#------------------------------------------------------------------------------ #$Date: 2022-10-03 15:40:12 +0100 (Mon, 03 Oct 2022) $ #$Revision: 278324 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010357.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_2010357 loop_ _publ_author_name 'Piorko, A.' 'Christie, S.' 'Zaworotko, M.J.' _publ_section_title ; Hexafluorophosphate Salts of Cyclopentadienyliron(II) Complexes of Dibenzodioxin and 1-Methyldibenzodioxin ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 26 _journal_page_last 29 _journal_paper_doi 10.1107/S010827019400363X _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C17 H13 Fe O2 , P F6' _chemical_formula_sum 'C17 H13 F6 Fe O2 P' _chemical_formula_weight 450.10 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 108.603(6) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 11.0301(14) _cell_length_b 13.7114(8) _cell_length_c 11.6012(12) _cell_measurement_reflns_used 24 _cell_measurement_temperature 290 _cell_measurement_theta_max 45 _cell_measurement_theta_min 35 _cell_volume 1662.9(3) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3072 _diffrn_reflns_theta_max 45 _diffrn_standards_decay_% .0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.07 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_type empirical _exptl_crystal_colour yellow-green _exptl_crystal_density_diffrn 1.80 _exptl_crystal_description cube _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.810 _refine_diff_density_min -0.630 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 5.38 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 244 _refine_ls_number_reflns 2281 _refine_ls_R_factor_obs 0.061 _refine_ls_shift/esd_max 0.109 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F~o~) + 0.000005(F~o~)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.061 _reflns_number_observed 2281 _reflns_number_total 2914 _reflns_observed_criterion I>2.5\s(I) _cod_data_source_file bk1012.cif _cod_data_source_block bk1012_structure_1_of_2 _cod_depositor_comments ; Adding the _atom_site_type_symbol data item. Antanas Vaitkus, 2017-01-26 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F~o~) + 0.000005(F~o~)^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F~o~) + 0.000005(F~o~)^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2010357 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 Fe Fe .36010(9) .80092(6) .10488(7) P P .7999(2) .53409(14) .07874(18) F(1) F .8369(7) .4313(4) .1312(5) F(2) F .8083(10) .5798(5) .1989(5) F(3) F .6587(3) .5046(4) .0558(7) F(4) F .7817(7) .4890(4) -.0483(5) F(5) F .9330(5) .5658(5) .0965(11) F(6) F .7550(6) .6348(3) .0195(5) O(5) O .0886(4) .8765(3) -.0618(4) O(10) O .2475(4) 1.0132(3) .1048(4) C(1) C .3316(6) .8856(5) .2441(5) C(2) C .3346(7) .7856(5) .2744(6) C(3) C .2574(7) .7177(5) .1923(6) C(4) C .1737(6) .7489(4) .0776(6) C(4a) C .1688(6) .8486(4) .0496(6) C(5a) C .0940(6) .9746(4) -.0912(6) C(6) C .0161(6) 1.0036(5) -.2046(6) C(7) C .0185(7) 1.1022(5) -.2363(6) C(8) C .0975(7) 1.1682(5) -.1570(7) C(9) C .1729(6) 1.1371(4) -.0453(6) C(9a) C .1703(6) 1.0405(4) -.0125(5) C(10a) C .2463(6) .9168(4) .1321(6) Cp(1) C .4328(9) .8562(6) -.0223(8) Cp(2) C .5262(7) .8600(6) .0929(8) Cp(3) C .5483(7) .7652(7) .1368(7) Cp(4) C .4693(8) .7017(5) .0495(8) Cp(5) C .3983(8) .7581(7) -.0484(7) H(1) H .395 .938 .306 H(2) H .398 .760 .364 H(3) H .262 .641 .217 H(4) H .115 .696 .013 H(6) H -.046 .952 -.268 H(7) H -.044 1.125 -.327 H(8) H .097 1.244 -.187 H(9) H .235 1.189 .019 H(Cp1) H .395 .918 -.082 H(Cp2) H .575 .925 .140 H(Cp3) H .616 .743 .226 H(Cp4) H .466 .622 .058 H(Cp5) H .326 .730 -.131 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C(4a) O(5) C(5a) 115.9(4) yes C(9a) O(10) C(10a) 115.8(4) yes C(2) C(1) C(10a) 118.7(6) yes C(1) C(2) C(3) 120.8(6) yes C(2) C(3) C(4) 120.4(6) yes C(3) C(4) C(4a) 118.4(6) yes O(5) C(4a) C(4) 117.2(5) yes O(5) C(4a) C(10a) 121.5(5) yes C(4) C(4a) C(10a) 121.2(6) yes O(5) C(5a) C(6) 116.7(5) yes O(5) C(5a) C(9a) 122.7(5) yes C(6) C(5a) C(9a) 120.6(6) yes C(5a) C(6) C(7) 118.0(6) yes C(6) C(7) C(8) 121.1(6) yes C(7) C(8) C(9) 119.4(6) yes C(8) C(9) C(9a) 120.0(6) yes O(10) C(9a) C(5a) 121.6(5) yes O(10) C(9a) C(9) 117.5(5) yes C(5a) C(9a) C(9) 120.8(6) yes O(10) C(10a) C(1) 117.2(5) yes O(10) C(10a) C(4a) 122.3(5) yes C(1) C(10a) C(4a) 120.4(6) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe C(1) 2.093(6) yes Fe C(2) 2.084(6) yes Fe C(3) 2.085(6) yes Fe C(4) 2.103(6) yes Fe C(4a) 2.104(6) yes Fe C(10a) 2.110(6) yes Fe Cp(1) 2.037(7) yes Fe Cp(2) 2.048(7) yes Fe Cp(3) 2.048(7) yes Fe Cp(4) 2.051(7) yes Fe Cp(5) 2.041(7) yes Cp(1) Cp(5) 1.405(13) yes Cp(1) Cp(2) 1.404(13) yes Cp(2) Cp(3) 1.389(13) yes Cp(3) Cp(4) 1.407(13) yes Cp(4) Cp(5) 1.391(13) yes P F(1) 1.538(5) yes P F(2) 1.505(5) yes P F(3) 1.548(6) yes P F(4) 1.551(5) yes P F(5) 1.481(6) yes P F(6) 1.552(5) yes C(1) C(2) 1.413(9) yes C(2) C(3) 1.408(10) yes C(3) C(4) 1.423(10) yes C(4) C(4a) 1.402(9) yes C(4a) C(10a) 1.414(9) yes C(1) C(10a) 1.406(9) yes O(5) C(4a) 1.368(7) yes O(5) C(5a) 1.393(7) yes O(10) C(9a) 1.406(7) yes O(10) C(10a) 1.360(7) yes C(5a) C(6) 1.381(9) yes C(6) C(7) 1.404(10) yes C(7) C(8) 1.382(11) yes C(8) C(9) 1.366(10) yes C(9) C(9a) 1.382(8) yes C(5a) C(9a) 1.367(8) yes F(1) F(3) 2.132(10) no F(1) F(4) 2.127(8) no F(2) F(3) 2.190(10) no F(2) F(5) 2.094(12) no F(2) F(6) 2.113(8) no F(3) F(4) 2.096(8) no F(3) F(6) 2.186(8) no F(5) F(6) 2.104(9) no C(1) H(1) 1.092(6) no C(2) H(2) 1.107(6) no C(3) H(3) 1.091(6) no C(4) H(4) 1.096(6) no C(6) H(6) 1.094(6) no C(7) H(7) 1.100(6) no C(8) H(8) 1.101(6) no C(9) H(9) 1.100(6) no Cp(1) H(Cp1) 1.091(7) no Cp(2) H(Cp2) 1.092(7) no Cp(3) H(Cp3) 1.107(7) no Cp(4) H(Cp4) 1.105(8) no Cp(5) H(Cp5) 1.101(7) no