# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Jiang-Gao Mao' _publ_contact_author_email mjg@fjirsm.ac.cn _publ_section_title ; Syntheses, Crystal Structures and Luminescent Properties of New Lanthanide(III) Organoarsonates ; _publ_author_name 'Jiang-Gao Mao' # Attachment '- qxy-paper.cif' data_C6H9AsLaNO9 _database_code_depnum_ccdc_archive 'CCDC 831371' #TrackingRef '- qxy-paper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 As La N O9' _chemical_formula_weight 452.97 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' As As 0.0499 2.0058 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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' _cell_length_a 12.453(4) _cell_length_b 7.313(2) _cell_length_c 12.823(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.244(5) _cell_angle_gamma 90.00 _cell_volume 1141.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3466 _cell_measurement_theta_min 2.5684 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1800 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 6.662 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7764 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9502 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2608 _reflns_number_gt 2299 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0238P)^2^+0.7390P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2608 _refine_ls_number_parameters 173 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _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 La1 La -0.168839(18) 0.28013(3) -0.209703(18) 0.01217(8) Uani 1 1 d . . . As1 As 0.05538(3) 0.21488(6) -0.76538(3) 0.01151(10) Uani 1 1 d . . . N1 N 0.0503(3) 0.2722(6) -0.3611(3) 0.0291(10) Uani 1 1 d . . . C1 C -0.0192(3) 0.2544(6) -0.4651(3) 0.0172(9) Uani 1 1 d . A . C2 C -0.1353(3) 0.2589(6) -0.4829(3) 0.0156(9) Uani 1 1 d . . . C3 C -0.1903(4) 0.2427(7) -0.5905(4) 0.0291(12) Uani 1 1 d . A . H3A H -0.2667 0.2415 -0.6063 0.035 Uiso 1 1 calc R . . C4 C -0.1363(4) 0.2286(7) -0.6732(4) 0.0299(12) Uani 1 1 d . . . H4A H -0.1761 0.2205 -0.7431 0.036 Uiso 1 1 calc R A . C5 C -0.0215(3) 0.2265(6) -0.6522(3) 0.0155(8) Uani 1 1 d . A . C6 C 0.0367(3) 0.2379(6) -0.5493(3) 0.0186(9) Uani 1 1 d . . . H6A H 0.1130 0.2348 -0.5349 0.022 Uiso 1 1 calc R A . O1W O 0.0131(2) 0.1975(5) -0.0741(2) 0.0284(8) Uani 1 1 d . . . H1WA H 0.0480 0.1173 -0.1016 0.043 Uiso 1 1 d R . . H1WB H 0.0525 0.2930 -0.0599 0.043 Uiso 1 1 d R . . O1 O -0.0346(2) 0.1925(4) -0.8806(2) 0.0229(7) Uani 1 1 d . . . O2W O -0.1483(3) 0.4689(5) -0.0334(3) 0.0449(10) Uani 1 1 d . . . H2WA H -0.2039 0.5383 -0.0378 0.067 Uiso 1 1 d R . . H2WB H -0.1446 0.3962 0.0189 0.067 Uiso 1 1 d R . . O2 O 0.1486(2) 0.0422(4) -0.7452(2) 0.0178(6) Uani 1 1 d . . . O3W O -0.2122(3) 0.1095(4) -0.0468(2) 0.0274(8) Uani 1 1 d . . . H3WA H -0.2299 -0.0003 -0.0642 0.041 Uiso 1 1 d R . . H3WB H -0.1556 0.1103 0.0037 0.041 Uiso 1 1 d R . . O3 O 0.1425(2) 0.3940(4) -0.7597(2) 0.0186(6) Uani 1 1 d . . . O4 O -0.1918(2) 0.2788(4) -0.4091(2) 0.0196(6) Uani 1 1 d . A . O5 O 0.0119(3) 0.2867(5) -0.2812(3) 0.0364(9) Uani 1 1 d . A . O6 O 0.1483(11) 0.317(2) -0.3551(11) 0.044(3) Uani 0.553(19) 1 d PU A 1 O6' O 0.1487(14) 0.220(3) -0.3485(14) 0.044(3) Uani 0.447(19) 1 d PU A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01279(12) 0.01278(13) 0.01126(12) 0.00008(9) 0.00324(8) 0.00004(9) As1 0.01146(19) 0.0142(2) 0.00924(19) -0.00063(15) 0.00309(14) -0.00014(16) N1 0.0183(19) 0.057(3) 0.0130(19) -0.0011(18) 0.0051(14) -0.0010(19) C1 0.017(2) 0.021(2) 0.014(2) -0.0009(17) 0.0031(15) 0.0006(17) C2 0.0151(19) 0.019(2) 0.014(2) 0.0009(17) 0.0072(15) 0.0000(16) C3 0.011(2) 0.057(4) 0.020(2) -0.002(2) 0.0044(17) 0.003(2) C4 0.018(2) 0.057(4) 0.015(2) -0.003(2) 0.0022(17) 0.000(2) C5 0.016(2) 0.018(2) 0.014(2) -0.0003(17) 0.0078(15) -0.0010(17) C6 0.0135(19) 0.025(3) 0.017(2) -0.0007(17) 0.0047(15) -0.0010(17) O1W 0.0196(16) 0.042(2) 0.0231(18) 0.0010(14) 0.0038(13) -0.0034(15) O1 0.0177(15) 0.037(2) 0.0118(15) -0.0012(13) -0.0004(11) 0.0003(14) O2W 0.081(3) 0.028(2) 0.025(2) -0.0025(16) 0.0092(19) 0.008(2) O2 0.0154(14) 0.0149(16) 0.0238(17) 0.0010(12) 0.0056(12) 0.0023(12) O3W 0.0301(18) 0.0276(19) 0.0221(17) 0.0021(14) 0.0001(13) -0.0119(15) O3 0.0196(15) 0.0124(16) 0.0236(17) 0.0031(12) 0.0045(12) -0.0011(12) O4 0.0196(15) 0.0281(17) 0.0131(15) 0.0029(12) 0.0080(11) 0.0069(13) O5 0.0239(17) 0.076(3) 0.0117(16) -0.0025(16) 0.0079(12) -0.0042(17) O6 0.016(2) 0.094(10) 0.022(3) -0.003(7) 0.0017(19) -0.004(7) O6' 0.016(2) 0.093(10) 0.022(3) -0.003(7) 0.001(2) -0.001(7) _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 La1 O3 2.448(3) 3_564 ? La1 O2 2.452(3) 3_554 ? La1 O4 2.511(3) . ? La1 O2 2.574(3) 4_566 ? La1 O3W 2.587(3) . ? La1 O5 2.604(3) . ? La1 O2W 2.615(3) . ? La1 O1W 2.618(3) . ? La1 O3 2.629(3) 4_566 ? La1 As1 3.3565(11) 4_566 ? La1 La1 4.1996(9) 2_444 ? La1 La1 4.1996(9) 2_454 ? As1 O1 1.662(3) . ? As1 O3 1.693(3) . ? As1 O2 1.698(3) . ? As1 C5 1.903(4) . ? As1 La1 3.3565(11) 4_665 ? N1 O5 1.224(5) . ? N1 O6 1.250(14) . ? N1 O6' 1.261(18) . ? N1 C1 1.434(5) . ? C1 C6 1.408(6) . ? C1 C2 1.415(6) . ? C2 O4 1.302(5) . ? C2 C3 1.409(6) . ? C3 C4 1.375(6) . ? C3 H3A 0.9300 . ? C4 C5 1.397(6) . ? C4 H4A 0.9300 . ? C5 C6 1.366(5) . ? C6 H6A 0.9300 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O2 La1 2.452(3) 3_554 ? O2 La1 2.574(3) 4_665 ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? O3 La1 2.448(3) 3_564 ? O3 La1 2.629(3) 4_665 ? 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 O3 La1 O2 150.89(10) 3_564 3_554 ? O3 La1 O4 80.27(10) 3_564 . ? O2 La1 O4 75.61(10) 3_554 . ? O3 La1 O2 67.88(9) 3_564 4_566 ? O2 La1 O2 125.07(7) 3_554 4_566 ? O4 La1 O2 85.19(9) . 4_566 ? O3 La1 O3W 131.06(10) 3_564 . ? O2 La1 O3W 77.07(10) 3_554 . ? O4 La1 O3W 145.28(10) . . ? O2 La1 O3W 93.37(10) 4_566 . ? O3 La1 O5 76.74(11) 3_564 . ? O2 La1 O5 78.18(11) 3_554 . ? O4 La1 O5 64.04(10) . . ? O2 La1 O5 136.48(10) 4_566 . ? O3W La1 O5 129.58(10) . . ? O3 La1 O2W 68.46(10) 3_564 . ? O2 La1 O2W 135.66(10) 3_554 . ? O4 La1 O2W 148.36(10) . . ? O2 La1 O2W 78.87(11) 4_566 . ? O3W La1 O2W 63.59(11) . . ? O5 La1 O2W 111.19(12) . . ? O3 La1 O1W 101.81(10) 3_564 . ? O2 La1 O1W 79.46(10) 3_554 . ? O4 La1 O1W 124.82(10) . . ? O2 La1 O1W 147.33(10) 4_566 . ? O3W La1 O1W 69.62(10) . . ? O5 La1 O1W 63.07(10) . . ? O2W La1 O1W 68.63(11) . . ? O3 La1 O3 125.13(7) 3_564 4_566 ? O2 La1 O3 66.93(9) 3_554 4_566 ? O4 La1 O3 81.18(9) . 4_566 ? O2 La1 O3 59.43(9) 4_566 4_566 ? O3W La1 O3 68.57(9) . 4_566 ? O5 La1 O3 135.82(10) . 4_566 ? O2W La1 O3 112.64(11) . 4_566 ? O1W La1 O3 130.78(9) . 4_566 ? O3 La1 As1 96.95(7) 3_564 4_566 ? O2 La1 As1 96.43(7) 3_554 4_566 ? O4 La1 As1 83.85(7) . 4_566 ? O2 La1 As1 29.70(6) 4_566 4_566 ? O3W La1 As1 78.33(7) . 4_566 ? O5 La1 As1 147.83(7) . 4_566 ? O2W La1 As1 94.94(9) . 4_566 ? O1W La1 As1 147.83(7) . 4_566 ? O3 La1 As1 29.82(6) 4_566 4_566 ? O3 La1 La1 151.85(7) 3_564 2_444 ? O2 La1 La1 34.25(7) 3_554 2_444 ? O4 La1 La1 78.52(7) . 2_444 ? O2 La1 La1 92.01(7) 4_566 2_444 ? O3W La1 La1 66.85(7) . 2_444 ? O5 La1 La1 109.64(8) . 2_444 ? O2W La1 La1 128.76(8) . 2_444 ? O1W La1 La1 105.44(7) . 2_444 ? O3 La1 La1 32.83(6) 4_566 2_444 ? As1 La1 La1 62.596(13) 4_566 2_444 ? O3 La1 La1 35.61(7) 3_564 2_454 ? O2 La1 La1 147.87(7) 3_554 2_454 ? O4 La1 La1 78.93(7) . 2_454 ? O2 La1 La1 32.43(6) 4_566 2_454 ? O3W La1 La1 116.53(7) . 2_454 ? O5 La1 La1 107.70(8) . 2_454 ? O2W La1 La1 72.94(8) . 2_454 ? O1W La1 La1 131.92(7) . 2_454 ? O3 La1 La1 90.18(6) 4_566 2_454 ? As1 La1 La1 61.366(13) 4_566 2_454 ? La1 La1 La1 121.06(2) 2_444 2_454 ? O1 As1 O3 114.81(15) . . ? O1 As1 O2 111.85(15) . . ? O3 As1 O2 99.07(14) . . ? O1 As1 C5 109.22(16) . . ? O3 As1 C5 110.75(16) . . ? O2 As1 C5 110.83(16) . . ? O1 As1 La1 131.03(11) . 4_665 ? O3 As1 La1 50.56(10) . 4_665 ? O2 As1 La1 48.69(10) . 4_665 ? C5 As1 La1 119.67(12) . 4_665 ? O5 N1 O6 118.4(7) . . ? O5 N1 O6' 117.5(9) . . ? O6 N1 O6' 33.2(7) . . ? O5 N1 C1 121.3(4) . . ? O6 N1 C1 118.0(7) . . ? O6' N1 C1 118.0(9) . . ? C6 C1 C2 122.2(4) . . ? C6 C1 N1 114.9(4) . . ? C2 C1 N1 122.9(4) . . ? O4 C2 C3 119.7(4) . . ? O4 C2 C1 125.2(4) . . ? C3 C2 C1 115.1(4) . . ? C4 C3 C2 123.1(4) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 As1 119.3(3) . . ? C4 C5 As1 120.9(3) . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? La1 O1W H1WA 109.3 . . ? La1 O1W H1WB 109.3 . . ? H1WA O1W H1WB 109.5 . . ? La1 O2W H2WA 109.2 . . ? La1 O2W H2WB 109.3 . . ? H2WA O2W H2WB 109.5 . . ? As1 O2 La1 141.27(15) . 3_554 ? As1 O2 La1 101.61(13) . 4_665 ? La1 O2 La1 113.32(11) 3_554 4_665 ? La1 O3W H3WA 109.3 . . ? La1 O3W H3WB 109.3 . . ? H3WA O3W H3WB 109.5 . . ? As1 O3 La1 148.50(15) . 3_564 ? As1 O3 La1 99.63(12) . 4_665 ? La1 O3 La1 111.56(10) 3_564 4_665 ? C2 O4 La1 141.1(3) . . ? N1 O5 La1 144.5(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.607 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.135 #===end data_C6H7AsGdNO8 _database_code_depnum_ccdc_archive 'CCDC 831372' #TrackingRef '- qxy-paper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H7 As Gd N O8' _chemical_formula_weight 453.30 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.197(3) _cell_length_b 21.153(7) _cell_length_c 6.964(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.650(7) _cell_angle_gamma 90.00 _cell_volume 1025.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2593 _cell_measurement_theta_min 3.0794 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.0500 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 9.699 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5779 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8009 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2344 _reflns_number_gt 2059 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0497P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2344 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _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 Gd1 Gd 1.04164(3) 1.459106(10) 0.26118(3) 0.01286(10) Uani 1 1 d . . . As1 As 1.23223(7) 1.08287(2) 0.31051(7) 0.01288(13) Uani 1 1 d . . . C1 C 1.1594(8) 1.1690(2) 0.2995(8) 0.0205(11) Uani 1 1 d . . . C2 C 0.9621(8) 1.1833(3) 0.2454(9) 0.0286(14) Uani 1 1 d . . . H2A H 0.8724 1.1507 0.2241 0.034 Uiso 1 1 calc R . . C3 C 0.9012(9) 1.2448(3) 0.2240(10) 0.0328(15) Uani 1 1 d . . . H3A H 0.7701 1.2532 0.1873 0.039 Uiso 1 1 calc R . . C4 C 1.0351(8) 1.2971(3) 0.2570(8) 0.0232(12) Uani 1 1 d . . . C5 C 1.2300(8) 1.2808(2) 0.3118(8) 0.0233(12) Uani 1 1 d . . . C6 C 1.2924(8) 1.2162(2) 0.3320(8) 0.0213(11) Uani 1 1 d . . . H6A H 1.4227 1.2066 0.3670 0.026 Uiso 1 1 calc R . . N1 N 1.3757(7) 1.3272(2) 0.3469(8) 0.0300(11) Uani 1 1 d . . . O1 O 1.1098(6) 1.04761(15) 0.0979(5) 0.0183(7) Uani 1 1 d . . . O2 O 1.1296(5) 1.04167(15) 0.4668(5) 0.0184(8) Uani 1 1 d . . . O3 O 1.4670(5) 1.07518(18) 0.3624(6) 0.0267(9) Uani 1 1 d . . . O4 O 0.9702(6) 1.35272(19) 0.2308(7) 0.0355(11) Uani 1 1 d . . . O5 O 1.3344(6) 1.38482(18) 0.3438(7) 0.0348(11) Uani 1 1 d . . . O6 O 1.5442(7) 1.3115(2) 0.3770(11) 0.0677(19) Uani 1 1 d . . . O1W O 1.3106(6) 1.52988(19) 0.3543(6) 0.0274(9) Uani 1 1 d . . . H1WA H 1.2704 1.5678 0.3461 0.041 Uiso 1 1 d R . . H1WC H 1.3832 1.5247 0.2765 0.041 Uiso 1 1 d R . . O2W O 0.6989(6) 1.43519(19) 0.2288(6) 0.0317(10) Uani 1 1 d . . . H2WA H 0.6847 1.3956 0.2395 0.048 Uiso 1 1 d R . . H2WB H 0.6332 1.4475 0.1159 0.048 Uiso 1 1 d R . . 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 Gd1 0.01774(15) 0.01076(14) 0.01053(16) 0.00073(8) 0.00442(10) 0.00245(8) As1 0.0159(2) 0.0106(2) 0.0124(3) -0.00049(19) 0.00404(19) -0.00129(17) C1 0.030(3) 0.012(2) 0.020(3) 0.000(2) 0.009(2) 0.002(2) C2 0.024(3) 0.020(3) 0.040(4) -0.001(2) 0.005(3) 0.002(2) C3 0.021(3) 0.022(3) 0.052(4) -0.004(3) 0.004(3) -0.002(2) C4 0.029(3) 0.017(3) 0.022(3) -0.001(2) 0.004(2) 0.001(2) C5 0.028(3) 0.018(2) 0.025(3) -0.001(2) 0.009(2) -0.002(2) C6 0.026(3) 0.014(2) 0.023(3) -0.004(2) 0.005(2) 0.000(2) N1 0.027(2) 0.021(2) 0.041(3) 0.003(2) 0.008(2) 0.002(2) O1 0.0266(19) 0.0163(16) 0.0126(18) -0.0037(14) 0.0059(15) -0.0039(14) O2 0.0236(19) 0.0169(17) 0.0164(19) -0.0004(14) 0.0082(15) -0.0054(13) O3 0.0193(19) 0.033(2) 0.028(2) -0.0033(19) 0.0062(16) -0.0021(17) O4 0.036(2) 0.0119(19) 0.059(3) 0.0014(18) 0.013(2) 0.0041(16) O5 0.032(2) 0.0154(18) 0.056(3) 0.0017(19) 0.010(2) 0.0074(17) O6 0.027(3) 0.025(2) 0.147(6) 0.006(3) 0.014(3) 0.001(2) O1W 0.022(2) 0.031(2) 0.029(2) -0.0011(18) 0.0075(17) -0.0080(17) O2W 0.026(2) 0.023(2) 0.042(3) 0.0000(19) 0.0025(19) -0.0051(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 Gd1 O1 2.276(4) 4_586 ? Gd1 O2 2.293(4) 4_585 ? Gd1 O4 2.306(4) . ? Gd1 O1W 2.403(4) . ? Gd1 O2 2.470(4) 2_755 ? Gd1 O2W 2.472(4) . ? Gd1 O1 2.489(3) 2_755 ? Gd1 O5 2.574(4) . ? Gd1 As1 3.2389(10) 2_755 ? Gd1 Gd1 3.9274(12) 3_786 ? Gd1 Gd1 3.9347(13) 3_785 ? As1 O3 1.644(4) . ? As1 O1 1.692(4) . ? As1 O2 1.702(3) . ? As1 C1 1.891(5) . ? As1 Gd1 3.2389(10) 2_745 ? C1 C6 1.362(7) . ? C1 C2 1.407(8) . ? C2 C3 1.368(8) . ? C2 H2A 0.9300 . ? C3 C4 1.447(8) . ? C3 H3A 0.9300 . ? C4 O4 1.263(7) . ? C4 C5 1.400(7) . ? C5 N1 1.411(7) . ? C5 C6 1.435(7) . ? C6 H6A 0.9300 . ? N1 O6 1.223(7) . ? N1 O5 1.254(6) . ? O1 Gd1 2.276(4) 4_585 ? O1 Gd1 2.489(3) 2_745 ? O2 Gd1 2.293(4) 4_586 ? O2 Gd1 2.470(3) 2_745 ? O1W H1WA 0.8500 . ? O1W H1WC 0.8500 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8499 . ? 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 O1 Gd1 O2 152.18(14) 4_586 4_585 ? O1 Gd1 O4 91.06(14) 4_586 . ? O2 Gd1 O4 90.95(13) 4_585 . ? O1 Gd1 O1W 79.15(13) 4_586 . ? O2 Gd1 O1W 81.96(13) 4_585 . ? O4 Gd1 O1W 141.12(15) . . ? O1 Gd1 O2 130.47(12) 4_586 2_755 ? O2 Gd1 O2 68.66(13) 4_585 2_755 ? O4 Gd1 O2 124.59(14) . 2_755 ? O1W Gd1 O2 88.27(14) . 2_755 ? O1 Gd1 O2W 91.79(14) 4_586 . ? O2 Gd1 O2W 114.31(14) 4_585 . ? O4 Gd1 O2W 66.28(14) . . ? O1W Gd1 O2W 150.38(14) . . ? O2 Gd1 O2W 76.23(13) 2_755 . ? O1 Gd1 O1 69.06(14) 4_586 2_755 ? O2 Gd1 O1 127.23(11) 4_585 2_755 ? O4 Gd1 O1 131.33(14) . 2_755 ? O1W Gd1 O1 80.11(14) . 2_755 ? O2 Gd1 O1 61.61(12) 2_755 2_755 ? O2W Gd1 O1 70.34(13) . 2_755 ? O1 Gd1 O5 77.33(14) 4_586 . ? O2 Gd1 O5 78.46(14) 4_585 . ? O4 Gd1 O5 64.90(14) . . ? O1W Gd1 O5 76.23(15) . . ? O2 Gd1 O5 145.33(13) 2_755 . ? O2W Gd1 O5 129.56(13) . . ? O1 Gd1 O5 141.84(14) 2_755 . ? O1 Gd1 As1 99.99(9) 4_586 2_755 ? O2 Gd1 As1 99.37(8) 4_585 2_755 ? O4 Gd1 As1 131.43(11) . 2_755 ? O1W Gd1 As1 87.44(11) . 2_755 ? O2 Gd1 As1 31.14(8) 2_755 2_755 ? O2W Gd1 As1 66.24(10) . 2_755 ? O1 Gd1 As1 30.99(8) 2_755 2_755 ? O5 Gd1 As1 163.67(9) . 2_755 ? O1 Gd1 Gd1 36.30(9) 4_586 3_786 ? O2 Gd1 Gd1 153.63(8) 4_585 3_786 ? O4 Gd1 Gd1 115.42(11) . 3_786 ? O1W Gd1 Gd1 77.41(10) . 3_786 ? O2 Gd1 Gd1 94.29(8) 2_755 3_786 ? O2W Gd1 Gd1 78.75(10) . 3_786 ? O1 Gd1 Gd1 32.76(8) 2_755 3_786 ? O5 Gd1 Gd1 111.79(11) . 3_786 ? As1 Gd1 Gd1 63.717(17) 2_755 3_786 ? O1 Gd1 Gd1 157.36(8) 4_586 3_785 ? O2 Gd1 Gd1 35.78(9) 4_585 3_785 ? O4 Gd1 Gd1 111.47(11) . 3_785 ? O1W Gd1 Gd1 84.23(10) . 3_785 ? O2 Gd1 Gd1 32.88(8) 2_755 3_785 ? O2W Gd1 Gd1 95.20(10) . 3_785 ? O1 Gd1 Gd1 93.10(8) 2_755 3_785 ? O5 Gd1 Gd1 113.56(11) . 3_785 ? As1 Gd1 Gd1 63.745(14) 2_755 3_785 ? Gd1 Gd1 Gd1 124.69(2) 3_786 3_785 ? O3 As1 O1 115.31(19) . . ? O3 As1 O2 113.39(19) . . ? O1 As1 O2 96.87(18) . . ? O3 As1 C1 111.3(2) . . ? O1 As1 C1 108.1(2) . . ? O2 As1 C1 111.0(2) . . ? O3 As1 Gd1 120.37(14) . 2_745 ? O1 As1 Gd1 49.24(12) . 2_745 ? O2 As1 Gd1 48.63(12) . 2_745 ? C1 As1 Gd1 128.36(18) . 2_745 ? C6 C1 C2 120.4(5) . . ? C6 C1 As1 121.6(4) . . ? C2 C1 As1 118.0(4) . . ? C3 C2 C1 120.5(5) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C2 C3 C4 121.8(5) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? O4 C4 C5 125.2(5) . . ? O4 C4 C3 118.8(5) . . ? C5 C4 C3 115.9(5) . . ? C4 C5 N1 121.8(5) . . ? C4 C5 C6 121.8(5) . . ? N1 C5 C6 116.4(5) . . ? C1 C6 C5 119.6(5) . . ? C1 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? O6 N1 O5 119.1(5) . . ? O6 N1 C5 120.2(5) . . ? O5 N1 C5 120.7(5) . . ? As1 O1 Gd1 149.1(2) . 4_585 ? As1 O1 Gd1 99.77(16) . 2_745 ? Gd1 O1 Gd1 110.94(14) 4_585 2_745 ? As1 O2 Gd1 146.92(18) . 4_586 ? As1 O2 Gd1 100.23(16) . 2_745 ? Gd1 O2 Gd1 111.34(13) 4_586 2_745 ? C4 O4 Gd1 146.2(4) . . ? N1 O5 Gd1 140.8(4) . . ? Gd1 O1W H1WA 109.5 . . ? Gd1 O1W H1WC 109.3 . . ? H1WA O1W H1WC 109.5 . . ? Gd1 O2W H2WA 109.5 . . ? Gd1 O2W H2WB 109.3 . . ? H2WA O2W H2WB 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.989 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.219 #===end data_C7H6AsSmNO9 _database_code_depnum_ccdc_archive 'CCDC 831373' #TrackingRef '- qxy-paper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H6 As N O9 Sm' _chemical_formula_weight 473.40 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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' _cell_length_a 7.0720(11) _cell_length_b 21.151(2) _cell_length_c 7.6662(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.421(8) _cell_angle_gamma 90.00 _cell_volume 1087.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2556 _cell_measurement_theta_min 3.0359 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 8.462 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7045 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8283 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2411 _reflns_number_gt 2141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0147P)^2^+4.9826P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2411 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.002 _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 Sm1 Sm 0.22158(5) 0.956466(15) 0.41458(4) 0.01347(11) Uani 1 1 d . . . As1 As 0.25147(10) 1.10809(3) 0.52075(9) 0.01504(17) Uani 1 1 d . . . C1 C 0.2500(11) 1.1819(3) 0.3794(10) 0.0227(16) Uani 1 1 d . . . C2 C 0.2788(12) 1.1804(3) 0.2027(11) 0.0327(19) Uani 1 1 d . . . H2A H 0.2954 1.1417 0.1517 0.039 Uiso 1 1 calc R . . C3 C 0.2825(12) 1.2350(3) 0.1074(10) 0.0307(18) Uani 1 1 d . . . H3B H 0.2919 1.2321 -0.0106 0.037 Uiso 1 1 calc R . . C4 C 0.2723(10) 1.2959(3) 0.1824(10) 0.0224(16) Uani 1 1 d . . . C5 C 0.2457(11) 1.2949(3) 0.3595(10) 0.0234(16) Uani 1 1 d . . . C6 C 0.2351(11) 1.2388(3) 0.4549(10) 0.0258(17) Uani 1 1 d . . . H6A H 0.2177 1.2408 0.5701 0.031 Uiso 1 1 calc R . . C7 C 0.0876(10) 1.0226(3) 0.0052(9) 0.0157(14) Uani 1 1 d . . . N1 N 0.2337(11) 1.3513(3) 0.4545(9) 0.0333(16) Uani 1 1 d . . . O1 O 0.0499(7) 1.06106(19) 0.4620(6) 0.0162(10) Uani 1 1 d . . . O2 O 0.4316(7) 1.05723(19) 0.5205(6) 0.0158(10) Uani 1 1 d . . . O3 O 0.2877(7) 1.1383(2) 0.7379(6) 0.0236(11) Uani 1 1 d . . . H3A H 0.2304 1.1159 0.7927 0.035 Uiso 1 1 calc R . . O4 O 0.2334(13) 1.3478(3) 0.6152(8) 0.067(2) Uani 1 1 d . . . O5 O 0.2171(9) 1.4032(2) 0.3783(7) 0.0344(13) Uani 1 1 d . . . O6 O 0.2848(8) 1.3458(2) 0.0908(7) 0.0289(12) Uani 1 1 d . . . O7 O 0.0784(7) 1.0517(2) -0.1400(6) 0.0227(11) Uani 1 1 d . . . O8 O 0.2233(7) 1.0269(2) 0.1556(6) 0.0208(11) Uani 1 1 d . . . O1W O 0.3580(7) 0.9565(2) 0.7486(6) 0.0215(11) Uani 1 1 d . . . H1WA H 0.3776 0.9187 0.7871 0.032 Uiso 1 1 d R . . H1WB H 0.4680 0.9765 0.7809 0.032 Uiso 1 1 d R . . 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 Sm1 0.0110(2) 0.01264(17) 0.01662(19) 0.00002(13) 0.00418(15) -0.00009(14) As1 0.0127(4) 0.0100(3) 0.0238(4) 0.0007(3) 0.0077(3) -0.0005(3) C1 0.019(4) 0.012(3) 0.038(4) 0.008(3) 0.010(3) 0.001(3) C2 0.042(6) 0.017(3) 0.045(5) -0.002(3) 0.021(4) -0.002(4) C3 0.036(5) 0.024(4) 0.030(4) -0.003(3) 0.008(4) -0.005(4) C4 0.013(4) 0.020(3) 0.032(4) -0.001(3) 0.005(3) 0.002(3) C5 0.022(4) 0.022(4) 0.026(4) -0.006(3) 0.006(3) 0.001(3) C6 0.029(5) 0.021(3) 0.031(4) 0.006(3) 0.015(4) 0.005(3) C7 0.011(4) 0.018(3) 0.017(3) -0.004(3) 0.003(3) 0.000(3) N1 0.046(5) 0.023(3) 0.036(4) 0.001(3) 0.021(4) 0.003(3) O1 0.012(3) 0.014(2) 0.022(2) -0.0007(18) 0.006(2) -0.0039(19) O2 0.012(3) 0.016(2) 0.021(2) -0.0002(18) 0.006(2) 0.0022(19) O3 0.024(3) 0.024(3) 0.027(3) -0.011(2) 0.015(2) -0.010(2) O4 0.146(8) 0.025(3) 0.040(4) 0.000(3) 0.044(4) 0.013(4) O5 0.046(4) 0.014(2) 0.044(3) 0.003(2) 0.016(3) 0.000(2) O6 0.038(3) 0.013(2) 0.037(3) 0.008(2) 0.014(3) 0.001(2) O7 0.018(3) 0.030(3) 0.018(2) 0.007(2) 0.002(2) -0.009(2) O8 0.021(3) 0.022(3) 0.017(2) 0.0007(19) 0.003(2) -0.008(2) O1W 0.013(3) 0.026(2) 0.021(3) 0.004(2) 0.000(2) -0.008(2) _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 Sm1 O6 2.341(4) 2_545 ? Sm1 O2 2.362(4) 3_676 ? Sm1 O1 2.422(4) 3_576 ? Sm1 O1W 2.434(4) . ? Sm1 O7 2.478(5) 3_575 ? Sm1 O8 2.485(4) . ? Sm1 O2 2.578(4) . ? Sm1 O1 2.604(4) . ? Sm1 O5 2.667(5) 2_545 ? Sm1 As1 3.2990(7) . ? As1 O2 1.668(4) . ? As1 O1 1.679(4) . ? As1 O3 1.725(4) . ? As1 C1 1.898(6) . ? C1 C6 1.354(9) . ? C1 C2 1.433(10) . ? C2 C3 1.371(10) . ? C2 H2A 0.9300 . ? C3 C4 1.422(10) . ? C3 H3B 0.9300 . ? C4 O6 1.287(8) . ? C4 C5 1.428(10) . ? C5 C6 1.409(9) . ? C5 N1 1.414(9) . ? C6 H6A 0.9300 . ? C7 O8 1.249(8) . ? C7 O7 1.255(8) . ? C7 C7 1.547(13) 3_575 ? N1 O5 1.232(7) . ? N1 O4 1.235(8) . ? O1 Sm1 2.422(4) 3_576 ? O2 Sm1 2.362(4) 3_676 ? O3 H3A 0.8200 . ? O5 Sm1 2.667(5) 2 ? O6 Sm1 2.341(4) 2 ? O7 Sm1 2.478(5) 3_575 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? 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 Sm1 O2 83.91(17) 2_545 3_676 ? O6 Sm1 O1 80.84(16) 2_545 3_576 ? O2 Sm1 O1 142.90(15) 3_676 3_576 ? O6 Sm1 O1W 91.06(16) 2_545 . ? O2 Sm1 O1W 74.82(15) 3_676 . ? O1 Sm1 O1W 71.88(15) 3_576 . ? O6 Sm1 O7 84.77(17) 2_545 3_575 ? O2 Sm1 O7 136.39(15) 3_676 3_575 ? O1 Sm1 O7 75.50(15) 3_576 3_575 ? O1W Sm1 O7 147.36(15) . 3_575 ? O6 Sm1 O8 126.17(16) 2_545 . ? O2 Sm1 O8 88.57(15) 3_676 . ? O1 Sm1 O8 127.47(15) 3_576 . ? O1W Sm1 O8 137.68(15) . . ? O7 Sm1 O8 65.29(15) 3_575 . ? O6 Sm1 O2 146.95(17) 2_545 . ? O2 Sm1 O2 65.07(16) 3_676 . ? O1 Sm1 O2 116.89(14) 3_576 . ? O1W Sm1 O2 70.77(14) . . ? O7 Sm1 O2 125.34(14) 3_575 . ? O8 Sm1 O2 66.93(14) . . ? O6 Sm1 O1 147.64(16) 2_545 . ? O2 Sm1 O1 125.03(14) 3_676 . ? O1 Sm1 O1 67.25(16) 3_576 . ? O1W Sm1 O1 84.26(15) . . ? O7 Sm1 O1 82.28(15) 3_575 . ? O8 Sm1 O1 73.87(14) . . ? O2 Sm1 O1 60.08(14) . . ? O6 Sm1 O5 64.55(16) 2_545 2_545 ? O2 Sm1 O5 72.02(16) 3_676 2_545 ? O1 Sm1 O5 128.62(16) 3_576 2_545 ? O1W Sm1 O5 140.35(16) . 2_545 ? O7 Sm1 O5 65.09(17) 3_575 2_545 ? O8 Sm1 O5 62.46(15) . 2_545 ? O2 Sm1 O5 112.55(15) . 2_545 ? O1 Sm1 O5 133.10(14) . 2_545 ? O6 Sm1 As1 167.33(12) 2_545 . ? O2 Sm1 As1 94.93(10) 3_676 . ? O1 Sm1 As1 92.82(10) 3_576 . ? O1W Sm1 As1 76.50(11) . . ? O7 Sm1 As1 104.36(11) 3_575 . ? O8 Sm1 As1 66.30(10) . . ? O2 Sm1 As1 29.88(10) . . ? O1 Sm1 As1 30.23(10) . . ? O5 Sm1 As1 127.11(11) 2_545 . ? O2 As1 O1 101.6(2) . . ? O2 As1 O3 111.1(2) . . ? O1 As1 O3 109.5(2) . . ? O2 As1 C1 113.3(3) . . ? O1 As1 C1 118.9(3) . . ? O3 As1 C1 102.7(3) . . ? O2 As1 Sm1 50.36(15) . . ? O1 As1 Sm1 51.32(15) . . ? O3 As1 Sm1 125.20(16) . . ? C1 As1 Sm1 132.1(2) . . ? C6 C1 C2 118.6(6) . . ? C6 C1 As1 118.3(5) . . ? C2 C1 As1 123.0(5) . . ? C3 C2 C1 121.1(7) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 122.4(7) . . ? C2 C3 H3B 118.8 . . ? C4 C3 H3B 118.8 . . ? O6 C4 C3 120.1(6) . . ? O6 C4 C5 125.6(6) . . ? C3 C4 C5 114.2(6) . . ? C6 C5 N1 114.9(6) . . ? C6 C5 C4 123.4(6) . . ? N1 C5 C4 121.7(6) . . ? C1 C6 C5 120.2(6) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? O8 C7 O7 126.3(6) . . ? O8 C7 C7 117.5(7) . 3_575 ? O7 C7 C7 116.2(7) . 3_575 ? O5 N1 O4 119.8(6) . . ? O5 N1 C5 121.3(6) . . ? O4 N1 C5 118.8(6) . . ? As1 O1 Sm1 134.1(2) . 3_576 ? As1 O1 Sm1 98.45(19) . . ? Sm1 O1 Sm1 112.75(16) 3_576 . ? As1 O2 Sm1 145.3(2) . 3_676 ? As1 O2 Sm1 99.8(2) . . ? Sm1 O2 Sm1 114.93(16) 3_676 . ? As1 O3 H3A 109.5 . . ? N1 O5 Sm1 139.4(5) . 2 ? C4 O6 Sm1 145.7(5) . 2 ? C7 O7 Sm1 120.6(4) . 3_575 ? C7 O8 Sm1 119.8(4) . . ? Sm1 O1W H1WA 109.4 . . ? Sm1 O1W H1WB 109.2 . . ? H1WA O1W H1WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O7 0.82 1.90 2.702(6) 164.7 1_556 O1W H1WA O4 0.85 1.95 2.689(7) 144.9 2_546 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.676 _refine_diff_density_min -1.280 _refine_diff_density_rms 0.211 #===end data_C7H6AsEuNO9 _database_code_depnum_ccdc_archive 'CCDC 831374' #TrackingRef '- qxy-paper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H6 As Eu N O9' _chemical_formula_weight 475.01 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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' _cell_length_a 7.047(7) _cell_length_b 21.094(19) _cell_length_c 7.656(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.527(17) _cell_angle_gamma 90.00 _cell_volume 1079.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 851 _cell_measurement_theta_min 3.0483 _cell_measurement_theta_max 27.3948 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 8.902 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6177 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8169 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.40 _reflns_number_total 2443 _reflns_number_gt 1945 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0243P)^2^+4.9111P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2443 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.000 _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 Eu1 Eu 0.27899(7) 0.04318(2) 0.58579(7) 0.01562(15) Uani 1 1 d . . . As1 As 0.24785(14) -0.10812(4) 0.47882(14) 0.0168(2) Uani 1 1 d . . . O1W O 0.1459(9) 0.0431(3) 0.2528(9) 0.0231(15) Uani 1 1 d . . . H1WA H 0.1274 0.0811 0.2138 0.035 Uiso 1 1 d R . . H1WC H 0.0352 0.0233 0.2188 0.035 Uiso 1 1 d R . . O1 O 0.0657(9) -0.0572(3) 0.4772(9) 0.0166(14) Uani 1 1 d . . . O2 O 0.4507(9) -0.0614(3) 0.5375(9) 0.0170(14) Uani 1 1 d . . . O3 O 0.2114(10) -0.1386(3) 0.2624(9) 0.0277(17) Uani 1 1 d . . . H3A H 0.2684 -0.1162 0.2072 0.042 Uiso 1 1 calc R . . O4 O 0.2157(10) -0.3466(3) 0.9083(10) 0.0280(17) Uani 1 1 d . . . O5 O 0.2823(11) -0.4035(3) 0.6218(11) 0.0344(19) Uani 1 1 d . . . O6 O 0.2609(18) -0.3478(4) 0.3816(12) 0.065(3) Uani 1 1 d . . . O7 O 0.2759(9) -0.0274(3) 0.8440(9) 0.0207(15) Uani 1 1 d . . . O8 O 0.4202(9) -0.0515(3) 1.1404(9) 0.0235(16) Uani 1 1 d . . . N1 N 0.2665(14) -0.3523(4) 0.5443(12) 0.033(2) Uani 1 1 d . . . C1 C 0.2484(14) -0.1820(4) 0.6229(13) 0.020(2) Uiso 1 1 d . . . C2 C 0.2628(15) -0.2392(5) 0.5439(15) 0.031(3) Uani 1 1 d . . . H2A H 0.2787 -0.2412 0.4281 0.037 Uiso 1 1 calc R . . C3 C 0.2528(15) -0.2953(5) 0.6417(15) 0.025(2) Uani 1 1 d . . . C4 C 0.2288(14) -0.2964(5) 0.8190(15) 0.024(2) Uani 1 1 d . . . C5 C 0.2179(17) -0.2353(5) 0.8970(16) 0.034(3) Uani 1 1 d . . . H5A H 0.2069 -0.2324 1.0146 0.041 Uiso 1 1 calc R . . C6 C 0.2234(17) -0.1803(5) 0.7999(17) 0.036(3) Uani 1 1 d . . . H6A H 0.2105 -0.1413 0.8518 0.043 Uiso 1 1 calc R . . C7 C 0.4119(13) -0.0223(4) 0.9964(13) 0.017(2) Uani 1 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 Eu1 0.0137(2) 0.0159(2) 0.0164(3) -0.0001(2) 0.00345(18) -0.00027(18) As1 0.0152(5) 0.0123(4) 0.0234(6) 0.0008(4) 0.0071(4) -0.0009(4) O1W 0.020(3) 0.027(4) 0.019(4) 0.002(3) 0.002(3) -0.004(3) O1 0.014(3) 0.013(3) 0.024(4) -0.002(3) 0.007(3) 0.000(2) O2 0.014(3) 0.019(3) 0.020(4) -0.001(3) 0.009(3) -0.002(3) O3 0.030(4) 0.036(4) 0.022(4) -0.013(3) 0.015(3) -0.009(3) O4 0.033(4) 0.015(3) 0.038(4) 0.006(3) 0.014(4) 0.005(3) O5 0.045(5) 0.015(3) 0.044(5) 0.005(3) 0.014(4) -0.006(3) O6 0.139(10) 0.028(5) 0.038(6) 0.005(4) 0.041(6) -0.001(5) O7 0.016(3) 0.029(4) 0.013(3) 0.002(3) -0.002(3) -0.004(3) O8 0.018(3) 0.031(4) 0.015(3) 0.004(3) -0.004(3) -0.010(3) N1 0.042(6) 0.022(5) 0.029(6) -0.001(4) 0.003(5) 0.005(4) C2 0.028(6) 0.028(6) 0.038(7) 0.008(5) 0.014(5) -0.003(5) C3 0.026(6) 0.015(5) 0.035(6) -0.001(5) 0.011(5) 0.008(4) C4 0.021(5) 0.021(5) 0.032(6) 0.000(5) 0.010(5) 0.000(4) C5 0.044(7) 0.026(6) 0.038(7) 0.001(5) 0.020(6) 0.004(5) C6 0.044(7) 0.023(6) 0.047(8) -0.004(5) 0.022(6) -0.003(5) C7 0.013(4) 0.024(5) 0.015(5) -0.001(4) 0.005(4) 0.008(4) _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 Eu1 O4 2.326(7) 2_556 ? Eu1 O1 2.340(6) 3_556 ? Eu1 O2 2.411(6) 3_656 ? Eu1 O1W 2.421(7) . ? Eu1 O8 2.469(6) 3_657 ? Eu1 O7 2.481(7) . ? Eu1 O1 2.577(6) . ? Eu1 O2 2.598(6) . ? Eu1 O5 2.661(8) 2_556 ? Eu1 As1 3.285(3) . ? Eu1 Eu1 4.150(4) 3_556 ? Eu1 Eu1 4.165(3) 3_656 ? As1 O1 1.671(6) . ? As1 O2 1.676(6) . ? As1 O3 1.719(7) . ? As1 C1 1.908(10) . ? O1W H1WA 0.8499 . ? O1W H1WC 0.8500 . ? O1 Eu1 2.340(6) 3_556 ? O2 Eu1 2.411(6) 3_656 ? O3 H3A 0.8200 . ? O4 C4 1.278(12) . ? O4 Eu1 2.326(7) 2_546 ? O5 N1 1.219(11) . ? O5 Eu1 2.661(8) 2_546 ? O6 N1 1.237(12) . ? O7 C7 1.257(11) . ? O8 C7 1.248(11) . ? O8 Eu1 2.469(6) 3_657 ? N1 C3 1.434(13) . ? C1 C2 1.368(14) . ? C1 C6 1.422(15) . ? C2 C3 1.414(14) . ? C2 H2A 0.9300 . ? C3 C4 1.421(15) . ? C4 C5 1.434(14) . ? C5 C6 1.384(15) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C7 1.544(18) 3_657 ? 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 O4 Eu1 O1 83.5(2) 2_556 3_556 ? O4 Eu1 O2 80.7(2) 2_556 3_656 ? O1 Eu1 O2 142.8(2) 3_556 3_656 ? O4 Eu1 O1W 91.1(2) 2_556 . ? O1 Eu1 O1W 75.7(2) 3_556 . ? O2 Eu1 O1W 71.2(2) 3_656 . ? O4 Eu1 O8 84.8(2) 2_556 3_657 ? O1 Eu1 O8 136.1(2) 3_556 3_657 ? O2 Eu1 O8 75.5(2) 3_656 3_657 ? O1W Eu1 O8 146.6(2) . 3_657 ? O4 Eu1 O7 126.1(2) 2_556 . ? O1 Eu1 O7 88.2(2) 3_556 . ? O2 Eu1 O7 128.0(2) 3_656 . ? O1W Eu1 O7 137.8(2) . . ? O8 Eu1 O7 65.7(2) 3_657 . ? O4 Eu1 O1 146.3(2) 2_556 . ? O1 Eu1 O1 64.9(2) 3_556 . ? O2 Eu1 O1 117.2(2) 3_656 . ? O1W Eu1 O1 70.7(2) . . ? O8 Eu1 O1 126.0(2) 3_657 . ? O7 Eu1 O1 67.2(2) . . ? O4 Eu1 O2 147.8(2) 2_556 . ? O1 Eu1 O2 125.3(2) 3_556 . ? O2 Eu1 O2 67.5(2) 3_656 . ? O1W Eu1 O2 83.8(2) . . ? O8 Eu1 O2 82.4(2) 3_657 . ? O7 Eu1 O2 74.1(2) . . ? O1 Eu1 O2 60.4(2) . . ? O4 Eu1 O5 64.3(2) 2_556 2_556 ? O1 Eu1 O5 71.6(2) 3_556 2_556 ? O2 Eu1 O5 128.5(2) 3_656 2_556 ? O1W Eu1 O5 140.7(2) . 2_556 ? O8 Eu1 O5 65.2(2) 3_657 2_556 ? O7 Eu1 O5 62.5(2) . 2_556 ? O1 Eu1 O5 112.6(2) . 2_556 ? O2 Eu1 O5 133.3(2) . 2_556 ? O4 Eu1 As1 167.31(18) 2_556 . ? O1 Eu1 As1 95.10(14) 3_556 . ? O2 Eu1 As1 93.18(15) 3_656 . ? O1W Eu1 As1 76.35(16) . . ? O8 Eu1 As1 104.58(16) 3_657 . ? O7 Eu1 As1 66.33(16) . . ? O1 Eu1 As1 30.15(13) . . ? O2 Eu1 As1 30.34(13) . . ? O5 Eu1 As1 127.22(16) 2_556 . ? O4 Eu1 Eu1 116.91(18) 2_556 3_556 ? O1 Eu1 Eu1 34.23(15) 3_556 3_556 ? O2 Eu1 Eu1 137.15(16) 3_656 3_556 ? O1W Eu1 Eu1 69.84(15) . 3_556 ? O8 Eu1 Eu1 140.48(16) 3_657 3_556 ? O7 Eu1 Eu1 75.01(14) . 3_556 ? O1 Eu1 Eu1 30.71(13) . 3_556 ? O2 Eu1 Eu1 91.12(15) . 3_556 ? O5 Eu1 Eu1 93.50(17) 2_556 3_556 ? As1 Eu1 Eu1 60.86(4) . 3_556 ? O4 Eu1 Eu1 115.75(18) 2_556 3_656 ? O1 Eu1 Eu1 145.26(16) 3_556 3_656 ? O2 Eu1 Eu1 35.19(15) 3_656 3_656 ? O1W Eu1 Eu1 75.28(16) . 3_656 ? O8 Eu1 Eu1 76.84(18) 3_657 3_656 ? O7 Eu1 Eu1 100.70(16) . 3_656 ? O1 Eu1 Eu1 87.53(15) . 3_656 ? O2 Eu1 Eu1 32.33(13) . 3_656 ? O5 Eu1 Eu1 142.00(17) 2_556 3_656 ? As1 Eu1 Eu1 59.59(4) . 3_656 ? Eu1 Eu1 Eu1 115.89(7) 3_556 3_656 ? O1 As1 O2 102.2(3) . . ? O1 As1 O3 110.7(3) . . ? O2 As1 O3 109.4(3) . . ? O1 As1 C1 112.9(4) . . ? O2 As1 C1 118.7(4) . . ? O3 As1 C1 102.9(4) . . ? O1 As1 Eu1 50.8(2) . . ? O2 As1 Eu1 51.5(2) . . ? O3 As1 Eu1 125.6(2) . . ? C1 As1 Eu1 131.4(3) . . ? Eu1 O1W H1WA 109.5 . . ? Eu1 O1W H1WC 109.5 . . ? H1WA O1W H1WC 109.5 . . ? As1 O1 Eu1 145.9(3) . 3_556 ? As1 O1 Eu1 99.1(3) . . ? Eu1 O1 Eu1 115.1(2) 3_556 . ? As1 O2 Eu1 134.5(3) . 3_656 ? As1 O2 Eu1 98.1(3) . . ? Eu1 O2 Eu1 112.5(2) 3_656 . ? As1 O3 H3A 109.5 . . ? C4 O4 Eu1 146.5(7) . 2_546 ? N1 O5 Eu1 140.3(7) . 2_546 ? C7 O7 Eu1 119.4(6) . . ? C7 O8 Eu1 120.1(6) . 3_657 ? O5 N1 O6 121.8(9) . . ? O5 N1 C3 120.0(9) . . ? O6 N1 C3 118.2(9) . . ? C2 C1 C6 119.5(9) . . ? C2 C1 As1 116.9(8) . . ? C6 C1 As1 123.6(7) . . ? C1 C2 C3 118.8(10) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C2 C3 C4 124.1(9) . . ? C2 C3 N1 113.8(10) . . ? C4 C3 N1 122.1(9) . . ? O4 C4 C3 125.1(9) . . ? O4 C4 C5 120.0(10) . . ? C3 C4 C5 114.9(9) . . ? C6 C5 C4 121.0(11) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C1 121.6(10) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? O8 C7 O7 125.8(9) . . ? O8 C7 C7 117.2(10) . 3_657 ? O7 C7 C7 117.0(10) . 3_657 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.794 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.280