# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_01
_database_code_depnum_ccdc_archive 'CCDC 1946683'
loop_
_audit_author_name
_audit_author_address
'Qi Wu'
;Hubei Normal University
China
;
_audit_update_record             
;
2019-08-12 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-08-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(F12 Pb7), 2(Cl)'
_chemical_formula_sum            'Cl2 F12 Pb7'
_chemical_formula_weight         1749.20
_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
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   10.236
_cell_length_b                   10.236
_cell_length_c                   3.971
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     360.3
_cell_formula_units_Z            1.00002
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.040
_shelx_estimated_absorpt_T_min   0.024
_exptl_absorpt_coefficient_mu    81.958
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    8.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1760
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         2.298
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.988
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                738
_reflns_number_total             773
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.873
_refine_diff_density_min         -10.194
_refine_diff_density_rms         1.164
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         773
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.148
_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)+(0.0555P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0970
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.52(7)
 0.48(7)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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 0.000000 0.000000 0.500000 0.0393(7) Uani 1 6 d S T P . .
Pb2 Pb 0.89288(13) 0.58512(14) 0.500000 0.0191(3) Uani 1 2 d S T P . .
Pb3 Pb 0.11397(12) 0.40051(13) 0.000000 0.0187(3) Uani 1 2 d S T P . .
Cl1 Cl 0.666667 0.333333 0.000000 0.023(3) Uani 1 6 d S T P . .
Cl2 Cl 0.333333 0.666667 0.500000 0.021(3) Uani 1 6 d S T P . .
F1 F 0.388(2) 0.425(2) 0.000000 0.018(4) Uani 1 2 d S T P . .
F2 F 0.164(2) 0.280(2) 0.500000 0.023(4) Uani 1 2 d S T P . .
F3 F 0.432(2) 0.045(3) 0.500000 0.021(4) Uani 1 2 d S T P . .
F4 F 0.211(3) 0.081(3) 0.000000 0.038(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 0.0184(7) 0.0184(7) 0.081(2) 0.000 0.000 0.0092(3)
Pb2 0.0164(6) 0.0201(6) 0.0198(6) 0.000 0.000 0.0084(5)
Pb3 0.0184(7) 0.0189(6) 0.0189(6) 0.000 0.000 0.0093(5)
Cl1 0.023(4) 0.023(4) 0.022(7) 0.000 0.000 0.012(2)
Cl2 0.022(4) 0.022(4) 0.020(6) 0.000 0.000 0.011(2)
F1 0.015(9) 0.025(10) 0.022(10) 0.000 0.000 0.015(8)
F2 0.022(10) 0.023(9) 0.018(7) 0.000 0.000 0.008(8)
F3 0.011(8) 0.024(9) 0.020(11) 0.000 0.000 0.002(7)
F4 0.047(15) 0.027(12) 0.048(13) 0.000 0.000 0.025(12)

_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 F2 2.49(2) 2 ?
Pb1 F2 2.49(2) 3 ?
Pb1 F2 2.49(2) . ?
Pb2 F1 2.408(10) 3_665 ?
Pb2 F1 2.408(10) 3_666 ?
Pb2 F2 2.43(2) 3_665 ?
Pb2 F3 2.41(2) 2_655 ?
Pb3 F1 2.688(18) . ?
Pb3 F1 2.645(19) 3_565 ?
Pb3 F2 2.524(13) . ?
Pb3 F2 2.524(13) 1_554 ?
Pb3 F3 2.528(13) 2 ?
Pb3 F3 2.528(13) 2_554 ?
Pb3 F4 2.47(2) 2 ?

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
F2 Pb1 F2 120.001(1) 2 . ?
F2 Pb1 F2 119.999(1) 2 3 ?
F2 Pb1 F2 120.000(1) . 3 ?
F1 Pb2 F1 111.1(7) 3_666 3_665 ?
F1 Pb2 F2 71.5(5) 3_666 3_665 ?
F1 Pb2 F2 71.5(5) 3_665 3_665 ?
F3 Pb2 F1 72.0(5) 2_655 3_666 ?
F3 Pb2 F1 72.0(5) 2_655 3_665 ?
F3 Pb2 F2 112.6(7) 2_655 3_665 ?
F1 Pb3 F1 130.2(6) 3_565 . ?
F2 Pb3 F1 128.1(4) . 3_565 ?
F2 Pb3 F1 65.6(5) . . ?
F2 Pb3 F1 128.1(4) 1_554 3_565 ?
F2 Pb3 F1 65.6(5) 1_554 . ?
F2 Pb3 F2 103.7(8) . 1_554 ?
F2 Pb3 F3 68.9(6) . 2 ?
F2 Pb3 F3 151.1(7) 1_554 2 ?
F2 Pb3 F3 68.9(6) 1_554 2_554 ?
F2 Pb3 F3 151.1(7) . 2_554 ?
F3 Pb3 F1 128.2(4) 2_554 . ?
F3 Pb3 F1 66.3(5) 2 3_565 ?
F3 Pb3 F1 128.2(4) 2 . ?
F3 Pb3 F1 66.3(5) 2_554 3_565 ?
F3 Pb3 F3 103.5(8) 2_554 2 ?
F4 Pb3 F1 109.1(7) 2 . ?
F4 Pb3 F1 120.7(7) 2 3_565 ?
F4 Pb3 F2 72.6(6) 2 1_554 ?
F4 Pb3 F2 72.6(6) 2 . ?
F4 Pb3 F3 78.6(5) 2 2 ?
F4 Pb3 F3 78.6(5) 2 2_554 ?
Pb2 F1 Pb2 111.1(7) 2_654 2_655 ?
Pb2 F1 Pb3 108.9(5) 2_654 2_665 ?
Pb2 F1 Pb3 109.1(5) 2_655 . ?
Pb2 F1 Pb3 108.9(5) 2_655 2_665 ?
Pb2 F1 Pb3 109.1(5) 2_654 . ?
Pb3 F1 Pb3 109.8(6) 2_665 . ?
Pb1 F2 Pb3 112.1(5) . 1_556 ?
Pb1 F2 Pb3 112.1(5) . . ?
Pb2 F2 Pb1 101.6(8) 2_655 . ?
Pb2 F2 Pb3 113.8(5) 2_655 . ?
Pb2 F2 Pb3 113.8(5) 2_655 1_556 ?
Pb3 F2 Pb3 103.7(8) . 1_556 ?
Pb2 F3 Pb3 112.9(6) 3_665 3_556 ?
Pb2 F3 Pb3 112.9(6) 3_665 3 ?
Pb3 F3 Pb3 103.5(8) 3 3_556 ?

_shelx_res_file                  
;
TITL 02
    01.res
    created by SHELXL-2016/6 at 13:14:29 on 05-Aug-2019
CELL 0.71075 10.2356 10.2356 3.9708 90 90 120
ZERR 1.00002 0 0 0 0 0 0
LATT -1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +X,+Y,-Z
SYMM -Y,+X-Y,-Z
SYMM +Y-X,-X,-Z
SFAC Cl F Pb
UNIT 2 12 7

L.S. 99
PLAN  20
SIZE 0.11 0.13 0.18
fmap 2 53
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\01.hkl">
REM </olex2.extras>

WGHT    0.055500
BASF   0.47796
FVAR       0.07839
PB1   3    0.000000    0.000000    0.500000    10.16667    0.01838    0.01838 =
         0.08125    0.00000    0.00000    0.00919
PB2   3    0.892876    0.585124    0.500000    10.50000    0.01642    0.02007 =
         0.01978    0.00000    0.00000    0.00842
PB3   3    0.113967    0.400512    0.000000    10.50000    0.01838    0.01886 =
         0.01893    0.00000    0.00000    0.00930
CL1   1    0.666667    0.333333    0.000000    10.16667    0.02330    0.02330 =
         0.02188    0.00000    0.00000    0.01165
CL2   1    0.333333    0.666667    0.500000    10.16667    0.02170    0.02170 =
         0.02016    0.00000    0.00000    0.01085
F1    2    0.388168    0.425417    0.000000    10.50000    0.01511    0.02477 =
         0.02156    0.00000    0.00000    0.01537
F2    2    0.164337    0.279758    0.500000    10.50000    0.02243    0.02298 =
         0.01795    0.00000    0.00000    0.00762
F3    2    0.432285    0.045074    0.500000    10.50000    0.01076    0.02395 =
         0.01965    0.00000    0.00000    0.00232
F4    2    0.211497    0.080728    0.000000    10.50000    0.04709    0.02745 =
         0.04809    0.00000    0.00000    0.02508
HKLF 4




REM  02
REM R1 =  0.0411 for     738 Fo > 4sig(Fo)  and  0.0431 for all     773 data
REM     44 parameters refined using      0 restraints

END

WGHT      0.0556      0.0000

REM Highest difference peak  1.873,  deepest hole-10.194,  1-sigma level  1.164
Q1    1   0.5142  0.1469  0.7517  11.00000  0.05    1.87
Q2    1   0.2212  0.2015 -0.2501  11.00000  0.05    1.81
Q3    1   0.2922  0.3562  0.2604  11.00000  0.05    1.79
Q4    1   0.4384  0.0612  0.2921  11.00000  0.05    1.78
Q5    1   0.3333  0.6667  0.7221  10.33333  0.05    1.74
Q6    1   0.1166  0.2191  0.2701  11.00000  0.05    1.73
Q7    1   0.4843  0.0421  0.7775  11.00000  0.05    1.72
Q8    1   0.3839  0.4381  0.2342  11.00000  0.05    1.67
Q9    1   0.2442  0.6543  0.2715  11.00000  0.05    1.66
Q10   1   0.3469 -0.0078  0.6072  11.00000  0.05    1.57
Q11   1   0.2283  0.0019 -0.2795  11.00000  0.05    1.56
Q12   1   0.2414  0.3017  0.5000  10.50000  0.05    1.55
Q13   1   0.0995 -0.1223  0.0000  10.50000  0.05    1.55
Q14   1   0.6609  0.4000 -0.2453  11.00000  0.05    1.53
Q15   1   0.3960  0.0756  0.7561  11.00000  0.05    1.53
Q16   1   0.0698  0.3130  0.5000  10.50000  0.05    1.51
Q17   1   0.2347  0.0962 -0.2264  11.00000  0.05    1.51
Q18   1   0.4173  0.5407  0.2581  11.00000  0.05    1.48
Q19   1   0.4936  0.0141  0.5000  10.50000  0.05    1.47
Q20   1   0.6667  0.3333  0.2176  10.33333  0.05    1.45
;
_shelx_res_checksum              4768
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.52(7)
2 0.48(7)

