#------------------------------------------------------------------------------ #$Date: 2011-06-21 19:59:32 +0300 (Tue, 21 Jun 2011) $ #$Revision: 20999 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7205734.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_7205734 loop_ _publ_author_name 'Pochodylo, Amy L.' 'LaDuca, Robert L.' _publ_section_title ; Topological diversity in zinc coordination polymers with 5-substituted isophthalate and bis(4-pyridylmethyl)piperazine ligands ; _journal_issue 7 _journal_name_full CrystEngComm _journal_page_first 2249 _journal_volume 13 _journal_year 2011 _chemical_formula_sum 'C25 H39 N4 O13 Zn' _chemical_formula_weight 668.97 _chemical_name_systematic ; ? ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _audit_update_record ; 2009-12-01 # Formatted by publCIF ; _cell_angle_alpha 90.00 _cell_angle_beta 113.689(1) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.6267(1) _cell_length_b 18.4669(3) _cell_length_c 9.7167(1) _cell_measurement_temperature 173(2) _cell_volume 1581.84(4) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _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 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 14139 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.29 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_correction_T_min 0.7011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 702 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _refine_diff_density_max 0.782 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 3737 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0630 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+1.5647P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1824 _refine_ls_wR_factor_ref 0.1961 _reflns_number_gt 2922 _reflns_number_total 3737 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0ce00715c.txt _[local]_cod_data_source_block p21m _[local]_cod_cif_authors_sg_H-M P2(1)/m _cod_original_cell_volume 1581.84(3) _cod_database_code 7205734 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 0.49162(6) 0.2500 0.28405(6) 0.0317(2) Uani 1 2 d S . . O1 O 0.2828(4) 0.2500 0.1443(4) 0.0498(11) Uani 1 2 d S . . O1W O -0.5298(10) 0.0550(5) -0.0030(8) 0.063(2) Uani 0.50 1 d P . . O2 O -0.2004(4) 0.2500 -0.3245(4) 0.0415(9) Uani 1 2 d S . . O2W O 0.3027(10) 0.2500 0.7154(13) 0.204(6) Uani 1 2 d S . . O3 O -0.4980(7) 0.2109(5) -0.0147(8) 0.079(3) Uani 0.50 1 d P . . O3W O 0.893(3) -0.0583(9) 0.280(2) 0.087(7) Uani 0.30 1 d P . . O4 O -0.3471(4) 0.2500 0.2097(4) 0.0452(10) Uani 1 2 d S . . O4W O 0.8955(9) -0.1300(5) 0.5241(9) 0.182(4) Uani 1 1 d . . . O5 O 0.2146(5) 0.2500 0.3327(4) 0.0705(16) Uani 1 2 d S . . N1 N 0.8941(5) -0.00012(19) 0.8437(5) 0.0646(13) Uani 1 1 d . . . N2 N 0.5572(3) 0.16055(18) 0.4190(3) 0.0349(7) Uani 1 1 d . . . C1 C 0.5079(4) 0.1465(2) 0.5270(4) 0.0373(8) Uani 1 1 d . . . H1 H 0.4308 0.1764 0.5342 0.045 Uiso 1 1 calc R . . C2 C 0.5635(5) 0.0910(2) 0.6274(5) 0.0461(10) Uani 1 1 d . . . H2 H 0.5256 0.0829 0.7026 0.055 Uiso 1 1 calc R . . C3 C 0.6766(5) 0.0463(2) 0.6184(5) 0.0532(11) Uani 1 1 d . . . C4 C 0.7256(6) 0.0598(3) 0.5055(6) 0.0568(12) Uani 1 1 d . . . H4 H 0.8007 0.0298 0.4945 0.068 Uiso 1 1 calc R . . C5 C 0.7402(6) -0.0164(3) 0.7253(6) 0.0696(16) Uani 1 1 d . . . H5A H 0.6703 -0.0280 0.7741 0.084 Uiso 1 1 calc R . . H5B H 0.7467 -0.0596 0.6677 0.084 Uiso 1 1 calc R . . C6 C 0.8850(7) 0.0536(3) 0.9514(6) 0.0770(19) Uani 1 1 d . . . H6A H 0.8151 0.0358 0.9959 0.092 Uiso 1 1 calc R . . H6B H 0.8433 0.0995 0.8981 0.092 Uiso 1 1 calc R . . C7 C 0.9604(7) -0.0676(2) 0.9246(7) 0.086(2) Uani 1 1 d . . . H7A H 0.9700 -0.1034 0.8531 0.103 Uiso 1 1 calc R . . H7B H 0.8922 -0.0882 0.9683 0.103 Uiso 1 1 calc R . . C8 C 0.1835(5) 0.2500 0.1979(5) 0.0316(10) Uani 1 2 d S . . C9 C 0.0219(5) 0.2500 0.0854(5) 0.0244(9) Uani 1 2 d S . . C10 C -0.0967(5) 0.2500 0.1329(5) 0.0285(10) Uani 1 2 d S . . H10 H -0.0764 0.2500 0.2370 0.034 Uiso 1 2 calc SR . . C11 C -0.2447(5) 0.2500 0.0261(5) 0.0330(11) Uani 1 2 d S . . C12 C -0.2758(5) 0.2500 -0.1260(5) 0.0343(11) Uani 1 2 d S . . H12 H -0.3778 0.2500 -0.1982 0.041 Uiso 1 2 calc SR . . C13 C -0.1567(5) 0.2500 -0.1720(5) 0.0289(10) Uani 1 2 d S . . C14 C -0.0087(5) 0.2500 -0.0690(5) 0.0269(9) Uani 1 2 d S . . H14 H 0.0721 0.2500 -0.1016 0.032 Uiso 1 2 calc SR . . C15 C -0.0808(7) 0.2500 -0.3775(6) 0.0538(17) Uani 1 2 d S . . C16 C -0.3742(7) 0.2500 0.0752(7) 0.073(3) Uani 1 2 d S . . C17 C 0.6650(5) 0.1172(2) 0.4085(5) 0.0481(10) Uani 1 1 d . . . H17 H 0.7005 0.1263 0.3319 0.058 Uiso 1 1 calc R . . O2WA O -0.569(2) 0.0117(10) -0.1292(13) 0.082(5) Uani 0.25 1 d P . . O2WB O -0.648(2) 0.1031(11) 0.025(2) 0.081(7) Uani 0.25 1 d P . . O1WA O -0.3998(19) 0.0941(10) 0.0025(17) 0.078(5) Uani 0.25 1 d P . . O3WA O 0.9080(17) -0.0280(16) 0.2932(16) 0.298(15) Uani 0.70 1 d P . . O1WB O -0.6109(19) 0.0820(13) -0.050(3) 0.105(11) Uani 0.25 1 d P . . 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 0.0161(3) 0.0497(4) 0.0254(3) 0.000 0.0044(2) 0.000 O1 0.0163(17) 0.091(3) 0.0341(19) 0.000 0.0022(15) 0.000 O1W 0.080(6) 0.089(5) 0.044(4) -0.029(4) 0.048(4) -0.033(5) O2 0.0261(19) 0.070(3) 0.0247(17) 0.000 0.0063(15) 0.000 O2W 0.061(5) 0.36(2) 0.164(10) 0.000 0.021(6) 0.000 O3 0.034(3) 0.141(7) 0.065(4) -0.043(4) 0.025(3) -0.043(4) O3W 0.094(13) 0.062(8) 0.061(10) 0.038(7) -0.013(8) -0.043(8) O4 0.0257(19) 0.081(3) 0.0289(18) 0.000 0.0113(16) 0.000 O4W 0.204(8) 0.199(8) 0.223(8) 0.090(7) 0.170(7) 0.086(6) O5 0.028(2) 0.148(5) 0.026(2) 0.000 0.0011(17) 0.000 N1 0.060(3) 0.0271(17) 0.064(2) -0.0008(16) -0.019(2) 0.0083(17) N2 0.0227(15) 0.0447(17) 0.0290(14) -0.0018(13) 0.0017(12) 0.0025(13) C1 0.0271(18) 0.044(2) 0.0330(18) -0.0010(16) 0.0042(15) 0.0006(16) C2 0.041(2) 0.045(2) 0.038(2) 0.0037(18) 0.0012(17) -0.0045(19) C3 0.040(2) 0.036(2) 0.054(3) 0.0005(19) -0.0126(19) -0.0007(19) C4 0.047(3) 0.050(3) 0.062(3) -0.005(2) 0.010(2) 0.014(2) C5 0.066(4) 0.037(2) 0.063(3) 0.001(2) -0.018(3) -0.002(2) C6 0.072(4) 0.032(2) 0.075(3) 0.000(2) -0.025(3) 0.013(2) C7 0.090(4) 0.025(2) 0.077(4) 0.000(2) -0.034(3) 0.007(2) C8 0.019(2) 0.038(3) 0.032(2) 0.000 0.0034(19) 0.000 C9 0.016(2) 0.024(2) 0.028(2) 0.000 0.0034(17) 0.000 C10 0.022(2) 0.031(2) 0.031(2) 0.000 0.0090(19) 0.000 C11 0.020(2) 0.049(3) 0.030(2) 0.000 0.0097(19) 0.000 C12 0.016(2) 0.054(3) 0.027(2) 0.000 0.0019(18) 0.000 C13 0.024(2) 0.034(2) 0.025(2) 0.000 0.0053(19) 0.000 C14 0.018(2) 0.029(2) 0.031(2) 0.000 0.0071(18) 0.000 C15 0.035(3) 0.098(5) 0.031(3) 0.000 0.016(2) 0.000 C16 0.024(3) 0.155(8) 0.039(3) 0.000 0.011(3) 0.000 C17 0.039(2) 0.054(3) 0.046(2) -0.0025(19) 0.0117(18) 0.012(2) O2WA 0.118(14) 0.100(12) 0.027(6) -0.002(7) 0.028(8) -0.052(11) O2WB 0.102(15) 0.092(12) 0.093(13) 0.013(10) 0.084(13) 0.008(10) O1WA 0.084(11) 0.098(12) 0.067(9) -0.035(9) 0.044(9) -0.038(10) O3WA 0.112(10) 0.68(4) 0.086(8) 0.016(16) 0.025(7) 0.121(18) O1WB 0.024(8) 0.107(16) 0.114(17) 0.070(15) -0.045(10) -0.035(9) 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' 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 Zn1 O4 119.92(16) . 1_655 ? O1 Zn1 N2 114.76(10) . . ? O4 Zn1 N2 98.65(10) 1_655 . ? O1 Zn1 N2 114.76(10) . 4_565 ? O4 Zn1 N2 98.65(10) 1_655 4_565 ? N2 Zn1 N2 107.78(17) . 4_565 ? C8 O1 Zn1 117.4(3) . . ? C13 O2 C15 116.5(4) . . ? C16 O4 Zn1 122.2(4) . 1_455 ? C6 N1 C7 109.1(4) . . ? C6 N1 C5 111.1(4) . . ? C7 N1 C5 108.8(4) . . ? C1 N2 C17 118.1(3) . . ? C1 N2 Zn1 122.9(3) . . ? C17 N2 Zn1 118.7(3) . . ? N2 C1 C2 123.0(4) . . ? C1 C2 C3 119.3(4) . . ? C4 C3 C2 117.9(4) . . ? C4 C3 C5 120.7(5) . . ? C2 C3 C5 121.4(5) . . ? C3 C4 C17 119.7(4) . . ? N1 C5 C3 112.1(4) . . ? N1 C6 C7 111.2(5) . 3_757 ? N1 C7 C6 110.9(4) . 3_757 ? O5 C8 O1 123.0(5) . . ? O5 C8 C9 121.2(4) . . ? O1 C8 C9 115.8(4) . . ? C10 C9 C14 120.3(4) . . ? C10 C9 C8 120.4(4) . . ? C14 C9 C8 119.3(4) . . ? C11 C10 C9 119.0(4) . . ? C12 C11 C10 121.1(4) . . ? C12 C11 C16 119.2(5) . . ? C10 C11 C16 119.8(4) . . ? C11 C12 C13 119.4(4) . . ? O2 C13 C14 124.5(4) . . ? O2 C13 C12 114.5(4) . . ? C14 C13 C12 121.0(4) . . ? C13 C14 C9 119.2(4) . . ? O4 C16 O3 116.0(5) . 4_565 ? O4 C16 O3 116.0(5) . . ? O3 C16 O3 63.8(9) 4_565 . ? O4 C16 C11 119.4(5) . . ? O3 C16 C11 114.7(5) 4_565 . ? O3 C16 C11 114.7(5) . . ? N2 C17 C4 122.1(4) . . ? 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 Zn1 O1 1.921(4) . ? Zn1 O4 1.958(3) 1_655 ? Zn1 N2 2.045(3) . ? Zn1 N2 2.045(3) 4_565 ? O1 C8 1.259(6) . ? O2 C13 1.368(5) . ? O2 C15 1.438(6) . ? O3 C16 1.367(8) . ? O4 C16 1.226(7) . ? O4 Zn1 1.958(3) 1_455 ? O5 C8 1.221(6) . ? N1 C6 1.470(7) . ? N1 C7 1.475(6) . ? N1 C5 1.496(6) . ? N2 C1 1.340(5) . ? N2 C17 1.347(5) . ? C1 C2 1.367(6) . ? C2 C3 1.397(7) . ? C3 C4 1.381(7) . ? C3 C5 1.511(6) . ? C4 C17 1.382(6) . ? C6 C7 1.514(7) 3_757 ? C7 C6 1.514(7) 3_757 ? C8 C9 1.499(6) . ? C9 C10 1.394(6) . ? C9 C14 1.408(6) . ? C10 C11 1.385(7) . ? C11 C12 1.385(7) . ? C11 C16 1.503(7) . ? C12 C13 1.388(6) . ? C13 C14 1.373(6) . ? C16 O3 1.367(8) 4_565 ? 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 O4 Zn1 O1 C8 180.0 1_655 . . . ? N2 Zn1 O1 C8 62.83(10) . . . . ? N2 Zn1 O1 C8 -62.83(10) 4_565 . . . ? O1 Zn1 N2 C1 -69.0(3) . . . . ? O4 Zn1 N2 C1 162.3(3) 1_655 . . . ? N2 Zn1 N2 C1 60.2(3) 4_565 . . . ? O1 Zn1 N2 C17 117.2(3) . . . . ? O4 Zn1 N2 C17 -11.5(3) 1_655 . . . ? N2 Zn1 N2 C17 -113.5(3) 4_565 . . . ? C17 N2 C1 C2 0.9(6) . . . . ? Zn1 N2 C1 C2 -172.9(3) . . . . ? N2 C1 C2 C3 -0.2(6) . . . . ? C1 C2 C3 C4 -1.0(6) . . . . ? C1 C2 C3 C5 -179.1(4) . . . . ? C2 C3 C4 C17 1.4(7) . . . . ? C5 C3 C4 C17 179.5(4) . . . . ? C6 N1 C5 C3 70.6(6) . . . . ? C7 N1 C5 C3 -169.2(6) . . . . ? C4 C3 C5 N1 77.9(6) . . . . ? C2 C3 C5 N1 -104.1(6) . . . . ? C7 N1 C6 C7 57.4(8) . . . 3_757 ? C5 N1 C6 C7 177.4(5) . . . 3_757 ? C6 N1 C7 C6 -57.3(8) . . . 3_757 ? C5 N1 C7 C6 -178.6(6) . . . 3_757 ? Zn1 O1 C8 O5 0.0 . . . . ? Zn1 O1 C8 C9 180.0 . . . . ? O5 C8 C9 C10 0.0 . . . . ? O1 C8 C9 C10 180.0 . . . . ? O5 C8 C9 C14 180.0 . . . . ? O1 C8 C9 C14 0.0 . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 180.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C16 180.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C16 C11 C12 C13 180.0 . . . . ? C15 O2 C13 C14 0.0 . . . . ? C15 O2 C13 C12 180.0 . . . . ? C11 C12 C13 O2 180.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? O2 C13 C14 C9 180.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 180.0 . . . . ? Zn1 O4 C16 O3 36.0(5) 1_455 . . 4_565 ? Zn1 O4 C16 O3 -36.0(5) 1_455 . . . ? Zn1 O4 C16 C11 180.0 1_455 . . . ? O3 O3 C16 O4 107.7(5) 4_565 . . . ? O3 O3 C16 C11 -106.7(5) 4_565 . . . ? C12 C11 C16 O4 180.0 . . . . ? C10 C11 C16 O4 0.0 . . . . ? C12 C11 C16 O3 -35.6(5) . . . 4_565 ? C10 C11 C16 O3 144.4(5) . . . 4_565 ? C12 C11 C16 O3 35.6(5) . . . . ? C10 C11 C16 O3 -144.4(5) . . . . ? C1 N2 C17 C4 -0.4(6) . . . . ? Zn1 N2 C17 C4 173.6(3) . . . . ? C3 C4 C17 N2 -0.7(7) . . . . ? O1WA O1W O2WA O1WB -108.8(18) . . . . ? O2WB O1W O2WA O1WB 21.1(16) . . . . ? O2WA O1W O2WA O1WB 152.5(15) 3_455 . . . ? O1WB O1W O2WA O1W -152.5(15) . . . 3_455 ? O1WA O1W O2WA O1W 98.7(11) . . . 3_455 ? O2WB O1W O2WA O1W -131.3(11) . . . 3_455 ? O2WA O1W O2WA O1W 0.0 3_455 . . 3_455 ? O2WA O1W O2WB O1WB -36(2) . . . . ? O1WA O1W O2WB O1WB 90(2) . . . . ? O2WA O1W O2WB O1WB -157(2) 3_455 . . . ? O2WA O1W O1WB O2WB 150(2) . . . . ? O1WA O1W O1WB O2WB -105(2) . . . . ? O2WA O1W O1WB O2WB 46(5) 3_455 . . . ? O1WA O1W O1WB O2WA 105.2(12) . . . . ? O2WB O1W O1WB O2WA -150(2) . . . . ? O2WA O1W O1WB O2WA -104(4) 3_455 . . . ? O1W O2WB O1WB O2WA 59(3) . . . . ? O1W O2WA O1WB O1W 29.7(16) 3_455 . . . ? O1W O2WA O1WB O2WB -72(4) . . . . ? O1W O2WA O1WB O2WB -43(4) 3_455 . . . ?