#------------------------------------------------------------------------------ #$Date: 2026-06-05 00:36:20 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306224 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721102.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_7721102 loop_ _publ_author_name 'Wessels, Vivien' 'Mikuta, Martina' 'H\"oppe, Henning A.' _publ_section_title ; Weakly Coordinating Borophosphates -- Ca0.5M(H2O)2[B(PO4)2]•H2O (M = Mg, Mn, Co, Zn, Cd) ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00484A _journal_year 2026 _chemical_formula_sum 'B Ca0.5 H6 Mn O11 P2' _chemical_formula_weight 329.78 _space_group_crystal_system trigonal _space_group_IT_number 152 _space_group_name_Hall 'P 31 2"' _space_group_name_H-M_alt 'P 31 2 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2026-05-08 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 9.5680(3) _cell_length_b 9.5680(3) _cell_length_c 15.8100(4) _cell_measurement_reflns_used 71696 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 29.998 _cell_measurement_theta_min 2.458 _cell_volume 1253.44(6) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 300(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'D8 Venture Bruker' _diffrn_measurement_method 'generic phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1104 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 71577 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.993 _diffrn_reflns_theta_min 2.458 _exptl_absorpt_coefficient_mu 2.323 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.6884 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour 'light pink' _exptl_crystal_density_diffrn 2.621 _exptl_crystal_description block _exptl_crystal_F_000 984 _exptl_crystal_size_max 0.081 _exptl_crystal_size_mid 0.067 _exptl_crystal_size_min 0.053 _exptl_transmission_factor_max 0.7463 _exptl_transmission_factor_min 0.6884 _refine_diff_density_max 0.428 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.083 _refine_ls_abs_structure_details ; Flack x determined using 864 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.003(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 174 _refine_ls_number_reflns 2440 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0261 _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^)+(0.0354P)^2^+0.5247P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.0650 _reflns_Friedel_coverage 0.722 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 2218 _reflns_number_total 2440 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00484a2.cif _cod_data_source_block VW68_C222 _cod_original_cell_volume 1253.44(8) _cod_original_formula_sum 'B Ca0.50 H6 Mn O11 P2' _cod_database_code 7721102 _shelx_shelxl_version_number 2018/3 _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_res_file ; TITL VW68_C222 in C222(1), C1 [Ausl. bed. durchbr.], C211 (a unique), P3_121 VW68_C222.res created by SHELXL-2018/3 at 11:34:12 on 08-May-2026 CELL 0.71073 9.56800 9.56800 15.81000 90.0000 90.000 120.0000 ZERR 6 0.00030 0.00030 0.00040 0.0000 0.000 0.0000 LATT -1 SYMM - Y , X - Y , 0.33333 + Z SYMM - X + Y , - X , 0.66667 + Z SYMM Y , X , - Z SYMM - X , - X + Y , 0.33333 - Z SYMM X - Y , - Y , 0.66667 - Z SFAC B H O P CA MN UNIT 6 36 66 12 3 6 LIST 4 TEMP 26.850 L.S. 10 BOND $H HTAB DFIX 0.99 0.01 O1 H11 DFIX 0.99 0.01 O1 H12 DFIX 1.565 0.01 H11 H12 DFIX 0.99 0.01 O2 H21 DFIX 0.99 0.01 O2 H22 DFIX 1.565 0.01 H21 H22 DFIX 0.99 0.01 O3 H31 DFIX 0.99 0.01 O3 H32 DFIX 1.565 0.01 H31 H32 DFIX 0.99 0.01 O4 H41 DFIX 0.99 0.01 O4 H42 DFIX 1.565 0.01 H41 H42 REM Instructions for hydrogen bonds EQIV $1 -y+1, x-y+1, z+1/3 HTAB O2 O11_$1 HTAB O2 O12_$1 HTAB O2 O13 EQIV $2 x-y+1, -y+1, -z+2/3 HTAB O3 O1_$2 HTAB O3 O13 HTAB O3 O4 HTAB O4 O3 EQIV $3 -y, x-y, z+1/3 HTAB O4 O22_$3 EQIV $4 -x, -x+y, -z+1/3 HTAB O4 O24_$4 REM Instructions for hydrogen bonds ENDE OMIT 0 60 FMAP 2 PLAN 10 ACTA EADP CA1A CA1B REM TWIN -1 0 0 0 -1 0 0 0 1 2 REM BASF 0.49127 REM EXTI 0.001042 WGHT 0.035400 0.524700 FVAR 0.10892 0.50618 MN1 6 0.096952 0.548435 0.416639 11.00000 0.01455 0.01978 = 0.01919 -0.00973 0.00001 0.00734 CA1A 5 0.105662 0.748337 0.256948 20.50000 0.02700 0.02673 = 0.01486 0.00087 0.00112 0.01407 CA1B 5 0.251380 0.894247 0.243313 -20.50000 0.02700 0.02673 = 0.01486 0.00087 0.00112 0.01407 P1 4 0.165999 0.385297 0.251928 11.00000 0.01288 0.01170 = 0.00702 -0.00108 0.00097 0.00439 P2 4 0.219359 0.385276 -0.085181 11.00000 0.01547 0.01102 = 0.00728 0.00124 0.00214 0.00667 O1 3 0.296393 0.811813 0.380211 11.00000 0.02176 0.02948 = 0.02326 -0.00692 0.00033 0.01302 H11 2 0.408155 0.833720 0.375787 11.00000 -1.20000 H12 2 0.263659 0.817822 0.322063 11.00000 -1.20000 O2 3 0.296969 0.484510 0.453131 11.00000 0.02138 0.02479 = 0.02496 -0.00870 -0.00162 0.00856 H21 2 0.395695 0.584093 0.470310 11.00000 -1.20000 H22 2 0.324928 0.458613 0.397213 11.00000 -1.20000 O11 3 0.182209 0.415208 0.154357 11.00000 0.01935 0.01197 = 0.00821 0.00037 0.00163 0.00538 O12 3 0.137315 0.513950 0.288225 11.00000 0.02979 0.01766 = 0.01400 -0.00232 0.00417 0.01208 O13 3 0.309468 0.381317 0.287591 11.00000 0.01245 0.02338 = 0.01412 -0.00148 -0.00332 0.00453 O14 3 0.019088 0.214046 0.266729 11.00000 0.01200 0.01350 = 0.01253 0.00229 -0.00095 0.00505 O21 3 0.232761 0.415213 0.012346 11.00000 0.02014 0.01169 = 0.00744 0.00039 0.00170 0.00553 O22 3 0.214084 0.194997 0.099553 11.00000 0.01336 0.01497 = 0.01355 0.00301 0.00304 0.00885 O23 3 0.376920 0.513688 -0.121532 11.00000 0.02275 0.01661 = 0.01546 0.00249 0.00733 0.00376 O24 3 0.071580 0.381110 -0.120855 11.00000 0.02461 0.02362 = 0.01526 0.00196 -0.00081 0.01797 B1 1 0.151464 0.303561 0.083166 11.00000 0.01377 0.01229 = 0.00779 0.00017 0.00133 0.00659 O3 3 0.145014 0.000000 0.333333 10.50000 0.04372 0.04151 = 0.14120 0.01214 0.00607 0.02075 H31 2 0.233818 0.047830 0.291517 10.50000 -1.20000 H32 2 0.150793 0.094556 0.362430 10.50000 -1.20000 O4 3 0.144840 0.144840 0.500000 10.50000 0.04654 0.04654 = 0.14427 0.00323 -0.00323 0.02789 H41 2 0.126323 0.094625 0.442572 10.50000 -1.20000 H42 2 0.071553 0.190905 0.500219 10.50000 -1.20000 REM REM VW68_C222.hkl REM HKLF 4 1 -0.5 -0.5 0 -0.5 0.5 0 0 0 -1 REM VW68_C222 in C222(1), C1 [Ausl. bed. durchbr.], C211 (a unique), P3_121 REM wR2 = 0.0650, GooF = S = 1.090, Restrained GooF = 1.088 for all data REM R1 = 0.0261 for 2218 Fo > 4sig(Fo) and 0.0301 for all 2440 data REM 174 parameters refined using 12 restraints END WGHT 0.0348 0.5419 REM Instructions for potential hydrogen bonds HTAB O1 O21_$1 HTAB O2 O11_$1 HTAB O2 O12_$1 HTAB O2 O13 HTAB O3 O1_$2 HTAB O3 O13 HTAB O3 O4 HTAB O4 O3 HTAB O4 O22_$3 HTAB O4 O24_$4 REM Highest difference peak 0.428, deepest hole -0.409, 1-sigma level 0.083 Q1 1 0.1882 0.7870 0.2464 11.00000 0.05 0.43 Q2 1 0.1784 0.3574 0.0411 11.00000 0.05 0.34 Q3 1 0.0561 0.1116 0.2669 11.00000 0.05 0.34 Q4 1 0.0663 0.3021 0.2634 11.00000 0.05 0.34 Q5 1 0.3173 0.8703 0.4193 11.00000 0.05 0.33 Q6 1 0.2418 0.3206 0.2631 11.00000 0.05 0.33 Q7 1 0.1326 0.6237 0.4097 11.00000 0.05 0.31 Q8 1 0.0370 -0.0726 0.3735 11.00000 0.05 0.28 Q9 1 0.2953 0.2271 0.0943 11.00000 0.05 0.27 Q10 1 0.2710 0.3848 0.4802 11.00000 0.05 0.27 ; _shelx_res_checksum 78148 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' '-x, -x+y, -z+1/3' 'x-y, -y, -z+2/3' 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 Mn1 Mn 0.09695(6) 0.54844(7) 0.41664(3) 0.01840(13) Uani 1 1 d . . . . . Ca1A Ca 0.1057(4) 0.7483(4) 0.25695(16) 0.0226(4) Uani 0.2531(19) 1 d . . P . . Ca1B Ca 0.2514(4) 0.8942(4) 0.24331(16) 0.0226(4) Uani 0.2469(19) 1 d . . P . . P1 P 0.16600(10) 0.38530(10) 0.25193(4) 0.01131(18) Uani 1 1 d . . . . . P2 P 0.21936(11) 0.38528(10) -0.08518(4) 0.01123(18) Uani 1 1 d . . . . . O1 O 0.2964(3) 0.8118(4) 0.38021(16) 0.0247(6) Uani 1 1 d D . . . . H11 H 0.408(2) 0.834(6) 0.376(2) 0.030 Uiso 1 1 d D U . . . H12 H 0.264(4) 0.818(6) 0.3221(12) 0.030 Uiso 1 1 d D U . . . O2 O 0.2970(3) 0.4845(3) 0.45313(16) 0.0250(6) Uani 1 1 d D . . . . H21 H 0.396(3) 0.584(3) 0.470(2) 0.030 Uiso 1 1 d D U . . . H22 H 0.325(5) 0.459(5) 0.3972(15) 0.030 Uiso 1 1 d D U . . . O11 O 0.1822(3) 0.4152(3) 0.15436(12) 0.0143(5) Uani 1 1 d . . . . . O12 O 0.1373(3) 0.5140(3) 0.28823(14) 0.0204(5) Uani 1 1 d . . . . . O13 O 0.3095(3) 0.3813(3) 0.28759(14) 0.0186(5) Uani 1 1 d . . . . . O14 O 0.0191(3) 0.2140(3) 0.26673(13) 0.0133(4) Uani 1 1 d . . . . . O21 O 0.2328(3) 0.4152(3) 0.01235(12) 0.0142(5) Uani 1 1 d . . . . . O22 O 0.2141(3) 0.1950(3) 0.09955(13) 0.0132(4) Uani 1 1 d . . . . . O23 O 0.3769(3) 0.5137(3) -0.12153(14) 0.0210(5) Uani 1 1 d . . . . . O24 O 0.0716(3) 0.3811(3) -0.12085(14) 0.0185(5) Uani 1 1 d . . . . . B1 B 0.1515(5) 0.3036(4) 0.08317(18) 0.0113(6) Uani 1 1 d . . . . . O3 O 0.1450(8) 0.000000 0.333333 0.076(2) Uani 1 2 d DS T P . . H31 H 0.234(11) 0.048(13) 0.292(7) 0.091 Uiso 0.5 1 d D U P . . H32 H 0.151(16) 0.095(9) 0.362(8) 0.091 Uiso 0.5 1 d D U P . . O4 O 0.1448(8) 0.1448(8) 0.500000 0.077(2) Uani 1 2 d DS T P . . H41 H 0.126(17) 0.095(17) 0.443(4) 0.092 Uiso 0.5 1 d D U P . . H42 H 0.072(14) 0.191(16) 0.500(9) 0.092 Uiso 0.5 1 d D U P . . 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 Mn1 0.0146(2) 0.0198(3) 0.0192(2) -0.00973(19) 0.00001(19) 0.0073(2) Ca1A 0.0270(12) 0.0267(12) 0.0149(7) 0.0009(7) 0.0011(7) 0.0141(9) Ca1B 0.0270(12) 0.0267(12) 0.0149(7) 0.0009(7) 0.0011(7) 0.0141(9) P1 0.0129(4) 0.0117(4) 0.0070(3) -0.0011(3) 0.0010(2) 0.0044(3) P2 0.0155(4) 0.0110(4) 0.0073(3) 0.0012(2) 0.0021(3) 0.0067(3) O1 0.0218(14) 0.0295(15) 0.0233(11) -0.0069(11) 0.0003(10) 0.0130(12) O2 0.0214(13) 0.0248(15) 0.0250(11) -0.0087(11) -0.0016(10) 0.0086(12) O11 0.0193(12) 0.0120(11) 0.0082(8) 0.0004(7) 0.0016(8) 0.0054(10) O12 0.0298(15) 0.0177(13) 0.0140(9) -0.0023(9) 0.0042(10) 0.0121(12) O13 0.0124(11) 0.0234(13) 0.0141(9) -0.0015(9) -0.0033(8) 0.0045(10) O14 0.0120(11) 0.0135(11) 0.0125(9) 0.0023(8) -0.0010(8) 0.0051(9) O21 0.0201(13) 0.0117(10) 0.0074(8) 0.0004(7) 0.0017(8) 0.0055(10) O22 0.0134(11) 0.0150(12) 0.0136(9) 0.0030(8) 0.0030(8) 0.0088(10) O23 0.0228(13) 0.0166(13) 0.0155(10) 0.0025(9) 0.0073(9) 0.0038(11) O24 0.0246(14) 0.0236(13) 0.0153(10) 0.0020(9) -0.0008(9) 0.0180(11) B1 0.0138(17) 0.0123(14) 0.0078(11) 0.0002(11) 0.0013(11) 0.0066(14) O3 0.044(3) 0.042(3) 0.141(7) 0.012(4) 0.006(2) 0.0208(17) O4 0.047(3) 0.047(3) 0.144(7) 0.003(2) -0.003(2) 0.028(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 O24 Mn1 O13 97.52(10) 5 6_565 ? O24 Mn1 O12 101.52(10) 5 . ? O13 Mn1 O12 90.46(10) 6_565 . ? O24 Mn1 O23 90.38(10) 5 3_565 ? O13 Mn1 O23 101.43(10) 6_565 3_565 ? O12 Mn1 O23 162.00(10) . 3_565 ? O24 Mn1 O1 176.28(10) 5 . ? O13 Mn1 O1 86.00(11) 6_565 . ? O12 Mn1 O1 79.57(9) . . ? O23 Mn1 O1 87.76(10) 3_565 . ? O24 Mn1 O2 85.99(10) 5 . ? O13 Mn1 O2 176.29(10) 6_565 . ? O12 Mn1 O2 87.67(10) . . ? O23 Mn1 O2 79.66(9) 3_565 . ? O1 Mn1 O2 90.51(9) . . ? O24 Mn1 Ca1A 130.97(9) 5 . ? O13 Mn1 Ca1A 51.32(9) 6_565 . ? O12 Mn1 Ca1A 51.31(9) . . ? O23 Mn1 Ca1A 128.17(10) 3_565 . ? O1 Mn1 Ca1A 52.41(9) . . ? O2 Mn1 Ca1A 125.27(9) . . ? O24 Mn1 Ca1B 51.31(9) 5 2_665 ? O13 Mn1 Ca1B 130.93(9) 6_565 2_665 ? O12 Mn1 Ca1B 128.19(10) . 2_665 ? O23 Mn1 Ca1B 51.27(9) 3_565 2_665 ? O1 Mn1 Ca1B 125.27(9) . 2_665 ? O2 Mn1 Ca1B 52.44(9) . 2_665 ? Ca1A Mn1 Ca1B 177.36(8) . 2_665 ? Ca1B Ca1A O4 84.3(2) . 3_564 ? Ca1B Ca1A O2 77.99(18) . 3_564 ? O4 Ca1A O2 76.91(14) 3_564 3_564 ? Ca1B Ca1A O12 114.9(3) . . ? O4 Ca1A O12 145.5(2) 3_564 . ? O2 Ca1A O12 79.52(13) 3_564 . ? Ca1B Ca1A O13 135.3(2) . 6_565 ? O4 Ca1A O13 111.76(15) 3_564 6_565 ? O2 Ca1A O13 144.89(18) 3_564 6_565 ? O12 Ca1A O13 75.57(12) . 6_565 ? Ca1B Ca1A O1 69.07(18) . . ? O4 Ca1A O1 143.9(2) 3_564 . ? O2 Ca1A O1 118.35(16) 3_564 . ? O12 Ca1A O1 70.16(12) . . ? O13 Ca1A O1 75.48(11) 6_565 . ? Ca1B Ca1A O3 62.1(2) . 1_565 ? O4 Ca1A O3 76.16(19) 3_564 1_565 ? O2 Ca1A O3 133.37(15) 3_564 1_565 ? O12 Ca1A O3 137.67(14) . 1_565 ? O13 Ca1A O3 80.97(12) 6_565 1_565 ? O1 Ca1A O3 70.10(16) . 1_565 ? Ca1B Ca1A O2 153.7(2) . 6_565 ? O4 Ca1A O2 72.14(15) 3_564 6_565 ? O2 Ca1A O2 85.35(14) 3_564 6_565 ? O12 Ca1A O2 81.20(13) . 6_565 ? O13 Ca1A O2 66.81(12) 6_565 6_565 ? O1 Ca1A O2 137.20(15) . 6_565 ? O3 Ca1A O2 120.7(2) 1_565 6_565 ? Ca1B Ca1A Mn1 115.9(2) . . ? O4 Ca1A Mn1 153.91(13) 3_564 . ? O2 Ca1A Mn1 121.58(14) 3_564 . ? O12 Ca1A Mn1 42.38(7) . . ? O13 Ca1A Mn1 42.33(7) 6_565 . ? O1 Ca1A Mn1 47.41(8) . . ? O3 Ca1A Mn1 98.09(9) 1_565 . ? O2 Ca1A Mn1 90.09(10) 6_565 . ? Ca1B Ca1A Ca1A 108.48(17) . 5 ? O4 Ca1A Ca1A 42.37(16) 3_564 5 ? O2 Ca1A Ca1A 51.84(9) 3_564 5 ? O12 Ca1A Ca1A 103.13(8) . 5 ? O13 Ca1A Ca1A 110.89(17) 6_565 5 ? O1 Ca1A Ca1A 169.79(15) . 5 ? O3 Ca1A Ca1A 118.10(13) 1_565 5 ? O2 Ca1A Ca1A 45.69(10) 6_565 5 ? Mn1 Ca1A Ca1A 132.27(11) . 5 ? Ca1B Ca1A Ca1B 51.97(15) . 6_675 ? O4 Ca1A Ca1B 103.92(19) 3_564 6_675 ? O2 Ca1A Ca1B 129.01(14) 3_564 6_675 ? O12 Ca1A Ca1B 110.48(11) . 6_675 ? O13 Ca1A Ca1B 83.34(10) 6_565 6_675 ? O1 Ca1A Ca1B 40.38(9) . 6_675 ? O3 Ca1A Ca1B 31.08(16) 1_565 6_675 ? O2 Ca1A Ca1B 144.50(14) 6_565 6_675 ? Mn1 Ca1A Ca1B 79.31(7) . 6_675 ? Ca1A Ca1A Ca1B 145.94(7) 5 6_675 ? Ca1B Ca1A Ca1B 116.3(2) . 5 ? O4 Ca1A Ca1B 35.54(14) 3_564 5 ? O2 Ca1A Ca1B 71.18(10) 3_564 5 ? O12 Ca1A Ca1B 112.29(13) . 5 ? O13 Ca1A Ca1B 95.90(12) 6_565 5 ? O1 Ca1A Ca1B 170.38(13) . 5 ? O3 Ca1A Ca1B 104.69(18) 1_565 5 ? O2 Ca1A Ca1B 38.03(8) 6_565 5 ? Mn1 Ca1A Ca1B 127.81(11) . 5 ? Ca1A Ca1A Ca1B 19.43(7) 5 5 ? Ca1B Ca1A Ca1B 135.55(13) 6_675 5 ? Ca1B Ca1A H12 56.6(13) . . ? O4 Ca1A H12 136.8(16) 3_564 . ? O2 Ca1A H12 108.3(12) 3_564 . ? O12 Ca1A H12 74.9(16) . . ? O13 Ca1A H12 88.6(11) 6_565 . ? O1 Ca1A H12 13.3(12) . . ? O3 Ca1A H12 69.8(15) 1_565 . ? O2 Ca1A H12 149.4(14) 6_565 . ? Mn1 Ca1A H12 59.3(13) . . ? Ca1A Ca1A H12 159.5(11) 5 . ? Ca1B Ca1A H12 38.7(15) 6_675 . ? Ca1B Ca1A H12 172.3(15) 5 . ? Ca1B Ca1A H22 172.0(9) . 6_565 ? O4 Ca1A H22 87.9(8) 3_564 6_565 ? O2 Ca1A H22 102.0(7) 3_564 6_565 ? O12 Ca1A H22 72.7(10) . 6_565 ? O13 Ca1A H22 47.0(6) 6_565 6_565 ? O1 Ca1A H22 117.2(6) . 6_565 ? O3 Ca1A H22 114.3(10) 1_565 6_565 ? O2 Ca1A H22 20.6(5) 6_565 6_565 ? Mn1 Ca1A H22 71.1(7) . 6_565 ? Ca1A Ca1A H22 66.3(6) 5 6_565 ? Ca1B Ca1A H22 128.9(7) 6_675 6_565 ? Ca1B Ca1A H22 56.8(6) 5 6_565 ? H12 Ca1A H22 130.0(14) . 6_565 ? Ca1B Ca1A H31 40.5(11) . 1_565 ? O4 Ca1A H31 73(3) 3_564 1_565 ? O2 Ca1A H31 112.1(11) 3_564 1_565 ? O12 Ca1A H31 141(3) . 1_565 ? O13 Ca1A H31 102.8(9) 6_565 1_565 ? O1 Ca1A H31 71(3) . 1_565 ? O3 Ca1A H31 22.4(6) 1_565 1_565 ? O2 Ca1A H31 135(3) 6_565 1_565 ? Mn1 Ca1A H31 111(3) . 1_565 ? Ca1A Ca1A H31 114(3) 5 1_565 ? Ca1B Ca1A H31 33(3) 6_675 1_565 ? Ca1B Ca1A H31 107(3) 5 1_565 ? H12 Ca1A H31 66(4) . 1_565 ? H22 Ca1A H31 134.8(19) 6_565 1_565 ? Ca1B Ca1A H32 78(3) . 6_565 ? O4 Ca1A H32 64(3) 3_564 6_565 ? O2 Ca1A H32 135(4) 3_564 6_565 ? O12 Ca1A H32 145(4) . 6_565 ? O13 Ca1A H32 73(4) 6_565 6_565 ? O1 Ca1A H32 87(2) . 6_565 ? O3 Ca1A H32 20.3(19) 1_565 6_565 ? O2 Ca1A H32 101(2) 6_565 6_565 ? Mn1 Ca1A H32 103(4) . 6_565 ? Ca1A Ca1A H32 103(2) 5 6_565 ? Ca1B Ca1A H32 50.4(18) 6_675 6_565 ? Ca1B Ca1A H32 87(2) 5 6_565 ? H12 Ca1A H32 89(2) . 6_565 ? H22 Ca1A H32 97(3) 6_565 6_565 ? H31 Ca1A H32 38(3) 1_565 6_565 ? Ca1B Ca1A H41 76(4) . 6_565 ? O4 Ca1A H41 26.2(4) 3_564 6_565 ? O2 Ca1A H41 100(2) 3_564 6_565 ? O12 Ca1A H41 168(3) . 6_565 ? O13 Ca1A H41 100(4) 6_565 6_565 ? O1 Ca1A H41 119.9(14) . 6_565 ? O3 Ca1A H41 50.3(8) 1_565 6_565 ? O2 Ca1A H41 87(3) 6_565 6_565 ? Mn1 Ca1A H41 138(3) . 6_565 ? Ca1A Ca1A H41 67.8(9) 5 6_565 ? Ca1B Ca1A H41 79.6(16) 6_675 6_565 ? Ca1B Ca1A H41 57(2) 5 6_565 ? H12 Ca1A H41 117(3) . 6_565 ? H22 Ca1A H41 96(4) 6_565 6_565 ? H31 Ca1A H41 51(4) 1_565 6_565 ? H32 Ca1A H41 38(3) 6_565 6_565 ? Ca1B Ca1A H42 58.7(9) . 3_564 ? O4 Ca1A H42 25.8(6) 3_564 3_564 ? O2 Ca1A H42 70(4) 3_564 3_564 ? O12 Ca1A H42 150(4) . 3_564 ? O13 Ca1A H42 132(3) 6_565 3_564 ? O1 Ca1A H42 124(2) . 3_564 ? O3 Ca1A H42 69(4) 1_565 3_564 ? O2 Ca1A H42 96.6(15) 6_565 3_564 ? Mn1 Ca1A H42 167(4) . 3_564 ? Ca1A Ca1A H42 58(3) 5 3_564 ? Ca1B Ca1A H42 89(3) 6_675 3_564 ? Ca1B Ca1A H42 58.7(16) 5 3_564 ? H12 Ca1A H42 114(2) . 3_564 ? H22 Ca1A H42 113.6(11) 6_565 3_564 ? H31 Ca1A H42 57(5) 1_565 3_564 ? H32 Ca1A H42 65(6) 6_565 3_564 ? H41 Ca1A H42 32(3) 6_565 3_564 ? Ca1A Ca1B O3 84.5(2) . 1_565 ? Ca1A Ca1B O1 77.84(18) . . ? O3 Ca1B O1 77.04(14) 1_565 . ? Ca1A Ca1B O23 114.9(3) . 2_665 ? O3 Ca1B O23 145.5(2) 1_565 2_665 ? O1 Ca1B O23 79.59(13) . 2_665 ? Ca1A Ca1B O24 135.2(2) . 4_565 ? O3 Ca1B O24 111.79(15) 1_565 4_565 ? O1 Ca1B O24 144.99(18) . 4_565 ? O23 Ca1B O24 75.39(12) 2_665 4_565 ? Ca1A Ca1B O2 68.97(17) . 3_564 ? O3 Ca1B O2 143.9(2) 1_565 3_564 ? O1 Ca1B O2 118.23(16) . 3_564 ? O23 Ca1B O2 70.23(12) 2_665 3_564 ? O24 Ca1B O2 75.40(11) 4_565 3_564 ? Ca1A Ca1B O4 62.3(2) . 3_564 ? O3 Ca1B O4 76.24(19) 1_565 3_564 ? O1 Ca1B O4 133.44(16) . 3_564 ? O23 Ca1B O4 137.56(14) 2_665 3_564 ? O24 Ca1B O4 80.84(12) 4_565 3_564 ? O2 Ca1B O4 70.02(16) 3_564 3_564 ? Ca1A Ca1B O1 153.9(2) . 6_675 ? O3 Ca1B O1 72.11(15) 1_565 6_675 ? O1 Ca1B O1 85.60(14) . 6_675 ? O23 Ca1B O1 81.12(14) 2_665 6_675 ? O24 Ca1B O1 66.78(12) 4_565 6_675 ? O2 Ca1B O1 137.15(15) 3_564 6_675 ? O4 Ca1B O1 120.5(2) 3_564 6_675 ? Ca1A Ca1B Mn1 115.8(2) . 3_564 ? O3 Ca1B Mn1 153.82(14) 1_565 3_564 ? O1 Ca1B Mn1 121.57(15) . 3_564 ? O23 Ca1B Mn1 42.32(7) 2_665 3_564 ? O24 Ca1B Mn1 42.22(7) 4_565 3_564 ? O2 Ca1B Mn1 47.44(8) 3_564 3_564 ? O4 Ca1B Mn1 97.96(9) 3_564 3_564 ? O1 Ca1B Mn1 90.02(11) 6_675 3_564 ? Ca1A Ca1B Ca1B 108.60(18) . 6_675 ? O3 Ca1B Ca1B 42.35(16) 1_565 6_675 ? O1 Ca1B Ca1B 52.06(9) . 6_675 ? O23 Ca1B Ca1B 103.13(9) 2_665 6_675 ? O24 Ca1B Ca1B 110.90(17) 4_565 6_675 ? O2 Ca1B Ca1B 169.88(15) 3_564 6_675 ? O4 Ca1B Ca1B 118.14(13) 3_564 6_675 ? O1 Ca1B Ca1B 45.71(10) 6_675 6_675 ? Mn1 Ca1B Ca1B 132.23(11) 3_564 6_675 ? Ca1A Ca1B Ca1A 116.4(2) . 6_675 ? O3 Ca1B Ca1A 35.56(14) 1_565 6_675 ? O1 Ca1B Ca1A 71.41(10) . 6_675 ? O23 Ca1B Ca1A 112.20(13) 2_665 6_675 ? O24 Ca1B Ca1A 95.89(12) 4_565 6_675 ? O2 Ca1B Ca1A 170.27(13) 3_564 6_675 ? O4 Ca1B Ca1A 104.71(18) 3_564 6_675 ? O1 Ca1B Ca1A 37.99(8) 6_675 6_675 ? Mn1 Ca1B Ca1A 127.70(11) 3_564 6_675 ? Ca1B Ca1B Ca1A 19.43(7) 6_675 6_675 ? Ca1A Ca1B Ca1A 52.09(15) . 5 ? O3 Ca1B Ca1A 104.06(19) 1_565 5 ? O1 Ca1B Ca1A 128.97(14) . 5 ? O23 Ca1B Ca1A 110.39(12) 2_665 5 ? O24 Ca1B Ca1A 83.18(11) 4_565 5 ? O2 Ca1B Ca1A 40.24(9) 3_564 5 ? O4 Ca1B Ca1A 31.13(16) 3_564 5 ? O1 Ca1B Ca1A 144.35(14) 6_675 5 ? Mn1 Ca1B Ca1A 79.17(7) 3_564 5 ? Ca1B Ca1B Ca1A 146.07(7) 6_675 5 ? Ca1A Ca1B Ca1A 135.64(13) 6_675 5 ? Ca1A Ca1B H12 70.5(15) . . ? O3 Ca1B H12 81.7(16) 1_565 . ? O1 Ca1B H12 8.9(17) . . ? O23 Ca1B H12 78.9(14) 2_665 . ? O24 Ca1B H12 150.0(14) 4_565 . ? O2 Ca1B H12 110.0(17) 3_564 . ? O4 Ca1B H12 129.1(14) 3_564 . ? O1 Ca1B H12 94.3(17) 6_675 . ? Mn1 Ca1B H12 119.5(15) 3_564 . ? Ca1B Ca1B H12 60.5(17) 6_675 . ? Ca1A Ca1B H12 79.7(17) 6_675 . ? Ca1A Ca1B H12 120.7(16) 5 . ? Ca1A Ca1B H31 108(2) . 1_565 ? O3 Ca1B H31 24.4(14) 1_565 1_565 ? O1 Ca1B H31 90(4) . 1_565 ? O23 Ca1B H31 132(4) 2_665 1_565 ? O24 Ca1B H31 89(2) 4_565 1_565 ? O2 Ca1B H31 149(5) 3_564 1_565 ? O4 Ca1B H31 81(5) 3_564 1_565 ? O1 Ca1B H31 52(3) 6_675 1_565 ? Mn1 Ca1B H31 130.2(17) 3_564 1_565 ? Ca1B Ca1B H31 41(5) 6_675 1_565 ? Ca1A Ca1B H31 24(5) 6_675 1_565 ? Ca1A Ca1B H31 112(5) 5 1_565 ? H12 Ca1B H31 97(4) . 1_565 ? Ca1A Ca1B H32 61.8(17) . 6_565 ? O3 Ca1B H32 25.8(6) 1_565 6_565 ? O1 Ca1B H32 85(3) . 6_565 ? O23 Ca1B H32 165(3) 2_665 6_565 ? O24 Ca1B H32 118(3) 4_565 6_565 ? O2 Ca1B H32 118.6(8) 3_564 6_565 ? O4 Ca1B H32 56(2) 3_564 6_565 ? O1 Ca1B H32 97.0(10) 6_675 6_565 ? Mn1 Ca1B H32 153(3) 3_564 6_565 ? Ca1B Ca1B H32 66.2(12) 6_675 6_565 ? Ca1A Ca1B H32 61.4(6) 6_675 6_565 ? Ca1A Ca1B H32 79.9(13) 5 6_565 ? H12 Ca1B H32 86(3) . 6_565 ? H31 Ca1B H32 46(2) 1_565 6_565 ? Ca1A Ca1B H41 65(4) . 6_565 ? O3 Ca1B H41 53.5(8) 1_565 6_565 ? O1 Ca1B H41 118(3) . 6_565 ? O23 Ca1B H41 160.0(12) 2_665 6_565 ? O24 Ca1B H41 91(4) 4_565 6_565 ? O2 Ca1B H41 92.2(12) 3_564 6_565 ? O4 Ca1B H41 22.8(7) 3_564 6_565 ? O1 Ca1B H41 108(3) 6_675 6_565 ? Mn1 Ca1B H41 118(2) 3_564 6_565 ? Ca1B Ca1B H41 95.5(9) 6_675 6_565 ? Ca1A Ca1B H41 83.6(17) 6_675 6_565 ? Ca1A Ca1B H41 52.2(15) 5 6_565 ? H12 Ca1B H41 117(4) . 6_565 ? H31 Ca1B H41 61(5) 1_565 6_565 ? H32 Ca1B H41 35(3) 6_565 6_565 ? Ca1A Ca1B H42 82(2) . 3_564 ? O3 Ca1B H42 81(5) 1_565 3_564 ? O1 Ca1B H42 151(3) . 3_564 ? O23 Ca1B H42 128(4) 2_665 3_564 ? O24 Ca1B H42 62(2) 4_565 3_564 ? O2 Ca1B H42 72(5) 3_564 3_564 ? O4 Ca1B H42 20(2) 3_564 3_564 ? O1 Ca1B H42 105(3) 6_675 3_564 ? Mn1 Ca1B H42 86(4) 3_564 3_564 ? Ca1B Ca1B H42 118(5) 6_675 3_564 ? Ca1A Ca1B H42 100(5) 6_675 3_564 ? Ca1A Ca1B H42 41(4) 5 3_564 ? H12 Ca1B H42 148(3) . 3_564 ? H31 Ca1B H42 77(7) 1_565 3_564 ? H32 Ca1B H42 67(5) 6_565 3_564 ? H41 Ca1B H42 33(3) 6_565 3_564 ? O13 P1 O12 114.90(15) . . ? O13 P1 O14 105.86(14) . . ? O12 P1 O14 111.53(15) . . ? O13 P1 O11 111.53(13) . . ? O12 P1 O11 105.61(13) . . ? O14 P1 O11 107.25(12) . . ? O23 P2 O24 115.06(15) . . ? O23 P2 O22 111.51(15) . 4 ? O24 P2 O22 105.91(14) . 4 ? O23 P2 O21 105.71(13) . . ? O24 P2 O21 111.40(13) . . ? O22 P2 O21 107.06(12) 4 . ? Mn1 O1 Ca1B 112.85(14) . . ? Mn1 O1 Ca1A 80.19(12) . . ? Ca1B O1 Ca1A 33.09(10) . . ? Mn1 O1 Ca1B 134.61(13) . 6_675 ? Ca1B O1 Ca1B 82.23(14) . 6_675 ? Ca1A O1 Ca1B 101.63(13) . 6_675 ? Mn1 O1 H11 117(3) . . ? Ca1B O1 H11 103(2) . . ? Ca1A O1 H11 125(2) . . ? Ca1B O1 H11 99(3) 6_675 . ? Mn1 O1 H12 100(3) . . ? Ca1B O1 H12 14(3) . . ? Ca1A O1 H12 23(2) . . ? Ca1B O1 H12 95(3) 6_675 . ? H11 O1 H12 105.4(17) . . ? Mn1 O2 Ca1A 112.72(13) . 2_665 ? Mn1 O2 Ca1B 80.12(12) . 2_665 ? Ca1A O2 Ca1B 33.03(10) 2_665 2_665 ? Mn1 O2 Ca1A 134.48(13) . 6_665 ? Ca1A O2 Ca1A 82.47(14) 2_665 6_665 ? Ca1B O2 Ca1A 101.73(13) 2_665 6_665 ? Mn1 O2 H21 109(3) . . ? Ca1A O2 H21 95(2) 2_665 . ? Ca1B O2 H21 111(2) 2_665 . ? Ca1A O2 H21 112(3) 6_665 . ? Mn1 O2 H22 102(3) . . ? Ca1A O2 H22 133(3) 2_665 . ? Ca1B O2 H22 142(2) 2_665 . ? Ca1A O2 H22 50(3) 6_665 . ? H21 O2 H22 103.8(17) . . ? B1 O11 P1 130.9(2) . . ? P1 O12 Mn1 127.91(15) . . ? P1 O12 Ca1A 145.76(14) . . ? Mn1 O12 Ca1A 86.31(10) . . ? P1 O13 Mn1 137.84(14) . 6_665 ? P1 O13 Ca1A 135.30(16) . 6_665 ? Mn1 O13 Ca1A 86.35(12) 6_665 6_665 ? B1 O14 P1 129.9(2) 5 . ? B1 O21 P2 130.7(2) . . ? B1 O22 P2 130.2(2) . 4 ? P2 O23 Mn1 127.95(15) . 2_664 ? P2 O23 Ca1B 145.63(14) . 3_564 ? Mn1 O23 Ca1B 86.40(10) 2_664 3_564 ? P2 O24 Mn1 137.82(14) . 5 ? P2 O24 Ca1B 135.23(16) . 4_455 ? Mn1 O24 Ca1B 86.47(12) 5 4_455 ? O14 B1 O22 103.7(2) 5 . ? O14 B1 O21 112.2(3) 5 . ? O22 B1 O21 113.3(3) . . ? O14 B1 O11 113.6(3) 5 . ? O22 B1 O11 112.1(3) . . ? O21 B1 O11 102.3(2) . . ? Ca1B O3 Ca1B 95.3(3) 1_545 6_665 ? Ca1B O3 Ca1A 33.47(11) 1_545 1_545 ? Ca1B O3 Ca1A 113.4(3) 6_665 1_545 ? Ca1B O3 Ca1A 113.4(3) 1_545 6_665 ? Ca1B O3 Ca1A 33.47(11) 6_665 6_665 ? Ca1A O3 Ca1A 142.1(3) 1_545 6_665 ? Ca1B O3 H31 47(7) 1_545 . ? Ca1B O3 H31 81(8) 6_665 . ? Ca1A O3 H31 79(7) 1_545 . ? Ca1A O3 H31 78(7) 6_665 . ? Ca1B O3 H32 150(7) 1_545 . ? Ca1B O3 H32 71(9) 6_665 . ? Ca1A O3 H32 175(8) 1_545 . ? Ca1A O3 H32 43(8) 6_665 . ? H31 O3 H32 104(2) . . ? Ca1A O4 Ca1A 95.3(3) 2_665 6_665 ? Ca1A O4 Ca1B 33.45(11) 2_665 2_665 ? Ca1A O4 Ca1B 113.3(3) 6_665 2_665 ? Ca1A O4 Ca1B 113.3(3) 2_665 6_665 ? Ca1A O4 Ca1B 33.45(11) 6_665 6_665 ? Ca1B O4 Ca1B 142.0(3) 2_665 6_665 ? Ca1A O4 H41 153(9) 2_665 . ? Ca1A O4 H41 63(9) 6_665 . ? Ca1B O4 H41 139(8) 2_665 . ? Ca1B O4 H41 57(8) 6_665 . ? Ca1A O4 H42 73(7) 2_665 . ? Ca1A O4 H42 118(9) 6_665 . ? Ca1B O4 H42 40(7) 2_665 . ? Ca1B O4 H42 149(9) 6_665 . ? H41 O4 H42 102.7(19) . . ? 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 Mn1 O24 2.119(3) 5 ? Mn1 O13 2.121(3) 6_565 ? Mn1 O12 2.123(2) . ? Mn1 O23 2.124(2) 3_565 ? Mn1 O1 2.348(3) . ? Mn1 O2 2.354(3) . ? Mn1 Ca1A 3.143(3) . ? Mn1 Ca1B 3.148(3) 2_665 ? Ca1A Ca1B 1.412(4) . ? Ca1A O4 2.267(6) 3_564 ? Ca1A O2 2.417(4) 3_564 ? Ca1A O12 2.459(4) . ? Ca1A O13 2.459(4) 6_565 ? Ca1A O1 2.528(4) . ? Ca1A O3 2.548(4) 1_565 ? Ca1A O2 2.656(4) 6_565 ? Ca1A Ca1A 3.349(5) 5 ? Ca1A Ca1B 4.022(4) 6_675 ? Ca1A Ca1B 4.026(4) 5 ? Ca1A H12 1.67(2) . ? Ca1A H22 2.16(5) 6_565 ? Ca1A H31 2.55(11) 1_565 ? Ca1A H32 1.94(12) 6_565 ? Ca1A H41 2.02(15) 6_565 ? Ca1A H42 2.19(13) 3_564 ? Ca1B O3 2.262(6) 1_565 ? Ca1B O1 2.415(4) . ? Ca1B O23 2.461(4) 2_665 ? Ca1B O24 2.462(4) 4_565 ? Ca1B O2 2.533(4) 3_564 ? Ca1B O4 2.548(4) 3_564 ? Ca1B O1 2.661(4) 6_675 ? Ca1B Ca1B 3.343(6) 6_675 ? Ca1B H12 1.48(2) . ? Ca1B H31 1.74(11) 1_565 ? Ca1B H32 2.15(15) 6_565 ? Ca1B H41 2.18(14) 6_565 ? Ca1B H42 1.89(11) 3_564 ? P1 O13 1.502(3) . ? P1 O12 1.503(3) . ? P1 O14 1.553(2) . ? P1 O11 1.562(2) . ? P2 O23 1.503(3) . ? P2 O24 1.504(3) . ? P2 O22 1.551(2) 4 ? P2 O21 1.562(2) . ? O1 H11 0.984(13) . ? O1 H12 0.982(13) . ? O2 H21 0.987(13) . ? O2 H22 0.990(13) . ? O11 B1 1.477(4) . ? O14 B1 1.454(4) 5 ? O21 B1 1.473(4) . ? O22 B1 1.459(4) . ? O3 H31 0.990(14) . ? O3 H32 0.992(14) . ? O4 H41 1.001(14) . ? O4 H42 0.998(14) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2 H21 O11 0.987(13) 1.801(15) 2.783(4) 173(3) 2_665 yes O2 H21 O12 0.987(13) 2.51(3) 3.119(4) 120(3) 2_665 yes O2 H22 O13 0.990(13) 1.861(16) 2.821(3) 162(3) . yes O3 H31 O1 0.990(14) 2.08(9) 2.915(7) 140(11) 6_665 yes O3 H32 O13 0.992(14) 2.66(10) 3.251(3) 119(8) . yes O3 H32 O4 0.992(14) 2.23(10) 2.978(2) 131(10) . yes O4 H41 O3 1.001(14) 2.00(4) 2.978(2) 165(12) . yes O4 H42 O22 0.998(14) 2.48(12) 3.039(6) 115(9) 2 yes O4 H42 O24 0.998(14) 2.29(5) 3.249(3) 161(12) 5 yes