#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015635.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_7015635 loop_ _publ_author_name 'Di Nicola, C.' 'Garau, F.' 'Marchetti, F.' 'Monari, M.' 'Pandolfo, L.' 'Pettinari, C.' 'Venzo, A.' _publ_section_title ; Synthesis, characterization, crystal structure and preliminary reactivity behaviour of new heteropolytopic ligands based on the 1,3,5-triazine spacer and pyrazolyl, tris-pyrazolylmethyl and tris-pyrazolylethoxy bonding fragments. ; _journal_issue 18 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4941 _journal_page_last 4953 _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C22 H20 F6 N12 O6 S2 Zn' _chemical_formula_weight 791.99 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 68.19(3) _cell_angle_beta 83.31(3) _cell_angle_gamma 82.96(3) _cell_formula_units_Z 1 _cell_length_a 7.9565(16) _cell_length_b 9.891(2) _cell_length_c 10.939(2) _cell_measurement_temperature 293(2) _cell_volume 790.9(3) _computing_cell_refinement SMART _computing_data_collection SMART _computing_data_reduction SAINT+ _computing_molecular_graphics 'SCHAKAL99 (Keller 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.922 _diffrn_measured_fraction_theta_max 0.942 _diffrn_measurement_device_type 'Bruker SMART Apex II CCD' _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 0.2370 _diffrn_reflns_av_sigmaI/netI 0.3756 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3488 _diffrn_reflns_theta_full 21.86 _diffrn_reflns_theta_max 21.86 _diffrn_reflns_theta_min 2.40 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.655 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.174 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 217 _refine_ls_number_reflns 1764 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.984 _refine_ls_R_factor_all 0.2976 _refine_ls_R_factor_gt 0.1524 _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^)+(0.1859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3195 _refine_ls_wR_factor_ref 0.3865 _reflns_number_gt 631 _reflns_number_total 1764 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file c0dt01787f.txt _[local]_cod_data_source_block comp-7 _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7015635 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -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 Zn Zn 0.5000 0.0000 1.0000 0.0566(17) Uani 1 2 d S . . S S 0.7499(9) 0.7011(8) 0.6547(7) 0.074(2) Uani 1 1 d . . . O1 O 0.841(3) 0.680(2) 0.7657(18) 0.121(7) Uani 1 1 d . . . N5 N 0.649(3) 0.072(2) 0.820(2) 0.080(7) Uani 1 1 d . . . C6 C 0.235(3) -0.068(3) 0.711(3) 0.069(8) Uani 1 1 d . . . H4 H 0.2005 -0.0278 0.6257 0.083 Uiso 1 1 calc R . . N2 N 0.309(2) 0.225(2) 0.7819(18) 0.060(4) Uani 1 1 d . . . N6 N 0.563(3) 0.125(2) 0.6999(19) 0.060(4) Uani 1 1 d D . . O2 O 0.625(3) 0.820(2) 0.622(3) 0.160(10) Uani 1 1 d . . . C8 C 0.832(3) 0.136(3) 0.647(4) 0.082(9) Uani 1 1 d . . . H22 H 0.9367 0.1538 0.5992 0.098 Uiso 1 1 calc R . . C11 C 0.388(3) 0.132(3) 0.713(3) 0.074(8) Uani 1 1 d D . . H11 H 0.3521 0.1768 0.6228 0.089 Uiso 1 1 calc R . . N1 N 0.334(2) 0.189(3) 0.9154(18) 0.078(7) Uani 1 1 d . . . N3 N 0.360(3) -0.089(2) 0.889(2) 0.071(6) Uani 1 1 d . . . N4 N 0.327(2) -0.007(2) 0.7641(19) 0.052(5) Uani 1 1 d D . . C1 C 0.256(5) 0.275(3) 0.966(3) 0.114(12) Uani 1 1 d . . . H3 H 0.2598 0.2765 1.0502 0.137 Uiso 1 1 calc R . . C3 C 0.189(3) 0.342(3) 0.748(3) 0.080(9) Uani 1 1 d . . . H1 H 0.1449 0.3859 0.6658 0.096 Uiso 1 1 calc R . . C5 C 0.202(4) -0.192(4) 0.797(3) 0.097(10) Uani 1 1 d . . . H5 H 0.1402 -0.2602 0.7848 0.116 Uiso 1 1 calc R . . C4 C 0.274(3) -0.207(3) 0.909(3) 0.086(9) Uani 1 1 d . . . H6 H 0.2657 -0.2867 0.9884 0.103 Uiso 1 1 calc R . . C7 C 0.801(5) 0.071(3) 0.781(3) 0.091(10) Uani 1 1 d . . . H8 H 0.8867 0.0303 0.8377 0.110 Uiso 1 1 calc R . . C9 C 0.673(4) 0.171(2) 0.597(3) 0.084(10) Uani 1 1 d . . . H7 H 0.6491 0.2164 0.5088 0.101 Uiso 1 1 calc R . . C10 C 0.639(4) 0.549(4) 0.704(4) 0.104(12) Uani 1 1 d . . . F1 F 0.538(3) 0.538(3) 0.805(4) 0.218(16) Uani 1 1 d . . . F2 F 0.726(3) 0.425(2) 0.740(2) 0.182(10) Uani 1 1 d . . . F3 F 0.550(3) 0.539(2) 0.614(3) 0.206(14) Uani 1 1 d . . . O3 O 0.841(3) 0.692(3) 0.545(2) 0.147(10) Uani 1 1 d . . . C2 C 0.149(3) 0.379(3) 0.848(3) 0.076(8) Uani 1 1 d . . . H10 H 0.0693 0.4556 0.8509 0.092 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 Zn 0.051(3) 0.055(3) 0.058(3) -0.015(2) -0.022(2) 0.014(2) S 0.077(5) 0.085(6) 0.066(5) -0.026(4) -0.014(5) -0.022(5) O1 0.141(18) 0.16(2) 0.097(15) -0.076(14) -0.037(14) -0.009(15) N5 0.034(13) 0.091(17) 0.12(2) -0.052(15) -0.007(14) 0.024(12) C6 0.065(17) 0.045(17) 0.12(2) -0.043(18) -0.041(17) 0.003(14) N2 0.058(10) 0.060(9) 0.050(9) -0.014(8) -0.001(8) 0.013(8) N6 0.058(10) 0.060(9) 0.050(9) -0.014(8) -0.001(8) 0.013(8) O2 0.16(2) 0.072(14) 0.21(2) -0.021(15) -0.072(19) 0.075(16) C8 0.034(18) 0.08(2) 0.15(3) -0.07(2) -0.003(19) -0.013(16) C11 0.048(17) 0.08(2) 0.10(2) -0.043(19) -0.030(16) 0.002(15) N1 0.079(15) 0.122(19) 0.047(14) -0.057(14) 0.028(11) -0.012(14) N3 0.071(14) 0.054(14) 0.082(17) -0.026(13) -0.016(13) 0.033(13) N4 0.059(13) 0.047(13) 0.053(14) -0.025(12) 0.000(11) -0.002(11) C1 0.21(4) 0.06(2) 0.08(2) -0.033(19) 0.05(3) -0.06(2) C3 0.064(19) 0.09(2) 0.07(2) -0.011(18) -0.042(16) 0.037(16) C5 0.09(2) 0.09(3) 0.13(3) -0.03(2) -0.03(2) -0.03(2) C4 0.072(18) 0.053(18) 0.14(3) -0.024(17) -0.033(19) -0.041(15) C7 0.09(3) 0.10(2) 0.06(2) -0.003(18) -0.010(19) 0.00(2) C9 0.11(3) 0.024(13) 0.067(18) 0.015(13) 0.04(2) 0.024(15) C10 0.06(2) 0.09(3) 0.16(4) -0.03(3) -0.05(2) 0.02(2) F1 0.13(2) 0.14(2) 0.31(4) 0.00(2) 0.04(2) -0.021(17) F2 0.23(2) 0.078(13) 0.24(2) -0.042(15) -0.12(2) 0.028(16) F3 0.22(2) 0.111(17) 0.28(3) -0.002(17) -0.17(3) -0.076(16) O3 0.137(19) 0.22(3) 0.087(15) -0.050(17) 0.032(14) -0.09(2) C2 0.09(2) 0.044(17) 0.09(2) -0.020(17) -0.013(18) 0.010(15) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 N5 Zn N5 180.000(3) . 2_657 ? N5 Zn N1 86.0(7) . . ? N5 Zn N1 94.0(7) 2_657 . ? N5 Zn N1 94.0(7) . 2_657 ? N5 Zn N1 86.0(7) 2_657 2_657 ? N1 Zn N1 180.0(11) . 2_657 ? N5 Zn N3 82.1(9) . . ? N5 Zn N3 97.9(9) 2_657 . ? N1 Zn N3 82.7(7) . . ? N1 Zn N3 97.3(7) 2_657 . ? N5 Zn N3 97.9(9) . 2_657 ? N5 Zn N3 82.1(9) 2_657 2_657 ? N1 Zn N3 97.3(7) . 2_657 ? N1 Zn N3 82.7(7) 2_657 2_657 ? N3 Zn N3 180.000(4) . 2_657 ? O3 S O2 111.1(15) . . ? O3 S O1 117.3(14) . . ? O2 S O1 116.3(15) . . ? O3 S C10 101.2(19) . . ? O2 S C10 104.8(16) . . ? O1 S C10 103.8(16) . . ? C7 N5 N6 104(2) . . ? C7 N5 Zn 138(2) . . ? N6 N5 Zn 117.8(15) . . ? C5 C6 N4 108(3) . . ? C3 N2 N1 107(2) . . ? C3 N2 C11 132(2) . . ? N1 N2 C11 120.0(19) . . ? C9 N6 C11 132(2) . . ? C9 N6 N5 110(2) . . ? C11 N6 N5 117(2) . . ? C7 C8 C9 105(2) . . ? N6 C11 N2 114.1(19) . . ? N6 C11 N4 113(2) . . ? N2 C11 N4 112.0(19) . . ? C1 N1 N2 115(3) . . ? C1 N1 Zn 130(2) . . ? N2 N1 Zn 115.6(14) . . ? N4 N3 C4 101(2) . . ? N4 N3 Zn 119.3(16) . . ? C4 N3 Zn 140(2) . . ? C6 N4 N3 114(2) . . ? C6 N4 C11 130(2) . . ? N3 N4 C11 116(2) . . ? N1 C1 C2 101(3) . . ? C2 C3 N2 108(2) . . ? C6 C5 C4 107(3) . . ? N3 C4 C5 110(3) . . ? N5 C7 C8 114(3) . . ? N6 C9 C8 106(2) . . ? F1 C10 F2 102(3) . . ? F1 C10 F3 107(3) . . ? F2 C10 F3 102(3) . . ? F1 C10 S 112(3) . . ? F2 C10 S 117(2) . . ? F3 C10 S 116(3) . . ? C3 C2 C1 109(2) . . ? 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 Zn N5 2.10(2) . ? Zn N5 2.10(2) 2_657 ? Zn N1 2.12(2) . ? Zn N1 2.12(2) 2_657 ? Zn N3 2.20(2) . ? Zn N3 2.20(2) 2_657 ? S O3 1.36(2) . ? S O2 1.412(19) . ? S O1 1.422(18) . ? S C10 1.71(4) . ? N5 C7 1.23(3) . ? N5 N6 1.44(2) . ? C6 C5 1.28(3) . ? C6 N4 1.30(3) . ? N2 C3 1.37(3) . ? N2 N1 1.40(2) . ? N2 C11 1.44(3) . ? N6 C9 1.31(2) . ? N6 C11 1.38(2) . ? C8 C7 1.37(3) . ? C8 C9 1.39(3) . ? C11 N4 1.40(2) . ? N1 C1 1.24(3) . ? N3 N4 1.34(2) . ? N3 C4 1.36(3) . ? C1 C2 1.59(4) . ? C3 C2 1.28(3) . ? C5 C4 1.37(3) . ? C10 F1 1.27(4) . ? C10 F2 1.28(3) . ? C10 F3 1.31(4) . ? _journal_paper_doi 10.1039/c0dt01787f