#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000434.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_4000434 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0493997 _journal_year 2004 _chemical_formula_moiety 'C22 H34 N4 O Zn' _chemical_formula_sum 'C22 H34 N4 O Zn' _chemical_formula_weight 435.90 _chemical_name_common '(8a) Zn(DIP)(Et)(MeIm)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 96.162(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.8842(14) _cell_length_b 16.646(3) _cell_length_c 15.350(2) _cell_measurement_reflns_used 930 _cell_measurement_temperature 168(2) _cell_measurement_theta_max 24.46 _cell_measurement_theta_min 2.61 _cell_volume 2256.9(6) _diffrn_ambient_temperature 168(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 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 11221 _diffrn_reflns_theta_max 25.27 _diffrn_reflns_theta_min 1.81 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.107 _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 1.283 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description hexagonal _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 260 _refine_ls_number_reflns 4025 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.090 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0429 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+1.3124P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.0894 _reflns_number_gt 3280 _reflns_number_total 4025 _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 4000434 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 0.96673(4) 0.228849(19) 0.98714(2) 0.02283(11) Uani 1 1 d . . . N1 N 1.1348(2) 0.18250(14) 0.91587(14) 0.0252(5) Uani 1 1 d . . . N2 N 1.3107(3) 0.17449(16) 0.82620(16) 0.0337(6) Uani 1 1 d . . . N3 N 1.0978(3) 0.30782(14) 1.06783(14) 0.0232(5) Uani 1 1 d . . . N4 N 1.2611(3) 0.35748(14) 1.17213(14) 0.0242(5) Uani 1 1 d . . . O1 O 0.9059(2) 0.31113(12) 0.89891(12) 0.0254(4) Uani 1 1 d . . . C1 C 1.2127(3) 0.22252(18) 0.86174(19) 0.0301(7) Uani 1 1 d . . . H1 H 1.2010 0.2782 0.8495 0.036 Uiso 1 1 calc R . . C2 C 1.1865(4) 0.10484(19) 0.9149(2) 0.0351(7) Uani 1 1 d . . . H2 H 1.1512 0.0616 0.9476 0.042 Uiso 1 1 calc R . . C3 C 1.2949(4) 0.0994(2) 0.8605(2) 0.0427(8) Uani 1 1 d . . . H3 H 1.3499 0.0526 0.8482 0.051 Uiso 1 1 calc R . . C4 C 1.4180(4) 0.1990(2) 0.7655(2) 0.0514(10) Uani 1 1 d . . . H4A H 1.3743 0.2429 0.7284 0.077 Uiso 1 1 calc R . . H4B H 1.4395 0.1532 0.7285 0.077 Uiso 1 1 calc R . . H4C H 1.5122 0.2172 0.7987 0.077 Uiso 1 1 calc R . . C5 C 1.1868(3) 0.29199(17) 1.13976(17) 0.0236(6) Uani 1 1 d . . . H5 H 1.1974 0.2402 1.1658 0.028 Uiso 1 1 calc R . . C6 C 1.1173(3) 0.38833(17) 1.05315(18) 0.0298(7) Uani 1 1 d . . . H6 H 1.0677 0.4176 1.0053 0.036 Uiso 1 1 calc R . . C7 C 1.2175(3) 0.41996(17) 1.11665(18) 0.0302(7) Uani 1 1 d . . . H7 H 1.2507 0.4742 1.1218 0.036 Uiso 1 1 calc R . . C8 C 1.3712(4) 0.3606(2) 1.24953(19) 0.0359(8) Uani 1 1 d . . . H8A H 1.3648 0.3111 1.2836 0.054 Uiso 1 1 calc R . . H8B H 1.3496 0.4069 1.2856 0.054 Uiso 1 1 calc R . . H8C H 1.4733 0.3658 1.2315 0.054 Uiso 1 1 calc R . . C9 C 0.7838(3) 0.34863(16) 0.86315(17) 0.0205(6) Uani 1 1 d . . . C10 C 0.7859(3) 0.38028(16) 0.77658(17) 0.0212(6) Uani 1 1 d . . . C11 C 0.6560(3) 0.41587(16) 0.73527(18) 0.0250(6) Uani 1 1 d . . . H11 H 0.6565 0.4352 0.6771 0.030 Uiso 1 1 calc R . . C12 C 0.5259(3) 0.42393(18) 0.77647(19) 0.0300(7) Uani 1 1 d . . . H12 H 0.4372 0.4470 0.7465 0.036 Uiso 1 1 calc R . . C13 C 0.5271(3) 0.39795(17) 0.86161(19) 0.0283(7) Uani 1 1 d . . . H13 H 0.4388 0.4053 0.8906 0.034 Uiso 1 1 calc R . . C14 C 0.6534(3) 0.36111(16) 0.90704(18) 0.0236(6) Uani 1 1 d . . . C15 C 0.9329(3) 0.37628(17) 0.73512(18) 0.0256(6) Uani 1 1 d . . . H15 H 0.9708 0.3198 0.7414 0.031 Uiso 1 1 calc R . . C16 C 1.0527(3) 0.43045(19) 0.7837(2) 0.0352(7) Uani 1 1 d . . . H16A H 1.0181 0.4864 0.7797 0.053 Uiso 1 1 calc R . . H16B H 1.1477 0.4255 0.7571 0.053 Uiso 1 1 calc R . . H16C H 1.0691 0.4143 0.8454 0.053 Uiso 1 1 calc R . . C17 C 0.9184(4) 0.39711(19) 0.63721(19) 0.0363(8) Uani 1 1 d . . . H17A H 0.8419 0.3624 0.6055 0.054 Uiso 1 1 calc R . . H17B H 1.0161 0.3888 0.6144 0.054 Uiso 1 1 calc R . . H17C H 0.8879 0.4534 0.6291 0.054 Uiso 1 1 calc R . . C18 C 0.6534(3) 0.33960(17) 1.00306(19) 0.0288(7) Uani 1 1 d . . . H18 H 0.7442 0.3052 1.0195 0.035 Uiso 1 1 calc R . . C19 C 0.6709(4) 0.4150(2) 1.0601(2) 0.0510(10) Uani 1 1 d . . . H19A H 0.7632 0.4436 1.0488 0.077 Uiso 1 1 calc R . . H19B H 0.6775 0.3996 1.1220 0.077 Uiso 1 1 calc R . . H19C H 0.5830 0.4501 1.0460 0.077 Uiso 1 1 calc R . . C20 C 0.5155(4) 0.2920(2) 1.0231(2) 0.0438(9) Uani 1 1 d . . . H20A H 0.4247 0.3253 1.0112 0.066 Uiso 1 1 calc R . . H20B H 0.5272 0.2759 1.0848 0.066 Uiso 1 1 calc R . . H20C H 0.5056 0.2439 0.9860 0.066 Uiso 1 1 calc R . . C21 C 0.8479(3) 0.14306(18) 1.03863(19) 0.0292(7) Uani 1 1 d . . . H21A H 0.9195 0.1046 1.0700 0.035 Uiso 1 1 calc R . . H21B H 0.7883 0.1678 1.0825 0.035 Uiso 1 1 calc R . . C22 C 0.7402(4) 0.0965(2) 0.9730(2) 0.0411(8) Uani 1 1 d . . . H22A H 0.6718 0.1341 0.9393 0.062 Uiso 1 1 calc R . . H22B H 0.6808 0.0587 1.0044 0.062 Uiso 1 1 calc R . . H22C H 0.7987 0.0667 0.9330 0.062 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 0.02348(18) 0.02210(18) 0.02296(18) 0.00060(15) 0.00273(12) 0.00083(15) N1 0.0232(12) 0.0276(14) 0.0243(13) -0.0029(11) 0.0002(10) 0.0039(11) N2 0.0308(14) 0.0394(16) 0.0325(14) -0.0069(12) 0.0107(11) 0.0021(12) N3 0.0277(13) 0.0196(12) 0.0225(12) -0.0013(10) 0.0024(10) -0.0005(10) N4 0.0262(13) 0.0258(13) 0.0205(12) -0.0009(10) 0.0022(10) 0.0015(10) O1 0.0224(10) 0.0287(11) 0.0257(10) 0.0089(9) 0.0047(8) 0.0050(9) C1 0.0301(16) 0.0272(17) 0.0328(16) -0.0026(14) 0.0031(13) 0.0033(14) C2 0.0398(19) 0.0292(17) 0.0366(18) 0.0014(14) 0.0054(15) 0.0075(14) C3 0.048(2) 0.0302(19) 0.052(2) -0.0080(16) 0.0124(17) 0.0138(16) C4 0.048(2) 0.060(2) 0.051(2) -0.0123(19) 0.0279(18) -0.0067(18) C5 0.0268(15) 0.0216(15) 0.0233(15) -0.0007(12) 0.0071(12) 0.0020(12) C6 0.0383(18) 0.0242(16) 0.0261(16) 0.0040(13) -0.0005(13) 0.0056(13) C7 0.0406(18) 0.0187(16) 0.0304(16) -0.0019(13) 0.0006(14) 0.0003(13) C8 0.0398(19) 0.0398(19) 0.0257(16) -0.0028(14) -0.0072(14) -0.0010(15) C9 0.0223(15) 0.0163(14) 0.0224(14) -0.0039(11) -0.0001(11) -0.0016(11) C10 0.0252(15) 0.0147(14) 0.0235(14) -0.0026(11) 0.0015(11) -0.0004(11) C11 0.0307(16) 0.0211(15) 0.0222(15) -0.0004(12) -0.0014(12) 0.0007(12) C12 0.0235(16) 0.0270(17) 0.0377(18) 0.0030(14) -0.0043(13) 0.0050(13) C13 0.0222(15) 0.0262(16) 0.0373(17) 0.0029(14) 0.0074(13) 0.0021(12) C14 0.0230(15) 0.0210(15) 0.0273(15) -0.0003(12) 0.0051(12) -0.0003(12) C15 0.0292(16) 0.0224(16) 0.0265(15) 0.0040(12) 0.0089(12) 0.0030(12) C16 0.0304(17) 0.0374(19) 0.0390(18) 0.0071(15) 0.0095(14) -0.0045(14) C17 0.0444(19) 0.0344(18) 0.0325(17) 0.0063(14) 0.0154(15) 0.0042(15) C18 0.0282(16) 0.0298(17) 0.0299(16) 0.0046(13) 0.0096(13) 0.0091(13) C19 0.068(3) 0.057(3) 0.0277(18) -0.0039(16) 0.0031(17) -0.012(2) C20 0.049(2) 0.042(2) 0.043(2) 0.0012(16) 0.0193(17) -0.0081(16) C21 0.0321(17) 0.0264(17) 0.0291(16) 0.0045(13) 0.0028(13) -0.0015(13) C22 0.045(2) 0.041(2) 0.0378(19) -0.0029(16) 0.0088(16) -0.0124(16)