data_NHMD01 _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca0.95 H Mn1.05 Na O9 Si3' _chemical_formula_weight 348.03 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' 'Na' 'Na' 0.0362 0.0249 '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' 'Mn' 'Mn' 0.3368 0.7283 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 7.8492(16) _cell_length_b 6.9752(14) _cell_length_c 6.9117(14) _cell_angle_alpha 90.79(3) _cell_angle_beta 94.45(3) _cell_angle_gamma 102.85(3) _cell_volume 367.64(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.144 _exptl_crystal_F_000 342 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 3.120 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7004 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.671 _diffrn_reflns_theta_max 36.382 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 7004 _reflns_number_gt 6746 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.1153P)^2^+0.3167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7004 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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_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 Na1 Na 0.55607(13) 0.24534(18) 0.34880(18) 0.0163(3) Uani 0.984(6) 1 d . . . . . M1MN Mn 0.84885(5) 0.59382(5) 0.14611(6) 0.00814(12) Uani 0.218(10) 1 d . . P . . M1CA Ca 0.84885(5) 0.59382(5) 0.14611(6) 0.00814(12) Uani 0.782(10) 1 d . . P . . M2MN Mn 0.85182(4) 0.08492(5) 0.13485(5) 0.00897(11) Uani 0.822(11) 1 d . . P . . M2CA Ca 0.85182(4) 0.08492(5) 0.13485(5) 0.00897(11) Uani 0.178(11) 1 d . . P . . Si1 Si 0.21966(7) 0.40688(8) 0.33593(9) 0.00653(13) Uani 1 1 d . . . . . Si2 Si 0.20684(7) 0.96015(8) 0.34933(9) 0.00669(13) Uani 1 1 d . . . . . Si3 Si 0.45072(7) 0.74630(8) 0.14308(9) 0.00659(13) Uani 1 1 d . . . . . O1 O 0.6571(2) 0.8063(3) 0.1226(3) 0.0109(3) Uani 1 1 d . . . . . O2 O 0.3257(2) 0.7231(3) 0.9441(2) 0.0108(3) Uani 1 1 d . . . . . O3 O 0.1912(2) 0.5097(2) 0.5387(2) 0.0103(3) Uani 1 1 d . . . . . O4 O 0.1563(2) 0.8533(2) 0.5497(2) 0.0115(3) Uani 1 1 d . . . . . O5 O 0.0607(2) 0.3851(3) 0.1717(2) 0.0097(3) Uani 1 1 d . . . . . O6 O 0.0567(2) 0.9035(2) 0.1732(3) 0.0105(3) Uani 1 1 d . . . . . O7 O 0.4036(2) 0.5335(2) 0.2566(3) 0.0115(3) Uani 1 1 d . . . . . O8 O 0.3915(2) 0.9047(2) 0.2925(3) 0.0104(3) Uani 1 1 d . . . . . O9 O 0.2653(2) 0.1966(2) 0.3922(2) 0.0093(3) Uani 1 1 d . . . . . H1 H 0.200(11) 0.547(13) 0.631(13) 0.015 Uiso 0.5 1 d . U P . . H2 H 0.153(11) 0.694(13) 0.539(12) 0.015 Uiso 0.5 1 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 Na1 0.0077(4) 0.0193(6) 0.0200(6) -0.0011(4) 0.0028(3) -0.0014(3) M1MN 0.00702(18) 0.00711(18) 0.00992(19) -0.00011(12) 0.00064(12) 0.00084(12) M1CA 0.00702(18) 0.00711(18) 0.00992(19) -0.00011(12) 0.00064(12) 0.00084(12) M2MN 0.00670(16) 0.00826(17) 0.01182(18) -0.00021(11) 0.00039(11) 0.00154(11) M2CA 0.00670(16) 0.00826(17) 0.01182(18) -0.00021(11) 0.00039(11) 0.00154(11) Si1 0.0055(2) 0.0056(2) 0.0082(2) -0.00046(17) -0.00053(17) 0.00102(16) Si2 0.0052(2) 0.0050(2) 0.0092(3) -0.00092(17) -0.00069(17) 0.00036(16) Si3 0.0041(2) 0.0066(2) 0.0085(2) -0.00088(17) -0.00006(16) 0.00046(17) O1 0.0055(5) 0.0110(6) 0.0161(7) -0.0005(5) 0.0026(5) 0.0009(5) O2 0.0089(6) 0.0122(6) 0.0098(6) -0.0015(5) -0.0026(5) 0.0001(5) O3 0.0122(6) 0.0101(6) 0.0091(6) -0.0023(5) 0.0005(5) 0.0039(5) O4 0.0148(7) 0.0081(6) 0.0117(7) 0.0014(5) 0.0036(5) 0.0017(5) O5 0.0070(6) 0.0122(6) 0.0096(6) -0.0001(5) -0.0013(5) 0.0019(5) O6 0.0074(6) 0.0099(6) 0.0128(7) -0.0015(5) -0.0031(5) 0.0007(5) O7 0.0079(6) 0.0087(6) 0.0177(7) 0.0035(5) 0.0025(5) 0.0009(5) O8 0.0075(5) 0.0102(6) 0.0141(7) -0.0041(5) 0.0006(5) 0.0031(5) O9 0.0087(6) 0.0052(5) 0.0135(6) -0.0002(5) -0.0008(5) 0.0010(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 Na1 O9 2.276(2) . ? Na1 O2 2.285(2) 2_666 ? Na1 O3 2.383(2) 2_666 ? Na1 O8 2.449(2) 1_545 ? Na1 O4 2.554(2) 2_666 ? Na1 O7 2.620(2) . ? Na1 O8 2.741(2) 2_666 ? Na1 Si2 3.0079(15) 1_545 ? Na1 Si1 3.0886(15) . ? Na1 M2MN 3.2358(15) . ? Na1 Si2 3.2461(17) 2_666 ? M1MN O3 2.3270(18) 2_666 ? M1MN O1 2.3341(18) . ? M1MN O5 2.3570(18) 2_665 ? M1MN O2 2.3741(19) 2_666 ? M1MN O6 2.3950(19) 1_655 ? M1MN O5 2.4398(18) 1_655 ? M2MN O2 2.1829(19) 2_666 ? M2MN O1 2.1848(18) 1_545 ? M2MN O4 2.2249(18) 2_666 ? M2MN O6 2.2595(18) 1_645 ? M2MN O6 2.2961(19) 2_665 ? M2MN O5 2.3517(19) 1_655 ? Si1 O5 1.6001(18) . ? Si1 O3 1.6186(18) . ? Si1 O9 1.6302(17) . ? Si1 O7 1.6535(17) . ? Si2 O6 1.6076(18) . ? Si2 O4 1.6167(18) . ? Si2 O9 1.6272(17) 1_565 ? Si2 O8 1.6551(17) . ? Si3 O1 1.5988(17) . ? Si3 O2 1.6103(18) 1_554 ? Si3 O8 1.6656(18) . ? Si3 O7 1.6700(18) . ? 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 O9 Na1 O2 125.34(8) . 2_666 ? O9 Na1 O3 134.05(8) . 2_666 ? O2 Na1 O3 84.80(7) 2_666 2_666 ? O9 Na1 O8 65.58(6) . 1_545 ? O2 Na1 O8 96.36(8) 2_666 1_545 ? O3 Na1 O8 153.33(8) 2_666 1_545 ? O9 Na1 O4 145.86(8) . 2_666 ? O2 Na1 O4 81.74(7) 2_666 2_666 ? O3 Na1 O4 60.02(6) 2_666 2_666 ? O8 Na1 O4 93.67(7) 1_545 2_666 ? O9 Na1 O7 63.17(6) . . ? O2 Na1 O7 88.26(8) 2_666 . ? O3 Na1 O7 87.28(7) 2_666 . ? O8 Na1 O7 119.37(7) 1_545 . ? O4 Na1 O7 146.40(7) 2_666 . ? O9 Na1 O8 89.03(7) . 2_666 ? O2 Na1 O8 140.34(8) 2_666 2_666 ? O3 Na1 O8 82.90(7) 2_666 2_666 ? O8 Na1 O8 79.32(7) 1_545 2_666 ? O4 Na1 O8 59.51(6) 2_666 2_666 ? O7 Na1 O8 128.44(7) . 2_666 ? O9 Na1 Si2 32.25(4) . 1_545 ? O2 Na1 Si2 115.23(7) 2_666 1_545 ? O3 Na1 Si2 159.87(7) 2_666 1_545 ? O8 Na1 Si2 33.35(4) 1_545 1_545 ? O4 Na1 Si2 122.00(6) 2_666 1_545 ? O7 Na1 Si2 91.28(5) . 1_545 ? O8 Na1 Si2 82.32(6) 2_666 1_545 ? O9 Na1 Si1 30.91(4) . . ? O2 Na1 Si1 110.76(7) 2_666 . ? O3 Na1 Si1 111.63(6) 2_666 . ? O8 Na1 Si1 92.95(6) 1_545 . ? O4 Na1 Si1 165.09(6) 2_666 . ? O7 Na1 Si1 32.37(4) . . ? O8 Na1 Si1 108.82(6) 2_666 . ? Si2 Na1 Si1 61.07(3) 1_545 . ? O9 Na1 M2MN 145.55(6) . . ? O2 Na1 M2MN 42.36(5) 2_666 . ? O3 Na1 M2MN 80.38(5) 2_666 . ? O8 Na1 M2MN 82.69(6) 1_545 . ? O4 Na1 M2MN 43.23(4) 2_666 . ? O7 Na1 M2MN 129.66(6) . . ? O8 Na1 M2MN 98.30(5) 2_666 . ? Si2 Na1 M2MN 115.26(4) 1_545 . ? Si1 Na1 M2MN 151.26(5) . . ? O9 Na1 Si2 117.23(7) . 2_666 ? O2 Na1 Si2 109.80(6) 2_666 2_666 ? O3 Na1 Si2 72.53(6) 2_666 2_666 ? O8 Na1 Si2 82.13(6) 1_545 2_666 ? O4 Na1 Si2 29.39(4) 2_666 2_666 ? O7 Na1 Si2 150.96(6) . 2_666 ? O8 Na1 Si2 30.64(4) 2_666 2_666 ? Si2 Na1 Si2 100.58(4) 1_545 2_666 ? Si1 Na1 Si2 139.43(5) . 2_666 ? M2MN Na1 Si2 68.31(3) . 2_666 ? O3 M1MN O1 99.38(7) 2_666 . ? O3 M1MN O5 161.15(6) 2_666 2_665 ? O1 M1MN O5 99.21(7) . 2_665 ? O3 M1MN O2 84.08(7) 2_666 2_666 ? O1 M1MN O2 105.53(6) . 2_666 ? O5 M1MN O2 87.94(7) 2_665 2_666 ? O3 M1MN O6 106.53(7) 2_666 1_655 ? O1 M1MN O6 80.27(6) . 1_655 ? O5 M1MN O6 79.76(7) 2_665 1_655 ? O2 M1MN O6 167.17(6) 2_666 1_655 ? O3 M1MN O5 81.42(6) 2_666 1_655 ? O1 M1MN O5 177.32(6) . 1_655 ? O5 M1MN O5 80.15(7) 2_665 1_655 ? O2 M1MN O5 77.07(6) 2_666 1_655 ? O6 M1MN O5 97.05(6) 1_655 1_655 ? O3 M1MN Na1 45.23(5) 2_666 . ? O1 M1MN Na1 92.40(5) . . ? O5 M1MN Na1 130.65(5) 2_665 . ? O2 M1MN Na1 42.88(5) 2_666 . ? O6 M1MN Na1 149.58(5) 1_655 . ? O5 M1MN Na1 89.97(5) 1_655 . ? O2 M2MN O1 97.96(7) 2_666 1_545 ? O2 M2MN O4 92.08(7) 2_666 2_666 ? O1 M2MN O4 95.78(7) 1_545 2_666 ? O2 M2MN O6 170.78(7) 2_666 1_645 ? O1 M2MN O6 86.61(6) 1_545 1_645 ? O4 M2MN O6 95.43(7) 2_666 1_645 ? O2 M2MN O6 90.90(7) 2_666 2_665 ? O1 M2MN O6 101.97(7) 1_545 2_665 ? O4 M2MN O6 161.41(6) 2_666 2_665 ? O6 M2MN O6 80.29(7) 1_645 2_665 ? O2 M2MN O5 82.74(6) 2_666 1_655 ? O1 M2MN O5 176.01(6) 1_545 1_655 ? O4 M2MN O5 80.27(7) 2_666 1_655 ? O6 M2MN O5 93.27(6) 1_645 1_655 ? O6 M2MN O5 81.92(7) 2_665 1_655 ? O2 M2MN Na1 44.86(5) 2_666 . ? O1 M2MN Na1 83.30(5) 1_545 . ? O4 M2MN Na1 51.83(5) 2_666 . ? O6 M2MN Na1 144.14(5) 1_645 . ? O6 M2MN Na1 135.48(5) 2_665 . ? O5 M2MN Na1 94.54(5) 1_655 . ? O5 Si1 O3 115.12(9) . . ? O5 Si1 O9 112.86(9) . . ? O3 Si1 O9 105.93(9) . . ? O5 Si1 O7 110.63(9) . . ? O3 Si1 O7 107.90(10) . . ? O9 Si1 O7 103.62(9) . . ? O5 Si1 Na1 130.73(7) . . ? O3 Si1 Na1 113.76(7) . . ? O9 Si1 Na1 45.82(7) . . ? O7 Si1 Na1 58.03(7) . . ? O5 Si1 Na1 137.00(7) . 2_666 ? O3 Si1 Na1 41.82(7) . 2_666 ? O9 Si1 Na1 109.16(7) . 2_666 ? O7 Si1 Na1 66.61(7) . 2_666 ? Na1 Si1 Na1 86.11(4) . 2_666 ? O6 Si2 O4 114.31(10) . . ? O6 Si2 O9 112.01(9) . 1_565 ? O4 Si2 O9 108.82(9) . 1_565 ? O6 Si2 O8 111.13(10) . . ? O4 Si2 O8 107.16(10) . . ? O9 Si2 O8 102.67(9) 1_565 . ? O6 Si2 Na1 127.72(8) . 1_565 ? O4 Si2 Na1 117.94(8) . 1_565 ? O9 Si2 Na1 48.26(7) 1_565 1_565 ? O8 Si2 Na1 54.45(6) . 1_565 ? O6 Si2 Na1 140.47(7) . 2_666 ? O4 Si2 Na1 50.83(7) . 2_666 ? O9 Si2 Na1 107.50(7) 1_565 2_666 ? O8 Si2 Na1 57.57(7) . 2_666 ? Na1 Si2 Na1 79.42(4) 1_565 2_666 ? O1 Si3 O2 116.35(10) . 1_554 ? O1 Si3 O8 110.45(9) . . ? O2 Si3 O8 108.84(10) 1_554 . ? O1 Si3 O7 109.09(9) . . ? O2 Si3 O7 107.73(10) 1_554 . ? O8 Si3 O7 103.58(9) . . ? O1 Si3 Na1 80.99(8) . 2_665 ? O2 Si3 Na1 35.44(7) 1_554 2_665 ? O8 Si3 Na1 127.83(7) . 2_665 ? O7 Si3 Na1 120.87(8) . 2_665 ? O1 Si3 Na1 100.65(8) . 2_666 ? O2 Si3 Na1 142.70(7) 1_554 2_666 ? O8 Si3 Na1 49.39(7) . 2_666 ? O7 Si3 Na1 60.96(7) . 2_666 ? Na1 Si3 Na1 177.11(4) 2_665 2_666 ? Si3 O1 M2MN 134.41(10) . 1_565 ? Si3 O1 M1MN 125.76(10) . . ? M2MN O1 M1MN 98.41(6) 1_565 . ? Si3 O2 M2MN 124.24(10) 1_556 2_666 ? Si3 O2 Na1 120.44(10) 1_556 2_666 ? M2MN O2 Na1 92.78(7) 2_666 2_666 ? Si3 O2 M1MN 117.93(10) 1_556 2_666 ? M2MN O2 M1MN 102.45(7) 2_666 2_666 ? Na1 O2 M1MN 92.13(7) 2_666 2_666 ? Si1 O3 M1MN 135.46(10) . 2_666 ? Si1 O3 Na1 111.25(9) . 2_666 ? M1MN O3 Na1 90.88(7) 2_666 2_666 ? Si2 O4 M2MN 142.13(10) . 2_666 ? Si2 O4 Na1 99.77(9) . 2_666 ? M2MN O4 Na1 84.94(7) 2_666 2_666 ? Si1 O5 M2MN 118.81(10) . 1_455 ? Si1 O5 M1MN 113.39(9) . 2_665 ? M2MN O5 M1MN 98.90(7) 1_455 2_665 ? Si1 O5 M1MN 125.39(10) . 1_455 ? M2MN O5 M1MN 95.77(6) 1_455 1_455 ? M1MN O5 M1MN 99.85(7) 2_665 1_455 ? Si2 O6 M2MN 118.83(10) . 1_465 ? Si2 O6 M2MN 116.74(9) . 2_665 ? M2MN O6 M2MN 99.71(7) 1_465 2_665 ? Si2 O6 M1MN 122.81(10) . 1_455 ? M2MN O6 M1MN 94.62(6) 1_465 1_455 ? M2MN O6 M1MN 99.38(7) 2_665 1_455 ? Si1 O7 Si3 132.08(11) . . ? Si1 O7 Na1 89.61(8) . . ? Si3 O7 Na1 137.98(9) . . ? Si2 O8 Si3 137.17(11) . . ? Si2 O8 Na1 92.20(8) . 1_565 ? Si3 O8 Na1 123.07(9) . 1_565 ? Si2 O8 Na1 91.79(8) . 2_666 ? Si3 O8 Na1 103.14(8) . 2_666 ? Na1 O8 Na1 100.68(7) 1_565 2_666 ? Si2 O9 Si1 144.01(11) 1_545 . ? Si2 O9 Na1 99.49(9) 1_545 . ? Si1 O9 Na1 103.27(9) . . ? _refine_diff_density_max 0.768 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.177 _shelx_res_file ; TITL JG1 in P-1 NHMD01.res created by SHELXL-2016/6 at 14:11:08 on 05-Sep-2020 CELL 0.71073 7.84920 6.97520 6.91170 90.7910 94.4522 102.8488 ZERR 2.00 0.00157 0.00139 0.00138 0.0300 0.0300 0.0300 LATT 1 SFAC O H NA SI MN CA UNIT 18 2 2 6 2.1 1.9 TEMP 25 ACTA L.S. 18 BOND FMAP 2 PLAN 20 EXYZ M1MN M1CA EADP M1MN M1CA EXYZ M2MN M2CA EADP M2MN M2CA WGHT 0.115300 0.316700 BASF 0.40209 FVAR 1.13020 0.21807 0.82237 NA1 3 0.556067 0.245338 0.348798 0.98407 0.00765 0.01933 = 0.01999 -0.00108 0.00279 -0.00137 M1MN 5 0.848845 0.593819 0.146115 21.00000 0.00702 0.00711 = 0.00992 -0.00011 0.00064 0.00084 M1CA 6 0.848845 0.593819 0.146115 -21.00000 0.00702 0.00711 = 0.00992 -0.00011 0.00064 0.00084 M2MN 5 0.851825 0.084919 0.134855 31.00000 0.00670 0.00826 = 0.01182 -0.00021 0.00039 0.00154 M2CA 6 0.851825 0.084919 0.134855 -31.00000 0.00670 0.00826 = 0.01182 -0.00021 0.00039 0.00154 SI1 4 0.219656 0.406876 0.335929 11.00000 0.00551 0.00562 = 0.00816 -0.00046 -0.00053 0.00102 SI2 4 0.206842 0.960152 0.349333 11.00000 0.00521 0.00503 = 0.00921 -0.00092 -0.00069 0.00036 SI3 4 0.450723 0.746298 0.143083 11.00000 0.00414 0.00663 = 0.00852 -0.00088 -0.00006 0.00046 O1 1 0.657144 0.806314 0.122564 11.00000 0.00552 0.01096 = 0.01605 -0.00047 0.00258 0.00095 O2 1 0.325733 0.723135 0.944147 11.00000 0.00889 0.01218 = 0.00979 -0.00149 -0.00257 0.00007 O3 1 0.191210 0.509662 0.538682 11.00000 0.01219 0.01006 = 0.00907 -0.00235 0.00053 0.00386 O4 1 0.156280 0.853311 0.549726 11.00000 0.01475 0.00806 = 0.01167 0.00136 0.00359 0.00172 O5 1 0.060670 0.385114 0.171675 11.00000 0.00696 0.01218 = 0.00957 -0.00014 -0.00134 0.00186 O6 1 0.056677 0.903486 0.173193 11.00000 0.00743 0.00995 = 0.01281 -0.00151 -0.00308 0.00065 O7 1 0.403574 0.533470 0.256557 11.00000 0.00791 0.00870 = 0.01772 0.00349 0.00253 0.00088 O8 1 0.391529 0.904664 0.292516 11.00000 0.00747 0.01016 = 0.01405 -0.00411 0.00058 0.00310 O9 1 0.265284 0.196634 0.392159 11.00000 0.00871 0.00522 = 0.01353 -0.00019 -0.00080 0.00102 H1 2 0.200201 0.547039 0.631056 10.50000 10.01500 H2 2 0.153482 0.694195 0.538559 10.50000 10.01500 HKLF 5 1 0 0 -1 0 -1 0 -1 0 0 REM JG1 in P-1 REM R1 = 0.0437 for 6746 Fo > 4sig(Fo) and 0.0445 for all 7004 data REM 146 parameters refined using 0 restraints END WGHT 0.1158 0.3030 REM Highest difference peak 0.768, deepest hole -0.860, 1-sigma level 0.177 Q1 1 0.7924 0.0804 0.2013 11.00000 0.05 0.77 Q2 1 0.9034 0.0772 0.0547 11.00000 0.05 0.76 Q3 1 0.3402 0.9358 0.3466 11.00000 0.05 0.75 Q4 1 0.9124 0.6397 0.0932 11.00000 0.05 0.72 Q5 1 0.1192 0.3977 0.1031 11.00000 0.05 0.71 Q6 1 0.8260 0.0075 0.1996 11.00000 0.05 0.70 Q7 1 0.8649 0.4928 0.2472 11.00000 0.05 0.62 Q8 1 0.7984 0.5977 0.2255 11.00000 0.05 0.62 Q9 1 0.8560 0.4641 0.1513 11.00000 0.05 0.62 Q10 1 0.2377 0.2651 0.3299 11.00000 0.05 0.61 Q11 1 -0.0066 0.8404 0.2228 11.00000 0.05 0.61 Q12 1 0.2114 0.3062 0.4072 11.00000 0.05 0.58 Q13 1 0.4378 0.6191 0.2255 11.00000 0.05 0.58 Q14 1 -0.0165 0.9167 0.2797 11.00000 0.05 0.57 Q15 1 0.2670 0.9387 0.2777 11.00000 0.05 0.57 Q16 1 0.1154 0.9564 0.2535 11.00000 0.05 0.55 Q17 1 0.1707 0.9395 0.5837 11.00000 0.05 0.54 Q18 1 0.9766 0.5631 0.1528 11.00000 0.05 0.54 Q19 1 0.0836 0.8316 0.1702 11.00000 0.05 0.54 Q20 1 0.1297 0.8905 0.0464 11.00000 0.05 0.54 ; _shelx_res_checksum 45545 _shelx_hkl_file ; 1 0 0 130.769 8.63033 2 1 0 0 2107.40 139.098 -2 1 0 0 2107.40 139.098 1 1 0 0 389.486 13.6196 1 2 0 0 1104.13 33.3926 2 2 0 0 1476.10 35.0770 1 2 0 0 8253.30 538.277 -2 2 0 0 8253.30 538.277 1 3 0 0 1645.92 32.6293 1 4 0 0 4428.73 114.271 2 4 0 0 6688.50 126.971 1 5 0 0 448.203 8.51124 1 6 0 0 1395.90 34.4335 2 6 0 0 2235.75 50.8311 1 7 0 0 337.513 8.86516 2 7 0 0 560.712 12.8415 1 8 0 0 261.560 6.54146 1 9 0 0 11.4056 1.27414 1 10 0 0 1086.88 28.7697 1 11 0 0 132.967 5.13242 1 -11 1 0 1.02825 0.49591 2 -11 1 0 1.27348 0.85181 1 -10 1 0 17.6489 1.62720 1 -9 1 0 7.09332 1.05634 2 -9 1 0 3.71344 0.84655 1 -8 1 0 43.1746 2.11121 1 -8 1 0 24.8454 1.29101 2 -7 1 0 17.5767 1.02583 2 -7 1 0 30.3505 1.31918 1 -6 1 0 228.943 5.03875 1 -6 1 0 135.543 3.47861 2 -5 1 0 50.5989 1.31499 1 -5 1 0 31.0596 1.09021 2 -4 1 0 51.8295 1.43137 1 -4 1 0 32.5936 1.33134 2 -3 1 0 730.354 15.1500 1 -3 1 0 469.472 10.4476 2 -2 1 0 1598.84 39.3966 2 -2 1 0 2472.34 51.2008 1 -2 1 0 4164.87 203.113 -2 -2 1 0 4164.87 203.113 1 -1 1 0 8.49317 0.86316 2 -1 1 0 44.2179 2.38495 -2 -1 1 0 44.2179 2.38495 1 -1 1 0 26.5674 1.34109 1 0 1 0 129.712 3.43151 -2 0 1 0 129.712 3.43151 1 1 1 0 8.11825 0.57222 -2 1 1 0 8.11825 0.57222 1 1 1 0 1.88683 0.11911 2 1 1 0 3.65356 0.20286 1 2 1 0 2682.78 84.6598 1 2 1 0 931.702 61.4055 2 3 1 0 181.310 4.54818 1 3 1 0 319.166 14.2974 -2 3 1 0 319.166 14.2974 1 3 1 0 134.572 4.20060 2 4 1 0 1133.26 23.6830 1 5 1 0 153.466 3.20034 1 6 1 0 221.345 5.55554 2 6 1 0 363.887 8.00528 1 7 1 0 16.3888 0.95856 2 7 1 0 29.5699 1.26950 1 8 1 0 273.033 7.43622 2 8 1 0 443.521 10.4559 1 9 1 0 68.7280 2.90787 1 10 1 0 22.8376 1.71944 1 10 1 0 13.4372 1.19627 2 11 1 0 1.41497 1.24361 1 11 1 0 3.39055 1.16207 2 -11 2 0 29.3630 2.26400 1 -11 2 0 17.4763 1.39609 2 -10 2 0 1.53813 0.50952 2 -10 2 0 1.35799 0.77897 1 -9 2 0 551.192 15.2786 1 -8 2 0 443.704 12.3570 1 -7 2 0 283.750 8.15414 1 -6 2 0 137.412 4.04851 2 -6 2 0 241.923 6.05617 1 -5 2 0 97.0391 2.95152 2 -5 2 0 176.719 4.20040 1 -4 2 0 609.991 13.2069 1 -4 2 0 349.133 9.19965 2 -3 2 0 788.116 38.8671 2 -3 2 0 426.260 9.81359 1 -2 2 0 392.562 10.1284 1 -2 2 0 212.270 6.50543 2 -2 2 0 591.353 29.0570 -2 -2 2 0 591.353 29.0570 1 -1 2 0 342.673 8.05066 -2 -1 2 0 342.673 8.05066 1 -1 2 0 97.1176 6.79368 2 -1 2 0 188.493 12.3989 1 0 2 0 551.969 10.3018 -2 0 2 0 551.969 10.3018 1 1 2 0 174.928 11.4557 1 1 2 0 113.137 7.63751 2 1 2 0 275.154 5.94110 -2 1 2 0 275.154 5.94110 1 2 2 0 2086.17 96.6356 2 2 2 0 3986.23 113.183 1 3 2 0 1085.34 24.1796 1 3 2 0 1890.17 82.5769 -2 3 2 0 1890.17 82.5769 1 3 2 0 796.076 23.6486 2 4 2 0 1234.64 24.6171 1 4 2 0 899.477 22.1291 2 5 2 0 3.52353 0.35262 2 5 2 0 4.11471 0.42812 1 6 2 0 781.534 18.2137 2 6 2 0 1188.23 22.4960 1 7 2 0 191.369 5.31324 2 7 2 0 286.561 6.54565 1 8 2 0 276.104 8.07311 1 9 2 0 97.0363 3.64222 1 10 2 0 171.416 7.73932 1 11 2 0 4.98743 1.25979 2 11 2 0 2.65814 1.36662 1 -11 3 0 -0.0402 0.44631 2 -11 3 0 0.23367 0.77763 1 -10 3 0 78.5552 3.79413 1 -10 3 0 39.1465 2.11149 2 -9 3 0 13.4404 1.37999 1 -8 3 0 12.2869 1.24867 1 -7 3 0 66.3922 2.37891 2 -7 3 0 121.195 4.04369 1 -6 3 0 59.2555 1.97102 1 -6 3 0 34.9976 1.49053 2 -5 3 0 72.9016 2.40363 2 -5 3 0 123.890 3.34901 1 -4 3 0 1146.06 56.5362 2 -4 3 0 569.094 12.4820 1 -3 3 0 784.294 21.2499 1 -3 3 0 408.592 13.5950 2 -3 3 0 1288.03 53.0951 -2 -3 3 0 1288.03 53.0951 1 -2 3 0 801.111 20.3775 -2 -2 3 0 801.111 20.3775 1 -2 3 0 467.260 14.4687 1 -1 3 0 214.293 4.52872 -2 -1 3 0 214.293 4.52872 1 0 3 0 545.464 8.81048 -2 0 3 0 545.464 8.81048 1 1 3 0 527.872 34.5419 2 1 3 0 1049.73 19.6283 -2 1 3 0 1049.73 19.6283 1 1 3 0 677.850 44.6766 1 2 3 0 1191.44 36.8233 2 2 3 0 3048.38 82.5362 -2 2 3 0 3048.38 82.5362 1 2 3 0 1838.55 48.0450 1 3 3 0 5.47497 0.33850 1 3 3 0 8.12651 1.15807 -2 3 3 0 8.12651 1.15807 1 3 3 0 3.68950 0.25805 2 4 3 0 1.12653 0.17932 2 4 3 0 1.43162 0.23405 1 5 3 0 130.930 3.38306 2 5 3 0 173.247 4.14398 1 6 3 0 1289.52 27.1619 1 6 3 0 919.910 21.3489 2 7 3 0 39.7908 1.55182 1 7 3 0 33.7159 1.46198 2 8 3 0 1.11336 0.38160 2 8 3 0 1.20848 0.58783 1 9 3 0 31.1395 2.74932 1 10 3 0 309.882 12.2573 1 -10 4 0 21.6894 1.57539 2 -10 4 0 47.3932 2.84578 1 -9 4 0 64.7450 2.58815 2 -9 4 0 137.733 5.47721 1 -8 4 0 241.343 8.05137 2 -8 4 0 475.853 12.9345 1 -7 4 0 864.427 18.2211 1 -6 4 0 1097.47 22.8162 1 -6 4 0 576.390 15.1790 2 -5 4 0 2.19925 0.31815 2 -5 4 0 1.64249 0.31197 1 -4 4 0 25.5404 0.91609 1 -4 4 0 43.6454 3.25820 2 -3 4 0 1140.21 30.7510 1 -3 4 0 1803.36 56.7090 -2 -3 4 0 1803.36 56.7090 1 -3 4 0 500.905 14.9516 2 -2 4 0 3176.48 209.351 2 -2 4 0 9999.99 223.872 -2 -2 4 0 9999.99 223.872 1 -2 4 0 7034.65 343.184 1 -1 4 0 240.236 4.72490 -2 -1 4 0 240.236 4.72490 1 0 4 0 176.760 3.48065 -2 0 4 0 176.760 3.48065 1 1 4 0 549.278 9.50688 -2 1 4 0 549.278 9.50688 1 2 4 0 4909.59 108.072 -2 2 4 0 4909.59 108.072 1 2 4 0 2873.25 72.2592 1 2 4 0 2070.35 52.2857 2 3 4 0 131.672 3.17669 2 3 4 0 192.933 4.22780 1 3 4 0 301.683 9.04186 -2 3 4 0 301.683 9.04186 1 4 4 0 288.740 6.27570 2 4 4 0 403.260 7.76363 1 5 4 0 24.5706 0.92012 2 5 4 0 30.8102 1.29836 1 6 4 0 116.045 3.65183 2 6 4 0 148.970 4.38279 1 7 4 0 3.43290 0.82239 1 7 4 0 3.62212 0.43603 2 8 4 0 151.229 5.78624 2 8 4 0 190.693 6.55738 1 9 4 0 92.3077 4.89560 1 10 4 0 67.4319 4.24921 1 -10 5 0 1.45405 0.89531 1 -10 5 0 0.76338 0.52404 2 -9 5 0 6.30720 0.81685 2 -9 5 0 13.9002 1.26874 1 -8 5 0 3.86616 0.68219 2 -8 5 0 9.31766 1.02472 1 -7 5 0 40.0480 1.60672 2 -7 5 0 80.2316 2.53578 1 -6 5 0 171.428 5.07920 2 -6 5 0 328.011 8.00366 1 -5 5 0 138.796 3.70715 1 -5 5 0 69.4309 2.19861 2 -4 5 0 44.7014 1.99102 2 -4 5 0 130.696 6.34035 -2 -4 5 0 130.696 6.34035 1 -4 5 0 91.6996 3.05984 1 -3 5 0 403.096 9.48799 -2 -3 5 0 403.096 9.48799 1 -2 5 0 115.874 2.79515 -2 -2 5 0 115.874 2.79515 1 -2 5 0 61.6204 4.67290 1 -2 5 0 40.6963 4.20506 2 -1 5 0 847.183 18.1663 -2 -1 5 0 847.183 18.1663 1 0 5 0 84.9063 1.94255 -2 0 5 0 84.9063 1.94255 1 1 5 0 24.7188 0.64527 -2 1 5 0 24.7188 0.64527 1 2 5 0 101.043 2.17657 -2 2 5 0 101.043 2.17657 1 2 5 0 67.1383 5.08656 1 2 5 0 48.9262 4.07748 2 3 5 0 230.361 10.9216 -2 3 5 0 230.361 10.9216 1 3 5 0 140.599 3.67339 1 3 5 0 100.586 2.98639 2 4 5 0 736.746 15.3803 1 4 5 0 551.721 12.6101 2 5 5 0 0.39472 0.42964 1 5 5 0 0.98273 0.23628 2 6 5 0 76.6391 3.78543 2 6 5 0 99.8920 4.23804 1 7 5 0 22.9932 2.59076 1 8 5 0 13.6784 1.71013 1 8 5 0 13.4939 1.97221 2 9 5 0 49.2298 2.88520 2 9 5 0 62.3520 3.94139 1 10 5 0 32.5230 2.99541 1 10 5 0 24.7425 3.33343 2 -9 6 0 13.4503 1.18456 2 -9 6 0 28.1068 1.77499 1 -8 6 0 24.2057 1.57213 1 -8 6 0 10.4046 1.00821 2 -7 6 0 497.466 11.9563 1 -7 6 0 246.582 6.41094 2 -6 6 0 365.409 9.02110 2 -6 6 0 715.385 16.7029 1 -5 6 0 301.444 7.42811 1 -5 6 0 152.065 4.16642 2 -4 6 0 798.455 20.6829 2 -4 6 0 1540.31 39.2680 1 -4 6 0 2296.37 112.250 -2 -4 6 0 2296.37 112.250 1 -3 6 0 25.0971 1.48218 -2 -3 6 0 25.0971 1.48218 1 -3 6 0 16.8647 1.65750 1 -3 6 0 8.32836 0.92367 2 -2 6 0 672.172 15.5020 -2 -2 6 0 672.172 15.5020 1 -1 6 0 1396.87 27.0093 -2 -1 6 0 1396.87 27.0093 1 0 6 0 5648.34 100.265 -2 0 6 0 5648.34 100.265 1 1 6 0 1194.88 21.3429 -2 1 6 0 1194.88 21.3429 1 2 6 0 1069.22 23.9856 -2 2 6 0 1069.22 23.9856 1 3 6 0 914.920 25.6824 1 3 6 0 611.443 17.6359 2 3 6 0 1412.31 61.8301 -2 3 6 0 1412.31 61.8301 1 4 6 0 1890.79 47.6572 1 4 6 0 1383.32 40.5161 2 5 6 0 54.8186 2.79398 1 5 6 0 47.4931 2.60680 2 6 6 0 909.821 27.9022 1 6 6 0 713.767 26.7221 2 7 6 0 199.777 10.1725 2 7 6 0 242.340 10.2766 1 8 6 0 191.737 10.1168 2 8 6 0 238.769 10.4312 1 9 6 0 88.6396 4.18019 2 9 6 0 107.790 4.67674 1 -9 7 0 2.04400 0.65165 2 -9 7 0 2.22803 0.73162 1 -8 7 0 47.0881 2.15658 2 -8 7 0 97.6972 3.64989 1 -7 7 0 16.1892 1.12198 2 -7 7 0 26.0821 1.39605 1 -6 7 0 86.1197 2.77070 1 -6 7 0 43.8166 1.78853 2 -5 7 0 39.2955 1.60676 1 -5 7 0 22.1522 1.21237 2 -4 7 0 380.021 20.2559 -2 -4 7 0 380.021 20.2559 1 -4 7 0 235.877 6.79989 1 -4 7 0 129.047 4.05300 2 -3 7 0 122.779 3.48965 -2 -3 7 0 122.779 3.48965 1 -2 7 0 1062.65 24.2622 -2 -2 7 0 1062.65 24.2622 1 -1 7 0 225.605 5.79273 -2 -1 7 0 225.605 5.79273 1 0 7 0 82.3598 2.45712 -2 0 7 0 82.3598 2.45712 1 1 7 0 90.5691 2.63443 -2 1 7 0 90.5691 2.63443 1 2 7 0 740.064 20.6081 -2 2 7 0 740.064 20.6081 1 3 7 0 48.5237 3.07746 1 3 7 0 38.6486 2.47944 2 3 7 0 80.1549 3.61418 -2 3 7 0 80.1549 3.61418 1 4 7 0 671.167 17.6726 1 4 7 0 489.150 14.9701 2 5 7 0 17.4286 1.25470 2 5 7 0 17.8999 1.62866 1 6 7 0 157.257 7.31473 1 6 7 0 126.384 6.88762 2 7 7 0 11.7939 2.19581 1 7 7 0 11.2850 1.79557 2 8 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100.156 3.82345 1 -6 9 0 54.0839 2.67807 2 -5 9 0 308.187 14.3355 -2 -5 9 0 308.187 14.3355 1 -5 9 0 207.799 8.58037 1 -5 9 0 113.365 6.18016 2 -4 9 0 5.87993 1.54400 -2 -4 9 0 5.87993 1.54400 1 -3 9 0 11.4806 1.53278 -2 -3 9 0 11.4806 1.53278 1 -2 9 0 10.0338 1.38058 -2 -2 9 0 10.0338 1.38058 1 -1 9 0 252.548 6.52649 -2 -1 9 0 252.548 6.52649 1 0 9 0 503.423 12.1277 -2 0 9 0 503.423 12.1277 1 1 9 0 257.086 8.05381 -2 1 9 0 257.086 8.05381 1 2 9 0 25.0162 1.85284 -2 2 9 0 25.0162 1.85284 1 3 9 0 34.2186 3.74253 1 3 9 0 22.0202 2.98325 2 3 9 0 57.6984 3.38199 -2 3 9 0 57.6984 3.38199 1 4 9 0 169.031 6.73069 2 4 9 0 223.299 7.99740 1 5 9 0 114.671 4.96861 1 5 9 0 95.5844 4.38773 2 6 9 0 46.7256 3.66965 1 6 9 0 37.1731 2.46587 2 -5 10 0 51.1532 3.35904 -2 -5 10 0 51.1532 3.35904 1 -5 10 0 17.3346 3.73848 2 -5 10 0 33.2832 3.58105 1 -4 10 0 64.9155 3.17971 -2 -4 10 0 64.9155 3.17971 1 -3 10 0 617.614 17.5213 -2 -3 10 0 617.614 17.5213 1 -2 10 0 325.274 8.32253 -2 -2 10 0 325.274 8.32253 1 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164.131 5.08613 1 -6 -2 9 97.4016 3.50494 2 -5 -2 9 86.9852 2.54665 2 -5 -2 9 126.588 3.91890 1 -4 -2 9 253.288 5.53446 2 -4 -2 9 369.181 8.09348 1 -3 -2 9 1351.70 32.0156 2 -3 -2 9 1934.13 41.5005 1 -2 -2 9 1.88362 0.29479 2 -2 -2 9 1.16561 0.41434 1 -1 -2 9 955.477 20.8629 1 -1 -2 9 665.608 15.2495 2 0 -2 9 1013.71 22.0970 1 0 -2 9 683.006 15.6713 2 1 -2 9 483.796 11.2982 2 1 -2 9 721.706 15.9939 1 2 -2 9 56.6738 1.73651 2 2 -2 9 76.3034 2.57560 1 3 -2 9 694.768 16.7245 1 3 -2 9 492.167 11.5785 2 4 -2 9 138.538 3.79680 2 4 -2 9 192.657 5.53989 1 5 -2 9 69.1883 2.61868 1 5 -2 9 49.9316 1.83857 2 6 -2 9 1.57071 0.62114 2 6 -2 9 1.89467 0.71094 1 7 -2 9 426.718 12.2340 2 7 -2 9 571.008 16.3397 1 -8 -1 9 178.251 6.66223 2 -8 -1 9 209.610 8.32852 1 -7 -1 9 94.2247 3.79177 2 -7 -1 9 129.184 5.62182 1 -6 -1 9 27.2900 1.53290 2 -6 -1 9 42.5356 2.24871 1 -5 -1 9 60.8971 1.94490 1 -5 -1 9 40.0659 1.30385 2 -4 -1 9 130.503 3.12905 2 -4 -1 9 202.328 4.79845 1 -3 -1 9 2.62974 0.58446 1 -3 -1 9 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