#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/18/2011833.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011833 loop_ _publ_author_name 'Purushothaman, Bhavana' 'Varghese, Babu' 'Bhyrappa, Puttaiah' _publ_section_title ; [5,10,15,20-Tetrakis(2-thienyl)porphyrinato]zinc(II) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 252 _journal_page_last 253 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Zn (C36 H20 N4 S4)]' _chemical_formula_sum 'C36 H20 N4 S4 Zn' _chemical_formula_weight 702.17 _chemical_name_systematic ; [5,10,15,20-Tetrakis(2-thienyl)porphyrinato]zinc(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 92.704(16) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.6009(11) _cell_length_b 10.9678(17) _cell_length_c 20.278(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 10 _cell_volume 1466.4(5) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'PLATON97 query' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .907 _diffrn_measured_fraction_theta_max .907 _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .037 _diffrn_reflns_av_sigmaI/netI .023 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 2879 _diffrn_reflns_theta_full 25.60 _diffrn_reflns_theta_max 25.60 _diffrn_reflns_theta_min 2.11 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_T_max .86 _exptl_absorpt_correction_T_min .75 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 716 _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _refine_diff_density_max .44 _refine_diff_density_min -.40 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 239 _refine_ls_number_reflns 2637 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all .055 _refine_ls_R_factor_gt .040 _refine_ls_shift/su_max .005 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0438P)^2^+2.6353P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .121 _reflns_number_gt 2163 _reflns_number_total 2637 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file vj1107.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2011833 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Zn 0.5 0.5 0 .03316(19) Uani d S 1 . . Zn S1 0.5960(9) 0.8250(7) .2303(3) .0565(11) Uani d P .615(5) . . S S1' 0.250(2) 0.9269(11) .1579(6) .056(2) Uani d P .386(5) . . S S2 -0.0579(4) 0.2251(3) .16214(13) .0564(6) Uani d P .719(6) . . S S2' -0.2896(13) 0.2522(12) .0532(6) .080(4) Uani d P .281(6) . . S N1 0.3080(4) 0.5291(3) .07163(13) .0324(6) Uani d . 1 . . N N2 0.6625(4) 0.6516(3) .02761(14) .0324(6) Uani d . 1 . . N C1 0.1453(5) 0.4585(3) .08613(17) .0349(8) Uani d . 1 . . C C2 0.0372(6) 0.5163(4) .13648(19) .0436(9) Uani d . 1 . . C H2 -0.0805 0.4878 .1547 .052 Uiso calc R 1 . . H C3 0.1360(6) 0.6190(3) .15267(18) .0406(9) Uani d . 1 . . C H3 0.0996 0.6750 .1844 .049 Uiso calc R 1 . . H C4 0.3072(5) 0.6276(3) .11260(17) .0342(8) Uani d . 1 . . C C5 0.4525(5) 0.7211(3) .11547(16) .0340(8) Uani d . 1 . . C C6 0.4296(5) 0.8162(3) .16527(18) .0373(8) Uani d . 1 . . C C7 0.279(5) 0.903(3) .1713(13) .052(6) Uani d P .614(6) . . C C7' 0.536(5) 0.818(4) .2225(19) .056(8) Uani d P .386(6) . . C C8 0.3097(8) 0.9800(4) .2284(2) .0604(12) Uani d . 1 . . C C9 0.4658(8) 0.9354(5) .2630(2) .0615(13) Uani d . 1 . . C C10 0.6131(5) 0.7326(3) .07504(17) .0346(8) Uani d . 1 . . C C11 0.7439(6) 0.8373(4) .0726(2) .0451(9) Uani d . 1 . . C H11 0.7422 0.9049 .1003 .054 Uiso calc R 1 . . H C12 0.8668(6) 0.8200(4) .0240(2) .0456(9) Uani d . 1 . . C H12 0.9669 0.8730 .0107 .055 Uiso calc R 1 . . H C13 0.8159(5) 0.7035(3) -.00424(17) .0350(8) Uani d . 1 . . C C14 0.0912(5) 0.3470(3) .05731(17) .0350(8) Uani d . 1 . . C C15 -0.0724(6) 0.2758(3) .08605(18) .0378(8) Uani d . 1 . . C C16 -0.256(2) 0.2399(14) .0557(7) .045(3) Uiso d P .719(6) . . C C16' -0.026(5) 0.204(3) .1462(16) .074(13) Uiso d P .281(6) . . C C17 -0.3764(7) 0.1705(5) .1016(3) .0707(14) Uani d . 1 . . C C18 -0.2752(9) 0.1552(5) .1570(3) .0724(15) Uani d . 1 . . C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn .0319(3) .0352(3) .0325(3) -.0051(2) .0031(2) -.0070(2) S1 .065(3) .0603(18) .0423(15) -.0068(18) -.0166(17) -.0095(13) S1' .061(4) .047(4) .061(5) .007(3) .005(4) -.016(4) S2 .0664(13) .0633(13) .0393(11) -.0168(11) .0004(10) .0099(10) S2' .036(4) .101(6) .101(5) -.020(4) -.011(3) .032(4) N1 .0326(15) .0340(16) .0307(14) -.0036(12) .0007(12) -.0016(12) N2 .0296(14) .0338(16) .0338(15) -.0024(12) .0001(11) -.0066(12) C1 .0350(18) .0355(18) .0343(18) -.0019(15) .0039(14) .0005(15) C2 .044(2) .044(2) .044(2) -.0048(17) .0152(16) -.0052(17) C3 .047(2) .038(2) .0371(19) -.0017(16) .0115(16) -.0076(16) C4 .0384(19) .0310(18) .0330(18) .0012(14) .0009(14) -.0033(14) C5 .0386(19) .0321(18) .0308(17) .0014(15) -.0027(14) -.0027(14) C6 .040(2) .036(2) .0360(19) -.0029(16) .0012(15) -.0061(15) C7 .055(11) .054(13) .046(8) -.005(8) -.002(6) -.001(6) C7' .063(19) .051(9) .053(15) -.001(13) -.007(12) -.032(9) C8 .077(3) .051(3) .055(3) -.007(2) .027(2) -.011(2) C9 .083(3) .059(3) .044(2) -.021(3) .012(2) -.013(2) C10 .0352(18) .0336(19) .0347(18) -.0027(15) -.0013(14) -.0066(14) C11 .044(2) .038(2) .054(2) -.0081(17) .0065(18) -.0158(18) C12 .043(2) .039(2) .055(2) -.0129(17) .0089(18) -.0115(18) C13 .0304(18) .0372(19) .0371(18) -.0032(15) -.0010(14) -.0032(15) C14 .0330(18) .0364(19) .0353(18) -.0017(15) .0001(14) .0005(15) C15 .039(2) .0372(19) .0373(19) -.0028(16) .0040(15) -.0018(16) C17 .050(3) .056(3) .108(4) -.012(2) .018(3) .003(3) C18 .099(4) .052(3) .070(3) -.013(3) .036(3) .004(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn N1 3_665 1.998(3) ? Zn N1 . 1.998(3) ? Zn N2 3_665 2.043(3) ? Zn N2 . 2.043(3) ? S1 C9 . 1.642(10) ? S1 C6 . 1.679(6) ? S1' C8 . 1.577(13) ? S1' C6 . 1.700(12) ? S2 C18 . 1.625(6) ? S2 C15 . 1.639(4) ? S2' C17 . 1.465(14) ? S2' C15 . 1.574(9) ? N1 C4 . 1.363(4) ? N1 C1 . 1.367(4) ? N2 C13 . 1.352(4) ? N2 C10 . 1.361(4) ? C1 C14 . 1.395(5) ? C1 C2 . 1.422(5) ? C2 C3 . 1.335(5) ? C3 C4 . 1.426(5) ? C4 C5 . 1.403(5) ? C5 C10 . 1.376(5) ? C5 C6 . 1.465(5) ? C6 C7' . 1.33(3) ? C6 C7 . 1.39(3) ? C7 C8 . 1.44(3) ? C7' C9 . 1.61(4) ? C8 C9 . 1.314(7) ? C10 C11 . 1.439(5) ? C11 C12 . 1.319(5) ? C12 C13 . 1.434(5) ? C13 C14 3_665 1.379(5) ? C14 C13 3_665 1.379(5) ? C14 C15 . 1.474(5) ? C15 C16 . 1.391(14) ? C15 C16' . 1.47(4) ? C16 C17 . 1.466(17) ? C16' C18 . 1.75(3) ? C17 C18 . 1.291(8) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle N1 Zn N1 3_665 . 180 N1 Zn N2 3_665 3_665 90.79(11) N1 Zn N2 . 3_665 89.21(11) N1 Zn N2 3_665 . 89.21(11) N1 Zn N2 . . 90.79(11) N2 Zn N2 3_665 . 180 C9 S1 C6 . . 91.4(4) C8 S1' C6 . . 92.3(6) C18 S2 C15 . . 95.0(3) C17 S2' C15 . . 101.2(7) C4 N1 C1 . . 107.0(3) C4 N1 Zn . . 126.2(2) C1 N1 Zn . . 126.7(2) C13 N2 C10 . . 105.8(3) C13 N2 Zn . . 127.4(2) C10 N2 Zn . . 125.8(2) N1 C1 C14 . . 126.5(3) N1 C1 C2 . . 109.2(3) C14 C1 C2 . . 124.3(3) C3 C2 C1 . . 107.2(3) C2 C3 C4 . . 107.9(3) N1 C4 C5 . . 125.6(3) N1 C4 C3 . . 108.7(3) C5 C4 C3 . . 125.7(3) C10 C5 C4 . . 125.9(3) C10 C5 C6 . . 116.9(3) C4 C5 C6 . . 117.1(3) C7' C6 C7 . . 105(2) C7' C6 C5 . . 123.1(17) C7 C6 C5 . . 130.4(13) C7' C6 S1 . . 9.3(19) C7 C6 S1 . . 109.7(13) C5 C6 S1 . . 119.8(4) C7' C6 S1' . . 113.8(18) C7 C6 S1' . . 10.3(14) C5 C6 S1' . . 122.9(5) S1 C6 S1' . . 117.2(5) C6 C7 C8 . . 113.5(18) C6 C7' C9 . . 108(2) C9 C8 C7 . . 106.7(10) C9 C8 S1' . . 120.3(6) C7 C8 S1' . . 15.1(11) C8 C9 C7' . . 105.2(11) C8 C9 S1 . . 118.1(4) C7' C9 S1 . . 15.0(10) N2 C10 C5 . . 125.3(3) N2 C10 C11 . . 109.4(3) C5 C10 C11 . . 125.1(3) C12 C11 C10 . . 107.5(3) C11 C12 C13 . . 106.7(3) N2 C13 C14 . 3_665 125.1(3) N2 C13 C12 . . 110.5(3) C14 C13 C12 3_665 . 124.4(3) C13 C14 C1 3_665 . 124.3(3) C13 C14 C15 3_665 . 117.2(3) C1 C14 C15 . . 118.5(3) C16 C15 C16' . . 111.1(16) C16 C15 C14 . . 127.9(7) C16' C15 C14 . . 118.9(14) C16 C15 S2' . . 7.2(10) C16' C15 S2' . . 114.4(15) C14 C15 S2' . . 126.1(5) C16 C15 S2 . . 109.4(7) C16' C15 S2 . . 15.7(12) C14 C15 S2 . . 122.7(3) S2' C15 S2 . . 110.7(5) C15 C16 C17 . . 110.7(10) C15 C16' C18 . . 96.2(19) C18 C17 S2' . . 117.4(6) C18 C17 C16 . . 110.3(7) S2' C17 C16 . . 10.3(8) C17 C18 S2 . . 114.4(4) C17 C18 C16' . . 107.5(12) S2 C18 C16' . . 14.9(10) _cod_database_fobs_code 2011833 _journal_paper_doi 10.1107/S0108270100018552