# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2023 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_710MPa _database_code_depnum_ccdc_archive 'CCDC 2223543' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C32.5 H19.5 O10, 2.84(C H4 O), 0.90(H2 O)' _chemical_formula_sum 'Sc2 C35.1 H35.5 O14.2' _chemical_formula_weight 723.19 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4760 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.799 Why? PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.44 Report PLAT088_ALERT_3_B Poor Data / Parameter Ratio .................... 7.53 Note The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- SHFSU01_ALERT_2_A The absolute value of parameter shift to su ratio > 0.20 Absolute value of the parameter shift to su ratio given 0.862 PLAT080_ALERT_2_A Maximum Shift/Error ............................ 0.86 Why ? PLAT245_ALERT_2_A U(iso) H5A Smaller than U(eq) O5 by 0.130 Ang**2 There is adsorbed solvate disordered over a special positiona in partially occupied sites, making them difficult to refine. The molecules were either placed as a rigid fragment or had it geometry restrained, and its occupancy set to its approximately refined value. #------------------------------------------------------------------------------- PLAT051_ALERT_1_A Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 62.96 % PLAT043_ALERT_1_B Calculated and Reported Mol. Weight Differ by .. 26.76 Check CHEMW01_ALERT_1_B The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.95 <> 1.05 Calculated formula weight = 774.4698 Formula weight given = 723.1900 The formula was ammended to properly account for the solvate. #------------------------------------------------------------------------------- PLAT420_ALERT_2_B D-H Bond Without Acceptor O2 --H2 . Please Check PLAT420_ALERT_2_B D-H Bond Without Acceptor O3 --H3A . Please Check These are correct. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc -0.3(9), Rep -0.16(13) ...... 6.92 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 7 Check PLAT733_ALERT_1_B Torsion Calc 0.3(9), Rep 0.16(13) ...... 6.92 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.476 79 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 13.37 0.476 0.857 596 511 85 #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.3445(19) _cell_length_b 23.984(3) _cell_length_c 13.1770(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2321.1(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1543 _cell_measurement_temperature 298 _cell_measurement_pressure 710000 _cell_measurement_theta_max 15.2480 _cell_measurement_theta_min 2.0940 _shelx_estimated_absorpt_T_max 0.989 _shelx_estimated_absorpt_T_min 0.978 _exptl_absorpt_coefficient_mu 0.34 _exptl_absorpt_correction_T_max 0.4245 _exptl_absorpt_correction_T_min 0.3115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. The \l/2 correction factor is not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.035 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 744.68 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1334 _diffrn_reflns_av_unetI/netI 0.0659 _diffrn_reflns_Laue_measured_fraction_full 0.799 _diffrn_reflns_Laue_measured_fraction_max 0.799 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 482 _diffrn_reflns_point_group_measured_fraction_full 0.799 _diffrn_reflns_point_group_measured_fraction_max 0.799 _diffrn_reflns_theta_full 13.374 _diffrn_reflns_theta_max 13.374 _diffrn_reflns_theta_min 2.411 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 710000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.799 _diffrn_measured_fraction_theta_max 0.799 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -17.20 -10.00 0.20 0.40 -90.00 -11.00 0.00 -- 36 2 \w -128.40-120.60 0.20 0.40 -- -11.00 70.00 -24.23 39 3 \w -129.60-120.40 0.20 0.40 -- -11.00 70.00 155.77 46 4 \w -107.80 -95.80 0.20 0.40 -- 12.00 70.00 155.77 60 5 \w -105.40 -96.00 0.20 0.40 -- 12.00 70.00 -24.23 47 6 \w -61.80 -50.60 0.20 0.40 -- 12.00 -70.00 24.23 56 7 \w -58.40 -48.80 0.20 0.40 -- 12.00 -70.00-155.77 48 8 \w -83.80 -72.00 0.20 0.40 -- -11.00 -70.00-155.77 59 9 \w -85.00 -72.80 0.20 0.40 -- -11.00 -70.00 24.23 61 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'Diamond Light Source I19 EH2' _diffrn_measurement_method '\w and \f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0556990000 _diffrn_orient_matrix_UB_12 0.0089095000 _diffrn_orient_matrix_UB_13 0.0113244000 _diffrn_orient_matrix_UB_21 0.0339820000 _diffrn_orient_matrix_UB_22 0.0169448000 _diffrn_orient_matrix_UB_23 0.0071678000 _diffrn_orient_matrix_UB_31 -0.0112799000 _diffrn_orient_matrix_UB_32 0.0064879000 _diffrn_orient_matrix_UB_33 -0.0344157000 _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4859 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 395 _reflns_number_total 482 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 1.061 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.145 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 2.065 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 482 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1523 _refine_ls_R_factor_gt 0.1371 _refine_ls_restrained_S_all 2.010 _refine_ls_shift/su_max 0.862 _refine_ls_shift/su_mean 0.081 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4127 _refine_ls_wR_factor_ref 0.4424 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H7A,H7B,H7C} of C7, All C(H,H) groups At 1.5 times of: All C(H,H,H,H,H,H) groups, {H8A,H8B,H8C} of C8, All O(H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 O4-C8 1.35 with sigma of 0.01 O3-C9 1.4 with sigma of 0.01 O3-H3A 0.875 with sigma of 0.001 H3A-C9 1.806 with sigma of 0.001 C9-H3A 1.806 with sigma of 0.01 O5-H5B 0.875 with sigma of 0.001 H5B-H5A 1.35 with sigma of 0.001 O5-H5A 0.875 with sigma of 0.001 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uiso(O4) = Uiso(C8) Uiso(O3) = Uiso(C9) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.1675) O4(0.22) H4A(0.11) C8(0.22) H8A(0.22) H8B(0.22) H8C(0.22) C7(0.0825) H7A(0.0825) H7B(0.165) H7C(0.165) O3(0.075) C9(0.075) H9A(0.075) H9B(0.075) H9C(0.075) H5A(0.3434) H5B(0.1717) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C), C9(H9A,H9B,H9C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) 6.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C) 6.d Idealised tetrahedral OH refined as rotating group: O4(H4A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.028(3) Uani 1 4 d S T P C . O2 O 0.500000 0.250000 0.4251(7) 0.033(5) Uani 1 4 d DS T P . . O1 O 0.3497(6) 0.3120(2) 0.6010(4) 0.053(4) Uani 1 1 d D . . . . C2 C 0.500000 0.3687(2) 0.7206(4) 0.053(4) Uani 1 2 d DS T P . . C6 C 0.500000 0.4838(3) 0.9647(6) 0.053(4) Uani 1 2 d DS T P . . C1 C 0.500000 0.3278(3) 0.6346(5) 0.053(4) Uani 1 2 d DS T P C . C5 C 0.500000 0.4446(3) 0.8815(5) 0.053(4) Uani 1 2 d DS T P . . C3 C 0.6630(6) 0.3879(2) 0.7614(4) 0.053(4) Uani 1 1 d D . . . . H3 H 0.773048 0.375408 0.734902 0.063 Uiso 1 1 calc R U . . . C4 C 0.6629(6) 0.4254(2) 0.8406(4) 0.053(4) Uani 1 1 d D . . . . H4 H 0.772942 0.437908 0.866995 0.063 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3587(7) 0.063 Uiso 0.67 4 d DS U P A 1 O4 O -0.045(9) 0.4694(14) 0.619(2) 0.096(13) Uiso 0.22 1 d D . P B -1 H4A H 0.014832 0.470420 0.671807 0.144 Uiso 0.11 1 calc R U P B -1 C8 C 0.037(11) 0.436(3) 0.552(4) 0.096(13) Uiso 0.22 1 d D . P B -1 H8A H -0.039579 0.430984 0.493465 0.144 Uiso 0.22 1 calc R U P B -1 H8B H 0.059053 0.399853 0.582465 0.144 Uiso 0.22 1 calc R U P B -1 H8C H 0.151055 0.451730 0.531389 0.144 Uiso 0.22 1 calc R U P B -1 C7 C 0.500000 0.250000 0.3190(10) 0.033(5) Uani 0.33 4 d DS T P C 2 H7A H 0.376765 0.250000 0.294697 0.039 Uiso 0.165 2 calc R U P C 2 H7B H 0.561617 0.282682 0.294697 0.039 Uiso 0.165 1 calc R U P C 2 H7C H 0.561617 0.217318 0.294697 0.039 Uiso 0.165 1 calc R U P C 2 O3 O 0.500000 0.250000 0.875(2) 0.14(3) Uiso 0.3 4 d DS . P . . O5 O 1.000000 0.3582(14) 0.923(5) 0.48(15) Uiso 0.49(15) 2 d DS . . . . C9 C 0.684(2) 0.250000 0.846(2) 0.14(3) Uiso 0.15 2 d DS . P . . H9A H 0.759308 0.250000 0.905067 0.209 Uiso 0.075 1 calc R U P D -1 H9B H 0.708732 0.217318 0.805967 0.209 Uiso 0.075 1 calc R U P D -1 H9C H 0.708732 0.282682 0.805967 0.209 Uiso 0.075 1 calc R U P D -1 H3A H 0.500000 0.2275(19) 0.927(2) 0.209 Uiso 1 2 d DS U P . . H5A H 1.1168(10) 0.3511(18) 0.922(8) 0.209 Uiso 0.3434 1 d D U P . . H5B H 1.000000 0.3922(12) 0.947(6) 0.209 Uiso 0.3434 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 Sc1 0.033(6) 0.027(4) 0.024(3) 0.000 -0.0061(19) 0.000 O2 0.044(16) 0.036(9) 0.018(6) 0.000 0.000 0.000 O1 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C2 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C6 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C1 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C5 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C3 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C4 0.040(9) 0.065(5) 0.052(4) -0.026(2) 0.003(4) -0.003(3) C7 0.044(16) 0.036(9) 0.018(6) 0.000 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 Sc1 Sc1 3.6723(9) 2 ? Sc1 Sc1 3.6722(10) 2_655 ? Sc1 O2 2.085(5) 13_556 ? Sc1 O2 2.085(5) . ? Sc1 O1 2.126(5) . ? Sc1 O1 2.126(5) 11_565 ? Sc1 O1 2.126(5) 13_556 ? Sc1 O1 2.126(5) 7_546 ? O2 H2 0.8750(11) . ? O2 C7 1.398(9) . ? O1 C1 1.249(5) . ? C2 C1 1.498(8) . ? C2 C3 1.391(5) . ? C2 C3 1.391(5) 12_655 ? C6 C6 1.212(18) 4_567 ? C6 C5 1.445(8) . ? C5 C4 1.391(5) 12_655 ? C5 C4 1.391(5) . ? C3 H3 0.9300 . ? C3 C4 1.376(7) . ? C4 H4 0.9300 . ? O4 H4A 0.9161 . ? O4 C8 1.348(11) . ? C8 H8A 0.9638 . ? C8 H8B 0.9651 . ? C8 H8C 0.9648 . ? C7 H7A 0.9600 12_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9599 2_655 ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7 H7C 0.9600 2_655 ? O3 C9 1.403(10) . ? O3 C9 1.403(10) 2_655 ? O3 H3A 0.8751(11) 2_655 ? O3 H3A 0.8750(11) . ? O5 H5A 0.8750(12) 12_755 ? O5 H5A 0.8750(12) . ? O5 H5B 0.8753(11) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 151.7(2) 13_556 2_655 ? O2 Sc1 Sc1 151.7(2) . 2 ? O2 Sc1 Sc1 28.3(2) 13_556 2 ? O2 Sc1 Sc1 28.3(2) . 2_655 ? O2 Sc1 O2 180.0 . 13_556 ? O2 Sc1 O1 90.4(2) 13_556 11_565 ? O2 Sc1 O1 89.6(2) . 11_565 ? O2 Sc1 O1 90.4(2) . 13_556 ? O2 Sc1 O1 89.6(2) 13_556 13_556 ? O2 Sc1 O1 90.4(2) 13_556 . ? O2 Sc1 O1 89.6(2) 13_556 7_546 ? O2 Sc1 O1 90.4(2) . 7_546 ? O2 Sc1 O1 89.6(2) . . ? O1 Sc1 Sc1 110.14(13) 13_556 2_655 ? O1 Sc1 Sc1 69.86(13) . 2_655 ? O1 Sc1 Sc1 110.14(13) 7_546 2_655 ? O1 Sc1 Sc1 69.86(13) 7_546 2 ? O1 Sc1 Sc1 69.86(13) 11_565 2_655 ? O1 Sc1 Sc1 110.14(13) 11_565 2 ? O1 Sc1 Sc1 110.14(13) . 2 ? O1 Sc1 Sc1 69.86(13) 13_556 2 ? O1 Sc1 O1 180.0(2) 11_565 7_546 ? O1 Sc1 O1 180.0 13_556 . ? O1 Sc1 O1 88.8(3) 13_556 7_546 ? O1 Sc1 O1 91.2(3) 7_546 . ? O1 Sc1 O1 88.8(3) 11_565 . ? O1 Sc1 O1 91.2(3) 13_556 11_565 ? Sc1 O2 Sc1 123.5(5) 2_655 . ? Sc1 O2 H2 118.3(2) . . ? Sc1 O2 H2 118.3(2) 2_655 . ? C7 O2 Sc1 118.3(2) . . ? C1 O1 Sc1 137.7(5) . . ? C3 C2 C1 120.6(3) 12_655 . ? C3 C2 C1 120.6(3) . . ? C3 C2 C3 118.8(6) . 12_655 ? C6 C6 C5 179.3(5) 4_567 . ? O1 C1 O1 124.3(8) . 12_655 ? O1 C1 C2 117.8(4) . . ? O1 C1 C2 117.8(4) 12_655 . ? C4 C5 C6 120.7(3) 12_655 . ? C4 C5 C6 120.7(3) . . ? C4 C5 C4 118.6(6) 12_655 . ? C2 C3 H3 119.7 . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3 119.7 . . ? C5 C4 H4 119.6 . . ? C3 C4 C5 120.7(4) . . ? C3 C4 H4 119.6 . . ? C8 O4 H4A 119.6 . . ? O4 C8 H8A 108.4 . . ? O4 C8 H8B 111.2 . . ? O4 C8 H8C 110.4 . . ? H8A C8 H8B 108.7 . . ? H8A C8 H8C 109.2 . . ? H8B C8 H8C 109.0 . . ? O2 C7 H7A 109.471(6) . 12_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.471(3) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7C 109.471(3) . 2_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 O3 C9 148(3) . 2_655 ? C9 O3 H3A 102.4(7) 2_655 2_655 ? C9 O3 H3A 102.4(8) 2_655 . ? C9 O3 H3A 102.4(8) . 2_655 ? C9 O3 H3A 102.4(7) . . ? H3A O3 H3A 76(8) . 2_655 ? H5A O5 H5A 157(5) . 12_755 ? H5A O5 H5B 100.96(17) . . ? H5B O5 H5A 100.96(17) . 12_755 ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 10.5(3) . . . 12_655 ? Sc1 O1 C1 C2 -169.7(3) . . . . ? C2 C3 C4 C5 0.1(2) . . . . ? C6 C5 C4 C3 179.85(19) . . . . ? C1 C2 C3 C4 -179.87(18) . . . . ? C3 C2 C1 O1 0.16(13) 12_655 . . . ? C3 C2 C1 O1 179.98(8) 12_655 . . 12_655 ? C3 C2 C1 O1 -179.98(8) . . . . ? C3 C2 C1 O1 -0.16(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 -0.1(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns_a.res in Cmma 710mpa.res created by SHELXL-2019/2 at 09:39:57 on 24-Oct-2022 REM Old TITL fullruns in Cmma REM SHELXT solution in Cmma: R1 0.201, Rweak 0.004, Alpha 0.036 REM 0.321 for 19 systematic absences, Orientation as input REM Formula found by SHELXT: C16 O7 Sc CELL 0.4859 7.3445 23.9839 13.177 90 90 90 ZERR 2 0.0019 0.0034 0.0013 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 70.04 73.44 28.08 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z EQIV $3 1-X,0.5-Y,+Z EQIV $4 +X,0.5-Y,+Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 DFIX 1.35 0.01 O4 C8 EADP O4 C8 DFIX 1.4 0.01 O3 C9 EADP O3 C9 DFIX 0.875 0.001 O3 H3a DFIX 1.806 0.001 H3a C9 DFIX 1.806 0.01 C9 H3a DFIX 0.875 0.001 O5 H5b DFIX 1.35 0.001 H5b H5a DFIX 0.875 0.001 O5 H5a EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF FREE H7a H7b_$4 FREE H7b H7c_$3 FREE H7b H7a_$1 FREE H7b H7a_$3 FREE H7b H7c FREE H7b H7b_$1 FREE H7c H7a_$4 FREE H7c H7a BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 0 2 OMIT 0 4 0 OMIT 1 7 4 OMIT 0 6 1 OMIT 0 8 2 OMIT 1 3 3 OMIT 0 2 1 OMIT 4 8 0 OMIT 0 6 0 OMIT 0 18 0 OMIT 0 10 1 OMIT 0 10 0 REM REM REM WGHT 0.200000 FVAR 1.10821 SC1 4 0.250000 0.250000 0.500000 10.25000 0.03291 0.02736 = 0.02394 0.00000 -0.00612 0.00000 O2 3 0.500000 0.250000 0.425057 10.25000 0.04400 0.03631 = 0.01751 0.00000 0.00000 0.00000 O1 3 0.349661 0.312004 0.601020 11.00000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 C2 1 0.500000 0.368661 0.720617 10.50000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 C6 1 0.500000 0.483800 0.964719 10.50000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 C1 1 0.500000 0.327843 0.634601 10.50000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 C5 1 0.500000 0.444615 0.881455 10.50000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 C3 1 0.663030 0.387931 0.761386 11.00000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 AFIX 43 H3 2 0.773048 0.375408 0.734902 11.00000 -1.20000 AFIX 0 C4 1 0.662927 0.425356 0.840553 11.00000 0.04027 0.06545 = 0.05218 -0.02633 0.00257 -0.00262 AFIX 43 H4 2 0.772942 0.437908 0.866995 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.358653 10.16750 -1.20000 PART -1 O4 3 -0.045242 0.469351 0.619389 10.22000 0.09573 AFIX 147 H4A 2 0.014832 0.470420 0.671807 10.11000 -1.50000 AFIX 0 C8 1 0.037259 0.435547 0.551813 10.22000 0.09573 AFIX 137 H8A 2 -0.039579 0.430984 0.493465 10.22000 -1.50000 H8B 2 0.059053 0.399853 0.582465 10.22000 -1.50000 H8C 2 0.151055 0.451730 0.531389 10.22000 -1.50000 AFIX 0 PART 2 C7 1 0.500000 0.250000 0.318982 10.08250 0.04400 0.03631 = 0.01751 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.376765 0.250000 0.294697 10.08250 -1.20000 H7B 2 0.561617 0.282682 0.294697 10.16500 -1.20000 H7C 2 0.561617 0.217318 0.294697 10.16500 -1.20000 AFIX 0 PART 0 O3 3 0.500000 0.250000 0.874767 10.07500 0.13931 O5 3 1.000000 0.358208 0.922892 0.24540 0.47976 C9 1 0.683683 0.250000 0.845644 10.07500 0.13931 PART -1 AFIX 33 H9A 2 0.759308 0.250000 0.905067 10.07500 -1.50000 H9B 2 0.708732 0.217318 0.805967 10.07500 -1.50000 H9C 2 0.708732 0.282682 0.805967 10.07500 -1.50000 AFIX 0 PART 0 H3A 2 0.500000 0.227509 0.927052 10.50000 -1.50000 H5A 2 1.116796 0.351052 0.921541 10.34340 -1.50000 H5B 2 1.000000 0.392190 0.947113 10.17170 -1.50000 HKLF 4 REM fullruns_a.res in Cmma REM wR2 = 0.4424, GooF = S = 2.065, Restrained GooF = 2.010 for all data REM R1 = 0.1371 for 395 Fo > 4sig(Fo) and 0.1523 for all 482 data REM 58 parameters refined using 36 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.061, deepest hole -0.489, 1-sigma level 0.145 Q1 1 0.5000 0.2228 0.2077 10.50000 0.05 0.77 Q2 1 0.0000 0.4204 0.5750 10.50000 0.05 0.74 ; _shelx_res_checksum 78782 _olex2_exptl_crystal_mounting_method ; The crystal is loaded in a miniature Merrill-Bassett diamond anvil cell in a hydrostatic medium of MeOH ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 34.783 _oxdiff_exptl_absorpt_empirical_full_min 0.339 #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_470MPa _database_code_depnum_ccdc_archive 'CCDC 2223545' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-04 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C32 H18 O10, (C3 H7 N O), 1.3(C H4 O)' _chemical_formula_sum 'Sc2 C35.8 H29.7 N O12.3' _chemical_formula_weight 761.36 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.000 Why? PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.37 Report PLAT088_ALERT_3_B Poor Data / Parameter Ratio .................... 7.22 Note The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- SHFSU01_ALERT_2_A The absolute value of parameter shift to su ratio > 0.20 PLAT080_ALERT_2_A Maximum Shift/Error ............................ 0.67 Why ? There is adsorbed solvate disordered over a special positiona in partially occupied sites, making them difficult to refine. The molecules were either placed as a rigid fragment or had it geometry restrained, and its occupancy set to its approximately refined value. #------------------------------------------------------------------------------- PLPLAT051_ALERT_1_A Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 68.08 % The formula was ammended to properly account for the solvate. #------------------------------------------------------------------------------- PLAT733_ALERT_1_A Torsion Calc 0.2(11), Rep 0.04(13) ...... 8.46 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_A Torsion Calc -0.2(11), Rep -0.04(13) ...... 8.46 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 7 Check PLAT733_ALERT_1_A Torsion Calc -179.9(7), Rep 180.00(8) ...... 8.75 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 12_655 # 8 Check PLAT733_ALERT_1_A Torsion Calc 179.9(7), Rep 180.00(8) ...... 8.75 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 1_555 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.510 283 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 13.26 0.500 0.582 662 385 277 13.53 0.510 0.579 694 402 292 #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' N N -0.0008 0.0012 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.3205(15) _cell_length_b 26.609(5) _cell_length_c 11.922(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2322.2(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1173 _cell_measurement_temperature 298 _cell_measurement_pressure 470000 _cell_measurement_theta_min 1.5850 _cell_measurement_theta_max 15.5720 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.34 _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_correction_T_min 0.3664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1122 before and 0.0733 after correction. The Ratio of minimum to maximum transmission is 0.4925. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 791.68 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1160 _diffrn_reflns_av_unetI/netI 0.1449 _diffrn_reflns_Laue_measured_fraction_full 0.499 _diffrn_reflns_Laue_measured_fraction_max 0.499 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 999 _diffrn_reflns_point_group_measured_fraction_full 0.499 _diffrn_reflns_point_group_measured_fraction_max 0.499 _diffrn_reflns_theta_full 13.533 _diffrn_reflns_theta_max 13.533 _diffrn_reflns_theta_min 2.417 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 470000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 230 _reflns_number_total 368 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.457 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.094 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.299 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 51 _refine_ls_number_reflns 368 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.1393 _refine_ls_restrained_S_all 1.293 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3403 _refine_ls_wR_factor_ref 0.3704 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 O4-C10 1.35 with sigma of 0.01 N1-C8 \\sim N1-C9 with sigma of 0.02 3. Restrained planarity C7, O3, N1, C8, C9 with sigma of 0.1 C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints C7 \\sim O3 \\sim N1 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uiso(O3) = Uiso(C7) = Uiso(N1) = Uiso(C8) = Uiso(C9) Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uiso(O4) = Uiso(C10) Uanis(C2) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C6) = Uanis(C3) 5. Rigid body (RIGU) restrains C7, O3, N1, C8, C9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: C7(0.065) O3(0.065) N1(0.13) C8(0.13) H8A(0.13) H8B(0.13) H8C(0.13) C9(0.065) H9A(0.065) H9B(0.065) H9C(0.065) O4(0.22) H4A(0.22) C10(0.22) H10A(0.22) H10B(0.22) H10C(0.22) 7.a Free rotating group: C7(O3,N1,C8,C9) 7.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) 7.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C) 7.d Idealised tetrahedral OH refined as rotating group: O4(H4A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.034(3) Uani 1 4 d S T P . . O2 O 0.500000 0.250000 0.4210(11) 0.049(9) Uani 1 4 d DS T P . . O1 O 0.3489(6) 0.3062(3) 0.6123(6) 0.056(4) Uani 1 1 d D . . . . C2 C 0.500000 0.3646(3) 0.7289(6) 0.056(4) Uani 1 2 d DS T P . . C6 C 0.500000 0.4830(3) 0.9658(6) 0.056(4) Uani 1 2 d DS T P . . C1 C 0.500000 0.3227(3) 0.6453(6) 0.056(4) Uani 1 2 d DS T P . . C5 C 0.500000 0.4426(3) 0.8850(6) 0.056(4) Uani 1 2 d DS T P . . C3 C 0.6637(6) 0.3842(3) 0.7683(5) 0.056(4) Uani 1 1 d D . . . . H3 H 0.773946 0.371316 0.742446 0.067 Uiso 1 1 calc R U . . . C4 C 0.6636(6) 0.4230(3) 0.8457(5) 0.056(4) Uani 1 1 d D . . . . H4 H 0.773792 0.435920 0.871617 0.067 Uiso 1 1 calc R U . . . C7 C 0.48(2) 0.294(2) 1.084(4) 0.016(10) Uiso 0.065 1 d G U P A -1 O3 O 0.49(3) 0.295(2) 1.188(4) 0.016(10) Uiso 0.065 1 d G U P A -1 N1 N 0.561(9) 0.2566(19) 1.016(2) 0.016(10) Uiso 0.13 1 d DG U P A -1 C8 C 0.580(11) 0.263(3) 0.895(2) 0.016(10) Uiso 0.13 1 d DG U P A -1 H8A H 0.476528 0.281196 0.866330 0.024 Uiso 0.13 1 calc R U P A -1 H8B H 0.588157 0.231015 0.859360 0.024 Uiso 0.13 1 calc R U P A -1 H8C H 0.689575 0.282115 0.879497 0.024 Uiso 0.13 1 calc R U P A -1 C9 C 0.63(3) 0.211(4) 1.066(5) 0.016(10) Uiso 0.065 1 d DG U P A -1 H9A H 0.595214 0.210319 1.143856 0.024 Uiso 0.065 1 calc R U P A -1 H9B H 0.756090 0.208842 1.057124 0.024 Uiso 0.065 1 calc R U P A -1 H9C H 0.569786 0.182725 1.028727 0.024 Uiso 0.065 1 calc R U P A -1 H2 H 0.500000 0.250000 0.3476(11) 0.019 Uiso 1 4 d DS U P . . O4 O -0.065(15) 0.462(3) 0.608(5) 0.15(3) Uiso 0.22 1 d D . P B -1 H4A H 0.006398 0.478351 0.646774 0.221 Uiso 0.22 1 calc R U P B -1 C10 C 0.030(19) 0.432(4) 0.538(8) 0.15(3) Uiso 0.22 1 d D . P B -1 H10A H -0.039937 0.402111 0.523155 0.221 Uiso 0.22 1 calc R U P B -1 H10B H 0.143743 0.422821 0.572489 0.221 Uiso 0.22 1 calc R U P B -1 H10C H 0.052974 0.449361 0.469163 0.221 Uiso 0.22 1 calc R U P B -1 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 Sc1 0.008(8) 0.041(4) 0.054(4) 0.000 0.000(4) 0.000 O2 0.05(3) 0.063(16) 0.033(10) 0.000 0.000 0.000 O1 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(4) C2 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(4) C6 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(4) C1 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(4) C5 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(4) C3 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(4) C4 0.026(12) 0.064(6) 0.079(5) -0.024(4) 0.006(6) 0.006(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 Sc1 Sc1 3.6602(7) 2 ? Sc1 Sc1 3.6602(7) 2_655 ? Sc1 O2 2.058(6) . ? Sc1 O2 2.058(6) 13_556 ? Sc1 O1 2.134(7) 7_546 ? Sc1 O1 2.134(7) 13_556 ? Sc1 O1 2.134(7) 11_565 ? Sc1 O1 2.134(7) . ? O2 H2 0.8750(11) . ? O1 C1 1.253(5) . ? C2 C1 1.495(8) . ? C2 C3 1.389(5) 12_655 ? C2 C3 1.389(5) . ? C6 C6 1.22(2) 4_567 ? C6 C5 1.445(8) . ? C5 C4 1.388(5) . ? C5 C4 1.388(5) 12_655 ? C3 H3 0.9300 . ? C3 C4 1.383(7) . ? C4 H4 0.9300 . ? C7 O3 1.2380 . ? C7 N1 1.4032 . ? N1 C8 1.4649 . ? N1 C9 1.4339 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? O4 H4A 0.8200 . ? O4 C10 1.350(11) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 27.2(3) . 2_655 ? O2 Sc1 Sc1 27.2(3) 13_556 2 ? O2 Sc1 Sc1 152.8(3) . 2 ? O2 Sc1 Sc1 152.8(3) 13_556 2_655 ? O2 Sc1 O2 180.0 13_556 . ? O2 Sc1 O1 89.2(3) . 11_565 ? O2 Sc1 O1 90.8(3) 13_556 11_565 ? O2 Sc1 O1 89.2(3) 13_556 13_556 ? O2 Sc1 O1 90.8(3) . 13_556 ? O2 Sc1 O1 89.2(3) . . ? O2 Sc1 O1 90.8(3) . 7_546 ? O2 Sc1 O1 89.2(3) 13_556 7_546 ? O2 Sc1 O1 90.8(3) 13_556 . ? O1 Sc1 Sc1 70.17(15) 11_565 2_655 ? O1 Sc1 Sc1 70.17(15) 13_556 2 ? O1 Sc1 Sc1 109.83(15) 13_556 2_655 ? O1 Sc1 Sc1 70.17(15) 7_546 2 ? O1 Sc1 Sc1 109.83(15) 7_546 2_655 ? O1 Sc1 Sc1 109.83(15) 11_565 2 ? O1 Sc1 Sc1 70.17(15) . 2_655 ? O1 Sc1 Sc1 109.83(15) . 2 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? O1 Sc1 O1 91.0(4) 7_546 . ? O1 Sc1 O1 91.0(4) 13_556 11_565 ? O1 Sc1 O1 89.0(4) 11_565 . ? O1 Sc1 O1 89.0(4) 13_556 7_546 ? O1 Sc1 O1 180.0 13_556 . ? Sc1 O2 Sc1 125.5(6) 2_655 . ? Sc1 O2 H2 117.2(3) 2_655 . ? Sc1 O2 H2 117.2(3) . . ? C1 O1 Sc1 137.9(6) . . ? C3 C2 C1 120.4(3) 12_655 . ? C3 C2 C1 120.4(3) . . ? C3 C2 C3 119.2(7) . 12_655 ? C6 C6 C5 179.8(5) 4_567 . ? O1 C1 O1 123.9(9) . 12_655 ? O1 C1 C2 118.0(5) 12_655 . ? O1 C1 C2 118.0(5) . . ? C4 C5 C6 120.3(3) 12_655 . ? C4 C5 C6 120.3(3) . . ? C4 C5 C4 119.3(7) 12_655 . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C5 C4 H4 119.8 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.8 . . ? O3 C7 N1 124.8 . . ? C7 N1 C8 121.5 . . ? C7 N1 C9 120.1 . . ? C9 N1 C8 118.4 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 O4 H4A 109.5 . . ? O4 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? O4 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 0.0(4) . . . 12_655 ? Sc1 O1 C1 C2 180.0(4) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C6 C5 C4 C3 179.99(19) . . . . ? C1 C2 C3 C4 -179.97(19) . . . . ? C3 C2 C1 O1 0.04(13) 12_655 . . . ? C3 C2 C1 O1 -0.04(13) . . . 12_655 ? C3 C2 C1 O1 180.00(8) 12_655 . . 12_655 ? C3 C2 C1 O1 180.00(8) . . . . ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.0(3) 12_655 . . . ? O3 C7 N1 C8 -167.19(12) . . . . ? O3 C7 N1 C9 11.57(8) . . . . ? _shelx_res_file ; TITL sad in Cmma mil53scedb_solvent.res created by SHELXL-2018/3 at 08:46:34 on 04-Oct-2022 CELL 0.4589 7.32046 26.60864 11.92163 90 90 90 ZERR 2 0.00146 0.00532 0.00238 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H N O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP N -0.0008 0.0012 8.1428 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 71.68 59.44 2.08 24.56 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z FLAT C7 O3 N1 C8 C9 SADI N1 C8 N1 C9 RIGU C7 O3 N1 C8 C9 SIMU C7 O3 N1 C8 C9 EADP O3 C7 N1 C8 C9 DFIX 0.875 0.001 O2 H2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 DFIX 1.35 0.01 O4 C10 EADP O4 C10 EADP C2 C1 C5 C4 C6 C3 L.S. 10 PLAN 3 SIZE 0.04 0.04 0.15 TEMP 0 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 1 1 1 OMIT 3 3 1 OMIT 4 24 7 OMIT 3 21 7 OMIT 2 16 7 OMIT 1 19 8 OMIT 2 6 11 OMIT 2 20 7 OMIT 2 12 4 OMIT 0 10 6 OMIT 4 22 1 OMIT 3 17 1 OMIT 2 4 10 OMIT 3 7 9 OMIT 3 3 7 OMIT 1 23 1 OMIT 0 2 1 OMIT 3 13 8 OMIT 3 15 1 OMIT 3 17 8 OMIT 3 23 2 REM REM REM WGHT 0.200000 FVAR 3.62210 SC1 5 0.250000 0.250000 0.500000 10.25000 0.00770 0.04140 = 0.05378 0.00000 0.00016 0.00000 O2 4 0.500000 0.250000 0.420990 10.25000 0.05015 0.06265 = 0.03321 0.00000 0.00000 0.00000 O1 4 0.348906 0.306199 0.612329 11.00000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 C2 1 0.500000 0.364562 0.728945 10.50000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 C6 1 0.500000 0.483029 0.965836 10.50000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 C1 1 0.500000 0.322690 0.645311 10.50000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 C5 1 0.500000 0.442592 0.884963 10.50000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 C3 1 0.663685 0.384246 0.768301 11.00000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 AFIX 43 H3 2 0.773946 0.371316 0.742446 11.00000 -1.20000 AFIX 0 C4 1 0.663594 0.422966 0.845719 11.00000 0.02607 0.06354 = 0.07865 -0.02366 0.00570 0.00580 AFIX 43 H4 2 0.773792 0.435920 0.871617 11.00000 -1.20000 AFIX 6 PART -1 C7 1 0.484183 0.294196 1.084161 10.06500 0.01601 O3 4 0.491204 0.294927 1.187901 10.06500 0.01601 N1 3 0.560973 0.256648 1.016291 10.13000 0.01601 C8 1 0.580490 0.263318 0.894911 10.13000 0.01601 AFIX 137 H8A 2 0.476528 0.281196 0.866330 10.13000 -1.50000 H8B 2 0.588157 0.231015 0.859360 10.13000 -1.50000 H8C 2 0.689575 0.282115 0.879497 10.13000 -1.50000 AFIX 5 C9 1 0.625878 0.210850 1.065571 10.06500 0.01601 AFIX 137 H9A 2 0.595214 0.210319 1.143856 10.06500 -1.50000 H9B 2 0.756090 0.208842 1.057124 10.06500 -1.50000 H9C 2 0.569786 0.182725 1.028727 10.06500 -1.50000 AFIX 0 PART 0 H2 2 0.500000 0.250000 0.347594 10.25000 -1.20000 PART -1 O4 4 -0.064988 0.462074 0.608177 10.22000 0.14716 AFIX 147 H4A 2 0.006398 0.478351 0.646774 10.22000 -1.50000 AFIX 0 C10 1 0.029788 0.431915 0.538196 10.22000 0.14716 AFIX 137 H10A 2 -0.039937 0.402111 0.523155 10.22000 -1.50000 H10B 2 0.143743 0.422821 0.572489 10.22000 -1.50000 H10C 2 0.052974 0.449361 0.469163 10.22000 -1.50000 AFIX 0 HKLF 4 REM sad in Cmma REM wR2 = 0.3704, GooF = S = 1.299, Restrained GooF = 1.293 for all data REM R1 = 0.1393 for 230 Fo > 4sig(Fo) and 0.1788 for all 368 data REM 51 parameters refined using 34 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.457, deepest hole -0.460, 1-sigma level 0.094 Q1 1 0.5000 0.2793 1.1781 10.50000 0.05 0.46 Q2 1 0.5000 0.3727 0.7079 10.50000 0.05 0.43 Q3 1 0.5000 0.1847 0.9590 10.50000 0.05 0.34 ; _shelx_res_checksum 38293 _olex2_submission_special_instructions 'No special instructions were received' #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_2130MPa _database_code_depnum_ccdc_archive 'CCDC 2223546' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.4 H21.1 O10, 4.10(C H4 O), 1.38(H2 O)' _chemical_formula_sum 'Sc2 C37.5 H41.26 O15.48' _chemical_formula_weight 829.57 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4412 RINTA01_ALERT_3_B The value of Rint is greater than 0.18 Rint given 0.19 PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.43 Report PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.851 Why? PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.1 Note The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The formula was ammended to account for the solvate that was calculated from SQUEEZE. The composition of the disordered solvate was approximated from a rough model of the solvate positions, which was then removed from the model and SQUEEZE performed. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.417 62 Report No information given in structure factor report. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.66 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.1(10), Rep 0.05(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -0.1(10), Rep -0.05(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.290(3) _cell_length_b 22.957(4) _cell_length_c 13.4286(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2247.4(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 774 _cell_measurement_temperature 298 _cell_measurement_pressure 2130000 _cell_measurement_theta_min 1.5900 _cell_measurement_theta_max 13.2510 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.36 _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_correction_T_min 0.1769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. The \l/2 correction factor is not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 864.2 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1913 _diffrn_reflns_av_unetI/netI 0.0728 _diffrn_reflns_Laue_measured_fraction_full 0.816 _diffrn_reflns_Laue_measured_fraction_max 0.817 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3192 _diffrn_reflns_point_group_measured_fraction_full 0.816 _diffrn_reflns_point_group_measured_fraction_max 0.817 _diffrn_reflns_theta_full 11.680 _diffrn_reflns_theta_max 11.680 _diffrn_reflns_theta_min 1.596 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 2130000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.816 _diffrn_measured_fraction_theta_max 0.817 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 265 _reflns_number_total 325 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.544 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.108 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.905 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 330 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.1425 _refine_ls_restrained_S_all 1.829 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4148 _refine_ls_wR_factor_ref 0.4296 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.0775) C7(0.1725) H7A(0.1725) H7B(0.345) H7C(0.345) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.073(4) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4259(8) 0.068(7) Uani 1 4 d DS T P . . O1 O 0.3485(6) 0.3146(3) 0.5968(5) 0.103(5) Uani 1 1 d D . . . . C2 C 0.500000 0.3705(3) 0.7182(5) 0.103(5) Uani 1 2 d DS T P . . C6 C 0.500000 0.4841(3) 0.9650(6) 0.103(5) Uani 1 2 d DS T P . . C1 C 0.500000 0.3301(3) 0.6306(6) 0.103(5) Uani 1 2 d DS T P B . C5 C 0.500000 0.4453(3) 0.8807(6) 0.103(5) Uani 1 2 d DS T P . . C3 C 0.6645(6) 0.3893(3) 0.7590(5) 0.103(5) Uani 1 1 d D . . . . H3 H 0.775043 0.376837 0.731899 0.123 Uiso 1 1 calc R U . . . C4 C 0.6646(6) 0.4265(3) 0.8399(5) 0.103(5) Uani 1 1 d D . . . . H4 H 0.775205 0.439038 0.866996 0.123 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3608(8) 0.123 Uiso 0.31 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3217(9) 0.068(7) Uani 0.69 4 d DS T P B 2 H7A H 0.375845 0.250000 0.297906 0.082 Uiso 0.345 2 calc R U P B 2 H7B H 0.562078 0.284144 0.297907 0.082 Uiso 0.345 1 calc R U P B 2 H7C H 0.562078 0.215856 0.297907 0.082 Uiso 0.345 1 calc R U P B 2 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 Sc1 0.137(9) 0.056(6) 0.027(5) 0.000 -0.001(3) 0.000 O2 0.11(2) 0.074(12) 0.017(8) 0.000 0.000 0.000 O1 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C2 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C6 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C1 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C5 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C3 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C4 0.159(13) 0.097(7) 0.051(6) -0.025(3) 0.003(6) 0.005(5) C7 0.11(2) 0.074(12) 0.017(8) 0.000 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 Sc1 Sc1 3.6450(13) 2_655 ? Sc1 Sc1 3.6450(13) 2 ? Sc1 O2 2.076(5) 13_556 ? Sc1 O2 2.076(5) . ? Sc1 O1 2.098(6) 7_546 ? Sc1 O1 2.098(6) . ? Sc1 O1 2.098(6) 13_556 ? Sc1 O1 2.098(6) 11_565 ? O2 H2 0.8750(11) . ? O2 C7 1.399(9) . ? O1 C1 1.246(5) . ? C2 C1 1.497(8) . ? C2 C3 1.388(5) 12_655 ? C2 C3 1.388(5) . ? C6 C6 1.19(2) 4_567 ? C6 C5 1.440(8) . ? C5 C4 1.388(5) 12_655 ? C5 C4 1.388(5) . ? C3 H3 0.9300 . ? C3 C4 1.381(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 28.6(3) . 2_655 ? O2 Sc1 Sc1 151.4(3) . 2 ? O2 Sc1 Sc1 28.6(3) 13_556 2 ? O2 Sc1 Sc1 151.4(3) 13_556 2_655 ? O2 Sc1 O2 180.0 . 13_556 ? O2 Sc1 O1 90.2(2) 13_556 . ? O2 Sc1 O1 89.8(2) . . ? O2 Sc1 O1 90.2(2) 13_556 11_565 ? O2 Sc1 O1 90.2(2) . 13_556 ? O2 Sc1 O1 89.8(2) 13_556 13_556 ? O2 Sc1 O1 89.8(2) 13_556 7_546 ? O2 Sc1 O1 90.2(2) . 7_546 ? O2 Sc1 O1 89.8(2) . 11_565 ? O1 Sc1 Sc1 69.98(14) 11_565 2_655 ? O1 Sc1 Sc1 69.98(14) . 2_655 ? O1 Sc1 Sc1 110.02(14) 13_556 2_655 ? O1 Sc1 Sc1 69.98(14) 7_546 2 ? O1 Sc1 Sc1 69.98(14) 13_556 2 ? O1 Sc1 Sc1 110.02(14) 11_565 2 ? O1 Sc1 Sc1 110.02(14) . 2 ? O1 Sc1 Sc1 110.02(14) 7_546 2_655 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? O1 Sc1 O1 89.9(4) 13_556 7_546 ? O1 Sc1 O1 90.1(4) 13_556 11_565 ? O1 Sc1 O1 89.9(4) 11_565 . ? O1 Sc1 O1 180.0(3) 13_556 . ? O1 Sc1 O1 90.1(4) 7_546 . ? Sc1 O2 Sc1 122.7(5) 2_655 . ? Sc1 O2 H2 118.6(2) . . ? Sc1 O2 H2 118.6(3) 2_655 . ? C7 O2 Sc1 118.6(3) . . ? C1 O1 Sc1 137.0(5) . . ? C3 C2 C1 120.2(3) 12_655 . ? C3 C2 C1 120.2(3) . . ? C3 C2 C3 119.6(6) . 12_655 ? C6 C6 C5 179.6(6) 4_567 . ? O1 C1 O1 124.7(9) . 12_655 ? O1 C1 C2 117.6(4) 12_655 . ? O1 C1 C2 117.6(4) . . ? C4 C5 C6 120.2(3) 12_655 . ? C4 C5 C6 120.2(3) . . ? C4 C5 C4 119.7(7) 12_655 . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3 119.9 . . ? C5 C4 H4 119.9 . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H4 119.9 . . ? O2 C7 H7A 109.469(8) . 2_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.469(4) . 12_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.469(3) . 2_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 14.7(4) . . . 12_655 ? Sc1 O1 C1 C2 -165.4(4) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C6 C5 C4 C3 179.97(19) . . . . ? C1 C2 C3 C4 -179.96(18) . . . . ? C3 C2 C1 O1 0.05(13) 12_655 . . . ? C3 C2 C1 O1 179.99(8) 12_655 . . 12_655 ? C3 C2 C1 O1 -179.99(8) . . . . ? C3 C2 C1 O1 -0.05(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.0(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns in Cmma mil53scedb_07.res created by SHELXL-2019/2 at 09:42:35 on 24-Oct-2022 CELL 0.4859 7.29004 22.95698 13.42864 90 90 90 ZERR 2 0.00267 0.00374 0.00138 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 66.76 47.04 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 4 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.200000 FVAR 4.54224 SC1 4 0.250000 0.250000 0.500000 10.25000 0.13660 0.05644 = 0.02680 0.00000 -0.00110 0.00000 O2 3 0.500000 0.250000 0.425916 10.25000 0.11314 0.07425 = 0.01700 0.00000 0.00000 0.00000 O1 3 0.348539 0.314569 0.596765 11.00000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 C2 1 0.500000 0.370509 0.718167 10.50000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 C6 1 0.500000 0.484126 0.964973 10.50000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 C1 1 0.500000 0.330130 0.630590 10.50000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 C5 1 0.500000 0.445338 0.880656 10.50000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 C3 1 0.664463 0.389330 0.759035 11.00000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 AFIX 43 H3 2 0.775043 0.376837 0.731899 11.00000 -1.20000 AFIX 0 C4 1 0.664613 0.426550 0.839866 11.00000 0.15919 0.09725 = 0.05133 -0.02538 0.00326 0.00512 AFIX 43 H4 2 0.775205 0.439038 0.866996 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.360756 10.07750 -1.20000 PART 2 C7 1 0.500000 0.250000 0.321736 10.17250 0.11314 0.07425 = 0.01700 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.375845 0.250000 0.297906 10.17250 -1.20000 H7B 2 0.562078 0.284144 0.297907 10.34500 -1.20000 H7C 2 0.562078 0.215856 0.297907 10.34500 -1.20000 AFIX 0 HKLF 4 REM fullruns in Cmma REM wR2 = 0.4296, GooF = S = 1.905, Restrained GooF = 1.829 for all data REM R1 = 0.1425 for 270 Fo > 4sig(Fo) and 0.1525 for all 330 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.544, deepest hole -0.512, 1-sigma level 0.108 Q1 1 0.5000 0.4563 0.8522 10.50000 0.05 0.54 Q2 1 0.5000 0.2500 0.6754 10.25000 0.05 0.45 Q3 1 0.5000 0.3806 0.6968 10.50000 0.05 0.44 Q4 1 0.6997 0.4023 0.9177 11.00000 0.05 0.37 ; _shelx_res_checksum 6254 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.046 0.250 0.000 247 100 ' ' 2 -0.046 0.750 0.000 247 100 ' ' 3 -0.055 0.500 0.500 252 73 ' ' 4 -0.055 1.000 0.500 252 73 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_230MPa _database_code_depnum_ccdc_archive 'CCDC 2223544' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-04 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.9 H22.2 O10, 1.6(C3 H7 N O), 0.2(C H4 O)' _chemical_formula_sum 'Sc2 C36.1 H28.4 N1.2 O11.7' _chemical_formula_weight 756.12 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.371 Why? The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT051_ALERT_1_A Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 68.05 % PLAT043_ALERT_1_B Calculated and Reported Mol. Weight Differ by .. 5.01 Check The formula was ammended to properly account for the solvate. #------------------------------------------------------------------------------- SHFSU01_ALERT_2_A The absolute value of parameter shift to su ratio > 0.20 Absolute value of the parameter shift to su ratio given 1.75 PLAT080_ALERT_2_A Maximum Shift/Error ............................ 1.75 Why ? There is DMF disordered over a special position and is in a partially occupied site, making it difficult to refine. The molecule was placed as a rigid fragment and its occupancy set to its approximately refined value. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc -0.1(8), Rep -0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc 0.1(8), Rep 0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 7 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.600 654 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 13.26 0.500 0.449 729 327 402 14.62 0.550 0.421 938 395 543 15.98 0.600 0.422 1146 484 662 16.68 0.625 0.426 1246 531 715 #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' N N -0.0008 0.0012 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.3533(15) _cell_length_b 26.584(5) _cell_length_c 11.879(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2322.2(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 433 _cell_measurement_temperature 298 _cell_measurement_pressure 230000 _cell_measurement_theta_min 2.2790 _cell_measurement_theta_max 17.4430 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.34 _exptl_absorpt_correction_T_max 0.7442 _exptl_absorpt_correction_T_min 0.5466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0815 before and 0.0636 after correction. The Ratio of minimum to maximum transmission is 0.7345. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 778 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_unetI/netI 0.0808 _diffrn_reflns_Laue_measured_fraction_full 0.371 _diffrn_reflns_Laue_measured_fraction_max 0.361 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1401 _diffrn_reflns_point_group_measured_fraction_full 0.371 _diffrn_reflns_point_group_measured_fraction_max 0.361 _diffrn_reflns_theta_full 15.982 _diffrn_reflns_theta_max 16.678 _diffrn_reflns_theta_min 2.574 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 230000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.371 _diffrn_measured_fraction_theta_max 0.361 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 320 _reflns_number_total 478 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.526 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 478 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.1025 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 1.746 _refine_ls_shift/su_mean 0.261 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2710 _refine_ls_wR_factor_ref 0.2879 _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups, H7 of C7, All O(H) groups At 1.2 times of: H2 of C9, H4 of C4, H3 of C3 2. Restrained distances O2-H2 0.875 with sigma of 0.001 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 O4-C10 1.35 with sigma of 0.01 N1-C8 \\sim N1-C9 with sigma of 0.02 3. Restrained planarity C7, O3, N1, C8, C9 with sigma of 0.1 C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints C7 \\sim O3 \\sim N1 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uiso(O3) = Uiso(C7) = Uiso(N1) = Uiso(C8) = Uiso(C9) Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uiso(O4) = Uiso(C10) 5. Rigid body (RIGU) restrains C7, O3, N1, C8, C9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: C7(0.1) H7(0.1) O3(0.1) N1(0.2) C8(0.2) H8A(0.2) H8B(0.2) H8C(0.2) C9(0.1) H9A(0.1) H9B(0.1) H9C(0.1) O4(0.125) H4A(0.125) C10(0.125) H10A(0.125) H10B(0.125) H10C(0.125) 7.a Free rotating group: C7(O3,N1,C8,C9) 7.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C7(H7) 7.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C) 7.d Idealised tetrahedral OH refined as rotating group: O4(H4A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.0248(11) Uani 1 4 d S T P . . O2 O 0.500000 0.250000 0.4181(9) 0.036(3) Uani 1 4 d DS T P . . O1 O 0.3492(4) 0.30589(19) 0.6113(5) 0.0450(17) Uani 1 1 d D . . . . C2 C 0.500000 0.3643(2) 0.7284(4) 0.0504(19) Uani 1 2 d DS T P . . C6 C 0.500000 0.4830(2) 0.9661(5) 0.0450(17) Uani 1 2 d DS T P . . C1 C 0.500000 0.3224(2) 0.6443(5) 0.0450(17) Uani 1 2 d DS T P . . C5 C 0.500000 0.4427(2) 0.8855(4) 0.0504(19) Uani 1 2 d DS T P . . C3 C 0.6629(5) 0.38418(18) 0.7682(4) 0.0504(19) Uani 1 1 d D . . . . H3 H 0.772629 0.371222 0.742152 0.060 Uiso 1 1 calc R U . . . C4 C 0.6637(5) 0.42277(18) 0.8455(4) 0.0504(19) Uani 1 1 d D . . . . H4 H 0.773678 0.435628 0.871354 0.060 Uiso 1 1 calc R U . . . C7 C 0.513(17) 0.2913(18) 1.095(2) 0.055(6) Uiso 0.1 1 d G U P A -1 H7 H 0.498580 0.323373 1.065233 0.083 Uiso 0.1 1 calc R U P A -1 O3 O 0.53(2) 0.2874(19) 1.198(2) 0.055(6) Uiso 0.1 1 d G U P A -1 N1 N 0.517(7) 0.2508(19) 1.0195(18) 0.055(6) Uiso 0.2 1 d DG U P A -1 C8 C 0.536(4) 0.259(2) 0.8985(17) 0.055(6) Uiso 0.2 1 d DG U P A -1 H8A H 0.477559 0.289707 0.877769 0.083 Uiso 0.2 1 calc R U P A -1 H8B H 0.480377 0.231359 0.858713 0.083 Uiso 0.2 1 calc R U P A -1 H8C H 0.662731 0.260491 0.879303 0.083 Uiso 0.2 1 calc R U P A -1 C9 C 0.505(13) 0.2002(19) 1.060(3) 0.055(6) Uiso 0.1 1 d DG U P A -1 H9A H 0.573495 0.178375 1.011555 0.083 Uiso 0.1 1 calc R U P A -1 H9B H 0.380528 0.189779 1.061520 0.083 Uiso 0.1 1 calc R U P A -1 H9C H 0.554743 0.198571 1.134996 0.083 Uiso 0.1 1 calc R U P A -1 H2 H 0.500000 0.250000 0.3444(9) 0.066 Uiso 1 4 d DS U P . . O4 O -0.033(8) 0.455(2) 0.632(5) 0.080(14) Uiso 0.125 1 d D . P B -1 H4A H -0.139237 0.464715 0.634053 0.120 Uiso 0.125 1 calc R U P B -1 C10 C -0.01(3) 0.423(3) 0.546(6) 0.080(14) Uiso 0.125 1 d D . P B -1 H10A H 0.107861 0.427526 0.512831 0.120 Uiso 0.125 1 calc R U P B -1 H10B H -0.102148 0.428137 0.490148 0.120 Uiso 0.125 1 calc R U P B -1 H10C H -0.019017 0.388757 0.573820 0.120 Uiso 0.125 1 calc R U P B -1 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 Sc1 0.0173(12) 0.029(3) 0.028(3) 0.000 -0.0024(10) 0.000 O2 0.018(4) 0.062(10) 0.028(10) 0.000 0.000 0.000 O1 0.0304(19) 0.055(5) 0.050(5) -0.020(2) -0.001(2) -0.007(3) C2 0.030(2) 0.056(5) 0.065(5) -0.027(2) 0.000 0.000 C6 0.0304(19) 0.055(5) 0.050(5) -0.020(2) -0.001(2) -0.007(3) C1 0.0304(19) 0.055(5) 0.050(5) -0.020(2) -0.001(2) -0.007(3) C5 0.030(2) 0.056(5) 0.065(5) -0.027(2) 0.000 0.000 C3 0.030(2) 0.056(5) 0.065(5) -0.027(2) 0.000 0.000 C4 0.030(2) 0.056(5) 0.065(5) -0.027(2) 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 Sc1 Sc1 3.6767(8) 2_655 ? Sc1 Sc1 3.6767(8) 2 ? Sc1 O2 2.080(5) . ? Sc1 O2 2.080(5) 13_556 ? Sc1 O1 2.118(5) 11_565 ? Sc1 O1 2.118(5) . ? Sc1 O1 2.118(5) 13_556 ? Sc1 O1 2.118(5) 7_546 ? O2 H2 0.8750(11) . ? O1 C1 1.255(4) . ? C2 C1 1.498(7) . ? C2 C3 1.391(5) 12_655 ? C2 C3 1.391(5) . ? C6 C6 1.213(15) 4_567 ? C6 C5 1.435(8) . ? C5 C4 1.398(5) . ? C5 C4 1.398(5) 12_655 ? C3 H3 0.9300 . ? C3 C4 1.378(6) . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? C7 O3 1.2338 . ? C7 N1 1.4005 . ? N1 C8 1.4597 . ? N1 C9 1.4322 . ? C8 H8A 0.9601 . ? C8 H8B 0.9601 . ? C8 H8C 0.9601 . ? C9 H9A 0.9997 . ? C9 H9B 0.9997 . ? C9 H9C 0.9997 . ? O4 H4A 0.8429 . ? O4 C10 1.36(3) . ? C10 H10A 0.9742 . ? C10 H10B 0.9945 . ? C10 H10C 0.9727 . ? 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 Sc1 Sc1 Sc1 180.0 2 2_655 ? O2 Sc1 Sc1 152.1(3) . 2 ? O2 Sc1 Sc1 152.1(3) 13_556 2_655 ? O2 Sc1 Sc1 27.9(3) . 2_655 ? O2 Sc1 Sc1 27.9(3) 13_556 2 ? O2 Sc1 O2 180.0 13_556 . ? O2 Sc1 O1 90.7(2) . 13_556 ? O2 Sc1 O1 89.3(2) 13_556 13_556 ? O2 Sc1 O1 90.7(2) 13_556 . ? O2 Sc1 O1 89.3(2) . . ? O2 Sc1 O1 90.7(2) . 7_546 ? O2 Sc1 O1 89.3(2) . 11_565 ? O2 Sc1 O1 90.7(2) 13_556 11_565 ? O2 Sc1 O1 89.3(2) 13_556 7_546 ? O1 Sc1 Sc1 69.86(10) 13_556 2 ? O1 Sc1 Sc1 69.86(10) . 2_655 ? O1 Sc1 Sc1 110.14(10) . 2 ? O1 Sc1 Sc1 69.86(10) 11_565 2_655 ? O1 Sc1 Sc1 110.14(10) 11_565 2 ? O1 Sc1 Sc1 110.14(10) 13_556 2_655 ? O1 Sc1 Sc1 69.86(10) 7_546 2 ? O1 Sc1 Sc1 110.14(10) 7_546 2_655 ? O1 Sc1 O1 90.9(3) 13_556 11_565 ? O1 Sc1 O1 180.0 11_565 7_546 ? O1 Sc1 O1 180.0 . 13_556 ? O1 Sc1 O1 89.1(3) 13_556 7_546 ? O1 Sc1 O1 89.1(3) . 11_565 ? O1 Sc1 O1 90.9(3) . 7_546 ? Sc1 O2 Sc1 124.2(5) 2_655 . ? Sc1 O2 H2 117.9(3) 2_655 . ? Sc1 O2 H2 117.9(3) . . ? C1 O1 Sc1 138.1(4) . . ? C3 C2 C1 120.6(3) 12_655 . ? C3 C2 C1 120.6(3) . . ? C3 C2 C3 118.9(5) . 12_655 ? C6 C6 C5 179.8(5) 4_567 . ? O1 C1 O1 124.1(7) . 12_655 ? O1 C1 C2 117.9(3) . . ? O1 C1 C2 117.9(3) 12_655 . ? C4 C5 C6 120.6(3) 12_655 . ? C4 C5 C6 120.6(3) . . ? C4 C5 C4 118.8(6) 12_655 . ? C2 C3 H3 119.6 . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 119.6 . . ? C5 C4 H4 119.8 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? O3 C7 H7 119.2 . . ? O3 C7 N1 124.7 . . ? N1 C7 H7 115.8 . . ? C7 N1 C8 121.4 . . ? C7 N1 C9 120.2 . . ? C9 N1 C8 118.4 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 113.7 . . ? N1 C9 H9B 113.7 . . ? N1 C9 H9C 113.7 . . ? H9A C9 H9B 105.0 . . ? H9A C9 H9C 105.0 . . ? H9B C9 H9C 105.0 . . ? C10 O4 H4A 106.5 . . ? O4 C10 H10A 108.7 . . ? O4 C10 H10B 118.4 . . ? O4 C10 H10C 107.7 . . ? H10A C10 H10B 104.9 . . ? H10A C10 H10C 107.7 . . ? H10B C10 H10C 109.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 0.2(3) . . . 12_655 ? Sc1 O1 C1 C2 -179.7(3) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C6 C5 C4 C3 -179.97(19) . . . . ? C1 C2 C3 C4 -179.99(18) . . . . ? C3 C2 C1 O1 -0.02(13) 12_655 . . . ? C3 C2 C1 O1 0.02(13) . . . 12_655 ? C3 C2 C1 O1 -179.99(8) 12_655 . . 12_655 ? C3 C2 C1 O1 179.99(8) . . . . ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.1(3) 12_655 . . . ? O3 C7 N1 C8 -167.11(8) . . . . ? O3 C7 N1 C9 11.64(5) . . . . ? _shelx_res_file ; TITL sad_a.res in Cmma mil53scedb_02_solvent.res created by SHELXL-2018/3 at 08:43:57 on 04-Oct-2022 REM Old TITL sad in Cmma REM SHELXT solution in Cmma: R1 0.190, Rweak 0.009, Alpha 0.063 REM 0.083 for 15 systematic absences, Orientation as input REM Formula found by SHELXT: C20 O7 Sc CELL 0.4589 7.3533 26.5839 11.8794 90 90 90 ZERR 2 0.0015 0.0053 0.0024 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H N O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP N -0.0008 0.0012 8.1428 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 72.4 60 3.2 23.6 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z FLAT C7 O3 N1 C8 C9 SADI N1 C8 N1 C9 RIGU C7 O3 N1 C8 C9 SIMU C7 O3 N1 C8 C9 EADP O3 C7 N1 C8 C9 DFIX 0.875 0.001 O2 H2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 DFIX 1.35 0.01 O4 C10 EADP O4 C10 L.S. 20 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 0 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 1 1 1 OMIT 3 3 1 OMIT 4 24 7 OMIT 3 21 7 OMIT 2 16 7 OMIT 2 2 1 OMIT 1 3 2 REM REM REM WGHT 0.200000 FVAR 6.85052 SC1 5 0.250000 0.250000 0.500000 10.25000 0.01732 0.02887 = 0.02819 0.00000 -0.00238 0.00000 O2 4 0.500000 0.250000 0.418059 10.25000 0.01834 0.06220 = 0.02765 0.00000 0.00000 0.00000 O1 4 0.349199 0.305891 0.611288 11.00000 0.03044 0.05467 = 0.04979 -0.02034 -0.00051 -0.00730 C2 1 0.500000 0.364347 0.728421 10.50000 0.02990 0.05595 = 0.06528 -0.02733 0.00000 0.00000 C6 1 0.500000 0.482958 0.966065 10.50000 0.03044 0.05467 = 0.04979 -0.02034 -0.00051 -0.00730 C1 1 0.500000 0.322380 0.644305 10.50000 0.03044 0.05467 = 0.04979 -0.02034 -0.00051 -0.00730 C5 1 0.500000 0.442724 0.885477 10.50000 0.02990 0.05595 = 0.06528 -0.02733 0.00000 0.00000 C3 1 0.662916 0.384179 0.768153 11.00000 0.02990 0.05595 = 0.06528 -0.02733 0.00000 0.00000 AFIX 43 H3 2 0.772629 0.371222 0.742152 11.00000 -1.20000 AFIX 0 C4 1 0.663694 0.422774 0.845538 11.00000 0.02990 0.05595 = 0.06528 -0.02733 0.00000 0.00000 AFIX 43 H4 2 0.773678 0.435628 0.871354 11.00000 -1.20000 AFIX 6 PART -1 C7 1 0.513495 0.291269 1.094935 10.10000 0.05514 AFIX 43 H7 2 0.498580 0.323373 1.065233 10.10000 -1.50000 AFIX 5 O3 4 0.528757 0.287384 1.197998 10.10000 0.05514 N1 3 0.517015 0.250812 1.019459 10.20000 0.05514 C8 1 0.536049 0.258773 0.898456 10.20000 0.05514 AFIX 137 H8A 2 0.477559 0.289707 0.877769 10.20000 -1.50000 H8B 2 0.480377 0.231359 0.858713 10.20000 -1.50000 H8C 2 0.662731 0.260491 0.879303 10.20000 -1.50000 AFIX 5 C9 1 0.505496 0.200214 1.060244 10.10000 0.05514 AFIX 137 H9A 2 0.573495 0.178375 1.011555 10.10000 -1.50000 H9B 2 0.380528 0.189779 1.061520 10.10000 -1.50000 H9C 2 0.554743 0.198571 1.134996 10.10000 -1.50000 AFIX 0 PART 0 H2 2 0.500000 0.250000 0.344403 10.25000 -1.20000 PART -1 O4 4 -0.032940 0.455428 0.632191 10.12500 0.08003 AFIX 147 H4A 2 -0.139237 0.464715 0.634053 10.12500 -1.50000 AFIX 0 C10 1 -0.009873 0.422556 0.545935 10.12500 0.08003 AFIX 137 H10A 2 0.107861 0.427526 0.512831 10.12500 -1.50000 H10B 2 -0.102148 0.428137 0.490148 10.12500 -1.50000 H10C 2 -0.019017 0.388757 0.573820 10.12500 -1.50000 AFIX 0 HKLF 4 REM sad_a.res in Cmma REM wR2 = 0.2879, GooF = S = 1.103, Restrained GooF = 1.106 for all data REM R1 = 0.1025 for 320 Fo > 4sig(Fo) and 0.1256 for all 478 data REM 55 parameters refined using 34 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.526, deepest hole -0.308, 1-sigma level 0.085 Q1 1 0.5000 0.2500 1.1234 10.25000 0.05 0.53 Q2 1 0.5000 0.3998 0.8008 10.50000 0.05 0.38 ; _shelx_res_checksum 9756 _olex2_submission_special_instructions 'No special instructions were received' #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_2610MPa _database_code_depnum_ccdc_archive 'CCDC 2223551' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.7 H21.6 O10, 4.10(C H4 O), 1.66(H2 O)' _chemical_formula_sum 'Sc2 C37.8 H41.32 O15.76' _chemical_formula_weight 837.71 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4404 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.851 Why? RINTA01_ALERT_3_B The value of Rint is greater than 0.18 Rint given 0.190 PLAT020_ALERT_3_B The Value of Rint is Greater Than 0.12 ......... 0.190 Report The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.2(10), Rep 0.02(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -0.2(10), Rep -0.02(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.416 55 Report No information given in structure factor report. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.66 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvent was modelled using SQUEEZE. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.241(4) _cell_length_b 22.814(7) _cell_length_c 13.473(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2225.6(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2011 _cell_measurement_temperature 298 _cell_measurement_pressure 2610000 _cell_measurement_theta_min 2.0510 _cell_measurement_theta_max 12.7380 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.37 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_correction_T_min 0.0207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. The \l/2 correction factor is not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 872.4 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1901 _diffrn_reflns_av_unetI/netI 0.0815 _diffrn_reflns_Laue_measured_fraction_full 0.851 _diffrn_reflns_Laue_measured_fraction_max 0.851 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3786 _diffrn_reflns_point_group_measured_fraction_full 0.851 _diffrn_reflns_point_group_measured_fraction_max 0.851 _diffrn_reflns_theta_full 11.661 _diffrn_reflns_theta_max 11.661 _diffrn_reflns_theta_min 1.599 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 2610000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.851 _diffrn_measured_fraction_theta_max 0.851 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 245 _reflns_number_total 331 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.462 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.089 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.470 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 331 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.1136 _refine_ls_restrained_S_all 1.410 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3519 _refine_ls_wR_factor_ref 0.3628 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.045) C7(0.205) H7A(0.205) H7B(0.41) H7C(0.41) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.067(4) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4275(8) 0.056(6) Uani 1 4 d DS T P . . O1 O 0.3475(7) 0.3155(3) 0.5963(5) 0.105(4) Uani 1 1 d D . . . . C2 C 0.500000 0.3710(3) 0.7176(5) 0.105(4) Uani 1 2 d DS T P . . C6 C 0.500000 0.4840(3) 0.9648(6) 0.105(4) Uani 1 2 d DS T P . . C1 C 0.500000 0.3307(3) 0.6296(6) 0.105(4) Uani 1 2 d DS T P B . C5 C 0.500000 0.4454(3) 0.8803(6) 0.105(4) Uani 1 2 d DS T P . . C3 C 0.6656(6) 0.3896(3) 0.7584(5) 0.105(4) Uani 1 1 d D . . . . H3 H 0.776883 0.377172 0.731082 0.126 Uiso 1 1 calc R U . . . C4 C 0.6658(6) 0.4267(3) 0.8395(5) 0.105(4) Uani 1 1 d D . . . . H4 H 0.777101 0.439144 0.866783 0.126 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3626(8) 0.126 Uiso 0.18 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3235(9) 0.056(6) Uani 0.82 4 d DS T P B 2 H7A H 0.374998 0.250000 0.299731 0.067 Uiso 0.41 2 calc R U P B 2 H7B H 0.562501 0.284358 0.299731 0.067 Uiso 0.41 1 calc R U P B 2 H7C H 0.562501 0.215642 0.299731 0.067 Uiso 0.41 1 calc R U P B 2 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 Sc1 0.140(8) 0.043(5) 0.020(4) 0.000 -0.003(3) 0.000 O2 0.08(2) 0.070(12) 0.016(7) 0.000 0.000 0.000 O1 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C2 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C6 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C1 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C5 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C3 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C4 0.163(11) 0.092(7) 0.060(6) -0.038(3) -0.006(6) 0.010(6) C7 0.08(2) 0.070(12) 0.016(7) 0.000 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 Sc1 Sc1 3.620(2) 2_655 ? Sc1 Sc1 3.620(2) 2 ? Sc1 O2 2.057(5) . ? Sc1 O2 2.057(5) 13_556 ? Sc1 O1 2.100(6) 7_546 ? Sc1 O1 2.100(6) 13_556 ? Sc1 O1 2.100(6) 11_565 ? Sc1 O1 2.100(6) . ? O2 H2 0.8750(11) . ? O2 C7 1.402(9) . ? O1 C1 1.242(5) . ? C2 C1 1.500(8) . ? C2 C3 1.386(5) 12_655 ? C2 C3 1.386(5) . ? C6 C6 1.20(2) 4_567 ? C6 C5 1.440(8) . ? C5 C4 1.387(5) . ? C5 C4 1.387(5) 12_655 ? C3 H3 0.9300 . ? C3 C4 1.383(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9601 2_655 ? C7 H7B 0.9601 12_655 ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 151.7(3) . 2 ? O2 Sc1 Sc1 28.3(3) . 2_655 ? O2 Sc1 Sc1 28.3(3) 13_556 2 ? O2 Sc1 Sc1 151.7(3) 13_556 2_655 ? O2 Sc1 O2 180.0 13_556 . ? O2 Sc1 O1 89.9(2) 13_556 7_546 ? O2 Sc1 O1 89.9(2) 13_556 13_556 ? O2 Sc1 O1 90.1(2) . 7_546 ? O2 Sc1 O1 89.9(2) . 11_565 ? O2 Sc1 O1 90.1(2) 13_556 . ? O2 Sc1 O1 90.1(2) . 13_556 ? O2 Sc1 O1 89.9(2) . . ? O2 Sc1 O1 90.1(2) 13_556 11_565 ? O1 Sc1 Sc1 70.37(14) 11_565 2_655 ? O1 Sc1 Sc1 70.37(14) 7_546 2 ? O1 Sc1 Sc1 109.63(14) 11_565 2 ? O1 Sc1 Sc1 109.63(14) . 2 ? O1 Sc1 Sc1 70.37(14) . 2_655 ? O1 Sc1 Sc1 70.37(14) 13_556 2 ? O1 Sc1 Sc1 109.63(14) 7_546 2_655 ? O1 Sc1 Sc1 109.63(14) 13_556 2_655 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? O1 Sc1 O1 90.6(4) 11_565 . ? O1 Sc1 O1 89.4(4) 7_546 . ? O1 Sc1 O1 89.4(4) 13_556 11_565 ? O1 Sc1 O1 90.6(4) 13_556 7_546 ? O1 Sc1 O1 180.0 13_556 . ? Sc1 O2 Sc1 123.3(5) 2_655 . ? Sc1 O2 H2 118.3(3) . . ? Sc1 O2 H2 118.3(3) 2_655 . ? C7 O2 Sc1 118.3(3) . . ? C1 O1 Sc1 136.1(5) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 C1 120.1(3) 12_655 . ? C3 C2 C3 119.8(6) . 12_655 ? C6 C6 C5 179.8(6) 4_567 . ? O1 C1 O1 125.6(9) . 12_655 ? O1 C1 C2 117.2(4) 12_655 . ? O1 C1 C2 117.2(4) . . ? C4 C5 C6 120.1(3) 12_655 . ? C4 C5 C6 120.1(3) . . ? C4 C5 C4 119.8(7) 12_655 . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3 119.9 . . ? C5 C4 H4 120.0 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? O2 C7 H7A 109.472(11) . 2_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.471(6) . 12_655 ? O2 C7 H7B 109.471(6) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 15.4(4) . . . 12_655 ? Sc1 O1 C1 C2 -164.6(4) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C6 C5 C4 C3 -179.99(19) . . . . ? C1 C2 C3 C4 -179.95(18) . . . . ? C3 C2 C1 O1 -0.02(13) . . . 12_655 ? C3 C2 C1 O1 -179.99(8) . . . . ? C3 C2 C1 O1 0.02(13) 12_655 . . . ? C3 C2 C1 O1 179.99(8) 12_655 . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.1(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns in Cmma mil53scedb_08.res created by SHELXL-2019/2 at 09:44:32 on 24-Oct-2022 CELL 0.4859 7.24065 22.81379 13.4732 90 90 90 ZERR 2 0.00412 0.00678 0.00276 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 67.28 49.12 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.200000 FVAR 4.41143 SC1 4 0.250000 0.250000 0.500000 10.25000 0.13958 0.04258 = 0.01972 0.00000 -0.00308 0.00000 O2 3 0.500000 0.250000 0.427508 10.25000 0.08241 0.07006 = 0.01618 0.00000 0.00000 0.00000 O1 3 0.347458 0.315458 0.596271 11.00000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 C2 1 0.500000 0.370955 0.717555 10.50000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 C6 1 0.500000 0.484027 0.964799 10.50000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 C1 1 0.500000 0.330677 0.629558 10.50000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 C5 1 0.500000 0.445391 0.880289 10.50000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 C3 1 0.665616 0.389626 0.758364 11.00000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 AFIX 43 H3 2 0.776883 0.377172 0.731082 11.00000 -1.20000 AFIX 0 C4 1 0.665794 0.426713 0.839517 11.00000 0.16255 0.09156 = 0.06027 -0.03849 -0.00568 0.00973 AFIX 43 H4 2 0.777101 0.439144 0.866783 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.362564 10.04500 -1.20000 PART 2 C7 1 0.500000 0.250000 0.323482 10.20500 0.08241 0.07006 = 0.01618 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.374998 0.250000 0.299731 10.20500 -1.20000 H7B 2 0.562501 0.284358 0.299731 10.41000 -1.20000 H7C 2 0.562501 0.215642 0.299731 10.41000 -1.20000 AFIX 0 HKLF 4 REM fullruns in Cmma REM wR2 = 0.3628, GooF = S = 1.470, Restrained GooF = 1.410 for all data REM R1 = 0.1136 for 245 Fo > 4sig(Fo) and 0.1265 for all 331 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.462, deepest hole -0.499, 1-sigma level 0.089 Q1 1 0.5000 0.4585 0.8536 10.50000 0.05 0.46 Q2 1 0.5000 0.2500 0.6668 10.25000 0.05 0.34 ; _shelx_res_checksum 35159 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.046 0.250 0.000 246 101 ' ' 2 -0.046 0.750 0.000 246 101 ' ' 3 -0.052 0.500 0.500 240 81 ' ' 4 -0.048 1.000 0.500 240 81 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_3200MPa _database_code_depnum_ccdc_archive 'CCDC 2223555' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.7 H21.6 O10, 3.90(C H4 O), 1.70(H2 O)' _chemical_formula_sum 'Sc2 C37.6 H40.6 O15.6' _chemical_formula_weight 832.03 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4809 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.859 Why? PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 6.0 Note The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.1(8), Rep 0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -179.9(5), Rep -179.98(7) ...... 7.14 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 12_655 # 7 Check PLAT733_ALERT_1_B Torsion Calc 179.9(5), Rep 179.98(7) ...... 7.14 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 1_555 # 8 Check PLAT733_ALERT_1_B Torsion Calc -0.1(8), Rep -0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.454 46 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 12.03 0.454 0.906 508 460 48 #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.72 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvent was modelled using SQUEEZE. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.180(2) _cell_length_b 22.587(4) _cell_length_c 13.5541(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2198.2(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1619 _cell_measurement_temperature 298 _cell_measurement_pressure 3200000 _cell_measurement_theta_min 1.5830 _cell_measurement_theta_max 14.9230 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.37 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_correction_T_min 0.4848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0923 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.6515. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 866 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1022 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_Laue_measured_fraction_full 0.859 _diffrn_reflns_Laue_measured_fraction_max 0.859 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4563 _diffrn_reflns_point_group_measured_fraction_full 0.859 _diffrn_reflns_point_group_measured_fraction_max 0.859 _diffrn_reflns_theta_full 12.749 _diffrn_reflns_theta_max 12.749 _diffrn_reflns_theta_min 1.605 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 3200000 _diffrn_orient_matrix_UB_11 -0.0511520000 _diffrn_orient_matrix_UB_12 0.0118147000 _diffrn_orient_matrix_UB_13 0.0125034000 _diffrn_orient_matrix_UB_21 0.0417558000 _diffrn_orient_matrix_UB_22 0.0168393000 _diffrn_orient_matrix_UB_23 0.0034845000 _diffrn_orient_matrix_UB_31 -0.0149397000 _diffrn_orient_matrix_UB_32 0.0062391000 _diffrn_orient_matrix_UB_33 -0.0334304000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.859 _diffrn_measured_fraction_theta_max 0.859 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 343 _reflns_number_total 434 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.650 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.090 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.663 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 418 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.1106 _refine_ls_restrained_S_all 1.609 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3495 _refine_ls_wR_factor_ref 0.3636 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.07) C7(0.18) H7A(0.18) H7B(0.36) H7C(0.36) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.075(3) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4250(6) 0.075(5) Uani 1 4 d DS T P . . O1 O 0.3466(6) 0.3146(2) 0.5971(4) 0.107(3) Uani 1 1 d D . . . . C2 C 0.500000 0.3703(2) 0.7181(4) 0.107(3) Uani 1 2 d DS T P . . C6 C 0.500000 0.4836(3) 0.9643(5) 0.107(3) Uani 1 2 d DS T P . . C1 C 0.500000 0.3299(3) 0.6304(5) 0.107(3) Uani 1 2 d DS T P B . C5 C 0.500000 0.4447(3) 0.8799(5) 0.107(3) Uani 1 2 d DS T P . . C3 C 0.6666(6) 0.3888(2) 0.7585(4) 0.107(3) Uani 1 1 d D . . . . H3 H 0.778192 0.376273 0.731174 0.128 Uiso 1 1 calc R U . . . C4 C 0.6666(6) 0.4261(2) 0.8395(4) 0.107(3) Uani 1 1 d D . . . . H4 H 0.778176 0.438569 0.866769 0.128 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3602(6) 0.128 Uiso 0.28 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3211(8) 0.075(5) Uani 0.72 4 d DS T P B 2 H7A H 0.374521 0.250000 0.297438 0.090 Uiso 0.36 2 calc R U P B 2 H7B H 0.562739 0.284396 0.297438 0.090 Uiso 0.36 1 calc R U P B 2 H7C H 0.562739 0.215604 0.297438 0.090 Uiso 0.36 1 calc R U P B 2 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 Sc1 0.162(6) 0.034(3) 0.027(3) 0.000 -0.0016(19) 0.000 O2 0.155(16) 0.053(7) 0.018(5) 0.000 0.000 0.000 O1 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C2 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C6 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C1 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C5 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C3 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C4 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C7 0.155(16) 0.053(7) 0.018(5) 0.000 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 Sc1 Sc1 3.6066(10) 2_655 ? Sc1 Sc1 3.6066(10) 2 ? Sc1 O2 2.068(4) 13_556 ? Sc1 O2 2.068(4) . ? Sc1 O1 2.090(5) 7_546 ? Sc1 O1 2.090(5) . ? Sc1 O1 2.090(5) 13_556 ? Sc1 O1 2.090(5) 11_565 ? O2 H2 0.8750(10) . ? O2 C7 1.402(9) . ? O1 C1 1.245(5) . ? C2 C1 1.499(8) . ? C2 C3 1.385(5) 12_655 ? C2 C3 1.385(5) . ? C6 C6 1.221(17) 4_567 ? C6 C5 1.442(8) . ? C5 C4 1.386(5) 12_655 ? C5 C4 1.386(5) . ? C3 H3 0.9300 . ? C3 C4 1.385(6) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 29.3(2) . 2_655 ? O2 Sc1 Sc1 150.7(2) . 2 ? O2 Sc1 Sc1 29.3(2) 13_556 2 ? O2 Sc1 Sc1 150.7(2) 13_556 2_655 ? O2 Sc1 O2 180.0 . 13_556 ? O2 Sc1 O1 89.1(2) 13_556 . ? O2 Sc1 O1 90.9(2) . . ? O2 Sc1 O1 89.1(2) 13_556 11_565 ? O2 Sc1 O1 89.1(2) . 13_556 ? O2 Sc1 O1 90.9(2) 13_556 13_556 ? O2 Sc1 O1 90.9(2) 13_556 7_546 ? O2 Sc1 O1 89.1(2) . 7_546 ? O2 Sc1 O1 90.9(2) . 11_565 ? O1 Sc1 Sc1 70.52(13) 11_565 2_655 ? O1 Sc1 Sc1 70.52(13) . 2_655 ? O1 Sc1 Sc1 109.48(13) 13_556 2_655 ? O1 Sc1 Sc1 70.52(13) 7_546 2 ? O1 Sc1 Sc1 70.52(13) 13_556 2 ? O1 Sc1 Sc1 109.48(13) 11_565 2 ? O1 Sc1 Sc1 109.48(13) . 2 ? O1 Sc1 Sc1 109.48(13) 7_546 2_655 ? O1 Sc1 O1 180.0(2) 11_565 7_546 ? O1 Sc1 O1 89.5(3) 13_556 7_546 ? O1 Sc1 O1 90.5(3) 13_556 11_565 ? O1 Sc1 O1 89.5(3) 11_565 . ? O1 Sc1 O1 180.0 13_556 . ? O1 Sc1 O1 90.5(3) 7_546 . ? Sc1 O2 Sc1 121.4(4) 2_655 . ? Sc1 O2 H2 119.3(2) . . ? Sc1 O2 H2 119.3(2) 2_655 . ? C7 O2 Sc1 119.3(2) . . ? C1 O1 Sc1 136.1(5) . . ? C3 C2 C1 119.8(3) 12_655 . ? C3 C2 C1 119.8(3) . . ? C3 C2 C3 120.3(6) . 12_655 ? C6 C6 C5 179.9(5) 4_567 . ? O1 C1 O1 125.5(7) . 12_655 ? O1 C1 C2 117.3(4) 12_655 . ? O1 C1 C2 117.3(4) . . ? C4 C5 C6 119.9(3) 12_655 . ? C4 C5 C6 119.9(3) . . ? C4 C5 C4 120.1(6) 12_655 . ? C2 C3 H3 120.1 . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3 120.1 . . ? C5 C4 H4 120.0 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.0 . . ? O2 C7 H7A 109.469(5) . 2_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.469(3) . 12_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.469(3) . 2_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 14.3(3) . . . 12_655 ? Sc1 O1 C1 C2 -165.7(3) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C6 C5 C4 C3 -179.98(18) . . . . ? C1 C2 C3 C4 -179.97(18) . . . . ? C3 C2 C1 O1 0.02(13) 12_655 . . . ? C3 C2 C1 O1 -179.98(7) 12_655 . . 12_655 ? C3 C2 C1 O1 179.98(7) . . . . ? C3 C2 C1 O1 -0.02(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.1(3) 12_655 . . . ? _shelx_res_file ; TITL FULLRUNS in Cmma mil53scedb_09.res created by SHELXL-2019/2 at 09:46:17 on 24-Oct-2022 CELL 0.4859 7.21315 22.78881 13.49662 90 90 90 ZERR 2 0.00197 0.00255 0.00125 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 66.88 47.52 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 0 10 OMIT 0 8 6 REM REM REM WGHT 0.200000 FVAR 2.78164 SC1 4 0.250000 0.250000 0.500000 10.25000 0.16235 0.03423 = 0.02726 0.00000 -0.00164 0.00000 O2 3 0.500000 0.250000 0.425048 10.25000 0.15489 0.05315 = 0.01780 0.00000 0.00000 0.00000 O1 3 0.346620 0.314562 0.597083 11.00000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C2 1 0.500000 0.370269 0.718116 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C6 1 0.500000 0.483554 0.964314 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C1 1 0.500000 0.329910 0.630430 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C5 1 0.500000 0.444729 0.879915 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C3 1 0.666619 0.388815 0.758452 11.00000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 AFIX 43 H3 2 0.778192 0.376273 0.731174 11.00000 -1.20000 AFIX 0 C4 1 0.666565 0.426070 0.839482 11.00000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 AFIX 43 H4 2 0.778176 0.438569 0.866769 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.360217 10.07000 -1.20000 PART 2 C7 1 0.500000 0.250000 0.321147 10.18000 0.15489 0.05315 = 0.01780 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.374521 0.250000 0.297438 10.18000 -1.20000 H7B 2 0.562739 0.284396 0.297438 10.36000 -1.20000 H7C 2 0.562739 0.215604 0.297438 10.36000 -1.20000 AFIX 0 HKLF 4 REM FULLRUNS in Cmma REM wR2 = 0.3636, GooF = S = 1.663, Restrained GooF = 1.609 for all data REM R1 = 0.1106 for 356 Fo > 4sig(Fo) and 0.1189 for all 418 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.650, deepest hole -0.424, 1-sigma level 0.090 Q1 1 0.5000 0.4581 0.8657 10.50000 0.05 0.65 Q2 1 0.5000 0.3820 0.7085 10.50000 0.05 0.49 ; _shelx_res_checksum 28595 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.050 0.250 0.000 242 102 ' ' 2 -0.050 0.750 0.000 242 102 ' ' 3 -0.052 0.500 0.500 243 74 ' ' 4 -0.052 1.000 0.500 243 74 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_4980MPa _database_code_depnum_ccdc_archive 'CCDC 2223547' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C34 H22.2 O10, 3.60(C H4 O), 1.90(H2 O)' _chemical_formula_sum 'Sc2 C37.6 H40.4 O15.5' _chemical_formula_weight 830.23 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- RINTA01_ALERT_3_A The value of Rint is greater than 0.25 Rint given 0.354 THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4408 PLAT020_ALERT_3_A The Value of Rint is Greater Than 0.12 ......... 0.354 Report PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.824 Why? PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.416 49 Report The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT733_ALERT_1_A Torsion Calc -0.1(12), Rep 0.00(13) ...... 9.23 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_A Torsion Calc 0.1(12), Rep 0.00(13) ...... 9.23 s These are correct. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.66 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.416 49 Report No information given in structure factor report. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvate was modelled using SQUEEZE. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.0143(12) _cell_length_b 21.941(7) _cell_length_c 13.6972(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2108.0(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 955 _cell_measurement_temperature 298 _cell_measurement_pressure 4980000 _cell_measurement_theta_max 11.6960 _cell_measurement_theta_min 1.6180 _shelx_estimated_absorpt_T_max 0.996 _shelx_estimated_absorpt_T_min 0.983 _exptl_absorpt_coefficient_mu 0.39 _exptl_absorpt_correction_T_max 0.7436 _exptl_absorpt_correction_T_min 0.3897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1113 before and 0.0759 after correction. The Ratio of minimum to maximum transmission is 0.5241. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.3538 _diffrn_reflns_av_unetI/netI 0.1084 _diffrn_reflns_Laue_measured_fraction_full 0.824 _diffrn_reflns_Laue_measured_fraction_max 0.824 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3488 _diffrn_reflns_point_group_measured_fraction_full 0.824 _diffrn_reflns_point_group_measured_fraction_max 0.824 _diffrn_reflns_theta_full 11.671 _diffrn_reflns_theta_max 11.671 _diffrn_reflns_theta_min 1.626 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 4980000 _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0265006000 _diffrn_orient_matrix_UB_12 -0.0180634000 _diffrn_orient_matrix_UB_13 0.0149443000 _diffrn_orient_matrix_UB_21 -0.0596838000 _diffrn_orient_matrix_UB_22 -0.0106974000 _diffrn_orient_matrix_UB_23 -0.0059546000 _diffrn_orient_matrix_UB_31 0.0237791000 _diffrn_orient_matrix_UB_32 -0.0066493000 _diffrn_orient_matrix_UB_33 -0.0316759000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.824 _diffrn_measured_fraction_theta_max 0.824 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 221 _reflns_number_total 309 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.558 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.076 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 309 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.1109 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3232 _refine_ls_wR_factor_ref 0.3328 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.005) C7(0.245) H7A(0.245) H7B(0.49) H7C(0.49) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.080(4) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4245(7) 0.082(7) Uani 1 4 d DS T P . . O1 O 0.3418(7) 0.3164(4) 0.5949(5) 0.122(5) Uani 1 1 d D . . . . C2 C 0.500000 0.3716(4) 0.7167(6) 0.122(5) Uani 1 2 d DS T P . . C6 C 0.500000 0.4840(3) 0.9652(7) 0.122(5) Uani 1 2 d DS T P . . C1 C 0.500000 0.3315(4) 0.6281(6) 0.122(5) Uani 1 2 d DS T P B . C5 C 0.500000 0.4455(3) 0.8802(6) 0.122(5) Uani 1 2 d DS T P . . C3 C 0.6713(7) 0.3900(3) 0.7573(6) 0.122(5) Uani 1 1 d D . . . . H3 H 0.785995 0.377498 0.729623 0.147 Uiso 1 1 calc R U . . . C4 C 0.6715(7) 0.4272(3) 0.8397(5) 0.122(5) Uani 1 1 d D . . . . H4 H 0.786160 0.439593 0.867382 0.147 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3606(7) 0.147 Uiso 0.02 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3209(9) 0.082(7) Uani 0.98 4 d DS T P B 2 H7A H 0.370963 0.250000 0.297554 0.099 Uiso 0.49 2 calc R U P B 2 H7B H 0.564519 0.285725 0.297554 0.099 Uiso 0.49 1 calc R U P B 2 H7C H 0.564518 0.214275 0.297554 0.099 Uiso 0.49 1 calc R U P B 2 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 Sc1 0.124(5) 0.068(8) 0.048(4) 0.000 -0.002(3) 0.000 O2 0.103(12) 0.10(2) 0.044(7) 0.000 0.000 0.000 O1 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C2 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C6 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C1 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C5 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C3 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C4 0.159(7) 0.103(12) 0.105(6) -0.042(5) 0.012(6) -0.012(6) C7 0.103(12) 0.10(2) 0.044(7) 0.000 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 Sc1 Sc1 3.5071(6) 2_655 ? Sc1 Sc1 3.5071(6) 2 ? Sc1 O2 2.036(5) 13_556 ? Sc1 O2 2.036(5) . ? Sc1 O1 2.056(8) 7_546 ? Sc1 O1 2.056(8) . ? Sc1 O1 2.056(8) 13_556 ? Sc1 O1 2.056(8) 11_565 ? O2 H2 0.8750(11) . ? O2 C7 1.419(9) . ? O1 C1 1.244(5) . ? C2 C1 1.498(8) . ? C2 C3 1.384(5) 12_655 ? C2 C3 1.384(5) . ? C6 C6 1.18(2) 4_567 ? C6 C5 1.438(8) . ? C5 C4 1.385(5) 12_655 ? C5 C4 1.385(5) . ? C3 H3 0.9300 . ? C3 C4 1.393(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 30.5(2) . 2_655 ? O2 Sc1 Sc1 149.5(2) . 2 ? O2 Sc1 Sc1 30.5(2) 13_556 2 ? O2 Sc1 Sc1 149.5(2) 13_556 2_655 ? O2 Sc1 O2 180.0 . 13_556 ? O2 Sc1 O1 87.1(2) 13_556 . ? O2 Sc1 O1 92.9(2) . . ? O2 Sc1 O1 87.1(2) 13_556 11_565 ? O2 Sc1 O1 87.1(2) . 13_556 ? O2 Sc1 O1 92.9(2) 13_556 13_556 ? O2 Sc1 O1 92.9(2) 13_556 7_546 ? O2 Sc1 O1 87.1(2) . 7_546 ? O2 Sc1 O1 92.9(2) . 11_565 ? O1 Sc1 Sc1 71.75(15) 11_565 2_655 ? O1 Sc1 Sc1 71.75(15) . 2_655 ? O1 Sc1 Sc1 108.25(15) 13_556 2_655 ? O1 Sc1 Sc1 71.75(15) 7_546 2 ? O1 Sc1 Sc1 71.75(15) 13_556 2 ? O1 Sc1 Sc1 108.25(15) 11_565 2 ? O1 Sc1 Sc1 108.25(15) . 2 ? O1 Sc1 Sc1 108.25(15) 7_546 2_655 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? O1 Sc1 O1 90.3(5) 13_556 7_546 ? O1 Sc1 O1 89.7(5) 13_556 11_565 ? O1 Sc1 O1 90.3(5) 11_565 . ? O1 Sc1 O1 180.0 13_556 . ? O1 Sc1 O1 89.7(5) 7_546 . ? Sc1 O2 Sc1 118.9(5) 2_655 . ? Sc1 O2 H2 120.5(2) . . ? Sc1 O2 H2 120.5(3) 2_655 . ? C7 O2 Sc1 120.5(2) . . ? C1 O1 Sc1 134.3(6) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 C1 119.7(3) 12_655 . ? C3 C2 C3 120.5(6) . 12_655 ? C6 C6 C5 179.7(6) 4_567 . ? O1 C1 O1 126.2(9) . 12_655 ? O1 C1 C2 116.9(5) . . ? O1 C1 C2 116.9(5) 12_655 . ? C4 C5 C6 119.7(3) . . ? C4 C5 C6 119.7(3) 12_655 . ? C4 C5 C4 120.6(7) 12_655 . ? C2 C3 H3 120.1 . . ? C2 C3 C4 119.8(4) . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7A 109.474(5) . 2_655 ? O2 C7 H7B 109.474(5) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.474(5) . 12_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 16.4(4) . . . 12_655 ? Sc1 O1 C1 C2 -163.6(5) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C6 C5 C4 C3 -179.89(19) . . . . ? C1 C2 C3 C4 -179.90(18) . . . . ? C3 C2 C1 O1 0.00(13) 12_655 . . . ? C3 C2 C1 O1 -179.98(8) 12_655 . . 12_655 ? C3 C2 C1 O1 179.98(8) . . . . ? C3 C2 C1 O1 0.00(13) . . . 12_655 ? C3 C2 C3 C4 0.1(2) 12_655 . . . ? C4 C5 C4 C3 0.2(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns in Cmma mil53scedb_15.res created by SHELXL-2019/2 at 09:54:32 on 24-Oct-2022 CELL 0.4859 7.01425 21.94073 13.69723 90 90 90 ZERR 2 0.0012 0.00695 0.00194 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 67.92 51.68 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.200000 FVAR 4.67578 SC1 4 0.250000 0.250000 0.500000 10.25000 0.12356 0.06773 = 0.04787 0.00000 -0.00181 0.00000 O2 3 0.500000 0.250000 0.424512 10.25000 0.10258 0.10012 = 0.04367 0.00000 0.00000 0.00000 O1 3 0.341810 0.316430 0.594912 11.00000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 C2 1 0.500000 0.371580 0.716681 10.50000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 C6 1 0.500000 0.484033 0.965158 10.50000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 C1 1 0.500000 0.331484 0.628138 10.50000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 C5 1 0.500000 0.445545 0.880201 10.50000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 C3 1 0.671343 0.389953 0.757279 11.00000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 AFIX 43 H3 2 0.785995 0.377498 0.729623 11.00000 -1.20000 AFIX 0 C4 1 0.671494 0.427166 0.839710 11.00000 0.15896 0.10266 = 0.10542 -0.04176 0.01218 -0.01230 AFIX 43 H4 2 0.786160 0.439593 0.867382 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.360630 10.00500 -1.20000 PART 2 C7 1 0.500000 0.250000 0.320917 10.24500 0.10258 0.10012 = 0.04367 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.370963 0.250000 0.297554 10.24500 -1.20000 H7B 2 0.564519 0.285725 0.297554 10.49000 -1.20000 H7C 2 0.564518 0.214275 0.297554 10.49000 -1.20000 AFIX 0 HKLF 4 REM fullruns in Cmma REM wR2 = 0.3328, GooF = S = 1.216, Restrained GooF = 1.178 for all data REM R1 = 0.1109 for 221 Fo > 4sig(Fo) and 0.1250 for all 309 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.558, deepest hole -0.332, 1-sigma level 0.076 Q1 1 0.5000 0.2500 0.5697 10.25000 0.05 0.37 Q2 1 0.5000 0.5000 1.0000 10.25000 0.05 0.26 ; _shelx_res_checksum 8685 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.044 0.250 0.000 229 91 ' ' 2 -0.044 0.750 0.000 229 91 ' ' 3 -0.054 0.500 0.500 216 77 ' ' 4 -0.054 1.000 0.500 216 77 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_3450MPa _database_code_depnum_ccdc_archive 'CCDC 2223552' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.6 H21.2 O10, 3.70(C H4 O), 1.56(H2 O)' _chemical_formula_sum 'Sc2 C37.3 H39.12 O15.26' _chemical_formula_weight 821.49 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4599 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.877 Why? PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.36 Report The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.69 Degree An absorption correction was applied in the programs, SADABS. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.2(10), Rep 0.06(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc 179.9(6), Rep 180.00(8) ...... 7.50 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 12_655 # 7 Check PLAT733_ALERT_1_B Torsion Calc -179.9(6), Rep 180.00(8) ...... 7.50 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 1_555 # 8 Check PLAT733_ALERT_1_B Torsion Calc -0.2(10), Rep -0.06(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.434 45 Report C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvent was modelled using SQUEEZE. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.434 45 Report No informaion given in structure factor report. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.1429(17) _cell_length_b 22.463(3) _cell_length_c 13.5504(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2174.2(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1624 _cell_measurement_temperature 298 _cell_measurement_pressure 3450000 _cell_measurement_theta_min 2.0450 _cell_measurement_theta_max 13.6700 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.37 _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_correction_T_min 0.6795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0738 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.9134. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 854 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_Laue_measured_fraction_full 0.877 _diffrn_reflns_Laue_measured_fraction_max 0.877 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4239 _diffrn_reflns_point_group_measured_fraction_full 0.877 _diffrn_reflns_point_group_measured_fraction_max 0.877 _diffrn_reflns_theta_full 12.185 _diffrn_reflns_theta_max 12.185 _diffrn_reflns_theta_min 1.610 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 3450000 _diffrn_orient_matrix_UB_11 -0.0489597000 _diffrn_orient_matrix_UB_12 0.0125695000 _diffrn_orient_matrix_UB_13 0.0136117000 _diffrn_orient_matrix_UB_21 0.0445356000 _diffrn_orient_matrix_UB_22 0.0162402000 _diffrn_orient_matrix_UB_23 0.0032045000 _diffrn_orient_matrix_UB_31 -0.0157670000 _diffrn_orient_matrix_UB_32 0.0067539000 _diffrn_orient_matrix_UB_33 -0.0330358000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.877 _diffrn_measured_fraction_theta_max 0.877 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 315 _reflns_number_total 386 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.546 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.100 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.598 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 383 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.1158 _refine_ls_restrained_S_all 1.545 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3457 _refine_ls_wR_factor_ref 0.3570 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.055) C7(0.195) H7A(0.195) H7B(0.39) H7C(0.39) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.075(3) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4256(6) 0.083(5) Uani 1 4 d DS T P . . O1 O 0.3451(6) 0.3150(3) 0.5961(4) 0.115(4) Uani 1 1 d D . . . . C2 C 0.500000 0.3707(3) 0.7175(5) 0.115(4) Uani 1 2 d DS T P . . C6 C 0.500000 0.4839(3) 0.9647(6) 0.115(4) Uani 1 2 d DS T P . . C1 C 0.500000 0.3302(3) 0.6295(5) 0.115(4) Uani 1 2 d DS T P B . C5 C 0.500000 0.4451(3) 0.8799(5) 0.115(4) Uani 1 2 d DS T P . . C3 C 0.6678(6) 0.3893(2) 0.7581(4) 0.115(4) Uani 1 1 d D . . . . H3 H 0.780477 0.376759 0.730735 0.138 Uiso 1 1 calc R U . . . C4 C 0.6682(6) 0.4266(2) 0.8394(4) 0.115(4) Uani 1 1 d D . . . . H4 H 0.780917 0.439072 0.866766 0.138 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3610(6) 0.138 Uiso 0.22 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3222(8) 0.083(5) Uani 0.78 4 d DS T P B 2 H7A H 0.373287 0.250000 0.298573 0.100 Uiso 0.39 2 calc R U P B 2 H7B H 0.563356 0.284894 0.298573 0.100 Uiso 0.39 1 calc R U P B 2 H7C H 0.563356 0.215106 0.298573 0.100 Uiso 0.39 1 calc R U P B 2 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 Sc1 0.142(5) 0.053(4) 0.032(3) 0.000 -0.002(2) 0.000 O2 0.157(15) 0.072(10) 0.020(5) 0.000 0.000 0.000 O1 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C2 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C6 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C1 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C5 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C3 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C4 0.169(8) 0.107(6) 0.068(5) -0.037(3) -0.010(4) 0.010(4) C7 0.157(15) 0.072(10) 0.020(5) 0.000 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 Sc1 Sc1 3.5714(9) 2 ? Sc1 Sc1 3.5714(9) 2_655 ? Sc1 O2 2.051(4) . ? Sc1 O2 2.051(4) 13_556 ? Sc1 O1 2.071(6) 11_565 ? Sc1 O1 2.071(6) 7_546 ? Sc1 O1 2.071(6) . ? Sc1 O1 2.071(6) 13_556 ? O2 H2 0.8750(11) . ? O2 C7 1.401(9) . ? O1 C1 1.243(5) . ? C2 C1 1.500(8) . ? C2 C3 1.384(5) 12_655 ? C2 C3 1.384(5) . ? C6 C6 1.199(18) 4_567 ? C6 C5 1.441(8) . ? C5 C4 1.385(5) 12_655 ? C5 C4 1.385(5) . ? C3 H3 0.9300 . ? C3 C4 1.383(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2 2_655 ? O2 Sc1 Sc1 29.5(2) 13_556 2 ? O2 Sc1 Sc1 150.5(2) 13_556 2_655 ? O2 Sc1 Sc1 29.5(2) . 2_655 ? O2 Sc1 Sc1 150.5(2) . 2 ? O2 Sc1 O2 180.0 13_556 . ? O2 Sc1 O1 88.6(2) . 7_546 ? O2 Sc1 O1 91.4(2) 13_556 7_546 ? O2 Sc1 O1 88.6(2) . 13_556 ? O2 Sc1 O1 88.6(2) 13_556 . ? O2 Sc1 O1 91.4(2) . . ? O2 Sc1 O1 91.4(2) . 11_565 ? O2 Sc1 O1 88.6(2) 13_556 11_565 ? O2 Sc1 O1 91.4(2) 13_556 13_556 ? O1 Sc1 Sc1 70.85(14) 13_556 2 ? O1 Sc1 Sc1 70.85(14) 7_546 2 ? O1 Sc1 Sc1 109.15(14) . 2 ? O1 Sc1 Sc1 70.85(14) 11_565 2_655 ? O1 Sc1 Sc1 70.85(14) . 2_655 ? O1 Sc1 Sc1 109.15(14) 13_556 2_655 ? O1 Sc1 Sc1 109.15(14) 7_546 2_655 ? O1 Sc1 Sc1 109.15(14) 11_565 2 ? O1 Sc1 O1 90.4(3) 13_556 11_565 ? O1 Sc1 O1 89.6(3) . 11_565 ? O1 Sc1 O1 180.0(3) . 13_556 ? O1 Sc1 O1 89.6(3) 13_556 7_546 ? O1 Sc1 O1 90.4(3) . 7_546 ? O1 Sc1 O1 180.0(2) 11_565 7_546 ? Sc1 O2 Sc1 121.1(4) 2_655 . ? Sc1 O2 H2 119.5(2) . . ? Sc1 O2 H2 119.5(2) 2_655 . ? C7 O2 Sc1 119.5(2) . . ? C1 O1 Sc1 135.6(5) . . ? C3 C2 C1 120.0(3) 12_655 . ? C3 C2 C1 120.0(3) . . ? C3 C2 C3 120.1(6) . 12_655 ? C6 C6 C5 179.8(5) 4_567 . ? O1 C1 O1 125.7(8) . 12_655 ? O1 C1 C2 117.1(4) 12_655 . ? O1 C1 C2 117.1(4) . . ? C4 C5 C6 119.9(3) 12_655 . ? C4 C5 C6 119.9(3) . . ? C4 C5 C4 120.3(6) 12_655 . ? C2 C3 H3 120.0 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 120.0 . . ? C5 C4 H4 120.1 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? O2 C7 H7A 109.473(6) . 2_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.473(3) . 12_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.473(3) . 2_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 15.0(4) . . . 12_655 ? Sc1 O1 C1 C2 -165.1(4) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C6 C5 C4 C3 179.96(18) . . . . ? C1 C2 C3 C4 -179.93(18) . . . . ? C3 C2 C1 O1 0.06(13) 12_655 . . . ? C3 C2 C1 O1 180.00(8) 12_655 . . 12_655 ? C3 C2 C1 O1 180.00(8) . . . . ? C3 C2 C1 O1 -0.06(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.0(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns in Cmma mil53scedb_11.res created by SHELXL-2019/2 at 09:48:49 on 24-Oct-2022 CELL 0.4859 7.1429 22.4632 13.55039 90 90 90 ZERR 2 0.00171 0.00349 0.00124 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 67.12 48.48 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 1 1 3 OMIT 0 8 2 OMIT 1 3 4 OMIT 1 1 5 OMIT 0 2 4 OMIT 1 1 4 OMIT 2 6 1 OMIT 0 4 4 OMIT 1 5 3 REM REM REM WGHT 0.200000 FVAR 2.15910 SC1 4 0.250000 0.250000 0.500000 10.25000 0.14158 0.05256 = 0.03211 0.00000 -0.00189 0.00000 O2 3 0.500000 0.250000 0.425587 10.25000 0.15746 0.07243 = 0.01994 0.00000 0.00000 0.00000 O1 3 0.345105 0.314973 0.596140 11.00000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 C2 1 0.500000 0.370690 0.717525 10.50000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 C6 1 0.500000 0.483933 0.964655 10.50000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 C1 1 0.500000 0.330247 0.629465 10.50000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 C5 1 0.500000 0.445143 0.879915 10.50000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 C3 1 0.667805 0.389305 0.758126 11.00000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 AFIX 43 H3 2 0.780477 0.376759 0.730735 11.00000 -1.20000 AFIX 0 C4 1 0.668179 0.426555 0.839413 11.00000 0.16910 0.10737 = 0.06766 -0.03655 -0.00998 0.00981 AFIX 43 H4 2 0.780917 0.439072 0.866766 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.361013 10.05500 -1.20000 PART 2 C7 1 0.500000 0.250000 0.322188 10.19500 0.15746 0.07243 = 0.01994 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.373287 0.250000 0.298573 10.19500 -1.20000 H7B 2 0.563356 0.284894 0.298573 10.39000 -1.20000 H7C 2 0.563356 0.215106 0.298573 10.39000 -1.20000 AFIX 0 HKLF 4 REM fullruns in Cmma REM wR2 = 0.3570, GooF = S = 1.598, Restrained GooF = 1.545 for all data REM R1 = 0.1158 for 312 Fo > 4sig(Fo) and 0.1266 for all 383 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.546, deepest hole -0.449, 1-sigma level 0.100 Q1 1 0.5000 0.4545 0.8629 10.50000 0.05 0.55 Q2 1 0.5000 0.3226 0.1164 10.50000 0.05 0.32 ; _shelx_res_checksum 41035 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.049 0.250 0.000 238 83 ' ' 2 -0.049 0.750 0.000 238 83 ' ' 3 -0.048 0.500 0.500 235 83 ' ' 4 -0.048 1.000 0.500 235 83 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_4110MPa _database_code_depnum_ccdc_archive 'CCDC 2223548' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.8 H21.8 O10, 3.70(C H4 O), 1.80(H2 O)' _chemical_formula_sum 'Sc2 C37.5 H40.2 O15.5' _chemical_formula_weight 828.82 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4583 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.900 Why? The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.433 41 Report No information given in structure factor report. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.68 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc -0.1(10), Rep 0.05(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -179.9(6), Rep -179.99(8) ...... 7.50 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 12_655 # 7 Check PLAT733_ALERT_1_B Torsion Calc 179.9(6), Rep 179.99(8) ...... 7.50 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 1_555 # 8 Check PLAT733_ALERT_1_B Torsion Calc 0.1(10), Rep -0.05(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvate was modelled using SQUEEZE. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.0769(14) _cell_length_b 22.232(4) _cell_length_c 13.6130(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2141.7(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1457 _cell_measurement_temperature 298 _cell_measurement_pressure 4110000 _cell_measurement_theta_min 1.6000 _cell_measurement_theta_max 13.6670 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.38 _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_correction_T_min 0.5330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0874 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.7165. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 862.4 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_unetI/netI 0.0490 _diffrn_reflns_Laue_measured_fraction_full 0.900 _diffrn_reflns_Laue_measured_fraction_max 0.900 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4190 _diffrn_reflns_point_group_measured_fraction_full 0.900 _diffrn_reflns_point_group_measured_fraction_max 0.900 _diffrn_reflns_theta_full 12.141 _diffrn_reflns_theta_max 12.141 _diffrn_reflns_theta_min 1.617 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 4110000 _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0404001000 _diffrn_orient_matrix_UB_12 -0.0139367000 _diffrn_orient_matrix_UB_13 -0.0176668000 _diffrn_orient_matrix_UB_21 0.0524574000 _diffrn_orient_matrix_UB_22 -0.0140221000 _diffrn_orient_matrix_UB_23 -0.0027487000 _diffrn_orient_matrix_UB_31 -0.0183497000 _diffrn_orient_matrix_UB_32 -0.0092607000 _diffrn_orient_matrix_UB_33 0.0309119000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.900 _diffrn_measured_fraction_theta_max 0.900 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 299 _reflns_number_total 388 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.488 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.074 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 388 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0904 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1424P)^2^+16.9721P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2598 _refine_ls_wR_factor_ref 0.2702 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.025) C7(0.225) H7A(0.225) H7B(0.45) H7C(0.45) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.071(2) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4242(6) 0.079(4) Uani 1 4 d DS T P . . O1 O 0.3432(6) 0.3161(3) 0.5950(4) 0.107(3) Uani 1 1 d D . . . . C2 C 0.500000 0.3715(3) 0.7168(5) 0.107(3) Uani 1 2 d DS T P . . C6 C 0.500000 0.4840(3) 0.9646(6) 0.107(3) Uani 1 2 d DS T P . . C1 C 0.500000 0.3314(3) 0.6285(5) 0.107(3) Uani 1 2 d DS T P B . C5 C 0.500000 0.4455(3) 0.8798(5) 0.107(3) Uani 1 2 d DS T P . . C3 C 0.6696(6) 0.3899(2) 0.7574(4) 0.107(3) Uani 1 1 d D . . . . H3 H 0.783196 0.377444 0.729833 0.129 Uiso 1 1 calc R U . . . C4 C 0.6701(6) 0.4271(2) 0.8394(4) 0.107(3) Uani 1 1 d D . . . . H4 H 0.783822 0.439602 0.867001 0.129 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3599(6) 0.129 Uiso 0.1 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3205(8) 0.079(4) Uani 0.9 4 d DS T P B 2 H7A H 0.372105 0.250000 0.296997 0.095 Uiso 0.45 2 calc R U P B 2 H7B H 0.563948 0.285258 0.296997 0.095 Uiso 0.45 1 calc R U P B 2 H7C H 0.563948 0.214742 0.296997 0.095 Uiso 0.45 1 calc R U P B 2 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 Sc1 0.125(4) 0.056(4) 0.030(3) 0.000 -0.001(2) 0.000 O2 0.129(11) 0.085(10) 0.023(5) 0.000 0.000 0.000 O1 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C2 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C6 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C1 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C5 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C3 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C4 0.147(6) 0.090(5) 0.084(4) -0.040(3) 0.008(4) -0.006(4) C7 0.129(11) 0.085(10) 0.023(5) 0.000 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 Sc1 Sc1 3.5384(7) 2_655 ? Sc1 Sc1 3.5384(7) 2 ? Sc1 O2 2.048(4) . ? Sc1 O2 2.048(4) 13_556 ? Sc1 O1 2.066(6) 7_546 ? Sc1 O1 2.066(6) . ? Sc1 O1 2.066(6) 13_556 ? Sc1 O1 2.066(6) 11_565 ? O2 H2 0.8750(11) . ? O2 C7 1.412(8) . ? O1 C1 1.247(5) . ? C2 C1 1.497(8) . ? C2 C3 1.384(5) 12_655 ? C2 C3 1.384(5) . ? C6 C6 1.198(17) 4_567 ? C6 C5 1.436(8) . ? C5 C4 1.385(5) 12_655 ? C5 C4 1.385(5) . ? C3 H3 0.9300 . ? C3 C4 1.390(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 149.8(2) 13_556 2_655 ? O2 Sc1 Sc1 30.2(2) 13_556 2 ? O2 Sc1 Sc1 149.8(2) . 2 ? O2 Sc1 Sc1 30.2(2) . 2_655 ? O2 Sc1 O2 180.0 13_556 . ? O2 Sc1 O1 92.3(2) . . ? O2 Sc1 O1 87.7(2) 13_556 . ? O2 Sc1 O1 92.3(2) . 11_565 ? O2 Sc1 O1 92.3(2) 13_556 13_556 ? O2 Sc1 O1 87.7(2) . 13_556 ? O2 Sc1 O1 87.7(2) . 7_546 ? O2 Sc1 O1 92.3(2) 13_556 7_546 ? O2 Sc1 O1 87.7(2) 13_556 11_565 ? O1 Sc1 Sc1 71.38(13) 11_565 2_655 ? O1 Sc1 Sc1 71.38(13) . 2_655 ? O1 Sc1 Sc1 108.62(13) 13_556 2_655 ? O1 Sc1 Sc1 71.38(13) 7_546 2 ? O1 Sc1 Sc1 71.38(13) 13_556 2 ? O1 Sc1 Sc1 108.62(13) 11_565 2 ? O1 Sc1 Sc1 108.62(13) . 2 ? O1 Sc1 Sc1 108.62(13) 7_546 2_655 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? O1 Sc1 O1 90.7(3) 13_556 7_546 ? O1 Sc1 O1 89.3(3) 13_556 11_565 ? O1 Sc1 O1 90.7(3) 11_565 . ? O1 Sc1 O1 180.0(2) 13_556 . ? O1 Sc1 O1 89.3(3) 7_546 . ? Sc1 O2 Sc1 119.5(4) 2_655 . ? Sc1 O2 H2 120.2(2) . . ? Sc1 O2 H2 120.2(2) 2_655 . ? C7 O2 Sc1 120.2(2) . . ? C1 O1 Sc1 135.0(5) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 C1 119.9(3) 12_655 . ? C3 C2 C3 120.3(6) . 12_655 ? C6 C6 C5 179.8(5) 4_567 . ? O1 C1 O1 125.8(8) . 12_655 ? O1 C1 C2 117.1(4) . . ? O1 C1 C2 117.1(4) 12_655 . ? C4 C5 C6 119.6(3) . . ? C4 C5 C6 119.6(3) 12_655 . ? C4 C5 C4 120.7(6) 12_655 . ? C2 C3 H3 120.0 . . ? C2 C3 C4 120.0(4) . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7A 109.468(5) . 2_655 ? O2 C7 H7B 109.467(4) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.467(4) . 12_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 16.3(3) . . . 12_655 ? Sc1 O1 C1 C2 -163.7(4) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C6 C5 C4 C3 -179.96(18) . . . . ? C1 C2 C3 C4 -179.92(18) . . . . ? C3 C2 C1 O1 0.05(13) 12_655 . . . ? C3 C2 C1 O1 -179.99(8) 12_655 . . 12_655 ? C3 C2 C1 O1 179.99(8) . . . . ? C3 C2 C1 O1 -0.05(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.1(3) 12_655 . . . ? _shelx_res_file ; TITL MIL53ScEDB_0 in Cmma mil53scedb_13.res created by SHELXL-2019/2 at 09:51:58 on 24-Oct-2022 CELL 0.4859 7.07686 22.23174 13.613 90 90 90 ZERR 2 0.00137 0.00432 0.0015 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 67.6 50.4 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.142400 16.972099 FVAR 2.03980 SC1 4 0.250000 0.250000 0.500000 10.25000 0.12544 0.05599 = 0.03037 0.00000 -0.00105 0.00000 O2 3 0.500000 0.250000 0.424215 10.25000 0.12872 0.08542 = 0.02250 0.00000 0.00000 0.00000 O1 3 0.343214 0.316127 0.594966 11.00000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 C2 1 0.500000 0.371486 0.716753 10.50000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 C6 1 0.500000 0.484023 0.964590 10.50000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 C1 1 0.500000 0.331351 0.628495 10.50000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 C5 1 0.500000 0.445533 0.879832 10.50000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 C3 1 0.669560 0.389943 0.757414 11.00000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 AFIX 43 H3 2 0.783196 0.377444 0.729833 11.00000 -1.20000 AFIX 0 C4 1 0.670124 0.427145 0.839438 11.00000 0.14734 0.08991 = 0.08439 -0.03972 0.00839 -0.00637 AFIX 43 H4 2 0.783822 0.439602 0.867001 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.359938 10.02500 -1.20000 PART 2 C7 1 0.500000 0.250000 0.320504 10.22500 0.12872 0.08542 = 0.02250 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.372105 0.250000 0.296997 10.22500 -1.20000 H7B 2 0.563948 0.285258 0.296997 10.45000 -1.20000 H7C 2 0.563948 0.214742 0.296997 10.45000 -1.20000 AFIX 0 HKLF 4 REM MIL53ScEDB_0 in Cmma REM wR2 = 0.2702, GooF = S = 1.104, Restrained GooF = 1.073 for all data REM R1 = 0.0904 for 299 Fo > 4sig(Fo) and 0.1048 for all 388 data REM 34 parameters refined using 28 restraints END WGHT 0.1674 12.2130 REM Highest difference peak 0.488, deepest hole -0.331, 1-sigma level 0.074 Q1 1 0.5000 0.4009 0.7003 10.50000 0.05 0.35 Q2 1 0.6346 0.4771 0.7822 11.00000 0.05 0.27 ; _shelx_res_checksum 51424 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.041 0.250 0.000 236 92 ' ' 2 -0.041 0.750 0.000 236 92 ' ' 3 -0.052 0.500 0.500 222 76 ' ' 4 -0.055 1.000 0.500 222 76 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_3850MPa _database_code_depnum_ccdc_archive 'CCDC 2223550' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.4 H20.9 O10, 3.90(C H4 O), 1.36(H2 O)' _chemical_formula_sum 'Sc2 C37.3 H39.22 O15.26' _chemical_formula_weight 821.59 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4767 PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.43 Report The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.1(10), Rep 0.05(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -0.1(10), Rep -0.05(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2 Report O2 C7 The ADPs of the hydroxide/methoxide bridge refine to physically unreasonable parameters, possibly due to low data completeness, so are their displacement parameters are refined isotropically. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.71 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvent was modelled was using SQUEEZE. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.450 54 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 11.92 0.450 0.888 509 452 57 #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.1069(18) _cell_length_b 22.297(4) _cell_length_c 13.5858(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2152.8(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1442 _cell_measurement_temperature 298 _cell_measurement_pressure 3850000 _cell_measurement_theta_min 1.6170 _cell_measurement_theta_max 14.0940 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.48 _exptl_absorpt_correction_T_max 0.7449 _exptl_absorpt_correction_T_min 0.5391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0944 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.7237. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 854.2 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1226 _diffrn_reflns_av_unetI/netI 0.0588 _diffrn_reflns_Laue_measured_fraction_full 0.878 _diffrn_reflns_Laue_measured_fraction_max 0.879 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4302 _diffrn_reflns_point_group_measured_fraction_full 0.878 _diffrn_reflns_point_group_measured_fraction_max 0.879 _diffrn_reflns_theta_full 12.636 _diffrn_reflns_theta_max 12.636 _diffrn_reflns_theta_min 1.615 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 3850000 _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0448083000 _diffrn_orient_matrix_UB_12 -0.0132052000 _diffrn_orient_matrix_UB_13 0.0161223000 _diffrn_orient_matrix_UB_21 -0.0488219000 _diffrn_orient_matrix_UB_22 -0.0151121000 _diffrn_orient_matrix_UB_23 0.0036500000 _diffrn_orient_matrix_UB_31 0.0169123000 _diffrn_orient_matrix_UB_32 -0.0084063000 _diffrn_orient_matrix_UB_33 -0.0317671000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.878 _diffrn_measured_fraction_theta_max 0.879 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 315 _reflns_number_total 427 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.596 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.104 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.807 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 32 _refine_ls_number_reflns 428 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.1301 _refine_ls_restrained_S_all 1.753 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4137 _refine_ls_wR_factor_ref 0.4264 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uiso(O2) = Uiso(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.08) C7(0.17) H7A(0.17) H7B(0.34) H7C(0.34) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.077(3) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4241(9) 0.068(5) Uiso 1 4 d DS . P . . O1 O 0.3443(6) 0.3154(3) 0.5958(5) 0.113(4) Uani 1 1 d D . . . . C2 C 0.500000 0.3710(3) 0.7173(5) 0.113(4) Uani 1 2 d DS T P . . C6 C 0.500000 0.4842(3) 0.9651(6) 0.113(4) Uani 1 2 d DS T P . . C1 C 0.500000 0.3306(3) 0.6290(6) 0.113(4) Uani 1 2 d DS T P B . C5 C 0.500000 0.4454(3) 0.8802(6) 0.113(4) Uani 1 2 d DS T P . . C3 C 0.6685(6) 0.3895(3) 0.7579(5) 0.113(4) Uani 1 1 d D . . . . H3 H 0.781757 0.376994 0.730444 0.136 Uiso 1 1 calc R U . . . C4 C 0.6689(6) 0.4269(3) 0.8396(5) 0.113(4) Uani 1 1 d D . . . . H4 H 0.782287 0.439367 0.866923 0.136 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3597(9) 0.136 Uiso 0.32 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3207(11) 0.068(5) Uiso 0.68 4 d DS . P B 2 H7A H 0.372645 0.250000 0.297169 0.082 Uiso 0.34 2 calc R U P B 2 H7B H 0.563678 0.285155 0.297170 0.082 Uiso 0.34 1 calc R U P B 2 H7C H 0.563677 0.214845 0.297169 0.082 Uiso 0.34 1 calc R U P B 2 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 Sc1 0.134(6) 0.062(5) 0.035(4) 0.000 -0.003(2) 0.000 O1 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(4) C2 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(4) C6 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(4) C1 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(4) C5 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(4) C3 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(4) C4 0.167(9) 0.101(6) 0.073(5) -0.039(3) -0.003(5) 0.007(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 Sc1 Sc1 3.5534(9) 2 ? Sc1 Sc1 3.5534(9) 2_655 ? Sc1 O2 2.054(6) 13_556 ? Sc1 O2 2.054(6) . ? Sc1 O1 2.065(6) 11_565 ? Sc1 O1 2.065(6) 7_546 ? Sc1 O1 2.065(6) . ? Sc1 O1 2.065(6) 13_556 ? O2 H2 0.8750(10) . ? O2 C7 1.405(9) . ? O1 C1 1.242(5) . ? C2 C1 1.501(8) . ? C2 C3 1.382(5) 12_655 ? C2 C3 1.382(5) . ? C6 C6 1.181(19) 4_567 ? C6 C5 1.441(8) . ? C5 C4 1.385(5) 12_655 ? C5 C4 1.385(5) . ? C3 H3 0.9300 . ? C3 C4 1.387(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2 2_655 ? O2 Sc1 Sc1 149.9(3) . 2 ? O2 Sc1 Sc1 30.1(3) . 2_655 ? O2 Sc1 Sc1 149.9(3) 13_556 2_655 ? O2 Sc1 Sc1 30.1(3) 13_556 2 ? O2 Sc1 O2 180.0 . 13_556 ? O2 Sc1 O1 92.0(3) 13_556 7_546 ? O2 Sc1 O1 88.0(3) . 7_546 ? O2 Sc1 O1 92.0(3) 13_556 13_556 ? O2 Sc1 O1 92.0(3) . . ? O2 Sc1 O1 88.0(3) 13_556 . ? O2 Sc1 O1 88.0(3) 13_556 11_565 ? O2 Sc1 O1 92.0(3) . 11_565 ? O2 Sc1 O1 88.0(3) . 13_556 ? O1 Sc1 Sc1 71.06(14) 13_556 2 ? O1 Sc1 Sc1 71.06(14) 7_546 2 ? O1 Sc1 Sc1 108.94(14) . 2 ? O1 Sc1 Sc1 71.06(14) 11_565 2_655 ? O1 Sc1 Sc1 71.06(14) . 2_655 ? O1 Sc1 Sc1 108.94(14) 13_556 2_655 ? O1 Sc1 Sc1 108.94(14) 7_546 2_655 ? O1 Sc1 Sc1 108.94(14) 11_565 2 ? O1 Sc1 O1 90.2(4) 13_556 11_565 ? O1 Sc1 O1 89.8(4) . 11_565 ? O1 Sc1 O1 180.0 . 13_556 ? O1 Sc1 O1 89.8(4) 13_556 7_546 ? O1 Sc1 O1 90.2(4) . 7_546 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? Sc1 O2 Sc1 119.8(6) 2_655 . ? Sc1 O2 H2 120.1(3) . . ? Sc1 O2 H2 120.1(3) 2_655 . ? C7 O2 Sc1 120.1(3) . . ? C1 O1 Sc1 135.3(5) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 C1 119.9(3) 12_655 . ? C3 C2 C3 120.2(6) . 12_655 ? C6 C6 C5 179.8(6) 4_567 . ? O1 C1 O1 125.9(9) . 12_655 ? O1 C1 C2 117.1(4) . . ? O1 C1 C2 117.1(4) 12_655 . ? C4 C5 C6 119.9(3) . . ? C4 C5 C6 119.9(3) 12_655 . ? C4 C5 C4 120.2(7) 12_655 . ? C2 C3 H3 120.0 . . ? C2 C3 C4 120.0(4) . . ? C4 C3 H3 120.0 . . ? C5 C4 H4 120.1 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? O2 C7 H7A 109.473(6) . 2_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.473(4) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.473(4) . 12_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 15.4(4) . . . 12_655 ? Sc1 O1 C1 C2 -164.7(4) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C6 C5 C4 C3 179.96(18) . . . . ? C1 C2 C3 C4 -179.94(18) . . . . ? C3 C2 C1 O1 0.05(13) 12_655 . . . ? C3 C2 C1 O1 179.99(8) 12_655 . . 12_655 ? C3 C2 C1 O1 -179.99(8) . . . . ? C3 C2 C1 O1 -0.05(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.0(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns in Cmma mil53scedb_12.res created by SHELXL-2019/2 at 09:50:38 on 24-Oct-2022 CELL 0.4859 7.10688 22.29673 13.58585 90 90 90 ZERR 2 0.00177 0.00446 0.00157 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 66.72 46.88 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 1 1 3 OMIT 0 2 4 OMIT 1 1 5 OMIT 1 3 4 OMIT 2 6 1 OMIT 0 8 2 OMIT 0 4 4 OMIT 1 1 4 REM REM REM WGHT 0.200000 FVAR 2.05945 SC1 4 0.250000 0.250000 0.500000 10.25000 0.13351 0.06171 = 0.03494 0.00000 -0.00311 0.00000 O2 3 0.500000 0.250000 0.424143 10.25000 0.06814 O1 3 0.344336 0.315355 0.595760 11.00000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 C2 1 0.500000 0.370989 0.717327 10.50000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 C6 1 0.500000 0.484199 0.965111 10.50000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 C1 1 0.500000 0.330559 0.629034 10.50000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 C5 1 0.500000 0.445448 0.880222 10.50000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 C3 1 0.668543 0.389543 0.757910 11.00000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 AFIX 43 H3 2 0.781757 0.376994 0.730444 11.00000 -1.20000 AFIX 0 C4 1 0.668943 0.426859 0.839553 11.00000 0.16700 0.10051 = 0.07289 -0.03857 -0.00275 0.00667 AFIX 43 H4 2 0.782287 0.439367 0.866923 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.359737 10.08000 -1.20000 PART 2 C7 1 0.500000 0.250000 0.320723 10.17000 0.06814 AFIX 33 H7A 2 0.372645 0.250000 0.297169 10.17000 -1.20000 H7B 2 0.563678 0.285155 0.297170 10.34000 -1.20000 H7C 2 0.563677 0.214845 0.297169 10.34000 -1.20000 AFIX 0 HKLF 4 REM fullruns in Cmma REM wR2 = 0.4264, GooF = S = 1.807, Restrained GooF = 1.753 for all data REM R1 = 0.1301 for 316 Fo > 4sig(Fo) and 0.1487 for all 428 data REM 32 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.596, deepest hole -1.069, 1-sigma level 0.104 Q1 1 0.5000 0.4573 0.8662 10.50000 0.05 0.60 Q2 1 0.5000 0.2500 0.2157 10.25000 0.05 0.41 ; _shelx_res_checksum 42791 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.043 0.250 0.000 235 82 ' ' 2 -0.042 0.750 0.000 235 82 ' ' 3 -0.050 0.500 0.500 230 84 ' ' 4 -0.050 1.000 0.500 230 84 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_2840MPa _database_code_depnum_ccdc_archive 'CCDC 2223549' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.4 H21.2 O10, 4.10(C H4 O), 1.44(H2 O)' _chemical_formula_sum 'Sc2 C37.5 H40.48 O15.76' _chemical_formula_weight 833.27 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4812 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.822 Why? PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.36 Report PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 6.0 Note PLAT733_ALERT_1_B Torsion Calc 0.1(8), Rep 0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -0.1(8), Rep -0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvent was modelled using SQUEEZE. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.72 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.1(8), Rep 0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -179.9(5), Rep -179.98(7) ...... 7.14 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 12_655 # 7 Check PLAT733_ALERT_1_B Torsion Calc 179.9(5), Rep 179.98(7) ...... 7.14 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 1_555 # 8 Check PLAT733_ALERT_1_B Torsion Calc -0.1(8), Rep -0.02(13) ...... 6.15 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.454 70 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 12.04 0.454 0.864 516 446 70 #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.213(2) _cell_length_b 22.789(3) _cell_length_c 13.4966(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2218.6(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2011 _cell_measurement_temperature 298 _cell_measurement_pressure 2840000 _cell_measurement_theta_min 2.0510 _cell_measurement_theta_max 12.7380 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.37 _exptl_absorpt_correction_T_max 0.7438 _exptl_absorpt_correction_T_min 0.5820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0929 before and 0.0793 after correction. The Ratio of minimum to maximum transmission is 0.7825. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 833.27 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_Laue_measured_fraction_full 0.822 _diffrn_reflns_Laue_measured_fraction_max 0.822 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4581 _diffrn_reflns_point_group_measured_fraction_full 0.822 _diffrn_reflns_point_group_measured_fraction_max 0.822 _diffrn_reflns_theta_full 12.758 _diffrn_reflns_theta_max 12.758 _diffrn_reflns_theta_min 1.599 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 2840000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.822 _diffrn_measured_fraction_theta_max 0.822 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 358 _reflns_number_total 420 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.650 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.090 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.663 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 418 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.1106 _refine_ls_restrained_S_all 1.609 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3495 _refine_ls_wR_factor_ref 0.3636 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.07) C7(0.18) H7A(0.18) H7B(0.36) H7C(0.36) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.075(3) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4250(6) 0.075(5) Uani 1 4 d DS T P . . O1 O 0.3466(6) 0.3146(2) 0.5971(4) 0.107(3) Uani 1 1 d D . . . . C2 C 0.500000 0.3703(2) 0.7181(4) 0.107(3) Uani 1 2 d DS T P . . C6 C 0.500000 0.4836(3) 0.9643(5) 0.107(3) Uani 1 2 d DS T P . . C1 C 0.500000 0.3299(3) 0.6304(5) 0.107(3) Uani 1 2 d DS T P B . C5 C 0.500000 0.4447(3) 0.8799(5) 0.107(3) Uani 1 2 d DS T P . . C3 C 0.6666(6) 0.3888(2) 0.7585(4) 0.107(3) Uani 1 1 d D . . . . H3 H 0.778192 0.376273 0.731174 0.128 Uiso 1 1 calc R U . . . C4 C 0.6666(6) 0.4261(2) 0.8395(4) 0.107(3) Uani 1 1 d D . . . . H4 H 0.778176 0.438569 0.866769 0.128 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3602(6) 0.128 Uiso 0.28 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3211(8) 0.075(5) Uani 0.72 4 d DS T P B 2 H7A H 0.374521 0.250000 0.297438 0.090 Uiso 0.36 2 calc R U P B 2 H7B H 0.562739 0.284396 0.297438 0.090 Uiso 0.36 1 calc R U P B 2 H7C H 0.562739 0.215604 0.297438 0.090 Uiso 0.36 1 calc R U P B 2 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 Sc1 0.162(6) 0.034(3) 0.027(3) 0.000 -0.0016(19) 0.000 O2 0.155(16) 0.053(7) 0.018(5) 0.000 0.000 0.000 O1 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C2 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C6 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C1 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C5 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C3 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C4 0.185(9) 0.088(4) 0.048(4) -0.031(2) -0.004(4) -0.001(4) C7 0.155(16) 0.053(7) 0.018(5) 0.000 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 Sc1 Sc1 3.6066(10) 2_655 ? Sc1 Sc1 3.6066(10) 2 ? Sc1 O2 2.068(4) 13_556 ? Sc1 O2 2.068(4) . ? Sc1 O1 2.090(5) 7_546 ? Sc1 O1 2.090(5) . ? Sc1 O1 2.090(5) 13_556 ? Sc1 O1 2.090(5) 11_565 ? O2 H2 0.8750(10) . ? O2 C7 1.402(9) . ? O1 C1 1.245(5) . ? C2 C1 1.499(8) . ? C2 C3 1.385(5) 12_655 ? C2 C3 1.385(5) . ? C6 C6 1.221(17) 4_567 ? C6 C5 1.442(8) . ? C5 C4 1.386(5) 12_655 ? C5 C4 1.386(5) . ? C3 H3 0.9300 . ? C3 C4 1.385(6) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 29.3(2) . 2_655 ? O2 Sc1 Sc1 150.7(2) . 2 ? O2 Sc1 Sc1 29.3(2) 13_556 2 ? O2 Sc1 Sc1 150.7(2) 13_556 2_655 ? O2 Sc1 O2 180.0 . 13_556 ? O2 Sc1 O1 89.1(2) 13_556 . ? O2 Sc1 O1 90.9(2) . . ? O2 Sc1 O1 89.1(2) 13_556 11_565 ? O2 Sc1 O1 89.1(2) . 13_556 ? O2 Sc1 O1 90.9(2) 13_556 13_556 ? O2 Sc1 O1 90.9(2) 13_556 7_546 ? O2 Sc1 O1 89.1(2) . 7_546 ? O2 Sc1 O1 90.9(2) . 11_565 ? O1 Sc1 Sc1 70.52(13) 11_565 2_655 ? O1 Sc1 Sc1 70.52(13) . 2_655 ? O1 Sc1 Sc1 109.48(13) 13_556 2_655 ? O1 Sc1 Sc1 70.52(13) 7_546 2 ? O1 Sc1 Sc1 70.52(13) 13_556 2 ? O1 Sc1 Sc1 109.48(13) 11_565 2 ? O1 Sc1 Sc1 109.48(13) . 2 ? O1 Sc1 Sc1 109.48(13) 7_546 2_655 ? O1 Sc1 O1 180.0(2) 11_565 7_546 ? O1 Sc1 O1 89.5(3) 13_556 7_546 ? O1 Sc1 O1 90.5(3) 13_556 11_565 ? O1 Sc1 O1 89.5(3) 11_565 . ? O1 Sc1 O1 180.0 13_556 . ? O1 Sc1 O1 90.5(3) 7_546 . ? Sc1 O2 Sc1 121.4(4) 2_655 . ? Sc1 O2 H2 119.3(2) . . ? Sc1 O2 H2 119.3(2) 2_655 . ? C7 O2 Sc1 119.3(2) . . ? C1 O1 Sc1 136.1(5) . . ? C3 C2 C1 119.8(3) 12_655 . ? C3 C2 C1 119.8(3) . . ? C3 C2 C3 120.3(6) . 12_655 ? C6 C6 C5 179.9(5) 4_567 . ? O1 C1 O1 125.5(7) . 12_655 ? O1 C1 C2 117.3(4) 12_655 . ? O1 C1 C2 117.3(4) . . ? C4 C5 C6 119.9(3) 12_655 . ? C4 C5 C6 119.9(3) . . ? C4 C5 C4 120.1(6) 12_655 . ? C2 C3 H3 120.1 . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3 120.1 . . ? C5 C4 H4 120.0 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.0 . . ? O2 C7 H7A 109.469(5) . 2_655 ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.469(3) . 12_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.469(3) . 2_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 14.3(3) . . . 12_655 ? Sc1 O1 C1 C2 -165.7(3) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C6 C5 C4 C3 -179.98(18) . . . . ? C1 C2 C3 C4 -179.97(18) . . . . ? C3 C2 C1 O1 0.02(13) 12_655 . . . ? C3 C2 C1 O1 -179.98(7) 12_655 . . 12_655 ? C3 C2 C1 O1 179.98(7) . . . . ? C3 C2 C1 O1 -0.02(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.1(3) 12_655 . . . ? _shelx_res_file ; TITL FULLRUNS in Cmma mil53scedb_09.res created by SHELXL-2019/2 at 09:46:17 on 24-Oct-2022 CELL 0.4859 7.21315 22.78881 13.49662 90 90 90 ZERR 2 0.00197 0.00255 0.00125 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 66.88 47.52 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 0 10 OMIT 0 8 6 REM REM REM WGHT 0.200000 FVAR 2.78164 SC1 4 0.250000 0.250000 0.500000 10.25000 0.16235 0.03423 = 0.02726 0.00000 -0.00164 0.00000 O2 3 0.500000 0.250000 0.425048 10.25000 0.15489 0.05315 = 0.01780 0.00000 0.00000 0.00000 O1 3 0.346620 0.314562 0.597083 11.00000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C2 1 0.500000 0.370269 0.718116 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C6 1 0.500000 0.483554 0.964314 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C1 1 0.500000 0.329910 0.630430 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C5 1 0.500000 0.444729 0.879915 10.50000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 C3 1 0.666619 0.388815 0.758452 11.00000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 AFIX 43 H3 2 0.778192 0.376273 0.731174 11.00000 -1.20000 AFIX 0 C4 1 0.666565 0.426070 0.839482 11.00000 0.18514 0.08789 = 0.04815 -0.03097 -0.00390 -0.00093 AFIX 43 H4 2 0.778176 0.438569 0.866769 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.360217 10.07000 -1.20000 PART 2 C7 1 0.500000 0.250000 0.321147 10.18000 0.15489 0.05315 = 0.01780 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.374521 0.250000 0.297438 10.18000 -1.20000 H7B 2 0.562739 0.284396 0.297438 10.36000 -1.20000 H7C 2 0.562739 0.215604 0.297438 10.36000 -1.20000 AFIX 0 HKLF 4 REM FULLRUNS in Cmma REM wR2 = 0.3636, GooF = S = 1.663, Restrained GooF = 1.609 for all data REM R1 = 0.1106 for 356 Fo > 4sig(Fo) and 0.1189 for all 418 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.650, deepest hole -0.424, 1-sigma level 0.090 Q1 1 0.5000 0.4581 0.8657 10.50000 0.05 0.65 Q2 1 0.5000 0.3820 0.7085 10.50000 0.05 0.49 ; _shelx_res_checksum 28595 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.048 0.250 0.000 247 100 ' ' 2 -0.048 0.750 0.000 247 100 ' ' 3 -0.054 0.500 0.500 248 78 ' ' 4 -0.054 1.000 0.500 248 78 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_4600MPa _database_code_depnum_ccdc_archive 'CCDC 2223554' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-04 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.7 H21.8 O10, 2.50(C H4 O), 1.70(H2 O)' _chemical_formula_sum 'Sc2 C36.2 H35.2 O14.2' _chemical_formula_weight 788.87 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4811 PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low . 0.871 Why? The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.72 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT733_ALERT_1_B Torsion Calc 0.1(10), Rep 0.04(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 12_655 1_555 1_555 1_555 # 6 Check PLAT733_ALERT_1_B Torsion Calc -0.1(10), Rep -0.04(13) ...... 7.69 s.u.-R C3 -C2 -C1 -O1 1_555 1_555 1_555 12_655 # 9 Check These are correct. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.454 55 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 12.04 0.454 0.884 510 451 59 #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The solvate was modelled using SQUEEZE. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.0380(15) _cell_length_b 22.061(6) _cell_length_c 13.652(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2119.8(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1290 _cell_measurement_temperature 298 _cell_measurement_pressure 4600000 _cell_measurement_theta_max 12.4980 _cell_measurement_theta_min 1.6110 _shelx_estimated_absorpt_T_max 0.996 _shelx_estimated_absorpt_T_min 0.983 _exptl_absorpt_coefficient_mu 0.38 _exptl_absorpt_correction_T_max 0.7440 _exptl_absorpt_correction_T_min 0.4288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0910 before and 0.0616 after correction. The Ratio of minimum to maximum transmission is 0.5763. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 817.8 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1271 _diffrn_reflns_av_unetI/netI 0.0676 _diffrn_reflns_Laue_measured_fraction_full 0.871 _diffrn_reflns_Laue_measured_fraction_max 0.871 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4470 _diffrn_reflns_point_group_measured_fraction_full 0.871 _diffrn_reflns_point_group_measured_fraction_max 0.871 _diffrn_reflns_theta_full 12.755 _diffrn_reflns_theta_max 12.755 _diffrn_reflns_theta_min 2.314 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 4600000 _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0351337000 _diffrn_orient_matrix_UB_12 -0.0152848000 _diffrn_orient_matrix_UB_13 -0.0180729000 _diffrn_orient_matrix_UB_21 0.0559187000 _diffrn_orient_matrix_UB_22 -0.0129336000 _diffrn_orient_matrix_UB_23 -0.0001688000 _diffrn_orient_matrix_UB_31 -0.0202863000 _diffrn_orient_matrix_UB_32 -0.0091101000 _diffrn_orient_matrix_UB_33 0.0306844000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.871 _diffrn_measured_fraction_theta_max 0.871 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 300 _reflns_number_total 427 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.421 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.070 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 427 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.1003 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1424P)^2^+17.0763P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2767 _refine_ls_wR_factor_ref 0.2932 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.0375) C7(0.2125) H7A(0.2125) H7B(0.425) H7C(0.425) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.075(2) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4234(7) 0.079(4) Uani 1 4 d DS T P . . O1 O 0.3425(6) 0.3157(3) 0.5953(4) 0.111(3) Uani 1 1 d D . . . . C2 C 0.500000 0.3713(3) 0.7173(5) 0.111(3) Uani 1 2 d DS T P . . C6 C 0.500000 0.4841(3) 0.9650(6) 0.111(3) Uani 1 2 d DS T P . . C1 C 0.500000 0.3310(3) 0.6290(5) 0.111(3) Uani 1 2 d DS T P B . C5 C 0.500000 0.4455(3) 0.8803(5) 0.111(3) Uani 1 2 d DS T P . . C3 C 0.6702(6) 0.3898(2) 0.7579(4) 0.111(3) Uani 1 1 d D . . . . H3 H 0.784456 0.377222 0.730323 0.133 Uiso 1 1 calc R U . . . C4 C 0.6711(6) 0.4271(2) 0.8398(4) 0.111(3) Uani 1 1 d D . . . . H4 H 0.785490 0.439524 0.867338 0.133 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3593(7) 0.133 Uiso 0.15 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3202(8) 0.079(4) Uani 0.85 4 d DS T P B 2 H7A H 0.371399 0.250000 0.296741 0.095 Uiso 0.425 2 calc R U P B 2 H7B H 0.564301 0.285530 0.296741 0.095 Uiso 0.425 1 calc R U P B 2 H7C H 0.564301 0.214470 0.296741 0.095 Uiso 0.425 1 calc R U P B 2 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 Sc1 0.128(4) 0.058(4) 0.037(3) 0.000 -0.003(2) 0.000 O2 0.127(11) 0.078(11) 0.033(6) 0.000 0.000 0.000 O1 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C2 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C6 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C1 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C5 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C3 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C4 0.166(6) 0.091(5) 0.078(4) -0.036(3) -0.001(4) -0.012(4) C7 0.127(11) 0.078(11) 0.033(6) 0.000 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 Sc1 Sc1 3.5190(8) 2 ? Sc1 Sc1 3.5190(8) 2_655 ? Sc1 O2 2.047(5) . ? Sc1 O2 2.047(5) 13_556 ? Sc1 O1 2.054(6) 11_565 ? Sc1 O1 2.054(6) 7_546 ? Sc1 O1 2.054(6) . ? Sc1 O1 2.054(6) 13_556 ? O2 H2 0.8750(11) . ? O2 C7 1.409(9) . ? O1 C1 1.246(5) . ? C2 C1 1.497(8) . ? C2 C3 1.382(5) 12_655 ? C2 C3 1.382(5) . ? C6 C6 1.185(17) 4_567 ? C6 C5 1.436(8) . ? C5 C4 1.386(5) 12_655 ? C5 C4 1.386(5) . ? C3 H3 0.9300 . ? C3 C4 1.388(7) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2 2_655 ? O2 Sc1 Sc1 30.7(2) 13_556 2 ? O2 Sc1 Sc1 149.3(2) 13_556 2_655 ? O2 Sc1 Sc1 30.7(2) . 2_655 ? O2 Sc1 Sc1 149.3(2) . 2 ? O2 Sc1 O2 180.0(4) 13_556 . ? O2 Sc1 O1 87.1(2) . 7_546 ? O2 Sc1 O1 92.9(2) 13_556 7_546 ? O2 Sc1 O1 87.1(2) . 13_556 ? O2 Sc1 O1 87.1(2) 13_556 . ? O2 Sc1 O1 92.9(2) . . ? O2 Sc1 O1 92.9(2) . 11_565 ? O2 Sc1 O1 87.1(2) 13_556 11_565 ? O2 Sc1 O1 92.9(2) 13_556 13_556 ? O1 Sc1 Sc1 71.51(13) 13_556 2 ? O1 Sc1 Sc1 71.51(13) 7_546 2 ? O1 Sc1 Sc1 108.49(13) . 2 ? O1 Sc1 Sc1 71.51(13) 11_565 2_655 ? O1 Sc1 Sc1 71.51(13) . 2_655 ? O1 Sc1 Sc1 108.49(13) 13_556 2_655 ? O1 Sc1 Sc1 108.49(13) 7_546 2_655 ? O1 Sc1 Sc1 108.49(13) 11_565 2 ? O1 Sc1 O1 90.3(3) 13_556 11_565 ? O1 Sc1 O1 89.7(3) . 11_565 ? O1 Sc1 O1 180.0 . 13_556 ? O1 Sc1 O1 89.7(3) 13_556 7_546 ? O1 Sc1 O1 90.3(3) . 7_546 ? O1 Sc1 O1 180.0(3) 11_565 7_546 ? Sc1 O2 Sc1 118.6(4) 2_655 . ? Sc1 O2 H2 120.7(2) . . ? Sc1 O2 H2 120.7(2) 2_655 . ? C7 O2 Sc1 120.7(2) . . ? C1 O1 Sc1 135.0(5) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 C1 119.9(3) 12_655 . ? C3 C2 C3 120.2(6) . 12_655 ? C6 C6 C5 180.0(5) 4_567 . ? O1 C1 O1 125.5(8) . 12_655 ? O1 C1 C2 117.2(4) . . ? O1 C1 C2 117.2(4) 12_655 . ? C4 C5 C6 119.7(3) . . ? C4 C5 C6 119.7(3) 12_655 . ? C4 C5 C4 120.6(6) 12_655 . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.2(4) . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7A 109.470(5) . 2_655 ? O2 C7 H7B 109.470(5) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.470(4) . 12_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 15.8(4) . . . 12_655 ? Sc1 O1 C1 C2 -164.2(4) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C6 C5 C4 C3 -179.98(18) . . . . ? C1 C2 C3 C4 -179.93(18) . . . . ? C3 C2 C1 O1 0.04(13) 12_655 . . . ? C3 C2 C1 O1 -179.99(7) 12_655 . . 12_655 ? C3 C2 C1 O1 179.99(7) . . . . ? C3 C2 C1 O1 -0.04(13) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.1(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns_a.res in Cmma mil53scedb_14.res created by SHELXL-2019/2 at 09:53:20 on 24-Oct-2022 REM Old TITL fullruns in Cmme #67 REM SHELXT solution in Cmma: R1 0.294, Rweak 0.020, Alpha 0.095 REM 0.812 for 20 systematic absences, Orientation as input REM Formula found by SHELXT: C19 O9 Sc CELL 0.4859 7.038 22.0614 13.6522 90 90 90 ZERR 2 0.0015 0.0057 0.002 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 67.4 49.6 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 2 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.142400 17.076300 FVAR 4.85722 SC1 4 0.250000 0.250000 0.500000 10.25000 0.12841 0.05846 = 0.03671 0.00000 -0.00297 0.00000 O2 3 0.500000 0.250000 0.423419 10.25000 0.12651 0.07806 = 0.03267 0.00000 0.00000 0.00000 O1 3 0.342543 0.315677 0.595340 11.00000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 C2 1 0.500000 0.371260 0.717264 10.50000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 C6 1 0.500000 0.484095 0.965037 10.50000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 C1 1 0.500000 0.330999 0.628973 10.50000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 C5 1 0.500000 0.445521 0.880317 10.50000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 C3 1 0.670220 0.389769 0.757914 11.00000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 AFIX 43 H3 2 0.784456 0.377222 0.730323 11.00000 -1.20000 AFIX 0 C4 1 0.671087 0.427050 0.839845 11.00000 0.16557 0.09053 = 0.07762 -0.03643 -0.00074 -0.01189 AFIX 43 H4 2 0.785490 0.439524 0.867338 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.359327 10.03750 -1.20000 PART 2 C7 1 0.500000 0.250000 0.320181 10.21250 0.12651 0.07806 = 0.03267 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.371399 0.250000 0.296741 10.21250 -1.20000 H7B 2 0.564301 0.285530 0.296741 10.42500 -1.20000 H7C 2 0.564301 0.214470 0.296741 10.42500 -1.20000 AFIX 0 HKLF 4 REM fullruns_a.res in Cmma REM wR2 = 0.2932, GooF = S = 1.095, Restrained GooF = 1.065 for all data REM R1 = 0.1003 for 300 Fo > 4sig(Fo) and 0.1225 for all 427 data REM 34 parameters refined using 28 restraints END WGHT 0.1482 16.0634 REM Highest difference peak 0.421, deepest hole -0.323, 1-sigma level 0.070 Q1 1 0.5000 0.3889 0.6958 10.50000 0.05 0.35 Q2 1 0.6346 0.4788 0.7801 11.00000 0.05 0.33 ; _shelx_res_checksum 31796 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.041 0.250 0.000 230 69 ' ' 2 -0.040 0.750 0.000 230 69 ' ' 3 -0.054 0.500 0.500 222 57 ' ' 4 -0.057 1.000 0.500 222 57 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_1610MPa _database_code_depnum_ccdc_archive 'CCDC 2223553' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C33.9 H22.2 O10, 3.48(C H4 O), 1.86(H2 O)' _chemical_formula_sum 'Sc2 C36.74 H35.36 O13.74' _chemical_formula_weight 786.66 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- CIF VALIDATION REPORT: #------------------------------------------------------------------------------- PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.44 Report PLAT934_ALERT_3_B Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 2 Check The crystal is in a diamond anvil cell at high-pressure, limiting data completeness to <40% and reducing the quality of the crystal. #------------------------------------------------------------------------------- PLAT911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L= 0.588 179 Report Theta sin(th)/Lambda Complete Expected Measured Total Missing 13.26 0.500 0.831 718 597 121 14.62 0.550 0.833 935 779 156 15.65 0.588 0.838 1114 933 181 #------------------------------------------------------------------------------- PLAT920_ALERT_1_B Theta(Max) in CIF and FCF Differ by ........... 0.95 Degree The reported values were output after applying an absorption correction in SADABS. #------------------------------------------------------------------------------- PLAT990_ALERT_1_B Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note The formula was ammended to account for the solvate that was calculated from SQUEEZE. The composition of the disordered solvate was approximated from a rough model of the solvate positions, which was then removed from the model and SQUEEZE performed. #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0007 0.0006 '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' O O -0.0001 0.0023 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.1054 0.1588 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.3292(16) _cell_length_b 23.332(3) _cell_length_c 13.3614(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2284.9(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2028 _cell_measurement_temperature 298 _cell_measurement_pressure 1610000 _cell_measurement_theta_min 2.0810 _cell_measurement_theta_max 16.5980 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.35 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_correction_T_min 0.4865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. The \l/2 correction factor is not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 815.44 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_unetI/netI 0.0588 _diffrn_reflns_Laue_measured_fraction_full 0.808 _diffrn_reflns_Laue_measured_fraction_max 0.809 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6455 _diffrn_reflns_point_group_measured_fraction_full 0.808 _diffrn_reflns_point_group_measured_fraction_max 0.809 _diffrn_reflns_theta_full 16.594 _diffrn_reflns_theta_max 16.594 _diffrn_reflns_theta_min 1.584 _diffrn_ambient_temperature 298 _diffrn_ambient_pressure 1610000 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.808 _diffrn_measured_fraction_theta_max 0.809 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -35.00 35.00 0.20 0.40 -90.00 -11.00 0.00 -- 350 2 \w -133.00 -85.00 0.20 0.40 -- -11.00 70.00 -24.23 240 3 \w -141.00 -85.00 0.20 0.40 -- -11.00 70.00 155.77 280 4 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 155.77 155 5 \w -113.00 -82.00 0.20 0.40 -- 12.00 70.00 -24.23 155 6 \w -101.00 -41.00 0.20 0.40 -- 12.00 -70.00 24.23 300 7 \w -102.00 -41.00 0.20 0.40 -- 12.00 -70.00-155.77 305 8 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00-155.77 165 9 \w -97.00 -64.00 0.20 0.40 -- -11.00 -70.00 24.23 165 ; _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'I19-2, Diamond Light Source' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.4589 _diffrn_source synchrotron _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 679 _reflns_number_total 887 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 1.357 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.147 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.888 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 887 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.1300 _refine_ls_restrained_S_all 1.893 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4145 _refine_ls_wR_factor_ref 0.4401 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H) groups 2. Restrained distances O2-H2 0.875 with sigma of 0.001 O2-C7 1.4 with sigma of 0.02 C7-O2 1.4 with sigma of 0.01 C4-C3 1.39 with sigma of 0.01 C5-C4 1.39 with sigma of 0.01 C6-C5 1.44 with sigma of 0.01 C3-C2 1.39 with sigma of 0.01 C2-C1 1.502 with sigma of 0.01 O1-C1 1.245 with sigma of 0.01 C6-C4 2.454 with sigma of 0.01 C1-C3 2.497 with sigma of 0.01 O1-C2 2.349 with sigma of 0.01 C3-C5 2.4 with sigma of 0.01 C2-C4 2.4 with sigma of 0.01 O1_$1-O1 2.213 with sigma of 0.01 C3_$1-C3 2.4 with sigma of 0.01 C4-C4_$1 2.4 with sigma of 0.01 C4_$1-C2 2.4 with sigma of 0.01 C5-C3_$1 2.4 with sigma of 0.01 3. Restrained planarity C1, O1, O1_$1, C2, C5, C6, C6_$2 with sigma of 0.01 C2, C5, C3_$1, C3, C4_$1, C1, C6, C4 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) Uanis(C6) = Uanis(O1) = Uanis(C1) Uanis(O2) = Uanis(C7) Uanis(C2) = Uanis(C6) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(O1) 5. Others Fixed Sof: H2(0.0175) C7(0.2325) H7A(0.2325) H7B(0.465) H7C(0.465) 6.a Me refined with riding coordinates: C7(H7A,H7B,H7C) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.0236(13) Uani 1 4 d S T P B . O2 O 0.500000 0.250000 0.4249(5) 0.035(3) Uani 1 4 d DS T P . . O1 O 0.3486(5) 0.31441(17) 0.5969(3) 0.0505(18) Uani 1 1 d D . . . . C2 C 0.500000 0.37042(19) 0.7173(4) 0.0505(18) Uani 1 2 d DS T P . . C6 C 0.500000 0.4844(2) 0.9638(5) 0.0505(18) Uani 1 2 d DS T P . . C1 C 0.500000 0.3297(2) 0.6302(4) 0.0505(18) Uani 1 2 d DS T P B . C5 C 0.500000 0.4456(2) 0.8794(4) 0.0505(18) Uani 1 2 d DS T P . . C3 C 0.6634(6) 0.38920(17) 0.7577(3) 0.0505(18) Uani 1 1 d D . . . . H3 H 0.773365 0.376708 0.730751 0.061 Uiso 1 1 calc R U . . . C4 C 0.6634(6) 0.42683(18) 0.8390(3) 0.0505(18) Uani 1 1 d D . . . . H4 H 0.773321 0.439351 0.865945 0.061 Uiso 1 1 calc R U . . . H2 H 0.500000 0.250000 0.3594(5) 0.061 Uiso 0.07 4 d DS U P A 1 C7 C 0.500000 0.250000 0.3193(6) 0.035(3) Uani 0.93 4 d DS T P B 2 H7A H 0.376508 0.250000 0.295310 0.042 Uiso 0.465 2 calc R U P B 2 H7B H 0.561746 0.283595 0.295310 0.042 Uiso 0.465 1 calc R U P B 2 H7C H 0.561746 0.216405 0.295310 0.042 Uiso 0.465 1 calc R U P B 2 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 Sc1 0.024(3) 0.0283(18) 0.0183(15) 0.000 -0.0009(11) 0.000 O2 0.052(9) 0.042(5) 0.011(3) 0.000 0.000 0.000 O1 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C2 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C6 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C1 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C5 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C3 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C4 0.042(5) 0.058(3) 0.051(2) -0.0306(16) -0.001(2) -0.006(2) C7 0.052(9) 0.042(5) 0.011(3) 0.000 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 Sc1 Sc1 3.6646(8) 2_655 ? Sc1 Sc1 3.6646(8) 2 ? Sc1 O2 2.089(3) . ? Sc1 O2 2.089(3) 13_556 ? Sc1 O1 2.112(4) 7_546 ? Sc1 O1 2.112(4) . ? Sc1 O1 2.112(4) 13_556 ? Sc1 O1 2.112(4) 11_565 ? O2 H2 0.8750(10) . ? O2 C7 1.411(8) . ? O1 C1 1.247(4) . ? C2 C1 1.502(7) . ? C2 C3 1.385(5) 12_655 ? C2 C3 1.385(5) . ? C6 C6 1.210(14) 4_567 ? C6 C5 1.447(7) . ? C5 C4 1.384(5) 12_655 ? C5 C4 1.384(5) . ? C3 H3 0.9300 . ? C3 C4 1.396(6) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 2_655 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 12_655 ? C7 H7B 0.9600 . ? C7 H7B 0.9600 2_655 ? C7 H7C 0.9600 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 151.29(16) 13_556 2_655 ? O2 Sc1 Sc1 28.71(16) 13_556 2 ? O2 Sc1 Sc1 151.29(16) . 2 ? O2 Sc1 Sc1 28.71(16) . 2_655 ? O2 Sc1 O2 180.0(3) 13_556 . ? O2 Sc1 O1 89.68(16) . . ? O2 Sc1 O1 90.32(16) 13_556 . ? O2 Sc1 O1 89.68(16) . 11_565 ? O2 Sc1 O1 89.68(16) 13_556 13_556 ? O2 Sc1 O1 90.32(16) . 13_556 ? O2 Sc1 O1 90.32(16) . 7_546 ? O2 Sc1 O1 89.68(16) 13_556 7_546 ? O2 Sc1 O1 90.32(16) 13_556 11_565 ? O1 Sc1 Sc1 69.98(11) 11_565 2_655 ? O1 Sc1 Sc1 69.98(11) . 2_655 ? O1 Sc1 Sc1 110.02(11) 13_556 2_655 ? O1 Sc1 Sc1 69.98(11) 7_546 2 ? O1 Sc1 Sc1 69.98(11) 13_556 2 ? O1 Sc1 Sc1 110.02(11) 11_565 2 ? O1 Sc1 Sc1 110.02(11) . 2 ? O1 Sc1 Sc1 110.02(11) 7_546 2_655 ? O1 Sc1 O1 180.00(19) 11_565 7_546 ? O1 Sc1 O1 90.7(2) 13_556 7_546 ? O1 Sc1 O1 89.3(2) 13_556 11_565 ? O1 Sc1 O1 90.7(2) 11_565 . ? O1 Sc1 O1 180.0 13_556 . ? O1 Sc1 O1 89.3(2) 7_546 . ? Sc1 O2 Sc1 122.6(3) 2_655 . ? Sc1 O2 H2 118.71(16) . . ? Sc1 O2 H2 118.71(16) 2_655 . ? C7 O2 Sc1 118.71(16) . . ? C1 O1 Sc1 136.6(4) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 C1 120.2(3) 12_655 . ? C3 C2 C3 119.7(5) . 12_655 ? C6 C6 C5 178.1(5) 4_567 . ? O1 C1 O1 125.6(6) . 12_655 ? O1 C1 C2 117.2(3) . . ? O1 C1 C2 117.2(3) 12_655 . ? C4 C5 C6 120.1(3) . . ? C4 C5 C6 120.1(3) 12_655 . ? C4 C5 C4 119.7(5) 12_655 . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.2(4) . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7A 109.471(5) . 2_655 ? O2 C7 H7B 109.469(2) . 2_655 ? O2 C7 H7B 109.5 . . ? O2 C7 H7B 109.469(2) . 12_655 ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 14.3(3) . . . 12_655 ? Sc1 O1 C1 C2 -166.1(3) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C6 C5 C4 C3 179.80(18) . . . . ? C1 C2 C3 C4 -179.75(17) . . . . ? C3 C2 C1 O1 0.28(12) 12_655 . . . ? C3 C2 C1 O1 179.93(7) 12_655 . . 12_655 ? C3 C2 C1 O1 -179.93(7) . . . . ? C3 C2 C1 O1 -0.28(12) . . . 12_655 ? C3 C2 C3 C4 0.0(2) 12_655 . . . ? C4 C5 C4 C3 0.0(3) 12_655 . . . ? _shelx_res_file ; TITL fullruns in Cmma mil53scedb_06.res created by SHELXL-2019/2 at 09:41:05 on 24-Oct-2022 CELL 0.4859 7.32919 23.33182 13.36144 90 90 90 ZERR 2 0.00156 0.00256 0.00106 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H O Sc DISP C -0.0007 0.0006 5.6364 DISP H 0 0 0.6034 DISP O -0.0001 0.0023 11.8357 DISP Sc 0.1054 0.1588 430.4159 UNIT 67.72 50.88 20 4 EQIV $1 1-X,+Y,+Z EQIV $2 +X,1-Y,2-Z DFIX 0.875 0.001 O2 H2 DFIX 1.4 O2 C7 DFIX 1.4 0.01 C7 O2 EADP C2 C5 C3 C4 EADP C6 O1 C1 DFIX 1.39 0.01 C4 C3 DFIX 1.39 0.01 C5 C4 DFIX 1.44 0.01 C6 C5 DFIX 1.39 0.01 C3 C2 DFIX 1.502 0.01 C2 C1 DFIX 1.245 0.01 O1 C1 DFIX 2.454 0.01 C6 C4 DFIX 2.497 0.01 C1 C3 DFIX 2.349 0.01 O1 C2 DFIX 2.4 0.01 C3 C5 DFIX 2.4 0.01 C2 C4 DFIX 2.213 0.01 O1_$1 O1 DFIX 2.4 0.01 C3_$1 C3 DFIX 2.4 0.01 C4 C4_$1 DFIX 2.4 0.01 C4_$1 C2 FLAT 0.01 C1 O1 O1_$1 C2 C5 C6 C6_$2 FLAT 0.01 C2 C5 C3_$1 C3 C4_$1 C1 C6 C4 DFIX 2.4 0.01 C5 C3_$1 EADP O2 C7 EADP C2 C6 C1 C5 C4 C3 O1 L.S. 10 PLAN 4 SIZE 0.04 0.04 0.15 TEMP 298 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.200000 FVAR 3.80663 SC1 4 0.250000 0.250000 0.500000 10.25000 0.02414 0.02829 = 0.01827 0.00000 -0.00093 0.00000 O2 3 0.500000 0.250000 0.424882 10.25000 0.05220 0.04221 = 0.01114 0.00000 0.00000 0.00000 O1 3 0.348636 0.314410 0.596945 11.00000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 C2 1 0.500000 0.370421 0.717279 10.50000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 C6 1 0.500000 0.484431 0.963813 10.50000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 C1 1 0.500000 0.329747 0.630187 10.50000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 C5 1 0.500000 0.445563 0.879418 10.50000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 C3 1 0.663380 0.389201 0.757749 11.00000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 AFIX 43 H3 2 0.773365 0.376708 0.730751 11.00000 -1.20000 AFIX 0 C4 1 0.663357 0.426832 0.838956 11.00000 0.04177 0.05845 = 0.05117 -0.03059 -0.00091 -0.00643 AFIX 43 H4 2 0.773321 0.439351 0.865945 11.00000 -1.20000 AFIX 0 PART 1 H2 2 0.500000 0.250000 0.359396 10.01750 -1.20000 PART 2 C7 1 0.500000 0.250000 0.319259 10.23250 0.05220 0.04221 = 0.01114 0.00000 0.00000 0.00000 AFIX 33 H7A 2 0.376508 0.250000 0.295310 10.23250 -1.20000 H7B 2 0.561746 0.283595 0.295310 10.46500 -1.20000 H7C 2 0.561746 0.216405 0.295310 10.46500 -1.20000 AFIX 0 HKLF 4 REM fullruns in Cmma REM wR2 = 0.4401, GooF = S = 1.888, Restrained GooF = 1.893 for all data REM R1 = 0.1300 for 679 Fo > 4sig(Fo) and 0.1452 for all 887 data REM 34 parameters refined using 28 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.357, deepest hole -0.902, 1-sigma level 0.147 Q1 1 0.5000 0.4593 0.8741 10.50000 0.05 1.11 Q2 1 0.6558 0.4140 0.7179 11.00000 0.05 0.71 Q3 1 0.6795 0.4480 0.7970 11.00000 0.05 0.70 Q4 1 0.3822 0.2197 0.4635 11.00000 0.05 0.46 ; _shelx_res_checksum 77679 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; # SQUEEZE RESULTS (Version = 70422) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.047 0.250 0.000 254 98 ' ' 2 -0.047 0.750 0.000 254 98 ' ' 3 -0.050 0.500 0.500 261 65 ' ' 4 -0.050 1.000 0.500 261 65 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? #END ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_Ambient _database_code_depnum_ccdc_archive 'CCDC 2223556' loop_ _audit_author_name _audit_author_address 'Stephen Moggach' ;The University of Western Australia Australia ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-06-19 downloaded from the CCDC. ; __audit_creation_date 2022-10-04 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _chemical_name_common GUF-1 _chemical_name_systematic ? _chemical_formula_moiety 'Sc2 C32 H18 O10, 1.2(C3 H7 NO)' _chemical_formula_sum 'Sc2 H24 N1.2 O10.6' _chemical_formula_weight 713.67 _chemical_melting_point ? _refine_special_details ; #------------------------------------------------------------------------------- DENSD01_ALERT_1_A The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.90 <> 1.10 Crystal density given = 1.041 Calculated crystal density = 0.438 SHFSU01_ALERT_2_A The absolute value of parameter shift to su ratio > 0.20 Absolute value of the parameter shift to su ratio given 1.854 Additional refinement cycles may be required. PLAT043_ALERT_1_A Calculated and Reported Mol. Weight Differ by .. 206.58 Check PLAT046_ALERT_1_A Reported Z, MW and D(calc) are Inconsistent .... 0.438 Check PLAT051_ALERT_1_A Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 11.16 % The reported values are correct. #------------------------------------------------------------------------------- PLAT080_ALERT_2_A Maximum Shift/Error ............................ 1.85 Why ? There is adsorbed solvate disordered over a special positiona in partially occupied sites, making them difficult to refine. The molecules were either placed as a rigid fragment or had it geometry restrained, and its occupancy set to its approximately refined value. #------------------------------------------------------------------------------- PLAT601_ALERT_2_A Unit Cell Contains Solvent Accessible VOIDS of . 270 Ang**3 The structure is a porous metal-organic framework/ #------------------------------------------------------------------------------- ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 67 _space_group_name_H-M_alt 'C m m e' _space_group_name_Hall '-C 2b 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 7.3054(5) _cell_length_b 26.5207(17) _cell_length_c 11.7550(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2277.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 28.26 _shelx_estimated_absorpt_T_max 0.986 _shelx_estimated_absorpt_T_min 0.950 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1290 before and 0.0709 after correction. The Ratio of minimum to maximum transmission is 0.9071. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 731 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_unetI/netI 0.0218 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 31343 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.323 _diffrn_reflns_theta_min 1.536 _diffrn_ambient_temperature 273.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1486 _reflns_number_total 1562 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 1.881 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.151 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 42 _refine_ls_number_reflns 1562 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0904 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 1.854 _refine_ls_shift/su_mean 0.206 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1612P)^2^+14.5173P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2662 _refine_ls_wR_factor_ref 0.2682 _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups, H7 of C7 At 1.2 times of: H4 of C4, H3 of C3, H2 of C9 2. Restrained distances O2-H2 0.875 with sigma of 0.001 N1-C8 \\sim N1-C9 with sigma of 0.02 3. Restrained planarity C7, O3, N1, C8, C9 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C7 \\sim O3 \\sim N1 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uiso(O3) = Uiso(C7) = Uiso(N1) = Uiso(C8) = Uiso(C9) Uanis(C6) = Uanis(C5) = Uanis(C3) = Uanis(C4) = Uanis(O1) = Uanis(C2) = Uanis(C1) 5. Rigid body (RIGU) restrains C7, O3, N1, C8, C9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: C7(0.075) H7(0.075) O3(0.075) N1(0.15) C8(0.15) H8A(0.15) H8B(0.15) H8C(0.15) C9(0.075) H9A(0.075) H9B(0.075) H9C(0.075) 7.a Free rotating group: C7(O3,N1,C8,C9) 7.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C7(H7) 7.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Sc1 Sc 0.250000 0.250000 0.500000 0.0134(4) Uani 1 4 d S T P . . O2 O 0.500000 0.250000 0.4175(4) 0.0226(9) Uani 1 4 d DS T P . . O1 O 0.3486(4) 0.30579(10) 0.6119(2) 0.0364(5) Uani 1 1 d . . . . . C2 C 0.500000 0.3662(2) 0.7236(5) 0.0364(5) Uani 1 2 d S T P . . C6 C 0.500000 0.4838(2) 0.9646(5) 0.0364(5) Uani 1 2 d S T P . . C1 C 0.500000 0.3227(2) 0.6422(5) 0.0364(5) Uani 1 2 d S T P . . C5 C 0.500000 0.4444(2) 0.8813(5) 0.0364(5) Uani 1 2 d S T P . . C3 C 0.6636(5) 0.38601(15) 0.7618(3) 0.0364(5) Uani 1 1 d . . . . . H3 H 0.773699 0.373304 0.734389 0.044 Uiso 1 1 calc R U . . . C4 C 0.6643(5) 0.42491(14) 0.8412(3) 0.0364(5) Uani 1 1 d . . . . . H4 H 0.774776 0.437869 0.867481 0.044 Uiso 1 1 calc R U . . . C7 C 0.502(13) 0.2911(10) 1.0927(19) 0.064(4) Uiso 0.075 1 d G U P A -1 H7 H 0.471654 0.322384 1.062041 0.096 Uiso 0.075 1 calc R U P A -1 O3 O 0.520(19) 0.2883(13) 1.1957(17) 0.064(4) Uiso 0.075 1 d G U P A -1 N1 N 0.522(6) 0.2508(9) 1.0179(13) 0.064(4) Uiso 0.15 1 d DG U P A -1 C8 C 0.536(5) 0.2587(13) 0.8966(13) 0.064(4) Uiso 0.15 1 d DG U P A -1 H8A H 0.452308 0.284831 0.874093 0.096 Uiso 0.15 1 calc R U P A -1 H8B H 0.505482 0.228035 0.857531 0.096 Uiso 0.15 1 calc R U P A -1 H8C H 0.658489 0.268518 0.877573 0.096 Uiso 0.15 1 calc R U P A -1 C9 C 0.534(10) 0.2004(9) 1.060(2) 0.064(4) Uiso 0.075 1 d DG U P A -1 H9A H 0.598815 0.179881 1.005591 0.096 Uiso 0.075 1 calc R U P A -1 H9B H 0.413404 0.187097 1.070730 0.096 Uiso 0.075 1 calc R U P A -1 H9C H 0.598958 0.200258 1.130779 0.096 Uiso 0.075 1 calc R U P A -1 H2 H 0.500000 0.250000 0.3430(4) 0.077 Uiso 1 4 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 Sc1 0.0113(6) 0.0135(6) 0.0154(6) 0.000 -0.0020(3) 0.000 O2 0.0140(19) 0.039(3) 0.0150(19) 0.000 0.000 0.000 O1 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) C2 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) C6 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) C1 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) C5 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) C3 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) C4 0.0266(8) 0.0388(9) 0.0437(10) -0.0260(7) 0.0012(8) -0.0046(7) _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 Sc1 Sc1 3.6527(3) 2_655 ? Sc1 Sc1 3.6527(3) 2 ? Sc1 O2 2.068(2) . ? Sc1 O2 2.068(2) 13_556 ? Sc1 O1 2.107(2) 13_556 ? Sc1 O1 2.107(2) 11_565 ? Sc1 O1 2.107(2) . ? Sc1 O1 2.107(2) 7_546 ? O2 H2 0.8750(10) . ? O1 C1 1.246(3) . ? C2 C1 1.498(7) . ? C2 C3 1.380(4) 12_655 ? C2 C3 1.380(4) . ? C6 C6 1.198(10) 9_667 ? C6 C5 1.431(7) . ? C5 C4 1.389(4) 12_655 ? C5 C4 1.389(4) . ? C3 H3 0.9300 . ? C3 C4 1.391(4) . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? C7 O3 1.2204 . ? C7 N1 1.3928 . ? N1 C8 1.4447 . ? N1 C9 1.4270 . ? C8 H8A 0.9603 . ? C8 H8B 0.9603 . ? C8 H8C 0.9603 . ? C9 H9A 1.0353 . ? C9 H9B 1.0353 . ? C9 H9C 1.0353 . ? 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 Sc1 Sc1 Sc1 180.0 2_655 2 ? O2 Sc1 Sc1 27.98(10) . 2_655 ? O2 Sc1 Sc1 27.98(10) 13_556 2 ? O2 Sc1 Sc1 152.02(10) . 2 ? O2 Sc1 Sc1 152.02(10) 13_556 2_655 ? O2 Sc1 O2 180.0 13_556 . ? O2 Sc1 O1 89.48(10) . 11_565 ? O2 Sc1 O1 90.52(10) . 13_556 ? O2 Sc1 O1 90.52(10) 13_556 11_565 ? O2 Sc1 O1 89.48(10) 13_556 13_556 ? O2 Sc1 O1 89.48(10) . . ? O2 Sc1 O1 90.52(10) . 7_546 ? O2 Sc1 O1 89.48(10) 13_556 7_546 ? O2 Sc1 O1 90.52(10) 13_556 . ? O1 Sc1 Sc1 70.00(7) 11_565 2_655 ? O1 Sc1 Sc1 70.00(7) 13_556 2 ? O1 Sc1 Sc1 110.00(7) 7_546 2_655 ? O1 Sc1 Sc1 70.00(7) 7_546 2 ? O1 Sc1 Sc1 110.00(7) 11_565 2 ? O1 Sc1 Sc1 110.00(7) 13_556 2_655 ? O1 Sc1 Sc1 110.00(7) . 2 ? O1 Sc1 Sc1 70.00(7) . 2_655 ? O1 Sc1 O1 180.00(12) 11_565 7_546 ? O1 Sc1 O1 89.22(17) 13_556 7_546 ? O1 Sc1 O1 90.78(17) 13_556 11_565 ? O1 Sc1 O1 90.78(17) 7_546 . ? O1 Sc1 O1 180.0 13_556 . ? O1 Sc1 O1 89.22(17) 11_565 . ? Sc1 O2 Sc1 124.0(2) 2_655 . ? Sc1 O2 H2 117.98(10) 2_655 . ? Sc1 O2 H2 117.98(10) . . ? C1 O1 Sc1 137.4(3) . . ? C3 C2 C1 120.0(2) 12_655 . ? C3 C2 C1 120.0(2) . . ? C3 C2 C3 119.9(4) 12_655 . ? C6 C6 C5 179.1(10) 9_667 . ? O1 C1 O1 125.2(4) . 12_655 ? O1 C1 C2 117.4(2) 12_655 . ? O1 C1 C2 117.4(2) . . ? C4 C5 C6 120.2(2) . . ? C4 C5 C6 120.2(2) 12_655 . ? C4 C5 C4 119.5(4) 12_655 . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.3(3) . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? O3 C7 H7 118.9 . . ? O3 C7 N1 124.5 . . ? N1 C7 H7 116.5 . . ? C7 N1 C8 121.3 . . ? C7 N1 C9 120.6 . . ? C9 N1 C8 118.1 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.4 . . ? H8A C8 H8C 109.4 . . ? H8B C8 H8C 109.4 . . ? N1 C9 H9A 117.5 . . ? N1 C9 H9B 117.5 . . ? N1 C9 H9C 117.5 . . ? H9A C9 H9B 100.4 . . ? H9A C9 H9C 100.4 . . ? H9B C9 H9C 100.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 O1 C1 O1 -4.5(11) . . . 12_655 ? Sc1 O1 C1 C2 177.0(4) . . . . ? C2 C3 C4 C5 -0.8(8) . . . . ? C6 C5 C4 C3 178.8(5) . . . . ? C1 C2 C3 C4 -177.2(5) . . . . ? C3 C2 C1 O1 0.2(9) . . . 12_655 ? C3 C2 C1 O1 -0.2(9) 12_655 . . . ? C3 C2 C1 O1 178.8(5) . . . . ? C3 C2 C1 O1 -178.8(5) 12_655 . . 12_655 ? C3 C2 C3 C4 1.8(9) 12_655 . . . ? C4 C5 C4 C3 -0.2(9) 12_655 . . . ? O3 C7 N1 C8 -167.07(7) . . . . ? O3 C7 N1 C9 11.6 . . . . ? _shelx_res_file ; TITL mo_ajt_8_236_rt_0m_a.res in Cmma mo_ajt_8_236_rt_0m.res created by SHELXL-2018/3 at 16:02:14 on 04-Oct-2022 REM Old TITL mo_AJT_8_236_RT_0m in Cmma REM SHELXT solution in Cmma: R1 0.163, Rweak 0.008, Alpha 0.020 REM 0.497 for 60 systematic absences, Orientation as input REM Formula found by SHELXT: C16 O6 Sc CELL 0.71073 7.3054 26.5207 11.755 90 90 90 ZERR 2 0.0005 0.0017 0.0009 0 0 0 LATT 7 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H N O Sc UNIT 68.8 48 2.4 21.2 4 FLAT C7 O3 N1 C8 C9 SADI N1 C8 N1 C9 RIGU C7 O3 N1 C8 C9 SIMU C7 O3 N1 C8 C9 EADP O3 C7 N1 C8 C9 DFIX 0.875 0.001 O2 H2 EADP C6 C5 C3 C4 O1 C2 C1 L.S. 10 PLAN 15 SIZE 0.04 0.04 0.15 TEMP 0 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.161200 14.517301 FVAR 3.94360 SC1 5 0.250000 0.250000 0.500000 10.25000 0.01134 0.01352 = 0.01537 0.00000 -0.00195 0.00000 O2 4 0.500000 0.250000 0.417457 10.25000 0.01402 0.03881 = 0.01495 0.00000 0.00000 0.00000 O1 4 0.348634 0.305789 0.611901 11.00000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 C2 1 0.500000 0.366203 0.723600 10.50000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 C6 1 0.500000 0.483754 0.964576 10.50000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 C1 1 0.500000 0.322741 0.642226 10.50000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 C5 1 0.500000 0.444405 0.881285 10.50000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 C3 1 0.663565 0.386012 0.761821 11.00000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 AFIX 43 H3 2 0.773699 0.373304 0.734389 11.00000 -1.20000 AFIX 0 C4 1 0.664283 0.424913 0.841223 11.00000 0.02661 0.03883 = 0.04366 -0.02596 0.00119 -0.00460 AFIX 43 H4 2 0.774776 0.437869 0.867481 11.00000 -1.20000 AFIX 6 PART -1 C7 1 0.501553 0.291126 1.092707 10.07500 0.06401 AFIX 43 H7 2 0.471654 0.322384 1.062041 10.07500 -1.50000 AFIX 5 O3 4 0.519965 0.288294 1.195693 10.07500 0.06401 N1 3 0.522207 0.250796 1.017906 10.15000 0.06401 C8 1 0.535758 0.258709 0.896601 10.15000 0.06401 AFIX 137 H8A 2 0.452308 0.284831 0.874093 10.15000 -1.50000 H8B 2 0.505482 0.228035 0.857531 10.15000 -1.50000 H8C 2 0.658489 0.268518 0.877573 10.15000 -1.50000 AFIX 5 C9 1 0.534339 0.200384 1.059668 10.07500 0.06401 AFIX 137 H9A 2 0.598815 0.179881 1.005591 10.07500 -1.50000 H9B 2 0.413404 0.187097 1.070730 10.07500 -1.50000 H9C 2 0.598958 0.200258 1.130779 10.07500 -1.50000 AFIX 0 PART 0 H2 2 0.500000 0.250000 0.343022 10.25000 -1.20000 HKLF 4 REM mo_ajt_8_236_rt_0m_a.res in Cmma REM wR2 = 0.2682, GooF = S = 1.073, Restrained GooF = 1.080 for all data REM R1 = 0.0904 for 1486 Fo > 4sig(Fo) and 0.0925 for all 1562 data REM 42 parameters refined using 8 restraints END WGHT 0.1609 14.3192 REM Highest difference peak 1.881, deepest hole -0.866, 1-sigma level 0.151 Q1 1 0.5000 0.2788 1.0732 10.50000 0.05 0.74 Q2 1 0.6461 0.4389 0.7983 11.00000 0.05 0.59 Q3 1 0.5000 0.2819 0.9568 10.50000 0.05 0.41 Q4 1 0.6646 0.3908 0.8194 11.00000 0.05 0.41 Q5 1 0.6544 0.4025 0.7182 11.00000 0.05 0.40 Q6 1 0.6483 0.3676 0.7934 11.00000 0.05 0.39 Q7 1 0.3377 0.3191 0.5745 11.00000 0.05 0.39 Q8 1 0.6527 0.4004 0.8742 11.00000 0.05 0.39 Q9 1 0.5000 0.3203 1.0158 10.50000 0.05 0.37 Q10 1 0.6661 0.4785 0.7875 11.00000 0.05 0.29 Q11 1 0.7733 0.4647 0.8071 11.00000 0.05 0.28 Q12 1 0.5000 0.4746 0.8031 10.50000 0.05 0.25 Q13 1 0.5000 0.4737 1.0508 10.50000 0.05 0.22 Q14 1 0.5509 0.4834 0.8176 11.00000 0.05 0.22 Q15 1 0.7437 0.4433 0.7354 11.00000 0.05 0.18 ; _shelx_res_checksum 38816 _olex2_submission_special_instructions 'No special instructions were received'