# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_Yyy
_database_code_depnum_ccdc_archive 'CCDC 1993317'
loop_
_audit_author_name
_audit_author_address
'Kuan Li'
;Xinjiang Technical Institute of Physics  Chemistry
China
;
_audit_update_record             
;
2020-03-28 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B I O7 Pb6'
_chemical_formula_weight         1492.85

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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'

_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+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   5.780(12)
_cell_length_b                   9.72(2)
_cell_length_c                   10.63(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     597(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    434
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      26.21

_exptl_crystal_description       flake
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      8.302
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    8.302
_exptl_crystal_F_000             1212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    86.859
_shelx_estimated_absorpt_T_min   0.024
_shelx_estimated_absorpt_T_max   0.038
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5243
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3651
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_av_R_equivalents  0.1764
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.916
_diffrn_reflns_theta_max         27.684
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             808
_reflns_number_gt                548
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.0476P)²] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00108(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         808
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1322
_refine_ls_wR_factor_gt          0.1192
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.973
_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 0.7500 0.52056(12) 0.38227(13) 0.0196(4) Uani 1 2 d S T P . .
Pb2 Pb 0.2500 0.45489(11) 0.16510(15) 0.0193(4) Uani 1 2 d S T P . .
Pb3 Pb 0.7500 0.7500 0.12874(19) 0.0178(5) Uani 1 4 d S T P . .
Pb4 Pb 0.2500 0.7500 0.3582(2) 0.0173(5) Uani 1 4 d S T P . .
B1 B 0.2500 0.2500 0.407(7) 0.032(16) Uani 1 4 d S T P . .
I1 I 0.7500 0.2500 0.1166(4) 0.0401(12) Uani 1 4 d S T P . .
O1 O 0.001(2) 0.6068(12) 0.2459(14) 0.013(3) Uani 1 1 d . . . . .
O2 O 0.2500 0.2500 0.547(3) 0.025(8) Uani 1 4 d S T P . .
O3 O 0.2500 0.377(2) 0.358(2) 0.025(6) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0198(8) 0.0142(6) 0.0250(10) 0.0045(5) 0.000 0.000
Pb2 0.0204(7) 0.0143(6) 0.0231(10) -0.0034(5) 0.000 0.000
Pb3 0.0184(10) 0.0154(8) 0.0194(12) 0.000 0.000 0.000
Pb4 0.0180(10) 0.0136(7) 0.0204(12) 0.000 0.000 0.000
B1 0.02(3) 0.06(4) 0.01(4) 0.000 0.000 0.000
I1 0.0198(19) 0.0317(18) 0.069(4) 0.000 0.000 0.000
O1 0.006(7) 0.014(7) 0.018(10) -0.004(6) -0.001(7) 0.002(5)
O2 0.06(2) 0.010(14) 0.01(2) 0.000 0.000 0.000
O3 0.032(15) 0.021(11) 0.022(16) 0.004(12) 0.000 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.216(15) 7_655 ?
Pb1 O1 2.216(15) 1_655 ?
Pb1 O2 2.355(12) 5_666 ?
Pb1 Pb3 3.498(5) . ?
Pb1 Pb4 3.659(6) . ?
Pb1 Pb4 3.659(6) 1_655 ?
Pb2 O3 2.19(3) . ?
Pb2 O1 2.233(13) 7_655 ?
Pb2 O1 2.233(13) . ?
Pb2 Pb4 3.527(6) . ?
Pb3 O1 2.365(14) 8_675 ?
Pb3 O1 2.365(14) 7_655 ?
Pb3 O1 2.365(14) 2_565 ?
Pb3 O1 2.365(14) 1_655 ?
Pb3 Pb1 3.498(5) 2_665 ?
Pb4 O1 2.331(14) 2_565 ?
Pb4 O1 2.331(14) 8_575 ?
Pb4 O1 2.331(14) 7_655 ?
Pb4 O1 2.331(14) . ?
Pb4 Pb2 3.527(6) 2_565 ?
Pb4 Pb1 3.659(6) 2_665 ?
Pb4 Pb1 3.659(6) 1_455 ?
Pb4 Pb1 3.659(6) 2_565 ?
B1 O3 1.33(3) 2 ?
B1 O3 1.33(3) . ?
B1 O2 1.48(7) . ?
O1 Pb1 2.216(15) 1_455 ?
O1 Pb3 2.365(14) 1_455 ?
O2 Pb1 2.355(12) 5_666 ?
O2 Pb1 2.355(12) 6_556 ?

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 81.8(7) 7_655 1_655 ?
O1 Pb1 O2 81.5(7) 7_655 5_666 ?
O1 Pb1 O2 81.5(7) 1_655 5_666 ?
O1 Pb1 Pb3 41.8(4) 7_655 . ?
O1 Pb1 Pb3 41.8(4) 1_655 . ?
O2 Pb1 Pb3 69.1(8) 5_666 . ?
O1 Pb1 Pb4 37.5(4) 7_655 . ?
O1 Pb1 Pb4 104.0(3) 1_655 . ?
O2 Pb1 Pb4 56.3(3) 5_666 . ?
Pb3 Pb1 Pb4 63.74(8) . . ?
O1 Pb1 Pb4 104.0(3) 7_655 1_655 ?
O1 Pb1 Pb4 37.5(4) 1_655 1_655 ?
O2 Pb1 Pb4 56.3(3) 5_666 1_655 ?
Pb3 Pb1 Pb4 63.74(8) . 1_655 ?
Pb4 Pb1 Pb4 104.32(16) . 1_655 ?
O3 Pb2 O1 82.5(6) . 7_655 ?
O3 Pb2 O1 82.5(6) . . ?
O1 Pb2 O1 80.2(7) 7_655 . ?
O3 Pb2 Pb4 74.8(6) . . ?
O1 Pb2 Pb4 40.4(4) 7_655 . ?
O1 Pb2 Pb4 40.4(4) . . ?
O1 Pb3 O1 116.5(7) 8_675 7_655 ?
O1 Pb3 O1 75.7(7) 8_675 2_565 ?
O1 Pb3 O1 72.1(6) 7_655 2_565 ?
O1 Pb3 O1 72.1(6) 8_675 1_655 ?
O1 Pb3 O1 75.7(7) 7_655 1_655 ?
O1 Pb3 O1 116.5(7) 2_565 1_655 ?
O1 Pb3 Pb1 88.3(3) 8_675 . ?
O1 Pb3 Pb1 38.7(4) 7_655 . ?
O1 Pb3 Pb1 88.3(3) 2_565 . ?
O1 Pb3 Pb1 38.7(4) 1_655 . ?
O1 Pb3 Pb1 38.7(4) 8_675 2_665 ?
O1 Pb3 Pb1 88.3(3) 7_655 2_665 ?
O1 Pb3 Pb1 38.7(4) 2_565 2_665 ?
O1 Pb3 Pb1 88.3(3) 1_655 2_665 ?
Pb1 Pb3 Pb1 79.22(17) . 2_665 ?
O1 Pb4 O1 76.2(7) 2_565 8_575 ?
O1 Pb4 O1 73.4(6) 2_565 7_655 ?
O1 Pb4 O1 118.4(7) 8_575 7_655 ?
O1 Pb4 O1 118.4(7) 2_565 . ?
O1 Pb4 O1 73.4(6) 8_575 . ?
O1 Pb4 O1 76.2(7) 7_655 . ?
O1 Pb4 Pb2 38.4(3) 2_565 2_565 ?
O1 Pb4 Pb2 38.4(3) 8_575 2_565 ?
O1 Pb4 Pb2 100.8(4) 7_655 2_565 ?
O1 Pb4 Pb2 100.8(4) . 2_565 ?
O1 Pb4 Pb2 100.8(4) 2_565 . ?
O1 Pb4 Pb2 100.8(4) 8_575 . ?
O1 Pb4 Pb2 38.4(3) 7_655 . ?
O1 Pb4 Pb2 38.4(3) . . ?
Pb2 Pb4 Pb2 108.83(17) 2_565 . ?
O1 Pb4 Pb1 85.0(3) 2_565 . ?
O1 Pb4 Pb1 152.5(4) 8_575 . ?
O1 Pb4 Pb1 35.4(4) 7_655 . ?
O1 Pb4 Pb1 99.2(3) . . ?
Pb2 Pb4 Pb1 122.43(9) 2_565 . ?
Pb2 Pb4 Pb1 62.94(9) . . ?
O1 Pb4 Pb1 35.4(4) 2_565 2_665 ?
O1 Pb4 Pb1 99.2(3) 8_575 2_665 ?
O1 Pb4 Pb1 85.0(3) 7_655 2_665 ?
O1 Pb4 Pb1 152.5(4) . 2_665 ?
Pb2 Pb4 Pb1 62.94(9) 2_565 2_665 ?
Pb2 Pb4 Pb1 122.43(9) . 2_665 ?
Pb1 Pb4 Pb1 75.10(16) . 2_665 ?
O1 Pb4 Pb1 152.5(4) 2_565 1_455 ?
O1 Pb4 Pb1 85.0(3) 8_575 1_455 ?
O1 Pb4 Pb1 99.2(3) 7_655 1_455 ?
O1 Pb4 Pb1 35.4(4) . 1_455 ?
Pb2 Pb4 Pb1 122.43(9) 2_565 1_455 ?
Pb2 Pb4 Pb1 62.94(9) . 1_455 ?
Pb1 Pb4 Pb1 104.32(16) . 1_455 ?
Pb1 Pb4 Pb1 171.98(8) 2_665 1_455 ?
O1 Pb4 Pb1 99.2(3) 2_565 2_565 ?
O1 Pb4 Pb1 35.4(4) 8_575 2_565 ?
O1 Pb4 Pb1 152.5(4) 7_655 2_565 ?
O1 Pb4 Pb1 85.0(3) . 2_565 ?
Pb2 Pb4 Pb1 62.94(9) 2_565 2_565 ?
Pb2 Pb4 Pb1 122.43(9) . 2_565 ?
Pb1 Pb4 Pb1 171.98(8) . 2_565 ?
Pb1 Pb4 Pb1 104.32(16) 2_665 2_565 ?
Pb1 Pb4 Pb1 75.10(16) 1_455 2_565 ?
O3 B1 O3 134(6) 2 . ?
O3 B1 O2 113(3) 2 . ?
O3 B1 O2 113(3) . . ?
Pb1 O1 Pb2 115.1(5) 1_455 . ?
Pb1 O1 Pb4 107.1(6) 1_455 . ?
Pb2 O1 Pb4 101.2(6) . . ?
Pb1 O1 Pb3 99.5(5) 1_455 1_455 ?
Pb2 O1 Pb3 125.6(7) . 1_455 ?
Pb4 O1 Pb3 107.3(5) . 1_455 ?
B1 O2 Pb1 108.7(8) . 5_666 ?
B1 O2 Pb1 108.7(8) . 6_556 ?
Pb1 O2 Pb1 142.5(16) 5_666 6_556 ?
B1 O3 Pb2 133(3) . . ?

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
O3 B1 O2 Pb1 180.000(5) 2 . . 5_666 ?
O3 B1 O2 Pb1 0.000(8) . . . 5_666 ?
O3 B1 O2 Pb1 0.000(5) 2 . . 6_556 ?
O3 B1 O2 Pb1 180.000(7) . . . 6_556 ?
O3 B1 O3 Pb2 0.000(10) 2 . . . ?
O2 B1 O3 Pb2 180.000(8) . . . . ?

_refine_diff_density_max         5.772
_refine_diff_density_min         -4.881
_refine_diff_density_rms         1.013

_shelxl_version_number           2013-2

_shelx_res_file                  
; 
TITL Yyy in Pmmn                 New: Pmmn 
CELL  0.71073    5.7800    9.7200   10.6300    90.000    90.000    90.000 
ZERR        2    0.0120    0.0200    0.0200     0.000     0.000     0.000 
LATT 1 
SYMM     0.50000 - X ,    0.50000 - Y ,              Z 
SYMM     0.50000 + X ,            - Y ,            - Z 
SYMM             - X ,    0.50000 + Y ,            - Z 
SFAC B  I  O  Pb 
UNIT 2  2  14  12 
L.S. 20 
ACTA 
BOND $H 
FMAP 2 
PLAN 10 
CONF 
SIZE 0.17 0.15  0.11 
WGHT    0.047600 
EXTI    0.001078 
FVAR       0.04259 
PB1   4    0.750000    0.520563    0.382265    10.50000    0.01978    0.01417 = 
         0.02500    0.00454    0.00000    0.00000 
PB2   4    0.250000    0.454888    0.165101    10.50000    0.02041    0.01427 = 
         0.02314   -0.00339    0.00000    0.00000 
PB3   4    0.750000    0.750000    0.128742    10.25000    0.01841    0.01543 = 
         0.01943    0.00000    0.00000    0.00000 
PB4   4    0.250000    0.750000    0.358189    10.25000    0.01800    0.01361 = 
         0.02039    0.00000    0.00000    0.00000 
B1    1    0.250000    0.250000    0.407204    10.25000    0.02212    0.06359 = 
         0.00884    0.00000    0.00000    0.00000 
I1    2    0.750000    0.250000    0.116575    10.25000    0.01977    0.03170 = 
         0.06891    0.00000    0.00000    0.00000 
O1    3    0.001131    0.606764    0.245860    11.00000    0.00560    0.01410 = 
         0.01822   -0.00389   -0.00126    0.00248 
O2    3    0.250000    0.250000    0.546576    10.25000    0.05770    0.01029 = 
         0.00613    0.00000    0.00000    0.00000 
O3    3    0.250000    0.376508    0.358310    10.50000    0.03228    0.02055 = 
         0.02201    0.00427    0.00000    0.00000 
HKLF 4 1  0.0000  1.0000  0.0000 -1.0000  0.0000  0.0000  0.0000  0.0000  1.0000 
  
REM  Yyy in Pmmn                 New: Pmmn 
REM R1 =  0.0565 for     548 Fo > 4sig(Fo)  and  0.0895 for all     808 data 
REM     49 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0468      0.0000 
  
REM Highest difference peak  5.772,  deepest hole -4.881,  1-sigma level  1.013 
Q1    1   0.0884  0.7500  0.3624  10.50000  0.05    5.77 
Q2    1   0.0776  0.4529  0.1634  11.00000  0.05    4.19 
Q3    1   0.9261  0.5201  0.3730  11.00000  0.05    4.06 
Q4    1   0.9227  0.7500  0.1352  10.50000  0.05    3.94 
Q5    1   0.2500  0.7500  0.3055  10.25000  0.05    3.29 
Q6    1   0.8722  0.6756  0.0529  11.00000  0.05    3.23 
Q7    1   0.1386  0.5291  0.0778  11.00000  0.05    3.19 
Q8    1   0.1421  0.2885  0.3995  11.00000  0.05    3.14 
Q9    1   0.8468  0.4156  0.4032  11.00000  0.05    3.09 
Q10   1   0.7500  0.5903  0.2783  10.50000  0.05    2.82 
;
_shelx_res_checksum              6584
