#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/71/2007105.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_2007105 loop_ _publ_author_name 'Errington, William' 'Spry, Marcus P.' 'Willey, Gerald R.' _publ_section_title ; Bis(acetonitrile-N)diaquatrichloroerbium(III) Acetonitrile Solvate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 290 _journal_page_last 291 _journal_paper_doi 10.1107/S0108270197015163 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Er Cl3 (C2 H3 N1)2 (H2 O1)2], C2 H3 N' _chemical_formula_moiety 'C6 H13 Cl3 Er N3 O2' _chemical_formula_sum 'C6 H13 Cl3 Er N3 O2' _chemical_formula_weight 432.80 _chemical_name_systematic ; Diacetonitrilediaquotrichloroerbium(III) Acetonitrile Solvate. ; _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 107.036(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.6642(6) _cell_length_b 9.5221(6) _cell_length_c 16.1965(4) _cell_measurement_reflns_used 6151 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 28.75 _cell_measurement_theta_min 2.21 _cell_volume 1425.06(13) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1994a)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXTL/PC _computing_structure_refinement 'SHELXL96 (Sheldrick, 1996b)' _computing_structure_solution 'SHELXTL/PC (Siemens, 1994b)' _diffrn_ambient_temperature 180(2) _diffrn_measurement_device 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 8331 _diffrn_reflns_theta_max 28.75 _diffrn_reflns_theta_min 2.21 _exptl_absorpt_coefficient_mu 6.438 _exptl_absorpt_correction_T_max 0.525 _exptl_absorpt_correction_T_min 0.276 _exptl_absorpt_correction_type 'multi-scan (SADABS; Sheldrick, 1996a)' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 2.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 820 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.86 _refine_diff_density_min '-1.285 e \%A^-3^ (0.80\%A from Er1)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.985 _refine_ls_goodness_of_fit_obs 1.023 _refine_ls_hydrogen_treatment 'H atoms: see below' _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 3346 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.984 _refine_ls_restrained_S_obs 1.022 _refine_ls_R_factor_all 0.034 _refine_ls_R_factor_obs .024 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.052 _refine_ls_wR_factor_obs .050 _reflns_number_observed 2796 _reflns_number_total 3346 _reflns_observed_criterion >2sigma(I) _cod_data_source_file mu1345.cif _cod_data_source_block mps _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P = (Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0249P)^2^] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1425.10(10) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2007105 _cod_database_fobs_code 2007105 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_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 Er1 .01657(9) .01680(9) .01342(9) -.00256(7) .00537(6) -.00142(7) Cl1 .0260(5) .0240(5) .0248(5) .0037(4) .0079(4) .0000(4) Cl2 .0239(5) .0181(4) .0184(4) -.0030(3) .0052(4) -.0033(3) Cl3 .0189(4) .0242(5) .0253(5) -.0005(4) .0038(4) .0008(4) O1 .0320(17) .0307(16) .0199(15) -.0168(12) .0128(13) -.0068(12) O2 .0269(15) .0270(15) .0190(15) -.0107(12) .0072(12) -.0009(12) N11 .0242(17) .0273(17) .0208(18) -.0076(14) .0083(14) -.0057(14) N21 .041(2) .037(2) .0216(18) -.0215(17) .0142(16) -.0054(15) N31 .055(3) .058(3) .031(2) -.031(2) .021(2) -.0055(19) C11 .041(3) .033(2) .021(2) -.0021(19) .0078(19) -.0070(18) C12 .0198(19) .023(2) .025(2) -.0048(15) .0081(16) -.0018(16) C21 .038(2) .031(2) .019(2) -.0004(18) .0132(18) -.0004(17) C22 .036(2) .024(2) .023(2) -.0109(17) .0113(18) -.0033(17) C31 .107(6) .111(6) .032(3) -.088(5) -.005(3) .005(3) C32 .048(3) .050(3) .020(2) -.023(2) .014(2) -.002(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Er1 .80308(2) .08601(2) .113730(10) .01539(6) Uani d . 1 . Er Cl1 1.01041(10) -.10059(9) .15243(6) .0248(2) Uani d . 1 . Cl Cl2 .95617(10) .28580(9) .21281(6) .02037(19) Uani d . 1 . Cl Cl3 .57582(9) .24644(10) .05305(6) .02334(19) Uani d . 1 . Cl O1 .9203(3) .1953(3) .02519(18) .0264(6) Uani d D 1 . O H1A .981(4) .251(4) .036(3) .032 Uiso d D 1 . H H1B .930(5) .167(5) -.0175(19) .032 Uiso d D 1 . H O2 .6378(3) -.0976(3) .11418(18) .0242(6) Uani d D 1 . O H2A .630(5) -.123(4) .1577(19) .029 Uiso d D 1 . H H2B .586(4) -.142(4) .078(2) .029 Uiso d D 1 . H N11 .7306(3) -.0223(3) -.0301(2) .0237(7) Uani d . 1 . N N21 .7591(4) .0678(4) .2539(2) .0321(8) Uani d . 1 . N N31 1.1312(5) .4017(4) .0772(3) .0462(11) Uani d . 1 . N C11 .6632(5) -.1200(4) -.1867(3) .0319(10) Uani d . 1 . C H11A .6354 -.0424 -.2279 .048 Uiso calc R 1 . H H11B .5821 -.1858 -.1957 .048 Uiso calc R 1 . H H11C .7471 -.1689 -.1953 .048 Uiso calc R 1 . H C12 .7004(4) -.0646(4) -.0986(3) .0224(8) Uani d . 1 . C C21 .7172(5) .0788(4) .4039(2) .0283(9) Uani d . 1 . C H21A .8108 .0852 .4485 .043 Uiso calc R 1 . H H21B .6662 -.0058 .4135 .043 Uiso calc R 1 . H H21C .6590 .1619 .4069 .043 Uiso calc R 1 . H C22 .7403(5) .0716(4) .3194(3) .0269(9) Uani d . 1 . C C31 1.3417(7) .5754(7) .1285(3) .089(3) Uani d . 1 . C H31A 1.3196 .6441 .1680 .133 Uiso calc R 1 . H H31B 1.3555 .6242 .0783 .133 Uiso calc R 1 . H H31C 1.4303 .5245 .1585 .133 Uiso calc R 1 . H C32 1.2239(5) .4779(5) .1006(3) .0384(11) Uani d . 1 . C 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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 O1 Er1 O2 141.73(9) ? O1 Er1 N21 149.21(10) ? O2 Er1 N21 69.10(10) y O1 Er1 N11 69.90(10) y O2 Er1 N11 71.80(10) y N21 Er1 N11 140.86(10) ? O1 Er1 Cl1 88.54(8) ? O2 Er1 Cl1 88.14(8) ? N21 Er1 Cl1 93.38(10) ? N11 Er1 Cl1 85.85(8) ? O1 Er1 Cl3 90.79(8) ? O2 Er1 Cl3 86.55(7) ? N21 Er1 Cl3 92.01(10) ? N11 Er1 Cl3 85.07(8) ? Cl1 Er1 Cl3 170.55(3) y O1 Er1 Cl2 76.38(7) y O2 Er1 Cl2 141.89(7) ? N21 Er1 Cl2 72.85(8) y N11 Er1 Cl2 146.26(7) ? Cl1 Er1 Cl2 95.18(3) y Cl3 Er1 Cl2 93.82(3) y C12 N11 Er1 175.5(3) ? C22 N21 Er1 174.0(3) ? N11 C12 C11 179.3(4) y N21 C22 C21 179.0(4) y N31 C32 C31 178.8(5) ? 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 Er1 O1 . 2.318(3) y Er1 O2 . 2.369(3) y Er1 N21 . 2.436(3) y Er1 N11 . 2.455(3) y Er1 Cl1 . 2.6132(9) y Er1 Cl3 . 2.6189(9) y Er1 Cl2 . 2.6443(9) y N11 C12 . 1.135(5) ? N21 C22 . 1.127(5) ? N31 C32 . 1.129(5) ? C11 C12 . 1.463(5) ? C21 C22 . 1.452(5) ? C31 C32 . 1.435(6) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O1 Er1 N11 C12 -18(4) O2 Er1 N11 C12 162(4) N21 Er1 N11 C12 161(4) Cl1 Er1 N11 C12 -108(4) Cl3 Er1 N11 C12 74(4) Cl2 Er1 N11 C12 -15(4) O1 Er1 N21 C22 33(4) O2 Er1 N21 C22 -148(4) N11 Er1 N21 C22 -147(3) Cl1 Er1 N21 C22 126(4) Cl3 Er1 N21 C22 -62(4) Cl2 Er1 N21 C22 31(3) Er1 N11 C12 C11 9E1(3) Er1 N21 C22 C21 -1E1(3)