# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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(1)2(1)2(1)
_database_code_depnum_ccdc_archive 'CCDC 1886438'
loop_
_audit_author_name
_audit_author_address
'Je Seung Lee'
;Kyung Hee University
South Korea
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H2 O4 Pb'
_chemical_formula_weight         297.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.4194 10.2008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   6.5227(8)
_cell_length_b                   7.4153(8)
_cell_length_c                   8.7646(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     423.92(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    3379
_cell_measurement_theta_min      2.745
_cell_measurement_theta_max      28.2625

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    4.657
_exptl_crystal_F_000             512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    39.405
_shelx_estimated_absorpt_T_min   0.021
_shelx_estimated_absorpt_T_max   0.044
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.0128
_exptl_absorpt_correction_T_max  0.0216
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan and phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3197
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.599
_diffrn_reflns_theta_max         27.970
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1021
_reflns_number_gt                987
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0298P)²+3.3987P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.98(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1021
_refine_ls_number_parameters     50
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0789
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.93043(7) 0.26150(7) 0.83256(7) 0.00287(18) Uani 1 1 d . . . . .
C1 C 0.422(2) 0.107(2) 0.8000(18) 0.007(3) Uiso 1 1 d . . . . .
H1 H 0.497702 0.037782 0.731920 0.008 Uiso 1 1 calc R U . . .
O1 O 0.5197(18) 0.2325(17) 0.8638(12) 0.011(2) Uani 1 1 d . . . . .
O4 O 1.1470(16) 0.4237(14) 0.6097(12) 0.005(2) Uiso 1 1 d . . . . .
O2 O 1.2409(16) 0.0621(15) 0.8141(15) 0.011(2) Uani 1 1 d . . . . .
C2 C 1.2483(19) 0.345(2) 0.5089(19) 0.005(3) Uiso 1 1 d . . . . .
H2 H 1.244302 0.219557 0.510059 0.006 Uiso 1 1 calc R U . . .
O3 O 0.8548(16) 0.0837(15) 0.5939(13) 0.006(2) Uani 1 1 d . . . . .

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
Pb1 0.0045(3) 0.0035(3) 0.0006(3) -0.0005(2) -0.00058(19) 0.00029(19)
O1 0.021(5) 0.012(6) 0.002(5) 0.001(5) -0.004(4) -0.001(5)
O2 0.017(6) 0.006(5) 0.010(7) 0.004(5) -0.003(5) 0.002(4)
O3 0.005(5) 0.008(6) 0.005(6) 0.004(5) 0.000(4) 0.002(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.512(11) . ?
Pb1 O3 2.521(12) . ?
Pb1 O4 2.605(11) 4_746 ?
Pb1 O4 2.694(11) . ?
Pb1 O1 2.702(12) . ?
Pb1 O1 2.725(11) 3_557 ?
C1 O2 1.233(17) 1_455 ?
C1 O1 1.259(19) . ?
C1 H1 0.9300 . ?
O4 C2 1.248(18) . ?
C2 O3 1.254(18) 3_556 ?
C2 H2 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 Pb1 O3 78.3(4) . . ?
O2 Pb1 O4 66.6(3) . 4_746 ?
O3 Pb1 O4 67.7(4) . 4_746 ?
O2 Pb1 O4 78.1(4) . . ?
O3 Pb1 O4 74.6(3) . . ?
O4 Pb1 O4 132.2(3) 4_746 . ?
O2 Pb1 O1 139.4(4) . . ?
O3 Pb1 O1 81.3(3) . . ?
O4 Pb1 O1 73.2(3) 4_746 . ?
O4 Pb1 O1 129.0(3) . . ?
O2 Pb1 O1 84.3(4) . 3_557 ?
O3 Pb1 O1 149.4(4) . 3_557 ?
O4 Pb1 O1 82.4(4) 4_746 3_557 ?
O4 Pb1 O1 126.1(3) . 3_557 ?
O1 Pb1 O1 96.6(3) . 3_557 ?
O2 C1 O1 129.8(15) 1_455 . ?
O2 C1 H1 115.1 1_455 . ?
O1 C1 H1 115.1 . . ?
C1 O1 Pb1 121.1(10) . . ?
C1 O1 Pb1 109.7(10) . 3_457 ?
Pb1 O1 Pb1 108.0(4) . 3_457 ?
C2 O4 Pb1 133.6(10) . 4_756 ?
C2 O4 Pb1 125.6(10) . . ?
Pb1 O4 Pb1 100.8(4) 4_756 . ?
C1 O2 Pb1 128.2(10) 1_655 . ?
O4 C2 O3 127.2(15) . 3_556 ?
O4 C2 H2 116.4 . . ?
O3 C2 H2 116.4 3_556 . ?
C2 O3 Pb1 118.9(10) 3_456 . ?

_refine_diff_density_max         1.834
_refine_diff_density_min         -3.812
_refine_diff_density_rms         0.507

_shelx_res_file                  
;
TITL P2(1)2(1)2(1) in P2(1)2(1)2(1)
    P2(1)2(1)2(1).res
    created by SHELXL-2017/1 at 20:20:17 on 04-Dec-2018
CELL  0.71073   6.5227   7.4153   8.7646   90.000   90.000   90.000
ZERR     4.00   0.0008   0.0008   0.0010    0.000    0.000    0.000
LATT -1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  1/2 + X, 1/2 - Y, - Z
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC C  H  O  Pb
DISP $C  0.00341  0.00169 11.32113!source kissel
DISP $H -0.00002  0.00000  0.66638!source kissel
DISP $O  0.01140  0.00623 32.03669!source kissel
DISP $Pb -3.41943 10.20082 41609.52882!source kissel
UNIT 8  8  16  4
LIST 4
MERG 2
OMIT -2 56
L.S. 10
TEMP 25
SIZE 0.43  0.25  0.21
ACTA
BOND   $H
FMAP 2
PLAN 10
TWIN
eqiv $1 2-x, y+0.5, 1.5-z
temp 24
WGHT    0.029800    3.398700
BASF   0.97902
FVAR       0.11529
PB1   4    0.930427    0.261499    0.832555    11.00000    0.00448    0.00348 =
         0.00065   -0.00049   -0.00058    0.00029
C1    1    0.421896    0.107100    0.800014    11.00000    0.00694
AFIX  43
H1    2    0.497702    0.037782    0.731920    11.00000   -1.20000
AFIX   0
O1    3    0.519661    0.232543    0.863752    11.00000    0.02123    0.01159 =
         0.00157    0.00066   -0.00406   -0.00099
O4    3    1.147018    0.423669    0.609718    11.00000    0.00469
O2    3    1.240855    0.062122    0.814123    11.00000    0.01738    0.00551 =
         0.00961    0.00395   -0.00298    0.00218
C2    1    1.248277    0.344917    0.508884    11.00000    0.00478
AFIX  43
H2    2    1.244302    0.219557    0.510059    11.00000   -1.20000
AFIX   0
O3    3    0.854807    0.083729    0.593859    11.00000    0.00504    0.00789 =
         0.00468    0.00437    0.00027    0.00238
HKLF 4




REM  P2(1)2(1)2(1) in P2(1)2(1)2(1)
REM R1 =  0.0301 for     987 Fo > 4sig(Fo)  and  0.0314 for all    1021 data
REM     50 parameters refined using      0 restraints

END

WGHT      0.0304      3.4445

REM Highest difference peak  1.834,  deepest hole -3.812,  1-sigma level  0.507
Q1    1   0.3482  0.1250  0.8336  11.00000  0.05    1.83
Q2    1   0.9151  0.2855  0.6774  11.00000  0.05    1.81
Q3    1   0.9243 -0.0024  0.6630  11.00000  0.05    1.73
Q4    1   0.9357  0.2939  0.9725  11.00000  0.05    1.68
Q5    1   0.9328  0.3477  0.7716  11.00000  0.05    1.61
Q6    1   0.9255  0.3399  0.8924  11.00000  0.05    1.53
Q7    1   0.6896  0.2839  0.8425  11.00000  0.05    1.41
Q8    1   0.4894 -0.1408  0.8189  11.00000  0.05    1.39
Q9    1   1.2561  0.2529  0.6716  11.00000  0.05    1.34
Q10   1   1.0801  0.3765  0.8737  11.00000  0.05    1.31
;
_shelx_res_checksum              21420
