#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007105.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, W.' 'Spry, M. P.' 'Willey, G. 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_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 0.024 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.052 _refine_ls_wR_factor_obs 0.050 _reflns_number_observed 2796 _reflns_number_total 3346 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file mu1345.cif _[local]_cod_data_source_block mps _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_original_cell_volume 1425.10(10) _cod_database_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 0.01657(9) 0.01680(9) 0.01342(9) -0.00256(7) 0.00537(6) -0.00142(7) Cl1 0.0260(5) 0.0240(5) 0.0248(5) 0.0037(4) 0.0079(4) 0.0000(4) Cl2 0.0239(5) 0.0181(4) 0.0184(4) -0.0030(3) 0.0052(4) -0.0033(3) Cl3 0.0189(4) 0.0242(5) 0.0253(5) -0.0005(4) 0.0038(4) 0.0008(4) O1 0.0320(17) 0.0307(16) 0.0199(15) -0.0168(12) 0.0128(13) -0.0068(12) O2 0.0269(15) 0.0270(15) 0.0190(15) -0.0107(12) 0.0072(12) -0.0009(12) N11 0.0242(17) 0.0273(17) 0.0208(18) -0.0076(14) 0.0083(14) -0.0057(14) N21 0.041(2) 0.037(2) 0.0216(18) -0.0215(17) 0.0142(16) -0.0054(15) N31 0.055(3) 0.058(3) 0.031(2) -0.031(2) 0.021(2) -0.0055(19) C11 0.041(3) 0.033(2) 0.021(2) -0.0021(19) 0.0078(19) -0.0070(18) C12 0.0198(19) 0.023(2) 0.025(2) -0.0048(15) 0.0081(16) -0.0018(16) C21 0.038(2) 0.031(2) 0.019(2) -0.0004(18) 0.0132(18) -0.0004(17) C22 0.036(2) 0.024(2) 0.023(2) -0.0109(17) 0.0113(18) -0.0033(17) C31 0.107(6) 0.111(6) 0.032(3) -0.088(5) -0.005(3) 0.005(3) C32 0.048(3) 0.050(3) 0.020(2) -0.023(2) 0.014(2) -0.002(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_type_symbol Er1 0.80308(2) 0.08601(2) 0.113730(10) 0.01539(6) Uani d . 1 Er Cl1 1.01041(10) -0.10059(9) 0.15243(6) 0.0248(2) Uani d . 1 Cl Cl2 0.95617(10) 0.28580(9) 0.21281(6) 0.02037(19) Uani d . 1 Cl Cl3 0.57582(9) 0.24644(10) 0.05305(6) 0.02334(19) Uani d . 1 Cl O1 0.9203(3) 0.1953(3) 0.02519(18) 0.0264(6) Uani d D 1 O H1A 0.981(4) 0.251(4) 0.036(3) 0.032 Uiso d D 1 H H1B 0.930(5) 0.167(5) -0.0175(19) 0.032 Uiso d D 1 H O2 0.6378(3) -0.0976(3) 0.11418(18) 0.0242(6) Uani d D 1 O H2A 0.630(5) -0.123(4) 0.1577(19) 0.029 Uiso d D 1 H H2B 0.586(4) -0.142(4) 0.078(2) 0.029 Uiso d D 1 H N11 0.7306(3) -0.0223(3) -0.0301(2) 0.0237(7) Uani d . 1 N N21 0.7591(4) 0.0678(4) 0.2539(2) 0.0321(8) Uani d . 1 N N31 1.1312(5) 0.4017(4) 0.0772(3) 0.0462(11) Uani d . 1 N C11 0.6632(5) -0.1200(4) -0.1867(3) 0.0319(10) Uani d . 1 C H11A 0.6354 -0.0424 -0.2279 0.048 Uiso calc R 1 H H11B 0.5821 -0.1858 -0.1957 0.048 Uiso calc R 1 H H11C 0.7471 -0.1689 -0.1953 0.048 Uiso calc R 1 H C12 0.7004(4) -0.0646(4) -0.0986(3) 0.0224(8) Uani d . 1 C C21 0.7172(5) 0.0788(4) 0.4039(2) 0.0283(9) Uani d . 1 C H21A 0.8108 0.0852 0.4485 0.043 Uiso calc R 1 H H21B 0.6662 -0.0058 0.4135 0.043 Uiso calc R 1 H H21C 0.6590 0.1619 0.4069 0.043 Uiso calc R 1 H C22 0.7403(5) 0.0716(4) 0.3194(3) 0.0269(9) Uani d . 1 C C31 1.3417(7) 0.5754(7) 0.1285(3) 0.089(3) Uani d . 1 C H31A 1.3196 0.6441 0.1680 0.133 Uiso calc R 1 H H31B 1.3555 0.6242 0.0783 0.133 Uiso calc R 1 H H31C 1.4303 0.5245 0.1585 0.133 Uiso calc R 1 H C32 1.2239(5) 0.4779(5) 0.1006(3) 0.0384(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_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)