# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Grepioni, Fabrizia' 'Maini, Lucia' 'Braga, Dario' _publ_contact_author_name 'Grepioni, Fabrizia' _publ_contact_author_email fabrizia.grepioni@unibo.it _publ_section_title ; From unexpected reactions to a new family of ionic co-crystals: the case of barbituric acid with alkali bromides and caesium iodide ; # Attachment '- BA_CsBr.cif' data_acbarb_c _database_code_depnum_ccdc_archive 'CCDC 787491' #TrackingRef '- BA_CsBr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Br Cs N2 O3' _chemical_formula_weight 340.90 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.0870(5) _cell_length_b 9.1380(4) _cell_length_c 10.4000(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.345(6) _cell_angle_gamma 90.00 _cell_volume 863.35(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1537 _cell_measurement_theta_min 2.9309 _cell_measurement_theta_max 28.9274 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 8.879 _exptl_absorpt_correction_T_min 0.63685 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2502 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 28.94 _reflns_number_total 2259 _reflns_number_gt 1330 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0253P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2259 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Cs01 Cs 0.22545(3) 0.60940(3) -0.13011(3) 0.03148(10) Uani 1 1 d . . . Br02 Br 0.49416(5) 0.31958(5) -0.13643(5) 0.03574(13) Uani 1 1 d . . . O6 O 0.1229(3) 0.3860(3) 0.0761(3) 0.0417(8) Uani 1 1 d . . . O2 O 0.1617(3) -0.1031(3) 0.0241(3) 0.0421(8) Uani 1 1 d . . . N3 N 0.3566(4) 0.0158(4) 0.1114(4) 0.0309(9) Uani 1 1 d . . . O4 O 0.5525(3) 0.1311(3) 0.2016(4) 0.0462(9) Uani 1 1 d . . . C5 C 0.3346(5) 0.2727(5) 0.1694(5) 0.0330(11) Uani 1 1 d . . . H5A H 0.3108 0.2883 0.2588 0.040 Uiso 1 1 calc R . . H5B H 0.3941 0.3551 0.1429 0.040 Uiso 1 1 calc R . . C6 C 0.1960(4) 0.2749(5) 0.0926(4) 0.0281(10) Uani 1 1 d . . . C2 C 0.2187(4) 0.0114(5) 0.0570(4) 0.0279(10) Uani 1 1 d . . . N1 N 0.1479(4) 0.1443(4) 0.0441(4) 0.0314(9) Uani 1 1 d . . . C4 C 0.4264(5) 0.1381(5) 0.1617(4) 0.0299(10) Uani 1 1 d . . . H100 H 0.062(4) 0.141(4) 0.016(4) 0.018(11) Uiso 1 1 d . . . H300 H 0.397(5) -0.056(5) 0.110(5) 0.049(17) Uiso 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 Cs01 0.02757(15) 0.02547(14) 0.04114(18) 0.00012(14) -0.00461(13) 0.00105(11) Br02 0.0368(2) 0.0321(2) 0.0381(3) -0.0075(2) -0.0046(2) 0.0105(2) O6 0.0343(17) 0.0310(17) 0.060(2) 0.0107(18) 0.0046(17) 0.0089(14) O2 0.0323(16) 0.0347(17) 0.059(2) -0.0083(19) -0.0144(17) 0.0000(15) N3 0.0208(18) 0.0248(19) 0.047(3) 0.000(2) -0.0063(19) 0.0032(17) O4 0.0272(16) 0.043(2) 0.068(3) 0.0156(19) -0.0137(18) -0.0039(15) C5 0.033(2) 0.030(2) 0.036(3) -0.001(2) 0.000(2) -0.001(2) C6 0.026(2) 0.029(2) 0.029(2) 0.007(2) 0.005(2) 0.0063(19) C2 0.026(2) 0.030(2) 0.027(2) 0.005(2) -0.001(2) 0.0038(19) N1 0.0229(19) 0.033(2) 0.038(2) 0.0020(19) -0.0073(19) 0.0056(17) C4 0.031(2) 0.028(2) 0.030(2) 0.008(2) 0.002(2) -0.0009(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cs01 O6 3.119(3) . ? Cs01 O2 3.139(3) 1_565 ? Cs01 O4 3.199(3) 4_565 ? Cs01 O4 3.212(3) 3_665 ? Cs01 O6 3.228(3) 3_565 ? Cs01 Br02 3.6039(5) . ? Cs01 Br02 3.6522(6) 2_554 ? Cs01 Br02 3.7770(6) 3_665 ? Cs01 C6 3.848(4) . ? Cs01 Cs01 5.2293(3) 2_544 ? Cs01 Cs01 5.2293(3) 2_554 ? Cs01 Cs01 5.3507(6) 3_565 ? Br02 Cs01 3.6522(6) 2_544 ? Br02 Cs01 3.7770(6) 3_665 ? O6 C6 1.223(5) . ? O6 Cs01 3.228(3) 3_565 ? O2 C2 1.213(5) . ? O2 Cs01 3.139(3) 1_545 ? N3 C2 1.363(5) . ? N3 C4 1.382(6) . ? O4 C4 1.211(5) . ? O4 Cs01 3.199(3) 4_666 ? O4 Cs01 3.212(3) 3_665 ? C5 C6 1.476(6) . ? C5 C4 1.489(6) . ? C6 N1 1.363(5) . ? C2 N1 1.380(5) . ? 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 Cs01 O2 97.74(9) . 1_565 ? O6 Cs01 O4 77.03(10) . 4_565 ? O2 Cs01 O4 139.50(7) 1_565 4_565 ? O6 Cs01 O4 147.33(10) . 3_665 ? O2 Cs01 O4 67.98(8) 1_565 3_665 ? O4 Cs01 O4 133.13(3) 4_565 3_665 ? O6 Cs01 O6 65.10(9) . 3_565 ? O2 Cs01 O6 72.95(8) 1_565 3_565 ? O4 Cs01 O6 68.47(8) 4_565 3_565 ? O4 Cs01 O6 130.88(8) 3_665 3_565 ? O6 Cs01 Br02 75.23(5) . . ? O2 Cs01 Br02 139.25(6) 1_565 . ? O4 Cs01 Br02 79.01(5) 4_565 . ? O4 Cs01 Br02 96.24(6) 3_665 . ? O6 Cs01 Br02 132.87(5) 3_565 . ? O6 Cs01 Br02 129.34(6) . 2_554 ? O2 Cs01 Br02 78.18(6) 1_565 2_554 ? O4 Cs01 Br02 75.17(6) 4_565 2_554 ? O4 Cs01 Br02 78.12(6) 3_665 2_554 ? O6 Cs01 Br02 65.54(6) 3_565 2_554 ? Br02 Cs01 Br02 137.238(11) . 2_554 ? O6 Cs01 Br02 79.34(6) . 3_665 ? O2 Cs01 Br02 67.08(6) 1_565 3_665 ? O4 Cs01 Br02 146.49(6) 4_565 3_665 ? O4 Cs01 Br02 68.07(7) 3_665 3_665 ? O6 Cs01 Br02 121.16(7) 3_565 3_665 ? Br02 Cs01 Br02 72.182(13) . 3_665 ? Br02 Cs01 Br02 138.263(9) 2_554 3_665 ? O6 Cs01 C6 16.30(7) . . ? O2 Cs01 C6 109.94(9) 1_565 . ? O4 Cs01 C6 75.12(10) 4_565 . ? O4 Cs01 C6 141.14(9) 3_665 . ? O6 Cs01 C6 79.83(9) 3_565 . ? Br02 Cs01 C6 58.93(6) . . ? Br02 Cs01 C6 140.65(7) 2_554 . ? Br02 Cs01 C6 75.52(7) 3_665 . ? O6 Cs01 Cs01 77.66(6) . 2_544 ? O2 Cs01 Cs01 173.59(6) 1_565 2_544 ? O4 Cs01 Cs01 35.42(5) 4_565 2_544 ? O4 Cs01 Cs01 118.26(6) 3_665 2_544 ? O6 Cs01 Cs01 100.91(6) 3_565 2_544 ? Br02 Cs01 Cs01 44.258(9) . 2_544 ? Br02 Cs01 Cs01 101.177(12) 2_554 2_544 ? Br02 Cs01 Cs01 115.881(10) 3_665 2_544 ? C6 Cs01 Cs01 66.48(6) . 2_544 ? O6 Cs01 Cs01 158.43(6) . 2_554 ? O2 Cs01 Cs01 62.05(6) 1_565 2_554 ? O4 Cs01 Cs01 112.70(7) 4_565 2_554 ? O4 Cs01 Cs01 35.26(6) 3_665 2_554 ? O6 Cs01 Cs01 99.58(5) 3_565 2_554 ? Br02 Cs01 Cs01 124.608(12) . 2_554 ? Br02 Cs01 Cs01 43.523(8) 2_554 2_554 ? Br02 Cs01 Cs01 97.830(10) 3_665 2_554 ? C6 Cs01 Cs01 171.48(7) . 2_554 ? Cs01 Cs01 Cs01 121.789(12) 2_544 2_554 ? O6 Cs01 Cs01 33.18(5) . 3_565 ? O2 Cs01 Cs01 84.36(6) 1_565 3_565 ? O4 Cs01 Cs01 69.37(6) 4_565 3_565 ? O4 Cs01 Cs01 152.33(6) 3_665 3_565 ? O6 Cs01 Cs01 31.92(6) 3_565 3_565 ? Br02 Cs01 Cs01 105.179(12) . 3_565 ? Br02 Cs01 Cs01 96.879(11) 2_554 3_565 ? Br02 Cs01 Cs01 101.795(11) 3_665 3_565 ? C6 Cs01 Cs01 48.24(6) . 3_565 ? Cs01 Cs01 Cs01 89.405(7) 2_544 3_565 ? Cs01 Cs01 Cs01 129.985(9) 2_554 3_565 ? Cs01 Br02 Cs01 92.219(12) . 2_544 ? Cs01 Br02 Cs01 107.818(13) . 3_665 ? Cs01 Br02 Cs01 157.961(14) 2_544 3_665 ? C6 O6 Cs01 118.0(3) . . ? C6 O6 Cs01 121.2(3) . 3_565 ? Cs01 O6 Cs01 114.90(9) . 3_565 ? C2 O2 Cs01 141.6(3) . 1_545 ? C2 N3 C4 126.2(4) . . ? C4 O4 Cs01 132.2(3) . 4_666 ? C4 O4 Cs01 118.4(3) . 3_665 ? Cs01 O4 Cs01 109.31(9) 4_666 3_665 ? C6 C5 C4 117.0(4) . . ? O6 C6 N1 120.4(4) . . ? O6 C6 C5 122.7(4) . . ? N1 C6 C5 116.8(4) . . ? O6 C6 Cs01 45.7(2) . . ? N1 C6 Cs01 119.9(3) . . ? C5 C6 Cs01 105.4(3) . . ? O2 C2 N3 121.6(4) . . ? O2 C2 N1 122.5(4) . . ? N3 C2 N1 115.9(4) . . ? C6 N1 C2 126.1(4) . . ? O4 C4 N3 120.6(4) . . ? O4 C4 C5 123.5(4) . . ? N3 C4 C5 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.453 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.111 # Attachment '- BA_CsI.cif' data_acbarb_csi_c_raccolta _database_code_depnum_ccdc_archive 'CCDC 787492' #TrackingRef '- BA_CsI.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Cs I N2 O3' _chemical_formula_weight 387.90 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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 7.302(5) _cell_length_b 7.510(5) _cell_length_c 9.400(5) _cell_angle_alpha 110.800(5) _cell_angle_beta 101.329(5) _cell_angle_gamma 94.472(5) _cell_volume 466.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8723 _cell_measurement_theta_min 2.3795 _cell_measurement_theta_max 29.1270 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 7.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56685 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14441 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 29.19 _reflns_number_total 2323 _reflns_number_gt 2002 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0196P)^2^+0.2469P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2323 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0432 _refine_ls_wR_factor_gt 0.0420 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Cs1 Cs 0.66913(3) 0.90397(3) 0.28415(2) 0.03685(7) Uani 1 1 d . . . I1 I 0.64163(3) 0.33871(3) 0.15597(2) 0.03465(7) Uani 1 1 d . . . O4 O 0.0771(3) 0.2044(3) -0.0455(2) 0.0351(5) Uani 1 1 d . . . O6 O 0.3475(4) 0.7443(3) 0.4161(3) 0.0495(6) Uani 1 1 d . . . N1 N 0.2286(4) 0.4618(4) 0.4229(3) 0.0401(7) Uani 1 1 d . . . N3 N 0.1148(4) 0.1888(4) 0.1931(3) 0.0309(6) Uani 1 1 d . . . O2 O 0.1164(4) 0.1753(3) 0.4294(3) 0.0578(8) Uani 1 1 d . . . C4 C 0.1214(4) 0.2883(4) 0.0972(3) 0.0276(6) Uani 1 1 d . . . C6 C 0.2614(5) 0.5806(4) 0.3451(3) 0.0330(7) Uani 1 1 d . . . C5 C 0.1769(4) 0.5008(4) 0.1741(3) 0.0291(6) Uani 1 1 d . . . H5A H 0.0655 0.5591 0.1549 0.035 Uiso 1 1 calc R . . H5B H 0.2668 0.5406 0.1234 0.035 Uiso 1 1 calc R . . C2 C 0.1506(5) 0.2688(4) 0.3540(3) 0.0349(7) Uani 1 1 d . . . H100 H 0.245(5) 0.505(5) 0.515(4) 0.035(9) Uiso 1 1 d . . . H300 H 0.072(4) 0.077(4) 0.150(3) 0.023(8) Uiso 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 Cs1 0.05221(14) 0.02944(10) 0.02896(11) 0.01037(8) 0.01282(9) 0.00249(9) I1 0.03824(13) 0.03597(12) 0.02939(11) 0.01329(9) 0.00557(8) 0.00603(9) O4 0.0451(13) 0.0334(11) 0.0219(10) 0.0068(9) 0.0063(9) -0.0007(9) O6 0.0691(18) 0.0296(12) 0.0369(13) 0.0002(10) 0.0158(12) -0.0140(11) N1 0.058(2) 0.0340(14) 0.0198(13) 0.0054(11) 0.0047(12) -0.0065(13) N3 0.0407(16) 0.0225(12) 0.0252(13) 0.0093(10) 0.0010(11) -0.0024(11) O2 0.087(2) 0.0484(14) 0.0346(13) 0.0247(11) -0.0006(13) -0.0150(14) C4 0.0266(16) 0.0272(14) 0.0270(15) 0.0080(12) 0.0069(12) 0.0033(12) C6 0.0374(18) 0.0279(15) 0.0324(16) 0.0085(13) 0.0123(13) 0.0018(13) C5 0.0350(17) 0.0251(14) 0.0271(15) 0.0101(12) 0.0074(12) 0.0033(12) C2 0.0414(19) 0.0327(16) 0.0276(15) 0.0130(13) 0.0011(13) -0.0016(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cs1 O4 3.115(3) 2_665 ? Cs1 O2 3.112(3) 2_666 ? Cs1 O6 3.135(3) 2_676 ? Cs1 O6 3.202(3) . ? Cs1 O2 3.452(3) 1_665 ? Cs1 I1 3.867(2) 1_565 ? Cs1 I1 3.956(3) . ? Cs1 I1 3.9873(18) 2_665 ? Cs1 Cs1 4.999(2) 2_676 ? Cs1 Cs1 5.380(3) 2_776 ? I1 Cs1 3.867(2) 1_545 ? I1 Cs1 3.9873(18) 2_665 ? O4 C4 1.223(3) . ? O4 Cs1 3.115(3) 2_665 ? O6 C6 1.218(4) . ? O6 Cs1 3.135(3) 2_676 ? N1 C6 1.374(4) . ? N1 C2 1.380(4) . ? N3 C4 1.365(4) . ? N3 C2 1.376(4) . ? O2 C2 1.206(4) . ? O2 Cs1 3.112(3) 2_666 ? O2 Cs1 3.452(3) 1_445 ? C4 C5 1.483(4) . ? C6 C5 1.481(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cs1 O2 104.68(8) 2_665 2_666 ? O4 Cs1 O6 137.91(6) 2_665 2_676 ? O2 Cs1 O6 73.55(8) 2_666 2_676 ? O4 Cs1 O6 145.48(6) 2_665 . ? O2 Cs1 O6 74.38(8) 2_666 . ? O6 Cs1 O6 75.87(7) 2_676 . ? O4 Cs1 O2 66.99(7) 2_665 1_665 ? O2 Cs1 O2 70.01(7) 2_666 1_665 ? O6 Cs1 O2 73.44(7) 2_676 1_665 ? O6 Cs1 O2 138.07(6) . 1_665 ? O4 Cs1 I1 81.44(5) 2_665 1_565 ? O2 Cs1 I1 137.06(4) 2_666 1_565 ? O6 Cs1 I1 74.34(6) 2_676 1_565 ? O6 Cs1 I1 123.41(5) . 1_565 ? O2 Cs1 I1 74.05(5) 1_665 1_565 ? O4 Cs1 I1 75.88(4) 2_665 . ? O2 Cs1 I1 72.23(5) 2_666 . ? O6 Cs1 I1 137.35(5) 2_676 . ? O6 Cs1 I1 71.02(5) . . ? O2 Cs1 I1 116.44(5) 1_665 . ? I1 Cs1 I1 147.47(3) 1_565 . ? O4 Cs1 I1 68.56(6) 2_665 2_665 ? O2 Cs1 I1 144.89(5) 2_666 2_665 ? O6 Cs1 I1 135.28(6) 2_676 2_665 ? O6 Cs1 I1 92.15(6) . 2_665 ? O2 Cs1 I1 129.78(4) 1_665 2_665 ? I1 Cs1 I1 77.43(3) 1_565 2_665 ? I1 Cs1 I1 72.738(12) . 2_665 ? O4 Cs1 Cs1 173.36(4) 2_665 2_676 ? O2 Cs1 Cs1 69.50(7) 2_666 2_676 ? O6 Cs1 Cs1 38.41(5) 2_676 2_676 ? O6 Cs1 Cs1 37.46(4) . 2_676 ? O2 Cs1 Cs1 107.33(6) 1_665 2_676 ? I1 Cs1 Cs1 100.57(3) 1_565 2_676 ? I1 Cs1 Cs1 104.649(9) . 2_676 ? I1 Cs1 Cs1 118.01(5) 2_665 2_676 ? O4 Cs1 Cs1 84.02(6) 2_665 2_776 ? O2 Cs1 Cs1 37.08(5) 2_666 2_776 ? O6 Cs1 Cs1 69.72(6) 2_676 2_776 ? O6 Cs1 Cs1 108.75(7) . 2_776 ? O2 Cs1 Cs1 32.93(4) 1_665 2_776 ? I1 Cs1 Cs1 104.31(2) 1_565 2_776 ? I1 Cs1 Cs1 96.264(10) . 2_776 ? I1 Cs1 Cs1 152.096(9) 2_665 2_776 ? Cs1 Cs1 Cs1 89.35(5) 2_676 2_776 ? Cs1 I1 Cs1 147.47(3) 1_545 . ? Cs1 I1 Cs1 102.57(3) 1_545 2_665 ? Cs1 I1 Cs1 107.262(12) . 2_665 ? C4 O4 Cs1 130.0(2) . 2_665 ? C6 O6 Cs1 136.0(2) . 2_676 ? C6 O6 Cs1 119.8(2) . . ? Cs1 O6 Cs1 104.13(7) 2_676 . ? C6 N1 C2 125.9(3) . . ? C4 N3 C2 125.7(3) . . ? C2 O2 Cs1 137.0(2) . 2_666 ? C2 O2 Cs1 112.9(2) . 1_445 ? Cs1 O2 Cs1 109.99(7) 2_666 1_445 ? O4 C4 N3 120.7(3) . . ? O4 C4 C5 122.4(3) . . ? N3 C4 C5 116.9(2) . . ? O6 C6 N1 120.9(3) . . ? O6 C6 C5 123.2(3) . . ? N1 C6 C5 115.8(3) . . ? C4 C5 C6 116.9(2) . . ? O2 C2 N1 122.5(3) . . ? O2 C2 N3 121.8(3) . . ? N1 C2 N3 115.7(3) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.378 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.112 # Attachment '- BA_KBr_2H2O.cif' data_pnma_centro _database_code_depnum_ccdc_archive 'CCDC 787493' #TrackingRef '- BA_KBr_2H2O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Br K N2 O5' _chemical_formula_weight 283.13 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' _symmetry_cell_setting Orthorombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 7.1114(3) _cell_length_b 8.1724(3) _cell_length_c 16.9065(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 982.56(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1602 _cell_measurement_theta_min 2.4048 _cell_measurement_theta_max 29.1011 _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 4.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62739 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3134 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 29.15 _reflns_number_total 1233 _reflns_number_gt 931 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0259P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1233 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0490 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _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 H200 H 0.337(3) 0.475(3) 0.4371(13) 0.039(7) Uiso 1 1 d . . . H100 H 0.331(4) 0.452(3) 0.7900(16) 0.056(10) Uiso 1 1 d . . . H101 H 0.432(5) 0.469(4) 0.734(2) 0.072(13) Uiso 1 1 d . . . C2 C 0.3514(4) 0.2500 0.4241(2) 0.0301(7) Uani 1 2 d S . . C4 C 0.2023(3) 0.4056(3) 0.53218(14) 0.0317(5) Uani 1 1 d . . . C5 C 0.1276(4) 0.2500 0.56594(19) 0.0348(8) Uani 1 2 d S . . H5A H -0.0079 0.2500 0.5594 0.042 Uiso 1 2 calc SR . . H5B H 0.1530 0.2500 0.6223 0.042 Uiso 1 2 calc SR . . N2 N 0.2992(3) 0.3924(2) 0.46277(11) 0.0320(5) Uani 1 1 d . . . O1 O 0.3913(3) 0.5192(2) 0.76570(13) 0.0467(5) Uani 1 1 d . . . O2 O 0.4353(3) 0.2500 0.36261(13) 0.0455(6) Uani 1 2 d S . . O4 O 0.1747(3) 0.53795(19) 0.56212(10) 0.0506(5) Uani 1 1 d . . . Br1 Br 0.39653(4) 0.7500 0.36368(2) 0.03472(13) Uani 1 2 d S . . K1 K 0.16740(10) 0.7500 0.68770(4) 0.03510(19) Uani 1 2 d S . . 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 C2 0.0282(18) 0.0297(16) 0.0325(18) 0.000 -0.0003(15) 0.000 C4 0.0307(13) 0.0318(12) 0.0326(13) -0.0020(10) -0.0016(11) 0.0032(10) C5 0.0298(18) 0.0417(18) 0.0331(18) 0.000 0.0068(16) 0.000 N2 0.0426(12) 0.0216(9) 0.0319(11) 0.0041(9) 0.0042(10) -0.0023(9) O1 0.0492(12) 0.0410(10) 0.0500(12) 0.0017(10) 0.0116(11) -0.0031(10) O2 0.0538(15) 0.0507(14) 0.0320(13) 0.000 0.0171(13) 0.000 O4 0.0701(12) 0.0323(9) 0.0494(11) -0.0152(8) 0.0043(10) 0.0067(8) Br1 0.0382(2) 0.02460(17) 0.0413(2) 0.000 0.00026(18) 0.000 K1 0.0414(4) 0.0310(4) 0.0330(4) 0.000 -0.0008(4) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 O2 1.198(4) . ? C2 N2 1.385(2) . ? C2 N2 1.385(2) 8_565 ? C4 O4 1.210(2) . ? C4 N2 1.365(3) . ? C4 C5 1.492(3) . ? C5 C4 1.492(3) 8_565 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N2 H200 0.84(2) . ? O1 K1 2.798(2) . ? O1 K1 2.834(2) 6_657 ? O1 H100 0.81(3) . ? O1 H101 0.73(3) . ? O2 K1 2.951(2) 5_666 ? O2 K1 3.046(2) 2_564 ? O4 K1 2.7411(17) . ? K1 O4 2.7411(17) 8_575 ? K1 O1 2.798(2) 8_575 ? K1 O1 2.834(2) 6_557 ? K1 O1 2.834(2) 3_466 ? K1 O2 2.951(2) 5_666 ? K1 O2 3.046(2) 2_565 ? K1 K1 4.1328(8) 6_657 ? K1 K1 4.1328(8) 6_557 ? K1 H101 3.07(3) . ? 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 O2 C2 N2 122.86(14) . . ? O2 C2 N2 122.86(14) . 8_565 ? N2 C2 N2 114.3(3) . 8_565 ? O4 C4 N2 120.8(2) . . ? O4 C4 C5 123.0(2) . . ? N2 C4 C5 116.17(19) . . ? C4 C5 C4 117.0(3) . 8_565 ? C4 C5 H5A 108.1 . . ? C4 C5 H5A 108.1 8_565 . ? C4 C5 H5B 108.1 . . ? C4 C5 H5B 108.1 8_565 . ? H5A C5 H5B 107.3 . . ? C4 N2 C2 127.4(2) . . ? C4 N2 H200 122.6(16) . . ? C2 N2 H200 110.0(16) . . ? K1 O1 K1 94.40(6) . 6_657 ? K1 O1 H100 113.2(19) . . ? K1 O1 H100 132.7(19) 6_657 . ? K1 O1 H101 105(3) . . ? K1 O1 H101 108(3) 6_657 . ? H100 O1 H101 101(3) . . ? C2 O2 K1 136.6(2) . 5_666 ? C2 O2 K1 136.3(2) . 2_564 ? K1 O2 K1 87.11(6) 5_666 2_564 ? C4 O4 K1 153.14(15) . . ? O4 K1 O4 78.42(7) . 8_575 ? O4 K1 O1 141.29(7) . 8_575 ? O4 K1 O1 85.88(6) 8_575 8_575 ? O4 K1 O1 85.88(6) . . ? O4 K1 O1 141.29(7) 8_575 . ? O1 K1 O1 84.75(8) 8_575 . ? O4 K1 O1 78.92(6) . 6_557 ? O4 K1 O1 130.47(7) 8_575 6_557 ? O1 K1 O1 135.37(4) 8_575 6_557 ? O1 K1 O1 79.32(5) . 6_557 ? O4 K1 O1 130.47(7) . 3_466 ? O4 K1 O1 78.92(6) 8_575 3_466 ? O1 K1 O1 79.32(5) 8_575 3_466 ? O1 K1 O1 135.37(4) . 3_466 ? O1 K1 O1 83.43(8) 6_557 3_466 ? O4 K1 O2 76.03(6) . 5_666 ? O4 K1 O2 76.03(6) 8_575 5_666 ? O1 K1 O2 65.86(6) 8_575 5_666 ? O1 K1 O2 65.86(6) . 5_666 ? O1 K1 O2 138.03(4) 6_557 5_666 ? O1 K1 O2 138.03(4) 3_466 5_666 ? O4 K1 O2 139.16(4) . 2_565 ? O4 K1 O2 139.16(4) 8_575 2_565 ? O1 K1 O2 71.27(6) 8_575 2_565 ? O1 K1 O2 71.27(6) . 2_565 ? O1 K1 O2 64.16(5) 6_557 2_565 ? O1 K1 O2 64.16(5) 3_466 2_565 ? O2 K1 O2 120.62(7) 5_666 2_565 ? O4 K1 K1 112.24(4) . 6_657 ? O4 K1 K1 112.24(4) 8_575 6_657 ? O1 K1 K1 43.14(4) 8_575 6_657 ? O1 K1 K1 43.14(4) . 6_657 ? O1 K1 K1 117.03(5) 6_557 6_657 ? O1 K1 K1 117.02(5) 3_466 6_657 ? O2 K1 K1 47.40(4) 5_666 6_657 ? O2 K1 K1 73.22(5) 2_565 6_657 ? O4 K1 K1 114.27(4) . 6_557 ? O4 K1 K1 114.27(4) 8_575 6_557 ? O1 K1 K1 104.44(5) 8_575 6_557 ? O1 K1 K1 104.44(5) . 6_557 ? O1 K1 K1 42.46(4) 6_557 6_557 ? O1 K1 K1 42.46(4) 3_466 6_557 ? O2 K1 K1 166.11(6) 5_666 6_557 ? O2 K1 K1 45.49(5) 2_565 6_557 ? K1 K1 K1 118.71(3) 6_657 6_557 ? O4 K1 H101 73.4(6) . . ? O4 K1 H101 131.3(6) 8_575 . ? O1 K1 H101 92.0(6) 8_575 . ? O1 K1 H101 13.2(6) . . ? O1 K1 H101 81.6(6) 6_557 . ? O1 K1 H101 148.2(6) 3_466 . ? O2 K1 H101 59.2(6) 5_666 . ? O2 K1 H101 84.1(6) 2_565 . ? K1 K1 H101 48.9(6) 6_657 . ? K1 K1 H101 113.3(6) 6_557 . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.368 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.066 # Attachment '- BA_NaBr_2H2O.cif' data_new _database_code_depnum_ccdc_archive 'CCDC 787494' #TrackingRef '- BA_NaBr_2H2O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Br N2 Na O5' _chemical_formula_weight 267.02 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' Br Br -0.2901 2.4595 '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' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 7.1308(3) _cell_length_b 7.8805(3) _cell_length_c 16.0515(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 902.00(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1391 _cell_measurement_theta_min 2.5327 _cell_measurement_theta_max 28.7304 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 4.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.39871 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2595 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.79 _reflns_number_total 1110 _reflns_number_gt 833 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0390P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0273(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1110 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 O1 O 0.6267(4) 0.5552(3) 0.75719(16) 0.0416(6) Uani 1 1 d . . . O4 O 0.1574(3) 0.4506(3) 0.42291(15) 0.0502(6) Uani 1 1 d . . . H300 H 0.319(4) 0.515(3) 0.5534(18) 0.024(7) Uiso 1 1 d . . . H100 H 0.563(6) 0.501(5) 0.729(3) 0.075(17) Uiso 1 1 d . . . H101 H 0.682(7) 0.472(6) 0.781(3) 0.082(17) Uiso 1 1 d . . . Br1 Br 0.60915(5) 0.7500 0.35670(3) 0.03112(19) Uani 1 2 d S . . Na1 Na 0.8604(3) 0.7500 0.69626(12) 0.0461(5) Uani 1 2 d S . . O2 O 0.4260(5) 0.7500 0.63009(18) 0.0476(9) Uani 1 2 d S . . C5 C 0.1207(6) 0.7500 0.4152(3) 0.0350(10) Uani 1 2 d S . . H5A H 0.1531 0.7500 0.3565 0.042 Uiso 1 2 calc SR . . H5B H -0.0151 0.7500 0.4188 0.042 Uiso 1 2 calc SR . . C2 C 0.3402(5) 0.7500 0.5645(3) 0.0290(9) Uani 1 2 d S . . N3 N 0.2887(3) 0.6017(3) 0.52515(15) 0.0313(6) Uani 1 1 d . . . C4 C 0.1904(4) 0.5882(3) 0.45232(18) 0.0300(6) 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 O1 0.0454(14) 0.0401(13) 0.0393(13) -0.0004(12) -0.0114(13) -0.0023(12) O4 0.0677(16) 0.0335(12) 0.0494(14) -0.0118(11) -0.0028(14) -0.0081(11) Br1 0.0324(3) 0.0241(2) 0.0368(3) 0.000 -0.0015(2) 0.000 Na1 0.0536(12) 0.0322(9) 0.0524(11) 0.000 0.0145(10) 0.000 O2 0.056(2) 0.054(2) 0.0332(17) 0.000 -0.0199(16) 0.000 C5 0.031(2) 0.039(2) 0.035(2) 0.000 -0.005(2) 0.000 C2 0.027(2) 0.033(2) 0.028(2) 0.000 0.000(2) 0.000 N3 0.0382(15) 0.0227(12) 0.0328(14) 0.0050(12) -0.0003(13) 0.0025(11) C4 0.0296(14) 0.0306(15) 0.0299(15) -0.0022(14) 0.0045(14) -0.0024(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 Na1 2.468(3) . ? O1 Na1 2.554(3) 6_557 ? O1 H100 0.77(5) . ? O1 H101 0.85(5) . ? O4 C4 1.206(3) . ? O4 Na1 2.485(3) 5_666 ? Na1 O1 2.468(3) 8_575 ? Na1 O4 2.485(3) 5_666 ? Na1 O4 2.485(3) 4_656 ? Na1 O1 2.554(3) 3_566 ? Na1 O1 2.554(3) 6_657 ? Na1 O2 2.826(4) 6_657 ? Na1 Na1 3.9609(17) 6_657 ? Na1 Na1 3.9609(17) 6_557 ? O2 C2 1.217(5) . ? O2 Na1 2.826(4) 6_557 ? C5 C4 1.492(3) 8_575 ? C5 C4 1.492(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C2 N3 1.379(3) . ? C2 N3 1.379(3) 8_575 ? N3 C4 1.367(4) . ? N3 H300 0.85(3) . ? 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 Na1 O1 Na1 104.13(10) . 6_557 ? Na1 O1 H100 121(3) . . ? Na1 O1 H100 94(3) 6_557 . ? Na1 O1 H101 110(3) . . ? Na1 O1 H101 132(3) 6_557 . ? H100 O1 H101 96(4) . . ? C4 O4 Na1 152.1(2) . 5_666 ? O1 Na1 O1 76.93(13) . 8_575 ? O1 Na1 O4 82.81(9) . 5_666 ? O1 Na1 O4 131.78(12) 8_575 5_666 ? O1 Na1 O4 131.78(12) . 4_656 ? O1 Na1 O4 82.81(9) 8_575 4_656 ? O4 Na1 O4 79.02(12) 5_666 4_656 ? O1 Na1 O1 139.48(9) . 3_566 ? O1 Na1 O1 90.70(8) 8_575 3_566 ? O4 Na1 O1 130.22(11) 5_666 3_566 ? O4 Na1 O1 83.16(9) 4_656 3_566 ? O1 Na1 O1 90.70(8) . 6_657 ? O1 Na1 O1 139.48(9) 8_575 6_657 ? O4 Na1 O1 83.16(9) 5_666 6_657 ? O4 Na1 O1 130.22(11) 4_656 6_657 ? O1 Na1 O1 73.91(12) 3_566 6_657 ? O1 Na1 O2 73.80(10) . 6_657 ? O1 Na1 O2 73.80(10) 8_575 6_657 ? O4 Na1 O2 140.15(6) 5_666 6_657 ? O4 Na1 O2 140.15(6) 4_656 6_657 ? O1 Na1 O2 65.69(9) 3_566 6_657 ? O1 Na1 O2 65.69(9) 6_657 6_657 ? O1 Na1 Na1 115.80(10) . 6_657 ? O1 Na1 Na1 115.80(10) 8_575 6_657 ? O4 Na1 Na1 112.42(7) 5_666 6_657 ? O4 Na1 Na1 112.42(7) 4_656 6_657 ? O1 Na1 Na1 37.17(6) 3_566 6_657 ? O1 Na1 Na1 37.17(6) 6_657 6_657 ? O2 Na1 Na1 54.65(9) 6_657 6_657 ? O1 Na1 Na1 38.69(7) . 6_557 ? O1 Na1 Na1 38.69(7) 8_575 6_557 ? O4 Na1 Na1 106.81(8) 5_666 6_557 ? O4 Na1 Na1 106.81(8) 4_656 6_557 ? O1 Na1 Na1 122.81(9) 3_566 6_557 ? O1 Na1 Na1 122.81(9) 6_657 6_557 ? O2 Na1 Na1 73.71(9) 6_657 6_557 ? Na1 Na1 Na1 128.36(10) 6_657 6_557 ? C2 O2 Na1 140.3(3) . 6_557 ? C4 C5 C4 117.4(3) 8_575 . ? C4 C5 H5A 108.0 8_575 . ? C4 C5 H5A 108.0 . . ? C4 C5 H5B 108.0 8_575 . ? C4 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? O2 C2 N3 122.04(17) . . ? O2 C2 N3 122.04(17) . 8_575 ? N3 C2 N3 115.9(3) . 8_575 ? C4 N3 C2 126.5(3) . . ? C4 N3 H300 121.7(19) . . ? C2 N3 H300 111.7(19) . . ? O4 C4 N3 120.3(3) . . ? O4 C4 C5 123.2(3) . . ? N3 C4 C5 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.102 # Attachment '- BA_RbBr.cif' data_acbarb_rbbr_d_raccolta _database_code_depnum_ccdc_archive 'CCDC 787495' #TrackingRef '- BA_RbBr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Br N2 O3 Rb' _chemical_formula_weight 293.47 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 8.984(5) _cell_length_b 8.756(5) _cell_length_c 10.296(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.949(5) _cell_angle_gamma 90.00 _cell_volume 808.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1644 _cell_measurement_theta_min 2.9382 _cell_measurement_theta_max 29.2875 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 11.021 _exptl_absorpt_correction_T_min 0.26022 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3512 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 29.30 _reflns_number_total 1843 _reflns_number_gt 1198 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0688P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1843 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 Rb1 Rb 0.21903(7) -0.11084(9) 0.37552(7) 0.0374(2) Uani 1 1 d . . . Br1 Br 0.48218(7) 0.17312(9) 0.35773(7) 0.0392(2) Uani 1 1 d . . . O2 O 0.1679(5) 0.6066(6) 0.5193(5) 0.0458(14) Uani 1 1 d . . . O4 O 0.5625(5) 0.3594(6) 0.7073(5) 0.0495(14) Uani 1 1 d . . . O5 O 0.1246(5) 0.0986(6) 0.5792(5) 0.0494(14) Uani 1 1 d . . . N3 N 0.3662(6) 0.4815(8) 0.6124(6) 0.0336(14) Uani 1 1 d . . . C6 C 0.1995(7) 0.2157(9) 0.5940(6) 0.0333(17) Uani 1 1 d . . . C4 C 0.4347(7) 0.3549(9) 0.6659(6) 0.0339(17) Uani 1 1 d . . . C2 C 0.2261(7) 0.4873(9) 0.5546(6) 0.0308(16) Uani 1 1 d . . . C5 C 0.3404(7) 0.2181(8) 0.6715(7) 0.0327(16) Uani 1 1 d . . . H5A H 0.3990 0.1313 0.6454 0.039 Uiso 1 1 calc R . . H5B H 0.3181 0.2020 0.7617 0.039 Uiso 1 1 calc R . . N1 N 0.1507(7) 0.3526(8) 0.5417(6) 0.0381(16) Uani 1 1 d . . . H300 H 0.404(7) 0.566(8) 0.609(6) 0.018(17) Uiso 1 1 d . . . H100 H 0.070(9) 0.355(10) 0.533(8) 0.06(3) Uiso 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 Rb1 0.0333(4) 0.0309(4) 0.0476(4) -0.0006(4) -0.0042(3) -0.0029(3) Br1 0.0383(4) 0.0338(5) 0.0450(4) 0.0069(4) -0.0040(3) -0.0069(3) O2 0.043(3) 0.034(3) 0.058(3) 0.009(3) -0.020(2) -0.003(2) O4 0.029(3) 0.052(4) 0.066(3) -0.011(3) -0.018(2) 0.006(2) O5 0.045(3) 0.040(4) 0.064(3) -0.011(3) 0.011(3) -0.015(2) N3 0.030(3) 0.026(4) 0.044(4) -0.003(3) -0.006(3) -0.003(3) C6 0.034(4) 0.039(5) 0.027(3) -0.012(3) 0.000(3) -0.009(3) C4 0.025(3) 0.038(5) 0.039(4) -0.007(3) 0.000(3) 0.003(3) C2 0.026(3) 0.039(5) 0.026(3) -0.003(3) -0.005(3) -0.006(3) C5 0.029(3) 0.030(4) 0.038(4) -0.001(3) -0.003(3) -0.001(3) N1 0.025(3) 0.037(4) 0.051(4) 0.005(3) -0.008(3) 0.000(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Rb1 O2 2.931(6) 1_545 ? Rb1 O5 2.943(5) . ? Rb1 O4 3.080(5) 3_656 ? Rb1 O4 3.094(5) 4_565 ? Rb1 O5 3.148(5) 3_556 ? Rb1 Br1 3.4422(17) . ? Rb1 Br1 3.4881(15) 2_545 ? Rb1 C6 3.648(7) . ? Rb1 Br1 3.7799(17) 3_656 ? Rb1 Rb1 5.129(2) 2_545 ? Rb1 Rb1 5.129(2) 2 ? Rb1 Rb1 5.183(2) 3_556 ? Br1 Rb1 3.4881(15) 2 ? Br1 Rb1 3.7799(17) 3_656 ? O2 C2 1.215(9) . ? O2 Rb1 2.931(6) 1_565 ? O4 C4 1.205(7) . ? O4 Rb1 3.080(5) 3_656 ? O4 Rb1 3.094(5) 4_666 ? O5 C6 1.232(8) . ? O5 Rb1 3.148(5) 3_556 ? N3 C2 1.365(8) . ? N3 C4 1.370(9) . ? C6 N1 1.376(10) . ? C6 C5 1.462(9) . ? C4 C5 1.471(9) . ? C2 N1 1.363(9) . ? 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 O2 Rb1 O5 96.20(16) 1_545 . ? O2 Rb1 O4 70.24(15) 1_545 3_656 ? O5 Rb1 O4 148.05(14) . 3_656 ? O2 Rb1 O4 143.59(13) 1_545 4_565 ? O5 Rb1 O4 79.41(16) . 4_565 ? O4 Rb1 O4 128.72(6) 3_656 4_565 ? O2 Rb1 O5 76.92(14) 1_545 3_556 ? O5 Rb1 O5 63.42(16) . 3_556 ? O4 Rb1 O5 135.14(14) 3_656 3_556 ? O4 Rb1 O5 68.77(14) 4_565 3_556 ? O2 Rb1 Br1 139.67(10) 1_545 . ? O5 Rb1 Br1 79.14(10) . . ? O4 Rb1 Br1 92.66(11) 3_656 . ? O4 Rb1 Br1 75.51(10) 4_565 . ? O5 Rb1 Br1 131.67(10) 3_556 . ? O2 Rb1 Br1 78.51(11) 1_545 2_545 ? O5 Rb1 Br1 132.09(10) . 2_545 ? O4 Rb1 Br1 75.01(9) 3_656 2_545 ? O4 Rb1 Br1 78.23(11) 4_565 2_545 ? O5 Rb1 Br1 69.08(10) 3_556 2_545 ? Br1 Rb1 Br1 133.48(3) . 2_545 ? O2 Rb1 C6 109.67(16) 1_545 . ? O5 Rb1 C6 17.73(13) . . ? O4 Rb1 C6 140.90(14) 3_656 . ? O4 Rb1 C6 75.67(16) 4_565 . ? O5 Rb1 C6 78.66(14) 3_556 . ? Br1 Rb1 C6 61.42(11) . . ? Br1 Rb1 C6 144.09(11) 2_545 . ? O2 Rb1 Br1 68.60(10) 1_545 3_656 ? O5 Rb1 Br1 78.00(11) . 3_656 ? O4 Rb1 Br1 70.14(9) 3_656 3_656 ? O4 Rb1 Br1 142.63(10) 4_565 3_656 ? O5 Rb1 Br1 124.23(11) 3_556 3_656 ? Br1 Rb1 Br1 71.27(4) . 3_656 ? Br1 Rb1 Br1 138.20(3) 2_545 3_656 ? C6 Rb1 Br1 73.74(11) . 3_656 ? O2 Rb1 Rb1 63.75(11) 1_545 2_545 ? O5 Rb1 Rb1 159.01(10) . 2_545 ? O4 Rb1 Rb1 33.92(9) 3_656 2_545 ? O4 Rb1 Rb1 112.53(11) 4_565 2_545 ? O5 Rb1 Rb1 103.67(10) 3_556 2_545 ? Br1 Rb1 Rb1 119.81(4) . 2_545 ? Br1 Rb1 Rb1 41.92(2) 2_545 2_545 ? C6 Rb1 Rb1 171.79(12) . 2_545 ? Br1 Rb1 Rb1 98.72(3) 3_656 2_545 ? O2 Rb1 Rb1 177.19(10) 1_545 2 ? O5 Rb1 Rb1 82.52(11) . 2 ? O4 Rb1 Rb1 112.11(12) 3_656 2 ? O4 Rb1 Rb1 33.74(9) 4_565 2 ? O5 Rb1 Rb1 100.27(10) 3_556 2 ? Br1 Rb1 Rb1 42.61(2) . 2 ? Br1 Rb1 Rb1 100.47(4) 2_545 2 ? C6 Rb1 Rb1 69.61(12) . 2 ? Br1 Rb1 Rb1 113.45(3) 3_656 2 ? Rb1 Rb1 Rb1 117.21(5) 2_545 2 ? O2 Rb1 Rb1 85.63(11) 1_545 3_556 ? O5 Rb1 Rb1 32.90(10) . 3_556 ? O4 Rb1 Rb1 155.83(11) 3_656 3_556 ? O4 Rb1 Rb1 71.07(11) 4_565 3_556 ? O5 Rb1 Rb1 30.52(10) 3_556 3_556 ? Br1 Rb1 Rb1 107.27(4) . 3_556 ? Br1 Rb1 Rb1 99.43(4) 2_545 3_556 ? C6 Rb1 Rb1 48.67(10) . 3_556 ? Br1 Rb1 Rb1 102.92(4) 3_656 3_556 ? Rb1 Rb1 Rb1 132.35(3) 2_545 3_556 ? Rb1 Rb1 Rb1 91.97(3) 2 3_556 ? Rb1 Br1 Rb1 95.47(4) . 2 ? Rb1 Br1 Rb1 108.73(4) . 3_656 ? Rb1 Br1 Rb1 154.42(3) 2 3_656 ? C2 O2 Rb1 143.2(5) . 1_565 ? C4 O4 Rb1 119.2(5) . 3_656 ? C4 O4 Rb1 128.2(5) . 4_666 ? Rb1 O4 Rb1 112.33(14) 3_656 4_666 ? C6 O5 Rb1 115.6(4) . . ? C6 O5 Rb1 119.1(5) . 3_556 ? Rb1 O5 Rb1 116.58(16) . 3_556 ? C2 N3 C4 126.2(6) . . ? O5 C6 N1 121.1(7) . . ? O5 C6 C5 122.1(7) . . ? N1 C6 C5 116.8(6) . . ? O5 C6 Rb1 46.7(3) . . ? N1 C6 Rb1 117.8(4) . . ? C5 C6 Rb1 106.3(4) . . ? O4 C4 N3 121.1(7) . . ? O4 C4 C5 123.6(7) . . ? N3 C4 C5 115.3(6) . . ? O2 C2 N1 120.7(6) . . ? O2 C2 N3 122.3(7) . . ? N1 C2 N3 116.9(7) . . ? C6 C5 C4 118.3(6) . . ? C2 N1 C6 124.7(6) . . ? _diffrn_measured_fraction_theta_max 0.834 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.358 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.198 # Attachment '- BA_RbBr_2H2O.cif' data_acbarb_rbbr_dd _database_code_depnum_ccdc_archive 'CCDC 787496' #TrackingRef '- BA_RbBr_2H2O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Br N2 O5 Rb' _chemical_formula_weight 329.50 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 7.223(2) _cell_length_b 8.3270(10) _cell_length_c 17.384(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1045.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 185 _cell_measurement_theta_min 2.4215 _cell_measurement_theta_max 28.8968 _cell_oxdiff_measurement_reflns_used 185 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 8.551 _exptl_absorpt_correction_T_min 0.06932 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2641 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 29.30 _reflns_number_total 1258 _reflns_number_gt 849 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0371P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1258 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _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 Rb1 Rb 0.33508(9) -0.2500 0.68652(3) 0.03560(18) Uani 1 2 d S . . Br1 Br -0.10006(9) 0.2500 0.63280(3) 0.03502(18) Uani 1 2 d S . . C5 C 0.3731(8) 0.2500 0.5599(3) 0.0352(14) Uani 1 2 d S . . H5A H 0.5058 0.2500 0.5513 0.042 Uiso 1 2 calc SR . . H5B H 0.3536 0.2500 0.6151 0.042 Uiso 1 2 calc SR . . O1 O 0.1075(5) -0.0019(4) 0.7654(2) 0.0513(10) Uani 1 1 d . . . O2 O 0.0702(6) 0.2500 0.3614(2) 0.0439(11) Uani 1 2 d S . . O4 O 0.3217(5) -0.0352(3) 0.55737(17) 0.0527(9) Uani 1 1 d . . . N3 N 0.2012(5) 0.1097(4) 0.45958(18) 0.0314(9) Uani 1 1 d . . . C4 C 0.2966(6) 0.0951(5) 0.5283(2) 0.0348(10) Uani 1 1 d . . . C2 C 0.1522(8) 0.2500 0.4224(3) 0.0299(13) Uani 1 2 d S . . H101 H 0.154(7) 0.052(5) 0.791(2) 0.043(17) Uiso 1 1 d . . . H300 H 0.177(7) 0.031(5) 0.436(2) 0.048(14) Uiso 1 1 d . . . H100 H 0.074(11) 0.053(8) 0.721(3) 0.13(3) Uiso 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 Rb1 0.0410(4) 0.0347(3) 0.0312(3) 0.000 -0.0014(3) 0.000 Br1 0.0385(4) 0.0257(3) 0.0409(3) 0.000 0.0000(3) 0.000 C5 0.032(4) 0.044(3) 0.030(3) 0.000 -0.006(2) 0.000 O1 0.057(3) 0.0435(19) 0.053(2) -0.0026(19) -0.0167(19) -0.0060(17) O2 0.049(3) 0.053(2) 0.030(2) 0.000 -0.012(2) 0.000 O4 0.074(3) 0.0347(17) 0.0496(18) 0.0194(15) -0.0055(16) 0.0054(16) N3 0.044(3) 0.0221(18) 0.0278(19) -0.0046(15) -0.0050(16) -0.0015(15) C4 0.035(3) 0.038(2) 0.031(2) -0.0018(18) 0.0043(18) 0.0067(19) C2 0.033(4) 0.030(3) 0.027(3) 0.000 -0.002(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Rb1 O4 2.872(3) 8 ? Rb1 O4 2.872(3) . ? Rb1 O1 2.973(4) 6_657 ? Rb1 O1 2.973(4) 3_546 ? Rb1 O1 2.975(4) 8 ? Rb1 O1 2.975(4) . ? Rb1 O2 3.043(4) 5_556 ? Rb1 O2 3.116(4) 2 ? Rb1 Rb1 4.2325(10) 6_657 ? Rb1 Rb1 4.2325(10) 6_557 ? C5 C4 1.507(5) . ? C5 C4 1.507(5) 8_565 ? O1 Rb1 2.973(4) 6_557 ? O2 C2 1.215(6) . ? O2 Rb1 3.043(4) 5_556 ? O2 Rb1 3.116(4) 2_554 ? O4 C4 1.211(5) . ? N3 C2 1.381(4) . ? N3 C4 1.385(5) . ? C2 N3 1.381(4) 8_565 ? 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 Rb1 O4 77.03(12) 8 . ? O4 Rb1 O1 132.43(10) 8 6_657 ? O4 Rb1 O1 79.00(10) . 6_657 ? O4 Rb1 O1 79.00(10) 8 3_546 ? O4 Rb1 O1 132.43(10) . 3_546 ? O1 Rb1 O1 88.05(14) 6_657 3_546 ? O4 Rb1 O1 84.80(9) 8 8 ? O4 Rb1 O1 140.73(11) . 8 ? O1 Rb1 O1 135.95(5) 6_657 8 ? O1 Rb1 O1 75.73(7) 3_546 8 ? O4 Rb1 O1 140.73(11) 8 . ? O4 Rb1 O1 84.80(9) . . ? O1 Rb1 O1 75.73(7) 6_657 . ? O1 Rb1 O1 135.95(5) 3_546 . ? O1 Rb1 O1 87.96(14) 8 . ? O4 Rb1 O2 75.74(9) 8 5_556 ? O4 Rb1 O2 75.74(9) . 5_556 ? O1 Rb1 O2 135.52(7) 6_657 5_556 ? O1 Rb1 O2 135.52(7) 3_546 5_556 ? O1 Rb1 O2 66.09(9) 8 5_556 ? O1 Rb1 O2 66.09(9) . 5_556 ? O4 Rb1 O2 140.36(6) 8 2 ? O4 Rb1 O2 140.36(6) . 2 ? O1 Rb1 O2 65.20(9) 6_657 2 ? O1 Rb1 O2 65.20(9) 3_546 2 ? O1 Rb1 O2 70.82(9) 8 2 ? O1 Rb1 O2 70.82(9) . 2 ? O2 Rb1 O2 118.56(12) 5_556 2 ? O4 Rb1 Rb1 115.88(7) 8 6_657 ? O4 Rb1 Rb1 115.88(7) . 6_657 ? O1 Rb1 Rb1 44.66(7) 6_657 6_657 ? O1 Rb1 Rb1 44.66(7) 3_546 6_657 ? O1 Rb1 Rb1 103.36(8) 8 6_657 ? O1 Rb1 Rb1 103.36(8) . 6_657 ? O2 Rb1 Rb1 164.44(7) 5_556 6_657 ? O2 Rb1 Rb1 45.88(8) 2 6_657 ? O4 Rb1 Rb1 112.26(7) 8 6_557 ? O4 Rb1 Rb1 112.26(7) . 6_557 ? O1 Rb1 Rb1 114.72(8) 6_657 6_557 ? O1 Rb1 Rb1 114.72(8) 3_546 6_557 ? O1 Rb1 Rb1 44.62(7) 8 6_557 ? O1 Rb1 Rb1 44.62(7) . 6_557 ? O2 Rb1 Rb1 47.31(7) 5_556 6_557 ? O2 Rb1 Rb1 71.26(8) 2 6_557 ? Rb1 Rb1 Rb1 117.14(3) 6_657 6_557 ? C4 C5 C4 117.7(5) . 8_565 ? Rb1 O1 Rb1 90.72(9) 6_557 . ? C2 O2 Rb1 135.0(4) . 5_556 ? C2 O2 Rb1 138.2(4) . 2_554 ? Rb1 O2 Rb1 86.81(9) 5_556 2_554 ? C4 O4 Rb1 152.8(3) . . ? C2 N3 C4 127.3(4) . . ? O4 C4 N3 120.9(4) . . ? O4 C4 C5 124.1(4) . . ? N3 C4 C5 114.9(3) . . ? O2 C2 N3 122.2(2) . 8_565 ? O2 C2 N3 122.2(2) . . ? N3 C2 N3 115.5(5) 8_565 . ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.527 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.147