#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/07/2200764.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_2200764 loop_ _publ_author_name 'Urs, Usha K.' 'Shalini, K.' 'Cameron, T. S.' 'Shivashankar, S. A.' 'Guru Row, T. N.' _publ_section_title ; Low-temperature structure of a twinned crystal of tris(2,4-pentanedionato)(1,10-phenanthroline)samarium(III) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m457 _journal_page_last m458 _journal_paper_doi 10.1107/S1600536801014398 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Sm (C5 H7 O2)3 (C12 H8 N2)]' _chemical_formula_moiety 'C27 H29 N2 O6 Sm' _chemical_formula_sum 'C27 H29 N2 O6 Sm' _chemical_formula_weight 627.87 _chemical_name_systematic ; tris(2,4-pentadionato)(1,10-phenanthroline)samarium(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 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 98.899(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.432(2) _cell_length_b 20.957(5) _cell_length_c 14.728(3) _cell_measurement_reflns_used 23142 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.04 _cell_measurement_theta_min 2.96 _cell_volume 2876.2(11) _computing_data_collection 'CrystalClear (Rigaku, 1999)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_measured_fraction_theta_full .835 _diffrn_measured_fraction_theta_max .835 _diffrn_measurement_device 'Rigaku AFC8 coupled with mercury CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 23142 _diffrn_reflns_theta_full 25.04 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_min 2.96 _exptl_absorpt_coefficient_mu 2.081 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1260 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _refine_diff_density_max 2.484 _refine_diff_density_min -1.882 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.323 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 332 _refine_ls_number_reflns 5098 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.323 _refine_ls_R_factor_gt .0729 _refine_ls_shift/su_max .005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+55.2376P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .2006 _reflns_number_gt 4253 _reflns_number_total 23142 _reflns_threshold_expression I>2\s(I) _cod_data_source_file wn6044.cif _cod_data_source_block I _cod_depositor_comments ; Changing ' ' values to '.' in '_atom_site' loop. Antanas Vaitkus, 2015-03-24 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 2876.0(10) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2200764 _cod_database_fobs_code 2200764 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_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Sm1 .41619(4) .154403(16) .16003(2) .02731(12) Uani d . 1 . . Sm O1 .2562(5) .1074(2) .0416(3) .0362(12) Uani d . 1 . . O O2 .4770(5) .0445(2) .1545(3) .0384(12) Uani d . 1 . . O O3 .5312(5) .2539(2) .2005(3) .0411(12) Uani d . 1 . . O C12 .7762(7) .1213(3) .1610(5) .0357(17) Uani d . 1 . . C H12 .7567 .0973 .2124 .043 Uiso calc R 1 . . H O4 .2371(5) .2346(2) .1495(3) .0370(12) Uani d . 1 . . O C4 .6053(9) .2482(3) -.0997(5) .0409(19) Uani d . 1 . . C C1 .3390(8) .2350(3) -.0540(5) .0404(19) Uani d . 1 . . C H1 .2455 .2315 -.0381 .048 Uiso calc R 1 . . H C13 .4191(8) -.0047(3) .1132(5) .0389(18) Uani d . 1 . . C C11 .9171(8) .1225(3) .1439(6) .042(2) Uani d . 1 . . C H11 .9907 .0994 .1813 .05 Uiso calc R 1 . . H C15 .2301(7) .0510(4) .0103(5) .0362(18) Uani d . 1 . . C N1 .4474(6) .2098(3) .0033(4) .0294(14) Uani d . 1 . . N C2 .3529(10) .2663(4) -.1355(5) .047(2) Uani d . 1 . . C H2 .2715 .2823 -.1751 .056 Uiso calc R 1 . . H C17 .4882(10) -.0675(4) .1437(6) .061(3) Uani d . 1 . . C H17A .5492 -.0622 .2033 .091 Uiso calc R 1 . . H H17B .5467 -.0822 .0982 .091 Uiso calc R 1 . . H H17C .4135 -.0992 .1492 .091 Uiso calc R 1 . . H C18 .2343(8) .2952(4) .1499(5) .042(2) Uani d . 1 . . C C22 .0896(9) .3260(4) .1337(7) .064(3) Uani d . 1 . . C H22A .0426 .3167 .071 .096 Uiso calc R 1 . . H H22B .1002 .3722 .1418 .096 Uiso calc R 1 . . H H22C .031 .3091 .1777 .096 Uiso calc R 1 . . H C5 .5805(7) .2154(3) -.0200(5) .0294(17) Uani d . 1 . . C C6 .6973(7) .1847(3) .0374(5) .0293(16) Uani d . 1 . . C C16 .1114(9) .0466(4) -.0711(5) .055(2) Uani d . 1 . . C H16A .0233 .0651 -.0548 .083 Uiso calc R 1 . . H H16B .0945 .0017 -.0882 .083 Uiso calc R 1 . . H H16C .1393 .07 -.1231 .083 Uiso calc R 1 . . H C10 .9460(8) .1583(4) .0711(5) .045(2) Uani d . 1 . . C H10 1.042 .1619 .0596 .054 Uiso calc R 1 . . H C9 .7499(10) .2522(4) -.1190(6) .059(3) Uani d . 1 . . C H9 .7683 .2753 -.1714 .071 Uiso calc R 1 . . H C8 .8592(10) .2241(4) -.0649(6) .056(2) Uani d . 1 . . C H8 .9534 .2274 -.0797 .067 Uiso calc R 1 . . H C7 .8365(7) .1895(4) .0139(5) .0364(18) Uani d . 1 . . C C21 .6206(10) .3590(4) .1927(7) .078(3) Uani d . 1 . . C H21A .6881 .3515 .2493 .117 Uiso calc R 1 . . H H21B .583 .4026 .1931 .117 Uiso calc R 1 . . H H21C .6701 .3534 .1395 .117 Uiso calc R 1 . . H C19 .3540(9) .3339(4) .1634(6) .051(2) Uani d . 1 . . C H19 .34 .3786 .1564 .061 Uiso calc R 1 . . H C14 .3025(9) -.0034(4) .0452(6) .047(2) Uani d . 1 . . C H14 .2682 -.0432 .0198 .056 Uiso calc R 1 . . H C20 .4963(9) .3114(4) .1869(5) .046(2) Uani d . 1 . . C O5 .2609(5) .1120(2) .2587(3) .0405(13) Uani d . 1 . . O O6 .5553(5) .1351(2) .3041(3) .0390(12) Uani d . 1 . . O N2 .6685(5) .1508(3) .1116(3) .0271(12) Uani d . 1 . . N C25 .2860(9) .0777(4) .3312(6) .052(2) Uani d . 1 . . C C23 .5438(9) .0959(4) .3682(6) .048(2) Uani d . 1 . . C C24 .4162(9) .0687(4) .3837(6) .065(3) Uani d . 1 . . C H24 .4199 .0414 .4356 .078 Uiso calc R 1 . . H C3 .4862(11) .2729(4) -.1559(5) .055(2) Uani d . 1 . . C H3 .4992 .2951 -.2103 .066 Uiso calc R 1 . . H C27 .6803(9) .0784(5) .4296(6) .070(3) Uani d . 1 . . C H27A .7415 .0536 .3947 .105 Uiso calc R 1 . . H H27B .6578 .0529 .4813 .105 Uiso calc R 1 . . H H27C .7307 .1174 .453 .105 Uiso calc R 1 . . H C26 .1510(10) .0466(6) .3589(8) .098(4) Uani d . 1 . . C H26A .0917 .0794 .382 .147 Uiso calc R 1 . . H H26B .1795 .0148 .4071 .147 Uiso calc R 1 . . H H26C .0958 .0257 .3052 .147 Uiso calc R 1 . . 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 Sm1 .0261(2) .02621(19) .0293(2) -.0001(2) .00346(14) -.00154(18) O1 .032(3) .034(3) .042(3) -.003(2) .004(2) -.007(2) O2 .033(3) .031(3) .049(3) .002(2) .002(2) -.002(2) O3 .048(3) .029(3) .044(3) -.003(2) -.003(2) -.004(2) C12 .033(5) .039(4) .034(4) .009(4) -.001(4) -.008(3) O4 .038(3) .031(3) .042(3) .005(2) .005(2) -.004(2) C4 .059(5) .033(4) .032(5) .002(4) .012(4) .001(3) C1 .036(5) .040(5) .042(5) .003(4) -.002(4) -.005(4) C13 .047(5) .032(4) .041(5) -.007(4) .016(4) -.006(4) C11 .031(4) .023(4) .066(6) .008(4) -.007(4) -.019(4) C15 .029(4) .043(5) .038(4) -.012(4) .011(3) -.007(4) N1 .030(4) .029(3) .028(3) .003(3) .001(3) .002(3) C2 .057(6) .048(5) .030(5) .013(4) -.008(4) .011(4) C17 .078(7) .028(5) .076(7) .005(4) .012(5) -.005(4) C18 .050(5) .041(5) .034(5) .014(4) .005(4) .002(4) C22 .065(6) .046(6) .084(7) .027(4) .021(5) .001(5) C5 .034(4) .024(4) .029(4) .000(3) .005(3) -.008(3) C6 .029(4) .026(4) .031(4) .000(3) .001(3) -.006(3) C16 .054(5) .055(5) .051(5) -.005(5) -.009(4) -.013(4) C10 .030(4) .046(5) .059(5) -.003(4) .011(4) -.022(5) C9 .074(7) .059(6) .054(6) -.010(5) .036(5) .004(5) C8 .048(6) .059(6) .066(6) -.008(5) .029(5) -.002(5) C7 .027(4) .042(4) .042(5) -.006(3) .012(4) -.013(4) C21 .069(7) .042(6) .113(9) -.024(5) -.014(6) -.006(5) C19 .063(6) .030(5) .056(5) .004(4) -.001(4) -.001(4) C14 .052(5) .027(4) .058(6) -.006(4) -.003(4) -.012(4) C20 .061(6) .039(5) .035(5) -.011(4) .000(4) -.009(4) O5 .037(3) .041(3) .044(3) .002(2) .008(2) .009(3) O6 .045(3) .041(3) .028(3) -.010(2) -.002(2) .006(2) N2 .014(3) .027(3) .037(3) .007(3) -.006(2) -.001(3) C25 .044(5) .053(5) .061(6) -.006(4) .011(4) .023(5) C23 .047(5) .051(5) .043(5) -.002(4) -.001(4) .005(4) C24 .054(6) .073(7) .066(6) -.007(5) .004(5) .041(5) C3 .084(7) .049(5) .030(5) .010(5) .004(5) .014(4) C27 .055(6) .090(8) .058(6) -.015(5) -.012(5) .037(5) C26 .057(6) .117(10) .121(10) .000(6) .015(6) .090(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -.1638 3.4418 '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 Sm1 O6 143.70(16) no O1 Sm1 O4 83.05(16) no O6 Sm1 O4 118.26(16) no O1 Sm1 O2 72.40(16) yes O6 Sm1 O2 76.16(16) no O4 Sm1 O2 149.06(16) no O1 Sm1 O3 140.45(16) no O6 Sm1 O3 75.84(16) no O4 Sm1 O3 71.83(17) yes O2 Sm1 O3 138.85(17) no O1 Sm1 O5 84.90(17) no O6 Sm1 O5 72.33(17) yes O4 Sm1 O5 78.80(16) no O2 Sm1 O5 80.49(16) no O3 Sm1 O5 118.13(17) no O1 Sm1 N2 107.26(16) no O6 Sm1 N2 80.50(16) no O4 Sm1 N2 132.74(17) no O2 Sm1 N2 74.04(16) no O3 Sm1 N2 72.09(17) no O5 Sm1 N2 146.42(17) no O1 Sm1 N1 71.34(16) no O6 Sm1 N1 137.93(16) no O4 Sm1 N1 78.79(16) no O2 Sm1 N1 109.60(16) no O3 Sm1 N1 74.11(17) no O5 Sm1 N1 148.99(17) no N2 Sm1 N1 62.65(16) yes C15 O1 Sm1 136.4(5) no C13 O2 Sm1 135.3(5) no C20 O3 Sm1 134.5(5) no N2 C12 C11 124.8(7) no C18 O4 Sm1 136.4(5) no C3 C4 C5 117.0(7) no C3 C4 C9 124.4(8) no C5 C4 C9 118.5(7) no N1 C1 C2 124.7(7) no O2 C13 C14 124.7(7) no O2 C13 C17 115.5(7) no C14 C13 C17 119.7(7) no C10 C11 C12 117.7(7) no O1 C15 C14 124.8(7) no O1 C15 C16 114.8(7) no C14 C15 C16 120.4(7) no C1 N1 C5 117.1(6) no C1 N1 Sm1 123.4(5) no C5 N1 Sm1 119.4(4) no C3 C2 C1 117.2(7) no O4 C18 C19 124.8(7) no O4 C18 C22 116.7(7) no C19 C18 C22 118.5(7) no N1 C5 C4 122.1(7) no N1 C5 C6 118.0(6) no C4 C5 C6 119.9(6) no N2 C6 C7 122.8(6) no N2 C6 C5 118.4(6) no C7 C6 C5 118.9(6) no C11 C10 C7 120.9(7) no C8 C9 C4 121.6(8) no C9 C8 C7 121.0(8) no C10 C7 C8 123.2(7) no C10 C7 C6 116.7(7) no C8 C7 C6 120.2(7) no C18 C19 C20 124.4(7) no C13 C14 C15 125.5(7) no O3 C20 C19 125.0(7) no O3 C20 C21 115.9(7) no C19 C20 C21 119.1(7) no C25 O5 Sm1 131.7(5) no C23 O6 Sm1 133.0(5) no C12 N2 C6 117.2(6) no C12 N2 Sm1 121.9(4) no C6 N2 Sm1 120.7(4) no O5 C25 C24 126.0(7) no O5 C25 C26 113.9(7) no C24 C25 C26 120.1(7) no O6 C23 C24 124.6(8) no O6 C23 C27 116.3(7) no C24 C23 C27 119.1(7) no C25 C24 C23 125.5(8) no C2 C3 C4 121.8(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm1 O1 . . 2.341(5) yes Sm1 O6 . . 2.351(5) yes Sm1 O4 . . 2.372(5) yes Sm1 O2 . . 2.378(5) yes Sm1 O3 . . 2.383(5) yes Sm1 O5 . . 2.388(5) yes Sm1 N2 . . 2.589(5) yes Sm1 N1 . . 2.641(5) yes O1 C15 . . 1.278(8) no O2 C13 . . 1.276(8) no O3 C20 . . 1.257(9) no C12 N2 . . 1.310(8) no C12 C11 . . 1.391(10) no O4 C18 . . 1.270(9) no C4 C3 . . 1.389(11) no C4 C5 . . 1.411(10) no C4 C9 . . 1.438(11) no C1 N1 . . 1.331(9) no C1 C2 . . 1.391(10) no C13 C14 . . 1.369(11) no C13 C17 . . 1.507(10) no C11 C10 . . 1.369(11) no C15 C14 . . 1.386(10) no C15 C16 . . 1.512(10) no N1 C5 . . 1.357(8) no C2 C3 . . 1.345(11) no C18 C19 . . 1.379(11) no C18 C22 . . 1.495(10) no C5 C6 . . 1.432(9) no C6 N2 . . 1.366(8) no C6 C7 . . 1.412(9) no C10 C7 . . 1.392(11) no C9 C8 . . 1.338(12) no C8 C7 . . 1.411(11) no C21 C20 . . 1.531(11) no C19 C20 . . 1.414(11) no O5 C25 . . 1.280(9) no O6 C23 . . 1.269(9) no C25 C24 . . 1.359(11) no C25 C26 . . 1.541(11) no C23 C24 . . 1.382(11) no C23 C27 . . 1.500(11) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139065068