#------------------------------------------------------------------------------ #$Date: 2023-03-14 03:09:47 +0000 (Tue, 14 Mar 2023) $ #$Revision: 281859 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244219.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2244219 loop_ _publ_author_name 'Clulow, Rebecca' 'Lightfoot, Philip' _publ_section_title ; Syntheses and crystal structures of three novel oxalate coordination compounds: Rb~2~Co(C~2~O~4~)~2~·4H~2~O, Rb~2~CoCl~2~(C~2~O~4~) and K~2~Li~2~Cu(C~2~O~4~)~3~·2H~2~O ; _journal_coeditor_code WM5668 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989023001822 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'Rb2 [Co (C2 O4)2 (H2 O)2], 2H2 O' _chemical_formula_moiety 'Rb2 Co1 C4 O12 H8' _chemical_formula_sum 'C4 H8 Co O12 Rb2' _chemical_formula_weight 477.97 _chemical_name_common ; Dirubidium cobalt(II) bis(oxalate) tetrahydrate ; _chemical_name_systematic ; Dirubidium diaquadioxalatocobalt(II) dihydrate ; _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 102.836(8) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.8434(5) _cell_length_b 7.0795(4) _cell_length_c 10.9133(7) _cell_measurement_reflns_used 935 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 1.9 _cell_volume 590.84(7) _computing_cell_refinement ; CrystalClear (Rigaku, 2015) ; _computing_data_collection ; CrystalClear (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear (Rigaku, 2015) ; _computing_molecular_graphics ; Ortep for Windows (Farrugia, 2012) ; _computing_publication_material ; WinGX (Farrugia, 2012) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 13.6612 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Rigaku Mercury2 (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_unetI/netI 0.0282 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5799 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.531 _diffrn_reflns_theta_min 2.915 _diffrn_source 'Sealed Tube' _exptl_absorpt_coefficient_mu 9.698 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 458 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.647 _refine_diff_density_min -0.642 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 1343 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.974 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0206 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0496 _reflns_number_gt 1169 _reflns_number_total 1343 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5668sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2244219 _shelx_hkl_file ; 0 0 -1 1.23 3.09 0 0 1 0.35 4.11 0 0 1 0.85 3.62 0 0 -1 3.88 3.78 0 0 1 3.61 7.08 0 0 -1 5.91 8.54 0 0 2 518.65 19.12 0 0 2 488.26 20.17 0 0 -2 471.92 22.18 0 0 3 0.85 3.94 0 0 3 -1.97 4.21 0 0 -3 -1.78 7.28 0 0 4 1470.75 47.75 0 0 4 1297.75 44.71 0 0 -4 1361.06 49.22 0 0 5 1.27 4.65 0 0 5 0.66 4.30 0 0 -5 -0.87 9.18 0 0 6 -1.46 4.37 0 0 6 2.59 6.09 0 0 -6 2.15 11.05 0 0 7 2.95 6.82 0 0 7 0.64 6.14 0 0 -7 8.30 13.37 0 0 8 6281.86 148.86 0 0 8 6492.66 155.45 0 0 -8 6713.19 151.20 0 0 9 0.94 7.27 0 0 9 3.12 8.06 0 0 -9 12.92 17.22 0 0 10 1220.04 53.66 0 0 10 1156.72 56.68 0 0 -10 1352.52 64.55 0 0 11 8.03 8.83 0 0 -11 23.40 24.86 0 0 12 120.70 9.62 0 0 -12 135.02 23.73 0 0 -13 -16.55 27.28 0 -1 0 2.76 7.19 0 1 0 4.58 8.99 0 1 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6 0 26.10 15.67 -7 6 0 7.87 21.96 -7 -6 -1 945.49 37.07 7 6 1 839.89 35.64 -7 6 -1 890.95 32.99 -7 -6 -2 13.33 18.21 7 6 2 7.98 17.56 -7 6 -2 3.73 26.86 -8 0 11 -3.22 23.52 -8 0 10 53.58 20.81 -8 0 9 0.02 15.13 8 0 -9 -7.83 16.76 -8 0 8 671.46 25.65 8 0 -8 615.39 22.77 -8 0 7 -6.52 15.86 8 0 -7 -12.15 14.55 -8 0 6 135.55 15.86 -8 0 6 178.78 22.73 8 0 -6 153.61 15.01 -8 0 5 -0.81 12.21 -8 0 5 -23.37 16.76 8 0 -5 -7.47 10.10 -8 0 4 2612.82 93.42 -8 0 4 2681.96 103.20 8 0 -4 2676.85 97.22 -8 0 3 -0.82 10.53 8 0 -3 -9.72 15.39 8 0 -3 1.23 8.87 -8 0 2 785.56 31.68 8 0 -2 895.93 39.00 8 0 -2 835.32 33.33 -8 0 1 6.43 15.13 8 0 -1 -4.51 17.38 -8 0 1 7.91 13.43 -8 0 0 252.58 18.76 8 0 0 254.28 17.51 -8 0 0 273.11 21.33 -8 0 -1 -7.35 10.50 8 0 1 2.85 11.07 -8 0 -1 -7.10 15.30 -8 0 -2 65.94 11.60 8 0 2 50.54 13.31 -8 0 -2 53.44 18.30 -8 0 -3 -0.68 17.80 -8 0 -3 -8.32 17.17 8 0 4 1241.87 65.90 8 0 5 -0.28 9.92 8 0 6 311.90 15.88 -8 -1 10 701.39 30.65 -8 1 10 753.24 30.99 8 -1 -10 573.49 28.25 -8 -1 9 403.26 30.96 -8 1 9 391.52 27.29 8 -1 -9 344.88 26.20 -8 -1 8 7.24 15.97 -8 1 8 29.23 18.67 8 -1 -8 1.40 16.42 -8 -1 7 565.13 25.15 -8 -1 7 611.37 27.69 -8 1 7 707.16 27.75 8 -1 -7 625.50 22.16 -8 -1 6 666.45 28.19 -8 1 6 763.32 29.81 8 1 -6 815.84 31.42 8 -1 -6 749.62 28.65 -8 1 5 -5.15 11.88 -8 -1 5 4.00 16.52 -8 1 5 3.43 14.38 8 1 -5 2.63 21.63 8 -1 -5 7.57 10.58 -8 1 4 12.12 12.56 -8 -1 4 17.97 13.39 -8 1 4 32.40 18.77 8 1 -4 29.61 12.07 8 -1 -4 14.10 11.12 -8 1 3 8.41 10.96 -8 -1 3 5.72 13.73 -8 1 3 4.78 15.47 8 1 -3 -27.45 15.91 8 -1 -3 0.66 10.51 -8 1 2 1356.33 50.78 -8 -1 2 1368.57 52.31 -8 1 2 1359.70 59.73 8 1 -2 1491.23 55.76 8 -1 -2 1575.15 58.86 -8 1 1 909.97 37.47 -8 -1 1 950.54 38.40 8 1 -1 1065.65 44.18 8 -1 -1 1016.37 41.68 -8 1 1 1150.69 49.78 -8 1 0 29.37 16.40 -8 -1 0 37.23 12.95 8 1 0 18.06 15.62 8 -1 0 22.37 14.42 -8 1 0 22.01 12.76 -8 1 -1 886.36 32.28 -8 -1 -1 836.38 31.77 8 1 1 844.39 30.18 8 -1 1 776.03 30.20 -8 1 -1 912.13 36.84 -8 -1 -2 636.26 28.40 8 -1 2 671.12 27.33 8 1 2 642.74 29.18 -8 1 -2 713.81 33.04 -8 -1 -3 7.03 15.02 8 -1 3 3.32 9.66 8 1 3 14.98 13.04 -8 1 -3 15.34 16.88 -8 -1 -4 36.87 13.71 8 -1 4 41.90 10.28 -8 1 -4 60.31 18.29 -8 -1 -5 14.48 17.54 8 -1 5 35.62 12.93 -8 1 -5 44.86 21.77 -8 2 10 15.07 21.76 8 2 -10 55.34 20.96 8 -2 -10 18.55 17.72 -8 2 9 296.59 24.21 8 2 -9 319.28 25.13 8 -2 -9 202.46 18.01 -8 -2 8 222.83 20.82 -8 2 8 226.06 19.07 8 2 -8 234.85 21.54 8 -2 -8 207.86 21.67 -8 -2 7 376.43 23.18 -8 2 7 407.56 20.31 8 2 -7 437.57 24.27 8 -2 -7 363.19 17.60 -8 -2 6 228.29 18.44 -8 2 6 260.52 21.28 8 2 -6 249.96 18.24 8 -2 -6 202.87 17.14 -8 -2 5 522.88 31.13 -8 2 5 539.75 26.79 8 2 -5 538.87 27.54 8 -2 -5 554.87 25.80 -8 -2 4 22.35 13.12 -8 2 4 21.64 18.05 8 2 -4 28.78 17.05 8 -2 -4 35.29 12.04 -8 2 3 448.09 22.14 -8 -2 3 502.36 23.92 -8 2 3 550.45 26.61 8 2 -3 559.82 24.06 8 -2 -3 551.57 22.36 -8 -2 2 201.05 15.70 8 -2 -2 193.93 13.06 -8 2 2 209.39 18.52 8 2 -2 193.61 18.95 8 -2 -2 230.14 14.88 -8 -2 1 673.70 29.95 8 -2 -1 656.36 24.15 8 2 -1 687.21 29.27 -8 -2 0 365.99 20.25 8 -2 0 331.35 17.71 8 2 0 356.18 21.00 8 -2 0 328.03 19.89 -8 2 0 348.71 23.57 -8 -2 -1 214.59 17.00 8 -2 1 188.55 13.66 8 2 1 215.43 20.35 -8 2 -1 239.71 19.17 -8 -2 -2 98.59 13.25 8 -2 2 96.37 10.48 8 2 2 105.80 13.79 -8 2 -2 110.13 17.13 -8 -2 -3 371.26 24.89 8 -2 3 396.81 22.80 8 2 3 347.58 22.81 -8 2 -3 429.64 32.66 -8 -2 -4 -1.42 18.21 8 -2 4 -7.16 13.60 -8 2 -4 5.15 13.46 -8 -2 -5 132.68 14.45 8 -2 5 159.70 14.68 -8 2 -5 147.53 20.97 -8 -3 9 155.25 21.70 -8 3 9 160.51 19.76 8 3 -9 159.99 23.73 8 -3 -9 172.09 19.93 -8 -3 8 -1.32 17.13 -8 3 8 -7.52 21.76 8 3 -8 1.13 15.35 8 -3 -8 -4.84 18.68 -8 -3 7 40.30 20.93 -8 3 7 42.59 13.63 8 3 -7 28.90 14.76 8 -3 -7 44.47 15.53 -8 -3 6 3.21 15.36 -8 3 6 -2.16 13.93 8 3 -6 13.27 16.09 8 -3 -6 1.59 11.39 -8 -3 5 1316.91 61.84 -8 3 5 1275.54 33.26 8 3 -5 1323.12 61.04 8 -3 -5 1226.43 29.29 -8 -3 4 29.93 19.85 -8 3 4 17.00 18.00 8 3 -4 24.86 16.08 8 -3 -4 21.92 13.54 -8 -3 3 1372.19 53.56 -8 3 3 1408.74 54.69 8 3 -3 1518.93 57.74 8 -3 -3 1487.79 54.52 -8 -3 2 -10.60 16.03 8 -3 -2 8.47 10.06 -8 3 2 -0.22 11.64 8 3 -2 -0.87 14.31 -8 -3 1 11.14 15.53 8 -3 -1 7.92 9.12 -8 3 1 18.46 18.02 8 3 -1 23.49 12.68 -8 3 1 -3.69 16.33 -8 -3 0 11.70 12.92 8 -3 0 16.97 10.18 8 3 0 26.01 13.18 -8 3 0 4.39 15.41 -8 -3 -1 79.80 18.11 8 -3 1 71.61 14.93 8 3 1 73.57 17.85 -8 3 -1 82.83 17.59 -8 -3 -2 -7.33 17.72 8 -3 2 8.08 10.00 8 3 2 8.56 20.06 -8 3 -2 16.63 19.18 -8 -3 -3 532.05 31.68 8 -3 3 471.08 25.42 8 3 3 448.53 26.67 -8 3 -3 538.97 31.99 -8 -3 -4 3.28 18.22 8 -3 4 13.90 13.33 -8 3 -4 38.85 20.81 -8 -4 8 581.77 28.70 -8 4 8 534.55 27.82 8 4 -8 574.14 29.36 8 -4 -8 564.90 28.38 -8 -4 7 141.45 17.89 -8 4 7 138.33 16.72 8 4 -7 172.19 18.78 8 -4 -7 132.18 16.88 -8 -4 6 36.87 24.94 -8 4 6 48.32 20.08 8 4 -6 32.69 14.28 8 -4 -6 41.84 15.25 -8 -4 5 69.71 20.99 -8 4 5 59.74 16.01 8 4 -5 67.31 16.15 8 -4 -5 83.13 15.98 -8 -4 4 29.20 17.73 -8 4 4 26.85 13.48 8 4 -4 27.74 17.09 8 -4 -4 24.23 14.20 -8 -4 3 215.88 26.24 -8 4 3 219.89 21.56 8 4 -3 225.72 17.57 8 -4 -3 230.94 20.02 -8 -4 2 349.70 23.72 -8 4 2 311.26 24.03 8 4 -2 391.44 27.90 8 -4 -2 409.03 25.41 -8 -4 1 270.90 21.12 8 4 -1 285.93 24.11 -8 4 1 281.90 27.10 -8 -4 0 976.43 52.87 8 -4 0 878.79 46.67 8 4 0 1031.97 55.92 -8 4 0 975.39 52.22 -8 -4 -1 52.36 17.62 8 -4 1 56.08 10.87 8 4 1 64.88 21.60 -8 4 -1 73.13 19.85 -8 -4 -2 147.76 16.54 8 -4 2 156.80 15.49 8 4 2 171.86 15.99 -8 4 -2 138.80 19.99 -8 -4 -3 178.46 18.29 8 -4 3 190.21 17.89 8 4 3 175.97 20.65 -8 4 -3 155.31 23.77 -8 -5 6 620.41 30.45 -8 5 6 555.23 27.40 8 5 -6 581.77 33.35 8 -5 -6 569.09 25.78 -8 -5 5 31.88 23.29 -8 5 5 34.58 19.93 8 5 -5 7.47 18.76 8 -5 -5 32.10 18.89 -8 -5 4 10.19 24.03 -8 5 4 9.19 12.81 8 5 -4 20.59 18.97 8 -5 -4 12.18 20.24 -8 -5 3 2.97 20.89 8 5 -3 -6.60 19.06 8 -5 -3 4.98 16.97 -8 -5 2 300.16 20.18 8 5 -2 328.96 20.91 8 -5 -2 318.36 23.03 -8 -5 1 347.22 25.37 8 5 -1 363.24 23.53 -8 5 1 305.45 20.90 -8 -5 0 26.53 16.02 8 5 0 21.98 24.71 -8 5 0 32.60 17.50 -8 -5 -1 194.44 19.11 8 5 1 160.15 24.02 -8 5 -1 184.23 23.19 -9 0 9 1276.39 45.22 -9 0 8 -11.38 18.21 -9 0 7 16.69 18.24 -9 0 6 -2.36 17.79 -9 0 5 25.52 15.63 9 0 -5 32.85 19.47 -9 0 4 2.63 13.89 9 0 -4 10.45 22.23 -9 0 3 109.73 17.63 9 0 -3 112.88 19.39 -9 0 2 3.37 12.34 9 0 -2 -11.88 17.55 -9 0 1 1481.54 67.53 9 0 -1 1491.93 68.97 -9 0 0 8.58 11.88 9 0 0 2.04 12.68 -9 0 -1 51.91 20.39 -9 0 -2 1.44 15.09 -9 1 9 232.51 28.49 -9 1 8 2.86 23.73 9 1 -8 8.29 20.86 -9 1 7 704.24 43.19 9 1 -7 693.72 37.81 -9 -1 6 668.05 38.60 -9 1 6 754.91 42.18 9 1 -6 809.96 44.69 9 -1 -6 677.90 37.36 -9 -1 5 70.26 16.47 -9 1 5 68.32 21.96 9 1 -5 60.93 16.73 9 -1 -5 67.60 13.59 -9 -1 4 504.16 31.17 -9 1 4 444.43 30.45 9 1 -4 620.86 37.80 9 -1 -4 437.73 24.60 -9 1 3 451.81 25.30 -9 -1 3 528.72 32.03 9 1 -3 592.72 35.16 9 -1 -3 570.33 32.84 9 -1 -3 494.69 27.90 -9 1 2 26.08 13.34 -9 -1 2 29.46 14.84 9 1 -2 29.82 18.26 9 -1 -2 33.03 19.15 9 -1 -2 34.38 14.59 -9 1 1 44.01 15.79 -9 -1 1 86.80 18.39 9 1 -1 62.82 20.03 9 -1 -1 64.03 17.78 -9 1 0 20.25 14.20 -9 -1 0 7.95 17.05 9 1 0 10.76 15.23 9 -1 0 7.59 18.55 -9 -1 -1 659.55 34.62 9 -1 1 666.46 33.94 9 1 1 676.60 39.53 -9 -1 -2 204.79 18.67 9 -1 2 185.27 13.25 -9 -1 -3 2.41 16.09 9 -1 3 19.61 13.35 -9 2 8 411.78 26.16 9 2 -8 440.61 26.20 9 -2 -8 361.38 24.05 -9 -2 7 78.79 17.09 -9 2 7 87.09 20.88 9 2 -7 87.52 18.98 9 -2 -7 69.39 17.97 -9 -2 6 118.99 22.50 -9 2 6 141.23 20.57 9 2 -6 156.12 18.33 9 -2 -6 109.66 13.88 -9 -2 5 1192.64 60.83 -9 2 5 1121.91 59.02 9 2 -5 1362.91 69.78 9 -2 -5 1185.32 61.81 -9 -2 4 457.78 30.08 -9 2 4 525.65 35.38 9 2 -4 525.68 34.15 9 -2 -4 496.98 30.85 -9 -2 3 -0.05 13.03 -9 2 3 -4.24 22.18 9 2 -3 1.27 15.85 9 -2 -3 8.79 14.39 -9 -2 2 69.83 18.76 9 -2 -2 56.96 11.91 -9 2 2 49.73 19.91 9 2 -2 88.72 19.14 9 -2 -2 82.14 19.82 -9 -2 1 1.29 15.73 9 -2 -1 -1.25 13.01 9 2 -1 5.03 17.92 9 -2 -1 13.63 19.22 -9 2 1 -4.97 13.07 -9 -2 0 363.46 25.89 9 -2 0 351.78 20.81 9 2 0 374.21 28.13 -9 2 0 377.42 24.94 -9 -2 -1 48.05 17.30 9 -2 1 60.65 10.78 9 2 1 48.44 19.31 -9 2 -1 49.29 19.56 -9 -2 -2 187.58 19.41 9 -2 2 172.61 13.57 -9 2 -2 188.16 23.03 -9 -3 7 -2.64 20.20 -9 3 7 -0.95 17.82 9 3 -7 -2.17 24.21 9 -3 -7 -17.18 18.21 -9 -3 6 105.58 18.17 -9 3 6 90.02 19.48 9 3 -6 82.19 18.55 9 -3 -6 120.27 18.77 -9 -3 5 14.02 21.53 -9 3 5 -4.78 15.32 9 3 -5 -11.52 18.54 9 -3 -5 -18.64 15.05 -9 -3 4 48.60 25.69 -9 3 4 40.60 19.72 9 3 -4 34.46 15.84 9 -3 -4 8.28 12.42 -9 -3 3 12.78 23.36 -9 3 3 -11.54 17.17 9 3 -3 1.26 20.71 9 -3 -3 -8.94 12.79 -9 -3 2 1071.58 52.82 9 3 -2 1205.98 57.54 9 -3 -2 1300.86 60.70 -9 -3 1 32.97 18.41 9 3 -1 29.99 20.72 -9 3 1 33.75 16.47 -9 -3 0 656.46 30.03 9 -3 0 532.78 20.27 9 3 0 570.64 26.61 -9 3 0 655.56 35.81 -9 -3 -1 -0.59 18.60 9 -3 1 -13.75 12.35 9 3 1 0.47 14.92 -9 3 -1 9.49 24.01 -9 -4 5 1487.71 52.14 -9 4 5 1349.31 47.77 9 4 -5 1519.68 52.86 9 -4 -5 1418.89 47.13 -9 -4 4 231.84 30.62 -9 4 4 149.28 20.29 9 4 -4 177.87 18.34 9 -4 -4 187.92 22.06 -9 -4 3 14.59 23.99 9 4 -3 6.88 24.02 9 -4 -3 21.78 14.77 -9 -4 2 128.37 22.55 9 4 -2 149.67 24.53 9 -4 -2 131.39 20.54 -9 -4 1 20.14 19.45 9 4 -1 51.04 18.36 -9 4 1 34.56 18.51 10 0 -5 0.98 24.48 10 0 -4 328.67 24.02 -10 0 3 6.57 18.14 10 0 -3 -6.70 17.86 -10 0 2 13.79 14.09 10 0 -2 57.04 23.33 -10 0 1 8.37 19.50 10 1 -5 155.94 26.01 -10 -1 4 311.05 21.30 10 1 -4 425.26 28.16 10 -1 -4 346.94 24.27 -10 -1 3 261.56 21.30 10 1 -3 280.30 28.51 10 -1 -3 300.86 24.86 -10 -1 2 142.01 17.93 10 1 -2 126.00 19.14 10 -1 -2 167.38 25.28 -10 1 1 50.11 19.57 -10 -1 1 58.08 22.22 10 1 -1 46.45 16.88 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 79005 _shelx_res_file ; TITL shelxt_a.res in P2(1)/n shelx.res created by SHELXL-2018/3 at 16:15:57 on 14-Dec-2022 CELL 0.71075 7.8434 7.0795 10.9133 90.000 102.836 90.000 ZERR 2.00 0.0005 0.0004 0.0007 0.000 0.008 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC RB CO C O H UNIT 4 2 8 24 16 MERG 2 FMAP 2 PLAN 20 ACTA TEMP 173 BOND HTAB LIST 4 L.S. 10 EQIV $14 -x+2, -y, -z+1 EQIV $12 -x+3/2, y+1/2, -z+3/2 EQIV $13 x-1/2, -y+1/2, z-1/2 HTAB O2 O4 HTAB O2 O4_$14 HTAB O2 O6_$14 HTAB O1 O5_$12 HTAB O1 O6_$13 WGHT 0.032300 FVAR 0.70621 RB1 1 0.815340 0.660299 0.379620 11.00000 0.01880 0.02412 = 0.01580 0.00010 0.00529 0.00190 CO1 2 0.500000 0.000000 0.500000 10.50000 0.01045 0.01303 = 0.00658 -0.00043 0.00112 0.00024 O1 4 0.516452 0.291172 0.491116 11.00000 0.01950 0.01417 = 0.01180 0.00045 -0.00203 -0.00333 O2 4 0.870455 0.240838 0.395528 11.00000 0.02481 0.02683 = 0.02307 0.00072 0.01379 -0.00021 O3 4 0.506307 0.019837 0.690600 11.00000 0.01234 0.02162 = 0.00833 -0.00107 0.00110 0.00095 O4 4 0.770668 -0.015197 0.572348 11.00000 0.01212 0.02023 = 0.00927 -0.00122 0.00242 0.00098 O5 4 0.691628 -0.031361 0.874221 11.00000 0.01801 0.02913 = 0.00815 0.00212 0.00165 -0.00002 O6 4 0.962715 0.032951 0.753260 11.00000 0.01257 0.03052 = 0.01261 0.00054 -0.00088 -0.00065 C1 3 0.657773 -0.001378 0.759376 11.00000 0.01383 0.01193 = 0.00988 -0.00188 0.00311 -0.00082 C2 3 0.812147 0.007569 0.691278 11.00000 0.01343 0.01028 = 0.01303 0.00141 0.00317 0.00200 H1 5 0.828373 0.168046 0.448596 11.00000 0.05631 H2 5 0.942403 0.172988 0.367192 11.00000 0.07865 H3 5 0.594019 0.342316 0.532306 11.00000 0.02272 H4 5 0.493795 0.345219 0.427213 11.00000 0.02909 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.0496, GooF = S = 0.974, Restrained GooF = 0.974 for all data REM R1 = 0.0206 for 1169 Fo > 4sig(Fo) and 0.0254 for all 1343 data REM 104 parameters refined using 0 restraints END WGHT 0.0323 0.0000 REM Instructions for potential hydrogen bonds HTAB O2 O4 HTAB O2 O4_$14 HTAB O2 O6_$14 HTAB O1 O5_$12 HTAB O1 O6_$13 REM Highest difference peak 0.647, deepest hole -0.642, 1-sigma level 0.099 Q1 1 0.8738 0.7423 0.3601 11.00000 0.05 0.65 Q2 1 0.7548 0.7432 0.4012 11.00000 0.05 0.56 Q3 1 0.8813 0.5774 0.3545 11.00000 0.05 0.56 Q4 1 0.7473 0.5829 0.4034 11.00000 0.05 0.45 Q5 1 0.7322 0.0107 0.7279 11.00000 0.05 0.44 Q6 1 0.7055 0.6865 0.4416 11.00000 0.05 0.41 Q7 1 0.9256 0.6427 0.3140 11.00000 0.05 0.37 Q8 1 0.4318 0.0739 0.5253 11.00000 0.05 0.36 Q9 1 0.5668 0.0776 0.4796 11.00000 0.05 0.32 Q10 1 0.8264 -0.0082 0.4648 11.00000 0.05 0.30 Q11 1 0.9040 0.1332 0.3620 11.00000 0.05 0.29 Q12 1 0.6559 -0.0585 0.8156 11.00000 0.05 0.26 Q13 1 0.7620 0.8058 0.2995 11.00000 0.05 0.26 Q14 1 0.6562 0.3775 0.5724 11.00000 0.05 0.26 Q15 1 0.5682 0.0001 0.7220 11.00000 0.05 0.25 Q16 1 0.5114 0.0373 0.6270 11.00000 0.05 0.25 Q17 1 0.7894 0.0052 0.8711 11.00000 0.05 0.25 Q18 1 0.4192 0.0183 0.7375 11.00000 0.05 0.25 Q19 1 0.5186 -0.1368 0.7569 11.00000 0.05 0.25 Q20 1 0.5782 0.1430 0.5598 11.00000 0.05 0.25 ; _shelx_res_checksum 7807 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rb Rb1 0.81534(3) 0.66030(3) 0.37962(2) 0.01935(9) Uani d 1 . . Co Co1 0.500000 0.000000 0.500000 0.01014(11) Uani d 1 . . O O1 0.5165(2) 0.2912(2) 0.49112(17) 0.0160(3) Uani d 1 . . O O2 0.8705(2) 0.2408(3) 0.39553(17) 0.0236(4) Uani d 1 . . O O3 0.50631(18) 0.0198(2) 0.69060(13) 0.0143(3) Uani d 1 . . O O4 0.77067(18) -0.0152(2) 0.57235(13) 0.0139(3) Uani d 1 . . O O5 0.6916(2) -0.0314(2) 0.87422(14) 0.0186(3) Uani d 1 . . O O6 0.96271(19) 0.0330(2) 0.75326(14) 0.0191(3) Uani d 1 . . C C1 0.6578(3) -0.0014(3) 0.75938(19) 0.0118(4) Uani d 1 . . C C2 0.8121(3) 0.0076(3) 0.69128(19) 0.0122(4) Uani d 1 . . H H1 0.828(5) 0.168(5) 0.449(4) 0.056(11) Uiso d 1 . . H H2 0.942(6) 0.173(6) 0.367(4) 0.079(15) Uiso d 1 . . H H3 0.594(4) 0.342(4) 0.532(3) 0.023(8) Uiso d 1 . . H H4 0.494(4) 0.345(4) 0.427(3) 0.029(9) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rb1 0.01880(14) 0.02412(14) 0.01580(13) 0.00190(8) 0.00529(9) 0.00010(8) Co1 0.0105(2) 0.01303(19) 0.00658(19) 0.00024(14) 0.00112(15) -0.00043(14) O1 0.0195(9) 0.0142(7) 0.0118(8) -0.0033(6) -0.0020(7) 0.0004(6) O2 0.0248(10) 0.0268(9) 0.0231(9) -0.0002(8) 0.0138(8) 0.0007(7) O3 0.0123(7) 0.0216(7) 0.0083(7) 0.0009(6) 0.0011(6) -0.0011(6) O4 0.0121(7) 0.0202(7) 0.0093(7) 0.0010(6) 0.0024(6) -0.0012(6) O5 0.0180(8) 0.0291(8) 0.0081(7) 0.0000(6) 0.0016(6) 0.0021(6) O6 0.0126(8) 0.0305(9) 0.0126(7) -0.0007(7) -0.0009(6) 0.0005(7) C1 0.0138(10) 0.0119(9) 0.0099(9) -0.0008(7) 0.0031(8) -0.0019(8) C2 0.0134(10) 0.0103(9) 0.0130(10) 0.0020(8) 0.0032(8) 0.0014(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 Rb1 O5 . 2_656 62.28(5) ? O2 Rb1 O3 . 4_665 62.87(4) ? O5 Rb1 O3 2_656 4_665 121.12(4) ? O2 Rb1 O2 . 2_655 105.67(5) ? O5 Rb1 O2 2_656 2_655 148.26(5) ? O3 Rb1 O2 4_665 2_655 67.65(4) ? O2 Rb1 O5 . 4_665 65.45(5) ? O5 Rb1 O5 2_656 4_665 95.16(4) ? O3 Rb1 O5 4_665 4_665 42.24(4) ? O2 Rb1 O5 2_655 4_665 106.35(5) ? O2 Rb1 O6 . 4_565 72.16(5) ? O5 Rb1 O6 2_656 4_565 90.38(4) ? O3 Rb1 O6 4_665 4_565 92.16(4) ? O2 Rb1 O6 2_655 4_565 58.00(5) ? O5 Rb1 O6 4_665 4_565 128.06(4) ? O2 Rb1 O2 . 3_766 95.58(5) ? O5 Rb1 O2 2_656 3_766 64.67(5) ? O3 Rb1 O2 4_665 3_766 101.60(4) ? O2 Rb1 O2 2_655 3_766 146.79(5) ? O5 Rb1 O2 4_665 3_766 59.77(4) ? O6 Rb1 O2 4_565 3_766 155.02(4) ? O2 Rb1 O4 . 1_565 135.32(4) ? O5 Rb1 O4 2_656 1_565 73.17(4) ? O3 Rb1 O4 4_665 1_565 151.80(4) ? O2 Rb1 O4 2_655 1_565 114.32(4) ? O5 Rb1 O4 4_665 1_565 117.99(4) ? O6 Rb1 O4 4_565 1_565 113.04(4) ? O2 Rb1 O4 3_766 1_565 60.44(4) ? O2 Rb1 O1 . 3_666 101.48(5) ? O5 Rb1 O1 2_656 3_666 59.06(4) ? O3 Rb1 O1 4_665 3_666 153.07(4) ? O2 Rb1 O1 2_655 3_666 98.78(5) ? O5 Rb1 O1 4_665 3_666 153.95(4) ? O6 Rb1 O1 4_565 3_666 61.33(4) ? O2 Rb1 O1 3_766 3_666 101.68(5) ? O4 Rb1 O1 1_565 3_666 54.53(4) ? O2 Rb1 O6 . 3_766 126.25(5) ? O5 Rb1 O6 2_656 3_766 143.03(4) ? O3 Rb1 O6 4_665 3_766 66.26(4) ? O2 Rb1 O6 2_655 3_766 68.49(4) ? O5 Rb1 O6 4_665 3_766 65.79(4) ? O6 Rb1 O6 4_565 3_766 126.49(2) ? O2 Rb1 O6 3_766 3_766 78.39(4) ? O4 Rb1 O6 1_565 3_766 87.81(4) ? O1 Rb1 O6 3_666 3_766 132.20(4) ? O2 Rb1 O3 . 3_666 140.70(5) ? O5 Rb1 O3 2_656 3_666 110.22(4) ? O3 Rb1 O3 4_665 3_666 125.45(2) ? O2 Rb1 O3 2_655 3_666 58.91(4) ? O5 Rb1 O3 4_665 3_666 149.98(4) ? O6 Rb1 O3 4_565 3_666 69.30(4) ? O2 Rb1 O3 3_766 3_666 116.60(4) ? O4 Rb1 O3 1_565 3_666 58.39(4) ? O1 Rb1 O3 3_666 3_666 52.51(4) ? O6 Rb1 O3 3_766 3_666 84.20(4) ? O1 Co1 O1 3_656 . 180.0 ? O1 Co1 O3 3_656 3_656 89.52(6) ? O1 Co1 O3 . 3_656 90.48(6) ? O1 Co1 O3 3_656 . 90.48(6) ? O1 Co1 O3 . . 89.52(6) ? O3 Co1 O3 3_656 . 180.0 ? O1 Co1 O4 3_656 . 89.98(6) ? O1 Co1 O4 . . 90.02(6) ? O3 Co1 O4 3_656 . 99.83(6) ? O3 Co1 O4 . . 80.17(6) ? O1 Co1 O4 3_656 3_656 90.02(6) ? O1 Co1 O4 . 3_656 89.98(6) ? O3 Co1 O4 3_656 3_656 80.17(6) ? O3 Co1 O4 . 3_656 99.83(6) ? O4 Co1 O4 . 3_656 180.0 ? Co1 O1 Rb1 . 3_666 91.19(6) ? Rb1 O2 Rb1 . 2_645 95.49(5) ? Rb1 O2 Rb1 . 3_766 84.42(4) ? Rb1 O2 Rb1 2_645 3_766 156.77(7) ? C1 O3 Co1 . . 113.38(13) ? C1 O3 Rb1 . 4_566 94.92(12) ? Co1 O3 Rb1 . 4_566 137.42(6) ? C1 O3 Rb1 . 3_666 140.90(12) ? Co1 O3 Rb1 . 3_666 88.13(5) ? Rb1 O3 Rb1 4_566 3_666 88.83(4) ? C2 O4 Co1 . . 112.61(13) ? C2 O4 Rb1 . 1_545 136.21(12) ? Co1 O4 Rb1 . 1_545 92.24(5) ? C1 O5 Rb1 . 2_646 141.22(13) ? C1 O5 Rb1 . 4_566 94.51(12) ? Rb1 O5 Rb1 2_646 4_566 84.84(4) ? C2 O6 Rb1 . 4_666 145.41(13) ? C2 O6 Rb1 . 3_766 112.75(13) ? Rb1 O6 Rb1 4_666 3_766 88.88(4) ? O5 C1 O3 . . 125.57(19) ? O5 C1 C2 . . 118.35(18) ? O3 C1 C2 . . 116.07(17) ? O6 C2 O4 . . 124.8(2) ? O6 C2 C1 . . 119.63(18) ? O4 C2 C1 . . 115.52(18) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rb1 O2 . 3.0003(18) ? Rb1 O5 2_656 3.0209(16) ? Rb1 O3 4_665 3.0819(15) ? Rb1 O2 2_655 3.0856(19) ? Rb1 O5 4_665 3.1023(16) ? Rb1 O6 4_565 3.1190(15) ? Rb1 O2 3_766 3.1461(19) ? Rb1 O4 1_565 3.1862(15) ? Rb1 O1 3_666 3.2421(17) ? Rb1 O6 3_766 3.3122(16) ? Rb1 O3 3_666 3.3497(15) ? Co1 O1 3_656 2.0690(16) ? Co1 O1 . 2.0690(16) ? Co1 O3 3_656 2.0744(14) ? Co1 O3 . 2.0744(14) ? Co1 O4 . 2.0969(14) ? Co1 O4 3_656 2.0969(14) ? O3 C1 . 1.265(2) ? O4 C2 . 1.276(3) ? O5 C1 . 1.240(3) ? O6 C2 . 1.237(3) ? C1 C2 . 1.556(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H1 O4 . 0.89(4) 2.00(4) 2.880(2) 171(4) yes O2 H2 O4 3_756 0.85(5) 2.47(5) 3.187(2) 143(4) yes O2 H2 O6 3_756 0.85(5) 2.20(5) 3.008(2) 159(4) yes O1 H3 O5 2_656 0.76(3) 1.98(3) 2.736(2) 174(3) yes O1 H4 O6 4_565 0.78(3) 2.05(3) 2.825(2) 172(3) yes _cod_database_fobs_code 2244219