#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:08:02 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224191 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/08/1550823.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_1550823
loop_
_publ_author_name
'D'Annibale, Andrea'
'Panetta, Riccardo'
'Tarquini, Ombretta'
'Colapietro, Marcello'
'Quaranta, Simone'
'Cassetta, Alberto'
'Barba, Luisa'
'Chita, Giuseppe'
'Latini, Alessandro'
_publ_section_title
;
 Synthesis, physico-chemical characterization and structure of the elusive
 hydroxylammonium lead iodide perovskite NH₃OHPbI₃.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5397
_journal_page_last               5407
_journal_paper_doi               10.1039/c9dt00690g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'I3 Pb, C6 H16 O2 S, 1[NH3OH]'
_chemical_formula_sum            'C6 H20 I3 N O3 Pb S'
_chemical_formula_weight         774.18
_chemical_melting_point          353(5)
_chemical_name_systematic        'Hydroxylammonium lead iodide'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Deliquescent,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_Hall           '-P 2a 2a'
_space_group_name_H-M_alt        'P m m a'
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.02.19 svn.r3573 for OlexSys, GUI svn.r5585)
;
_audit_update_record
;
2019-03-28 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.920(6)
_cell_length_b                   9.030(4)
_cell_length_c                   10.770(2)
_cell_measurement_reflns_used    1364
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.9739
_cell_measurement_theta_min      1.86231
_cell_volume                     770.2(7)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XRD1 Beamline control software'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Area detector diffractometer'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  'Si(111) double crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6502
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.974
_diffrn_reflns_theta_min         2.221
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    17.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.338
_exptl_crystal_density_meas      2.9(5)
_exptl_crystal_density_method    pycnometric
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             688
_exptl_crystal_recrystallization_method 'vapor diffusion'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.860
_refine_diff_density_min         -2.248
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       0.0061(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1360
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0394
_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)+(0.0747P)²+2.9611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1271
_reflns_number_total             1360
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00690g2.cif
_cod_data_source_block           i
_cod_depositor_comments          'Adding full bibliography for 1550823.cif.'
_cod_original_cell_volume        770.245(6)
_cod_database_code               1550823
_shelx_shelxl_version_number     2018/3
_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   0.280
_shelx_estimated_absorpt_t_min   0.280
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O2-N3
 1.415 with sigma of 0.001
 S4-C2AA \\sim S4-C2AB
 with sigma of 0.01
 C2AA-C1 \\sim C2AB-C1
 with sigma of 0.01
3. Rigid bond restraints
 S4, C2AA, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S4, C2AB, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2AB \\sim C2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2AB) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H1BD(0.5) H1BC(0.5) H1AB(0.5) H1AA(0.5) C2AB(0.5) H2AA(0.5)
 H2AB(0.5) C2AA(0.5) H2AC(0.5) H2AD(0.5) O2(0.25) H2(0.25) N3(0.25) H3A(0.25)
 H3B(0.25) H3C(0.25)
 Fixed U12: Pb1(0) I2(0) I3(0) S4(0) C1(0) O3(0)
 Fixed U13: I2(0) I3(0) S4(0) O3(0)
 Fixed U23: Pb1(0) I2(0) S4(0) C1(0)
 Fixed Uiso: O2(0.07) N3(0.07)
 Fixed X: Pb1(1) I2(0.75) I3(0.75) S4(0.75) O3(0.75)
 Fixed Y: Pb1(-0.5) I2(-0.5) S4(0) C1(0)
 Fixed Z: Pb1(0)
6.a Riding coordinates:
 O2(H2), N3(H3A,H3B,H3C)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1BD,H1BC), C1(H1AB,H1AA), C2AB(H2AA,H2AB), C2AA(H2AC,H2AD)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'x+1/2, -y, -z'
'-x, y, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'-x-1/2, y, z'
'x, -y, 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 1.000000 -0.500000 0.000000 0.0325(2) Uani 1 4 d S T P . .
I2 I 0.750000 -0.500000 0.23412(8) 0.0418(3) Uani 1 4 d S T P . .
I3 I 0.750000 -0.26183(8) -0.12446(7) 0.0445(2) Uani 1 2 d S T P . .
S4 S 0.750000 0.000000 0.4032(5) 0.0692(13) Uani 1 4 d DS TU P . .
C1 C 0.8460(15) 0.000000 0.1734(14) 0.064(3) Uani 1 2 d DS TU P . .
H1BD H 0.887508 0.102986 0.165396 0.077 Uiso 0.5 1 calc R . . A -1
H1BC H 0.887507 -0.056907 0.100988 0.077 Uiso 0.5 1 calc R . . A -1
H1AB H 0.884254 0.078281 0.115501 0.077 Uiso 0.5 1 calc R . . B -2
H1AA H 0.884254 -0.095924 0.138878 0.077 Uiso 0.5 1 calc R . . B -2
O3 O 0.750000 0.114(3) 0.4810(19) 0.148(9) Uani 1 2 d S T P C .
C2AB C 0.916(3) -0.068(4) 0.2929(14) 0.089(6) Uani 0.5 1 d D U . C -1
H2AA H 1.029715 -0.029600 0.313669 0.107 Uiso 0.5 1 calc R . . C -1
H2AB H 0.919877 -0.177944 0.288842 0.107 Uiso 0.5 1 calc R . . C -1
C2AA C 0.937(2) 0.024(4) 0.2975(14) 0.090(6) Uani 0.5 1 d D U . C -2
H2AC H 0.987135 0.123857 0.303971 0.107 Uiso 0.5 1 calc R . . C -2
H2AD H 1.025056 -0.052100 0.312542 0.107 Uiso 0.5 1 calc R . . C -2
O2 O 0.478(3) 0.367(4) 0.467(3) 0.070 Uiso 0.25 1 d D . . D -1
H2 H 0.441901 0.453381 0.454100 0.105 Uiso 0.25 1 d R . . D -1
N3 N 0.609(3) 0.379(4) 0.556(3) 0.070 Uiso 0.25 1 d D . . D -1
H3A H 0.681589 0.303836 0.537710 0.084 Uiso 0.25 1 d R . . D -1
H3B H 0.658459 0.467136 0.536489 0.084 Uiso 0.25 1 d R . . D -1
H3C H 0.585229 0.377356 0.638800 0.084 Uiso 0.25 1 d R . . D -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 -0.4630 1.7726 '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'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.0345 9.9071 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1218 0.1207 '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 . 5_745
I2 Pb1 I3 93.005(13) 5_745 2_645
I2 Pb1 I3 86.995(13) 5_745 5_745
I2 Pb1 I3 93.005(13) . 6_655
I2 Pb1 I3 93.005(13) . 5_745
I2 Pb1 I3 86.995(13) 5_745 6_655
I2 Pb1 I3 86.995(13) . .
I2 Pb1 I3 86.995(13) . 2_645
I2 Pb1 I3 93.005(13) 5_745 .
I3 Pb1 I3 96.06(2) 2_645 5_745
I3 Pb1 I3 180.0 5_745 .
I3 Pb1 I3 83.94(2) 2_645 .
I3 Pb1 I3 180.00(2) 6_655 2_645
I3 Pb1 I3 83.94(2) 6_655 5_745
I3 Pb1 I3 96.06(2) 6_655 .
Pb1 I2 Pb1 76.281(19) 2_645 .
Pb1 I3 Pb1 76.003(14) 2_645 .
O3 S4 O3 102(3) . 2_655
O3 S4 C2AB 130.9(12) . .
O3 S4 C2AB 98.3(12) 2_655 .
O3 S4 C2AA 107.1(12) . .
O3 S4 C2AA 118.1(12) 2_655 .
C1 C1 H1BD 109.4 2_655 .
C1 C1 H1BC 109.4 2_655 .
C1 C1 H1AB 107.8 2_655 .
C1 C1 H1AA 107.8 2_655 .
C1 C1 C2AB 111.3(10) 2_655 .
C1 C1 C2AA 118.0(8) 2_655 .
H1BD C1 H1BC 108.0 . .
H1AB C1 H1AA 107.1 . .
C2AB C1 H1BD 109.4 . .
C2AB C1 H1BC 109.4 . .
C2AA C1 H1AB 107.8 . .
C2AA C1 H1AA 107.8 . .
S4 C2AB H2AA 112.1 . .
S4 C2AB H2AB 112.1 . .
C1 C2AB S4 98.3(10) . .
C1 C2AB H2AA 112.1 . .
C1 C2AB H2AB 112.1 . .
H2AA C2AB H2AB 109.8 . .
S4 C2AA H2AC 112.1 . .
S4 C2AA H2AD 112.1 . .
C1 C2AA S4 98.1(10) . .
C1 C2AA H2AC 112.1 . .
C1 C2AA H2AD 112.1 . .
H2AC C2AA H2AD 109.8 . .
N3 O2 H2 107.4 . .
O2 N3 H3A 104.9 . .
O2 N3 H3B 102.7 . .
O2 N3 H3C 120.3 . .
H3A N3 H3B 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I2 3.2060(7) .
Pb1 I2 3.2060(7) 5_745
Pb1 I3 3.2160(5) .
Pb1 I3 3.2159(5) 5_745
Pb1 I3 3.2159(5) 6_655
Pb1 I3 3.2159(5) 2_645
S4 O3 1.33(2) .
S4 O3 1.33(2) 2_655
S4 C2AB 1.878(15) .
S4 C2AA 1.881(15) .
C1 C1 1.52(2) 2_655
C1 H1BD 0.9900 .
C1 H1BC 0.9900 .
C1 H1AB 0.9900 .
C1 H1AA 0.9900 .
C1 C2AB 1.53(2) .
C1 C2AA 1.53(2) .
C2AB H2AA 0.9900 .
C2AB H2AB 0.9900 .
C2AA H2AC 0.9900 .
C2AA H2AD 0.9900 .
O2 H2 0.8401 .
O2 N3 1.4151(10) .
N3 H3A 0.9099 .
N3 H3B 0.9100 .
N3 H3C 0.9101 .
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
C1 C1 C2AB S4 -35.2(18) 2_655
C1 C1 C2AA S4 12(2) 2_655
O3 S4 C2AB C1 -100(2) .
O3 S4 C2AB C1 147.1(17) 2_655
O3 S4 C2AA C1 -130.7(18) .
O3 S4 C2AA C1 115.5(18) 2_655
