#------------------------------------------------------------------------------
#$Date: 2020-12-19 04:33:33 +0100 (Sat 19 de Dec de 2020) $
#$Revision: 260001 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/61/7706148.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_7706148
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         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3092(5)
_cell_length_b                   7.5086(5)
_cell_length_c                   21.5925(17)
_cell_measurement_reflns_used    948
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.9
_cell_volume                     1347.17(16)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5443
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         1.886
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    13.296
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.0063(5)
_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   1.229
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         653
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0240
_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)+(0.0234P)²+6.7571P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                636
_reflns_number_total             653
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02936j3.cif
_cod_data_source_block           T2PbCl4_298K
_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_database_code               7706148
_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 Cmcm
    shelx.res
    created by SHELXL-2018/3 at 11:50:16 on 14-Jul-2020
REM Old TITL  YGPL113
REM SHELXT solution in Cmcm: R1 0.095, Rweak 0.015, Alpha 0.016
REM <I/s>   0.236 for   59 systematic absences,  Orientation a'=b, b'=a, c'=-c
REM Formula found by SHELXT:  Pb Cl4 C10

CELL  0.71075   8.3092   7.5086  21.5925   90.000   90.000   90.000
ZERR    4.000   0.0005   0.0005   0.0017    0.000    0.000    0.000
LATT  7
SYMM -X, -Y, 1/2+Z
SYMM -X, Y, 1/2-Z
SYMM X, -Y, -Z
SFAC PB CL N C H
UNIT 4  16  24 16 32
L.S. 10
BOND
HTAB
HTAB N1 Cl1
EQIV $8 -x+1/2, -y+1/2, -z+1
HTAB N2 N2_$8
ACTA
DFIX 0.91 N1 H2
EADP C2 N2
EXYZ N2 C2
FREE C2 N2
OMIT -3 50
OMIT 2 2 1
LIST 6
FMAP 2
PLAN 10
WGHT    0.023400    6.757100
EXTI    0.006262
FVAR       0.29696
PB1   1    0.500000    0.154449    0.750000    10.25000    0.01978    0.02823 =
         0.03479    0.00000    0.00000    0.00000
CL1   2    0.500000    0.159608    0.617261    10.50000    0.03075    0.09545 =
         0.03813    0.00146    0.00000    0.00000
CL2   2    0.733767    0.418492    0.750000    10.50000    0.13180    0.15523 =
         0.08012    0.00000    0.00000   -0.12163
C1    4    0.000000    0.150579    0.633341    10.50000    0.08385    0.07626 =
         0.05281    0.01191    0.00000    0.00000
AFIX  43
H1    5    0.000000    0.122003    0.675250    10.50000   -1.20000
AFIX   0
N1    3    0.123464    0.174124    0.598809    11.00000    0.03802    0.08411 =
         0.08001   -0.01251   -0.02261    0.01148
H2    5    0.227488    0.168203    0.610528    11.00000    0.10208
N2    3    0.079110    0.214040    0.542137    10.50000    0.05845    0.12112 =
         0.05658    0.00169    0.01884   -0.00974
AFIX  43
H3    5    0.141177    0.235844    0.511180    10.50000   -1.20000
AFIX   0
C2    4    0.079110    0.214040    0.542137    10.50000    0.05845    0.12112 =
         0.05658    0.00169    0.01884   -0.00974
HKLF 4




REM  shelxt_a.res in Cmcm
REM wR2 = 0.0559, GooF = S = 1.229, Restrained GooF = 1.228 for all data
REM R1 = 0.0240 for 636 Fo > 4sig(Fo) and 0.0250 for all 653 data
REM 46 parameters refined using 1 restraints

END

WGHT      0.0234      6.7652

REM Instructions for potential hydrogen bonds
EQIV $3 x-1/2, y-1/2, z
HTAB C1 Cl2_$3
EQIV $7 -x+1/2, y-1/2, -z+3/2
HTAB C1 Cl2_$7
HTAB N1 Cl1
HTAB N2 N2_$8

REM Highest difference peak  1.091,  deepest hole -1.261,  1-sigma level  0.171
Q1    1   0.7580  0.3498  0.7500  10.50000  0.05    1.09
Q2    1   0.6779  0.4698  0.7500  10.50000  0.05    0.96
Q3    1   0.0000  0.0999  0.7500  10.25000  0.05    0.57
Q4    1   0.0000  0.2801  0.7500  10.25000  0.05    0.53
Q5    1   0.0000  0.2637  0.5435  10.50000  0.05    0.43
Q6    1   0.5000  0.0275  0.7500  10.25000  0.05    0.38
Q7    1   0.0717  0.1054  0.6096  11.00000  0.05    0.33
Q8    1   0.9006  0.3677  0.7500  10.50000  0.05    0.32
Q9    1   0.0585  0.1592  0.5403  11.00000  0.05    0.30
Q10   1   0.9128  0.3982  0.8214  11.00000  0.05    0.26
;
_shelx_res_checksum              8438
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
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 0.15445(5) 0.750000 0.0276(2) Uani 1 4 d S T P . .
Cl1 Cl 0.500000 0.1596(4) 0.61726(11) 0.0548(6) Uani 1 2 d S T P . .
Cl2 Cl 0.7338(5) 0.4185(6) 0.750000 0.1224(18) Uani 1 2 d S T P . .
C1 C 0.000000 0.1506(15) 0.6333(6) 0.071(3) Uani 1 2 d S T P . .
H1 H 0.000000 0.122003 0.675250 0.085 Uiso 1 2 calc R U P . .
N1 N 0.1235(8) 0.1741(9) 0.5988(4) 0.0674(19) Uani 1 1 d D . . . .
H2 H 0.227(4) 0.168(13) 0.611(5) 0.10(3) Uiso 1 1 d D . . . .
N2 N 0.0791(9) 0.2140(13) 0.5421(4) 0.079(2) Uani 0.5 1 d . . P . .
H3 H 0.141177 0.235844 0.511180 0.094 Uiso 0.5 1 calc R U P . .
C2 C 0.0791(9) 0.2140(13) 0.5421(4) 0.079(2) Uani 0.5 1 d . . P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0198(3) 0.0282(3) 0.0348(3) 0.000 0.000 0.000
Cl1 0.0307(10) 0.0954(19) 0.0381(11) 0.0015(11) 0.000 0.000
Cl2 0.132(3) 0.155(4) 0.080(2) 0.000 0.000 -0.122(3)
C1 0.084(9) 0.076(8) 0.053(7) 0.012(5) 0.000 0.000
N1 0.038(3) 0.084(5) 0.080(5) -0.013(3) -0.023(3) 0.011(3)
N2 0.058(4) 0.121(6) 0.057(4) 0.002(4) 0.019(4) -0.010(4)
C2 0.058(4) 0.121(6) 0.057(4) 0.002(4) 0.019(4) -0.010(4)
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'
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'
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
Cl2 Pb1 Cl2 88.8(2) 3_656 . ?
Cl2 Pb1 Cl2 84.277(8) 3_656 5_445 ?
Cl2 Pb1 Cl2 173.1(2) . 5_445 ?
Cl2 Pb1 Cl2 173.1(2) 3_656 7_646 ?
Cl2 Pb1 Cl2 84.277(8) . 7_646 ?
Cl2 Pb1 Cl2 102.6(2) 5_445 7_646 ?
Cl2 Pb1 Cl1 89.45(4) 3_656 10_557 ?
Cl2 Pb1 Cl1 89.45(4) . 10_557 ?
Cl2 Pb1 Cl1 90.48(3) 5_445 10_557 ?
Cl2 Pb1 Cl1 90.48(3) 7_646 10_557 ?
Cl2 Pb1 Cl1 89.45(4) 3_656 . ?
Cl2 Pb1 Cl1 89.45(4) . . ?
Cl2 Pb1 Cl1 90.48(3) 5_445 . ?
Cl2 Pb1 Cl1 90.48(3) 7_646 . ?
Cl1 Pb1 Cl1 178.45(11) 10_557 . ?
Pb1 Cl2 Pb1 173.1(2) . 5 ?
N1 C1 N1 106.5(11) . 12 ?
C1 N1 N2 110.5(7) . . ?
N1 N2 N2 106.3(4) . 12 ?
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 Cl2 2.776(3) 3_656 ?
Pb1 Cl2 2.776(3) . ?
Pb1 Cl2 2.834(3) 5_445 ?
Pb1 Cl2 2.834(3) 7_646 ?
Pb1 Cl1 2.866(2) 10_557 ?
Pb1 Cl1 2.866(2) . ?
C1 N1 1.280(10) . ?
C1 N1 1.281(10) 12 ?
N1 N2 1.313(10) . ?
N2 N2 1.315(15) 12 ?
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 H2 Cl1 0.90(2) 2.27(3) 3.156(6) 167(10) . yes
N2 H3 N2 0.86 2.62 3.416(14) 154.2 13_556 yes
