# 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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -17.20 -10.00   0.20    0.40 -90.00 -11.00   0.00    --    36
  2  ω   -128.40-120.60   0.20    0.40    --  -11.00  70.00 -24.23   39
  3  ω   -129.60-120.40   0.20    0.40    --  -11.00  70.00 155.77   46
  4  ω   -107.80 -95.80   0.20    0.40    --   12.00  70.00 155.77   60
  5  ω   -105.40 -96.00   0.20    0.40    --   12.00  70.00 -24.23   47
  6  ω    -61.80 -50.60   0.20    0.40    --   12.00 -70.00  24.23   56
  7  ω    -58.40 -48.80   0.20    0.40    --   12.00 -70.00-155.77   48
  8  ω    -83.80 -72.00   0.20    0.40    --  -11.00 -70.00-155.77   59
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <I/s> 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 <olex2.extras>
REM <HklSrc "%./710MPa.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%.\\mil53scedb_solvent_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_07_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <I/s> 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 <olex2.extras>
REM <HklSrc "%.\\mil53scedb_02_solvent_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_08_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_09_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_15_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_11_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.1424P)²+16.9721P] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_13_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_12_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_09_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.1424P)²+17.0763P] where P=(Fo²+2Fc²)/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 <I/s> 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 <olex2.extras>
REM <HklSrc "%./mil53scedb_14_sqd.hkl">
REM </olex2.extras>

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 λ/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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  35.00   0.20    0.40 -90.00 -11.00   0.00    --   350
  2  ω   -133.00 -85.00   0.20    0.40    --  -11.00  70.00 -24.23  240
  3  ω   -141.00 -85.00   0.20    0.40    --  -11.00  70.00 155.77  280
  4  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 155.77  155
  5  ω   -113.00 -82.00   0.20    0.40    --   12.00  70.00 -24.23  155
  6  ω   -101.00 -41.00   0.20    0.40    --   12.00 -70.00  24.23  300
  7  ω   -102.00 -41.00   0.20    0.40    --   12.00 -70.00-155.77  305
  8  ω    -97.00 -64.00   0.20    0.40    --  -11.00 -70.00-155.77  165
  9  ω    -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       'ω and φ 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 > 2σ(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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 <olex2.extras>
REM <HklSrc "%./mil53scedb_06_sqd.hkl">
REM </olex2.extras>

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 λ/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       'φ and ω 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 > 2σ(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/[σ²(Fo²)+(0.1612P)²+14.5173P] where P=(Fo²+2Fc²)/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 <I/s> 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 <olex2.extras>
REM <HklSrc "%.\\mo_ajt_8_236_rt_0m_sqd.hkl">
REM </olex2.extras>

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'
