# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_pbbe2b2o6
_database_code_depnum_ccdc_archive 'CCDC 2094337'
loop_
_audit_author_name
_audit_author_address
'Yigang Chen'
;Shanxi Normal University
China
;
_audit_update_record             
;
2022-10-10 deposited with the CCDC.	2022-10-13 downloaded from the CCDC.
;
_audit_creation_date             2022-10-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(B4 Be4 O12 Pb2)'
_chemical_formula_sum            'B2 Be2 O6 Pb'
_chemical_formula_weight         342.83
_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
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   10.737(2)
_cell_length_b                   4.7501(11)
_cell_length_c                   4.5368(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     231.39(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      3.80
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    36.403
_exptl_absorpt_correction_T_max  0.1701
_exptl_absorpt_correction_T_min  0.0379
_exptl_absorpt_correction_type   'multi-scan and numerical'
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for empirical absorption correction (multi-scan).
wR2(int) was 0.1628 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.2228.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   
; 
SADABS-2016/2 - Bruker AXS area detector scaling and face absorption correction (numerical). 
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10.
Mean and maximum errors in direction cosine check function =   0.000   0.000.
The mean error should not exceed 0.005, and is usually caused by matrix 
changes during data processing.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.921
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6469
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.442
_diffrn_reflns_theta_min         3.795
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                730
_reflns_number_total             730
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_coef       0.065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         730
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0173
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+1.0296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0425
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.54(3)
 0.46(3)
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
;
_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
Pb1 Pb 0.0000 -0.82387(5) -0.14392(15) 0.01651(17) Uani 1 2 d S T P . .
O1 O 0.1363(5) -0.9042(11) -0.635(8) 0.0429(18) Uani 1 1 d . U . . .
O2 O -0.1327(6) -1.2016(12) -0.2800(13) 0.0180(11) Uani 1 1 d . . . . .
Be1 Be -0.2489(11) -1.3208(16) -0.207(2) 0.017(2) Uani 1 1 d . . . . .
O3 O -0.2911(6) -1.6194(13) -0.2370(12) 0.0172(10) Uani 1 1 d . U . . .
B1 B 0.1581(9) -1.1617(15) -0.5750(18) 0.0155(18) Uani 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
Pb1 O1 2.69(3) . ?
Pb1 O1 2.69(3) 3 ?
Pb1 O2 2.373(6) . ?
Pb1 O2 2.373(6) 3 ?
O1 Be1 1.664(14) 4_534 ?
O1 B1 1.275(12) . ?
O2 Be1 1.409(13) . ?
O2 B1 1.379(10) 3 ?
Be1 O1 1.664(14) 4_435 ?
Be1 O3 2.194(11) 2_425 ?
Be1 O3 1.495(10) . ?
Be1 B1 2.076(13) 3 ?
O3 Be1 2.194(11) 2_424 ?
O3 B1 1.385(10) 4_425 ?
B1 O2 1.379(10) 3 ?
B1 Be1 2.075(13) 3 ?
B1 O3 1.385(10) 4_524 ?

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 Pb1 O1 65.9(8) 3 . ?
O2 Pb1 O1 90.2(3) . . ?
O2 Pb1 O1 90.2(3) 3 3 ?
O2 Pb1 O1 49.5(3) 3 . ?
O2 Pb1 O1 49.5(3) . 3 ?
O2 Pb1 O2 73.8(3) 3 . ?
Be1 O1 Pb1 118.3(12) 4_534 . ?
B1 O1 Pb1 93.4(16) . . ?
B1 O1 Be1 121.5(7) . 4_534 ?
Be1 O2 Pb1 140.7(5) . . ?
B1 O2 Pb1 105.5(4) 3 . ?
B1 O2 Be1 96.2(7) 3 . ?
O1 Be1 O3 92.1(12) 4_435 2_425 ?
O1 Be1 B1 105.8(11) 4_435 3 ?
O2 Be1 O1 116.3(6) . 4_435 ?
O2 Be1 O3 96.1(6) . 2_425 ?
O2 Be1 O3 128.9(8) . . ?
O2 Be1 B1 41.3(4) . 3 ?
O3 Be1 O1 113.8(7) . 4_435 ?
O3 Be1 O3 91.4(5) . 2_425 ?
O3 Be1 B1 114.5(6) . 3 ?
B1 Be1 O3 137.5(6) 3 2_425 ?
Be1 O3 Be1 98.7(5) . 2_424 ?
B1 O3 Be1 119.7(5) 4_425 2_424 ?
B1 O3 Be1 141.5(7) 4_425 . ?
O1 B1 O2 107.6(16) . 3 ?
O1 B1 Be1 127.4(14) . 3 ?
O1 B1 O3 132.8(17) . 4_524 ?
O2 B1 Be1 42.5(5) 3 3 ?
O2 B1 O3 119.3(6) 3 4_524 ?
O3 B1 Be1 88.2(5) 4_524 3 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54(3)
2 0.46(3)

