#------------------------------------------------------------------------------ #$Date: 2017-12-10 02:00:36 +0000 (Sun, 10 Dec 2017) $ #$Revision: 204127 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003351.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_2003351 loop_ _publ_author_name 'Zou, J.-Z.' 'Xu, Z.' 'Li, M.' 'You, X.-Z.' 'Wang, H.-Q.' _publ_section_title ; 7,8,17,18-Tetrabromo-5,10,15,20-tetraphenylporphyrin, C~44~H~26~Br~4~N~4~ ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 760 _journal_page_last 761 _journal_paper_doi 10.1107/S0108270194000053 _journal_volume 51 _journal_year 1995 _chemical_compound_source ; From layering a solution of (I) in CHCl~3~ with petroleum (333-363 K)--piperidine ; _chemical_formula_sum 'C44 H26 Br4 N4' _chemical_formula_weight 930 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 101.4(9) _cell_angle_gamma 90. _cell_formula_units_Z 2 _cell_length_a 13.945(8) _cell_length_b 6.751(8) _cell_length_c 19.326(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 14 _cell_measurement_theta_min 10 _cell_volume 1784(6) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 3532 _diffrn_reflns_theta_max 25 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.5 _exptl_absorpt_correction_T_max 1.12 _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_type empirical _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.73 _exptl_crystal_density_meas 1.774 _exptl_crystal_description Prism _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.64 _refine_diff_density_min 0.0 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 3.89 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 283 _refine_ls_number_reflns 1517 _refine_ls_R_factor_obs 0.074 _refine_ls_shift/esd_max 0.08 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\sF^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.081 _reflns_number_observed 1931 _reflns_number_total 2204 _reflns_observed_criterion F~o~>3\s(F~o~) _cod_data_source_file hu1026.cif _cod_data_source_block hu1026a _cod_depositor_comments ; Adding _space_group_symop_id data item values that were accidentally left out in the previous revision. Antanas Vaitkus, 2017-11-10 Changing the space group from '-P 2yac' to '-P 2yn' after consulting the original publication. All related space group information was changed accordingly. Antanas Vaitkus, 2017-07-04 Adding the _atom_site_type_symbol data item. Antanas Vaitkus, 2017-01-19 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/\sF^2^' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/\sF^2^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1783.3 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2003351 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,y+1/2,-z+1/2 3 -x,-y,-z 4 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_B_iso_or_equiv Br1 Br .3823(1) .4604(3) .0159(1) 5.07(4) Br2 Br .2451(1) .7266(2) .10589(8) 3.72(3) C12 C .2054(9) .479(2) .0658(7) 2.6(3) C13 C .2557(9) .385(2) .0241(7) 2.4(3) C11 C .117(1) .368(2) .0668(7) 2.6(3) C14 C .1984(9) .211(2) -.0047(7) 2.02(2) N1 N .1145(7) .207(2) .0230(5) 2.3(2) N2 N .0778(7) -.153(1) -.0622(6) 2.0(2) C1 C .0491(9) .405(2) .1083(7) 2.5(3) C2 C .2222(9) .078(2) -.0532(7) 2.4(3) C21 C .0691(9) .555(2) .1648(7) 2.5(3) C22 C .136(1) .514(2) .2272(7) 3.4(3) C23 C .152(1) .651(2) .2808(7) 3.3(3) C24 C .104(1) .827(2) .2732(9) 4.6(4) C25 C .040(1) .873(2) .2133(9) 4.3(4) C26 C .020(1) .737(2) .1597(7) 3.3(3) C31 C .3055(9) .110(2) -.0875(7) 2.7(3) C32 C .295(1) .259(3) -.1409(9) 4.9(4) C33 C .460(1) .185(3) -.1560(9) 5.7(5) C34 C .381(1) .299(3) -.170(1) 5.7(5) C35 C .469(1) .034(4) -.106(1) 6.0(5) C36 C .388(1) .001(2) -.0732(8) 4.0(3) C41 C .165(1) -.089(2) -.0778(7) 2.6(3) C42 C .1831(9) -.219(2) -.1345(6) 2.6(3) C43 C .105(1) -.344(2) -.1504(7) 3.2(3) C44 C .0397(9) -.310(2) -.1052(7) 2.2(2) HN2 H .0478 -.0969 -.0267 ? H22 H .171 .389 .232 ? H23 H .197 .622 .324 ? H24 H .116 .922 .311 ? H25 H .007 .999 .209 ? H26 H -.028 .766 .118 ? H32 H .244 .352 -.162 ? H33 H .525 .126 -.154 ? H34 H .333 .400 -.188 ? H35 H .532 -.028 -.104 ? H36 H .392 -.103 -.039 ? H42 H .240 -.215 -.156 ? H43 H .082 -.457 -.180 ? 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 _geom_angle_publ_flag Br2 C12 C13 . . 122.0(10) yes Br2 C12 C11 . . 130.0(10) yes C13 C12 C11 . . 108.0(10) yes Br1 C13 C12 . . 123.0(10) yes Br1 C13 C14 . . 129.0(10) yes C12 C13 C14 . . 108.0(10) yes C11 N1 C14 . . 108.0(10) yes C41 N2 C44 . . 111.0(10) yes C11 C1 C21 . . 120.0(10) yes C11 C1 C44 . 2 127.0(10) yes C21 C1 C44 . 2 113.0(10) yes C14 C2 C31 . . 122.0(10) yes C14 C2 C41 . . 123.0(10) yes C31 C2 C41 . . 114.0(10) yes C12 C11 C1 . . 127.0(10) yes N1 C11 C1 . . 124.0(10) yes C13 C14 N1 . . 108.0(10) yes C13 C14 C2 . . 126.0(10) yes N1 C14 C2 . . 126.0(10) yes N2 C41 C2 . . 130.0(10) yes N2 C41 C42 . . 105.0(10) yes C2 C41 C42 . . 124.0(10) yes C41 C42 C43 . . 107.0(10) yes C42 C43 C44 . . 110.0(10) yes N2 C44 C1 . 2 128.0(10) yes N2 C44 C43 . . 106.0(10) yes C1 C44 C43 2 . 126.0(10) yes C12 C11 N1 . . 109.0(10) yes 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 Br1 C13 . 1.860(10) yes Br2 C12 . 1.880(10) yes C12 C13 . 1.33(2) yes C12 C11 . 1.45(2) yes C13 C14 . 1.47(2) yes N1 C11 . 1.38(2) yes N1 C14 . 1.38(2) yes N2 C41 . 1.38(2) yes N2 C44 . 1.38(2) yes C1 C11 . 1.38(2) yes C1 C21 . 1.47(2) yes C1 C44 2 1.39(2) yes C2 C14 . 1.38(2) yes C2 C31 . 1.46(2) yes C2 C41 . 1.41(2) yes C21 C22 . 1.40(2) no C21 C26 . 1.40(2) no C22 C23 . 1.37(2) no C22 H22 . 0.968(14) no C23 C24 . 1.36(2) no C23 H23 . 0.962(13) no C24 C25 . 1.35(2) no C24 H24 . 0.97(2) no C25 C26 . 1.37(2) no C25 H25 . 0.963(15) no C26 H26 . 0.957(13) no C31 C32 . 1.43(2) no C31 C36 . 1.35(2) no C32 C34 . 1.44(3) no C32 H32 . 0.98(2) no C33 C34 . 1.33(3) no C33 C35 . 1.39(3) no C33 H33 . 0.98(2) no C34 H34 . 0.97(2) no C35 C36 . 1.42(3) no C35 H35 . 0.97(2) no C41 C42 . 1.47(2) yes C42 C43 . 1.36(2) yes C42 H42 . 0.962(13) no C43 C44 . 1.40(2) yes C43 H43 . 0.975(15) no