#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000435.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000435 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_name_common '(9) Zn(DBP)(Et)(py)2' _chemical_formula_moiety 'C26 H36 N2 O Zn' _chemical_formula_sum 'C26 H36 N2 O Zn' _chemical_formula_weight 457.94 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.177(4) _cell_length_b 21.960(7) _cell_length_c 20.531(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.108(5) _cell_angle_gamma 90.00 _cell_volume 4976(3) _cell_formula_units_Z 8 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 168(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 21843 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.1209 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.28 _reflns_number_total 8581 _reflns_number_gt 5156 _reflns_threshold_expression >2sigma(I) _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^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8581 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 Zn1 Zn 0.46818(5) 0.22505(2) 0.89430(3) 0.03217(17) Uani 1 1 d . . . Zn2 Zn 0.83384(6) 1.02933(3) 0.76859(3) 0.04098(19) Uani 1 1 d . . . N1 N 0.5660(3) 0.28279(17) 0.83907(18) 0.0315(10) Uani 1 1 d . . . N2 N 0.2977(3) 0.22828(18) 0.82675(18) 0.0336(10) Uani 1 1 d . . . N3 N 0.6980(4) 1.01486(18) 0.6805(2) 0.0407(11) Uani 1 1 d . . . N4 N 0.7328(4) 0.96657(18) 0.81748(19) 0.0412(11) Uani 1 1 d . . . O1 O 0.4479(3) 0.28223(13) 0.96358(15) 0.0322(8) Uani 1 1 d . . . O2 O 0.9648(3) 0.97497(14) 0.75519(14) 0.0355(8) Uani 1 1 d . . . C1 C 0.6620(5) 0.2631(2) 0.8171(3) 0.0489(15) Uani 1 1 d . . . H1 H 0.6854 0.2218 0.8245 0.059 Uiso 1 1 calc R . . C2 C 0.7315(6) 0.3004(3) 0.7833(3) 0.082(2) Uani 1 1 d . . . H2 H 0.8012 0.2846 0.7680 0.098 Uiso 1 1 calc R . . C3 C 0.6990(7) 0.3594(3) 0.7723(3) 0.0641(19) Uani 1 1 d . . . H3 H 0.7454 0.3856 0.7492 0.077 Uiso 1 1 calc R . . C4 C 0.6007(6) 0.3799(3) 0.7944(4) 0.087(2) Uani 1 1 d . . . H4 H 0.5753 0.4210 0.7874 0.104 Uiso 1 1 calc R . . C5 C 0.5372(5) 0.3406(3) 0.8275(3) 0.075(2) Uani 1 1 d . . . H5 H 0.4675 0.3558 0.8433 0.090 Uiso 1 1 calc R . . C6 C 0.2503(5) 0.1749(2) 0.8062(3) 0.0448(14) Uani 1 1 d . . . H6 H 0.2949 0.1392 0.8201 0.054 Uiso 1 1 calc R . . C7 C 0.1411(5) 0.1684(3) 0.7660(3) 0.0499(15) Uani 1 1 d . . . H7 H 0.1117 0.1290 0.7526 0.060 Uiso 1 1 calc R . . C8 C 0.0751(5) 0.2189(3) 0.7457(3) 0.0552(16) Uani 1 1 d . . . H8 H -0.0010 0.2155 0.7178 0.066 Uiso 1 1 calc R . . C9 C 0.1207(5) 0.2749(3) 0.7662(3) 0.0601(17) Uani 1 1 d . . . H9 H 0.0769 0.3110 0.7529 0.072 Uiso 1 1 calc R . . C10 C 0.2317(5) 0.2775(3) 0.8068(2) 0.0473(14) Uani 1 1 d . . . H10 H 0.2627 0.3163 0.8212 0.057 Uiso 1 1 calc R . . C11 C 0.4507(4) 0.28469(19) 1.0291(2) 0.0281(11) Uani 1 1 d . . . C12 C 0.3398(4) 0.2829(2) 1.0562(2) 0.0321(12) Uani 1 1 d . . . C13 C 0.3452(4) 0.2887(2) 1.1240(2) 0.0360(13) Uani 1 1 d . . . H13 H 0.2718 0.2900 1.1418 0.043 Uiso 1 1 calc R . . C14 C 0.4538(5) 0.2927(2) 1.1661(2) 0.0410(14) Uani 1 1 d . . . H14 H 0.4554 0.2948 1.2125 0.049 Uiso 1 1 calc R . . C15 C 0.5599(5) 0.2936(2) 1.1402(3) 0.0415(14) Uani 1 1 d . . . H15 H 0.6346 0.2961 1.1695 0.050 Uiso 1 1 calc R . . C16 C 0.5616(4) 0.29105(19) 1.0729(2) 0.0317(12) Uani 1 1 d . . . C17 C 0.2155(4) 0.2754(2) 1.0116(2) 0.0354(12) Uani 1 1 d . . . C18 C 0.2096(4) 0.2127(2) 0.9783(2) 0.0434(14) Uani 1 1 d . . . H18A H 0.1346 0.2094 0.9465 0.065 Uiso 1 1 calc R . . H18B H 0.2112 0.1808 1.0118 0.065 Uiso 1 1 calc R . . H18C H 0.2794 0.2077 0.9552 0.065 Uiso 1 1 calc R . . C19 C 0.1955(5) 0.3274(2) 0.9615(3) 0.0501(15) Uani 1 1 d . . . H19A H 0.2627 0.3285 0.9361 0.075 Uiso 1 1 calc R . . H19B H 0.1920 0.3662 0.9848 0.075 Uiso 1 1 calc R . . H19C H 0.1192 0.3210 0.9316 0.075 Uiso 1 1 calc R . . C20 C 0.1092(4) 0.2777(3) 1.0509(3) 0.0563(16) Uani 1 1 d . . . H20A H 0.1083 0.3173 1.0728 0.084 Uiso 1 1 calc R . . H20B H 0.1188 0.2453 1.0842 0.084 Uiso 1 1 calc R . . H20C H 0.0327 0.2719 1.0209 0.084 Uiso 1 1 calc R . . C21 C 0.6854(4) 0.2975(2) 1.0478(3) 0.0390(13) Uani 1 1 d . . . C22 C 0.6818(5) 0.3538(2) 1.0025(3) 0.0580(17) Uani 1 1 d . . . H22A H 0.6683 0.3905 1.0275 0.087 Uiso 1 1 calc R . . H22B H 0.6157 0.3492 0.9652 0.087 Uiso 1 1 calc R . . H22C H 0.7590 0.3573 0.9859 0.087 Uiso 1 1 calc R . . C23 C 0.7903(5) 0.3067(3) 1.1052(3) 0.0591(17) Uani 1 1 d . . . H23A H 0.8669 0.3094 1.0878 0.089 Uiso 1 1 calc R . . H23B H 0.7933 0.2723 1.1357 0.089 Uiso 1 1 calc R . . H23C H 0.7773 0.3445 1.1286 0.089 Uiso 1 1 calc R . . C24 C 0.7163(4) 0.2394(2) 1.0124(3) 0.0468(14) Uani 1 1 d . . . H24A H 0.7947 0.2445 0.9975 0.070 Uiso 1 1 calc R . . H24B H 0.6534 0.2318 0.9743 0.070 Uiso 1 1 calc R . . H24C H 0.7204 0.2049 1.0429 0.070 Uiso 1 1 calc R . . C25 C 0.5282(4) 0.13933(19) 0.9002(2) 0.0341(12) Uani 1 1 d . . . H25A H 0.5021 0.1191 0.8572 0.041 Uiso 1 1 calc R . . H25B H 0.6179 0.1399 0.9083 0.041 Uiso 1 1 calc R . . C26 C 0.4840(5) 0.1018(2) 0.9542(3) 0.0520(16) Uani 1 1 d . . . H26A H 0.5087 0.1216 0.9970 0.078 Uiso 1 1 calc R . . H26B H 0.5194 0.0609 0.9551 0.078 Uiso 1 1 calc R . . H26C H 0.3954 0.0987 0.9451 0.078 Uiso 1 1 calc R . . C27 C 0.6064(5) 1.0542(2) 0.6708(3) 0.0411(13) Uani 1 1 d . . . H27 H 0.6097 1.0886 0.6990 0.049 Uiso 1 1 calc R . . C28 C 0.5080(5) 1.0480(3) 0.6227(3) 0.0524(15) Uani 1 1 d . . . H28 H 0.4452 1.0775 0.6176 0.063 Uiso 1 1 calc R . . C29 C 0.5014(5) 0.9979(3) 0.5816(3) 0.0661(18) Uani 1 1 d . . . H29 H 0.4330 0.9917 0.5485 0.079 Uiso 1 1 calc R . . C30 C 0.5974(5) 0.9567(3) 0.5899(3) 0.0660(18) Uani 1 1 d . . . H30 H 0.5961 0.9217 0.5625 0.079 Uiso 1 1 calc R . . C31 C 0.6939(5) 0.9678(3) 0.6388(3) 0.0513(15) Uani 1 1 d . . . H31 H 0.7611 0.9408 0.6431 0.062 Uiso 1 1 calc R . . C32 C 0.6680(4) 0.9818(2) 0.8633(2) 0.0407(13) Uani 1 1 d . . . H32 H 0.6678 1.0232 0.8766 0.049 Uiso 1 1 calc R . . C33 C 0.6004(5) 0.9406(2) 0.8928(3) 0.0506(16) Uani 1 1 d . . . H33 H 0.5530 0.9537 0.9247 0.061 Uiso 1 1 calc R . . C34 C 0.6030(5) 0.8803(3) 0.8750(3) 0.0481(15) Uani 1 1 d . . . H34 H 0.5584 0.8507 0.8950 0.058 Uiso 1 1 calc R . . C35 C 0.6703(6) 0.8637(2) 0.8285(3) 0.0639(19) Uani 1 1 d . . . H35 H 0.6731 0.8225 0.8148 0.077 Uiso 1 1 calc R . . C36 C 0.7341(6) 0.9079(2) 0.8015(3) 0.070(2) Uani 1 1 d . . . H36 H 0.7821 0.8958 0.7695 0.083 Uiso 1 1 calc R . . C37 C 1.0837(5) 0.98691(19) 0.7635(2) 0.0316(12) Uani 1 1 d . . . C38 C 1.1403(4) 1.0050(2) 0.7087(2) 0.0252(11) Uani 1 1 d . . . C39 C 1.2613(5) 1.0230(2) 0.7197(2) 0.0370(13) Uani 1 1 d . . . H39 H 1.2966 1.0373 0.6835 0.044 Uiso 1 1 calc R . . C40 C 1.3317(5) 1.0208(2) 0.7808(3) 0.0490(15) Uani 1 1 d . . . H40 H 1.4133 1.0346 0.7874 0.059 Uiso 1 1 calc R . . C41 C 1.2793(6) 0.9979(2) 0.8325(3) 0.0542(16) Uani 1 1 d . . . H41 H 1.3283 0.9947 0.8746 0.065 Uiso 1 1 calc R . . C42 C 1.1591(6) 0.9794(2) 0.8262(2) 0.0413(14) Uani 1 1 d . . . C43 C 1.0714(4) 1.0032(2) 0.6374(2) 0.0316(12) Uani 1 1 d . . . C44 C 1.0177(5) 0.9395(2) 0.6226(2) 0.0409(13) Uani 1 1 d . . . H44A H 0.9682 0.9285 0.6562 0.061 Uiso 1 1 calc R . . H44B H 1.0835 0.9099 0.6232 0.061 Uiso 1 1 calc R . . H44C H 0.9672 0.9394 0.5790 0.061 Uiso 1 1 calc R . . C45 C 1.1552(5) 1.0156(3) 0.5859(2) 0.0476(15) Uani 1 1 d . . . H45A H 1.1082 1.0130 0.5414 0.071 Uiso 1 1 calc R . . H45B H 1.2204 0.9853 0.5906 0.071 Uiso 1 1 calc R . . H45C H 1.1903 1.0565 0.5928 0.071 Uiso 1 1 calc R . . C46 C 0.9728(4) 1.0526(2) 0.6263(2) 0.0386(13) Uani 1 1 d . . . H46A H 0.9294 1.0499 0.5811 0.058 Uiso 1 1 calc R . . H46B H 1.0105 1.0929 0.6335 0.058 Uiso 1 1 calc R . . H46C H 0.9157 1.0466 0.6574 0.058 Uiso 1 1 calc R . . C47 C 1.1141(6) 0.9483(3) 0.8850(2) 0.0620(18) Uani 1 1 d . . . C48 C 1.2157(7) 0.9374(3) 0.9430(3) 0.092(3) Uani 1 1 d . . . H48A H 1.2808 0.9141 0.9278 0.139 Uiso 1 1 calc R . . H48B H 1.1839 0.9146 0.9775 0.139 Uiso 1 1 calc R . . H48C H 1.2475 0.9767 0.9607 0.139 Uiso 1 1 calc R . . C49 C 1.0197(6) 0.9889(3) 0.9115(3) 0.072(2) Uani 1 1 d . . . H49A H 1.0584 1.0268 0.9291 0.108 Uiso 1 1 calc R . . H49B H 0.9872 0.9673 0.9466 0.108 Uiso 1 1 calc R . . H49C H 0.9536 0.9983 0.8756 0.108 Uiso 1 1 calc R . . C50 C 1.0565(7) 0.8867(3) 0.8629(3) 0.085(2) Uani 1 1 d . . . H50A H 0.9917 0.8929 0.8253 0.127 Uiso 1 1 calc R . . H50B H 1.0226 0.8682 0.8994 0.127 Uiso 1 1 calc R . . H50C H 1.1183 0.8597 0.8499 0.127 Uiso 1 1 calc R . . C51 C 0.8241(5) 1.1155(2) 0.7964(3) 0.0531(16) Uani 1 1 d . . . H51A H 0.8502 1.1413 0.7616 0.064 Uiso 1 1 calc R . . H51B H 0.7377 1.1250 0.7972 0.064 Uiso 1 1 calc R . . C52 C 0.8959(6) 1.1356(3) 0.8624(3) 0.0665(18) Uani 1 1 d . . . H52A H 0.8727 1.1105 0.8978 0.100 Uiso 1 1 calc R . . H52B H 0.8783 1.1784 0.8703 0.100 Uiso 1 1 calc R . . H52C H 0.9827 1.1307 0.8614 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0330(3) 0.0212(3) 0.0437(4) -0.0020(3) 0.0104(3) -0.0012(3) Zn2 0.0549(4) 0.0241(3) 0.0501(4) 0.0006(3) 0.0271(3) 0.0023(3) N1 0.036(3) 0.021(2) 0.038(2) 0.0001(19) 0.0057(19) -0.004(2) N2 0.033(2) 0.024(2) 0.046(3) -0.002(2) 0.012(2) 0.000(2) N3 0.044(3) 0.029(3) 0.054(3) 0.001(2) 0.023(2) -0.002(2) N4 0.058(3) 0.029(3) 0.043(3) 0.001(2) 0.028(2) 0.002(2) O1 0.034(2) 0.0247(19) 0.040(2) -0.0010(15) 0.0138(16) 0.0002(15) O2 0.046(2) 0.0271(19) 0.037(2) -0.0009(15) 0.0171(17) 0.0017(17) C1 0.061(4) 0.029(3) 0.066(4) -0.007(3) 0.036(3) -0.001(3) C2 0.106(6) 0.059(5) 0.100(6) -0.029(4) 0.077(5) -0.023(4) C3 0.093(6) 0.059(5) 0.040(4) 0.003(3) 0.011(3) -0.042(4) C4 0.058(5) 0.039(4) 0.161(7) 0.050(4) 0.008(5) -0.013(4) C5 0.038(4) 0.038(4) 0.155(7) 0.024(4) 0.034(4) 0.006(3) C6 0.038(4) 0.037(3) 0.059(4) -0.010(3) 0.005(3) 0.004(3) C7 0.036(4) 0.050(4) 0.062(4) -0.019(3) 0.005(3) -0.004(3) C8 0.046(4) 0.079(5) 0.038(3) 0.001(3) -0.001(3) -0.012(4) C9 0.055(4) 0.055(4) 0.065(4) 0.032(3) -0.008(3) -0.003(3) C10 0.053(4) 0.036(3) 0.052(4) 0.005(3) 0.008(3) -0.012(3) C11 0.030(3) 0.016(3) 0.041(3) -0.004(2) 0.013(2) -0.004(2) C12 0.032(3) 0.025(3) 0.040(3) -0.004(2) 0.009(2) 0.002(2) C13 0.034(3) 0.025(3) 0.052(4) 0.000(2) 0.019(3) -0.006(2) C14 0.049(4) 0.038(3) 0.036(3) -0.002(2) 0.008(3) -0.010(3) C15 0.028(3) 0.037(3) 0.056(4) 0.004(3) -0.001(3) -0.006(2) C16 0.033(3) 0.018(3) 0.044(3) -0.005(2) 0.007(3) -0.001(2) C17 0.023(3) 0.039(3) 0.046(3) -0.004(3) 0.010(2) -0.001(2) C18 0.033(3) 0.048(4) 0.050(3) -0.005(3) 0.008(3) -0.009(3) C19 0.044(4) 0.039(4) 0.065(4) 0.004(3) 0.004(3) 0.012(3) C20 0.026(3) 0.080(5) 0.064(4) -0.019(3) 0.011(3) -0.001(3) C21 0.026(3) 0.031(3) 0.060(4) -0.012(3) 0.008(3) 0.002(2) C22 0.042(4) 0.041(4) 0.097(5) -0.004(3) 0.030(3) -0.005(3) C23 0.036(4) 0.063(4) 0.079(4) -0.029(3) 0.012(3) -0.001(3) C24 0.031(3) 0.047(4) 0.062(4) -0.020(3) 0.003(3) 0.005(3) C25 0.037(3) 0.019(3) 0.048(3) -0.004(2) 0.011(2) -0.003(2) C26 0.062(4) 0.026(3) 0.075(4) 0.009(3) 0.032(3) 0.002(3) C27 0.036(3) 0.034(3) 0.058(4) 0.002(3) 0.019(3) 0.000(3) C28 0.034(4) 0.043(4) 0.084(5) 0.005(3) 0.021(3) -0.001(3) C29 0.027(4) 0.063(5) 0.108(5) -0.012(4) 0.011(3) -0.008(3) C30 0.038(4) 0.053(4) 0.107(5) -0.026(4) 0.012(4) -0.010(3) C31 0.033(4) 0.045(4) 0.079(4) -0.006(3) 0.018(3) 0.001(3) C32 0.050(4) 0.027(3) 0.048(3) 0.001(2) 0.017(3) 0.006(3) C33 0.060(4) 0.039(4) 0.061(4) 0.013(3) 0.037(3) 0.009(3) C34 0.050(4) 0.044(4) 0.053(4) 0.018(3) 0.018(3) -0.005(3) C35 0.117(6) 0.025(3) 0.060(4) -0.002(3) 0.045(4) -0.008(3) C36 0.127(6) 0.028(4) 0.070(4) 0.000(3) 0.064(4) 0.005(4) C37 0.048(4) 0.014(3) 0.033(3) -0.005(2) 0.005(3) 0.003(2) C38 0.030(3) 0.018(3) 0.027(3) -0.005(2) 0.002(2) 0.007(2) C39 0.038(3) 0.029(3) 0.044(3) -0.008(2) 0.005(3) 0.004(2) C40 0.041(4) 0.033(3) 0.067(4) -0.017(3) -0.011(3) 0.009(3) C41 0.077(5) 0.033(3) 0.046(4) -0.014(3) -0.011(3) 0.019(3) C42 0.069(4) 0.021(3) 0.031(3) -0.010(2) -0.002(3) 0.014(3) C43 0.027(3) 0.040(3) 0.028(3) -0.001(2) 0.006(2) 0.000(2) C44 0.049(3) 0.042(3) 0.030(3) -0.006(2) 0.002(2) -0.004(3) C45 0.043(3) 0.066(4) 0.036(3) 0.000(3) 0.009(3) 0.000(3) C46 0.033(3) 0.041(3) 0.042(3) 0.010(3) 0.006(2) -0.001(3) C47 0.114(6) 0.048(4) 0.021(3) -0.001(3) 0.000(3) 0.002(4) C48 0.165(8) 0.064(5) 0.041(4) 0.011(3) -0.005(4) 0.018(5) C49 0.118(6) 0.068(5) 0.034(3) -0.004(3) 0.027(4) -0.010(4) C50 0.169(8) 0.038(4) 0.046(4) 0.017(3) 0.012(4) -0.013(4) C51 0.068(4) 0.024(3) 0.074(4) -0.001(3) 0.033(3) -0.001(3) C52 0.085(5) 0.038(4) 0.081(5) -0.024(3) 0.028(4) -0.008(3)