#------------------------------------------------------------------------------ #$Date: 2026-06-05 00:36:20 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306224 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721105.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_7721105 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 Cd H6 O11 P2' _chemical_formula_weight 387.24 _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-2019/3 _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 9.679(2) _cell_length_b 9.679(2) _cell_length_c 15.927(3) _cell_measurement_reflns_used 26356 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 29.989 _cell_measurement_theta_min 2.430 _cell_volume 1292.2(4) _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _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 0.2097 _diffrn_reflns_av_unetI/netI 0.1318 _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 26315 _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 29.988 _diffrn_reflns_theta_min 2.430 _exptl_absorpt_coefficient_mu 3.256 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_correction_T_min 0.6588 _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 2.986 _exptl_crystal_description block _exptl_crystal_F_000 1122 _exptl_crystal_size_max 0.086 _exptl_crystal_size_mid 0.076 _exptl_crystal_size_min 0.063 _exptl_transmission_factor_max 0.7466 _exptl_transmission_factor_min 0.6563 _refine_diff_density_max 1.129 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.172 _refine_ls_abs_structure_details ; Flack x determined using 568 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.023(13) _refine_ls_extinction_coef 0.0015(3) _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 0.947 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 2533 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 0.945 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0277 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0119P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0463 _reflns_Friedel_coverage 0.725 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 1669 _reflns_number_total 2533 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00484a2.cif _cod_data_source_block mo_MM23_2_0m_a _cod_original_cell_volume 1292.3(6) _cod_original_formula_sum 'B Ca0.50 H6 Cd O11 P2' _cod_database_code 7721105 _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_res_file ; TITL mo_MM23_2_0m_a.res in P6(1)22, C211 mo_MM23_2_0m_a.res created by SHELXL-2019/3 at 15:22:51 on 24-Apr-2026 CELL 0.71073 9.6792 9.6792 15.9275 90.000 90.00 120.000 ZERR 6 0.0020 0.0020 0.0030 0.000 0.000 0.000 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 CD 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 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 WGHT 0.011900 EXTI 0.001508 FVAR 0.25396 0.49895 CD1 6 0.095875 0.547982 0.416574 11.00000 0.02090 0.02983 = 0.02539 -0.01688 0.00018 0.01048 CA1A 5 0.099980 0.744836 0.258339 20.50000 0.02657 0.02388 = 0.01202 0.00087 0.00268 0.01311 CA1B 5 0.255049 0.899871 0.242550 -20.50000 0.02657 0.02388 = 0.01202 0.00087 0.00268 0.01311 P1 4 0.162385 0.383934 0.250879 11.00000 0.01856 0.01071 = 0.00686 -0.00168 0.00115 0.00586 P2 4 0.220992 0.384004 -0.083976 11.00000 0.01968 0.00964 = 0.00744 0.00133 0.00241 0.00503 O1 3 0.299874 0.816361 0.377021 11.00000 0.02071 0.03032 = 0.02566 -0.00700 0.00044 0.01250 H11 2 0.239515 0.784409 0.324165 11.00000 -1.20000 H12 2 0.405411 0.830814 0.362593 11.00000 -1.20000 O2 3 0.299282 0.483171 0.456125 11.00000 0.02314 0.02402 = 0.02457 -0.00495 -0.00225 0.00600 H21 2 0.398983 0.579293 0.472974 11.00000 -1.20000 H22 2 0.315872 0.469503 0.395881 11.00000 -1.20000 O11 3 0.185501 0.414128 0.154313 11.00000 0.02733 0.00888 = 0.00759 0.00090 0.00093 0.00545 O12 3 0.131037 0.510935 0.284064 11.00000 0.03951 0.01815 = 0.01399 -0.00510 0.00250 0.01428 O13 3 0.300478 0.381170 0.291336 11.00000 0.01680 0.02856 = 0.01124 0.00015 -0.00601 0.00567 O14 3 0.017251 0.213867 0.264653 11.00000 0.01653 0.01263 = 0.01148 0.00028 -0.00238 0.00701 O21 3 0.227965 0.413947 0.012123 11.00000 0.02858 0.01113 = 0.00609 0.00070 0.00344 0.00656 O22 3 0.214709 0.197254 0.097219 11.00000 0.01041 0.01013 = 0.01446 0.00179 -0.00122 0.00313 O23 3 0.379779 0.510871 -0.116325 11.00000 0.02801 0.01471 = 0.01805 0.00325 0.00880 -0.00004 O24 3 0.079959 0.380862 -0.123286 11.00000 0.03292 0.02710 = 0.01744 -0.00063 -0.00154 0.02234 B1 1 0.151834 0.303985 0.082374 11.00000 0.02144 0.01218 = 0.00328 -0.00035 0.00095 0.00777 O3 3 0.144769 0.000000 0.333333 10.50000 0.04404 0.05432 = 0.13373 0.02286 0.01143 0.02716 H31 2 0.250640 0.074409 0.309035 10.50000 -1.20000 H32 2 0.077529 0.046311 0.317134 10.50000 -1.20000 O4 3 0.145687 0.145687 0.500000 10.50000 0.05261 0.05261 = 0.15706 0.01118 -0.01118 0.03150 H41 2 0.066501 0.141811 0.459096 10.50000 -1.20000 H42 2 0.097303 0.141072 0.555732 10.50000 -1.20000 REM REM //cfs-physik.physik.uni-augsburg.de/wesselvi/Dokumente/Doktorand/Publi= REM =kationen/CaM(H2O)2[BP2O12]H2O-Paper/Einkristalldaten/P3121/_tri= REM =gonal/Cd-3/mo_MM23_2_0m_a.hkl REM HKLF 4 REM mo_MM23_2_0m_a.res in P6(1)22, C211 REM wR2 = 0.0463, GooF = S = 0.947, Restrained GooF = 0.945 for all data REM R1 = 0.0277 for 1669 Fo > 4sig(Fo) and 0.0687 for all 2533 data REM 175 parameters refined using 12 restraints END WGHT 0.0128 0.0000 REM Instructions for potential hydrogen bonds EQIV $6 -y+1, x-y+1, z+1/3 HTAB O2 O11_$6 HTAB O2 O12_$6 HTAB O2 O13 EQIV $4 x-y+1, -y+1, -z+2/3 HTAB O3 O1_$4 HTAB O3 O14 EQIV $14 -y, x-y, z+1/3 HTAB O4 O22_$14 EQIV $3 -x, -x+y, -z+1/3 HTAB O4 O24_$3 HTAB O4 O3_$14 REM Highest difference peak 1.129, deepest hole -1.232, 1-sigma level 0.172 Q1 1 0.1322 0.6038 0.3941 11.00000 0.05 1.13 Q2 1 0.1352 0.5125 0.4342 11.00000 0.05 0.87 Q3 1 0.3647 0.4224 0.2637 11.00000 0.05 0.70 Q4 1 0.2356 0.6180 0.4302 11.00000 0.05 0.66 Q5 1 0.3858 0.8648 0.4122 11.00000 0.05 0.66 Q6 1 0.1878 0.1909 0.2481 11.00000 0.05 0.64 Q7 1 -0.0353 0.0278 0.4020 11.00000 0.05 0.60 Q8 1 0.1672 0.7626 0.2507 11.00000 0.05 0.57 Q9 1 0.0473 0.3160 0.2371 11.00000 0.05 0.56 Q10 1 0.4214 0.5727 -0.1262 11.00000 0.05 0.56 ; _shelx_res_checksum 43291 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 Cd1 Cd 0.09587(4) 0.54798(5) 0.41657(3) 0.02635(14) Uani 1 1 d . . . . . Ca1A Ca 0.1000(6) 0.7448(6) 0.2583(3) 0.0206(7) Uani 0.249(2) 1 d . . P . . Ca1B Ca 0.2550(6) 0.8999(6) 0.2426(3) 0.0206(7) Uani 0.251(2) 1 d . . P . . P1 P 0.16238(17) 0.38393(16) 0.25088(8) 0.0127(3) Uani 1 1 d . . . . . P2 P 0.22099(18) 0.38400(16) -0.08398(8) 0.0133(3) Uani 1 1 d . . . . . O1 O 0.2999(4) 0.8164(5) 0.3770(2) 0.0257(9) Uani 1 1 d D . . . . H11 H 0.240(4) 0.784(6) 0.3242(17) 0.031 Uiso 1 1 d D U . . . H12 H 0.405(3) 0.831(6) 0.363(3) 0.031 Uiso 1 1 d D U . . . O2 O 0.2993(4) 0.4832(5) 0.4561(2) 0.0265(10) Uani 1 1 d D . . . . H21 H 0.399(3) 0.579(4) 0.473(2) 0.032 Uiso 1 1 d D U . . . H22 H 0.316(5) 0.470(6) 0.3959(12) 0.032 Uiso 1 1 d D U . . . O11 O 0.1855(4) 0.4141(4) 0.15431(19) 0.0162(8) Uani 1 1 d . . . . . O12 O 0.1310(5) 0.5109(4) 0.2841(2) 0.0239(9) Uani 1 1 d . . . . . O13 O 0.3005(4) 0.3812(4) 0.2913(2) 0.0214(9) Uani 1 1 d . . . . . O14 O 0.0173(4) 0.2139(4) 0.2647(2) 0.0137(8) Uani 1 1 d . . . . . O21 O 0.2280(4) 0.4139(4) 0.01212(19) 0.0168(8) Uani 1 1 d . . . . . O22 O 0.2147(4) 0.1973(4) 0.0972(2) 0.0126(8) Uani 1 1 d . . . . . O23 O 0.3798(4) 0.5109(4) -0.1163(2) 0.0250(9) Uani 1 1 d . . . . . O24 O 0.0800(4) 0.3809(4) -0.1233(2) 0.0226(9) Uani 1 1 d . . . . . B1 B 0.1518(8) 0.3040(6) 0.0824(3) 0.0126(12) Uani 1 1 d . . . . . O3 O 0.1448(7) 0.000000 0.333333 0.076(3) Uani 1 2 d DS T P . . H31 H 0.251(6) 0.074(13) 0.309(9) 0.091 Uiso 0.5 1 d D U P . . H32 H 0.078(10) 0.046(14) 0.317(10) 0.091 Uiso 0.5 1 d D U P . . O4 O 0.1457(9) 0.1457(9) 0.500000 0.085(3) Uani 1 2 d DS T P . . H41 H 0.067(14) 0.14(2) 0.459(8) 0.102 Uiso 0.5 1 d D U P . . H42 H 0.097(16) 0.14(2) 0.556(5) 0.102 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 Cd1 0.0209(2) 0.0298(3) 0.0254(2) -0.0169(2) 0.0002(2) 0.0105(2) Ca1A 0.027(2) 0.024(2) 0.0120(17) 0.0009(15) 0.0027(15) 0.0131(14) Ca1B 0.027(2) 0.024(2) 0.0120(17) 0.0009(15) 0.0027(15) 0.0131(14) P1 0.0186(8) 0.0107(7) 0.0069(7) -0.0017(5) 0.0012(6) 0.0059(6) P2 0.0197(9) 0.0096(7) 0.0074(7) 0.0013(5) 0.0024(6) 0.0050(6) O1 0.021(2) 0.030(2) 0.026(2) -0.007(2) 0.0004(18) 0.013(2) O2 0.023(2) 0.024(2) 0.025(2) -0.005(2) -0.0023(18) 0.0060(19) O11 0.027(2) 0.0089(17) 0.0076(17) 0.0009(14) 0.0009(16) 0.0055(17) O12 0.040(2) 0.018(2) 0.014(2) -0.0051(19) 0.002(2) 0.0143(19) O13 0.017(2) 0.029(2) 0.011(2) 0.0002(18) -0.0060(17) 0.0057(17) O14 0.017(2) 0.0126(19) 0.011(2) 0.0003(16) -0.0024(15) 0.0070(16) O21 0.029(2) 0.0111(17) 0.0061(17) 0.0007(15) 0.0034(16) 0.0066(16) O22 0.0104(19) 0.0101(19) 0.014(2) 0.0018(15) -0.0012(16) 0.0031(17) O23 0.028(2) 0.015(2) 0.018(2) 0.0033(19) 0.0088(17) 0.0000(18) O24 0.033(2) 0.027(2) 0.017(2) -0.0006(18) -0.0015(18) 0.0223(19) B1 0.021(4) 0.012(3) 0.003(3) 0.000(2) 0.001(3) 0.008(3) O3 0.044(3) 0.054(5) 0.134(9) 0.023(5) 0.011(3) 0.027(3) O4 0.053(4) 0.053(4) 0.157(9) 0.011(3) -0.011(3) 0.031(4) 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' Cd Cd -0.8075 1.2024 '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 O12 Cd1 O23 164.63(13) . 3_565 ? O12 Cd1 O24 101.40(14) . 5 ? O23 Cd1 O24 88.73(14) 3_565 5 ? O12 Cd1 O13 88.42(14) . 6_565 ? O23 Cd1 O13 101.91(13) 3_565 6_565 ? O24 Cd1 O13 97.05(12) 5 6_565 ? O12 Cd1 O2 89.73(14) . . ? O23 Cd1 O2 79.36(13) 3_565 . ? O24 Cd1 O2 86.06(13) 5 . ? O13 Cd1 O2 176.64(13) 6_565 . ? O12 Cd1 O1 79.40(13) . . ? O23 Cd1 O1 89.85(14) 3_565 . ? O24 Cd1 O1 176.69(13) 5 . ? O13 Cd1 O1 86.17(14) 6_565 . ? O2 Cd1 O1 90.74(11) . . ? O12 Cd1 Ca1A 51.18(14) . . ? O23 Cd1 Ca1A 128.73(13) 3_565 . ? O24 Cd1 Ca1A 130.65(13) 5 . ? O13 Cd1 Ca1A 50.14(13) 6_565 . ? O2 Cd1 Ca1A 126.68(13) . . ? O1 Cd1 Ca1A 52.28(13) . . ? O12 Cd1 Ca1B 128.76(14) . 2_665 ? O23 Cd1 Ca1B 50.88(14) 3_565 2_665 ? O24 Cd1 Ca1B 50.54(13) 5 2_665 ? O13 Cd1 Ca1B 130.88(12) 6_565 2_665 ? O2 Cd1 Ca1B 52.28(13) . 2_665 ? O1 Cd1 Ca1B 126.52(13) . 2_665 ? Ca1A Cd1 Ca1B 178.72(11) . 2_665 ? Ca1B Ca1A O4 82.8(3) . 3_564 ? Ca1B Ca1A O2 76.9(3) . 3_564 ? O4 Ca1A O2 76.6(2) 3_564 3_564 ? Ca1B Ca1A O13 136.9(3) . 6_565 ? O4 Ca1A O13 111.0(2) 3_564 6_565 ? O2 Ca1A O13 144.9(3) 3_564 6_565 ? Ca1B Ca1A O12 114.9(4) . . ? O4 Ca1A O12 143.9(3) 3_564 . ? O2 Ca1A O12 77.30(19) 3_564 . ? O13 Ca1A O12 78.38(19) 6_565 . ? Ca1B Ca1A O1 67.2(3) . . ? O4 Ca1A O1 142.3(3) 3_564 . ? O2 Ca1A O1 115.8(2) 3_564 . ? O13 Ca1A O1 79.91(18) 6_565 . ? O12 Ca1A O1 72.56(19) . . ? Ca1B Ca1A O3 61.4(3) . 1_565 ? O4 Ca1A O3 76.1(2) 3_564 1_565 ? O2 Ca1A O3 132.3(2) 3_564 1_565 ? O13 Ca1A O3 81.92(18) 6_565 1_565 ? O12 Ca1A O3 139.9(2) . 1_565 ? O1 Ca1A O3 69.7(2) . 1_565 ? Ca1B Ca1A O2 151.6(4) . 6_565 ? O4 Ca1A O2 72.4(2) 3_564 6_565 ? O2 Ca1A O2 84.0(2) 3_564 6_565 ? O13 Ca1A O2 67.23(18) 6_565 6_565 ? O12 Ca1A O2 80.41(19) . 6_565 ? O1 Ca1A O2 141.0(2) . 6_565 ? O3 Ca1A O2 122.8(3) 1_565 6_565 ? Ca1B Ca1A Cd1 115.9(3) . . ? O4 Ca1A Cd1 155.9(2) 3_564 . ? O2 Ca1A Cd1 120.8(2) 3_564 . ? O13 Ca1A Cd1 45.00(12) 6_565 . ? O12 Ca1A Cd1 44.00(11) . . ? O1 Ca1A Cd1 49.21(13) . . ? O3 Ca1A Cd1 98.87(15) 1_565 . ? O2 Ca1A Cd1 91.84(17) 6_565 . ? Ca1B Ca1A Ca1A 106.4(3) . 5 ? O4 Ca1A Ca1A 42.5(2) 3_564 5 ? O2 Ca1A Ca1A 50.99(16) 3_564 5 ? O13 Ca1A Ca1A 110.8(2) 6_565 5 ? O12 Ca1A Ca1A 101.36(14) . 5 ? O1 Ca1A Ca1A 166.8(2) . 5 ? O3 Ca1A Ca1A 118.32(15) 1_565 5 ? O2 Ca1A Ca1A 45.53(15) 6_565 5 ? Cd1 Ca1A Ca1A 133.55(15) . 5 ? Ca1B Ca1A Ca1B 52.3(3) . 6_675 ? O4 Ca1A Ca1B 104.1(3) 3_564 6_675 ? O2 Ca1A Ca1B 128.0(2) 3_564 6_675 ? O13 Ca1A Ca1B 84.63(18) 6_565 6_675 ? O12 Ca1A Ca1B 111.66(19) . 6_675 ? O1 Ca1A Ca1B 39.25(13) . 6_675 ? O3 Ca1A Ca1B 31.28(16) 1_565 6_675 ? O2 Ca1A Ca1B 146.9(2) 6_565 6_675 ? Cd1 Ca1A Ca1B 79.03(12) . 6_675 ? Ca1A Ca1A Ca1B 145.93(12) 5 6_675 ? Ca1B Ca1A Ca1B 115.2(4) . 5 ? O4 Ca1A Ca1B 35.65(17) 3_564 5 ? O2 Ca1A Ca1B 71.98(16) 3_564 5 ? O13 Ca1A Ca1B 94.21(18) 6_565 5 ? O12 Ca1A Ca1B 111.6(2) . 5 ? O1 Ca1A Ca1B 172.2(2) . 5 ? O3 Ca1A Ca1B 104.4(2) 1_565 5 ? O2 Ca1A Ca1B 37.58(12) 6_565 5 ? Cd1 Ca1A Ca1B 128.89(17) . 5 ? Ca1A Ca1A Ca1B 21.04(11) 5 5 ? Ca1B Ca1A Ca1B 135.6(2) 6_675 5 ? Ca1B Ca1A H11 64.7(18) . . ? O4 Ca1A H11 144.3(19) 3_564 . ? O2 Ca1A H11 108.1(14) 3_564 . ? O13 Ca1A H11 85.8(16) 6_565 . ? O12 Ca1A H11 68.5(18) . . ? O1 Ca1A H11 7.8(14) . . ? O3 Ca1A H11 75.5(16) 1_565 . ? O2 Ca1A H11 142.5(19) 6_565 . ? Cd1 Ca1A H11 51.2(18) . . ? Ca1A Ca1A H11 159.0(14) 5 . ? Ca1B Ca1A H11 44.4(17) 6_675 . ? Ca1B Ca1A H11 179.9(17) 5 . ? Ca1B Ca1A H31 64(2) . 6_565 ? O4 Ca1A H31 98.2(10) 3_564 6_565 ? O2 Ca1A H31 141(2) 3_564 6_565 ? O13 Ca1A H31 74(2) 6_565 6_565 ? O12 Ca1A H31 117.8(10) . 6_565 ? O1 Ca1A H31 48.7(11) . 6_565 ? O3 Ca1A H31 22.1(9) 1_565 6_565 ? O2 Ca1A H31 132(2) 6_565 6_565 ? Cd1 Ca1A H31 78.6(14) . 6_565 ? Ca1A Ca1A H31 140.4(9) 5 6_565 ? Ca1B Ca1A H31 15(2) 6_675 6_565 ? Ca1B Ca1A H31 124.7(12) 5 6_565 ? H11 Ca1A H31 55(2) . 6_565 ? Ca1B Ca1A H42 73(5) . 3_564 ? O4 Ca1A H42 25.6(7) 3_564 3_564 ? O2 Ca1A H42 97(3) 3_564 3_564 ? O13 Ca1A H42 102(5) 6_565 3_564 ? O12 Ca1A H42 169(2) . 3_564 ? O1 Ca1A H42 118.6(19) . 3_564 ? O3 Ca1A H42 50.5(7) 1_565 3_564 ? O2 Ca1A H42 89(4) 6_565 3_564 ? Cd1 Ca1A H42 142(4) . 3_564 ? Ca1A Ca1A H42 67.9(8) 5 3_564 ? Ca1B Ca1A H42 79.4(16) 6_675 3_564 ? Ca1B Ca1A H42 57(3) 5 3_564 ? H11 Ca1A H42 123(3) . 3_564 ? H31 Ca1A H42 72.6(11) 6_565 3_564 ? Ca1A Ca1B O3 82.8(3) . 1_565 ? Ca1A Ca1B O1 77.1(3) . . ? O3 Ca1B O1 77.27(19) 1_565 . ? Ca1A Ca1B O24 136.4(3) . 4_565 ? O3 Ca1B O24 111.1(2) 1_565 4_565 ? O1 Ca1B O24 145.1(3) . 4_565 ? Ca1A Ca1B O23 114.9(4) . 2_665 ? O3 Ca1B O23 144.2(3) 1_565 2_665 ? O1 Ca1B O23 77.0(2) . 2_665 ? O24 Ca1B O23 78.37(18) 4_565 2_665 ? Ca1A Ca1B O2 67.5(3) . 3_564 ? O3 Ca1B O2 142.0(3) 1_565 3_564 ? O1 Ca1B O2 116.0(2) . 3_564 ? O24 Ca1B O2 78.94(18) 4_565 3_564 ? O23 Ca1B O2 72.64(19) 2_665 3_564 ? Ca1A Ca1B O4 61.4(3) . 3_564 ? O3 Ca1B O4 76.0(2) 1_565 3_564 ? O1 Ca1B O4 132.7(2) . 3_564 ? O24 Ca1B O4 81.44(19) 4_565 3_564 ? O23 Ca1B O4 139.6(2) 2_665 3_564 ? O2 Ca1B O4 69.3(2) 3_564 3_564 ? Ca1A Ca1B O1 151.9(3) . 6_675 ? O3 Ca1B O1 72.74(18) 1_565 6_675 ? O1 Ca1B O1 84.2(2) . 6_675 ? O24 Ca1B O1 67.62(17) 4_565 6_675 ? O23 Ca1B O1 80.21(19) 2_665 6_675 ? O2 Ca1B O1 140.4(2) 3_564 6_675 ? O4 Ca1B O1 123.0(3) 3_564 6_675 ? Ca1A Ca1B Cd1 115.9(3) . 3_564 ? O3 Ca1B Cd1 155.6(2) 1_565 3_564 ? O1 Ca1B Cd1 120.7(2) . 3_564 ? O24 Ca1B Cd1 44.51(11) 4_565 3_564 ? O23 Ca1B Cd1 44.24(11) 2_665 3_564 ? O2 Ca1B Cd1 48.91(13) 3_564 3_564 ? O4 Ca1B Cd1 98.37(15) 3_564 3_564 ? O1 Ca1B Cd1 91.63(16) 6_675 3_564 ? Ca1A Ca1B Ca1B 106.6(3) . 6_675 ? O3 Ca1B Ca1B 42.87(18) 1_565 6_675 ? O1 Ca1B Ca1B 51.37(15) . 6_675 ? O24 Ca1B Ca1B 111.2(2) 4_565 6_675 ? O23 Ca1B Ca1B 101.29(14) 2_665 6_675 ? O2 Ca1B Ca1B 167.3(2) 3_564 6_675 ? O4 Ca1B Ca1B 118.64(16) 3_564 6_675 ? O1 Ca1B Ca1B 45.54(14) 6_675 6_675 ? Cd1 Ca1B Ca1B 133.50(15) 3_564 6_675 ? Ca1A Ca1B Ca1A 115.4(3) . 6_675 ? O3 Ca1B Ca1A 35.92(15) 1_565 6_675 ? O1 Ca1B Ca1A 72.42(16) . 6_675 ? O24 Ca1B Ca1A 94.51(18) 4_565 6_675 ? O23 Ca1B Ca1A 111.5(2) 2_665 6_675 ? O2 Ca1B Ca1A 171.5(2) 3_564 6_675 ? O4 Ca1B Ca1A 104.6(2) 3_564 6_675 ? O1 Ca1B Ca1A 37.67(12) 6_675 6_675 ? Cd1 Ca1B Ca1A 128.71(17) 3_564 6_675 ? Ca1B Ca1B Ca1A 21.10(11) 6_675 6_675 ? Ca1A Ca1B Ca1A 52.6(3) . 5 ? O3 Ca1B Ca1A 103.9(2) 1_565 5 ? O1 Ca1B Ca1A 128.3(2) . 5 ? O24 Ca1B Ca1A 83.78(18) 4_565 5 ? O23 Ca1B Ca1A 111.55(19) 2_665 5 ? O2 Ca1B Ca1A 39.05(13) 3_564 5 ? O4 Ca1B Ca1A 31.05(19) 3_564 5 ? O1 Ca1B Ca1A 146.6(2) 6_675 5 ? Cd1 Ca1B Ca1A 78.61(12) 3_564 5 ? Ca1B Ca1B Ca1A 146.24(12) 6_675 5 ? Ca1A Ca1B Ca1A 135.6(2) 6_675 5 ? Ca1A Ca1B H11 59.8(11) . . ? O3 Ca1B H11 83.5(14) 1_565 . ? O1 Ca1B H11 18.8(12) . . ? O24 Ca1B H11 157.7(13) 4_565 . ? O23 Ca1B H11 80.1(13) 2_665 . ? O2 Ca1B H11 100.2(13) 3_564 . ? O4 Ca1B H11 119.4(12) 3_564 . ? O1 Ca1B H11 102.9(12) 6_675 . ? Cd1 Ca1B H11 119.0(14) 3_564 . ? Ca1B Ca1B H11 67.5(13) 6_675 . ? Ca1A Ca1B H11 87.9(13) 6_675 . ? Ca1A Ca1B H11 109.8(12) 5 . ? Ca1A Ca1B H12 91.5(9) . . ? O3 Ca1B H12 94.7(7) 1_565 . ? O1 Ca1B H12 21.5(5) . . ? O24 Ca1B H12 126.2(7) 4_565 . ? O23 Ca1B H12 56.0(5) 2_665 . ? O2 Ca1B H12 108.7(9) 3_564 . ? O4 Ca1B H12 152.0(8) 3_564 . ? O1 Ca1B H12 77.3(10) 6_675 . ? Cd1 Ca1B H12 100.2(6) 3_564 . ? Ca1B Ca1B H12 59.5(9) 6_675 . ? Ca1A Ca1B H12 79.5(9) 6_675 . ? Ca1A Ca1B H12 135.7(10) 5 . ? H11 Ca1B H12 32.6(14) . . ? Ca1A Ca1B H31 108.4(6) . 1_565 ? O3 Ca1B H31 25.7(5) 1_565 1_565 ? O1 Ca1B H31 84(3) . 1_565 ? O24 Ca1B H31 91(2) 4_565 1_565 ? O23 Ca1B H31 127(2) 2_665 1_565 ? O2 Ca1B H31 157(3) 3_564 1_565 ? O4 Ca1B H31 88(3) 3_564 1_565 ? O1 Ca1B H31 48.2(13) 6_675 1_565 ? Cd1 Ca1B H31 132.6(12) 3_564 1_565 ? Ca1B Ca1B H31 35(3) 6_675 1_565 ? Ca1A Ca1B H31 16(3) 6_675 1_565 ? Ca1A Ca1B H31 119(3) 5 1_565 ? H11 Ca1B H31 97(3) . 1_565 ? H12 Ca1B H31 94(4) . 1_565 ? Ca1A Ca1B H31 74(3) . 6_565 ? O3 Ca1B H31 25.7(4) 1_565 6_565 ? O1 Ca1B H31 52.0(8) . 6_565 ? O24 Ca1B H31 134(2) 4_565 6_565 ? O23 Ca1B H31 126(2) 2_665 6_565 ? O2 Ca1B H31 142(3) 3_564 6_565 ? O4 Ca1B H31 93(3) 3_564 6_565 ? O1 Ca1B H31 78(3) 6_675 6_565 ? Cd1 Ca1B H31 167(3) 3_564 6_565 ? Ca1B Ca1B H31 34(3) 6_675 6_565 ? Ca1A Ca1B H31 42(3) 6_675 6_565 ? Ca1A Ca1B H31 114(3) 5 6_565 ? H11 Ca1B H31 58.0(15) . 6_565 ? H12 Ca1B H31 71.0(15) . 6_565 ? H31 Ca1B H31 42(3) 1_565 6_565 ? Ca1A Ca1B H42 63(4) . 3_564 ? O3 Ca1B H42 54.6(18) 1_565 3_564 ? O1 Ca1B H42 119(3) . 3_564 ? O24 Ca1B H42 91(4) 4_565 3_564 ? O23 Ca1B H42 161(2) 2_665 3_564 ? O2 Ca1B H42 90(2) 3_564 3_564 ? O4 Ca1B H42 21.4(19) 3_564 3_564 ? O1 Ca1B H42 110(3) 6_675 3_564 ? Cd1 Ca1B H42 118(3) 3_564 3_564 ? Ca1B Ca1B H42 97.3(18) 6_675 3_564 ? Ca1A Ca1B H42 85(2) 6_675 3_564 ? Ca1A Ca1B H42 51(2) 5 3_564 ? H11 Ca1B H42 112(4) . 3_564 ? H12 Ca1B H42 140(3) . 3_564 ? H31 Ca1B H42 69(3) 1_565 3_564 ? H31 Ca1B H42 73(3) 6_565 3_564 ? O13 P1 O12 114.3(2) . . ? O13 P1 O14 105.2(2) . . ? O12 P1 O14 111.8(2) . . ? O13 P1 O11 112.5(2) . . ? O12 P1 O11 105.2(2) . . ? O14 P1 O11 107.83(19) . . ? O24 P2 O23 115.2(2) . . ? O24 P2 O22 105.7(2) . 4 ? O23 P2 O22 111.6(2) . 4 ? O24 P2 O21 111.9(2) . . ? O23 P2 O21 104.8(2) . . ? O22 P2 O21 107.51(19) 4 . ? Ca1B O1 Cd1 113.78(19) . . ? Ca1B O1 Ca1A 35.71(15) . . ? Cd1 O1 Ca1A 78.51(16) . . ? Ca1B O1 Ca1B 83.1(2) . 6_675 ? Cd1 O1 Ca1B 132.37(19) . 6_675 ? Ca1A O1 Ca1B 103.08(19) . 6_675 ? Ca1B O1 H11 33(3) . . ? Cd1 O1 H11 81(3) . . ? Ca1A O1 H11 13(2) . . ? Ca1B O1 H11 111(3) 6_675 . ? Ca1B O1 H12 95(3) . . ? Cd1 O1 H12 116(3) . . ? Ca1A O1 H12 117(2) . . ? Ca1B O1 H12 105(3) 6_675 . ? H11 O1 H12 104.8(18) . . ? Ca1A O2 Cd1 113.92(19) 2_665 . ? Ca1A O2 Ca1B 35.55(15) 2_665 2_665 ? Cd1 O2 Ca1B 78.81(16) . 2_665 ? Ca1A O2 Ca1A 83.5(2) 2_665 6_665 ? Cd1 O2 Ca1A 132.37(19) . 6_665 ? Ca1B O2 Ca1A 103.37(19) 2_665 6_665 ? Ca1A O2 H21 95(3) 2_665 . ? Cd1 O2 H21 111(3) . . ? Ca1B O2 H21 114(2) 2_665 . ? Ca1A O2 H21 111(3) 6_665 . ? Ca1A O2 H22 143(3) 2_665 . ? Cd1 O2 H22 89(3) . . ? Ca1B O2 H22 142(2) 2_665 . ? Ca1A O2 H22 60(3) 6_665 . ? H21 O2 H22 104.0(18) . . ? B1 O11 P1 131.8(3) . . ? P1 O12 Cd1 125.7(2) . . ? P1 O12 Ca1A 149.5(2) . . ? Cd1 O12 Ca1A 84.82(15) . . ? P1 O13 Cd1 134.2(2) . 6_665 ? P1 O13 Ca1A 139.6(2) . 6_665 ? Cd1 O13 Ca1A 84.86(17) 6_665 6_665 ? B1 O14 P1 130.6(4) 5 . ? B1 O21 P2 131.2(3) . . ? B1 O22 P2 131.1(4) . 4 ? P2 O23 Cd1 125.1(2) . 2_664 ? P2 O23 Ca1B 150.0(2) . 3_564 ? Cd1 O23 Ca1B 84.88(15) 2_664 3_564 ? P2 O24 Cd1 135.1(2) . 5 ? P2 O24 Ca1B 138.9(2) . 4_455 ? Cd1 O24 Ca1B 84.95(17) 5 4_455 ? O14 B1 O22 103.8(3) 5 . ? O14 B1 O21 112.5(5) 5 . ? O22 B1 O21 113.7(5) . . ? O14 B1 O11 113.2(5) 5 . ? O22 B1 O11 111.4(5) . . ? O21 B1 O11 102.6(3) . . ? Ca1B O3 Ca1B 94.3(4) 1_545 6_665 ? Ca1B O3 Ca1A 35.85(15) 1_545 1_545 ? Ca1B O3 Ca1A 112.8(3) 6_665 1_545 ? Ca1B O3 Ca1A 112.8(3) 1_545 6_665 ? Ca1B O3 Ca1A 35.85(15) 6_665 6_665 ? Ca1A O3 Ca1A 143.8(4) 1_545 6_665 ? Ca1B O3 H31 62(9) 1_545 . ? Ca1B O3 H31 64(8) 6_665 . ? Ca1A O3 H31 98(9) 1_545 . ? Ca1A O3 H31 57(10) 6_665 . ? Ca1B O3 H32 125(10) 1_545 . ? Ca1B O3 H32 128(10) 6_665 . ? Ca1A O3 H32 119(10) 1_545 . ? Ca1A O3 H32 94(9) 6_665 . ? H31 O3 H32 104.1(19) . . ? Ca1A O4 Ca1A 95.0(4) 2_665 6_665 ? Ca1A O4 Ca1B 35.80(15) 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 35.80(15) 6_665 6_665 ? Ca1B O4 Ca1B 144.2(4) 2_665 6_665 ? Ca1A O4 H41 117(10) 2_665 . ? Ca1A O4 H41 95(9) 6_665 . ? Ca1B O4 H41 85(10) 2_665 . ? Ca1B O4 H41 110(10) 6_665 . ? Ca1A O4 H42 58(10) 2_665 . ? Ca1A O4 H42 152(9) 6_665 . ? Ca1B O4 H42 50(10) 2_665 . ? Ca1B O4 H42 143(10) 6_665 . ? 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 Cd1 O12 2.196(3) . ? Cd1 O23 2.215(3) 3_565 ? Cd1 O24 2.225(4) 5 ? Cd1 O13 2.235(4) 6_565 ? Cd1 O2 2.429(4) . ? Cd1 O1 2.432(4) . ? Cd1 Ca1A 3.148(5) . ? Cd1 Ca1B 3.162(5) 2_665 ? Ca1A Ca1B 1.522(6) . ? Ca1A O4 2.284(8) 3_564 ? Ca1A O2 2.419(6) 3_564 ? Ca1A O13 2.426(6) 6_565 ? Ca1A O12 2.463(7) . ? Ca1A O1 2.541(6) . ? Ca1A O3 2.578(6) 1_565 ? Ca1A O2 2.634(6) 6_565 ? Ca1A Ca1A 3.367(10) 5 ? Ca1A Ca1B 4.050(7) 6_675 ? Ca1A Ca1B 4.067(7) 5 ? Ca1A H11 1.598(18) . ? Ca1A H31 2.19(17) 6_565 ? Ca1A H42 1.95(17) 3_564 ? Ca1B O3 2.281(7) 1_565 ? Ca1B O1 2.404(6) . ? Ca1B O24 2.451(6) 4_565 ? Ca1B O23 2.463(7) 2_665 ? Ca1B O2 2.550(6) 3_564 ? Ca1B O4 2.581(6) 3_564 ? Ca1B O1 2.631(6) 6_675 ? Ca1B Ca1B 3.344(10) 6_675 ? Ca1B H11 1.67(4) . ? Ca1B H12 2.68(4) . ? Ca1B H31 2.01(15) 1_565 ? Ca1B H31 2.05(14) 6_565 ? Ca1B H42 2.08(19) 3_564 ? P1 O13 1.496(4) . ? P1 O12 1.502(4) . ? P1 O14 1.555(3) . ? P1 O11 1.561(3) . ? P2 O24 1.488(4) . ? P2 O23 1.499(4) . ? P2 O22 1.551(3) 4 ? P2 O21 1.553(3) . ? O1 H11 0.982(13) . ? O1 H12 0.986(13) . ? O2 H21 0.985(14) . ? O2 H22 0.993(13) . ? O11 B1 1.486(6) . ? O14 B1 1.451(7) 5 ? O21 B1 1.464(6) . ? O22 B1 1.457(7) . ? O3 H31 0.990(14) . ? O3 H32 0.991(14) . ? O4 H41 0.992(14) . ? O4 H42 0.994(14) . ?