# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2228 data_General _audit_creation_date 'Sat Sep 30 10:12:53 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hisashi Okawa' _publ_contact_author_address ; Dept. of Chem., Fac. Of Sci., Kyushu Univ., Hakozaki 6-1-1, Higashi-ku, Fukuoka 812-8581, Japan ; _publ_contact_author_email ' okawascc@mbox.nc.kyushu-u.ac.jp ' _publ_contact_author_fax ' 81-92-642-2607 ' _publ_contact_author_phone ' 81-92-642-2596 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' JCS Dalton trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_Mn[Cu(HL)]2_4DMF #(1) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C44 H50 Cu2 N12 Mn O12 ' _chemical_formula_moiety 'C44 H50 Cu2 N12 Mn O12 ' _chemical_formula_weight 1120.98 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 24.904(4) _cell_length_b 10.229(2) _cell_length_c 19.581(2) _cell_angle_alpha 90 _cell_angle_beta 103.93(1) _cell_angle_gamma 90 _cell_volume 4841(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.887 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6015 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5564 _reflns_number_gt 2996 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0511 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2996 _refine_ls_number_parameters 321 _refine_ls_goodness_of_fit_ref 1.462 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_shift/su_max 0.1369 _refine_diff_density_max 0.37 _refine_diff_density_min -0.34 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.12243(2) 0.04346(6) 0.47875(3) 0.0390(1) Uani 1.00 d . . . Mn(1) Mn 0.0000 -0.2219(1) 0.2500 0.0441(3) Uani 1.00 d S . . O(1) O 0.0648(1) -0.0765(3) 0.2820(2) 0.0502(10) Uani 1.00 d . . . O(2) O 0.0118(1) -0.2008(3) 0.3628(1) 0.0456(9) Uani 1.00 d . . . O(3) O 0.1641(2) 0.3049(4) 0.5255(2) 0.075(1) Uani 1.00 d . . . O(4) O 0.1347(2) 0.1801(4) 0.6125(2) 0.068(1) Uani 1.00 d . . . O(5) O 0.2045(1) -0.0704(4) 0.5346(2) 0.067(1) Uani 1.00 d . . . O(6) O 0.0604(2) -0.3734(4) 0.2500(2) 0.070(1) Uani 1.00 d . . . N(1) N 0.1256(1) 0.0086(4) 0.3797(2) 0.039(1) Uani 1.00 d . . . N(2) N 0.0664(1) -0.1002(4) 0.4622(2) 0.0354(10) Uani 1.00 d . . . N(3) N 0.1627(2) 0.2130(4) 0.4750(2) 0.050(1) Uani 1.00 d . . . N(4) N 0.1089(2) 0.0776(4) 0.5725(2) 0.046(1) Uani 1.00 d . . . N(5) N 0.2949(2) -0.1217(4) 0.5551(2) 0.055(1) Uani 1.00 d . . . N(6) N 0.1085(2) -0.5117(5) 0.1990(2) 0.058(1) Uani 1.00 d . . . C(1) C 0.1637(2) 0.0579(5) 0.3425(2) 0.042(1) Uani 1.00 d . . . C(2) C 0.1729(2) -0.0026(5) 0.2826(3) 0.054(2) Uani 1.00 d . . . C(3) C 0.2118(2) 0.0449(6) 0.2492(3) 0.069(2) Uani 1.00 d . . . C(4) C 0.2429(2) 0.1528(7) 0.2754(3) 0.075(2) Uani 1.00 d . . . C(5) C 0.2352(2) 0.2128(6) 0.3348(3) 0.064(2) Uani 1.00 d . . . C(6) C 0.1953(2) 0.1679(5) 0.3694(3) 0.049(1) Uani 1.00 d . . . C(7) C 0.1900(2) 0.2421(5) 0.4297(3) 0.056(2) Uani 1.00 d . . . C(8) C 0.0805(2) 0.0082(5) 0.6048(2) 0.048(1) Uani 1.00 d . . . C(9) C 0.0413(2) -0.1631(5) 0.5111(2) 0.038(1) Uani 1.00 d . . . C(10) C 0.0110(2) -0.2789(5) 0.4969(3) 0.056(2) Uani 1.00 d . . . C(11) C -0.0140(2) -0.3343(6) 0.5458(3) 0.069(2) Uani 1.00 d . . . C(12) C -0.0084(2) -0.2791(7) 0.6106(3) 0.070(2) Uani 1.00 d . . . C(13) C 0.0222(2) -0.1674(6) 0.6271(3) 0.058(2) Uani 1.00 d . . . C(14) C 0.0485(2) -0.1082(5) 0.5789(2) 0.042(1) Uani 1.00 d . . . C(15) C 0.0824(2) -0.0588(4) 0.3469(2) 0.038(1) Uani 1.00 d . . . C(16) C 0.0498(2) -0.1266(4) 0.3937(2) 0.036(1) Uani 1.00 d . . . C(17) C 0.2492(2) -0.0665(5) 0.5193(3) 0.054(2) Uani 1.00 d . . . C(18) C 0.2960(3) -0.1979(8) 0.6166(3) 0.092(3) Uani 1.00 d . . . C(19) C 0.3462(3) -0.1138(7) 0.5341(5) 0.107(3) Uani 1.00 d . . . C(20) C 0.0812(2) -0.4047(6) 0.2017(3) 0.061(2) Uani 1.00 d . . . C(21) C 0.1161(4) -0.6046(7) 0.2558(4) 0.109(3) Uani 1.00 d . . . C(22) C 0.1309(3) -0.5449(7) 0.1398(4) 0.087(2) Uani 1.00 d . . . H(1) H 0.1512 -0.0910 0.2654 0.0740 Uiso 1.00 calc . . . H(2) H 0.2191 -0.0034 0.2027 0.0740 Uiso 1.00 calc . . . H(3) H 0.2718 0.1907 0.2510 0.0740 Uiso 1.00 calc . . . H(4) H 0.2594 0.2922 0.3582 0.0740 Uiso 1.00 calc . . . H(5) H 0.2079 0.3339 0.4437 0.0740 Uiso 1.00 calc . . . H(6) H 0.1578 0.2297 0.5746 0.0740 Uiso 1.00 calc . . . H(7) H 0.0762 0.0348 0.6534 0.0740 Uiso 1.00 calc . . . H(8) H 0.0283 -0.1199 0.6739 0.0740 Uiso 1.00 calc . . . H(9) H -0.0262 -0.3106 0.6482 0.0740 Uiso 1.00 calc . . . H(10) H -0.0347 -0.4163 0.5340 0.0740 Uiso 1.00 calc . . . H(11) H 0.0010 -0.3192 0.4462 0.0740 Uiso 1.00 calc . . . H(12) H 0.2490 -0.0050 0.4722 0.0740 Uiso 1.00 calc . . . H(13) H 0.2842 -0.1487 0.6517 0.1070 Uiso 1.00 calc . . . H(14) H 0.2704 -0.2720 0.6046 0.1070 Uiso 1.00 calc . . . H(15) H 0.3316 -0.2335 0.6362 0.1070 Uiso 1.00 calc . . . H(16) H 0.3754 -0.1592 0.5654 0.1232 Uiso 1.00 calc . . . H(17) H 0.3424 -0.1513 0.4874 0.1232 Uiso 1.00 calc . . . H(18) H 0.3576 -0.0243 0.5311 0.1232 Uiso 1.00 calc . . . H(19) H 0.0769 -0.3445 0.1613 0.0730 Uiso 1.00 calc . . . H(20) H 0.0810 -0.6368 0.2617 0.1258 Uiso 1.00 calc . . . H(21) H 0.1366 -0.6805 0.2464 0.1258 Uiso 1.00 calc . . . H(22) H 0.1356 -0.5683 0.2994 0.1258 Uiso 1.00 calc . . . H(23) H 0.1502 -0.6267 0.1465 0.1035 Uiso 1.00 calc . . . H(24) H 0.1026 -0.5501 0.0969 0.1035 Uiso 1.00 calc . . . H(25) H 0.1572 -0.4790 0.1327 0.1035 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0392(3) 0.0413(3) 0.0351(3) -0.0019(3) 0.0060(2) -0.0011(3) Mn(1) 0.0442(6) 0.0544(7) 0.0301(5) 0.0000 0.0021(4) 0.0000 O(1) 0.049(2) 0.070(2) 0.030(2) -0.013(2) 0.005(1) 0.003(2) O(2) 0.042(2) 0.061(2) 0.032(2) -0.015(2) 0.007(1) -0.003(2) O(3) 0.114(3) 0.047(2) 0.059(2) -0.022(2) 0.014(2) -0.012(2) O(4) 0.082(3) 0.073(3) 0.054(2) -0.029(2) 0.025(2) -0.030(2) O(5) 0.051(2) 0.074(3) 0.075(3) 0.018(2) 0.011(2) 0.004(2) O(6) 0.080(3) 0.079(3) 0.051(2) 0.028(2) 0.015(2) 0.008(2) N(1) 0.037(2) 0.042(2) 0.036(2) 0.001(2) 0.008(2) 0.002(2) N(2) 0.036(2) 0.041(2) 0.028(2) 0.000(2) 0.004(1) 0.002(2) N(3) 0.057(3) 0.040(2) 0.048(2) -0.005(2) 0.003(2) -0.001(2) N(4) 0.042(2) 0.053(3) 0.043(2) -0.003(2) 0.008(2) -0.012(2) N(5) 0.053(3) 0.047(3) 0.068(3) 0.013(2) 0.022(2) 0.011(2) N(6) 0.060(3) 0.055(3) 0.056(3) 0.011(2) 0.010(2) 0.006(2) C(1) 0.034(2) 0.047(3) 0.044(3) 0.007(2) 0.009(2) 0.016(2) C(2) 0.052(3) 0.061(3) 0.051(3) -0.002(3) 0.019(2) 0.007(3) C(3) 0.068(4) 0.080(4) 0.067(4) 0.004(4) 0.034(3) 0.010(3) C(4) 0.057(4) 0.097(5) 0.078(4) -0.010(4) 0.030(3) 0.019(4) C(5) 0.048(3) 0.070(4) 0.071(4) -0.014(3) 0.011(3) 0.018(3) C(6) 0.046(3) 0.049(3) 0.048(3) -0.003(2) 0.006(2) 0.013(2) C(7) 0.059(3) 0.045(3) 0.059(3) -0.015(3) 0.005(3) 0.006(3) C(8) 0.049(3) 0.060(3) 0.038(3) 0.004(3) 0.015(2) -0.007(2) C(9) 0.032(2) 0.043(3) 0.036(2) 0.003(2) 0.006(2) 0.008(2) C(10) 0.066(4) 0.060(3) 0.039(3) -0.015(3) 0.006(2) 0.007(3) C(11) 0.074(4) 0.071(4) 0.060(4) -0.025(3) 0.014(3) 0.010(3) C(12) 0.073(4) 0.087(5) 0.062(4) -0.008(4) 0.038(3) 0.016(3) C(13) 0.060(3) 0.070(4) 0.047(3) 0.000(3) 0.022(3) 0.003(3) C(14) 0.037(2) 0.051(3) 0.039(3) 0.008(2) 0.008(2) 0.007(2) C(15) 0.036(2) 0.042(3) 0.034(2) 0.004(2) 0.007(2) 0.006(2) C(16) 0.034(2) 0.040(3) 0.033(2) 0.003(2) 0.006(2) 0.005(2) C(17) 0.060(3) 0.046(3) 0.055(3) 0.011(3) 0.010(3) 0.002(2) C(18) 0.080(5) 0.122(6) 0.073(4) 0.027(5) 0.015(4) 0.026(4) C(19) 0.071(4) 0.096(6) 0.174(8) 0.028(4) 0.070(5) 0.039(5) C(20) 0.066(4) 0.053(3) 0.058(3) 0.003(3) 0.007(3) 0.007(3) C(21) 0.150(7) 0.086(5) 0.086(5) 0.047(5) 0.019(5) 0.023(4) C(22) 0.085(5) 0.089(5) 0.093(5) 0.006(4) 0.031(4) -0.013(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Cu(1) O(5) 2.378(4) . . yes Cu(1) N(1) 1.991(4) . . yes Cu(1) N(2) 1.998(4) . . yes Cu(1) N(3) 2.014(4) . . yes Cu(1) N(4) 1.976(4) . . yes Mn(1) O(1) 2.174(3) . . yes Mn(1) O(1) 2.174(3) . 2_555 yes Mn(1) O(2) 2.167(3) . . yes Mn(1) O(2) 2.167(3) . 2_555 yes Mn(1) O(6) 2.159(4) . . yes Mn(1) O(6) 2.159(4) . 2_555 yes O(1) C(15) 1.254(5) . . yes O(2) C(16) 1.252(5) . . yes O(3) N(3) 1.359(5) . . yes O(4) N(4) 1.371(5) . . yes O(4) H(6) 1.159 . . no O(5) C(17) 1.220(6) . . yes O(6) C(20) 1.225(6) . . yes N(1) C(1) 1.421(5) . . yes N(1) C(15) 1.308(5) . . yes N(2) C(9) 1.418(5) . . yes N(2) C(16) 1.331(5) . . yes N(3) C(7) 1.276(6) . . yes N(4) C(8) 1.273(6) . . yes N(5) C(17) 1.312(6) . . yes N(5) C(18) 1.431(7) . . yes N(5) C(19) 1.436(7) . . yes N(6) C(20) 1.296(7) . . yes N(6) C(21) 1.440(8) . . yes N(6) C(22) 1.443(7) . . yes C(1) C(2) 1.395(7) . . yes C(1) C(6) 1.401(7) . . yes C(2) C(3) 1.380(7) . . yes C(2) H(1) 1.065 . . no C(3) C(4) 1.375(9) . . yes C(3) H(2) 1.089 . . no C(4) C(5) 1.370(8) . . yes C(4) H(3) 1.030 . . no C(5) C(6) 1.407(7) . . yes C(5) H(4) 1.048 . . no C(6) C(7) 1.436(7) . . yes C(7) H(5) 1.046 . . no C(8) C(14) 1.454(7) . . yes C(8) H(7) 1.020 . . no C(9) C(10) 1.397(7) . . yes C(9) C(14) 1.414(6) . . yes C(10) C(11) 1.382(7) . . yes C(10) H(11) 1.048 . . no C(11) C(12) 1.366(8) . . yes C(11) H(10) 0.982 . . no C(12) C(13) 1.368(8) . . yes C(12) H(9) 0.999 . . no C(13) C(14) 1.408(6) . . yes C(13) H(8) 1.016 . . no C(15) C(16) 1.530(6) . . yes C(17) H(12) 1.116 . . no C(18) H(13) 0.952 . . no C(18) H(14) 0.982 . . no C(18) H(15) 0.949 . . no C(19) H(16) 0.950 . . no C(19) H(17) 0.974 . . no C(19) H(18) 0.964 . . no C(20) H(19) 0.987 . . no C(21) H(20) 0.967 . . no C(21) H(21) 0.970 . . no C(21) H(22) 0.951 . . no C(22) H(23) 0.959 . . no C(22) H(24) 0.957 . . no C(22) H(25) 0.973 . . no #------------------------------------------------------------------------------ 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 O(5) Cu(1) N(1) 97.4(1) . 1_555 1_555 yes O(5) Cu(1) N(2) 101.8(1) . 1_555 1_555 yes O(5) Cu(1) N(3) 93.3(2) . 1_555 1_555 yes O(5) Cu(1) N(4) 88.8(1) . 1_555 1_555 yes N(1) Cu(1) N(2) 84.2(1) . 1_555 1_555 yes N(1) Cu(1) N(3) 89.0(2) . 1_555 1_555 yes N(1) Cu(1) N(4) 172.7(1) . 1_555 1_555 yes N(2) Cu(1) N(3) 164.1(1) . 1_555 1_555 yes N(2) Cu(1) N(4) 90.7(1) . 1_555 1_555 yes N(3) Cu(1) N(4) 94.6(2) . 1_555 1_555 yes O(1) Mn(1) O(1) 93.6(2) . 1_555 2_555 yes O(1) Mn(1) O(2) 74.3(1) . 1_555 1_555 yes O(1) Mn(1) O(2) 97.7(1) . 1_555 2_555 yes O(1) Mn(1) O(6) 91.3(1) . 1_555 1_555 yes O(1) Mn(1) O(6) 163.8(1) . 1_555 2_555 yes O(1) Mn(1) O(2) 97.7(1) . 2_555 1_555 yes O(1) Mn(1) O(2) 74.3(1) . 2_555 2_555 yes O(1) Mn(1) O(6) 163.8(1) . 2_555 1_555 yes O(1) Mn(1) O(6) 91.3(1) . 2_555 2_555 yes O(2) Mn(1) O(2) 168.6(2) . 1_555 2_555 yes O(2) Mn(1) O(6) 98.5(1) . 1_555 1_555 yes O(2) Mn(1) O(6) 89.7(1) . 1_555 2_555 yes O(2) Mn(1) O(6) 89.7(1) . 2_555 1_555 yes O(2) Mn(1) O(6) 98.5(1) . 2_555 2_555 yes O(6) Mn(1) O(6) 88.3(2) . 1_555 2_555 yes Mn(1) O(1) C(15) 116.4(3) . 1_555 1_555 yes Mn(1) O(2) C(16) 117.1(3) . 1_555 1_555 yes N(4) O(4) H(6) 102.0 . 1_555 1_555 no Cu(1) O(5) C(17) 127.2(4) . 1_555 1_555 yes Mn(1) O(6) C(20) 127.7(4) . 1_555 1_555 yes Cu(1) N(1) C(1) 128.6(3) . 1_555 1_555 yes Cu(1) N(1) C(15) 110.7(3) . 1_555 1_555 yes C(1) N(1) C(15) 120.4(4) . 1_555 1_555 yes Cu(1) N(2) C(9) 128.9(3) . 1_555 1_555 yes Cu(1) N(2) C(16) 110.4(3) . 1_555 1_555 yes C(9) N(2) C(16) 120.5(4) . 1_555 1_555 yes Cu(1) N(3) O(3) 119.6(3) . 1_555 1_555 yes Cu(1) N(3) C(7) 125.5(4) . 1_555 1_555 yes O(3) N(3) C(7) 114.8(4) . 1_555 1_555 yes Cu(1) N(4) O(4) 120.3(3) . 1_555 1_555 yes Cu(1) N(4) C(8) 127.1(3) . 1_555 1_555 yes O(4) N(4) C(8) 112.5(4) . 1_555 1_555 yes C(17) N(5) C(18) 121.4(5) . 1_555 1_555 yes C(17) N(5) C(19) 122.8(5) . 1_555 1_555 yes C(18) N(5) C(19) 115.7(5) . 1_555 1_555 yes C(20) N(6) C(21) 119.9(5) . 1_555 1_555 yes C(20) N(6) C(22) 122.6(5) . 1_555 1_555 yes C(21) N(6) C(22) 117.5(5) . 1_555 1_555 yes N(1) C(1) C(2) 122.7(4) . 1_555 1_555 yes N(1) C(1) C(6) 118.5(4) . 1_555 1_555 yes C(2) C(1) C(6) 118.7(4) . 1_555 1_555 yes C(1) C(2) C(3) 121.2(5) . 1_555 1_555 yes C(1) C(2) H(1) 117.9 . 1_555 1_555 no C(3) C(2) H(1) 120.7 . 1_555 1_555 no C(2) C(3) C(4) 120.3(6) . 1_555 1_555 yes C(2) C(3) H(2) 120.8 . 1_555 1_555 no C(4) C(3) H(2) 118.9 . 1_555 1_555 no C(3) C(4) C(5) 119.6(5) . 1_555 1_555 yes C(3) C(4) H(3) 121.6 . 1_555 1_555 no C(5) C(4) H(3) 118.8 . 1_555 1_555 no C(4) C(5) C(6) 121.5(5) . 1_555 1_555 yes C(4) C(5) H(4) 122.4 . 1_555 1_555 no C(6) C(5) H(4) 116.0 . 1_555 1_555 no C(1) C(6) C(5) 118.7(5) . 1_555 1_555 yes C(1) C(6) C(7) 125.3(5) . 1_555 1_555 yes C(5) C(6) C(7) 116.0(5) . 1_555 1_555 yes N(3) C(7) C(6) 128.1(5) . 1_555 1_555 yes N(3) C(7) H(5) 106.9 . 1_555 1_555 no C(6) C(7) H(5) 124.9 . 1_555 1_555 no N(4) C(8) C(14) 127.4(4) . 1_555 1_555 yes N(4) C(8) H(7) 120.7 . 1_555 1_555 no C(14) C(8) H(7) 111.8 . 1_555 1_555 no N(2) C(9) C(10) 123.8(4) . 1_555 1_555 yes N(2) C(9) C(14) 118.6(4) . 1_555 1_555 yes C(10) C(9) C(14) 117.6(4) . 1_555 1_555 yes C(9) C(10) C(11) 121.5(5) . 1_555 1_555 yes C(9) C(10) H(11) 121.0 . 1_555 1_555 no C(11) C(10) H(11) 116.8 . 1_555 1_555 no C(10) C(11) C(12) 120.8(5) . 1_555 1_555 yes C(10) C(11) H(10) 119.0 . 1_555 1_555 no C(12) C(11) H(10) 120.1 . 1_555 1_555 no C(11) C(12) C(13) 119.4(5) . 1_555 1_555 yes C(11) C(12) H(9) 126.0 . 1_555 1_555 no C(13) C(12) H(9) 114.6 . 1_555 1_555 no C(12) C(13) C(14) 121.6(5) . 1_555 1_555 yes C(12) C(13) H(8) 124.5 . 1_555 1_555 no C(14) C(13) H(8) 113.9 . 1_555 1_555 no C(8) C(14) C(9) 126.0(4) . 1_555 1_555 yes C(8) C(14) C(13) 115.0(4) . 1_555 1_555 yes C(9) C(14) C(13) 119.0(5) . 1_555 1_555 yes O(1) C(15) N(1) 128.3(4) . 1_555 1_555 yes O(1) C(15) C(16) 115.9(4) . 1_555 1_555 yes N(1) C(15) C(16) 115.8(4) . 1_555 1_555 yes O(2) C(16) N(2) 128.8(4) . 1_555 1_555 yes O(2) C(16) C(15) 115.7(4) . 1_555 1_555 yes N(2) C(16) C(15) 115.5(4) . 1_555 1_555 yes O(5) C(17) N(5) 125.5(5) . 1_555 1_555 yes O(5) C(17) H(12) 113.6 . 1_555 1_555 no N(5) C(17) H(12) 120.9 . 1_555 1_555 no N(5) C(18) H(13) 111.9 . 1_555 1_555 no N(5) C(18) H(14) 109.8 . 1_555 1_555 no N(5) C(18) H(15) 112.0 . 1_555 1_555 no H(13) C(18) H(14) 106.6 . 1_555 1_555 no H(13) C(18) H(15) 109.4 . 1_555 1_555 no H(14) C(18) H(15) 106.9 . 1_555 1_555 no N(5) C(19) H(16) 112.5 . 1_555 1_555 no N(5) C(19) H(17) 110.6 . 1_555 1_555 no N(5) C(19) H(18) 111.4 . 1_555 1_555 no H(16) C(19) H(17) 107.5 . 1_555 1_555 no H(16) C(19) H(18) 108.3 . 1_555 1_555 no H(17) C(19) H(18) 106.3 . 1_555 1_555 no O(6) C(20) N(6) 125.1(5) . 1_555 1_555 yes O(6) C(20) H(19) 118.1 . 1_555 1_555 no N(6) C(20) H(19) 116.8 . 1_555 1_555 no N(6) C(21) H(20) 111.3 . 1_555 1_555 no N(6) C(21) H(21) 111.0 . 1_555 1_555 no N(6) C(21) H(22) 112.3 . 1_555 1_555 no H(20) C(21) H(21) 106.4 . 1_555 1_555 no H(20) C(21) H(22) 107.9 . 1_555 1_555 no H(21) C(21) H(22) 107.6 . 1_555 1_555 no N(6) C(22) H(23) 112.0 . 1_555 1_555 no N(6) C(22) H(24) 111.9 . 1_555 1_555 no N(6) C(22) H(25) 110.8 . 1_555 1_555 no H(23) C(22) H(24) 108.1 . 1_555 1_555 no H(23) C(22) H(25) 106.8 . 1_555 1_555 no H(24) C(22) H(25) 106.9 . 1_555 1_555 no data_Co[Cu(HL)]2_4DMF #(2) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C44 H50 Co Cu2 N12 O12 ' _chemical_formula_moiety 'C44 H50 Co Cu2 N12 O12 ' _chemical_formula_weight 1124.98 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 24.903(5) _cell_length_b 10.222(4) _cell_length_c 19.569(6) _cell_angle_alpha 90 _cell_angle_beta 103.87(2) _cell_angle_gamma 90 _cell_volume 4836(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.3 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'browm' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 0.879 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6044 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.28 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5562 _reflns_number_gt 2831 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.0583 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2831 _refine_ls_number_parameters 321 _refine_ls_goodness_of_fit_ref 1.640 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.5020 _refine_diff_density_max 0.35 _refine_diff_density_min -0.62 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Co' 'Co' 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.12244(3) 0.04367(7) 0.47891(3) 0.0376(2) Uani 1.00 d . . . Co(1) Co 0.0000 -0.2212(1) 0.2500 0.0537(4) Uani 1.00 d S . . O(1) O 0.0647(2) -0.0755(4) 0.2819(2) 0.049(1) Uani 1.00 d . . . O(2) O 0.0115(1) -0.2006(4) 0.3626(2) 0.044(1) Uani 1.00 d . . . O(3) O 0.1645(2) 0.3044(4) 0.5257(2) 0.072(2) Uani 1.00 d . . . O(4) O 0.1351(2) 0.1788(5) 0.6129(2) 0.068(2) Uani 1.00 d . . . O(5) O 0.2044(2) -0.0704(5) 0.5343(2) 0.065(2) Uani 1.00 d . . . O(6) O 0.0605(2) -0.3724(5) 0.2501(2) 0.071(2) Uani 1.00 d . . . N(1) N 0.1253(2) 0.0088(4) 0.3799(2) 0.036(1) Uani 1.00 d . . . N(2) N 0.0666(2) -0.1006(4) 0.4619(2) 0.035(1) Uani 1.00 d . . . N(3) N 0.1626(2) 0.2126(5) 0.4751(3) 0.050(2) Uani 1.00 d . . . N(4) N 0.1092(2) 0.0774(5) 0.5736(2) 0.046(1) Uani 1.00 d . . . N(5) N 0.2950(2) -0.1217(5) 0.5551(3) 0.054(2) Uani 1.00 d . . . N(6) N 0.1084(2) -0.5109(5) 0.1992(3) 0.058(2) Uani 1.00 d . . . C(1) C 0.1638(2) 0.0592(6) 0.3426(3) 0.041(2) Uani 1.00 d . . . C(2) C 0.1729(2) -0.0036(6) 0.2822(3) 0.051(2) Uani 1.00 d . . . C(3) C 0.2116(3) 0.0448(8) 0.2491(4) 0.068(2) Uani 1.00 d . . . C(4) C 0.2426(3) 0.1530(9) 0.2757(4) 0.077(3) Uani 1.00 d . . . C(5) C 0.2352(3) 0.2138(7) 0.3339(4) 0.063(2) Uani 1.00 d . . . C(6) C 0.1955(2) 0.1685(6) 0.3695(3) 0.047(2) Uani 1.00 d . . . C(7) C 0.1903(3) 0.2437(6) 0.4305(4) 0.058(2) Uani 1.00 d . . . C(8) C 0.0801(2) 0.0071(6) 0.6051(3) 0.045(2) Uani 1.00 d . . . C(9) C 0.0415(2) -0.1639(6) 0.5114(3) 0.038(2) Uani 1.00 d . . . C(10) C 0.0109(3) -0.2779(6) 0.4968(3) 0.052(2) Uani 1.00 d . . . C(11) C -0.0146(3) -0.3350(7) 0.5460(4) 0.066(2) Uani 1.00 d . . . C(12) C -0.0083(3) -0.2785(8) 0.6108(4) 0.065(2) Uani 1.00 d . . . C(13) C 0.0224(3) -0.1686(7) 0.6270(3) 0.054(2) Uani 1.00 d . . . C(14) C 0.0485(2) -0.1081(6) 0.5790(3) 0.040(2) Uani 1.00 d . . . C(15) C 0.0823(2) -0.0588(5) 0.3468(3) 0.037(2) Uani 1.00 d . . . C(16) C 0.0491(2) -0.1265(5) 0.3937(3) 0.034(1) Uani 1.00 d . . . C(17) C 0.2487(3) -0.0663(6) 0.5194(3) 0.054(2) Uani 1.00 d . . . C(18) C 0.2961(3) -0.1978(9) 0.6163(4) 0.091(3) Uani 1.00 d . . . C(19) C 0.3469(3) -0.1129(9) 0.5344(6) 0.108(4) Uani 1.00 d . . . C(20) C 0.0811(3) -0.4032(7) 0.2016(4) 0.060(2) Uani 1.00 d . . . C(21) C 0.1156(4) -0.6040(9) 0.2557(5) 0.108(4) Uani 1.00 d . . . C(22) C 0.1306(3) -0.5452(8) 0.1396(4) 0.086(3) Uani 1.00 d . . . H(1) H 0.1481 -0.0839 0.2649 0.0712 Uiso 1.00 calc . . . H(2) H 0.2194 0.0000 0.1970 0.0712 Uiso 1.00 calc . . . H(3) H 0.2718 0.1637 0.2512 0.0712 Uiso 1.00 calc . . . H(4) H 0.2631 0.2883 0.3542 0.0712 Uiso 1.00 calc . . . H(5) H 0.2059 0.3412 0.4367 0.0712 Uiso 1.00 calc . . . H(6) H 0.1471 0.2505 0.5781 0.0712 Uiso 1.00 calc . . . H(7) H 0.0777 0.0335 0.6570 0.0712 Uiso 1.00 calc . . . H(8) H 0.0282 -0.1198 0.6741 0.0712 Uiso 1.00 calc . . . H(9) H -0.0232 -0.3394 0.6457 0.0712 Uiso 1.00 calc . . . H(10) H -0.0348 -0.4325 0.5211 0.0712 Uiso 1.00 calc . . . H(11) H 0.0019 -0.3154 0.4480 0.0712 Uiso 1.00 calc . . . H(12) H 0.2559 -0.0048 0.4822 0.0712 Uiso 1.00 calc . . . H(13) H 0.2844 -0.1503 0.6514 0.1038 Uiso 1.00 calc . . . H(14) H 0.2710 -0.2732 0.6039 0.1038 Uiso 1.00 calc . . . H(15) H 0.3320 -0.2337 0.6355 0.1038 Uiso 1.00 calc . . . H(16) H 0.3756 -0.1606 0.5667 0.1243 Uiso 1.00 calc . . . H(17) H 0.3435 -0.1520 0.4885 0.1243 Uiso 1.00 calc . . . H(18) H 0.3586 -0.0253 0.5325 0.1243 Uiso 1.00 calc . . . H(19) H 0.0717 -0.3584 0.1475 0.0712 Uiso 1.00 calc . . . H(20) H 0.0803 -0.6368 0.2608 0.1223 Uiso 1.00 calc . . . H(21) H 0.1368 -0.6786 0.2473 0.1223 Uiso 1.00 calc . . . H(22) H 0.1342 -0.5665 0.2998 0.1223 Uiso 1.00 calc . . . H(23) H 0.1500 -0.6259 0.1465 0.1026 Uiso 1.00 calc . . . H(24) H 0.1021 -0.5499 0.0971 0.1026 Uiso 1.00 calc . . . H(25) H 0.1566 -0.4782 0.1322 0.1026 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0403(4) 0.0400(4) 0.0329(4) -0.0018(3) 0.0095(3) -0.0011(3) Co(1) 0.0555(7) 0.0659(8) 0.0377(7) 0.0000 0.0071(6) 0.0000 O(1) 0.046(2) 0.069(3) 0.030(2) -0.012(2) 0.007(2) 0.005(2) O(2) 0.045(2) 0.057(3) 0.031(2) -0.012(2) 0.010(2) -0.004(2) O(3) 0.113(4) 0.049(3) 0.057(3) -0.021(3) 0.024(3) -0.014(2) O(4) 0.087(3) 0.070(3) 0.052(3) -0.029(3) 0.029(2) -0.025(2) O(5) 0.048(3) 0.073(3) 0.075(3) 0.015(2) 0.015(2) 0.005(3) O(6) 0.084(3) 0.078(3) 0.055(3) 0.032(3) 0.023(3) 0.012(3) N(1) 0.036(2) 0.042(3) 0.032(2) -0.004(2) 0.009(2) 0.002(2) N(2) 0.035(2) 0.040(3) 0.029(2) 0.000(2) 0.007(2) 0.000(2) N(3) 0.060(3) 0.042(3) 0.045(3) -0.007(3) 0.007(3) -0.005(2) N(4) 0.047(3) 0.051(3) 0.037(3) -0.003(2) 0.009(2) -0.010(2) N(5) 0.055(3) 0.043(3) 0.067(4) 0.014(3) 0.023(3) 0.011(3) N(6) 0.063(3) 0.055(3) 0.057(3) 0.008(3) 0.014(3) 0.002(3) C(1) 0.036(3) 0.047(4) 0.041(3) 0.001(3) 0.009(2) 0.016(3) C(2) 0.050(4) 0.064(4) 0.045(4) 0.000(3) 0.020(3) 0.007(3) C(3) 0.063(4) 0.084(5) 0.065(5) -0.003(4) 0.034(4) 0.010(4) C(4) 0.059(5) 0.105(7) 0.080(6) -0.002(5) 0.042(4) 0.021(5) C(5) 0.046(4) 0.070(5) 0.071(5) -0.014(4) 0.013(3) 0.022(4) C(6) 0.046(3) 0.048(4) 0.048(4) -0.008(3) 0.009(3) 0.009(3) C(7) 0.064(4) 0.045(4) 0.061(4) -0.017(3) 0.008(3) 0.008(3) C(8) 0.048(3) 0.056(4) 0.034(3) 0.003(3) 0.016(3) -0.003(3) C(9) 0.036(3) 0.043(3) 0.034(3) 0.004(3) 0.006(2) 0.009(3) C(10) 0.060(4) 0.056(4) 0.039(3) -0.016(3) 0.011(3) 0.005(3) C(11) 0.074(5) 0.065(5) 0.056(4) -0.024(4) 0.015(4) 0.011(4) C(12) 0.071(5) 0.079(5) 0.054(4) -0.011(4) 0.030(4) 0.014(4) C(13) 0.058(4) 0.067(4) 0.043(4) 0.008(4) 0.025(3) 0.007(3) C(14) 0.039(3) 0.049(4) 0.035(3) 0.010(3) 0.013(2) 0.008(3) C(15) 0.036(3) 0.039(3) 0.034(3) 0.002(3) 0.007(2) 0.000(3) C(16) 0.032(3) 0.038(3) 0.031(3) 0.006(3) 0.007(2) 0.004(2) C(17) 0.062(4) 0.042(4) 0.057(4) 0.007(3) 0.013(3) 0.004(3) C(18) 0.084(6) 0.123(7) 0.069(5) 0.025(6) 0.024(4) 0.025(5) C(19) 0.078(6) 0.091(7) 0.177(10) 0.028(5) 0.073(6) 0.043(7) C(20) 0.066(5) 0.061(4) 0.053(4) 0.004(4) 0.013(4) 0.008(4) C(21) 0.155(9) 0.084(6) 0.083(6) 0.047(6) 0.027(6) 0.029(5) C(22) 0.089(6) 0.086(6) 0.088(6) 0.007(5) 0.035(5) -0.011(5) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Cu(1) O(5) 2.375(4) . . yes Cu(1) N(1) 1.988(4) . . yes Cu(1) N(2) 1.999(4) . . yes Cu(1) N(3) 2.007(5) . . yes Cu(1) N(4) 1.989(5) . . yes Co(1) O(1) 2.173(4) . . yes Co(1) O(1) 2.173(4) . 2_555 yes Co(1) O(2) 2.162(3) . . yes Co(1) O(2) 2.162(3) . 2_555 yes Co(1) O(6) 2.159(5) . . yes Co(1) O(6) 2.159(5) . 2_555 yes O(1) C(15) 1.251(6) . . yes O(2) C(16) 1.245(6) . . yes O(3) N(3) 1.357(6) . . yes O(4) N(4) 1.357(6) . . yes O(4) H(6) 1.090 . . no O(5) C(17) 1.207(7) . . yes O(6) C(20) 1.223(7) . . yes N(1) C(1) 1.433(6) . . yes N(1) C(15) 1.309(6) . . yes N(2) C(9) 1.427(6) . . yes N(2) C(16) 1.328(6) . . yes N(3) C(7) 1.274(7) . . yes N(4) C(8) 1.278(7) . . yes N(5) C(17) 1.324(8) . . yes N(5) C(18) 1.423(8) . . yes N(5) C(19) 1.447(9) . . yes N(6) C(20) 1.300(8) . . yes N(6) C(21) 1.437(9) . . yes N(6) C(22) 1.449(9) . . yes C(1) C(2) 1.410(8) . . yes C(1) C(6) 1.396(8) . . yes C(2) C(3) 1.376(8) . . yes C(2) H(1) 1.033 . . no C(3) C(4) 1.38(1) . . yes C(3) H(2) 1.175 . . no C(4) C(5) 1.349(10) . . yes C(4) H(3) 0.967 . . no C(5) C(6) 1.416(8) . . yes C(5) H(4) 1.043 . . no C(6) C(7) 1.453(9) . . yes C(7) H(5) 1.065 . . no C(8) C(14) 1.440(8) . . yes C(8) H(7) 1.067 . . no C(9) C(10) 1.384(8) . . yes C(9) C(14) 1.414(7) . . yes C(10) C(11) 1.400(8) . . yes C(10) H(11) 1.003 . . no C(11) C(12) 1.369(9) . . yes C(11) H(10) 1.168 . . no C(12) C(13) 1.353(9) . . yes C(12) H(9) 1.055 . . no C(13) C(14) 1.407(8) . . yes C(13) H(8) 1.027 . . no C(15) C(16) 1.538(7) . . yes C(17) H(12) 1.010 . . no C(18) H(13) 0.943 . . no C(18) H(14) 0.985 . . no C(18) H(15) 0.957 . . no C(19) H(16) 0.967 . . no C(19) H(17) 0.969 . . no C(19) H(18) 0.946 . . no C(20) H(19) 1.125 . . no C(21) H(20) 0.968 . . no C(21) H(21) 0.963 . . no C(21) H(22) 0.957 . . no C(22) H(23) 0.949 . . no C(22) H(24) 0.956 . . no C(22) H(25) 0.979 . . no #------------------------------------------------------------------------------ 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 O(5) Cu(1) N(1) 97.4(2) . 1_555 1_555 yes O(5) Cu(1) N(2) 101.6(2) . 1_555 1_555 yes O(5) Cu(1) N(3) 93.3(2) . 1_555 1_555 yes O(5) Cu(1) N(4) 88.6(2) . 1_555 1_555 yes N(1) Cu(1) N(2) 83.8(2) . 1_555 1_555 yes N(1) Cu(1) N(3) 89.0(2) . 1_555 1_555 yes N(1) Cu(1) N(4) 172.7(2) . 1_555 1_555 yes N(2) Cu(1) N(3) 164.1(2) . 1_555 1_555 yes N(2) Cu(1) N(4) 91.1(2) . 1_555 1_555 yes N(3) Cu(1) N(4) 94.7(2) . 1_555 1_555 yes O(1) Co(1) O(1) 93.5(2) . 1_555 2_555 yes O(1) Co(1) O(2) 74.5(1) . 1_555 1_555 yes O(1) Co(1) O(2) 97.7(1) . 1_555 2_555 yes O(1) Co(1) O(6) 91.2(2) . 1_555 1_555 yes O(1) Co(1) O(6) 163.8(1) . 1_555 2_555 yes O(1) Co(1) O(2) 97.7(1) . 2_555 1_555 yes O(1) Co(1) O(2) 74.5(1) . 2_555 2_555 yes O(1) Co(1) O(6) 163.8(1) . 2_555 1_555 yes O(1) Co(1) O(6) 91.2(2) . 2_555 2_555 yes O(2) Co(1) O(2) 168.8(2) . 1_555 2_555 yes O(2) Co(1) O(6) 98.4(2) . 1_555 1_555 yes O(2) Co(1) O(6) 89.6(2) . 1_555 2_555 yes O(2) Co(1) O(6) 89.6(2) . 2_555 1_555 yes O(2) Co(1) O(6) 98.4(2) . 2_555 2_555 yes O(6) Co(1) O(6) 88.5(3) . 1_555 2_555 yes Co(1) O(1) C(15) 116.1(3) . 1_555 1_555 yes Co(1) O(2) C(16) 117.2(3) . 1_555 1_555 yes N(4) O(4) H(6) 108.9 . 1_555 1_555 no Cu(1) O(5) C(17) 127.4(4) . 1_555 1_555 yes Co(1) O(6) C(20) 127.3(5) . 1_555 1_555 yes Cu(1) N(1) C(1) 128.1(4) . 1_555 1_555 yes Cu(1) N(1) C(15) 111.2(3) . 1_555 1_555 yes C(1) N(1) C(15) 120.4(5) . 1_555 1_555 yes Cu(1) N(2) C(9) 128.4(3) . 1_555 1_555 yes Cu(1) N(2) C(16) 111.2(3) . 1_555 1_555 yes C(9) N(2) C(16) 120.0(4) . 1_555 1_555 yes Cu(1) N(3) O(3) 119.9(4) . 1_555 1_555 yes Cu(1) N(3) C(7) 126.6(4) . 1_555 1_555 yes O(3) N(3) C(7) 113.4(5) . 1_555 1_555 yes Cu(1) N(4) O(4) 119.8(4) . 1_555 1_555 yes Cu(1) N(4) C(8) 126.2(4) . 1_555 1_555 yes O(4) N(4) C(8) 113.8(5) . 1_555 1_555 yes C(17) N(5) C(18) 121.1(6) . 1_555 1_555 yes C(17) N(5) C(19) 123.3(6) . 1_555 1_555 yes C(18) N(5) C(19) 115.6(6) . 1_555 1_555 yes C(20) N(6) C(21) 120.3(6) . 1_555 1_555 yes C(20) N(6) C(22) 122.5(6) . 1_555 1_555 yes C(21) N(6) C(22) 117.2(6) . 1_555 1_555 yes N(1) C(1) C(2) 121.7(5) . 1_555 1_555 yes N(1) C(1) C(6) 118.8(5) . 1_555 1_555 yes C(2) C(1) C(6) 119.4(5) . 1_555 1_555 yes C(1) C(2) C(3) 120.2(6) . 1_555 1_555 yes C(1) C(2) H(1) 115.6 . 1_555 1_555 no C(3) C(2) H(1) 124.2 . 1_555 1_555 no C(2) C(3) C(4) 120.2(7) . 1_555 1_555 yes C(2) C(3) H(2) 123.2 . 1_555 1_555 no C(4) C(3) H(2) 116.6 . 1_555 1_555 no C(3) C(4) C(5) 120.8(6) . 1_555 1_555 yes C(3) C(4) H(3) 108.8 . 1_555 1_555 no C(5) C(4) H(3) 129.6 . 1_555 1_555 no C(4) C(5) C(6) 121.2(7) . 1_555 1_555 yes C(4) C(5) H(4) 116.3 . 1_555 1_555 no C(6) C(5) H(4) 122.2 . 1_555 1_555 no C(1) C(6) C(5) 118.4(6) . 1_555 1_555 yes C(1) C(6) C(7) 125.4(5) . 1_555 1_555 yes C(5) C(6) C(7) 116.2(6) . 1_555 1_555 yes N(3) C(7) C(6) 126.9(6) . 1_555 1_555 yes N(3) C(7) H(5) 113.4 . 1_555 1_555 no C(6) C(7) H(5) 119.1 . 1_555 1_555 no N(4) C(8) C(14) 127.8(5) . 1_555 1_555 yes N(4) C(8) H(7) 119.0 . 1_555 1_555 no C(14) C(8) H(7) 113.2 . 1_555 1_555 no N(2) C(9) C(10) 123.5(5) . 1_555 1_555 yes N(2) C(9) C(14) 118.5(5) . 1_555 1_555 yes C(10) C(9) C(14) 118.1(5) . 1_555 1_555 yes C(9) C(10) C(11) 121.9(6) . 1_555 1_555 yes C(9) C(10) H(11) 120.3 . 1_555 1_555 no C(11) C(10) H(11) 117.3 . 1_555 1_555 no C(10) C(11) C(12) 119.3(6) . 1_555 1_555 yes C(10) C(11) H(10) 106.9 . 1_555 1_555 no C(12) C(11) H(10) 133.5 . 1_555 1_555 no C(11) C(12) C(13) 120.0(6) . 1_555 1_555 yes C(11) C(12) H(9) 111.7 . 1_555 1_555 no C(13) C(12) H(9) 127.2 . 1_555 1_555 no C(12) C(13) C(14) 122.3(6) . 1_555 1_555 yes C(12) C(13) H(8) 124.3 . 1_555 1_555 no C(14) C(13) H(8) 113.4 . 1_555 1_555 no C(8) C(14) C(9) 126.6(5) . 1_555 1_555 yes C(8) C(14) C(13) 115.1(5) . 1_555 1_555 yes C(9) C(14) C(13) 118.3(6) . 1_555 1_555 yes O(1) C(15) N(1) 128.4(5) . 1_555 1_555 yes O(1) C(15) C(16) 115.9(5) . 1_555 1_555 yes N(1) C(15) C(16) 115.8(5) . 1_555 1_555 yes O(2) C(16) N(2) 129.8(5) . 1_555 1_555 yes O(2) C(16) C(15) 115.5(5) . 1_555 1_555 yes N(2) C(16) C(15) 114.6(5) . 1_555 1_555 yes O(5) C(17) N(5) 125.9(6) . 1_555 1_555 yes O(5) C(17) H(12) 121.9 . 1_555 1_555 no N(5) C(17) H(12) 111.3 . 1_555 1_555 no N(5) C(18) H(13) 112.7 . 1_555 1_555 no N(5) C(18) H(14) 109.7 . 1_555 1_555 no N(5) C(18) H(15) 111.6 . 1_555 1_555 no H(13) C(18) H(14) 107.1 . 1_555 1_555 no H(13) C(18) H(15) 109.4 . 1_555 1_555 no H(14) C(18) H(15) 106.0 . 1_555 1_555 no N(5) C(19) H(16) 110.9 . 1_555 1_555 no N(5) C(19) H(17) 110.4 . 1_555 1_555 no N(5) C(19) H(18) 112.1 . 1_555 1_555 no H(16) C(19) H(17) 106.6 . 1_555 1_555 no H(16) C(19) H(18) 108.4 . 1_555 1_555 no H(17) C(19) H(18) 108.3 . 1_555 1_555 no O(6) C(20) N(6) 124.4(7) . 1_555 1_555 yes O(6) C(20) H(19) 126.4 . 1_555 1_555 no N(6) C(20) H(19) 107.7 . 1_555 1_555 no N(6) C(21) H(20) 111.0 . 1_555 1_555 no N(6) C(21) H(21) 111.5 . 1_555 1_555 no N(6) C(21) H(22) 111.9 . 1_555 1_555 no H(20) C(21) H(21) 106.9 . 1_555 1_555 no H(20) C(21) H(22) 107.4 . 1_555 1_555 no H(21) C(21) H(22) 107.8 . 1_555 1_555 no N(6) C(22) H(23) 112.1 . 1_555 1_555 no N(6) C(22) H(24) 111.4 . 1_555 1_555 no N(6) C(22) H(25) 110.1 . 1_555 1_555 no H(23) C(22) H(24) 109.1 . 1_555 1_555 no H(23) C(22) H(25) 107.2 . 1_555 1_555 no H(24) C(22) H(25) 106.7 . 1_555 1_555 no data_Ni[Cu(HL)]2_4DMF #(3) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C44 H50 Cu2 N12 O12 Ni ' _chemical_formula_moiety 'C44 H50 Cu2 N12 O12 Ni ' _chemical_formula_weight 1124.74 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 24.86(1) _cell_length_b 10.279(3) _cell_length_c 19.373(5) _cell_angle_alpha 90 _cell_angle_beta 104.86(3) _cell_angle_gamma 90 _cell_volume 4784(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 11.4 _cell_measurement_theta_max 12.2 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.345 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.994 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5627 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9989 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 10.85 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5498 _reflns_number_gt 1537 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.0681 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1537 _refine_ls_number_parameters 321 _refine_ls_goodness_of_fit_ref 1.810 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.2858 _refine_diff_density_max 0.50 _refine_diff_density_min -0.57 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.12279(7) 0.0433(2) 0.47592(9) 0.0420(5) Uani 1.00 d . . . Ni(1) Ni 0.0000 -0.2109(3) 0.2500 0.0404(8) Uani 1.00 d S . . O(1) O 0.0625(3) -0.0753(10) 0.2759(4) 0.046(3) Uani 1.00 d . . . O(2) O 0.0105(3) -0.2000(10) 0.3568(4) 0.043(3) Uani 1.00 d . . . O(3) O 0.1665(5) 0.301(1) 0.5244(5) 0.077(4) Uani 1.00 d . . . O(4) O 0.1331(4) 0.181(1) 0.6099(5) 0.068(4) Uani 1.00 d . . . O(5) O 0.2061(4) -0.067(1) 0.5351(5) 0.065(4) Uani 1.00 d . . . O(6) O 0.0569(4) -0.357(1) 0.2597(5) 0.065(4) Uani 1.00 d . . . N(1) N 0.1244(4) 0.010(1) 0.3752(5) 0.040(4) Uani 1.00 d . . . N(2) N 0.0672(4) -0.100(1) 0.4586(6) 0.034(3) Uani 1.00 d . . . N(3) N 0.1630(5) 0.212(1) 0.4737(7) 0.053(4) Uani 1.00 d . . . N(4) N 0.1083(5) 0.078(1) 0.5708(6) 0.043(4) Uani 1.00 d . . . N(5) N 0.2964(5) -0.121(1) 0.5494(7) 0.057(5) Uani 1.00 d . . . N(6) N 0.1052(5) -0.494(1) 0.2076(6) 0.054(5) Uani 1.00 d . . . C(1) C 0.1635(5) 0.060(2) 0.3382(7) 0.042(5) Uani 1.00 d . . . C(2) C 0.1719(6) -0.001(2) 0.2767(8) 0.060(6) Uani 1.00 d . . . C(3) C 0.2092(7) 0.046(2) 0.2425(9) 0.074(7) Uani 1.00 d . . . C(4) C 0.2406(7) 0.154(2) 0.2681(9) 0.072(7) Uani 1.00 d . . . C(5) C 0.2339(6) 0.210(2) 0.3285(8) 0.064(6) Uani 1.00 d . . . C(6) C 0.1944(6) 0.170(2) 0.3638(8) 0.049(5) Uani 1.00 d . . . C(7) C 0.1908(6) 0.242(1) 0.4260(9) 0.051(5) Uani 1.00 d . . . C(8) C 0.0787(6) 0.011(2) 0.6003(7) 0.047(5) Uani 1.00 d . . . C(9) C 0.0420(5) -0.165(1) 0.5076(8) 0.041(5) Uani 1.00 d . . . C(10) C 0.0131(6) -0.279(2) 0.4928(7) 0.046(5) Uani 1.00 d . . . C(11) C -0.0130(7) -0.333(2) 0.5416(9) 0.069(6) Uani 1.00 d . . . C(12) C -0.0071(7) -0.274(2) 0.6083(8) 0.063(6) Uani 1.00 d . . . C(13) C 0.0223(6) -0.168(2) 0.6230(7) 0.050(5) Uani 1.00 d . . . C(14) C 0.0489(5) -0.109(2) 0.5768(7) 0.038(4) Uani 1.00 d . . . C(15) C 0.0808(5) -0.056(2) 0.3424(7) 0.040(4) Uani 1.00 d . . . C(16) C 0.0485(6) -0.123(1) 0.3886(8) 0.040(5) Uani 1.00 d . . . C(17) C 0.2487(7) -0.063(2) 0.5159(8) 0.063(6) Uani 1.00 d . . . C(18) C 0.2984(7) -0.200(2) 0.6111(9) 0.093(7) Uani 1.00 d . . . C(19) C 0.3459(7) -0.113(2) 0.524(1) 0.114(9) Uani 1.00 d . . . C(20) C 0.0783(6) -0.385(2) 0.2105(9) 0.056(6) Uani 1.00 d . . . C(21) C 0.1112(9) -0.591(2) 0.2626(10) 0.106(8) Uani 1.00 d . . . C(22) C 0.1278(6) -0.524(2) 0.1466(8) 0.079(7) Uani 1.00 d . . . H(1) H 0.1496 -0.0803 0.2583 0.0717 Uiso 1.00 calc . . . H(2) H 0.2146 0.0015 0.2002 0.0877 Uiso 1.00 calc . . . H(3) H 0.2665 0.1904 0.2434 0.0833 Uiso 1.00 calc . . . H(4) H 0.2572 0.2857 0.3485 0.0811 Uiso 1.00 calc . . . H(5) H 0.2121 0.3247 0.4338 0.0588 Uiso 1.00 calc . . . H(6) H 0.1488 0.2681 0.5864 0.0648 Uiso 1.00 calc . . . H(7) H 0.0746 0.0450 0.6463 0.0543 Uiso 1.00 calc . . . H(8) H 0.0263 -0.1286 0.6700 0.0598 Uiso 1.00 calc . . . H(9) H -0.0263 -0.3110 0.6415 0.0697 Uiso 1.00 calc . . . H(10) H -0.0343 -0.4123 0.5294 0.0739 Uiso 1.00 calc . . . H(11) H 0.0115 -0.3234 0.4478 0.0547 Uiso 1.00 calc . . . H(12) H 0.2501 -0.0133 0.4722 0.0720 Uiso 1.00 calc . . . H(13) H 0.2880 -0.1538 0.6488 0.0991 Uiso 1.00 calc . . . H(14) H 0.2731 -0.2743 0.5993 0.0991 Uiso 1.00 calc . . . H(15) H 0.3350 -0.2372 0.6316 0.0991 Uiso 1.00 calc . . . H(16) H 0.3578 -0.0246 0.5233 0.1243 Uiso 1.00 calc . . . H(17) H 0.3403 -0.1499 0.4785 0.1243 Uiso 1.00 calc . . . H(18) H 0.3766 -0.1597 0.5565 0.1243 Uiso 1.00 calc . . . H(19) H 0.0756 -0.3220 0.1714 0.0639 Uiso 1.00 calc . . . H(20) H 0.0767 -0.6216 0.2688 0.1131 Uiso 1.00 calc . . . H(21) H 0.1324 -0.5573 0.3089 0.1131 Uiso 1.00 calc . . . H(22) H 0.1321 -0.6666 0.2535 0.1131 Uiso 1.00 calc . . . H(23) H 0.1467 -0.6055 0.1521 0.0910 Uiso 1.00 calc . . . H(24) H 0.0997 -0.5237 0.1030 0.0910 Uiso 1.00 calc . . . H(25) H 0.1551 -0.4577 0.1427 0.0910 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.040(1) 0.050(1) 0.034(1) -0.002(1) 0.0064(8) -0.002(1) Ni(1) 0.036(2) 0.058(2) 0.023(1) 0.0000 0.001(1) 0.0000 O(1) 0.043(6) 0.078(9) 0.018(5) -0.006(5) 0.008(4) 0.013(5) O(2) 0.040(6) 0.054(7) 0.035(6) -0.011(6) 0.008(5) 0.003(5) O(3) 0.106(9) 0.064(9) 0.061(8) -0.026(7) 0.021(7) -0.019(7) O(4) 0.075(7) 0.065(8) 0.064(7) -0.027(7) 0.020(6) -0.036(6) O(5) 0.043(6) 0.081(9) 0.073(8) 0.022(7) 0.016(6) 0.011(7) O(6) 0.067(8) 0.095(10) 0.028(6) 0.017(7) 0.002(5) 0.003(6) N(1) 0.038(7) 0.049(9) 0.036(7) -0.008(6) 0.016(6) -0.002(6) N(2) 0.036(7) 0.039(8) 0.026(6) -0.004(6) 0.004(5) -0.008(6) N(3) 0.058(8) 0.033(8) 0.054(9) -0.008(7) -0.012(7) -0.009(7) N(4) 0.043(8) 0.049(10) 0.039(8) 0.001(7) 0.011(6) 0.003(7) N(5) 0.058(9) 0.037(9) 0.08(1) 0.011(7) 0.022(8) 0.002(8) N(6) 0.056(9) 0.06(1) 0.043(8) 0.009(8) 0.002(7) 0.006(7) C(1) 0.025(8) 0.05(1) 0.047(9) 0.010(9) 0.009(7) 0.018(9) C(2) 0.046(9) 0.09(2) 0.046(10) -0.001(10) 0.019(8) 0.006(9) C(3) 0.07(1) 0.10(2) 0.07(1) -0.01(1) 0.031(10) 0.02(1) C(4) 0.07(1) 0.12(2) 0.04(1) -0.01(1) 0.035(9) 0.02(1) C(5) 0.036(9) 0.10(2) 0.06(1) -0.01(1) 0.015(8) 0.03(1) C(6) 0.037(9) 0.06(1) 0.047(10) -0.001(9) 0.006(8) 0.017(9) C(7) 0.06(1) 0.04(1) 0.05(1) -0.020(8) 0.004(9) 0.005(8) C(8) 0.041(9) 0.06(1) 0.036(9) 0.006(9) 0.005(7) -0.005(8) C(9) 0.033(9) 0.04(1) 0.044(9) 0.004(8) -0.006(7) 0.002(8) C(10) 0.054(10) 0.05(1) 0.032(8) -0.016(9) 0.009(7) 0.005(8) C(11) 0.08(1) 0.06(1) 0.07(1) -0.032(10) 0.011(10) 0.01(1) C(12) 0.08(1) 0.07(1) 0.05(1) -0.02(1) 0.032(9) 0.01(1) C(13) 0.06(1) 0.06(1) 0.039(9) -0.003(10) 0.023(8) 0.012(9) C(14) 0.028(8) 0.05(1) 0.031(8) 0.022(8) 0.005(7) 0.005(8) C(15) 0.028(7) 0.06(1) 0.032(8) -0.001(9) 0.010(7) 0.002(9) C(16) 0.039(9) 0.04(1) 0.044(9) -0.001(8) 0.014(8) 0.006(8) C(17) 0.07(1) 0.05(1) 0.06(1) 0.03(1) 0.010(10) 0.016(10) C(18) 0.08(1) 0.12(2) 0.06(1) 0.03(1) 0.00(1) 0.01(1) C(19) 0.06(1) 0.12(2) 0.19(2) 0.04(1) 0.08(1) 0.06(2) C(20) 0.04(1) 0.04(1) 0.07(1) 0.017(9) -0.007(9) 0.02(1) C(21) 0.17(2) 0.07(2) 0.08(1) 0.04(1) 0.03(1) 0.04(1) C(22) 0.08(1) 0.11(2) 0.06(1) 0.02(1) 0.027(10) 0.00(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Cu(1) O(5) 2.382(10) . . yes Cu(1) N(1) 1.99(1) . . yes Cu(1) N(2) 1.99(1) . . yes Cu(1) N(3) 2.01(1) . . yes Cu(1) N(4) 1.99(1) . . yes Ni(1) O(1) 2.052(9) . . yes Ni(1) O(1) 2.052(9) . 2_555 yes Ni(1) O(2) 2.022(9) . . yes Ni(1) O(2) 2.022(9) . 2_555 yes Ni(1) O(6) 2.04(1) . . yes Ni(1) O(6) 2.04(1) . 2_555 yes O(1) C(15) 1.27(1) . . yes O(2) C(16) 1.26(1) . . yes O(3) N(3) 1.33(1) . . yes O(4) N(4) 1.35(1) . . yes O(4) H(6) 1.120 . . no O(5) C(17) 1.21(2) . . yes O(6) C(20) 1.24(2) . . yes N(1) C(1) 1.44(2) . . yes N(1) C(15) 1.30(2) . . yes N(2) C(9) 1.43(2) . . yes N(2) C(16) 1.34(2) . . yes N(3) C(7) 1.32(2) . . yes N(4) C(8) 1.25(2) . . yes N(5) C(17) 1.34(2) . . yes N(5) C(18) 1.44(2) . . yes N(5) C(19) 1.44(2) . . yes N(6) C(20) 1.31(2) . . yes N(6) C(21) 1.44(2) . . yes N(6) C(22) 1.47(2) . . yes C(1) C(2) 1.41(2) . . yes C(1) C(6) 1.39(2) . . yes C(2) C(3) 1.36(2) . . yes C(2) H(1) 0.995 . . no C(3) C(4) 1.37(2) . . yes C(3) H(2) 0.979 . . no C(4) C(5) 1.35(2) . . yes C(4) H(3) 0.970 . . no C(5) C(6) 1.39(2) . . yes C(5) H(4) 0.987 . . no C(6) C(7) 1.44(2) . . yes C(7) H(5) 0.992 . . no C(8) C(14) 1.45(2) . . yes C(8) H(7) 0.984 . . no C(9) C(10) 1.37(2) . . yes C(9) C(14) 1.43(2) . . yes C(10) C(11) 1.39(2) . . yes C(10) H(11) 0.976 . . no C(11) C(12) 1.40(2) . . yes C(11) H(10) 0.971 . . no C(12) C(13) 1.31(2) . . yes C(12) H(9) 0.972 . . no C(13) C(14) 1.38(2) . . yes C(13) H(8) 0.977 . . no C(15) C(16) 1.51(2) . . yes C(17) H(12) 0.995 . . no C(18) H(13) 0.962 . . no C(18) H(14) 0.975 . . no C(18) H(15) 0.971 . . no C(19) H(16) 0.955 . . no C(19) H(17) 0.941 . . no C(19) H(18) 0.981 . . no C(20) H(19) 0.985 . . no C(21) H(20) 0.948 . . no C(21) H(21) 0.981 . . no C(21) H(22) 0.975 . . no C(22) H(23) 0.950 . . no C(22) H(24) 0.948 . . no C(22) H(25) 0.981 . . no #------------------------------------------------------------------------------ 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 O(5) Cu(1) N(1) 99.1(4) . 1_555 1_555 yes O(5) Cu(1) N(2) 102.1(4) . 1_555 1_555 yes O(5) Cu(1) N(3) 92.7(4) . 1_555 1_555 yes O(5) Cu(1) N(4) 89.0(4) . 1_555 1_555 yes N(1) Cu(1) N(2) 84.0(4) . 1_555 1_555 yes N(1) Cu(1) N(3) 89.5(5) . 1_555 1_555 yes N(1) Cu(1) N(4) 171.0(5) . 1_555 1_555 yes N(2) Cu(1) N(3) 164.6(4) . 1_555 1_555 yes N(2) Cu(1) N(4) 90.4(5) . 1_555 1_555 yes N(3) Cu(1) N(4) 94.1(5) . 1_555 1_555 yes O(1) Ni(1) O(1) 94.4(5) . 1_555 2_555 yes O(1) Ni(1) O(2) 79.7(3) . 1_555 1_555 yes O(1) Ni(1) O(2) 96.0(3) . 1_555 2_555 yes O(1) Ni(1) O(6) 90.8(4) . 1_555 1_555 yes O(1) Ni(1) O(6) 170.8(4) . 1_555 2_555 yes O(1) Ni(1) O(2) 96.0(3) . 2_555 1_555 yes O(1) Ni(1) O(2) 79.7(3) . 2_555 2_555 yes O(1) Ni(1) O(6) 170.8(4) . 2_555 1_555 yes O(1) Ni(1) O(6) 90.8(4) . 2_555 2_555 yes O(2) Ni(1) O(2) 173.6(6) . 1_555 2_555 yes O(2) Ni(1) O(6) 92.4(4) . 1_555 1_555 yes O(2) Ni(1) O(6) 92.3(4) . 1_555 2_555 yes O(2) Ni(1) O(6) 92.3(4) . 2_555 1_555 yes O(2) Ni(1) O(6) 92.4(4) . 2_555 2_555 yes O(6) Ni(1) O(6) 85.1(7) . 1_555 2_555 yes Ni(1) O(1) C(15) 113.9(9) . 1_555 1_555 yes Ni(1) O(2) C(16) 114.6(9) . 1_555 1_555 yes N(4) O(4) H(6) 123.6 . 1_555 1_555 no Cu(1) O(5) C(17) 123(1) . 1_555 1_555 yes Ni(1) O(6) C(20) 121(1) . 1_555 1_555 yes Cu(1) N(1) C(1) 127.8(9) . 1_555 1_555 yes Cu(1) N(1) C(15) 110.3(9) . 1_555 1_555 yes C(1) N(1) C(15) 121(1) . 1_555 1_555 yes Cu(1) N(2) C(9) 129.6(8) . 1_555 1_555 yes Cu(1) N(2) C(16) 110.6(9) . 1_555 1_555 yes C(9) N(2) C(16) 119(1) . 1_555 1_555 yes Cu(1) N(3) O(3) 121(1) . 1_555 1_555 yes Cu(1) N(3) C(7) 124(1) . 1_555 1_555 yes O(3) N(3) C(7) 113(1) . 1_555 1_555 yes Cu(1) N(4) O(4) 119.5(9) . 1_555 1_555 yes Cu(1) N(4) C(8) 126(1) . 1_555 1_555 yes O(4) N(4) C(8) 114(1) . 1_555 1_555 yes C(17) N(5) C(18) 119(1) . 1_555 1_555 yes C(17) N(5) C(19) 122(1) . 1_555 1_555 yes C(18) N(5) C(19) 117(1) . 1_555 1_555 yes C(20) N(6) C(21) 121(1) . 1_555 1_555 yes C(20) N(6) C(22) 121(1) . 1_555 1_555 yes C(21) N(6) C(22) 117(1) . 1_555 1_555 yes N(1) C(1) C(2) 122(1) . 1_555 1_555 yes N(1) C(1) C(6) 119(1) . 1_555 1_555 yes C(2) C(1) C(6) 118(1) . 1_555 1_555 yes C(1) C(2) C(3) 121(1) . 1_555 1_555 yes C(1) C(2) H(1) 118.4 . 1_555 1_555 no C(3) C(2) H(1) 120.4 . 1_555 1_555 no C(2) C(3) C(4) 120(1) . 1_555 1_555 yes C(2) C(3) H(2) 119.5 . 1_555 1_555 no C(4) C(3) H(2) 119.7 . 1_555 1_555 no C(3) C(4) C(5) 118(1) . 1_555 1_555 yes C(3) C(4) H(3) 121.3 . 1_555 1_555 no C(5) C(4) H(3) 120.7 . 1_555 1_555 no C(4) C(5) C(6) 123(1) . 1_555 1_555 yes C(4) C(5) H(4) 119.0 . 1_555 1_555 no C(6) C(5) H(4) 117.0 . 1_555 1_555 no C(1) C(6) C(5) 117(1) . 1_555 1_555 yes C(1) C(6) C(7) 124(1) . 1_555 1_555 yes C(5) C(6) C(7) 117(1) . 1_555 1_555 yes N(3) C(7) C(6) 128(1) . 1_555 1_555 yes N(3) C(7) H(5) 116.5 . 1_555 1_555 no C(6) C(7) H(5) 114.9 . 1_555 1_555 no N(4) C(8) C(14) 129(1) . 1_555 1_555 yes N(4) C(8) H(7) 115.6 . 1_555 1_555 no C(14) C(8) H(7) 114.7 . 1_555 1_555 no N(2) C(9) C(10) 123(1) . 1_555 1_555 yes N(2) C(9) C(14) 117(1) . 1_555 1_555 yes C(10) C(9) C(14) 118(1) . 1_555 1_555 yes C(9) C(10) C(11) 120(1) . 1_555 1_555 yes C(9) C(10) H(11) 119.4 . 1_555 1_555 no C(11) C(10) H(11) 119.9 . 1_555 1_555 no C(10) C(11) C(12) 120(1) . 1_555 1_555 yes C(10) C(11) H(10) 119.4 . 1_555 1_555 no C(12) C(11) H(10) 120.5 . 1_555 1_555 no C(11) C(12) C(13) 118(1) . 1_555 1_555 yes C(11) C(12) H(9) 119.6 . 1_555 1_555 no C(13) C(12) H(9) 121.6 . 1_555 1_555 no C(12) C(13) C(14) 124(1) . 1_555 1_555 yes C(12) C(13) H(8) 117.9 . 1_555 1_555 no C(14) C(13) H(8) 118.0 . 1_555 1_555 no C(8) C(14) C(9) 124(1) . 1_555 1_555 yes C(8) C(14) C(13) 117(1) . 1_555 1_555 yes C(9) C(14) C(13) 118(1) . 1_555 1_555 yes O(1) C(15) N(1) 128(1) . 1_555 1_555 yes O(1) C(15) C(16) 115(1) . 1_555 1_555 yes N(1) C(15) C(16) 116(1) . 1_555 1_555 yes O(2) C(16) N(2) 128(1) . 1_555 1_555 yes O(2) C(16) C(15) 116(1) . 1_555 1_555 yes N(2) C(16) C(15) 114(1) . 1_555 1_555 yes O(5) C(17) N(5) 124(1) . 1_555 1_555 yes O(5) C(17) H(12) 120.3 . 1_555 1_555 no N(5) C(17) H(12) 114.9 . 1_555 1_555 no N(5) C(18) H(13) 113.0 . 1_555 1_555 no N(5) C(18) H(14) 111.4 . 1_555 1_555 no N(5) C(18) H(15) 113.0 . 1_555 1_555 no H(13) C(18) H(14) 106.5 . 1_555 1_555 no H(13) C(18) H(15) 106.7 . 1_555 1_555 no H(14) C(18) H(15) 105.7 . 1_555 1_555 no N(5) C(19) H(16) 111.1 . 1_555 1_555 no N(5) C(19) H(17) 111.2 . 1_555 1_555 no N(5) C(19) H(18) 110.3 . 1_555 1_555 no H(16) C(19) H(17) 109.9 . 1_555 1_555 no H(16) C(19) H(18) 106.6 . 1_555 1_555 no H(17) C(19) H(18) 107.6 . 1_555 1_555 no O(6) C(20) N(6) 123(1) . 1_555 1_555 yes O(6) C(20) H(19) 118.8 . 1_555 1_555 no N(6) C(20) H(19) 117.5 . 1_555 1_555 no N(6) C(21) H(20) 113.5 . 1_555 1_555 no N(6) C(21) H(21) 111.0 . 1_555 1_555 no N(6) C(21) H(22) 112.2 . 1_555 1_555 no H(20) C(21) H(21) 107.1 . 1_555 1_555 no H(20) C(21) H(22) 107.6 . 1_555 1_555 no H(21) C(21) H(22) 105.0 . 1_555 1_555 no N(6) C(22) H(23) 112.3 . 1_555 1_555 no N(6) C(22) H(24) 111.6 . 1_555 1_555 no N(6) C(22) H(25) 109.2 . 1_555 1_555 no H(23) C(22) H(24) 109.6 . 1_555 1_555 no H(23) C(22) H(25) 106.9 . 1_555 1_555 no H(24) C(22) H(25) 107.0 . 1_555 1_555 no #------------------------------------------------------------------------------ data_Zn[Cu(HL)]2_4DMF #(4) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C44 H50 Cu2 N12 O12 Zn ' _chemical_formula_moiety 'C44 H50 Cu2 N12 O12 Zn ' _chemical_formula_weight 1131.42 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 24.910(4) _cell_length_b 10.245(3) _cell_length_c 19.459(3) _cell_angle_alpha 90 _cell_angle_beta 104.72(1) _cell_angle_gamma 90 _cell_volume 4802(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.4 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.448 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5640 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9989 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.42 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5513 _reflns_number_gt 2082 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.0501 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2082 _refine_ls_number_parameters 321 _refine_ls_goodness_of_fit_ref 1.405 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_shift/su_max 0.3533 _refine_diff_density_max 0.43 _refine_diff_density_min -0.36 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Zn' 'Zn' 0.284 1.430 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn(1) Zn 0.0000 -0.2147(2) 0.2500 0.0413(4) Uani 1.00 d S . . Cu(1) Cu 0.12273(4) 0.0435(1) 0.47704(5) 0.0365(3) Uani 1.00 d . . . O(1) O 0.0638(2) -0.0754(6) 0.2779(3) 0.044(2) Uani 1.00 d . . . O(2) O 0.0104(2) -0.1993(6) 0.3584(2) 0.040(2) Uani 1.00 d . . . O(3) O 0.1652(3) 0.3045(6) 0.5243(3) 0.071(2) Uani 1.00 d . . . O(4) O 0.1343(3) 0.1799(6) 0.6111(3) 0.062(2) Uani 1.00 d . . . O(5) O 0.2056(2) -0.0681(6) 0.5345(3) 0.059(2) Uani 1.00 d . . . O(6) O 0.0583(3) -0.3638(6) 0.2561(3) 0.065(2) Uani 1.00 d . . . N(1) N 0.1251(3) 0.0090(6) 0.3772(3) 0.036(2) Uani 1.00 d . . . N(2) N 0.0665(3) -0.1014(6) 0.4595(3) 0.032(2) Uani 1.00 d . . . N(3) N 0.1635(3) 0.2122(7) 0.4742(3) 0.044(2) Uani 1.00 d . . . N(4) N 0.1085(3) 0.0774(7) 0.5714(3) 0.042(2) Uani 1.00 d . . . N(5) N 0.2962(3) -0.1203(7) 0.5521(4) 0.054(3) Uani 1.00 d . . . N(6) N 0.1060(3) -0.5007(8) 0.2032(4) 0.057(3) Uani 1.00 d . . . C(1) C 0.1637(3) 0.0594(8) 0.3405(4) 0.037(2) Uani 1.00 d . . . C(2) C 0.1723(4) -0.0015(9) 0.2797(5) 0.052(3) Uani 1.00 d . . . C(3) C 0.2110(4) 0.047(1) 0.2463(5) 0.067(3) Uani 1.00 d . . . C(4) C 0.2413(4) 0.158(1) 0.2721(6) 0.070(4) Uani 1.00 d . . . C(5) C 0.2338(4) 0.217(1) 0.3326(5) 0.058(3) Uani 1.00 d . . . C(6) C 0.1943(4) 0.1702(9) 0.3673(4) 0.044(3) Uani 1.00 d . . . C(7) C 0.1902(4) 0.2447(9) 0.4278(4) 0.049(3) Uani 1.00 d . . . C(8) C 0.0797(4) 0.0069(9) 0.6026(4) 0.044(3) Uani 1.00 d . . . C(9) C 0.0415(3) -0.1645(8) 0.5089(4) 0.037(2) Uani 1.00 d . . . C(10) C 0.0113(3) -0.2783(9) 0.4943(4) 0.044(3) Uani 1.00 d . . . C(11) C -0.0136(4) -0.3345(10) 0.5429(5) 0.063(3) Uani 1.00 d . . . C(12) C -0.0089(4) -0.277(1) 0.6077(5) 0.062(3) Uani 1.00 d . . . C(13) C 0.0217(4) -0.1657(9) 0.6241(4) 0.047(3) Uani 1.00 d . . . C(14) C 0.0484(3) -0.1099(9) 0.5765(4) 0.037(2) Uani 1.00 d . . . C(15) C 0.0814(3) -0.0591(8) 0.3433(4) 0.036(2) Uani 1.00 d . . . C(16) C 0.0493(3) -0.1264(8) 0.3903(4) 0.031(2) Uani 1.00 d . . . C(17) C 0.2491(4) -0.0644(9) 0.5171(5) 0.056(3) Uani 1.00 d . . . C(18) C 0.2978(4) -0.194(1) 0.6139(5) 0.086(4) Uani 1.00 d . . . C(19) C 0.3462(5) -0.115(1) 0.5277(7) 0.110(5) Uani 1.00 d . . . C(20) C 0.0800(4) -0.3919(10) 0.2073(5) 0.053(3) Uani 1.00 d . . . C(21) C 0.1110(6) -0.597(1) 0.2582(6) 0.106(5) Uani 1.00 d . . . C(22) C 0.1281(4) -0.533(1) 0.1433(6) 0.078(4) Uani 1.00 d . . . H(1) H 0.1502 -0.0793 0.2602 0.0645 Uiso 1.00 calc . . . H(2) H 0.2126 -0.0051 0.1999 0.0608 Uiso 1.00 calc . . . H(3) H 0.2730 0.1857 0.2492 0.0608 Uiso 1.00 calc . . . H(4) H 0.2617 0.2958 0.3518 0.0608 Uiso 1.00 calc . . . H(5) H 0.2078 0.3428 0.4352 0.0608 Uiso 1.00 calc . . . H(6) H 0.1552 0.2477 0.5653 0.0608 Uiso 1.00 calc . . . H(7) H 0.0729 0.0497 0.6527 0.0608 Uiso 1.00 calc . . . H(8) H 0.0308 -0.1196 0.6809 0.0608 Uiso 1.00 calc . . . H(9) H -0.0278 -0.3155 0.6412 0.0719 Uiso 1.00 calc . . . H(10) H -0.0343 -0.4158 0.5307 0.0739 Uiso 1.00 calc . . . H(11) H 0.0070 -0.3196 0.4480 0.0535 Uiso 1.00 calc . . . H(12) H 0.2512 -0.0162 0.4744 0.0639 Uiso 1.00 calc . . . H(13) H 0.3335 -0.2308 0.6341 0.0997 Uiso 1.00 calc . . . H(14) H 0.2869 -0.1439 0.6495 0.0997 Uiso 1.00 calc . . . H(15) H 0.2717 -0.2678 0.6028 0.0997 Uiso 1.00 calc . . . H(16) H 0.3759 -0.1632 0.5599 0.1232 Uiso 1.00 calc . . . H(17) H 0.3583 -0.0285 0.5250 0.1232 Uiso 1.00 calc . . . H(18) H 0.3405 -0.1557 0.4820 0.1232 Uiso 1.00 calc . . . H(19) H 0.0721 -0.3263 0.1630 0.0608 Uiso 1.00 calc . . . H(20) H 0.1292 -0.5626 0.3038 0.1199 Uiso 1.00 calc . . . H(21) H 0.0744 -0.6265 0.2613 0.1199 Uiso 1.00 calc . . . H(22) H 0.1307 -0.6732 0.2499 0.1199 Uiso 1.00 calc . . . H(23) H 0.1554 -0.4695 0.1380 0.0928 Uiso 1.00 calc . . . H(24) H 0.1459 -0.6170 0.1488 0.0928 Uiso 1.00 calc . . . H(25) H 0.0995 -0.5343 0.0997 0.0928 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0409(9) 0.054(1) 0.0262(7) 0.0000 0.0036(6) 0.0000 Cu(1) 0.0380(6) 0.0387(6) 0.0327(5) -0.0026(6) 0.0090(4) -0.0015(5) O(1) 0.043(3) 0.064(4) 0.026(3) -0.010(3) 0.008(3) 0.007(3) O(2) 0.039(3) 0.054(4) 0.028(3) -0.014(3) 0.007(3) -0.007(3) O(3) 0.115(6) 0.046(4) 0.058(4) -0.028(4) 0.034(4) -0.012(4) O(4) 0.069(4) 0.070(5) 0.052(4) -0.028(4) 0.022(3) -0.024(4) O(5) 0.047(4) 0.063(5) 0.069(4) 0.010(4) 0.017(3) 0.009(4) O(6) 0.072(5) 0.077(5) 0.045(4) 0.028(4) 0.017(4) 0.010(4) N(1) 0.037(4) 0.039(4) 0.033(4) -0.002(3) 0.013(3) 0.004(3) N(2) 0.037(4) 0.036(4) 0.021(3) 0.003(3) 0.005(3) -0.005(3) N(3) 0.053(5) 0.034(4) 0.041(4) -0.006(4) 0.003(4) -0.008(4) N(4) 0.047(5) 0.046(5) 0.033(4) -0.003(4) 0.010(4) -0.009(4) N(5) 0.049(5) 0.042(5) 0.070(5) 0.012(4) 0.013(4) 0.013(4) N(6) 0.065(6) 0.055(6) 0.050(5) 0.006(5) 0.014(4) 0.007(4) C(1) 0.039(5) 0.034(5) 0.036(4) 0.004(4) 0.009(4) 0.012(4) C(2) 0.043(6) 0.065(7) 0.050(6) -0.010(5) 0.015(5) -0.001(5) C(3) 0.063(7) 0.093(8) 0.055(6) -0.011(7) 0.033(5) -0.005(6) C(4) 0.052(7) 0.094(9) 0.073(7) -0.019(6) 0.033(6) 0.009(7) C(5) 0.050(6) 0.068(7) 0.055(6) -0.010(6) 0.012(5) 0.020(6) C(6) 0.040(5) 0.044(6) 0.045(5) -0.002(5) 0.004(4) 0.017(5) C(7) 0.069(7) 0.041(6) 0.038(5) -0.012(5) 0.013(5) 0.001(4) C(8) 0.043(5) 0.058(6) 0.035(5) 0.014(5) 0.020(4) -0.002(4) C(9) 0.028(4) 0.047(6) 0.033(4) 0.005(4) 0.004(4) 0.011(4) C(10) 0.047(6) 0.043(6) 0.039(5) -0.008(5) 0.002(4) 0.000(5) C(11) 0.069(7) 0.069(8) 0.053(6) -0.026(6) 0.018(5) 0.009(6) C(12) 0.073(7) 0.069(8) 0.057(6) -0.007(6) 0.038(6) 0.020(6) C(13) 0.048(6) 0.056(7) 0.044(5) 0.001(5) 0.022(5) 0.008(5) C(14) 0.027(4) 0.051(6) 0.033(4) 0.007(4) 0.009(4) 0.002(4) C(15) 0.032(4) 0.045(6) 0.027(4) 0.010(4) 0.000(4) 0.001(4) C(16) 0.035(5) 0.029(5) 0.035(4) 0.002(4) 0.017(4) 0.006(4) C(17) 0.069(7) 0.045(7) 0.054(6) 0.007(6) 0.016(6) 0.010(5) C(18) 0.079(8) 0.12(1) 0.063(7) 0.041(8) 0.016(6) 0.027(7) C(19) 0.078(9) 0.091(10) 0.19(1) 0.033(8) 0.095(9) 0.057(10) C(20) 0.049(6) 0.044(6) 0.062(6) 0.006(5) 0.005(5) 0.007(6) C(21) 0.16(1) 0.083(9) 0.067(7) 0.046(9) 0.017(8) 0.024(7) C(22) 0.076(8) 0.081(8) 0.085(8) 0.017(7) 0.036(7) -0.012(7) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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(1) O(1) 2.103(5) . . yes Zn(1) O(1) 2.103(5) . 2_555 yes Zn(1) O(2) 2.064(5) . . yes Zn(1) O(2) 2.064(5) . 2_555 yes Zn(1) O(6) 2.089(6) . . yes Zn(1) O(6) 2.089(6) . 2_555 yes Cu(1) O(5) 2.376(6) . . yes Cu(1) N(1) 1.991(6) . . yes Cu(1) N(2) 2.009(6) . . yes Cu(1) N(3) 2.012(7) . . yes Cu(1) N(4) 1.987(6) . . yes O(1) C(15) 1.247(8) . . yes O(2) C(16) 1.255(8) . . yes O(3) N(3) 1.350(8) . . yes O(3) H(6) 1.067 . . no O(4) N(4) 1.363(8) . . yes O(5) C(17) 1.22(1) . . yes O(6) C(20) 1.24(1) . . yes N(1) C(1) 1.432(9) . . yes N(1) C(15) 1.321(9) . . yes N(2) C(9) 1.426(9) . . yes N(2) C(16) 1.331(9) . . yes N(3) C(7) 1.293(10) . . yes N(4) C(8) 1.276(10) . . yes N(5) C(17) 1.33(1) . . yes N(5) C(18) 1.41(1) . . yes N(5) C(19) 1.44(1) . . yes N(6) C(20) 1.30(1) . . yes N(6) C(21) 1.44(1) . . yes N(6) C(22) 1.45(1) . . yes C(1) C(2) 1.40(1) . . yes C(1) C(6) 1.39(1) . . yes C(2) C(3) 1.39(1) . . yes C(2) H(1) 0.988 . . no C(3) C(4) 1.38(1) . . yes C(3) H(2) 1.058 . . no C(4) C(5) 1.38(1) . . yes C(4) H(3) 1.040 . . no C(5) C(6) 1.41(1) . . yes C(5) H(4) 1.071 . . no C(6) C(7) 1.43(1) . . yes C(7) H(5) 1.091 . . no C(8) C(14) 1.45(1) . . yes C(8) H(7) 1.119 . . no C(9) C(10) 1.38(1) . . yes C(9) C(14) 1.40(1) . . yes C(10) C(11) 1.38(1) . . yes C(10) H(11) 0.977 . . no C(11) C(12) 1.37(1) . . yes C(11) H(10) 0.977 . . no C(12) C(13) 1.37(1) . . yes C(12) H(9) 0.975 . . no C(13) C(14) 1.39(1) . . yes C(13) H(8) 1.169 . . no C(15) C(16) 1.525(10) . . yes C(17) H(12) 0.980 . . no C(18) H(13) 0.952 . . no C(18) H(14) 0.957 . . no C(18) H(15) 0.982 . . no C(19) H(16) 0.973 . . no C(19) H(17) 0.945 . . no C(19) H(18) 0.959 . . no C(20) H(19) 1.072 . . no C(21) H(20) 0.957 . . no C(21) H(21) 0.976 . . no C(21) H(22) 0.957 . . no C(22) H(23) 0.966 . . no C(22) H(24) 0.958 . . no C(22) H(25) 0.959 . . no #------------------------------------------------------------------------------ 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 O(1) Zn(1) O(1) 94.5(3) . 1_555 2_555 yes O(1) Zn(1) O(2) 78.1(2) . 1_555 1_555 yes O(1) Zn(1) O(2) 95.8(2) . 1_555 2_555 yes O(1) Zn(1) O(6) 90.7(2) . 1_555 1_555 yes O(1) Zn(1) O(6) 168.4(2) . 1_555 2_555 yes O(1) Zn(1) O(2) 95.8(2) . 2_555 1_555 yes O(1) Zn(1) O(2) 78.1(2) . 2_555 2_555 yes O(1) Zn(1) O(6) 168.4(2) . 2_555 1_555 yes O(1) Zn(1) O(6) 90.7(2) . 2_555 2_555 yes O(2) Zn(1) O(2) 171.2(3) . 1_555 2_555 yes O(2) Zn(1) O(6) 95.4(2) . 1_555 1_555 yes O(2) Zn(1) O(6) 91.1(2) . 1_555 2_555 yes O(2) Zn(1) O(6) 91.1(2) . 2_555 1_555 yes O(2) Zn(1) O(6) 95.4(2) . 2_555 2_555 yes O(6) Zn(1) O(6) 86.1(4) . 1_555 2_555 yes O(5) Cu(1) N(1) 97.8(2) . 1_555 1_555 yes O(5) Cu(1) N(2) 102.1(2) . 1_555 1_555 yes O(5) Cu(1) N(3) 92.4(3) . 1_555 1_555 yes O(5) Cu(1) N(4) 89.3(2) . 1_555 1_555 yes N(1) Cu(1) N(2) 84.0(2) . 1_555 1_555 yes N(1) Cu(1) N(3) 89.2(3) . 1_555 1_555 yes N(1) Cu(1) N(4) 171.7(3) . 1_555 1_555 yes N(2) Cu(1) N(3) 164.7(3) . 1_555 1_555 yes N(2) Cu(1) N(4) 90.3(3) . 1_555 1_555 yes N(3) Cu(1) N(4) 94.9(3) . 1_555 1_555 yes Zn(1) O(1) C(15) 113.6(5) . 1_555 1_555 yes Zn(1) O(2) C(16) 115.6(5) . 1_555 1_555 yes N(3) O(3) H(6) 100.8 . 1_555 1_555 no Cu(1) O(5) C(17) 125.7(6) . 1_555 1_555 yes Zn(1) O(6) C(20) 123.9(6) . 1_555 1_555 yes Cu(1) N(1) C(1) 127.8(5) . 1_555 1_555 yes Cu(1) N(1) C(15) 110.9(5) . 1_555 1_555 yes C(1) N(1) C(15) 121.0(7) . 1_555 1_555 yes Cu(1) N(2) C(9) 128.7(5) . 1_555 1_555 yes Cu(1) N(2) C(16) 110.3(5) . 1_555 1_555 yes C(9) N(2) C(16) 120.7(7) . 1_555 1_555 yes Cu(1) N(3) O(3) 120.3(5) . 1_555 1_555 yes Cu(1) N(3) C(7) 126.3(6) . 1_555 1_555 yes O(3) N(3) C(7) 113.3(7) . 1_555 1_555 yes Cu(1) N(4) O(4) 119.2(5) . 1_555 1_555 yes Cu(1) N(4) C(8) 126.5(6) . 1_555 1_555 yes O(4) N(4) C(8) 114.1(7) . 1_555 1_555 yes C(17) N(5) C(18) 119.9(8) . 1_555 1_555 yes C(17) N(5) C(19) 122.7(9) . 1_555 1_555 yes C(18) N(5) C(19) 117.3(8) . 1_555 1_555 yes C(20) N(6) C(21) 119.5(9) . 1_555 1_555 yes C(20) N(6) C(22) 122.9(9) . 1_555 1_555 yes C(21) N(6) C(22) 117.5(9) . 1_555 1_555 yes N(1) C(1) C(2) 121.7(8) . 1_555 1_555 yes N(1) C(1) C(6) 118.6(7) . 1_555 1_555 yes C(2) C(1) C(6) 119.6(8) . 1_555 1_555 yes C(1) C(2) C(3) 120.6(9) . 1_555 1_555 yes C(1) C(2) H(1) 119.6 . 1_555 1_555 no C(3) C(2) H(1) 119.8 . 1_555 1_555 no C(2) C(3) C(4) 120.3(9) . 1_555 1_555 yes C(2) C(3) H(2) 113.4 . 1_555 1_555 no C(4) C(3) H(2) 126.2 . 1_555 1_555 no C(3) C(4) C(5) 119.3(9) . 1_555 1_555 yes C(3) C(4) H(3) 118.3 . 1_555 1_555 no C(5) C(4) H(3) 121.8 . 1_555 1_555 no C(4) C(5) C(6) 121.6(9) . 1_555 1_555 yes C(4) C(5) H(4) 114.4 . 1_555 1_555 no C(6) C(5) H(4) 123.9 . 1_555 1_555 no C(1) C(6) C(5) 118.5(8) . 1_555 1_555 yes C(1) C(6) C(7) 126.8(8) . 1_555 1_555 yes C(5) C(6) C(7) 114.8(9) . 1_555 1_555 yes N(3) C(7) C(6) 126.5(8) . 1_555 1_555 yes N(3) C(7) H(5) 113.9 . 1_555 1_555 no C(6) C(7) H(5) 119.4 . 1_555 1_555 no N(4) C(8) C(14) 128.3(7) . 1_555 1_555 yes N(4) C(8) H(7) 114.8 . 1_555 1_555 no C(14) C(8) H(7) 116.2 . 1_555 1_555 no N(2) C(9) C(10) 123.7(7) . 1_555 1_555 yes N(2) C(9) C(14) 118.9(7) . 1_555 1_555 yes C(10) C(9) C(14) 117.4(8) . 1_555 1_555 yes C(9) C(10) C(11) 121.9(8) . 1_555 1_555 yes C(9) C(10) H(11) 118.8 . 1_555 1_555 no C(11) C(10) H(11) 119.2 . 1_555 1_555 no C(10) C(11) C(12) 120.3(9) . 1_555 1_555 yes C(10) C(11) H(10) 119.5 . 1_555 1_555 no C(12) C(11) H(10) 120.2 . 1_555 1_555 no C(11) C(12) C(13) 119.0(8) . 1_555 1_555 yes C(11) C(12) H(9) 120.1 . 1_555 1_555 no C(13) C(12) H(9) 120.8 . 1_555 1_555 no C(12) C(13) C(14) 121.3(8) . 1_555 1_555 yes C(12) C(13) H(8) 121.4 . 1_555 1_555 no C(14) C(13) H(8) 116.9 . 1_555 1_555 no C(8) C(14) C(9) 125.8(7) . 1_555 1_555 yes C(8) C(14) C(13) 114.3(7) . 1_555 1_555 yes C(9) C(14) C(13) 119.8(8) . 1_555 1_555 yes O(1) C(15) N(1) 127.7(8) . 1_555 1_555 yes O(1) C(15) C(16) 116.8(7) . 1_555 1_555 yes N(1) C(15) C(16) 115.5(6) . 1_555 1_555 yes O(2) C(16) N(2) 128.8(7) . 1_555 1_555 yes O(2) C(16) C(15) 115.4(6) . 1_555 1_555 yes N(2) C(16) C(15) 115.9(7) . 1_555 1_555 yes O(5) C(17) N(5) 125.4(9) . 1_555 1_555 yes O(5) C(17) H(12) 119.6 . 1_555 1_555 no N(5) C(17) H(12) 115.0 . 1_555 1_555 no N(5) C(18) H(13) 112.4 . 1_555 1_555 no N(5) C(18) H(14) 112.0 . 1_555 1_555 no N(5) C(18) H(15) 110.4 . 1_555 1_555 no H(13) C(18) H(14) 108.7 . 1_555 1_555 no H(13) C(18) H(15) 106.7 . 1_555 1_555 no H(14) C(18) H(15) 106.3 . 1_555 1_555 no N(5) C(19) H(16) 110.4 . 1_555 1_555 no N(5) C(19) H(17) 111.5 . 1_555 1_555 no N(5) C(19) H(18) 110.7 . 1_555 1_555 no H(16) C(19) H(17) 108.0 . 1_555 1_555 no H(16) C(19) H(18) 106.9 . 1_555 1_555 no H(17) C(19) H(18) 109.2 . 1_555 1_555 no O(6) C(20) N(6) 124.5(9) . 1_555 1_555 yes O(6) C(20) H(19) 116.4 . 1_555 1_555 no N(6) C(20) H(19) 118.7 . 1_555 1_555 no N(6) C(21) H(20) 111.6 . 1_555 1_555 no N(6) C(21) H(21) 110.7 . 1_555 1_555 no N(6) C(21) H(22) 112.6 . 1_555 1_555 no H(20) C(21) H(21) 106.7 . 1_555 1_555 no H(20) C(21) H(22) 108.3 . 1_555 1_555 no H(21) C(21) H(22) 106.7 . 1_555 1_555 no N(6) C(22) H(23) 110.4 . 1_555 1_555 no N(6) C(22) H(24) 112.0 . 1_555 1_555 no N(6) C(22) H(25) 111.3 . 1_555 1_555 no H(23) C(22) H(24) 107.5 . 1_555 1_555 no H(23) C(22) H(25) 107.4 . 1_555 1_555 no H(24) C(22) H(25) 108.1 . 1_555 1_555 no #------------------------------------------------------------------------------