#------------------------------------------------------------------------------
#$Date: 2020-12-19 04:33:33 +0100 (Sat 19 de Dec de 2020) $
#$Revision: 260001 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/61/7706150.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_7706150
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                   8.3060(5)
_cell_length_b                   7.4959(5)
_cell_length_c                   21.5814(17)
_cell_measurement_reflns_used    961
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.9
_cell_volume                     1343.68(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      173(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  0.0506
_diffrn_reflns_av_unetI/netI     0.0269
_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            5412
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         1.887
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    13.331
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.418
_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         1.191
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.0084(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   1.235
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         651
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0269
_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)+(0.0192P)²+13.5951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                624
_reflns_number_total             651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02936j3.cif
_cod_data_source_block           T2PbCl4_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_database_code               7706150
_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 11:46:53 on 14-Jul-2020
REM Old TITL  RC14RTB
REM SHELXT solution in Cmcm: R1 0.104, Rweak 0.015, Alpha 0.010
REM <I/s>   0.326 for   60 systematic absences,  Orientation a'=b, b'=a, c'=-c
REM Formula found by SHELXT:  Pb Cl2 N2 C10

CELL  0.71075   8.3060   7.4959  21.5814   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
DFIX 0.91 N1 H2
ACTA
EADP C2 N2
EXYZ N2 C2
FREE C2 N2
OMIT -3 50
OMIT 2 0 4
LIST 6
FMAP 2
PLAN 10
WGHT    0.019200   13.595100
EXTI    0.008360
FVAR       0.30654
PB1   1    0.500000    0.151394    0.750000    10.25000    0.01952    0.02725 =
         0.03465    0.00000    0.00000    0.00000
CL1   2    0.500000    0.156732    0.617144    10.50000    0.03043    0.09106 =
         0.03760    0.00130    0.00000    0.00000
CL2   2    0.732566    0.415181    0.750000    10.50000    0.13932    0.16585 =
         0.07702    0.00000    0.00000   -0.13128
C1    4    0.000000    0.146664    0.632879    10.50000    0.08993    0.06843 =
         0.05291    0.01429    0.00000    0.00000
AFIX  43
H1    5    0.000000    0.115534    0.674593    10.50000   -1.20000
AFIX   0
N1    3    0.124466    0.172374    0.598425    11.00000    0.03760    0.07902 =
         0.08090   -0.01347   -0.02395    0.01256
H2    5    0.227218    0.155506    0.611136    11.00000    0.08223
N2    3    0.079118    0.212398    0.541999    10.50000    0.05731    0.10860 =
         0.05549   -0.00026    0.01800   -0.01014
AFIX  43
H3    5    0.140913    0.234421    0.510953    10.50000   -1.20000
AFIX   0
C2    4    0.079118    0.212398    0.541999    10.50000    0.05731    0.10860 =
         0.05549   -0.00026    0.01800   -0.01014
HKLF 4




REM  shelxt_a.res in Cmcm
REM wR2 = 0.0623, GooF = S = 1.235, Restrained GooF = 1.234 for all data
REM R1 = 0.0269 for 624 Fo > 4sig(Fo) and 0.0288 for all 651 data
REM 46 parameters refined using 1 restraints

END

WGHT      0.0190     13.5887

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  1.191,  deepest hole -1.471,  1-sigma level  0.198
Q1    1   0.7636  0.3514  0.7500  10.50000  0.05    1.19
Q2    1   0.6766  0.4724  0.7500  10.50000  0.05    1.05
Q3    1   0.5000 -0.1270  0.7500  10.25000  0.05    0.70
Q4    1   0.0000  0.3737  0.7032  10.50000  0.05    0.69
Q5    1   0.0000  0.2645  0.7500  10.25000  0.05    0.63
Q6    1   0.7006  0.1971  0.7500  10.50000  0.05    0.58
Q7    1   0.0000  0.0963  0.7500  10.25000  0.05    0.52
Q8    1   0.7100  0.6028  0.7500  10.50000  0.05    0.51
Q9    1   0.9168  0.3450  0.7500  10.50000  0.05    0.48
Q10   1   0.0000  0.2686  0.5458  10.50000  0.05    0.41
;
_shelx_res_checksum              94369
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 0.15139(6) 0.750000 0.0271(3) Uani 1 4 d S T P . .
Cl1 Cl 0.500000 0.1567(4) 0.61714(12) 0.0530(7) Uani 1 2 d S T P . .
Cl2 Cl 0.7326(6) 0.4152(8) 0.750000 0.127(2) Uani 1 2 d S T P . .
C1 C 0.000000 0.1467(18) 0.6329(7) 0.070(4) Uani 1 2 d S T P . .
H1 H 0.000000 0.115534 0.674593 0.085 Uiso 1 2 calc R U P . .
N1 N 0.1245(9) 0.1724(10) 0.5984(4) 0.066(2) Uani 1 1 d D . . . .
H2 H 0.227(5) 0.156(13) 0.611(5) 0.08(3) Uiso 1 1 d D . . . .
N2 N 0.0791(10) 0.2124(14) 0.5420(4) 0.074(2) Uani 0.5 1 d . . P . .
H3 H 0.140913 0.234421 0.510953 0.089 Uiso 0.5 1 calc R U P . .
C2 C 0.0791(10) 0.2124(14) 0.5420(4) 0.074(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 0.0195(3) 0.0273(3) 0.0347(3) 0.000 0.000 0.000
Cl1 0.0304(12) 0.091(2) 0.0376(13) 0.0013(13) 0.000 0.000
Cl2 0.139(4) 0.166(5) 0.077(2) 0.000 0.000 -0.131(4)
C1 0.090(11) 0.068(9) 0.053(7) 0.014(6) 0.000 0.000
N1 0.038(4) 0.079(5) 0.081(6) -0.013(4) -0.024(4) 0.013(3)
N2 0.057(4) 0.109(7) 0.055(5) 0.000(5) 0.018(4) -0.010(5)
C2 0.057(4) 0.109(7) 0.055(5) 0.000(5) 0.018(4) -0.010(5)
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 88.7(3) 3_656 . ?
Cl2 Pb1 Cl2 84.228(10) 3_656 5_445 ?
Cl2 Pb1 Cl2 172.9(3) . 5_445 ?
Cl2 Pb1 Cl2 172.9(3) 3_656 7_646 ?
Cl2 Pb1 Cl2 84.227(10) . 7_646 ?
Cl2 Pb1 Cl2 102.9(3) 5_445 7_646 ?
Cl2 Pb1 Cl1 89.43(5) 3_656 . ?
Cl2 Pb1 Cl1 89.43(5) . . ?
Cl2 Pb1 Cl1 90.50(4) 5_445 . ?
Cl2 Pb1 Cl1 90.50(4) 7_646 . ?
Cl2 Pb1 Cl1 89.43(5) 3_656 10_557 ?
Cl2 Pb1 Cl1 89.43(5) . 10_557 ?
Cl2 Pb1 Cl1 90.50(4) 5_445 10_557 ?
Cl2 Pb1 Cl1 90.50(4) 7_646 10_557 ?
Cl1 Pb1 Cl1 178.40(13) . 10_557 ?
Pb1 Cl2 Pb1 172.9(3) . 5 ?
N1 C1 N1 106.8(12) 12 . ?
C1 N1 N2 109.9(8) . . ?
N1 N2 N2 106.7(5) . 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 2.764(3) 3_656 ?
Pb1 Cl2 2.764(3) . ?
Pb1 Cl2 2.841(3) 5_445 ?
Pb1 Cl2 2.841(3) 7_646 ?
Pb1 Cl1 2.868(3) . ?
Pb1 Cl1 2.868(3) 10_557 ?
C1 N1 1.288(12) 12 ?
C1 N1 1.288(12) . ?
N1 N2 1.310(12) . ?
N2 N2 1.314(17) 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 0.91(2) 2.27(4) 3.147(7) 163(9) . yes
N2 H3 N2 0.86 2.62 3.415(16) 153.9 13_556 yes
