Synthesis, physico-chemical characterization and structure of the elusive hydroxylammonium lead iodide perovskite NH<sub>3</sub>OHPbI<sub>3</sub>.
D'Annibale, Andrea; Panetta, Riccardo; Tarquini, Ombretta; Colapietro, Marcello; Quaranta, Simone; Cassetta, Alberto; Barba, Luisa; Chita, Giuseppe; Latini, Alessandro; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5397–5407; doi:10.1039/c9dt00690g

data_1550823
_publ_section_title
;
 Synthesis, physico-chemical characterization and structure of the elusive
 hydroxylammonium lead iodide perovskite NH<sub>3</sub>OHPbI<sub>3</sub>.
;
_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       \w/2\q
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0747P)^2^+2.9611P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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
_shelx_res_checksum              44797
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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;