# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1544585'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br3 Pb, C5 H14 O P'
_chemical_formula_sum            'C5 H14 Br3 O P Pb'
_chemical_formula_weight         568.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   11.240(2)
_cell_length_b                   15.986(3)
_cell_length_c                   7.7734(16)
_cell_angle_alpha                90
_cell_angle_beta                 97.15(3)
_cell_angle_gamma                90
_cell_volume                     1385.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1018
_cell_measurement_theta_min      2.2891
_cell_measurement_theta_max      27.3891

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.723
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_absorpt_coefficient_mu    20.899
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4006
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9413
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.136
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3163
_reflns_number_gt                2127
_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       'CrystalClear (Rigaku Inc.,2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc.,2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc.,2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-V (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.0147P)²+7.6805P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00535(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3163
_refine_ls_number_parameters     105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0906
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_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 0.76404(4) 0.25099(3) 0.35754(5) 0.03118(16) Uani 1 1 d . . . . .
Br3 Br 0.76467(12) 0.39498(7) 0.59699(15) 0.0422(3) Uani 1 1 d . . . . .
Br1 Br 0.94795(11) 0.32415(8) 0.14503(16) 0.0490(3) Uani 1 1 d . . . . .
Br2 Br 0.58605(11) 0.16997(8) 0.57933(16) 0.0493(4) Uani 1 1 d . . . . .
P1 P 0.2225(3) 0.09353(18) 0.3321(4) 0.0390(7) Uani 1 1 d . . . . .
O1 O 0.3306(8) 0.1235(5) 0.0643(11) 0.059(2) Uani 1 1 d . . . . .
C2 C 0.2350(15) 0.0318(9) 0.5208(18) 0.086(5) Uani 1 1 d . . . . .
H2A H 0.1648 0.0391 0.5780 0.128 Uiso 1 1 calc R U . . .
H2B H 0.3046 0.0487 0.5972 0.128 Uiso 1 1 calc R U . . .
H2C H 0.2425 -0.0259 0.4901 0.128 Uiso 1 1 calc R U . . .
C1 C 0.0896(11) 0.0691(9) 0.1994(18) 0.071(4) Uani 1 1 d . . . . .
H1A H 0.0741 0.0102 0.2064 0.106 Uiso 1 1 calc R U . . .
H1B H 0.0975 0.0839 0.0817 0.106 Uiso 1 1 calc R U . . .
H1C H 0.0243 0.0998 0.2375 0.106 Uiso 1 1 calc R U . . .
C3 C 0.2278(12) 0.1999(7) 0.3914(16) 0.056(4) Uani 1 1 d . . . . .
H3A H 0.1603 0.2130 0.4509 0.085 Uiso 1 1 calc R U . . .
H3B H 0.2255 0.2339 0.2892 0.085 Uiso 1 1 calc R U . . .
H3C H 0.3006 0.2108 0.4664 0.085 Uiso 1 1 calc R U . . .
C4 C 0.3464(10) 0.0724(7) 0.2131(16) 0.045(3) Uani 1 1 d . . . . .
H4A H 0.4217 0.0854 0.2831 0.054 Uiso 1 1 calc R U . . .
H4B H 0.3471 0.0139 0.1804 0.054 Uiso 1 1 calc R U . . .
C5 C 0.4216(14) 0.1123(9) -0.0436(19) 0.078(5) Uani 1 1 d . . . . .
H5A H 0.4984 0.1224 0.0219 0.117 Uiso 1 1 calc R U . . .
H5B H 0.4095 0.1509 -0.1388 0.117 Uiso 1 1 calc R U . . .
H5C H 0.4187 0.0561 -0.0874 0.117 Uiso 1 1 calc R U . . .

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 0.0371(3) 0.0378(3) 0.0201(2) -0.00089(17) 0.00901(16) -0.00084(19)
Br3 0.0527(7) 0.0338(6) 0.0395(7) -0.0022(5) 0.0031(5) 0.0003(6)
Br1 0.0399(7) 0.0574(8) 0.0520(8) 0.0009(6) 0.0147(6) -0.0092(6)
Br2 0.0399(7) 0.0628(9) 0.0462(8) 0.0021(6) 0.0093(6) -0.0154(6)
P1 0.0416(18) 0.0346(17) 0.0422(19) 0.0007(13) 0.0100(15) 0.0030(14)
O1 0.053(6) 0.062(6) 0.067(6) 0.018(5) 0.032(5) 0.021(5)
C2 0.128(16) 0.058(10) 0.075(11) 0.018(8) 0.028(10) 0.019(10)
C1 0.038(8) 0.079(10) 0.095(12) -0.013(8) 0.004(8) -0.001(7)
C3 0.064(9) 0.046(8) 0.063(9) -0.007(6) 0.021(7) 0.009(7)
C4 0.027(6) 0.045(7) 0.062(9) -0.011(6) 0.006(6) 0.013(5)
C5 0.073(11) 0.089(12) 0.084(11) -0.012(9) 0.055(9) -0.002(9)

_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 Br3 2.9597(12) . ?
Pb1 Br2 3.0329(15) 4_565 ?
Pb1 Br1 3.0364(14) . ?
Pb1 Br2 3.0840(14) . ?
Pb1 Br3 3.0905(12) 4_565 ?
Pb1 Br1 3.0920(16) 4_566 ?
Br3 Pb1 3.0905(12) 4_566 ?
Br1 Pb1 3.0920(16) 4_565 ?
Br2 Pb1 3.0330(15) 4_566 ?
P1 C1 1.751(13) . ?
P1 C2 1.758(13) . ?
P1 C3 1.760(12) . ?
P1 C4 1.798(11) . ?
O1 C4 1.409(13) . ?
O1 C5 1.412(14) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
Br3 Pb1 Br2 94.25(4) . 4_565 ?
Br3 Pb1 Br1 95.40(4) . . ?
Br2 Pb1 Br1 83.39(4) 4_565 . ?
Br3 Pb1 Br2 85.76(4) . . ?
Br2 Pb1 Br2 99.06(5) 4_565 . ?
Br1 Pb1 Br2 177.22(4) . . ?
Br3 Pb1 Br3 177.96(4) . 4_565 ?
Br2 Pb1 Br3 84.40(4) 4_565 4_565 ?
Br1 Pb1 Br3 82.94(4) . 4_565 ?
Br2 Pb1 Br3 95.96(4) . 4_565 ?
Br3 Pb1 Br1 84.18(4) . 4_566 ?
Br2 Pb1 Br1 178.24(4) 4_565 4_566 ?
Br1 Pb1 Br1 95.95(4) . 4_566 ?
Br2 Pb1 Br1 81.64(4) . 4_566 ?
Br3 Pb1 Br1 97.15(4) 4_565 4_566 ?
Pb1 Br3 Pb1 79.92(3) . 4_566 ?
Pb1 Br1 Pb1 78.72(3) . 4_565 ?
Pb1 Br2 Pb1 78.90(3) 4_566 . ?
C1 P1 C2 109.9(8) . . ?
C1 P1 C3 111.6(6) . . ?
C2 P1 C3 109.1(7) . . ?
C1 P1 C4 108.3(6) . . ?
C2 P1 C4 109.7(6) . . ?
C3 P1 C4 108.2(6) . . ?
C4 O1 C5 112.8(10) . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 P1 106.7(7) . . ?
O1 C4 H4A 110.4 . . ?
P1 C4 H4A 110.4 . . ?
O1 C4 H4B 110.4 . . ?
P1 C4 H4B 110.4 . . ?
H4A C4 H4B 108.6 . . ?
O1 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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
C5 O1 C4 P1 -179.1(9) . . . . ?
C1 P1 C4 O1 59.9(10) . . . . ?
C2 P1 C4 O1 179.9(9) . . . . ?
C3 P1 C4 O1 -61.2(9) . . . . ?

_refine_diff_density_max         1.126
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.242

_shelx_res_file                  
;

    2.res created by SHELXL-2014/7

TITL 2 in Pc                     New: P21/c
CELL  0.71073   11.2400   15.9860    7.7734    90.000    97.150    90.000
ZERR  4           0.0020    0.0030    0.0016     0.000     0.030     0.000
LATT 1
SYMM             - X ,    0.50000 + Y ,    0.50000 - Z
SFAC C  H  Br O  P  Pb
UNIT 20 56 12 4 4 4
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 10
CONF
WGHT    0.014700    7.680500
EXTI    0.005352
FVAR       0.10589
PB1   6    0.764037    0.250994    0.357540    11.00000    0.03706    0.03780 =
         0.02006   -0.00089    0.00901   -0.00084
BR3   3    0.764674    0.394983    0.596990    11.00000    0.05270    0.03382 =
         0.03948   -0.00217    0.00309    0.00034
BR1   3    0.947948    0.324155    0.145034    11.00000    0.03989    0.05741 =
         0.05204    0.00093    0.01466   -0.00923
BR2   3    0.586053    0.169967    0.579330    11.00000    0.03992    0.06277 =
         0.04618    0.00214    0.00929   -0.01542
P1    5    0.222489    0.093532    0.332150    11.00000    0.04157    0.03456 =
         0.04216    0.00069    0.01003    0.00303
O1    4    0.330612    0.123471    0.064318    11.00000    0.05307    0.06234 =
         0.06654    0.01829    0.03242    0.02062
C2    1    0.235048    0.031825    0.520756    11.00000    0.12765    0.05799 =
         0.07497    0.01780    0.02819    0.01945
AFIX 137
H2A   2    0.164815    0.039057    0.577952    11.00000   -1.50000
H2B   2    0.304643    0.048666    0.597176    11.00000   -1.50000
H2C   2    0.242544   -0.025943    0.490126    11.00000   -1.50000
AFIX   0
C1    1    0.089592    0.069097    0.199444    11.00000    0.03769    0.07866 =
         0.09461   -0.01294    0.00371   -0.00106
AFIX 137
H1A   2    0.074086    0.010215    0.206360    11.00000   -1.50000
H1B   2    0.097521    0.083851    0.081700    11.00000   -1.50000
H1C   2    0.024288    0.099824    0.237496    11.00000   -1.50000
AFIX   0
C3    1    0.227822    0.199870    0.391417    11.00000    0.06379    0.04608 =
         0.06272   -0.00699    0.02140    0.00949
AFIX 137
H3A   2    0.160272    0.212957    0.450919    11.00000   -1.50000
H3B   2    0.225463    0.233851    0.289223    11.00000   -1.50000
H3C   2    0.300639    0.210795    0.466430    11.00000   -1.50000
AFIX   0
C4    1    0.346432    0.072396    0.213093    11.00000    0.02669    0.04528 =
         0.06197   -0.01062    0.00553    0.01331
AFIX  23
H4A   2    0.421706    0.085425    0.283121    11.00000   -1.20000
H4B   2    0.347149    0.013856    0.180402    11.00000   -1.20000
AFIX   0
C5    1    0.421571    0.112338   -0.043633    11.00000    0.07283    0.08891 =
         0.08439   -0.01210    0.05455   -0.00163
AFIX 137
H5A   2    0.498394    0.122401    0.021917    11.00000   -1.50000
H5B   2    0.409461    0.150928   -0.138828    11.00000   -1.50000
H5C   2    0.418687    0.056118   -0.087366    11.00000   -1.50000
AFIX   0
HKLF 4

REM  2 in Pc                     New: P21/c
REM R1 =  0.0526 for    2127 Fo > 4sig(Fo)  and  0.0894 for all    3163 data
REM    105 parameters refined using      0 restraints

END

WGHT      0.0147      7.6696

REM Highest difference peak  1.126,  deepest hole -1.417,  1-sigma level  0.242
Q1    1   0.9378  0.2552  0.2440  11.00000  0.05    1.13
Q2    1   0.8030  0.3002  0.3123  11.00000  0.05    1.06
Q3    1   0.7170  0.2120  0.3916  11.00000  0.05    1.03
Q4    1   0.6129  0.0874  0.5323  11.00000  0.05    0.97
Q5    1   0.8582  0.2565  0.2832  11.00000  0.05    0.95
Q6    1   0.8002  0.2000  0.3087  11.00000  0.05    0.91
Q7    1   0.5031  0.0108  0.0035  11.00000  0.05    0.87
Q8    1   0.4044  0.1224  0.5064  11.00000  0.05    0.81
Q9    1   0.7528  0.2522  0.4991  11.00000  0.05    0.80
Q10   1   0.8554  0.3204  0.0426  11.00000  0.05    0.79
;
_shelx_res_checksum              78389
####################################################################### 
# 
# 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_2C
_database_code_depnum_ccdc_archive 'CCDC 1544586'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C5 O P), Br3 Pb1'
_chemical_formula_sum            'C5 Br3 O P Pb'
_chemical_formula_weight         553.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   10.27(3)
_cell_length_b                   17.79(5)
_cell_length_c                   7.95(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.0340(12)
_cell_angle_gamma                90
_cell_volume                     1452(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    418(2)
_cell_measurement_reflns_used    1018
_cell_measurement_theta_min      2.2891
_cell_measurement_theta_max      27.3891

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.533
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_absorpt_coefficient_mu    19.939
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4006
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      418(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1285
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.2891
_diffrn_reflns_theta_max         27.3891
_diffrn_reflns_theta_full        24.927
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1285
_reflns_number_gt                530
_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       'CrystalClear (Rigaku Inc.,2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc.,2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc.,2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-V (Sheldrick, 2014)'
_computing_publication_material  Solid
_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)+(0.2000P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1285
_refine_ls_number_parameters     74
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.3454
_refine_ls_R_factor_gt           0.2261
_refine_ls_wR_factor_ref         0.5998
_refine_ls_wR_factor_gt          0.5483
_refine_ls_goodness_of_fit_ref   1.713
_refine_ls_restrained_S_all      1.849
_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 0.5000 0.5000 0.0000 0.144(3) Uani 1 2 d S U P . .
Br2 Br 0.5000 0.3675(7) 0.2500 0.199(6) Uani 1 2 d S TU P . .
Br1 Br 0.3052(7) 0.5632(4) 0.2488(9) 0.144(3) Uani 1 1 d . U . . .
P1 P -0.015(6) 0.328(4) 0.509(4) 0.52(6) Uani 0.5 1 d D U P . .
C4 C -0.004(8) 0.396(4) 0.430(3) 0.52(6) Uani 0.5 1 d D U P . .
C2 C 0.110(7) 0.306(6) 0.548(8) 0.52(6) Uani 0.5 1 d D U P . .
C1 C -0.060(9) 0.278(5) 0.390(10) 0.52(6) Uani 0.5 1 d D U P . .
C3 C -0.088(9) 0.331(7) 0.639(6) 0.52(6) Uani 0.5 1 d D U P . .
O1 O 0.0000 0.371(6) 0.2500 0.52(6) Uani 1 2 d DS TU P . .
C5 C 0.118(6) 0.323(7) 0.273(8) 0.52(6) Uani 0.5 1 d D U 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 0.145(4) 0.170(4) 0.117(3) 0.0012(18) -0.009(2) 0.006(2)
Br2 0.282(16) 0.132(8) 0.183(10) 0.000 -0.002(11) 0.000
Br1 0.145(4) 0.170(4) 0.117(3) 0.0012(18) -0.009(2) 0.006(2)
P1 0.51(8) 0.52(8) 0.54(7) 0.00(2) -0.01(5) -0.01(4)
C4 0.50(8) 0.52(8) 0.54(7) -0.003(19) -0.01(6) 0.00(3)
C2 0.51(8) 0.52(10) 0.54(7) 0.00(6) -0.01(6) -0.01(6)
C1 0.51(8) 0.52(8) 0.54(7) 0.00(3) -0.01(6) -0.01(4)
C3 0.51(9) 0.52(10) 0.54(7) -0.01(4) -0.01(6) -0.02(7)
O1 0.50(8) 0.52(8) 0.54(7) 0.000 -0.01(6) 0.000
C5 0.50(8) 0.51(9) 0.54(7) 0.00(3) -0.01(6) 0.00(2)

_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 Br1 3.030(8) . ?
Pb1 Br1 3.030(8) 5_665 ?
Pb1 Br1 3.041(9) 6_565 ?
Pb1 Br1 3.041(9) 2_655 ?
Pb1 Br2 3.083(11) 5_665 ?
Pb1 Br2 3.083(11) . ?
Br2 Pb1 3.083(11) 2_655 ?
Br1 Pb1 3.041(9) 2_655 ?
P1 C3 1.281(16) . ?
P1 C2 1.375(18) . ?
P1 C1 1.373(18) . ?
P1 C4 1.373(18) . ?
P1 C5 2.49(9) 2 ?
P1 O1 2.200(7) . ?
P1 C5 2.319(17) . ?
C4 O1 1.50(2) . ?
C1 C5 1.64(15) 2 ?
O1 C5 1.50(2) 2 ?
O1 C5 1.50(2) . ?
O1 C4 1.50(2) 2 ?
O1 P1 2.200(7) 2 ?
C5 C1 1.64(15) 2 ?
C5 P1 2.49(9) 2 ?
C5 C5 2.46(13) 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
Br1 Pb1 Br1 180.0 . 5_665 ?
Br1 Pb1 Br1 97.5(3) . 6_565 ?
Br1 Pb1 Br1 82.5(3) 5_665 6_565 ?
Br1 Pb1 Br1 82.5(3) . 2_655 ?
Br1 Pb1 Br1 97.5(3) 5_665 2_655 ?
Br1 Pb1 Br1 180.0 6_565 2_655 ?
Br1 Pb1 Br2 97.9(2) . 5_665 ?
Br1 Pb1 Br2 82.1(2) 5_665 5_665 ?
Br1 Pb1 Br2 81.9(2) 6_565 5_665 ?
Br1 Pb1 Br2 98.1(2) 2_655 5_665 ?
Br1 Pb1 Br2 82.1(2) . . ?
Br1 Pb1 Br2 97.9(2) 5_665 . ?
Br1 Pb1 Br2 98.1(2) 6_565 . ?
Br1 Pb1 Br2 81.9(2) 2_655 . ?
Br2 Pb1 Br2 180.0 5_665 . ?
Pb1 Br2 Pb1 80.2(3) 2_655 . ?
Pb1 Br1 Pb1 81.8(3) . 2_655 ?
C3 P1 C2 112.2(13) . . ?
C3 P1 C1 112.3(13) . . ?
C2 P1 C1 106.5(12) . . ?
C3 P1 C4 112.3(13) . . ?
C2 P1 C4 106.5(12) . . ?
C1 P1 C4 106.6(12) . . ?
C3 P1 C5 119(3) . 2 ?
C2 P1 C5 126(4) . 2 ?
C1 P1 C5 38(4) . 2 ?
C4 P1 C5 70(3) . 2 ?
C3 P1 O1 141.4(14) . . ?
C2 P1 O1 104.3(10) . . ?
C1 P1 O1 66.8(17) . . ?
C4 P1 O1 42.2(9) . . ?
C5 P1 O1 36.7(12) 2 . ?
C3 P1 C5 179.9(17) . . ?
C2 P1 C5 67.7(7) . . ?
C1 P1 C5 67.7(7) . . ?
C4 P1 C5 67.7(7) . . ?
C5 P1 C5 61(3) 2 . ?
O1 P1 C5 38.7(6) . . ?
P1 C4 O1 99.8(13) . . ?
C5 C1 P1 111(5) 2 . ?
C5 O1 C5 110(8) 2 . ?
C5 O1 C4 106(4) 2 . ?
C5 O1 C4 94.4(12) . . ?
C5 O1 C4 94.4(12) 2 2 ?
C5 O1 C4 106(4) . 2 ?
C4 O1 C4 145(5) . 2 ?
C5 O1 P1 74.9(8) 2 2 ?
C5 O1 P1 82(4) . 2 ?
C4 O1 P1 176(4) . 2 ?
C4 O1 P1 38.0(7) 2 2 ?
C5 O1 P1 82(4) 2 . ?
C5 O1 P1 74.9(8) . . ?
C4 O1 P1 38.0(7) . . ?
C4 O1 P1 176(4) 2 . ?
P1 O1 P1 139(5) 2 . ?
C1 C5 O1 83(5) 2 . ?
C1 C5 P1 31.0(14) 2 2 ?
O1 C5 P1 61(3) . 2 ?
C1 C5 C5 61(4) 2 2 ?
O1 C5 C5 35(4) . 2 ?
P1 C5 C5 56(2) 2 2 ?
C1 C5 P1 117(8) 2 . ?
O1 C5 P1 66.4(6) . . ?
P1 C5 P1 118(2) 2 . ?
C5 C5 P1 62.6(18) 2 . ?

_refine_diff_density_max         5.141
_refine_diff_density_min         -3.978
_refine_diff_density_rms         0.445

_shelx_res_file                  
;

    2C.res created by SHELXL-2014/7

TITL 2C in C2/c
CELL 0.71073  10.2720  17.7917   7.9472  90.000  90.034  90.000
ZERR   4.00   0.0271   0.0476   0.0204   0.000   0.0012   0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C  O  P  Br Pb
UNIT 20  4  4  12  4
OMIT   0.00  50.00
L.S. 99
ACTA
BOND
FMAP 2
PLAN 10
delu
simu
eadp br1 pb1
isor c1  c2  c3  c4
dfix 2.8 0.05 p1 c5
dfix 2.2 0.005 c1 c2 p1 o1 c1 c3 c1 c4 c2 c3 c2 c4 c3 c4 c5 c4 c5 c1 c5 c2
dfix 1.5 0.02 p1 c1
dfix 1.5 0.02 p1 c2
dfix 1.5 0.02 p1 c3
dfix 1.5 0.02 p1 c4 c4 o1 o1 c5
temp 145
WGHT    0.200000
FVAR       0.18403
PB1   5    0.500000    0.500000    0.000000    10.50000    0.14499    0.17017 =
         0.11682    0.00117   -0.00902    0.00640
BR2   4    0.500000    0.367474    0.250000    10.50000    0.28231    0.13207 =
         0.18252    0.00000   -0.00232    0.00000
BR1   4    0.305211    0.563191    0.248785    11.00000    0.14499    0.17017 =
         0.11682    0.00117   -0.00902    0.00640
P1    3   -0.014592    0.328091    0.508872    10.50000    0.50872    0.51645 =
         0.54076   -0.00425   -0.01037   -0.00672
C4    1   -0.003836    0.396498    0.430045    10.50000    0.50363    0.51679 =
         0.54412   -0.00250   -0.00815   -0.00325
C2    1    0.109953    0.305710    0.547665    10.50000    0.51191    0.51836 =
         0.54265    0.00021   -0.01432   -0.00526
C1    1   -0.060101    0.278410    0.390362    10.50000    0.51015    0.51899 =
         0.53603   -0.00331   -0.00883   -0.00759
C3    1   -0.087948    0.331010    0.639061    10.50000    0.51029    0.52084 =
         0.54007   -0.01023   -0.00996   -0.02031
O1    2    0.000000    0.371095    0.250000    10.50000    0.50029    0.51539 =
         0.54337    0.00000   -0.00949    0.00000
C5    1    0.118381    0.322747    0.273450    10.50000    0.50144    0.51326 =
         0.54273   -0.00049   -0.01189   -0.00073
HKLF 4

REM  2C in C2/c
REM R1 =  0.2261 for     530 Fo > 4sig(Fo)  and  0.3454 for all    1285 data
REM     74 parameters refined using    101 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  5.141,  deepest hole -3.978,  1-sigma level  0.445
Q1    1   0.3820  0.6121  0.2796  11.00000  0.05    1.47
Q2    1   0.5000  0.6274  0.2500  10.50000  0.05    1.24
Q3    1   0.2905  0.5418  0.3697  11.00000  0.05    1.11
Q4    1   0.2795  0.5425  0.1311  11.00000  0.05    1.09
Q5    1   0.2645  0.5295  0.1508  11.00000  0.05    1.08
Q6    1   0.2639  0.5016  0.2308  11.00000  0.05    1.03
Q7    1   0.3160  0.5899  0.1309  11.00000  0.05    1.02
Q8    1   0.6284  0.4079  0.2423  11.00000  0.05    0.99
Q9    1   0.3421  0.6025  0.1447  11.00000  0.05    0.99
Q10   1   0.0022  0.3319  0.1736  11.00000  0.05    0.99
;
_shelx_res_checksum              6299

# start Validation Reply Form
_vrf_PLAT082_2C                  
;
PROBLEM: High R1 Value ..................................       0.23 Report
RESPONSE: Due to the too high temperature,we could not obtain high-quality diffraction data.
;
_vrf_PLAT084_2C                  
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.60 Report
RESPONSE: Due to the too high temperature,we could not obtain high-quality diffraction data.
;
# start Validation Reply Form
_vrf_PLAT972_2C                  
;
PROBLEM: Check Calcd Residual Density  0.06A From     Br1      -4.13 eA-3  
RESPONSE: The diffraction in the high 2-theta region is too weak.
;
_vrf_PLAT973_2C                  
;
PROBLEM: Check Calcd Positive Residual Density on     Pb1       6.13 eA-3  
RESPONSE: The diffraction in the high 2-theta region is too weak.
;
_vrf_PLAT920_2C                  
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       2.46 Degree
RESPONSE: The diffraction in the high 2-theta region is too weak.
;
# end Validation Reply Form




