# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_i
_database_code_depnum_ccdc_archive 'CCDC 1894399'
loop_
_audit_author_name
_audit_author_address
'Marcello Colapietro'
;CNR  Istituto di Cristallografia
Italy
;
#Added by publCIF



_audit_update_record             
;
2019-03-28 deposited with the CCDC.	2019-04-01 downloaded from the CCDC.
;


_cell_special_details            none
#Added by publCIF




_diffrn_radiation_monochromator  'Si(111) double crystal'
# publcif _publ_body_element loop end
_audit_creation_date             2019-03-21
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.02.19 svn.r3573 for OlexSys, GUI svn.r5585)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Hydroxylammonium lead iodide'
_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)
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_H-M_alt        'P m m a'
_space_group_name_Hall           '-P 2a 2a'
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'

_cell_length_a                   7.920(6)
_cell_length_b                   9.030(4)
_cell_length_c                   10.770(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     770.245(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1364
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.9739
_cell_measurement_theta_min      1.86231
_shelx_estimated_absorpt_T_max   0.280
_shelx_estimated_absorpt_T_min   0.280
_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_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_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_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1271
_reflns_number_total             1360
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0394
_refine_ls_restrained_S_all      1.155
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
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 . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_special_details  ?
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'



_publcif_funding_html            
;
;
_exptl_crystal_recrystallization_method 'vapor diffusion'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Hygroscopic,Deliquescent,Heat-sensitive,Oxygen-sensitive
