#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_Na[Cu2(HL)(L)(H2O)] (2') _database_code_CSD 162982 #data_General _journal_coden_Cambridge 186 _audit_creation_date 'Wed Nov 1 21:00:23 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 ; Hakozaki 6-10-1, Higashi-ku, Fykuoka 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 ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #--------------------------------------------------------------------------- #-- # TITLE AND AUTHOR LIST _publ_section_title ; inuclear CuII and NiII Complexes of 3-Formylsalicylic Acid Oxime: Cis/trans Topology and Extension of Cis-CuII2 Complex to A Pentanuclear CuIICuIIMnIICuIICuII Complex ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name #_publ_author_footnote #_publ_author_address 'Ikeda, Kazuhide' 'Ohba, Masaaki' 'Okawa, H.' _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_Na[Cu2(HL)(L)(H2O)] (2') #--------------------------------------------------------------------------- #-- # CHEMICAL DATA _chemical_formula_sum 'C16 H11 Cu2 N2 Na O9 ' _chemical_formula_moiety '?' _chemical_formula_weight 525.35 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.347(3) _cell_length_b 11.033(2) _cell_length_c 8.607(2) _cell_angle_alpha 101.65(2) _cell_angle_beta 92.07(2) _cell_angle_gamma 75.28(2) _cell_volume 840.7(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.617 _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 1.000 #--------------------------------------------------------------------------- # 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 4108 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0016 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0016 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.64 #--------------------------------------------------------------------------- # 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 3853 _reflns_number_gt 3258 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0485 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3258 _refine_ls_number_parameters 281 _refine_ls_goodness_of_fit_ref 1.917 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.2935 _refine_diff_density_max 0.76 _refine_diff_density_min -0.73 _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) ; 'Na' 'Na' 0.036 0.025 ;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 0.60097(4) 0.01558(3) -0.16667(4) 0.02037(10) Uani 1.00 d . . . Cu(2) Cu 0.82935(4) 0.00598(3) 0.08114(4) 0.02087(10) Uani 1.00 d . . . Na(1) Na 1.0516(2) 0.1170(2) 0.5467(3) 0.0483(6) Uani 0.77 d P . . Na(2) Na 1.0519(6) -0.0109(6) 0.3413(7) 0.029(2) Uani 0.23 d P . . O(1) O 0.3059(3) 0.1073(2) -0.2692(3) 0.0389(7) Uani 1.00 d . . . O(2) O 0.6457(2) 0.1141(2) 0.0368(2) 0.0224(5) Uani 1.00 d . . . O(3) O 0.8663(2) 0.1168(2) 0.2664(2) 0.0224(5) Uani 1.00 d . . . O(4) O 0.8237(3) 0.2895(2) 0.4543(3) 0.0327(6) Uani 1.00 d . . . O(5) O 0.4441(2) -0.0975(2) -0.4237(3) 0.0312(6) Uani 1.00 d . . . O(6) O 0.7863(2) -0.0968(2) -0.1134(3) 0.0240(5) Uani 1.00 d . . . O(7) O 1.0147(2) -0.1062(2) 0.1052(3) 0.0230(5) Uani 1.00 d . . . O(8) O 1.1597(3) -0.2970(2) 0.1049(3) 0.0334(6) Uani 1.00 d . . . O(9) O 0.7341(2) 0.1166(2) -0.3086(3) 0.0265(6) Uani 1.00 d . . . N(1) N 0.4130(3) 0.1410(3) -0.1688(3) 0.0247(6) Uani 1.00 d . . . N(2) N 0.5708(3) -0.1207(3) -0.3371(3) 0.0225(6) Uani 1.00 d . . . C(1) C 0.5932(3) 0.2377(3) 0.1049(3) 0.0181(7) Uani 1.00 d . . . C(2) C 0.4659(3) 0.3099(3) 0.0412(4) 0.0205(7) Uani 1.00 d . . . C(3) C 0.4085(3) 0.4382(3) 0.1117(4) 0.0271(8) Uani 1.00 d . . . C(4) C 0.4723(4) 0.4952(3) 0.2429(4) 0.0318(8) Uani 1.00 d . . . C(5) C 0.5947(4) 0.4245(3) 0.3071(4) 0.0278(8) Uani 1.00 d . . . C(6) C 0.6577(3) 0.2962(3) 0.2410(3) 0.0196(7) Uani 1.00 d . . . C(7) C 0.3801(3) 0.2557(3) -0.0866(4) 0.0231(7) Uani 1.00 d . . . C(8) C 0.7899(3) 0.2313(3) 0.3270(3) 0.0208(7) Uani 1.00 d . . . C(9) C 0.8506(3) -0.2215(3) -0.1647(3) 0.0189(7) Uani 1.00 d . . . C(10) C 0.7904(3) -0.2887(3) -0.2981(4) 0.0219(7) Uani 1.00 d . . . C(11) C 0.8551(4) -0.4194(3) -0.3523(4) 0.0288(8) Uani 1.00 d . . . C(12) C 0.9740(4) -0.4846(3) -0.2771(4) 0.0322(9) Uani 1.00 d . . . C(13) C 1.0317(3) -0.4185(3) -0.1479(4) 0.0259(8) Uani 1.00 d . . . C(14) C 0.9735(3) -0.2877(3) -0.0889(3) 0.0201(7) Uani 1.00 d . . . C(15) C 0.6569(3) -0.2344(3) -0.3776(4) 0.0249(7) Uani 1.00 d . . . C(16) C 1.0538(3) -0.2289(3) 0.0490(3) 0.0203(7) Uani 1.00 d . . . H(1) H 0.3280 0.4865 0.0692 0.0299 Uiso 1.00 calc . . . H(2) H 0.4257 0.5790 0.2908 0.0299 Uiso 1.00 calc . . . H(3) H 0.6382 0.4674 0.4038 0.0299 Uiso 1.00 calc . . . H(4) H 0.2814 0.3079 -0.1060 0.0299 Uiso 1.00 calc . . . H(5) H 0.8092 -0.4616 -0.4340 0.0299 Uiso 1.00 calc . . . H(6) H 1.0253 -0.5821 -0.3217 0.0299 Uiso 1.00 calc . . . H(7) H 1.1108 -0.4618 -0.0975 0.0299 Uiso 1.00 calc . . . H(8) H 0.6257 -0.2951 -0.4626 0.0299 Uiso 1.00 calc . . . H(9) H 0.3390 -0.0105 -0.3721 0.0299 Uiso 1.00 calc . . . H(10) H 0.7346 0.1913 -0.2394 0.0299 Uiso 1.00 calc . . . H(11) H 0.6929 0.1435 -0.3729 0.0299 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) 0.0181(2) 0.0190(2) 0.0195(2) -0.0011(1) -0.0091(1) -0.0005(1) Cu(2) 0.0196(2) 0.0152(2) 0.0197(2) 0.0033(1) -0.0100(1) -0.0037(1) Na(1) 0.049(1) 0.047(1) 0.046(1) -0.0090(10) -0.0107(10) 0.0073(10) Na(2) 0.027(3) 0.032(3) 0.024(3) 0.000(2) -0.005(2) 0.003(2) O(1) 0.023(1) 0.036(1) 0.046(2) -0.001(1) -0.024(1) -0.007(1) O(2) 0.022(1) 0.0161(10) 0.021(1) 0.0038(8) -0.0096(8) -0.0034(8) O(3) 0.023(1) 0.0153(10) 0.021(1) 0.0026(8) -0.0085(8) -0.0038(8) O(4) 0.039(1) 0.021(1) 0.026(1) 0.0044(10) -0.0174(10) -0.0066(9) O(5) 0.027(1) 0.033(1) 0.028(1) -0.0054(10) -0.0195(10) -0.0003(10) O(6) 0.026(1) 0.0142(10) 0.024(1) 0.0019(8) -0.0121(9) -0.0035(8) O(7) 0.022(1) 0.0151(10) 0.024(1) 0.0024(8) -0.0101(9) -0.0033(8) O(8) 0.032(1) 0.021(1) 0.037(1) 0.0050(9) -0.019(1) 0.0012(10) O(9) 0.027(1) 0.028(1) 0.021(1) -0.0038(9) -0.0089(9) 0.0047(9) N(1) 0.018(1) 0.028(1) 0.026(1) -0.004(1) -0.010(1) 0.005(1) N(2) 0.020(1) 0.025(1) 0.021(1) -0.006(1) -0.0090(10) 0.003(1) C(1) 0.019(1) 0.014(1) 0.017(1) 0.000(1) -0.001(1) 0.000(1) C(2) 0.017(1) 0.019(1) 0.021(1) 0.001(1) -0.003(1) 0.003(1) C(3) 0.026(2) 0.018(1) 0.032(2) 0.004(1) -0.007(1) 0.005(1) C(4) 0.033(2) 0.016(1) 0.036(2) 0.005(1) -0.004(1) -0.003(1) C(5) 0.033(2) 0.018(1) 0.026(2) -0.002(1) -0.003(1) -0.003(1) C(6) 0.019(1) 0.016(1) 0.020(1) 0.000(1) -0.003(1) 0.002(1) C(7) 0.015(1) 0.025(1) 0.025(2) 0.002(1) -0.007(1) 0.007(1) C(8) 0.023(1) 0.017(1) 0.019(1) -0.001(1) -0.004(1) 0.000(1) C(9) 0.019(1) 0.015(1) 0.019(1) -0.002(1) -0.001(1) 0.000(1) C(10) 0.024(1) 0.021(1) 0.019(1) -0.006(1) -0.003(1) -0.002(1) C(11) 0.029(2) 0.023(2) 0.028(2) -0.006(1) -0.005(1) -0.007(1) C(12) 0.037(2) 0.017(1) 0.034(2) -0.001(1) -0.001(1) -0.007(1) C(13) 0.027(2) 0.016(1) 0.030(2) 0.000(1) -0.005(1) 0.001(1) C(14) 0.022(1) 0.016(1) 0.020(1) -0.002(1) -0.001(1) 0.000(1) C(15) 0.025(2) 0.026(2) 0.020(1) -0.007(1) -0.008(1) -0.002(1) C(16) 0.020(1) 0.018(1) 0.019(1) 0.000(1) -0.002(1) 0.002(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 SAPI91 _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(2) 1.958(2) . . yes Cu(1) O(6) 1.957(2) . . yes Cu(1) O(9) 2.376(2) . . yes Cu(1) N(1) 1.943(3) . . yes Cu(1) N(2) 1.946(3) . . yes Cu(2) Na(2) 3.002(5) . . yes Cu(2) O(2) 1.900(2) . . yes Cu(2) O(3) 1.883(2) . . yes Cu(2) O(6) 1.915(2) . . yes Cu(2) O(7) 1.888(2) . . yes Na(1) Na(1) 2.935(4) . 2_756 yes Na(1) Na(2) 2.027(6) . . yes Na(1) Na(2) 2.082(7) . 2_756 yes Na(1) O(4) 2.687(3) . . yes Na(2) Na(2) 2.88(1) . 2_756 yes Na(2) O(3) 2.111(6) . . yes Na(2) O(7) 2.152(6) . . yes Na(2) O(9) 2.040(6) . 2_755 yes O(1) N(1) 1.373(3) . . yes O(2) C(1) 1.342(3) . . yes O(3) C(8) 1.296(3) . . yes O(4) C(8) 1.227(4) . . yes O(5) N(2) 1.372(3) . . yes O(5) H(9) 1.210 . . no O(6) C(9) 1.343(3) . . yes O(7) C(16) 1.302(3) . . yes O(8) C(16) 1.229(4) . . yes O(9) H(10) 0.916 . . no O(9) H(11) 0.732 . . no N(1) C(7) 1.285(4) . . yes N(2) C(15) 1.293(4) . . yes C(1) C(2) 1.413(4) . . yes C(1) C(6) 1.412(4) . . yes C(2) C(3) 1.396(4) . . yes C(2) C(7) 1.459(4) . . yes C(3) C(4) 1.372(5) . . yes C(3) H(1) 0.916 . . no C(4) C(5) 1.378(4) . . yes C(4) H(2) 0.932 . . no C(5) C(6) 1.397(4) . . yes C(5) H(3) 0.998 . . no C(6) C(8) 1.512(4) . . yes C(7) H(4) 0.984 . . no C(9) C(10) 1.417(4) . . yes C(9) C(14) 1.410(4) . . yes C(10) C(11) 1.402(4) . . yes C(10) C(15) 1.453(4) . . yes C(11) C(12) 1.380(5) . . yes C(11) H(5) 0.919 . . no C(12) C(13) 1.374(4) . . yes C(12) H(6) 1.058 . . no C(13) C(14) 1.400(4) . . yes C(13) H(7) 0.918 . . no C(14) C(16) 1.506(4) . . yes C(15) H(8) 0.977 . . 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(2) Cu(1) O(6) 78.75(8) . 1_555 1_555 yes O(2) Cu(1) O(9) 91.62(9) . 1_555 1_555 yes O(2) Cu(1) N(1) 89.62(10) . 1_555 1_555 yes O(2) Cu(1) N(2) 164.17(10) . 1_555 1_555 yes O(6) Cu(1) O(9) 90.52(9) . 1_555 1_555 yes O(6) Cu(1) N(1) 167.2(1) . 1_555 1_555 yes O(6) Cu(1) N(2) 90.02(10) . 1_555 1_555 yes O(9) Cu(1) N(1) 95.12(10) . 1_555 1_555 yes O(9) Cu(1) N(2) 99.69(9) . 1_555 1_555 yes N(1) Cu(1) N(2) 100.3(1) . 1_555 1_555 yes Na(2) Cu(2) O(2) 139.2(1) . 1_555 1_555 yes Na(2) Cu(2) O(3) 44.2(1) . 1_555 1_555 yes Na(2) Cu(2) O(6) 139.1(1) . 1_555 1_555 yes Na(2) Cu(2) O(7) 45.5(1) . 1_555 1_555 yes O(2) Cu(2) O(3) 95.73(9) . 1_555 1_555 yes O(2) Cu(2) O(6) 81.21(9) . 1_555 1_555 yes O(2) Cu(2) O(7) 174.82(9) . 1_555 1_555 yes O(3) Cu(2) O(6) 176.14(9) . 1_555 1_555 yes O(3) Cu(2) O(7) 88.56(9) . 1_555 1_555 yes O(6) Cu(2) O(7) 94.38(9) . 1_555 1_555 yes Na(1) Na(1) Na(2) 45.2(2) . 2_756 1_555 yes Na(1) Na(1) Na(2) 43.7(2) . 2_756 2_756 yes Na(1) Na(1) O(4) 100.8(1) . 2_756 1_555 yes Na(2) Na(1) Na(2) 88.8(2) . 1_555 2_756 yes Na(2) Na(1) O(4) 92.2(2) . 1_555 1_555 yes Na(2) Na(1) O(4) 103.2(2) . 2_756 1_555 yes Cu(2) Na(2) Na(1) 127.8(2) . 1_555 1_555 yes Cu(2) Na(2) Na(1) 93.3(2) . 1_555 2_756 yes Cu(2) Na(2) Na(2) 118.3(3) . 1_555 2_756 yes Cu(2) Na(2) O(3) 38.5(1) . 1_555 1_555 yes Cu(2) Na(2) O(7) 38.7(1) . 1_555 1_555 yes Cu(2) Na(2) O(9) 123.9(2) . 1_555 2_755 yes Na(1) Na(2) Na(1) 91.2(2) . 1_555 2_756 yes Na(1) Na(2) Na(2) 46.4(2) . 1_555 2_756 yes Na(1) Na(2) O(3) 89.7(2) . 1_555 1_555 yes Na(1) Na(2) O(7) 165.6(3) . 1_555 1_555 yes Na(1) Na(2) O(9) 104.9(3) . 1_555 2_755 yes Na(1) Na(2) Na(2) 44.8(2) . 2_756 2_756 yes Na(1) Na(2) O(3) 100.7(3) . 2_756 1_555 yes Na(1) Na(2) O(7) 94.7(3) . 2_756 1_555 yes Na(1) Na(2) O(9) 104.6(3) . 2_756 2_755 yes Na(2) Na(2) O(3) 97.5(3) . 2_756 1_555 yes Na(2) Na(2) O(7) 137.8(4) . 2_756 1_555 yes Na(2) Na(2) O(9) 111.3(3) . 2_756 2_755 yes O(3) Na(2) O(7) 76.3(2) . 1_555 1_555 yes O(3) Na(2) O(9) 150.4(3) . 1_555 2_755 yes O(7) Na(2) O(9) 86.4(2) . 1_555 2_755 yes Cu(1) O(2) Cu(2) 100.22(9) . 1_555 1_555 yes Cu(1) O(2) C(1) 131.0(2) . 1_555 1_555 yes Cu(2) O(2) C(1) 125.9(2) . 1_555 1_555 yes Cu(2) O(3) Na(2) 97.3(2) . 1_555 1_555 yes Cu(2) O(3) C(8) 128.5(2) . 1_555 1_555 yes Na(2) O(3) C(8) 134.0(2) . 1_555 1_555 yes Na(1) O(4) C(8) 103.0(2) . 1_555 1_555 yes N(2) O(5) H(9) 120.4 . 1_555 1_555 no Cu(1) O(6) Cu(2) 99.74(9) . 1_555 1_555 yes Cu(1) O(6) C(9) 132.8(2) . 1_555 1_555 yes Cu(2) O(6) C(9) 125.4(2) . 1_555 1_555 yes Cu(2) O(7) Na(2) 95.8(2) . 1_555 1_555 yes Cu(2) O(7) C(16) 126.5(2) . 1_555 1_555 yes Na(2) O(7) C(16) 126.4(2) . 1_555 1_555 yes Cu(1) O(9) Na(2) 109.4(2) . 1_555 2_755 yes Cu(1) O(9) H(10) 103.3 . 1_555 1_555 no Cu(1) O(9) H(11) 114.4 . 1_555 1_555 no Na(2) O(9) H(10) 107.4 . 2_755 1_555 no Na(2) O(9) H(11) 121.2 . 2_755 1_555 no H(10) O(9) H(11) 98.8 . 1_555 1_555 no Cu(1) N(1) O(1) 118.2(2) . 1_555 1_555 yes Cu(1) N(1) C(7) 125.7(2) . 1_555 1_555 yes O(1) N(1) C(7) 116.1(2) . 1_555 1_555 yes Cu(1) N(2) O(5) 118.1(2) . 1_555 1_555 yes Cu(1) N(2) C(15) 127.0(2) . 1_555 1_555 yes O(5) N(2) C(15) 114.9(2) . 1_555 1_555 yes O(2) C(1) C(2) 118.7(2) . 1_555 1_555 yes O(2) C(1) C(6) 122.1(2) . 1_555 1_555 yes C(2) C(1) C(6) 119.2(3) . 1_555 1_555 yes C(1) C(2) C(3) 119.5(3) . 1_555 1_555 yes C(1) C(2) C(7) 123.8(3) . 1_555 1_555 yes C(3) C(2) C(7) 116.4(3) . 1_555 1_555 yes C(2) C(3) C(4) 121.2(3) . 1_555 1_555 yes C(2) C(3) H(1) 120.1 . 1_555 1_555 no C(4) C(3) H(1) 118.6 . 1_555 1_555 no C(3) C(4) C(5) 119.5(3) . 1_555 1_555 yes C(3) C(4) H(2) 118.2 . 1_555 1_555 no C(5) C(4) H(2) 122.1 . 1_555 1_555 no C(4) C(5) C(6) 121.8(3) . 1_555 1_555 yes C(4) C(5) H(3) 118.2 . 1_555 1_555 no C(6) C(5) H(3) 120.0 . 1_555 1_555 no C(1) C(6) C(5) 118.8(3) . 1_555 1_555 yes C(1) C(6) C(8) 125.8(3) . 1_555 1_555 yes C(5) C(6) C(8) 115.4(3) . 1_555 1_555 yes N(1) C(7) C(2) 126.9(3) . 1_555 1_555 yes N(1) C(7) H(4) 115.0 . 1_555 1_555 no C(2) C(7) H(4) 117.8 . 1_555 1_555 no O(3) C(8) O(4) 120.9(3) . 1_555 1_555 yes O(3) C(8) C(6) 120.4(2) . 1_555 1_555 yes O(4) C(8) C(6) 118.7(3) . 1_555 1_555 yes O(6) C(9) C(10) 118.3(3) . 1_555 1_555 yes O(6) C(9) C(14) 122.4(3) . 1_555 1_555 yes C(10) C(9) C(14) 119.2(3) . 1_555 1_555 yes C(9) C(10) C(11) 119.2(3) . 1_555 1_555 yes C(9) C(10) C(15) 124.4(3) . 1_555 1_555 yes C(11) C(10) C(15) 116.2(3) . 1_555 1_555 yes C(10) C(11) C(12) 121.6(3) . 1_555 1_555 yes C(10) C(11) H(5) 117.1 . 1_555 1_555 no C(12) C(11) H(5) 121.0 . 1_555 1_555 no C(11) C(12) C(13) 118.7(3) . 1_555 1_555 yes C(11) C(12) H(6) 121.2 . 1_555 1_555 no C(13) C(12) H(6) 119.9 . 1_555 1_555 no C(12) C(13) C(14) 122.5(3) . 1_555 1_555 yes C(12) C(13) H(7) 118.9 . 1_555 1_555 no C(14) C(13) H(7) 118.7 . 1_555 1_555 no C(9) C(14) C(13) 118.7(3) . 1_555 1_555 yes C(9) C(14) C(16) 125.5(3) . 1_555 1_555 yes C(13) C(14) C(16) 115.7(3) . 1_555 1_555 yes N(2) C(15) C(10) 126.8(3) . 1_555 1_555 yes N(2) C(15) H(8) 118.4 . 1_555 1_555 no C(10) C(15) H(8) 114.4 . 1_555 1_555 no O(7) C(16) O(8) 120.2(3) . 1_555 1_555 yes O(7) C(16) C(14) 120.4(2) . 1_555 1_555 yes O(8) C(16) C(14) 119.4(3) . 1_555 1_555 yes #--------------------------------------------------------------------------- #-- 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 Cu(2) Na(2) 3.002(5) . . ? Na(1) Na(1) 2.935(4) . 2_756 ? Na(1) O(4) 2.687(3) . . ? Na(2) Na(2) 2.88(1) . 2_756 ? Cu(1) O(2) 3.335(2) . 2_655 ? Cu(2) O(1) 2.747(3) . 2_655 ? Cu(2) O(7) 2.761(2) . 2_755 ? Cu(2) Na(2) 3.002(5) . . ? Cu(2) N(1) 3.289(3) . 2_655 ? Cu(2) C(16) 3.326(3) . 2_755 ? Cu(2) Cu(2) 3.490(1) . 2_755 ? Na(1) O(4) 2.687(3) . . ? Na(1) O(1) 2.800(3) . 1_656 ? Na(1) O(3) 2.919(3) . . ? Na(1) O(7) 3.113(3) . 2_756 ? Na(1) C(8) 3.195(4) . . ? Na(1) O(9) 3.224(3) . 2_755 ? Na(1) O(3) 3.227(3) . 2_756 ? Na(1) O(9) 3.261(3) . 1_556 ? Na(1) C(16) 3.535(4) . 2_756 ? Na(1) O(8) 3.587(3) . 2_756 ? Na(2) O(6) 3.101(7) . 2_755 ? Na(2) C(16) 3.107(6) . . ? Na(2) C(8) 3.152(6) . . ? Na(2) O(8) 3.325(6) . . ? Na(2) O(4) 3.426(6) . . ? Na(2) C(9) 3.546(7) . 2_755 ? O(1) O(3) 3.279(3) . 2_655 ? O(1) O(7) 3.362(4) . 2_655 ? O(1) O(2) 3.394(4) . 2_655 ? O(1) O(6) 3.466(4) . 2_655 ? O(1) O(5) 3.558(4) . 2_654 ? O(2) N(2) 3.318(3) . 2_655 ? O(2) N(1) 3.412(4) . 2_655 ? O(2) O(7) 3.417(3) . 2_755 ? O(2) O(8) 3.447(3) . 2_755 ? O(2) O(5) 3.515(3) . 2_655 ? O(2) C(16) 3.517(4) . 2_755 ? O(3) C(14) 3.300(4) . 2_755 ? O(3) O(5) 3.319(3) . 2_655 ? O(3) C(9) 3.351(4) . 2_755 ? O(3) C(16) 3.380(4) . 2_755 ? O(3) O(7) 3.394(3) . 2_755 ? O(3) O(6) 3.486(3) . 2_755 ? O(4) O(9) 3.319(4) . 1_556 ? O(4) C(11) 3.385(4) . 1_566 ? O(4) C(12) 3.571(4) . 1_566 ? O(5) O(9) 2.799(3) . 2_654 ? O(5) O(5) 3.135(5) . 2_654 ? O(5) C(8) 3.150(4) . 2_655 ? O(5) C(6) 3.278(4) . 2_655 ? O(5) N(2) 3.445(4) . 2_654 ? O(5) C(1) 3.479(4) . 2_655 ? O(6) O(7) 3.245(3) . 2_755 ? O(6) N(1) 3.298(4) . 2_655 ? O(6) C(7) 3.354(4) . 2_655 ? O(7) O(9) 2.871(3) . 2_755 ? O(7) O(7) 3.194(4) . 2_755 ? O(8) O(9) 2.737(3) . 2_755 ? O(8) C(3) 3.249(4) . 1_645 ? O(8) C(1) 3.251(4) . 2_755 ? O(8) C(6) 3.487(4) . 2_755 ? O(8) C(4) 3.557(4) . 1_645 ? O(8) C(12) 3.560(4) . 2_745 ? O(9) C(16) 3.205(4) . 2_755 ? N(2) C(1) 3.206(4) . 2_655 ? N(2) C(6) 3.445(4) . 2_655 ? C(1) C(15) 3.383(4) . 2_655 ? C(1) C(16) 3.571(4) . 2_755 ? C(2) C(10) 3.399(4) . 2_655 ? C(2) C(15) 3.477(4) . 2_655 ? C(2) C(9) 3.598(4) . 2_655 ? C(3) C(3) 3.310(7) . 2_665 ? C(3) C(11) 3.348(5) . 2_655 ? C(3) C(10) 3.405(4) . 2_655 ? C(3) C(4) 3.558(5) . 2_665 ? C(4) C(11) 3.574(5) . 2_655 ? C(6) C(15) 3.476(4) . 2_655 ? C(6) C(16) 3.574(4) . 2_755 ? C(7) C(9) 3.248(4) . 2_655 ? C(7) C(14) 3.589(4) . 2_655 ? C(8) C(14) 3.320(4) . 2_755 ? C(8) C(13) 3.557(4) . 2_755 ? C(8) C(16) 3.591(4) . 2_755 ? C(11) C(12) 3.463(5) . 2_744 ? C(13) C(13) 3.544(7) . 2_745 ? #--------------------------------------------------------------------------- #-- data_[Ni2(HL)2(H2O)4]8H2O(3') _database_code_CSD 162983 _journal_coden_Cambridge 186 #data_General _audit_creation_date 'Wed Nov 1 21:09:56 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 ; Hakozaki 6-10-1, Higashi-ku, Fykuoka 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 ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #--------------------------------------------------------------------------- # TITLE AND AUTHOR LIST _publ_section_title ; inuclear CuII and NiII Complexes of 3-Formylsalicylic Acid Oxime: Cis/trans Topology and Extension of Cis-CuII2 Complex to A Pentanuclear CuIICuIIMnIICuIICuII Complex ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name #_publ_author_footnote #_publ_author_address 'Ikeda, Kazuhide' 'Ohba, Masaaki' 'Okawa, H.' _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_[Ni2(HL)2(H2O)4]8H2O(3') #--------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C16 H34 N2 O20 Ni2 ' _chemical_formula_moiety '?' _chemical_formula_weight 691.85 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 7.779(4) _cell_length_b 15.561(4) _cell_length_c 11.124(2) _cell_angle_alpha 90 _cell_angle_beta 99.07(2) _cell_angle_gamma 90 _cell_volume 1329.7(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'green' _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 1.728 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.824 _exptl_absorpt_correction_T_max 0.999 #--------------------------------------------------------------------------- # 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 3396 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.09 #--------------------------------------------------------------------------- # 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 3053 _reflns_number_gt 2379 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0428 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2379 _refine_ls_number_parameters 181 _refine_ls_goodness_of_fit_ref 1.743 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_shift/su_max 0.6533 _refine_diff_density_max 0.71 _refine_diff_density_min -0.38 _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) ; '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 Ni Ni -0.01292(4) 0.06535(2) 0.09917(3) 0.02370(9) Uani 1.00 d . . . O(1) O 0.0647(4) -0.1045(2) -0.3589(2) 0.0521(7) Uani 1.00 d . . . O(2) O 0.0029(2) 0.0645(1) -0.0803(2) 0.0246(5) Uani 1.00 d . . . O(3) O -0.0215(3) 0.1940(1) 0.0931(2) 0.0346(5) Uani 1.00 d . . . O(4) O -0.0588(3) 0.3217(1) 0.0055(2) 0.0367(6) Uani 1.00 d . . . O(5) O -0.2829(3) 0.0612(1) 0.0673(2) 0.0349(6) Uani 1.00 d . . . O(6) O 0.2629(3) 0.0738(1) 0.1434(2) 0.0309(5) Uani 1.00 d . . . O(7) O 0.3684(3) 0.1495(2) 0.3734(2) 0.0539(8) Uani 1.00 d . . . O(8) O 0.6621(3) 0.2104(2) 0.2886(2) 0.0499(7) Uani 1.00 d . . . O(9) O 0.3716(4) 0.0396(2) 0.5691(3) 0.079(1) Uani 1.00 d . . . O(10) O 0.4690(3) 0.0567(1) 0.8210(2) 0.0410(6) Uani 1.00 d . . . N(1) N 0.0128(3) -0.0434(2) -0.2790(2) 0.0296(6) Uani 1.00 d . . . C(1) C -0.0864(3) 0.1187(2) -0.1581(2) 0.0236(6) Uani 1.00 d . . . C(2) C -0.1278(4) 0.0972(2) -0.2833(2) 0.0274(7) Uani 1.00 d . . . C(3) C -0.2269(4) 0.1529(2) -0.3651(3) 0.0361(8) Uani 1.00 d . . . C(4) C -0.2865(4) 0.2300(2) -0.3266(3) 0.0402(9) Uani 1.00 d . . . C(5) C -0.2360(4) 0.2546(2) -0.2075(3) 0.0332(8) Uani 1.00 d . . . C(6) C -0.1337(3) 0.2016(2) -0.1223(2) 0.0265(7) Uani 1.00 d . . . C(7) C -0.0618(4) 0.0214(2) -0.3383(3) 0.0325(8) Uani 1.00 d . . . C(8) C -0.0684(3) 0.2402(2) -0.0001(3) 0.0276(7) Uani 1.00 d . . . H(1) H -0.2538 0.1301 -0.4552 0.0467 Uiso 1.00 calc . . . H(2) H -0.3512 0.2723 -0.3830 0.0467 Uiso 1.00 calc . . . H(3) H -0.2621 0.3141 -0.1740 0.0467 Uiso 1.00 calc . . . H(4) H 0.1508 -0.1415 -0.3063 0.0467 Uiso 1.00 calc . . . H(5) H -0.3350 0.1135 0.0783 0.0467 Uiso 1.00 calc . . . H(6) H -0.3302 0.0151 0.1125 0.0467 Uiso 1.00 calc . . . H(7) H 0.3057 0.1151 0.1002 0.0467 Uiso 1.00 calc . . . H(8) H 0.2949 0.0980 0.2173 0.0467 Uiso 1.00 calc . . . H(9) H 0.2885 0.1941 0.3590 0.0467 Uiso 1.00 calc . . . H(10) H 0.3637 0.1204 0.4560 0.0467 Uiso 1.00 calc . . . H(11) H 0.6003 0.2420 0.2183 0.0467 Uiso 1.00 calc . . . H(12) H 0.5725 0.1907 0.3317 0.0467 Uiso 1.00 calc . . . H(13) H 0.2992 0.0838 0.5816 0.0467 Uiso 1.00 calc . . . H(14) H 0.4192 0.0648 0.6519 0.0467 Uiso 1.00 calc . . . H(15) H 0.4734 0.1042 0.8711 0.0467 Uiso 1.00 calc . . . H(16) H 0.5706 0.0348 0.8558 0.0467 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 Ni 0.0261(2) 0.0218(2) 0.0235(2) 0.0011(1) 0.0046(1) -0.0006(1) O(1) 0.075(2) 0.052(2) 0.031(1) 0.032(1) 0.012(1) -0.005(1) O(2) 0.0274(9) 0.0222(9) 0.0241(9) 0.0024(8) 0.0039(7) 0.0014(7) O(3) 0.044(1) 0.026(1) 0.033(1) 0.0014(9) 0.0033(9) -0.0025(9) O(4) 0.047(1) 0.022(1) 0.042(1) -0.0003(9) 0.0099(10) -0.0019(9) O(5) 0.028(1) 0.032(1) 0.045(1) 0.0033(9) 0.0077(9) 0.0044(9) O(6) 0.030(1) 0.031(1) 0.032(1) -0.0027(9) 0.0050(8) 0.0014(8) O(7) 0.051(2) 0.061(2) 0.049(1) 0.002(1) 0.007(1) 0.002(1) O(8) 0.044(1) 0.054(2) 0.052(1) 0.010(1) 0.008(1) 0.011(1) O(9) 0.086(2) 0.086(2) 0.058(2) -0.007(2) -0.011(2) 0.000(2) O(10) 0.041(1) 0.037(1) 0.044(1) 0.0023(10) 0.0026(10) -0.0007(10) N(1) 0.033(1) 0.031(1) 0.026(1) 0.004(1) 0.0087(10) -0.0058(10) C(1) 0.019(1) 0.024(1) 0.028(1) -0.001(1) 0.0057(10) 0.002(1) C(2) 0.027(1) 0.028(1) 0.028(1) 0.000(1) 0.005(1) 0.002(1) C(3) 0.038(2) 0.038(2) 0.031(2) 0.004(1) 0.001(1) 0.004(1) C(4) 0.039(2) 0.038(2) 0.041(2) 0.008(1) -0.001(1) 0.011(1) C(5) 0.028(1) 0.027(1) 0.044(2) 0.004(1) 0.004(1) 0.004(1) C(6) 0.024(1) 0.025(1) 0.031(1) 0.000(1) 0.006(1) 0.002(1) C(7) 0.034(2) 0.036(2) 0.029(1) 0.004(1) 0.008(1) 0.001(1) C(8) 0.024(1) 0.025(1) 0.036(2) 0.000(1) 0.010(1) -0.001(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 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 Ni O(2) 2.019(2) . . yes Ni O(2) 2.035(2) . 3_555 yes Ni O(3) 2.004(2) . . yes Ni O(5) 2.075(2) . . yes Ni O(6) 2.129(2) . . yes Ni N(1) 2.029(2) . 3_555 yes O(1) N(1) 1.403(3) . . yes O(2) C(1) 1.324(3) . . yes O(3) C(8) 1.267(3) . . yes O(4) C(8) 1.270(3) . . yes N(1) C(7) 1.292(4) . . yes C(1) C(2) 1.418(4) . . yes C(1) C(6) 1.416(4) . . yes C(2) C(3) 1.397(4) . . yes C(2) C(7) 1.459(4) . . yes C(3) C(4) 1.379(4) . . yes C(4) C(5) 1.375(4) . . yes C(5) C(6) 1.405(4) . . yes C(6) C(8) 1.499(4) . . yes #--------------------------------------------------------------------------- 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(2) Ni O(2) 83.22(7) . 1_555 3_555 yes O(2) Ni O(3) 88.85(8) . 1_555 1_555 yes O(2) Ni O(5) 92.79(8) . 1_555 1_555 yes O(2) Ni O(6) 90.73(7) . 1_555 1_555 yes O(2) Ni N(1) 169.36(8) . 1_555 3_555 yes O(2) Ni O(3) 172.07(8) . 3_555 1_555 yes O(2) Ni O(5) 90.35(8) . 3_555 1_555 yes O(2) Ni O(6) 91.79(7) . 3_555 1_555 yes O(2) Ni N(1) 86.60(8) . 3_555 3_555 yes O(3) Ni O(5) 89.85(8) . 1_555 1_555 yes O(3) Ni O(6) 88.48(8) . 1_555 1_555 yes O(3) Ni N(1) 101.33(9) . 1_555 3_555 yes O(5) Ni O(6) 176.08(8) . 1_555 1_555 yes O(5) Ni N(1) 90.36(9) . 1_555 3_555 yes O(6) Ni N(1) 86.49(9) . 1_555 3_555 yes Ni O(2) Ni 96.78(7) . 1_555 3_555 yes Ni O(2) C(1) 122.4(2) . 1_555 1_555 yes Ni O(2) C(1) 126.1(2) . 3_555 1_555 yes Ni O(3) C(8) 126.8(2) . 1_555 1_555 yes Ni N(1) O(1) 123.7(2) . 3_555 1_555 yes Ni N(1) C(7) 124.4(2) . 3_555 1_555 yes O(1) N(1) C(7) 110.9(2) . 1_555 1_555 yes O(2) C(1) C(2) 120.5(2) . 1_555 1_555 yes O(2) C(1) C(6) 121.9(2) . 1_555 1_555 yes C(2) C(1) C(6) 117.5(2) . 1_555 1_555 yes C(1) C(2) C(3) 120.7(3) . 1_555 1_555 yes C(1) C(2) C(7) 124.2(2) . 1_555 1_555 yes C(3) C(2) C(7) 115.0(3) . 1_555 1_555 yes C(2) C(3) C(4) 121.0(3) . 1_555 1_555 yes C(3) C(4) C(5) 118.8(3) . 1_555 1_555 yes C(4) C(5) C(6) 122.2(3) . 1_555 1_555 yes C(1) C(6) C(5) 119.3(3) . 1_555 1_555 yes C(1) C(6) C(8) 123.7(2) . 1_555 1_555 yes C(5) C(6) C(8) 116.8(2) . 1_555 1_555 yes N(1) C(7) C(2) 125.2(3) . 1_555 1_555 yes O(3) C(8) O(4) 121.2(3) . 1_555 1_555 yes O(3) C(8) C(6) 121.8(2) . 1_555 1_555 yes O(4) C(8) C(6) 117.0(3) . 1_555 1_555 yes #--------------------------------------------------------------------------- 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 O(1) O(8) 2.706(3) . 3_655 ? O(1) O(7) 3.420(4) . 3_555 ? O(1) O(9) 3.461(4) . 1_554 ? O(1) O(8) 3.528(4) . 2_545 ? O(1) C(3) 3.579(4) . 3_554 ? O(3) O(8) 2.829(3) . 4_455 ? O(3) O(8) 3.542(3) . 1_455 ? O(4) O(6) 2.756(3) . 4_455 ? O(4) O(5) 2.816(3) . 4_555 ? O(4) O(10) 2.825(3) . 4_454 ? O(4) O(8) 3.378(3) . 4_455 ? O(5) O(10) 2.753(3) . 3_556 ? O(5) O(10) 3.093(3) . 1_454 ? O(5) O(8) 3.460(3) . 1_455 ? O(6) O(7) 2.819(3) . . ? O(6) O(10) 2.893(3) . 3_656 ? O(7) O(9) 2.766(4) . . ? O(7) O(8) 2.772(4) . . ? O(7) O(8) 2.781(4) . 4_455 ? O(7) N(1) 3.412(4) . 3_555 ? O(7) C(7) 3.553(4) . 3_555 ? O(7) O(9) 3.572(4) . 3_656 ? O(8) C(8) 3.508(4) . 4_555 ? O(9) O(10) 2.797(4) . . ? O(9) O(9) 2.973(7) . 3_656 ? O(9) C(7) 3.369(4) . 3_555 ? O(9) C(3) 3.560(5) . 1_656 ? O(10) C(5) 3.332(4) . 4_556 ? O(10) C(1) 3.562(4) . 1_656 ? O(10) C(2) 3.567(4) . 1_656 ? C(1) C(5) 3.478(4) . 4_555 ? C(5) C(6) 3.444(4) . 4_455 ? #--------------------------------------------------------------------------- data_[Mn{Cu2(HL)(L)}2(H2O)4]4H2O.2dmf _database_code_CSD 162984 #data_General _journal_coden_Cambridge 186 _audit_creation_date 'Wed Nov 1 22:56:37 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 ; Hakozaki 6-10-1, Higashi-ku, Fykuoka 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 ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #--------------------------------------------------------------------------- #-- # TITLE AND AUTHOR LIST _publ_section_title ; inuclear CuII and NiII Complexes of 3-Formylsalicylic Acid Oxime: Cis/trans Topology and Extension of Cis-CuII2 Complex to A Pentanuclear CuIICuIIMnIICuIICuII Complex ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name #_publ_author_footnote #_publ_author_address 'Ikeda, Kazuhide' 'Ohba, Masaaki' 'Okawa, H.' _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. ; _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{Cu2(HL)(L)}2(H2O)4]4H2O.2dmf #--------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C38 H48 Cu4 N6 Mn O26 ' _chemical_formula_moiety '?' _chemical_formula_weight 1313.94 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.2151(7) _cell_length_b 13.1298(7) _cell_length_c 8.2073(4) _cell_angle_alpha 94.744(2) _cell_angle_beta 99.760(2) _cell_angle_gamma 77.517(3) _cell_volume 1161.6(1) _cell_formula_units_Z 1 _cell_measurement_reflns_used 5077 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 183.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.110 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.167 _exptl_absorpt_correction_type none #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10852 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9861 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9861 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 #--------------------------------------------------------------------------- #-- # 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 5246 _reflns_number_gt 3506 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0389 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3506 _refine_ls_number_parameters 340 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_shift/su_max 0.0143 _refine_diff_density_max 0.41 _refine_diff_density_min -0.55 _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) ; 'Mn' 'Mn' 0.337 0.728 ;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) ; #--------------------------------------------------------------------------- #-- # 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 -0.13013(4) 0.53641(3) 0.10908(5) 0.0159(1) Uani 1.00 d . . . Cu(2) Cu 0.00768(4) 0.34690(3) 0.28974(5) 0.0174(1) Uani 1.00 d . . . Mn Mn 0.0000 0.0000 0.5000 0.0237(2) Uani 1.00 d S . . O(1) O -0.3139(2) 0.6410(2) -0.1475(3) 0.0268(7) Uani 1.00 d . . . O(2) O -0.1446(2) 0.3941(2) 0.1446(3) 0.0179(6) Uani 1.00 d . . . O(3) O -0.0269(2) 0.2161(2) 0.3140(3) 0.0231(7) Uani 1.00 d . . . O(4) O -0.1336(3) 0.0933(2) 0.3038(4) 0.0290(7) Uani 1.00 d . . . O(5) O -0.1248(2) 0.7177(2) -0.0614(3) 0.0220(7) Uani 1.00 d . . . O(6) O 0.0162(2) 0.4893(2) 0.2708(3) 0.0178(6) Uani 1.00 d . . . O(7) O 0.1377(2) 0.3246(2) 0.4718(3) 0.0212(7) Uani 1.00 d . . . O(8) O 0.2565(2) 0.3739(2) 0.6931(3) 0.0210(6) Uani 1.00 d . . . O(9) O -0.1177(3) 0.0474(2) 0.6918(4) 0.0356(8) Uani 1.00 d . . . O(10) O 0.1000(3) 0.1207(2) 0.5945(4) 0.0404(9) Uani 1.00 d . . . O(11) O -0.1175(4) 0.9365(2) -0.0367(4) 0.055(1) Uani 1.00 d . . . O(12) O 0.2889(3) 0.1747(2) 0.8140(3) 0.0285(7) Uani 1.00 d . . . O(13) O -0.3559(3) 0.1120(3) 0.5750(4) 0.0424(10) Uani 1.00 d . . . N(1) N -0.2755(3) 0.5507(2) -0.0594(4) 0.0182(7) Uani 1.00 d . . . N(2) N -0.0659(3) 0.6571(2) 0.0704(4) 0.0172(7) Uani 1.00 d . . . N(3) N -0.5089(3) 0.0993(3) 0.3602(4) 0.0304(9) Uani 1.00 d . . . C(1) C -0.2324(3) 0.3396(3) 0.0864(4) 0.0150(8) Uani 1.00 d . . . C(2) C -0.3353(3) 0.3855(3) -0.0283(4) 0.0176(9) Uani 1.00 d . . . C(3) C -0.4269(4) 0.3293(3) -0.0899(5) 0.0237(10) Uani 1.00 d . . . C(4) C -0.4189(4) 0.2294(3) -0.0444(5) 0.030(1) Uani 1.00 d . . . C(5) C -0.3186(4) 0.1843(3) 0.0663(5) 0.0240(10) Uani 1.00 d . . . C(6) C -0.2246(3) 0.2367(3) 0.1354(4) 0.0176(9) Uani 1.00 d . . . C(7) C -0.3499(3) 0.4872(3) -0.0947(4) 0.0190(9) Uani 1.00 d . . . C(8) C -0.1232(4) 0.1796(3) 0.2573(5) 0.0202(9) Uani 1.00 d . . . C(9) C 0.1069(3) 0.5375(3) 0.3465(4) 0.0156(8) Uani 1.00 d . . . C(10) C 0.1117(3) 0.6366(3) 0.2951(4) 0.0184(9) Uani 1.00 d . . . C(11) C 0.2074(4) 0.6853(3) 0.3699(5) 0.0224(10) Uani 1.00 d . . . C(12) C 0.2962(4) 0.6391(3) 0.4942(5) 0.027(1) Uani 1.00 d . . . C(13) C 0.2896(3) 0.5447(3) 0.5471(5) 0.0227(9) Uani 1.00 d . . . C(14) C 0.1950(3) 0.4925(3) 0.4774(4) 0.0176(9) Uani 1.00 d . . . C(15) C 0.0273(3) 0.6892(3) 0.1579(4) 0.0181(9) Uani 1.00 d . . . C(16) C 0.1958(3) 0.3911(3) 0.5509(4) 0.0184(9) Uani 1.00 d . . . C(17) C -0.3945(4) 0.0752(3) 0.4378(5) 0.030(1) Uani 1.00 d . . . C(18) C -0.5464(5) 0.0535(4) 0.1983(6) 0.045(1) Uani 1.00 d . . . C(19) C -0.5996(5) 0.1756(4) 0.4339(7) 0.051(2) Uani 1.00 d . . . H(1) H -0.4857 0.3555 -0.1670 0.0287 Uiso 1.00 calc . . . H(2) H -0.4838 0.1996 -0.0777 0.0287 Uiso 1.00 calc . . . H(3) H -0.3276 0.1244 0.0754 0.0287 Uiso 1.00 calc . . . H(4) H -0.4243 0.5071 -0.1717 0.0287 Uiso 1.00 calc . . . H(5) H 0.2199 0.7503 0.3282 0.0287 Uiso 1.00 calc . . . H(6) H 0.3566 0.6740 0.5353 0.0287 Uiso 1.00 calc . . . H(7) H 0.3350 0.5142 0.6417 0.0287 Uiso 1.00 calc . . . H(8) H 0.0627 0.7553 0.1069 0.0287 Uiso 1.00 calc . . . H(9) H -0.2255 0.6592 -0.1070 0.0287 Uiso 1.00 calc . . . H(10) H -0.1907 0.0648 0.6668 0.0287 Uiso 1.00 calc . . . H(11) H -0.1136 -0.0187 0.7635 0.0287 Uiso 1.00 calc . . . H(12) H 0.0867 0.1657 0.5420 0.0287 Uiso 1.00 calc . . . H(13) H 0.1618 0.1272 0.6757 0.0287 Uiso 1.00 calc . . . H(14) H -0.1115 0.8709 -0.0335 0.0287 Uiso 1.00 calc . . . H(15) H -0.0823 0.9348 0.0729 0.0287 Uiso 1.00 calc . . . H(16) H 0.2474 0.1858 0.9042 0.0287 Uiso 1.00 calc . . . H(17) H 0.2729 0.2326 0.7725 0.0287 Uiso 1.00 calc . . . H(18) H -0.3510 0.0241 0.3651 0.0287 Uiso 1.00 calc . . . H(19) H -0.4754 0.0136 0.1390 0.0287 Uiso 1.00 calc . . . H(20) H -0.6135 0.0248 0.1978 0.0287 Uiso 1.00 calc . . . H(21) H -0.5812 0.1247 0.1213 0.0287 Uiso 1.00 calc . . . H(22) H -0.6818 0.1584 0.4036 0.0287 Uiso 1.00 calc . . . H(23) H -0.6186 0.2313 0.3792 0.0287 Uiso 1.00 calc . . . H(24) H -0.5841 0.1950 0.5496 0.0287 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) 0.0183(2) 0.0135(2) 0.0150(2) -0.0026(2) -0.0006(2) 0.0046(2) Cu(2) 0.0179(2) 0.0145(2) 0.0192(2) -0.0044(2) -0.0035(2) 0.0068(2) Mn 0.0248(4) 0.0210(4) 0.0247(4) -0.0089(3) -0.0047(4) 0.0040(3) O(1) 0.028(2) 0.019(1) 0.029(1) -0.001(1) -0.009(1) 0.013(1) O(2) 0.018(1) 0.015(1) 0.020(1) -0.0032(10) -0.001(1) 0.005(1) O(3) 0.021(1) 0.020(1) 0.028(1) -0.008(1) -0.006(1) 0.010(1) O(4) 0.028(2) 0.022(1) 0.039(2) -0.012(1) -0.007(1) 0.018(1) O(5) 0.030(1) 0.017(1) 0.019(1) -0.003(1) -0.001(1) 0.009(1) O(6) 0.019(1) 0.014(1) 0.019(1) -0.004(1) -0.003(1) 0.0037(10) O(7) 0.022(1) 0.018(1) 0.021(1) -0.006(1) -0.006(1) 0.007(1) O(8) 0.024(1) 0.023(1) 0.015(1) -0.004(1) -0.001(1) 0.003(1) O(9) 0.031(2) 0.036(2) 0.038(2) -0.001(1) 0.004(1) 0.011(1) O(10) 0.056(2) 0.027(2) 0.038(2) -0.022(1) -0.021(2) 0.021(1) O(11) 0.099(3) 0.029(2) 0.036(2) -0.018(2) -0.001(2) 0.010(1) O(12) 0.028(2) 0.026(1) 0.029(1) -0.003(1) 0.002(1) 0.003(1) O(13) 0.041(2) 0.047(2) 0.039(2) -0.008(2) 0.004(2) 0.003(2) N(1) 0.024(2) 0.014(1) 0.015(1) 0.000(1) 0.005(1) 0.005(1) N(2) 0.023(2) 0.013(1) 0.016(1) 0.000(1) 0.004(1) 0.005(1) N(3) 0.029(2) 0.033(2) 0.028(2) 0.002(2) 0.007(2) 0.008(2) C(1) 0.013(2) 0.018(2) 0.015(2) -0.006(1) 0.003(1) 0.000(1) C(2) 0.018(2) 0.018(2) 0.015(2) -0.001(1) 0.002(1) 0.004(1) C(3) 0.021(2) 0.026(2) 0.021(2) -0.005(2) -0.007(2) 0.005(2) C(4) 0.023(2) 0.032(2) 0.036(2) -0.013(2) -0.006(2) 0.004(2) C(5) 0.028(2) 0.020(2) 0.026(2) -0.011(2) 0.001(2) 0.005(2) C(6) 0.017(2) 0.017(2) 0.019(2) -0.003(1) 0.001(1) 0.004(1) C(7) 0.016(2) 0.021(2) 0.017(2) 0.001(1) -0.002(1) 0.004(1) C(8) 0.024(2) 0.017(2) 0.020(2) -0.002(2) 0.006(2) 0.004(1) C(9) 0.017(2) 0.016(2) 0.015(2) -0.004(1) 0.006(1) -0.002(1) C(10) 0.022(2) 0.016(2) 0.016(2) -0.002(1) 0.003(2) 0.003(1) C(11) 0.026(2) 0.022(2) 0.022(2) -0.011(2) 0.005(2) 0.000(2) C(12) 0.028(2) 0.029(2) 0.028(2) -0.016(2) 0.003(2) -0.004(2) C(13) 0.020(2) 0.029(2) 0.018(2) -0.005(2) 0.003(2) 0.002(2) C(14) 0.017(2) 0.020(2) 0.017(2) -0.006(1) 0.004(1) -0.002(1) C(15) 0.020(2) 0.016(2) 0.019(2) -0.002(1) 0.007(2) 0.002(1) C(16) 0.012(2) 0.021(2) 0.020(2) 0.000(1) 0.002(1) 0.003(1) C(17) 0.029(2) 0.032(2) 0.032(2) -0.004(2) 0.011(2) 0.006(2) C(18) 0.042(3) 0.064(3) 0.034(3) -0.020(2) 0.004(2) 0.005(2) C(19) 0.044(3) 0.052(3) 0.050(3) 0.021(2) 0.019(3) 0.019(3) #--------------------------------------------------------------------------- #-- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _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(2) 1.960(2) . . yes Cu(1) O(6) 1.948(2) . . yes Cu(1) O(8) 2.402(3) . 2_566 yes Cu(1) N(1) 1.937(3) . . yes Cu(1) N(2) 1.946(3) . . yes Cu(2) O(2) 1.922(2) . . yes Cu(2) O(3) 1.873(3) . . yes Cu(2) O(5) 2.459(3) . 2_565 yes Cu(2) O(6) 1.913(2) . . yes Cu(2) O(7) 1.896(2) . . yes Mn O(4) 2.248(2) . . yes Mn O(4) 2.248(2) . 2_556 yes Mn O(9) 2.190(3) . . yes Mn O(9) 2.190(3) . 2_556 yes Mn O(10) 2.155(3) . . yes Mn O(10) 2.155(3) . 2_556 yes O(1) N(1) 1.388(4) . . yes O(1) H(9) 1.062 . . no O(2) C(1) 1.340(4) . . yes O(3) C(8) 1.277(5) . . yes O(4) C(8) 1.259(4) . . yes O(5) N(2) 1.383(3) . . yes O(6) C(9) 1.349(4) . . yes O(7) C(16) 1.272(4) . . yes O(8) C(16) 1.259(4) . . yes O(9) H(10) 0.796 . . no O(9) H(11) 1.077 . . no O(10) H(12) 0.734 . . no O(10) H(13) 0.889 . . no O(11) H(14) 0.852 . . no O(11) H(15) 0.919 . . no O(12) H(16) 0.925 . . no O(12) H(17) 0.830 . . no O(13) C(17) 1.235(5) . . yes N(1) C(7) 1.287(5) . . yes N(2) C(15) 1.293(5) . . yes N(3) C(17) 1.317(5) . . yes N(3) C(18) 1.446(6) . . yes N(3) C(19) 1.439(6) . . yes C(1) C(2) 1.416(5) . . yes C(1) C(6) 1.422(5) . . yes C(2) C(3) 1.394(5) . . yes C(2) C(7) 1.450(5) . . yes C(3) C(4) 1.373(5) . . yes C(3) H(1) 0.866 . . no C(4) C(5) 1.376(5) . . yes C(4) H(2) 0.893 . . no C(5) C(6) 1.397(5) . . yes C(5) H(3) 0.826 . . no C(6) C(8) 1.492(5) . . yes C(7) H(4) 0.958 . . no C(9) C(10) 1.415(5) . . yes C(9) C(14) 1.405(5) . . yes C(10) C(11) 1.395(5) . . yes C(10) C(15) 1.458(5) . . yes C(11) C(12) 1.377(5) . . yes C(11) H(5) 0.990 . . no C(12) C(13) 1.368(5) . . yes C(12) H(6) 0.902 . . no C(13) C(14) 1.401(5) . . yes C(13) H(7) 0.923 . . no C(14) C(16) 1.505(5) . . yes C(15) H(8) 1.162 . . no C(17) H(18) 0.967 . . no C(18) H(19) 1.027 . . no C(18) H(20) 0.911 . . no C(18) H(21) 1.133 . . no C(19) H(22) 0.983 . . no C(19) H(23) 0.858 . . no C(19) H(24) 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(2) Cu(1) O(6) 77.75(10) . 1_555 1_555 yes O(2) Cu(1) O(8) 97.69(10) . 1_555 2_566 yes O(2) Cu(1) N(1) 90.2(1) . 1_555 1_555 yes O(2) Cu(1) N(2) 163.1(1) . 1_555 1_555 yes O(6) Cu(1) O(8) 95.78(9) . 1_555 2_566 yes O(6) Cu(1) N(1) 167.4(1) . 1_555 1_555 yes O(6) Cu(1) N(2) 90.2(1) . 1_555 1_555 yes O(8) Cu(1) N(1) 89.5(1) . 2_566 1_555 yes O(8) Cu(1) N(2) 95.3(1) . 2_566 1_555 yes N(1) Cu(1) N(2) 100.7(1) . 1_555 1_555 yes O(2) Cu(2) O(3) 94.1(1) . 1_555 1_555 yes O(2) Cu(2) O(5) 93.78(10) . 1_555 2_565 yes O(2) Cu(2) O(6) 79.51(10) . 1_555 1_555 yes O(2) Cu(2) O(7) 165.5(1) . 1_555 1_555 yes O(3) Cu(2) O(5) 93.3(1) . 1_555 2_565 yes O(3) Cu(2) O(6) 170.7(1) . 1_555 1_555 yes O(3) Cu(2) O(7) 90.3(1) . 1_555 1_555 yes O(5) Cu(2) O(6) 93.81(10) . 2_565 1_555 yes O(5) Cu(2) O(7) 99.8(1) . 2_565 1_555 yes O(6) Cu(2) O(7) 94.4(1) . 1_555 1_555 yes O(4) Mn O(4) 180.0 . 1_555 2_556 yes O(4) Mn O(9) 94.5(1) . 1_555 1_555 yes O(4) Mn O(9) 85.5(1) . 1_555 2_556 yes O(4) Mn O(10) 96.72(10) . 1_555 1_555 yes O(4) Mn O(10) 83.28(10) . 1_555 2_556 yes O(4) Mn O(9) 85.5(1) . 2_556 1_555 yes O(4) Mn O(9) 94.5(1) . 2_556 2_556 yes O(4) Mn O(10) 83.28(10) . 2_556 1_555 yes O(4) Mn O(10) 96.72(10) . 2_556 2_556 yes O(9) Mn O(9) 180.0 . 1_555 2_556 yes O(9) Mn O(10) 89.4(1) . 1_555 1_555 yes O(9) Mn O(10) 90.6(1) . 1_555 2_556 yes O(9) Mn O(10) 90.6(1) . 2_556 1_555 yes O(9) Mn O(10) 89.4(1) . 2_556 2_556 yes O(10) Mn O(10) 180.0 . 1_555 2_556 yes N(1) O(1) H(9) 89.1 . 1_555 1_555 no Cu(1) O(2) Cu(2) 100.8(1) . 1_555 1_555 yes Cu(1) O(2) C(1) 132.0(2) . 1_555 1_555 yes Cu(2) O(2) C(1) 127.1(2) . 1_555 1_555 yes Cu(2) O(3) C(8) 130.1(2) . 1_555 1_555 yes Mn O(4) C(8) 124.9(3) . 1_555 1_555 yes Cu(2) O(5) N(2) 105.5(2) . 2_565 1_555 yes Cu(1) O(6) Cu(2) 101.6(1) . 1_555 1_555 yes Cu(1) O(6) C(9) 131.8(2) . 1_555 1_555 yes Cu(2) O(6) C(9) 126.6(2) . 1_555 1_555 yes Cu(2) O(7) C(16) 127.9(2) . 1_555 1_555 yes Cu(1) O(8) C(16) 107.7(2) . 2_566 1_555 yes Mn O(9) H(10) 120.2 . 1_555 1_555 no Mn O(9) H(11) 109.3 . 1_555 1_555 no H(10) O(9) H(11) 99.7 . 1_555 1_555 no Mn O(10) H(12) 114.1 . 1_555 1_555 no Mn O(10) H(13) 135.9 . 1_555 1_555 no H(12) O(10) H(13) 109.4 . 1_555 1_555 no H(14) O(11) H(15) 86.5 . 1_555 1_555 no H(16) O(12) H(17) 104.0 . 1_555 1_555 no Cu(1) N(1) O(1) 119.8(2) . 1_555 1_555 yes Cu(1) N(1) C(7) 126.9(2) . 1_555 1_555 yes O(1) N(1) C(7) 113.1(3) . 1_555 1_555 yes Cu(1) N(2) O(5) 118.5(2) . 1_555 1_555 yes Cu(1) N(2) C(15) 126.7(2) . 1_555 1_555 yes O(5) N(2) C(15) 114.8(3) . 1_555 1_555 yes C(17) N(3) C(18) 121.7(4) . 1_555 1_555 yes C(17) N(3) C(19) 120.0(4) . 1_555 1_555 yes C(18) N(3) C(19) 118.2(4) . 1_555 1_555 yes O(2) C(1) C(2) 119.1(3) . 1_555 1_555 yes O(2) C(1) C(6) 121.9(3) . 1_555 1_555 yes C(2) C(1) C(6) 119.0(3) . 1_555 1_555 yes C(1) C(2) C(3) 119.5(3) . 1_555 1_555 yes C(1) C(2) C(7) 124.1(3) . 1_555 1_555 yes C(3) C(2) C(7) 116.3(3) . 1_555 1_555 yes C(2) C(3) C(4) 121.6(3) . 1_555 1_555 yes C(2) C(3) H(1) 118.8 . 1_555 1_555 no C(4) C(3) H(1) 119.2 . 1_555 1_555 no C(3) C(4) C(5) 119.1(4) . 1_555 1_555 yes C(3) C(4) H(2) 118.1 . 1_555 1_555 no C(5) C(4) H(2) 122.3 . 1_555 1_555 no C(4) C(5) C(6) 122.4(3) . 1_555 1_555 yes C(4) C(5) H(3) 105.7 . 1_555 1_555 no C(6) C(5) H(3) 131.9 . 1_555 1_555 no C(1) C(6) C(5) 118.4(3) . 1_555 1_555 yes C(1) C(6) C(8) 124.9(3) . 1_555 1_555 yes C(5) C(6) C(8) 116.8(3) . 1_555 1_555 yes N(1) C(7) C(2) 126.9(3) . 1_555 1_555 yes N(1) C(7) H(4) 118.9 . 1_555 1_555 no C(2) C(7) H(4) 114.1 . 1_555 1_555 no O(3) C(8) O(4) 119.8(3) . 1_555 1_555 yes O(3) C(8) C(6) 121.4(3) . 1_555 1_555 yes O(4) C(8) C(6) 118.8(3) . 1_555 1_555 yes O(6) C(9) C(10) 119.2(3) . 1_555 1_555 yes O(6) C(9) C(14) 121.5(3) . 1_555 1_555 yes C(10) C(9) C(14) 119.3(3) . 1_555 1_555 yes C(9) C(10) C(11) 119.4(3) . 1_555 1_555 yes C(9) C(10) C(15) 124.0(3) . 1_555 1_555 yes C(11) C(10) C(15) 116.5(3) . 1_555 1_555 yes C(10) C(11) C(12) 121.1(3) . 1_555 1_555 yes C(10) C(11) H(5) 121.7 . 1_555 1_555 no C(12) C(11) H(5) 116.9 . 1_555 1_555 no C(11) C(12) C(13) 119.5(4) . 1_555 1_555 yes C(11) C(12) H(6) 116.6 . 1_555 1_555 no C(13) C(12) H(6) 123.9 . 1_555 1_555 no C(12) C(13) C(14) 121.8(3) . 1_555 1_555 yes C(12) C(13) H(7) 125.4 . 1_555 1_555 no C(14) C(13) H(7) 111.8 . 1_555 1_555 no C(9) C(14) C(13) 118.8(3) . 1_555 1_555 yes C(9) C(14) C(16) 124.7(3) . 1_555 1_555 yes C(13) C(14) C(16) 116.5(3) . 1_555 1_555 yes N(2) C(15) C(10) 126.6(3) . 1_555 1_555 yes N(2) C(15) H(8) 117.8 . 1_555 1_555 no C(10) C(15) H(8) 114.0 . 1_555 1_555 no O(7) C(16) O(8) 121.1(3) . 1_555 1_555 yes O(7) C(16) C(14) 121.2(3) . 1_555 1_555 yes O(8) C(16) C(14) 117.8(3) . 1_555 1_555 yes O(13) C(17) N(3) 125.2(4) . 1_555 1_555 yes O(13) C(17) H(18) 129.5 . 1_555 1_555 no N(3) C(17) H(18) 105.3 . 1_555 1_555 no N(3) C(18) H(19) 115.3 . 1_555 1_555 no N(3) C(18) H(20) 110.8 . 1_555 1_555 no N(3) C(18) H(21) 102.1 . 1_555 1_555 no H(19) C(18) H(20) 119.2 . 1_555 1_555 no H(19) C(18) H(21) 101.1 . 1_555 1_555 no H(20) C(18) H(21) 105.6 . 1_555 1_555 no N(3) C(19) H(22) 110.5 . 1_555 1_555 no N(3) C(19) H(23) 109.6 . 1_555 1_555 no N(3) C(19) H(24) 119.9 . 1_555 1_555 no H(22) C(19) H(23) 94.5 . 1_555 1_555 no H(22) C(19) H(24) 110.8 . 1_555 1_555 no H(23) C(19) H(24) 108.6 . 1_555 1_555 no #--------------------------------------------------------------------------- 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 O(1) C(19) 3.380(5) . 2_465 ? O(1) O(12) 3.516(4) . 2_566 ? O(3) O(11) 3.303(5) . 2_565 ? O(4) O(11) 3.338(5) . 1_545 ? O(4) C(17) 3.357(5) . . ? O(4) O(13) 3.573(4) . . ? O(5) O(11) 2.881(4) . . ? O(5) O(12) 3.029(4) . 2_566 ? O(7) C(19) 3.212(5) . 1_655 ? O(7) O(12) 3.534(4) . . ? O(8) O(12) 2.802(4) . . ? O(8) C(19) 3.513(6) . 1_655 ? O(9) O(13) 2.657(4) . . ? O(9) O(11) 2.760(4) . 1_546 ? O(9) C(17) 3.399(5) . . ? O(9) O(11) 3.554(5) . 2_566 ? O(10) O(12) 2.716(4) . . ? O(11) O(11) 3.360(8) . 2_575 ? O(11) O(12) 3.466(5) . 2_566 ? O(11) C(8) 3.509(6) . 2_565 ? O(12) N(2) 3.179(4) . 2_566 ? O(12) C(4) 3.492(5) . 1_656 ? O(12) C(19) 3.553(6) . 1_655 ? O(12) C(16) 3.576(4) . . ? O(13) C(11) 3.395(5) . 2_566 ? O(13) C(18) 3.430(6) . 2_456 ? O(13) C(4) 3.481(6) . 1_556 ? O(13) N(3) 3.550(5) . 2_456 ? O(13) C(12) 3.582(5) . 2_566 ? N(3) C(17) 3.387(5) . 2_456 ? N(3) N(3) 3.565(7) . 2_456 ? C(3) C(7) 3.527(5) . 2_465 ? C(16) C(19) 3.418(6) . 1_655 ? C(17) C(19) 3.555(7) . 2_456 ? #---------------------------------------------------------------------------