# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_(2cepiH)PbBr3
_database_code_depnum_ccdc_archive 'CCDC 2038518'
loop_
_audit_author_name
_audit_author_address
'Zhikai Qi'
;Shanxi Normal University
China
;
_audit_update_record             
;
2020-10-15 deposited with the CCDC.	2021-02-02 downloaded from the CCDC.
;
_audit_creation_date             2020-10-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'Br3 Pb, C7 H15 Cl N'
_chemical_formula_sum            'C7 H15 Br3 Cl N Pb'
_chemical_formula_weight         595.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         C/H/N/Pb/Br
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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   10.9554(13)
_cell_length_b                   16.2655(17)
_cell_length_c                   7.9831(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.324(12)
_cell_angle_gamma                90.00
_cell_volume                     1342.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2391
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4670
_cell_measurement_theta_min      3.7370
_exptl_absorpt_coefficient_mu    21.659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.947
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.1335
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7907
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         3.69
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  44.00   1.00   50.00    --   24.13 -19.00-180.00   42
  2  ω     35.00  92.00   1.00   50.00    --   24.13 178.00 -60.00   57
  3  ω      6.00  91.00   1.00   50.00    --   24.13  38.00   0.00   85
  4  ω    -48.00   1.00   1.00   50.00    --  -24.44 -77.00-150.00   49
  5  ω    -80.00 -45.00   1.00   50.00    --  -24.44 131.00 -59.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0679710000
_diffrn_orient_matrix_UB_12      0.0038332000
_diffrn_orient_matrix_UB_13      -0.0383747000
_diffrn_orient_matrix_UB_21      0.0059525000
_diffrn_orient_matrix_UB_22      0.0434830000
_diffrn_orient_matrix_UB_23      0.0044385000
_diffrn_orient_matrix_UB_31      0.0056727000
_diffrn_orient_matrix_UB_32      0.0006188000
_diffrn_orient_matrix_UB_33      -0.0859952000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2287
_reflns_number_total             3698
_reflns_odcompleteness_completeness 98.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 97-2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         3.983
_refine_diff_density_min         -7.004
_refine_diff_density_rms         0.742
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3698
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.1128
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1640P)²+23.1073P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2531
_refine_ls_wR_factor_ref         0.3068
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C1(H1a,H1b), C7(H7a,H7b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C3(H3a,H3b)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Pb1 Pb 0.18290(8) 0.25136(4) 0.02475(10) 0.0278(3) Uani 1 1 d . . .
Br1 Br -0.0173(2) 0.31840(13) -0.3421(3) 0.0322(5) Uani 1 1 d . . .
Br2 Br 0.3731(2) 0.31648(14) -0.1544(3) 0.0347(5) Uani 1 1 d . . .
Br3 Br 0.1892(2) 0.10736(12) -0.1706(3) 0.0319(5) Uani 1 1 d . . .
C2 C 0.730(3) 0.3567(12) 0.006(3) 0.040(6) Uani 1 1 d . . .
H2A H 0.6465 0.3818 -0.0526 0.048 Uiso 1 1 calc R . .
H2B H 0.7347 0.3060 -0.0560 0.048 Uiso 1 1 calc R . .
N1 N 0.7484(19) 0.4148(10) 0.301(2) 0.028(4) Uani 1 1 d . . .
H1 H 0.7737 0.3989 0.4164 0.033 Uiso 1 1 calc R . .
Cl1 Cl 0.5904(8) 0.3809(5) 0.5523(9) 0.0557(19) Uani 1 1 d . . .
C1 C 0.745(2) 0.3386(12) 0.193(3) 0.032(5) Uani 1 1 d . . .
H1A H 0.8241 0.3078 0.2464 0.039 Uiso 1 1 calc R . .
H1B H 0.6733 0.3043 0.1969 0.039 Uiso 1 1 calc R . .
C7 C 0.529(3) 0.4009(15) 0.322(3) 0.041(6) Uani 1 1 d . . .
H7A H 0.5153 0.3493 0.2578 0.049 Uiso 1 1 calc R . .
H7B H 0.4462 0.4285 0.2940 0.049 Uiso 1 1 calc R . .
C4 C 0.836(3) 0.4955(13) 0.099(3) 0.037(5) Uani 1 1 d . . .
H4A H 0.9051 0.5321 0.0961 0.045 Uiso 1 1 calc R . .
H4B H 0.7541 0.5233 0.0427 0.045 Uiso 1 1 calc R . .
C5 C 0.850(2) 0.4748(16) 0.284(3) 0.041(6) Uani 1 1 d . . .
H5A H 0.8440 0.5250 0.3466 0.049 Uiso 1 1 calc R . .
H5B H 0.9347 0.4513 0.3407 0.049 Uiso 1 1 calc R . .
C6 C 0.622(2) 0.4547(14) 0.262(3) 0.035(5) Uani 1 1 d . . .
H6A H 0.5854 0.4650 0.1360 0.042 Uiso 1 1 calc R . .
H6B H 0.6333 0.5072 0.3234 0.042 Uiso 1 1 calc R . .
C3 C 0.841(3) 0.4169(15) -0.002(3) 0.046(7) Uani 1 1 d . . .
H3A H 0.9244 0.3907 0.0498 0.055 Uiso 1 1 calc R . .
H3B H 0.8301 0.4299 -0.1250 0.055 Uiso 1 1 calc R . .

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 0.0249(5) 0.0353(5) 0.0235(4) -0.0002(3) 0.0085(3) -0.0002(3)
Br1 0.0225(11) 0.0411(11) 0.0331(10) 0.0024(8) 0.0091(9) 0.0012(10)
Br2 0.0237(11) 0.0442(11) 0.0329(10) -0.0001(9) 0.0048(9) -0.0091(10)
Br3 0.0309(12) 0.0341(10) 0.0325(10) -0.0021(8) 0.0130(9) 0.0003(9)
C2 0.061(19) 0.025(9) 0.024(9) 0.004(8) -0.001(11) 0.026(11)
N1 0.018(9) 0.030(8) 0.036(9) 0.007(7) 0.010(8) 0.007(8)
Cl1 0.055(5) 0.082(5) 0.034(3) 0.006(3) 0.021(3) -0.011(4)
C1 0.025(12) 0.026(9) 0.042(12) 0.006(8) 0.005(10) 0.011(9)
C7 0.035(15) 0.048(13) 0.044(13) -0.009(11) 0.019(12) -0.014(12)
C4 0.031(13) 0.038(11) 0.045(13) 0.004(10) 0.016(12) -0.014(11)
C5 0.025(11) 0.066(15) 0.035(11) -0.016(10) 0.015(10) -0.036(12)
C6 0.021(11) 0.046(12) 0.042(12) 0.003(10) 0.014(11) -0.006(10)
C3 0.06(2) 0.044(13) 0.040(13) 0.001(10) 0.027(15) 0.002(13)

_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 2.961(2) 4_566 ?
Pb1 Br1 3.213(2) . ?
Pb1 Br2 2.931(2) 4_566 ?
Pb1 Br2 3.079(2) . ?
Pb1 Br3 2.827(2) . ?
Br1 Pb1 2.961(2) 4_565 ?
Br2 Pb1 2.931(2) 4_565 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.48(3) . ?
C2 C3 1.58(4) . ?
N1 H1 0.9100 . ?
N1 C1 1.50(3) . ?
N1 C5 1.52(3) . ?
N1 C6 1.46(3) . ?
Cl1 C7 1.76(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C6 1.53(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.48(3) . ?
C4 C3 1.52(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 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 95.39(8) 4_566 . ?
Br1 Pb1 Br2 173.64(7) 4_566 . ?
Br2 Pb1 Br1 86.50(7) 4_566 4_566 ?
Br2 Pb1 Br1 176.24(6) 4_566 . ?
Br2 Pb1 Br1 79.79(6) . . ?
Br2 Pb1 Br2 98.08(8) 4_566 . ?
Br3 Pb1 Br1 84.97(7) . . ?
Br3 Pb1 Br1 92.10(6) . 4_566 ?
Br3 Pb1 Br2 83.39(6) . . ?
Br3 Pb1 Br2 91.71(7) . 4_566 ?
Pb1 Br1 Pb1 80.44(6) 4_565 . ?
Pb1 Br2 Pb1 83.20(6) 4_565 . ?
H2A C2 H2B 108.2 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C1 C2 C3 110(2) . . ?
C3 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C1 N1 H1 106.7 . . ?
C1 N1 C5 111.2(16) . . ?
C5 N1 H1 106.7 . . ?
C6 N1 H1 106.7 . . ?
C6 N1 C1 113.7(19) . . ?
C6 N1 C5 111.4(18) . . ?
C2 C1 N1 112.7(16) . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
Cl1 C7 H7A 109.3 . . ?
Cl1 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C6 C7 Cl1 111.4(19) . . ?
C6 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H4A C4 H4B 108.3 . . ?
C5 C4 H4A 109.8 . . ?
C5 C4 H4B 109.8 . . ?
C5 C4 C3 109.2(19) . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
N1 C5 H5A 108.8 . . ?
N1 C5 H5B 108.8 . . ?
C4 C5 N1 113.6(19) . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N1 C6 C7 111(2) . . ?
N1 C6 H6A 109.4 . . ?
N1 C6 H6B 109.4 . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C2 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
C4 C3 C2 109.7(19) . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?

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
Br1 Pb1 Br1 Pb1 -137.34(8) 4_566 . . 4_565 ?
Br1 Pb1 Br2 Pb1 -38.64(6) . . . 4_565 ?
Br1 Pb1 Br2 Pb1 2.3(6) 4_566 . . 4_565 ?
Br2 Pb1 Br1 Pb1 -17.3(10) 4_566 . . 4_565 ?
Br2 Pb1 Br1 Pb1 38.48(6) . . . 4_565 ?
Br2 Pb1 Br2 Pb1 138.22(8) 4_566 . . 4_565 ?
Br3 Pb1 Br1 Pb1 -45.69(6) . . . 4_565 ?
Br3 Pb1 Br2 Pb1 47.42(7) . . . 4_565 ?
Cl1 C7 C6 N1 60(2) . . . . ?
C1 C2 C3 C4 -58(3) . . . . ?
C1 N1 C5 C4 54(3) . . . . ?
C1 N1 C6 C7 67(2) . . . . ?
C5 N1 C1 C2 -53(3) . . . . ?
C5 N1 C6 C7 -166.3(18) . . . . ?
C5 C4 C3 C2 58(3) . . . . ?
C6 N1 C1 C2 74(3) . . . . ?
C6 N1 C5 C4 -74(3) . . . . ?
C3 C2 C1 N1 55(3) . . . . ?
C3 C4 C5 N1 -57(3) . . . . ?

_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 4.503
_oxdiff_exptl_absorpt_empirical_full_min 0.336
