#------------------------------------------------------------------------------
#$Date: 2019-11-02 03:58:21 +0100 (Sat 02 de Nov de 2019) $
#$Revision: 220641 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/73/4127359.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_4127359
loop_
_publ_author_name
'Straus, Daniel B.'
'Guo, Shu'
'Cava, Robert J.'
_publ_section_title
;
 Kinetically Stable Single Crystals of Perovskite-Phase CsPbI₃.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11435
_journal_page_last               11439
_journal_paper_doi               10.1021/jacs.9b06055
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.25(Cs4 I12 Pb4)'
_chemical_formula_sum            'Cs I3 Pb'
_chemical_formula_weight         720.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8637(8)
_cell_length_b                   12.4838(12)
_cell_length_c                   8.5783(8)
_cell_measurement_reflns_used    1148
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      3.26
_cell_volume                     949.21(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.03
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7193
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.213
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1047 before and 0.0076 after correction.
The Ratio of minimum to maximum transmission is 0.8194.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.612
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         1231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+7.5935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                839
_reflns_number_total             1231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b06055_si_003.cif
_cod_data_source_block           mo_cp295_0ma
_cod_database_code               4127359
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z+1/2'
4 '-x, y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z-1/2'
8 'x, -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_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.0000 0.0000 0.0000 0.03112(13) Uani 1 d 2 S T P
Cs1 Cs 0.43839(17) 0.2500 0.02006(17) 0.0786(4) Uani 1 d 2 S T P
I1 I 0.50303(16) 0.2500 0.56458(16) 0.0700(4) Uani 1 d 2 S T P
I2 I 0.19871(9) 0.03272(7) 0.30445(9) 0.0550(2) Uani 1 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 0.0293(2) 0.0292(2) 0.0349(2) -0.0018(2) 0.0003(3) 0.0009(2)
Cs1 0.0849(9) 0.0610(7) 0.0898(9) 0.000 -0.0240(8) 0.000
I1 0.0939(9) 0.0217(4) 0.0943(9) 0.000 0.0191(8) 0.000
I2 0.0440(4) 0.0725(5) 0.0485(4) -0.0030(4) -0.0219(3) 0.0045(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 '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'
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
I1 Pb1 I1 180.0 6_556 2_554
I1 Pb1 I2 89.29(3) 2_554 .
I1 Pb1 I2 91.56(3) 6_556 2_554
I1 Pb1 I2 89.29(3) 6_556 5
I1 Pb1 I2 88.44(3) 6_556 6_556
I1 Pb1 I2 90.71(3) 2_554 5
I1 Pb1 I2 88.44(3) 2_554 2_554
I1 Pb1 I2 90.71(3) 6_556 .
I1 Pb1 I2 91.56(3) 2_554 6_556
I2 Pb1 I2 90.883(9) . 6_556
I2 Pb1 I2 89.117(9) . 2_554
I2 Pb1 I2 90.883(9) 5 2_554
I2 Pb1 I2 180.000(16) 5 .
I2 Pb1 I2 89.117(9) 5 6_556
I2 Pb1 I2 180.000(15) 6_556 2_554
I1 Cs1 I1 87.69(4) 6_556 1_554
I1 Cs1 I2 68.36(2) 6_556 2_554
I1 Cs1 I2 130.15(3) 1_554 8_565
I1 Cs1 I2 130.15(3) 1_554 .
I1 Cs1 I2 66.61(2) 1_554 2_554
I1 Cs1 I2 67.19(3) 6_556 .
I1 Cs1 I2 68.36(2) 6_556 7_665
I1 Cs1 I2 67.19(3) 6_556 8_565
I1 Cs1 I2 66.61(2) 1_554 7_665
I2 Cs1 I1 131.19(3) 6_656 6_556
I2 Cs1 I1 131.19(3) 3 6_556
I2 Cs1 I1 107.38(4) 3 1_554
I2 Cs1 I1 107.38(4) 6_656 1_554
I2 Cs1 I2 75.68(2) 6_656 2_554
I2 Cs1 I2 160.28(4) 6_656 7_665
I2 Cs1 I2 64.241(13) 7_665 8_565
I2 Cs1 I2 67.947(19) 3 8_565
I2 Cs1 I2 130.85(4) 2_554 8_565
I2 Cs1 I2 67.947(19) 6_656 .
I2 Cs1 I2 75.68(2) 3 7_665
I2 Cs1 I2 121.74(4) 3 .
I2 Cs1 I2 160.28(4) 3 2_554
I2 Cs1 I2 121.74(4) 6_656 8_565
I2 Cs1 I2 64.241(13) 2_554 .
I2 Cs1 I2 130.85(4) 7_665 .
I2 Cs1 I2 89.11(4) 3 6_656
I2 Cs1 I2 79.96(4) 8_565 .
I2 Cs1 I2 115.82(4) 2_554 7_665
Pb1 I1 Pb1 159.85(5) 2 3
Pb1 I1 Cs1 99.89(2) 3 1_556
Pb1 I1 Cs1 99.89(2) 2 1_556
Pb1 I1 Cs1 88.62(2) 2 6_656
Pb1 I1 Cs1 88.62(3) 3 6_656
Cs1 I1 Cs1 109.00(5) 6_656 1_556
Pb1 I2 Pb1 151.99(3) . 2
Pb1 I2 Cs1 83.49(3) . .
Pb1 I2 Cs1 84.37(3) 2 2
Pb1 I2 Cs1 112.70(3) 2 6_556
Pb1 I2 Cs1 87.98(3) 2 .
Pb1 I2 Cs1 95.41(3) . 2
Pb1 I2 Cs1 94.56(3) . 6_556
Cs1 I2 Cs1 104.32(2) 6_556 2
Cs1 I2 Cs1 161.39(3) 2 .
Cs1 I2 Cs1 94.28(3) 6_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.1698(4) 6_556
Pb1 I1 3.1698(4) 2_554
Pb1 I2 3.1801(7) 6_556
Pb1 I2 3.1764(7) .
Pb1 I2 3.1764(7) 5
Pb1 I2 3.1801(7) 2_554
Cs1 I1 3.949(2) 1_554
Cs1 I1 3.927(2) 6_556
Cs1 I2 4.2217(15) 8_565
Cs1 I2 4.1659(12) 7_665
Cs1 I2 3.8663(13) 6_656
Cs1 I2 4.2217(15) .
Cs1 I2 3.8663(13) 3
Cs1 I2 4.1659(12) 2_554
I1 Pb1 3.1698(4) 2
I1 Pb1 3.1698(4) 3
I1 Cs1 3.927(2) 6_656
I1 Cs1 3.949(2) 1_556
I2 Pb1 3.1801(7) 2
I2 Cs1 4.1659(12) 2
I2 Cs1 3.8663(13) 6_556
