# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_furil_p1_crystal3_0ma
_database_code_depnum_ccdc_archive 'CCDC 2343198'
loop_
_audit_author_name
_audit_author_address
'Dongzhou Zhang'
;Hawaii Institute of Geophysics and Planetology, University of Hawaii at Manoa
United States of America
;
_audit_update_record             
;
2024-03-25 deposited with the CCDC.	2025-01-02 downloaded from the CCDC.
;
_audit_creation_date             2023-06-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            'Furil, phase I'
_chemical_name_systematic        Di(furan-2-yl)ethanedione
_chemical_formula_moiety         'C10 H6 O4'
_chemical_formula_sum            'C10 H6 O4'
_chemical_formula_weight         190.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0022 0.0020 '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'

_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           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   14.6170(9)
_cell_length_b                   30.092(12)
_cell_length_c                   3.6052(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1585.7(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    152
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      12.025
_cell_measurement_theta_min      3.405
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.050
_exptl_absorpt_correction_T_max  0.7274
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1081 before and 0.0808 after correction.
The Ratio of minimum to maximum transmission is 0.8952.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.1262
_diffrn_reflns_Laue_measured_fraction_full 0.317
_diffrn_reflns_Laue_measured_fraction_max 0.184
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            969
_diffrn_reflns_point_group_measured_fraction_full 0.315
_diffrn_reflns_point_group_measured_fraction_max 0.175
_diffrn_reflns_theta_full        15.094
_diffrn_reflns_theta_max         23.224
_diffrn_reflns_theta_min         3.404
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.317
_diffrn_measured_fraction_theta_max 0.184
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       ?
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.434
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    0.313
_reflns_Friedel_fraction_max     0.164
_reflns_number_gt                205
_reflns_number_total             439
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Flack x determined using 62 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   5.4(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         439
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2018
_refine_ls_R_factor_gt           0.1158
_refine_ls_restrained_S_all      1.363
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2823
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C004(H004), C005(H005), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_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
O001 O 0.5789(4) 0.5912(10) 0.474(3) 0.041(3) Uiso 1 1 d . . . . .
C003 C 0.5009(8) 0.5225(12) 0.575(3) 0.035(3) Uiso 1 1 d . . . . .
C004 C 0.6602(6) 0.5328(11) 0.298(3) 0.039(3) Uiso 1 1 d . . . . .
H004 H 0.677832 0.503680 0.251282 0.046 Uiso 1 1 calc R U . . .
C005 C 0.6629(8) 0.6078(15) 0.329(4) 0.054(4) Uiso 1 1 d . . . . .
H005 H 0.680689 0.637373 0.305667 0.064 Uiso 1 1 calc R U . . .
C1 C 0.7109(7) 0.5714(11) 0.233(4) 0.045(3) Uiso 1 1 d . . . . .
H1 H 0.769841 0.571806 0.135676 0.053 Uiso 1 1 calc R U . . .
C3 C 0.5810(6) 0.5468(14) 0.442(4) 0.034(4) Uiso 1 1 d . . . . .
O1 O 0.4316(4) 0.5436(9) 0.702(2) 0.050(3) Uiso 1 1 d . . . . .

_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
O001 C005 1.43(2) . ?
O001 C3 1.34(4) . ?
C003 C003 1.36(7) 2_665 ?
C003 C3 1.46(3) . ?
C003 O1 1.28(3) . ?
C004 H004 0.9300 . ?
C004 C1 1.40(4) . ?
C004 C3 1.34(3) . ?
C005 H005 0.9300 . ?
C005 C1 1.35(5) . ?
C1 H1 0.9300 . ?

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
C3 O001 C005 107.4(18) . . ?
C003 C003 C3 121(2) 2_665 . ?
O1 C003 C003 118.6(17) . 2_665 ?
O1 C003 C3 120(3) . . ?
C1 C004 H004 127.3 . . ?
C3 C004 H004 127.3 . . ?
C3 C004 C1 105(3) . . ?
O001 C005 H005 127.6 . . ?
C1 C005 O001 105(3) . . ?
C1 C005 H005 127.6 . . ?
C004 C1 H1 124.6 . . ?
C005 C1 C004 110.9(15) . . ?
C005 C1 H1 124.6 . . ?
O001 C3 C003 117(2) . . ?
C004 C3 O001 111(2) . . ?
C004 C3 C003 132(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
O001 C005 C1 C004 2.1(18) . . . . ?
C003 C003 C3 O001 -175.9(10) 2_665 . . . ?
C003 C003 C3 C004 1.9(19) 2_665 . . . ?
C005 O001 C3 C003 -180.0(11) . . . . ?
C005 O001 C3 C004 1.8(15) . . . . ?
C1 C004 C3 O001 -0.6(17) . . . . ?
C1 C004 C3 C003 -178.4(13) . . . . ?
C3 O001 C005 C1 -2.3(15) . . . . ?
C3 C004 C1 C005 -1.0(19) . . . . ?
O1 C003 C3 O001 2.6(19) . . . . ?
O1 C003 C3 C004 -179.6(12) . . . . ?

_shelx_res_file                  
;
TITL furil_p1_crystal3_0ma_a.res in Fdd2
    furil_p1_crystal3_0ma.res
    created by SHELXL-2019/1 at 13:58:01 on 29-Jun-2023
REM Old TITL __TMP__ in Fdd2
REM SHELXT solution in Fdd2: R1 0.252, Rweak 0.058, Alpha 0.191
REM <I/s> 0.979 for 9 systematic absences, Orientation as input
REM Flack x = -0.670 ( 2.836 ) from 69 Parsons' quotients
REM Formula found by SHELXT: C3 O2
CELL 0.434 14.617 30.0917 3.6052 90 90 90
ZERR 8 0.0009 0.0124 0.0003 0 0 0
LATT -4
SYMM -X,-Y,+Z
SYMM 0.25+X,0.25-Y,0.25+Z
SYMM 0.25-X,0.25+Y,0.25+Z
SFAC C O H
DISP C 0.0001 0.0005 5.3074
DISP H 0 0 0.6003
DISP O 0.0022 0.002 10.704
UNIT 80 32 48

L.S. 10
PLAN  5
TEMP 0
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\Furil_P1_crystal3_0ma.hkl">
REM </olex2.extras>

WGHT    0.100000
FVAR       0.55933
O001  2    0.578879    0.591152    0.474480    11.00000    0.04125
C003  1    0.500921    0.522520    0.575201    11.00000    0.03526
C004  1    0.660217    0.532844    0.298026    11.00000    0.03868
AFIX  43
H004  3    0.677832    0.503680    0.251282    11.00000   -1.20000
AFIX   0
C005  1    0.662920    0.607829    0.328952    11.00000    0.05353
AFIX  43
H005  3    0.680689    0.637373    0.305667    11.00000   -1.20000
AFIX   0
C1    1    0.710891    0.571362    0.232656    11.00000    0.04453
AFIX  43
H1    3    0.769841    0.571806    0.135676    11.00000   -1.20000
AFIX   0
C3    1    0.581000    0.546769    0.442063    11.00000    0.03371
O1    2    0.431573    0.543576    0.701891    11.00000    0.05000
HKLF 4




REM  furil_p1_crystal3_0ma_a.res in Fdd2
REM wR2 = 0.2823, GooF = S = 1.365, Restrained GooF = 1.363 for all data
REM R1 = 0.1158 for 205 Fo > 4sig(Fo) and 0.2018 for all 439 data
REM 29 parameters refined using 1 restraints

END

WGHT      0.1928      0.2609

REM Highest difference peak  0.325,  deepest hole -0.275,  1-sigma level  0.063
Q1    1   0.4277  0.5477  0.5341  11.00000  0.05    0.33
Q2    1   0.5822  0.5828  0.3129  11.00000  0.05    0.29
Q3    1   0.5781  0.5877  0.6454  11.00000  0.05    0.28
Q4    1   0.4317  0.5442  0.8723  11.00000  0.05    0.23
Q5    1   0.6534  0.5889  0.5102  11.00000  0.05    0.22
;
_shelx_res_checksum              88560
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_ATOM007_furil_p1_crystal3_0ma 
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Anisotropic ADP refinement leads to unphysical thermal ellipsoid 
parameters because of the low peak/parameter ratio limited by the DAC opening 
angle.
;
_vrf_PLAT029_furil_p1_crystal3_0ma 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.317 Why?  
RESPONSE: Collection ability is limited by the opening angle of the diamond 
anvil cell.
;
####################################################################### 
# 
# 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_p2_0m_5
_database_code_depnum_ccdc_archive 'CCDC 2343200'
loop_
_audit_author_name
_audit_author_address
'Dongzhou Zhang'
;Hawaii Institute of Geophysics and Planetology, University of Hawaii at Manoa
United States of America
;
_audit_update_record             
;
2024-03-25 deposited with the CCDC.	2025-01-02 downloaded from the CCDC.
;
_audit_creation_date             2023-06-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            'Furil, phase II'
_chemical_name_systematic        Di(furan-2-yl)ethanedione
_chemical_formula_moiety         'C10 H6 O4'
_chemical_formula_sum            'C10 H6 O4'
_chemical_formula_weight         190.15
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0022 0.0020 '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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.586(5)
_cell_length_b                   7.0535(14)
_cell_length_c                   3.4512(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.132(15)
_cell_angle_gamma                90
_cell_volume                     354.55(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    106
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      15.235
_cell_measurement_theta_min      3.631
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1403 before and 0.0892 after correction.
 
For component 2:
 wR2(int) was 0.1409 before and 0.0766 after correction.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             196
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.2943
_diffrn_reflns_Laue_measured_fraction_full 0.307
_diffrn_reflns_Laue_measured_fraction_max 0.159
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       1
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            554
_diffrn_reflns_point_group_measured_fraction_full 0.307
_diffrn_reflns_point_group_measured_fraction_max 0.159
_diffrn_reflns_theta_full        15.094
_diffrn_reflns_theta_max         23.366
_diffrn_reflns_theta_min         1.959
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.307
_diffrn_measured_fraction_theta_max 0.159
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       ?
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.434
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                228
_reflns_number_total             554
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2663
_refine_ls_R_factor_gt           0.1550
_refine_ls_restrained_S_all      1.130
_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)+(0.1856P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3424
_refine_ls_wR_factor_ref         0.3880
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.609(13)
 0.391(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C004(H004), C006(H006), C007(H007)
;
_atom_sites_solution_hydrogens   geom
_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
O001 O 0.6838(16) 0.2909(9) 0.454(3) 0.028(3) Uiso 1 1 d . . . . .
O002 O 0.5869(13) 0.6065(8) 0.252(3) 0.035(3) Uiso 1 1 d . . . . .
C003 C 0.546(2) 0.4839(16) 0.434(5) 0.033(4) Uiso 1 1 d . . . . .
C004 C 0.568(2) 0.1473(11) 0.723(4) 0.022(3) Uiso 1 1 d . . . . .
H004 H 0.510067 0.128847 0.811655 0.026 Uiso 1 1 calc R U . . .
C005 C 0.599(3) 0.3075(14) 0.562(5) 0.037(5) Uiso 1 1 d . . . . .
C006 C 0.714(2) 0.1113(13) 0.557(4) 0.029(3) Uiso 1 1 d . . . . .
H006 H 0.770976 0.058600 0.522341 0.035 Uiso 1 1 calc R U . . .
C007 C 0.635(2) 0.0212(13) 0.731(4) 0.024(3) Uiso 1 1 d . . . . .
H007 H 0.633094 -0.101491 0.829055 0.028 Uiso 1 1 calc R U . . .

_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
O001 C005 1.31(4) . ?
O001 C006 1.379(18) . ?
O002 C003 1.24(2) . ?
C003 C003 1.46(6) 3_666 ?
C003 C005 1.52(3) . ?
C004 H004 0.9300 . ?
C004 C005 1.35(2) . ?
C004 C007 1.32(4) . ?
C006 H006 0.9300 . ?
C006 C007 1.46(3) . ?
C007 H007 0.9300 . ?

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
C005 O001 C006 107.2(15) . . ?
O002 C003 C003 121.7(17) . 3_666 ?
O002 C003 C005 118(3) . . ?
C003 C003 C005 120(2) 3_666 . ?
C005 C004 H004 126.0 . . ?
C007 C004 H004 126.0 . . ?
C007 C004 C005 108(3) . . ?
O001 C005 C003 117.6(18) . . ?
O001 C005 C004 113(2) . . ?
C004 C005 C003 129(4) . . ?
O001 C006 H006 127.4 . . ?
O001 C006 C007 105(2) . . ?
C007 C006 H006 127.4 . . ?
C004 C007 C006 106.9(12) . . ?
C004 C007 H007 126.6 . . ?
C006 C007 H007 126.6 . . ?

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
O001 C006 C007 C004 -0.4(14) . . . . ?
O002 C003 C005 O001 -4(3) . . . . ?
O002 C003 C005 C004 -171.9(17) . . . . ?
C003 C003 C005 O001 -176(2) 3_666 . . . ?
C003 C003 C005 C004 16(4) 3_666 . . . ?
C005 O001 C006 C007 1.4(18) . . . . ?
C005 C004 C007 C006 -0.7(16) . . . . ?
C006 O001 C005 C003 -172.0(13) . . . . ?
C006 O001 C005 C004 -2(2) . . . . ?
C007 C004 C005 O001 2(2) . . . . ?
C007 C004 C005 C003 170.4(16) . . . . ?

_shelx_res_file                  
;
TITL P2_0m_5 in P2(1)/n
    p2_0m_5.res
    created by SHELXL-2019/1 at 13:33:25 on 29-Jun-2023
CELL 0.434 14.5864 7.0535 3.4512 90 93.1315 90
ZERR 2 0.0053 0.0014 0.0006 0 0.0152 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C O H
DISP C 0.0001 0.0005 5.3074
DISP H 0 0 0.6003
DISP O 0.0022 0.002 10.704
UNIT 20 8 12

L.S. 10
PLAN  5
TEMP 0
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT -6 7 2
OMIT 5 6 2
OMIT 0 9 2
OMIT -5 5 1
REM <olex2.extras>
REM <HklSrc "%.\\P2_0m_5.hkl">
REM </olex2.extras>

WGHT    0.185600
BASF   0.39102
FVAR       0.12599
O001  2    0.683801    0.290935    0.453951    11.00000    0.02800
O002  2    0.586909    0.606463    0.251917    11.00000    0.03497
C003  1    0.546172    0.483913    0.433861    11.00000    0.03333
C004  1    0.568433    0.147252    0.722522    11.00000    0.02190
AFIX  43
H004  3    0.510067    0.128847    0.811655    11.00000   -1.20000
AFIX   0
C005  1    0.599496    0.307461    0.562078    11.00000    0.03703
C006  1    0.713528    0.111253    0.556592    11.00000    0.02939
AFIX  43
H006  3    0.770976    0.058600    0.522341    11.00000   -1.20000
AFIX   0
C007  1    0.635256    0.021151    0.731047    11.00000    0.02357
AFIX  43
H007  3    0.633094   -0.101491    0.829055    11.00000   -1.20000
AFIX   0
HKLF 5




REM  P2_0m_5 in P2(1)/n
REM wR2 = 0.3880, GooF = S = 1.130, Restrained GooF = 1.130 for all data
REM R1 = 0.1550 for 228 Fo > 4sig(Fo) and 0.2663 for all 554 data
REM 30 parameters refined using 0 restraints

END

WGHT      0.1864      0.0000

REM Highest difference peak  0.293,  deepest hole -0.271,  1-sigma level  0.086
Q1    1   0.7511  0.2355  0.1801  11.00000  0.05    0.29
Q2    1   0.4662  0.2205  0.4160  11.00000  0.05    0.28
Q3    1   0.7404 -0.1761  0.4507  11.00000  0.05    0.28
Q4    1   0.5374  0.3211  0.8787  11.00000  0.05    0.28
Q5    1   0.6327  0.6106  0.3993  11.00000  0.05    0.27
;
_shelx_res_checksum              20333
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.609(13)
2 0.391(13)

# start Validation Reply Form
_vrf_ATOM007_p2_0m_5             
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Anisotropic ADP refinement leads to unphysical thermal ellipsoid 
parameters because of the low peak/parameter ratio limited by the DAC opening 
angle.
;
_vrf_PLAT029_p2_0m_5             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.310 Why?  
RESPONSE: Collection ability is imited by the opening of the diamond 
anvil cell.
;
####################################################################### 
# 
# 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_samp3_0m_4
_database_code_depnum_ccdc_archive 'CCDC 2343199'
loop_
_audit_author_name
_audit_author_address
'Dongzhou Zhang'
;Hawaii Institute of Geophysics and Planetology, University of Hawaii at Manoa
United States of America
;
_audit_update_record             
;
2024-03-25 deposited with the CCDC.	2025-01-02 downloaded from the CCDC.
;
_audit_creation_date             2023-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            'Furil, phase II'
_chemical_name_systematic        Di(furan-2-yl)ethanedione
_chemical_formula_moiety         '2(C10 H6 O4)'
_chemical_formula_sum            'C20 H12 O8'
_chemical_formula_weight         380.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0009 0.0005 '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 -0.0008 0.0020 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   3.313(3)
_cell_length_b                   6.957(7)
_cell_length_c                   14.228(16)
_cell_angle_alpha                90
_cell_angle_beta                 94.48(3)
_cell_angle_gamma                90
_cell_volume                     326.9(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    76
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      11.861
_cell_measurement_theta_min      3.579
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 2560 reflections, Rint = 0.9728
 (570 with I > 3sig(I), Rint = 0.9750)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             196
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.6302
_diffrn_reflns_Laue_measured_fraction_full 0.459
_diffrn_reflns_Laue_measured_fraction_max 0.285
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            571
_diffrn_reflns_point_group_measured_fraction_full 0.459
_diffrn_reflns_point_group_measured_fraction_max 0.285
_diffrn_reflns_theta_full        15.094
_diffrn_reflns_theta_max         23.095
_diffrn_reflns_theta_min         3.577
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.459
_diffrn_measured_fraction_theta_max 0.285
_diffrn_measurement_device_type  'APS 13-BM-C'
_diffrn_measurement_method       ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.434
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                227
_reflns_number_total             571
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.5162
_refine_ls_R_factor_gt           0.4104
_refine_ls_restrained_S_all      2.297
_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          0.6897
_refine_ls_wR_factor_ref         0.7248
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C003(H003), C004(H004), C007(H007)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
O001 O 0.540(3) 0.2825(13) 0.3137(13) 0.023(4) Uiso 1 1 d . . . . .
O002 O 0.755(3) 0.6123(12) 0.4142(14) 0.027(4) Uiso 1 1 d . . . . .
C003 C 0.266(5) 0.138(2) 0.432(2) 0.028(5) Uiso 1 1 d . . . . .
H003 H 0.161052 0.121922 0.490098 0.034 Uiso 1 1 calc R . . . .
C004 C 0.430(6) 0.106(2) 0.293(3) 0.040(6) Uiso 1 1 d . . . . .
H004 H 0.457379 0.052130 0.234061 0.048 Uiso 1 1 calc R . . . .
C005 C 0.437(5) 0.3031(19) 0.402(2) 0.027(5) Uiso 1 1 d . . . . .
C006 C 0.558(5) 0.4871(18) 0.449(2) 0.025(5) Uiso 1 1 d . . . . .
C007 C 0.271(5) 0.0036(17) 0.365(2) 0.021(5) Uiso 1 1 d . . . . .
H007 H 0.189720 -0.124285 0.366182 0.025 Uiso 1 1 calc R . . . .

_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
O001 C004 1.31(2) . ?
O001 C005 1.33(3) . ?
O002 C006 1.21(2) . ?
C003 H003 0.9300 . ?
C003 C005 1.36(3) . ?
C003 C007 1.34(4) . ?
C004 H004 0.9300 . ?
C004 C007 1.38(4) . ?
C005 C006 1.48(3) . ?
C006 C006 1.55(6) 3_666 ?
C007 H007 0.9300 . ?

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
C004 O001 C005 103(2) . . ?
C005 C003 H003 125.2 . . ?
C007 C003 H003 125.2 . . ?
C007 C003 C005 110(3) . . ?
O001 C004 H004 122.2 . . ?
O001 C004 C007 116(3) . . ?
C007 C004 H004 122.2 . . ?
O001 C005 C003 110.4(19) . . ?
O001 C005 C006 115.8(18) . . ?
C003 C005 C006 133(3) . . ?
O002 C006 C005 125(2) . . ?
O002 C006 C006 118.5(18) . 3_666 ?
C005 C006 C006 116.4(19) . 3_666 ?
C003 C007 C004 101.2(15) . . ?
C003 C007 H007 129.4 . . ?
C004 C007 H007 129.4 . . ?

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
O001 C004 C007 C003 4(2) . . . . ?
O001 C005 C006 O002 -3(3) . . . . ?
O001 C005 C006 C006 -179.6(19) . . . 3_666 ?
C003 C005 C006 O002 170(2) . . . . ?
C003 C005 C006 C006 -6(3) . . . 3_666 ?
C004 O001 C005 C003 -0.2(18) . . . . ?
C004 O001 C005 C006 174.8(15) . . . . ?
C005 O001 C004 C007 -2.4(19) . . . . ?
C005 C003 C007 C004 -4(2) . . . . ?
C007 C003 C005 O001 3(2) . . . . ?
C007 C003 C005 C006 -171.0(17) . . . . ?

_shelx_res_file                  
;
TITL furil_p3_4p4gpa_crystal2_8s_0m_a.res in P2(1)/n
    samp3_0m_4.res
    created by SHELXL-2019/1 at 11:05:48 on 05-Dec-2023
CELL 0.434 3.3129 6.9569 14.2278 90 94.483 90
ZERR 1 0.003 0.0066 0.0159 0 0.033 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H O
DISP C -0.0009 0.0005 5.3074
DISP H 0 0 0.6003
DISP O -0.0008 0.002 10.704
UNIT 20 12 8

L.S. 20
PLAN  3
TEMP 0
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT -2 11 4
OMIT 2 11 2
OMIT 2 10 3
OMIT -2 11 5
OMIT 0 5 5
OMIT 1 7 2
OMIT -3 3 5
OMIT 0 7 4
OMIT 2 11 4
OMIT 3 2 3
OMIT 2 4 8
OMIT -2 11 -1
OMIT -2 8 7
OMIT 2 11 5
OMIT 2 11 5
OMIT 2 11 3
OMIT -2 11 6
OMIT -2 7 12
OMIT -2 11 2
OMIT 0 8 0
OMIT -3 4 6
OMIT 1 9 2
OMIT -2 2 0
OMIT -2 2 0
REM <olex2.extras>
REM <HklSrc "%.\\SamP3_0m_4.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       1.41172
O001  3    0.540045    0.282498    0.313711    11.00000    0.02334
O002  3    0.754554    0.612301    0.414232    11.00000    0.02681
C003  1    0.265557    0.138264    0.431832    11.00000    0.02809
AFIX  43
H003  2    0.161052    0.121922    0.490098    11.00000   -1.20000
AFIX   0
C004  1    0.430062    0.105549    0.293147    11.00000    0.04016
AFIX  43
H004  2    0.457379    0.052130    0.234061    11.00000   -1.20000
AFIX   0
C005  1    0.436512    0.303125    0.401659    11.00000    0.02707
C006  1    0.557978    0.487123    0.448601    11.00000    0.02483
C007  1    0.271069    0.003563    0.364825    11.00000    0.02082
AFIX  43
H007  2    0.189720   -0.124285    0.366182    11.00000   -1.20000
AFIX   0
HKLF 4




REM  furil_p3_4p4gpa_crystal2_8s_0m_a.res in P2(1)/n
REM wR2 = 0.7248, GooF = S = 2.297, Restrained GooF = 2.297 for all data
REM R1 = 0.4104 for 227 Fo > 4sig(Fo) and 0.5162 for all 571 data
REM 29 parameters refined using 0 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.695,  deepest hole -0.715,  1-sigma level  0.208
Q1    1   0.0823 -0.0519  0.3175  11.00000  0.05    0.69
Q2    1  -0.2138 -0.1328  0.3432  11.00000  0.05    0.68
Q3    1   0.2586  0.1170  0.4044  11.00000  0.05    0.68
;
_shelx_res_checksum              15585
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_ATOM007_samp3_0m_4          
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Anisotropic ADP refinement leads to unphysical thermal ellipsoid 
parameters because of the low peak/parameter ratio limited by the DAC opening 
angle.
;
_vrf_PLAT029_samp3_0m_4          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.459 Why?  
RESPONSE: Collection ability is imited by the opening of the diamond
anvil cell.
;
_vrf_PLAT082_samp3_0m_4          
;
PROBLEM: High R1 Value ..................................       0.41 Report
RESPONSE: Collection ability is limited by DAC opening angle, and crystal 
quality was low at high pressures.
;
_vrf_PLAT084_samp3_0m_4          
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.72 Report
RESPONSE: Collection ability is limited by DAC opening angle, and crystal 
quality was low at high pressures.
;
_vrf_PLAT881_samp3_0m_4          
;
PROBLEM: No Datum for _diffrn_reflns_av_R_equivalents ...     Please Do !  
RESPONSE: For merged dataset, Req is unavailable.
;
