data_argandite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 As0.54 Mn7 O16 V1.46' _chemical_formula_weight 763.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.5038(2) _cell_length_b 12.2665(5) _cell_length_c 10.1055(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.559(4) _cell_angle_gamma 90.00 _cell_volume 679.04(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 725 _exptl_absorpt_coefficient_mu 8.635 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7752 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 29.14 _reflns_number_total 1661 _reflns_number_gt 1246 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1661 _refine_ls_number_parameters 133 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.003 _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 Mn1 Mn 1.0000 0.5000 0.5000 0.0105(3) Uani 0.952(4) 2 d SP . . Mn2 Mn 0.23235(11) 0.17921(5) 0.79338(7) 0.0120(2) Uani 0.957(4) 1 d P . . Mn3 Mn 0.74927(11) 0.56820(5) 0.99173(7) 0.0095(2) Uani 0.913(3) 1 d P . . Mn4 Mn 0.24910(11) 0.20769(5) 0.50088(7) 0.0103(2) Uani 0.915(4) 1 d P . . V V 0.53430(10) 0.42008(4) 0.70834(6) 0.0079(2) Uani 0.4232(16) 1 d P . . As As 0.53430(10) 0.42008(4) 0.70834(6) 0.0079(2) Uani 0.4232(16) 1 d P . . OH1 O 0.0535(5) 0.3060(2) 0.8875(3) 0.0138(7) Uani 1 1 d D . . O2 O 0.5617(4) 0.42947(19) 0.8817(3) 0.0126(7) Uani 1 1 d . . . OH3 O 0.0784(5) 0.3449(2) 0.4060(3) 0.0156(7) Uani 1 1 d D . . O4 O 0.4159(5) 0.2965(2) 0.6677(3) 0.0177(8) Uani 1 1 d . . . OH5 O 1.0749(5) 0.5612(2) 0.8870(3) 0.0152(7) Uani 1 1 d D . . OH6 O 0.5433(5) 0.6824(2) 0.8724(3) 0.0151(7) Uani 1 1 d D . . O7 O 0.3496(5) 0.5203(2) 0.6375(3) 0.0154(7) Uani 1 1 d . . . O8 O 0.8205(5) 0.4273(2) 0.6616(3) 0.0182(7) Uani 1 1 d . . . H1 H 0.013(8) 0.347(3) 0.807(3) 0.053 Uiso 1 1 d D . . H3 H 0.193(6) 0.361(4) 0.342(4) 0.053 Uiso 1 1 d D . . H5 H 1.056(8) 0.527(3) 0.801(3) 0.053 Uiso 1 1 d D . . H6 H 0.640(7) 0.746(2) 0.864(5) 0.053 Uiso 1 1 d 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 Mn1 0.0117(5) 0.0098(5) 0.0098(6) -0.0010(4) 0.0003(4) -0.0016(4) Mn2 0.0112(4) 0.0119(4) 0.0124(4) 0.0019(3) -0.0019(3) -0.0008(3) Mn3 0.0072(4) 0.0094(4) 0.0116(4) -0.0002(3) -0.0003(3) 0.0001(3) Mn4 0.0100(4) 0.0104(4) 0.0105(4) -0.0012(3) 0.0006(3) 0.0000(3) V 0.0074(3) 0.0082(3) 0.0078(4) 0.0004(3) -0.0002(2) -0.0001(2) As 0.0074(3) 0.0082(3) 0.0078(4) 0.0004(3) -0.0002(2) -0.0001(2) OH1 0.0139(15) 0.0149(16) 0.0126(17) 0.0008(13) 0.0008(13) -0.0005(12) O2 0.0104(15) 0.0143(15) 0.0126(16) 0.0004(13) -0.0014(12) -0.0002(11) OH3 0.0128(16) 0.0156(15) 0.0183(19) -0.0007(14) 0.0009(13) 0.0005(12) O4 0.0232(17) 0.0135(16) 0.0156(18) -0.0016(13) -0.0021(14) -0.0046(12) OH5 0.0123(15) 0.0138(16) 0.0192(18) -0.0011(13) 0.0008(13) 0.0004(11) OH6 0.0139(16) 0.0157(16) 0.0158(17) 0.0028(14) 0.0018(13) -0.0017(12) O7 0.0162(16) 0.0127(15) 0.0165(18) 0.0026(13) -0.0025(13) 0.0029(12) O8 0.0135(16) 0.0270(17) 0.0142(17) 0.0048(14) 0.0016(13) 0.0017(12) _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 Mn1 O8 2.180(3) . ? Mn1 O8 2.180(3) 3_766 ? Mn1 OH3 2.187(3) 1_655 ? Mn1 OH3 2.187(3) 3_666 ? Mn1 O7 2.275(2) 1_655 ? Mn1 O7 2.275(2) 3_666 ? Mn2 OH1 2.115(3) . ? Mn2 O7 2.133(3) 2_546 ? Mn2 OH3 2.143(3) 4_666 ? Mn2 OH6 2.149(3) 2_546 ? Mn2 O4 2.225(3) . ? Mn2 Mn4 2.9867(10) . ? Mn3 OH6 2.107(3) . ? Mn3 OH5 2.170(3) . ? Mn3 OH5 2.175(3) 3_767 ? Mn3 OH1 2.189(3) 3_667 ? Mn3 O2 2.231(2) . ? Mn3 O2 2.234(3) 3_667 ? Mn3 Mn3 3.2180(12) 3_767 ? Mn3 Mn3 3.2319(12) 3_667 ? Mn3 Mn4 3.2398(9) 2_556 ? Mn4 OH3 2.112(3) . ? Mn4 OH1 2.126(3) 4_665 ? Mn4 O4 2.138(3) . ? Mn4 OH6 2.173(3) 2_546 ? Mn4 O2 2.259(2) 4_565 ? Mn4 OH5 2.289(3) 2_646 ? Mn4 Mn3 3.2398(9) 2_546 ? V O4 1.685(2) . ? V O8 1.690(3) . ? V O7 1.708(2) . ? V O2 1.747(3) . ? OH1 Mn4 2.126(3) 4_566 ? OH1 Mn3 2.189(3) 3_667 ? OH1 H1 0.965(19) . ? O2 Mn3 2.234(3) 3_667 ? O2 Mn4 2.259(2) 4_666 ? OH3 Mn2 2.143(3) 4_565 ? OH3 Mn1 2.187(3) 1_455 ? OH3 H3 0.967(19) . ? OH5 Mn3 2.175(3) 3_767 ? OH5 Mn4 2.289(3) 2_656 ? OH5 H5 0.960(19) . ? OH6 Mn2 2.149(3) 2_556 ? OH6 Mn4 2.173(3) 2_556 ? OH6 H6 0.951(19) . ? O7 Mn2 2.133(3) 2_556 ? O7 Mn1 2.275(2) 1_455 ? 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 O8 Mn1 O8 180.000(1) . 3_766 ? O8 Mn1 OH3 95.28(10) . 1_655 ? O8 Mn1 OH3 84.72(10) 3_766 1_655 ? O8 Mn1 OH3 84.72(10) . 3_666 ? O8 Mn1 OH3 95.28(10) 3_766 3_666 ? OH3 Mn1 OH3 180.000(1) 1_655 3_666 ? O8 Mn1 O7 90.30(10) . 1_655 ? O8 Mn1 O7 89.70(10) 3_766 1_655 ? OH3 Mn1 O7 99.77(9) 1_655 1_655 ? OH3 Mn1 O7 80.23(9) 3_666 1_655 ? O8 Mn1 O7 89.70(10) . 3_666 ? O8 Mn1 O7 90.30(10) 3_766 3_666 ? OH3 Mn1 O7 80.23(9) 1_655 3_666 ? OH3 Mn1 O7 99.77(9) 3_666 3_666 ? O7 Mn1 O7 180.0 1_655 3_666 ? OH1 Mn2 O7 113.71(11) . 2_546 ? OH1 Mn2 OH3 106.93(11) . 4_666 ? O7 Mn2 OH3 84.54(10) 2_546 4_666 ? OH1 Mn2 OH6 90.74(10) . 2_546 ? O7 Mn2 OH6 96.70(10) 2_546 2_546 ? OH3 Mn2 OH6 160.20(11) 4_666 2_546 ? OH1 Mn2 O4 92.19(10) . . ? O7 Mn2 O4 154.11(11) 2_546 . ? OH3 Mn2 O4 87.90(10) 4_666 . ? OH6 Mn2 O4 82.43(10) 2_546 . ? OH1 Mn2 Mn4 114.80(8) . . ? O7 Mn2 Mn4 117.30(8) 2_546 . ? OH3 Mn2 Mn4 115.53(8) 4_666 . ? OH6 Mn2 Mn4 46.63(8) 2_546 . ? O4 Mn2 Mn4 45.60(7) . . ? OH6 Mn3 OH5 99.85(11) . . ? OH6 Mn3 OH5 173.51(10) . 3_767 ? OH5 Mn3 OH5 84.42(12) . 3_767 ? OH6 Mn3 OH1 93.46(10) . 3_667 ? OH5 Mn3 OH1 84.90(10) . 3_667 ? OH5 Mn3 OH1 91.77(10) 3_767 3_667 ? OH6 Mn3 O2 91.42(10) . . ? OH5 Mn3 O2 95.21(10) . . ? OH5 Mn3 O2 83.29(10) 3_767 . ? OH1 Mn3 O2 175.02(10) 3_667 . ? OH6 Mn3 O2 85.38(10) . 3_667 ? OH5 Mn3 O2 174.13(10) . 3_667 ? OH5 Mn3 O2 90.59(10) 3_767 3_667 ? OH1 Mn3 O2 92.18(10) 3_667 3_667 ? O2 Mn3 O2 87.25(10) . 3_667 ? OH6 Mn3 Mn3 141.90(9) . 3_767 ? OH5 Mn3 Mn3 42.27(7) . 3_767 ? OH5 Mn3 Mn3 42.15(8) 3_767 3_767 ? OH1 Mn3 Mn3 87.76(7) 3_667 3_767 ? O2 Mn3 Mn3 88.99(7) . 3_767 ? O2 Mn3 Mn3 132.67(7) 3_667 3_767 ? OH6 Mn3 Mn3 87.79(8) . 3_667 ? OH5 Mn3 Mn3 138.62(7) . 3_667 ? OH5 Mn3 Mn3 85.79(7) 3_767 3_667 ? OH1 Mn3 Mn3 135.55(8) 3_667 3_667 ? O2 Mn3 Mn3 43.67(7) . 3_667 ? O2 Mn3 Mn3 43.58(6) 3_667 3_667 ? Mn3 Mn3 Mn3 117.15(4) 3_767 3_667 ? OH6 Mn3 Mn4 41.58(8) . 2_556 ? OH5 Mn3 Mn4 140.65(7) . 2_556 ? OH5 Mn3 Mn4 134.75(8) 3_767 2_556 ? OH1 Mn3 Mn4 89.44(7) 3_667 2_556 ? O2 Mn3 Mn4 93.58(7) . 2_556 ? O2 Mn3 Mn4 44.17(6) 3_667 2_556 ? Mn3 Mn3 Mn4 175.69(4) 3_767 2_556 ? Mn3 Mn3 Mn4 63.08(2) 3_667 2_556 ? OH3 Mn4 OH1 99.07(11) . 4_665 ? OH3 Mn4 O4 95.16(10) . . ? OH1 Mn4 O4 99.47(11) 4_665 . ? OH3 Mn4 OH6 93.36(10) . 2_546 ? OH1 Mn4 OH6 166.74(10) 4_665 2_546 ? O4 Mn4 OH6 83.91(11) . 2_546 ? OH3 Mn4 O2 101.04(10) . 4_565 ? OH1 Mn4 O2 89.81(10) 4_665 4_565 ? O4 Mn4 O2 159.84(10) . 4_565 ? OH6 Mn4 O2 83.24(10) 2_546 4_565 ? OH3 Mn4 OH5 177.13(12) . 2_646 ? OH1 Mn4 OH5 83.52(10) 4_665 2_646 ? O4 Mn4 OH5 83.15(10) . 2_646 ? OH6 Mn4 OH5 84.17(10) 2_546 2_646 ? O2 Mn4 OH5 80.15(9) 4_565 2_646 ? OH3 Mn4 Mn2 119.16(9) . . ? OH1 Mn4 Mn2 128.72(8) 4_665 . ? O4 Mn4 Mn2 48.03(8) . . ? OH6 Mn4 Mn2 45.95(7) 2_546 . ? O2 Mn4 Mn2 112.60(7) 4_565 . ? OH5 Mn4 Mn2 58.01(8) 2_646 . ? OH3 Mn4 Mn3 95.22(7) . 2_546 ? OH1 Mn4 Mn3 133.15(7) 4_665 2_546 ? O4 Mn4 Mn3 123.41(8) . 2_546 ? OH6 Mn4 Mn3 40.04(7) 2_546 2_546 ? O2 Mn4 Mn3 43.55(7) 4_565 2_546 ? OH5 Mn4 Mn3 83.83(7) 2_646 2_546 ? Mn2 Mn4 Mn3 78.93(2) . 2_546 ? O4 V O8 109.12(14) . . ? O4 V O7 110.18(12) . . ? O8 V O7 112.24(13) . . ? O4 V O2 107.30(13) . . ? O8 V O2 106.54(13) . . ? O7 V O2 111.28(13) . . ? Mn2 OH1 Mn4 127.57(12) . 4_566 ? Mn2 OH1 Mn3 122.79(12) . 3_667 ? Mn4 OH1 Mn3 97.44(11) 4_566 3_667 ? Mn2 OH1 H1 95(3) . . ? Mn4 OH1 H1 111(3) 4_566 . ? Mn3 OH1 H1 99(3) 3_667 . ? V O2 Mn3 122.75(13) . . ? V O2 Mn3 125.33(13) . 3_667 ? Mn3 O2 Mn3 92.75(10) . 3_667 ? V O2 Mn4 118.43(13) . 4_666 ? Mn3 O2 Mn4 97.87(10) . 4_666 ? Mn3 O2 Mn4 92.28(10) 3_667 4_666 ? Mn4 OH3 Mn2 117.67(12) . 4_565 ? Mn4 OH3 Mn1 126.43(14) . 1_455 ? Mn2 OH3 Mn1 98.53(11) 4_565 1_455 ? Mn4 OH3 H3 100(3) . . ? Mn2 OH3 H3 106(3) 4_565 . ? Mn1 OH3 H3 106(3) 1_455 . ? V O4 Mn4 140.97(16) . . ? V O4 Mn2 128.97(16) . . ? Mn4 O4 Mn2 86.36(9) . . ? Mn3 OH5 Mn3 95.58(12) . 3_767 ? Mn3 OH5 Mn4 93.29(11) . 2_656 ? Mn3 OH5 Mn4 98.63(11) 3_767 2_656 ? Mn3 OH5 H5 116(3) . . ? Mn3 OH5 H5 101(3) 3_767 . ? Mn4 OH5 H5 143(3) 2_656 . ? Mn3 OH6 Mn2 137.23(13) . 2_556 ? Mn3 OH6 Mn4 98.38(12) . 2_556 ? Mn2 OH6 Mn4 87.41(10) 2_556 2_556 ? Mn3 OH6 H6 108(3) . . ? Mn2 OH6 H6 108(3) 2_556 . ? Mn4 OH6 H6 113(3) 2_556 . ? V O7 Mn2 131.03(15) . 2_556 ? V O7 Mn1 127.67(13) . 1_455 ? Mn2 O7 Mn1 96.14(9) 2_556 1_455 ? V O8 Mn1 137.16(15) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.775 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.184