# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_m2
_database_code_depnum_ccdc_archive 'CCDC 1961610'
loop_
_audit_author_name
_audit_author_address
'Ruling Tang'
;ShanghaiTech University
China
;
_audit_update_record             
;
2019-10-28 deposited with the CCDC.	2019-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'I O7 P Pb2'
_chemical_formula_weight         684.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   7.3740(3)
_cell_length_b                   6.8144(3)
_cell_length_c                   13.6077(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.973(4)
_cell_angle_gamma                90.00
_cell_volume                     660.56(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3169
_cell_measurement_theta_min      3.5730
_cell_measurement_theta_max      29.0190

_exptl_crystal_description       bulk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_absorpt_coefficient_mu    55.812
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_T_max  2.733
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       ccd
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6133
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         27.10
_reflns_number_total             1438
_reflns_number_gt                1225
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0609P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1438
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1213
_refine_ls_wR_factor_gt          0.1146
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb2 Pb 0.22333(8) 0.86727(9) 0.45667(4) 0.0159(2) Uani 1 1 d . . .
Pb1 Pb -0.08776(8) 0.35171(9) 0.28846(5) 0.0193(2) Uani 1 1 d . . .
I1 I 0.55533(13) 0.62870(13) 0.68531(7) 0.0127(3) Uani 1 1 d . . .
P1 P 0.2196(5) 0.3466(6) 0.5036(3) 0.0127(8) Uani 1 1 d . . .
O5 O 0.3919(18) 0.8395(16) 0.6600(9) 0.023(3) Uani 1 1 d . . .
O4 O 0.3952(15) 0.2366(19) 0.4910(9) 0.026(3) Uani 1 1 d . . .
O1 O 0.0540(14) 0.1954(16) 0.4793(8) 0.016(2) Uani 1 1 d . . .
O6 O 0.7697(14) 0.7499(18) 0.7563(9) 0.022(2) Uani 1 1 d . . .
O3 O 0.2530(16) 0.427(2) 0.6112(9) 0.028(3) Uani 1 1 d . . .
O2 O 0.1640(15) 0.5076(17) 0.4221(8) 0.020(2) Uani 1 1 d . . .
O7 O 0.4807(16) 0.5435(16) 0.7964(7) 0.019(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
Pb2 0.0163(3) 0.0149(4) 0.0159(4) 0.0004(2) 0.0029(2) 0.0001(2)
Pb1 0.0165(3) 0.0210(4) 0.0205(4) -0.0010(2) 0.0048(3) 0.0003(2)
I1 0.0113(4) 0.0143(6) 0.0127(5) -0.0010(3) 0.0032(4) -0.0006(3)
P1 0.0126(18) 0.013(2) 0.0129(19) -0.0013(13) 0.0033(15) -0.0009(13)
O5 0.032(7) 0.021(7) 0.016(6) 0.003(4) 0.006(5) 0.011(5)
O4 0.013(5) 0.026(7) 0.038(7) 0.000(5) 0.007(5) -0.005(5)
O1 0.011(5) 0.017(6) 0.019(6) -0.006(4) 0.004(4) -0.006(4)
O6 0.008(5) 0.031(7) 0.029(6) -0.011(5) 0.009(4) -0.006(5)
O3 0.021(6) 0.039(8) 0.026(6) -0.011(5) 0.012(5) -0.011(5)
O2 0.022(6) 0.017(6) 0.022(6) 0.000(5) 0.007(5) -0.009(5)
O7 0.030(6) 0.021(7) 0.010(5) -0.006(4) 0.011(5) -0.015(5)

_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
Pb2 O1 2.458(10) 3_566 ?
Pb2 O7 2.512(10) 4_575 ?
Pb2 O2 2.513(11) . ?
Pb2 O1 2.618(11) 1_565 ?
Pb2 O5 2.731(12) . ?
Pb1 O2 2.477(11) . ?
Pb1 O3 2.545(12) 3_566 ?
Pb1 O6 2.663(10) 3_666 ?
Pb1 O5 2.715(11) 4_575 ?
Pb1 O7 2.737(11) 4_565 ?
Pb1 O1 2.752(11) . ?
I1 O6 1.823(11) . ?
I1 O7 1.831(10) . ?
I1 O5 1.849(11) . ?
P1 O3 1.523(12) . ?
P1 O2 1.538(12) . ?
P1 O4 1.544(12) . ?
P1 O1 1.567(11) . ?
O5 Pb1 2.715(11) 4_676 ?
O1 Pb2 2.458(10) 3_566 ?
O1 Pb2 2.618(11) 1_545 ?
O6 Pb1 2.663(10) 3_666 ?
O3 Pb1 2.545(12) 3_566 ?
O7 Pb2 2.513(10) 4_676 ?
O7 Pb1 2.737(11) 4_666 ?

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 Pb2 O7 83.0(3) 3_566 4_575 ?
O1 Pb2 O2 77.1(4) 3_566 . ?
O7 Pb2 O2 91.3(4) 4_575 . ?
O1 Pb2 O1 68.9(4) 3_566 1_565 ?
O7 Pb2 O1 69.0(3) 4_575 1_565 ?
O2 Pb2 O1 142.2(3) . 1_565 ?
O1 Pb2 O5 80.3(4) 3_566 . ?
O7 Pb2 O5 158.7(3) 4_575 . ?
O2 Pb2 O5 97.7(3) . . ?
O1 Pb2 O5 92.6(3) 1_565 . ?
O2 Pb1 O3 74.0(4) . 3_566 ?
O2 Pb1 O6 75.1(4) . 3_666 ?
O3 Pb1 O6 148.1(4) 3_566 3_666 ?
O2 Pb1 O5 92.7(4) . 4_575 ?
O3 Pb1 O5 86.1(4) 3_566 4_575 ?
O6 Pb1 O5 87.7(4) 3_666 4_575 ?
O2 Pb1 O7 107.3(4) . 4_565 ?
O3 Pb1 O7 132.1(4) 3_566 4_565 ?
O6 Pb1 O7 65.7(3) 3_666 4_565 ?
O5 Pb1 O7 140.1(3) 4_575 4_565 ?
O2 Pb1 O1 56.2(3) . . ?
O3 Pb1 O1 80.8(4) 3_566 . ?
O6 Pb1 O1 88.5(3) 3_666 . ?
O5 Pb1 O1 148.5(3) 4_575 . ?
O7 Pb1 O1 63.9(3) 4_565 . ?
O6 I1 O7 96.3(5) . . ?
O6 I1 O5 100.4(6) . . ?
O7 I1 O5 94.6(5) . . ?
O3 P1 O2 112.5(7) . . ?
O3 P1 O4 110.5(7) . . ?
O2 P1 O4 109.9(7) . . ?
O3 P1 O1 111.3(6) . . ?
O2 P1 O1 105.6(6) . . ?
O4 P1 O1 106.7(6) . . ?
I1 O5 Pb1 123.9(6) . 4_676 ?
I1 O5 Pb2 110.3(5) . . ?
Pb1 O5 Pb2 122.2(4) 4_676 . ?
P1 O1 Pb2 135.6(6) . 3_566 ?
P1 O1 Pb2 102.5(5) . 1_545 ?
Pb2 O1 Pb2 111.1(4) 3_566 1_545 ?
P1 O1 Pb1 91.7(5) . . ?
Pb2 O1 Pb1 104.7(4) 3_566 . ?
Pb2 O1 Pb1 107.2(3) 1_545 . ?
I1 O6 Pb1 117.1(5) . 3_666 ?
P1 O3 Pb1 138.4(7) . 3_566 ?
P1 O2 Pb1 103.5(5) . . ?
P1 O2 Pb2 124.0(6) . . ?
Pb1 O2 Pb2 128.1(5) . . ?
I1 O7 Pb2 110.0(5) . 4_676 ?
I1 O7 Pb1 111.8(4) . 4_666 ?
Pb2 O7 Pb1 110.8(4) 4_676 4_666 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         3.789
_refine_diff_density_min         -3.791
_refine_diff_density_rms         0.705
