data_wmuk _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 'Al0.50 H2 Ca Fe3 Mg Mn O31 Si8 Ti0.50' _chemical_formula_weight 1047.06 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' 'Mg' 'Mg' 0.0486 0.0363 '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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 2/m' _space_group_name_Hall '-C 2y' _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' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.759(3) _cell_length_b 17.911(4) _cell_length_c 5.2740(11) _cell_angle_alpha 90 _cell_angle_beta 106.44(3) _cell_angle_gamma 90 _cell_volume 1246.6(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_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.790 _exptl_crystal_F_000 1029 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 3.125 _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 293(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 4430 _diffrn_reflns_av_unetI/netI 0.0297 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.274 _diffrn_reflns_theta_max 25.113 _diffrn_reflns_theta_full 25.113 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 1158 _reflns_number_gt 902 _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 ? _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 ? _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^)+(0.0432P)^2^+8.1720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1158 _refine_ls_number_parameters 114 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 Fe1 Fe 0.500000 0.41482(5) 0.000000 0.0141(4) Uani 0.927(5) 2 d S T . . . Mn1 Mn 0.500000 0.32016(6) 0.500000 0.0176(5) Uani 0.761(10) 2 d S T P . . Mg1 Mg 0.500000 0.32016(6) 0.500000 0.0176(5) Uani 0.239(10) 2 d S T P . . Ca1 Ca 0.500000 0.500000 0.500000 0.016(2) Uani 0.310(9) 4 d S T . . . Si1 Si 0.29185(10) 0.41475(6) -0.4735(3) 0.0141(4) Uani 1 1 d . . . . . Si2 Si 0.29111(10) 0.33414(7) 0.0234(2) 0.0145(4) Uani 1 1 d . . . . . O1 O 0.250000 0.250000 0.000000 0.0234(12) Uani 1 2 d S . P . . O2 O 0.2519(4) 0.500000 -0.4983(9) 0.0210(11) Uani 1 2 d S T P . . O3 O 0.4126(3) 0.33818(17) 0.1123(6) 0.0180(8) Uani 1 1 d . . . . . O4 O 0.4223(4) 0.500000 0.0941(10) 0.0192(11) Uani 1 2 d DS T P . . H4 H 0.4965(4) 0.500000 0.15(2) 0.08(4) Uiso 1 2 d DS . P . . O5 O 0.4138(3) 0.40880(17) -0.3778(6) 0.0189(8) Uani 1 1 d . . . . . O6 O 0.2462(2) 0.37649(18) -0.7604(6) 0.0191(8) Uani 1 1 d . . . . . O7 O 0.2430(2) 0.37297(18) -0.2643(6) 0.0194(8) Uani 1 1 d . . . . . O8 O 0.4080(4) 0.2393(3) 0.5942(9) 0.0485(12) Uani 1 1 d . . . . . OW1 O 0.4264(11) 0.000000 1.199(3) 0.157(6) Uani 1 2 d S T P . . OW2 O 0.500000 0.1415(6) 1.000000 0.098(3) Uani 1 2 d S T 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 Fe1 0.0218(7) 0.0148(6) 0.0058(6) 0.000 0.0043(5) 0.000 Mn1 0.0241(8) 0.0219(7) 0.0057(7) 0.000 0.0025(5) 0.000 Mg1 0.0241(8) 0.0219(7) 0.0057(7) 0.000 0.0025(5) 0.000 Ca1 0.018(4) 0.021(4) 0.011(4) 0.000 0.008(3) 0.000 Si1 0.0218(8) 0.0137(6) 0.0075(7) -0.0005(5) 0.0052(6) -0.0008(5) Si2 0.0240(8) 0.0133(7) 0.0067(7) -0.0003(5) 0.0052(6) -0.0019(5) O1 0.035(3) 0.015(2) 0.021(3) -0.0025(19) 0.009(2) -0.007(2) O2 0.028(3) 0.017(2) 0.017(3) 0.000 0.005(2) 0.000 O3 0.0255(19) 0.0178(16) 0.0124(17) 0.0017(13) 0.0083(15) -0.0014(14) O4 0.021(3) 0.017(2) 0.024(3) 0.000 0.013(2) 0.000 O5 0.026(2) 0.0204(17) 0.0093(17) -0.0013(13) 0.0037(15) 0.0007(14) O6 0.0258(18) 0.0223(18) 0.0091(16) -0.0053(13) 0.0048(14) -0.0018(14) O7 0.0269(18) 0.0222(18) 0.0090(16) 0.0036(13) 0.0050(14) -0.0009(14) O8 0.058(3) 0.056(3) 0.030(3) -0.004(2) 0.010(2) -0.010(2) OW1 0.161(12) 0.120(10) 0.232(17) 0.000 0.126(12) 0.000 OW2 0.073(6) 0.128(8) 0.083(7) 0.000 0.006(5) 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 Fe1 O4 2.004(3) . ? Fe1 O4 2.004(3) 5_665 ? Fe1 O5 2.013(3) 2_655 ? Fe1 O5 2.013(3) . ? Fe1 O3 2.021(3) . ? Fe1 O3 2.021(3) 2_655 ? Fe1 Ca1 3.0465(7) . ? Fe1 Ca1 3.0465(7) 1_554 ? Mn1 O8 2.074(5) . ? Mn1 O8 2.074(5) 2_656 ? Mn1 O3 2.083(3) . ? Mn1 O3 2.083(3) 2_656 ? Mn1 O5 2.185(3) 2_655 ? Mn1 O5 2.185(3) 1_556 ? Mn1 Ca1 3.2211(13) . ? Ca1 O4 2.105(5) . ? Ca1 O4 2.105(5) 5_666 ? Ca1 O5 2.218(3) 5_665 ? Ca1 O5 2.218(3) 1_556 ? Ca1 O5 2.218(3) 6_566 ? Ca1 O5 2.218(3) 2_655 ? Si1 O5 1.614(4) . ? Si1 O2 1.6155(19) . ? Si1 O6 1.617(3) . ? Si1 O7 1.628(3) . ? Si2 O1 1.6021(12) . ? Si2 O3 1.605(4) . ? Si2 O6 1.630(3) 1_556 ? Si2 O7 1.630(3) . ? 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 Fe1 O4 80.8(2) . 5_665 ? O4 Fe1 O5 90.10(17) . 2_655 ? O4 Fe1 O5 94.58(17) 5_665 2_655 ? O4 Fe1 O5 94.58(17) . . ? O4 Fe1 O5 90.10(17) 5_665 . ? O5 Fe1 O5 173.86(18) 2_655 . ? O4 Fe1 O3 92.37(14) . . ? O4 Fe1 O3 173.17(14) 5_665 . ? O5 Fe1 O3 84.60(13) 2_655 . ? O5 Fe1 O3 91.22(13) . . ? O4 Fe1 O3 173.17(14) . 2_655 ? O4 Fe1 O3 92.37(14) 5_665 2_655 ? O5 Fe1 O3 91.22(13) 2_655 2_655 ? O5 Fe1 O3 84.61(13) . 2_655 ? O3 Fe1 O3 94.42(19) . 2_655 ? O4 Fe1 Ca1 43.44(14) . . ? O4 Fe1 Ca1 87.92(13) 5_665 . ? O5 Fe1 Ca1 46.70(9) 2_655 . ? O5 Fe1 Ca1 137.69(10) . . ? O3 Fe1 Ca1 86.60(9) . . ? O3 Fe1 Ca1 137.70(9) 2_655 . ? O4 Fe1 Ca1 87.92(13) . 1_554 ? O4 Fe1 Ca1 43.44(14) 5_665 1_554 ? O5 Fe1 Ca1 137.69(10) 2_655 1_554 ? O5 Fe1 Ca1 46.69(9) . 1_554 ? O3 Fe1 Ca1 137.70(9) . 1_554 ? O3 Fe1 Ca1 86.60(9) 2_655 1_554 ? Ca1 Fe1 Ca1 119.90(3) . 1_554 ? O8 Mn1 O8 91.4(3) . 2_656 ? O8 Mn1 O3 96.99(15) . . ? O8 Mn1 O3 95.44(15) 2_656 . ? O8 Mn1 O3 95.44(15) . 2_656 ? O8 Mn1 O3 96.99(15) 2_656 2_656 ? O3 Mn1 O3 162.17(18) . 2_656 ? O8 Mn1 O5 175.46(15) . 2_655 ? O8 Mn1 O5 91.05(17) 2_656 2_655 ? O3 Mn1 O5 78.96(12) . 2_655 ? O3 Mn1 O5 88.07(13) 2_656 2_655 ? O8 Mn1 O5 91.04(17) . 1_556 ? O8 Mn1 O5 175.46(16) 2_656 1_556 ? O3 Mn1 O5 88.07(13) . 1_556 ? O3 Mn1 O5 78.96(12) 2_656 1_556 ? O5 Mn1 O5 86.79(18) 2_655 1_556 ? O8 Mn1 Ca1 134.30(14) . . ? O8 Mn1 Ca1 134.30(14) 2_656 . ? O3 Mn1 Ca1 81.09(9) . . ? O3 Mn1 Ca1 81.09(9) 2_656 . ? O5 Mn1 Ca1 43.39(9) 2_655 . ? O5 Mn1 Ca1 43.39(9) 1_556 . ? O4 Ca1 O4 180.0 . 5_666 ? O4 Ca1 O5 82.17(12) . 5_665 ? O4 Ca1 O5 97.83(12) 5_666 5_665 ? O4 Ca1 O5 97.83(12) . 1_556 ? O4 Ca1 O5 82.17(12) 5_666 1_556 ? O5 Ca1 O5 180.0 5_665 1_556 ? O4 Ca1 O5 97.83(12) . 6_566 ? O4 Ca1 O5 82.17(12) 5_666 6_566 ? O5 Ca1 O5 85.15(17) 5_665 6_566 ? O5 Ca1 O5 94.85(17) 1_556 6_566 ? O4 Ca1 O5 82.17(12) . 2_655 ? O4 Ca1 O5 97.83(12) 5_666 2_655 ? O5 Ca1 O5 94.85(17) 5_665 2_655 ? O5 Ca1 O5 85.15(17) 1_556 2_655 ? O5 Ca1 O5 180.00(15) 6_566 2_655 ? O4 Ca1 Fe1 40.89(8) . . ? O4 Ca1 Fe1 139.11(8) 5_666 . ? O5 Ca1 Fe1 89.23(8) 5_665 . ? O5 Ca1 Fe1 90.77(8) 1_556 . ? O5 Ca1 Fe1 138.68(8) 6_566 . ? O5 Ca1 Fe1 41.32(8) 2_655 . ? O4 Ca1 Fe1 139.11(8) . 5_666 ? O4 Ca1 Fe1 40.89(8) 5_666 5_666 ? O5 Ca1 Fe1 90.77(8) 5_665 5_666 ? O5 Ca1 Fe1 89.23(8) 1_556 5_666 ? O5 Ca1 Fe1 41.32(8) 6_566 5_666 ? O5 Ca1 Fe1 138.68(8) 2_655 5_666 ? Fe1 Ca1 Fe1 180.0 . 5_666 ? O4 Ca1 Fe1 139.11(8) . 1_556 ? O4 Ca1 Fe1 40.89(8) 5_666 1_556 ? O5 Ca1 Fe1 138.68(8) 5_665 1_556 ? O5 Ca1 Fe1 41.32(8) 1_556 1_556 ? O5 Ca1 Fe1 89.23(8) 6_566 1_556 ? O5 Ca1 Fe1 90.77(8) 2_655 1_556 ? Fe1 Ca1 Fe1 119.90(3) . 1_556 ? Fe1 Ca1 Fe1 60.11(3) 5_666 1_556 ? O4 Ca1 Fe1 40.89(8) . 5_665 ? O4 Ca1 Fe1 139.11(8) 5_666 5_665 ? O5 Ca1 Fe1 41.32(8) 5_665 5_665 ? O5 Ca1 Fe1 138.68(9) 1_556 5_665 ? O5 Ca1 Fe1 90.77(8) 6_566 5_665 ? O5 Ca1 Fe1 89.23(8) 2_655 5_665 ? Fe1 Ca1 Fe1 60.10(3) . 5_665 ? Fe1 Ca1 Fe1 119.89(3) 5_666 5_665 ? Fe1 Ca1 Fe1 180.0 1_556 5_665 ? O4 Ca1 Mn1 90.0 . . ? O4 Ca1 Mn1 90.0 5_666 . ? O5 Ca1 Mn1 137.42(8) 5_665 . ? O5 Ca1 Mn1 42.58(8) 1_556 . ? O5 Ca1 Mn1 137.42(8) 6_566 . ? O5 Ca1 Mn1 42.58(8) 2_655 . ? Fe1 Ca1 Mn1 59.948(17) . . ? Fe1 Ca1 Mn1 120.053(17) 5_666 . ? Fe1 Ca1 Mn1 59.947(17) 1_556 . ? Fe1 Ca1 Mn1 120.053(17) 5_665 . ? O5 Si1 O2 112.8(2) . . ? O5 Si1 O6 111.02(18) . . ? O2 Si1 O6 107.0(2) . . ? O5 Si1 O7 110.51(18) . . ? O2 Si1 O7 107.0(2) . . ? O6 Si1 O7 108.30(17) . . ? O5 Si1 Ca1 37.00(12) . 1_554 ? O2 Si1 Ca1 80.67(17) . 1_554 ? O6 Si1 Ca1 105.64(13) . 1_554 ? O7 Si1 Ca1 140.83(13) . 1_554 ? O1 Si2 O3 112.39(14) . . ? O1 Si2 O6 107.24(14) . 1_556 ? O3 Si2 O6 110.15(18) . 1_556 ? O1 Si2 O7 106.75(13) . . ? O3 Si2 O7 111.59(18) . . ? O6 Si2 O7 108.54(17) 1_556 . ? Si2 O1 Si2 180.00(3) . 7 ? Si1 O2 Si1 141.9(3) . 6_565 ? Si2 O3 Fe1 127.01(19) . . ? Si2 O3 Mn1 122.94(18) . . ? Fe1 O3 Mn1 99.61(14) . . ? Fe1 O4 Fe1 99.2(2) . 5_665 ? Fe1 O4 Ca1 95.68(16) . . ? Fe1 O4 Ca1 95.68(16) 5_665 . ? Si1 O5 Fe1 125.1(2) . . ? Si1 O5 Mn1 123.98(18) . 1_554 ? Fe1 O5 Mn1 96.56(13) . 1_554 ? Si1 O5 Ca1 117.04(17) . 1_554 ? Fe1 O5 Ca1 91.99(13) . 1_554 ? Mn1 O5 Ca1 94.03(13) 1_554 1_554 ? Si1 O6 Si2 136.7(2) . 1_554 ? Si1 O7 Si2 133.7(2) . . ? _refine_diff_density_max 0.599 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.122 _shelx_res_file ; TITL wmuk in C2/m wmuk.res created by SHELXL-2016/6 at 11:54:14 on 01-May-2019 CELL 0.71073 13.7590 17.9110 5.2740 90.000 106.440 90.000 ZERR 2.00 0.0028 0.0036 0.0011 0.000 0.030 0.000 LATT 7 SYMM -X, Y, -Z SFAC O MG SI MN FE CA H TI Al UNIT 62 2 16 2 6 2 4 1 1 L.S. 10 BOND FMAP 2 PLAN 20 EADP FE1 EXYZ FE1 EADP MN1 MG1 EXYZ MN1 MG1 ACTA WGHT 0.043200 8.172000 FVAR 0.32153 0.76110 0.62688 MOLE 1 FE1 5 0.500000 0.414821 0.000000 0.46368 0.02179 0.01484 = 0.00578 0.00000 0.00432 0.00000 MN1 4 0.500000 0.320163 0.500000 20.50000 0.02415 0.02193 = 0.00568 0.00000 0.00249 0.00000 MG1 2 0.500000 0.320163 0.500000 -20.50000 0.02415 0.02193 = 0.00568 0.00000 0.00249 0.00000 CA1 6 0.500000 0.500000 0.500000 0.07746 0.01843 0.02058 = 0.01100 0.00000 0.00761 0.00000 SI1 3 0.291852 0.414749 -0.473530 11.00000 0.02175 0.01367 = 0.00747 -0.00050 0.00524 -0.00082 SI2 3 0.291114 0.334136 0.023417 11.00000 0.02404 0.01333 = 0.00674 -0.00029 0.00518 -0.00186 O1 1 0.250000 0.250000 0.000000 10.50000 0.03470 0.01530 = 0.02080 -0.00247 0.00882 -0.00747 O2 1 0.251911 0.500000 -0.498291 10.50000 0.02838 0.01679 = 0.01681 0.00000 0.00490 0.00000 O3 1 0.412623 0.338182 0.112297 11.00000 0.02548 0.01781 = 0.01245 0.00172 0.00831 -0.00142 O4 1 0.422326 0.500000 0.094051 10.50000 0.02062 0.01728 = 0.02356 0.00000 0.01255 0.00000 H4 7 0.496546 0.500000 0.154991 10.50000 0.08121 dfix 0.98 0.001 H4 O4 O5 1 0.413841 0.408800 -0.377849 11.00000 0.02621 0.02038 = 0.00929 -0.00131 0.00368 0.00070 O6 1 0.246217 0.376486 -0.760423 11.00000 0.02578 0.02233 = 0.00911 -0.00534 0.00480 -0.00183 O7 1 0.242977 0.372972 -0.264254 11.00000 0.02687 0.02218 = 0.00903 0.00355 0.00496 -0.00087 O8 1 0.408043 0.239275 0.594214 11.00000 0.05806 0.05613 = 0.03000 -0.00395 0.01032 -0.00970 OW1 1 0.426381 0.000000 1.199497 10.50000 0.16052 0.11997 = 0.23232 0.00000 0.12581 0.00000 OW2 1 0.500000 0.141514 1.000000 10.50000 0.07264 0.12826 = 0.08304 0.00000 0.00640 0.00000 HKLF 4 REM wmuk in C2/m REM R1 = 0.0401 for 902 Fo > 4sig(Fo) and 0.0586 for all 1158 data REM 114 parameters refined using 1 restraints END WGHT 0.0432 8.1656 REM Highest difference peak 0.599, deepest hole -0.494, 1-sigma level 0.122 Q1 1 0.4203 0.4010 -0.0544 11.00000 0.05 0.60 Q2 1 0.3634 0.4268 -0.4236 11.00000 0.05 0.54 Q3 1 0.4304 0.3195 0.4825 11.00000 0.05 0.53 Q4 1 0.4194 0.5000 0.2632 10.50000 0.05 0.52 Q5 1 0.3636 0.3348 0.0662 11.00000 0.05 0.45 Q6 1 0.2127 0.4116 -0.5191 11.00000 0.05 0.44 Q7 1 0.3856 0.0000 1.0940 10.50000 0.05 0.43 Q8 1 0.3851 0.5000 0.0542 10.50000 0.05 0.43 Q9 1 0.5000 0.1678 0.5000 10.50000 0.05 0.43 Q10 1 0.4389 0.4412 -0.0134 11.00000 0.05 0.42 Q11 1 0.5000 0.2423 1.0000 10.50000 0.05 0.40 Q12 1 0.2978 0.0000 1.0505 10.50000 0.05 0.39 Q13 1 0.4318 0.2023 0.7094 11.00000 0.05 0.39 Q14 1 0.2117 0.3134 -0.0121 11.00000 0.05 0.39 Q15 1 0.5000 0.5000 0.0000 10.25000 0.05 0.36 Q16 1 0.3148 0.5000 -0.0753 10.50000 0.05 0.35 Q17 1 0.5000 -0.0345 1.5000 10.50000 0.05 0.35 Q18 1 0.3482 0.2088 0.4623 11.00000 0.05 0.34 Q19 1 0.1557 0.4736 -0.4693 11.00000 0.05 0.33 Q20 1 0.4467 0.0558 1.2882 11.00000 0.05 0.32 ; _shelx_res_checksum 33086 _shelx_hkl_file ; -2 0 0 12.35 2.08 2 0 0 20.40 2.32 -4 0 0 9715.35 184.62 4 0 0 9261.93 238.71 -6 0 0 1023.27 21.94 6 0 0 977.71 27.55 -8 0 0 1123.49 23.97 8 0 0 1074.42 26.21 -10 0 0 2410.30 54.14 10 0 0 2327.25 62.43 -12 0 0 601.69 20.07 12 0 0 635.20 23.53 -14 0 0 911.64 26.50 14 0 0 906.80 31.27 -3 -1 0 9.33 3.20 3 -1 0 3.24 4.00 -3 1 0 9.68 3.15 3 1 0 19.14 4.09 -5 -1 0 1062.51 23.25 5 -1 0 1050.10 29.07 -5 1 0 1119.15 25.40 5 1 0 992.22 35.97 -7 -1 0 159.78 6.56 7 -1 0 158.47 8.45 -7 1 0 156.60 7.57 7 1 0 162.31 7.98 -9 -1 0 1118.48 24.48 9 -1 0 1077.46 31.69 -9 1 0 1140.19 27.81 9 1 0 1090.82 31.22 -11 -1 0 411.46 14.39 11 -1 0 469.14 19.54 -11 1 0 420.27 16.70 11 1 0 441.32 19.26 -13 -1 0 164.08 11.63 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