#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000433.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_4000433 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0493997 _journal_year 2004 _chemical_formula_moiety 'C24 H32 N2 O Zn' _chemical_formula_sum 'C24 H32 N2 O Zn' _chemical_formula_weight 429.89 _chemical_name_common '(8) Zn(DIP)(Et)(py)2' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 94.455(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.9458(11) _cell_length_b 17.864(2) _cell_length_c 14.3718(17) _cell_measurement_reflns_used 996 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 25.07 _cell_measurement_theta_min 2.60 _cell_volume 2289.7(5) _diffrn_ambient_temperature 203(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15804 _diffrn_reflns_theta_max 25.24 _diffrn_reflns_theta_min 1.82 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 258 _refine_ls_number_reflns 4116 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0299 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.9609P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.0782 _reflns_number_gt 3753 _reflns_number_total 4116 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'NONE' changed to 'none' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P21/n _cod_database_code 4000433 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.03902(2) 0.760896(12) 0.019022(15) 0.02927(9) Uani 1 1 d . . . N1 N -0.14172(17) 0.79811(9) 0.09759(11) 0.0340(4) Uani 1 1 d . . . N2 N -0.09598(17) 0.69722(8) -0.08124(11) 0.0297(3) Uani 1 1 d . . . O1 O 0.08517(14) 0.67624(7) 0.09994(9) 0.0315(3) Uani 1 1 d . . . C1 C -0.2144(3) 0.75141(12) 0.15076(17) 0.0437(5) Uani 1 1 d . . . H1 H -0.1846 0.7010 0.1537 0.052 Uiso 1 1 calc R . . C2 C -0.3313(3) 0.77374(14) 0.20160(18) 0.0532(6) Uani 1 1 d . . . H2 H -0.3797 0.7393 0.2385 0.064 Uiso 1 1 calc R . . C3 C -0.3755(3) 0.84725(14) 0.19713(18) 0.0547(6) Uani 1 1 d . . . H3 H -0.4546 0.8640 0.2311 0.066 Uiso 1 1 calc R . . C4 C -0.3024(3) 0.89605(14) 0.14229(18) 0.0552(6) Uani 1 1 d . . . H4 H -0.3312 0.9466 0.1378 0.066 Uiso 1 1 calc R . . C5 C -0.1865(2) 0.86954(12) 0.09403(15) 0.0425(5) Uani 1 1 d . . . H5 H -0.1365 0.9032 0.0569 0.051 Uiso 1 1 calc R . . C6 C -0.1231(2) 0.62425(10) -0.06870(13) 0.0342(4) Uani 1 1 d . . . H6 H -0.0758 0.6002 -0.0162 0.041 Uiso 1 1 calc R . . C7 C -0.2172(2) 0.58311(11) -0.12931(14) 0.0385(5) Uani 1 1 d . . . H7 H -0.2338 0.5321 -0.1182 0.046 Uiso 1 1 calc R . . C8 C -0.2865(2) 0.61797(12) -0.20660(14) 0.0399(5) Uani 1 1 d . . . H8 H -0.3515 0.5911 -0.2489 0.048 Uiso 1 1 calc R . . C9 C -0.2590(2) 0.69307(12) -0.22096(14) 0.0379(5) Uani 1 1 d . . . H9 H -0.3047 0.7182 -0.2731 0.046 Uiso 1 1 calc R . . C10 C -0.1631(2) 0.73028(11) -0.15712(14) 0.0332(4) Uani 1 1 d . . . H10 H -0.1438 0.7812 -0.1672 0.040 Uiso 1 1 calc R . . C11 C 0.1442(3) 0.84670(12) -0.03566(15) 0.0433(5) Uani 1 1 d . . . H11A H 0.2220 0.8261 -0.0727 0.052 Uiso 1 1 calc R . . H11B H 0.0716 0.8724 -0.0791 0.052 Uiso 1 1 calc R . . C12 C 0.2159(4) 0.90413(16) 0.0283(2) 0.0759(9) Uani 1 1 d . . . H12A H 0.1426 0.9235 0.0684 0.114 Uiso 1 1 calc R . . H12B H 0.2537 0.9447 -0.0081 0.114 Uiso 1 1 calc R . . H12C H 0.2983 0.8816 0.0663 0.114 Uiso 1 1 calc R . . C13 C 0.20676(19) 0.64056(9) 0.13524(12) 0.0261(4) Uani 1 1 d . . . C14 C 0.3360(2) 0.63040(10) 0.08580(13) 0.0297(4) Uani 1 1 d . . . C15 C 0.4608(2) 0.59517(11) 0.13082(15) 0.0360(4) Uani 1 1 d . . . H15 H 0.5477 0.5894 0.0987 0.043 Uiso 1 1 calc R . . C16 C 0.4607(2) 0.56842(11) 0.22098(14) 0.0366(4) Uani 1 1 d . . . H16 H 0.5472 0.5462 0.2504 0.044 Uiso 1 1 calc R . . C17 C 0.3318(2) 0.57483(10) 0.26727(13) 0.0325(4) Uani 1 1 d . . . H17 H 0.3304 0.5552 0.3279 0.039 Uiso 1 1 calc R . . C18 C 0.2042(2) 0.60961(9) 0.22646(12) 0.0278(4) Uani 1 1 d . . . C19 C 0.3390(2) 0.65377(12) -0.01563(14) 0.0380(5) Uani 1 1 d . . . H19 H 0.2427 0.6791 -0.0338 0.046 Uiso 1 1 calc R . . C20 C 0.4648(3) 0.70935(16) -0.03111(18) 0.0575(6) Uani 1 1 d . . . H20A H 0.4526 0.7537 0.0064 0.086 Uiso 1 1 calc R . . H20B H 0.4607 0.7232 -0.0965 0.086 Uiso 1 1 calc R . . H20C H 0.5609 0.6863 -0.0131 0.086 Uiso 1 1 calc R . . C21 C 0.3490(3) 0.58556(15) -0.07849(16) 0.0584(6) Uani 1 1 d . . . H21A H 0.4398 0.5579 -0.0602 0.088 Uiso 1 1 calc R . . H21B H 0.3509 0.6017 -0.1428 0.088 Uiso 1 1 calc R . . H21C H 0.2625 0.5536 -0.0725 0.088 Uiso 1 1 calc R . . C22 C 0.0593(2) 0.61482(11) 0.27452(13) 0.0344(4) Uani 1 1 d . . . H22 H 0.0214 0.6666 0.2657 0.041 Uiso 1 1 calc R . . C23 C -0.0593(2) 0.56250(13) 0.22771(17) 0.0469(5) Uani 1 1 d . . . H23A H -0.0713 0.5731 0.1614 0.070 Uiso 1 1 calc R . . H23B H -0.1540 0.5703 0.2548 0.070 Uiso 1 1 calc R . . H23C H -0.0277 0.5109 0.2373 0.070 Uiso 1 1 calc R . . C24 C 0.0760(3) 0.60004(15) 0.37952(16) 0.0540(6) Uani 1 1 d . . . H24A H 0.1077 0.5487 0.3908 0.081 Uiso 1 1 calc R . . H24B H -0.0194 0.6082 0.4056 0.081 Uiso 1 1 calc R . . H24C H 0.1504 0.6338 0.4089 0.081 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 0.03072(14) 0.02476(13) 0.03230(14) 0.00059(8) 0.00219(9) 0.00106(8) N1 0.0332(8) 0.0330(9) 0.0355(9) -0.0028(7) 0.0019(7) 0.0057(7) N2 0.0329(8) 0.0263(8) 0.0301(8) 0.0003(6) 0.0034(6) 0.0025(6) O1 0.0269(6) 0.0333(7) 0.0342(7) 0.0073(6) 0.0019(5) 0.0045(5) C1 0.0414(12) 0.0363(11) 0.0544(14) 0.0019(9) 0.0089(10) 0.0052(9) C2 0.0507(13) 0.0521(15) 0.0592(15) 0.0024(12) 0.0195(12) 0.0004(11) C3 0.0503(14) 0.0563(15) 0.0603(15) -0.0123(12) 0.0217(12) 0.0095(11) C4 0.0668(16) 0.0401(13) 0.0608(15) -0.0066(11) 0.0195(12) 0.0168(11) C5 0.0503(12) 0.0342(11) 0.0440(12) -0.0016(9) 0.0106(10) 0.0057(9) C6 0.0423(11) 0.0264(10) 0.0336(10) 0.0031(8) 0.0017(8) 0.0023(8) C7 0.0503(12) 0.0262(10) 0.0392(11) -0.0019(8) 0.0049(9) -0.0038(9) C8 0.0454(12) 0.0391(12) 0.0347(10) -0.0064(9) -0.0001(9) -0.0046(9) C9 0.0451(11) 0.0368(11) 0.0314(10) 0.0018(8) -0.0005(9) 0.0025(9) C10 0.0401(11) 0.0255(10) 0.0344(10) 0.0028(8) 0.0049(8) 0.0012(8) C11 0.0513(13) 0.0370(11) 0.0427(12) 0.0009(9) 0.0096(10) -0.0074(9) C12 0.099(2) 0.0611(17) 0.0719(18) -0.0196(14) 0.0317(17) -0.0389(16) C13 0.0279(9) 0.0186(8) 0.0314(9) -0.0035(7) 0.0000(7) -0.0014(7) C14 0.0317(10) 0.0234(9) 0.0344(10) -0.0016(7) 0.0050(8) -0.0009(7) C15 0.0288(10) 0.0307(10) 0.0491(12) -0.0032(9) 0.0062(8) 0.0024(8) C16 0.0320(10) 0.0291(10) 0.0470(12) -0.0013(8) -0.0073(9) 0.0041(8) C17 0.0409(10) 0.0237(9) 0.0317(10) -0.0012(7) -0.0046(8) -0.0002(8) C18 0.0334(10) 0.0195(8) 0.0302(9) -0.0037(7) 0.0015(8) -0.0010(7) C19 0.0377(11) 0.0394(11) 0.0380(11) 0.0032(9) 0.0108(9) 0.0084(9) C20 0.0638(16) 0.0563(15) 0.0553(15) 0.0093(12) 0.0236(12) -0.0051(12) C21 0.0782(18) 0.0572(15) 0.0400(13) -0.0074(11) 0.0053(12) 0.0052(13) C22 0.0397(11) 0.0289(10) 0.0354(10) 0.0054(8) 0.0089(8) 0.0051(8) C23 0.0411(12) 0.0407(12) 0.0605(14) 0.0084(10) 0.0137(10) -0.0075(10) C24 0.0640(15) 0.0600(15) 0.0400(12) 0.0107(11) 0.0172(11) 0.0132(12)