#------------------------------------------------------------------------------
#$Date: 2019-11-24 17:27:07 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238823 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/79/7237999.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_7237999
loop_
_publ_author_name
'Wei, Wen-Juan'
'Li, Chao'
'Li, Lin-Sui'
'Tang, Yun-Zhi'
'Jiang, Xing-Xing'
'Lin, Zhe-Shuai'
_publ_section_title
;
 Phase transition, optical and dielectric properties regulated by
 anion-substitution in a homologous series of 2D hybrid organic--inorganic
 perovskites
;
_journal_issue                   38
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              11964
_journal_paper_doi               10.1039/C9TC04479E
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'Cl8 Pb2, 4(C5.32 N S0.68)'
_chemical_formula_sum            'C21.28 Cl8 N4 Pb2 S2.72'
_chemical_formula_weight         1096.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.397(7)
_cell_length_b                   7.7997(13)
_cell_length_c                   7.7943(14)
_cell_measurement_reflns_used    2448
_cell_measurement_temperature    415
_cell_measurement_theta_max      27.430
_cell_measurement_theta_min      2.514
_cell_volume                     1969.5(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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)'
_diffrn_ambient_temperature      415
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6234
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.586
_diffrn_reflns_theta_min         3.749
_exptl_absorpt_coefficient_mu    9.240
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4328
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.688
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1160
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0291
_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)+(0.0374P)²+1.1929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                787
_reflns_number_total             1160
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9tc04479e2.cif
_cod_data_source_block           mo_ly18_2415k_0m
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               7237999
_shelx_shelxl_version_number     2014/7
_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_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.168
_olex2_refinement_description
;
1. Shared sites
{S10, C0AA}
2. Uiso/Uaniso restraints and constraints
Uanis(S10) = Uanis(C0AA)
3. Rigid body (RIGU) restrains
 C2, S10, C1, C3, C0AA, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C0AA)=1-FVAR(1)
 Sof(S10)=FVAR(1)
 Fixed Sof: N1(0.5)
;
_shelx_res_file
;
    mo_ly18_2415k_0m.res created by SHELXL-2014/7

TITL mo_ly18_2415k_0m_a.res in Cmca
REM Old TITL mo_ly18_2415k_0m_b.res in Cmmm
REM SHELXT solution in Cmca
REM R1 0.278, Rweak 0.001, Alpha 0.016, Orientation as input
REM Formula found by SHELXT: C2 Cl4 Pb
CELL 0.71073 32.3975 7.7997 7.7943 90 90 90
ZERR 2 0.0067 0.0013 0.0014 0 0 0
LATT 7
SYMM -X,0.5-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC C Cl N Pb S
UNIT 42.56 16 8 4 5.44
EQIV $1 +X,-Y,1-Z
RIGU 0.001 0.001 C2 S10 C1 C3 C0AA N1
EADP S10 C0AA
EXYZ S10 C0AA

L.S. 10
PLAN  20
SIZE 0.1 0.2 0.3
TEMP 141.85
FREE S10 S10_$1
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\mo_LY18_2415K_0m.hkl">
REM </olex2.extras>

WGHT    0.037400    1.192900
FVAR       0.23468   0.33974
PB1   4    0.500000    0.500000    0.500000    10.25000    0.10056    0.04199 =
         0.04103    0.00001    0.00000    0.00000
CL2   2    0.500000    0.181244    0.318987    10.50000    0.14310    0.06404 =
         0.06368   -0.02314    0.00000    0.00000
CL1   2    0.587670    0.500000    0.500000    10.50000    0.10542    0.12643 =
         0.11978   -0.00066    0.00000    0.00000
PART 1
S10   5    0.674229   -0.116366    0.616661    21.00000    0.18189    0.28875 =
         0.24477    0.07013   -0.01614    0.03936
PART 0
C2    1    0.647482    0.000000    0.500000    10.50000    0.14612    0.18683 =
         0.16538    0.00874    0.00000    0.00000
C1    1    0.714185   -0.066608    0.558505    11.00000    0.18200    0.34629 =
         0.26779    0.07109   -0.01092    0.02585
PART -1
N1    3    0.580017    0.073834    0.576164    10.50000    0.13349    0.08864 =
         0.10416    0.04814   -0.00895   -0.01551
PART 0
C3    1    0.601929    0.000000    0.500000    10.50000    0.15243    0.14433 =
         0.14982    0.01764    0.00000    0.00000
PART 2
C0AA  1    0.674229   -0.116366    0.616661   -21.00000    0.18189    0.28875 =
         0.24477    0.07013   -0.01614    0.03936
HKLF 4

REM  mo_ly18_2415k_0m_a.res in Cmca
REM R1 =  0.0291 for     787 Fo > 4sig(Fo)  and  0.0488 for all    1160 data
REM     54 parameters refined using     30 restraints

END

WGHT      0.0418      2.2481

REM Highest difference peak  0.688,  deepest hole -1.221,  1-sigma level  0.097
Q1    1   0.5384  0.5000  0.5000  10.50000  0.05    0.61
Q2    1   0.5822  0.1236  0.5258  11.00000  0.05    0.41
Q3    1   0.5888  0.0125  0.6497  11.00000  0.05    0.37
Q4    1   0.7297 -0.0258  0.4713  11.00000  0.05    0.34
Q5    1   0.6825 -0.1487  0.4895  11.00000  0.05    0.33
Q6    1   0.5669  0.0188  0.5852  11.00000  0.05    0.32
Q7    1   0.6083  0.1013  0.5222  11.00000  0.05    0.29
Q8    1   0.6554 -0.1809  0.6657  11.00000  0.05    0.26
Q9    1   0.7088 -0.1751  0.6590  11.00000  0.05    0.22
Q10   1   0.6884 -0.0452  0.6276  11.00000  0.05    0.21
Q11   1   0.5000  0.4748  0.5779  10.50000  0.05    0.21
Q12   1   0.5325  0.2368  0.2730  11.00000  0.05    0.21
Q13   1   0.6718  0.0044  0.6715  11.00000  0.05    0.20
Q14   1   0.5956  0.1968  0.4003  11.00000  0.05    0.19
Q15   1   0.5412  0.3705  0.3037  11.00000  0.05    0.19
Q16   1   0.4541  0.2468  0.2511  11.00000  0.05    0.19
Q17   1   0.5784  0.2643  0.5072  11.00000  0.05    0.18
Q18   1   0.5000  0.2071  0.4919  10.50000  0.05    0.18
Q19   1   0.7219 -0.2362  0.6665  11.00000  0.05    0.18
Q20   1   0.5491  0.4814  0.6988  11.00000  0.05    0.18
;
_shelx_res_checksum              46052
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, 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 0.5000 0.5000 0.5000 0.06120(17) Uani 1 4 d S T P . .
Cl2 Cl 0.5000 0.1812(2) 0.3190(3) 0.0903(6) Uani 1 2 d S T P . .
Cl1 Cl 0.58767(10) 0.5000 0.5000 0.1172(10) Uani 1 2 d S T P . .
S10 S 0.6742(2) -0.1164(12) 0.6167(12) 0.238(6) Uani 0.340(17) 1 d . U . A 1
C2 C 0.6475(6) 0.0000 0.5000 0.166(5) Uani 1 2 d S TU P . .
C1 C 0.7142(6) -0.067(4) 0.559(3) 0.265(9) Uani 1 1 d . U . . .
N1 N 0.5800(4) 0.0738(16) 0.5762(18) 0.109(3) Uani 0.5 1 d . U . A -1
C3 C 0.6019(7) 0.0000 0.5000 0.149(4) Uani 1 2 d S TU P A .
C0AA C 0.6742(2) -0.1164(12) 0.6167(12) 0.238(6) Uani 0.660(17) 1 d . U . A 2
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 0.1006(3) 0.0420(2) 0.0410(2) 0.00001(14) 0.000 0.000
Cl2 0.1431(18) 0.0640(9) 0.0637(11) -0.0231(10) 0.000 0.000
Cl1 0.1054(19) 0.126(3) 0.120(3) -0.0007(14) 0.000 0.000
S10 0.182(5) 0.289(11) 0.245(10) 0.070(9) -0.016(4) 0.039(4)
C2 0.146(6) 0.187(10) 0.165(9) 0.009(6) 0.000 0.000
C1 0.182(6) 0.346(17) 0.268(15) 0.071(13) -0.011(4) 0.026(4)
N1 0.133(6) 0.089(7) 0.104(8) 0.048(6) -0.009(4) -0.016(4)
C3 0.152(6) 0.144(9) 0.150(9) 0.018(6) 0.000 0.000
C0AA 0.182(5) 0.289(11) 0.245(10) 0.070(9) -0.016(4) 0.039(4)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
Cl2 Pb1 Cl2 180.0 9_666 .
Cl2 Pb1 Cl2 180.0 2_655 10_566
Cl2 Pb1 Cl2 90.05(2) . 10_566
Cl2 Pb1 Cl2 89.95(2) . 2_655
Cl2 Pb1 Cl2 89.95(2) 9_666 10_566
Cl2 Pb1 Cl2 90.05(2) 9_666 2_655
Cl1 Pb1 Cl2 90.0 9_666 2_655
Cl1 Pb1 Cl2 90.0 . 9_666
Cl1 Pb1 Cl2 90.0 . .
Cl1 Pb1 Cl2 90.0 . 2_655
Cl1 Pb1 Cl2 90.0 9_666 .
Cl1 Pb1 Cl2 90.0 9_666 9_666
Cl1 Pb1 Cl2 90.0 9_666 10_566
Cl1 Pb1 Cl2 90.0 . 10_566
Cl1 Pb1 Cl1 180.0 9_666 .
Pb1 Cl2 Pb1 149.20(8) . 2_654
C1 S10 C2 99.3(11) . .
S10 C2 S10 112.0(14) 4_556 .
C3 C2 S10 124.0(7) . .
C3 C2 S10 124.0(7) . 4_556
C3 C2 C0AA 124.0(7) . 4_556
C3 C2 C0AA 124.0(7) . .
C0AA C2 C0AA 112.0(14) . 4_556
C1 C1 S10 114.5(9) 4_556 .
C1 C1 C0AA 114.5(9) 4_556 .
N1 C3 C2 130.6(12) . .
C1 C0AA C2 99.3(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Cl2 2.8586(17) 9_666
Pb1 Cl2 2.8601(18) 10_566
Pb1 Cl2 2.8601(18) 2_655
Pb1 Cl2 2.8586(17) .
Pb1 Cl1 2.840(3) .
Pb1 Cl1 2.840(3) 9_666
Cl2 Pb1 2.8601(18) 2_654
S10 C2 1.550(12) .
S10 C1 1.425(18) .
C2 S10 1.550(12) 4_556
C2 C3 1.48(3) .
C2 C0AA 1.550(12) .
C2 C0AA 1.550(12) 4_556
C1 C1 1.38(4) 4_556
C1 C0AA 1.425(18) .
N1 C3 1.090(16) .
