Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Christopher David Johnson' 'Jorg Feldmann' 'Magnus G. Johnston' 'Donald E. Macphee' 'Jan Skakle' _publ_contact_author_name 'Dr Christopher David Johnson' _publ_contact_author_address ; Dept of Geological Sciences University of Durham Science Laboratories South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email C.D.JOHNSON@DURHAM.AC.UK _publ_section_title ; Hydrothermal synthesis, crystal structure and aqueous stability of two cadmium arsenate phases, CdNH4(HAsO4)OH and Cd5H2(AsO4)4.4H2O. ; data_cj3 _database_code_CSD 204641 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'H6 As Cd N O5' _chemical_formula_sum 'H6 As Cd N O5' _chemical_formula_weight 284.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' As As 0.0499 2.0058 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.682(4) _cell_length_b 6.0098(12) _cell_length_c 5.1917(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 551.68(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1424 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 9.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.802 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method \f-\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5288 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 32.49 _reflns_number_total 1068 _reflns_number_gt 791 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortex in OSCAIL (McArdle, 1994, 2000) ATOMS (Dowty, 1999) ORTEP-III for Windows (Farrugia, 1999) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms were not located within the unit cell, due to the presence of the high electron density Cd atoms ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0293P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1068 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.26195(3) 0.2500 0.39200(8) 0.02242(12) Uani 1 2 d . . . As1 As 0.14275(3) 0.2500 0.82664(11) 0.01991(14) Uani 1 2 d . . . O1 O 0.1576(2) 0.2500 1.1436(8) 0.0316(10) Uani 1 2 d . . . O2 O 0.3572(3) 0.2500 0.7115(9) 0.0362(11) Uani 1 2 d . . . O3 O 0.18402(18) 0.0291(5) 0.6770(5) 0.0313(7) Uani 1 1 d . . . O4 O 0.0490(2) 0.2500 0.7714(10) 0.0430(12) Uani 1 2 d . . . N1 N -0.0155(3) 0.2500 0.2890(13) 0.0496(17) Uani 1 2 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 Cd1 0.0371(2) 0.01363(18) 0.01647(19) 0.000 0.00407(17) 0.000 As1 0.0265(3) 0.0134(3) 0.0199(3) 0.000 0.0013(2) 0.000 O1 0.037(2) 0.035(3) 0.022(2) 0.000 0.0020(17) 0.000 O2 0.043(3) 0.033(3) 0.033(3) 0.000 -0.005(2) 0.000 O3 0.055(2) 0.0178(15) 0.0206(15) 0.0023(12) 0.0036(12) 0.0111(14) O4 0.027(2) 0.051(3) 0.051(3) 0.000 -0.004(2) 0.000 N1 0.041(4) 0.048(4) 0.060(4) 0.000 0.019(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O3 2.230(3) 2_554 ? Cd1 O3 2.230(3) 8_665 ? Cd1 O1 2.251(4) 1_554 ? Cd1 O2 2.364(5) . ? Cd1 O3 2.419(3) . ? Cd1 O3 2.419(3) 7_565 ? Cd1 As1 3.0876(8) . ? As1 O1 1.667(4) . ? As1 O4 1.682(4) . ? As1 O3 1.703(3) 7_565 ? As1 O3 1.703(3) . ? O1 Cd1 2.251(4) 1_556 ? O3 Cd1 2.230(3) 2 ? 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 O3 Cd1 O3 97.56(16) 2_554 8_665 ? O3 Cd1 O1 93.70(10) 2_554 1_554 ? O3 Cd1 O1 93.70(10) 8_665 1_554 ? O3 Cd1 O2 92.64(10) 2_554 . ? O3 Cd1 O2 92.64(10) 8_665 . ? O1 Cd1 O2 170.37(15) 1_554 . ? O3 Cd1 O3 97.90(7) 2_554 . ? O3 Cd1 O3 164.41(12) 8_665 . ? O1 Cd1 O3 83.31(11) 1_554 . ? O2 Cd1 O3 88.65(12) . . ? O3 Cd1 O3 164.41(12) 2_554 7_565 ? O3 Cd1 O3 97.90(7) 8_665 7_565 ? O1 Cd1 O3 83.31(11) 1_554 7_565 ? O2 Cd1 O3 88.65(12) . 7_565 ? O3 Cd1 O3 66.58(13) . 7_565 ? O3 Cd1 As1 131.17(8) 2_554 . ? O3 Cd1 As1 131.17(8) 8_665 . ? O1 Cd1 As1 81.90(11) 1_554 . ? O2 Cd1 As1 88.47(12) . . ? O3 Cd1 As1 33.29(7) . . ? O3 Cd1 As1 33.29(7) 7_565 . ? O1 As1 O4 108.9(2) . . ? O1 As1 O3 112.53(13) . 7_565 ? O4 As1 O3 110.15(14) . 7_565 ? O1 As1 O3 112.53(12) . . ? O4 As1 O3 110.15(14) . . ? O3 As1 O3 102.5(2) 7_565 . ? O1 As1 Cd1 127.90(16) . . ? O4 As1 Cd1 123.23(18) . . ? O3 As1 Cd1 51.24(10) 7_565 . ? O3 As1 Cd1 51.24(10) . . ? As1 O1 Cd1 134.0(2) . 1_556 ? As1 O3 Cd1 122.81(14) . 2 ? As1 O3 Cd1 95.47(12) . . ? Cd1 O3 Cd1 118.36(13) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.083 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.199 #===END data_revision _database_code_CSD 204642 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'H10 As4 Cd5 O20' _chemical_formula_sum 'H10 As4 Cd5 O20' _chemical_formula_weight 1191.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' As As 0.0499 2.0058 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.382(2) _cell_length_b 9.7192(13) _cell_length_c 9.9791(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.369(3) _cell_angle_gamma 90.00 _cell_volume 1771.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5723 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 29.44 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 13.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # absolute Tmin and Tmax unknown, but SADABS gives ratio as 0.701 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6928 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 15 _diffrn_reflns_number 5553 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 29.44 _reflns_number_total 2246 _reflns_number_gt 2206 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortex in OSCAIL (McArdle, 1994, 2000) ATOMS (Dowty, 1999) ORTEP-III for Windows (Farrugia, 1999) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms were not located within the unit cell, due to the presence of the high electron density Cd atoms ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+9.4738P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2246 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.212 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.10421(5) -0.2500 0.00620(13) Uani 1 d S . . Cd2 Cd 0.321527(18) 0.08535(3) -0.31358(3) 0.00682(12) Uani 1 d . . . Cd3 Cd 0.177759(18) -0.02813(3) -0.13440(3) 0.00632(12) Uani 1 d . . . As1 As 0.08373(3) -0.17680(5) -0.41298(5) 0.00546(14) Uani 1 d . . . As2 As 0.16141(3) 0.25870(4) -0.37582(5) 0.00466(13) Uani 1 d . . . O1 O 0.1583(2) -0.2751(4) -0.3736(4) 0.0111(7) Uani 1 d . . . O2 O 0.0101(2) -0.2870(4) -0.4248(4) 0.0148(8) Uani 1 d . . . O3 O 0.0790(2) -0.0645(4) -0.2892(4) 0.0101(7) Uani 1 d . . . O4 O 0.0848(2) -0.1021(4) -0.5633(4) 0.0100(7) Uani 1 d . . . O5 O 0.1658(2) 0.2337(3) -0.5426(3) 0.0068(6) Uani 1 d . . . O6 O 0.07228(19) 0.2635(3) -0.3486(4) 0.0075(6) Uani 1 d . . . O7 O 0.20288(19) 0.4084(3) -0.3317(4) 0.0086(7) Uani 1 d . . . O8 O 0.20526(19) 0.1286(4) -0.2889(4) 0.0098(7) Uani 1 d . . . O9 O 0.4240(3) -0.0165(5) -0.3600(6) 0.0247(10) Uani 1 d . . . O10 O 0.2581(2) 0.0885(3) 0.0322(4) 0.0094(7) Uani 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 Cd1 0.0047(2) 0.0071(2) 0.0066(2) 0.000 -0.00018(18) 0.000 Cd2 0.00553(19) 0.00756(18) 0.0076(2) 0.00098(10) 0.00174(14) 0.00049(10) Cd3 0.00484(19) 0.00694(18) 0.0072(2) 0.00118(10) 0.00081(14) 0.00027(10) As1 0.0048(2) 0.0066(2) 0.0049(2) 0.00039(14) 0.00004(18) -0.00038(14) As2 0.0037(2) 0.0054(2) 0.0049(2) -0.00005(14) 0.00026(18) -0.00007(14) O1 0.0097(17) 0.0140(16) 0.0099(15) 0.0035(13) 0.0034(14) 0.0048(12) O2 0.0111(18) 0.0203(18) 0.0117(16) 0.0061(15) -0.0043(14) -0.0087(14) O3 0.0118(16) 0.0093(14) 0.0083(15) -0.0040(12) -0.0020(14) 0.0035(12) O4 0.0073(16) 0.0158(16) 0.0069(16) 0.0060(12) 0.0008(13) -0.0017(12) O5 0.0070(15) 0.0083(15) 0.0052(14) -0.0015(11) 0.0017(12) 0.0015(11) O6 0.0024(15) 0.0126(15) 0.0079(15) 0.0004(12) 0.0015(13) -0.0004(11) O7 0.0071(15) 0.0072(14) 0.0117(16) -0.0040(12) 0.0023(14) -0.0038(11) O8 0.0067(15) 0.0112(15) 0.0118(16) 0.0044(13) 0.0022(14) 0.0017(12) O9 0.019(2) 0.021(2) 0.036(3) 0.0043(18) 0.009(2) 0.0019(16) O10 0.0091(16) 0.0113(15) 0.0078(16) -0.0005(12) 0.0011(14) -0.0008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O3 2.253(4) 2_554 ? Cd1 O3 2.253(4) . ? Cd1 O4 2.293(3) 5_554 ? Cd1 O4 2.293(3) 6_556 ? Cd1 O6 2.328(4) . ? Cd1 O6 2.328(4) 2_554 ? Cd2 O8 2.219(4) . ? Cd2 O9 2.222(5) . ? Cd2 O5 2.299(3) 7_554 ? Cd2 O1 2.305(3) 4_554 ? Cd2 O7 2.325(4) 4_544 ? Cd2 O10 2.487(3) 6 ? Cd3 O5 2.219(3) 6_556 ? Cd3 O8 2.265(4) . ? Cd3 O3 2.277(3) . ? Cd3 O4 2.301(4) 6_556 ? Cd3 O7 2.340(4) 4_544 ? Cd3 O10 2.384(3) . ? As1 O3 1.658(4) . ? As1 O4 1.669(4) . ? As1 O1 1.682(4) . ? As1 O2 1.720(4) . ? As2 O7 1.679(3) . ? As2 O8 1.686(3) . ? As2 O6 1.691(4) . ? As2 O5 1.692(3) . ? O1 Cd2 2.305(4) 4_544 ? O4 Cd1 2.293(3) 5_554 ? O4 Cd3 2.301(4) 6 ? O5 Cd3 2.219(3) 6 ? O5 Cd2 2.299(3) 7_554 ? O7 Cd2 2.325(4) 4_554 ? O7 Cd3 2.340(4) 4_554 ? O10 Cd2 2.487(3) 6_556 ? 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 O3 Cd1 O3 86.6(2) 2_554 . ? O3 Cd1 O4 75.00(12) 2_554 5_554 ? O3 Cd1 O4 104.21(13) . 5_554 ? O3 Cd1 O4 104.21(13) 2_554 6_556 ? O3 Cd1 O4 75.00(12) . 6_556 ? O4 Cd1 O4 178.96(18) 5_554 6_556 ? O3 Cd1 O6 165.11(12) 2_554 . ? O3 Cd1 O6 90.08(13) . . ? O4 Cd1 O6 91.79(12) 5_554 . ? O4 Cd1 O6 88.90(13) 6_556 . ? O3 Cd1 O6 90.08(13) 2_554 2_554 ? O3 Cd1 O6 165.11(12) . 2_554 ? O4 Cd1 O6 88.90(13) 5_554 2_554 ? O4 Cd1 O6 91.79(12) 6_556 2_554 ? O6 Cd1 O6 96.61(17) . 2_554 ? O8 Cd2 O9 163.16(16) . . ? O8 Cd2 O5 95.15(13) . 7_554 ? O9 Cd2 O5 93.64(16) . 7_554 ? O8 Cd2 O1 82.45(14) . 4_554 ? O9 Cd2 O1 111.56(17) . 4_554 ? O5 Cd2 O1 92.15(12) 7_554 4_554 ? O8 Cd2 O7 79.41(12) . 4_544 ? O9 Cd2 O7 91.57(15) . 4_544 ? O5 Cd2 O7 174.56(12) 7_554 4_544 ? O1 Cd2 O7 87.39(13) 4_554 4_544 ? O8 Cd2 O10 78.81(13) . 6 ? O9 Cd2 O10 85.34(15) . 6 ? O5 Cd2 O10 101.92(11) 7_554 6 ? O1 Cd2 O10 157.42(13) 4_554 6 ? O7 Cd2 O10 76.92(12) 4_544 6 ? O5 Cd3 O8 157.95(13) 6_556 . ? O5 Cd3 O3 91.87(13) 6_556 . ? O8 Cd3 O3 82.16(13) . . ? O5 Cd3 O4 104.88(14) 6_556 6_556 ? O8 Cd3 O4 93.98(13) . 6_556 ? O3 Cd3 O4 74.40(13) . 6_556 ? O5 Cd3 O7 87.71(13) 6_556 4_544 ? O8 Cd3 O7 78.18(12) . 4_544 ? O3 Cd3 O7 123.42(13) . 4_544 ? O4 Cd3 O7 158.45(12) 6_556 4_544 ? O5 Cd3 O10 102.84(12) 6_556 . ? O8 Cd3 O10 89.26(13) . . ? O3 Cd3 O10 158.79(12) . . ? O4 Cd3 O10 86.97(12) 6_556 . ? O7 Cd3 O10 73.02(13) 4_544 . ? O3 As1 O4 112.94(18) . . ? O3 As1 O1 107.98(17) . . ? O4 As1 O1 111.49(19) . . ? O3 As1 O2 110.8(2) . . ? O4 As1 O2 107.28(17) . . ? O1 As1 O2 106.12(19) . . ? O7 As2 O8 109.74(17) . . ? O7 As2 O6 110.71(17) . . ? O8 As2 O6 110.76(17) . . ? O7 As2 O5 108.22(18) . . ? O8 As2 O5 109.00(17) . . ? O6 As2 O5 108.34(17) . . ? As1 O1 Cd2 125.2(2) . 4_544 ? As1 O3 Cd1 134.15(18) . . ? As1 O3 Cd3 120.27(19) . . ? Cd1 O3 Cd3 104.48(14) . . ? As1 O4 Cd1 130.7(2) . 5_554 ? As1 O4 Cd3 126.85(19) . 6 ? Cd1 O4 Cd3 102.47(14) 5_554 6 ? As2 O5 Cd3 123.59(18) . 6 ? As2 O5 Cd2 121.54(17) . 7_554 ? Cd3 O5 Cd2 114.17(15) 6 7_554 ? As2 O6 Cd1 131.14(18) . . ? As2 O7 Cd2 133.7(2) . 4_554 ? As2 O7 Cd3 126.62(19) . 4_554 ? Cd2 O7 Cd3 98.29(12) 4_554 4_554 ? As2 O8 Cd2 119.77(19) . . ? As2 O8 Cd3 136.4(2) . . ? Cd2 O8 Cd3 103.80(13) . . ? Cd3 O10 Cd2 108.67(13) . 6_556 ? _diffrn_measured_fraction_theta_max 0.402 _diffrn_reflns_theta_full 29.44 _diffrn_measured_fraction_theta_full 0.402 _refine_diff_density_max 3.302 _refine_diff_density_min -1.899 _refine_diff_density_rms 0.664