ? C13 H04 O2 115.48 . . 4_555 ? #=================END