#------------------------------------------------------------------------------ #$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/49/4504984.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4504984 loop_ _publ_author_name 'Michaelides, Adonis' 'Skoulika, Stavroula' _publ_contact_author 'Stavroula Skoulika' _publ_section_title ; Reactive Microporous Rare-Earth Coordination Polymers that Exhibit Single-Crystal-to-Single-Crystal Dehydration and Rehydration ; _journal_issue 2 _journal_name_full 'Crystal Growth & Design' _journal_page_first 529 _journal_paper_doi 10.1021/cg049725v _journal_volume 5 _journal_year 2005 _chemical_formula_sum 'C12 H16 La2 O20' _chemical_formula_weight 758.08 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 95.630(10) _cell_angle_beta 115.610(10) _cell_angle_gamma 110.260(10) _cell_formula_units_Z 2 _cell_length_a 8.3070(10) _cell_length_b 8.7690(10) _cell_length_c 9.2040(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 10.5 _cell_volume 542.31(14) _computing_cell_refinement XSCANS _computing_data_collection XSCANS _computing_data_reduction XSCANS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type P4 _diffrn_measurement_method scintillation _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2017 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.57 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 3.983 _exptl_absorpt_correction_type none _exptl_crystal_colour cplorless _exptl_crystal_density_diffrn 2.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 362 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.668 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type fullcycle _refine_ls_number_parameters 172 _refine_ls_number_reflns 1873 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.131 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0203 _refine_ls_shift/su_max 0.120 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.3052P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.0537 _reflns_number_gt 1819 _reflns_number_total 1873 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cg049725vsi20040805_010139.cif _[local]_cod_data_source_block laacet _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.3052P] 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^)+(0.0206P)^2^+0.3052P] 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 542.31(9) _cod_database_code 4504984 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag La La 0.07992(2) 0.00859(2) 0.269681(19) 0.01618(8) Uani 1 d O1 O -0.1546(3) 0.0260(3) -0.0113(3) 0.0246(5) Uani 1 d O2 O 0.3959(4) 0.0124(4) 0.2626(3) 0.0296(6) Uani 1 d O3 O -0.0939(4) -0.2988(3) 0.0939(3) 0.0334(6) Uani 1 d O4 O -0.0727(5) -0.4885(4) 0.2369(3) 0.0548(11) Uani 1 d O5 O 0.3711(4) 0.2003(3) 0.5497(3) 0.0313(6) Uani 1 d O6 O -0.1909(4) -0.1295(4) 0.3275(4) 0.0395(7) Uani 1 d O7 O 0.2606(4) 0.2964(4) 0.2436(3) 0.0325(6) Uani 1 d O8 O -0.0324(4) 0.2283(4) 0.3418(4) 0.0314(6) Uani 1 d O9 O 0.2123(4) -0.1676(3) 0.4607(3) 0.0267(6) Uani 1 d C1 C 0.3287(5) -0.0048(4) 0.1076(4) 0.0212(7) Uani 1 d C2 C 0.4534(5) -0.0012(5) 0.0334(5) 0.0268(8) Uani 1 d C3 C -0.1508(6) -0.4451(5) 0.1101(5) 0.0305(9) Uani 1 d C4 C 0.3314(6) -0.4241(5) 0.0401(5) 0.0311(9) Uani 1 d C5 C 0.4758(6) -0.3255(5) 0.1653(5) 0.0267(8) Uani 1 d C6 C 0.3491(5) 0.2101(4) 0.6751(4) 0.0217(7) Uani 1 d O10 O 0.6678(6) 0.4410(5) 0.4269(6) 0.0890(16) Uani 1 d H82 H -0.095(9) 0.219(8) 0.404(8) 0.080 Uiso 1 d H71 H 0.227(10) 0.304(9) 0.163(8) 0.080 Uiso 1 d H92 H 0.169(10) -0.260(8) 0.408(8) 0.080 Uiso 1 d H91 H 0.329(10) -0.133(8) 0.521(8) 0.080 Uiso 1 d H72 H 0.430(10) 0.349(8) 0.311(8) 0.080 Uiso 1 d H81 H -0.035(10) 0.313(9) 0.313(8) 0.080 Uiso 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.01429(12) 0.01563(13) 0.01414(12) 0.00413(8) 0.00512(9) 0.00440(9) O1 0.0179(12) 0.0369(15) 0.0187(12) 0.0085(10) 0.0067(10) 0.0146(11) O2 0.0224(13) 0.0462(16) 0.0217(13) 0.0121(11) 0.0098(11) 0.0173(12) O3 0.0391(16) 0.0182(13) 0.0216(13) 0.0038(10) 0.0051(12) 0.0039(12) O4 0.066(3) 0.0247(16) 0.0268(17) 0.0107(13) -0.0058(17) 0.0078(16) O5 0.0315(14) 0.0312(14) 0.0171(12) 0.0028(10) 0.0069(11) 0.0067(12) O6 0.0255(14) 0.0339(16) 0.0568(19) 0.0175(14) 0.0215(14) 0.0080(12) O7 0.0298(15) 0.0285(14) 0.0261(14) 0.0113(12) 0.0102(13) 0.0028(12) O8 0.0439(16) 0.0299(15) 0.0373(16) 0.0180(12) 0.0265(14) 0.0235(13) O9 0.0251(14) 0.0230(13) 0.0251(14) 0.0074(11) 0.0072(11) 0.0100(11) C1 0.0195(17) 0.0263(18) 0.0206(17) 0.0083(14) 0.0106(14) 0.0117(14) C2 0.0237(18) 0.037(2) 0.0255(18) 0.0144(16) 0.0132(15) 0.0169(16) C3 0.037(2) 0.0211(19) 0.0193(17) 0.0019(14) 0.0072(16) 0.0074(16) C4 0.034(2) 0.0215(19) 0.0232(19) 0.0074(16) 0.0075(18) 0.0052(17) C5 0.034(2) 0.0217(18) 0.0214(18) 0.0065(15) 0.0134(17) 0.0091(17) C6 0.0190(17) 0.0165(16) 0.0232(18) 0.0062(13) 0.0063(14) 0.0063(14) O10 0.044(2) 0.040(2) 0.123(4) 0.001(2) -0.003(2) 0.0176(18) 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' La La -0.2871 2.4523 '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_site_symmetry_1 _geom_angle_site_symmetry_3 O6 La O5 105.16(10) . . O6 La O3 74.64(10) . . O5 La O3 139.97(9) . . O6 La O1 92.37(9) . . O5 La O1 139.84(9) . . O3 La O1 79.15(8) . . O6 La O7 138.49(10) . . O5 La O7 69.35(9) . . O3 La O7 136.60(9) . . O1 La O7 73.59(9) . . O6 La O8 70.91(10) . . O5 La O8 77.64(9) . . O3 La O8 135.09(9) . . O1 La O8 74.46(9) . . O7 La O8 67.73(10) . . O6 La O9 77.94(9) . . O5 La O9 69.39(9) . . O3 La O9 71.58(8) . . O1 La O9 150.64(8) . . O7 La O9 130.92(9) . . O8 La O9 126.07(9) . . O6 La O2 148.03(9) . . O5 La O2 73.95(9) . . O3 La O2 85.92(9) . . O1 La O2 108.86(8) . . O7 La O2 72.16(10) . . O8 La O2 136.87(9) . . O9 La O2 71.87(8) . . O6 La O1 138.08(9) . 2 O5 La O1 115.97(8) . 2 O3 La O1 68.96(9) . 2 O1 La O1 61.35(9) . 2 O7 La O1 68.47(9) . 2 O8 La O1 124.27(8) . 2 O9 La O1 108.44(8) . 2 O2 La O1 48.48(7) . 2 O6 La C1 151.63(10) . . O5 La C1 94.61(9) . . O3 La C1 77.14(10) . . O1 La C1 85.02(8) . . O7 La C1 67.54(10) . . O8 La C1 134.40(9) . . O9 La C1 90.62(9) . . O2 La C1 24.17(8) . . O1 La C1 24.34(8) 2 . C1 O1 La 145.6(2) 2 . C1 O1 La 92.72(19) 2 2 La O1 La 118.65(9) . 2 C1 O2 La 96.4(2) . . C3 O3 La 139.6(2) . . C6 O5 La 118.7(2) . . C6 O6 La 168.3(3) 2_556 . La O7 H71 116(6) . . La O7 H72 115(4) . . H71 O7 H72 109(6) . . La O8 H82 124(4) . . La O8 H81 133(5) . . H82 O8 H81 103(6) . . La O9 H92 110(5) . . La O9 H91 119(5) . . H92 O9 H91 110(6) . . O2 C1 O1 122.2(3) . 2 O2 C1 C2 120.0(3) . . O1 C1 C2 117.7(3) 2 . O2 C1 La 59.40(18) . . O1 C1 La 62.94(17) 2 . C2 C1 La 176.9(3) . . C2 C2 C1 176.8(5) 2_655 . O4 C3 O3 126.9(3) . . O4 C3 C4 118.3(3) . 2_545 O3 C3 C4 114.9(3) . 2_545 C5 C4 C3 176.4(4) . 2_545 C4 C5 C6 176.9(4) . 2_656 O5 C6 O6 124.6(3) . 2_556 O5 C6 C5 116.1(3) . 2_656 O6 C6 C5 119.3(3) 2_556 2_656 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 La O6 2.467(3) . La O5 2.503(3) . La O3 2.529(3) . La O1 2.537(2) . La O7 2.547(3) . La O8 2.560(3) . La O9 2.594(3) . La O2 2.642(3) . La O1 2.720(2) 2 La C1 3.051(3) . O1 C1 1.259(4) 2 O1 La 2.720(2) 2 O2 C1 1.257(4) . O3 C3 1.253(5) . O4 C3 1.238(5) . O5 C6 1.244(4) . O6 C6 1.246(4) 2_556 O7 H71 0.69(6) . O7 H72 1.15(7) . O8 H82 0.92(7) . O8 H81 0.82(7) . O9 H92 0.77(6) . O9 H91 0.80(7) . C1 O1 1.259(4) 2 C1 C2 1.461(5) . C2 C2 1.176(7) 2_655 C3 C4 1.477(5) 2_545 C4 C5 1.186(5) . C4 C3 1.477(5) 2_545 C5 C6 1.462(5) 2_656 C6 O6 1.246(4) 2_556 C6 C5 1.462(5) 2_656 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 O6 La O1 C1 7.7(4) . 2 O5 La O1 C1 -109.3(4) . 2 O3 La O1 C1 81.6(4) . 2 O7 La O1 C1 -132.5(4) . 2 O8 La O1 C1 -61.7(4) . 2 O9 La O1 C1 77.1(4) . 2 O2 La O1 C1 163.4(4) . 2 O1 La O1 C1 153.4(5) 2 2 C1 La O1 C1 159.4(4) . 2 O6 La O1 La -145.69(11) . 2 O5 La O1 La 97.25(15) . 2 O3 La O1 La -71.82(12) . 2 O7 La O1 La 74.03(12) . 2 O8 La O1 La 144.88(13) . 2 O9 La O1 La -76.4(2) . 2 O2 La O1 La 10.01(13) . 2 O1 La O1 La 0.0 2 2 C1 La O1 La 6.00(11) . 2 O6 La O2 C1 119.3(2) . . O5 La O2 C1 -147.7(2) . . O3 La O2 C1 67.3(2) . . O1 La O2 C1 -9.8(2) . . O7 La O2 C1 -74.7(2) . . O8 La O2 C1 -96.9(2) . . O9 La O2 C1 139.2(2) . . O1 La O2 C1 2.0(2) 2 . O6 La O3 C3 -51.0(4) . . O5 La O3 C3 44.4(5) . . O1 La O3 C3 -146.5(4) . . O7 La O3 C3 161.9(4) . . O8 La O3 C3 -91.9(4) . . O9 La O3 C3 31.1(4) . . O2 La O3 C3 103.4(4) . . O1 La O3 C3 150.2(4) 2 . C1 La O3 C3 126.2(4) . . O6 La O5 C6 -2.6(3) . . O3 La O5 C6 -86.6(3) . . O1 La O5 C6 110.2(3) . . O7 La O5 C6 134.1(3) . . O8 La O5 C6 63.5(3) . . O9 La O5 C6 -73.1(3) . . O2 La O5 C6 -149.4(3) . . O1 La O5 C6 -174.2(2) 2 . C1 La O5 C6 -162.0(3) . . O5 La O6 C6 171.1(13) . 2_556 O3 La O6 C6 -50.5(13) . 2_556 O1 La O6 C6 27.6(13) . 2_556 O7 La O6 C6 95.2(13) . 2_556 O8 La O6 C6 100.2(13) . 2_556 O9 La O6 C6 -124.5(13) . 2_556 O2 La O6 C6 -105.1(13) . 2_556 O1 La O6 C6 -20.2(13) 2 2_556 C1 La O6 C6 -56.3(13) . 2_556 La O2 C1 O1 -3.8(4) . 2 La O2 C1 C2 176.5(3) . . O6 La C1 O2 -103.5(3) . . O5 La C1 O2 31.0(2) . . O3 La C1 O2 -109.3(2) . . O1 La C1 O2 170.7(2) . . O7 La C1 O2 96.4(2) . . O8 La C1 O2 108.2(2) . . O9 La C1 O2 -38.4(2) . . O1 La C1 O2 -176.4(4) 2 . O6 La C1 O1 72.9(3) . 2 O5 La C1 O1 -152.6(2) . 2 O3 La C1 O1 67.1(2) . 2 O1 La C1 O1 -12.9(2) . 2 O7 La C1 O1 -87.2(2) . 2 O8 La C1 O1 -75.4(2) . 2 O9 La C1 O1 138.1(2) . 2 O2 La C1 O1 176.4(4) . 2 O6 La C1 C2 176(4) . . O5 La C1 C2 -50(4) . . O3 La C1 C2 170(4) . . O1 La C1 C2 90(4) . . O7 La C1 C2 16(4) . . O8 La C1 C2 28(4) . . O9 La C1 C2 -119(4) . . O2 La C1 C2 -81(4) . . O1 La C1 C2 103(4) 2 . O2 C1 C2 C2 -176(10) . 2_655 O1 C1 C2 C2 4(10) 2 2_655 La C1 C2 C2 -98(11) . 2_655 La O3 C3 O4 -31.4(7) . . La O3 C3 C4 148.1(3) . 2_545 C3 C4 C5 C6 -15(14) 2_545 2_656 La O5 C6 O6 0.6(5) . 2_556 La O5 C6 C5 -179.5(2) . 2_656