# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_shi_4457_ilgu
_database_code_depnum_ccdc_archive 'CCDC 2058837'
loop_
_audit_author_name
_audit_author_address
'Ilya Guralskiy'
;Taras Shevchenko National University of Kyiv
Ukraine
;
_audit_update_record             
;
2021-01-26 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_audit_creation_date             2020-12-01
_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            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H8 N O2, H2 O, I3 Pb'
_chemical_formula_sum            'C3 H10 I3 N O3 Pb'
_chemical_formula_weight         696.01
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 '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'

_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           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   22.6435(14)
_cell_length_b                   6.4529(4)
_cell_length_c                   9.0191(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.107(6)
_cell_angle_gamma                90
_cell_volume                     1316.95(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8820
_cell_measurement_theta_min      2.2550
_shelx_estimated_absorpt_T_max   0.504
_shelx_estimated_absorpt_T_min   0.090
_exptl_absorpt_coefficient_mu    19.818
_exptl_absorpt_correction_T_max  0.473
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    3.510
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 0 13 0.0851
-13 7 6 0.0538
-32 0 0 0.0180
-5 -8 -5 0.0885
24 5 3 0.0507
11 -8 1 0.0777
7 0 -13 0.0866
32 0 0 0.0217
-6 9 -3 0.1035

_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.352
_diffrn_reflns_theta_min         1.800
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  45.00   1.00   10.00    --  -15.52  77.00 -30.00   87
  2  ω    -33.00  50.00   1.00   10.00    --  -15.52  77.00  60.00   83
  3  ω     -4.00  73.00   1.00   10.00    --   17.94  77.00 -30.00   77
  4  ω     32.00  58.00   1.00   10.00    --   17.94  77.00  30.00   26
  5  ω     -9.00  86.00   1.00   10.00    --   17.94  77.00-150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2388
_reflns_number_total             2684
_reflns_special_details          
;
 _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         4.571
_refine_diff_density_min         -3.105
_refine_diff_density_rms         0.441
_refine_ls_abs_structure_details 
;
 Flack x determined using 865 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2684
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0563
_refine_ls_restrained_S_all      1.107
_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)+(0.0849P)²+9.3035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1560
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.795(11)
 0.205(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3.a Riding coordinates:
 O2(H2A), O1W(H1WA,H1WB)
3.b Ternary CH refined with riding coordinates:
 C2(H2)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.7387(11) 1.224(5) 0.194(3) 0.037(5) Uani 1 1 d . . . . .
C2 C 0.6898(14) 1.072(4) 0.219(3) 0.044(7) Uani 1 1 d . . . . .
H2 H 0.660140 1.141599 0.277403 0.053 Uiso 1 1 calc R . . . .
C3 C 0.7114(16) 0.887(5) 0.305(4) 0.077(12) Uani 1 1 d . . . . .
H3A H 0.750201 0.849819 0.273913 0.115 Uiso 1 1 calc GR . . . .
H3B H 0.684941 0.772505 0.286448 0.115 Uiso 1 1 calc GR . . . .
H3C H 0.713025 0.918773 0.408607 0.115 Uiso 1 1 calc GR . . . .
N1 N 0.6606(9) 1.012(3) 0.073(2) 0.037(4) Uani 1 1 d . . . . .
H1A H 0.684812 0.931347 0.023344 0.045 Uiso 1 1 calc GR . . . .
H1B H 0.652454 1.125903 0.020348 0.045 Uiso 1 1 calc GR . . . .
H1C H 0.627305 0.944110 0.089216 0.045 Uiso 1 1 calc GR . . . .
O1 O 0.7536(9) 1.266(3) 0.070(2) 0.053(6) Uani 1 1 d . . . . .
O2 O 0.7601(11) 1.294(3) 0.314(2) 0.064(6) Uani 1 1 d . . . . .
H2A H 0.787591 1.375875 0.311333 0.095 Uiso 1 1 d R . . . .
O1W O 0.8526(10) 1.518(4) 0.269(3) 0.088(8) Uani 1 1 d . . . . .
H1WA H 0.888455 1.485193 0.251320 0.132 Uiso 1 1 d R . . . .
H1WB H 0.856105 1.622543 0.326550 0.132 Uiso 1 1 d R . . . .
I1 I 0.51430(8) 0.9844(5) 0.25161(18) 0.0488(5) Uani 1 1 d . . . . .
I2 I 0.59938(6) 0.5038(3) -0.00139(15) 0.0326(4) Uani 1 1 d . . . . .
I3 I 0.60322(7) 0.4837(4) 0.52043(15) 0.0402(5) Uani 1 1 d . . . . .
Pb1 Pb 0.50514(4) 0.48449(16) 0.25704(7) 0.0307(3) 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
C1 0.027(12) 0.043(13) 0.042(14) -0.006(13) 0.009(11) 0.010(13)
C2 0.059(18) 0.040(15) 0.036(13) 0.000(11) 0.032(13) -0.008(13)
C3 0.06(2) 0.08(2) 0.09(2) 0.07(2) -0.006(19) -0.007(19)
N1 0.033(10) 0.027(10) 0.054(10) 0.007(10) 0.012(8) -0.016(10)
O1 0.036(11) 0.069(16) 0.055(12) 0.011(10) 0.004(9) -0.016(10)
O2 0.058(15) 0.076(16) 0.056(13) -0.022(11) 0.001(11) -0.020(12)
O1W 0.049(13) 0.10(2) 0.110(16) -0.03(2) -0.014(12) -0.017(19)
I1 0.0472(9) 0.0190(8) 0.0814(12) -0.0034(9) 0.0201(8) -0.0025(11)
I2 0.0317(7) 0.0275(9) 0.0387(7) -0.0027(9) 0.0007(6) -0.0023(9)
I3 0.0349(8) 0.0508(12) 0.0349(7) 0.0046(11) 0.0017(6) -0.0019(12)
Pb1 0.0334(5) 0.0269(5) 0.0320(4) -0.0003(5) 0.0021(3) 0.0000(7)

_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
C1 C2 1.50(4) . ?
C1 O1 1.21(3) . ?
C1 O2 1.25(3) . ?
C2 H2 0.9800 . ?
C2 C3 1.50(4) . ?
C2 N1 1.50(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
O2 H2A 0.8173 . ?
O1W H1WA 0.8581 . ?
O1W H1WB 0.8567 . ?
I1 Pb1 3.233(3) . ?
I1 Pb1 3.234(3) 1_565 ?
I2 Pb1 3.2200(17) . ?
I2 Pb1 3.2453(15) 2_655 ?
I3 Pb1 3.1918(15) . ?
I3 Pb1 3.2265(16) 2_656 ?

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 C1 C2 121(2) . . ?
O1 C1 O2 127(3) . . ?
O2 C1 C2 112(2) . . ?
C1 C2 H2 107.7 . . ?
C3 C2 C1 112(3) . . ?
C3 C2 H2 107.7 . . ?
N1 C2 C1 110.1(18) . . ?
N1 C2 H2 107.7 . . ?
N1 C2 C3 112(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 O2 H2A 118.4 . . ?
H1WA O1W H1WB 103.7 . . ?
Pb1 I1 Pb1 172.38(7) . 1_565 ?
Pb1 I2 Pb1 91.57(4) . 2_655 ?
Pb1 I3 Pb1 86.49(4) . 2_656 ?
I1 Pb1 I1 172.38(7) . 1_545 ?
I1 Pb1 I2 89.80(5) . 2_655 ?
I1 Pb1 I2 94.19(5) 1_545 2_655 ?
I2 Pb1 I1 89.03(5) . 1_545 ?
I2 Pb1 I1 84.60(5) . . ?
I2 Pb1 I2 88.26(4) . 2_655 ?
I2 Pb1 I3 171.78(5) . 2_656 ?
I3 Pb1 I1 88.07(6) . 1_545 ?
I3 Pb1 I1 93.54(5) 2_656 . ?
I3 Pb1 I1 93.35(6) 2_656 1_545 ?
I3 Pb1 I1 88.26(6) . . ?
I3 Pb1 I2 83.72(4) 2_656 2_655 ?
I3 Pb1 I2 176.52(6) . 2_655 ?
I3 Pb1 I2 94.43(4) . . ?
I3 Pb1 I3 93.51(4) . 2_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A O1 0.89 1.97 2.85(3) 172.7 4_645 yes
N1 H1B I2 0.89 2.72 3.52(2) 149.2 1_565 yes
N1 H1C I1 0.89 3.01 3.741(19) 141.2 . yes
N1 H1C I2 0.89 3.02 3.62(2) 126.3 . yes
O2 H2A O1W 0.82 1.79 2.59(3) 166.5 . yes
O1W H1WA I1 0.86 2.85 3.68(2) 162.3 3 yes
O1W H1WB I3 0.86 2.84 3.68(3) 164.6 4_666 yes

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
O1 C1 C2 C3 118(3) . . . . ?
O1 C1 C2 N1 -7(4) . . . . ?
O2 C1 C2 C3 -62(3) . . . . ?
O2 C1 C2 N1 173(2) . . . . ?

_iucr_refine_instructions_details 
;
TITL shi_4457_ilgu_c.res in C2
    shi_4457_ilgu.res
    created by SHELXL-2017/1 at 16:37:48 on 01-Dec-2020
REM Old TITL shI_4457_IlGu in C2
REM SHELXT solution in C2
REM R1 0.117, Rweak 0.014, Alpha 0.106, Orientation as input
REM Flack x = 0.176 ( 0.010 ) from Parsons' quotients
REM Formula found by SHELXT: C3 N O I3 Pb
CELL 0.71073 22.6435 6.4529 9.0191 90 92.107 90
ZERR 4 0.0014 0.0004 0.0006 0 0.006 0
LATT -7
SYMM -X,+Y,-Z
SFAC C H I N O Pb
UNIT 12 40 12 4 12 4
EQIV $1 +X,1+Y,+Z
EQIV $2 1.5-X,-0.5+Y,-Z
EQIV $3 0.5+X,0.5+Y,+Z
EQIV $4 1.5-X,1.5+Y,1-Z

L.S. 10
PLAN  10
SIZE 0.04 0.163 0.234
HTAB N1 O1_$2
HTAB N1 I2_$1
HTAB N1 I1
HTAB N1 I2
HTAB O2 O1W
HTAB O1W I1_$3
HTAB O1W I3_$4
CONF
htab
BOND $H
LIST 4
MORE -1
fmap 2
acta
SHEL 99 0.8
REM <olex2.extras>
REM <HklSrc "%.\\shi_4457_ilgu_tw.hkl">
REM </olex2.extras>

WGHT    0.084900    9.303500
BASF   0.20532
FVAR       3.47024
C1    1    0.738722    1.223831    0.194155    11.00000    0.02700    0.04257 =
         0.04242   -0.00571    0.00910    0.00999
C2    1    0.689784    1.071899    0.218590    11.00000    0.05869    0.04010 =
         0.03616    0.00042    0.03206   -0.00800
AFIX  13
H2    2    0.660140    1.141599    0.277403    11.00000   -1.20000
AFIX   0
C3    1    0.711431    0.886615    0.304612    11.00000    0.06187    0.08091 =
         0.08632    0.06844   -0.00575   -0.00708
AFIX 137
H3A   2    0.750201    0.849819    0.273913    11.00000   -1.50000
H3B   2    0.684941    0.772505    0.286448    11.00000   -1.50000
H3C   2    0.713025    0.918773    0.408607    11.00000   -1.50000
AFIX   0
N1    4    0.660633    1.012270    0.073128    11.00000    0.03281    0.02659 =
         0.05380    0.00736    0.01224   -0.01564
AFIX 137
H1A   2    0.684812    0.931347    0.023344    11.00000   -1.20000
H1B   2    0.652454    1.125903    0.020348    11.00000   -1.20000
H1C   2    0.627305    0.944110    0.089216    11.00000   -1.20000
AFIX   0
O1    5    0.753607    1.266477    0.069941    11.00000    0.03571    0.06868 =
         0.05547    0.01071    0.00353   -0.01571
O2    5    0.760050    1.294275    0.314243    11.00000    0.05807    0.07622 =
         0.05612   -0.02220    0.00086   -0.01962
AFIX   3
H2A   2    0.787591    1.375875    0.311333    11.00000   -1.50000
AFIX   0

O1W   5    0.852615    1.517603    0.268710    11.00000    0.04939    0.10287 =
         0.11003   -0.02750   -0.01360   -0.01662
AFIX   3
H1WA  2    0.888455    1.485193    0.251320    11.00000   -1.50000
H1WB  2    0.856105    1.622543    0.326550    11.00000   -1.50000
AFIX   0

I1    3    0.514304    0.984354    0.251611    11.00000    0.04720    0.01902 =
         0.08144   -0.00336    0.02006   -0.00247
I2    3    0.599381    0.503771   -0.001391    11.00000    0.03170    0.02747 =
         0.03870   -0.00269    0.00066   -0.00230
I3    3    0.603219    0.483650    0.520426    11.00000    0.03495    0.05084 =
         0.03487    0.00464    0.00171   -0.00193
PB1   6    0.505137    0.484491    0.257045    11.00000    0.03336    0.02688 =
         0.03204   -0.00032    0.00212   -0.00004
HKLF 5




REM  shi_4457_ilgu_c.res in C2
REM R1 =  0.0563 for    2388 Fo > 4sig(Fo)  and  0.0620 for all    2684 data
REM    103 parameters refined using      1 restraints

END  
     
WGHT      0.0848      9.3752 

REM Instructions for potential hydrogen bonds
HTAB N1 O1_$2
HTAB N1 I2_$1
HTAB N1 I1
HTAB N1 I2
HTAB O2 O1W
HTAB O1W I1_$3
HTAB O1W I3_$4

REM Highest difference peak  4.571,  deepest hole -3.105,  1-sigma level  0.441
Q1    1   0.5107  0.4891  0.3470  11.00000  0.05    4.57
Q2    1   0.5072  0.4776  0.1434  11.00000  0.05    3.43
Q3    1   0.5961  0.4772  0.4145  11.00000  0.05    2.80
Q4    1   0.5132  0.9882  0.1344  11.00000  0.05    2.59
Q5    1   0.6016  0.5021 -0.0973  11.00000  0.05    2.58
Q6    1   0.5192  0.9785  0.3632  11.00000  0.05    2.06
Q7    1   0.5171  0.5627  0.4525  11.00000  0.05    1.51
Q8    1   0.4880  0.3868  0.0460  11.00000  0.05    1.33
Q9    1   0.6122  0.5149  0.0998  11.00000  0.05    1.25
Q10   1   0.5000  0.2498  0.0000  10.50000  0.05    1.15

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0563 for 2388 Fo > 4sig(Fo) and 0.0620 for all 2684 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 4.57, deepest hole -3.11
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0620
  REM R1_gt = 0.0563
  REM wR_ref = 0.1560
  REM GOOF = 1.107
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2684
  REM Reflections_gt = 2388
  REM Parameters = n/a
  REM Hole = -3.11
  REM Peak = 4.57
  REM Flack = 0.031(11)

  
;
_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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.795(11)
2 0.205(11)

####################################################################### 
# 
# 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_shi_4456_ilgu
_database_code_depnum_ccdc_archive 'CCDC 2058838'
loop_
_audit_author_name
_audit_author_address
'Ilya Guralskiy'
;Taras Shevchenko National University of Kyiv
Ukraine
;
_audit_update_record             
;
2021-01-26 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_audit_creation_date             2020-12-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H8 N O2, H2 O'
_chemical_formula_sum            'C3 H10 Br3 N O3 Pb'
_chemical_formula_weight         555.04
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'

_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           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   21.836(4)
_cell_length_b                   6.0904(11)
_cell_length_c                   8.790(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.41(2)
_cell_angle_gamma                90
_cell_volume                     1167.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1212
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.0030
_cell_measurement_theta_min      2.3180
_shelx_estimated_absorpt_T_max   0.192
_shelx_estimated_absorpt_T_min   0.051
_exptl_absorpt_coefficient_mu    24.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.157
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4219
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.347
_diffrn_reflns_theta_min         1.867
_diffrn_ambient_temperature      296.0
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  50.00   1.00   12.50    --  -15.52  77.00  30.00   84
  2  ω     25.00  52.00   1.00   12.50    --  -15.52  77.00  60.00   27
  3  ω    -23.00  46.00   1.00   12.50    --  -15.52  77.00 -60.00   69
  4  ω     -5.00  81.00   1.00   12.50    --   17.94  77.00-180.00   86
  5  ω     -4.00  81.00   1.00   12.50    --   17.94  77.00 -60.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2081
_reflns_number_total             2392
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0436
_refine_ls_restrained_S_all      1.060
_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)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1037
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O2B-C1 \\sim O2A-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(O2B) = Uiso(O2A)
4. Others
 Fixed Sof: O2B(0.5) H2B(0.5) O2A(0.5) H2A(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2B(H2B), O2A(H2A)
5.b Ternary CH refined with riding coordinates:
 C2(H2)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.49600(2) 0.50451(16) 0.24414(6) 0.0300(2) Uani 1 1 d . . . . .
Br1 Br 0.59422(7) 0.5185(4) 0.49892(19) 0.0362(5) Uani 1 1 d . . . . .
Br2 Br 0.59670(7) 0.5034(6) 0.02706(19) 0.0446(4) Uani 1 1 d . . . . .
Br3 Br 0.48770(8) 0.9918(9) 0.2519(2) 0.0551(6) Uani 1 1 d . . . . .
N1 N 0.6545(5) 0.025(2) 0.5645(15) 0.036(3) Uani 1 1 d . . . . .
H1A H 0.625010 -0.074075 0.574216 0.044 Uiso 1 1 calc R U . . .
H1B H 0.682193 -0.026040 0.502162 0.044 Uiso 1 1 calc R U . . .
H1C H 0.638320 0.148670 0.526333 0.044 Uiso 1 1 calc R U . . .
O1W O 0.8555(6) 0.539(2) 0.7933(18) 0.075(5) Uani 1 1 d . . . . .
H1WA H 0.853113 0.661160 0.841901 0.113 Uiso 1 1 d R U . . .
H1WB H 0.894193 0.507740 0.793551 0.113 Uiso 1 1 d R U . . .
C1 C 0.7358(7) 0.234(3) 0.692(2) 0.035(4) Uani 1 1 d D . . . .
O1 O 0.7519(5) 0.285(2) 0.5750(15) 0.043(3) Uani 1 1 d . . . . .
O2B O 0.7658(12) 0.264(5) 0.828(2) 0.044(5) Uiso 0.5 1 d D . P A 2
H2B H 0.798299 0.342637 0.815292 0.066 Uiso 0.5 1 d R U P A 2
C2 C 0.6841(9) 0.070(3) 0.715(2) 0.041(5) Uani 1 1 d . . . . .
H2 H 0.653850 0.140939 0.777915 0.049 Uiso 1 1 calc R U . . .
C3 C 0.7040(11) -0.136(4) 0.791(3) 0.068(7) Uani 1 1 d . . . . .
H3A H 0.669059 -0.208667 0.830685 0.101 Uiso 1 1 calc R U . . .
H3B H 0.732994 -0.103018 0.872968 0.101 Uiso 1 1 calc R U . . .
H3C H 0.722817 -0.230128 0.718886 0.101 Uiso 1 1 calc R U . . .
O2A O 0.7527(13) 0.330(4) 0.826(2) 0.044(5) Uiso 0.5 1 d D . P A 1
H2A H 0.785365 0.408115 0.816360 0.066 Uiso 0.5 1 d R U P A 1

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 0.0310(3) 0.0244(3) 0.0347(3) 0.0002(5) 0.0015(2) -0.0002(6)
Br1 0.0288(8) 0.0292(10) 0.0501(9) -0.0061(16) -0.0025(6) -0.0012(14)
Br2 0.0330(8) 0.0535(11) 0.0470(9) 0.007(2) 0.0003(7) -0.005(2)
Br3 0.0536(11) 0.0285(11) 0.0847(14) 0.0059(13) 0.0219(9) 0.003(2)
N1 0.025(6) 0.025(7) 0.059(9) 0.008(9) 0.004(6) 0.000(7)
O1W 0.049(8) 0.055(10) 0.120(13) -0.018(11) -0.014(8) -0.004(8)
C1 0.026(9) 0.030(8) 0.048(12) -0.009(9) 0.002(8) 0.008(8)
O1 0.039(8) 0.044(8) 0.045(8) 0.006(6) 0.013(6) -0.017(6)
C2 0.044(11) 0.043(12) 0.038(10) -0.010(8) 0.005(8) 0.001(8)
C3 0.076(17) 0.063(14) 0.065(17) 0.014(13) 0.020(14) -0.018(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 3.060(2) 2_656 ?
Pb1 Br1 3.0363(17) . ?
Pb1 Br2 3.0617(18) 2_655 ?
Pb1 Br2 2.9713(19) . ?
Pb1 Br3 2.974(5) . ?
Pb1 Br3 3.129(5) 1_545 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.47(2) . ?
O1W H1WA 0.8613 . ?
O1W H1WB 0.8657 . ?
C1 O1 1.15(2) . ?
C1 O2B 1.35(2) . ?
C1 C2 1.52(3) . ?
C1 O2A 1.35(2) . ?
O2B H2B 0.8685 . ?
C2 H2 0.9800 . ?
C2 C3 1.48(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
O2A H2A 0.8639 . ?

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 84.93(5) . 2_656 ?
Br1 Pb1 Br2 98.60(5) 2_656 2_655 ?
Br1 Pb1 Br2 176.13(7) . 2_655 ?
Br1 Pb1 Br3 88.40(8) 2_656 1_545 ?
Br1 Pb1 Br3 92.96(7) . 1_545 ?
Br2 Pb1 Br1 87.41(5) . . ?
Br2 Pb1 Br1 172.23(5) . 2_656 ?
Br2 Pb1 Br2 89.02(5) . 2_655 ?
Br2 Pb1 Br3 93.69(8) . . ?
Br2 Pb1 Br3 88.73(9) 2_655 1_545 ?
Br2 Pb1 Br3 93.26(8) . 1_545 ?
Br3 Pb1 Br1 89.83(7) . . ?
Br3 Pb1 Br1 85.04(7) . 2_656 ?
Br3 Pb1 Br2 88.91(9) . 2_655 ?
Br3 Pb1 Br3 172.62(7) . 1_545 ?
Pb1 Br1 Pb1 94.98(5) . 2_656 ?
Pb1 Br2 Pb1 90.98(5) . 2_655 ?
Pb1 Br3 Pb1 172.62(7) . 1_565 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1WA O1W H1WB 105.5 . . ?
O1 C1 O2B 127(2) . . ?
O1 C1 C2 123.5(17) . . ?
O1 C1 O2A 126(2) . . ?
O2B C1 C2 108(2) . . ?
O2A C1 C2 110(2) . . ?
C1 O2B H2B 108.9 . . ?
N1 C2 C1 107.8(15) . . ?
N1 C2 H2 107.9 . . ?
N1 C2 C3 110.9(14) . . ?
C1 C2 H2 107.9 . . ?
C3 C2 C1 114.1(16) . . ?
C3 C2 H2 107.9 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 O2A H2A 110.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Br1 0.89 2.65 3.395(14) 142.2 1_545 yes
N1 H1A Br3 0.89 2.98 3.564(13) 125.0 2_646 yes
N1 H1B O1 0.89 1.98 2.833(18) 159.4 4_646 yes
N1 H1C Br1 0.89 2.46 3.320(14) 163.4 . yes
O1W H1WA Br2 0.86 2.60 3.384(15) 151.6 4_656 yes
O1W H1WB Br3 0.87 2.63 3.475(14) 166.3 4_646 yes
O2B H2B O1W 0.87 1.75 2.61(3) 170.5 . yes
O2A H2A O1W 0.86 1.75 2.61(3) 173.9 . yes

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
O1 C1 C2 N1 -9(2) . . . . ?
O1 C1 C2 C3 115(2) . . . . ?
O2B C1 C2 N1 -175.7(17) . . . . ?
O2B C1 C2 C3 -52(2) . . . . ?
O2A C1 C2 N1 161.9(17) . . . . ?
O2A C1 C2 C3 -74(2) . . . . ?

_shelx_res_file                  
;
TITL shi_4456_ilgu_b.res in C2
    shi_4456_ilgu.res
    created by SHELXL-2018/3 at 13:36:11 on 01-Dec-2020
REM Old TITL shi_4456_ilgu_a.res in C2/m
REM SHELXT solution in C2: R1 0.109, Rweak 0.008, Alpha 0.041
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.449 ( 0.036 ) from 826 Parsons' quotients
REM Formula found by SHELXT: N2 O Br3 Pb
CELL 0.71073 21.8361 6.0904 8.7896 90 92.407 90
ZERR 4 0.0043 0.0011 0.0029 0 0.02 0
LATT -7
SYMM -X,+Y,-Z
SFAC C H Br N O Pb
UNIT 12 40 12 4 12 4
EQIV $1 +X,-1+Y,+Z
EQIV $2 1-X,-1+Y,1-Z
EQIV $3 1.5-X,-0.5+Y,1-Z
EQIV $4 1.5-X,0.5+Y,1-Z
EADP O2B O2A
SADI 0.01 O2B C1 O2A C1

L.S. 15
PLAN  7
SIZE 0.1 0.15 0.3
TEMP 22.85
HTAB N1 Br1_$1
HTAB N1 Br3_$2
HTAB N1 O1_$3
HTAB N1 Br1
HTAB O1W Br2_$4
HTAB O1W Br3_$3
HTAB O2B O1W
HTAB O2A O1W
CONF
htab
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
SHEL 99 0.8
OMIT -2 0 1
OMIT -21 -3 1
OMIT -2 2 1
REM <olex2.extras>
REM <HklSrc "%.\\shi_4456_ilgu.hkl">
REM </olex2.extras>

WGHT    0.043700
FVAR       0.16797
PB1   6    0.495996    0.504510    0.244138    11.00000    0.03098    0.02438 =
         0.03469    0.00015    0.00147   -0.00023
BR1   3    0.594219    0.518504    0.498924    11.00000    0.02880    0.02921 =
         0.05014   -0.00608   -0.00253   -0.00118
BR2   3    0.596700    0.503446    0.027057    11.00000    0.03304    0.05348 =
         0.04702    0.00742    0.00034   -0.00505
BR3   3    0.487696    0.991755    0.251885    11.00000    0.05363    0.02850 =
         0.08474    0.00594    0.02192    0.00254
N1    4    0.654481    0.025269    0.564520    11.00000    0.02533    0.02501 =
         0.05876    0.00832    0.00405   -0.00006
AFIX 137
H1A   2    0.625010   -0.074075    0.574216    11.00000   -1.20000
H1B   2    0.682193   -0.026040    0.502162    11.00000   -1.20000
H1C   2    0.638320    0.148670    0.526333    11.00000   -1.20000
AFIX   0

O1W   5    0.855503    0.538840    0.793331    11.00000    0.04880    0.05460 =
         0.12044   -0.01845   -0.01444   -0.00388
AFIX   3
H1WA  2    0.853113    0.661160    0.841901    11.00000   -1.50000
H1WB  2    0.894193    0.507740    0.793551    11.00000   -1.50000
AFIX   0

C1    1    0.735845    0.233863    0.692248    11.00000    0.02638    0.02987 =
         0.04822   -0.00872    0.00174    0.00755
O1    5    0.751938    0.285204    0.574960    11.00000    0.03928    0.04447 =
         0.04530    0.00615    0.01260   -0.01730
PART 2
O2B   5    0.765849    0.263537    0.828392    10.50000    0.04401
AFIX   3
H2B   2    0.798299    0.342637    0.815292    10.50000   -1.50000
AFIX   0
PART 0
C2    1    0.684126    0.070352    0.714804    11.00000    0.04403    0.04251 =
         0.03750   -0.00977    0.00532    0.00107
AFIX  13
H2    2    0.653850    0.140939    0.777915    11.00000   -1.20000
AFIX   0
C3    1    0.703996   -0.136007    0.791038    11.00000    0.07634    0.06278 =
         0.06488    0.01440    0.01999   -0.01782
AFIX 137
H3A   2    0.669059   -0.208667    0.830685    11.00000   -1.50000
H3B   2    0.732994   -0.103018    0.872968    11.00000   -1.50000
H3C   2    0.722817   -0.230128    0.718886    11.00000   -1.50000
AFIX   0
PART 1
O2A   5    0.752655    0.330485    0.826150    10.50000    0.04401
AFIX   3
H2A   2    0.785365    0.408115    0.816360    10.50000   -1.50000
AFIX   0
HKLF 4




REM  shi_4456_ilgu_b.res in C2
REM wR2 = 0.1037, GooF = S = 1.061, Restrained GooF = 1.060 for all data
REM R1 = 0.0436 for 2081 Fo > 4sig(Fo) and 0.0513 for all 2392 data
REM 100 parameters refined using 2 restraints

END

WGHT      0.0437      0.0000

REM Instructions for potential hydrogen bonds
HTAB N1 Br1_$1
HTAB N1 Br3_$2
HTAB N1 O1_$3
HTAB N1 Br1
HTAB O1W Br2_$4
HTAB O1W Br3_$3
HTAB O2B O1W
EQIV $8 x, y-1, z+1
HTAB C3 Br2_$8
HTAB O2A O1W

REM Highest difference peak  1.328,  deepest hole -0.981,  1-sigma level  0.179
Q1    1   0.4613  0.5047  0.1568  11.00000  0.05    1.33
Q2    1   0.5203  0.5086  0.1568  11.00000  0.05    1.06
Q3    1   0.5298  0.5039  0.3572  11.00000  0.05    1.01
Q4    1   0.4775  0.4850  0.3409  11.00000  0.05    0.98
Q5    1   0.6136  0.5015  0.4201  11.00000  0.05    0.88
Q6    1   0.5894  0.5069 -0.1233  11.00000  0.05    0.70
Q7    1   0.6220  0.5222  0.1361  11.00000  0.05    0.67
;
_shelx_res_checksum              23971
_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
;
####################################################################### 
# 
# 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_shi_4452_ilgu_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2058840'
loop_
_audit_author_name
_audit_author_address
'Ilya Guralskiy'
;Taras Shevchenko National University of Kyiv
Ukraine
;
_audit_update_record             
;
2021-01-26 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_audit_creation_date             2020-12-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H8 N O2, H2 O, I3 Pb'
_chemical_formula_sum            'C3 H10 I3 N O3 Pb'
_chemical_formula_weight         696.01
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 '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'

_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           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   22.560(3)
_cell_length_b                   6.4430(5)
_cell_length_c                   8.9978(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.204(9)
_cell_angle_gamma                90
_cell_volume                     1306.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.6980
_cell_measurement_theta_min      2.2150
_shelx_estimated_absorpt_T_max   0.267
_shelx_estimated_absorpt_T_min   0.045
_exptl_absorpt_coefficient_mu    19.971
_exptl_absorpt_correction_T_max  0.07810
_exptl_absorpt_correction_T_min  0.05214
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.537
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_exptl_crystal_size_rad          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3595
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_min         2.265
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                3066
_reflns_number_total             3595
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.369
_refine_diff_density_min         -3.007
_refine_diff_density_rms         0.500
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0873
_refine_ls_restrained_S_all      1.082
_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)+(0.2000P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2570
_refine_ls_wR_factor_ref         0.2665
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.659(5)
 0.341(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 H1A-I1
 2.7 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Riding coordinates:
 O2(H2A), O1W(H1WA,H1WB)
5.b Ternary CH refined with riding coordinates:
 C2(H2)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.260(2) -0.471(8) 0.313(5) 0.041(11) Uani 1 1 d . U . . .
C2 C 0.310(2) -0.320(7) 0.283(5) 0.043(11) Uani 1 1 d . U . . .
H2 H 0.340352 -0.392123 0.226106 0.051 Uiso 1 1 calc R U . . .
C3 C 0.288(3) -0.141(9) 0.194(6) 0.067(16) Uani 1 1 d . U . . .
H3A H 0.251942 -0.090058 0.235447 0.100 Uiso 1 1 calc R U . . .
H3B H 0.279774 -0.183387 0.093123 0.100 Uiso 1 1 calc R U . . .
H3C H 0.317050 -0.032464 0.196490 0.100 Uiso 1 1 calc R U . . .
N1 N 0.3381(16) -0.252(5) 0.430(3) 0.040(7) Uani 1 1 d . U . . .
H1A H 0.356525 -0.131279 0.418387 0.048 Uiso 1 1 calc DR U . . .
H1B H 0.364156 -0.347115 0.461997 0.048 Uiso 1 1 calc R U . . .
H1C H 0.309985 -0.237588 0.495751 0.048 Uiso 1 1 calc R U . . .
O1 O 0.2454(18) -0.514(5) 0.431(4) 0.053(10) Uani 1 1 d . U . . .
O2 O 0.2354(18) -0.546(6) 0.186(3) 0.055(9) Uani 1 1 d . U . . .
H2A H 0.204670 -0.613868 0.208719 0.083 Uiso 1 1 d R U . . .
O1W O 0.1435(19) -0.781(6) 0.233(5) 0.085(15) Uani 1 1 d . . . . .
H1WA H 0.142477 -0.892133 0.178545 0.127 Uiso 1 1 d R U . . .
H1WB H 0.106197 -0.753113 0.234185 0.127 Uiso 1 1 d R U . . .
I1 I 0.40066(13) 0.2430(5) 0.5018(3) 0.0386(8) Uani 1 1 d D . . . .
I2 I 0.39682(13) 0.2623(6) 0.9796(3) 0.0463(9) Uani 1 1 d . . . . .
I3 I 0.51431(14) 0.7628(10) 0.7516(3) 0.0553(9) Uani 1 1 d . . . . .
Pb1 Pb 0.50504(7) 0.2620(3) 0.75751(14) 0.0378(5) 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
C1 0.035(16) 0.038(15) 0.049(16) -0.005(13) -0.005(12) -0.008(13)
C2 0.044(17) 0.046(16) 0.037(14) 0.004(12) 0.004(13) 0.003(13)
C3 0.07(3) 0.07(3) 0.05(2) 0.03(2) -0.01(2) -0.01(2)
N1 0.022(16) 0.030(16) 0.067(17) 0.013(17) 0.001(13) -0.007(17)
O1 0.053(10) 0.053(10) 0.053(10) 0.000(3) 0.002(3) -0.001(3)
O2 0.034(18) 0.08(2) 0.052(17) 0.002(14) -0.012(14) -0.025(17)
O1W 0.04(2) 0.08(4) 0.14(3) -0.04(3) -0.01(2) 0.01(3)
I1 0.0327(15) 0.0342(17) 0.0488(14) -0.0037(17) -0.0014(11) -0.0037(17)
I2 0.0353(16) 0.057(2) 0.0462(14) 0.004(2) 0.0008(12) -0.002(2)
I3 0.0493(19) 0.0279(14) 0.090(2) 0.0032(16) 0.0155(16) -0.002(2)
Pb1 0.0357(9) 0.0358(9) 0.0416(8) 0.0006(10) -0.0001(7) -0.0011(16)

_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
C1 C2 1.52(7) . ?
C1 O1 1.16(5) . ?
C1 O2 1.34(5) . ?
C2 H2 0.9800 . ?
C2 C3 1.48(6) . ?
C2 N1 1.51(6) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
O2 H2A 0.8525 . ?
O1W H1WA 0.8673 . ?
O1W H1WB 0.8609 . ?
I1 Pb1 3.220(3) 2_656 ?
I1 Pb1 3.231(3) . ?
I2 Pb1 3.177(3) 2_657 ?
I2 Pb1 3.214(3) . ?
I3 Pb1 3.224(6) 1_565 ?
I3 Pb1 3.234(6) . ?

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 C1 C2 124(4) . . ?
O1 C1 O2 124(5) . . ?
O2 C1 C2 112(4) . . ?
C1 C2 H2 108.7 . . ?
C3 C2 C1 111(5) . . ?
C3 C2 H2 108.7 . . ?
C3 C2 N1 112(4) . . ?
N1 C2 C1 108(3) . . ?
N1 C2 H2 108.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 O2 H2A 107.5 . . ?
H1WA O1W H1WB 100.1 . . ?
Pb1 I1 Pb1 91.76(8) 2_656 . ?
Pb1 I2 Pb1 86.49(9) 2_657 . ?
Pb1 I3 Pb1 172.26(12) 1_565 . ?
I1 Pb1 I1 88.07(8) 2_656 . ?
I1 Pb1 I3 88.92(9) 2_656 . ?
I1 Pb1 I3 94.12(10) . . ?
I1 Pb1 I3 84.54(10) 2_656 1_545 ?
I2 Pb1 I1 171.69(10) . 2_656 ?
I2 Pb1 I1 83.82(8) . . ?
I2 Pb1 I1 176.58(12) 2_657 . ?
I2 Pb1 I1 94.51(8) 2_657 2_656 ?
I2 Pb1 I2 93.51(9) 2_657 . ?
I2 Pb1 I3 88.17(11) 2_657 . ?
I2 Pb1 I3 93.56(9) . 1_545 ?
I2 Pb1 I3 93.49(11) . . ?
I2 Pb1 I3 88.23(11) 2_657 1_545 ?
I3 Pb1 I1 89.79(9) 1_545 . ?
I3 Pb1 I3 172.26(12) 1_545 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A I1 0.89 2.70 3.54(3) 156.4 . yes
N1 H1A I3 0.89 3.41 3.77(3) 106.7 2_646 yes
N1 H1B I1 0.89 2.79 3.60(4) 152.0 1_545 yes
N1 H1C O1 0.89 2.04 2.77(5) 138.9 4_556 yes
N1 H1C O1W 0.89 2.63 3.05(5) 109.8 4_556 yes
O2 H2A O1W 0.85 1.77 2.62(6) 171.2 . yes
O1W H1WA I2 0.87 2.77 3.61(4) 162.7 4_536 yes
O1W H1WB I3 0.86 2.73 3.58(4) 169.9 4_536 yes

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
O1 C1 C2 C3 -119(5) . . . . ?
O1 C1 C2 N1 4(7) . . . . ?
O2 C1 C2 C3 60(6) . . . . ?
O2 C1 C2 N1 -177(4) . . . . ?

_shelx_res_file                  
;
TITL shi_4452_ilgu_twin1_hklf4_b.res in C2
    shi_4452_ilgu_twin1_hklf4.res
    created by SHELXL-2018/3 at 15:13:26 on 01-Dec-2020
REM Old TITL shi_4452_ilgu_twin1_hklf4_a.res in C2/m
REM SHELXT solution in C2: R1 0.200, Rweak 0.013, Alpha 0.126
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.290 ( 0.068 ) from 551 Parsons' quotients
REM Formula found by SHELXT: C3 N4 O9 I6 Pb2
CELL 0.71073 22.5596 6.443 8.9978 90 92.204 90
ZERR 4 0.0025 0.0005 0.0007 0 0.009 0
LATT -7
SYMM -X,+Y,-Z
SFAC C H I N O Pb
UNIT 12 40 12 4 12 4
EQIV $1 0.5-X,0.5+Y,1-Z
EQIV $2 +X,-1+Y,+Z
EQIV $3 1-X,-1+Y,1-Z
EQIV $4 0.5-X,-1.5+Y,1-Z
ISOR 0.01 0.02 C1 C2 C3 O2 N1
ISOR 0.001 0.002 O1
DFIX 2.7 0.01 H1a I1

L.S. 10
PLAN  10
SIZE 0.09 0.24 0.41
TEMP 19.85
HTAB N1 I1
HTAB N1 I3_$3
HTAB N1 O1W_$1
HTAB N1 I1_$2
HTAB N1 O1_$1
HTAB O2 O1W
HTAB O1W I2_$4
HTAB O1W I3_$4
CONF
htab
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
SHEL 99 0.8
OMIT 2 0 0
OMIT -23 1 4
OMIT 2 0 -1
OMIT -23 -3 4
OMIT -17 -3 3
OMIT -26 2 0
REM <olex2.extras>
REM <HklSrc "%.\\shI_4452_IlGu_twin1_hklf4.hkl">
REM </olex2.extras>

WGHT    0.200000   10.000000
BASF   0.34068
FVAR       0.45257
C1    1    0.260369   -0.471139    0.312560    11.00000    0.03472    0.03789 =
         0.04863   -0.00463   -0.00497   -0.00768
C2    1    0.310295   -0.320041    0.282604    11.00000    0.04420    0.04639 =
         0.03743    0.00434    0.00418    0.00342
AFIX  13
H2    2    0.340352   -0.392123    0.226106    11.00000   -1.20000
AFIX   0
C3    1    0.287783   -0.140699    0.194127    11.00000    0.07327    0.07169 =
         0.05401    0.02807   -0.00841   -0.00558
AFIX 137
H3A   2    0.251942   -0.090058    0.235447    11.00000   -1.50000
H3B   2    0.279774   -0.183387    0.093123    11.00000   -1.50000
H3C   2    0.317050   -0.032464    0.196490    11.00000   -1.50000
AFIX   0
N1    4    0.338088   -0.252038    0.429764    11.00000    0.02185    0.03016 =
         0.06720    0.01303    0.00139   -0.00685
AFIX 137
H1A   2    0.356525   -0.131279    0.418387    11.00000   -1.20000
H1B   2    0.364156   -0.347115    0.461997    11.00000   -1.20000
H1C   2    0.309985   -0.237588    0.495751    11.00000   -1.20000
AFIX   0
O1    5    0.245426   -0.513906    0.430652    11.00000    0.05257    0.05305 =
         0.05325    0.00008    0.00173   -0.00079
O2    5    0.235420   -0.545708    0.185999    11.00000    0.03391    0.07845 =
         0.05182    0.00173   -0.01222   -0.02456
AFIX   3
H2A   2    0.204670   -0.613868    0.208719    11.00000   -1.50000
AFIX   0

O1W   5    0.143497   -0.780973    0.232945    11.00000    0.03845    0.07731 =
         0.13740   -0.04427   -0.00686    0.00794
AFIX   3
H1WA  2    0.142477   -0.892133    0.178545    11.00000   -1.50000
H1WB  2    0.106197   -0.753113    0.234185    11.00000   -1.50000
AFIX   0

I1    3    0.400655    0.242998    0.501800    11.00000    0.03268    0.03419 =
         0.04878   -0.00366   -0.00137   -0.00374
I2    3    0.396823    0.262282    0.979562    11.00000    0.03531    0.05739 =
         0.04616    0.00432    0.00085   -0.00198
I3    3    0.514311    0.762765    0.751561    11.00000    0.04933    0.02794 =
         0.08971    0.00322    0.01552   -0.00154
PB1   6    0.505041    0.262031    0.757505    11.00000    0.03571    0.03585 =
         0.04163    0.00057   -0.00013   -0.00110
HKLF 5




REM  shi_4452_ilgu_twin1_hklf4_b.res in C2
REM wR2 = 0.2665, GooF = S = 1.086, Restrained GooF = 1.082 for all data
REM R1 = 0.0873 for 3066 Fo > 4sig(Fo) and 0.0946 for all 3595 data
REM 103 parameters refined using 38 restraints

END

WGHT      0.2000      0.0000

REM Instructions for potential hydrogen bonds
EQIV $8 x, y, z-1
HTAB C3 I2_$8
HTAB N1 I1
HTAB N1 I1_$2
HTAB N1 O1_$1
HTAB O2 O1W
HTAB O1W I2_$4
HTAB O1W I3_$4

REM Highest difference peak  3.369,  deepest hole -3.007,  1-sigma level  0.500
Q1    1   0.5071  0.2004  0.6528  11.00000  0.05    3.37
Q2    1   0.3990  0.2616  1.0816  11.00000  0.05    3.26
Q3    1   0.5044  0.4229  0.7631  11.00000  0.05    3.07
Q4    1   0.5083  0.3139  0.6549  11.00000  0.05    2.97
Q5    1   0.3953  0.2680  0.6012  11.00000  0.05    2.96
Q6    1   0.5034  0.0997  0.7629  11.00000  0.05    2.96
Q7    1   0.4944  0.2305  0.8749  11.00000  0.05    2.38
Q8    1   0.4963  0.3087  0.8643  11.00000  0.05    2.26
Q9    1   0.3984  0.3918  0.4864  11.00000  0.05    2.10
Q10   1   0.3984  0.0979  0.4930  11.00000  0.05    1.87
;
_shelx_res_checksum              62507
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.659(5)
2 0.341(5)

####################################################################### 
# 
# 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_shi_4459_ilgu
_database_code_depnum_ccdc_archive 'CCDC 2058839'
loop_
_audit_author_name
_audit_author_address
'Ilya Guralskiy'
;Taras Shevchenko National University of Kyiv
Ukraine
;
_audit_update_record             
;
2021-01-26 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_audit_creation_date             2020-12-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H8 N O2, H2 O'
_chemical_formula_sum            'C3 H10 Br3 N O3 Pb'
_chemical_formula_weight         555.04
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'

_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           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   21.8559(18)
_cell_length_b                   6.0868(6)
_cell_length_c                   8.7692(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.177(8)
_cell_angle_gamma                90
_cell_volume                     1164.80(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1531
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7230
_cell_measurement_theta_min      1.8660
_shelx_estimated_absorpt_T_max   0.371
_shelx_estimated_absorpt_T_min   0.050
_exptl_absorpt_coefficient_mu    24.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    3.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2397
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.353
_diffrn_reflns_theta_min         1.866
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  46.00   1.00   20.00    --  -15.52  77.00  30.00   74
  2  ω      6.00  51.00   1.00   20.00    --  -15.52  77.00-150.00   45
  3  ω     -9.00  86.00   1.00   20.00    --   17.94  77.00  90.00   95
  4  ω     11.00  79.00   1.00   20.00    --   17.94  77.00-180.00   68
  5  ω      9.00  71.00   1.00   20.00    --   17.94  77.00 -90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2024
_reflns_number_total             2397
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         5.166
_refine_diff_density_min         -4.146
_refine_diff_density_rms         0.387
_refine_ls_abs_structure_details 
;
 Flack x determined using 661 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0603
_refine_ls_restrained_S_all      1.048
_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)+(0.0697P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1506
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.665(7)
 0.335(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 O2B-C1 \\sim O2A-C1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(O2A) = Uiso(O2B)
5. Others
 Fixed Sof: O2A(0.5) H2A(0.5) O2B(0.5) H2B(0.5)
6.a Riding coordinates:
 O2A(H2A), O2B(H2B), O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 C2(H2)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_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
Br1 Br 0.40570(10) 0.8423(5) 1.0008(3) 0.0349(6) Uani 1 1 d . . . . .
Br2 Br 0.48751(11) 0.3717(12) 0.7519(3) 0.0530(8) Uani 1 1 d . . . . .
Br3 Br 0.40331(10) 0.8565(8) 0.4728(3) 0.0436(6) Uani 1 1 d . . . . .
Pb1 Pb 0.49591(3) 0.8568(3) 0.74440(8) 0.0291(3) Uani 1 1 d . . . . .
C1 C 0.2631(11) 0.133(5) 0.804(4) 0.043(7) Uani 1 1 d D . . . .
C2 C 0.3159(12) 0.291(4) 0.787(3) 0.031(6) Uani 1 1 d . . . . .
H2 H 0.345929 0.219678 0.724133 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2962(15) 0.492(5) 0.712(4) 0.064(10) Uani 1 1 d . . . . .
H3A H 0.267195 0.565581 0.772055 0.096 Uiso 1 1 calc R U . . .
H3B H 0.277346 0.458310 0.612906 0.096 Uiso 1 1 calc R U . . .
H3C H 0.331007 0.585462 0.699927 0.096 Uiso 1 1 calc R U . . .
N1 N 0.3448(7) 0.335(3) 0.9344(19) 0.030(4) Uani 1 1 d . . . . .
H1A H 0.378371 0.415291 0.923950 0.036 Uiso 1 1 calc R U . . .
H1B H 0.355091 0.208589 0.980125 0.036 Uiso 1 1 calc R U . . .
H1C H 0.319027 0.408051 0.990814 0.036 Uiso 1 1 calc R U . . .
O1 O 0.2484(8) 0.078(3) 0.923(2) 0.046(5) Uani 1 1 d . . . . .
O2A O 0.2362(17) 0.099(6) 0.669(3) 0.038(6) Uiso 0.5 1 d D . P A 1
H2A H 0.207862 0.001514 0.671752 0.057 Uiso 0.5 1 d R U P A 1
O2B O 0.2472(18) 0.033(6) 0.676(3) 0.038(6) Uiso 0.5 1 d D . P A 2
H2B H 0.218440 -0.062052 0.687701 0.057 Uiso 0.5 1 d R U P A 2
O1W O 0.1451(8) -0.181(3) 0.706(3) 0.073(7) Uani 1 1 d . . . . .
H1WA H 0.109331 -0.133301 0.729298 0.110 Uiso 1 1 d R U . . .
H1WB H 0.137761 -0.296751 0.657568 0.110 Uiso 1 1 d 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
Br1 0.0303(11) 0.0308(15) 0.0431(12) -0.007(2) -0.0011(9) 0.0011(17)
Br2 0.0482(15) 0.0282(16) 0.084(2) -0.0054(17) 0.0196(13) -0.002(3)
Br3 0.0328(12) 0.0596(17) 0.0385(12) 0.002(3) 0.0027(9) 0.003(3)
Pb1 0.0325(5) 0.0279(5) 0.0271(5) -0.0004(6) 0.0029(3) -0.0003(8)
C1 0.032(15) 0.036(14) 0.06(2) -0.005(15) -0.005(13) 0.004(12)
C2 0.042(14) 0.036(14) 0.018(11) -0.003(9) 0.016(10) -0.015(10)
C3 0.07(2) 0.07(2) 0.05(2) 0.028(17) -0.009(18) -0.029(18)
N1 0.021(8) 0.024(10) 0.046(11) -0.008(11) 0.021(7) -0.001(9)
O1 0.036(11) 0.052(13) 0.048(13) 0.004(9) -0.015(10) -0.014(8)
O1W 0.032(10) 0.050(14) 0.13(2) -0.040(14) -0.023(11) -0.012(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
Br1 Pb1 3.015(2) 2_657 ?
Br1 Pb1 3.073(2) . ?
Br2 Pb1 2.959(7) . ?
Br2 Pb1 3.140(7) 1_545 ?
Br3 Pb1 2.991(2) 2_656 ?
Br3 Pb1 3.039(2) . ?
C1 C2 1.52(3) . ?
C1 O1 1.16(3) . ?
C1 O2A 1.31(3) . ?
C1 O2B 1.31(3) . ?
C2 H2 0.9800 . ?
C2 C3 1.44(3) . ?
C2 N1 1.43(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
O2A H2A 0.8603 . ?
O2B H2B 0.8631 . ?
O1W H1WA 0.8670 . ?
O1W H1WB 0.8353 . ?

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
Pb1 Br1 Pb1 94.66(7) 2_657 . ?
Pb1 Br2 Pb1 172.54(10) . 1_545 ?
Pb1 Br3 Pb1 90.98(6) 2_656 . ?
Br1 Pb1 Br1 85.24(7) 2_657 . ?
Br1 Pb1 Br2 93.09(9) 2_657 1_565 ?
Br1 Pb1 Br2 88.44(10) . 1_565 ?
Br1 Pb1 Br3 175.88(10) 2_657 . ?
Br2 Pb1 Br1 84.96(9) . . ?
Br2 Pb1 Br1 89.83(10) . 2_657 ?
Br2 Pb1 Br2 172.54(10) . 1_565 ?
Br2 Pb1 Br3 88.70(12) . . ?
Br2 Pb1 Br3 93.57(12) . 2_656 ?
Br3 Pb1 Br1 98.46(7) . . ?
Br3 Pb1 Br1 172.34(7) 2_656 . ?
Br3 Pb1 Br1 87.24(7) 2_656 2_657 ?
Br3 Pb1 Br2 88.84(12) . 1_565 ?
Br3 Pb1 Br2 93.43(11) 2_656 1_565 ?
Br3 Pb1 Br3 89.02(6) 2_656 . ?
O1 C1 C2 122(2) . . ?
O1 C1 O2A 130(3) . . ?
O1 C1 O2B 125(3) . . ?
O2A C1 C2 108(3) . . ?
O2B C1 C2 112(3) . . ?
C1 C2 H2 108.2 . . ?
C3 C2 C1 112(2) . . ?
C3 C2 H2 108.2 . . ?
N1 C2 C1 109.0(19) . . ?
N1 C2 H2 108.2 . . ?
N1 C2 C3 111.1(19) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 O2A H2A 111.9 . . ?
C1 O2B H2B 111.4 . . ?
H1WA O1W H1WB 104.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Br1 0.89 2.74 3.400(19) 131.7 . yes
N1 H1A Br2 0.89 2.90 3.590(16) 135.1 . yes
N1 H1B Br1 0.89 2.49 3.318(19) 154.9 1_545 yes
N1 H1C O1 0.89 1.98 2.86(3) 168.4 4_557 yes
O2A H2A O1W 0.86 1.80 2.66(5) 170.3 . yes
O2B H2B O1W 0.86 1.77 2.61(5) 161.9 . yes
O1W H1WA Br2 0.87 2.68 3.503(19) 158.7 3_445 yes
O1W H1WB Br3 0.84 2.54 3.366(18) 169.8 4_536 yes

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
O1 C1 C2 C3 -118(3) . . . . ?
O1 C1 C2 N1 6(4) . . . . ?
O2A C1 C2 C3 55(3) . . . . ?
O2A C1 C2 N1 178(2) . . . . ?
O2B C1 C2 C3 77(3) . . . . ?
O2B C1 C2 N1 -160(2) . . . . ?

_shelx_res_file                  
;
TITL shi_4459_ilgu_c.res in C2
    shi_4459_ilgu.res
    created by SHELXL-2018/3 at 13:32:39 on 01-Dec-2020
REM Old TITL shi_4459_ilgu_a.res in C2/m
REM SHELXT solution in C2
REM R1 0.129, Rweak 0.010, Alpha 0.060, Orientation as input
REM Flack x = 0.323 ( 0.027 ) from Parsons' quotients
REM Formula found by SHELXT: C12 O1w Br6 Pb2
CELL 0.71073 21.8559 6.0868 8.7692 90 93.177 90
ZERR 4 0.0018 0.0006 0.0008 0 0.008 0
LATT -7
SYMM -X,+Y,-Z
SFAC C H Br N O Pb
UNIT 12 40 12 4 12 4
EQIV $1 +X,-1+Y,+Z
EQIV $2 0.5-X,0.5+Y,2-Z
EQIV $3 -0.5+X,-0.5+Y,+Z
EQIV $4 0.5-X,-1.5+Y,1-Z
SADI 0.01 O2B C1 O2A C1
EADP O2A O2B

L.S. 10
PLAN  7
SIZE 0.05 0.1 0.3
HTAB N1 Br1
HTAB N1 Br2
HTAB N1 Br1_$1
HTAB N1 O1_$2
HTAB O2B O1w
HTAB O1w Br2_$3
HTAB O1w Br3_$4
HTAB O2A O1w
CONF
htab
BOND $H
LIST 4
MORE -1
fmap 2
acta
SHEL 99 0.8
REM <olex2.extras>
REM <HklSrc "%.\\shi_4459_ilgu.hkl">
REM </olex2.extras>

WGHT    0.069700
BASF   0.33503
FVAR       0.59635
BR1   3    0.405701    0.842319    1.000780    11.00000    0.03027    0.03084 =
         0.04315   -0.00702   -0.00107    0.00113
BR2   3    0.487512    0.371693    0.751858    11.00000    0.04822    0.02817 =
         0.08424   -0.00536    0.01965   -0.00200
BR3   3    0.403313    0.856527    0.472784    11.00000    0.03281    0.05958 =
         0.03850    0.00222    0.00273    0.00290
PB1   6    0.495908    0.856811    0.744396    11.00000    0.03251    0.02787 =
         0.02713   -0.00037    0.00291   -0.00026
C1    1    0.263076    0.132741    0.804468    11.00000    0.03195    0.03629 =
         0.05861   -0.00512   -0.00452    0.00422
C2    1    0.315904    0.291094    0.786685    11.00000    0.04211    0.03593 =
         0.01777   -0.00254    0.01626   -0.01482
AFIX  13
H2    2    0.345929    0.219678    0.724133    11.00000   -1.20000
AFIX   0
C3    1    0.296217    0.491907    0.711614    11.00000    0.07203    0.06626 =
         0.05161    0.02766   -0.00861   -0.02875
AFIX 137
H3A   2    0.267195    0.565581    0.772055    11.00000   -1.50000
H3B   2    0.277346    0.458310    0.612906    11.00000   -1.50000
H3C   2    0.331007    0.585462    0.699927    11.00000   -1.50000
AFIX   0
N1    4    0.344846    0.334916    0.934418    11.00000    0.02093    0.02407 =
         0.04627   -0.00799    0.02092   -0.00137
AFIX 137
H1A   2    0.378371    0.415291    0.923950    11.00000   -1.20000
H1B   2    0.355091    0.208589    0.980125    11.00000   -1.20000
H1C   2    0.319027    0.408051    0.990814    11.00000   -1.20000
AFIX   0
O1    5    0.248355    0.078108    0.923280    11.00000    0.03617    0.05210 =
         0.04822    0.00384   -0.01505   -0.01434
PART 1
O2A   5    0.236192    0.099364    0.669312    10.50000    0.03775
AFIX   3
H2A   2    0.207862    0.001514    0.671752    10.50000   -1.50000
AFIX   0
PART 2
O2B   5    0.247200    0.032558    0.675761    10.50000    0.03775
AFIX   3
H2B   2    0.218440   -0.062052    0.687701    10.50000   -1.50000
AFIX   0

PART 0
O1W   5    0.145051   -0.180781    0.706168    11.00000    0.03186    0.05012 =
         0.13407   -0.03954   -0.02314   -0.01211
AFIX   3
H1WA  2    0.109331   -0.133301    0.729298    11.00000   -1.50000
H1WB  2    0.137761   -0.296751    0.657568    11.00000   -1.50000
AFIX   0
HKLF 5




REM  shi_4459_ilgu_c.res in C2
REM wR2 = 0.1506, GooF = S = 1.049, Restrained GooF = 1.048 for all data
REM R1 = 0.0603 for 2024 Fo > 4sig(Fo) and 0.0694 for all 2397 data
REM 101 parameters refined using 2 restraints

END

WGHT      0.0698      0.0000

REM Instructions for potential hydrogen bonds
EQIV $8 -x+1/2, y+1/2, -z+1
HTAB C3 O2A_$8
HTAB C3 O2B_$8
HTAB C3 Br3
HTAB N1 Br1
HTAB N1 Br2
HTAB N1 Br1_$1
HTAB N1 O1_$2
HTAB O2A O1W
HTAB O2B O1W
HTAB O1W Br2_$3
HTAB O1W Br3_$4

REM Highest difference peak  5.166,  deepest hole -4.146,  1-sigma level  0.387
Q1    1   0.4945  0.8567  0.8938  11.00000  0.05    5.17
Q2    1   0.4924  0.8574  0.6060  11.00000  0.05    3.98
Q3    1   0.4088  0.8560  0.6329  11.00000  0.05    2.35
Q4    1   0.4070  0.8455  1.1361  11.00000  0.05    2.09
Q5    1   0.4895  0.3657  0.8989  11.00000  0.05    1.75
Q6    1   0.4903  0.3749  0.6106  11.00000  0.05    1.52
Q7    1   0.4813  0.7695  0.4986  11.00000  0.05    1.31
;
_shelx_res_checksum              90870
_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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.665(7)
2 0.335(7)

