#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000428.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_4000428 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_name_common '(3) Zn4(ONep)4(Et)4' _chemical_formula_sum 'C22 H38 N2 O2 Zn2' _chemical_formula_weight 493.28 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 9.0356(12) _cell_length_b 16.287(2) _cell_length_c 9.0483(12) _cell_angle_alpha 90.00 _cell_angle_beta 110.124(2) _cell_angle_gamma 90.00 _cell_volume 1250.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.199 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.936 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10317 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.22 _reflns_number_total 2857 _reflns_number_gt 2410 _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^)+(0.0400P)^2^+0.6889P] 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 2857 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn 0.63778(3) 1.007652(16) 0.15283(3) 0.02777(11) Uani 1 1 d . . . O1 O 0.58561(18) 1.02696(10) -0.07647(19) 0.0279(4) Uani 1 1 d . . . N1 N 0.7451(2) 0.88811(12) 0.1790(2) 0.0316(5) Uani 1 1 d . . . C1 C 0.7539(4) 1.08320(18) 0.3263(4) 0.0423(7) Uani 1 1 d . . . C2 C 0.6892(5) 1.1704(2) 0.3032(5) 0.0616(10) Uani 1 1 d . . . C3 C 0.6829(3) 1.04701(15) -0.1646(3) 0.0325(6) Uani 1 1 d . . . C4 C 0.7284(5) 0.9688(2) -0.2304(5) 0.0495(8) Uani 1 1 d . . . C5 C 0.5929(4) 1.1040(2) -0.2985(4) 0.0462(7) Uani 1 1 d . . . C6 C 0.8296(4) 1.0899(2) -0.0563(4) 0.0478(7) Uani 1 1 d . . . C7 C 0.6760(4) 0.82771(19) 0.0828(4) 0.0470(8) Uani 1 1 d . . . C8 C 0.7396(5) 0.7506(2) 0.0933(5) 0.0570(9) Uani 1 1 d . . . C9 C 0.8806(4) 0.7351(2) 0.2080(5) 0.0569(9) Uani 1 1 d . . . C10 C 0.9528(4) 0.7963(2) 0.3080(5) 0.0560(9) Uani 1 1 d . . . C11 C 0.8824(3) 0.87199(19) 0.2911(3) 0.0407(6) Uani 1 1 d . . . H1 H 0.747(3) 1.0662(19) 0.422(4) 0.047(9) Uiso 1 1 d . . . H2 H 0.866(3) 1.0825(18) 0.334(3) 0.038(8) Uiso 1 1 d . . . H3 H 0.686(4) 1.193(2) 0.201(5) 0.064(11) Uiso 1 1 d . . . H4 H 0.581(5) 1.173(2) 0.295(5) 0.079(13) Uiso 1 1 d . . . H5 H 0.743(5) 1.208(3) 0.377(5) 0.093(14) Uiso 1 1 d . . . H6 H 0.644(4) 0.942(2) -0.290(4) 0.046(9) Uiso 1 1 d . . . H7 H 0.785(4) 0.931(2) -0.148(4) 0.063(10) Uiso 1 1 d . . . H8 H 0.789(5) 0.980(2) -0.296(5) 0.069(11) Uiso 1 1 d . . . H9 H 0.504(3) 1.0787(18) -0.363(3) 0.036(8) Uiso 1 1 d . . . H10 H 0.657(4) 1.120(2) -0.355(4) 0.049(9) Uiso 1 1 d . . . H11 H 0.557(4) 1.153(2) -0.258(4) 0.063(10) Uiso 1 1 d . . . H12 H 0.898(4) 1.104(2) -0.115(4) 0.061(10) Uiso 1 1 d . . . H13 H 0.796(4) 1.141(2) -0.019(4) 0.057(10) Uiso 1 1 d . . . H14 H 0.885(4) 1.058(2) 0.028(4) 0.056(10) Uiso 1 1 d . . . H15 H 0.591(4) 0.837(2) 0.019(4) 0.050(10) Uiso 1 1 d . . . H16 H 0.697(4) 0.719(2) 0.035(4) 0.048(10) Uiso 1 1 d . . . H17 H 0.923(4) 0.688(2) 0.208(4) 0.058(10) Uiso 1 1 d . . . H18 H 1.048(5) 0.791(3) 0.384(5) 0.096(15) Uiso 1 1 d . . . H19 H 0.926(3) 0.9134(18) 0.357(3) 0.036(8) 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 Zn1 0.02563(17) 0.02577(16) 0.02631(17) -0.00180(11) 0.00178(12) -0.00091(11) O1 0.0213(8) 0.0336(9) 0.0267(9) 0.0035(7) 0.0055(7) -0.0008(7) N1 0.0283(11) 0.0312(11) 0.0307(11) 0.0026(9) 0.0044(9) 0.0018(8) C1 0.0451(18) 0.0406(15) 0.0308(15) -0.0060(12) -0.0002(13) -0.0069(13) C2 0.074(3) 0.0375(17) 0.051(2) -0.0160(15) -0.0062(19) -0.0046(16) C3 0.0325(14) 0.0331(13) 0.0334(14) 0.0030(10) 0.0132(11) 0.0010(10) C4 0.055(2) 0.0494(18) 0.051(2) -0.0024(16) 0.0272(18) 0.0091(16) C5 0.055(2) 0.0481(18) 0.0387(17) 0.0112(14) 0.0200(16) 0.0021(15) C6 0.0345(17) 0.058(2) 0.052(2) 0.0046(16) 0.0168(15) -0.0105(14) C7 0.0380(17) 0.0423(16) 0.0463(18) -0.0027(13) -0.0040(15) 0.0069(13) C8 0.061(2) 0.0339(16) 0.072(2) -0.0098(16) 0.0182(19) 0.0006(15) C9 0.053(2) 0.0356(16) 0.091(3) 0.0232(17) 0.0356(19) 0.0195(15) C10 0.0371(18) 0.057(2) 0.067(2) 0.0228(17) 0.0085(16) 0.0146(15) C11 0.0279(14) 0.0488(17) 0.0380(16) 0.0075(13) 0.0021(12) 0.0010(12)