#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005690.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_2005690 loop_ _publ_author_name 'Abrahams, B. F.' 'Hoskins, B. F.' 'Robson, R.' _publ_section_title ; mer-Triaqua(chloranilato-O,O')chloroiron(III) Pentahydrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2766 _journal_page_last 2768 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Fe Cl (C6 Cl2 O4) (H2 O1)3], 5H2 O1' _chemical_formula_sum 'C6 H16 Cl3 Fe O12' _chemical_formula_weight 442.39 _chemical_name_systematic ; mer-triaquaO,O'chloranilatoiron(III) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 110.93(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.880(5) _cell_length_b 7.044(4) _cell_length_c 16.836(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 16.2 _cell_measurement_theta_min 6.2 _cell_volume 1648.2(14) _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4F' _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 0.71069 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 3833 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 1.57 _diffrn_standards_decay_% 1 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.454 _exptl_absorpt_correction_T_max 0.9490 _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_type 'analytical, indexed crystal faces' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_meas 1.77(2) _exptl_crystal_density_method 'flotation in chloroform/1,2-dibromoethane' _exptl_crystal_description 'flat needle' _exptl_crystal_F_000 900 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.308 _refine_diff_density_min -0.269 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 2901 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.024 _refine_ls_restrained_S_obs 1.067 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_obs 0.0345 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0309P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.0740 _refine_ls_wR_factor_obs 0.0663 _reflns_number_observed 2207 _reflns_number_total 2901 _reflns_observed_criterion >2\s(I) _[local]_cod_data_source_file ta1074.cif _[local]_cod_data_source_block fecan _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (18 times). '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (35 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1648.2(13) _cod_database_code 2005690 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Fe 1 0.47044(3) 0.15006(7) 0.22442(3) 0.02459(14) Uani d . Fe Cl1 1 0.35393(5) 0.14030(13) 0.47288(5) 0.0309(2) Uani d . Cl Cl2 1 0.74748(6) 0.44015(15) 0.45119(5) 0.0376(2) Uani d . Cl Cl3 1 0.54999(6) 0.15857(14) 0.13292(5) 0.0394(2) Uani d . Cl O1 1 0.41106(14) 0.1828(3) 0.31871(12) 0.0267(5) Uani d . O O2 1 0.56726(15) 0.3169(3) 0.30933(12) 0.0301(6) Uani d . O O3 1 0.5313(2) 0.2749(4) 0.61509(12) 0.0337(6) Uani d . O O4 1 0.69270(15) 0.3984(4) 0.60539(12) 0.0333(6) Uani d . O O5 1 0.3804(2) 0.3563(4) 0.1623(2) 0.0345(6) Uani d D O O6 1 0.3681(2) -0.0419(4) 0.1663(2) 0.0323(6) Uani d D O O7 1 0.5437(2) -0.0763(4) 0.2902(2) 0.0347(6) Uani d D O C1 1 0.4726(2) 0.2362(5) 0.3903(2) 0.0227(7) Uani d . C C2 1 0.5655(2) 0.3115(4) 0.3850(2) 0.0239(7) Uani d . C C3 1 0.6396(2) 0.3649(5) 0.4571(2) 0.0245(7) Uani d . C C4 1 0.6297(2) 0.3537(5) 0.5371(2) 0.0235(7) Uani d . C C5 1 0.5347(2) 0.2818(4) 0.5434(2) 0.0225(7) Uani d . C C6 1 0.4602(2) 0.2275(5) 0.4672(2) 0.0231(7) Uani d . C O8 1 0.6952(2) 0.3583(4) 0.77274(15) 0.0349(6) Uani d D O O9 1 0.7308(2) -0.1001(4) 0.3473(2) 0.0415(7) Uani d D O O10 1 0.8742(2) -0.0032(5) 0.5152(2) 0.0439(7) Uani d D O O11 1 0.8282(2) 0.0721(5) 0.2587(2) 0.0447(7) Uani d D O O12 1 0.9560(3) 0.2089(5) 0.4144(2) 0.0544(8) Uani d D O H51 1 0.3808(26) 0.3929(53) 0.1186(16) 0.045(12) Uiso d D H H52 1 0.3534(26) 0.4313(47) 0.1802(23) 0.049(14) Uiso d D H H61 1 0.3569(31) -0.1342(43) 0.1885(25) 0.060(15) Uiso d D H H62 1 0.3180(20) -0.0028(61) 0.1358(22) 0.063(15) Uiso d D H H71 1 0.6013(15) -0.0777(53) 0.3059(21) 0.035(11) Uiso d D H H72 1 0.5267(30) -0.1319(57) 0.3229(22) 0.065(16) Uiso d D H H81 1 0.6823(30) 0.3542(66) 0.7233(14) 0.066(15) Uiso d D H H82 1 0.7517(15) 0.3533(64) 0.7891(24) 0.058(15) Uiso d D H H91 1 0.7612(24) -0.0541(54) 0.3218(21) 0.045(13) Uiso d D H H92 1 0.7641(29) -0.0955(69) 0.3966(15) 0.078(17) Uiso d D H H101 1 0.8968(28) 0.0734(48) 0.4933(24) 0.053(15) Uiso d D H H102 1 0.9158(27) -0.0817(54) 0.5309(28) 0.075(19) Uiso d D H H111 1 0.8013(31) 0.1516(52) 0.2248(23) 0.072(17) Uiso d D H H112 1 0.8520(39) 0.0038(75) 0.2346(33) 0.124(26) Uiso d D H H121 1 0.9624(39) 0.3224(32) 0.4152(32) 0.090(20) Uiso d D H H122 1 0.9259(30) 0.1726(64) 0.3681(17) 0.074(17) Uiso d D H 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 Fe 0.0245(2) 0.0285(3) 0.0203(2) -0.0008(2) 0.0074(2) 0.0000(2) Cl1 0.0252(4) 0.0379(5) 0.0309(4) -0.0052(4) 0.0117(3) 0.0012(4) Cl2 0.0262(4) 0.0537(6) 0.0336(4) -0.0103(4) 0.0114(4) -0.0011(4) Cl3 0.0473(5) 0.0420(5) 0.0379(5) -0.0015(5) 0.0261(4) 0.0001(4) O1 0.0216(11) 0.0357(14) 0.0215(10) -0.0042(11) 0.0061(9) -0.0040(10) O2 0.0297(12) 0.042(2) 0.0201(11) -0.0122(11) 0.0105(9) -0.0034(10) O3 0.0355(13) 0.047(2) 0.0194(11) -0.0074(12) 0.0114(10) 0.0028(11) O4 0.0261(12) 0.047(2) 0.0226(11) -0.0049(11) 0.0031(10) 0.0024(11) O5 0.044(2) 0.0329(15) 0.0278(13) 0.0126(13) 0.0149(12) 0.0054(13) O6 0.0234(13) 0.033(2) 0.0319(13) 0.0004(13) -0.0007(11) 0.0001(12) O7 0.0222(13) 0.041(2) 0.0404(14) 0.0055(13) 0.0111(12) 0.0156(13) C1 0.022(2) 0.020(2) 0.025(2) 0.0004(14) 0.0057(13) 0.0033(14) C2 0.026(2) 0.021(2) 0.025(2) -0.0003(14) 0.0096(13) 0.0010(13) C3 0.022(2) 0.025(2) 0.025(2) -0.0008(15) 0.0077(13) 0.0023(14) C4 0.022(2) 0.022(2) 0.023(2) 0.004(2) 0.0038(13) 0.0027(14) C5 0.025(2) 0.017(2) 0.026(2) 0.0005(14) 0.0083(14) 0.0033(14) C6 0.021(2) 0.025(2) 0.024(2) -0.0024(14) 0.0088(13) -0.0001(14) O8 0.0355(15) 0.044(2) 0.0233(13) 0.0037(14) 0.0086(11) 0.0017(12) O9 0.0283(13) 0.056(2) 0.038(2) -0.0061(14) 0.0102(13) 0.0049(14) O10 0.050(2) 0.046(2) 0.0369(15) -0.002(2) 0.0165(14) -0.0020(14) O11 0.053(2) 0.044(2) 0.041(2) 0.009(2) 0.0208(14) 0.0053(15) O12 0.072(2) 0.042(2) 0.044(2) 0.001(2) 0.014(2) 0.001(2) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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_publ_flag O5 Fe O2 97.08(11) y O5 Fe O6 89.11(12) y O2 Fe O6 165.20(10) y O5 Fe O7 171.15(11) y O2 Fe O7 87.84(11) y O6 Fe O7 84.44(12) y O5 Fe O1 86.03(10) y O2 Fe O1 77.57(9) y O6 Fe O1 89.51(10) y O7 Fe O1 87.85(10) y O5 Fe Cl3 92.34(8) y O2 Fe Cl3 93.02(7) y O6 Fe Cl3 100.18(8) y O7 Fe Cl3 94.76(8) y O1 Fe Cl3 170.15(7) y C1 O1 Fe 113.1(2) y C2 O2 Fe 115.2(2) y O1 C1 C6 125.6(3) y O1 C1 C2 114.2(3) y C6 C1 C2 120.3(3) y O2 C2 C3 125.2(3) y O2 C2 C1 114.3(3) y C3 C2 C1 120.5(3) y C2 C3 C4 120.4(3) y C2 C3 Cl2 120.3(2) y C4 C3 Cl2 119.3(2) y O4 C4 C3 124.9(3) y O4 C4 C5 115.4(3) y C3 C4 C5 119.8(3) y O3 C5 C6 125.9(3) y O3 C5 C4 116.2(3) y C6 C5 C4 117.9(3) y C1 C6 C5 121.1(3) y C1 C6 Cl1 120.1(2) y C5 C6 Cl1 118.8(2) y loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe O5 2.000(3) y Fe O2 2.007(2) y Fe O6 2.010(3) y Fe O7 2.024(3) y Fe O1 2.087(2) y Fe Cl3 2.2540(13) y Cl1 C6 1.731(3) y Cl2 C3 1.727(3) y O1 C1 1.282(3) y O2 C2 1.284(3) y O3 C5 1.227(3) y O4 C4 1.237(3) y C1 C6 1.373(4) y C1 C2 1.513(4) y C2 C3 1.369(4) y C3 C4 1.407(4) y C4 C5 1.541(4) y C5 C6 1.415(4) y