#------------------------------------------------------------------------------
#$Date: 2018-11-10 01:21:05 +0200 (Sat, 10 Nov 2018) $
#$Revision: 211871 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/02/1550207.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_1550207
loop_
_publ_author_name
'Li, Tianyang'
'Dunlap-Shohl, Wiley'
'Reinheimer, Eric W.'
'LeMagueres, Pierre'
'Mitzi, David B.'
_publ_section_title
;
 Melting Temperature Suppression of Layered Hybrid Lead Halide Perovskites
 via Organic Ammonium Cation Branching
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03863E
_journal_year                    2019
_chemical_formula_moiety         '0.5(I8 Pb2), C8 H26 N2'
_chemical_formula_sum            'C8 H26 I4 N2 Pb'
_chemical_formula_weight         865.10
_space_group_crystal_system      tetragonal
_space_group_IT_number           138
_space_group_name_Hall           '-P 4ac 2ac'
_space_group_name_H-M_alt        'P 42/n c m'
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-24 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9353(2)
_cell_length_b                   8.9353(2)
_cell_length_c                   24.9636(13)
_cell_measurement_reflns_used    6263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2310
_cell_measurement_theta_min      2.7640
_cell_volume                     1993.08(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.3a (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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11096
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.804
_diffrn_source                   'microfocused sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.644
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'metallic orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.883
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.749
_refine_diff_density_min         -2.003
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         972
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          1.026
_refine_ls_shift/su_mean         0.087
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1568P)²+7.2173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                905
_reflns_number_total             972
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc03863e2.cif
_cod_data_source_block           1me-pa_roomt_feb
_cod_original_cell_volume        1993.10(15)
_cod_database_code               1550207
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3
 1.47 with sigma of 0.02
 C4-C8
 1.54 with sigma of 0.02
 C8-C4 \\sim C4-C3
 with sigma of 0.001
 C5-C3 \\sim C4-C3
 with sigma of 0.001
 C8-C4 \\sim C4-C3 \\sim C5-C3
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C4) = Uanis(C3) = Uanis(N1)
Uanis(C8) = Uanis(C4) = Uanis(C5) = Uanis(C3) = Uanis(N1)
Uanis(C3) = Uanis(C8)
4. Rigid body (RIGU) restrains
 N1, C3, C4, C5, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) C4(0.5) H4A(0.5) H4B(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
6.a Ternary CH refined with riding coordinates:
 C3(H3B), C3(H3A)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C)
;
_shelx_res_file
;
    1me-pa_roomt_feb.res created by SHELXL-2014/7

TITL Me-PA_RoomT in P4(2)/ncm
CELL 0.71073 8.935346 8.935346 24.963554 90 90 90
ZERR 4 0.000237 0.000237 0.001316 0 0 0
LATT 1
SYMM 0.5-Y,+X,0.5+Z
SYMM 0.5-X,0.5-Y,+Z
SYMM +Y,0.5-X,0.5+Z
SYMM 0.5+X,-Y,0.5-Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+Y,0.5+X,-Z
SYMM -Y,-X,-Z
SFAC C H I N Pb
UNIT 32 104 16 8 4
DFIX 1.47 N1 C3
DFIX 1.54 C4 C8
SADI 0.001 C8 C4 C4 C3
SADI 0.001 C5 C3 C4 C3
SADI 0.005 C8 C4 C4 C3 C5 C3
RIGU 0.001 0.001 N1 C3 C4 C5 C8
RIGU 0.001 0.001 C8
EADP C8 C4 C3 N1
EADP C8 C4 C5 C3 N1
EADP C3 C8

L.S. 20
PLAN  1
FREE C8 C5
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
SHEL 10 0.84
REM <olex2.extras>
REM <HklSrc "%.\\1Me-PA_RoomT_Feb.hkl">
REM </olex2.extras>

WGHT    0.156800    7.217300
FVAR       0.46041
PB1   5    0.500000    0.500000    0.500000    10.25000    0.07478    0.07478 =
         0.09416   -0.00478   -0.00478   -0.01633
I2    3    0.750000    0.750000    0.475582    10.25000    0.06654    0.06654 =
         0.09329    0.00000    0.00000   -0.02807
I3    3    0.250000    0.750000    0.500000    10.25000    0.06774    0.06774 =
         0.11914    0.00000    0.00000    0.01157
I4    3    0.441380    0.441380    0.375841    10.50000    0.13748    0.13748 =
         0.08881   -0.00158   -0.00158   -0.01636
N1    4    0.464837    0.035163    0.410282    10.50000    0.14873    0.14873 =
         0.15435   -0.02918    0.02918    0.00077
PART -1
AFIX 137
H1A   2    0.507711    0.121778    0.418907    10.50000   -1.20000
H1B   2    0.496868   -0.036070    0.432408    10.50000   -1.20000
H1C   2    0.365909    0.043803    0.413045    10.50000   -1.20000
AFIX   0
PART 0
C3    1    0.504901   -0.004901    0.354392    10.50000    0.14873    0.14873 =
         0.15435   -0.02918    0.02918    0.00077
PART 2
AFIX  13
H3B   2    0.443867    0.056138    0.330173    10.50000   -1.20000
AFIX  13
PART 0
PART 1
H3A   2    0.437320    0.062683    0.335136    10.50000   -1.20000
AFIX   0
PART 0
PART 2
C4    1    0.667069    0.005272    0.336099    10.50000    0.14873    0.14873 =
         0.15435   -0.02918    0.02918    0.00077
AFIX  23
H4A   2    0.702693    0.102012    0.348274    10.50000   -1.20000
H4B   2    0.720993   -0.068934    0.356879    10.50000   -1.20000
AFIX   0
C8    1    0.723442   -0.011188    0.278850    10.50000    0.14873    0.14873 =
         0.15435   -0.02918    0.02918    0.00077
AFIX 137
H8A   2    0.826422    0.019038    0.277073    10.50000   -1.50000
H8B   2    0.664739    0.050805    0.255505    10.50000   -1.50000
H8C   2    0.714713   -0.113785    0.267873    10.50000   -1.50000
AFIX   0
PART 0
PART 1
C5    1    0.432613   -0.153975    0.340230    10.50000    0.14873    0.14873 =
         0.15435   -0.02918    0.02918    0.00077
AFIX 137
H5A   2    0.329371   -0.138151    0.331220    10.50000   -1.50000
H5B   2    0.439174   -0.220418    0.370359    10.50000   -1.50000
H5C   2    0.483698   -0.197384    0.310179    10.50000   -1.50000
AFIX   0
HKLF 4

REM  Me-PA_RoomT in P4(2)/ncm
REM R1 =  0.0609 for     905 Fo > 4sig(Fo)  and  0.0627 for all     972 data
REM     38 parameters refined using     29 restraints

END

WGHT      0.1570      7.0093

REM Highest difference peak  2.749,  deepest hole -2.003,  1-sigma level  0.300
Q1    1   0.2500  0.7500  0.4862  10.50000  0.05    2.33
;
_shelx_res_checksum              47431
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z+1/2'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'y-1/2, -x, -z-1/2'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
'-y-1/2, -x-1/2, z'
'y, x, 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 0.0812(6) Uani 1 4 d S T P . .
I2 I 0.7500 0.7500 0.47558(8) 0.0755(6) Uani 1 4 d S T P . .
I3 I 0.2500 0.7500 0.5000 0.0849(7) Uani 1 4 d S T P . .
I4 I 0.44138(17) 0.44138(17) 0.37584(7) 0.1213(8) Uani 1 2 d S T P . .
N1 N 0.465(3) 0.035(3) 0.4103(14) 0.151(7) Uani 1 2 d DS TU P D .
H1A H 0.5077 0.1218 0.4189 0.181 Uiso 0.5 1 calc GR . . A -1
H1B H 0.4969 -0.0361 0.4324 0.181 Uiso 0.5 1 calc GR . . A -1
H1C H 0.3659 0.0438 0.4130 0.181 Uiso 0.5 1 calc GR . . A -1
C3 C 0.505(3) -0.005(3) 0.3544(14) 0.151(7) Uani 1 2 d DS TU P . .
H3B H 0.4439 0.0561 0.3302 0.181 Uiso 1 2 calc RS T P B 2
H3A H 0.4373 0.0627 0.3351 0.181 Uiso 1 2 calc RS T P C 1
C4 C 0.667(2) 0.005(5) 0.3361(9) 0.151(7) Uani 0.5 1 d D U . D 2
H4A H 0.7027 0.1020 0.3483 0.181 Uiso 0.5 1 calc R . . D 2
H4B H 0.7210 -0.0689 0.3569 0.181 Uiso 0.5 1 calc R . . D 2
C8 C 0.723(6) -0.011(4) 0.2789(10) 0.151(7) Uani 0.5 1 d D U . D 2
H8A H 0.8264 0.0190 0.2771 0.226 Uiso 0.5 1 calc GR . . D 2
H8B H 0.6647 0.0508 0.2555 0.226 Uiso 0.5 1 calc GR . . D 2
H8C H 0.7147 -0.1138 0.2679 0.226 Uiso 0.5 1 calc GR . . D 2
C5 C 0.433(4) -0.154(3) 0.340(2) 0.151(7) Uani 0.5 1 d D U . D 1
H5A H 0.3294 -0.1382 0.3312 0.226 Uiso 0.5 1 calc GR . . D 1
H5B H 0.4392 -0.2204 0.3704 0.226 Uiso 0.5 1 calc GR . . D 1
H5C H 0.4837 -0.1974 0.3102 0.226 Uiso 0.5 1 calc GR . . D 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 0.0748(7) 0.0748(7) 0.0942(9) -0.0048(3) -0.0048(3) -0.0163(4)
I2 0.0665(7) 0.0665(7) 0.0933(12) 0.000 0.000 -0.0281(6)
I3 0.0677(7) 0.0677(7) 0.1191(17) 0.000 0.000 0.0116(7)
I4 0.1375(11) 0.1375(11) 0.0888(10) -0.0016(7) -0.0016(7) -0.0164(12)
N1 0.149(11) 0.149(11) 0.154(16) -0.029(9) 0.029(9) 0.001(11)
C3 0.149(11) 0.149(11) 0.154(16) -0.029(9) 0.029(9) 0.001(11)
C4 0.149(11) 0.149(11) 0.154(16) -0.029(9) 0.029(9) 0.001(11)
C8 0.149(11) 0.149(11) 0.154(16) -0.029(9) 0.029(9) 0.001(11)
C5 0.149(11) 0.149(11) 0.154(16) -0.029(9) 0.029(9) 0.001(11)
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'
Pb Pb -3.3944 10.1111 '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
I2 Pb1 I2 180.0 . 9_666
I3 Pb1 I2 90.0 9_666 9_666
I3 Pb1 I2 90.0 . 9_666
I3 Pb1 I2 90.0 9_666 .
I3 Pb1 I2 90.0 . .
I3 Pb1 I3 180.0 9_666 .
I3 Pb1 I4 90.0 9_666 9_666
I3 Pb1 I4 90.0 . .
I3 Pb1 I4 90.0 . 9_666
I3 Pb1 I4 90.0 9_666 .
I4 Pb1 I2 87.48(5) . 9_666
I4 Pb1 I2 87.48(5) 9_666 .
I4 Pb1 I2 92.52(5) 9_666 9_666
I4 Pb1 I2 92.52(5) . .
I4 Pb1 I4 180.0 . 9_666
Pb1 I2 Pb1 158.16(7) 3_665 .
Pb1 I3 Pb1 180.0 3_565 .
H1A N1 H1B 109.4 . .
H1A N1 H1C 109.4 . .
H1B N1 H1C 109.4 . .
C3 N1 H1A 109.5 . .
C3 N1 H1B 109.5 . .
C3 N1 H1C 109.6 . .
N1 C3 H3B 108.3 . .
N1 C3 H3A 99.5 . .
N1 C3 C4 120(2) . 15_665
N1 C3 C4 120(2) . .
N1 C3 C5 109(2) . 15_665
N1 C3 C5 109(2) . .
C4 C3 H3B 108.1 15_665 .
C4 C3 H3B 108.1 . .
C4 C3 C4 91(4) 15_665 .
C5 C3 H3A 99.4 15_665 .
C5 C3 H3A 99.4 . .
C5 C3 C5 134(4) . 15_665
C3 C4 H4A 106.0 . .
C3 C4 H4B 105.5 . .
H4A C4 H4B 106.2 . .
C8 C4 C3 126(3) . .
C8 C4 H4A 106.1 . .
C8 C4 H4B 105.4 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.4 . .
C4 C8 H8C 110.1 . .
H8A C8 H8B 109.3 . .
H8A C8 H8C 109.3 . .
H8B C8 H8C 109.2 . .
C3 C5 H5A 111.2 . .
C3 C5 H5B 111.0 . .
C3 C5 H5C 111.4 . .
H5A C5 H5B 107.7 . .
H5A C5 H5C 107.7 . .
H5B C5 H5C 107.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I2 3.2174(4) 9_666
Pb1 I2 3.2174(4) .
Pb1 I3 3.15912(9) 9_666
Pb1 I3 3.15912(9) .
Pb1 I4 3.1867(19) .
Pb1 I4 3.1868(19) 9_666
I2 Pb1 3.2174(4) 3_665
I3 Pb1 3.15912(9) 3_565
N1 H1A 0.8904 .
N1 H1B 0.8904 .
N1 H1C 0.8904 .
N1 C3 1.484(19) .
C3 H3B 0.9800 .
C3 H3A 0.9800 .
C3 C4 1.522(15) 15_665
C3 C4 1.522(14) .
C3 C5 1.522(15) .
C3 C5 1.522(15) 15_665
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C8 1.522(15) .
C8 H8A 0.9621 .
C8 H8B 0.9620 .
C8 H8C 0.9622 .
C5 H5A 0.9775 .
C5 H5B 0.9773 .
C5 H5C 0.9778 .
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
N1 C3 C4 C8 -171(4) .
C4 C3 C4 C8 63(6) 15_665
