#------------------------------------------------------------------------------
#$Date: 2020-12-19 04:33:33 +0100 (Sat 19 de Dec de 2020) $
#$Revision: 260001 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/61/7706149.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7706149
loop_
_publ_author_name
'Guo, Yuan-Yuan'
'Yang, Lin-Jie'
'McNulty, Jason A.'
'Slawin, Alexandra M. Z.'
'Lightfoot, Philip'
_publ_section_title
;
 Structural variations in (001)-oriented layered lead halide perovskites,
 templated by 1,2,4-triazolium.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17274
_journal_page_last               17280
_journal_paper_doi               10.1039/d0dt02936j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'Br4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Br4 N6 Pb'
_chemical_formula_weight         666.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.016(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6451(7)
_cell_length_b                   8.4001(5)
_cell_length_c                   8.3932(5)
_cell_measurement_reflns_used    921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     674.92(8)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5445
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.988
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    24.319
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.279
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.322
_refine_ls_extinction_coef       0.0057(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0263
_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)+(0.0438P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1076
_reflns_number_total             1172
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02936j3.cif
_cod_data_source_block           T2PbBr4-II_173K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7706149
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/c
    shelx.res
    created by SHELXL-2018/3 at 15:06:01 on 15-Aug-2020
REM Old TITL  RC14RTB
REM SHELXT solution in P2(1)/c: R1 0.059, Rweak 0.004, Alpha 0.016
REM <I/s>   0.565 for  102 systematic absences,  Orientation a'=c, b'=-b, c'=a
REM Formula found by SHELXT:  Pb Br4 N6 C4

CELL  0.71075   9.6451   8.4001   8.3932   90.000   97.016   90.000
ZERR    2.000   0.0007   0.0005   0.0005    0.000    0.008    0.000
LATT  1
SYMM -X, 1/2+Y, 1/2-Z
SFAC PB BR N C H
UNIT 2  8 12 8 16
L.S. 10
BOND
HTAB
EQIV $5 x, y, z+1
HTAB N1 Br1_$5
EQIV $6 -x+1, -y+1, -z+2
HTAB N1 Br2_$6
HTAB N3 Br1
ACTA
OMIT -3 50
OMIT -1 2 2
LIST 6
FMAP 2
PLAN 20
WGHT    0.043800
EXTI    0.005700
FVAR       0.39649
PB1   1    0.500000    0.500000    0.500000    10.50000    0.01441    0.01006 =
         0.00991   -0.00001    0.00021    0.00057
BR1   2    0.191866    0.563919    0.441498    11.00000    0.01674    0.02534 =
         0.01702    0.00107    0.00115   -0.00252
BR2   2    0.491810    0.282047    0.780737    11.00000    0.02475    0.02057 =
         0.02048    0.00976    0.00420    0.00313
N1    3    0.212409    0.472950    1.052984    11.00000    0.03143    0.01981 =
         0.02254    0.00030   -0.00956   -0.00116
AFIX  43
H1    5    0.253709    0.511912    1.140998    11.00000   -1.20000
AFIX   0
N2    3    0.115392    0.356473    1.045965    11.00000    0.03506    0.02809 =
         0.01763    0.00164    0.00137   -0.00200
N3    3    0.153827    0.433705    0.806571    11.00000    0.02570    0.02940 =
         0.01323   -0.00343    0.00424    0.00396
AFIX  43
H2    5    0.147345    0.439191    0.703612    11.00000   -1.20000
AFIX   0
C1    4    0.081335    0.335208    0.892957    11.00000    0.02710    0.01759 =
         0.02465   -0.00004   -0.00438    0.00286
AFIX  43
H1A   5    0.015549    0.261677    0.848624    11.00000   -1.20000
AFIX   0
C2    4    0.236270    0.519751    0.909425    11.00000    0.01672    0.02018 =
         0.03261    0.00316    0.00828    0.00106
AFIX  43
H2A   5    0.298785    0.597890    0.885369    11.00000   -1.20000
AFIX   0
HKLF 4




REM  shelxt_a.res in P2(1)/c
REM wR2 = 0.0675, GooF = S = 1.082, Restrained GooF = 1.082 for all data
REM R1 = 0.0263 for 1076 Fo > 4sig(Fo) and 0.0285 for all 1172 data
REM 71 parameters refined using 0 restraints

END

WGHT      0.0437      0.0000

REM Instructions for potential hydrogen bonds
HTAB N1 Br1_$5
HTAB N1 Br2_$6
HTAB N3 Br1
EQIV $7 x, -y+3/2, z+1/2
HTAB C2 Br1_$7
EQIV $3 -x+1, y+1/2, -z+3/2
HTAB C2 Br2_$3

REM Highest difference peak  2.279,  deepest hole -1.081,  1-sigma level  0.322
Q1    1   0.4948  0.3731  0.6382  11.00000  0.05    2.28
Q2    1   0.5007  0.1307  0.8701  11.00000  0.05    1.98
Q3    1   0.4625  0.3207  0.5057  11.00000  0.05    0.96
Q4    1   0.5444  0.3236  0.4956  11.00000  0.05    0.95
Q5    1   0.1872  0.6552  0.6649  11.00000  0.05    0.94
Q6    1   0.1846  0.1718  1.0231  11.00000  0.05    0.92
Q7    1   0.5464  0.2806  0.9541  11.00000  0.05    0.87
Q8    1   0.4540  0.5040  0.2992  11.00000  0.05    0.83
Q9    1   0.1222  0.2967  0.9780  11.00000  0.05    0.83
Q10   1   0.3947  0.7778  1.0104  11.00000  0.05    0.81
Q11   1   0.1367  0.6934  0.9920  11.00000  0.05    0.80
Q12   1   0.1874  0.4803  0.3723  11.00000  0.05    0.77
Q13   1  -0.0763  0.2956  1.0093  11.00000  0.05    0.77
Q14   1   0.5024  0.1394  0.6368  11.00000  0.05    0.77
Q15   1   0.4651  0.2766  1.0159  11.00000  0.05    0.72
Q16   1   0.4523  0.4666  0.7773  11.00000  0.05    0.72
Q17   1   0.3867  0.4737  1.1975  11.00000  0.05    0.71
Q18   1   0.4006  0.2507  0.9780  11.00000  0.05    0.66
Q19   1   0.2734  0.4575  1.2214  11.00000  0.05    0.66
Q20   1   0.0326  0.2763  0.9992  11.00000  0.05    0.65
;
_shelx_res_checksum              57183
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.500000 0.500000 0.500000 0.01156(18) Uani 1 2 d S . P . .
Br1 Br 0.19187(6) 0.56392(8) 0.44150(7) 0.0198(2) Uani 1 1 d . . . . .
Br2 Br 0.49181(7) 0.28205(8) 0.78074(8) 0.0218(2) Uani 1 1 d . . . . .
N1 N 0.2124(7) 0.4730(7) 1.0530(8) 0.0257(14) Uani 1 1 d . . . . .
H1 H 0.253709 0.511912 1.140998 0.031 Uiso 1 1 calc R U . . .
N2 N 0.1154(6) 0.3565(7) 1.0460(7) 0.0271(13) Uani 1 1 d . . . . .
N3 N 0.1538(6) 0.4337(7) 0.8066(7) 0.0226(13) Uani 1 1 d . . . . .
H2 H 0.147345 0.439191 0.703612 0.027 Uiso 1 1 calc R U . . .
C1 C 0.0813(7) 0.3352(8) 0.8930(8) 0.0237(15) Uani 1 1 d . . . . .
H1A H 0.015549 0.261677 0.848624 0.028 Uiso 1 1 calc R U . . .
C2 C 0.2363(8) 0.5198(8) 0.9094(9) 0.0227(16) Uani 1 1 d . . . . .
H2A H 0.298785 0.597890 0.885369 0.027 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0144(2) 0.0101(2) 0.0099(2) -0.00001(11) 0.00021(14) 0.00057(11)
Br1 0.0167(3) 0.0253(4) 0.0170(4) 0.0011(3) 0.0011(2) -0.0025(3)
Br2 0.0248(4) 0.0206(3) 0.0205(4) 0.0098(3) 0.0042(3) 0.0031(3)
N1 0.031(4) 0.020(3) 0.023(3) 0.000(3) -0.010(3) -0.001(2)
N2 0.035(3) 0.028(3) 0.018(3) 0.002(3) 0.001(2) -0.002(3)
N3 0.026(3) 0.029(3) 0.013(3) -0.003(2) 0.004(2) 0.004(3)
C1 0.027(4) 0.018(3) 0.025(4) 0.000(3) -0.004(3) 0.003(3)
C2 0.017(4) 0.020(4) 0.033(4) 0.003(3) 0.008(3) 0.001(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
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'
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
Br2 Pb1 Br2 180.0 . 3_666 ?
Br2 Pb1 Br2 89.920(6) . 4_565 ?
Br2 Pb1 Br2 90.080(6) 3_666 4_565 ?
Br2 Pb1 Br2 90.080(6) . 2_656 ?
Br2 Pb1 Br2 89.920(6) 3_666 2_656 ?
Br2 Pb1 Br2 180.00(2) 4_565 2_656 ?
Br2 Pb1 Br1 96.744(18) . . ?
Br2 Pb1 Br1 83.257(18) 3_666 . ?
Br2 Pb1 Br1 95.147(18) 4_565 . ?
Br2 Pb1 Br1 84.853(18) 2_656 . ?
Br2 Pb1 Br1 83.256(19) . 3_666 ?
Br2 Pb1 Br1 96.743(19) 3_666 3_666 ?
Br2 Pb1 Br1 84.853(18) 4_565 3_666 ?
Br2 Pb1 Br1 95.147(18) 2_656 3_666 ?
Br1 Pb1 Br1 180.0 . 3_666 ?
Pb1 Br2 Pb1 165.12(3) . 2_646 ?
C2 N1 N2 112.0(6) . . ?
C1 N2 N1 103.5(6) . . ?
C2 N3 C1 107.2(6) . . ?
N2 C1 N3 111.2(6) . . ?
N1 C2 N3 106.1(6) . . ?
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 Br2 2.9926(6) . ?
Pb1 Br2 2.9926(6) 3_666 ?
Pb1 Br2 2.9951(6) 4_565 ?
Pb1 Br2 2.9951(6) 2_656 ?
Pb1 Br1 3.0009(6) . ?
Pb1 Br1 3.0009(6) 3_666 ?
N1 C2 1.314(10) . ?
N1 N2 1.350(9) . ?
N2 C1 1.298(9) . ?
N3 C2 1.316(10) . ?
N3 C1 1.350(9) . ?
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 H1 Br1 0.86 2.70 3.379(7) 137.1 1_556 yes
N1 H1 Br2 0.86 3.01 3.654(6) 133.3 3_667 yes
N3 H2 Br1 0.86 2.52 3.316(6) 154.2 . yes
