# 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_190713_1_mo
_database_code_depnum_ccdc_archive 'CCDC 1811892'
loop_
_audit_author_name
_audit_author_address
'Yue-Qiao Hu'
;Baoji University of Arts and Sciences
China
;
_audit_update_record             
;
2019-07-15 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_audit_creation_date             2019-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            1
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, C4 H14 N2 S2, H2 O'
_chemical_formula_sum            'C4 H16 Br5 N2 O Pb S2'
_chemical_formula_weight         779.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C4H17Br5N2OPbS2
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.0824(3)
_cell_length_b                   8.3838(2)
_cell_length_c                   10.9546(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.184(4)
_cell_angle_gamma                90
_cell_volume                     897.75(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6529
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      2.4550
_shelx_estimated_absorpt_T_max   0.647
_shelx_estimated_absorpt_T_min   0.317
_exptl_absorpt_coefficient_mu    20.739
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   R(int)
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.882
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             702
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 5 0.0104
2 0 -5 0.0124
0 -1 0 0.0386
0 1 0 0.0336
-5 0 -1 0.0149
5 0 1 0.0149

_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.023
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9974 0.0004 4.9913 0.0597 -0.1409 -0.2917
1.9974 -0.0004 -4.9913 -0.0597 0.1409 0.2917
0.0001 -0.9992 -0.0000 -0.0480 0.0583 -0.0380
-0.0001 0.9992 0.0000 0.0480 -0.0583 0.0380
-4.9972 -0.0013 -0.9987 -0.3069 -0.2284 0.0371
4.9972 0.0013 0.9987 0.3069 0.2284 -0.0371

_exptl_transmission_factor_max   0.649
_exptl_transmission_factor_min   0.348
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9646
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.700
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.870
_diffrn_reflns_theta_min         2.462
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  15.00   0.50    2.00    --    4.91 -86.00  70.00   68
  2  ω    -18.00  28.00   0.50    2.00    --   -6.94 -99.00  30.00   92
  3  ω    -20.00  28.00   0.50    2.00    --   -6.94 -99.00   0.00   96
  4  ω    -21.00  24.00   0.50    2.00    --    4.91 -99.00-150.00   90
  5  ω    -66.00  21.00   0.50    2.00    --    4.91 -57.00 -30.00  174
  6  ω    -11.00  40.00   0.50    2.00    --    4.91  86.00-171.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0546462000
_diffrn_orient_matrix_UB_12      0.0480283000
_diffrn_orient_matrix_UB_13      0.0338244000
_diffrn_orient_matrix_UB_21      0.0475630000
_diffrn_orient_matrix_UB_22      -0.0583532000
_diffrn_orient_matrix_UB_23      -0.0091855000
_diffrn_orient_matrix_UB_31      0.0039375000
_diffrn_orient_matrix_UB_32      0.0380177000
_diffrn_orient_matrix_UB_33      -0.0568624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.855
_reflns_Friedel_fraction_max     0.581
_reflns_number_gt                3686
_reflns_number_total             3953
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.875
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 
;
 Flack x determined using 1363 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      0.993
_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)+(0.0163P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0471
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1F,H1G)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E), C3(H3A,H3B), C4(H4A,H4B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.87469(3) 0.62046(4) 0.80179(3) 0.00895(7) Uani 1 1 d . . . . .
Br1 Br 0.77098(9) 0.86893(9) 0.61729(9) 0.0162(2) Uani 1 1 d . . . . .
Br2 Br 1.01672(9) 0.84523(9) 1.01173(10) 0.0155(2) Uani 1 1 d . . . . .
Br3 Br 1.14033(8) 0.60927(15) 0.70829(8) 0.01712(18) Uani 1 1 d . . . . .
Br4 Br 0.72439(9) 0.37816(9) 0.61719(9) 0.0150(2) Uani 1 1 d . . . . .
Br5 Br 0.63080(8) 0.68741(10) 0.88744(8) 0.01391(18) Uani 1 1 d . . . . .
S1 S 0.45105(19) 0.1601(2) 0.7095(2) 0.0152(5) Uani 1 1 d . . . . .
S2 S 0.3395(2) -0.0168(2) 0.7660(2) 0.0145(4) Uani 1 1 d . . . . .
N1 N 0.7403(6) 0.0749(7) 0.8815(7) 0.0157(15) Uani 1 1 d . . . . .
H1A H 0.790372 -0.000055 0.929059 0.019 Uiso 1 1 calc GR . . . .
H1B H 0.794300 0.154464 0.869906 0.019 Uiso 1 1 calc GR . . . .
H1C H 0.698353 0.033349 0.807281 0.019 Uiso 1 1 calc GR . . . .
N2 N 0.0624(7) 0.0030(8) 0.5643(7) 0.0175(16) Uani 1 1 d . . . . .
H2A H 0.028676 -0.075765 0.602064 0.021 Uiso 1 1 calc GR . . . .
H2B H 0.137357 -0.030583 0.542901 0.021 Uiso 1 1 calc GR . . . .
H2C H 0.000267 0.032963 0.495483 0.021 Uiso 1 1 calc GR . . . .
C1 C 0.6367(8) 0.1362(13) 0.9451(8) 0.0151(16) Uani 1 1 d . . . . .
H1D H 0.682056 0.191684 1.021652 0.018 Uiso 1 1 calc R . . . .
H1E H 0.585724 0.047633 0.968040 0.018 Uiso 1 1 calc R . . . .
C2 C 0.5391(8) 0.2491(9) 0.8588(8) 0.0138(17) Uani 1 1 d . . . . .
H2D H 0.590123 0.341322 0.842145 0.017 Uiso 1 1 calc R . . . .
H2E H 0.471572 0.286228 0.901862 0.017 Uiso 1 1 calc R . . . .
C3 C 0.1832(8) 0.0861(10) 0.7782(8) 0.019(2) Uani 1 1 d . . . . .
H3A H 0.129009 0.014721 0.816126 0.022 Uiso 1 1 calc R . . . .
H3B H 0.207692 0.177613 0.833285 0.022 Uiso 1 1 calc R . . . .
C4 C 0.0976(8) 0.1417(12) 0.6524(8) 0.0174(19) Uani 1 1 d . . . . .
H4A H 0.014289 0.191070 0.663514 0.021 Uiso 1 1 calc R . . . .
H4B H 0.147854 0.220618 0.617109 0.021 Uiso 1 1 calc R . . . .
O1 O 0.4350(6) 0.6127(11) 0.6032(7) 0.0350(16) Uani 1 1 d . . . . .
H1F H 0.362235 0.578845 0.620353 0.052 Uiso 1 1 d G . . . .
H1G H 0.408371 0.687417 0.550402 0.052 Uiso 1 1 d G . . . .


_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 2.9124(9) . ?
Pb1 Br2 3.0984(10) 2_747 ?
Pb1 Br2 3.0457(10) . ?
Pb1 Br3 3.0945(9) . ?
Pb1 Br4 3.0017(9) . ?
Pb1 Br5 2.8936(9) . ?
S1 S2 2.047(3) . ?
S1 C2 1.819(8) . ?
S2 C3 1.830(8) . ?
N1 C1 1.483(11) . ?
N2 C4 1.497(11) . ?
C1 C2 1.517(12) . ?
C3 C4 1.509(12) . ?

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 Br2 95.96(3) . . ?
Br1 Pb1 Br2 177.43(3) . 2_747 ?
Br1 Pb1 Br3 89.12(3) . . ?
Br1 Pb1 Br4 88.88(2) . . ?
Br2 Pb1 Br2 86.454(8) . 2_747 ?
Br2 Pb1 Br3 89.07(3) . . ?
Br3 Pb1 Br2 90.06(3) . 2_747 ?
Br4 Pb1 Br2 88.78(3) . 2_747 ?
Br4 Pb1 Br2 173.57(3) . . ?
Br4 Pb1 Br3 95.25(3) . . ?
Br5 Pb1 Br1 84.10(3) . . ?
Br5 Pb1 Br2 85.11(3) . . ?
Br5 Pb1 Br2 96.99(3) . 2_747 ?
Br5 Pb1 Br3 170.55(3) . . ?
Br5 Pb1 Br4 91.20(2) . . ?
Pb1 Br2 Pb1 169.54(3) . 2_757 ?
C2 S1 S2 102.1(3) . . ?
C3 S2 S1 103.1(3) . . ?
N1 C1 C2 110.3(7) . . ?
C1 C2 S1 113.8(6) . . ?
C4 C3 S2 112.9(6) . . ?
N2 C4 C3 109.9(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.834
_oxdiff_exptl_absorpt_empirical_full_min 0.512
####################################################################### 
# 
# 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_pbbr-2d-20190713
_database_code_depnum_ccdc_archive 'CCDC 1811893'
loop_
_audit_author_name
_audit_author_address
'Yue-Qiao Hu'
;Baoji University of Arts and Sciences
China
;
_audit_update_record             
;
2019-07-15 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_audit_creation_date             2019-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            2
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.15(Br16 Pb4), 0.62(C4 H14 N2 S2)'
_chemical_formula_sum            'C2.46 H8.62 Br2.46 N1.23 Pb0.62 S1.23'
_chemical_formula_weight         419.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         C4H14Br4N2PbS2
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   11.3898(3)
_cell_length_b                   11.6104(3)
_cell_length_c                   22.8884(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.983(2)
_cell_angle_gamma                90
_cell_volume                     3026.32(14)
_cell_formula_units_Z            13
_cell_measurement_reflns_used    7311
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.8670
_cell_measurement_theta_min      2.4900
_shelx_estimated_absorpt_T_max   0.398
_shelx_estimated_absorpt_T_min   0.218
_exptl_absorpt_coefficient_mu    21.956
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   R(int)
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 5 -1 0.0278
-5 -5 1 0.0328
0 0 1 0.0010
0 0 -1 0.0407
-4 5 -1 0.0306
4 -5 1 0.0516

_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.042
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.9950 4.9971 -0.9814 0.0137 0.0221 0.4355
-4.9950 -4.9971 0.9814 -0.0137 -0.0221 -0.4355
0.0000 0.0001 0.9994 -0.0291 -0.0106 -0.0003
-0.0000 -0.0001 -0.9994 0.0291 0.0106 0.0003
-3.9964 4.9973 -0.9860 -0.1020 0.3816 0.0221
3.9964 -4.9973 0.9860 0.1020 -0.3816 -0.0221

_exptl_transmission_factor_max   0.451
_exptl_transmission_factor_min   0.242
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12759
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.890
_diffrn_reflns_theta_min         2.505
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  77.00   0.50    3.00    --    4.91  63.00  -0.00  180
  2  ω    -18.00  33.00   0.50    3.00    --    4.91 -99.00-180.00  102
  3  ω    -11.00  19.00   0.50    3.00    --   -7.10 -99.00-150.00   60
  4  ω    -60.00  21.00   0.50    3.00    --    4.91 -63.00-137.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0128839000
_diffrn_orient_matrix_UB_12      -0.0158598000
_diffrn_orient_matrix_UB_13      -0.0291339000
_diffrn_orient_matrix_UB_21      -0.0399693000
_diffrn_orient_matrix_UB_22      0.0422992000
_diffrn_orient_matrix_UB_23      -0.0105842000
_diffrn_orient_matrix_UB_31      0.0459865000
_diffrn_orient_matrix_UB_32      0.0411240000
_diffrn_orient_matrix_UB_33      -0.0003449000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3369
_reflns_number_total             3766
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0209
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0191P)²+3.7890P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0442
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(HF,HG), C1(HH,HI), C3(HJ,HK), C2(HL,HM)
2.b Idealised Me refined as rotating group:
 N1(H,HA,HB), N2(HC,HD,HE)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.74191(2) 0.59821(2) 0.75484(2) 0.00969(4) Uani 1 1 d . . . . .
Br1 Br 0.81833(3) 0.35362(3) 0.75501(2) 0.01330(8) Uani 1 1 d . . . . .
Br3 Br 1.000000 0.65303(4) 0.750000 0.01421(10) Uani 1 2 d S T P . .
Br4 Br 0.74656(3) 0.57327(3) 0.88985(2) 0.01371(8) Uani 1 1 d . . . . .
Br5 Br 0.500000 0.51359(4) 0.750000 0.01631(11) Uani 1 2 d S T P . .
Br2 Br 0.75176(3) 0.59108(3) 0.62721(2) 0.01422(8) Uani 1 1 d . . . . .
S1 S 0.41157(9) 0.30926(8) 0.50680(4) 0.01730(19) Uani 1 1 d . . . . .
S2 S 0.47705(9) 0.14529(7) 0.50636(4) 0.01530(18) Uani 1 1 d . . . . .
N1 N 0.4094(3) 0.3360(2) 0.64263(13) 0.0138(6) Uani 1 1 d . . . . .
H H 0.367085 0.278068 0.627943 0.017 Uiso 1 1 calc GR . . . .
HA H 0.372635 0.402258 0.635456 0.017 Uiso 1 1 calc GR . . . .
HB H 0.418392 0.326647 0.681041 0.017 Uiso 1 1 calc GR . . . .
N2 N 0.5026(3) 0.0695(2) 0.36808(13) 0.0152(6) Uani 1 1 d . . . . .
HC H 0.479557 0.082608 0.331319 0.018 Uiso 1 1 calc GR . . . .
HD H 0.440714 0.050076 0.389178 0.018 Uiso 1 1 calc GR . . . .
HE H 0.554676 0.012369 0.368914 0.018 Uiso 1 1 calc GR . . . .
C4 C 0.5579(4) 0.1767(3) 0.39312(16) 0.0180(8) Uani 1 1 d . . . . .
HF H 0.501536 0.239279 0.391539 0.022 Uiso 1 1 calc R . . . .
HG H 0.624657 0.198441 0.369759 0.022 Uiso 1 1 calc R . . . .
C1 C 0.5275(3) 0.3377(3) 0.61475(16) 0.0153(7) Uani 1 1 d . . . . .
HH H 0.559249 0.260159 0.613802 0.018 Uiso 1 1 calc R . . . .
HI H 0.580878 0.385284 0.637742 0.018 Uiso 1 1 calc R . . . .
C3 C 0.5981(4) 0.1581(3) 0.45567(16) 0.0174(8) Uani 1 1 d . . . . .
HJ H 0.647646 0.222101 0.467701 0.021 Uiso 1 1 calc R . . . .
HK H 0.645241 0.088579 0.457778 0.021 Uiso 1 1 calc R . . . .
C2 C 0.5178(3) 0.3842(3) 0.55372(16) 0.0174(8) Uani 1 1 d . . . . .
HL H 0.594403 0.379878 0.535930 0.021 Uiso 1 1 calc R . . . .
HM H 0.496056 0.464893 0.555675 0.021 Uiso 1 1 calc R . . . .


_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 3.0512(3) 4_656 ?
Pb1 Br1 2.9702(3) . ?
Pb1 Br3 3.01158(17) . ?
Pb1 Br4 3.1032(4) . ?
Pb1 Br5 2.9256(2) . ?
Pb1 Br2 2.9264(4) . ?
S1 S2 2.0447(12) . ?
S1 C2 1.825(4) . ?
S2 C3 1.823(4) . ?
N1 H 0.8900 . ?
N1 HA 0.8900 . ?
N1 HB 0.8900 . ?
N1 C1 1.499(5) . ?
N2 HC 0.8900 . ?
N2 HD 0.8900 . ?
N2 HE 0.8900 . ?
N2 C4 1.505(4) . ?
C4 HF 0.9700 . ?
C4 HG 0.9700 . ?
C4 C3 1.511(5) . ?
C1 HH 0.9700 . ?
C1 HI 0.9700 . ?
C1 C2 1.500(5) . ?
C3 HJ 0.9700 . ?
C3 HK 0.9700 . ?
C2 HL 0.9700 . ?
C2 HM 0.9700 . ?

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 174.173(5) . 4_656 ?
Br1 Pb1 Br3 85.176(11) . . ?
Br1 Pb1 Br4 84.803(9) . . ?
Br1 Pb1 Br4 99.456(9) 4_656 . ?
Br3 Pb1 Br1 90.590(11) . 4_656 ?
Br3 Pb1 Br4 93.230(8) . . ?
Br5 Pb1 Br1 96.497(12) . 4_656 ?
Br5 Pb1 Br1 87.406(11) . . ?
Br5 Pb1 Br3 171.429(11) . . ?
Br5 Pb1 Br4 90.362(8) . . ?
Br5 Pb1 Br2 90.282(8) . . ?
Br2 Pb1 Br1 88.059(10) . 4_656 ?
Br2 Pb1 Br1 87.595(10) . . ?
Br2 Pb1 Br3 85.130(8) . . ?
Br2 Pb1 Br4 172.334(10) . . ?
Pb1 Br1 Pb1 149.720(13) . 4_646 ?
Pb1 Br3 Pb1 155.599(17) 2_756 . ?
Pb1 Br5 Pb1 140.751(18) . 2_656 ?
C2 S1 S2 102.05(12) . . ?
C3 S2 S1 101.95(12) . . ?
H N1 HA 109.5 . . ?
H N1 HB 109.5 . . ?
HA N1 HB 109.5 . . ?
C1 N1 H 109.5 . . ?
C1 N1 HA 109.5 . . ?
C1 N1 HB 109.5 . . ?
HC N2 HD 109.5 . . ?
HC N2 HE 109.5 . . ?
HD N2 HE 109.5 . . ?
C4 N2 HC 109.5 . . ?
C4 N2 HD 109.5 . . ?
C4 N2 HE 109.5 . . ?
N2 C4 HF 109.4 . . ?
N2 C4 HG 109.4 . . ?
N2 C4 C3 111.1(3) . . ?
HF C4 HG 108.0 . . ?
C3 C4 HF 109.4 . . ?
C3 C4 HG 109.4 . . ?
N1 C1 HH 109.6 . . ?
N1 C1 HI 109.6 . . ?
N1 C1 C2 110.4(3) . . ?
HH C1 HI 108.1 . . ?
C2 C1 HH 109.6 . . ?
C2 C1 HI 109.6 . . ?
S2 C3 HJ 108.9 . . ?
S2 C3 HK 108.9 . . ?
C4 C3 S2 113.2(3) . . ?
C4 C3 HJ 108.9 . . ?
C4 C3 HK 108.9 . . ?
HJ C3 HK 107.7 . . ?
S1 C2 HL 108.7 . . ?
S1 C2 HM 108.7 . . ?
C1 C2 S1 114.4(3) . . ?
C1 C2 HL 108.7 . . ?
C1 C2 HM 108.7 . . ?
HL C2 HM 107.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.927
_oxdiff_exptl_absorpt_empirical_full_min 0.560
