# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Ion Bulimestru' 'Olivier Mentre' 'Nathalie Tancret' 'Aurelie Rolle' 'Nora Djela' 'Laurence Burylo' 'Nicoleta Cornei' 'Nelea Popa' 'Aurelian Gulea' _publ_contact_author_name ' Olivier Mentre' _publ_contact_author_email olivier.mentre@ensc-lille.fr _publ_section_title ; Heterobimetallic Ba-Co aminopolycarboxylate complexes as precursors for BaCoO3-\^I' oxides ; towards a one-stage-deposition of cobaltites films ; # Attachment '- BaCo(cdta)-5H2O.CIF' ################################################## # Heterobimetallic Ba-Co aminopolycarboxylate complexes as precursors # for BaCoO3-? oxides ; towards a one-stage-deposition of cobaltites films # # Ion Bulimestru1, Olivier Mentr\'e2,*, Nathalie Tancret2, Aur\'elie Rolle2, # Nora Djelal2, Laurence Burylo2, Nicoleta Cornei3, Nelea Popa1, Aurelian Gulea1 # # # 1 Moldova State University, Coordination Chemistry Laboratory, # 60 Mateevici str., Chisinau MD 2009, Moldova. # # 2 Universit\'e Lille Nord de France. Unit\'e de Catalyse et de Chimie # du Solide, # CNRS UMR 8181, ENSC Lille # - UST Lille, BP 90108, 59652 Villeneuve d?Ascq cedex, France. # # 3 Facult\'e de Chimie, D\'epartement de Chimie Inorganique, #Universit\'e "Al. I. Cuza", # Boulevard Carol I nr. 11, 6600 Iasi, Romania. # # subm. J Mater Chem 2010 ################################################### data_lo3_0m _database_code_depnum_ccdc_archive 'CCDC 772915' #TrackingRef '- BaCo(cdta)-5H2O.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BaCo(cdta)-5H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum C14H28Ba1Co1N2O13 _chemical_formula_weight 628.58 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.8694(2) _cell_length_b 15.0670(3) _cell_length_c 22.1339(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.4690(10) _cell_angle_gamma 90.00 _cell_volume 4290.42(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.2925 _cell_measurement_theta_max 34.469 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 2.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8755 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G\"ottingen Germany (2006).' ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44606 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 34.49 _reflns_number_total 8635 _reflns_number_gt 7585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker X8' _computing_cell_refinement 'Bruker X8/SAINT' _computing_data_reduction 'Bruker X8/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+4.6029P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00008(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8635 _refine_ls_number_parameters 325 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.0000 0.205826(9) 0.2500 0.01837(4) Uani 1 2 d S . . Ba2 Ba 0.0000 0.513491(10) 0.2500 0.02398(4) Uani 1 2 d S . . Co3 Co 0.216722(17) 0.063684(15) 0.329241(10) 0.01728(5) Uani 1 1 d . . . N1 N 0.23385(11) 0.09951(10) 0.42679(7) 0.0202(3) Uani 1 1 d . . . N2 N 0.17985(11) -0.06708(10) 0.37357(7) 0.0205(3) Uani 1 1 d . . . O1 O 0.16854(11) 0.20391(9) 0.33741(6) 0.0242(3) Uani 1 1 d . . . O2 O -0.12188(10) 0.59540(10) 0.33877(6) 0.0262(3) Uani 1 1 d . . . O3 O 0.05118(10) 0.05496(8) 0.32220(6) 0.0226(2) Uani 1 1 d . . . O4 O -0.21026(11) 0.46529(9) 0.27562(6) 0.0251(3) Uani 1 1 d . . . O5 O -0.08324(11) -0.03780(10) 0.31679(8) 0.0313(3) Uani 1 1 d . . . O6 O -0.11590(13) 0.34298(11) 0.28202(8) 0.0367(4) Uani 1 1 d . . . O7 O -0.00067(13) 0.66061(16) 0.39740(8) 0.0482(5) Uani 1 1 d . . . O8 O 0.0483(2) 0.27125(16) 0.39024(11) 0.0690(8) Uani 1 1 d . . . C1 C 0.16311(14) -0.05227(13) 0.43930(8) 0.0244(3) Uani 1 1 d . . . H1 H 0.0933 -0.0271 0.4430 0.029 Uiso 1 1 calc R . . C2 C 0.1670(2) -0.13779(16) 0.47758(12) 0.0388(5) Uani 1 1 d . . . H2A H 0.1125 -0.1778 0.4635 0.047 Uiso 1 1 calc R . . H2B H 0.2332 -0.1671 0.4723 0.047 Uiso 1 1 calc R . . C3 C 0.1530(2) -0.1182(2) 0.54456(12) 0.0473(6) Uani 1 1 d . . . H3A H 0.0842 -0.0939 0.5504 0.057 Uiso 1 1 calc R . . H3B H 0.1589 -0.1729 0.5675 0.057 Uiso 1 1 calc R . . C4 C 0.2340(2) -0.0528(2) 0.56763(10) 0.0431(6) Uani 1 1 d . . . H4A H 0.3028 -0.0779 0.5635 0.052 Uiso 1 1 calc R . . H4B H 0.2237 -0.0410 0.6101 0.052 Uiso 1 1 calc R . . C5 C 0.22550(19) 0.03312(17) 0.53203(9) 0.0353(5) Uani 1 1 d . . . H5A H 0.2780 0.0745 0.5469 0.042 Uiso 1 1 calc R . . H5B H 0.1579 0.0596 0.5381 0.042 Uiso 1 1 calc R . . C6 C 0.24006(14) 0.01690(13) 0.46381(8) 0.0232(3) Uani 1 1 d . . . H6 H 0.3100 -0.0076 0.4593 0.028 Uiso 1 1 calc R . . C7 C 0.14202(15) 0.15471(13) 0.43818(9) 0.0246(3) Uani 1 1 d . . . H7A H 0.1544 0.1897 0.4745 0.030 Uiso 1 1 calc R . . H7B H 0.0825 0.1168 0.4447 0.030 Uiso 1 1 calc R . . C8 C 0.11864(16) 0.21600(13) 0.38535(9) 0.0282(4) Uani 1 1 d . . . C9 C 0.32908(15) 0.15363(14) 0.43373(9) 0.0259(4) Uani 1 1 d . . . H9A H 0.3601 0.1429 0.4735 0.031 Uiso 1 1 calc R . . H9B H 0.3103 0.2159 0.4315 0.031 Uiso 1 1 calc R . . C10 C -0.09116(15) 0.63428(13) 0.38648(9) 0.0259(4) Uani 1 1 d . . . C11 C 0.08293(14) -0.09794(12) 0.34255(9) 0.0240(3) Uani 1 1 d . . . H11A H 0.0474 -0.1392 0.3686 0.029 Uiso 1 1 calc R . . H11B H 0.1004 -0.1293 0.3059 0.029 Uiso 1 1 calc R . . C12 C 0.01041(13) -0.02135(11) 0.32658(8) 0.0201(3) Uani 1 1 d . . . C13 C -0.23356(15) 0.37163(12) 0.36095(10) 0.0256(3) Uani 1 1 d . . . H13A H -0.2594 0.3112 0.3598 0.031 Uiso 1 1 calc R . . H13B H -0.1814 0.3757 0.3932 0.031 Uiso 1 1 calc R . . C14 C -0.18439(13) 0.39333(12) 0.30133(9) 0.0234(3) Uani 1 1 d . . . OW1 O 0.14917(18) 0.20856(12) 0.71173(11) 0.0504(5) Uani 1 1 d D . . HW1A H 0.130(3) 0.1594(13) 0.6968(15) 0.050 Uiso 1 1 d D . . HW1B H 0.2054(15) 0.231(2) 0.6998(14) 0.050 Uiso 1 1 d D . . OW2 O 0.11605(13) 0.65843(11) 0.29654(8) 0.0348(3) Uani 1 1 d D . . HW2A H 0.110(3) 0.7056(13) 0.2757(13) 0.050 Uiso 1 1 d D . . HW2B H 0.082(2) 0.675(2) 0.3271(10) 0.050 Uiso 1 1 d D . . OW3 O -0.18436(11) 0.10810(10) 0.26956(7) 0.0255(3) Uani 1 1 d D . . HW3A H -0.2409(15) 0.120(2) 0.2866(14) 0.050 Uiso 1 1 d D . . HW3B H -0.163(2) 0.0611(13) 0.2869(13) 0.050 Uiso 1 1 d D . . OW4 O 0.0568(3) 0.44844(18) 0.36082(14) 0.0871(10) Uani 1 1 d D . . HW4A H 0.1127(18) 0.434(2) 0.3409(15) 0.050 Uiso 1 1 d D . . HW4B H 0.078(3) 0.4946(14) 0.3798(14) 0.050 Uiso 1 1 d D . . OW51 O -0.0648(5) 0.3444(4) 0.4824(3) 0.0618(9) Uiso 0.50 1 d PD . . OW52 O -0.0459(5) 0.3762(4) 0.4774(3) 0.0618(9) Uiso 0.50 1 d PD . . H51A H -0.021(3) 0.318(3) 0.459(2) 0.050 Uiso 0.50 1 d PD . . H51B H -0.118(3) 0.310(3) 0.485(3) 0.050 Uiso 0.50 1 d PD . . H52A H 0.0000 0.4221(10) 0.481(3) 0.050 Uiso 0.50 1 d PD . . H52B H -0.027(5) 0.348(3) 0.5107(18) 0.050 Uiso 0.50 1 d PD . . 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 Ba1 0.01506(6) 0.01432(6) 0.02568(7) 0.000 -0.00071(5) 0.000 Ba2 0.01962(7) 0.02220(7) 0.03039(8) 0.000 0.00577(5) 0.000 Co3 0.01507(9) 0.01690(10) 0.01987(10) -0.00135(8) 0.00038(7) 0.00074(7) N1 0.0166(6) 0.0240(7) 0.0199(6) -0.0017(5) 0.0012(5) 0.0010(5) N2 0.0158(6) 0.0204(6) 0.0252(7) 0.0014(5) 0.0000(5) 0.0024(5) O1 0.0274(6) 0.0212(6) 0.0239(6) -0.0009(5) -0.0009(5) -0.0011(5) O2 0.0196(6) 0.0354(7) 0.0238(6) -0.0071(5) 0.0028(5) -0.0032(5) O3 0.0178(5) 0.0188(5) 0.0309(7) 0.0034(5) -0.0024(5) -0.0013(4) O4 0.0247(6) 0.0210(6) 0.0298(7) -0.0015(5) 0.0043(5) 0.0023(5) O5 0.0176(6) 0.0260(7) 0.0499(9) 0.0048(6) -0.0059(6) -0.0028(5) O6 0.0303(7) 0.0305(7) 0.0496(10) -0.0066(7) 0.0069(7) 0.0120(6) O7 0.0226(7) 0.0882(15) 0.0340(8) -0.0170(9) 0.0028(6) -0.0192(8) O8 0.0789(16) 0.0617(13) 0.0682(14) 0.0275(11) 0.0350(12) 0.0491(12) C1 0.0200(7) 0.0282(8) 0.0250(8) 0.0067(7) 0.0019(6) 0.0019(6) C2 0.0392(12) 0.0366(12) 0.0407(12) 0.0160(9) 0.0030(10) -0.0033(9) C3 0.0420(13) 0.0596(16) 0.0408(13) 0.0250(12) 0.0104(11) -0.0005(12) C4 0.0437(13) 0.0607(16) 0.0252(10) 0.0150(10) 0.0055(9) 0.0109(12) C5 0.0381(11) 0.0480(13) 0.0200(9) 0.0028(8) 0.0020(8) 0.0068(10) C6 0.0197(7) 0.0299(9) 0.0201(8) 0.0035(6) 0.0008(6) 0.0033(6) C7 0.0228(8) 0.0281(8) 0.0231(8) -0.0014(7) 0.0040(6) 0.0061(7) C8 0.0303(9) 0.0239(8) 0.0306(9) 0.0013(7) 0.0046(7) 0.0063(7) C9 0.0212(7) 0.0326(9) 0.0237(8) -0.0070(7) 0.0003(6) -0.0036(7) C10 0.0195(7) 0.0342(10) 0.0241(8) -0.0016(7) 0.0009(6) -0.0034(7) C11 0.0192(7) 0.0179(7) 0.0348(9) 0.0005(7) -0.0025(7) -0.0003(6) C12 0.0181(7) 0.0200(7) 0.0222(8) 0.0003(6) -0.0004(6) -0.0005(5) C13 0.0211(7) 0.0210(8) 0.0346(10) 0.0034(7) -0.0003(7) 0.0061(6) C14 0.0173(7) 0.0200(7) 0.0327(9) -0.0055(7) 0.0001(6) 0.0008(6) OW1 0.0507(11) 0.0295(9) 0.0717(14) -0.0074(9) 0.0170(10) -0.0122(8) OW2 0.0313(8) 0.0326(8) 0.0408(9) -0.0023(7) 0.0103(7) 0.0001(6) OW3 0.0215(6) 0.0250(6) 0.0301(7) 0.0058(5) 0.0040(5) -0.0003(5) OW4 0.139(3) 0.0499(14) 0.0696(18) -0.0007(13) -0.0470(18) 0.0043(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O6 2.6555(15) 2 ? Ba1 O6 2.6555(15) . ? Ba1 OW3 2.8351(14) . ? Ba1 OW3 2.8351(14) 2 ? Ba1 O3 2.8461(13) 2 ? Ba1 O3 2.8461(13) . ? Ba1 O1 2.8694(13) . ? Ba1 O1 2.8694(13) 2 ? Ba1 O8 3.301(3) . ? Ba1 O8 3.301(3) 2 ? Ba1 C8 3.331(2) . ? Ba1 C8 3.331(2) 2 ? Ba2 OW4 2.724(3) 2 ? Ba2 OW4 2.724(3) . ? Ba2 OW2 2.8252(17) . ? Ba2 OW2 2.8252(17) 2 ? Ba2 O2 2.8287(13) . ? Ba2 O2 2.8287(13) 2 ? Ba2 O4 2.8723(14) . ? Ba2 O4 2.8723(14) 2 ? Ba2 O6 3.0629(18) . ? Ba2 O6 3.0629(18) 2 ? Ba2 C14 3.2153(19) . ? Ba2 C14 3.2153(19) 2 ? Ba2 HW4A 2.73(4) . ? Co3 O4 2.1323(14) 3_545 ? Co3 O3 2.1362(13) . ? Co3 O2 2.1365(13) 3_545 ? Co3 O1 2.2106(13) . ? Co3 N1 2.2310(15) . ? Co3 N2 2.2569(15) . ? Co3 OW3 2.3145(15) 2 ? N1 C7 1.472(2) . ? N1 C9 1.477(2) . ? N1 C6 1.491(2) . ? N2 C13 1.479(2) 3_545 ? N2 C11 1.483(2) . ? N2 C1 1.493(2) . ? O1 C8 1.267(2) . ? O2 C10 1.262(2) . ? O2 Co3 2.1365(13) 3_455 ? O3 C12 1.269(2) . ? O4 C14 1.265(2) . ? O4 Co3 2.1323(14) 3_455 ? O5 C12 1.244(2) . ? O6 C14 1.247(2) . ? O7 C10 1.248(2) . ? O8 C8 1.237(3) . ? C1 C6 1.528(3) . ? C1 C2 1.542(3) . ? C1 H1 0.9800 . ? C2 C3 1.527(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.513(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.518(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.546(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6 0.9800 . ? C7 C8 1.514(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.512(3) 3_545 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C9 1.512(3) 3_455 ? C11 C12 1.520(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 N2 1.479(2) 3_455 ? C13 C14 1.514(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? OW1 HW1A 0.844(10) . ? OW1 HW1B 0.845(10) . ? OW2 HW2A 0.850(10) . ? OW2 HW2B 0.854(10) . ? OW3 Co3 2.3145(15) 2 ? OW3 HW3A 0.848(10) . ? OW3 HW3B 0.847(10) . ? OW4 HW4A 0.881(10) . ? OW4 HW4B 0.855(10) . ? OW51 OW52 0.551(7) . ? OW51 H51A 0.865(10) . ? OW51 H51B 0.861(10) . ? OW51 H52B 0.78(3) . ? OW52 H51A 1.02(3) . ? OW52 H51B 1.376(17) . ? OW52 H52A 0.911(10) . ? OW52 H52B 0.878(10) . ? 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 _geom_angle_publ_flag O6 Ba1 O6 77.81(8) 2 . ? O6 Ba1 OW3 157.36(5) 2 . ? O6 Ba1 OW3 83.42(5) . . ? O6 Ba1 OW3 83.42(5) 2 2 ? O6 Ba1 OW3 157.36(5) . 2 ? OW3 Ba1 OW3 117.42(6) . 2 ? O6 Ba1 O3 126.52(5) 2 2 ? O6 Ba1 O3 130.38(5) . 2 ? OW3 Ba1 O3 59.23(4) . 2 ? OW3 Ba1 O3 71.46(4) 2 2 ? O6 Ba1 O3 130.38(5) 2 . ? O6 Ba1 O3 126.52(5) . . ? OW3 Ba1 O3 71.46(4) . . ? OW3 Ba1 O3 59.23(4) 2 . ? O3 Ba1 O3 74.00(5) 2 . ? O6 Ba1 O1 76.57(5) 2 . ? O6 Ba1 O1 104.36(5) . . ? OW3 Ba1 O1 120.86(4) . . ? OW3 Ba1 O1 58.44(4) 2 . ? O3 Ba1 O1 122.05(4) 2 . ? O3 Ba1 O1 56.86(4) . . ? O6 Ba1 O1 104.36(5) 2 2 ? O6 Ba1 O1 76.57(5) . 2 ? OW3 Ba1 O1 58.44(4) . 2 ? OW3 Ba1 O1 120.86(4) 2 2 ? O3 Ba1 O1 56.86(4) 2 2 ? O3 Ba1 O1 122.05(4) . 2 ? O1 Ba1 O1 178.85(5) . 2 ? O6 Ba1 O8 85.71(6) 2 . ? O6 Ba1 O8 67.05(5) . . ? OW3 Ba1 O8 98.60(6) . . ? OW3 Ba1 O8 99.25(5) 2 . ? O3 Ba1 O8 143.31(5) 2 . ? O3 Ba1 O8 71.05(4) . . ? O1 Ba1 O8 41.25(5) . . ? O1 Ba1 O8 139.28(5) 2 . ? O6 Ba1 O8 67.05(5) 2 2 ? O6 Ba1 O8 85.71(6) . 2 ? OW3 Ba1 O8 99.25(5) . 2 ? OW3 Ba1 O8 98.60(6) 2 2 ? O3 Ba1 O8 71.05(4) 2 2 ? O3 Ba1 O8 143.31(5) . 2 ? O1 Ba1 O8 139.28(5) . 2 ? O1 Ba1 O8 41.25(5) 2 2 ? O8 Ba1 O8 145.24(8) . 2 ? O6 Ba1 C8 87.51(5) 2 . ? O6 Ba1 C8 88.39(5) . . ? OW3 Ba1 C8 104.64(5) . . ? OW3 Ba1 C8 78.18(4) 2 . ? O3 Ba1 C8 129.49(4) 2 . ? O3 Ba1 C8 55.78(4) . . ? O1 Ba1 C8 22.01(4) . . ? O1 Ba1 C8 158.13(5) 2 . ? O8 Ba1 C8 21.50(5) . . ? O8 Ba1 C8 154.55(5) 2 . ? O6 Ba1 C8 88.39(5) 2 2 ? O6 Ba1 C8 87.51(5) . 2 ? OW3 Ba1 C8 78.18(4) . 2 ? OW3 Ba1 C8 104.64(5) 2 2 ? O3 Ba1 C8 55.78(4) 2 2 ? O3 Ba1 C8 129.49(4) . 2 ? O1 Ba1 C8 158.13(5) . 2 ? O1 Ba1 C8 22.01(4) 2 2 ? O8 Ba1 C8 154.55(5) . 2 ? O8 Ba1 C8 21.50(5) 2 2 ? C8 Ba1 C8 174.73(7) . 2 ? OW4 Ba2 OW4 137.82(12) 2 . ? OW4 Ba2 OW2 137.19(8) 2 . ? OW4 Ba2 OW2 79.79(8) . . ? OW4 Ba2 OW2 79.79(7) 2 2 ? OW4 Ba2 OW2 137.19(8) . 2 ? OW2 Ba2 OW2 78.76(7) . 2 ? OW4 Ba2 O2 129.92(9) 2 . ? OW4 Ba2 O2 70.87(8) . . ? OW2 Ba2 O2 72.95(4) . . ? OW2 Ba2 O2 67.59(5) 2 . ? OW4 Ba2 O2 70.87(8) 2 2 ? OW4 Ba2 O2 129.92(9) . 2 ? OW2 Ba2 O2 67.59(5) . 2 ? OW2 Ba2 O2 72.95(4) 2 2 ? O2 Ba2 O2 128.27(6) . 2 ? OW4 Ba2 O4 81.63(9) 2 . ? OW4 Ba2 O4 87.92(9) . . ? OW2 Ba2 O4 127.98(4) . . ? OW2 Ba2 O4 77.03(4) 2 . ? O2 Ba2 O4 55.33(4) . . ? O2 Ba2 O4 142.13(4) 2 . ? OW4 Ba2 O4 87.92(9) 2 2 ? OW4 Ba2 O4 81.63(9) . 2 ? OW2 Ba2 O4 77.03(4) . 2 ? OW2 Ba2 O4 127.98(4) 2 2 ? O2 Ba2 O4 142.13(4) . 2 ? O2 Ba2 O4 55.33(4) 2 2 ? O4 Ba2 O4 150.71(5) . 2 ? OW4 Ba2 O6 77.61(8) 2 . ? OW4 Ba2 O6 67.10(8) . . ? OW2 Ba2 O6 145.09(5) . . ? OW2 Ba2 O6 118.47(5) 2 . ? O2 Ba2 O6 85.60(4) . . ? O2 Ba2 O6 143.96(5) 2 . ? O4 Ba2 O6 43.57(4) . . ? O4 Ba2 O6 107.48(4) 2 . ? OW4 Ba2 O6 67.10(8) 2 2 ? OW4 Ba2 O6 77.61(8) . 2 ? OW2 Ba2 O6 118.47(5) . 2 ? OW2 Ba2 O6 145.09(5) 2 2 ? O2 Ba2 O6 143.96(5) . 2 ? O2 Ba2 O6 85.60(4) 2 2 ? O4 Ba2 O6 107.48(4) . 2 ? O4 Ba2 O6 43.57(4) 2 2 ? O6 Ba2 O6 65.98(6) . 2 ? OW4 Ba2 C14 86.11(9) 2 . ? OW4 Ba2 C14 70.28(9) . . ? OW2 Ba2 C14 133.98(5) . . ? OW2 Ba2 C14 100.14(5) 2 . ? O2 Ba2 C14 64.71(4) . . ? O2 Ba2 C14 156.71(5) 2 . ? O4 Ba2 C14 23.12(4) . . ? O4 Ba2 C14 129.42(4) 2 . ? O6 Ba2 C14 22.74(4) . . ? O6 Ba2 C14 88.72(4) 2 . ? OW4 Ba2 C14 70.28(9) 2 2 ? OW4 Ba2 C14 86.11(9) . 2 ? OW2 Ba2 C14 100.14(5) . 2 ? OW2 Ba2 C14 133.98(5) 2 2 ? O2 Ba2 C14 156.71(5) . 2 ? O2 Ba2 C14 64.71(4) 2 2 ? O4 Ba2 C14 129.42(4) . 2 ? O4 Ba2 C14 23.12(4) 2 2 ? O6 Ba2 C14 88.72(4) . 2 ? O6 Ba2 C14 22.74(4) 2 2 ? C14 Ba2 C14 111.46(6) . 2 ? OW4 Ba2 HW4A 129.2(6) 2 . ? OW4 Ba2 HW4A 18.6(2) . . ? OW2 Ba2 HW4A 78.7(8) . . ? OW2 Ba2 HW4A 151.0(6) 2 . ? O2 Ba2 HW4A 88.5(4) . . ? O2 Ba2 HW4A 114.2(4) 2 . ? O4 Ba2 HW4A 103.3(5) . . ? O4 Ba2 HW4A 63.2(3) 2 . ? O6 Ba2 HW4A 73.4(7) . . ? O6 Ba2 HW4A 63.2(6) 2 . ? C14 Ba2 HW4A 82.8(6) . . ? C14 Ba2 HW4A 68.3(3) 2 . ? O4 Co3 O3 111.69(5) 3_545 . ? O4 Co3 O2 76.66(5) 3_545 3_545 ? O3 Co3 O2 170.47(5) . 3_545 ? O4 Co3 O1 146.99(5) 3_545 . ? O3 Co3 O1 77.49(5) . . ? O2 Co3 O1 92.99(6) 3_545 . ? O4 Co3 N1 132.29(5) 3_545 . ? O3 Co3 N1 99.16(5) . . ? O2 Co3 N1 77.21(5) 3_545 . ? O1 Co3 N1 73.18(5) . . ? O4 Co3 N2 74.67(5) 3_545 . ? O3 Co3 N2 75.97(5) . . ? O2 Co3 N2 111.53(6) 3_545 . ? O1 Co3 N2 137.42(5) . . ? N1 Co3 N2 78.88(6) . . ? O4 Co3 OW3 75.30(5) 3_545 2 ? O3 Co3 OW3 78.11(5) . 2 ? O2 Co3 OW3 100.34(5) 3_545 2 ? O1 Co3 OW3 75.93(5) . 2 ? N1 Co3 OW3 148.80(5) . 2 ? N2 Co3 OW3 128.93(5) . 2 ? O4 Co3 Ba1 116.87(4) 3_545 . ? O3 Co3 Ba1 45.58(3) . . ? O2 Co3 Ba1 127.17(4) 3_545 . ? O1 Co3 Ba1 46.58(3) . . ? N1 Co3 Ba1 110.76(4) . . ? N2 Co3 Ba1 121.29(4) . . ? OW3 Co3 Ba1 46.10(3) 2 . ? C7 N1 C9 109.75(15) . . ? C7 N1 C6 114.17(14) . . ? C9 N1 C6 111.78(14) . . ? C7 N1 Co3 104.04(10) . . ? C9 N1 Co3 107.18(11) . . ? C6 N1 Co3 109.42(11) . . ? C13 N2 C11 110.22(14) 3_545 . ? C13 N2 C1 113.92(14) 3_545 . ? C11 N2 C1 110.93(14) . . ? C13 N2 Co3 107.17(11) 3_545 . ? C11 N2 Co3 104.84(10) . . ? C1 N2 Co3 109.29(11) . . ? C8 O1 Co3 110.79(12) . . ? C8 O1 Ba1 99.94(12) . . ? Co3 O1 Ba1 99.40(5) . . ? C10 O2 Co3 117.99(12) . 3_455 ? C10 O2 Ba2 128.04(12) . . ? Co3 O2 Ba2 112.88(5) 3_455 . ? C12 O3 Co3 117.63(11) . . ? C12 O3 Ba1 132.58(11) . . ? Co3 O3 Ba1 102.00(5) . . ? C14 O4 Co3 117.40(12) . 3_455 ? C14 O4 Ba2 93.85(11) . . ? Co3 O4 Ba2 111.40(5) 3_455 . ? C14 O6 Ba1 166.38(15) . . ? C14 O6 Ba2 85.51(12) . . ? Ba1 O6 Ba2 108.11(6) . . ? C8 O8 Ba1 80.63(16) . . ? N2 C1 C6 109.85(14) . . ? N2 C1 C2 114.01(17) . . ? C6 C1 C2 111.32(17) . . ? N2 C1 H1 107.1 . . ? C6 C1 H1 107.1 . . ? C2 C1 H1 107.1 . . ? C3 C2 C1 111.6(2) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 110.9(2) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 C5 109.9(2) . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 C6 111.3(2) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N1 C6 C1 110.44(14) . . ? N1 C6 C5 113.50(16) . . ? C1 C6 C5 111.16(17) . . ? N1 C6 H6 107.1 . . ? C1 C6 H6 107.1 . . ? C5 C6 H6 107.1 . . ? N1 C7 C8 110.90(15) . . ? N1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? O8 C8 O1 123.9(2) . . ? O8 C8 C7 118.31(19) . . ? O1 C8 C7 117.65(17) . . ? O8 C8 Ba1 77.87(16) . . ? O1 C8 Ba1 58.05(10) . . ? C7 C8 Ba1 138.07(13) . . ? N1 C9 C10 113.44(15) . 3_545 ? N1 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 3_545 . ? N1 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 3_545 . ? H9A C9 H9B 107.7 . . ? O7 C10 O2 125.47(19) . . ? O7 C10 C9 116.82(18) . 3_455 ? O2 C10 C9 117.67(16) . 3_455 ? N2 C11 C12 111.95(14) . . ? N2 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N2 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? O5 C12 O3 124.61(16) . . ? O5 C12 C11 118.40(16) . . ? O3 C12 C11 116.95(15) . . ? N2 C13 C14 111.31(15) 3_455 . ? N2 C13 H13A 109.4 3_455 . ? C14 C13 H13A 109.4 . . ? N2 C13 H13B 109.4 3_455 . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? O6 C14 O4 123.19(19) . . ? O6 C14 C13 118.85(18) . . ? O4 C14 C13 117.78(16) . . ? O6 C14 Ba2 71.75(12) . . ? O4 C14 Ba2 63.04(10) . . ? C13 C14 Ba2 139.32(12) . . ? HW1A OW1 HW1B 118(3) . . ? Ba2 OW2 HW2A 114(2) . . ? Ba2 OW2 HW2B 103(2) . . ? HW2A OW2 HW2B 98(3) . . ? Co3 OW3 Ba1 97.87(5) 2 . ? Co3 OW3 HW3A 110(2) 2 . ? Ba1 OW3 HW3A 134(2) . . ? Co3 OW3 HW3B 103(2) 2 . ? Ba1 OW3 HW3B 104(2) . . ? HW3A OW3 HW3B 104(3) . . ? Ba2 OW4 HW4A 81(2) . . ? Ba2 OW4 HW4B 103(2) . . ? HW4A OW4 HW4B 101(4) . . ? OW52 OW51 H51A 90(4) . . ? OW52 OW51 H51B 154(4) . . ? H51A OW51 H51B 107(2) . . ? OW52 OW51 H52B 80(3) . . ? H51A OW51 H52B 96(6) . . ? H51B OW51 H52B 117(5) . . ? OW51 OW52 H51A 58(3) . . ? OW51 OW52 H51B 16(3) . . ? H51A OW52 H51B 68.7(17) . . ? OW51 OW52 H52A 159(3) . . ? H51A OW52 H52A 119(3) . . ? H51B OW52 H52A 168(4) . . ? OW51 OW52 H52B 61(3) . . ? H51A OW52 H52B 80(5) . . ? H51B OW52 H52B 73(4) . . ? H52A OW52 H52B 98(2) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 34.49 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 2.326 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.110 # Attachment '- BaCo(nta)CH3COO-2H2O .CIF' ################################################## # Heterobimetallic Ba-Co aminopolycarboxylate complexes as precursors # for BaCoO3-? oxides ; towards a one-stage-deposition of cobaltites films # # Ion Bulimestru1, Olivier Mentr\'e2,*, Nathalie Tancret2, Aur\'elie Rolle2, # Nora Djelal2, Laurence Burylo2, Nicoleta Cornei3, Nelea Popa1, Aurelian Gulea1 # # # 1 Moldova State University, Coordination Chemistry Laboratory, # 60 Mateevici str., Chisinau MD 2009, Moldova. # # 2 Universit\'e Lille Nord de France. Unit\'e de Catalyse et de Chimie # du Solide, # CNRS UMR 8181, ENSC Lille # - UST Lille, BP 90108, 59652 Villeneuve d?Ascq cedex, France. # # 3 Facult\'e de Chimie, D\'epartement de Chimie Inorganique, #Universit\'e "Al. I. Cuza", # Boulevard Carol I nr. 11, 6600 Iasi, Romania. # # subm. J .Mater .Chem .2010 ################################################### data_ionlo15 _database_code_depnum_ccdc_archive 'CCDC 772916' #TrackingRef '- BaCo(nta)CH3COO-2H2O .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BaCo(nta)CH3COO-2H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H13 Ba Co N O10' _chemical_formula_weight 479.46 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5979(3) _cell_length_b 9.6686(3) _cell_length_c 9.7505(3) _cell_angle_alpha 64.9820(10) _cell_angle_beta 60.7790(10) _cell_angle_gamma 64.6230(10) _cell_volume 686.79(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9562 _cell_measurement_theta_min 2.422 _cell_measurement_theta_max 38.667 _exptl_crystal_description parallepipedic _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 4.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6010 _exptl_absorpt_correction_T_max 0.7755 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G\"ottingen Germany (2006).' ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75961 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 39.71 _reflns_number_total 7818 _reflns_number_gt 7211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker X8' _computing_cell_refinement 'Bruker X8/SAINT' _computing_data_reduction 'Bruker X8/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.2645P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0278(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7818 _refine_ls_number_parameters 207 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.750370(7) 0.656866(7) 0.506864(8) 0.01974(3) Uani 1 1 d . . . Co2 Co 0.309453(18) 0.587420(18) 0.770467(18) 0.01763(3) Uani 1 1 d . . . N1 N 0.07530(12) 0.78499(12) 0.80628(12) 0.02058(15) Uani 1 1 d . . . C1 C -0.01776(16) 0.7569(2) 0.98390(17) 0.0313(3) Uani 1 1 d . . . H1A H -0.0944 0.6976 1.0183 0.038 Uiso 1 1 calc R . . H1B H -0.0825 0.8582 1.0094 0.038 Uiso 1 1 calc R . . C2 C 0.09743(19) 0.6655(2) 1.07691(16) 0.0309(3) Uani 1 1 d . . . O1 O 0.19496(12) 0.54008(11) 0.67463(14) 0.02706(18) Uani 1 1 d . . . O2 O 1.04534(18) 0.6686(2) 0.21979(14) 0.0473(3) Uani 1 1 d . . . C3 C 0.13412(16) 0.92681(15) 0.73656(18) 0.0286(2) Uani 1 1 d . . . H3A H 0.1509 0.9422 0.8189 0.034 Uiso 1 1 calc R . . H3B H 0.0497 1.0195 0.7051 0.034 Uiso 1 1 calc R . . C4 C 0.29629(13) 0.91214(13) 0.58797(14) 0.01982(16) Uani 1 1 d . . . O3 O 0.39464(10) 0.77244(10) 0.58933(11) 0.02369(15) Uani 1 1 d . . . O4 O 0.32660(13) 1.03432(11) 0.47841(12) 0.02884(18) Uani 1 1 d . . . C5 C -0.01308(17) 0.78524(17) 0.7182(2) 0.0318(3) Uani 1 1 d . . . H5A H -0.0206 0.8840 0.6324 0.038 Uiso 1 1 calc R . . H5B H -0.1255 0.7813 0.7932 0.038 Uiso 1 1 calc R . . C6 C 0.07062(14) 0.64729(14) 0.64318(15) 0.02102(17) Uani 1 1 d . . . O5 O 0.01461(13) 0.64469(13) 0.55329(14) 0.0310(2) Uani 1 1 d . . . O6 O 0.24213(17) 0.58512(17) 1.00215(14) 0.0417(3) Uani 1 1 d . . . C7 C 0.6865(2) 0.16860(19) 0.7874(3) 0.0450(4) Uani 1 1 d . . . H7A H 0.7700 0.1999 0.7853 0.068 Uiso 1 1 calc R . . H7B H 0.7271 0.1373 0.6902 0.068 Uiso 1 1 calc R . . H7C H 0.6612 0.0808 0.8814 0.068 Uiso 1 1 calc R . . C8 C 0.53194(15) 0.30600(14) 0.79531(16) 0.02452(19) Uani 1 1 d . . . O7 O 0.54769(13) 0.44514(11) 0.71484(14) 0.03030(19) Uani 1 1 d . . . O8 O 0.39192(15) 0.28356(16) 0.87910(17) 0.0408(3) Uani 1 1 d . . . OW1 O 0.5920(2) 0.68093(19) 0.82064(16) 0.0495(3) Uani 1 1 d D . . HW1A H 0.638(3) 0.597(2) 0.877(3) 0.050 Uiso 1 1 d D . . HW1B H 0.595(3) 0.750(2) 0.848(3) 0.050 Uiso 1 1 d D . . OW2 O 0.64175(15) 0.90951(18) 0.25053(15) 0.0389(2) Uani 1 1 d D . . HW2A H 0.637(3) 0.863(3) 0.196(3) 0.050 Uiso 1 1 d D . . HW2B H 0.5485(19) 0.959(3) 0.306(3) 0.050 Uiso 1 1 d 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 Ba1 0.01432(3) 0.02093(4) 0.02516(4) -0.01277(2) -0.00375(2) -0.00386(2) Co2 0.01471(6) 0.01847(6) 0.01829(6) -0.00548(5) -0.00506(4) -0.00428(4) N1 0.0159(3) 0.0236(4) 0.0236(4) -0.0127(3) -0.0029(3) -0.0058(3) C1 0.0207(5) 0.0428(7) 0.0265(5) -0.0169(5) 0.0035(4) -0.0128(5) C2 0.0324(6) 0.0432(7) 0.0200(5) -0.0129(5) 0.0001(4) -0.0205(5) O1 0.0251(4) 0.0237(4) 0.0419(5) -0.0188(4) -0.0200(4) 0.0035(3) O2 0.0471(7) 0.0831(10) 0.0221(4) -0.0240(6) 0.0044(4) -0.0379(7) C3 0.0218(5) 0.0228(5) 0.0349(6) -0.0161(4) 0.0011(4) -0.0065(4) C4 0.0172(4) 0.0180(4) 0.0231(4) -0.0072(3) -0.0062(3) -0.0041(3) O3 0.0155(3) 0.0176(3) 0.0263(4) -0.0042(3) -0.0027(3) -0.0024(2) O4 0.0321(5) 0.0175(3) 0.0284(4) -0.0038(3) -0.0071(3) -0.0071(3) C5 0.0248(5) 0.0306(6) 0.0487(8) -0.0245(6) -0.0209(5) 0.0068(4) C6 0.0191(4) 0.0210(4) 0.0266(5) -0.0105(4) -0.0099(4) -0.0031(3) O5 0.0297(4) 0.0361(5) 0.0386(5) -0.0179(4) -0.0208(4) -0.0018(4) O6 0.0407(6) 0.0522(7) 0.0249(4) -0.0165(5) -0.0147(4) 0.0022(5) C7 0.0296(7) 0.0245(6) 0.0692(12) -0.0111(7) -0.0220(7) 0.0049(5) C8 0.0206(4) 0.0203(4) 0.0317(5) -0.0090(4) -0.0109(4) -0.0016(3) O7 0.0230(4) 0.0191(4) 0.0427(5) -0.0071(4) -0.0119(4) -0.0025(3) O8 0.0252(5) 0.0401(6) 0.0507(7) -0.0157(5) -0.0038(4) -0.0128(4) OW1 0.0716(10) 0.0466(7) 0.0282(5) -0.0071(5) -0.0230(6) -0.0126(7) OW2 0.0296(5) 0.0559(7) 0.0349(5) -0.0228(5) -0.0010(4) -0.0178(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O5 2.7333(10) 1_655 ? Ba1 OW1 2.7356(13) . ? Ba1 O4 2.8018(10) 2_676 ? Ba1 O1 2.8496(9) 2_666 ? Ba1 O2 2.8518(12) . ? Ba1 O7 2.8527(10) . ? Ba1 O3 2.8917(9) . ? Ba1 O5 2.9070(11) 2_666 ? Ba1 OW2 2.9152(15) . ? Ba1 C6 3.2549(11) 2_666 ? Ba1 Co2 3.9143(2) . ? Ba1 Ba1 4.40898(18) 2_766 ? Co2 O6 2.0164(11) . ? Co2 O1 2.0213(9) . ? Co2 O7 2.0345(10) . ? Co2 O3 2.0395(9) . ? Co2 N1 2.2226(10) . ? N1 C3 1.4702(16) . ? N1 C5 1.4714(17) . ? N1 C1 1.4733(16) . ? C1 C2 1.513(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.2386(16) 1_456 ? C2 O6 1.2767(19) . ? O1 C6 1.2732(14) . ? O1 Ba1 2.8496(9) 2_666 ? O2 C2 1.2386(16) 1_654 ? C3 C4 1.5247(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O4 1.2430(14) . ? C4 O3 1.2727(13) . ? O4 Ba1 2.8018(10) 2_676 ? C5 C6 1.5140(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.2443(14) . ? C6 Ba1 3.2549(11) 2_666 ? O5 Ba1 2.7333(10) 1_455 ? O5 Ba1 2.9070(11) 2_666 ? C7 C8 1.5024(19) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O8 1.2445(17) . ? C8 O7 1.2704(16) . ? OW1 HW1A 0.840(10) . ? OW1 HW1B 0.830(10) . ? OW2 HW2A 0.853(10) . ? OW2 HW2B 0.841(10) . ? 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 _geom_angle_publ_flag O5 Ba1 OW1 80.95(5) 1_655 . ? O5 Ba1 O4 77.16(3) 1_655 2_676 ? OW1 Ba1 O4 67.72(4) . 2_676 ? O5 Ba1 O1 118.31(3) 1_655 2_666 ? OW1 Ba1 O1 139.22(4) . 2_666 ? O4 Ba1 O1 147.43(3) 2_676 2_666 ? O5 Ba1 O2 65.75(4) 1_655 . ? OW1 Ba1 O2 145.84(5) . . ? O4 Ba1 O2 96.38(4) 2_676 . ? O1 Ba1 O2 68.76(4) 2_666 . ? O5 Ba1 O7 123.59(3) 1_655 . ? OW1 Ba1 O7 67.67(4) . . ? O4 Ba1 O7 125.63(3) 2_676 . ? O1 Ba1 O7 71.98(3) 2_666 . ? O2 Ba1 O7 137.66(4) . . ? O5 Ba1 O3 146.95(3) 1_655 . ? OW1 Ba1 O3 70.27(4) . . ? O4 Ba1 O3 77.13(3) 2_676 . ? O1 Ba1 O3 94.40(3) 2_666 . ? O2 Ba1 O3 137.79(4) . . ? O7 Ba1 O3 59.66(3) . . ? O5 Ba1 O5 77.21(3) 1_655 2_666 ? OW1 Ba1 O5 118.57(4) . 2_666 ? O4 Ba1 O5 152.05(3) 2_676 2_666 ? O1 Ba1 O5 45.25(3) 2_666 2_666 ? O2 Ba1 O5 62.72(4) . 2_666 ? O7 Ba1 O5 78.59(3) . 2_666 ? O3 Ba1 O5 130.78(3) . 2_666 ? O5 Ba1 OW2 120.87(4) 1_655 . ? OW1 Ba1 OW2 119.91(4) . . ? O4 Ba1 OW2 65.26(3) 2_676 . ? O1 Ba1 OW2 82.60(3) 2_666 . ? O2 Ba1 OW2 74.70(4) . . ? O7 Ba1 OW2 115.37(3) . . ? O3 Ba1 OW2 64.63(3) . . ? O5 Ba1 OW2 120.66(3) 2_666 . ? O5 Ba1 C6 97.52(3) 1_655 2_666 ? OW1 Ba1 C6 132.21(4) . 2_666 ? O4 Ba1 C6 158.90(3) 2_676 2_666 ? O1 Ba1 C6 22.86(3) 2_666 2_666 ? O2 Ba1 C6 63.22(4) . 2_666 ? O7 Ba1 C6 74.44(3) . 2_666 ? O3 Ba1 C6 113.69(3) . 2_666 ? O5 Ba1 C6 22.39(3) 2_666 2_666 ? OW2 Ba1 C6 101.92(3) . 2_666 ? O5 Ba1 Co2 138.52(2) 1_655 . ? OW1 Ba1 Co2 60.26(4) . . ? O4 Ba1 Co2 99.08(2) 2_676 . ? O1 Ba1 Co2 87.13(2) 2_666 . ? O2 Ba1 Co2 153.83(3) . . ? O7 Ba1 Co2 30.102(19) . . ? O3 Ba1 Co2 30.406(17) . . ? O5 Ba1 Co2 107.48(2) 2_666 . ? OW2 Ba1 Co2 92.83(2) . . ? C6 Ba1 Co2 98.21(2) 2_666 . ? O5 Ba1 Ba1 40.01(2) 1_655 2_766 ? OW1 Ba1 Ba1 102.58(4) . 2_766 ? O4 Ba1 Ba1 116.40(2) 2_676 2_766 ? O1 Ba1 Ba1 80.201(18) 2_666 2_766 ? O2 Ba1 Ba1 56.17(4) . 2_766 ? O7 Ba1 Ba1 102.27(2) . 2_766 ? O3 Ba1 Ba1 161.852(17) . 2_766 ? O5 Ba1 Ba1 37.196(19) 2_666 2_766 ? OW2 Ba1 Ba1 130.87(2) . 2_766 ? C6 Ba1 Ba1 58.094(19) 2_666 2_766 ? Co2 Ba1 Ba1 131.490(4) . 2_766 ? O6 Co2 O1 129.62(6) . . ? O6 Co2 O7 103.10(5) . . ? O1 Co2 O7 108.14(4) . . ? O6 Co2 O3 117.15(6) . . ? O1 Co2 O3 102.04(4) . . ? O7 Co2 O3 89.08(4) . . ? O6 Co2 N1 78.10(4) . . ? O1 Co2 N1 79.41(4) . . ? O7 Co2 N1 167.56(4) . . ? O3 Co2 N1 79.53(4) . . ? O6 Co2 Ba1 109.53(4) . . ? O1 Co2 Ba1 120.55(3) . . ? O7 Co2 Ba1 44.69(3) . . ? O3 Co2 Ba1 45.86(2) . . ? N1 Co2 Ba1 123.04(3) . . ? C3 N1 C5 112.95(12) . . ? C3 N1 C1 111.33(10) . . ? C5 N1 C1 113.81(11) . . ? C3 N1 Co2 103.27(7) . . ? C5 N1 Co2 108.15(7) . . ? C1 N1 Co2 106.51(8) . . ? N1 C1 C2 111.60(10) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? O2 C2 O6 124.40(16) 1_456 . ? O2 C2 C1 119.03(15) 1_456 . ? O6 C2 C1 116.53(11) . . ? C6 O1 Co2 118.50(7) . . ? C6 O1 Ba1 96.75(7) . 2_666 ? Co2 O1 Ba1 142.14(4) . 2_666 ? C2 O2 Ba1 138.85(11) 1_654 . ? N1 C3 C4 111.85(9) . . ? N1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O4 C4 O3 124.64(11) . . ? O4 C4 C3 119.26(10) . . ? O3 C4 C3 116.06(10) . . ? C4 O3 Co2 117.71(7) . . ? C4 O3 Ba1 130.65(7) . . ? Co2 O3 Ba1 103.74(3) . . ? C4 O4 Ba1 131.01(8) . 2_676 ? N1 C5 C6 113.23(10) . . ? N1 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N1 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? O5 C6 O1 123.25(11) . . ? O5 C6 C5 118.25(11) . . ? O1 C6 C5 118.50(10) . . ? O5 C6 Ba1 62.88(7) . 2_666 ? O1 C6 Ba1 60.39(6) . 2_666 ? C5 C6 Ba1 178.22(9) . 2_666 ? C6 O5 Ba1 149.24(9) . 1_455 ? C6 O5 Ba1 94.72(7) . 2_666 ? Ba1 O5 Ba1 102.79(3) 1_455 2_666 ? C2 O6 Co2 120.31(10) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O8 C8 O7 120.95(12) . . ? O8 C8 C7 120.57(14) . . ? O7 C8 C7 118.48(13) . . ? C8 O7 Co2 103.84(8) . . ? C8 O7 Ba1 150.86(8) . . ? Co2 O7 Ba1 105.21(4) . . ? Ba1 OW1 HW1A 106.2(19) . . ? Ba1 OW1 HW1B 123.0(19) . . ? HW1A OW1 HW1B 101(3) . . ? Ba1 OW2 HW2A 105.9(19) . . ? Ba1 OW2 HW2B 100.9(19) . . ? HW2A OW2 HW2B 114(3) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 39.71 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 1.465 _refine_diff_density_min -1.486 _refine_diff_density_rms 0.131