#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cao, Rong' 'Hong, Maochun' 'Liang, Yucang' 'Shi, Qian' 'Su, Weiping' 'Sun, Daofeng' _publ_contact_author_name 'Prof Maochun Hong' _publ_contact_author_address ; Prof Maochun Hong State Key Lab of Structural Chemistry, Fujian Inst of Research on Structure of M Chinese Academy of Sciences Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email 'HMC@MS.FJIRSM.AC.CN' _publ_section_title ; Hydrothermal syntheses, structures and properties of terephthalate-bridged polymeric complexes with zig-zag chain and rhombus channel structures ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; data_[Co(ta)(phen)(H2O)]n _database_code_CSD 151561 #-------------------------------------------------------------------- _audit_creation_date 'Sun Mar 12 09:33:45 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #-------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #-------------------------------------------------------------------- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 421.27 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H14 Co N2 O5 ' _chemical_formula_moiety 'C20 H14 Co N2 O5 ' _chemical_formula_structural ? _chemical_melting_point ? #-------------------------------------------------------------------- _cell_length_a 9.279(1) _cell_length_b 10.3777(9) _cell_length_c 11.271(1) _cell_angle_alpha 112.207(2) _cell_angle_beta 94.849(3) _cell_angle_gamma 114.170(4) _cell_volume 879.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #-------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #-------------------------------------------------------------------- _exptl_crystal_description 'rhombic' _exptl_crystal_colour 'violet-red' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 430.00 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #-------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku unknown' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3961 _reflns_number_total 3961 _reflns_number_gt 3450 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.021 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #-------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Co' 'Co' 0.349 0.972 ;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) ; '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) ; #-------------------------------------------------------------------- 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co -0.01593(3) 0.88959(3) 0.21412(3) 0.02016(8) Uani 1.00 d . . . O O -0.1842(2) 0.7903(2) 0.3035(1) 0.0254(4) Uani 1.00 d . . . O(11) O 0.1898(2) 1.0971(2) 0.2612(1) 0.0285(4) Uani 1.00 d . . . O(12) O 0.1069(2) 1.1550(2) 0.4415(1) 0.0328(4) Uani 1.00 d . . . O(21) O -0.1834(2) 0.9226(2) 0.1230(1) 0.0267(4) Uani 1.00 d . . . O(22) O -0.3231(2) 0.9532(2) 0.2744(1) 0.0324(5) Uani 1.00 d . . . N(1) N 0.1368(2) 0.8055(2) 0.2774(2) 0.0236(5) Uani 1.00 d . . . N(2) N 0.0191(2) 0.7643(2) 0.0339(2) 0.0217(4) Uani 1.00 d . . . C(1) C 0.1975(3) 0.8301(3) 0.3998(2) 0.0320(6) Uani 1.00 d . . . C(01) C 0.1875(2) 0.7287(2) 0.1772(2) 0.0223(5) Uani 1.00 d . . . C(2) C 0.3092(3) 0.7810(3) 0.4288(2) 0.0390(7) Uani 1.00 d . . . C(02) C 0.1237(2) 0.7060(2) 0.0457(2) 0.0215(5) Uani 1.00 d . . . C(3) C 0.3598(3) 0.7034(3) 0.3283(3) 0.0372(7) Uani 1.00 d . . . C(4) C 0.2989(3) 0.6740(2) 0.1968(2) 0.0283(6) Uani 1.00 d . . . C(5) C 0.3444(3) 0.5945(3) 0.0845(3) 0.0343(7) Uani 1.00 d . . . C(6) C 0.2848(3) 0.5734(3) -0.0384(2) 0.0328(6) Uani 1.00 d . . . C(7) C 0.1730(3) 0.6296(2) -0.0620(2) 0.0259(6) Uani 1.00 d . . . C(8) C 0.1101(3) 0.6166(3) -0.1864(2) 0.0319(6) Uani 1.00 d . . . C(9) C 0.0073(3) 0.6776(3) -0.1974(2) 0.0325(6) Uani 1.00 d . . . C(10) C -0.0359(3) 0.7505(2) -0.0855(2) 0.0276(6) Uani 1.00 d . . . C(11) C 0.2080(2) 1.1915(2) 0.3781(2) 0.0203(5) Uani 1.00 d . . . C(12) C 0.3585(2) 1.3516(2) 0.4410(2) 0.0182(5) Uani 1.00 d . . . C(13) C 0.3792(3) 1.4680(2) 0.5647(2) 0.0246(5) Uani 1.00 d . . . C(14) C 0.5194(3) 1.6147(2) 0.6234(2) 0.0250(5) Uani 1.00 d . . . C(21) C -0.2945(2) 0.9502(2) 0.1672(2) 0.0211(5) Uani 1.00 d . . . C(22) C -0.4004(2) 0.9772(2) 0.0811(2) 0.0191(5) Uani 1.00 d . . . C(23) C -0.3862(2) 0.9549(2) -0.0461(2) 0.0205(5) Uani 1.00 d . . . C(24) C -0.4847(2) 0.9776(2) -0.1265(2) 0.0209(5) Uani 1.00 d . . . H(1) H 0.1625 0.8842 0.4717 0.0382 Uiso 1.00 calc . . . H(2) H 0.3504 0.8019 0.5188 0.0463 Uiso 1.00 calc . . . H(3) H 0.4356 0.6675 0.3473 0.0446 Uiso 1.00 calc . . . H(5) H 0.4205 0.5567 0.0975 0.0407 Uiso 1.00 calc . . . H(6) H 0.3165 0.5185 -0.1123 0.0392 Uiso 1.00 calc . . . H(8) H 0.1384 0.5640 -0.2643 0.0372 Uiso 1.00 calc . . . H(9) H -0.0343 0.6706 -0.2820 0.0387 Uiso 1.00 calc . . . H(10) H -0.1083 0.7939 -0.0938 0.0326 Uiso 1.00 calc . . . H(13A) H 0.5321 1.6937 0.7086 0.0289 Uiso 1.00 calc . . . H(13B) H 0.5321 1.6937 0.7086 0.0289 Uiso 1.00 calc . . . H(23) H -0.3069 0.9241 -0.0772 0.0236 Uiso 1.00 calc . . . H(24) H -0.4749 0.9619 -0.2145 0.0251 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 Co 0.0191(2) 0.0222(2) 0.0210(2) 0.0099(1) 0.0075(1) 0.0109(1) O 0.0272(8) 0.0260(7) 0.0226(8) 0.0095(6) 0.0102(6) 0.0134(6) O(11) 0.0267(8) 0.0223(7) 0.0236(8) 0.0067(6) 0.0071(7) 0.0034(6) O(12) 0.0239(8) 0.0376(9) 0.0243(8) 0.0029(7) 0.0062(7) 0.0150(7) O(21) 0.0243(8) 0.0428(9) 0.0281(8) 0.0221(7) 0.0140(7) 0.0222(7) O(22) 0.0327(9) 0.054(1) 0.0222(8) 0.0277(8) 0.0125(7) 0.0193(8) N(1) 0.0247(10) 0.0252(9) 0.0209(9) 0.0118(8) 0.0055(8) 0.0107(8) N(2) 0.0193(9) 0.0206(8) 0.0216(9) 0.0075(7) 0.0035(7) 0.0086(7) C(1) 0.036(1) 0.035(1) 0.025(1) 0.018(1) 0.007(1) 0.012(1) C(01) 0.021(1) 0.0193(10) 0.025(1) 0.0073(8) 0.0056(9) 0.0106(9) C(2) 0.043(2) 0.048(1) 0.031(1) 0.025(1) 0.003(1) 0.020(1) C(02) 0.020(1) 0.0171(9) 0.024(1) 0.0062(8) 0.0052(9) 0.0080(9) C(3) 0.035(1) 0.043(1) 0.042(1) 0.024(1) 0.005(1) 0.021(1) C(4) 0.026(1) 0.028(1) 0.034(1) 0.0141(10) 0.008(1) 0.016(1) C(5) 0.034(1) 0.032(1) 0.044(1) 0.022(1) 0.013(1) 0.015(1) C(6) 0.035(1) 0.028(1) 0.037(1) 0.019(1) 0.016(1) 0.010(1) C(7) 0.027(1) 0.0186(10) 0.027(1) 0.0091(9) 0.0094(10) 0.0066(9) C(8) 0.037(1) 0.029(1) 0.021(1) 0.013(1) 0.011(1) 0.0056(9) C(9) 0.037(1) 0.037(1) 0.020(1) 0.016(1) 0.005(1) 0.0111(10) C(10) 0.025(1) 0.028(1) 0.025(1) 0.0108(9) 0.0033(9) 0.0108(10) C(11) 0.020(1) 0.0219(10) 0.021(1) 0.0101(8) 0.0036(9) 0.0112(9) C(12) 0.018(1) 0.0200(9) 0.0174(10) 0.0092(8) 0.0047(8) 0.0094(8) C(13) 0.024(1) 0.026(1) 0.021(1) 0.0097(9) 0.0127(9) 0.0094(9) C(14) 0.027(1) 0.022(1) 0.019(1) 0.0103(9) 0.0103(9) 0.0031(9) C(21) 0.018(1) 0.0221(10) 0.020(1) 0.0081(8) 0.0052(9) 0.0081(9) C(22) 0.016(1) 0.0184(10) 0.0187(10) 0.0060(8) 0.0048(8) 0.0063(8) C(23) 0.017(1) 0.0233(10) 0.021(1) 0.0106(8) 0.0084(8) 0.0079(9) C(24) 0.021(1) 0.0235(10) 0.0169(10) 0.0103(8) 0.0083(8) 0.0078(8) #-------------------------------------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3450 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0406 _refine_ls_wR_factor_gt 0.0406 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.516 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.21 _refine_diff_density_max 0.39 #-------------------------------------------------------------------- _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 Co O 2.061(1) 1_555 1_555 yes Co O(11) 2.040(1) 1_555 1_555 yes Co O(21) 2.005(1) 1_555 1_555 yes Co N(1) 2.143(2) 1_555 1_555 yes Co N(2) 2.094(2) 1_555 1_555 yes O(11) C(11) 1.255(2) 1_555 1_555 yes O(12) C(11) 1.249(2) 1_555 1_555 yes O(21) C(21) 1.271(2) 1_555 1_555 yes O(22) C(21) 1.250(2) 1_555 1_555 yes N(1) C(1) 1.331(3) 1_555 1_555 yes N(1) C(01) 1.359(3) 1_555 1_555 yes N(2) C(02) 1.359(3) 1_555 1_555 yes N(2) C(10) 1.330(3) 1_555 1_555 yes C(1) C(2) 1.394(3) 1_555 1_555 yes C(01) C(02) 1.441(3) 1_555 1_555 yes C(01) C(4) 1.405(3) 1_555 1_555 yes C(2) C(3) 1.364(4) 1_555 1_555 yes C(02) C(7) 1.405(3) 1_555 1_555 yes C(3) C(4) 1.409(3) 1_555 1_555 yes C(4) C(5) 1.432(3) 1_555 1_555 yes C(5) C(6) 1.347(3) 1_555 1_555 yes C(6) C(7) 1.433(3) 1_555 1_555 yes C(7) C(8) 1.407(3) 1_555 1_555 yes C(8) C(9) 1.363(3) 1_555 1_555 yes C(9) C(10) 1.392(3) 1_555 1_555 yes C(11) C(12) 1.502(3) 1_555 1_555 yes C(12) C(13) 1.390(3) 1_555 1_555 yes C(12) C(14) 1.393(3) 1_555 2_686 yes C(13) C(14) 1.385(3) 1_555 1_555 yes C(21) C(22) 1.502(3) 1_555 1_555 yes C(22) C(23) 1.390(3) 1_555 1_555 yes C(22) C(24) 1.393(3) 1_555 2_475 yes C(23) C(24) 1.381(3) 1_555 1_555 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 Co O(11) 139.32(6) 1_555 1_555 1_555 yes O Co O(21) 89.05(6) 1_555 1_555 1_555 yes O Co N(1) 89.64(6) 1_555 1_555 1_555 yes O Co N(2) 125.42(6) 1_555 1_555 1_555 yes O(11) Co O(21) 99.42(6) 1_555 1_555 1_555 yes O(11) Co N(1) 89.30(6) 1_555 1_555 1_555 yes O(11) Co N(2) 94.03(6) 1_555 1_555 1_555 yes O(21) Co N(1) 168.01(6) 1_555 1_555 1_555 yes O(21) Co N(2) 92.95(6) 1_555 1_555 1_555 yes N(1) Co N(2) 78.15(6) 1_555 1_555 1_555 yes Co O(11) C(11) 106.5(1) 1_555 1_555 1_555 yes Co O(21) C(21) 127.1(1) 1_555 1_555 1_555 yes Co N(1) C(1) 129.1(1) 1_555 1_555 1_555 yes Co N(1) C(01) 113.0(1) 1_555 1_555 1_555 yes C(1) N(1) C(01) 117.6(2) 1_555 1_555 1_555 yes Co N(2) C(02) 114.8(1) 1_555 1_555 1_555 yes Co N(2) C(10) 127.1(1) 1_555 1_555 1_555 yes C(02) N(2) C(10) 117.7(2) 1_555 1_555 1_555 yes N(1) C(1) C(2) 123.0(2) 1_555 1_555 1_555 yes N(1) C(1) H(1) 118.5(2) 1_555 1_555 1_555 no C(2) C(1) H(1) 118.5(2) 1_555 1_555 1_555 no N(1) C(01) C(02) 117.1(2) 1_555 1_555 1_555 yes N(1) C(01) C(4) 123.3(2) 1_555 1_555 1_555 yes C(02) C(01) C(4) 119.6(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.5(2) 1_555 1_555 1_555 yes C(1) C(2) H(2) 120.2(2) 1_555 1_555 1_555 no C(3) C(2) H(2) 120.4(2) 1_555 1_555 1_555 no N(2) C(02) C(01) 116.7(2) 1_555 1_555 1_555 yes N(2) C(02) C(7) 123.3(2) 1_555 1_555 1_555 yes C(01) C(02) C(7) 120.0(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.7(2) 1_555 1_555 1_555 yes C(2) C(3) H(3) 120.0(2) 1_555 1_555 1_555 no C(4) C(3) H(3) 120.3(2) 1_555 1_555 1_555 no C(01) C(4) C(3) 116.8(2) 1_555 1_555 1_555 yes C(01) C(4) C(5) 118.9(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 124.3(2) 1_555 1_555 1_555 yes C(4) C(5) C(6) 121.4(2) 1_555 1_555 1_555 yes C(4) C(5) H(5) 119.2(2) 1_555 1_555 1_555 no C(6) C(5) H(5) 119.4(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 121.3(2) 1_555 1_555 1_555 yes C(5) C(6) H(6) 119.7(2) 1_555 1_555 1_555 no C(7) C(6) H(6) 119.0(2) 1_555 1_555 1_555 no C(02) C(7) C(6) 118.7(2) 1_555 1_555 1_555 yes C(02) C(7) C(8) 116.7(2) 1_555 1_555 1_555 yes C(6) C(7) C(8) 124.5(2) 1_555 1_555 1_555 yes C(7) C(8) C(9) 119.8(2) 1_555 1_555 1_555 yes C(7) C(8) H(8) 120.4(2) 1_555 1_555 1_555 no C(9) C(8) H(8) 119.7(2) 1_555 1_555 1_555 no C(8) C(9) C(10) 119.6(2) 1_555 1_555 1_555 yes C(8) C(9) H(9) 120.0(2) 1_555 1_555 1_555 no C(10) C(9) H(9) 120.4(2) 1_555 1_555 1_555 no N(2) C(10) C(9) 122.9(2) 1_555 1_555 1_555 yes N(2) C(10) H(10) 118.0(2) 1_555 1_555 1_555 no C(9) C(10) H(10) 119.2(2) 1_555 1_555 1_555 no O(11) C(11) O(12) 122.1(2) 1_555 1_555 1_555 yes O(11) C(11) C(12) 117.4(2) 1_555 1_555 1_555 yes O(12) C(11) C(12) 120.5(2) 1_555 1_555 1_555 yes C(11) C(12) C(13) 120.7(2) 1_555 1_555 1_555 yes C(11) C(12) C(14) 120.4(2) 1_555 1_555 2_686 yes C(13) C(12) C(14) 118.9(2) 1_555 1_555 2_686 yes C(12) C(13) C(14) 120.6(2) 1_555 1_555 1_555 yes C(12) C(13) H(13) 119.9(2) 1_555 1_555 1_555 no C(14) C(13) H(13) 119.6(2) 1_555 1_555 1_555 no C(12) C(14) C(13) 120.6(2) 2_686 1_555 1_555 yes C(12) C(14) H(13) 119.7(2) 2_686 1_555 1_555 no C(13) C(14) H(13) 119.7(2) 1_555 1_555 1_555 no O(21) C(21) O(22) 124.9(2) 1_555 1_555 1_555 yes O(21) C(21) C(22) 116.5(2) 1_555 1_555 1_555 yes O(22) C(21) C(22) 118.6(2) 1_555 1_555 1_555 yes C(21) C(22) C(23) 120.2(2) 1_555 1_555 1_555 yes C(21) C(22) C(24) 120.6(2) 1_555 1_555 2_475 yes C(23) C(22) C(24) 119.2(2) 1_555 1_555 2_475 yes C(22) C(23) C(24) 120.5(2) 1_555 1_555 1_555 yes C(22) C(23) H(23) 119.1(2) 1_555 1_555 1_555 no C(24) C(23) H(23) 120.5(2) 1_555 1_555 1_555 no C(22) C(24) C(23) 120.3(2) 2_475 1_555 1_555 yes C(22) C(24) H(24) 119.3(2) 2_475 1_555 1_555 no C(23) C(24) H(24) 120.3(2) 1_555 1_555 1_555 no #-------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co O(11) C(11) O(12) -3.2(2) 1_555 1_555 1_555 1_555 yes Co O(11) C(11) C(12) 176.2(1) 1_555 1_555 1_555 1_555 yes Co O(21) C(21) O(22) -4.0(3) 1_555 1_555 1_555 1_555 yes Co O(21) C(21) C(22) 177.5(1) 1_555 1_555 1_555 1_555 yes Co N(1) C(1) C(2) -173.4(2) 1_555 1_555 1_555 1_555 yes Co N(1) C(01) C(02) -4.2(2) 1_555 1_555 1_555 1_555 yes Co N(1) C(01) C(4) 174.9(2) 1_555 1_555 1_555 1_555 yes Co N(2) C(02) C(01) 3.8(2) 1_555 1_555 1_555 1_555 yes Co N(2) C(02) C(7) -174.8(1) 1_555 1_555 1_555 1_555 yes Co N(2) C(10) C(9) 173.5(2) 1_555 1_555 1_555 1_555 yes O Co O(11) C(11) -5.6(2) 1_555 1_555 1_555 1_555 yes O Co O(21) C(21) 31.6(2) 1_555 1_555 1_555 1_555 yes O Co N(1) C(1) -55.3(2) 1_555 1_555 1_555 1_555 yes O Co N(1) C(01) 131.1(1) 1_555 1_555 1_555 1_555 yes O Co N(2) C(02) -85.5(1) 1_555 1_555 1_555 1_555 yes O Co N(2) C(10) 101.8(2) 1_555 1_555 1_555 1_555 yes O(11) Co O(21) C(21) -108.4(2) 1_555 1_555 1_555 1_555 yes O(11) Co N(1) C(1) 84.0(2) 1_555 1_555 1_555 1_555 yes O(11) Co N(1) C(01) -89.6(1) 1_555 1_555 1_555 1_555 yes O(11) Co N(2) C(02) 83.9(1) 1_555 1_555 1_555 1_555 yes O(11) Co N(2) C(10) -88.8(2) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(13) 173.6(2) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(14) -7.0(3) 1_555 1_555 1_555 2_686 yes O(12) C(11) C(12) C(13) -7.0(3) 1_555 1_555 1_555 1_555 yes O(12) C(11) C(12) C(14) 172.3(2) 1_555 1_555 1_555 2_686 yes O(21) Co O(11) C(11) 94.0(1) 1_555 1_555 1_555 1_555 yes O(21) Co N(1) C(1) -139.0(3) 1_555 1_555 1_555 1_555 yes O(21) Co N(1) C(01) 47.4(4) 1_555 1_555 1_555 1_555 yes O(21) Co N(2) C(02) -176.5(1) 1_555 1_555 1_555 1_555 yes O(21) Co N(2) C(10) 10.8(2) 1_555 1_555 1_555 1_555 yes O(21) C(21) C(22) C(23) 6.8(3) 1_555 1_555 1_555 1_555 yes O(21) C(21) C(22) C(24) -174.1(2) 1_555 1_555 1_555 2_475 yes O(22) C(21) C(22) C(23) -171.8(2) 1_555 1_555 1_555 1_555 yes O(22) C(21) C(22) C(24) 7.3(3) 1_555 1_555 1_555 2_475 yes N(1) Co O(11) C(11) -94.2(1) 1_555 1_555 1_555 1_555 yes N(1) Co O(21) C(21) 115.4(3) 1_555 1_555 1_555 1_555 yes N(1) Co N(2) C(02) -4.6(1) 1_555 1_555 1_555 1_555 yes N(1) Co N(2) C(10) -177.3(2) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(2) C(3) -0.3(4) 1_555 1_555 1_555 1_555 yes N(1) C(01) C(02) N(2) 0.4(3) 1_555 1_555 1_555 1_555 yes N(1) C(01) C(02) C(7) 179.1(2) 1_555 1_555 1_555 1_555 yes N(1) C(01) C(4) C(3) -0.6(3) 1_555 1_555 1_555 1_555 yes N(1) C(01) C(4) C(5) 180.0(2) 1_555 1_555 1_555 1_555 yes N(2) Co O(11) C(11) -172.3(1) 1_555 1_555 1_555 1_555 yes N(2) Co O(21) C(21) 157.0(2) 1_555 1_555 1_555 1_555 yes N(2) Co N(1) C(1) 178.3(2) 1_555 1_555 1_555 1_555 yes N(2) Co N(1) C(01) 4.7(1) 1_555 1_555 1_555 1_555 yes N(2) C(02) C(01) C(4) -178.7(2) 1_555 1_555 1_555 1_555 yes N(2) C(02) C(7) C(6) 179.6(2) 1_555 1_555 1_555 1_555 yes N(2) C(02) C(7) C(8) 0.8(3) 1_555 1_555 1_555 1_555 yes N(2) C(10) C(9) C(8) 0.1(3) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(01) C(02) -178.6(2) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(01) C(4) 0.5(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 0.1(4) 1_555 1_555 1_555 1_555 yes C(01) N(1) C(1) C(2) 0.0(3) 1_555 1_555 1_555 1_555 yes C(01) C(02) N(2) C(10) 177.3(2) 1_555 1_555 1_555 1_555 yes C(01) C(02) C(7) C(6) 1.0(3) 1_555 1_555 1_555 1_555 yes C(01) C(02) C(7) C(8) -177.8(2) 1_555 1_555 1_555 1_555 yes C(01) C(4) C(3) C(2) 0.3(3) 1_555 1_555 1_555 1_555 yes C(01) C(4) C(5) C(6) 1.0(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 179.7(2) 1_555 1_555 1_555 1_555 yes C(02) N(2) C(10) C(9) 1.0(3) 1_555 1_555 1_555 1_555 yes C(02) C(01) C(4) C(3) 178.5(2) 1_555 1_555 1_555 1_555 yes C(02) C(01) C(4) C(5) -0.9(3) 1_555 1_555 1_555 1_555 yes C(02) C(7) C(6) C(5) -1.0(3) 1_555 1_555 1_555 1_555 yes C(02) C(7) C(8) C(9) 0.3(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -178.4(2) 1_555 1_555 1_555 1_555 yes C(4) C(01) C(02) C(7) 0.0(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 0.0(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 177.8(2) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -178.4(2) 1_555 1_555 1_555 1_555 yes C(7) C(02) N(2) C(10) -1.4(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -0.8(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 178.9(2) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(14) C(13) -178.9(2) 1_555 1_555 2_686 2_686 yes C(21) C(22) C(23) C(24) 179.2(2) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(24) C(23) -179.2(2) 1_555 1_555 2_475 2_475 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 O(12) 2.681(2) 1_555 2_576 ? O C(13) 3.487(2) 1_555 2_576 ? O C(6) 3.487(3) 1_555 2_565 ? O C(11) 3.552(2) 1_555 2_576 ? O(11) C(23) 3.171(2) 1_555 2_575 ? O(11) C(24) 3.455(3) 1_555 2_575 ? O(11) C(10) 3.494(3) 1_555 2_575 ? O(12) C(1) 3.494(3) 1_555 2_576 ? O(21) C(10) 3.377(3) 1_555 2_575 ? O(21) C(9) 3.490(3) 1_555 2_575 ? O(22) C(4) 3.272(3) 1_555 1_455 ? O(22) C(1) 3.285(3) 1_555 2_576 ? O(22) C(3) 3.316(3) 1_555 1_455 ? O(22) C(5) 3.378(3) 1_555 1_455 ? O(22) C(2) 3.389(3) 1_555 2_576 ? N(2) C(23) 3.406(3) 1_555 2_575 ? N(2) C(5) 3.496(3) 1_555 2_565 ? N(2) C(6) 3.508(3) 1_555 2_565 ? C(01) C(24) 3.452(3) 1_555 2_575 ? C(01) C(7) 3.483(3) 1_555 2_565 ? C(01) C(8) 3.565(3) 1_555 2_565 ? C(02) C(24) 3.324(3) 1_555 2_575 ? C(02) C(23) 3.359(3) 1_555 2_575 ? C(02) C(7) 3.530(3) 1_555 2_565 ? C(02) C(02) 3.584(4) 1_555 2_565 ? C(4) C(9) 3.594(3) 1_555 2_565 ? C(5) C(21) 3.530(3) 1_555 1_655 ? C(5) C(10) 3.558(3) 1_555 2_565 ? C(6) C(22) 3.599(3) 1_555 1_655 ? C(7) C(24) 3.501(3) 1_555 2_575 ? C(7) C(23) 3.553(3) 1_555 2_575 ? C(8) C(22) 3.580(3) 1_555 2_575 ? C(9) C(21) 3.545(3) 1_555 2_575 ? C(9) C(22) 3.578(3) 1_555 2_575 ? C(10) C(23) 3.559(3) 1_555 2_575 ? #-------------------------------------------------------------------- data_[Cu(ta)(phen)]n _database_code_CSD 151562 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H12 Cu N2 O4' _chemical_formula_weight 407.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.286(7) _cell_length_b 10.143(3) _cell_length_c 10.490(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.77(3) _cell_angle_gamma 90.00 _cell_volume 1622.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3198 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1999 _reflns_number_gt 1721 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+1.5932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 1999 _refine_ls_number_parameters 244 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 1.108 _refine_ls_shift/su_mean 0.187 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.36353(17) 0.05035(3) 0.7808(3) 0.03095(16) Uani 1 1 d . . . N1 N 0.3142(6) 0.2012(10) 0.6758(10) 0.033(2) Uani 1 1 d . . . N2 N 0.4190(6) 0.2017(9) 0.8841(10) 0.033(2) Uani 1 1 d . . . O1 O 0.5263(7) -0.0550(10) 0.7580(10) 0.056(3) Uani 1 1 d . . . O2 O 0.4207(5) -0.0791(8) 0.8956(8) 0.042(2) Uani 1 1 d . . . O3 O 0.7063(6) -0.4450(9) 1.3037(10) 0.052(3) Uani 1 1 d . . . O4 O 0.8078(5) -0.4231(9) 1.1681(9) 0.041(2) Uani 1 1 d . . . C1 C 0.2593(8) 0.1981(11) 0.5776(12) 0.046(4) Uani 1 1 d . . . H1A H 0.2407 0.1160 0.5471 0.056 Uiso 1 1 calc R . . C2 C 0.2260(9) 0.3083(13) 0.5142(12) 0.054(4) Uani 1 1 d . . . H2A H 0.1930 0.2987 0.4371 0.065 Uiso 1 1 calc R . . C3 C 0.2412(9) 0.4323(14) 0.5642(16) 0.053(4) Uani 1 1 d . . . H3A H 0.2118 0.5061 0.5307 0.064 Uiso 1 1 calc R . . C4 C 0.3024(9) 0.4414(12) 0.6668(15) 0.039(4) Uani 1 1 d . . . C5 C 0.3388(9) 0.5628(11) 0.7354(17) 0.051(4) Uani 1 1 d . . . H5A H 0.3193 0.6446 0.7054 0.061 Uiso 1 1 calc R . . C6 C 0.3982(10) 0.5602(14) 0.8382(17) 0.059(4) Uani 1 1 d . . . H6A H 0.4204 0.6376 0.8751 0.070 Uiso 1 1 calc R . . C7 C 0.4237(10) 0.4407(14) 0.8843(16) 0.045(4) Uani 1 1 d . . . C8 C 0.4799(10) 0.4326(13) 0.9969(17) 0.058(4) Uani 1 1 d . . . H8A H 0.4981 0.5103 1.0376 0.070 Uiso 1 1 calc R . . C9 C 0.5082(9) 0.3159(14) 1.0475(13) 0.054(4) Uani 1 1 d . . . H9A H 0.5511 0.3130 1.1146 0.065 Uiso 1 1 calc R . . C10 C 0.4706(7) 0.1986(12) 0.9951(11) 0.041(3) Uani 1 1 d . . . H10A H 0.4812 0.1187 1.0369 0.049 Uiso 1 1 calc R . . C11 C 0.3964(7) 0.3209(11) 0.8403(10) 0.031(2) Uani 1 1 d . . . C12 C 0.3373(7) 0.3224(10) 0.7294(11) 0.035(3) Uani 1 1 d . . . C13 C 0.5006(7) -0.0978(11) 0.8622(11) 0.031(3) Uani 1 1 d . . . C14 C 0.5563(7) -0.1764(11) 0.9460(11) 0.028(2) Uani 1 1 d . . . C15 C 0.5365(8) -0.1980(11) 1.0750(9) 0.032(3) Uani 1 1 d . . . H15A H 0.4843 -0.1654 1.1034 0.039 Uiso 1 1 calc R . . C16 C 0.5927(7) -0.2659(12) 1.1583(11) 0.037(3) Uani 1 1 d . . . H16A H 0.5802 -0.2760 1.2433 0.045 Uiso 1 1 calc R . . C17 C 0.6690(8) -0.3198(11) 1.1137(10) 0.031(3) Uani 1 1 d . . . C18 C 0.6889(8) -0.3030(11) 0.9920(11) 0.040(3) Uani 1 1 d . . . H18A H 0.7395 -0.3408 0.9636 0.048 Uiso 1 1 calc R . . C19 C 0.6336(7) -0.2285(11) 0.9073(10) 0.035(3) Uani 1 1 d . . . H19A H 0.6493 -0.2142 0.8243 0.043 Uiso 1 1 calc R . . C20 C 0.7325(9) -0.4013(12) 1.2081(12) 0.039(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0281(3) 0.0286(2) 0.0351(3) -0.0004(10) -0.00580(17) 0.0017(9) N1 0.027(5) 0.043(5) 0.028(4) -0.008(4) -0.003(3) -0.005(4) N2 0.029(5) 0.028(5) 0.040(5) -0.012(4) -0.001(4) -0.008(4) O1 0.062(7) 0.068(6) 0.038(6) 0.024(5) -0.005(5) 0.007(5) O2 0.036(6) 0.037(4) 0.052(6) 0.014(4) -0.008(5) 0.002(4) O3 0.049(6) 0.056(5) 0.051(6) 0.014(5) -0.003(5) 0.007(4) O4 0.030(6) 0.041(5) 0.051(6) -0.003(4) -0.012(5) 0.009(4) C1 0.053(8) 0.036(6) 0.052(7) 0.006(6) 0.015(6) 0.003(5) C2 0.057(7) 0.060(7) 0.041(6) -0.001(5) -0.024(5) 0.000(6) C3 0.049(7) 0.058(8) 0.051(9) 0.013(6) -0.010(6) 0.024(6) C4 0.041(8) 0.025(5) 0.054(8) 0.011(4) 0.014(6) 0.014(5) C5 0.054(8) 0.017(4) 0.082(10) 0.006(4) 0.007(6) -0.001(4) C6 0.066(8) 0.044(6) 0.066(8) -0.007(5) 0.010(7) -0.016(5) C7 0.044(8) 0.050(7) 0.041(6) -0.006(5) -0.003(5) 0.003(5) C8 0.063(9) 0.040(7) 0.072(11) -0.027(7) 0.011(7) -0.008(6) C9 0.040(6) 0.064(7) 0.058(7) -0.031(6) 0.005(5) -0.018(5) C10 0.031(6) 0.057(7) 0.033(5) -0.004(5) -0.021(4) 0.000(5) C11 0.022(5) 0.046(6) 0.025(5) -0.004(4) 0.002(4) 0.008(4) C12 0.035(7) 0.017(4) 0.053(7) 0.001(4) 0.011(5) 0.009(4) C13 0.027(6) 0.029(5) 0.038(6) -0.001(4) -0.004(4) 0.001(4) C14 0.021(5) 0.026(5) 0.036(6) -0.007(5) 0.005(4) -0.002(4) C15 0.030(6) 0.046(6) 0.021(5) 0.004(5) 0.003(4) 0.000(5) C16 0.032(7) 0.051(7) 0.028(5) -0.007(5) 0.002(5) 0.013(5) C17 0.039(6) 0.025(5) 0.028(6) 0.006(4) -0.015(4) 0.000(5) C18 0.028(6) 0.037(6) 0.054(8) -0.013(6) -0.002(5) 0.013(5) C19 0.038(8) 0.038(6) 0.029(6) 0.009(4) -0.001(5) -0.006(5) C20 0.050(8) 0.029(5) 0.035(7) 0.002(5) -0.020(5) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O4 1.912(9) 4_444 ? Cu O2 1.950(9) . ? Cu N1 2.003(11) . ? Cu N2 2.032(10) . ? N1 C1 1.285(18) . ? N1 C12 1.388(15) . ? N2 C11 1.331(16) . ? N2 C10 1.363(16) . ? O1 C13 1.263(16) . ? O2 C13 1.306(14) . ? O3 C20 1.190(17) . ? O4 C20 1.271(16) . ? O4 Cu 1.912(9) 4_545 ? C1 C2 1.380(17) . ? C2 C3 1.376(19) . ? C3 C4 1.38(2) . ? C4 C12 1.458(15) . ? C4 C5 1.51(2) . ? C5 C6 1.364(8) . ? C6 C7 1.35(2) . ? C7 C11 1.356(18) . ? C7 C8 1.42(2) . ? C8 C9 1.36(2) . ? C9 C10 1.417(16) . ? C11 C12 1.426(6) . ? C13 C14 1.426(15) . ? C14 C19 1.380(17) . ? C14 C15 1.423(15) . ? C15 C16 1.370(15) . ? C16 C17 1.396(17) . ? C17 C18 1.343(17) . ? C17 C20 1.574(15) . ? C18 C19 1.405(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cu O2 95.22(11) 4_444 . ? O4 Cu N1 92.3(4) 4_444 . ? O2 Cu N1 172.4(4) . . ? O4 Cu N2 173.2(4) 4_444 . ? O2 Cu N2 91.4(4) . . ? N1 Cu N2 81.10(13) . . ? C1 N1 C12 118.8(11) . . ? C1 N1 Cu 128.6(9) . . ? C12 N1 Cu 112.2(8) . . ? C11 N2 C10 116.0(10) . . ? C11 N2 Cu 114.4(9) . . ? C10 N2 Cu 129.5(8) . . ? C13 O2 Cu 108.7(7) . . ? C20 O4 Cu 106.9(8) . 4_545 ? N1 C1 C2 124.5(11) . . ? C3 C2 C1 120.6(11) . . ? C2 C3 C4 116.5(12) . . ? C3 C4 C12 120.3(13) . . ? C3 C4 C5 129.3(12) . . ? C12 C4 C5 110.3(14) . . ? C6 C5 C4 124.4(15) . . ? C7 C6 C5 117.5(16) . . ? C6 C7 C11 127.3(18) . . ? C6 C7 C8 119.7(15) . . ? C11 C7 C8 112.8(13) . . ? C9 C8 C7 122.5(12) . . ? C8 C9 C10 118.0(13) . . ? N2 C10 C9 120.6(11) . . ? N2 C11 C7 129.0(13) . . ? N2 C11 C12 115.3(12) . . ? C7 C11 C12 115.6(14) . . ? N1 C12 C11 116.9(12) . . ? N1 C12 C4 118.4(12) . . ? C11 C12 C4 124.7(14) . . ? O1 C13 O2 122.2(12) . . ? O1 C13 C14 121.2(11) . . ? O2 C13 C14 116.5(11) . . ? C19 C14 C15 117.4(10) . . ? C19 C14 C13 121.4(10) . . ? C15 C14 C13 121.1(10) . . ? C16 C15 C14 121.3(10) . . ? C15 C16 C17 119.1(10) . . ? C18 C17 C16 121.0(10) . . ? C18 C17 C20 119.7(12) . . ? C16 C17 C20 119.3(10) . . ? C17 C18 C19 120.3(11) . . ? C14 C19 C18 120.8(10) . . ? O3 C20 O4 125.1(13) . . ? O3 C20 C17 119.9(13) . . ? O4 C20 C17 114.7(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.309 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.056 data_[Zn(ta)(phen)(H2O)]n _database_code_CSD 151563 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 N2 O5 Zn' _chemical_formula_weight 427.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1894(4) _cell_length_b 10.5765(5) _cell_length_c 11.5636(6) _cell_angle_alpha 114.6210(10) _cell_angle_beta 91.562(2) _cell_angle_gamma 115.1470(10) _cell_volume 895.91(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4676 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3135 _reflns_number_gt 2626 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.0911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3135 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn -0.02505(5) 0.89151(4) 0.20392(4) 0.03189(17) Uani 1 1 d . . . O1 O 0.1618(3) 1.1108(3) 0.2649(2) 0.0403(6) Uani 1 1 d . . . O2 O 0.1213(3) 1.1507(3) 0.4609(3) 0.0466(7) Uani 1 1 d . . . O3 O -0.1967(3) 0.9106(3) 0.1091(3) 0.0416(6) Uani 1 1 d . . . O4 O -0.3177(4) 0.9783(4) 0.2721(3) 0.0532(8) Uani 1 1 d . . . O5 O -0.2005(4) 0.8022(3) 0.2946(3) 0.0385(6) Uani 1 1 d . . . H5B H -0.242(7) 0.853(6) 0.294(5) 0.064(18) Uiso 1 1 d . . . H5C H -0.177(6) 0.807(6) 0.364(5) 0.069(17) Uiso 1 1 d . . . N1 N 0.0189(4) 0.7629(3) 0.0254(3) 0.0351(7) Uani 1 1 d . . . N2 N 0.1276(4) 0.8083(4) 0.2646(3) 0.0373(7) Uani 1 1 d . . . C1 C 0.5965(5) 1.5438(5) 0.4211(4) 0.0406(9) Uani 1 1 d . . . C2 C 0.4531(5) 1.3986(5) 0.3673(4) 0.0428(10) Uani 1 1 d . . . H2A H 0.422(5) 1.329(5) 0.275(4) 0.045(11) Uiso 1 1 d . . . C3 C 0.3564(4) 1.3539(4) 0.4459(3) 0.0310(8) Uani 1 1 d . . . C4 C 0.2021(4) 1.1949(4) 0.3883(3) 0.0308(8) Uani 1 1 d . . . C5 C -0.6109(4) 1.0513(4) 0.0503(4) 0.0325(8) Uani 1 1 d . . . H5A H -0.686(5) 1.085(4) 0.076(4) 0.033(10) Uiso 1 1 d . . . C6 C -0.5133(4) 1.0327(4) 0.1272(4) 0.0338(8) Uani 1 1 d . . . H6A H -0.524(4) 1.057(4) 0.217(4) 0.030(9) Uiso 1 1 d . . . C7 C -0.4023(4) 0.9794(4) 0.0778(3) 0.0317(8) Uani 1 1 d . . . C8 C -0.2976(4) 0.9560(4) 0.1598(4) 0.0346(8) Uani 1 1 d . . . C9 C 0.1823(6) 0.8346(5) 0.3848(4) 0.0462(10) Uani 1 1 d . . . H9A H 0.145(5) 0.889(5) 0.450(4) 0.037(10) Uiso 1 1 d . . . C10 C 0.2951(6) 0.7880(6) 0.4112(5) 0.0564(12) Uani 1 1 d . . . H10A H 0.337(5) 0.810(5) 0.495(4) 0.045(11) Uiso 1 1 d . . . C11 C 0.3500(6) 0.7111(6) 0.3110(5) 0.0567(12) Uani 1 1 d . . . H11A H 0.427(6) 0.683(5) 0.331(4) 0.049(12) Uiso 1 1 d . . . C12 C 0.2927(5) 0.6787(5) 0.1832(4) 0.0415(9) Uani 1 1 d . . . C13 C 0.3422(6) 0.5974(5) 0.0712(5) 0.0528(11) Uani 1 1 d . . . H13A H 0.417(6) 0.571(5) 0.087(4) 0.053(13) Uiso 1 1 d . . . C14 C 0.2862(6) 0.5724(5) -0.0493(5) 0.0515(11) Uani 1 1 d . . . H14A H 0.328(6) 0.530(5) -0.119(5) 0.060(14) Uiso 1 1 d . . . C15 C 0.1760(5) 0.6278(4) -0.0697(4) 0.0412(9) Uani 1 1 d . . . C16 C 0.1172(6) 0.6107(5) -0.1921(4) 0.0494(10) Uani 1 1 d . . . H16A H 0.150(5) 0.552(5) -0.267(4) 0.050(12) Uiso 1 1 d . . . C17 C 0.0154(6) 0.6698(5) -0.2018(4) 0.0515(11) Uani 1 1 d . . . H17A H -0.026(7) 0.664(6) -0.274(5) 0.071(16) Uiso 1 1 d . . . C18 C -0.0323(5) 0.7459(5) -0.0920(4) 0.0423(9) Uani 1 1 d . . . H18A H -0.104(6) 0.786(5) -0.097(4) 0.051(13) Uiso 1 1 d . . . C19 C 0.1223(4) 0.7052(4) 0.0364(4) 0.0333(8) Uani 1 1 d . . . C20 C 0.1817(4) 0.7313(4) 0.1651(4) 0.0335(8) Uani 1 1 d . . . H1A H 0.661(5) 1.574(4) 0.373(4) 0.034(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0299(3) 0.0308(2) 0.0324(3) 0.01597(19) 0.00907(17) 0.01154(19) O1 0.0431(15) 0.0303(13) 0.0311(14) 0.0132(12) 0.0068(11) 0.0056(12) O2 0.0392(15) 0.0457(16) 0.0374(15) 0.0213(13) 0.0104(12) 0.0043(13) O3 0.0394(15) 0.0598(17) 0.0425(15) 0.0314(14) 0.0171(12) 0.0303(14) O4 0.0627(19) 0.080(2) 0.0380(16) 0.0319(15) 0.0195(14) 0.0476(18) O5 0.0372(15) 0.0412(15) 0.0399(17) 0.0260(13) 0.0140(12) 0.0142(13) N1 0.0330(16) 0.0306(15) 0.0360(17) 0.0164(14) 0.0079(13) 0.0097(13) N2 0.0388(17) 0.0393(17) 0.0303(16) 0.0150(14) 0.0095(13) 0.0173(14) C1 0.042(2) 0.038(2) 0.032(2) 0.0180(18) 0.0179(17) 0.0091(18) C2 0.049(2) 0.033(2) 0.0258(19) 0.0100(17) 0.0124(17) 0.0066(18) C3 0.0332(18) 0.0283(17) 0.0287(18) 0.0138(15) 0.0082(14) 0.0121(15) C4 0.0312(19) 0.0290(18) 0.0332(19) 0.0162(16) 0.0065(15) 0.0137(15) C5 0.0285(18) 0.0322(18) 0.038(2) 0.0173(16) 0.0138(16) 0.0143(16) C6 0.0323(19) 0.0363(19) 0.032(2) 0.0180(17) 0.0129(15) 0.0140(16) C7 0.0309(19) 0.0272(17) 0.0323(19) 0.0141(15) 0.0072(15) 0.0102(15) C8 0.0299(19) 0.0329(19) 0.036(2) 0.0165(17) 0.0082(15) 0.0103(16) C9 0.051(2) 0.047(2) 0.040(2) 0.021(2) 0.0123(19) 0.023(2) C10 0.063(3) 0.070(3) 0.048(3) 0.033(2) 0.009(2) 0.036(3) C11 0.053(3) 0.065(3) 0.065(3) 0.036(3) 0.011(2) 0.035(3) C12 0.038(2) 0.038(2) 0.049(2) 0.0235(19) 0.0131(18) 0.0161(18) C13 0.053(3) 0.052(3) 0.067(3) 0.030(2) 0.022(2) 0.033(2) C14 0.060(3) 0.046(2) 0.056(3) 0.024(2) 0.029(2) 0.031(2) C15 0.040(2) 0.0286(18) 0.042(2) 0.0116(17) 0.0124(17) 0.0107(17) C16 0.056(3) 0.042(2) 0.039(2) 0.014(2) 0.017(2) 0.020(2) C17 0.056(3) 0.051(3) 0.033(2) 0.018(2) 0.007(2) 0.016(2) C18 0.041(2) 0.045(2) 0.035(2) 0.0197(19) 0.0098(17) 0.0152(19) C19 0.0309(18) 0.0234(16) 0.036(2) 0.0141(15) 0.0120(15) 0.0052(15) C20 0.0314(19) 0.0258(17) 0.041(2) 0.0176(16) 0.0113(16) 0.0096(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O1 2.003(2) . ? Zn O3 2.023(2) . ? Zn O5 2.053(3) . ? Zn N1 2.109(3) . ? Zn N2 2.178(3) . ? O1 C4 1.264(4) . ? O2 C4 1.241(4) . ? O3 C8 1.268(4) . ? O4 C8 1.253(4) . ? N1 C18 1.336(5) . ? N1 C19 1.357(5) . ? N2 C9 1.336(5) . ? N2 C20 1.352(5) . ? C1 C3 1.380(5) 2_686 ? C1 C2 1.387(5) . ? C2 C3 1.372(5) . ? C3 C1 1.380(5) 2_686 ? C3 C4 1.507(5) . ? C5 C6 1.374(5) . ? C5 C7 1.399(5) 2_475 ? C6 C7 1.391(5) . ? C7 C5 1.399(5) 2_475 ? C7 C8 1.494(5) . ? C9 C10 1.397(6) . ? C10 C11 1.361(7) . ? C11 C12 1.400(6) . ? C12 C20 1.400(5) . ? C12 C13 1.435(6) . ? C13 C14 1.347(7) . ? C14 C15 1.425(6) . ? C15 C19 1.400(5) . ? C15 C16 1.410(6) . ? C16 C17 1.352(7) . ? C17 C18 1.389(6) . ? C19 C20 1.440(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn O3 97.44(11) . . ? O1 Zn O5 130.95(11) . . ? O3 Zn O5 87.42(12) . . ? O1 Zn N1 101.47(11) . . ? O3 Zn N1 91.60(11) . . ? O5 Zn N1 127.27(12) . . ? O1 Zn N2 94.70(11) . . ? O3 Zn N2 165.14(11) . . ? O5 Zn N2 91.09(13) . . ? N1 Zn N2 77.57(11) . . ? C4 O1 Zn 112.7(2) . . ? C8 O3 Zn 125.4(2) . . ? C18 N1 C19 118.2(3) . . ? C18 N1 Zn 126.6(3) . . ? C19 N1 Zn 114.9(2) . . ? C9 N2 C20 118.4(3) . . ? C9 N2 Zn 128.8(3) . . ? C20 N2 Zn 112.6(2) . . ? C3 C1 C2 120.6(4) 2_686 . ? C3 C2 C1 120.5(4) . . ? C2 C3 C1 119.0(3) . 2_686 ? C2 C3 C4 120.7(3) . . ? C1 C3 C4 120.4(3) 2_686 . ? O2 C4 O1 122.8(3) . . ? O2 C4 C3 120.3(3) . . ? O1 C4 C3 116.9(3) . . ? C6 C5 C7 120.7(3) . 2_475 ? C5 C6 C7 120.5(3) . . ? C6 C7 C5 118.9(3) . 2_475 ? C6 C7 C8 121.0(3) . . ? C5 C7 C8 120.2(3) 2_475 . ? O4 C8 O3 124.2(3) . . ? O4 C8 C7 118.4(3) . . ? O3 C8 C7 117.3(3) . . ? N2 C9 C10 122.3(4) . . ? C11 C10 C9 119.2(4) . . ? C10 C11 C12 120.0(4) . . ? C11 C12 C20 117.3(4) . . ? C11 C12 C13 124.2(4) . . ? C20 C12 C13 118.5(4) . . ? C14 C13 C12 121.8(4) . . ? C13 C14 C15 120.7(4) . . ? C19 C15 C16 116.9(4) . . ? C19 C15 C14 119.3(4) . . ? C16 C15 C14 123.7(4) . . ? C17 C16 C15 119.7(4) . . ? C16 C17 C18 120.2(4) . . ? N1 C18 C17 122.0(4) . . ? N1 C19 C15 122.9(3) . . ? N1 C19 C20 117.2(3) . . ? C15 C19 C20 119.8(4) . . ? N2 C20 C12 122.7(3) . . ? N2 C20 C19 117.5(3) . . ? C12 C20 C19 119.8(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.840 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.083 data_[Cd(ta)1/2)(phen)Cl]n _database_code_CSD 151564 #-------------------------------------------------------------------- _audit_creation_date 'Sun Mar 12 10:01:51 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #-------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #-------------------------------------------------------------------- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 410.13 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H10 Cd Cl N2 O2 ' _chemical_formula_moiety 'C16 H10 Cd Cl N2 O2 ' _chemical_formula_structural ? _chemical_melting_point ? #-------------------------------------------------------------------- _cell_length_a 23.099(3) _cell_length_b 10.5089(5) _cell_length_c 16.804(2) _cell_angle_alpha 90.00 _cell_angle_beta 135.783(3) _cell_angle_gamma 90.00 _cell_volume 2844.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #-------------------------------------------------------------------- _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? 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 #-------------------------------------------------------------------- _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608.00 _exptl_absorpt_coefficient_mu 1.732 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #-------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku unknown' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 6092 _reflns_number_total 3416 _reflns_number_gt 3178 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_av_sigmaI/netI 0.013 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #-------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Cd' 'Cd' -0.807 1.202 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;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) ; '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) ; #-------------------------------------------------------------------- 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.132269(7) 0.69936(1) 0.889509(9) 0.01236(4) Uani 1.00 d . . . Cl Cl 0.23364(3) 0.84957(4) 1.06632(3) 0.0198(1) Uani 1.00 d . . . O(1) O 0.09253(8) 0.8426(1) 0.7622(1) 0.0270(3) Uani 1.00 d . . . O(2) O -0.03051(7) 0.7500(1) 0.6193(1) 0.0216(3) Uani 1.00 d . . . N(1) N 0.08971(9) 0.4999(1) 0.7898(1) 0.0182(4) Uani 1.00 d . . . N(2) N 0.15640(9) 0.5329(1) 1.0033(1) 0.0192(4) Uani 1.00 d . . . C(1) C 0.0248(1) 0.8303(2) 0.6587(1) 0.0153(4) Uani 1.00 d . . . C(2) C 0.01175(9) 0.9180(1) 0.5760(1) 0.0123(4) Uani 1.00 d . . . C(3) C 0.07942(10) 0.9748(2) 0.6056(1) 0.0169(4) Uani 1.00 d . . . C(4) C -0.06805(10) 0.9432(2) 0.4693(1) 0.0162(4) Uani 1.00 d . . . C(5) C 0.0568(1) 0.4840(2) 0.6855(2) 0.0266(5) Uani 1.00 d . . . C(6) C 0.0459(1) 0.3634(2) 0.6404(2) 0.0398(7) Uani 1.00 d . . . C(7) C 0.0695(2) 0.2580(2) 0.7051(3) 0.0484(8) Uani 1.00 d . . . C(8) C 0.1053(1) 0.2705(2) 0.8160(2) 0.0362(6) Uani 1.00 d . . . C(9) C 0.1140(1) 0.3952(2) 0.8546(2) 0.0222(5) Uani 1.00 d . . . C(10) C 0.1326(2) 0.1632(3) 0.8898(3) 0.0532(10) Uani 1.00 d . . . C(11) C 0.1631(2) 0.1811(2) 0.9936(3) 0.0508(8) Uani 1.00 d . . . C(12) C 0.1485(1) 0.4131(2) 0.9678(2) 0.0215(4) Uani 1.00 d . . . C(13) C 0.1705(1) 0.3057(2) 1.0346(2) 0.0355(6) Uani 1.00 d . . . C(14) C 0.1971(1) 0.3277(2) 1.1392(2) 0.0430(6) Uani 1.00 d . . . C(15) C 0.2016(1) 0.4485(2) 1.1725(2) 0.0380(6) Uani 1.00 d . . . C(16) C 0.1816(1) 0.5501(2) 1.1024(2) 0.0281(5) Uani 1.00 d . . . H(3) H 0.1348 0.9580 0.6789 0.0202 Uiso 1.00 calc . . . H(4) H -0.1150 0.9045 0.4483 0.0191 Uiso 1.00 calc . . . H(5) H 0.0397 0.5577 0.6388 0.0327 Uiso 1.00 calc . . . H(6) H 0.0212 0.3545 0.5643 0.0465 Uiso 1.00 calc . . . H(7) H 0.1287 0.0785 0.8642 0.0634 Uiso 1.00 calc . . . H(10) H 0.0618 0.1751 0.6750 0.0584 Uiso 1.00 calc . . . H(11) H 0.1800 0.1091 1.0420 0.0573 Uiso 1.00 calc . . . H(14) H 0.2104 0.2576 1.1858 0.0496 Uiso 1.00 calc . . . H(15) H 0.2186 0.4644 1.2431 0.0461 Uiso 1.00 calc . . . H(16) H 0.1859 0.6362 1.1267 0.0340 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 Cd 0.01543(8) 0.01092(8) 0.01170(8) 0.00150(4) 0.01005(7) 0.00160(4) Cl 0.0174(2) 0.0235(2) 0.0212(2) -0.0033(2) 0.0148(2) -0.0093(2) O(1) 0.0259(7) 0.0267(7) 0.0163(6) -0.0026(6) 0.0110(6) 0.0087(5) O(2) 0.0248(7) 0.0193(6) 0.0271(7) -0.0039(5) 0.0208(6) 0.0030(5) N(1) 0.0186(7) 0.0161(7) 0.0235(7) -0.0014(6) 0.0163(6) -0.0022(6) N(2) 0.0185(7) 0.0196(7) 0.0194(7) 0.0015(6) 0.0136(7) 0.0060(6) C(1) 0.0191(8) 0.0128(7) 0.0193(8) 0.0035(6) 0.0156(7) 0.0040(6) C(2) 0.0156(7) 0.0102(7) 0.0137(7) 0.0006(6) 0.0113(7) 0.0011(6) C(3) 0.0120(7) 0.0190(8) 0.0141(7) 0.0002(6) 0.0075(7) 0.0031(6) C(4) 0.0145(7) 0.0190(8) 0.0176(8) -0.0014(6) 0.0122(7) 0.0022(6) C(5) 0.0273(10) 0.029(1) 0.0266(10) -0.0039(8) 0.0203(9) -0.0082(8) C(6) 0.047(1) 0.041(1) 0.043(1) -0.013(1) 0.037(1) -0.023(1) C(7) 0.062(2) 0.029(1) 0.079(2) -0.017(1) 0.059(2) -0.030(1) C(8) 0.045(1) 0.0153(9) 0.066(2) -0.0018(9) 0.046(1) -0.0055(10) C(9) 0.0220(9) 0.0146(9) 0.0364(10) 0.0003(7) 0.0231(8) -0.0006(8) C(10) 0.069(2) 0.012(1) 0.107(3) 0.005(1) 0.072(2) 0.004(1) C(11) 0.059(2) 0.019(1) 0.089(2) 0.015(1) 0.058(2) 0.026(1) C(12) 0.0187(8) 0.0169(8) 0.0313(10) 0.0038(7) 0.0187(8) 0.0092(7) C(13) 0.029(1) 0.023(1) 0.051(1) 0.0080(8) 0.028(1) 0.0203(9) C(14) 0.032(1) 0.047(1) 0.044(1) 0.009(1) 0.025(1) 0.031(1) C(15) 0.027(1) 0.056(2) 0.0239(10) -0.0030(10) 0.0160(9) 0.0152(10) C(16) 0.0260(10) 0.037(1) 0.0205(9) -0.0021(8) 0.0164(8) 0.0046(8) #-------------------------------------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3178 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0154 _refine_ls_R_factor_gt 0.0154 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0252 _refine_ls_wR_factor_gt 0.0252 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.891 _refine_ls_shift/su_max 0.0066 _refine_ls_shift/su_mean 0.0017 _refine_diff_density_min -0.29 _refine_diff_density_max 0.33 #-------------------------------------------------------------------- _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 Cd Cl 2.6132(4) 1_555 1_555 yes Cd Cl 2.6671(5) 1_555 7_567 yes Cd O(1) 2.207(1) 1_555 1_555 yes Cd O(2) 2.309(1) 1_555 2_556 yes Cd N(1) 2.409(1) 1_555 1_555 yes Cd N(2) 2.345(1) 1_555 1_555 yes O(1) C(1) 1.260(2) 1_555 1_555 yes O(2) C(1) 1.253(2) 1_555 1_555 yes N(1) C(5) 1.330(2) 1_555 1_555 yes N(1) C(9) 1.355(2) 1_555 1_555 yes N(2) C(12) 1.349(2) 1_555 1_555 yes N(2) C(16) 1.326(2) 1_555 1_555 yes C(1) C(2) 1.507(2) 1_555 1_555 yes C(2) C(3) 1.390(2) 1_555 1_555 yes C(2) C(4) 1.395(2) 1_555 1_555 yes C(3) C(4) 1.385(2) 1_555 3_576 yes C(5) C(6) 1.403(3) 1_555 1_555 yes C(6) C(7) 1.362(4) 1_555 1_555 yes C(7) C(8) 1.402(4) 1_555 1_555 yes C(8) C(9) 1.411(3) 1_555 1_555 yes C(8) C(10) 1.444(4) 1_555 1_555 yes C(9) C(12) 1.455(3) 1_555 1_555 yes C(10) C(11) 1.347(4) 1_555 1_555 yes C(11) C(13) 1.431(3) 1_555 1_555 yes C(12) C(13) 1.405(3) 1_555 1_555 yes C(13) C(14) 1.404(4) 1_555 1_555 yes C(14) C(15) 1.361(4) 1_555 1_555 yes C(15) C(16) 1.401(3) 1_555 1_555 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 Cl Cd Cl 83.37(1) 1_555 1_555 7_567 yes Cl Cd O(1) 95.83(4) 1_555 1_555 1_555 yes Cl Cd O(2) 88.58(3) 1_555 1_555 2_556 yes Cl Cd N(1) 154.49(4) 1_555 1_555 1_555 yes Cl Cd N(2) 91.60(4) 1_555 1_555 1_555 yes Cl Cd O(1) 89.68(4) 7_567 1_555 1_555 yes Cl Cd O(2) 171.14(3) 7_567 1_555 2_556 yes Cl Cd N(1) 80.75(3) 7_567 1_555 1_555 yes Cl Cd N(2) 94.54(4) 7_567 1_555 1_555 yes O(1) Cd O(2) 94.81(5) 1_555 1_555 2_556 yes O(1) Cd N(1) 103.89(5) 1_555 1_555 1_555 yes O(1) Cd N(2) 171.84(5) 1_555 1_555 1_555 yes O(2) Cd N(1) 105.47(5) 2_556 1_555 1_555 yes O(2) Cd N(2) 81.97(5) 2_556 1_555 1_555 yes N(1) Cd N(2) 70.01(5) 1_555 1_555 1_555 yes Cd Cl Cd 96.63(1) 1_555 1_555 7_567 yes Cd O(1) C(1) 120.7(1) 1_555 1_555 1_555 yes Cd O(2) C(1) 142.6(1) 2_556 1_555 1_555 yes Cd N(1) C(5) 126.1(1) 1_555 1_555 1_555 yes Cd N(1) C(9) 114.8(1) 1_555 1_555 1_555 yes C(5) N(1) C(9) 118.2(2) 1_555 1_555 1_555 yes Cd N(2) C(12) 117.3(1) 1_555 1_555 1_555 yes Cd N(2) C(16) 123.8(1) 1_555 1_555 1_555 yes C(12) N(2) C(16) 118.8(2) 1_555 1_555 1_555 yes O(1) C(1) O(2) 125.8(2) 1_555 1_555 1_555 yes O(1) C(1) C(2) 116.1(1) 1_555 1_555 1_555 yes O(2) C(1) C(2) 118.1(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.1(1) 1_555 1_555 1_555 yes C(1) C(2) C(4) 120.5(1) 1_555 1_555 1_555 yes C(3) C(2) C(4) 119.3(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.6(1) 1_555 1_555 3_576 yes C(2) C(3) H(3) 120.1(2) 1_555 1_555 1_555 no C(4) C(3) H(3) 119.3(2) 3_576 1_555 1_555 no C(2) C(4) C(3) 120.1(1) 1_555 1_555 3_576 yes C(2) C(4) H(4) 119.8(1) 1_555 1_555 1_555 no C(3) C(4) H(4) 120.1(2) 3_576 1_555 1_555 no N(1) C(5) C(6) 122.4(2) 1_555 1_555 1_555 yes N(1) C(5) H(5) 119.1(2) 1_555 1_555 1_555 no C(6) C(5) H(5) 118.5(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 119.3(2) 1_555 1_555 1_555 yes C(5) C(6) H(6) 120.7(2) 1_555 1_555 1_555 no C(7) C(6) H(6) 120.0(2) 1_555 1_555 1_555 no C(6) C(7) C(8) 120.2(2) 1_555 1_555 1_555 yes C(6) C(7) H(10) 120.0(3) 1_555 1_555 1_555 no C(8) C(7) H(10) 119.8(3) 1_555 1_555 1_555 no C(7) C(8) C(9) 116.8(2) 1_555 1_555 1_555 yes C(7) C(8) C(10) 123.2(2) 1_555 1_555 1_555 yes C(9) C(8) C(10) 120.0(2) 1_555 1_555 1_555 yes N(1) C(9) C(8) 123.0(2) 1_555 1_555 1_555 yes N(1) C(9) C(12) 118.0(2) 1_555 1_555 1_555 yes C(8) C(9) C(12) 119.0(2) 1_555 1_555 1_555 yes C(8) C(10) C(11) 120.3(2) 1_555 1_555 1_555 yes C(8) C(10) H(7) 119.6(3) 1_555 1_555 1_555 no C(11) C(10) H(7) 120.1(3) 1_555 1_555 1_555 no C(10) C(11) C(13) 121.5(2) 1_555 1_555 1_555 yes C(10) C(11) H(11) 120.1(3) 1_555 1_555 1_555 no C(13) C(11) H(11) 118.4(3) 1_555 1_555 1_555 no N(2) C(12) C(9) 118.2(1) 1_555 1_555 1_555 yes N(2) C(12) C(13) 122.7(2) 1_555 1_555 1_555 yes C(9) C(12) C(13) 119.1(2) 1_555 1_555 1_555 yes C(11) C(13) C(12) 120.0(2) 1_555 1_555 1_555 yes C(11) C(13) C(14) 123.1(2) 1_555 1_555 1_555 yes C(12) C(13) C(14) 116.8(2) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120.3(2) 1_555 1_555 1_555 yes C(13) C(14) H(14) 119.8(3) 1_555 1_555 1_555 no C(15) C(14) H(14) 119.9(3) 1_555 1_555 1_555 no C(14) C(15) C(16) 119.0(2) 1_555 1_555 1_555 yes C(14) C(15) H(15) 120.9(2) 1_555 1_555 1_555 no C(16) C(15) H(15) 120.1(2) 1_555 1_555 1_555 no N(2) C(16) C(15) 122.4(2) 1_555 1_555 1_555 yes N(2) C(16) H(16) 118.6(2) 1_555 1_555 1_555 no C(15) C(16) H(16) 119.1(2) 1_555 1_555 1_555 no #-------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd Cl Cd Cl 0.0 1_555 1_555 7_567 7_567 yes Cd Cl Cd O(1) -95.90(4) 1_555 1_555 7_567 7_567 yes Cd Cl Cd N(1) 159.97(4) 1_555 1_555 7_567 7_567 yes Cd Cl Cd N(2) 91.09(4) 1_555 1_555 7_567 7_567 yes Cd Cl Cd Cl 0.0 1_555 7_567 7_567 1_555 yes Cd Cl Cd O(1) 89.00(4) 1_555 7_567 7_567 7_567 yes Cd Cl Cd N(1) -51.74(8) 1_555 7_567 7_567 7_567 yes Cd Cl Cd N(2) -94.38(4) 1_555 7_567 7_567 7_567 yes Cd O(1) C(1) O(2) 9.7(2) 1_555 1_555 1_555 1_555 yes Cd O(1) C(1) C(2) -168.2(1) 1_555 1_555 1_555 1_555 yes Cd O(2) C(1) O(1) 71.8(3) 1_555 2_556 2_556 2_556 yes Cd O(2) C(1) C(2) -110.3(2) 1_555 2_556 2_556 2_556 yes Cd N(1) C(5) C(6) 169.6(1) 1_555 1_555 1_555 1_555 yes Cd N(1) C(9) C(8) -170.8(1) 1_555 1_555 1_555 1_555 yes Cd N(1) C(9) C(12) 10.9(2) 1_555 1_555 1_555 1_555 yes Cd N(2) C(12) C(9) -9.0(2) 1_555 1_555 1_555 1_555 yes Cd N(2) C(12) C(13) 172.5(1) 1_555 1_555 1_555 1_555 yes Cd N(2) C(16) C(15) -174.9(1) 1_555 1_555 1_555 1_555 yes Cl Cd Cl Cd 0.0 1_555 1_555 7_567 7_567 yes Cl Cd O(1) C(1) -158.1(1) 1_555 1_555 1_555 1_555 yes Cl Cd O(2) C(1) 85.9(2) 1_555 1_555 2_556 2_556 yes Cl Cd N(1) C(5) -134.2(1) 1_555 1_555 1_555 1_555 yes Cl Cd N(1) C(9) 35.1(2) 1_555 1_555 1_555 1_555 yes Cl Cd N(2) C(12) -151.5(1) 1_555 1_555 1_555 1_555 yes Cl Cd N(2) C(16) 24.6(1) 1_555 1_555 1_555 1_555 yes Cl Cd Cl Cd 0.0 1_555 7_567 7_567 1_555 yes Cl Cd O(1) C(1) -118.6(1) 1_555 7_567 7_567 7_567 yes Cl Cd N(1) C(5) 82.0(1) 1_555 7_567 7_567 7_567 yes Cl Cd N(1) C(9) -87.3(1) 1_555 7_567 7_567 7_567 yes Cl Cd N(2) C(12) 68.0(1) 1_555 7_567 7_567 7_567 yes Cl Cd N(2) C(16) -108.1(1) 1_555 7_567 7_567 7_567 yes O(1) Cd O(2) C(1) -9.8(2) 1_555 1_555 2_556 2_556 yes O(1) Cd N(1) C(5) 5.3(1) 1_555 1_555 1_555 1_555 yes O(1) Cd N(1) C(9) 174.6(1) 1_555 1_555 1_555 1_555 yes O(1) Cd N(2) C(12) 52.9(4) 1_555 1_555 1_555 1_555 yes O(1) Cd N(2) C(16) -131.0(3) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(3) 21.3(2) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(4) -158.7(2) 1_555 1_555 1_555 1_555 yes O(2) Cd O(1) C(1) -69.0(1) 1_555 2_556 2_556 2_556 yes O(2) Cd N(1) C(5) 104.4(1) 1_555 2_556 2_556 2_556 yes O(2) Cd N(1) C(9) -86.3(1) 1_555 2_556 2_556 2_556 yes O(2) Cd N(2) C(12) 120.2(1) 1_555 2_556 2_556 2_556 yes O(2) Cd N(2) C(16) -63.8(1) 1_555 2_556 2_556 2_556 yes O(2) C(1) C(2) C(3) -156.8(2) 1_555 1_555 1_555 1_555 yes O(2) C(1) C(2) C(4) 23.3(2) 1_555 1_555 1_555 1_555 yes N(1) Cd O(1) C(1) 38.3(1) 1_555 1_555 1_555 1_555 yes N(1) Cd O(2) C(1) -115.7(2) 1_555 1_555 2_556 2_556 yes N(1) Cd N(2) C(12) 10.4(1) 1_555 1_555 1_555 1_555 yes N(1) Cd N(2) C(16) -173.5(1) 1_555 1_555 1_555 1_555 yes N(1) C(5) C(6) C(7) 0.0(3) 1_555 1_555 1_555 1_555 yes N(1) C(9) C(8) C(7) -0.1(3) 1_555 1_555 1_555 1_555 yes N(1) C(9) C(8) C(10) 180.0(2) 1_555 1_555 1_555 1_555 yes N(1) C(9) C(12) N(2) -1.6(2) 1_555 1_555 1_555 1_555 yes N(1) C(9) C(12) C(13) 177.0(2) 1_555 1_555 1_555 1_555 yes N(2) Cd O(1) C(1) -2.6(4) 1_555 1_555 1_555 1_555 yes N(2) Cd O(2) C(1) 177.7(2) 1_555 1_555 2_556 2_556 yes N(2) Cd N(1) C(5) 179.7(1) 1_555 1_555 1_555 1_555 yes N(2) Cd N(1) C(9) -11.0(1) 1_555 1_555 1_555 1_555 yes N(2) C(12) C(9) C(8) -180.0(2) 1_555 1_555 1_555 1_555 yes N(2) C(12) C(13) C(11) -178.1(2) 1_555 1_555 1_555 1_555 yes N(2) C(12) C(13) C(14) 3.6(3) 1_555 1_555 1_555 1_555 yes N(2) C(16) C(15) C(14) 1.6(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -179.3(1) 1_555 1_555 1_555 3_576 yes C(1) C(2) C(4) C(3) 179.3(1) 1_555 1_555 1_555 3_576 yes C(5) N(1) C(9) C(8) -0.6(2) 1_555 1_555 1_555 1_555 yes C(5) N(1) C(9) C(12) -178.9(2) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -0.7(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) N(1) C(9) 0.7(3) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 0.8(3) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(10) -179.3(2) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(12) 178.2(2) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(10) C(11) -176.9(2) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(12) C(13) -1.4(3) 1_555 1_555 1_555 1_555 yes C(8) C(10) C(11) C(13) -1.0(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(10) C(11) 3.0(4) 1_555 1_555 1_555 1_555 yes C(9) C(12) N(2) C(16) 174.7(2) 1_555 1_555 1_555 1_555 yes C(9) C(12) C(13) C(11) 3.3(3) 1_555 1_555 1_555 1_555 yes C(9) C(12) C(13) C(14) -174.9(2) 1_555 1_555 1_555 1_555 yes C(10) C(8) C(9) C(12) -1.7(3) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(13) C(12) -2.2(4) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(13) C(14) 176.0(2) 1_555 1_555 1_555 1_555 yes C(11) C(13) C(14) C(15) -179.0(2) 1_555 1_555 1_555 1_555 yes C(12) N(2) C(16) C(15) 1.1(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -0.8(3) 1_555 1_555 1_555 1_555 yes C(13) C(12) N(2) C(16) -3.8(3) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -1.7(3) 1_555 1_555 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 Cd Cl 2.6132(4) 1_555 1_555 ? Cd Cl 2.6671(5) 1_555 7_567 ? C(3) C(7) 3.501(3) 1_555 1_565 ? C(4) C(7) 3.595(3) 1_555 3_566 ? C(5) C(15) 3.575(3) 1_555 4_564 ? #-------------------------------------------------------------------- data_[Mn(ta)(phen)]n _database_code_CSD 151565 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H12 Mn N2 O4' _chemical_formula_weight 399.26 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.510(6) _cell_length_b 10.394(3) _cell_length_c 9.373(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.88(2) _cell_angle_gamma 90.00 _cell_volume 1696.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.05 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method ? _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3403 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1706 _reflns_number_observed 1498 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+1.6815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(6) _refine_ls_number_reflns 1705 _refine_ls_number_parameters 244 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_obs 0.0372 _refine_ls_wR_factor_all 0.1050 _refine_ls_wR_factor_obs 0.0973 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max 0.798 _refine_ls_shift/esd_mean 0.202 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn Mn 0.1209(2) 0.55192(5) 0.4796(3) 0.0228(2) Uani 1 d . . O1 O 0.0302(5) 0.5608(8) 0.6168(10) 0.042(2) Uani 1 d . . O2 O 0.0471(4) 0.5818(9) 0.8570(8) 0.033(2) Uani 1 d . . O3 O -0.2888(5) 0.9379(8) 0.8419(9) 0.039(2) Uani 1 d . . O4 O -0.3076(5) 0.9214(10) 0.6020(10) 0.046(3) Uani 1 d . . N1 N 0.1762(6) 0.7357(11) 0.5905(11) 0.037(3) Uani 1 d . . N2 N 0.0630(6) 0.7388(10) 0.3651(10) 0.028(2) Uani 1 d . . C1 C -0.2712(6) 0.9001(11) 0.7244(13) 0.031(3) Uani 1 d . . C2 C -0.1973(6) 0.8239(10) 0.7274(11) 0.022(2) Uani 1 d . . C3 C -0.1618(6) 0.7720(12) 0.8582(11) 0.033(3) Uani 1 d . . H3A H -0.1830(6) 0.7852(12) 0.9440(11) 0.039 Uiso 1 calc R . C4 C -0.0949(6) 0.7016(12) 0.8548(12) 0.032(3) Uani 1 d . . H4A H -0.0713(6) 0.6692(12) 0.9408(12) 0.038 Uiso 1 calc R . C5 C -0.0625(6) 0.6777(10) 0.7341(13) 0.026(3) Uani 1 d . . C6 C -0.0959(6) 0.7278(12) 0.6071(11) 0.029(3) Uani 1 d . . H6A H -0.0733(6) 0.7113(12) 0.5234(11) 0.034 Uiso 1 calc R . C7 C -0.1628(6) 0.8028(12) 0.5988(11) 0.029(3) Uani 1 d . . H7A H -0.1839(6) 0.8376(12) 0.5121(11) 0.034 Uiso 1 calc R . C8 C 0.0113(6) 0.5999(11) 0.7358(10) 0.021(2) Uani 1 d . . C9 C 0.0043(8) 0.7376(16) 0.2574(16) 0.052(4) Uani 1 d . . H9A H -0.0114(8) 0.6606(16) 0.2129(16) 0.063 Uiso 1 calc R . C10 C -0.0328(7) 0.8553(14) 0.2136(14) 0.052(4) Uani 1 d . . H10A H -0.0766(7) 0.8543(14) 0.1485(14) 0.063 Uiso 1 calc R . C11 C -0.0044(8) 0.9678(12) 0.2663(19) 0.060(5) Uani 1 d . . H11A H -0.0265(8) 1.0447(12) 0.2321(19) 0.072 Uiso 1 calc R . C12 C 0.0580(7) 0.9701(12) 0.3724(14) 0.033(3) Uani 1 d . . C13 C 0.0900(7) 1.0832(14) 0.4250(14) 0.051(4) Uani 1 d . . H13A H 0.0675(7) 1.1589(14) 0.3881(14) 0.062 Uiso 1 calc R . C14 C 0.1518(7) 1.0961(11) 0.5262(16) 0.046(4) Uani 1 d . . H14A H 0.1717(7) 1.1759(11) 0.5556(16) 0.055 Uiso 1 calc R . C15 C 0.1852(9) 0.9720(11) 0.5860(16) 0.044(4) Uani 1 d . . C16 C 0.2481(6) 0.9668(12) 0.6938(14) 0.042(3) Uani 1 d . . H16A H 0.2731(6) 1.0416(12) 0.7272(14) 0.050 Uiso 1 calc R . C17 C 0.2713(8) 0.8480(12) 0.7480(15) 0.050(4) Uani 1 d . . H17A H 0.3112(8) 0.8414(12) 0.8213(15) 0.060 Uiso 1 calc R . C18 C 0.2343(6) 0.7386(11) 0.6913(12) 0.030(3) Uani 1 d . . H18A H 0.2522(6) 0.6599(11) 0.7281(12) 0.036 Uiso 1 calc R . C19 C 0.1510(7) 0.8576(12) 0.5372(12) 0.034(3) Uani 1 d . . C20 C 0.0881(6) 0.8492(11) 0.4209(12) 0.027(3) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0201(3) 0.0230(4) 0.0250(3) -0.0015(10) 0.0002(2) 0.0001(10) O1 0.031(5) 0.040(5) 0.055(6) -0.002(4) 0.006(4) 0.018(4) O2 0.016(4) 0.056(5) 0.023(4) 0.002(4) -0.013(3) 0.022(4) O3 0.031(5) 0.065(6) 0.023(4) -0.006(4) 0.018(3) 0.015(4) O4 0.049(6) 0.034(5) 0.057(6) 0.005(5) 0.009(4) 0.011(4) N1 0.037(6) 0.040(6) 0.033(5) 0.000(5) -0.001(4) 0.009(5) N2 0.034(5) 0.018(5) 0.031(5) 0.000(4) -0.005(4) 0.009(4) C1 0.019(6) 0.019(6) 0.055(8) 0.015(5) 0.008(5) 0.003(5) C2 0.021(6) 0.028(5) 0.017(5) 0.003(5) -0.001(4) 0.001(5) C3 0.033(6) 0.044(7) 0.018(4) 0.001(5) -0.010(4) 0.015(5) C4 0.025(5) 0.035(6) 0.033(6) 0.002(5) -0.010(5) 0.014(5) C5 0.018(5) 0.016(5) 0.043(7) -0.007(5) 0.002(5) 0.006(4) C6 0.025(5) 0.041(7) 0.023(5) -0.004(5) 0.019(4) 0.006(5) C7 0.032(6) 0.038(6) 0.017(5) 0.003(5) 0.002(4) 0.003(5) C8 0.020(5) 0.025(6) 0.018(5) -0.004(4) -0.001(4) -0.001(4) C9 0.049(8) 0.050(8) 0.053(8) -0.001(7) -0.020(6) 0.010(7) C10 0.043(7) 0.067(10) 0.047(7) 0.016(6) -0.002(5) 0.024(6) C11 0.083(11) 0.021(6) 0.077(11) 0.012(6) 0.013(9) 0.006(6) C12 0.019(5) 0.041(7) 0.036(6) 0.015(5) -0.005(5) -0.001(4) C13 0.056(8) 0.043(7) 0.054(7) 0.017(6) 0.001(6) 0.025(6) C14 0.052(7) 0.003(4) 0.081(9) 0.008(4) 0.002(6) 0.007(4) C15 0.067(9) 0.013(5) 0.053(8) 0.011(5) 0.005(7) -0.009(5) C16 0.032(6) 0.047(7) 0.042(7) 0.000(5) -0.021(5) -0.017(5) C17 0.058(8) 0.030(7) 0.055(7) 0.011(6) -0.026(6) 0.003(5) C18 0.043(7) 0.018(5) 0.029(5) -0.002(4) -0.003(4) 0.003(5) C19 0.043(6) 0.030(6) 0.030(5) 0.013(5) 0.002(5) -0.004(5) C20 0.021(5) 0.019(5) 0.042(6) 0.015(4) 0.003(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O4 2.105(10) 3_545 ? Mn O1 2.145(9) . ? Mn O3 2.144(7) 4_564 ? Mn O2 2.150(8) 2_564 ? Mn N1 2.336(11) . ? Mn N2 2.395(9) . ? O1 C8 1.263(13) . ? O2 C8 1.254(12) . ? O2 Mn 2.150(8) 2_565 ? O3 C1 1.237(15) . ? O3 Mn 2.144(7) 4_465 ? O4 C1 1.273(15) . ? O4 Mn 2.105(10) 3_455 ? N1 C18 1.316(14) . ? N1 C19 1.42(2) . ? N2 C20 1.32(2) . ? N2 C9 1.36(2) . ? C1 C2 1.515(15) . ? C2 C7 1.42(2) . ? C2 C3 1.423(14) . ? C3 C4 1.38(2) . ? C4 C5 1.34(2) . ? C5 C6 1.37(2) . ? C5 C8 1.523(14) . ? C6 C7 1.40(2) . ? C9 C10 1.43(2) . ? C10 C11 1.34(2) . ? C11 C12 1.40(2) . ? C12 C13 1.37(2) . ? C12 C20 1.42(2) . ? C13 C14 1.371(9) . ? C14 C15 1.50(2) . ? C15 C19 1.39(2) . ? C15 C16 1.42(2) . ? C16 C17 1.38(2) . ? C17 C18 1.39(2) . ? C19 C20 1.470(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn O1 97.8(3) 3_545 . ? O4 Mn O3 85.8(4) 3_545 4_564 ? O1 Mn O3 174.69(10) . 4_564 ? O4 Mn O2 99.55(13) 3_545 2_564 ? O1 Mn O2 84.6(3) . 2_564 ? O3 Mn O2 98.6(3) 4_564 2_564 ? O4 Mn N1 95.1(4) 3_545 . ? O1 Mn N1 89.8(4) . . ? O3 Mn N1 86.0(4) 4_564 . ? O2 Mn N1 164.9(4) 2_564 . ? O4 Mn N2 165.6(4) 3_545 . ? O1 Mn N2 85.9(3) . . ? O3 Mn N2 89.7(4) 4_564 . ? O2 Mn N2 94.6(3) 2_564 . ? N1 Mn N2 70.95(12) . . ? C8 O1 Mn 145.2(8) . . ? C8 O2 Mn 143.0(8) . 2_565 ? C1 O3 Mn 144.9(8) . 4_465 ? C1 O4 Mn 144.9(9) . 3_455 ? C18 N1 C19 115.0(10) . . ? C18 N1 Mn 126.4(9) . . ? C19 N1 Mn 118.3(8) . . ? C20 N2 C9 119.8(11) . . ? C20 N2 Mn 114.8(8) . . ? C9 N2 Mn 125.2(9) . . ? O3 C1 O4 126.8(11) . . ? O3 C1 C2 116.1(11) . . ? O4 C1 C2 117.0(11) . . ? C7 C2 C3 119.2(10) . . ? C7 C2 C1 120.1(10) . . ? C3 C2 C1 120.7(10) . . ? C4 C3 C2 118.5(10) . . ? C5 C4 C3 123.3(10) . . ? C4 C5 C6 118.8(10) . . ? C4 C5 C8 121.4(10) . . ? C6 C5 C8 119.7(10) . . ? C5 C6 C7 122.5(10) . . ? C6 C7 C2 117.6(10) . . ? O2 C8 O1 126.8(10) . . ? O2 C8 C5 115.7(9) . . ? O1 C8 C5 117.4(9) . . ? N2 C9 C10 119.4(13) . . ? C11 C10 C9 120.0(12) . . ? C10 C11 C12 120.5(11) . . ? C13 C12 C11 122.0(12) . . ? C13 C12 C20 121.3(12) . . ? C11 C12 C20 116.7(12) . . ? C14 C13 C12 126.6(15) . . ? C13 C14 C15 115.1(15) . . ? C19 C15 C16 118.7(11) . . ? C19 C15 C14 118.3(14) . . ? C16 C15 C14 122.9(12) . . ? C17 C16 C15 118.3(10) . . ? C16 C17 C18 118.9(11) . . ? N1 C18 C17 126.2(11) . . ? C15 C19 N1 122.8(12) . . ? C15 C19 C20 124.1(13) . . ? N1 C19 C20 113.0(13) . . ? N2 C20 C12 123.1(11) . . ? N2 C20 C19 122.7(13) . . ? C12 C20 C19 114.2(13) . . ? _refine_diff_density_max 0.442 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.071