#------------------------------------------------------------------------------ #$Date: 2026-05-05 23:56:31 +0100 (Tue, 05 May 2026) $ #$Revision: 305876 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720986.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7720986 loop_ _publ_author_name 'Li, Haowen' 'Wang, Xiao' 'Chai, Hui' 'Zhang, Fangfang' _publ_section_title ; Design of borate-squarate hybrid crystals with large birefringence by synergistic assembly of planar π-conjugated groups. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d6dt00783j _journal_year 2026 _chemical_formula_moiety 'C4 H10 B2 Cs2 O12' _chemical_formula_sum 'C4 H10 B2 Cs2 O12' _chemical_formula_weight 537.56 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2026-03-05 _audit_creation_method ; Olex2 1.5 (compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) ; _audit_update_record ; 2026-03-05 deposited with the CCDC. 2026-04-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.4512(6) _cell_length_b 7.0876(2) _cell_length_c 12.3802(4) _cell_measurement_reflns_used 9935 _cell_measurement_temperature 298 _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 2.97 _cell_volume 1443.53(8) _computing_cell_refinement 'SAINT V8.41 (?, 2016)' _computing_data_reduction 'SAINT V8.41 (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 298.00 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21763 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.488 _diffrn_reflns_theta_min 2.874 _exptl_absorpt_coefficient_mu 5.103 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5928 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0849 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.7951. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.473 _exptl_crystal_description block _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.100 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.069 _refine_ls_abs_structure_details ; Flack x determined using 1338 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.009(12) _refine_ls_extinction_coef 0.00048(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/2 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 3303 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0170 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0143P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0359 _reflns_Friedel_coverage 0.899 _reflns_Friedel_fraction_full 0.994 _reflns_Friedel_fraction_max 0.989 _reflns_number_gt 3044 _reflns_number_total 3303 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00783j2.cif _cod_data_source_block Cs_2 _cod_database_code 7720986 _shelx_shelxl_version_number 2019/3 _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_max 0.604 _shelx_estimated_absorpt_t_min 0.535 _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All O(H) groups, All O(H,H) groups 2.a Free rotating group: O2(H2A,H2B) 2.b Idealised tetrahedral OH refined as rotating group: O3(H3), O4(H4), O5(H5), O6(H6), O7(H7), O8(H8) ; _shelx_res_file ; TITL cs_s_a.res in Pca2(1) cs_s.res created by SHELXL-2019/3 at 12:33:01 on 05-Mar-2026 REM Old TITL Cs_s in Pca2(1) REM SHELXT solution in Pca2(1): R1 0.062, Rweak 0.010, Alpha 0.006 REM 0.839 for 185 systematic absences, Orientation as input REM Flack x = 0.038 ( 0.012 ) from 1301 Parsons' quotients REM Formula found by SHELXT: C6 O12 Cs2 CELL 0.71073 16.4512 7.0876 12.3802 90 90 90 ZERR 4 0.0006 0.0002 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H B Cs O UNIT 16 40 8 8 48 L.S. 20 0 0 PLAN 1 SIZE 0.11 0.13 0.14 TEMP 24.85 CONF list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 2 0 0 REM REM REM WGHT 0.014300 EXTI 0.000480 FVAR 0.24419 B1 3 0.910118 0.777389 0.327166 11.00000 0.02561 0.03796 = 0.02676 0.00163 0.00270 -0.00319 B2 3 0.573227 0.269583 0.576038 11.00000 0.02760 0.04761 = 0.02384 0.00079 0.00085 0.00080 C1 1 0.561611 0.769969 0.493785 11.00000 0.02451 0.03449 = 0.02471 -0.00017 0.00101 0.00017 C2 1 0.538152 0.764311 0.380864 11.00000 0.02343 0.03474 = 0.02543 0.00000 -0.00096 -0.00039 C3 1 0.452692 0.743937 0.412161 11.00000 0.02342 0.04439 = 0.02113 0.00183 0.00240 0.00081 C4 1 0.476542 0.749927 0.526989 11.00000 0.02314 0.04118 = 0.02475 0.00091 -0.00267 0.00217 CS1 4 0.770575 0.466852 0.524098 11.00000 0.03109 0.04232 = 0.02985 0.00297 0.00411 -0.00076 CS2 4 0.204200 0.893740 0.271630 11.00000 0.03810 0.04159 = 0.03400 -0.00085 0.00313 0.00030 O1 5 0.713836 0.546444 0.277645 11.00000 0.03579 0.05114 = 0.05237 0.00343 0.00408 0.00425 AFIX 6 O2 5 0.764656 0.022778 0.525145 11.00000 0.02706 0.04037 = 0.04758 -0.01219 0.00997 -0.00151 H2A 2 0.805632 -0.040281 0.504031 11.00000 -1.50000 H2B 2 0.729961 -0.060191 0.543369 11.00000 -1.50000 AFIX 0 O3 5 0.600415 0.282334 0.471743 11.00000 0.02400 0.08431 = 0.02378 0.00148 0.00074 -0.00290 AFIX 147 H3 2 0.561508 0.294008 0.430884 11.00000 -1.50000 AFIX 0 O4 5 0.493336 0.238894 0.594381 11.00000 0.02476 0.08471 = 0.02276 0.00012 0.00041 -0.00665 AFIX 147 H4 2 0.484644 0.240128 0.659597 11.00000 -1.50000 AFIX 0 O5 5 0.630903 0.289043 0.652909 11.00000 0.02766 0.09462 = 0.02294 0.00183 0.00321 -0.00876 AFIX 147 H5 2 0.609927 0.280169 0.712777 11.00000 -1.50000 AFIX 0 O6 5 0.990567 0.758130 0.307118 11.00000 0.02547 0.07940 = 0.02122 -0.00027 0.00109 0.00065 AFIX 147 H6 2 0.997319 0.729562 0.243564 11.00000 -1.50000 AFIX 0 O7 5 0.884580 0.788744 0.434044 11.00000 0.02232 0.06239 = 0.02508 -0.00076 0.00487 -0.00112 AFIX 147 H7 2 0.924312 0.797901 0.473692 11.00000 -1.50000 AFIX 0 O8 5 0.850332 0.790241 0.253034 11.00000 0.02618 0.06111 = 0.02751 0.00001 0.00126 0.00126 AFIX 147 H8 2 0.870357 0.800862 0.192685 11.00000 -1.50000 AFIX 0 O9 5 0.628444 0.784868 0.543292 11.00000 0.02105 0.06464 = 0.03005 -0.00130 -0.00113 -0.00338 O10 5 0.574992 0.773307 0.292147 11.00000 0.02534 0.06172 = 0.01935 0.00219 0.00429 -0.00162 O11 5 0.387466 0.726560 0.362550 11.00000 0.02093 0.09213 = 0.02277 0.00059 -0.00082 -0.00474 O12 5 0.440665 0.738917 0.614580 11.00000 0.02528 0.07314 = 0.02430 0.00028 0.00242 -0.00160 H1A 2 0.659370 0.615350 0.290412 11.00000 0.07193 H1B 2 0.758989 0.639091 0.293950 11.00000 0.11193 HKLF 4 REM cs_s_a.res in Pca2(1) REM wR2 = 0.0359, GooF = S = 1.012, Restrained GooF = 1.012 for all data REM R1 = 0.0170 for 3044 Fo > 4sig(Fo) and 0.0212 for all 3303 data REM 199 parameters refined using 1 restraints END WGHT 0.0143 0.0000 REM Highest difference peak 1.100, deepest hole -0.363, 1-sigma level 0.069 Q1 1 0.7035 0.3844 0.2732 11.00000 0.05 1.10 ; _shelx_res_checksum 45253 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.9101(3) 0.7774(8) 0.3272(4) 0.0301(11) Uani 1 1 d . . . . . B2 B 0.5732(4) 0.2696(9) 0.5760(5) 0.0330(12) Uani 1 1 d . . . . . C1 C 0.5616(3) 0.7700(6) 0.4938(3) 0.0279(10) Uani 1 1 d . . . . . C2 C 0.5382(3) 0.7643(7) 0.3809(4) 0.0279(9) Uani 1 1 d . . . . . C3 C 0.4527(3) 0.7439(7) 0.4122(4) 0.0296(10) Uani 1 1 d . . . . . C4 C 0.4765(2) 0.7499(6) 0.5270(5) 0.0297(8) Uani 1 1 d . . . . . Cs1 Cs 0.77057(2) 0.46685(4) 0.52410(3) 0.03442(8) Uani 1 1 d . . . . . Cs2 Cs 0.20420(2) 0.89374(4) 0.27163(3) 0.03790(8) Uani 1 1 d . . . . . O1 O 0.7138(2) 0.5464(5) 0.2776(5) 0.0464(8) Uani 1 1 d . . . . . O2 O 0.76466(16) 0.0228(4) 0.5251(6) 0.0383(7) Uani 1 1 d G . . . . H2A H 0.805632 -0.040281 0.504031 0.058 Uiso 1 1 d G U . . . H2B H 0.729961 -0.060191 0.543369 0.058 Uiso 1 1 d G U . . . O3 O 0.6004(2) 0.2823(7) 0.4717(3) 0.0440(10) Uani 1 1 d . . . . . H3 H 0.561508 0.294008 0.430884 0.066 Uiso 1 1 calc R U . . . O4 O 0.4933(2) 0.2389(6) 0.5944(3) 0.0441(9) Uani 1 1 d . . . . . H4 H 0.484644 0.240128 0.659597 0.066 Uiso 1 1 calc R U . . . O5 O 0.6309(2) 0.2890(7) 0.6529(3) 0.0484(10) Uani 1 1 d . . . . . H5 H 0.609927 0.280169 0.712777 0.073 Uiso 1 1 calc R U . . . O6 O 0.99057(19) 0.7581(7) 0.3071(3) 0.0420(9) Uani 1 1 d . . . . . H6 H 0.997319 0.729562 0.243564 0.063 Uiso 1 1 calc R U . . . O7 O 0.88458(18) 0.7887(6) 0.4340(3) 0.0366(8) Uani 1 1 d . . . . . H7 H 0.924312 0.797901 0.473692 0.055 Uiso 1 1 calc R U . . . O8 O 0.85033(18) 0.7902(5) 0.2530(3) 0.0383(8) Uani 1 1 d . . . . . H8 H 0.870357 0.800862 0.192685 0.057 Uiso 1 1 calc R U . . . O9 O 0.62844(18) 0.7849(5) 0.5433(3) 0.0386(8) Uani 1 1 d . . . . . O10 O 0.57499(18) 0.7733(5) 0.2921(3) 0.0355(8) Uani 1 1 d . . . . . O11 O 0.3875(2) 0.7266(7) 0.3626(3) 0.0453(10) Uani 1 1 d . . . . . O12 O 0.4407(2) 0.7389(6) 0.6146(3) 0.0409(10) Uani 1 1 d . . . . . H1A H 0.659(4) 0.615(8) 0.290(7) 0.07(2) Uiso 1 1 d . . . . . H1B H 0.759(6) 0.639(10) 0.294(9) 0.11(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 B1 0.026(2) 0.038(3) 0.027(3) 0.002(2) 0.003(2) -0.003(2) B2 0.028(3) 0.048(3) 0.024(3) 0.001(2) 0.001(2) 0.001(2) C1 0.025(2) 0.034(2) 0.025(2) -0.0002(17) 0.0010(16) 0.0002(18) C2 0.023(2) 0.035(2) 0.025(2) 0.0000(19) -0.0010(17) -0.0004(17) C3 0.023(2) 0.044(3) 0.021(2) 0.002(2) 0.0024(19) 0.001(2) C4 0.0231(18) 0.041(2) 0.025(2) 0.001(2) -0.003(2) 0.0022(15) Cs1 0.03109(13) 0.04232(14) 0.02985(14) 0.00297(17) 0.0041(2) -0.00076(10) Cs2 0.03810(15) 0.04159(14) 0.03400(15) -0.00085(16) 0.00313(14) 0.00030(13) O1 0.0358(17) 0.051(2) 0.052(2) 0.003(3) 0.0041(19) 0.0042(16) O2 0.0271(13) 0.0404(15) 0.0476(18) -0.012(3) 0.010(3) -0.0015(13) O3 0.0240(17) 0.084(3) 0.0238(18) 0.0015(18) 0.0007(15) -0.0029(19) O4 0.0248(17) 0.085(3) 0.0228(19) 0.0001(18) 0.0004(14) -0.0066(17) O5 0.0277(19) 0.095(3) 0.0229(18) 0.0018(19) 0.0032(15) -0.0088(19) O6 0.0255(16) 0.079(3) 0.0212(17) -0.0003(15) 0.0011(13) 0.0006(16) O7 0.0223(16) 0.062(2) 0.0251(17) -0.0008(16) 0.0049(13) -0.0011(15) O8 0.0262(15) 0.061(2) 0.028(2) 0.0000(16) 0.0013(14) 0.0013(15) O9 0.0210(14) 0.065(2) 0.030(2) -0.0013(17) -0.0011(14) -0.0034(13) O10 0.0253(15) 0.062(2) 0.019(2) 0.0022(15) 0.0043(13) -0.0016(14) O11 0.0209(16) 0.092(3) 0.0228(19) 0.0006(19) -0.0008(13) -0.0047(17) O12 0.0253(18) 0.073(3) 0.0243(19) 0.0003(17) 0.0024(15) -0.0016(17) 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 B1 O7 118.4(4) . . ? O8 B1 O6 126.5(5) . . ? O8 B1 O7 115.0(4) . . ? O3 B2 Cs1 60.7(3) . . ? O4 B2 Cs1 166.3(4) . . ? O4 B2 O3 119.1(5) . . ? O5 B2 Cs1 56.7(3) . . ? O5 B2 O3 115.3(5) . . ? O5 B2 O4 125.5(5) . . ? C2 C1 C4 90.8(4) . . ? O9 C1 C2 134.5(4) . . ? O9 C1 C4 134.7(4) . . ? C1 C2 C3 90.2(4) . . ? C1 C2 Cs2 97.5(3) . 3_575 ? C3 C2 Cs2 145.7(3) . 3_575 ? O10 C2 C1 135.5(4) . . ? O10 C2 C3 134.4(4) . . ? O10 C2 Cs2 47.6(2) . 3_575 ? C2 C3 C4 89.8(3) . . ? C2 C3 Cs1 159.2(4) . 3_465 ? C4 C3 Cs1 82.1(2) . 3_465 ? O11 C3 C2 135.0(5) . . ? O11 C3 C4 135.1(4) . . ? O11 C3 Cs1 55.5(3) . 3_465 ? C1 C4 C3 89.2(4) . . ? C1 C4 Cs1 155.1(3) . 3_465 ? C3 C4 Cs1 74.7(2) . 3_465 ? O12 C4 C1 135.0(5) . . ? O12 C4 C3 135.7(4) . . ? O12 C4 Cs1 63.1(2) . 3_465 ? B2 Cs1 C3 130.93(13) . 3_565 ? B2 Cs1 C4 131.34(12) . 3_565 ? B2 Cs1 H1B 105.2(17) . . ? C3 Cs1 C4 23.13(12) 3_565 3_565 ? C3 Cs1 H1B 82.1(16) 3_565 . ? C4 Cs1 H1B 103.1(16) 3_565 . ? O1 Cs1 B2 88.02(12) 4_655 . ? O1 Cs1 B2 88.62(12) . . ? O1 Cs1 C3 87.12(10) . 3_565 ? O1 Cs1 C3 112.44(10) 4_655 3_565 ? O1 Cs1 C4 89.45(11) 4_655 3_565 ? O1 Cs1 C4 110.08(11) . 3_565 ? O1 Cs1 O1 156.38(11) 4_655 . ? O1 Cs1 O9 75.01(10) . . ? O1 Cs1 O9 82.18(9) 4_655 . ? O1 Cs1 O12 71.43(9) 4_655 3_565 ? O1 Cs1 O12 129.17(9) . 3_565 ? O1 Cs1 H1B 146.7(16) 4_655 . ? O1 Cs1 H1B 18.2(17) . . ? O2 Cs1 B2 65.31(11) . . ? O2 Cs1 C3 67.36(11) . 3_565 ? O2 Cs1 C4 67.38(8) . 3_565 ? O2 Cs1 O1 99.73(16) . . ? O2 Cs1 O1 100.06(16) . 4_655 ? O2 Cs1 O3 63.86(10) . . ? O2 Cs1 O7 137.92(10) . . ? O2 Cs1 O9 132.02(8) . . ? O2 Cs1 O12 65.74(10) . 3_565 ? O2 Cs1 H1B 113.3(16) . . ? O3 Cs1 B2 22.22(11) . . ? O3 Cs1 C3 118.94(11) . 3_565 ? O3 Cs1 C4 129.68(11) . 3_565 ? O3 Cs1 O1 67.87(10) . . ? O3 Cs1 O1 110.21(9) . 4_655 ? O3 Cs1 O9 70.43(10) . . ? O3 Cs1 O12 129.00(11) . 3_565 ? O3 Cs1 H1B 85.4(17) . . ? O5 Cs1 B2 21.61(12) . . ? O5 Cs1 C3 130.45(12) . 3_565 ? O5 Cs1 C4 120.50(11) . 3_565 ? O5 Cs1 O1 110.20(10) . . ? O5 Cs1 O1 67.82(10) . 4_655 ? O5 Cs1 O2 64.16(13) . . ? O5 Cs1 O3 43.31(11) . . ? O5 Cs1 O7 157.74(11) . . ? O5 Cs1 O9 73.06(11) . . ? O5 Cs1 O11 128.27(12) . 3_565 ? O5 Cs1 O12 105.85(11) . 3_565 ? O5 Cs1 H1B 126.3(17) . . ? O7 Cs1 B2 151.80(12) . . ? O7 Cs1 C3 70.83(10) . 3_565 ? O7 Cs1 C4 76.16(9) . 3_565 ? O7 Cs1 O1 73.31(9) . . ? O7 Cs1 O1 99.87(9) . 4_655 ? O7 Cs1 O3 138.91(10) . . ? O7 Cs1 O9 87.26(9) . . ? O7 Cs1 O12 86.35(10) . 3_565 ? O7 Cs1 H1B 55.1(17) . . ? O9 Cs1 B2 66.89(12) . . ? O9 Cs1 C3 155.10(10) . 3_565 ? O9 Cs1 C4 159.89(9) . 3_565 ? O9 Cs1 O12 151.30(9) . 3_565 ? O9 Cs1 H1B 75.6(15) . . ? O11 Cs1 B2 120.32(13) 3_565 . ? O11 Cs1 C3 19.33(10) 3_565 3_565 ? O11 Cs1 C4 42.05(11) 3_565 3_565 ? O11 Cs1 O1 131.48(9) 3_565 4_655 ? O11 Cs1 O1 69.36(10) 3_565 . ? O11 Cs1 O2 65.11(14) 3_565 . ? O11 Cs1 O3 103.58(10) 3_565 . ? O11 Cs1 O7 73.90(11) 3_565 . ? O11 Cs1 O9 143.12(10) 3_565 . ? O11 Cs1 O12 60.26(9) 3_565 3_565 ? O11 Cs1 H1B 67.6(15) 3_565 . ? O12 Cs1 B2 121.72(12) 3_565 . ? O12 Cs1 C3 42.04(9) 3_565 3_565 ? O12 Cs1 C4 19.24(11) 3_565 3_565 ? O12 Cs1 H1B 122.0(16) 3_565 . ? C2 Cs2 Cs1 137.25(7) 3_475 2_664 ? O1 Cs2 C2 130.44(11) 3_465 3_475 ? O1 Cs2 Cs1 51.46(11) 3_465 2_664 ? O1 Cs2 O2 101.68(13) 3_465 2_664 ? O1 Cs2 O2 98.00(11) 3_465 3_465 ? O1 Cs2 O3 68.03(13) 3_465 3_465 ? O1 Cs2 O5 65.34(11) 3_465 2_664 ? O1 Cs2 O6 77.54(10) 3_465 1_455 ? O1 Cs2 O8 130.06(9) 3_465 3_475 ? O1 Cs2 O10 140.48(9) 3_465 3_475 ? O1 Cs2 O11 66.58(11) 3_465 . ? O1 Cs2 O12 73.48(12) 3_465 4_554 ? O2 Cs2 C2 76.86(8) 3_465 3_475 ? O2 Cs2 C2 109.49(9) 2_664 3_475 ? O2 Cs2 Cs1 50.43(6) 2_664 2_664 ? O2 Cs2 Cs1 143.00(5) 3_465 2_664 ? O2 Cs2 O2 145.82(6) 2_664 3_465 ? O2 Cs2 O3 153.37(9) 2_664 3_465 ? O2 Cs2 O5 61.01(9) 2_664 2_664 ? O2 Cs2 O5 103.86(8) 3_465 2_664 ? O2 Cs2 O6 108.72(7) 2_664 1_455 ? O2 Cs2 O6 102.63(8) 3_465 1_455 ? O2 Cs2 O8 71.69(9) 2_664 3_475 ? O2 Cs2 O10 92.67(8) 2_664 3_475 ? O2 Cs2 O11 59.45(8) 3_465 . ? O2 Cs2 O11 103.88(8) 2_664 . ? O2 Cs2 O12 66.74(9) 2_664 4_554 ? O3 Cs2 C2 66.84(10) 3_465 3_475 ? O3 Cs2 Cs1 113.02(8) 3_465 2_664 ? O3 Cs2 O2 60.66(9) 3_465 3_465 ? O3 Cs2 O5 127.64(11) 3_465 2_664 ? O3 Cs2 O6 46.10(8) 3_465 1_455 ? O3 Cs2 O8 134.13(9) 3_465 3_475 ? O3 Cs2 O11 94.52(9) 3_465 . ? O3 Cs2 O12 86.65(9) 3_465 4_554 ? O5 Cs2 C2 164.18(11) 2_664 3_475 ? O5 Cs2 Cs1 48.24(7) 2_664 2_664 ? O5 Cs2 O6 136.68(10) 2_664 1_455 ? O5 Cs2 O11 45.39(9) 2_664 . ? O6 Cs2 C2 56.61(10) 1_455 3_475 ? O6 Cs2 Cs1 91.36(7) 1_455 2_664 ? O8 Cs2 C2 96.49(9) 3_475 3_475 ? O8 Cs2 Cs1 107.72(6) 3_475 2_664 ? O8 Cs2 O2 74.23(8) 3_475 3_465 ? O8 Cs2 O5 68.95(10) 3_475 2_664 ? O8 Cs2 O6 152.30(10) 3_475 1_455 ? O8 Cs2 O11 67.43(10) 3_475 . ? O10 Cs2 C2 16.94(9) 3_475 3_475 ? O10 Cs2 Cs1 126.99(6) 3_475 2_664 ? O10 Cs2 O2 89.57(8) 3_475 3_465 ? O10 Cs2 O3 82.73(10) 3_475 3_465 ? O10 Cs2 O5 149.61(10) 3_475 2_664 ? O10 Cs2 O6 62.97(9) 3_475 1_455 ? O10 Cs2 O8 89.36(9) 3_475 3_475 ? O10 Cs2 O11 144.71(10) 3_475 . ? O10 Cs2 O12 79.02(9) 3_475 4_554 ? O11 Cs2 C2 135.87(9) . 3_475 ? O11 Cs2 Cs1 86.54(7) . 2_664 ? O11 Cs2 O6 135.41(10) . 1_455 ? O12 Cs2 C2 84.49(10) 4_554 3_475 ? O12 Cs2 Cs1 53.60(7) 4_554 2_664 ? O12 Cs2 O2 146.62(9) 4_554 3_465 ? O12 Cs2 O5 101.54(9) 4_554 2_664 ? O12 Cs2 O6 44.31(8) 4_554 1_455 ? O12 Cs2 O8 136.02(9) 4_554 3_475 ? O12 Cs2 O11 136.13(11) 4_554 . ? Cs1 O1 Cs1 150.46(13) 4_654 . ? Cs1 O1 H1A 108(5) 4_654 . ? Cs1 O1 H1A 101(5) . . ? Cs1 O1 H1B 105(6) 4_654 . ? Cs1 O1 H1B 73(6) . . ? Cs2 O1 Cs1 78.73(11) 3_565 4_654 ? Cs2 O1 Cs1 82.14(10) 3_565 . ? Cs2 O1 H1A 116(3) 3_565 . ? Cs2 O1 H1B 134(5) 3_565 . ? H1A O1 H1B 107(6) . . ? Cs1 O2 Cs2 79.12(12) . 2_665 ? Cs1 O2 Cs2 80.13(13) . 3_565 ? Cs1 O2 H2A 120.0 . . ? Cs1 O2 H2B 135.5 . . ? Cs2 O2 Cs2 157.51(10) 2_665 3_565 ? Cs2 O2 H2A 92.3 3_565 . ? Cs2 O2 H2A 105.5 2_665 . ? Cs2 O2 H2B 89.0 2_665 . ? Cs2 O2 H2B 99.9 3_565 . ? H2A O2 H2B 104.5 . . ? B2 O3 Cs1 97.1(3) . . ? B2 O3 Cs2 149.7(4) . 3_565 ? B2 O3 H3 109.5 . . ? Cs1 O3 Cs2 81.38(8) . 3_565 ? Cs1 O3 H3 141.0 . . ? Cs2 O3 H3 88.8 3_565 . ? B2 O4 H4 109.5 . . ? B2 O5 Cs1 101.6(3) . . ? B2 O5 Cs2 147.1(4) . 2_665 ? B2 O5 H5 109.5 . . ? Cs1 O5 Cs2 77.30(8) . 2_665 ? Cs1 O5 H5 144.7 . . ? Cs2 O5 H5 85.1 2_665 . ? B1 O6 Cs2 158.7(4) . 1_655 ? B1 O6 H6 109.5 . . ? Cs2 O6 H6 79.6 1_655 . ? B1 O7 Cs1 118.3(3) . . ? B1 O7 H7 109.5 . . ? Cs1 O7 H7 108.6 . . ? B1 O8 Cs2 122.1(3) . 3_575 ? B1 O8 H8 109.5 . . ? Cs2 O8 H8 107.1 3_575 . ? C1 O9 Cs1 122.1(3) . . ? C2 O10 Cs2 115.4(3) . 3_575 ? C3 O11 Cs1 105.1(3) . 3_465 ? C3 O11 Cs2 152.5(4) . . ? Cs1 O11 Cs2 79.57(7) 3_465 . ? C4 O12 Cs1 97.6(3) . 3_465 ? C4 O12 Cs2 148.1(3) . 4 ? Cs2 O12 Cs1 74.67(8) 4 3_465 ? 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 B1 O6 1.353(6) . ? B1 O7 1.391(6) . ? B1 O8 1.348(6) . ? B2 Cs1 3.593(6) . ? B2 O3 1.369(7) . ? B2 O4 1.351(7) . ? B2 O5 1.351(7) . ? C1 C2 1.451(6) . ? C1 C4 1.466(6) . ? C1 O9 1.263(5) . ? C2 C3 1.465(6) . ? C2 Cs2 3.894(5) 3_575 ? C2 O10 1.256(6) . ? C3 C4 1.475(7) . ? C3 Cs1 3.623(5) 3_465 ? C3 O11 1.242(6) . ? C4 Cs1 3.721(4) 3_465 ? C4 O12 1.237(7) . ? Cs1 O1 3.240(6) . ? Cs1 O1 3.200(6) 4_655 ? Cs1 O2 3.149(3) . ? Cs1 O3 3.157(4) . ? Cs1 O5 3.068(4) . ? Cs1 O7 3.157(4) . ? Cs1 O9 3.256(3) . ? Cs1 O11 3.095(4) 3_565 ? Cs1 O12 3.348(4) 3_565 ? Cs1 H1B 3.11(11) . ? Cs2 O1 3.125(4) 3_465 ? Cs2 O2 3.150(8) 2_664 ? Cs2 O2 3.345(8) 3_465 ? Cs2 O3 3.257(4) 3_465 ? Cs2 O5 3.346(4) 2_664 ? Cs2 O6 3.670(3) 1_455 ? Cs2 O8 3.294(3) 3_475 ? Cs2 O10 3.186(3) 3_475 ? Cs2 O11 3.429(4) . ? Cs2 O12 3.266(4) 4_554 ? O1 H1A 1.03(6) . ? O1 H1B 1.01(9) . ? O2 H2A 0.8500 . ? O2 H2B 0.8500 . ? O3 H3 0.8200 . ? O4 H4 0.8200 . ? O5 H5 0.8200 . ? O6 H6 0.8200 . ? O7 H7 0.8200 . ? O8 H8 0.8200 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 0.1(4) . . . . ? C1 C2 C3 Cs1 -66.7(10) . . . 3_465 ? C1 C2 C3 O11 -179.2(7) . . . . ? C1 C2 O10 Cs2 -47.6(7) . . . 3_575 ? C1 C4 O12 Cs1 -158.7(5) . . . 3_465 ? C1 C4 O12 Cs2 128.1(5) . . . 4 ? C2 C1 C4 C3 0.1(4) . . . . ? C2 C1 C4 Cs1 49.2(8) . . . 3_465 ? C2 C1 C4 O12 178.8(6) . . . . ? C2 C1 O9 Cs1 -63.3(6) . . . . ? C2 C3 C4 C1 -0.1(4) . . . . ? C2 C3 C4 Cs1 -160.8(3) . . . 3_465 ? C2 C3 C4 O12 -178.8(6) . . . . ? C2 C3 O11 Cs1 156.6(6) . . . 3_465 ? C2 C3 O11 Cs2 -106.9(8) . . . . ? C3 C2 O10 Cs2 132.2(6) . . . 3_575 ? C3 C4 O12 Cs1 19.5(6) . . . 3_465 ? C3 C4 O12 Cs2 -53.7(9) . . . 4 ? C4 C1 C2 C3 -0.1(4) . . . . ? C4 C1 C2 Cs2 146.4(2) . . . 3_575 ? C4 C1 C2 O10 179.8(6) . . . . ? C4 C1 O9 Cs1 116.1(5) . . . . ? C4 C3 O11 Cs1 -22.3(7) . . . 3_465 ? C4 C3 O11 Cs2 74.2(10) . . . . ? Cs1 B2 O3 Cs2 85.0(5) . . . 3_565 ? Cs1 B2 O5 Cs2 -84.6(5) . . . 2_665 ? Cs1 C3 C4 C1 160.7(3) 3_465 . . . ? Cs1 C3 C4 O12 -18.0(5) 3_465 . . . ? Cs1 C3 O11 Cs2 96.5(6) 3_465 . . . ? Cs1 C4 O12 Cs2 -73.2(5) 3_465 . . 4 ? Cs2 C2 C3 C4 -103.6(5) 3_575 . . . ? Cs2 C2 C3 Cs1 -170.4(5) 3_575 . . 3_465 ? Cs2 C2 C3 O11 77.1(9) 3_575 . . . ? O3 B2 O5 Cs1 16.6(6) . . . . ? O3 B2 O5 Cs2 -68.0(9) . . . 2_665 ? O4 B2 O3 Cs1 164.3(5) . . . . ? O4 B2 O3 Cs2 -110.7(6) . . . 3_565 ? O4 B2 O5 Cs1 -163.6(5) . . . . ? O4 B2 O5 Cs2 111.8(6) . . . 2_665 ? O5 B2 O3 Cs1 -15.9(6) . . . . ? O5 B2 O3 Cs2 69.1(9) . . . 3_565 ? O6 B1 O7 Cs1 -116.7(4) . . . . ? O6 B1 O8 Cs2 -134.7(5) . . . 3_575 ? O7 B1 O6 Cs2 -80.0(10) . . . 1_655 ? O7 B1 O8 Cs2 44.1(6) . . . 3_575 ? O8 B1 O6 Cs2 98.8(9) . . . 1_655 ? O8 B1 O7 Cs1 64.4(5) . . . . ? O9 C1 C2 C3 179.5(5) . . . . ? O9 C1 C2 Cs2 -34.0(6) . . . 3_575 ? O9 C1 C2 O10 -0.6(10) . . . . ? O9 C1 C4 C3 -179.5(5) . . . . ? O9 C1 C4 Cs1 -130.4(7) . . . 3_465 ? O9 C1 C4 O12 -0.8(9) . . . . ? O10 C2 C3 C4 -179.8(6) . . . . ? O10 C2 C3 Cs1 113.4(9) . . . 3_465 ? O10 C2 C3 O11 0.9(12) . . . . ? O11 C3 C4 C1 179.2(7) . . . . ? O11 C3 C4 Cs1 18.4(6) . . . 3_465 ? O11 C3 C4 O12 0.5(10) . . . . ?