data_gysinite-(Ce) _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'gysinite-(Ce)' _chemical_compound_source 'Abendrothe Mine, St. Andreasberg, Germany' _chemical_formula_sum 'C2 H3 Ce1.13 O8 Pb0.87' _chemical_formula_weight 493.63 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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P m c n' _space_group_name_Hall '-p 2n 2a' _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+1/2, -y, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y, z' 'x, -y-1/2, z-1/2' _cell_length_a 5.0780(4) _cell_length_b 8.6689(6) _cell_length_c 7.3255(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 322.47(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2453 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'equant' _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 5.084 _exptl_crystal_F_000 432 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 30.564 _shelx_estimated_absorpt_T_min 0.223 _shelx_estimated_absorpt_T_max 0.223 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 2706 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.641 _diffrn_reflns_theta_max 27.431 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 410 _reflns_number_gt 396 _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_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _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^)+(0.0156P)^2^+2.0060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 410 _refine_ls_number_parameters 41 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0535 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.192 _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 Pb Pb 0.250000 0.34480(4) 0.65103(5) 0.01881(18) Uani 0.44(3) 2 d S T P . . Ce Ce 0.250000 0.34480(4) 0.65103(5) 0.01881(18) Uani 0.56(3) 2 d S T P . . C C 0.750000 0.1925(9) 0.8153(10) 0.0145(16) Uani 1 2 d S T P . . O1 O 0.750000 0.3231(7) 0.7328(10) 0.0297(17) Uani 1 2 d S T P . . O2 O 0.5314(9) 0.1242(5) 0.8495(5) 0.0244(12) Uani 1 1 d . . . . . O3 O 0.250000 0.4162(9) 0.9792(10) 0.044(2) Uani 1 2 d DS T P . . H1 H 0.250000 0.504(14) 1.02(4) 0.053 Uiso 0.5 2 d DS U P . . H2A H 0.250000 0.46(2) 1.081(13) 0.053 Uiso 0.5 2 d DS U P . . H2B H 0.250000 0.492(16) 0.91(2) 0.053 Uiso 0.5 2 d DS 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 Pb 0.0148(2) 0.0239(3) 0.0177(2) 0.00277(13) 0.000 0.000 Ce 0.0148(2) 0.0239(3) 0.0177(2) 0.00277(13) 0.000 0.000 C 0.014(4) 0.017(4) 0.012(3) -0.003(3) 0.000 0.000 O1 0.018(3) 0.027(3) 0.044(4) 0.012(3) 0.000 0.000 O2 0.014(2) 0.028(2) 0.031(3) 0.0026(16) 0.0031(17) -0.0044(18) O3 0.058(5) 0.053(5) 0.022(4) 0.006(3) 0.000 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 Pb O3 2.483(7) . ? Pb O3 2.589(8) 2_554 ? Pb O1 2.6155(18) 1_455 ? Pb O1 2.6155(18) . ? Pb O2 2.644(4) 2_554 ? Pb O2 2.644(4) 8_565 ? Pb O2 2.665(5) 4_656 ? Pb O2 2.665(5) 6_567 ? Pb O2 2.795(5) 7_655 ? Pb O2 2.795(5) . ? Pb C 3.024(8) 6_567 ? Pb C 3.105(5) . ? Pb H2B 2.3(2) . ? C O2 1.283(6) . ? C O2 1.283(6) 7_755 ? C O1 1.284(10) . ? O1 H2A 2.35(11) 3_567 ? O3 H1 0.82(3) . ? O3 H2A 0.83(3) . ? O3 H2B 0.83(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 O3 Pb O3 133.5(2) . 2_554 ? O3 Pb O1 78.24(17) . 1_455 ? O3 Pb O1 92.78(16) 2_554 1_455 ? O3 Pb O1 78.24(17) . . ? O3 Pb O1 92.78(16) 2_554 . ? O1 Pb O1 152.2(3) 1_455 . ? O3 Pb O2 141.58(14) . 2_554 ? O3 Pb O2 71.50(17) 2_554 2_554 ? O1 Pb O2 70.97(19) 1_455 2_554 ? O1 Pb O2 136.32(19) . 2_554 ? O3 Pb O2 141.58(14) . 8_565 ? O3 Pb O2 71.50(17) 2_554 8_565 ? O1 Pb O2 136.32(19) 1_455 8_565 ? O1 Pb O2 70.97(19) . 8_565 ? O2 Pb O2 65.4(2) 2_554 8_565 ? O3 Pb O2 76.98(19) . 4_656 ? O3 Pb O2 142.53(15) 2_554 4_656 ? O1 Pb O2 118.04(17) 1_455 4_656 ? O1 Pb O2 70.20(16) . 4_656 ? O2 Pb O2 97.56(9) 2_554 4_656 ? O2 Pb O2 71.41(15) 8_565 4_656 ? O3 Pb O2 76.98(19) . 6_567 ? O3 Pb O2 142.53(15) 2_554 6_567 ? O1 Pb O2 70.20(16) 1_455 6_567 ? O1 Pb O2 118.04(17) . 6_567 ? O2 Pb O2 71.41(14) 2_554 6_567 ? O2 Pb O2 97.56(9) 8_565 6_567 ? O2 Pb O2 49.2(2) 4_656 6_567 ? O3 Pb O2 70.54(18) . 7_655 ? O3 Pb O2 69.82(17) 2_554 7_655 ? O1 Pb O2 48.35(16) 1_455 7_655 ? O1 Pb O2 109.15(16) . 7_655 ? O2 Pb O2 103.16(14) 2_554 7_655 ? O2 Pb O2 141.29(9) 8_565 7_655 ? O2 Pb O2 146.69(8) 4_656 7_655 ? O2 Pb O2 114.19(4) 6_567 7_655 ? O3 Pb O2 70.54(18) . . ? O3 Pb O2 69.82(17) 2_554 . ? O1 Pb O2 109.15(16) 1_455 . ? O1 Pb O2 48.35(16) . . ? O2 Pb O2 141.29(9) 2_554 . ? O2 Pb O2 103.16(14) 8_565 . ? O2 Pb O2 114.19(4) 4_656 . ? O2 Pb O2 146.69(8) 6_567 . ? O2 Pb O2 61.49(18) 7_655 . ? O3 Pb C 70.9(2) . 6_567 ? O3 Pb C 155.6(2) 2_554 6_567 ? O1 Pb C 93.03(14) 1_455 6_567 ? O1 Pb C 93.03(14) . 6_567 ? O2 Pb C 88.11(15) 2_554 6_567 ? O2 Pb C 88.11(15) 8_565 6_567 ? O2 Pb C 25.05(10) 4_656 6_567 ? O2 Pb C 25.05(10) 6_567 6_567 ? O2 Pb C 129.74(14) 7_655 6_567 ? O2 Pb C 129.74(14) . 6_567 ? O3 Pb C 74.39(16) . . ? O3 Pb C 79.43(17) 2_554 . ? O1 Pb C 132.42(18) 1_455 . ? O1 Pb C 24.04(18) . . ? O2 Pb C 143.98(16) 2_554 . ? O2 Pb C 85.69(16) 8_565 . ? O2 Pb C 92.67(17) 4_656 . ? O2 Pb C 136.72(17) 6_567 . ? O2 Pb C 85.72(15) 7_655 . ? O2 Pb C 24.39(15) . . ? C Pb C 113.10(13) 6_567 . ? O3 Pb H2B 19.4(9) . . ? O3 Pb H2B 153.0(10) 2_554 . ? O1 Pb H2B 81.4(2) 1_455 . ? O1 Pb H2B 81.4(2) . . ? O2 Pb H2B 129.6(7) 2_554 . ? O2 Pb H2B 129.6(7) 8_565 . ? O2 Pb H2B 59.6(8) 4_656 . ? O2 Pb H2B 59.6(8) 6_567 . ? O2 Pb H2B 87.1(8) 7_655 . ? O2 Pb H2B 87.1(8) . . ? C Pb H2B 51.4(10) 6_567 . ? C Pb H2B 85.1(6) . . ? O2 C O2 119.9(7) . 7_755 ? O2 C O1 119.9(4) . . ? O2 C O1 119.9(4) 7_755 . ? O2 C Pb 61.6(4) . 6_657 ? O2 C Pb 61.6(4) 7_755 6_657 ? O1 C Pb 156.6(6) . 6_657 ? O2 C Pb 64.2(3) . . ? O2 C Pb 168.5(5) 7_755 . ? O1 C Pb 56.10(14) . . ? Pb C Pb 117.11(15) 6_657 . ? O2 C Pb 168.5(5) . 1_655 ? O2 C Pb 64.2(3) 7_755 1_655 ? O1 C Pb 56.10(14) . 1_655 ? Pb C Pb 117.11(15) 6_657 1_655 ? Pb C Pb 109.7(2) . 1_655 ? O2 C Pb 116.2(5) . 2_655 ? O2 C Pb 37.2(3) 7_755 2_655 ? O1 C Pb 114.0(3) . 2_655 ? Pb C Pb 81.53(16) 6_657 2_655 ? Pb C Pb 153.1(2) . 2_655 ? Pb C Pb 73.87(5) 1_655 2_655 ? O2 C Pb 37.2(3) . 2 ? O2 C Pb 116.2(5) 7_755 2 ? O1 C Pb 114.0(3) . 2 ? Pb C Pb 81.53(16) 6_657 2 ? Pb C Pb 73.87(5) . 2 ? Pb C Pb 153.1(2) 1_655 2 ? Pb C Pb 91.33(17) 2_655 2 ? C O1 H2A 116(5) . 3_567 ? C O1 Pb 99.85(15) . . ? H2A O1 Pb 94.3(11) 3_567 . ? C O1 Pb 99.86(15) . 1_655 ? H2A O1 Pb 94.3(11) 3_567 1_655 ? Pb O1 Pb 152.2(3) . 1_655 ? C O1 Pb 163.7(5) . 5_666 ? H2A O1 Pb 80(5) 3_567 5_666 ? Pb O1 Pb 77.79(14) . 5_666 ? Pb O1 Pb 77.79(14) 1_655 5_666 ? C O2 Pb 125.8(4) . 2 ? C O2 Pb 93.3(4) . 6_657 ? Pb O2 Pb 108.59(14) 2 6_657 ? C O2 Pb 91.4(4) . . ? Pb O2 Pb 95.10(15) 2 . ? Pb O2 Pb 146.52(17) 6_657 . ? Pb O3 Pb 104.6(3) . 2 ? Pb O3 H1 127(10) . . ? Pb O3 H1 129(10) 2 . ? Pb O3 H2A 170(10) . . ? Pb O3 H2A 86(10) 2 . ? H1 O3 H2A 43(10) . . ? Pb O3 H2B 66(10) . . ? Pb O3 H2B 171(10) 2 . ? H1 O3 H2B 60(10) . . ? H2A O3 H2B 103(5) . . ? 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 O3 H1 O1 0.82(3) 2.34(15) 3.091(11) 152(29) 5_667 O3 H2B O2 0.83(3) 2.48(7) 3.207(8) 147(11) 4_656 _refine_diff_density_max 1.898 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.415 _shelx_res_file ; TITL GM-4 GM4.res created by SHELXL-2016/6 at 10:38:00 on 31-Mar-2023 REM transformed to space group : Pmcn:bca CELL 0.71075 5.0780 8.6689 7.3255 90.000 90.000 90.000 ZERR 2 0.0004 0.0006 0.0006 0.000 0.000 0.000 LATT 1 SYMM 1/2-X,1/2-Y,1/2+Z SYMM 1/2+X,-Y,-Z SYMM -X,1/2+Y,1/2-Z SFAC H O C PB CE UNIT 6 16 4 1.74 2.26 L.S. 20 OMIT 1 1 0 OMIT 1 0 2 EXYZ PB CE EADP PB CE CONN 12 3.0 PB FMAP 2 PLAN 20 HTAB EQIV $1 -x+1, -y+1, -z+2 EQIV $2 -x+1, y+0.5, -z+1.5 EQIV $3 x+0.5, -y+1, -z+2 HTAB O3 O1_$1 HTAB O3 O2_$2 BIND O1 H2A_$3 ACTA BOND $H DFIX 0.82 0.03 O3 H1 O3 H2a O3 H2b DFIX 1.3 0.03 H2a H2b SIZE 0.070 0.070 0.070 WGHT 0.015600 2.006000 FVAR 0.37800 0.43515 PB 4 0.250000 0.344801 0.651026 20.50000 0.01484 0.02389 = 0.01769 0.00277 0.00000 0.00000 CE 5 0.250000 0.344801 0.651026 -20.50000 0.01484 0.02389 = 0.01769 0.00277 0.00000 0.00000 C 3 0.750000 0.192451 0.815258 10.50000 0.01399 0.01701 = 0.01246 -0.00316 0.00000 0.00000 O1 2 0.750000 0.323129 0.732806 10.50000 0.01820 0.02708 = 0.04394 0.01201 0.00000 0.00000 O2 2 0.531391 0.124238 0.849544 11.00000 0.01444 0.02790 = 0.03094 0.00256 0.00305 -0.00439 O3 2 0.250000 0.416246 0.979213 10.50000 0.05755 0.05292 = 0.02173 0.00617 0.00000 0.00000 H1 1 0.250000 0.503912 1.021817 10.25000 -1.20000 H2A 1 0.250000 0.456340 1.081453 10.25000 -1.20000 H2B 1 0.250000 0.491529 0.909654 10.25000 -1.20000 HKLF 4 REM GM-4 REM R1 = 0.0266 for 396 Fo > 4sig(Fo) and 0.0278 for all 410 data REM 41 parameters refined using 4 restraints END WGHT 0.0156 2.0058 REM Instructions for potential hydrogen bonds HTAB O3 O1_$1 EQIV $13 -x+1/2, -y+1/2, z+1/2 HTAB O3 O2_$13 EQIV $22 x, -y+1/2, z+1/2 HTAB O3 O2_$22 REM Highest difference peak 1.898, deepest hole -1.240, 1-sigma level 0.415 Q1 1 0.3170 0.3508 0.7345 11.00000 0.05 1.90 Q2 1 0.2500 0.2668 0.6513 10.50000 0.05 1.86 Q3 1 0.3459 0.3470 0.5931 11.00000 0.05 1.72 Q4 1 0.2500 0.4264 0.6351 10.50000 0.05 1.55 Q5 1 0.7500 0.0424 0.8957 10.50000 0.05 1.12 Q6 1 0.2500 0.2461 0.5242 10.50000 0.05 1.08 Q7 1 0.7852 0.3948 0.6249 11.00000 0.05 1.00 Q8 1 0.7500 0.2914 0.6478 10.50000 0.05 0.98 Q9 1 0.7500 0.0432 0.7805 10.50000 0.05 0.95 Q10 1 0.7500 0.1140 0.9863 10.50000 0.05 0.92 Q11 1 0.2500 0.2523 0.7574 10.50000 0.05 0.90 Q12 1 0.7500 0.2845 0.8195 10.50000 0.05 0.87 Q13 1 0.2500 0.4691 1.1561 10.50000 0.05 0.84 Q14 1 0.2155 0.5251 1.0575 11.00000 0.05 0.83 Q15 1 0.7500 0.1962 0.5968 10.50000 0.05 0.83 Q16 1 0.7500 0.2138 1.0131 10.50000 0.05 0.83 Q17 1 0.2500 0.5064 1.2712 10.50000 0.05 0.78 Q18 1 0.2500 0.4427 0.5181 10.50000 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