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#$Date: 2018-01-06 03:42:11 +0200 (Sat, 06 Jan 2018) $
#$Revision: 204785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/28/4002874.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_4002874
loop_
_publ_author_name
'Wong, Man Kwong'
'Liu, Fangzhou'
'Kam, Chun Sing'
'Leung, Tik Lun'
'Tam, Ho Won'
'Djurišić, Aleksandra B.'
'Popović, Jasminka'
'Li, Hangkong'
'Shih, Kaimin'
'Low, Kam-Hung'
'Chan, Wai Kin'
'Chen, Wei'
'He, Zhubing'
'Ng, Annie'
'Surya, Charles'
_publ_section_title
;
 Synthesis of Lead-Free Perovskite Films by Combinatorial Evaporation:
 Fast Processes for Screening Different Precursor Combinations
;
_journal_issue                   23
_journal_name_full               'Chemistry of Materials'
_journal_page_first              9946
_journal_paper_doi               10.1021/acs.chemmater.7b03293
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety         'I4 Sn, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 I4 N2 Sn'
_chemical_formula_weight         774.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4218(12)
_cell_length_b                   8.9253(13)
_cell_length_c                   26.110(4)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.8
_cell_volume                     1962.6(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE FIXED-CHI PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56243
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.460
_diffrn_reflns_theta_min         2.878
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.577
_exptl_absorpt_correction_T_max  0.2065
_exptl_absorpt_correction_T_min  0.1192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.392
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         2025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.392
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+103.4506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1844
_reflns_number_total             2025
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm7b03293_si_002.cif
_cod_data_source_block           mo_CHEM0432
_cod_depositor_comments
'Adding full bibliography for 4002873--4002875.cif.'
_cod_database_code               4002874
_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_min   0.190
_shelx_estimated_absorpt_t_max   0.736
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'
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
I1 I -0.07628(12) 0.53070(11) 0.38268(4) 0.0234(3) Uani 1 1 d . . .
I2 I -0.20473(11) 0.79061(11) 0.52162(4) 0.0225(3) Uani 1 1 d . . .
Sn1 Sn 0.0000 0.5000 0.5000 0.0169(3) Uani 1 2 d S . P
N1 N 0.4854(15) 0.5698(14) 0.5956(5) 0.025(3) Uani 1 1 d . . .
H1A H 0.5172 0.5032 0.5713 0.037 Uiso 1 1 calc R U .
H1B H 0.4969 0.6648 0.5834 0.037 Uiso 1 1 calc R U .
H1C H 0.3817 0.5531 0.6035 0.037 Uiso 1 1 calc R U .
C1 C 0.5832(18) 0.5510(16) 0.6418(6) 0.023(3) Uani 1 1 d . . .
H1D H 0.5660 0.6373 0.6650 0.028 Uiso 1 1 calc R U .
H1E H 0.6968 0.5497 0.6320 0.028 Uiso 1 1 calc R U .
C2 C 0.543(2) 0.4074(19) 0.6698(6) 0.030(4) Uani 1 1 d . . .
H2A H 0.5514 0.3224 0.6456 0.036 Uiso 1 1 calc R U .
H2B H 0.4315 0.4126 0.6817 0.036 Uiso 1 1 calc R U .
C3 C 0.6496(19) 0.3772(18) 0.7155(6) 0.028(4) Uani 1 1 d . . .
H3A H 0.7614 0.3724 0.7038 0.034 Uiso 1 1 calc R U .
H3B H 0.6404 0.4613 0.7401 0.034 Uiso 1 1 calc R U .
C4 C 0.608(2) 0.2335(18) 0.7423(7) 0.034(4) Uani 1 1 d . . .
H4A H 0.4949 0.2338 0.7511 0.051 Uiso 1 1 calc R U .
H4B H 0.6713 0.2244 0.7737 0.051 Uiso 1 1 calc R U .
H4C H 0.6309 0.1487 0.7197 0.051 Uiso 1 1 calc R U .
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'
N N 0.0061 0.0033 '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'
Sn Sn -0.6537 1.4246 '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
Sn1 I2 Sn1 151.76(3) 2_466 .
I1 Sn1 I1 180.0 . 5_566
I1 Sn1 I2 93.72(3) . 6
I1 Sn1 I2 86.28(3) 5_566 6
I1 Sn1 I2 86.28(3) . 2_566
I1 Sn1 I2 93.72(3) 5_566 2_566
I2 Sn1 I2 180.0 6 2_566
I1 Sn1 I2 89.49(3) . .
I1 Sn1 I2 90.51(3) 5_566 .
I2 Sn1 I2 91.381(13) 6 .
I2 Sn1 I2 88.619(13) 2_566 .
I1 Sn1 I2 90.51(3) . 5_566
I1 Sn1 I2 89.49(3) 5_566 5_566
I2 Sn1 I2 88.619(14) 6 5_566
I2 Sn1 I2 91.381(14) 2_566 5_566
I2 Sn1 I2 180.0 . 5_566
C1 N1 H1A 109.5 . .
C1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
N1 C1 C2 111.6(12) . .
N1 C1 H1D 109.3 . .
C2 C1 H1D 109.3 . .
N1 C1 H1E 109.3 . .
C2 C1 H1E 109.3 . .
H1D C1 H1E 108.0 . .
C1 C2 C3 113.4(14) . .
C1 C2 H2A 108.9 . .
C3 C2 H2A 108.9 . .
C1 C2 H2B 108.9 . .
C3 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
C4 C3 C2 112.3(14) . .
C4 C3 H3A 109.1 . .
C2 C3 H3A 109.1 . .
C4 C3 H3B 109.1 . .
C2 C3 H3B 109.1 . .
H3A C3 H3B 107.9 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Sn1 3.1418(10) .
I2 Sn1 3.1615(10) 2_466
I2 Sn1 3.1653(10) .
Sn1 I1 3.1418(10) 5_566
Sn1 I2 3.1615(10) 6
Sn1 I2 3.1615(10) 2_566
Sn1 I2 3.1654(10) 5_566
N1 C1 1.470(19) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
C1 C2 1.51(2) .
C1 H1D 0.9900 .
C1 H1E 0.9900 .
C2 C3 1.52(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.50(2) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
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
N1 C1 C2 C3 175.5(13)
C1 C2 C3 C4 -179.5(14)
