#------------------------------------------------------------------------------ #$Date: 2019-07-13 13:10:59 +0300 (Sat, 13 Jul 2019) $ #$Revision: 217014 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/21/1552105.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_1552105 loop_ _publ_author_name 'Gokila, Govindharajan' 'Thiruvalluvar, Aravazhi Amalan' 'Ramachandra Raja, Chidambaram' _publ_section_title ; Bis(2-methyllactato)borate tetrahydrate ; _journal_issue 7 _journal_name_full IUCrData _journal_page_first x190982 _journal_paper_doi 10.1107/S2414314619009829 _journal_volume 4 _journal_year 2019 _chemical_formula_iupac 'C8 H12 B O6, 4H2 O' _chemical_formula_moiety 'C8 H12 B O6, 4(H2 O)' _chemical_formula_sum 'C8 H20 B O10' _chemical_formula_weight 287.05 _chemical_name_common ; Bis(2-methyllactato)borate tetrahydrate ; _chemical_name_systematic ; 3,3,8,8-Tetramethyl-1,4,6,9-tetraoxa-\l^4^-boraspiro[4.4]nonane-2,7-dione tetrahydrate ; _space_group_crystal_system orthorhombic _space_group_IT_number 18 _space_group_name_Hall 'P 2 2ab' _space_group_name_H-M_alt 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_space_group_name_H-M 'P 21 21 2' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.08090(10) _cell_length_b 16.7912(3) _cell_length_c 6.50010(10) _cell_measurement_reflns_used 6304 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 30.39 _cell_measurement_theta_min 3.12 _cell_volume 772.84(2) _computing_cell_refinement ; APEX3 and SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT and XPREP (Bruker, 2016) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009) ; _computing_publication_material ; SHELXL2018 (Sheldrick, 2015b), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker Kappa APEX3 CMOS' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 18957 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.997 _diffrn_reflns_theta_min 3.764 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.234 _exptl_crystal_description Block _exptl_crystal_F_000 306 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.208 _refine_diff_density_min -0.118 _refine_ls_abs_structure_details ; Flack x determined using 587 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.4(4) _refine_ls_extinction_coef 0.26(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 1680 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0360 _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^)+(0.0444P)^2^+0.1071P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.0942 _reflns_number_gt 1585 _reflns_number_total 1680 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ff4030sup1.cif _cod_data_source_block I _cod_database_code 1552105 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.983 _shelx_estimated_absorpt_t_max 0.989 _shelx_hkl_file ; 0 0 1 154.58 8.90 0 0 -3 9563.24 469.65 0 0 3 8758.52 469.65 0 0 -3 9074.89 467.95 0 0 4 136.79 9.30 0 0 4 130.09 10.90 0 0 -4 116.79 8.80 0 0 4 137.19 9.20 0 0 -4 129.49 9.00 0 0 -4 127.69 11.50 0 0 -4 126.19 8.60 0 0 -4 118.99 10.50 0 0 5 94.19 8.20 0 0 -5 81.99 7.00 0 0 5 79.79 9.20 0 0 -5 85.79 10.80 0 0 -5 88.69 7.60 0 0 -5 82.09 6.80 0 0 -6 -4.50 6.90 0 0 6 -3.50 3.20 0 0 -6 -1.60 3.90 0 0 6 -1.00 3.30 0 0 -7 35.40 4.50 0 0 -7 38.10 6.00 0 0 7 25.90 5.10 0 0 -7 25.90 4.20 0 0 7 26.90 5.80 0 0 -7 23.40 10.90 0 0 8 5.70 6.00 0 0 -8 7.10 5.60 0 0 -9 30.60 6.30 0 0 9 21.10 8.80 -1 0 0 0.40 0.60 1 0 -2 5900.51 309.17 -1 0 2 6190.48 308.27 -1 0 2 5839.72 308.07 1 0 -2 5927.81 308.17 1 0 -2 6105.09 308.17 -1 0 2 5709.53 309.17 -1 0 -2 6362.86 308.57 -1 0 3 1986.90 112.19 -1 0 -3 2163.48 112.99 -1 0 -3 2181.98 112.09 -1 0 -3 2050.69 111.99 1 0 -3 2256.67 112.79 1 0 -3 2464.65 113.79 -1 0 3 2105.49 114.69 1 0 -3 2308.17 114.49 -1 0 3 2292.47 112.89 1 0 3 2163.38 111.79 -1 0 -3 2186.28 113.69 -1 0 3 2228.98 113.99 1 0 -3 2126.89 112.89 -1 0 3 2024.40 112.59 1 0 3 2116.69 113.69 1 0 -3 2031.50 113.09 1 0 4 1268.97 69.59 -1 0 4 1292.67 66.89 -1 0 4 1188.48 70.09 -1 0 -4 1176.68 67.09 -1 0 -4 1324.87 68.69 -1 0 -4 1180.08 68.59 -1 0 4 1271.77 67.39 1 0 4 1309.37 66.89 1 0 -4 1281.37 68.19 1 0 -4 1303.97 70.59 1 0 -4 1249.18 68.59 -1 0 4 1257.07 67.89 -1 0 -4 1240.18 67.69 1 0 -4 1281.27 68.09 -1 0 -4 1280.27 67.19 -1 0 4 1428.66 68.29 -1 0 -4 1292.17 69.69 1 0 -4 1428.26 69.49 -1 0 5 49.30 7.90 -1 0 -5 61.39 9.30 1 0 -5 41.70 8.50 -1 0 -5 47.80 8.80 -1 0 5 67.49 7.10 -1 0 -5 54.29 4.90 1 0 -5 47.70 9.20 1 0 5 51.89 6.70 -1 0 -5 53.59 6.00 -1 0 -5 47.20 5.00 1 0 -5 51.39 5.60 -1 0 5 64.69 7.60 1 0 5 57.59 5.50 1 0 -5 51.79 6.90 1 0 -5 59.09 5.60 -1 0 -5 60.19 7.40 1 0 -6 16.30 5.50 -1 0 -6 26.30 3.70 1 0 -6 13.30 3.40 1 0 6 29.20 5.40 1 0 6 15.20 4.20 -1 0 6 16.30 5.20 -1 0 6 31.60 5.60 -1 0 -6 23.40 8.10 -1 0 -6 25.70 4.90 1 0 -6 19.40 3.50 -1 0 6 19.10 6.30 1 0 6 27.90 4.50 -1 0 -6 21.70 3.20 1 0 -6 13.60 8.30 -1 0 -7 17.80 5.20 1 0 -7 26.00 4.70 -1 0 7 24.40 6.90 1 0 -7 27.70 4.60 1 0 7 26.00 5.80 -1 0 -7 22.40 9.60 1 0 -7 15.90 11.10 1 0 7 21.40 5.20 -1 0 -7 28.30 4.30 -1 0 7 33.60 5.30 -1 0 -7 25.30 3.80 1 0 -7 39.60 6.90 1 0 7 28.80 4.80 1 0 8 24.40 6.40 1 0 -8 7.90 6.00 -1 0 -8 14.10 5.50 -1 0 8 13.00 6.30 -1 0 8 24.10 7.10 -1 0 -8 10.70 3.90 1 0 -9 9.10 9.10 1 0 -9 10.20 6.70 1 0 9 12.60 8.60 -1 0 9 5.00 9.20 -2 0 0 324.37 17.30 2 0 0 348.37 18.90 2 0 0 309.37 18.30 2 0 0 320.17 18.90 -2 0 0 335.17 18.70 -2 0 0 357.56 19.10 -2 0 0 298.57 18.30 -2 0 1 590.34 32.40 2 0 -1 507.85 32.60 2 0 1 672.03 32.60 -2 0 1 597.34 32.80 2 0 -1 560.24 32.40 2 0 -1 612.14 32.10 -2 0 -1 569.74 31.60 -2 0 1 584.74 32.40 -2 0 1 527.35 32.00 2 0 1 585.04 31.70 2 0 -1 633.54 32.40 -2 0 -1 631.14 32.60 2 0 1 616.54 32.00 -2 0 -1 607.44 32.10 -2 0 2 8742.62 454.45 -2 0 2 8915.81 453.55 -2 0 2 9434.96 454.15 2 0 -2 9172.48 454.25 2 0 -2 8261.37 453.35 2 0 -2 8645.83 454.85 2 0 -2 7793.12 453.55 -2 0 -2 8973.30 452.95 -2 0 2 9628.84 453.95 -2 0 -3 527.05 29.50 -2 0 3 538.55 30.00 2 0 -3 542.75 30.80 -2 0 -3 511.85 28.60 -2 0 3 542.55 30.30 2 0 -3 489.35 30.00 -2 0 3 482.95 31.20 2 0 -3 520.45 31.70 -2 0 -3 539.35 29.10 2 0 3 505.25 29.90 -2 0 -3 546.05 30.10 -2 0 3 509.35 30.50 2 0 -3 549.74 30.10 2 0 -3 604.04 31.80 2 0 3 549.74 28.80 -2 0 3 562.44 30.20 2 0 -4 972.20 53.99 2 0 4 984.00 54.29 -2 0 -4 1018.90 54.49 -2 0 4 1021.20 54.09 -2 0 -4 932.71 52.29 2 0 -4 926.21 54.39 -2 0 -4 995.20 53.29 -2 0 -4 994.60 52.59 -2 0 4 980.60 53.19 -2 0 -4 904.91 56.99 -2 0 4 1012.00 53.69 2 0 -4 923.21 55.39 -2 0 4 1012.20 55.59 2 0 -4 1019.20 53.89 -2 0 4 943.11 55.69 -2 0 4 1018.70 53.49 2 0 -4 1142.09 55.79 2 0 5 2.00 2.70 2 0 -5 -3.00 7.70 2 0 5 -2.90 3.50 -2 0 -5 3.70 3.60 -2 0 -5 0.70 1.90 -2 0 5 -1.50 3.60 -2 0 5 0.20 4.40 -2 0 -5 1.00 6.00 2 0 -5 -5.40 4.80 -2 0 5 -1.70 3.20 -2 0 -5 -2.10 4.70 -2 0 -5 0.90 1.80 2 0 5 2.80 3.10 2 0 -5 -6.70 4.10 2 0 6 -1.30 3.30 2 0 -6 6.00 8.30 -2 0 6 0.00 3.70 -2 0 6 1.00 5.70 -2 0 -6 0.80 3.90 2 0 6 -3.20 3.30 -2 0 -6 5.20 5.50 -2 0 6 -4.70 3.80 -2 0 -6 2.30 2.50 -2 0 -6 1.40 2.60 2 0 6 4.00 3.30 2 0 -6 -1.60 3.20 -2 0 -6 14.90 7.20 2 0 -6 5.30 5.90 2 0 -6 2.20 3.60 -2 0 6 1.80 3.10 -2 0 -7 12.90 8.90 2 0 7 21.20 5.20 2 0 7 19.50 4.60 2 0 7 21.00 4.10 2 0 -7 18.10 4.50 2 0 -7 26.90 12.90 -2 0 -7 13.30 4.00 2 0 -7 18.80 5.90 -2 0 -7 25.10 4.40 -2 0 7 28.30 4.20 -2 0 8 6.20 6.80 -2 0 -8 22.20 6.30 2 0 -8 22.90 10.40 -2 0 8 -3.40 6.90 2 0 8 7.90 6.00 2 0 -8 10.70 5.60 2 0 9 8.60 9.40 2 0 -9 -0.20 7.80 2 0 -9 21.30 10.10 -2 0 9 3.10 15.40 3 0 0 -4.40 5.10 3 0 0 -4.00 2.80 -3 0 0 -3.40 3.60 -3 0 0 -5.90 3.80 3 0 0 -0.40 3.40 -3 0 0 -1.70 1.40 -3 0 0 -0.60 2.90 3 0 0 -1.20 2.80 -3 0 -1 1130.09 68.79 -3 0 1 1293.57 69.59 -3 0 -1 1196.38 68.09 -3 0 -1 1384.66 68.89 -3 0 1 1306.47 68.79 3 0 -1 1181.48 68.79 -3 0 -1 1290.27 69.19 -3 0 1 1272.27 69.59 3 0 1 1353.26 69.19 -3 0 1 1356.26 69.19 3 0 -1 1352.86 68.89 3 0 1 1350.96 68.29 3 0 -1 1326.07 68.09 3 0 -1 1305.47 69.69 3 0 2 415.66 24.70 -3 0 2 488.85 27.80 -3 0 -2 461.95 26.50 -3 0 2 488.65 26.90 3 0 2 475.65 25.90 3 0 2 424.86 26.10 3 0 -2 454.05 27.00 -3 0 2 424.06 29.70 3 0 -2 464.55 27.10 -3 0 -2 460.45 26.80 3 0 2 503.75 26.60 -3 0 2 448.46 26.90 3 0 -2 489.95 27.90 -3 0 -2 467.55 27.60 3 0 -2 485.15 26.90 -3 0 2 469.85 27.70 -3 0 -2 445.06 25.70 -3 0 3 777.72 41.90 -3 0 -3 740.43 40.40 -3 0 3 778.92 41.90 3 0 3 783.72 39.70 3 0 -3 757.72 41.40 3 0 3 779.52 40.00 -3 0 -3 704.13 40.80 3 0 3 683.73 39.80 3 0 -3 644.54 41.20 3 0 3 798.02 39.70 -3 0 -3 832.82 42.30 3 0 3 716.73 39.90 3 0 -3 746.73 42.20 3 0 -3 721.13 42.30 -3 0 -3 731.83 39.80 3 0 -3 652.93 42.60 -3 0 3 732.03 41.20 -3 0 3 741.83 42.30 -3 0 3 725.03 41.80 3 0 4 67.99 6.30 3 0 -4 66.19 9.90 3 0 -4 65.29 9.40 3 0 4 58.69 5.90 -3 0 -4 71.79 9.30 -3 0 4 66.09 9.30 -3 0 4 63.79 8.10 3 0 -4 74.39 7.40 -3 0 4 71.89 8.40 -3 0 -4 75.29 6.40 3 0 4 80.09 6.60 -3 0 4 72.89 6.90 3 0 -4 64.89 8.50 3 0 -4 62.19 7.40 -3 0 4 70.29 8.10 -3 0 4 62.59 6.40 -3 0 -4 68.39 7.10 -3 0 -4 52.69 5.20 3 0 -5 5.30 8.50 -3 0 5 -9.70 5.80 -3 0 5 2.10 4.40 -3 0 -5 7.00 6.20 -3 0 -5 1.90 3.90 3 0 5 7.00 3.50 -3 0 5 -0.30 4.50 -3 0 -5 2.40 5.60 3 0 -5 -2.20 4.20 -3 0 -5 4.80 2.30 3 0 -5 9.10 5.90 -3 0 5 -1.60 2.20 -3 0 6 7.40 3.90 -3 0 6 9.10 4.00 -3 0 -6 6.90 4.30 3 0 -6 8.10 10.50 3 0 6 11.10 3.80 3 0 -6 -1.40 6.80 3 0 -6 16.40 3.90 -3 0 6 14.40 5.50 -3 0 -6 8.30 7.70 -3 0 -6 9.90 3.10 -3 0 -6 4.00 2.50 3 0 -6 7.20 3.40 -3 0 -6 2.90 6.10 3 0 6 2.00 3.50 -3 0 6 10.70 4.20 3 0 6 10.40 3.50 3 0 -7 28.90 4.80 -3 0 7 35.00 5.90 -3 0 -7 19.20 10.00 -3 0 -7 29.70 4.90 -3 0 7 16.10 6.00 -3 0 7 22.30 6.00 -3 0 -7 16.00 7.40 3 0 7 31.10 5.70 3 0 -7 38.40 6.00 3 0 7 23.50 4.60 -3 0 -8 4.50 3.10 3 0 -8 -5.30 6.70 -3 0 8 -6.40 7.40 -3 0 -8 6.40 6.20 -3 0 8 2.60 9.00 3 0 8 -3.90 6.70 3 0 -8 2.00 7.40 4 0 0 119.99 9.80 -4 0 0 123.09 10.40 4 0 0 124.89 10.70 -4 0 0 122.59 9.70 -4 0 0 119.59 7.50 4 0 0 121.59 10.00 -4 0 0 126.69 11.00 -4 0 0 133.29 11.10 -4 0 -1 1272.87 65.39 -4 0 -1 1176.98 65.79 -4 0 -1 1123.29 64.49 -4 0 1 1304.67 66.69 -4 0 1 1290.27 65.99 4 0 1 1273.17 64.79 4 0 -1 1213.58 65.19 -4 0 -1 1280.47 66.19 4 0 1 1171.88 64.89 -4 0 1 1188.28 65.09 4 0 -1 1103.09 65.99 4 0 -1 1159.48 65.39 -4 0 1 1133.19 63.79 4 0 2 183.28 13.00 -4 0 2 179.78 14.50 -4 0 2 202.28 14.90 -4 0 2 204.08 15.10 -4 0 -2 187.68 12.70 4 0 2 190.58 13.00 4 0 -2 191.08 14.30 -4 0 -2 200.98 13.90 -4 0 2 207.48 13.40 -4 0 -2 224.08 15.10 4 0 2 195.18 13.40 -4 0 2 179.88 13.50 4 0 -2 190.08 14.50 -4 0 -2 202.48 14.20 4 0 -2 191.98 13.90 4 0 3 52.89 5.90 -4 0 3 48.80 6.20 4 0 3 42.10 6.60 -4 0 -3 57.59 8.40 4 0 -3 38.00 8.00 4 0 -3 36.00 6.10 4 0 3 47.50 6.30 4 0 3 54.19 4.90 -4 0 -3 42.60 4.70 -4 0 3 50.99 5.80 -4 0 -3 42.60 5.40 -4 0 3 44.70 7.90 -4 0 3 43.30 5.90 4 0 -3 40.90 6.70 -4 0 3 47.80 7.60 -4 0 -3 57.49 7.50 4 0 -3 38.50 9.50 -4 0 -4 613.54 36.60 -4 0 -4 628.14 35.10 4 0 4 556.34 33.20 4 0 4 503.75 33.10 4 0 -4 607.24 35.80 4 0 4 619.54 33.70 -4 0 4 641.24 36.10 -4 0 4 613.44 36.20 4 0 -4 587.14 36.70 -4 0 4 644.84 35.50 4 0 -4 589.44 35.70 -4 0 4 558.04 36.30 4 0 -4 650.03 38.50 -4 0 -4 600.44 34.10 -4 0 -4 569.14 33.10 -4 0 4 637.24 36.10 -4 0 5 181.08 15.10 4 0 -5 184.48 15.60 4 0 -5 173.08 14.00 4 0 5 191.68 12.70 -4 0 -5 180.28 13.40 -4 0 -5 202.08 13.60 4 0 -5 169.18 14.80 -4 0 -5 203.28 16.50 4 0 -5 229.48 19.20 -4 0 5 188.28 13.70 -4 0 5 195.68 14.80 4 0 5 196.48 12.80 -4 0 5 185.58 13.50 -4 0 5 166.98 15.80 -4 0 6 37.40 4.30 -4 0 -6 42.90 11.00 -4 0 6 42.70 7.00 -4 0 -6 44.20 4.20 -4 0 6 38.20 5.60 4 0 -6 37.90 5.20 4 0 -6 42.50 5.10 -4 0 -6 32.80 6.40 4 0 -6 24.20 8.00 4 0 6 44.80 5.70 4 0 6 37.90 5.70 -4 0 -6 52.09 5.30 -4 0 -7 32.20 23.70 4 0 -7 28.30 6.80 -4 0 -7 26.60 5.30 4 0 7 30.40 6.00 -4 0 7 24.90 6.40 -4 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33.20 9.20 3 21 -2 17.30 9.00 3 -21 2 13.20 9.70 -3 -21 -2 22.50 5.60 3 21 -2 11.70 8.20 -3 21 2 10.10 11.60 3 -21 2 15.10 8.00 -3 -21 -2 1.20 10.60 -3 21 -2 0.00 8.70 3 -21 -2 6.80 9.20 -3 21 -2 13.80 8.80 -3 -21 2 5.70 7.10 -3 -21 2 5.30 10.20 3 -21 -2 23.30 7.50 3 21 -3 9.40 9.80 3 -21 3 25.80 8.90 3 -21 3 13.10 10.90 -3 -21 -3 0.50 5.40 3 21 -3 -1.10 10.00 -3 -21 -3 22.50 10.60 -3 21 3 7.50 12.20 -3 21 -3 2.70 9.70 -3 -21 3 1.30 10.90 -3 -21 3 11.50 8.20 3 -21 -3 -2.50 7.60 -3 21 -3 11.40 10.10 3 -21 -3 2.10 11.10 -4 21 0 40.60 9.30 4 -21 0 42.60 12.00 -4 -21 0 38.70 11.30 -4 21 0 29.10 9.40 4 -21 1 87.29 9.70 4 21 -1 64.99 9.50 -4 21 1 72.59 9.80 4 21 -1 77.89 13.80 -4 21 1 70.99 11.00 -4 -21 -1 59.89 8.40 4 -21 -1 71.39 9.00 -4 -21 1 53.99 11.00 -4 -21 1 79.29 9.60 4 21 -2 44.10 10.20 4 21 -2 64.89 11.50 4 -21 2 65.59 14.70 -4 21 2 22.20 13.50 -4 -21 -2 48.70 7.30 -4 -21 -2 23.00 11.20 4 -21 -2 53.59 14.60 -4 21 -2 37.90 10.50 -4 21 -2 39.00 10.40 -4 -21 2 70.59 9.50 -4 -21 2 54.59 11.10 0 -22 0 27.30 6.90 0 22 0 27.20 7.80 0 -22 0 32.30 11.50 0 22 -1 0.20 8.30 0 -22 -1 5.50 11.70 0 22 -1 5.70 7.40 0 -22 1 9.30 7.30 0 -22 1 -3.00 9.70 0 -22 -1 19.50 6.30 0 -22 -2 22.00 6.40 0 22 -2 9.90 8.30 0 -22 2 22.00 7.30 0 -22 2 12.80 9.90 0 -22 -2 20.30 11.80 0 22 -2 25.70 8.90 0 -22 3 4.90 11.20 0 -22 3 -3.10 8.40 0 -22 -3 5.10 13.60 0 22 -3 -0.70 9.70 0 22 -3 -4.00 9.20 0 -22 -3 4.60 6.30 -1 -22 0 9.10 9.60 1 -22 0 10.40 6.40 -1 -22 0 8.70 6.00 1 22 0 20.40 7.70 1 22 0 13.10 6.60 -1 22 0 7.20 6.70 1 -22 0 10.40 9.30 1 -22 1 63.89 8.10 -1 -22 -1 64.19 7.70 1 22 -1 49.20 8.20 1 -22 1 36.50 10.90 -1 22 1 67.89 11.10 1 22 -1 55.09 9.40 -1 -22 1 62.89 7.60 -1 22 -1 66.99 9.50 1 -22 -1 36.50 12.60 -1 22 -1 54.89 8.70 1 -22 -1 48.70 7.10 1 22 -2 9.90 8.90 -1 -22 -2 8.20 6.00 1 -22 2 7.80 10.30 1 -22 2 19.80 7.50 1 22 -2 4.10 8.30 -1 -22 -2 5.20 12.90 -1 -22 2 9.50 10.00 -1 22 -2 -0.60 8.60 1 -22 -2 3.30 13.30 -1 22 -2 19.20 9.10 -1 -22 2 12.30 7.40 1 -22 -2 14.50 6.00 1 22 -3 -1.10 9.70 -1 -22 -3 8.90 5.90 1 22 -3 2.40 9.70 1 -22 3 14.80 8.60 -1 -22 -3 0.70 13.00 1 -22 3 15.60 11.60 -1 22 -3 -9.30 9.60 -1 22 -3 -5.30 9.60 -1 -22 3 18.70 12.20 1 -22 -3 31.20 13.70 -1 -22 3 1.90 8.50 1 -22 -3 5.90 6.80 -2 22 0 29.70 8.70 -2 -22 0 35.50 9.90 2 22 0 53.59 13.30 -2 22 0 25.80 7.40 2 -22 0 47.40 7.60 2 -22 0 22.60 9.00 -2 -22 0 41.20 7.00 -2 22 1 34.30 11.90 2 -22 1 9.50 9.40 2 -22 1 33.80 9.30 -2 -22 -1 17.30 10.90 2 22 -1 10.30 7.80 2 22 -1 16.50 8.60 -2 -22 -1 23.00 6.30 -2 22 -1 15.10 8.80 -2 -22 1 26.50 7.30 -2 22 -1 15.00 8.20 2 -22 -1 32.80 8.70 -2 -22 1 13.90 11.30 2 -22 -1 11.70 12.40 -2 -22 -2 9.70 5.80 2 22 -2 7.60 9.50 -2 22 2 -7.40 10.50 2 -22 2 19.50 8.20 -2 -22 -2 7.00 11.40 2 22 -2 -3.30 9.00 2 -22 2 20.30 10.60 2 -22 -2 12.00 10.40 -2 -22 2 15.70 10.80 -2 -22 2 3.50 7.40 2 -22 -2 20.00 7.30 -2 22 -2 7.70 9.30 -2 22 -2 1.00 9.00 2 22 -3 1.60 10.30 2 22 -3 12.50 10.50 -2 -22 -3 5.70 5.80 -2 22 3 2.00 12.80 -2 -22 -3 28.10 11.40 2 -22 -3 6.70 14.60 -2 22 -3 18.80 10.40 -2 22 -3 5.10 9.80 2 -22 -3 30.30 8.30 -2 -22 3 29.30 13.60 3 -22 0 18.10 10.40 -3 22 0 32.10 9.10 -3 22 0 37.10 9.40 -3 -22 0 13.30 10.90 -3 -22 0 31.20 7.50 3 -22 0 49.60 8.20 3 22 -1 45.10 9.40 3 -22 1 53.89 9.10 3 22 -1 39.50 10.60 -3 -22 -1 26.80 12.00 3 -22 1 19.30 10.90 -3 -22 -1 39.90 7.80 -3 -22 1 54.69 8.10 -3 22 -1 46.90 12.60 -3 -22 1 35.30 12.00 -3 22 -1 27.60 9.50 -3 22 2 -0.70 12.00 -3 -22 -2 0.20 12.30 -3 -22 -2 10.70 6.30 3 22 -2 0.30 9.50 3 22 -2 20.90 11.40 3 -22 2 12.50 9.10 -3 22 -2 6.90 10.20 3 -22 -2 5.40 8.30 -3 22 -2 8.40 10.50 3 -22 -2 13.60 11.80 -3 -22 2 22.60 12.10 0 -23 0 3.20 11.30 0 23 0 -6.00 12.60 0 -23 0 -1.40 7.10 0 -23 1 73.59 10.30 0 23 -1 51.09 10.80 0 -23 -1 54.99 7.80 0 -23 2 15.00 12.60 0 23 -2 6.50 10.30 0 -23 2 18.50 9.90 0 -23 -2 28.70 8.10 0 -23 -2 0.50 15.30 0 23 -2 6.00 9.60 1 -23 0 17.30 11.40 1 -23 0 5.60 8.20 -1 -23 0 -2.70 10.60 -1 -23 0 17.80 7.50 -1 23 0 18.10 8.30 -1 23 0 17.20 10.30 1 23 -1 20.10 8.70 1 -23 1 21.70 8.80 -1 -23 -1 20.90 11.20 1 -23 1 13.30 11.30 1 23 -1 33.20 10.60 -1 23 -1 22.10 8.50 1 -23 -1 30.40 7.50 -1 23 -1 5.60 9.90 -1 -23 1 16.70 7.60 1 -23 -1 12.80 13.70 -1 -23 1 23.00 11.60 1 23 -2 6.40 10.50 1 -23 2 -10.20 14.80 -1 -23 -2 8.80 7.00 -1 -23 -2 13.40 14.20 1 -23 2 14.10 13.30 1 23 -2 10.30 9.70 -1 -23 2 16.80 12.70 -1 23 -2 -0.30 10.60 -1 23 -2 -2.10 9.50 1 -23 -2 20.30 7.90 1 -23 -2 8.20 14.00 -2 23 0 48.60 13.00 -2 -23 0 34.30 9.00 -2 -23 0 20.50 13.00 2 -23 0 40.20 10.30 2 -23 1 11.60 11.50 2 23 -1 20.70 18.30 2 23 -1 10.60 8.60 -2 -23 -1 -4.10 12.00 -2 -23 -1 23.40 7.40 -2 -23 1 19.70 12.80 -2 -23 1 32.20 12.90 -2 23 -1 18.40 10.30 -2 23 -1 3.30 9.60 2 -23 -1 40.40 15.30 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 64015 _shelx_res_file ; TITL MBAT_a.res in P2(1)2(1)2 Z=2 C8 H12 B O6, 4(H2 O) shelx.res created by SHELXL-2018/3 at 16:34:28 on 26-Jun-2019 CELL 0.71073 7.0809 16.7912 6.5001 90.000 90.000 90.000 ZERR 2.00 0.0001 0.0003 0.0001 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O B UNIT 16 40 20 2 MERG 2 OMIT -3.00 54.00 OMIT 0 0 1 OMIT 2 0 0 OMIT 0 2 2 HTAB O4 O3 EQIV $1 -x+1, -y+1, z-1 HTAB O5 O2_$1 EQIV $2 -x+1/2, y-1/2, -z+1 HTAB O5 O2_$2 HTAB O4 O5 DFIX 0.9 0.02 O4 H1 O4 H2 O5 H3 O5 H4 DFIX 1.48 0.02 H1 H2 H3 H4 FMAP 2 PLAN 20 SIZE 0.10 0.15 0.15 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.044400 0.107100 EXTI 0.264978 FVAR 2.58176 B1 4 0.500000 0.500000 0.621599 10.50000 0.05107 0.03155 = 0.05106 0.00000 0.00000 0.00681 C1 1 0.460374 0.629077 0.733473 11.00000 0.04581 0.03077 = 0.05837 0.00086 0.00078 0.00523 C2 1 0.303940 0.613350 0.580201 11.00000 0.04654 0.02984 = 0.05891 0.00005 -0.00175 0.00855 C3 1 0.114825 0.610577 0.690790 11.00000 0.04978 0.06637 = 0.09936 -0.00733 0.01005 0.00002 AFIX 33 H3A 2 0.085017 0.662541 0.743128 11.00000 -1.50000 H3B 2 0.018307 0.594026 0.596294 11.00000 -1.50000 H3C 2 0.121754 0.573415 0.802770 11.00000 -1.50000 AFIX 0 C4 1 0.305245 0.673959 0.406586 11.00000 0.08583 0.05341 = 0.07215 0.01649 -0.00644 0.01459 AFIX 33 H4A 2 0.273454 0.725527 0.460141 11.00000 -1.50000 H4B 2 0.428708 0.675832 0.345758 11.00000 -1.50000 H4C 2 0.214397 0.658807 0.304184 11.00000 -1.50000 AFIX 0 O1 3 0.568717 0.566353 0.755803 11.00000 0.05512 0.03532 = 0.06831 -0.00360 -0.01471 0.01248 O2 3 0.486132 0.691071 0.828678 11.00000 0.06513 0.03604 = 0.08699 -0.01315 -0.01238 0.00825 O3 3 0.351615 0.535884 0.500252 11.00000 0.06403 0.03699 = 0.06400 -0.00907 -0.01579 0.01601 O4 3 0.163785 0.479425 0.180235 11.00000 0.06866 0.06309 = 0.06732 -0.01560 -0.00775 0.00981 O5 3 0.229928 0.329199 0.125046 11.00000 0.08203 0.04208 = 0.10980 -0.00424 0.03353 -0.01004 H1 2 0.222780 0.490666 0.298818 11.00000 0.12382 H2 2 0.179691 0.425949 0.152719 11.00000 0.13162 H3 2 0.319229 0.322008 0.031737 11.00000 0.10334 H4 2 0.160084 0.287072 0.146231 11.00000 0.10948 HKLF 4 REM MBAT_a.res in P2(1)2(1)2 Z=2 C8 H12 B O6, 4(H2 O) REM wR2 = 0.0942, GooF = S = 1.081, Restrained GooF = 1.080 for all data REM R1 = 0.0360 for 1585 Fo > 4sig(Fo) and 0.0383 for all 1680 data REM 104 parameters refined using 6 restraints END WGHT 0.0444 0.1071 REM Highest difference peak 0.208, deepest hole -0.118, 1-sigma level 0.028 Q1 1 0.0000 0.5000 0.1862 10.50000 0.05 0.21 Q2 1 0.1212 0.4536 0.2894 11.00000 0.05 0.15 Q3 1 0.1687 0.3275 0.0130 11.00000 0.05 0.12 Q4 1 0.3330 0.6411 0.4985 11.00000 0.05 0.11 Q5 1 0.5514 0.5877 0.7508 11.00000 0.05 0.09 Q6 1 0.2179 0.6189 0.6177 11.00000 0.05 0.08 Q7 1 0.5941 0.5647 0.6144 11.00000 0.05 0.08 Q8 1 0.3672 0.7292 0.4743 11.00000 0.05 0.08 Q9 1 0.4912 0.6888 0.7095 11.00000 0.05 0.08 Q10 1 0.5222 0.5408 0.6836 11.00000 0.05 0.08 Q11 1 0.5048 0.5776 0.8354 11.00000 0.05 0.08 Q12 1 0.3760 0.5275 0.6140 11.00000 0.05 0.08 Q13 1 0.2200 0.4897 -0.0115 11.00000 0.05 0.07 Q14 1 0.1565 0.7150 0.5713 11.00000 0.05 0.07 Q15 1 0.0729 0.7140 0.6637 11.00000 0.05 0.07 Q16 1 0.5692 0.5482 0.6424 11.00000 0.05 0.07 Q17 1 0.4071 0.6332 0.6214 11.00000 0.05 0.07 Q18 1 0.1213 0.7607 0.5863 11.00000 0.05 0.07 Q19 1 0.3001 0.4823 0.0122 11.00000 0.05 0.07 Q20 1 0.0286 0.6190 0.5567 11.00000 0.05 0.07 ; _shelx_res_checksum 56904 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 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 B B1 0.500000 0.500000 0.6216(5) 0.0446(7) Uani d 1 C C1 0.4604(3) 0.62908(10) 0.7335(3) 0.0450(5) Uani d 1 C C2 0.3039(3) 0.61335(11) 0.5802(3) 0.0451(5) Uani d 1 C C3 0.1148(3) 0.61058(17) 0.6908(5) 0.0718(7) Uani d 1 H H3A 0.085017 0.662541 0.743128 0.108 Uiso calc 1 H H3B 0.018307 0.594026 0.596294 0.108 Uiso calc 1 H H3C 0.121754 0.573415 0.802770 0.108 Uiso calc 1 C C4 0.3052(5) 0.67396(15) 0.4066(4) 0.0705(7) Uani d 1 H H4A 0.273454 0.725527 0.460141 0.106 Uiso calc 1 H H4B 0.428708 0.675832 0.345758 0.106 Uiso calc 1 H H4C 0.214397 0.658807 0.304184 0.106 Uiso calc 1 O O1 0.5687(2) 0.56635(8) 0.7558(3) 0.0529(4) Uani d 1 O O2 0.4861(3) 0.69107(8) 0.8287(3) 0.0627(5) Uani d 1 O O3 0.3516(2) 0.53588(8) 0.5003(3) 0.0550(4) Uani d 1 O O4 0.1638(3) 0.47942(11) 0.1802(3) 0.0664(5) Uani d 1 O O5 0.2299(3) 0.32920(10) 0.1250(4) 0.0780(6) Uani d 1 H H1 0.223(6) 0.491(2) 0.299(5) 0.124(14) Uiso d 1 H H2 0.180(6) 0.4259(15) 0.153(7) 0.132(16) Uiso d 1 H H3 0.319(4) 0.322(2) 0.032(5) 0.103(12) Uiso d 1 H H4 0.160(5) 0.2871(18) 0.146(6) 0.109(12) 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 B1 0.0511(17) 0.0316(13) 0.0511(16) 0.0068(12) 0.000 0.000 C1 0.0458(10) 0.0308(8) 0.0584(10) 0.0052(7) 0.0008(8) 0.0009(7) C2 0.0465(10) 0.0298(8) 0.0589(11) 0.0086(7) -0.0018(9) 0.0000(8) C3 0.0498(13) 0.0664(15) 0.0994(19) 0.0000(11) 0.0100(13) -0.0073(14) C4 0.0858(18) 0.0534(13) 0.0721(15) 0.0146(12) -0.0064(14) 0.0165(11) O1 0.0551(8) 0.0353(7) 0.0683(9) 0.0125(6) -0.0147(7) -0.0036(6) O2 0.0651(10) 0.0360(7) 0.0870(11) 0.0082(7) -0.0124(9) -0.0131(7) O3 0.0640(9) 0.0370(7) 0.0640(9) 0.0160(6) -0.0158(7) -0.0091(7) O4 0.0687(11) 0.0631(11) 0.0673(10) 0.0098(8) -0.0077(8) -0.0156(8) O5 0.0820(13) 0.0421(9) 0.1098(16) -0.0100(8) 0.0335(12) -0.0042(9) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 O3 B1 O3 2_665 . 113.9(2) O3 B1 O1 2_665 . 113.09(9) O3 B1 O1 . . 104.13(7) O3 B1 O1 2_665 2_665 104.13(7) O3 B1 O1 . 2_665 113.09(9) O1 B1 O1 . 2_665 108.7(2) O2 C1 O1 . . 122.67(19) O2 C1 C2 . . 126.17(17) O1 C1 C2 . . 111.17(16) O3 C2 C1 . . 102.92(15) O3 C2 C4 . . 109.59(18) C1 C2 C4 . . 111.57(19) O3 C2 C3 . . 110.44(18) C1 C2 C3 . . 109.80(18) C4 C2 C3 . . 112.1(2) C2 C3 H3A . . 109.5 C2 C3 H3B . . 109.5 H3A C3 H3B . . 109.5 C2 C3 H3C . . 109.5 H3A C3 H3C . . 109.5 H3B C3 H3C . . 109.5 C2 C4 H4A . . 109.5 C2 C4 H4B . . 109.5 H4A C4 H4B . . 109.5 C2 C4 H4C . . 109.5 H4A C4 H4C . . 109.5 H4B C4 H4C . . 109.5 C1 O1 B1 . . 110.08(14) C2 O3 B1 . . 110.48(14) H1 O4 H2 . . 108(3) H3 O5 H4 . . 114(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance B1 O3 2_665 1.445(2) B1 O3 . 1.445(2) B1 O1 . 1.496(2) B1 O1 2_665 1.496(2) C1 O2 . 1.225(2) C1 O1 . 1.311(2) C1 C2 . 1.513(3) C2 O3 . 1.441(2) C2 C4 . 1.520(3) C2 C3 . 1.521(3) C3 H3A . 0.9600 C3 H3B . 0.9600 C3 H3C . 0.9600 C4 H4A . 0.9600 C4 H4B . 0.9600 C4 H4C . 0.9600 O4 H1 . 0.90(2) O4 H2 . 0.92(2) O5 H3 . 0.88(2) O5 H4 . 0.87(2) 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 O4 H1 O3 . 0.90(2) 1.77(2) 2.645(2) 165(4) yes O5 H3 O2 2_664 0.88(2) 1.92(2) 2.805(3) 179(3) yes O5 H4 O2 3_546 0.87(2) 1.92(2) 2.795(2) 175(4) yes O4 H2 O5 . 0.92(2) 1.67(2) 2.591(2) 173(4) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion O2 C1 C2 O3 . 174.2(2) O1 C1 C2 O3 . -6.5(2) O2 C1 C2 C4 . 56.7(3) O1 C1 C2 C4 . -123.9(2) O2 C1 C2 C3 . -68.2(3) O1 C1 C2 C3 . 111.1(2) O2 C1 O1 B1 . 179.2(2) C2 C1 O1 B1 . -0.2(2) O3 B1 O1 C1 2_665 130.86(18) O3 B1 O1 C1 . 6.8(2) O1 B1 O1 C1 2_665 -114.04(16) C1 C2 O3 B1 . 10.8(2) C4 C2 O3 B1 . 129.6(2) C3 C2 O3 B1 . -106.4(2) O3 B1 O3 C2 2_665 -134.64(16) O1 B1 O3 C2 . -11.0(2) O1 B1 O3 C2 2_665 106.76(18) _cod_database_fobs_code 1552105