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#$Date: 2019-11-22 23:20:33 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231550 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/33/4003376.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_4003376
loop_
_publ_author_name
'Fateev, Sergey A.'
'Petrov, Andrey A.'
'Khrustalev, Victor N.'
'Dorovatovskii, Pavel V.'
'Zubavichus, Yan V.'
'Goodilin, Eugene A.'
'Tarasov, Alexey B.'
_publ_section_title
;
 Solution Processing of Methylammonium Lead Iodide Perovskite from
 γ-Butyrolactone: Crystallization Mediated by Solvation Equilibrium
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5237
_journal_paper_doi               10.1021/acs.chemmater.8b01906
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'I8 Pb3, C4 H6 O2, 2(C H6 N)'
_chemical_formula_sum            'C6 H18 I8 N2 O2 Pb3'
_chemical_formula_weight         1787.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 101.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.822(4)
_cell_length_b                   4.5979(9)
_cell_length_c                   16.653(3)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.0
_cell_volume                     1635.6(6)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_unetI/netI     0.1958
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7812
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.348
_diffrn_reflns_theta_min         1.705
_exptl_absorpt_coefficient_mu    25.955
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.629
_exptl_crystal_description       needle
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.890
_refine_diff_density_min         -3.734
_refine_diff_density_rms         0.559
_refine_ls_extinction_coef       0.00026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1923
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1273
_reflns_number_total             1923
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b01906_si_002.cif
_cod_data_source_block           igla1
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4003376
_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   0.072
_shelx_estimated_absorpt_t_max   0.779
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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 0.58656(5) 0.5000 0.74939(6) 0.0333(4) Uani 1 2 d S T P . .
Pb2 Pb 0.5000 1.0000 0.5000 0.0276(5) Uani 1 4 d S T P . .
I1 I 0.68838(7) 0.0000 0.79855(10) 0.0431(5) Uani 1 2 d S T P . .
I2 I 0.54468(10) 0.5000 0.91237(9) 0.0568(7) Uani 1 2 d S T P . .
I3 I 0.47803(6) 1.0000 0.68619(8) 0.0301(5) Uani 1 2 d S T P . .
I4 I 0.39407(6) 0.5000 0.45398(8) 0.0307(5) Uani 1 2 d S T P . .
N1 N 0.8923(9) 0.5000 0.908(2) 0.135(15) Uani 1 2 d DS T P A 1
H1A H 0.9247 0.5000 0.9517 0.202 Uiso 1 2 d R U P A 1
H1B H 0.8947 0.3397 0.8763 0.202 Uiso 1 1 d R U . A 1
C1 C 0.8323(10) 0.5000 0.935(2) 0.135(15) Uani 1 2 d DS T P A 1
H1C H 0.7971 0.5000 0.8880 0.202 Uiso 1 2 d R U P A 1
H1D H 0.8299 0.6726 0.9690 0.202 Uiso 1 1 d R U . A 1
O1 O 0.8249(6) 0.559(2) 0.7354(7) 0.068(8) Uani 0.25 1 d D . P B 2
O2 O 0.8636(5) 0.959(3) 0.8018(7) 0.068(8) Uani 0.25 1 d D . P B 2
C2 C 0.8410(3) 0.845(2) 0.7371(6) 0.068(8) Uani 0.25 1 d D . P B 2
C3 C 0.8263(8) 0.969(3) 0.6520(7) 0.068(8) Uani 0.25 1 d D . P B 2
H3A H 0.8645 1.0003 0.6294 0.082 Uiso 0.25 1 d R U P B 2
H3B H 0.8050 1.1594 0.6512 0.082 Uiso 0.25 1 d R U P B 2
C4 C 0.7815(8) 0.747(3) 0.6042(7) 0.068(8) Uani 0.25 1 d D . P B 2
H4A H 0.7880 0.7291 0.5473 0.082 Uiso 0.25 1 d R U P B 2
H4B H 0.7371 0.7954 0.6027 0.082 Uiso 0.25 1 d R U P B 2
C5 C 0.7990(7) 0.469(3) 0.6526(9) 0.068(8) Uani 0.25 1 d D . P B 2
H5A H 0.7624 0.3403 0.6509 0.082 Uiso 0.25 1 d R U P B 2
H5B H 0.8310 0.3616 0.6299 0.082 Uiso 0.25 1 d R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0070 0.0030 '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 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0210 0.0120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.0340 3.1360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -9.9000 4.0740 '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 I1 95.27(5) . .
I1 Pb1 I1 92.38(5) 1_565 .
I2 Pb1 I3 87.58(5) . .
I1 Pb1 I3 89.80(3) 1_565 .
I1 Pb1 I3 176.23(4) . .
I1 Pb1 I3 176.23(4) 1_565 1_545
I1 Pb1 I3 89.80(3) . 1_545
I3 Pb1 I3 87.85(4) . 1_545
I3 Pb2 I4 89.33(4) . .
I4 Pb2 I4 89.57(4) 5_666 .
Pb1 I1 Pb1 92.38(5) 1_545 .
Pb2 I3 Pb1 93.91(4) . .
Pb1 I3 Pb1 87.85(4) . 1_565
C1 N1 H1A 111.0 . .
C1 N1 H1B 109.7 . .
H1A N1 H1B 109.6 . .
N1 C1 H1C 110.4 . .
N1 C1 H1D 109.5 . .
H1C C1 H1D 109.6 . .
C2 O1 C5 110.38(6) . .
O2 C2 O1 119.60(10) . .
O2 C2 C3 130.37(10) . .
O1 C2 C3 110.04(6) . .
C2 C3 C4 103.37(8) . .
C2 C3 H3A 112.3 . .
C4 C3 H3A 113.5 . .
C2 C3 H3B 111.1 . .
C4 C3 H3B 109.6 . .
H3A C3 H3B 107.1 . .
C5 C4 C3 102.80(9) . .
C5 C4 H4A 111.5 . .
C3 C4 H4A 110.8 . .
C5 C4 H4B 109.9 . .
C3 C4 H4B 112.6 . .
H4A C4 H4B 109.1 . .
O1 C5 C4 105.76(8) . .
O1 C5 H5A 110.8 . .
C4 C5 H5A 111.9 . .
O1 C5 H5B 109.9 . .
C4 C5 H5B 109.8 . .
H5A C5 H5B 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I2 3.036(2) .
Pb1 I1 3.1856(13) .
Pb1 I3 3.3139(12) .
Pb1 I3 3.3140(13) 1_545
Pb2 I3 3.2329(14) 5_676
Pb2 I3 3.2329(14) .
Pb2 I4 3.2390(10) 5_676
Pb2 I4 3.2390(10) 5_666
Pb2 I4 3.2390(10) 1_565
Pb2 I4 3.2391(10) .
I1 Pb1 3.1856(13) 1_545
I3 Pb1 3.3140(12) 1_565
I4 Pb2 3.2391(10) 1_545
N1 C1 1.4750(11) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
C1 H1C 0.9800 .
C1 H1D 0.9800 .
O1 C2 1.3598(9) .
O1 C5 1.4402(10) .
O2 C2 1.2084(8) .
C2 C3 1.4996(9) .
C3 C4 1.5202(11) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.5197(10) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
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
O2 C2 C3 C4 -163.0(2)
O1 C2 C3 C4 16.9(2)
C2 C3 C4 C5 -25.8(3)
C2 O1 C5 C4 -17.2(2)
C3 C4 C5 O1 26.5(4)
