data_tiragalloite _publ_contact_author ; Athos Maria Callegari ; _publ_contact_author_email ; athosmaria.callegari@unipv.it ; loop_ _publ_author_name _publ_author_address 'Callegari A.M.' 'Dip. Scienze della Terra e Dell'Ambiente, University of Pavia, Pavia, Italy' 'Boiocchi M.' 'Centro Grandi Strumenti, University of Pavia, Pavia, Italy' 'Zema M.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' 'Tarantino S.C.' 'Dip. Scienze della Terra e Dell'Ambiente, CNR-IGG, U.O.S. Pavia, Pavia, Italy' _publ_section_title ; Crystal structure of tiragalloite ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As0.925 Ca0.088 H Mn3.912 O13 Si3.075' _chemical_formula_sum 'As0.925 Ca0.088 H Mn3.912 O13 Si3.075' _chemical_formula_weight 583.11 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' 'Si' 'Si' 0.0817 0.0704 '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' '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; loop_ _space_group_symop_operation_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 6.6702(2) _cell_length_b 19.9336(7) _cell_length_c 7.5759(2) _cell_angle_alpha 90 _cell_angle_beta 95.5181(14) _cell_angle_gamma 90 _cell_volume 1002.63(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3938 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 37.9 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.863 _exptl_crystal_F_000 1112.5 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 8.341 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker-Axs Smart-Apex CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 40972 _diffrn_reflns_av_unetI/netI 0.0481 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.043 _diffrn_reflns_theta_max 45.030 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8242 _reflns_number_gt 6149 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SMART (Bruker-Axs Inc)' _computing_cell_refinement 'SAINT (Bruker-Axs Inc)' _computing_data_reduction 'SAINT (Bruker-Axs Inc)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _refine_special_details ; DFIX geometrical restrain was used to refine the position for H site. ; _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^)+(0.0384P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8242 _refine_ls_number_parameters 195 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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_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 Mn1 Mn 0.25914(4) 0.64847(2) -0.14605(4) 0.01127(5) Uani 1 1 d . . . . . Mn2 Mn -0.45779(4) 0.58383(2) 0.54598(4) 0.01121(5) Uani 1 1 d . . . . . MN3A Ca 0.76325(4) 0.50880(2) 0.24555(4) 0.01274(6) Uani 0.028(6) 1 d . . P . . Mn3B Mn 0.76325(4) 0.50880(2) 0.24555(4) 0.01274(6) Uani 0.972(6) 1 d . . P . . MN4A Ca 0.05278(4) 0.74592(2) 0.13914(4) 0.01155(6) Uani 0.060(6) 1 d . . P . . Mn4B Mn 0.05278(4) 0.74592(2) 0.13914(4) 0.01155(6) Uani 0.940(6) 1 d . . P . . T1 Si 0.23132(7) 0.36792(3) 0.08053(6) 0.00875(7) Uani 1 1 d . . . . . T2 Si 0.26718(7) 0.52069(3) 0.16133(6) 0.00851(7) Uani 1 1 d . . . . . T3 Si 0.04811(7) 0.59790(3) 0.44020(6) 0.00886(8) Uani 1 1 d . . . . . T4A Si 0.43075(3) 0.30154(2) -0.21219(2) 0.00896(5) Uani 0.075(2) 1 d . . P . . T4B As 0.43075(3) 0.30154(2) -0.21219(2) 0.00896(5) Uani 0.925(2) 1 d . . P . . O1 O 0.2709(2) 0.23814(7) -0.18170(19) 0.0128(2) Uani 1 1 d . . . . . O2 O 0.4614(2) 0.32016(7) -0.42049(18) 0.0138(2) Uani 1 1 d . . . . . O3 O 0.6501(2) 0.28989(9) -0.0898(2) 0.0163(2) Uani 1 1 d . . . . . O4 O 0.3167(2) 0.37005(7) -0.12197(17) 0.0118(2) Uani 1 1 d . . . . . O5 O 0.0314(2) 0.32393(7) 0.07261(19) 0.0126(2) Uani 1 1 d . . . . . O6 O 0.4157(2) 0.34325(7) 0.22044(17) 0.0116(2) Uani 1 1 d . . . . . O7 O 0.1772(2) 0.44575(7) 0.1148(2) 0.0145(2) Uani 1 1 d . . . . . O8 O 0.3016(2) 0.55369(7) -0.02577(17) 0.0126(2) Uani 1 1 d . . . . . O9 O 0.45893(19) 0.51565(7) 0.30833(17) 0.01108(19) Uani 1 1 d . . . . . O10 O 0.0855(2) 0.55869(7) 0.25411(18) 0.0125(2) Uani 1 1 d . . . . . O11 O 0.0508(2) 0.67828(7) 0.38331(19) 0.0154(2) Uani 1 1 d D . . . . H H 0.122(5) 0.7041(4) 0.479(2) 0.023 Uiso 1 1 calc DR U . . . O12 O 0.22284(19) 0.58619(7) 0.60133(17) 0.01085(19) Uani 1 1 d . . . . . O13 O -0.1665(2) 0.56894(8) 0.47824(18) 0.0128(2) Uani 1 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 Mn1 0.01181(10) 0.01086(11) 0.01116(10) 0.00035(7) 0.00128(7) 0.00068(7) Mn2 0.01062(10) 0.01127(11) 0.01187(10) 0.00011(8) 0.00172(7) 0.00022(7) MN3A 0.01201(11) 0.01405(12) 0.01216(10) -0.00271(8) 0.00112(8) -0.00232(8) Mn3B 0.01201(11) 0.01405(12) 0.01216(10) -0.00271(8) 0.00112(8) -0.00232(8) MN4A 0.01171(10) 0.01131(11) 0.01162(10) -0.00130(8) 0.00108(8) 0.00006(8) Mn4B 0.01171(10) 0.01131(11) 0.01162(10) -0.00130(8) 0.00108(8) 0.00006(8) T1 0.00889(17) 0.00832(18) 0.00884(16) -0.00004(13) -0.00022(13) -0.00074(13) T2 0.00917(17) 0.00832(18) 0.00795(16) -0.00022(13) 0.00034(13) 0.00041(13) T3 0.00843(17) 0.00949(19) 0.00853(16) -0.00048(13) 0.00012(13) 0.00039(13) T4A 0.00922(7) 0.00962(8) 0.00798(7) 0.00056(5) 0.00058(5) -0.00029(5) T4B 0.00922(7) 0.00962(8) 0.00798(7) 0.00056(5) 0.00058(5) -0.00029(5) O1 0.0133(5) 0.0099(5) 0.0156(5) 0.0001(4) 0.0037(4) -0.0014(4) O2 0.0218(6) 0.0113(5) 0.0088(4) 0.0003(4) 0.0042(4) 0.0010(4) O3 0.0106(5) 0.0233(7) 0.0143(5) -0.0021(5) -0.0021(4) 0.0036(4) O4 0.0142(5) 0.0117(5) 0.0099(4) 0.0002(4) 0.0028(4) 0.0006(4) O5 0.0103(5) 0.0125(5) 0.0152(5) -0.0016(4) 0.0022(4) -0.0024(4) O6 0.0109(5) 0.0137(5) 0.0098(4) 0.0009(4) -0.0018(4) 0.0004(4) O7 0.0139(5) 0.0098(5) 0.0193(6) -0.0037(4) -0.0009(4) -0.0007(4) O8 0.0156(5) 0.0127(5) 0.0096(4) 0.0010(4) 0.0014(4) 0.0000(4) O9 0.0093(4) 0.0136(5) 0.0099(4) 0.0001(4) -0.0008(3) -0.0010(4) O10 0.0114(5) 0.0151(6) 0.0111(5) -0.0031(4) 0.0011(4) 0.0033(4) O11 0.0219(6) 0.0107(5) 0.0130(5) 0.0007(4) -0.0015(4) 0.0002(4) O12 0.0105(4) 0.0123(5) 0.0094(4) 0.0000(4) -0.0008(3) 0.0003(4) O13 0.0097(5) 0.0156(6) 0.0133(5) -0.0010(4) 0.0019(4) -0.0007(4) _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 2.1048(15) . ? Mn1 O5 2.1388(14) 3_565 ? Mn1 O3 2.2049(16) 3_665 ? Mn1 O1 2.2107(15) 2_554 ? Mn1 O12 2.2745(13) 1_554 ? Mn1 O6 2.2987(14) 3_665 ? Mn2 O13 2.0781(14) . ? Mn2 O2 2.1360(15) 3_565 ? Mn2 O12 2.2109(13) 1_455 ? Mn2 O9 2.2699(14) 3_566 ? Mn2 O9 2.2814(14) 1_455 ? Mn2 O6 2.2864(14) 3_566 ? MN3A O8 2.0911(14) 3_665 ? MN3A O9 2.1333(13) . ? MN3A O13 2.1460(14) 1_655 ? MN3A O12 2.2178(14) 3_666 ? MN3A O10 2.3636(15) 1_655 ? MN3A O4 2.6262(14) 3_665 ? MN3A O7 2.9395(16) 3_665 ? MN4A O5 2.1574(14) 3_565 ? MN4A O3 2.1724(15) 3_665 ? MN4A O6 2.2128(14) 2 ? MN4A O2 2.2165(14) 2_554 ? MN4A O1 2.2364(14) 3_565 ? MN4A O11 2.2901(15) . ? T1 O5 1.5925(14) . ? T1 O7 1.6196(15) . ? T1 O6 1.6208(14) . ? T1 O4 1.6875(14) . ? T2 O8 1.5992(14) . ? T2 O9 1.6162(13) . ? T2 O7 1.6356(15) . ? T2 O10 1.6432(14) . ? T3 O13 1.5952(14) . ? T3 O12 1.6215(14) . ? T3 O10 1.6518(14) . ? T3 O11 1.6599(16) . ? T4A O2 1.6529(13) . ? T4A O3 1.6712(14) . ? T4A O1 1.6835(14) . ? T4A O4 1.7354(14) . ? O1 Mn1 2.2108(15) 2_544 ? O1 Mn4B 2.2364(14) 3_565 ? O1 MN4A 2.2364(14) 3_565 ? O2 Mn2 2.1360(15) 3_565 ? O2 Mn4B 2.2164(14) 2_544 ? O2 MN4A 2.2164(14) 2_544 ? O3 Mn4B 2.1724(15) 3_665 ? O3 MN4A 2.1724(15) 3_665 ? O3 Mn1 2.2050(16) 3_665 ? O4 MN3A 2.6261(14) 3_665 ? O5 Mn1 2.1388(14) 3_565 ? O5 Mn4B 2.1575(14) 3_565 ? O5 MN4A 2.1575(14) 3_565 ? O6 Mn4B 2.2128(14) 2_545 ? O6 MN4A 2.2128(14) 2_545 ? O6 Mn2 2.2864(14) 3_566 ? O6 Mn1 2.2987(14) 3_665 ? O8 Mn3B 2.0911(14) 3_665 ? O8 MN3A 2.0911(14) 3_665 ? O9 Mn2 2.2699(14) 3_566 ? O9 Mn2 2.2813(14) 1_655 ? O10 Mn3B 2.3636(14) 1_455 ? O10 MN3A 2.3636(14) 1_455 ? O11 H 0.975(10) . ? O12 Mn2 2.2108(13) 1_655 ? O12 Mn3B 2.2178(14) 3_666 ? O12 MN3A 2.2178(14) 3_666 ? O12 Mn1 2.2745(13) 1_556 ? O13 Mn3B 2.1461(14) 1_455 ? O13 MN3A 2.1461(14) 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 O5 101.88(6) . 3_565 ? O8 Mn1 O3 97.71(6) . 3_665 ? O5 Mn1 O3 80.26(5) 3_565 3_665 ? O8 Mn1 O1 169.12(5) . 2_554 ? O5 Mn1 O1 84.98(5) 3_565 2_554 ? O3 Mn1 O1 91.73(6) 3_665 2_554 ? O8 Mn1 O12 82.72(5) . 1_554 ? O5 Mn1 O12 109.48(5) 3_565 1_554 ? O3 Mn1 O12 170.01(5) 3_665 1_554 ? O1 Mn1 O12 87.04(5) 2_554 1_554 ? O8 Mn1 O6 94.57(5) . 3_665 ? O5 Mn1 O6 160.93(5) 3_565 3_665 ? O3 Mn1 O6 88.09(5) 3_665 3_665 ? O1 Mn1 O6 80.30(5) 2_554 3_665 ? O12 Mn1 O6 81.93(5) 1_554 3_665 ? O13 Mn2 O2 89.37(6) . 3_565 ? O13 Mn2 O12 172.18(6) . 1_455 ? O2 Mn2 O12 95.48(6) 3_565 1_455 ? O13 Mn2 O9 92.42(5) . 3_566 ? O2 Mn2 O9 177.12(5) 3_565 3_566 ? O12 Mn2 O9 82.99(5) 1_455 3_566 ? O13 Mn2 O9 83.25(5) . 1_455 ? O2 Mn2 O9 101.01(5) 3_565 1_455 ? O12 Mn2 O9 89.79(5) 1_455 1_455 ? O9 Mn2 O9 81.45(5) 3_566 1_455 ? O13 Mn2 O6 103.52(5) . 3_566 ? O2 Mn2 O6 76.71(5) 3_565 3_566 ? O12 Mn2 O6 83.60(5) 1_455 3_566 ? O9 Mn2 O6 100.66(5) 3_566 3_566 ? O9 Mn2 O6 172.74(5) 1_455 3_566 ? O8 MN3A O9 95.01(5) 3_665 . ? O8 MN3A O13 177.38(6) 3_665 1_655 ? O9 MN3A O13 85.32(5) . 1_655 ? O8 MN3A O12 84.43(5) 3_665 3_666 ? O9 MN3A O12 86.04(5) . 3_666 ? O13 MN3A O12 93.00(5) 1_655 3_666 ? O8 MN3A O10 112.98(5) 3_665 1_655 ? O9 MN3A O10 148.13(5) . 1_655 ? O13 MN3A O10 67.43(5) 1_655 1_655 ? O12 MN3A O10 110.65(5) 3_666 1_655 ? O8 MN3A O4 104.16(5) 3_665 3_665 ? O9 MN3A O4 81.70(5) . 3_665 ? O13 MN3A O4 78.46(5) 1_655 3_665 ? O12 MN3A O4 165.55(5) 3_666 3_665 ? O10 MN3A O4 77.04(5) 1_655 3_665 ? O8 MN3A O7 58.68(5) 3_665 3_665 ? O9 MN3A O7 113.82(5) . 3_665 ? O13 MN3A O7 123.53(5) 1_655 3_665 ? O12 MN3A O7 138.27(5) 3_666 3_665 ? O10 MN3A O7 72.06(4) 1_655 3_665 ? O4 MN3A O7 55.00(4) 3_665 3_665 ? O5 MN4A O3 80.59(6) 3_565 3_665 ? O5 MN4A O6 158.32(5) 3_565 2 ? O3 MN4A O6 108.95(6) 3_665 2 ? O5 MN4A O2 83.44(5) 3_565 2_554 ? O3 MN4A O2 93.73(6) 3_665 2_554 ? O6 MN4A O2 76.66(5) 2 2_554 ? O5 MN4A O1 90.75(5) 3_565 3_565 ? O3 MN4A O1 168.79(6) 3_665 3_565 ? O6 MN4A O1 81.64(5) 2 3_565 ? O2 MN4A O1 92.31(6) 2_554 3_565 ? O5 MN4A O11 101.50(5) 3_565 . ? O3 MN4A O11 91.24(6) 3_665 . ? O6 MN4A O11 97.79(5) 2 . ? O2 MN4A O11 173.51(5) 2_554 . ? O1 MN4A O11 83.48(6) 3_565 . ? O5 T1 O7 109.55(8) . . ? O5 T1 O6 115.95(8) . . ? O7 T1 O6 110.65(8) . . ? O5 T1 O4 109.53(7) . . ? O7 T1 O4 102.80(8) . . ? O6 T1 O4 107.52(7) . . ? O8 T2 O9 117.69(8) . . ? O8 T2 O7 105.41(8) . . ? O9 T2 O7 109.97(8) . . ? O8 T2 O10 111.36(8) . . ? O9 T2 O10 107.53(7) . . ? O7 T2 O10 104.04(8) . . ? O13 T3 O12 113.86(8) . . ? O13 T3 O10 101.23(8) . . ? O12 T3 O10 114.70(7) . . ? O13 T3 O11 115.38(8) . . ? O12 T3 O11 108.03(8) . . ? O10 T3 O11 103.23(8) . . ? O2 T4A O3 112.24(8) . . ? O2 T4A O1 115.96(7) . . ? O3 T4A O1 110.60(8) . . ? O2 T4A O4 107.37(7) . . ? O3 T4A O4 106.53(7) . . ? O1 T4A O4 103.26(7) . . ? T4A O1 Mn1 123.28(7) . 2_544 ? T4A O1 Mn4B 123.09(8) . 3_565 ? Mn1 O1 Mn4B 99.55(6) 2_544 3_565 ? T4A O1 MN4A 123.09(8) . 3_565 ? Mn1 O1 MN4A 99.55(6) 2_544 3_565 ? Mn4B O1 MN4A 0.0 3_565 3_565 ? T4A O2 Mn2 128.97(8) . 3_565 ? T4A O2 Mn4B 124.28(8) . 2_544 ? Mn2 O2 Mn4B 105.53(6) 3_565 2_544 ? T4A O2 MN4A 124.28(8) . 2_544 ? Mn2 O2 MN4A 105.53(6) 3_565 2_544 ? Mn4B O2 MN4A 0.0 2_544 2_544 ? T4A O3 Mn4B 135.63(9) . 3_665 ? T4A O3 MN4A 135.63(9) . 3_665 ? Mn4B O3 MN4A 0.0 3_665 3_665 ? T4A O3 Mn1 121.98(8) . 3_665 ? Mn4B O3 Mn1 97.97(6) 3_665 3_665 ? MN4A O3 Mn1 97.97(6) 3_665 3_665 ? T1 O4 T4A 122.50(8) . . ? T1 O4 MN3A 105.82(6) . 3_665 ? T4A O4 MN3A 131.68(7) . 3_665 ? T1 O5 Mn1 128.68(8) . 3_565 ? T1 O5 Mn4B 122.71(8) . 3_565 ? Mn1 O5 Mn4B 100.49(6) 3_565 3_565 ? T1 O5 MN4A 122.71(8) . 3_565 ? Mn1 O5 MN4A 100.49(6) 3_565 3_565 ? Mn4B O5 MN4A 0.0 3_565 3_565 ? T1 O6 Mn4B 127.70(8) . 2_545 ? T1 O6 MN4A 127.70(8) . 2_545 ? Mn4B O6 MN4A 0.0 2_545 2_545 ? T1 O6 Mn2 110.01(7) . 3_566 ? Mn4B O6 Mn2 100.74(5) 2_545 3_566 ? MN4A O6 Mn2 100.74(5) 2_545 3_566 ? T1 O6 Mn1 119.50(7) . 3_665 ? Mn4B O6 Mn1 97.62(5) 2_545 3_665 ? MN4A O6 Mn1 97.62(5) 2_545 3_665 ? Mn2 O6 Mn1 95.48(5) 3_566 3_665 ? T1 O7 T2 145.74(10) . . ? T2 O8 Mn3B 115.11(8) . 3_665 ? T2 O8 MN3A 115.11(8) . 3_665 ? Mn3B O8 MN3A 0.0 3_665 3_665 ? T2 O8 Mn1 136.73(9) . . ? Mn3B O8 Mn1 100.43(6) 3_665 . ? MN3A O8 Mn1 100.43(6) 3_665 . ? T2 O9 MN3A 123.86(7) . . ? T2 O9 Mn2 110.48(7) . 3_566 ? MN3A O9 Mn2 95.75(5) . 3_566 ? T2 O9 Mn2 128.55(8) . 1_655 ? MN3A O9 Mn2 92.83(5) . 1_655 ? Mn2 O9 Mn2 98.55(5) 3_566 1_655 ? T2 O10 T3 139.58(9) . . ? T2 O10 Mn3B 120.03(8) . 1_455 ? T3 O10 Mn3B 90.63(6) . 1_455 ? T2 O10 MN3A 120.03(8) . 1_455 ? T3 O10 MN3A 90.63(6) . 1_455 ? Mn3B O10 MN3A 0.0 1_455 1_455 ? T3 O11 MN4A 141.18(9) . . ? T3 O11 H 109.5 . . ? MN4A O11 H 104.5 . . ? T3 O12 Mn2 119.75(7) . 1_655 ? T3 O12 Mn3B 120.50(8) . 3_666 ? Mn2 O12 Mn3B 95.07(5) 1_655 3_666 ? T3 O12 MN3A 120.50(8) . 3_666 ? Mn2 O12 MN3A 95.07(5) 1_655 3_666 ? Mn3B O12 MN3A 0.0 3_666 3_666 ? T3 O12 Mn1 124.44(8) . 1_556 ? Mn2 O12 Mn1 98.32(5) 1_655 1_556 ? Mn3B O12 Mn1 91.73(5) 3_666 1_556 ? MN3A O12 Mn1 91.73(5) 3_666 1_556 ? T3 O13 Mn2 150.39(9) . . ? T3 O13 Mn3B 100.52(7) . 1_455 ? Mn2 O13 Mn3B 98.46(6) . 1_455 ? T3 O13 MN3A 100.52(7) . 1_455 ? Mn2 O13 MN3A 98.46(6) . 1_455 ? Mn3B O13 MN3A 0.0 1_455 1_455 ? 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 O11 H O1 0.98 1.77 2.726(2) 167.8 2 _refine_diff_density_max 1.946 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.238 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL CELL 0.71073 6.6702 19.9336 7.5759 90.0000 95.5181 90.0000 ZERR 4 0.0002 0.0007 0.0002 0.0000 0.0014 0.0000 LATT 1 SYMM 0.50000-X, 0.50000+Y, 0.50000-Z SFAC H SFAC O SFAC SI SFAC CA SFAC MN SFAC AS UNIT 4 52 12.12 0.4 15.6 3.88 MERG 2 L.S. 10 BOND $H ACTA list 4 rem OMIT 0 2 0 DFIX 0.98 0.01 O11 H CONN 4 T3 CONN 6 MN1 CONN 6 MN2 CONN 7 1.5 MN3A CONN 6 MN4A CONN 4 T1 CONN 4 T2 CONN 4 T4A EQIV $5 x+1, y, z FREE MN3A T3_$5 EQIV $3 -x+1, -y+1, -z BIND MN3A O7_$3 EQIV $12 -x+1/2, y+1/2, -z+1/2 HTAB O11 O1_$12 FMAP 2 PLAN 25 WGHT 0.038400 FVAR 0.33058 0.02802 0.05996 0.07528 MN1 5 0.259142 0.648471 -0.146053 11.00000 0.01181 0.01086 = 0.01116 0.00035 0.00128 0.00068 MN2 5 -0.457791 0.583834 0.545976 11.00000 0.01062 0.01127 = 0.01187 0.00011 0.00172 0.00022 MN3A 4 0.763246 0.508795 0.245545 21.00000 0.01201 0.01405 = 0.01216 -0.00271 0.00112 -0.00232 MN3B 5 0.763246 0.508795 0.245545 -21.00000 0.01201 0.01405 = 0.01216 -0.00271 0.00112 -0.00232 MN4A 4 0.052784 0.745923 0.139141 31.00000 0.01171 0.01131 = 0.01162 -0.00130 0.00108 0.00006 MN4B 5 0.052784 0.745923 0.139141 -31.00000 0.01171 0.01131 = 0.01162 -0.00130 0.00108 0.00006 T1 3 0.231320 0.367921 0.080528 11.00000 0.00889 0.00832 = 0.00884 -0.00004 -0.00022 -0.00074 T2 3 0.267180 0.520690 0.161334 11.00000 0.00917 0.00832 = 0.00795 -0.00022 0.00034 0.00041 T3 3 0.048107 0.597898 0.440204 11.00000 0.00843 0.00949 = 0.00853 -0.00048 0.00012 0.00039 T4A 3 0.430746 0.301535 -0.212193 41.00000 0.00922 0.00962 = 0.00798 0.00056 0.00058 -0.00029 T4B 6 0.430746 0.301535 -0.212193 -41.00000 0.00922 0.00962 = 0.00798 0.00056 0.00058 -0.00029 O1 2 0.270944 0.238135 -0.181699 11.00000 0.01331 0.00988 = 0.01565 0.00006 0.00368 -0.00142 O2 2 0.461442 0.320157 -0.420489 11.00000 0.02181 0.01133 = 0.00878 0.00033 0.00422 0.00099 O3 2 0.650099 0.289895 -0.089846 11.00000 0.01059 0.02331 = 0.01432 -0.00215 -0.00214 0.00361 O4 2 0.316686 0.370054 -0.121973 11.00000 0.01422 0.01166 = 0.00985 0.00019 0.00277 0.00057 O5 2 0.031366 0.323931 0.072615 11.00000 0.01034 0.01246 = 0.01516 -0.00157 0.00218 -0.00238 O6 2 0.415693 0.343249 0.220435 11.00000 0.01088 0.01369 = 0.00983 0.00086 -0.00175 0.00042 O7 2 0.177164 0.445755 0.114809 11.00000 0.01393 0.00982 = 0.01930 -0.00369 -0.00086 -0.00069 O8 2 0.301620 0.553695 -0.025766 11.00000 0.01561 0.01267 = 0.00955 0.00105 0.00144 0.00004 O9 2 0.458930 0.515651 0.308334 11.00000 0.00935 0.01362 = 0.00994 0.00005 -0.00079 -0.00103 O10 2 0.085501 0.558687 0.254115 11.00000 0.01137 0.01512 = 0.01109 -0.00310 0.00110 0.00331 O11 2 0.050786 0.678284 0.383307 11.00000 0.02186 0.01072 = 0.01301 0.00066 -0.00151 0.00017 AFIX 88 H 1 0.121995 0.704123 0.479066 11.00000 -1.50000 AFIX 0 O12 2 0.222841 0.586192 0.601335 11.00000 0.01052 0.01232 = 0.00939 0.00001 -0.00077 0.00032 O13 2 -0.166491 0.568935 0.478240 11.00000 0.00974 0.01560 = 0.01333 -0.00097 0.00186 -0.00069 EXYZ MN3A MN3B EADP MN3A MN3B EXYZ MN4A MN4B EADP MN4A MN4B EXYZ T4A T4B EADP T4A T4B SUMP 0.1 0.01 1. 2 1. 3 REM SUMP 3.03 0.001 1. 6 1. 7 1. 8 1. 9 HKLF 4 REM REM R1 = 0.0373 for 6149 Fo > 4sig(Fo) and 0.0583 for all 8242 data REM 195 parameters refined using 2 restraints END WGHT 0.0384 0.0000 REM Highest difference peak 1.946, deepest hole -0.920, 1-sigma level 0.238 Q1 1 0.5160 0.3037 -0.2316 11.00000 0.05 1.42 Q2 1 0.6957 0.5068 0.2718 11.00000 0.05 1.11 Q3 1 -0.4737 0.6032 0.5048 11.00000 0.05 1.07 Q4 1 -0.0184 0.7444 0.1559 11.00000 0.05 1.07 Q5 1 -0.3757 0.5763 0.5025 11.00000 0.05 1.05 Q6 1 0.5191 0.2991 -0.1021 11.00000 0.05 1.02 Q7 1 0.3478 0.2989 -0.1924 11.00000 0.05 1.01 Q8 1 0.5831 0.2738 -0.0776 11.00000 0.05 0.99 Q9 1 0.1797 0.6499 -0.1310 11.00000 0.05 0.98 Q10 1 0.2692 0.6764 -0.1395 11.00000 0.05 0.95 Q11 1 0.0159 0.7646 0.0839 11.00000 0.05 0.95 Q12 1 -0.5408 0.5787 0.5601 11.00000 0.05 0.94 Q13 1 0.0558 0.7157 0.1478 11.00000 0.05 0.93 Q14 1 0.0605 0.7658 0.5440 11.00000 0.05 0.91 Q15 1 0.3561 0.5148 0.1647 11.00000 0.05 0.90 Q16 1 0.2374 0.4572 0.1594 11.00000 0.05 0.90 Q17 1 0.4070 0.3037 -0.4772 11.00000 0.05 0.87 Q18 1 0.1573 0.3674 0.0918 11.00000 0.05 0.87 Q19 1 0.7600 0.2940 -0.2765 11.00000 0.05 0.87 Q20 1 0.1950 0.5273 0.2014 11.00000 0.05 0.86 Q21 1 0.2615 0.6116 0.5869 11.00000 0.05 0.86 Q22 1 0.2970 0.6082 0.6540 11.00000 0.05 0.85 Q23 1 -0.0417 0.5923 0.4840 11.00000 0.05 0.84 Q24 1 0.4564 0.2794 -0.4235 11.00000 0.05 0.84 Q25 1 0.4066 0.3225 -0.2660 11.00000 0.05 0.84 ; _shelx_res_checksum 26611 _shelx_hkl_file ; 1 0 0 1.93403 1.30803 2 1 0 0 0.60418 1.14593 1 2 0 0 17.5936 4.57639 1 2 0 0 25.3918 4.67926 2 3 0 0 -4.6560 2.98022 1 3 0 0 -6.3829 2.82314 2 4 0 0 5879.98 224.342 1 4 0 0 6120.62 225.881 2 5 0 0 -2.5468 4.41538 2 5 0 0 4.15178 5.46201 1 6 0 0 3504.99 130.172 3 6 0 0 3570.26 119.647 7 6 0 0 3659.19 148.219 1 6 0 0 3904.36 145.484 2 7 0 0 -1.4028 5.72756 1 7 0 0 -2.3335 6.24764 6 7 0 0 3.57640 4.87747 7 7 0 0 2.37280 4.13871 3 8 0 0 258.864 18.1336 3 8 0 0 278.734 18.5081 6 8 0 0 282.311 17.6056 7 8 0 0 230.897 26.2056 1 9 0 0 4.38801 5.65708 7 -9 0 0 13.3860 9.65371 1 9 0 0 2.46753 5.26424 3 10 0 0 1103.97 51.6117 3 11 0 0 2.33713 6.07067 3 11 0 0 3.54139 6.46859 7 12 0 0 -0.6730 7.47283 7 12 0 0 2.50050 7.79598 3 13 0 0 8.16392 9.35143 3 -13 0 0 -13.410 7.19302 7 0 -1 0 0.09902 0.22613 2 0 1 0 -0.0816 0.27921 1 1 -1 0 461.806 19.0996 1 1 -1 0 454.272 19.3177 2 1 1 0 425.810 18.7454 1 1 1 0 454.776 17.9356 2 2 -1 0 3174.75 120.351 1 2 -1 0 3258.81 122.208 2 2 1 0 3186.49 120.215 1 2 1 0 3310.90 120.682 2 3 -1 0 420.776 22.0314 1 3 -1 0 429.345 21.5682 2 3 1 0 395.374 19.6535 2 3 1 0 391.186 21.6605 1 4 -1 0 6213.33 229.423 2 4 -1 0 5771.24 226.511 1 4 1 0 5984.85 227.164 1 4 1 0 6308.81 227.617 2 5 -1 0 4.29912 5.21873 1 5 -1 0 12.5951 6.09918 2 5 1 0 17.3491 7.10954 1 5 1 0 16.8512 6.10676 2 6 -1 0 953.819 50.1791 1 6 -1 0 874.500 38.9371 3 6 -1 0 969.776 36.2996 7 6 -1 0 988.289 47.2173 2 6 1 0 980.430 50.5472 1 6 1 0 967.603 39.3577 3 6 1 0 934.433 36.3325 7 7 -1 0 7.82179 5.26068 3 7 -1 0 7.72521 5.35589 7 7 -1 0 1.87505 6.97495 6 7 -1 0 -0.3445 5.61306 1 7 1 0 10.1417 6.64965 6 7 1 0 4.12632 7.24851 1 7 1 0 5.75967 5.29919 7 7 1 0 8.79344 5.27188 3 8 -1 0 34.3658 7.71969 3 8 -1 0 42.4113 8.00640 7 8 -1 0 40.1404 9.76496 6 8 1 0 33.0720 12.4020 1 8 1 0 35.2359 9.14652 6 8 1 0 43.0383 8.44363 3 8 1 0 41.5680 7.93617 7 9 -1 0 36.1427 8.46333 3 9 -1 0 54.2955 9.27735 7 9 1 0 34.0985 8.05960 7 -9 1 0 49.9010 15.1281 1 9 1 0 30.1489 8.56614 3 10 -1 0 246.312 18.9419 7 10 -1 0 176.505 17.8830 3 10 1 0 183.638 17.8825 3 10 1 0 193.065 17.0352 7 11 -1 0 8.58650 7.15893 3 11 -1 0 4.05206 7.03516 7 11 1 0 7.34485 6.60135 7 11 1 0 -12.578 4.28265 3 12 -1 0 38.9663 11.4134 3 12 1 0 41.3341 11.5886 3 12 1 0 56.8339 12.9528 7 -13 -1 0 18.9118 10.1248 7 13 -1 0 17.4474 10.6799 3 -13 1 0 23.7353 10.3274 7 13 1 0 16.6304 10.7672 3 0 -2 0 13.9888 1.68149 2 0 2 0 13.6584 1.94965 1 1 -2 0 1.44451 1.79494 2 1 2 0 1.59181 1.55472 1 -1 2 0 0.47023 1.33113 1 2 -2 0 4384.49 161.007 1 2 -2 0 4328.40 163.974 2 2 2 0 4402.61 160.847 1 2 2 0 4360.54 160.969 2 3 -2 0 1675.23 69.3998 1 3 -2 0 1724.55 70.2734 2 3 2 0 1690.41 69.5147 1 3 2 0 1794.19 67.0435 2 4 -2 0 477.195 27.7304 1 4 -2 0 516.652 27.7006 2 4 2 0 526.994 24.8034 2 4 2 0 535.834 28.9024 1 5 -2 0 17.5285 6.92121 2 5 -2 0 17.0316 6.88056 1 5 2 0 19.2794 8.16542 1 5 2 0 13.2460 5.57291 2 6 -2 0 69.1389 8.08727 7 6 -2 0 42.2170 10.6798 1 6 -2 0 58.2618 10.6671 2 6 -2 0 55.6431 7.63132 3 6 2 0 67.1874 8.74465 6 6 2 0 48.9475 7.17449 3 6 2 0 48.5319 10.7729 1 6 2 0 61.6857 7.62636 7 7 -2 0 246.867 16.3158 3 7 -2 0 255.635 17.2887 6 7 -2 0 240.520 15.3853 7 7 2 0 223.094 15.3133 7 7 2 0 237.877 16.0483 3 7 2 0 289.678 26.1234 1 7 2 0 245.931 16.4931 6 8 -2 0 339.856 20.6731 3 8 -2 0 349.945 19.7933 7 8 2 0 332.203 19.7063 7 8 2 0 343.839 21.0176 3 8 2 0 329.344 20.6866 6 8 2 0 332.857 31.6095 1 -8 2 0 302.431 29.3019 1 9 -2 0 44.5456 8.84464 7 9 -2 0 51.1943 9.47018 3 9 2 0 27.2002 13.3815 1 -9 2 0 43.6275 14.3077 1 9 2 0 51.1104 9.90284 3 9 2 0 31.7441 7.95646 7 10 -2 0 -0.3343 6.50952 7 10 -2 0 -1.7719 5.28610 3 -10 -2 0 -3.0774 6.04783 6 10 2 0 6.17090 6.38904 3 10 2 0 18.2169 7.73756 7 11 -2 0 -2.8671 5.15957 3 11 -2 0 -1.2205 6.67329 7 11 2 0 -5.8447 4.63159 7 11 2 0 -6.8915 5.41248 3 12 -2 0 2.33260 7.53205 3 12 2 0 0.28414 6.84562 3 12 2 0 -7.7628 7.99479 7 13 -2 0 7.82260 9.88212 3 -13 2 0 -0.4606 9.56029 7 13 2 0 -7.4768 7.89295 3 0 -3 0 -0.1549 1.18679 2 0 3 0 -0.0366 1.48584 1 1 -3 0 635.865 27.5042 2 1 3 0 650.228 26.5000 1 -1 3 0 625.275 26.1861 1 2 -3 0 264.741 15.2418 2 2 3 0 226.609 13.8875 1 -2 3 0 251.238 13.8771 1 3 -3 0 310.811 19.3536 2 3 3 0 315.867 19.2720 1 3 3 0 360.998 15.8326 2 4 -3 0 47.2431 8.78054 1 4 -3 0 58.3857 9.33841 2 4 3 0 68.4939 6.91258 2 4 3 0 68.7892 9.85573 1 5 -3 0 182.961 16.6892 2 5 -3 0 189.373 17.5506 1 5 3 0 167.178 13.1248 2 5 3 0 178.450 17.3010 1 6 -3 0 65.3882 7.88745 7 6 -3 0 56.7287 7.63434 3 6 -3 0 60.8189 11.0454 2 6 3 0 87.7108 9.46863 6 6 3 0 64.2146 12.1120 1 6 3 0 58.3141 7.56791 3 6 3 0 64.1054 7.83643 7 7 -3 0 164.835 13.5041 3 7 -3 0 182.547 13.0370 7 7 -3 0 206.483 20.6806 2 7 3 0 198.343 14.5265 6 7 3 0 162.596 13.4038 3 -7 3 0 153.588 18.9049 1 7 3 0 132.283 18.9656 1 7 3 0 200.087 13.9176 7 8 -3 0 188.044 15.1664 3 8 -3 0 207.445 15.1573 7 8 3 0 166.449 14.7206 3 8 3 0 151.709 15.0752 6 8 3 0 196.170 15.0150 7 -8 3 0 170.339 21.8780 1 8 3 0 119.922 20.3115 1 9 -3 0 13.0096 7.01253 7 9 -3 0 7.26543 5.99704 3 9 3 0 12.6795 10.0056 1 -9 3 0 19.8154 10.7265 1 9 3 0 10.7664 6.79163 3 9 3 0 12.3158 6.49193 7 -10 -3 0 28.0371 7.82715 6 10 -3 0 28.9721 8.88653 7 10 -3 0 27.4933 8.95586 3 10 3 0 14.9917 8.06871 3 10 3 0 22.8138 8.37047 7 11 -3 0 16.9202 8.58109 7 11 -3 0 0.17934 6.01273 3 11 3 0 19.8946 7.87232 7 11 3 0 -1.7867 5.80184 3 12 -3 0 57.0428 13.2299 3 12 3 0 135.422 16.3737 7 -12 3 0 53.6491 11.8114 7 12 3 0 72.7282 13.8171 3 13 -3 0 111.765 17.0502 3 13 3 0 77.4904 14.8366 3 0 -4 0 183.775 9.75969 2 0 4 0 193.536 10.5632 1 1 -4 0 -5.9976 2.58724 2 1 4 0 -4.9699 2.13209 1 -1 4 0 -4.0160 2.30318 1 2 -4 0 0.55084 3.81168 2 2 4 0 15.1757 4.43910 1 -2 4 0 1.42469 2.97736 1 3 -4 0 1343.45 56.3509 2 -3 4 0 1252.65 53.9371 1 3 4 0 1288.28 54.7346 1 4 -4 0 1.40132 4.65491 2 -4 4 0 -1.3225 3.75631 1 4 4 0 0.19671 4.22057 1 4 4 0 2.10448 3.12496 2 5 -4 0 349.284 23.7005 2 5 4 0 299.906 22.8821 1 -5 4 0 304.426 22.1078 1 6 -4 0 57.7241 7.37311 7 6 -4 0 67.5307 11.6207 2 6 -4 0 79.0785 8.48174 3 -6 4 0 94.7278 13.4496 1 6 4 0 49.4927 7.39722 7 6 4 0 79.3199 9.11033 6 6 4 0 51.5984 11.4967 1 6 4 0 68.7302 8.07766 3 7 -4 0 -2.5348 5.75872 2 7 -4 0 10.7682 5.35687 7 7 -4 0 6.65705 4.59722 3 -7 4 0 4.29950 6.48756 1 7 4 0 9.19195 5.27066 7 7 4 0 9.79829 8.32961 1 7 4 0 0.05489 3.63950 3 7 4 0 3.12756 6.19501 6 8 -4 0 14.9751 5.88598 3 8 -4 0 11.1057 6.59029 7 8 4 0 16.2457 8.23254 6 8 4 0 14.2171 6.31293 7 8 4 0 16.2651 9.50558 1 -8 4 0 11.7553 8.78704 1 8 4 0 10.6123 5.52684 3 9 -4 0 289.555 20.3458 3 9 -4 0 289.781 19.8488 7 9 4 0 281.616 19.9254 7 9 4 0 237.946 29.7920 1 9 4 0 298.561 21.0531 3 -9 4 0 304.307 30.9496 1 -10 -4 0 20.1059 7.78127 6 10 -4 0 9.25420 7.63955 7 10 -4 0 21.6876 8.31766 3 10 4 0 16.2324 7.67767 7 10 4 0 -0.3522 6.02285 3 11 -4 0 -1.4230 6.01911 3 -11 -4 0 6.46593 6.06951 6 11 4 0 3.67991 6.61941 7 11 4 0 6.76955 6.87083 3 12 -4 0 9.66694 8.92187 3 12 4 0 1.27916 7.97354 7 12 4 0 -4.0005 6.29680 3 -12 4 0 -1.7202 7.98266 7 13 -4 0 16.8877 10.8609 3 13 4 0 25.5772 10.2247 7 13 4 0 14.6937 10.7362 3 0 -5 0 -3.4372 2.46169 2 0 5 0 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