data_grandaite _publ_contact_author_name 'Fernando Camara' _publ_contact_author_address 'Dip. di Scienze della Terra, University of Turin' _publ_contact_author_email fernando.camaraartigas@unito.it _publ_contact_author_phone +390116705132 _publ_contact_author_fax +390116705128 loop_ _publ_author_name _publ_author_address 'Fernando Camara' 'Dip. di Scienze della Terra, University of Turin' _chemical_name_mineral 'grandaite' _chemical_compound_source 'La Valletta mine, Maira Valley, Italy' _chemical_formula_analytical 'Al1.26 As3.84 Ba0.08 Ca1.24 Fe0.28 H2.00 O18.00 Pb0.04 Sr2.80 V0.04' _chemical_formula_sum 'Al1.62 As3.54 Ba0.16 Ca0.90 Fe0.36 H2.00 O18.00 Sr2.94 V0.46' _chemical_formula_weight 958.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Al' 'Al' 0.0645 0.0514 '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' 'Ba' 'Ba' -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Sr' 'Sr' -1.5307 3.2498 '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' 'V' 'V' 0.3005 0.5294 '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' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 21/m' _space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.5764(5) _cell_length_b 5.9507(4) _cell_length_c 8.8050(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.551(2) _cell_angle_gamma 90.00 _cell_volume 366.62(4) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2404 _cell_measurement_theta_min 2.505 _cell_measurement_theta_max 36.160 _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour pink-salmon _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 4.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442.8 _exptl_absorpt_coefficient_mu 20.150 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.1778 _exptl_absorpt_correction_T_max 0.2935 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS SMART-APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 6095 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 34.96 _reflns_number_total 1734 _reflns_number_gt 1442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT V6.45A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 1734 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group T1A As 0.43733(5) 0.2500 0.17111(4) 0.01236(11) Uani 0.886(9) 2 d SP . . T1B V 0.43733(5) 0.2500 0.17111(4) 0.01236(11) Uani 0.114(9) 2 d SP . . T2A As 0.03113(4) 0.2500 0.33393(4) 0.01032(11) Uani 0.884(9) 2 d SP . . T2B V 0.03113(4) 0.2500 0.33393(4) 0.01032(11) Uani 0.116(9) 2 d SP . . MA Al 0.0000 0.0000 0.0000 0.0106(2) Uani 0.815(5) 2 d SP . . MB Fe 0.0000 0.0000 0.0000 0.0106(2) Uani 0.185(5) 2 d SP . . A1A Sr 0.25931(6) 0.2500 0.73723(6) 0.01875(14) Uani 0.548(5) 2 d SP . . A1B Ca 0.25931(6) 0.2500 0.73723(6) 0.01875(14) Uani 0.452(5) 2 d SP . . A2A Sr 0.67546(4) 0.2500 0.58860(4) 0.01325(10) Uani 0.921(7) 2 d SP . . A2B Ba 0.67546(4) 0.2500 0.58860(4) 0.01325(10) Uani 0.079(7) 2 d SP . . O1 O 0.0231(3) 0.5144(3) 0.7853(2) 0.0203(4) Uani 1 1 d . . . O2 O 0.2635(4) 0.2500 0.4501(3) 0.0265(6) Uani 1 2 d S . . O3 O 0.9109(4) 0.2500 0.4550(4) 0.0320(7) Uani 1 2 d S . . O4 O 0.5055(2) 0.0223(3) 0.2905(2) 0.0197(4) Uani 1 1 d . . . O5 O 0.5209(5) 0.2500 0.0207(4) 0.0391(8) Uani 1 2 d S . . O6 O 0.1923(3) 0.2500 0.0638(3) 0.0210(5) Uani 1 2 d S . . O7 O 0.8303(3) 0.2500 0.9207(3) 0.0137(5) Uani 1 2 d S . . H7 H 0.7043 0.2500 0.9230 0.020 Uiso 1 2 d S . . 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 T1A 0.01242(17) 0.01138(16) 0.01137(17) 0.000 0.00242(12) 0.000 T1B 0.01242(17) 0.01138(16) 0.01137(17) 0.000 0.00242(12) 0.000 T2A 0.01242(18) 0.01054(17) 0.00925(17) 0.000 0.00556(12) 0.000 T2B 0.01242(18) 0.01054(17) 0.00925(17) 0.000 0.00556(12) 0.000 MA 0.0139(4) 0.0087(4) 0.0090(4) 0.0000(2) 0.0039(3) -0.0004(2) MB 0.0139(4) 0.0087(4) 0.0090(4) 0.0000(2) 0.0039(3) -0.0004(2) A1A 0.0179(2) 0.0206(2) 0.0226(2) 0.000 0.01310(18) 0.000 A1B 0.0179(2) 0.0206(2) 0.0226(2) 0.000 0.01310(18) 0.000 A2A 0.01466(15) 0.01477(14) 0.01246(15) 0.000 0.00758(10) 0.000 A2B 0.01466(15) 0.01477(14) 0.01246(15) 0.000 0.00758(10) 0.000 O1 0.0330(10) 0.0132(7) 0.0156(8) 0.0020(6) 0.0105(7) 0.0025(6) O2 0.0152(12) 0.0399(16) 0.0217(13) 0.000 0.0041(10) 0.000 O3 0.0334(15) 0.0410(16) 0.0345(17) 0.000 0.0273(14) 0.000 O4 0.0226(8) 0.0153(8) 0.0177(8) 0.0026(6) 0.0039(7) 0.0017(6) O5 0.0413(18) 0.059(2) 0.0276(16) 0.000 0.0249(14) 0.000 O6 0.0149(11) 0.0216(12) 0.0207(12) 0.000 0.0005(9) 0.000 O7 0.0121(10) 0.0150(11) 0.0124(10) 0.000 0.0029(8) 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 T1A O4 1.6708(17) 4_565 ? T1A O4 1.6708(17) . ? T1A O5 1.673(3) . ? T1A O6 1.730(2) . ? T1A A2A 3.4178(5) . ? T1A A1A 3.5301(6) 1_554 ? T1A A1B 3.5301(6) 1_554 ? T1A A1B 3.6556(4) 3_666 ? T1A A1A 3.6556(4) 3_666 ? T1A A1A 3.6556(4) 3_656 ? T1A A1B 3.6556(4) 3_656 ? T2A O3 1.647(3) 1_455 ? T2A O2 1.663(3) . ? T2A O1 1.7042(17) 2_546 ? T2A O1 1.7042(17) 3_566 ? T2A A1A 3.3000(6) . ? T2A A1B 3.6097(3) 3_556 ? T2A A1A 3.6097(3) 3_556 ? T2A A1A 3.6097(3) 3_566 ? T2A A1B 3.6097(3) 3_566 ? T2A A2A 3.6189(3) 3_666 ? T2A A2B 3.6189(3) 3_666 ? MA O7 1.9143(14) 3_656 ? MA O7 1.9143(14) 1_454 ? MA O1 1.9664(17) 4_564 ? MA O1 1.9664(17) 2_546 ? MA O6 2.0061(16) 3 ? MA O6 2.0061(16) . ? MA MA 2.9754(2) 2_545 ? MA MB 2.9754(2) 2 ? MA MA 2.9754(2) 2 ? MA MB 2.9754(2) 2_545 ? MA A2A 3.8143(3) 1_454 ? MA A2B 3.8143(3) 3_656 ? A1A O4 2.4888(17) 2_656 ? A1A O4 2.4888(17) 3_656 ? A1A O5 2.523(3) 1_556 ? A1A O1 2.5374(17) . ? A1A O1 2.5374(18) 4_565 ? A1A O2 2.541(3) . ? A1A O3 2.848(3) 1_455 ? A1A O6 3.105(3) 1_556 ? A1A T1B 3.5301(6) 1_556 ? A1A T1A 3.5301(6) 1_556 ? A2A O3 2.485(3) . ? A2A O4 2.5995(18) 3_656 ? A2A O4 2.5995(17) 2_656 ? A2A O7 2.701(3) . ? A2A O4 2.7911(18) . ? A2A O4 2.7911(18) 4_565 ? A2A O2 2.883(3) . ? A2A O1 2.9856(18) 1_655 ? A2A O1 2.9856(18) 4_665 ? A2A O2 3.0502(6) 3_666 ? A2A O2 3.0502(6) 3_656 ? A2A H7 2.8677(3) . ? O1 T2B 1.7042(17) 3_566 ? O1 T2A 1.7042(17) 3_566 ? O1 MB 1.9664(17) 2_556 ? O1 MA 1.9664(17) 2_556 ? O1 A2B 2.9856(18) 1_455 ? O1 A2A 2.9856(18) 1_455 ? O2 A2B 3.0502(6) 3_666 ? O2 A2A 3.0502(6) 3_666 ? O2 A2A 3.0502(6) 3_656 ? O2 A2B 3.0502(6) 3_656 ? O3 T2B 1.647(3) 1_655 ? O3 T2A 1.647(3) 1_655 ? O3 A1B 2.848(3) 1_655 ? O3 A1A 2.848(3) 1_655 ? O4 A1B 2.4888(17) 3_656 ? O4 A1A 2.4888(17) 3_656 ? O4 A2B 2.5995(17) 3_656 ? O4 A2A 2.5995(17) 3_656 ? O5 A1B 2.523(3) 1_554 ? O5 A1A 2.523(3) 1_554 ? O6 MB 2.0061(16) 2 ? O6 MA 2.0061(16) 2 ? O6 A1B 3.105(3) 1_554 ? O6 A1A 3.105(3) 1_554 ? O7 MB 1.9143(14) 2_656 ? O7 MA 1.9143(14) 2_656 ? O7 MB 1.9143(14) 1_656 ? O7 MA 1.9143(14) 1_656 ? O7 H7 0.963(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 O4 T1A O4 108.38(12) 4_565 . ? O4 T1A O5 112.25(9) 4_565 . ? O4 T1A O5 112.25(9) . . ? O4 T1A O6 110.59(8) 4_565 . ? O4 T1A O6 110.59(8) . . ? O5 T1A O6 102.72(15) . . ? O4 T1A A2A 54.19(6) 4_565 . ? O4 T1A A2A 54.19(6) . . ? O5 T1A A2A 130.35(11) . . ? O6 T1A A2A 126.92(9) . . ? O4 T1A A1A 125.35(6) 4_565 1_554 ? O4 T1A A1A 125.35(6) . 1_554 ? O5 T1A A1A 41.13(11) . 1_554 ? O6 T1A A1A 61.59(9) . 1_554 ? A2A T1A A1A 171.486(15) . 1_554 ? O4 T1A A1B 125.35(6) 4_565 1_554 ? O4 T1A A1B 125.35(6) . 1_554 ? O5 T1A A1B 41.13(11) . 1_554 ? O6 T1A A1B 61.59(9) . 1_554 ? A2A T1A A1B 171.486(15) . 1_554 ? A1A T1A A1B 0.000(6) 1_554 1_554 ? O4 T1A A1B 35.37(6) 4_565 3_666 ? O4 T1A A1B 120.31(6) . 3_666 ? O5 T1A A1B 77.17(6) . 3_666 ? O6 T1A A1B 124.932(13) . 3_666 ? A2A T1A A1B 74.614(9) . 3_666 ? A1A T1A A1B 100.712(10) 1_554 3_666 ? A1B T1A A1B 100.712(10) 1_554 3_666 ? O4 T1A A1A 35.37(6) 4_565 3_666 ? O4 T1A A1A 120.31(6) . 3_666 ? O5 T1A A1A 77.17(6) . 3_666 ? O6 T1A A1A 124.932(13) . 3_666 ? A2A T1A A1A 74.614(9) . 3_666 ? A1A T1A A1A 100.712(10) 1_554 3_666 ? A1B T1A A1A 100.712(10) 1_554 3_666 ? A1B T1A A1A 0.00(2) 3_666 3_666 ? O4 T1A A1A 120.31(6) 4_565 3_656 ? O4 T1A A1A 35.37(6) . 3_656 ? O5 T1A A1A 77.17(6) . 3_656 ? O6 T1A A1A 124.932(13) . 3_656 ? A2A T1A A1A 74.614(9) . 3_656 ? A1A T1A A1A 100.712(11) 1_554 3_656 ? A1B T1A A1A 100.712(11) 1_554 3_656 ? A1B T1A A1A 108.958(14) 3_666 3_656 ? A1A T1A A1A 108.958(14) 3_666 3_656 ? O4 T1A A1B 120.31(6) 4_565 3_656 ? O4 T1A A1B 35.37(6) . 3_656 ? O5 T1A A1B 77.17(6) . 3_656 ? O6 T1A A1B 124.932(13) . 3_656 ? A2A T1A A1B 74.614(9) . 3_656 ? A1A T1A A1B 100.712(11) 1_554 3_656 ? A1B T1A A1B 100.712(11) 1_554 3_656 ? A1B T1A A1B 108.958(14) 3_666 3_656 ? A1A T1A A1B 108.958(14) 3_666 3_656 ? A1A T1A A1B 0.000(15) 3_656 3_656 ? O3 T2A O2 108.64(15) 1_455 . ? O3 T2A O1 109.65(8) 1_455 2_546 ? O2 T2A O1 109.10(8) . 2_546 ? O3 T2A O1 109.65(8) 1_455 3_566 ? O2 T2A O1 109.10(8) . 3_566 ? O1 T2A O1 110.67(12) 2_546 3_566 ? O3 T2A A1A 59.65(11) 1_455 . ? O2 T2A A1A 49.00(10) . . ? O1 T2A A1A 124.45(6) 2_546 . ? O1 T2A A1A 124.45(6) 3_566 . ? O3 T2A A1B 70.17(6) 1_455 3_556 ? O2 T2A A1B 122.54(2) . 3_556 ? O1 T2A A1B 39.48(6) 2_546 3_556 ? O1 T2A A1B 125.74(6) 3_566 3_556 ? A1A T2A A1B 102.690(10) . 3_556 ? O3 T2A A1A 70.17(6) 1_455 3_556 ? O2 T2A A1A 122.54(2) . 3_556 ? O1 T2A A1A 39.48(6) 2_546 3_556 ? O1 T2A A1A 125.74(6) 3_566 3_556 ? A1A T2A A1A 102.690(10) . 3_556 ? A1B T2A A1A 0.00(2) 3_556 3_556 ? O3 T2A A1A 70.17(6) 1_455 3_566 ? O2 T2A A1A 122.54(2) . 3_566 ? O1 T2A A1A 125.74(6) 2_546 3_566 ? O1 T2A A1A 39.48(6) 3_566 3_566 ? A1A T2A A1A 102.690(10) . 3_566 ? A1B T2A A1A 111.028(14) 3_556 3_566 ? A1A T2A A1A 111.028(14) 3_556 3_566 ? O3 T2A A1B 70.17(6) 1_455 3_566 ? O2 T2A A1B 122.54(2) . 3_566 ? O1 T2A A1B 125.74(6) 2_546 3_566 ? O1 T2A A1B 39.48(6) 3_566 3_566 ? A1A T2A A1B 102.690(10) . 3_566 ? A1B T2A A1B 111.028(14) 3_556 3_566 ? A1A T2A A1B 111.028(14) 3_556 3_566 ? A1A T2A A1B 0.00(2) 3_566 3_566 ? O3 T2A A2A 109.28(6) 1_455 3_666 ? O2 T2A A2A 56.98(2) . 3_666 ? O1 T2A A2A 141.07(6) 2_546 3_666 ? O1 T2A A2A 54.93(6) 3_566 3_666 ? A1A T2A A2A 76.511(8) . 3_666 ? A1B T2A A2A 179.198(13) 3_556 3_666 ? A1A T2A A2A 179.198(13) 3_556 3_666 ? A1A T2A A2A 69.178(8) 3_566 3_666 ? A1B T2A A2A 69.178(8) 3_566 3_666 ? O3 T2A A2B 109.28(6) 1_455 3_666 ? O2 T2A A2B 56.98(2) . 3_666 ? O1 T2A A2B 141.07(6) 2_546 3_666 ? O1 T2A A2B 54.93(6) 3_566 3_666 ? A1A T2A A2B 76.511(8) . 3_666 ? A1B T2A A2B 179.198(13) 3_556 3_666 ? A1A T2A A2B 179.198(13) 3_556 3_666 ? A1A T2A A2B 69.178(8) 3_566 3_666 ? A1B T2A A2B 69.178(8) 3_566 3_666 ? A2A T2A A2B 0.000(16) 3_666 3_666 ? O7 MA O7 180.00(12) 3_656 1_454 ? O7 MA O1 91.25(9) 3_656 4_564 ? O7 MA O1 88.75(9) 1_454 4_564 ? O7 MA O1 88.75(9) 3_656 2_546 ? O7 MA O1 91.25(9) 1_454 2_546 ? O1 MA O1 180.00(14) 4_564 2_546 ? O7 MA O6 80.78(7) 3_656 3 ? O7 MA O6 99.22(7) 1_454 3 ? O1 MA O6 91.22(9) 4_564 3 ? O1 MA O6 88.78(9) 2_546 3 ? O7 MA O6 99.22(7) 3_656 . ? O7 MA O6 80.78(7) 1_454 . ? O1 MA O6 88.78(9) 4_564 . ? O1 MA O6 91.22(9) 2_546 . ? O6 MA O6 180.0 3 . ? O7 MA MA 39.00(5) 3_656 2_545 ? O7 MA MA 141.00(5) 1_454 2_545 ? O1 MA MA 87.49(5) 4_564 2_545 ? O1 MA MA 92.51(5) 2_546 2_545 ? O6 MA MA 42.13(5) 3 2_545 ? O6 MA MA 137.87(5) . 2_545 ? O7 MA MB 141.00(5) 3_656 2 ? O7 MA MB 39.00(5) 1_454 2 ? O1 MA MB 92.51(5) 4_564 2 ? O1 MA MB 87.49(5) 2_546 2 ? O6 MA MB 137.87(5) 3 2 ? O6 MA MB 42.13(5) . 2 ? MA MA MB 180.0 2_545 2 ? O7 MA MA 141.00(5) 3_656 2 ? O7 MA MA 39.00(5) 1_454 2 ? O1 MA MA 92.51(5) 4_564 2 ? O1 MA MA 87.49(5) 2_546 2 ? O6 MA MA 137.87(5) 3 2 ? O6 MA MA 42.13(5) . 2 ? MA MA MA 180.0 2_545 2 ? MB MA MA 0.0 2 2 ? O7 MA MB 39.00(5) 3_656 2_545 ? O7 MA MB 141.00(5) 1_454 2_545 ? O1 MA MB 87.49(5) 4_564 2_545 ? O1 MA MB 92.51(5) 2_546 2_545 ? O6 MA MB 42.13(5) 3 2_545 ? O6 MA MB 137.87(5) . 2_545 ? MA MA MB 0.0 2_545 2_545 ? MB MA MB 180.0 2 2_545 ? MA MA MB 180.0 2 2_545 ? O7 MA A2A 138.38(7) 3_656 1_454 ? O7 MA A2A 41.62(7) 1_454 1_454 ? O1 MA A2A 50.70(5) 4_564 1_454 ? O1 MA A2A 129.30(5) 2_546 1_454 ? O6 MA A2A 83.62(6) 3 1_454 ? O6 MA A2A 96.38(6) . 1_454 ? MA MA A2A 112.956(3) 2_545 1_454 ? MB MA A2A 67.044(3) 2 1_454 ? MA MA A2A 67.044(3) 2 1_454 ? MB MA A2A 112.956(3) 2_545 1_454 ? O7 MA A2B 41.62(7) 3_656 3_656 ? O7 MA A2B 138.38(7) 1_454 3_656 ? O1 MA A2B 129.30(5) 4_564 3_656 ? O1 MA A2B 50.70(5) 2_546 3_656 ? O6 MA A2B 96.38(6) 3 3_656 ? O6 MA A2B 83.62(6) . 3_656 ? MA MA A2B 67.044(3) 2_545 3_656 ? MB MA A2B 112.956(3) 2 3_656 ? MA MA A2B 112.956(3) 2 3_656 ? MB MA A2B 67.044(3) 2_545 3_656 ? A2A MA A2B 180.000(8) 1_454 3_656 ? O4 A1A O4 81.24(8) 2_656 3_656 ? O4 A1A O5 77.09(6) 2_656 1_556 ? O4 A1A O5 77.09(6) 3_656 1_556 ? O4 A1A O1 100.94(6) 2_656 . ? O4 A1A O1 175.87(6) 3_656 . ? O5 A1A O1 99.90(7) 1_556 . ? O4 A1A O1 175.87(6) 2_656 4_565 ? O4 A1A O1 100.94(6) 3_656 4_565 ? O5 A1A O1 99.90(7) 1_556 4_565 ? O1 A1A O1 76.66(8) . 4_565 ? O4 A1A O2 67.64(6) 2_656 . ? O4 A1A O2 67.64(6) 3_656 . ? O5 A1A O2 132.81(9) 1_556 . ? O1 A1A O2 116.40(6) . . ? O1 A1A O2 116.40(6) 4_565 . ? O4 A1A O3 111.91(6) 2_656 1_455 ? O4 A1A O3 111.91(6) 3_656 1_455 ? O5 A1A O3 167.66(8) 1_556 1_455 ? O1 A1A O3 70.64(6) . 1_455 ? O1 A1A O3 70.64(6) 4_565 1_455 ? O2 A1A O3 59.53(8) . 1_455 ? O4 A1A O6 117.92(5) 2_656 1_556 ? O4 A1A O6 117.92(5) 3_656 1_556 ? O5 A1A O6 55.20(8) 1_556 1_556 ? O1 A1A O6 57.96(5) . 1_556 ? O1 A1A O6 57.96(5) 4_565 1_556 ? O2 A1A O6 171.98(7) . 1_556 ? O3 A1A O6 112.46(7) 1_455 1_556 ? O4 A1A T2A 89.64(4) 2_656 . ? O4 A1A T2A 89.64(4) 3_656 . ? O5 A1A T2A 162.41(7) 1_556 . ? O1 A1A T2A 93.87(4) . . ? O1 A1A T2A 93.87(4) 4_565 . ? O2 A1A T2A 29.60(6) . . ? O3 A1A T2A 29.93(6) 1_455 . ? O6 A1A T2A 142.39(5) 1_556 . ? O4 A1A T1B 96.63(4) 2_656 1_556 ? O4 A1A T1B 96.63(4) 3_656 1_556 ? O5 A1A T1B 25.86(7) 1_556 1_556 ? O1 A1A T1B 79.68(4) . 1_556 ? O1 A1A T1B 79.68(4) 4_565 1_556 ? O2 A1A T1B 158.68(6) . 1_556 ? O3 A1A T1B 141.80(6) 1_455 1_556 ? O6 A1A T1B 29.34(4) 1_556 1_556 ? T2A A1A T1B 171.729(17) . 1_556 ? O4 A1A T1A 96.63(4) 2_656 1_556 ? O4 A1A T1A 96.63(4) 3_656 1_556 ? O5 A1A T1A 25.86(7) 1_556 1_556 ? O1 A1A T1A 79.68(4) . 1_556 ? O1 A1A T1A 79.68(4) 4_565 1_556 ? O2 A1A T1A 158.68(6) . 1_556 ? O3 A1A T1A 141.80(6) 1_455 1_556 ? O6 A1A T1A 29.34(4) 1_556 1_556 ? T2A A1A T1A 171.729(17) . 1_556 ? T1B A1A T1A 0.000(12) 1_556 1_556 ? O3 A2A O4 141.34(4) . 3_656 ? O3 A2A O4 141.34(4) . 2_656 ? O4 A2A O4 77.12(8) 3_656 2_656 ? O3 A2A O7 114.81(9) . . ? O4 A2A O7 68.60(5) 3_656 . ? O4 A2A O7 68.60(5) 2_656 . ? O3 A2A O4 73.20(7) . . ? O4 A2A O4 87.53(6) 3_656 . ? O4 A2A O4 124.20(3) 2_656 . ? O7 A2A O4 150.48(4) . . ? O3 A2A O4 73.20(7) . 4_565 ? O4 A2A O4 124.20(3) 3_656 4_565 ? O4 A2A O4 87.53(6) 2_656 4_565 ? O7 A2A O4 150.48(4) . 4_565 ? O4 A2A O4 58.08(7) . 4_565 ? O3 A2A O2 131.08(9) . . ? O4 A2A O2 61.16(5) 3_656 . ? O4 A2A O2 61.16(5) 2_656 . ? O7 A2A O2 114.11(7) . . ? O4 A2A O2 64.40(6) . . ? O4 A2A O2 64.40(6) 4_565 . ? O3 A2A O1 68.94(7) . 1_655 ? O4 A2A O1 125.28(5) 3_656 1_655 ? O4 A2A O1 85.44(5) 2_656 1_655 ? O7 A2A O1 56.75(5) . 1_655 ? O4 A2A O1 141.95(5) . 1_655 ? O4 A2A O1 106.01(5) 4_565 1_655 ? O2 A2A O1 144.75(4) . 1_655 ? O3 A2A O1 68.94(7) . 4_665 ? O4 A2A O1 85.44(5) 3_656 4_665 ? O4 A2A O1 125.28(5) 2_656 4_665 ? O7 A2A O1 56.75(5) . 4_665 ? O4 A2A O1 106.01(5) . 4_665 ? O4 A2A O1 141.95(5) 4_565 4_665 ? O2 A2A O1 144.75(4) . 4_665 ? O1 A2A O1 63.62(6) 1_655 4_665 ? O3 A2A O2 77.29(5) . 3_666 ? O4 A2A O2 141.27(6) 3_656 3_666 ? O4 A2A O2 64.15(6) 2_656 3_666 ? O7 A2A O2 95.70(5) . 3_666 ? O4 A2A O2 113.80(6) . 3_666 ? O4 A2A O2 57.07(6) 4_565 3_666 ? O2 A2A O2 97.97(5) . 3_666 ? O1 A2A O2 54.04(6) 1_655 3_666 ? O1 A2A O2 116.18(6) 4_665 3_666 ? O3 A2A O2 77.29(5) . 3_656 ? O4 A2A O2 64.15(6) 3_656 3_656 ? O4 A2A O2 141.27(6) 2_656 3_656 ? O7 A2A O2 95.70(5) . 3_656 ? O4 A2A O2 57.07(6) . 3_656 ? O4 A2A O2 113.80(6) 4_565 3_656 ? O2 A2A O2 97.97(5) . 3_656 ? O1 A2A O2 116.18(6) 1_655 3_656 ? O1 A2A O2 54.04(6) 4_665 3_656 ? O2 A2A O2 154.57(10) 3_666 3_656 ? O3 A2A T1A 70.71(8) . . ? O4 A2A T1A 107.25(4) 3_656 . ? O4 A2A T1A 107.25(4) 2_656 . ? O7 A2A T1A 174.48(5) . . ? O4 A2A T1A 29.04(3) . . ? O4 A2A T1A 29.04(3) 4_565 . ? O2 A2A T1A 60.37(6) . . ? O1 A2A T1A 127.46(3) 1_655 . ? O1 A2A T1A 127.46(3) 4_665 . ? O2 A2A T1A 85.41(5) 3_666 . ? O2 A2A T1A 85.41(5) 3_656 . ? O3 A2A H7 134.43(8) . . ? O4 A2A H7 54.84(4) 3_656 . ? O4 A2A H7 54.84(4) 2_656 . ? O7 A2A H7 19.62(4) . . ? O4 A2A H7 142.33(4) . . ? O4 A2A H7 142.33(4) 4_565 . ? O2 A2A H7 94.48(6) . . ? O1 A2A H7 72.64(3) 1_655 . ? O1 A2A H7 72.64(3) 4_665 . ? O2 A2A H7 99.18(5) 3_666 . ? O2 A2A H7 99.18(5) 3_656 . ? T1A A2A H7 154.858(12) . . ? T2B O1 T2A 0.00(4) 3_566 3_566 ? T2B O1 MB 122.60(9) 3_566 2_556 ? T2A O1 MB 122.60(9) 3_566 2_556 ? T2B O1 MA 122.60(9) 3_566 2_556 ? T2A O1 MA 122.60(9) 3_566 2_556 ? MB O1 MA 0.0 2_556 2_556 ? T2B O1 A1A 115.24(8) 3_566 . ? T2A O1 A1A 115.24(8) 3_566 . ? MB O1 A1A 117.50(8) 2_556 . ? MA O1 A1A 117.50(8) 2_556 . ? T2B O1 A2B 97.22(7) 3_566 1_455 ? T2A O1 A2B 97.22(7) 3_566 1_455 ? MB O1 A2B 98.66(7) 2_556 1_455 ? MA O1 A2B 98.66(7) 2_556 1_455 ? A1A O1 A2B 95.63(5) . 1_455 ? T2B O1 A2A 97.22(7) 3_566 1_455 ? T2A O1 A2A 97.22(7) 3_566 1_455 ? MB O1 A2A 98.66(7) 2_556 1_455 ? MA O1 A2A 98.66(7) 2_556 1_455 ? A1A O1 A2A 95.63(5) . 1_455 ? A2B O1 A2A 0.000(9) 1_455 1_455 ? T2A O2 A1A 101.41(12) . . ? T2A O2 A2A 168.38(15) . . ? A1A O2 A2A 90.21(8) . . ? T2A O2 A2B 95.82(5) . 3_666 ? A1A O2 A2B 99.87(5) . 3_666 ? A2A O2 A2B 82.03(5) . 3_666 ? T2A O2 A2A 95.82(5) . 3_666 ? A1A O2 A2A 99.87(5) . 3_666 ? A2A O2 A2A 82.03(5) . 3_666 ? A2B O2 A2A 0.00(2) 3_666 3_666 ? T2A O2 A2A 95.82(5) . 3_656 ? A1A O2 A2A 99.87(5) . 3_656 ? A2A O2 A2A 82.03(5) . 3_656 ? A2B O2 A2A 154.57(10) 3_666 3_656 ? A2A O2 A2A 154.57(10) 3_666 3_656 ? T2A O2 A2B 95.82(5) . 3_656 ? A1A O2 A2B 99.87(5) . 3_656 ? A2A O2 A2B 82.03(5) . 3_656 ? A2B O2 A2B 154.57(10) 3_666 3_656 ? A2A O2 A2B 154.57(10) 3_666 3_656 ? A2A O2 A2B 0.00(2) 3_656 3_656 ? T2B O3 T2A 0.000(12) 1_655 1_655 ? T2B O3 A2A 169.18(19) 1_655 . ? T2A O3 A2A 169.18(19) 1_655 . ? T2B O3 A1B 90.42(12) 1_655 1_655 ? T2A O3 A1B 90.42(12) 1_655 1_655 ? A2A O3 A1B 100.40(10) . 1_655 ? T2B O3 A1A 90.42(12) 1_655 1_655 ? T2A O3 A1A 90.42(12) 1_655 1_655 ? A2A O3 A1A 100.40(10) . 1_655 ? A1B O3 A1A 0.000(17) 1_655 1_655 ? T1A O4 A1B 121.76(9) . 3_656 ? T1A O4 A1A 121.76(9) . 3_656 ? A1B O4 A1A 0.00(2) 3_656 3_656 ? T1A O4 A2B 132.75(9) . 3_656 ? A1B O4 A2B 98.29(6) 3_656 3_656 ? A1A O4 A2B 98.29(6) 3_656 3_656 ? T1A O4 A2A 132.75(9) . 3_656 ? A1B O4 A2A 98.29(6) 3_656 3_656 ? A1A O4 A2A 98.29(6) 3_656 3_656 ? A2B O4 A2A 0.000(18) 3_656 3_656 ? T1A O4 A2A 96.77(7) . . ? A1B O4 A2A 108.60(6) 3_656 . ? A1A O4 A2A 108.60(6) 3_656 . ? A2B O4 A2A 92.47(6) 3_656 . ? A2A O4 A2A 92.47(6) 3_656 . ? T1A O5 A1B 113.01(15) . 1_554 ? T1A O5 A1A 113.01(15) . 1_554 ? A1B O5 A1A 0.00(3) 1_554 1_554 ? T1A O6 MA 131.68(5) . . ? T1A O6 MB 131.68(5) . 2 ? MA O6 MB 95.73(10) . 2 ? T1A O6 MA 131.68(5) . 2 ? MA O6 MA 95.73(10) . 2 ? MB O6 MA 0.0 2 2 ? T1A O6 A1B 89.07(10) . 1_554 ? MA O6 A1B 95.73(8) . 1_554 ? MB O6 A1B 95.73(8) 2 1_554 ? MA O6 A1B 95.73(8) 2 1_554 ? T1A O6 A1A 89.07(10) . 1_554 ? MA O6 A1A 95.73(8) . 1_554 ? MB O6 A1A 95.73(8) 2 1_554 ? MA O6 A1A 95.73(8) 2 1_554 ? A1B O6 A1A 0.000(3) 1_554 1_554 ? MB O7 MA 0.0 2_656 2_656 ? MB O7 MB 102.00(10) 2_656 1_656 ? MA O7 MB 102.00(10) 2_656 1_656 ? MB O7 MA 102.00(10) 2_656 1_656 ? MA O7 MA 102.00(10) 2_656 1_656 ? MB O7 MA 0.0 1_656 1_656 ? MB O7 A2A 110.31(8) 2_656 . ? MA O7 A2A 110.31(8) 2_656 . ? MB O7 A2A 110.31(8) 1_656 . ? MA O7 A2A 110.31(8) 1_656 . ? MB O7 H7 121.66(9) 2_656 . ? MA O7 H7 121.66(9) 2_656 . ? MB O7 H7 121.66(9) 1_656 . ? MA O7 H7 121.66(9) 1_656 . ? A2A O7 H7 90.01(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 34.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.574 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.238