# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_204_11_pl
_database_code_depnum_ccdc_archive 'CCDC 2300602'
loop_
_audit_author_name
_audit_author_address
'Yi Zhou'
;ShanghaiTech University
China
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_audit_creation_date             2023-10-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 Ga O5'
_chemical_formula_sum            'C34 O10 Ga2'
_chemical_formula_weight         353.90
_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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 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           10
_space_group_name_H-M_alt        P2/m
_space_group_name_Hall           '-P 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, z'

_cell_length_a                   6.504
_cell_length_b                   15.971
_cell_length_c                   10.970
_cell_angle_alpha                90
_cell_angle_beta                 103.40
_cell_angle_gamma                90
_cell_volume                     1108.5
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4307
_cell_measurement_temperature    298
_cell_measurement_theta_max      0.898
_cell_measurement_theta_min      0.304
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       nanocrystal
_exptl_crystal_F_000             119
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.1406
_diffrn_reflns_Laue_measured_fraction_full 0.706
_diffrn_reflns_Laue_measured_fraction_max 0.674
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4294
_diffrn_reflns_point_group_measured_fraction_full 0.706
_diffrn_reflns_point_group_measured_fraction_max 0.674
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.960
_diffrn_reflns_theta_min         0.045
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.706
_diffrn_measured_fraction_theta_max 0.674
_diffrn_measurement_device_type  'JEM-F200 with Cheetah 1800 camera'
_diffrn_measurement_method       ?
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                713
_reflns_number_total             1940
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         0.154
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.373
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1940
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.2898
_refine_ls_R_factor_gt           0.1798
_refine_ls_restrained_S_all      1.375
_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          0.4635
_refine_ls_wR_factor_ref         0.5143
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C4-C2 = C3-C2 = C6-C3 = C7-C6 = C7-C5 = C5-C4
 1.39 with sigma of 0.02
2. Restrained planarity
 C3, C2, C4, C5, C7, C6
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C5 \\sim C6 \\sim C2 \\sim C7: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
;
_atom_sites_solution_hydrogens   .
_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
Ga2 Ga 1.000000 0.000000 0.500000 0.091(4) Uani 1 4 d S T P . .
Ga1 Ga 0.500000 0.000000 0.500000 0.086(4) Uani 1 4 d S T P . .
O3 O 0.537(3) 0.0924(6) 0.3847(10) 0.127(7) Uani 1 1 d . . . . .
O1 O 0.774(4) 0.000000 0.5809(10) 0.100(8) Uani 1 2 d S T P . .
O2 O 0.880(3) 0.0924(5) 0.3873(9) 0.122(7) Uani 1 1 d . . . . .
C4 C 0.827(3) 0.2440(6) 0.2539(10) 0.138(7) Uani 1 1 d D U . . .
C3 C 0.464(3) 0.2245(7) 0.2312(12) 0.158(8) Uani 1 1 d D U . . .
C5 C 0.787(3) 0.3163(7) 0.1868(14) 0.149(8) Uani 1 1 d D U . . .
C9 C 0.590(4) 0.500000 0.1191(11) 0.118(10) Uani 1 2 d S T P . .
C6 C 0.419(3) 0.2945(7) 0.1529(13) 0.154(7) Uani 1 1 d D U . . .
C8 C 0.548(2) 0.4224(4) 0.0613(7) 0.097(6) Uani 1 1 d . . . . .
C1 C 0.699(3) 0.1203(5) 0.3538(9) 0.075(5) Uani 1 1 d . . . . .
C2 C 0.661(2) 0.1971(4) 0.2791(8) 0.088(5) Uani 1 1 d D U . . .
C7 C 0.583(2) 0.3427(4) 0.1308(8) 0.099(6) Uani 1 1 d D U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga2 0.191(13) 0.0176(19) 0.059(3) 0.000 0.016(5) 0.000
Ga1 0.183(13) 0.018(2) 0.052(3) 0.000 0.019(5) 0.000
O3 0.19(2) 0.073(6) 0.110(7) 0.056(5) 0.013(10) 0.001(8)
O1 0.20(3) 0.036(5) 0.063(7) 0.000 0.039(11) 0.000
O2 0.25(2) 0.035(4) 0.088(6) 0.037(4) 0.048(9) 0.033(7)
C4 0.201(19) 0.071(7) 0.138(9) 0.080(7) 0.029(11) 0.009(9)
C3 0.21(2) 0.086(8) 0.167(12) 0.091(8) 0.032(13) 0.031(10)
C5 0.20(2) 0.072(7) 0.163(11) 0.065(8) 0.022(13) 0.007(9)
C9 0.27(3) 0.018(5) 0.050(7) 0.000 0.005(10) 0.000
C6 0.23(2) 0.070(7) 0.158(11) 0.073(7) 0.044(12) 0.001(9)
C8 0.219(19) 0.014(3) 0.045(4) -0.001(3) 0.002(6) -0.004(5)
C1 0.134(16) 0.022(4) 0.075(6) 0.016(4) 0.041(9) -0.007(6)
C2 0.161(16) 0.026(4) 0.071(6) 0.015(4) 0.017(7) 0.017(6)
C7 0.212(18) 0.020(3) 0.064(6) 0.009(3) 0.029(8) -0.005(6)

_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
Ga2 O1 1.885(19) 3_756 ?
Ga2 O1 1.885(19) . ?
Ga2 O2 1.968(10) 4 ?
Ga2 O2 1.968(10) 2_756 ?
Ga2 O2 1.968(10) 3_756 ?
Ga2 O2 1.968(10) . ?
Ga1 O3 1.994(9) 3_656 ?
Ga1 O3 1.994(10) . ?
Ga1 O3 1.994(9) 2_656 ?
Ga1 O3 1.994(9) 4 ?
Ga1 O1 1.80(2) . ?
Ga1 O1 1.80(2) 3_656 ?
O3 C1 1.26(2) . ?
O2 C1 1.23(2) . ?
C4 C5 1.361(12) . ?
C4 C2 1.392(15) . ?
C3 C6 1.398(12) . ?
C3 C2 1.344(15) . ?
C5 C7 1.393(15) . ?
C9 C8 1.390(8) . ?
C9 C8 1.390(8) 4_565 ?
C6 C7 1.386(16) . ?
C8 C8 1.345(16) 2_655 ?
C8 C7 1.474(10) . ?
C1 C2 1.465(12) . ?

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
O1 Ga2 O1 180.0 3_756 . ?
O1 Ga2 O2 86.8(6) . 3_756 ?
O1 Ga2 O2 93.2(6) 3_756 2_756 ?
O1 Ga2 O2 86.8(6) . 2_756 ?
O1 Ga2 O2 93.2(6) . 4 ?
O1 Ga2 O2 86.8(6) 3_756 . ?
O1 Ga2 O2 93.2(6) 3_756 3_756 ?
O1 Ga2 O2 86.8(6) 3_756 4 ?
O1 Ga2 O2 93.2(6) . . ?
O2 Ga2 O2 180.0 3_756 . ?
O2 Ga2 O2 97.2(7) 2_756 3_756 ?
O2 Ga2 O2 180.0(3) 4 2_756 ?
O2 Ga2 O2 82.8(7) 4 3_756 ?
O2 Ga2 O2 82.8(7) 2_756 . ?
O2 Ga2 O2 97.2(7) 4 . ?
O3 Ga1 O3 95.4(8) . 4 ?
O3 Ga1 O3 180.0(7) . 3_656 ?
O3 Ga1 O3 84.6(8) . 2_656 ?
O3 Ga1 O3 95.4(8) 2_656 3_656 ?
O3 Ga1 O3 84.6(8) 4 3_656 ?
O3 Ga1 O3 180.0(5) 4 2_656 ?
O1 Ga1 O3 93.5(6) . 4 ?
O1 Ga1 O3 93.5(6) . . ?
O1 Ga1 O3 86.5(6) 3_656 . ?
O1 Ga1 O3 93.5(6) 3_656 3_656 ?
O1 Ga1 O3 86.5(6) . 3_656 ?
O1 Ga1 O3 86.5(6) 3_656 4 ?
O1 Ga1 O3 86.5(6) . 2_656 ?
O1 Ga1 O3 93.5(6) 3_656 2_656 ?
O1 Ga1 O1 180.0 . 3_656 ?
C1 O3 Ga1 131.6(13) . . ?
Ga1 O1 Ga2 124.0(6) . . ?
C1 O2 Ga2 132.3(12) . . ?
C5 C4 C2 120.4(13) . . ?
C2 C3 C6 123.0(14) . . ?
C4 C5 C7 122.4(13) . . ?
C8 C9 C8 126.1(10) . 4_565 ?
C7 C6 C3 119.4(15) . . ?
C9 C8 C7 122.9(7) . . ?
C8 C8 C9 116.9(5) 2_655 . ?
C8 C8 C7 119.9(5) 2_655 . ?
O3 C1 C2 113.7(14) . . ?
O2 C1 O3 126.3(11) . . ?
O2 C1 C2 119.8(13) . . ?
C4 C2 C1 121.5(12) . . ?
C3 C2 C4 117.5(10) . . ?
C3 C2 C1 120.9(11) . . ?
C5 C7 C8 120.6(11) . . ?
C6 C7 C5 116.8(10) . . ?
C6 C7 C8 122.4(12) . . ?

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
Ga2 O2 C1 O3 -2(2) . . . . ?
Ga2 O2 C1 C2 172.8(6) . . . . ?
Ga1 O3 C1 O2 3(2) . . . . ?
Ga1 O3 C1 C2 -171.9(8) . . . . ?
O3 Ga1 O1 Ga2 -47.8(4) . . . . ?
O3 Ga1 O1 Ga2 47.8(4) 4 . . . ?
O3 Ga1 O1 Ga2 -132.2(4) 2_656 . . . ?
O3 Ga1 O1 Ga2 132.2(4) 3_656 . . . ?
O3 C1 C2 C4 169.5(10) . . . . ?
O3 C1 C2 C3 -11.2(13) . . . . ?
O2 Ga2 O1 Ga1 48.7(4) . . . . ?
O2 Ga2 O1 Ga1 -48.7(4) 4 . . . ?
O2 Ga2 O1 Ga1 -131.3(4) 3_756 . . . ?
O2 Ga2 O1 Ga1 131.3(4) 2_756 . . . ?
O2 C1 C2 C4 -5.8(14) . . . . ?
O2 C1 C2 C3 173.6(11) . . . . ?
C4 C5 C7 C6 4(2) . . . . ?
C4 C5 C7 C8 178.6(10) . . . . ?
C3 C6 C7 C5 1.7(19) . . . . ?
C3 C6 C7 C8 -172.9(9) . . . . ?
C5 C4 C2 C3 2.2(14) . . . . ?
C5 C4 C2 C1 -178.4(10) . . . . ?
C9 C8 C7 C5 -67.5(19) . . . . ?
C9 C8 C7 C6 106.9(18) . . . . ?
C6 C3 C2 C4 3.5(14) . . . . ?
C6 C3 C2 C1 -175.9(11) . . . . ?
C8 C9 C8 C8 -1(3) 4_565 . . 2_655 ?
C8 C9 C8 C7 -175.4(14) 4_565 . . . ?
C8 C8 C7 C5 119(2) 2_655 . . . ?
C8 C8 C7 C6 -67(2) 2_655 . . . ?
C2 C4 C5 C7 -6.0(19) . . . . ?
C2 C3 C6 C7 -5.5(19) . . . . ?

_shelx_res_file                  
;
TITL 204_11 P 2/m R = 0.40 New:P2/m
    204_11_pl.res
    created by SHELXL-2018/3 at 10:50:25 on 09-Oct-2023
CELL 0.02508 6.504 15.971 10.97 90 103.4 90
ZERR 2 0 0 0 0 0 0
LATT 1
SYMM -X,+Y,-Z
SFAC  C 0.731 36.995 1.195 11.297 0.456 2.814 0.125 0.346 0 0 0 0 0.77 12.011
SFAC  GA 2.321 65.602 2.486 15.458 1.688 2.581 0.599 0.351 0 0 0 0 1.26 69.72
SFAC  O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999
UNIT 34 2 10

DFIX 1.39 C4 C2 C3 C2 C6 C3 C7 C6 C7 C5 C5 C4
FLAT C3 C2 C4 C5 C7 C6
SIMU C4 C3 C5 C6 C2 C7

L.S. 20
PLAN  5
TEMP 24.85
CONF
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\204_11_sx.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       4.02688
GA2   2    1.000000    0.000000    0.500000    10.25000    0.19091    0.01762 =
         0.05888    0.00000    0.01601    0.00000
GA1   2    0.500000    0.000000    0.500000    10.25000    0.18290    0.01827 =
         0.05235    0.00000    0.01888    0.00000
O3    3    0.537112    0.092355    0.384692    11.00000    0.18624    0.07325 =
         0.10973    0.05601    0.01314    0.00052
O1    3    0.774027    0.000000    0.580886    10.50000    0.20440    0.03642 =
         0.06298    0.00000    0.03867    0.00000
O2    3    0.879644    0.092428    0.387312    11.00000    0.24668    0.03489 =
         0.08818    0.03715    0.04773    0.03273
C4    1    0.826995    0.244042    0.253943    11.00000    0.20107    0.07121 =
         0.13785    0.07977    0.02938    0.00905
C3    1    0.463636    0.224502    0.231169    11.00000    0.21436    0.08631 =
         0.16746    0.09058    0.03182    0.03125
C5    1    0.787478    0.316305    0.186785    11.00000    0.20291    0.07192 =
         0.16322    0.06500    0.02170    0.00700
C9    1    0.590293    0.500000    0.119065    10.50000    0.27133    0.01758 =
         0.04958    0.00000    0.00517    0.00000
C6    1    0.418614    0.294473    0.152947    11.00000    0.23399    0.07000 =
         0.15849    0.07319    0.04409    0.00150
C8    1    0.547643    0.422417    0.061343    11.00000    0.21897    0.01396 =
         0.04491   -0.00088    0.00174   -0.00418
C1    1    0.699342    0.120271    0.353794    11.00000    0.13445    0.02243 =
         0.07505    0.01614    0.04099   -0.00684
C2    1    0.661197    0.197147    0.279089    11.00000    0.16126    0.02570 =
         0.07147    0.01468    0.01748    0.01724
C7    1    0.583256    0.342726    0.130843    11.00000    0.21172    0.02022 =
         0.06352    0.00919    0.02853   -0.00470
HKLF 4




REM  204_11 P 2/m R = 0.40 New:P2/m
REM wR2 = 0.5143, GooF = S = 1.373, Restrained GooF = 1.375 for all data
REM R1 = 0.1798 for 713 Fo > 4sig(Fo) and 0.2898 for all 1940 data
REM 111 parameters refined using 45 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.154,  deepest hole -0.143,  1-sigma level  0.035
Q1    1   0.6520  0.5000  0.2270  10.50000  0.05    0.15
Q2    1   0.5000  0.3661  0.5000  10.50000  0.05    0.15
Q3    1   1.0659  0.0000  0.5116  10.50000  0.05    0.12
Q4    1   0.4418  0.0317  0.0164  11.00000  0.05    0.12
Q5    1   1.0000  0.3573  0.5000  10.50000  0.05    0.09
;
_shelx_res_checksum              13411
_olex2_submission_special_instructions 'No special instructions were received'


# start Validation Reply Form
_vrf_PLAT084_204_11_pl           
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.51 Report
RESPONSE: Electron diffraction data normally has high R1 values.
;
_vrf_PLAT602_204_11_pl           
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check 
RESPONSE: This is a porous MOF crystal.
;
_vrf_PLAT082_204_11_pl           
;
PROBLEM: High R1 Value ..................................       0.18 Report
RESPONSE: Electron diffraction data normally has high R1 values.
;
_vrf_PLAT213_204_11_pl           
;
PROBLEM: Atom C8              has ADP max/min Ratio .....        4.1 prolat
RESPONSE: The atoms suffered from electron beam damage.
;
_vrf_PLAT250_204_11_pl           
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        7.9 Note  
RESPONSE: The atoms suffered from electron beam damage.
;
_vrf_PLAT341_204_11_pl           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0154 Ang.  
RESPONSE: The atoms suffered from electron beam damage.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_203highsymmetry_24
_database_code_depnum_ccdc_archive 'CCDC 2300604'
loop_
_audit_author_name
_audit_author_address
'Yi Zhou'
;ShanghaiTech University
China
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_audit_creation_date             2023-10-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H18 O10 V2'
_chemical_formula_sum            'C34 H18 O10 V2'
_chemical_formula_weight         172.10
_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 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 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           55
_space_group_name_H-M_alt        Pcma
_space_group_name_Hall           '-P 2ac 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, -z+1/2'
'-x, y, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y, z-1/2'
'x, -y, z'

_cell_length_a                   6.496
_cell_length_b                   15.835
_cell_length_c                   21.590
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2220.7
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    298
_cell_measurement_theta_max      0.898
_cell_measurement_theta_min      0.304
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       nanocrystals
_exptl_crystal_F_000             262
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_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  0.1464
_diffrn_reflns_av_unetI/netI     0.1520
_diffrn_reflns_Laue_measured_fraction_full 0.865
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8802
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.969
_diffrn_reflns_theta_min         0.045
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_device_type  'JEM-F200 with Cheetah 1800 camera'
_diffrn_measurement_method       ?
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1578
_reflns_number_total             2411
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    ?
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2411
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.2940
_refine_ls_R_factor_gt           0.2649
_refine_ls_restrained_S_all      1.966
_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          0.5686
_refine_ls_wR_factor_ref         0.5788
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C3 \\sim C4-C5 \\sim C6-C7
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C8, C6, C7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C2 \\sim C7 \\sim C6 \\sim C5: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
Uanis(V1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C4(H4), C6(H6), C7(H7)
;
_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
V1 V 0.4263(5) 0.000000 0.7583(3) 0.0247(15) Uani 1 2 d S TU P . .
O2 O 0.1584(13) 0.000000 0.7102(7) 0.028(3) Uani 1 2 d S TU P . .
C8 C 0.5455(14) 0.4225(4) 0.5300(7) 0.047(4) Uani 1 1 d . . . . .
C1 C 0.6477(12) 0.1190(5) 0.6754(6) 0.036(4) Uani 1 1 d . . . . .
C5 C 0.5786(14) 0.3428(5) 0.5641(7) 0.047(3) Uani 1 1 d D U . . .
O3 O 0.3103(11) 0.0912(5) 0.8131(6) 0.049(4) Uani 1 1 d . . . . .
C9 C 0.581(2) 0.500000 0.5585(10) 0.053(6) Uani 1 2 d S T P . .
H9 H 0.630897 0.500000 0.598902 0.064 Uiso 1 2 calc R U P . .
O1 O 0.4838(10) 0.0901(5) 0.6974(6) 0.043(3) Uani 1 1 d . . . . .
C3 C 0.7887(13) 0.2452(6) 0.6217(6) 0.053(4) Uani 1 1 d D U . . .
H3 H 0.920223 0.228933 0.633784 0.063 Uiso 1 1 calc R U . . .
C4 C 0.7637(14) 0.3197(6) 0.5876(7) 0.056(4) Uani 1 1 d D U . . .
H4 H 0.877175 0.354296 0.580830 0.067 Uiso 1 1 calc R U . . .
C6 C 0.4155(15) 0.2932(6) 0.5828(8) 0.061(4) Uani 1 1 d D U . . .
H6 H 0.283054 0.310318 0.572394 0.073 Uiso 1 1 calc R U . . .
C2 C 0.6255(10) 0.1963(4) 0.6375(4) 0.028(2) Uani 1 1 d D U . . .
C7 C 0.4381(14) 0.2202(6) 0.6160(7) 0.052(4) Uani 1 1 d D U . . .
H7 H 0.323714 0.186474 0.623804 0.063 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0040(13) 0.0105(14) 0.060(4) 0.000 0.0034(18) 0.000
O2 0.008(3) 0.027(4) 0.049(8) 0.000 0.003(4) 0.000
C8 0.041(5) 0.004(3) 0.097(14) 0.000(4) -0.027(6) 0.001(3)
C1 0.017(4) 0.015(3) 0.076(12) 0.009(5) -0.010(4) 0.008(3)
C5 0.031(5) 0.017(4) 0.092(10) 0.018(5) -0.012(6) 0.001(3)
O3 0.017(3) 0.031(4) 0.099(12) -0.025(5) 0.012(4) 0.005(2)
C9 0.075(11) 0.008(5) 0.078(18) 0.000 -0.047(11) 0.000
O1 0.013(3) 0.029(3) 0.086(10) 0.029(4) -0.008(4) -0.012(2)
C3 0.018(4) 0.037(5) 0.104(11) 0.041(6) -0.016(5) -0.009(3)
C4 0.030(5) 0.025(4) 0.111(11) 0.027(5) -0.011(6) -0.018(3)
C6 0.030(5) 0.036(5) 0.116(11) 0.030(6) -0.014(6) 0.015(4)
C2 0.008(3) 0.015(3) 0.061(7) 0.012(4) -0.010(3) -0.004(2)
C7 0.025(4) 0.031(4) 0.100(11) 0.031(5) -0.007(5) 0.003(3)

_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
V1 O2 1.654(10) 6_657 ?
V1 O2 2.027(12) . ?
V1 O3 2.014(9) . ?
V1 O3 2.014(9) 8 ?
V1 O1 1.975(9) . ?
V1 O1 1.975(9) 8 ?
C8 C8 1.42(3) 4_656 ?
C8 C5 1.478(12) . ?
C8 C9 1.393(13) . ?
C1 O3 1.170(10) 6_657 ?
C1 O1 1.253(11) . ?
C1 C2 1.480(11) . ?
C5 C4 1.355(11) . ?
C5 C6 1.380(14) . ?
C9 H9 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.400(13) . ?
C3 C2 1.356(10) . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.367(12) . ?
C2 C7 1.357(11) . ?
C7 H7 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
O2 V1 O2 173.5(4) 6_657 . ?
O2 V1 O3 95.7(5) 6_657 . ?
O2 V1 O3 95.7(5) 6_657 8 ?
O2 V1 O1 95.8(4) 6_657 . ?
O2 V1 O1 95.8(4) 6_657 8 ?
O3 V1 O2 88.8(4) . . ?
O3 V1 O2 88.8(4) 8 . ?
O3 V1 O3 91.7(6) . 8 ?
O1 V1 O2 79.7(4) . . ?
O1 V1 O2 79.7(4) 8 . ?
O1 V1 O3 168.5(4) . 8 ?
O1 V1 O3 86.8(5) . . ?
O1 V1 O3 86.8(5) 8 8 ?
O1 V1 O3 168.5(4) 8 . ?
O1 V1 O1 92.5(7) 8 . ?
V1 O2 V1 124.9(8) 6_557 . ?
C8 C8 C5 120.9(6) 4_656 . ?
C9 C8 C8 118.1(9) . 4_656 ?
C9 C8 C5 120.5(13) . . ?
O3 C1 O1 123.3(9) 6_657 . ?
O3 C1 C2 121.0(8) 6_657 . ?
O1 C1 C2 115.4(7) . . ?
C4 C5 C8 123.1(8) . . ?
C4 C5 C6 114.7(9) . . ?
C6 C5 C8 121.4(8) . . ?
C1 O3 V1 137.0(8) 6_557 . ?
C8 C9 C8 123.6(18) . 8_565 ?
C8 C9 H9 118.2 . . ?
C8 C9 H9 118.2 8_565 . ?
C1 O1 V1 132.6(6) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.5(8) . . ?
C5 C4 C3 121.8(8) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C5 C6 H6 118.2 . . ?
C7 C6 C5 123.5(9) . . ?
C7 C6 H6 118.2 . . ?
C3 C2 C1 122.4(7) . . ?
C3 C2 C7 117.1(8) . . ?
C7 C2 C1 120.5(7) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 C6 120.7(9) . . ?
C2 C7 H7 119.7 . . ?

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
C8 C8 C5 C4 126.6(16) 4_656 . . . ?
C8 C8 C5 C6 -64(2) 4_656 . . . ?
C8 C8 C9 C8 -5(3) 4_656 . . 8_565 ?
C8 C5 C4 C3 177.6(13) . . . . ?
C8 C5 C6 C7 -178.2(14) . . . . ?
C1 C2 C7 C6 177.5(12) . . . . ?
C5 C8 C9 C8 -177.5(11) . . . 8_565 ?
C5 C6 C7 C2 6(2) . . . . ?
O3 C1 O1 V1 4(2) 6_657 . . . ?
O3 C1 C2 C3 -9.6(13) 6_657 . . . ?
O3 C1 C2 C7 169.1(13) 6_657 . . . ?
C9 C8 C5 C4 -61(2) . . . . ?
C9 C8 C5 C6 108.5(16) . . . . ?
O1 C1 C2 C3 165.5(12) . . . . ?
O1 C1 C2 C7 -15.8(12) . . . . ?
C3 C2 C7 C6 -3.7(19) . . . . ?
C4 C5 C6 C7 -8(2) . . . . ?
C4 C3 C2 C1 -177.7(11) . . . . ?
C4 C3 C2 C7 3.5(17) . . . . ?
C6 C5 C4 C3 8(2) . . . . ?
C2 C1 O1 V1 -171.0(8) . . . . ?
C2 C3 C4 C5 -6(2) . . . . ?

_shelx_res_file                  
;
TITL 203highsymmetry
    203highsymmetry_24.res
    created by SHELXL-2018/3 at 09:48:26 on 09-Oct-2023
REM Shelx file produced by Sir2014 on Thu Nov 25 2021 at 17:43:40
REM Structure name: 203highsymmetry
REM ------ Electron scattering factors ------
REM SFAC Species a(1) b(1) a(2) b(2) a(3) b(3) =
REM a(4) b(4) c f' f'' mu cov_radius weight
CELL 0.02508 6.4956 15.835 21.59 90 90 90
ZERR 8 0 0 0 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,-Y,0.5-Z
SYMM -X,+Y,-Z
SFAC  C 0.731 36.995 1.195 11.297 0.456 2.814 0.125 0.346 0 0 0 0 0.77 12.011
SFAC  H 0.037 0.561 0.127 3.791 0.236 13.556 0.129 37.723 0 0 0 0 0.32 1.008
SFAC  O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999
SFAC  V 3.245 76.379 2.698 17.726 1.86 3.363 0.486 0.374 0 0 0 0 1.22 50.942
UNIT 68 36 20 4

SADI C2 C3 C4 C5 C6 C7
FLAT C1 C2 C3 C4 C5 C8 C6 C7
SIMU 0.02 0.04 2 C4 C3 C2 C7 C6 C5
ISOR 0.01 0.02 V1
ISOR 0.01 0.02 C2
ISOR 0.01 0.02 O2

L.S. 20
PLAN  7
CONF
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\xds.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR      23.13600
V1    4    0.426337    0.000000    0.758276    10.50000    0.00401    0.01052 =
         0.05972    0.00000    0.00336    0.00000
O2    3    0.158369    0.000000    0.710189    10.50000    0.00818    0.02741 =
         0.04859    0.00000    0.00290    0.00000
C8    1    0.545520    0.422505    0.529959    11.00000    0.04101    0.00364 =
         0.09742    0.00032   -0.02714    0.00107
C1    1    0.647745    0.119004    0.675437    11.00000    0.01671    0.01500 =
         0.07614    0.00918   -0.00954    0.00791
C5    1    0.578611    0.342769    0.564103    11.00000    0.03074    0.01673 =
         0.09243    0.01843   -0.01246    0.00144
O3    3    0.310310    0.091239    0.813111    11.00000    0.01712    0.03104 =
         0.09900   -0.02523    0.01238    0.00455
C9    1    0.580909    0.500000    0.558537    10.50000    0.07477    0.00780 =
         0.07777    0.00000   -0.04719    0.00000
AFIX  43
H9    2    0.630897    0.500000    0.598902    10.50000   -1.20000
AFIX   0
O1    3    0.483789    0.090080    0.697437    11.00000    0.01342    0.02950 =
         0.08617    0.02875   -0.00779   -0.01153
C3    1    0.788697    0.245240    0.621678    11.00000    0.01754    0.03691 =
         0.10379    0.04103   -0.01569   -0.00915
AFIX  43
H3    2    0.920223    0.228933    0.633784    11.00000   -1.20000
AFIX   0
C4    1    0.763654    0.319706    0.587567    11.00000    0.02991    0.02533 =
         0.11147    0.02654   -0.01100   -0.01811
AFIX  43
H4    2    0.877175    0.354296    0.580830    11.00000   -1.20000
AFIX   0
C6    1    0.415505    0.293165    0.582845    11.00000    0.02965    0.03631 =
         0.11603    0.02971   -0.01392    0.01508
AFIX  43
H6    2    0.283054    0.310318    0.572394    11.00000   -1.20000
AFIX   0
C2    1    0.625540    0.196321    0.637478    11.00000    0.00816    0.01471 =
         0.06148    0.01203   -0.00973   -0.00356
C7    1    0.438059    0.220158    0.615952    11.00000    0.02544    0.03105 =
         0.10006    0.03102   -0.00667    0.00252
AFIX  43
H7    2    0.323714    0.186474    0.623804    11.00000   -1.20000
AFIX   0
HKLF 4




REM  203highsymmetry
REM wR2 = 0.5788, GooF = S = 1.963, Restrained GooF = 1.966 for all data
REM R1 = 0.2649 for 1578 Fo > 4sig(Fo) and 0.2940 for all 2411 data
REM 109 parameters refined using 62 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.336,  deepest hole -0.391,  1-sigma level  0.074
Q1    1   0.4243  0.0000  0.8231  10.50000  0.05    0.34
Q2    1   0.4332  0.0000  0.6911  10.50000  0.05    0.33
Q3    1   0.6290  0.1239  0.7507  11.00000  0.05    0.31
Q4    1   0.3872  0.5000  0.5172  10.50000  0.05    0.28
Q5    1   1.1179  0.2567  0.6187  11.00000  0.05    0.23
Q6    1   0.9147  0.5000  0.5184  10.50000  0.05    0.22
Q7    1   1.0868  0.3944  0.5721  11.00000  0.05    0.22
;
_shelx_res_checksum              45773
_olex2_submission_special_instructions 'No special instructions were received'


# start Validation Reply Form
_vrf_RINTA01_203highsymmetry_24  
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Electron diffraction data normally has high Rint values.
;
_vrf_PLAT082_203highsymmetry_24  
;
PROBLEM: High R1 Value ..................................       0.26 Report
RESPONSE: Electron diffraction data normally has high R1 values.
;
_vrf_PLAT084_203highsymmetry_24  
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.58 Report
RESPONSE: Electron diffraction data normally has high wR2 values.
;
_vrf_PLAT213_203highsymmetry_24  
;
PROBLEM: Atom C8              has ADP max/min Ratio .....        5.2 prolat
RESPONSE: The atom suffered from electron beam damage.
;
_vrf_PLAT602_203highsymmetry_24  
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check 
RESPONSE: This is a porous MOF crystal.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_201_92
_database_code_depnum_ccdc_archive 'CCDC 2300603'
loop_
_audit_author_name
_audit_author_address
'Yi Zhou'
;ShanghaiTech University
China
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_audit_creation_date             2023-10-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 O10 V2'
_chemical_formula_weight         197.59
_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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 'Peng, L.M. (1999) Micron 30, 625-648'
_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           10
_space_group_name_H-M_alt        P2/m
_space_group_name_Hall           '-P 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, z'

_cell_length_a                   6.760
_cell_length_b                   15.696
_cell_length_c                   15.638
_cell_angle_alpha                90
_cell_angle_beta                 103.4
_cell_angle_gamma                90
_cell_volume                     1614.1
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7246
_cell_measurement_temperature    298
_cell_measurement_theta_max      0.898
_cell_measurement_theta_min      0.304
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.813
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       nanoplate
_exptl_crystal_F_000             147
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_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  0.2861
_diffrn_reflns_av_unetI/netI     0.2028
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19349
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.912
_diffrn_reflns_theta_min         0.046
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'JEM-F200 with Cheetah 1800 camera'
_diffrn_measurement_method       ?
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1593
_reflns_number_total             3235
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         0.473
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.135
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3235
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.4050
_refine_ls_R_factor_gt           0.3530
_refine_ls_restrained_S_all      2.137
_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          0.6583
_refine_ls_wR_factor_ref         0.6919
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C8-C9 \\sim C8_$1-C11_$1 \\sim C12_$1-C12_$2 \\sim C11_$2-C8_$2 \\sim
C9_$3-C8_$3 \\sim C11_$3-
 C12_$3 \\sim C12-C11 \\sim C10-C10_$3
 with sigma of 0.02
 C8-C11 \\sim C9-C8 \\sim C9-C8_$1 \\sim C8_$1-C11_$1 \\sim C11_$1-C10 \\sim
C11-C10
 with sigma of 0.02
 C8-C10 \\sim C9-C11_$1
 with sigma of 0.02
 C8-C11_$1 \\sim C11-C8_$1 \\sim C10-C9
 with sigma of 0.02
 C12-C10_$3 \\sim C12_$3-C10 \\sim C11_$3-C11
 with sigma of 0.02
 C12-C10 \\sim C12_$3-C10_$3
 with sigma of 0.02
 C10-C12_$2 \\sim C10_$3-C12_$1 \\sim C11_$2-C11_$1
 with sigma of 0.02
 C10-C12_$1 \\sim C10_$3-C12_$2
 with sigma of 0.02
 C11_$3-C8_$2 \\sim C8_$3-C11_$2 \\sim C9_$3-C10_$3
 with sigma of 0.02
 C11_$3-C11_$2 \\sim C8_$3-C8_$2
 with sigma of 0.02
 C7-C2 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C7-C6
 with sigma of 0.02
 C7-C4 \\sim C2-C5 \\sim C3-C6
 with sigma of 0.02
 C7-C5 \\sim C2-C4
 with sigma of 0.02
2. Restrained planarity
 C11, C10, C10_$3, C11_$3, C12_$3, C12
 with sigma of 0.1
 C11_$1, C12_$1, C12_$2, C11_$2, C10_$3, C10
 with sigma of 0.1
 C1, C2, C7, C6, C5, C4, C3, C8
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C12 \\sim C10 \\sim C11 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C4 \\sim C3 \\sim C2 \\sim C7 \\sim C6 \\sim C5: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12) = Uanis(C11) = Uanis(C10)
;
_atom_sites_solution_hydrogens   .
_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
V001 V 1.000000 1.000000 0.500000 0.040(2) Uani 1 4 d S T P . .
V002 V 0.500000 1.000000 0.500000 0.056(3) Uani 1 4 d S T P . .
O1 O 0.775(2) 1.000000 0.5548(5) 0.037(3) Uani 1 2 d S T P . .
C1 C 0.701(3) 0.8858(6) 0.3892(7) 0.061(4) Uani 1 1 d . . . . .
O3 O 0.550(2) 0.9099(5) 0.4176(6) 0.067(4) Uani 1 1 d . . . . .
O2 O 0.873(2) 0.9107(6) 0.4174(6) 0.069(4) Uani 1 1 d . . . . .
C2 C 0.654(3) 0.8265(7) 0.3142(7) 0.091(5) Uani 1 1 d D U . . .
C11 C 0.542(3) 0.5896(4) 0.0812(4) 0.213(8) Uani 1 1 d D U . . .
C5 C 0.588(5) 0.7152(16) 0.1761(15) 0.189(11) Uani 1 1 d D U . . .
C8 C 0.548(5) 0.6788(6) 0.0813(4) 0.206(11) Uani 1 1 d D U . . .
C9 C 0.500000 0.7239(8) 0.000000 0.227(16) Uani 1 2 d DS TU P . .
C3 C 0.814(3) 0.7955(13) 0.2835(14) 0.139(8) Uani 1 1 d D U . . .
C7 C 0.465(3) 0.7946(14) 0.2820(13) 0.146(8) Uani 1 1 d D U . . .
C10 C 0.500000 0.5445(4) 0.000000 0.213(8) Uani 1 2 d DS TU P . .
C6 C 0.429(4) 0.7374(18) 0.2131(19) 0.213(12) Uani 1 1 d D U . . .
C12 C 0.585(5) 0.5454(4) 0.1630(6) 0.213(8) Uani 1 1 d D U . . .
C4 C 0.782(4) 0.7408(18) 0.2139(18) 0.201(11) Uani 1 1 d D U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V001 0.083(7) 0.016(2) 0.008(2) 0.000 -0.019(3) 0.000
V002 0.140(10) 0.013(2) 0.026(3) 0.000 0.043(4) 0.000
O1 0.070(11) 0.026(4) 0.010(4) 0.000 0.002(5) 0.000
C1 0.104(15) 0.033(5) 0.050(6) -0.007(4) 0.028(8) 0.008(6)
O3 0.110(13) 0.048(4) 0.039(4) -0.023(4) 0.006(5) 0.004(5)
O2 0.104(13) 0.051(5) 0.047(5) -0.032(4) 0.007(6) -0.019(6)
C2 0.093(9) 0.095(7) 0.085(7) -0.051(6) 0.020(7) -0.002(6)
C11 0.55(2) 0.034(4) 0.027(4) 0.017(4) 0.006(8) 0.015(8)
C5 0.192(14) 0.187(13) 0.190(13) -0.003(9) 0.047(9) 0.000(9)
C8 0.52(3) 0.040(6) 0.039(7) 0.002(6) 0.030(13) 0.023(12)
C9 0.56(5) 0.050(10) 0.033(9) 0.000 -0.011(18) 0.000
C3 0.140(11) 0.145(10) 0.130(10) -0.024(8) 0.027(8) 0.003(8)
C7 0.152(12) 0.150(11) 0.138(10) -0.019(8) 0.040(8) -0.011(8)
C10 0.55(2) 0.034(4) 0.027(4) 0.017(4) 0.006(8) 0.015(8)
C6 0.218(14) 0.212(14) 0.209(14) -0.013(9) 0.049(9) -0.003(9)
C12 0.55(2) 0.034(4) 0.027(4) 0.017(4) 0.006(8) 0.015(8)
C4 0.201(14) 0.203(13) 0.196(14) -0.011(9) 0.041(9) 0.007(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V001 O1 1.910(12) . ?
V001 O1 1.910(12) 3_776 ?
V001 O2 1.964(9) 2_756 ?
V001 O2 1.964(9) 4_575 ?
V001 O2 1.964(9) 3_776 ?
V001 O2 1.964(9) . ?
V002 O1 1.859(13) . ?
V002 O1 1.859(13) 3_676 ?
V002 O3 1.994(8) 4_575 ?
V002 O3 1.994(8) 3_676 ?
V002 O3 1.994(8) 2_656 ?
V002 O3 1.994(8) . ?
C1 O3 1.261(18) . ?
C1 O2 1.212(19) . ?
C1 C2 1.473(15) . ?
C2 C3 1.370(14) . ?
C2 C7 1.353(14) . ?
C11 C8 1.401(8) . ?
C11 C10 1.424(7) . ?
C11 C12 1.424(8) . ?
C5 C8 1.55(2) . ?
C5 C6 1.378(15) . ?
C5 C4 1.368(15) . ?
C8 C9 1.425(8) . ?
C3 C4 1.364(15) . ?
C7 C6 1.380(15) . ?
C10 C10 1.397(12) 4_565 ?
C12 C12 1.425(12) 4_565 ?

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
O1 V001 O1 180.0(4) . 3_776 ?
O1 V001 O2 88.6(5) 3_776 4_575 ?
O1 V001 O2 91.4(5) . . ?
O1 V001 O2 88.6(5) . 3_776 ?
O1 V001 O2 91.4(5) 3_776 2_756 ?
O1 V001 O2 91.4(5) 3_776 3_776 ?
O1 V001 O2 88.6(5) 3_776 . ?
O1 V001 O2 91.4(5) . 4_575 ?
O1 V001 O2 88.6(5) . 2_756 ?
O2 V001 O2 180.0 4_575 2_756 ?
O2 V001 O2 91.1(6) 3_776 2_756 ?
O2 V001 O2 180.0 3_776 . ?
O2 V001 O2 91.1(6) 4_575 . ?
O2 V001 O2 88.9(6) 3_776 4_575 ?
O2 V001 O2 88.9(6) 2_756 . ?
O1 V002 O1 180.0 . 3_676 ?
O1 V002 O3 89.9(4) 3_676 3_676 ?
O1 V002 O3 90.1(4) . 2_656 ?
O1 V002 O3 89.9(4) . . ?
O1 V002 O3 90.1(4) 3_676 4_575 ?
O1 V002 O3 90.1(4) 3_676 . ?
O1 V002 O3 89.9(5) 3_676 2_656 ?
O1 V002 O3 90.1(4) . 3_676 ?
O1 V002 O3 89.9(5) . 4_575 ?
O3 V002 O3 89.6(6) 3_676 4_575 ?
O3 V002 O3 90.4(6) . 4_575 ?
O3 V002 O3 89.6(6) . 2_656 ?
O3 V002 O3 180.0(3) 4_575 2_656 ?
O3 V002 O3 180.0 . 3_676 ?
O3 V002 O3 90.4(6) 3_676 2_656 ?
V002 O1 V001 127.5(4) . . ?
O3 C1 C2 115.3(15) . . ?
O2 C1 O3 124.4(13) . . ?
O2 C1 C2 120.2(14) . . ?
C1 O3 V002 135.3(11) . . ?
C1 O2 V001 134.8(11) . . ?
C3 C2 C1 117.5(15) . . ?
C7 C2 C1 122.8(15) . . ?
C7 C2 C3 119.3(10) . . ?
C8 C11 C10 119.8(5) . . ?
C8 C11 C12 119.1(5) . . ?
C10 C11 C12 121.1(4) . . ?
C6 C5 C8 121(2) . . ?
C4 C5 C8 117(2) . . ?
C4 C5 C6 120.5(12) . . ?
C11 C8 C5 111.5(11) . . ?
C11 C8 C9 119.7(5) . . ?
C9 C8 C5 128.4(11) . . ?
C8 C9 C8 120.4(7) 2_655 . ?
C4 C3 C2 120.8(13) . . ?
C2 C7 C6 121.0(11) . . ?
C11 C10 C11 120.4(5) . 2_655 ?
C10 C10 C11 119.8(2) 4_565 2_655 ?
C10 C10 C11 119.8(2) 4_565 . ?
C5 C6 C7 118.4(13) . . ?
C11 C12 C12 119.1(3) . 4_565 ?
C3 C4 C5 119.2(11) . . ?

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
C1 C2 C3 C4 -179.5(19) . . . . ?
C1 C2 C7 C6 -178.3(18) . . . . ?
O3 V002 O1 V001 45.2(3) . . . . ?
O3 V002 O1 V001 -134.8(3) 3_676 . . . ?
O3 V002 O1 V001 -45.2(3) 4_575 . . . ?
O3 V002 O1 V001 134.8(3) 2_656 . . . ?
O3 C1 O2 V001 -8.5(19) . . . . ?
O3 C1 C2 C3 -177.1(13) . . . . ?
O3 C1 C2 C7 -4.9(13) . . . . ?
O2 C1 O3 V002 9.2(19) . . . . ?
O2 C1 C2 C3 5.5(14) . . . . ?
O2 C1 C2 C7 177.8(14) . . . . ?
C2 C1 O3 V002 -168.0(8) . . . . ?
C2 C1 O2 V001 168.6(7) . . . . ?
C2 C3 C4 C5 -2(4) . . . . ?
C2 C7 C6 C5 -2(4) . . . . ?
C11 C8 C9 C8 -2.2(19) . . . 2_655 ?
C5 C8 C9 C8 -175(3) . . . 2_655 ?
C8 C11 C10 C11 -2.2(19) . . . 2_655 ?
C8 C11 C10 C10 177.8(19) . . . 4_565 ?
C8 C11 C12 C12 -177.8(19) . . . 4_565 ?
C8 C5 C6 C7 -158(2) . . . . ?
C8 C5 C4 C3 160(2) . . . . ?
C3 C2 C7 C6 -6(3) . . . . ?
C7 C2 C3 C4 8(3) . . . . ?
C10 C11 C8 C5 177.9(17) . . . . ?
C10 C11 C8 C9 4(4) . . . . ?
C10 C11 C12 C12 -0.4(13) . . . 4_565 ?
C6 C5 C8 C11 -92(3) . . . . ?
C6 C5 C8 C9 80(4) . . . . ?
C6 C5 C4 C3 -7(5) . . . . ?
C12 C11 C8 C5 -5(3) . . . . ?
C12 C11 C8 C9 -178.2(19) . . . . ?
C12 C11 C10 C11 -179.6(13) . . . 2_655 ?
C12 C11 C10 C10 0.4(13) . . . 4_565 ?
C4 C5 C8 C11 101(3) . . . . ?
C4 C5 C8 C9 -86(4) . . . . ?
C4 C5 C6 C7 8(5) . . . . ?

_shelx_res_file                  
;
TITL 201_92_a.res in P2/m
    201_92.res
    created by SHELXL-2018/3 at 10:45:25 on 08-Oct-2023
REM Old TITL 201_92_a.res in P2/m
REM SHELXT solution in P2/m: R1 0.494, Rweak 0.174, Alpha 0.122
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C27 O5 V2
REM ------ Electron scattering factors ------
REM SFAC Species a(1) b(1) a(2) b(2) a(3) b(3) =
REM a(4) b(4) c f' f'' mu cov_radius weight
CELL 0.02508 6.760 15.696 15.638 90 103.4 90
ZERR 4 0 0 0 0 0 0
LATT 1
SYMM -X,+Y,-Z
SFAC  C 0.731 36.995 1.195 11.297 0.456 2.814 0.125 0.346 0 0 0 0 0.77 12.011
SFAC  O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999
SFAC  V 3.245 76.379 2.698 17.726 1.86 3.363 0.486 0.374 0 0 0 0 1.22 50.942
UNIT 44 10 2

EQIV $1 1-X,+Y,-Z
EQIV $2 1-X,1-Y,-Z
EQIV $3 +X,1-Y,+Z
SADI C8 C9 C8_$1 C11_$1 C12_$1 C12_$2 C11_$2 C8_$2 C9_$3 C8_$3 C11_$3 =
 C12_$3 C12 C11 C10 C10_$3
SADI C8 C11 C9 C8 C9 C8_$1 C8_$1 C11_$1 C11_$1 C10 C11 C10
SADI C8 C10 C9 C11_$1
SADI C8 C11_$1 C11 C8_$1 C10 C9
SADI C12 C10_$3 C12_$3 C10 C11_$3 C11
SADI C12 C10 C12_$3 C10_$3
SADI C10 C12_$2 C10_$3 C12_$1 C11_$2 C11_$1
SADI C10 C12_$1 C10_$3 C12_$2
SADI C11_$3 C8_$2 C8_$3 C11_$2 C9_$3 C10_$3
SADI C11_$3 C11_$2 C8_$3 C8_$2
SADI C7 C2 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6
SADI C7 C4 C2 C5 C3 C6
SADI C7 C5 C2 C4
FLAT C11 C10 C10_$3 C11_$3 C12_$3 C12
FLAT C11_$1 C12_$1 C12_$2 C11_$2 C10_$3 C10
FLAT C1 C2 C7 C6 C5 C4 C3 C8
SIMU C12 C10 C11 C8 C9
SIMU C4 C3 C2 C7 C6 C5
EADP C12 C11 C10
ISOR 0.01 0.02 C5 C6 C7 C2 C3 C4

L.S. 50
PLAN  10
CONF
LIST 6
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\201_92.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       1.82697
V001  3    1.000000    1.000000    0.500000    10.25000    0.08269    0.01580 =
         0.00764    0.00000   -0.01893    0.00000
V002  3    0.500000    1.000000    0.500000    10.25000    0.14047    0.01278 =
         0.02635    0.00000    0.04269    0.00000
O1    2    0.775199    1.000000    0.554795    10.50000    0.07007    0.02649 =
         0.01037    0.00000    0.00238    0.00000
C1    1    0.700553    0.885841    0.389218    11.00000    0.10444    0.03312 =
         0.05016   -0.00708    0.02840    0.00783
O3    2    0.549618    0.909889    0.417587    11.00000    0.10980    0.04812 =
         0.03901   -0.02325    0.00606    0.00418
O2    2    0.873134    0.910652    0.417365    11.00000    0.10355    0.05092 =
         0.04710   -0.03212    0.00659   -0.01914
C2    1    0.653663    0.826496    0.314246    11.00000    0.09256    0.09538 =
         0.08450   -0.05128    0.01970   -0.00167
C11   1    0.541508    0.589555    0.081229    11.00000    0.54908    0.03391 =
         0.02749    0.01719    0.00597    0.01498
C5    1    0.587681    0.715245    0.176102    11.00000    0.19194    0.18722 =
         0.19047   -0.00338    0.04691   -0.00041
C8    1    0.548436    0.678772    0.081273    11.00000    0.52296    0.03953 =
         0.03918    0.00190    0.02959    0.02271
C9    1    0.500000    0.723886    0.000000    10.50000    0.55791    0.04976 =
         0.03333    0.00000   -0.01127    0.00000
C3    1    0.813524    0.795475    0.283523    11.00000    0.14031    0.14471 =
         0.13009   -0.02423    0.02650    0.00302
C7    1    0.465210    0.794555    0.281988    11.00000    0.15150    0.15038 =
         0.13793   -0.01913    0.03974   -0.01071
C10   1    0.500000    0.544505    0.000000    10.50000    0.54908    0.03391 =
         0.02749    0.01719    0.00597    0.01498
C6    1    0.428672    0.737399    0.213085    11.00000    0.21820    0.21180 =
         0.20864   -0.01251    0.04879   -0.00277
C12   1    0.584504    0.545379    0.162982    11.00000    0.54908    0.03391 =
         0.02749    0.01719    0.00597    0.01498
C4    1    0.781713    0.740786    0.213896    11.00000    0.20134    0.20303 =
         0.19596   -0.01053    0.04063    0.00731
HKLF 4




REM  201_92_a.res in P2/m
REM wR2 = 0.6919, GooF = S = 2.135, Restrained GooF = 2.137 for all data
REM R1 = 0.3530 for 1593 Fo > 4sig(Fo) and 0.4050 for all 3235 data
REM 123 parameters refined using 208 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.473,  deepest hole -0.445,  1-sigma level  0.092
Q1    1   1.0082  0.5000  0.1048  10.50000  0.05    0.31
Q2    1   0.6542  0.6570  0.2401  11.00000  0.05    0.26
Q3    1   0.6712  0.7908  0.3418  11.00000  0.05    0.24
Q4    1   0.0000  0.5954  0.0000  10.50000  0.05    0.24
Q5    1   0.7631  1.0000  0.1870  10.50000  0.05    0.22
Q6    1   0.9573  0.7718  0.3563  11.00000  0.05    0.19
Q7    1   0.8327  0.6829  0.2827  11.00000  0.05    0.19
Q8    1   0.9137  0.7596  0.3381  11.00000  0.05    0.19
Q9    1   1.0035  0.7920  0.4123  11.00000  0.05    0.19
Q10   1   1.0109  1.0000  0.0875  10.50000  0.05    0.18
;
_shelx_res_checksum              60536
_olex2_submission_special_instructions 'No special instructions were received'


# start Validation Reply Form
_vrf_RINTA01_201_92              
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Merged electron diffraction data.
;
_vrf_PLAT020_201_92              
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.286 Report
RESPONSE: Merged electron diffraction data.
;
_vrf_PLAT082_201_92              
;
PROBLEM: High R1 Value ..................................       0.35 Report
RESPONSE: Electron diffraction data normally has high R1 values, and this data
 quality is not good enough.
;
_vrf_PLAT084_201_92              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.69 Report
RESPONSE: Electron diffraction data normally has high wR2 values.
;
_vrf_PLAT213_201_92              
;
PROBLEM: Atom V001            has ADP max/min Ratio .....        5.7 prolat
RESPONSE: The atom suffered from electron beam damage , and this data quality is
 not good enough.
;
_vrf_PLAT602_201_92              
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check 
RESPONSE: Checked. This is a porous MOF crystal.
;
_vrf_PLAT049_201_92              
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.8131 Check 
RESPONSE: This is a porous MOF crystal.
;
_vrf_PLAT113_201_92              
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Cmmm Check 
RESPONSE: Experimental data shows more like to be monoclinic.
;
_vrf_PLAT341_201_92              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02053 Ang.  
RESPONSE: The atoms suffered from electron beam damage.
;
# end Validation Reply Form
