#------------------------------------------------------------------------------ #$Date: 2026-06-05 00:36:20 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306224 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721106.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_7721106 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 'B1.5 Ca0.75 H9 Mg1.5 O16.5 P3' _chemical_formula_weight 448.72 _space_group_crystal_system trigonal _space_group_IT_number 154 _space_group_name_Hall 'P 32 2"' _space_group_name_H-M_alt 'P 32 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 4 _cell_length_a 9.4505(7) _cell_length_b 9.4505(7) _cell_length_c 15.7298(13) _cell_measurement_reflns_used 35037 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 29.977 _cell_measurement_theta_min 2.489 _cell_volume 1216.64(16) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (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 0.1628 _diffrn_reflns_av_unetI/netI 0.0593 _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 34942 _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 29.973 _diffrn_reflns_theta_min 2.489 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_T_max 0.7361 _exptl_absorpt_correction_T_min 0.6848 _exptl_absorpt_correction_type multi-scan _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 colourless _exptl_crystal_density_diffrn 2.450 _exptl_crystal_description block _exptl_crystal_F_000 906 _exptl_crystal_size_max 0.132 _exptl_crystal_size_mid 0.089 _exptl_crystal_size_min 0.072 _exptl_transmission_factor_max 0.7361 _exptl_transmission_factor_min 0.6848 _refine_diff_density_max 0.505 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.080 _refine_ls_abs_structure_details ; Flack x determined using 681 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 174 _refine_ls_number_reflns 2366 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0285 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.0697 _reflns_Friedel_coverage 0.722 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 1926 _reflns_number_total 2366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00484a2.cif _cod_data_source_block mo_MM10_2_0m_a _cod_original_cell_volume 1216.6(2) _cod_original_formula_sum 'B1.50 H9 Ca0.75 Mg1.50 O16.50 P3' _cod_database_code 7721106 _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 mo_MM10_2_0m_a.res in C211 mo_MM10_2_0m_a.res created by SHELXL-2018/3 at 18:58:59 on 21-Apr-2026 CELL 0.71073 9.4505 9.4505 15.7298 90.000 90.0 120.000 ZERR 4 0.0007 0.0007 0.0013 0.000 0.00 0.000 LATT -1 SYMM - Y , X - Y , 0.66667 + Z SYMM - X + Y , - X , 0.33333 + Z SYMM Y , X , - Z SYMM - X , - X + Y , 0.66667 - Z SYMM X - Y , - Y , 0.33333 - Z SFAC B H O P CA MG 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 $6 -y+1, x-y, z-1/3 HTAB O1 O11_$6 HTAB O1 O21_$6 HTAB O2 O11_$6 HTAB O2 O12_$6 HTAB O2 O13 EQIV $4 x-y, -y+1, -z+4/3 HTAB O3 O1_$4 HTAB O3 O13 HTAB O3 O14 EQIV $14 x-y+1, -y+2, -z+4/3 HTAB O4 O22_$14 EQIV $15 -y+2, x-y+1, z-1/3 HTAB O4 O22_$15 EQIV $3 -x+2, -x+y+1, -z+5/3 HTAB O4 O24_$3 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 (4) BASF=0.5 FVAR 0.585 REM TWIN 0 1 0 1 0 0 0 0 -1 2 REM (7) BASF=0.0 FVAR 0.512 REM TWIN 1 -1 0 0 -1 0 0 0 -1 2 REM (8) BASF=0.0 FVAR 0.512 REM TWIN -1 0 0 -1 1 0 0 0 -1 2 REM (9) BASF=0.0 FVAR 0.512 REM TWIN 0 -1 0 -1 0 0 0 0 -1 2 REM (10) BASF=0.5 FVAR 0.585 REM TWIN -1 1 0 0 1 0 0 0 -1 2 REM (11) BASF=0.0 FVAR 0.512 REM TWIN 1 0 0 1 -1 0 0 0 -1 2 REM (12) BASF=0.0 FVAR 0.512 REM BASF 0.5 REM EXTI 0.001688 WGHT 0.034700 FVAR 0.43716 0.51264 MG1 6 0.897820 0.448905 0.583359 11.00000 0.00991 0.01343 = 0.01387 -0.00552 0.00008 0.00543 CA1A 5 0.889140 0.249786 0.743821 20.50000 0.02483 0.02636 = 0.01299 -0.00010 0.00011 0.01548 CA1B 5 0.751390 0.110823 0.755954 -20.50000 0.02483 0.02636 = 0.01299 -0.00010 0.00011 0.01548 P1 4 0.829643 0.612995 0.747066 11.00000 0.00864 0.00856 = 0.00689 -0.00113 0.00036 0.00312 P2 4 0.783030 0.613037 1.086124 11.00000 0.01127 0.00824 = 0.00657 0.00076 0.00176 0.00499 O1 3 0.707276 0.195493 0.616469 11.00000 0.01498 0.02375 = 0.02214 -0.00576 -0.00048 0.00925 H11 2 0.601335 0.189851 0.611658 11.00000 -1.20000 H12 2 0.713506 0.165826 0.675885 11.00000 -1.20000 O2 3 0.707158 0.511881 0.549715 11.00000 0.01600 0.01872 = 0.02157 -0.00826 -0.00074 0.00619 H21 2 0.616117 0.408960 0.528335 11.00000 -1.20000 H22 2 0.668098 0.526843 0.605875 11.00000 -1.20000 O11 3 0.819308 0.583266 0.845474 11.00000 0.01309 0.00872 = 0.00746 0.00036 0.00196 0.00368 O12 3 0.858820 0.484796 0.707813 11.00000 0.02147 0.01538 = 0.01239 -0.00284 0.00211 0.00968 O13 3 0.681724 0.616932 0.714782 11.00000 0.01010 0.02078 = 0.01129 -0.00247 -0.00184 0.00584 O14 3 0.978249 0.787761 0.731640 11.00000 0.00884 0.01165 = 0.01132 0.00268 -0.00084 0.00385 O21 3 0.764387 0.583945 0.987841 11.00000 0.01528 0.00854 = 0.00423 -0.00029 0.00286 0.00318 O22 3 0.787330 0.808634 0.899010 11.00000 0.00996 0.01162 = 0.01094 0.00129 0.00116 0.00670 O23 3 0.626038 0.484836 1.125329 11.00000 0.01619 0.01191 = 0.01389 0.00133 0.00557 0.00251 O24 3 0.935720 0.617754 1.118424 11.00000 0.01716 0.01935 = 0.01266 0.00060 -0.00167 0.01409 B1 1 0.849379 0.697706 0.916942 11.00000 0.00978 0.01140 = 0.00684 -0.00133 0.00129 0.00600 O3 3 0.851306 1.000000 0.666667 10.50000 0.03863 0.03011 = 0.12684 0.01504 0.00752 0.01505 H31 2 0.766205 0.992052 0.706667 10.50000 -1.20000 H32 2 0.837745 0.888387 0.668912 10.50000 -1.20000 O4 3 0.851010 0.851010 0.500000 10.50000 0.04016 0.04016 = 0.14035 0.00718 -0.00718 0.02731 H41 2 0.897857 0.969142 0.487367 10.50000 -1.20000 H42 2 0.944742 0.832267 0.491966 10.50000 -1.20000 REM REM mo_MM10_2_0m_a.hkl REM HKLF 4 1 -0.5 -0.5 0 -0.5 0.5 0 0 0 -1 REM mo_MM10_2_0m_a.res in C211 REM wR2 = 0.0697, GooF = S = 1.040, Restrained GooF = 1.038 for all data REM R1 = 0.0285 for 1926 Fo > 4sig(Fo) and 0.0357 for all 2366 data REM 174 parameters refined using 12 restraints END WGHT 0.0347 0.0000 REM Instructions for potential hydrogen bonds HTAB O1 O11_$6 HTAB O1 O21_$6 HTAB O2 O11_$6 HTAB O2 O12_$6 HTAB O2 O13 HTAB O3 O1_$4 HTAB O3 O13 HTAB O3 O14 HTAB O4 O22_$14 HTAB O4 O22_$15 HTAB O4 O24_$3 REM Highest difference peak 0.505, deepest hole -0.471, 1-sigma level 0.080 Q1 1 0.7968 0.1993 0.7486 11.00000 0.05 0.51 Q2 1 0.8208 0.6411 0.9602 11.00000 0.05 0.36 Q3 1 0.6803 0.1300 0.5763 11.00000 0.05 0.36 Q4 1 0.8379 0.6445 0.8682 11.00000 0.05 0.32 Q5 1 0.9610 0.8306 0.6983 11.00000 0.05 0.30 Q6 1 0.5159 0.4529 1.0957 11.00000 0.05 0.29 Q7 1 0.9394 0.5151 0.6436 11.00000 0.05 0.28 Q8 1 0.8111 0.6418 1.0219 11.00000 0.05 0.27 Q9 1 0.7490 0.5650 1.0291 11.00000 0.05 0.27 Q10 1 0.6788 0.4893 1.0811 11.00000 0.05 0.25 ; _shelx_res_checksum 88794 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' '-x, -x+y, -z+2/3' 'x-y, -y, -z+1/3' 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 Mg1 Mg 0.89782(13) 0.44890(16) 0.58336(7) 0.0126(3) Uani 1 1 d . . . . . Ca1A Ca 0.8891(4) 0.2498(4) 0.74382(17) 0.0202(4) Uani 0.2563(17) 1 d . . P . . Ca1B Ca 0.7514(4) 0.1108(5) 0.75595(18) 0.0202(4) Uani 0.2437(17) 1 d . . P . . P1 P 0.82964(11) 0.61300(10) 0.74707(5) 0.0085(2) Uani 1 1 d . . . . . P2 P 0.78303(11) 0.61304(10) 1.08612(5) 0.0086(2) Uani 1 1 d . . . . . O1 O 0.7073(3) 0.1955(3) 0.61647(16) 0.0205(6) Uani 1 1 d D . . . . H11 H 0.601(3) 0.190(5) 0.6117(19) 0.025 Uiso 1 1 d D U . . . H12 H 0.714(4) 0.166(5) 0.6759(11) 0.025 Uiso 1 1 d D U . . . O2 O 0.7072(3) 0.5119(3) 0.54972(15) 0.0199(6) Uani 1 1 d D . . . . H21 H 0.616(3) 0.409(3) 0.5283(19) 0.024 Uiso 1 1 d D U . . . H22 H 0.668(4) 0.527(4) 0.6059(13) 0.024 Uiso 1 1 d D U . . . O11 O 0.8193(3) 0.5833(3) 0.84547(13) 0.0105(5) Uani 1 1 d . . . . . O12 O 0.8588(3) 0.4848(3) 0.70781(14) 0.0162(6) Uani 1 1 d . . . . . O13 O 0.6817(3) 0.6169(3) 0.71478(14) 0.0149(5) Uani 1 1 d . . . . . O14 O 0.9782(3) 0.7878(3) 0.73164(14) 0.0112(5) Uani 1 1 d . . . . . O21 O 0.7644(3) 0.5839(3) 0.98784(12) 0.0106(5) Uani 1 1 d . . . . . O22 O 0.7873(3) 0.8086(3) 0.89901(13) 0.0103(5) Uani 1 1 d . . . . . O23 O 0.6260(3) 0.4848(3) 1.12533(14) 0.0160(6) Uani 1 1 d . . . . . O24 O 0.9357(3) 0.6178(3) 1.11842(14) 0.0142(5) Uani 1 1 d . . . . . B1 B 0.8494(5) 0.6977(4) 0.9169(2) 0.0090(7) Uani 1 1 d . . . . . O3 O 0.8513(6) 1.000000 0.666667 0.0661(18) Uani 1 2 d DS T P . . H31 H 0.766(9) 0.992(11) 0.707(5) 0.079 Uiso 0.5 1 d D U P . . H32 H 0.838(13) 0.888(6) 0.669(6) 0.079 Uiso 0.5 1 d D U P . . O4 O 0.8510(6) 0.8510(6) 0.500000 0.0703(18) Uani 1 2 d DS T P . . H41 H 0.898(12) 0.969(4) 0.487(7) 0.084 Uiso 0.5 1 d D U P . . H42 H 0.945(8) 0.832(12) 0.492(8) 0.084 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 Mg1 0.0099(5) 0.0134(7) 0.0139(5) -0.0055(4) 0.0001(4) 0.0054(6) Ca1A 0.0248(12) 0.0264(12) 0.0130(8) -0.0001(8) 0.0001(8) 0.0155(9) Ca1B 0.0248(12) 0.0264(12) 0.0130(8) -0.0001(8) 0.0001(8) 0.0155(9) P1 0.0086(5) 0.0086(4) 0.0069(3) -0.0011(3) 0.0004(3) 0.0031(4) P2 0.0113(5) 0.0082(4) 0.0066(3) 0.0008(3) 0.0018(3) 0.0050(4) O1 0.0150(15) 0.0237(15) 0.0221(13) -0.0058(11) -0.0005(11) 0.0092(13) O2 0.0160(15) 0.0187(15) 0.0216(13) -0.0083(11) -0.0007(11) 0.0062(13) O11 0.0131(13) 0.0087(12) 0.0075(9) 0.0004(8) 0.0020(9) 0.0037(10) O12 0.0215(15) 0.0154(14) 0.0124(11) -0.0028(10) 0.0021(10) 0.0097(12) O13 0.0101(12) 0.0208(14) 0.0113(10) -0.0025(10) -0.0018(9) 0.0058(11) O14 0.0088(12) 0.0116(13) 0.0113(10) 0.0027(9) -0.0008(9) 0.0038(11) O21 0.0153(13) 0.0085(12) 0.0042(9) -0.0003(8) 0.0029(8) 0.0032(11) O22 0.0100(13) 0.0116(13) 0.0109(10) 0.0013(9) 0.0012(9) 0.0067(11) O23 0.0162(13) 0.0119(14) 0.0139(11) 0.0013(9) 0.0056(10) 0.0025(11) O24 0.0172(14) 0.0193(14) 0.0127(11) 0.0006(10) -0.0017(10) 0.0141(12) B1 0.0098(19) 0.0114(17) 0.0068(13) -0.0013(14) 0.0013(13) 0.0060(17) O3 0.039(3) 0.030(3) 0.127(6) 0.015(4) 0.0075(18) 0.0151(16) O4 0.040(3) 0.040(3) 0.140(6) 0.0072(19) -0.0072(19) 0.027(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' Mg Mg 0.0486 0.0363 '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 O13 Mg1 O24 96.10(11) 6_666 5_766 ? O13 Mg1 O12 91.25(11) 6_666 . ? O24 Mg1 O12 100.66(11) 5_766 . ? O13 Mg1 O23 100.76(10) 6_666 3_664 ? O24 Mg1 O23 91.28(11) 5_766 3_664 ? O12 Mg1 O23 162.11(11) . 3_664 ? O13 Mg1 O1 86.64(11) 6_666 . ? O24 Mg1 O1 176.89(12) 5_766 . ? O12 Mg1 O1 80.72(10) . . ? O23 Mg1 O1 86.74(11) 3_664 . ? O13 Mg1 O2 177.14(11) 6_666 . ? O24 Mg1 O2 86.39(12) 5_766 . ? O12 Mg1 O2 86.92(10) . . ? O23 Mg1 O2 80.53(10) 3_664 . ? O1 Mg1 O2 90.90(10) . . ? O13 Mg1 Ca1A 52.33(9) 6_666 . ? O24 Mg1 Ca1A 129.98(10) 5_766 . ? O12 Mg1 Ca1A 51.39(9) . . ? O23 Mg1 Ca1A 128.11(11) 3_664 . ? O1 Mg1 Ca1A 53.02(9) . . ? O2 Mg1 Ca1A 124.90(10) . . ? O13 Mg1 Ca1B 129.97(10) 6_666 2_654 ? O24 Mg1 Ca1B 52.19(10) 5_766 2_654 ? O12 Mg1 Ca1B 127.98(11) . 2_654 ? O23 Mg1 Ca1B 51.49(10) 3_664 2_654 ? O1 Mg1 Ca1B 124.79(11) . 2_654 ? O2 Mg1 Ca1B 52.79(9) . 2_654 ? Ca1A Mg1 Ca1B 177.40(9) . 2_654 ? O13 Mg1 Ca1B 64.61(9) 6_666 . ? O24 Mg1 Ca1B 147.41(9) 5_766 . ? O12 Mg1 Ca1B 56.58(9) . . ? O23 Mg1 Ca1B 117.07(10) 3_664 . ? O1 Mg1 Ca1B 35.49(8) . . ? O2 Mg1 Ca1B 112.54(9) . . ? Ca1A Mg1 Ca1B 17.88(7) . . ? Ca1B Mg1 Ca1B 159.71(8) 2_654 . ? O13 Mg1 Ca1A 147.42(9) 6_666 2_654 ? O24 Mg1 Ca1A 64.66(9) 5_766 2_654 ? O12 Mg1 Ca1A 117.10(10) . 2_654 ? O23 Mg1 Ca1A 56.46(9) 3_664 2_654 ? O1 Mg1 Ca1A 112.22(9) . 2_654 ? O2 Mg1 Ca1A 35.25(8) . 2_654 ? Ca1A Mg1 Ca1A 159.56(8) . 2_654 ? Ca1B Mg1 Ca1A 17.94(7) 2_654 2_654 ? Ca1B Mg1 Ca1A 143.90(7) . 2_654 ? Ca1B Ca1A O4 85.7(2) . 3_665 ? Ca1B Ca1A O2 78.1(2) . 3_665 ? O4 Ca1A O2 76.51(12) 3_665 3_665 ? Ca1B Ca1A O12 115.6(3) . . ? O4 Ca1A O12 145.80(19) 3_665 . ? O2 Ca1A O12 81.92(13) 3_665 . ? Ca1B Ca1A O13 134.2(2) . 6_666 ? O4 Ca1A O13 112.37(15) 3_665 6_666 ? O2 Ca1A O13 145.42(17) 3_665 6_666 ? O12 Ca1A O13 72.95(11) . 6_666 ? Ca1B Ca1A O3 62.0(2) . 1_545 ? O4 Ca1A O3 77.34(17) 3_665 1_545 ? O2 Ca1A O3 133.34(16) 3_665 1_545 ? O12 Ca1A O3 135.62(14) . 1_545 ? O13 Ca1A O3 80.68(12) 6_666 1_545 ? Ca1B Ca1A O1 71.3(2) . . ? O4 Ca1A O1 146.3(2) 3_665 . ? O2 Ca1A O1 120.15(16) 3_665 . ? O12 Ca1A O1 67.84(11) . . ? O13 Ca1A O1 71.73(11) 6_666 . ? O3 Ca1A O1 70.30(14) 1_545 . ? Ca1B Ca1A O2 155.0(2) . 6_666 ? O4 Ca1A O2 71.02(14) 3_665 6_666 ? O2 Ca1A O2 87.48(14) 3_665 6_666 ? O12 Ca1A O2 81.92(13) . 6_666 ? O13 Ca1A O2 66.10(11) 6_666 6_666 ? O3 Ca1A O2 118.94(19) 1_545 6_666 ? O1 Ca1A O2 133.64(15) . 6_666 ? Ca1B Ca1A Mg1 115.6(2) . . ? O4 Ca1A Mg1 152.83(15) 3_665 . ? O2 Ca1A Mg1 122.57(14) 3_665 . ? O12 Ca1A Mg1 40.99(7) . . ? O13 Ca1A Mg1 40.71(7) 6_666 . ? O3 Ca1A Mg1 97.12(9) 1_545 . ? O1 Ca1A Mg1 44.79(8) . . ? O2 Ca1A Mg1 89.45(11) 6_666 . ? Ca1B Ca1A Ca1A 109.9(2) . 5_766 ? O4 Ca1A Ca1A 41.39(14) 3_665 5_766 ? O2 Ca1A Ca1A 52.94(9) 3_665 5_766 ? O12 Ca1A Ca1A 104.47(9) . 5_766 ? O13 Ca1A Ca1A 110.75(18) 6_666 5_766 ? O3 Ca1A Ca1A 118.18(12) 1_545 5_766 ? O1 Ca1A Ca1A 171.23(12) . 5_766 ? O2 Ca1A Ca1A 45.88(10) 6_666 5_766 ? Mg1 Ca1A Ca1A 131.81(12) . 5_766 ? Ca1B Ca1A Mg1 46.95(18) . 3_665 ? O4 Ca1A Mg1 83.25(9) 3_665 3_665 ? O2 Ca1A Mg1 31.86(8) 3_665 3_665 ? O12 Ca1A Mg1 92.26(11) . 3_665 ? O13 Ca1A Mg1 164.01(14) 6_666 3_665 ? O3 Ca1A Mg1 107.17(13) 1_545 3_665 ? O1 Ca1A Mg1 97.39(12) . 3_665 ? O2 Ca1A Mg1 118.82(10) 6_666 3_665 ? Mg1 Ca1A Mg1 123.43(10) . 3_665 ? Ca1A Ca1A Mg1 78.31(10) 5_766 3_665 ? Ca1B Ca1A Ca1B 51.71(17) . 6_556 ? O4 Ca1A Ca1B 104.50(17) 3_665 6_556 ? O2 Ca1A Ca1B 129.04(15) 3_665 6_556 ? O12 Ca1A Ca1B 109.70(11) . 6_556 ? O13 Ca1A Ca1B 82.60(11) 6_666 6_556 ? O3 Ca1A Ca1B 30.34(14) 1_545 6_556 ? O1 Ca1A Ca1B 41.88(9) . 6_556 ? O2 Ca1A Ca1B 142.12(14) 6_666 6_556 ? Mg1 Ca1A Ca1B 79.14(8) . 6_556 ? Ca1A Ca1A Ca1B 145.71(7) 5_766 6_556 ? Mg1 Ca1A Ca1B 97.19(9) 3_665 6_556 ? Ca1B Ca1A H12 54.0(9) . . ? O4 Ca1A H12 135.7(11) 3_665 . ? O2 Ca1A H12 107.6(9) 3_665 . ? O12 Ca1A H12 76.1(11) . . ? O13 Ca1A H12 89.3(8) 6_666 . ? O3 Ca1A H12 68.4(12) 1_545 . ? O1 Ca1A H12 18.0(8) . . ? O2 Ca1A H12 151.1(9) 6_666 . ? Mg1 Ca1A H12 61.6(9) . . ? Ca1A Ca1A H12 159.4(9) 5_766 . ? Mg1 Ca1A H12 81.1(8) 3_665 . ? Ca1B Ca1A H12 38.0(12) 6_556 . ? Ca1B Ca1A H31 38.9(6) . 1_545 ? O4 Ca1A H31 78(3) 3_665 1_545 ? O2 Ca1A H31 113.0(12) 3_665 1_545 ? O12 Ca1A H31 135(3) . 1_545 ? O13 Ca1A H31 101.6(12) 6_666 1_545 ? O3 Ca1A H31 23.1(5) 1_545 1_545 ? O1 Ca1A H31 68(3) . 1_545 ? O2 Ca1A H31 137.7(18) 6_666 1_545 ? Mg1 Ca1A H31 107(2) . 1_545 ? Ca1A Ca1A H31 118(3) 5_766 1_545 ? Mg1 Ca1A H31 84.5(7) 3_665 1_545 ? Ca1B Ca1A H31 28(2) 6_556 1_545 ? H12 Ca1A H31 59(3) . 1_545 ? Ca1B Ca1A H32 84.6(9) . 6_666 ? O4 Ca1A H32 77(2) 3_665 6_666 ? O2 Ca1A H32 149(2) 3_665 6_666 ? O12 Ca1A H32 129(2) . 6_666 ? O13 Ca1A H32 61.2(15) 6_666 6_666 ? O3 Ca1A H32 22.6(9) 1_545 6_666 ? O1 Ca1A H32 77(2) . 6_666 ? O2 Ca1A H32 98.5(12) 6_666 6_666 ? Mg1 Ca1A H32 88(2) . 6_666 ? Ca1A Ca1A H32 112(2) 5_766 6_666 ? Mg1 Ca1A H32 128.9(11) 3_665 6_666 ? Ca1B Ca1A H32 45.6(16) 6_556 6_666 ? H12 Ca1A H32 81(2) . 6_666 ? H31 Ca1A H32 45.7(10) 1_545 6_666 ? Ca1B Ca1A H42 60.1(7) . 3_665 ? O4 Ca1A H42 25.7(7) 3_665 3_665 ? O2 Ca1A H42 76(3) 3_665 3_665 ? O12 Ca1A H42 158(3) . 3_665 ? O13 Ca1A H42 127(3) 6_666 3_665 ? O3 Ca1A H42 64(3) 1_545 3_665 ? O1 Ca1A H42 124.4(16) . 3_665 ? O2 Ca1A H42 96.7(8) 6_666 3_665 ? Mg1 Ca1A H42 161(3) . 3_665 ? Ca1A Ca1A H42 61.4(18) 5_766 3_665 ? Mg1 Ca1A H42 69(2) 3_665 3_665 ? Ca1B Ca1A H42 85(2) 6_556 3_665 ? H12 Ca1A H42 110.7(15) . 3_665 ? H31 Ca1A H42 57(3) 1_545 3_665 ? H32 Ca1A H42 74(4) 6_666 3_665 ? Ca1A Ca1B O3 86.4(2) . 1_545 ? Ca1A Ca1B O1 77.8(2) . . ? O3 Ca1B O1 76.66(13) 1_545 . ? Ca1A Ca1B O23 114.7(3) . 2_654 ? O3 Ca1B O23 145.6(2) 1_545 2_654 ? O1 Ca1B O23 81.66(14) . 2_654 ? Ca1A Ca1B O24 134.3(2) . 4_547 ? O3 Ca1B O24 112.54(17) 1_545 4_547 ? O1 Ca1B O24 145.22(18) . 4_547 ? O23 Ca1B O24 72.82(11) 2_654 4_547 ? Ca1A Ca1B O4 62.6(2) . 3_665 ? O3 Ca1B O4 77.67(17) 1_545 3_665 ? O1 Ca1B O4 133.67(16) . 3_665 ? O23 Ca1B O4 135.45(15) 2_654 3_665 ? O24 Ca1B O4 80.62(12) 4_547 3_665 ? Ca1A Ca1B O2 71.0(2) . 3_665 ? O3 Ca1B O2 146.7(2) 1_545 3_665 ? O1 Ca1B O2 119.88(17) . 3_665 ? O23 Ca1B O2 67.67(12) 2_654 3_665 ? O24 Ca1B O2 71.60(11) 4_547 3_665 ? O4 Ca1B O2 70.32(14) 3_665 3_665 ? Ca1A Ca1B O1 155.7(2) . 6_556 ? O3 Ca1B O1 71.23(14) 1_545 6_556 ? O1 Ca1B O1 87.58(14) . 6_556 ? O23 Ca1B O1 81.62(13) 2_654 6_556 ? O24 Ca1B O1 65.97(12) 4_547 6_556 ? O4 Ca1B O1 119.1(2) 3_665 6_556 ? O2 Ca1B O1 133.26(15) 3_665 6_556 ? Ca1A Ca1B Mg1 115.1(2) . 3_665 ? O3 Ca1B Mg1 152.84(16) 1_545 3_665 ? O1 Ca1B Mg1 122.24(15) . 3_665 ? O23 Ca1B Mg1 40.92(7) 2_654 3_665 ? O24 Ca1B Mg1 40.58(7) 4_547 3_665 ? O4 Ca1B Mg1 97.03(10) 3_665 3_665 ? O2 Ca1B Mg1 44.73(8) 3_665 3_665 ? O1 Ca1B Mg1 89.08(11) 6_556 3_665 ? Ca1A Ca1B Ca1B 110.2(2) . 6_556 ? O3 Ca1B Ca1B 41.28(15) 1_545 6_556 ? O1 Ca1B Ca1B 53.07(10) . 6_556 ? O23 Ca1B Ca1B 104.41(9) 2_654 6_556 ? O24 Ca1B Ca1B 110.85(19) 4_547 6_556 ? O4 Ca1B Ca1B 118.39(13) 3_665 6_556 ? O2 Ca1B Ca1B 171.02(12) 3_665 6_556 ? O1 Ca1B Ca1B 46.12(11) 6_556 6_556 ? Mg1 Ca1B Ca1B 131.70(12) 3_665 6_556 ? Ca1A Ca1B Mg1 46.56(18) . . ? O3 Ca1B Mg1 83.42(9) 1_545 . ? O1 Ca1B Mg1 31.89(8) . . ? O23 Ca1B Mg1 92.06(12) 2_654 . ? O24 Ca1B Mg1 163.65(14) 4_547 . ? O4 Ca1B Mg1 107.36(14) 3_665 . ? O2 Ca1B Mg1 97.22(13) 3_665 . ? O1 Ca1B Mg1 118.98(11) 6_556 . ? Mg1 Ca1B Mg1 123.20(11) 3_665 . ? Ca1B Ca1B Mg1 78.42(11) 6_556 . ? Ca1A Ca1B Ca1A 117.5(2) . 6_556 ? O3 Ca1B Ca1A 34.83(13) 1_545 6_556 ? O1 Ca1B Ca1A 71.04(10) . 6_556 ? O23 Ca1B Ca1A 112.47(13) 2_654 6_556 ? O24 Ca1B Ca1A 97.10(13) 4_547 6_556 ? O4 Ca1B Ca1A 105.68(18) 3_665 6_556 ? O2 Ca1B Ca1A 168.35(15) 3_665 6_556 ? O1 Ca1B Ca1A 38.41(8) 6_556 6_556 ? Mg1 Ca1B Ca1A 127.36(12) 3_665 6_556 ? Ca1B Ca1B Ca1A 18.07(7) 6_556 6_556 ? Mg1 Ca1B Ca1A 94.42(8) . 6_556 ? Ca1A Ca1B H12 79.5(14) . . ? O3 Ca1B H12 82.0(13) 1_545 . ? O1 Ca1B H12 5.6(13) . . ? O23 Ca1B H12 76.1(12) 2_654 . ? O24 Ca1B H12 141.6(13) 4_547 . ? O4 Ca1B H12 137.7(13) 3_665 . ? O2 Ca1B H12 116.0(15) 3_665 . ? O1 Ca1B H12 87.8(15) 6_556 . ? Mg1 Ca1B H12 116.7(13) 3_665 . ? Ca1B Ca1B H12 56.5(15) 6_556 . ? Mg1 Ca1B H12 33.0(14) . . ? Ca1A Ca1B H12 74.5(15) 6_556 . ? Ca1A Ca1B H31 106(3) . 1_545 ? O3 Ca1B H31 19(3) 1_545 1_545 ? O1 Ca1B H31 83(4) . 1_545 ? O23 Ca1B H31 132(3) 2_654 1_545 ? O24 Ca1B H31 97(3) 4_547 1_545 ? O4 Ca1B H31 86(4) 3_665 1_545 ? O2 Ca1B H31 155(4) 3_665 1_545 ? O1 Ca1B H31 53(3) 6_556 1_545 ? Mg1 Ca1B H31 135(3) 3_665 1_545 ? Ca1B Ca1B H31 34(4) 6_556 1_545 ? Mg1 Ca1B H31 98(3) . 1_545 ? Ca1A Ca1B H31 20(4) 6_556 1_545 ? H12 Ca1B H31 87(4) . 1_545 ? Ca1A Ca1B H32 61.5(10) . 6_666 ? O3 Ca1B H32 24.9(10) 1_545 6_666 ? O1 Ca1B H32 73(2) . 6_666 ? O23 Ca1B H32 155(2) 2_654 6_666 ? O24 Ca1B H32 128.9(19) 4_547 6_666 ? O4 Ca1B H32 67(2) 3_665 6_666 ? O2 Ca1B H32 126.5(14) 3_665 6_666 ? O1 Ca1B H32 95.9(11) 6_556 6_666 ? Mg1 Ca1B H32 164(2) 3_665 6_666 ? Ca1B Ca1B H32 59.2(15) 6_556 6_666 ? Mg1 Ca1B H32 67.3(19) . 6_666 ? Ca1A Ca1B H32 58.3(11) 6_556 6_666 ? H12 Ca1B H32 79(3) . 6_666 ? H31 Ca1B H32 44(3) 1_545 6_666 ? Ca1A Ca1B H42 83.9(14) . 3_665 ? O3 Ca1B H42 75(3) 1_545 3_665 ? O1 Ca1B H42 147(3) . 3_665 ? O23 Ca1B H42 132(3) 2_654 3_665 ? O24 Ca1B H42 64(3) 4_547 3_665 ? O4 Ca1B H42 21.5(13) 3_665 3_665 ? O2 Ca1B H42 79(3) 3_665 3_665 ? O1 Ca1B H42 98.7(14) 6_556 3_665 ? Mg1 Ca1B H42 91(3) 3_665 3_665 ? Ca1B Ca1B H42 110(3) 6_556 3_665 ? Mg1 Ca1B H42 127(2) . 3_665 ? Ca1A Ca1B H42 94(3) 6_556 3_665 ? H12 Ca1B H42 152(3) . 3_665 ? H31 Ca1B H42 76(5) 1_545 3_665 ? H32 Ca1B H42 73(4) 6_666 3_665 ? O12 P1 O13 115.36(15) . . ? O12 P1 O14 110.99(15) . . ? O13 P1 O14 106.06(15) . . ? O12 P1 O11 106.34(13) . . ? O13 P1 O11 111.24(13) . . ? O14 P1 O11 106.59(12) . . ? O23 P2 O24 115.48(15) . . ? O23 P2 O22 111.11(14) . 4_557 ? O24 P2 O22 106.11(14) . 4_557 ? O23 P2 O21 106.57(14) . . ? O24 P2 O21 111.09(13) . . ? O22 P2 O21 106.16(12) 4_557 . ? Mg1 O1 Ca1B 112.63(14) . . ? Mg1 O1 Ca1A 82.19(12) . . ? Ca1B O1 Ca1A 30.84(10) . . ? Mg1 O1 Ca1B 136.82(14) . 6_556 ? Ca1B O1 Ca1B 80.81(14) . 6_556 ? Ca1A O1 Ca1B 99.72(12) . 6_556 ? Mg1 O1 H11 107(2) . . ? Ca1B O1 H11 112.9(17) . . ? Ca1A O1 H11 130.4(18) . . ? Ca1B O1 H11 104(2) 6_556 . ? Mg1 O1 H12 113(2) . . ? Ca1B O1 H12 8.4(19) . . ? Ca1A O1 H12 34(2) . . ? Ca1B O1 H12 86(2) 6_556 . ? H11 O1 H12 105.2(17) . . ? Mg1 O2 Ca1A 112.89(14) . 2_654 ? Mg1 O2 Ca1B 82.48(12) . 2_654 ? Ca1A O2 Ca1B 30.89(10) 2_654 2_654 ? Mg1 O2 Ca1A 136.73(13) . 6_566 ? Ca1A O2 Ca1A 81.18(13) 2_654 6_566 ? Ca1B O2 Ca1A 99.82(13) 2_654 6_566 ? Mg1 O2 H21 104(2) . . ? Ca1A O2 H21 92(2) 2_654 . ? Ca1B O2 H21 104.8(18) 2_654 . ? Ca1A O2 H21 117(2) 6_566 . ? Mg1 O2 H22 104(2) . . ? Ca1A O2 H22 135(2) 2_654 . ? Ca1B O2 H22 148(2) 2_654 . ? Ca1A O2 H22 54(2) 6_566 . ? H21 O2 H22 104.0(17) . . ? B1 O11 P1 130.1(2) . . ? P1 O12 Mg1 130.23(15) . . ? P1 O12 Ca1A 142.14(15) . . ? Mg1 O12 Ca1A 87.62(11) . . ? P1 O13 Mg1 140.71(14) . 6_566 ? P1 O13 Ca1A 132.02(16) . 6_566 ? Mg1 O13 Ca1A 86.96(12) 6_566 6_566 ? B1 O14 P1 128.4(2) 5_766 . ? B1 O21 P2 130.2(2) . . ? B1 O22 P2 129.2(2) . 4_557 ? P2 O23 Mg1 130.20(15) . 2_655 ? P2 O23 Ca1B 142.19(15) . 3_665 ? Mg1 O23 Ca1B 87.59(12) 2_655 3_665 ? P2 O24 Mg1 140.59(14) . 5_766 ? P2 O24 Ca1B 131.92(16) . 4_657 ? Mg1 O24 Ca1B 87.24(13) 5_766 4_657 ? O14 B1 O22 102.8(2) 5_766 . ? O14 B1 O21 112.6(3) 5_766 . ? O22 B1 O21 113.6(3) . . ? O14 B1 O11 114.4(3) 5_766 . ? O22 B1 O11 112.1(3) . . ? O21 B1 O11 101.8(2) . . ? Ca1B O3 Ca1B 97.4(3) 1_565 6_566 ? Ca1B O3 Ca1A 31.62(11) 1_565 1_565 ? Ca1B O3 Ca1A 114.8(3) 6_566 1_565 ? Ca1B O3 Ca1A 114.8(3) 1_565 6_566 ? Ca1B O3 Ca1A 31.62(11) 6_566 6_566 ? Ca1A O3 Ca1A 141.8(3) 1_565 6_566 ? Ca1B O3 H31 28(5) 1_565 . ? Ca1B O3 H31 82(6) 6_566 . ? Ca1A O3 H31 60(5) 1_565 . ? Ca1A O3 H31 90(6) 6_566 . ? Ca1B O3 H32 128(5) 1_565 . ? Ca1B O3 H32 85(7) 6_566 . ? Ca1A O3 H32 149(6) 1_565 . ? Ca1A O3 H32 53(7) 6_566 . ? H31 O3 H32 103.1(19) . . ? Ca1A O4 Ca1A 97.2(3) 2_654 6_566 ? Ca1A O4 Ca1B 31.71(11) 2_654 2_654 ? Ca1A O4 Ca1B 114.9(3) 6_566 2_654 ? Ca1A O4 Ca1B 114.9(3) 2_654 6_566 ? Ca1A O4 Ca1B 31.71(11) 6_566 6_566 ? Ca1B O4 Ca1B 142.1(3) 2_654 6_566 ? Ca1A O4 H41 129(7) 2_654 . ? Ca1A O4 H41 114(6) 6_566 . ? Ca1B O4 H41 129(6) 2_654 . ? Ca1B O4 H41 83(6) 6_566 . ? Ca1A O4 H42 77(6) 2_654 . ? Ca1A O4 H42 134(7) 6_566 . ? Ca1B O4 H42 46(6) 2_654 . ? Ca1B O4 H42 158(7) 6_566 . ? H41 O4 H42 104(2) . . ? 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 Mg1 O13 2.041(3) 6_666 ? Mg1 O24 2.042(3) 5_766 ? Mg1 O12 2.051(2) . ? Mg1 O23 2.055(2) 3_664 ? Mg1 O1 2.222(3) . ? Mg1 O2 2.226(3) . ? Mg1 Ca1A 3.125(3) . ? Mg1 Ca1B 3.135(3) 2_654 ? Mg1 Ca1B 3.882(4) . ? Mg1 Ca1A 3.885(3) 2_654 ? Ca1A Ca1B 1.321(4) . ? Ca1A O4 2.233(5) 3_665 ? Ca1A O2 2.434(4) 3_665 ? Ca1A O12 2.444(4) . ? Ca1A O13 2.477(4) 6_666 ? Ca1A O3 2.516(4) 1_545 ? Ca1A O1 2.520(4) . ? Ca1A O2 2.705(4) 6_666 ? Ca1A Ca1A 3.350(6) 5_766 ? Ca1A Ca1B 3.998(5) 6_556 ? Ca1A H12 1.79(3) . ? Ca1A H31 2.19(9) 1_545 ? Ca1A H32 2.08(11) 6_666 ? Ca1A H42 2.23(10) 3_665 ? Ca1B O3 2.225(5) 1_545 ? Ca1B O1 2.442(4) . ? Ca1B O23 2.455(4) 2_654 ? Ca1B O24 2.480(4) 4_547 ? Ca1B O4 2.507(4) 3_665 ? Ca1B O2 2.518(4) 3_665 ? Ca1B O1 2.708(5) 6_556 ? Ca1B Ca1B 3.344(6) 6_556 ? Ca1B H12 1.473(14) . ? Ca1B H31 1.43(7) 1_545 ? Ca1B H32 2.36(11) 6_666 ? Ca1B H42 1.95(10) 3_665 ? P1 O12 1.503(3) . ? P1 O13 1.505(3) . ? P1 O14 1.562(2) . ? P1 O11 1.568(2) . ? P2 O23 1.501(3) . ? P2 O24 1.509(3) . ? P2 O22 1.558(2) 4_557 ? P2 O21 1.565(2) . ? O1 H11 0.979(13) . ? O1 H12 0.986(13) . ? O2 H21 0.981(13) . ? O2 H22 0.994(13) . ? O11 B1 1.486(4) . ? O14 B1 1.459(4) 5_766 ? O21 B1 1.477(4) . ? O22 B1 1.462(4) . ? O3 H31 0.994(14) . ? O3 H32 0.998(14) . ? O4 H41 0.994(14) . ? O4 H42 0.994(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 O1 H11 O11 0.979(13) 2.539(19) 3.381(3) 144(2) 2_654 yes O1 H11 O21 0.979(13) 1.836(19) 2.750(4) 154(3) 2_654 yes O2 H21 O11 0.981(13) 1.791(17) 2.743(4) 163(3) 2_654 yes O2 H21 O12 0.981(13) 2.56(3) 3.197(3) 122(2) 2_654 yes O2 H22 O13 0.994(13) 1.889(15) 2.833(3) 157(3) . yes O3 H31 O1 0.994(14) 2.16(8) 2.899(5) 129(7) 6_566 yes O3 H32 O13 0.998(14) 2.34(5) 3.232(3) 148(7) . yes O3 H32 O14 0.998(14) 2.21(8) 2.985(5) 133(9) . yes O4 H41 O22 0.994(14) 2.02(3) 2.998(5) 167(10) 6_676 yes O4 H42 O22 0.994(14) 2.34(9) 2.998(5) 123(8) 2_764 yes O4 H42 O24 0.994(14) 2.38(7) 3.226(3) 142(9) 5_766 yes