data_pararaisaite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'pararaisaite' _chemical_compound_source 'North Star mine, Utah' _chemical_formula_sum 'Cu1.90 H28 Mg2.15 O24 Te1.95' _chemical_formula_weight 834.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'Te' 'Te' -0.5308 1.6751 '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' '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 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6838(5) _cell_length_b 5.75175(19) _cell_length_c 17.6339(12) _cell_angle_alpha 90 _cell_angle_beta 90.553(6) _cell_angle_gamma 90 _cell_volume 982.14(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.820 _exptl_crystal_F_000 805 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.035 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 5.082 _shelx_estimated_absorpt_T_min 0.401 _shelx_estimated_absorpt_T_max 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8155 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.110 _diffrn_reflns_theta_max 25.018 _diffrn_reflns_theta_full 25.018 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.972 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_Laue_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_point_group_measured_fraction_full 0.972 _reflns_number_total 1685 _reflns_number_gt 1435 _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 'SHELXT 2014/5 (Sheldrick, 2014)' _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^)+(0.0212P)^2^] 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 1685 _refine_ls_number_parameters 183 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0485 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 Te Te 0.25107(2) 0.51711(3) 0.75467(2) 0.00807(9) Uani 0.980(3) 1 d . . P . . MgT Mg 0.25107(2) 0.51711(3) 0.75467(2) 0.00807(9) Uani 0.020(3) 1 d . . P . . Cu Cu 0.24963(3) 1.01683(5) 0.75423(2) 0.01049(18) Uani 0.941(5) 1 d . . P . . MgC Mg 0.24963(3) 1.01683(5) 0.75423(2) 0.01049(18) Uani 0.059(5) 1 d . . P . . Mg1 Mg 0.000000 0.500000 0.000000 0.0135(3) Uani 1 2 d S . P . . Mg2 Mg 0.500000 0.500000 0.500000 0.0135(3) Uani 1 2 d S . P . . O1 O 0.2386(2) 0.7629(3) 0.82643(12) 0.0154(5) Uani 1 1 d . . . . . O2 O 0.2576(2) 0.2720(3) 0.82697(12) 0.0150(5) Uani 1 1 d . . . . . O3 O 0.2527(2) 0.2724(3) 0.68119(12) 0.0140(5) Uani 1 1 d . . . . . O4 O 0.2534(2) 0.7613(3) 0.68093(12) 0.0145(5) Uani 1 1 d . . . . . OH1 O 0.4541(2) 0.5215(3) 0.75699(12) 0.0196(5) Uani 1 1 d D . . . . H1 H 0.476(3) 0.650(4) 0.7666(17) 0.029 Uiso 1 1 d D U . . . OH2 O 0.0478(2) 0.5133(3) 0.75100(12) 0.0186(5) Uani 1 1 d D . . . . H2 H 0.027(3) 0.384(3) 0.7560(17) 0.028 Uiso 1 1 d D U . . . OW1 O 0.8134(2) 0.6068(4) 0.03343(12) 0.0232(5) Uani 1 1 d D . . . . H1A H 0.752(2) 0.641(6) 0.0056(12) 0.028 Uiso 1 1 d D U . . . H1B H 0.796(3) 0.648(5) 0.0754(10) 0.028 Uiso 1 1 d D U . . . OW2 O 0.9083(2) 0.2295(3) 0.93724(12) 0.0212(5) Uani 1 1 d D . . . . H2A H 0.859(3) 0.242(4) 0.9005(14) 0.025 Uiso 1 1 d D U . . . H2B H 0.955(3) 0.118(4) 0.9329(15) 0.025 Uiso 1 1 d D U . . . OW3 O -0.0110(2) 0.7367(3) 0.90816(12) 0.0194(5) Uani 1 1 d D . . . . H3A H -0.075(2) 0.749(5) 0.8786(15) 0.023 Uiso 1 1 d D U . . . H3B H 0.060(2) 0.735(5) 0.8795(15) 0.023 Uiso 1 1 d D U . . . OW4 O 0.3124(2) 0.6056(4) 0.46473(12) 0.0227(5) Uani 1 1 d D . . . . H4A H 0.294(3) 0.658(5) 0.4221(10) 0.027 Uiso 1 1 d D U . . . H4B H 0.250(2) 0.635(6) 0.4911(13) 0.027 Uiso 1 1 d D U . . . OW5 O 0.4089(2) 0.2327(3) 0.56357(11) 0.0198(5) Uani 1 1 d D . . . . H5A H 0.456(3) 0.117(4) 0.5698(15) 0.024 Uiso 1 1 d D U . . . H5B H 0.371(3) 0.250(4) 0.6041(13) 0.024 Uiso 1 1 d D U . . . OW6 O 0.4908(2) 0.7395(3) 0.59108(12) 0.0191(5) Uani 1 1 d D . . . . H6A H 0.426(2) 0.740(5) 0.6208(15) 0.023 Uiso 1 1 d D U . . . H6B H 0.5601(19) 0.747(5) 0.6181(15) 0.023 Uiso 1 1 d D U . . . 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 Te 0.01138(14) 0.00517(14) 0.00767(13) 0.00004(6) 0.00012(8) 0.00037(7) MgT 0.01138(14) 0.00517(14) 0.00767(13) 0.00004(6) 0.00012(8) 0.00037(7) Cu 0.0203(3) 0.0033(3) 0.0079(3) -0.00011(12) 0.00055(17) -0.00043(14) MgC 0.0203(3) 0.0033(3) 0.0079(3) -0.00011(12) 0.00055(17) -0.00043(14) Mg1 0.0147(8) 0.0131(7) 0.0126(8) -0.0002(5) 0.0007(6) 0.0017(5) Mg2 0.0145(8) 0.0137(8) 0.0123(8) 0.0004(5) 0.0012(6) 0.0006(5) O1 0.0265(14) 0.0097(12) 0.0101(11) -0.0021(7) -0.0001(9) 0.0000(8) O2 0.0243(14) 0.0115(11) 0.0092(11) 0.0028(7) 0.0020(9) 0.0000(8) O3 0.0220(13) 0.0116(12) 0.0085(11) -0.0004(7) 0.0022(9) 0.0004(8) O4 0.0221(13) 0.0116(12) 0.0098(12) -0.0014(7) 0.0011(9) -0.0017(8) OH1 0.0130(12) 0.0146(12) 0.0312(14) 0.0023(8) -0.0013(9) -0.0001(9) OH2 0.0117(12) 0.0144(12) 0.0297(14) -0.0023(8) 0.0011(9) 0.0003(9) OW1 0.0196(13) 0.0368(13) 0.0132(12) -0.0011(10) 0.0018(9) 0.0098(10) OW2 0.0240(15) 0.0215(12) 0.0179(13) -0.0045(9) -0.0070(10) 0.0043(9) OW3 0.0191(14) 0.0266(12) 0.0124(12) 0.0038(9) 0.0012(9) 0.0039(9) OW4 0.0199(14) 0.0349(13) 0.0135(12) 0.0024(9) 0.0004(9) 0.0089(10) OW5 0.0243(15) 0.0199(12) 0.0153(12) 0.0032(8) 0.0054(10) 0.0039(9) OW6 0.0199(14) 0.0242(12) 0.0131(12) -0.0030(8) 0.0015(9) -0.0002(9) _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 Te O2 1.9015(19) . ? Te O1 1.9018(18) . ? Te O3 1.9134(19) . ? Te O4 1.9142(19) . ? Te OH1 1.966(2) . ? Te OH2 1.969(2) . ? Te Cu 2.8743(3) . ? Te Cu 2.8775(3) 1_545 ? Te Cu 4.8392(4) 2_646 ? Te Cu 4.8497(4) 2_546 ? Cu O1 1.9413(19) . ? Cu O2 1.9503(19) 1_565 ? Cu O3 1.9547(19) 1_565 ? Cu O4 1.9579(18) . ? Cu OH1 2.878(2) 2_656 ? Cu OH2 2.881(2) 2_556 ? Mg1 OW1 2.002(2) 3_665 ? Mg1 OW1 2.002(2) 1_455 ? Mg1 OW2 2.1012(19) 3_666 ? Mg1 OW2 2.1012(19) 1_454 ? Mg1 OW3 2.118(2) 3_566 ? Mg1 OW3 2.118(2) 1_554 ? Mg2 OW4 2.009(2) . ? Mg2 OW4 2.009(2) 3_666 ? Mg2 OW5 2.1018(19) 3_666 ? Mg2 OW5 2.1019(19) . ? Mg2 OW6 2.119(2) . ? Mg2 OW6 2.119(2) 3_666 ? 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 O2 Te O1 96.13(9) . . ? O2 Te O3 84.73(9) . . ? O1 Te O3 176.77(8) . . ? O2 Te O4 177.31(8) . . ? O1 Te O4 84.72(9) . . ? O3 Te O4 94.57(9) . . ? O2 Te OH1 88.20(9) . . ? O1 Te OH1 92.65(9) . . ? O3 Te OH1 90.49(9) . . ? O4 Te OH1 89.21(9) . . ? O2 Te OH2 92.33(9) . . ? O1 Te OH2 87.74(9) . . ? O3 Te OH2 89.11(9) . . ? O4 Te OH2 90.26(9) . . ? OH1 Te OH2 179.31(7) . . ? O2 Te Cu 138.01(6) . . ? O1 Te Cu 42.12(6) . . ? O3 Te Cu 137.22(6) . . ? O4 Te Cu 42.66(6) . . ? OH1 Te Cu 89.55(5) . . ? OH2 Te Cu 90.36(5) . . ? O2 Te Cu 42.31(6) . 1_545 ? O1 Te Cu 138.13(6) . 1_545 ? O3 Te Cu 42.49(6) . 1_545 ? O4 Te Cu 137.05(6) . 1_545 ? OH1 Te Cu 91.01(5) . 1_545 ? OH2 Te Cu 89.08(5) . 1_545 ? Cu Te Cu 179.372(15) . 1_545 ? O2 Te Cu 89.69(7) . 2_646 ? O1 Te Cu 95.25(7) . 2_646 ? O3 Te Cu 87.87(7) . 2_646 ? O4 Te Cu 87.69(7) . 2_646 ? OH1 Te Cu 3.15(6) . 2_646 ? OH2 Te Cu 176.20(6) . 2_646 ? Cu Te Cu 90.290(8) . 2_646 ? Cu Te Cu 90.251(9) 1_545 2_646 ? O2 Te Cu 92.77(7) . 2_546 ? O1 Te Cu 87.25(7) . 2_546 ? O3 Te Cu 89.59(7) . 2_546 ? O4 Te Cu 89.82(7) . 2_546 ? OH1 Te Cu 179.03(6) . 2_546 ? OH2 Te Cu 0.62(5) . 2_546 ? Cu Te Cu 89.739(8) . 2_546 ? Cu Te Cu 89.701(8) 1_545 2_546 ? Cu Te Cu 176.287(8) 2_646 2_546 ? O1 Cu O2 97.88(9) . 1_565 ? O1 Cu O3 177.73(8) . 1_565 ? O2 Cu O3 82.34(9) 1_565 1_565 ? O1 Cu O4 82.51(9) . . ? O2 Cu O4 176.64(8) 1_565 . ? O3 Cu O4 97.41(9) 1_565 . ? O1 Cu Te 41.07(6) . . ? O2 Cu Te 138.65(6) 1_565 . ? O3 Cu Te 138.90(6) 1_565 . ? O4 Cu Te 41.49(6) . . ? O1 Cu Te 138.68(6) . 1_565 ? O2 Cu Te 41.02(6) 1_565 1_565 ? O3 Cu Te 41.39(6) 1_565 1_565 ? O4 Cu Te 138.79(6) . 1_565 ? Te Cu Te 179.370(15) . 1_565 ? O1 Cu OH1 96.50(8) . 2_656 ? O2 Cu OH1 90.28(8) 1_565 2_656 ? O3 Cu OH1 85.75(8) 1_565 2_656 ? O4 Cu OH1 86.35(8) . 2_656 ? Te Cu OH1 90.27(4) . 2_656 ? Te Cu OH1 89.20(4) 1_565 2_656 ? O1 Cu OH2 87.39(8) . 2_556 ? O2 Cu OH2 93.43(8) 1_565 2_556 ? O3 Cu OH2 90.34(8) 1_565 2_556 ? O4 Cu OH2 89.93(8) . 2_556 ? Te Cu OH2 89.87(4) . 2_556 ? Te Cu OH2 90.69(4) 1_565 2_556 ? OH1 Cu OH2 174.22(5) 2_656 2_556 ? OW1 Mg1 OW1 180.00(12) 3_665 1_455 ? OW1 Mg1 OW2 90.25(9) 3_665 3_666 ? OW1 Mg1 OW2 89.75(9) 1_455 3_666 ? OW1 Mg1 OW2 89.75(9) 3_665 1_454 ? OW1 Mg1 OW2 90.25(9) 1_455 1_454 ? OW2 Mg1 OW2 180.00(10) 3_666 1_454 ? OW1 Mg1 OW3 89.38(8) 3_665 3_566 ? OW1 Mg1 OW3 90.62(8) 1_455 3_566 ? OW2 Mg1 OW3 93.18(8) 3_666 3_566 ? OW2 Mg1 OW3 86.82(8) 1_454 3_566 ? OW1 Mg1 OW3 90.62(8) 3_665 1_554 ? OW1 Mg1 OW3 89.38(8) 1_455 1_554 ? OW2 Mg1 OW3 86.82(8) 3_666 1_554 ? OW2 Mg1 OW3 93.18(8) 1_454 1_554 ? OW3 Mg1 OW3 180.00(10) 3_566 1_554 ? OW1 Mg1 Cu 99.74(6) 3_665 2_545 ? OW1 Mg1 Cu 80.26(6) 1_455 2_545 ? OW2 Mg1 Cu 130.28(6) 3_666 2_545 ? OW2 Mg1 Cu 49.72(6) 1_454 2_545 ? OW3 Mg1 Cu 135.07(6) 3_566 2_545 ? OW3 Mg1 Cu 44.93(6) 1_554 2_545 ? OW1 Mg1 Cu 80.26(6) 3_665 4_575 ? OW1 Mg1 Cu 99.74(6) 1_455 4_575 ? OW2 Mg1 Cu 49.72(6) 3_666 4_575 ? OW2 Mg1 Cu 130.28(6) 1_454 4_575 ? OW3 Mg1 Cu 44.93(6) 3_566 4_575 ? OW3 Mg1 Cu 135.07(6) 1_554 4_575 ? Cu Mg1 Cu 180.0 2_545 4_575 ? OW4 Mg2 OW4 180.0 . 3_666 ? OW4 Mg2 OW5 89.80(9) . 3_666 ? OW4 Mg2 OW5 90.20(9) 3_666 3_666 ? OW4 Mg2 OW5 90.20(9) . . ? OW4 Mg2 OW5 89.80(9) 3_666 . ? OW5 Mg2 OW5 180.0 3_666 . ? OW4 Mg2 OW6 89.63(9) . . ? OW4 Mg2 OW6 90.37(9) 3_666 . ? OW5 Mg2 OW6 87.10(8) 3_666 . ? OW5 Mg2 OW6 92.90(8) . . ? OW4 Mg2 OW6 90.37(9) . 3_666 ? OW4 Mg2 OW6 89.63(9) 3_666 3_666 ? OW5 Mg2 OW6 92.89(8) 3_666 3_666 ? OW5 Mg2 OW6 87.11(8) . 3_666 ? OW6 Mg2 OW6 180.0 . 3_666 ? OW4 Mg2 Cu 134.39(6) . 2_646 ? OW4 Mg2 Cu 45.60(6) 3_666 2_646 ? OW5 Mg2 Cu 104.38(6) 3_666 2_646 ? OW5 Mg2 Cu 75.62(6) . 2_646 ? OW6 Mg2 Cu 49.22(6) . 2_646 ? OW6 Mg2 Cu 130.78(6) 3_666 2_646 ? OW4 Mg2 Cu 45.61(6) . 4_575 ? OW4 Mg2 Cu 134.40(6) 3_666 4_575 ? OW5 Mg2 Cu 75.62(6) 3_666 4_575 ? OW5 Mg2 Cu 104.38(6) . 4_575 ? OW6 Mg2 Cu 130.78(6) . 4_575 ? OW6 Mg2 Cu 49.22(6) 3_666 4_575 ? Cu Mg2 Cu 180.0 2_646 4_575 ? Te O1 Cu 96.81(10) . . ? Te O2 Cu 96.67(10) . 1_545 ? Te O3 Cu 96.13(9) . 1_545 ? Te O4 Cu 95.85(9) . . ? Te OH1 Cu 174.71(11) . 2_646 ? Te OH1 Cu 55.94(5) . . ? Cu OH1 Cu 125.16(6) 2_646 . ? Te OH1 Cu 54.97(5) . 1_545 ? Cu OH1 Cu 123.60(6) 2_646 1_545 ? Cu OH1 Cu 110.90(6) . 1_545 ? Te OH2 Cu 178.95(8) . 2_546 ? Te OH2 Cu 56.24(5) . 1_545 ? Cu OH2 Cu 124.81(6) 2_546 1_545 ? Te OH2 Cu 55.34(5) . . ? Cu OH2 Cu 123.61(6) 2_546 . ? Cu OH2 Cu 111.58(6) 1_545 . ? Mg1 OW2 Cu 106.95(7) 1_656 2_646 ? Mg1 OW3 Cu 112.36(7) 1_556 2_546 ? Mg1 OW3 Cu 137.72(8) 1_556 . ? Cu OW3 Cu 90.32(4) 2_546 . ? Mg2 OW4 Cu 112.33(7) . 4_575 ? Mg2 OW5 Cu 149.42(8) . 1_545 ? Mg2 OW6 Cu 106.53(7) . 2_646 ? Mg2 OW6 Cu 145.42(9) . . ? Cu OW6 Cu 90.27(4) 2_646 . ? 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 OW1 H1A OW5 0.793(16) 2.038(17) 2.831(3) 178(3) 2_655 OW1 H1B O2 0.798(16) 1.859(17) 2.656(3) 175(3) 3_666 OW2 H2A O4 0.806(17) 1.795(17) 2.601(3) 178(3) 2_646 OW2 H2B OW3 0.789(16) 2.26(2) 2.986(3) 153(3) 1_645 OW3 H3A O3 0.806(17) 2.018(16) 2.817(3) 171(3) 2_556 OW3 H3B O1 0.856(16) 1.983(16) 2.830(3) 170(3) . OW4 H4A O1 0.827(16) 1.824(17) 2.645(3) 172(3) 4_575 OW4 H4B OW2 0.783(16) 2.070(17) 2.852(3) 177(4) 2_656 OW5 H5A OW6 0.814(16) 2.23(2) 2.984(3) 154(3) 1_545 OW5 H5B O3 0.813(16) 1.790(17) 2.589(3) 167(3) . OW6 H6A O4 0.819(16) 1.994(16) 2.807(3) 172(3) . OW6 H6B O2 0.820(17) 2.011(16) 2.827(3) 173(3) 2_656 _refine_diff_density_max 1.044 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.131 _shelx_res_file ; TITL Adan14 adan14.res created by SHELXL-2016/6 at 18:24:12 on 19-Nov-2017 CELL 0.71075 9.68383 5.75175 17.63390 90.00000 90.55330 90.00000 ZERR 2 0.00047 0.00019 0.00124 0.00000 0.00640 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC CU MG TE O H UNIT 3.8 4.3 3.9 48 56 SHEL 99999 0.84 L.S. 8 omit 0 1 7 omit 0 1 2 omit 0 2 2 omit 0 2 4 omit 0 6 10 CONN 9 3.2 CU EQIV $20 -x+1, y+1/2, -z+1/2 HTAB OW1 OW5_$20 EQIV $16 -x+1, -y+1, -z+1 HTAB OW1 O2_$16 EQIV $7 -x+1, y-1/2, -z+3/2 HTAB OW2 O4_$7 EQIV $21 x+1, y-1, z HTAB OW2 OW3_$21 EQIV $2 -x, y+1/2, -z+3/2 HTAB OW3 O3_$2 HTAB OW3 O1 EQIV $8 x, -y+3/2, z-1/2 HTAB OW4 O1_$8 EQIV $3 -x+1, y+1/2, -z+3/2 HTAB OW4 OW2_$3 EQIV $4 x, y-1, z HTAB OW5 OW6_$4 HTAB OW5 O3 HTAB OW6 O4 HTAB OW6 O2_$3 EXYZ TE MGT EADP TE MGT EXYZ CU MGC EADP CU MGC FMAP 2 PLAN 10 ACTA HTAB DFIX 0.82 0.02 OH1 H1 OH2 H2 OW1 H1a OW1 H1b OW2 H2a OW2 H2b OW3 H3a OW3 H3b DFIX 0.82 0.02 OW4 H4a OW4 H4b OW5 H5a OW5 H5b OW6 H6a OW6 H6b DFIX 1.30 0.02 H1a H1b H2a H2b H3a H3b H4a H4b H5a H5b H6a H6b SIZE 0.220 0.035 0.020 WGHT 0.021200 FVAR 0.23404 0.98015 0.94127 TE 3 0.251067 0.517113 0.754666 21.00000 0.01138 0.00517 = 0.00767 0.00004 0.00012 0.00037 MGT 2 0.251067 0.517113 0.754666 -21.00000 0.01138 0.00517 = 0.00767 0.00004 0.00012 0.00037 CU 1 0.249632 1.016827 0.754234 31.00000 0.02029 0.00327 = 0.00792 -0.00011 0.00055 -0.00043 MGC 2 0.249632 1.016827 0.754234 -31.00000 0.02029 0.00327 = 0.00792 -0.00011 0.00055 -0.00043 MG1 2 0.000000 0.500000 0.000000 10.50000 0.01475 0.01309 = 0.01257 -0.00024 0.00068 0.00173 MG2 2 0.500000 0.500000 0.500000 10.50000 0.01452 0.01373 = 0.01233 0.00036 0.00116 0.00065 O1 4 0.238632 0.762861 0.826432 11.00000 0.02646 0.00968 = 0.01006 -0.00208 -0.00009 0.00003 O2 4 0.257633 0.272016 0.826971 11.00000 0.02431 0.01149 = 0.00920 0.00277 0.00199 -0.00003 O3 4 0.252747 0.272363 0.681191 11.00000 0.02198 0.01159 = 0.00850 -0.00040 0.00216 0.00041 O4 4 0.253442 0.761288 0.680931 11.00000 0.02205 0.01163 = 0.00976 -0.00141 0.00115 -0.00175 OH1 4 0.454089 0.521489 0.756993 11.00000 0.01302 0.01464 = 0.03116 0.00231 -0.00127 -0.00013 H1 5 0.476066 0.650486 0.766621 11.00000 -1.50000 OH2 4 0.047772 0.513269 0.750998 11.00000 0.01174 0.01443 = 0.02974 -0.00228 0.00106 0.00028 H2 5 0.026816 0.384323 0.756019 11.00000 -1.50000 OW1 4 0.813438 0.606807 0.033432 11.00000 0.01964 0.03680 = 0.01321 -0.00108 0.00180 0.00980 H1A 5 0.752012 0.641300 0.005555 11.00000 -1.20000 H1B 5 0.795772 0.648253 0.075421 11.00000 -1.20000 OW2 4 0.908314 0.229495 0.937238 11.00000 0.02397 0.02146 = 0.01792 -0.00455 -0.00705 0.00434 H2A 5 0.858760 0.242299 0.900479 11.00000 -1.20000 H2B 5 0.955167 0.118177 0.932949 11.00000 -1.20000 OW3 4 -0.010980 0.736746 0.908158 11.00000 0.01915 0.02664 = 0.01240 0.00375 0.00122 0.00393 H3A 5 -0.074603 0.748832 0.878644 11.00000 -1.20000 H3B 5 0.059798 0.735161 0.879495 11.00000 -1.20000 OW4 4 0.312395 0.605604 0.464731 11.00000 0.01988 0.03486 = 0.01347 0.00236 0.00041 0.00892 H4A 5 0.294437 0.658243 0.422108 11.00000 -1.20000 H4B 5 0.250310 0.635148 0.491136 11.00000 -1.20000 OW5 4 0.408922 0.232672 0.563569 11.00000 0.02434 0.01985 = 0.01530 0.00320 0.00542 0.00393 H5A 5 0.456298 0.117226 0.569761 11.00000 -1.20000 H5B 5 0.370826 0.249991 0.604058 11.00000 -1.20000 OW6 4 0.490804 0.739535 0.591076 11.00000 0.01994 0.02424 = 0.01315 -0.00303 0.00153 -0.00016 H6A 5 0.426228 0.740437 0.620756 11.00000 -1.20000 H6B 5 0.560070 0.747393 0.618075 11.00000 -1.20000 HKLF 4 REM Adan14 REM R1 = 0.0207 for 1435 Fo > 4sig(Fo) and 0.0259 for all 1685 data REM 183 parameters refined using 20 restraints END WGHT 0.0212 0.0000 REM Instructions for potential hydrogen bonds HTAB OW1 OW5_$20 HTAB OW1 O2_$16 HTAB OW2 O4_$7 HTAB OW2 OW3_$21 HTAB OW3 O3_$2 HTAB OW3 O1 HTAB OW3 OH2 HTAB OW4 O1_$8 HTAB OW4 OW2_$3 HTAB OW5 OW6_$4 HTAB OW5 O3 HTAB OW6 O4 HTAB OW6 O2_$3 REM Highest difference peak 1.044, deepest hole -0.388, 1-sigma level 0.131 Q1 1 0.1445 0.5090 0.7500 11.00000 0.05 1.04 Q2 1 0.3576 0.5106 0.7556 11.00000 0.05 0.97 Q3 1 0.1560 0.9923 0.7515 11.00000 0.05 0.61 Q4 1 0.3483 1.0033 0.7576 11.00000 0.05 0.59 Q5 1 0.3221 0.3380 0.8029 11.00000 0.05 0.53 Q6 1 0.2513 0.2510 0.7606 11.00000 0.05 0.50 Q7 1 0.2433 0.7818 0.7592 11.00000 0.05 0.49 Q8 1 0.1556 0.6951 0.8126 11.00000 0.05 0.44 Q9 1 0.1546 0.1780 0.7174 11.00000 0.05 0.42 Q10 1 0.3668 0.1785 0.8042 11.00000 0.05 0.42 ; _shelx_res_checksum 12469 _shelx_hkl_file ; 1 0 -2 13.45 0.79 -1 0 2 15.48 0.72 1 0 -2 15.95 1.08 -1 0 2 17.22 0.78 -1 0 -2 22.58 0.98 1 0 2 23.62 1.00 1 0 2 21.45 0.74 -1 0 -2 20.52 0.73 0 0 3 1.53 0.50 0 0 -3 1.82 0.78 0 1 0 0.49 0.06 0 -1 0 -0.08 0.04 0 1 -1 2.47 0.35 0 1 1 1.53 0.24 1 0 -3 0.38 0.47 -1 0 3 0.61 0.49 -1 0 3 0.62 0.40 1 0 -3 0.55 0.39 -1 0 -3 0.02 0.30 1 0 3 0.69 0.50 -1 0 -3 0.49 0.51 1 -1 0 7.31 0.51 -1 1 0 7.32 0.50 -1 -1 0 7.15 0.48 1 1 0 7.36 0.34 2 0 0 4065.48 117.35 -2 0 0 3959.61 113.61 2 0 0 4234.10 118.57 -2 0 0 4252.12 119.36 0 1 -2 2.49 0.61 0 1 2 2.72 0.35 0 -1 -2 3.12 0.50 1 -1 -1 124.22 2.20 -1 1 1 129.39 2.25 -1 1 1 130.64 3.26 -1 -1 1 127.16 2.34 1 1 -1 126.15 1.95 1 -1 1 1228.78 24.72 1 1 1 1379.33 25.37 -1 -1 -1 1368.56 25.06 -1 1 -1 1228.24 24.77 2 0 -1 2.47 0.66 -2 0 1 2.53 0.70 -2 0 1 1.87 0.64 2 0 -1 1.49 0.70 -2 0 -1 1.79 0.69 2 0 1 1.55 0.68 2 0 1 1.56 0.66 -2 0 -1 2.50 0.65 0 0 4 7539.60 248.94 0 0 -4 7864.23 257.92 -1 1 2 2.66 0.47 -1 -1 2 1.98 0.44 1 1 -2 2.81 0.44 -1 1 2 3.33 0.48 1 -1 -2 1.99 0.46 1 -1 -2 2.22 0.45 1 1 2 44.89 1.48 -1 1 -2 41.23 1.93 1 1 2 41.17 1.11 1 -1 2 41.61 1.40 -1 -1 -2 39.71 1.53 2 0 -2 6812.56 222.03 2 0 -2 6896.60 223.37 -2 0 2 6811.68 222.91 -2 0 2 6623.29 215.86 2 0 2 6659.02 218.40 2 0 2 6627.80 212.35 -2 0 -2 6276.31 203.13 -2 0 -2 6624.06 215.43 0 1 -3 8.94 0.78 0 -1 -3 10.71 0.69 0 1 3 12.03 0.71 1 0 -4 28.21 1.12 -1 0 4 28.34 1.48 1 0 -4 29.19 1.44 -1 0 -4 22.80 1.54 -1 1 3 1143.20 23.49 1 -1 -3 1102.41 22.71 -1 1 3 1080.43 20.83 -1 -1 3 1142.85 23.37 1 -1 -3 1101.36 21.56 1 1 -3 1126.13 22.84 -1 -1 -3 101.21 2.39 1 -1 3 96.48 2.69 1 1 3 98.46 1.64 -1 1 -3 103.22 3.58 -2 0 3 0.93 0.62 2 0 -3 -0.17 0.62 2 0 -3 0.33 0.64 -2 0 3 1.38 0.63 2 0 3 -0.02 0.54 -2 0 -3 1.09 0.72 2 0 3 0.48 0.69 -2 0 -3 1.43 0.57 2 1 0 33.02 1.24 -2 1 0 39.34 1.76 -2 -1 0 37.16 1.68 2 -1 0 35.62 2.19 2 1 0 38.75 2.53 -2 1 0 36.30 1.47 -2 -1 0 32.79 1.22 2 -1 0 34.18 1.59 2 1 -1 3.66 0.95 2 -1 -1 3.96 0.73 -2 1 1 5.13 0.85 2 -1 -1 3.16 1.27 -2 1 1 3.55 0.71 -2 -1 1 3.49 0.60 2 1 -1 5.10 1.45 -2 1 -1 2.13 0.74 2 -1 1 3.45 0.73 -2 -1 -1 2.62 0.59 2 1 1 2.48 0.61 2 1 1 4.28 0.71 -2 -1 -1 3.27 0.73 -2 1 -1 2.98 1.37 0 0 5 1.92 0.78 0 0 -5 1.01 0.77 0 1 4 1.94 0.60 0 -1 -4 2.40 0.59 0 -1 -4 1.46 0.31 0 1 -4 0.89 0.64 -2 1 2 3.71 0.85 2 -1 -2 6.21 0.87 2 1 -2 5.40 1.14 2 1 -2 6.10 0.77 -2 -1 2 6.59 0.72 -2 1 2 4.67 0.85 2 -1 -2 5.25 0.81 2 1 2 4.87 0.78 2 1 2 4.78 1.12 2 -1 2 6.24 0.93 -2 1 -2 6.94 1.06 -2 -1 -2 5.01 0.76 -2 1 -2 4.52 0.89 -2 -1 -2 5.50 0.78 -1 0 5 0.02 0.97 1 0 -5 -0.30 0.43 1 0 -5 1.08 0.60 -1 0 -5 0.44 1.10 -1 1 4 6.39 0.75 1 -1 -4 7.42 0.71 -1 -1 4 5.64 0.86 1 1 -4 7.14 0.89 -1 1 4 6.18 0.91 1 -1 -4 6.79 0.85 -1 -1 -4 50.35 0.83 1 1 4 46.12 0.75 -1 1 -4 47.80 2.06 -1 -1 -4 45.65 1.83 2 0 -4 2688.50 72.75 2 0 -4 2801.77 72.02 -2 0 4 2630.16 70.09 -2 0 4 2724.15 71.24 2 0 4 2907.99 73.09 -2 0 -4 2689.08 73.77 -2 0 -4 2696.79 71.44 2 0 4 2675.60 75.68 3 0 0 0.70 0.78 3 0 0 0.79 0.81 -3 0 0 0.31 0.82 -3 0 0 1.75 1.18 -3 0 1 1.59 0.84 -3 0 1 0.39 0.74 3 0 -1 0.32 0.83 3 0 -1 1.44 0.79 -3 0 -1 0.55 0.82 3 0 1 1.94 0.81 3 0 1 1.06 0.83 -3 0 -1 0.65 0.85 2 1 -3 30.31 1.98 -2 1 3 27.32 2.09 2 1 -3 32.36 1.46 2 -1 -3 28.35 1.51 -2 1 3 30.42 1.54 -2 -1 3 31.63 2.10 2 -1 -3 27.73 1.44 -2 1 -3 45.92 2.12 2 1 3 46.76 2.05 2 -1 3 44.11 2.12 -2 -1 -3 48.46 1.83 2 1 3 48.60 1.92 -2 1 -3 47.64 2.15 -2 -1 -3 47.32 1.53 3 0 -2 251.36 6.58 3 0 -2 249.59 6.21 -3 0 2 245.78 6.49 -3 0 2 251.88 6.24 3 0 2 303.39 7.46 -3 0 -2 323.25 9.52 -3 0 -2 303.95 9.06 3 0 2 315.22 7.71 0 1 5 20.75 1.36 0 1 -5 21.15 2.09 0 -1 -5 20.09 1.32 0 0 -6 3781.01 108.85 -1 1 5 110.09 3.28 1 -1 -5 117.36 3.25 1 -1 -5 99.69 1.83 1 1 -5 110.92 3.22 -1 -1 5 108.28 3.28 -1 1 5 111.33 1.97 -1 -1 -5 764.28 17.96 1 1 5 802.62 12.44 -1 -1 -5 814.09 12.65 -1 1 -5 740.18 18.10 2 0 -5 1.35 0.79 -2 0 5 0.33 1.22 -2 0 5 0.21 0.64 -2 1 4 16.77 1.37 -2 1 4 16.01 1.68 2 1 -4 19.99 1.68 -2 -1 4 13.59 1.33 2 -1 -4 14.92 1.06 2 1 -4 19.64 1.29 2 -1 -4 17.46 1.37 -3 0 3 1.15 0.84 3 0 -3 0.95 0.91 3 0 -3 3.60 1.37 -3 0 3 1.45 0.90 0 2 -1 118.54 1.80 0 2 -1 117.58 1.71 2 0 5 -0.16 0.87 -2 0 -5 1.62 0.91 -2 0 -5 0.74 0.56 2 -1 4 19.56 2.29 -2 -1 -4 12.27 1.26 -2 -1 -4 17.43 1.36 2 1 4 13.71 0.83 2 1 4 7.02 1.95 -2 1 -4 15.67 2.19 1 0 -6 208.38 4.54 -1 0 6 209.80 5.60 1 0 -6 206.22 5.47 -3 0 -3 0.12 0.73 -3 0 -3 1.39 0.47 3 0 3 0.25 0.73 3 0 3 0.02 0.83 -3 0 -3 -0.70 0.81 -3 -1 0 1.86 0.72 3 -1 0 2.09 0.87 3 1 0 2.39 0.73 -3 -1 0 1.13 0.97 3 1 0 1.43 0.93 -3 1 0 0.68 1.29 3 -1 0 0.74 0.79 3 -1 0 2.48 0.98 -3 1 0 0.87 0.99 -1 0 -6 217.69 6.50 3 1 -1 86.24 2.74 -3 1 1 83.00 3.19 3 1 -1 85.79 3.32 3 -1 -1 82.68 3.28 -3 -1 1 86.73 3.73 -3 -1 1 81.75 3.43 -3 1 1 78.71 3.99 3 -1 -1 83.40 2.95 -3 -1 -1 55.95 2.22 -3 1 -1 60.22 3.51 -3 -1 -1 56.42 2.54 3 1 1 63.59 3.19 3 1 1 60.96 2.57 3 -1 1 59.98 2.73 3 -1 1 60.37 2.54 -3 1 -1 56.18 2.82 -1 2 0 0.20 0.28 1 -2 0 0.12 0.28 1 2 0 0.23 0.09 -1 -2 0 0.42 0.14 0 -2 -2 4329.97 110.12 0 2 2 4551.49 115.12 0 2 -2 4083.06 108.56 0 2 -2 4301.55 114.59 -1 2 1 174.85 2.97 1 -2 -1 172.77 3.40 1 2 -1 169.36 2.30 -1 -2 1 186.04 2.49 1 -2 1 121.02 2.37 -1 2 -1 121.19 2.33 -1 -2 -1 117.61 1.56 3 -1 -2 173.09 5.04 -3 -1 2 180.97 5.68 3 1 -2 179.15 4.61 3 1 -2 189.08 5.55 -3 -1 2 179.41 5.81 -3 1 2 187.71 5.34 3 -1 -2 185.37 5.02 -3 1 2 176.62 4.94 -3 1 -2 147.52 4.83 3 -1 2 143.85 4.35 3 -1 2 144.87 5.79 3 1 2 147.90 4.13 -3 -1 -2 136.52 3.98 3 1 2 145.46 4.09 -3 1 -2 135.71 4.31 1 2 -2 76.53 1.48 1 -2 -2 78.82 2.12 -1 -2 2 80.49 1.52 -1 2 2 83.51 2.13 1 -2 2 76.44 1.93 -1 2 -2 73.46 1.85 -1 -2 -2 73.30 1.28 0 -1 -6 -0.54 0.74 0 1 6 0.95 0.77 0 -1 -6 1.18 0.51 0 1 -6 1.52 0.82 3 0 -4 141.36 4.27 -3 0 4 136.63 4.43 3 0 -4 130.69 4.19 -3 0 4 135.94 4.44 -3 0 -4 112.86 3.57 3 0 4 123.24 3.65 -3 0 -4 114.79 5.71 3 0 4 119.84 4.13 0 2 -3 254.14 5.02 0 2 -3 265.97 4.87 0 2 3 267.80 4.54 0 -2 -3 261.13 4.83 2 1 -5 63.91 2.48 -2 -1 5 65.00 3.59 2 -1 -5 60.88 2.61 2 -1 -5 54.81 1.87 -2 1 5 60.54 2.57 -2 1 5 61.95 2.67 3 -1 -3 33.77 2.02 3 -1 -3 36.67 2.13 -3 1 3 37.80 2.20 3 1 -3 41.01 2.52 -3 -1 3 36.04 1.95 3 1 -3 38.48 1.97 -3 1 3 38.67 3.05 -2 -1 -5 20.10 1.34 2 1 5 22.99 0.92 2 1 5 21.76 1.83 -2 -1 -5 20.96 1.71 2 -1 5 20.55 1.85 1 1 -6 236.39 5.95 -1 1 6 230.43 4.31 1 -1 -6 237.48 5.89 -1 1 6 232.76 6.10 -1 -1 6 228.73 5.99 1 -1 -6 199.98 3.45 -3 -1 -3 99.37 3.19 3 1 3 103.33 3.16 3 1 3 109.88 3.55 3 -1 3 104.78 3.81 -3 -1 -3 100.42 3.42 -3 1 -3 101.31 3.78 -3 1 -3 109.88 5.37 2 0 -6 495.96 11.86 2 0 -6 499.77 11.08 -2 0 6 484.48 11.99 -1 -1 -6 123.73 3.70 -1 1 -6 117.84 4.25 -1 -1 -6 109.40 1.61 -1 -1 -6 121.64 4.16 0 0 -7 0.30 0.78 -2 0 -6 455.34 9.79 -2 0 -6 446.46 11.87 2 0 6 460.00 12.17 -1 2 3 57.65 1.70 -1 2 3 62.49 1.64 1 -2 -3 57.44 2.11 -1 -2 3 61.57 1.56 1 2 -3 59.57 1.53 1 -2 3 128.09 3.22 -1 2 -3 122.91 3.87 -1 -2 -3 122.13 2.31 -1 -2 -3 121.90 2.40 -2 2 0 1298.87 32.34 -2 2 0 1290.99 28.87 -2 -2 0 1290.19 26.68 2 2 0 1279.44 26.04 2 -2 0 1315.42 29.34 -2 2 1 15.18 2.21 -2 2 1 16.61 1.04 -2 -2 1 14.35 0.73 2 -2 -1 14.03 1.00 2 2 -1 13.26 0.74 -2 2 -1 6.46 1.46 -2 -2 -1 10.07 0.93 2 2 1 11.57 1.24 2 2 1 10.29 0.97 2 -2 1 10.31 1.03 1 0 -7 -0.23 0.98 -1 0 7 -1.80 0.97 -1 0 -7 2.44 1.15 -1 0 -7 0.86 1.01 4 0 0 8356.02 313.99 4 0 0 8270.52 313.10 -4 0 0 7896.49 301.72 -4 0 0 8072.88 303.50 0 -2 -4 9551.05 340.36 0 2 -4 9642.42 355.56 0 2 -4 9999.00 360.24 4 0 -1 1.78 1.07 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