#------------------------------------------------------------------------------
#$Date: 2024-08-07 04:58:51 +0300 (Wed, 07 Aug 2024) $
#$Revision: 294019 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023234.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023234
loop_
_publ_author_name
'Tonoyan, Gayane S.'
'Giester, Gerald'
'Ghazaryan, Vahram V.'
'Chilingaryan, Ruben Yu.'
'Margaryan, Arthur A.'
'Mkrtchyan, Artak H.'
'Petrosyan, Aram M.'
_publ_section_title
;
 Crystal structure of hexaglycinium dodecaiodotriplumbate
;
_journal_coeditor_code           JY2048
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024007606
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '(C2 H6 N O2)6 [Pb3 I12]'
_chemical_formula_moiety         '6(C2 H6 N O2 +), I12 Pb3 6-'
_chemical_formula_sum            'C12 H36 I12 N6 O12 Pb3'
_chemical_formula_weight         2600.84
_chemical_name_common            'hexaglycinium dodecaiodo-triplumbate '
_chemical_name_systematic
;
Hexaglycinium tetra-μ-iodido-octaiodidotriplumbate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                105.900(2)
_cell_angle_beta                 92.647(2)
_cell_angle_gamma                111.477(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5437(5)
_cell_length_b                   11.2672(7)
_cell_length_c                   14.8534(9)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.87
_cell_measurement_theta_min      2.60
_cell_volume                     1262.40(13)
_computing_cell_refinement
;
APEX5 Bruker (2024)
;
_computing_data_collection
;
APEX5 Bruker (2024)
;
_computing_data_reduction
;
APEX5 Bruker (2024)
;
_computing_publication_material
;
ShelXle (Hübschle et al., 2011)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54402
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.210
_diffrn_reflns_theta_min         2.045
_exptl_absorpt_coefficient_mu    17.358
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.294
_refine_diff_density_min         -2.485
_refine_ls_extinction_coef       0.00049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019/2 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         9640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0216
_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)+(0.0087P)²+2.5693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0385
_reflns_number_gt                8389
_reflns_number_total             9640
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jy2048.cif
_cod_data_source_block           I
_cod_database_code               2023234
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.500000 0.500000 0.500000 0.02041(3) Uani d 1 . .
Pb Pb2 0.38342(2) 0.18885(2) 0.25654(2) 0.02316(3) Uani d 1 . .
I I1 0.19064(2) 0.40522(2) 0.33606(2) 0.02537(4) Uani d 1 . .
I I2 0.74935(2) 0.46827(2) 0.34936(2) 0.02390(4) Uani d 1 . .
I I3 0.41471(2) 0.19237(2) 0.49364(2) 0.02463(4) Uani d 1 . .
I I4 0.42551(3) 0.22381(2) 0.06337(2) 0.03591(5) Uani d 1 . .
I I5 0.03007(3) -0.03864(2) 0.16590(2) 0.03305(5) Uani d 1 . .
I I6 0.59810(3) 0.01929(2) 0.23522(2) 0.03749(6) Uani d 1 . .
O O1A 1.0289(4) 0.4863(2) 0.11937(18) 0.0392(6) Uani d 1 . .
H H1A 1.044(5) 0.540(3) 0.0923(19) 0.059 Uiso calc 1 . .
O O2A 0.8915(4) 0.3408(2) -0.02294(17) 0.0389(6) Uani d 1 . .
C C1A 0.9400(4) 0.3667(3) 0.0605(2) 0.0263(6) Uani d 1 . .
C C2A 0.9034(5) 0.2593(3) 0.1076(2) 0.0330(7) Uani d 1 . .
H H21A 1.011081 0.252552 0.127759 0.040 Uiso calc 1 . .
H H22A 0.852011 0.282924 0.164719 0.040 Uiso calc 1 . .
N N1A 0.7854(4) 0.1293(3) 0.0409(2) 0.0366(7) Uani d 1 . .
H H11A 0.774867 0.062872 0.066806 0.055 Uiso calc 1 . .
H H12A 0.826984 0.112846 -0.014398 0.055 Uiso calc 1 . .
H H13A 0.681464 0.132077 0.029277 0.055 Uiso calc 1 . .
O O1B 0.6686(3) 0.5891(3) 0.10354(18) 0.0352(6) Uani d 1 . .
H H1B 0.6483(17) 0.542(5) 0.048(3) 0.053 Uiso calc 1 . .
O O2B 0.3916(3) 0.5535(3) 0.07956(16) 0.0347(5) Uani d 1 . .
C C1B 0.5289(4) 0.5982(3) 0.1296(2) 0.0270(6) Uani d 1 . .
C C2B 0.5538(5) 0.6726(4) 0.2331(2) 0.0316(7) Uani d 1 . .
H H21B 0.578315 0.619973 0.271200 0.038 Uiso calc 1 . .
H H22B 0.652301 0.759908 0.248893 0.038 Uiso calc 1 . .
N N1B 0.3990(4) 0.6954(3) 0.2566(2) 0.0316(6) Uani d 1 . .
H H11B 0.404495 0.721763 0.320722 0.047 Uiso calc 1 . .
H H12B 0.305401 0.618023 0.229916 0.047 Uiso calc 1 . .
H H13B 0.391713 0.760631 0.233660 0.047 Uiso calc 1 . .
O O1C 1.0019(3) 0.1093(3) 0.6226(2) 0.0377(6) Uani d 1 . .
H H1C 0.985(5) 0.104(4) 0.681(3) 0.057 Uiso calc 1 . .
O O2C 0.8283(3) 0.2202(3) 0.64327(18) 0.0373(6) Uani d 1 . .
N N1C 0.8615(4) 0.2696(3) 0.4769(2) 0.0352(7) Uani d 1 . .
H H11C 0.867623 0.269306 0.415860 0.053 Uiso calc 1 . .
H H12C 0.923265 0.353762 0.517012 0.053 Uiso calc 1 . .
H H13C 0.750789 0.243678 0.485806 0.053 Uiso calc 1 . .
C C1C 0.9138(4) 0.1728(3) 0.5965(2) 0.0268(6) Uani d 1 . .
C C2C 0.9311(4) 0.1753(4) 0.4965(2) 0.0304(7) Uani d 1 . .
H H21C 1.052603 0.204456 0.488863 0.037 Uiso calc 1 . .
H H22C 0.867896 0.084242 0.451120 0.037 Uiso calc 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
I I -0.4742 1.8119 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
I1 Pb1 I1 2_666 . 180.0 ?
I1 Pb1 I2 2_666 2_666 91.363(7) ?
I1 Pb1 I2 . 2_666 88.637(8) ?
I1 Pb1 I2 2_666 . 88.637(7) ?
I1 Pb1 I2 . . 91.363(7) ?
I2 Pb1 I2 2_666 . 180.0 ?
I1 Pb1 I3 2_666 . 88.797(5) ?
I1 Pb1 I3 . . 91.203(5) ?
I2 Pb1 I3 2_666 . 91.693(5) ?
I2 Pb1 I3 . . 88.307(5) ?
I1 Pb1 I3 2_666 2_666 91.203(5) ?
I1 Pb1 I3 . 2_666 88.797(6) ?
I2 Pb1 I3 2_666 2_666 88.307(5) ?
I2 Pb1 I3 . 2_666 91.693(5) ?
I3 Pb1 I3 . 2_666 180.0 ?
I4 Pb2 I6 . . 92.576(7) ?
I4 Pb2 I5 . . 88.198(8) ?
I6 Pb2 I5 . . 98.865(9) ?
I4 Pb2 I1 . . 98.685(7) ?
I6 Pb2 I1 . . 166.133(7) ?
I5 Pb2 I1 . . 89.602(8) ?
I4 Pb2 I2 . . 88.550(7) ?
I6 Pb2 I2 . . 88.468(8) ?
I5 Pb2 I2 . . 172.104(7) ?
I1 Pb2 I2 . . 83.779(8) ?
Pb1 I1 Pb2 . . 76.444(6) ?
Pb1 I2 Pb2 . . 75.892(6) ?
C1A O1A H1A . . 109.5 ?
O2A C1A O1A . . 125.6(3) ?
O2A C1A C2A . . 122.0(3) ?
O1A C1A C2A . . 112.4(3) ?
N1A C2A C1A . . 109.8(3) ?
N1A C2A H21A . . 109.7 ?
C1A C2A H21A . . 109.7 ?
N1A C2A H22A . . 109.7 ?
C1A C2A H22A . . 109.7 ?
H21A C2A H22A . . 108.2 ?
C2A N1A H11A . . 109.5 ?
C2A N1A H12A . . 109.5 ?
H11A N1A H12A . . 109.5 ?
C2A N1A H13A . . 109.5 ?
H11A N1A H13A . . 109.5 ?
H12A N1A H13A . . 109.5 ?
C1B O1B H1B . . 109.5 ?
O2B C1B O1B . . 126.6(3) ?
O2B C1B C2B . . 121.3(3) ?
O1B C1B C2B . . 112.1(3) ?
N1B C2B C1B . . 110.1(3) ?
N1B C2B H21B . . 109.6 ?
C1B C2B H21B . . 109.6 ?
N1B C2B H22B . . 109.6 ?
C1B C2B H22B . . 109.6 ?
H21B C2B H22B . . 108.2 ?
C2B N1B H11B . . 109.5 ?
C2B N1B H12B . . 109.5 ?
H11B N1B H12B . . 109.5 ?
C2B N1B H13B . . 109.5 ?
H11B N1B H13B . . 109.5 ?
H12B N1B H13B . . 109.5 ?
C1C O1C H1C . . 109.5 ?
C2C N1C H11C . . 109.5 ?
C2C N1C H12C . . 109.5 ?
H11C N1C H12C . . 109.5 ?
C2C N1C H13C . . 109.5 ?
H11C N1C H13C . . 109.5 ?
H12C N1C H13C . . 109.5 ?
O2C C1C O1C . . 126.1(3) ?
O2C C1C C2C . . 123.3(3) ?
O1C C1C C2C . . 110.6(3) ?
N1C C2C C1C . . 108.8(3) ?
N1C C2C H21C . . 109.9 ?
C1C C2C H21C . . 109.9 ?
N1C C2C H22C . . 109.9 ?
C1C C2C H22C . . 109.9 ?
H21C C2C H22C . . 108.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 I1 2_666 3.1575(3) ?
Pb1 I1 . 3.1575(2) ?
Pb1 I2 2_666 3.1988(2) ?
Pb1 I2 . 3.1988(2) ?
Pb1 I3 . 3.2432(3) ?
Pb1 I3 2_666 3.2432(3) ?
Pb2 I4 . 3.0213(3) ?
Pb2 I6 . 3.0663(3) ?
Pb2 I5 . 3.0926(3) ?
Pb2 I1 . 3.4049(3) ?
Pb2 I2 . 3.4063(3) ?
O1A C1A . 1.304(4) ?
O1A H1A . 0.79(5) ?
O2A C1A . 1.209(4) ?
C1A C2A . 1.502(4) ?
C2A N1A . 1.474(4) ?
C2A H21A . 0.9900 ?
C2A H22A . 0.9900 ?
N1A H11A . 0.9100 ?
N1A H12A . 0.9100 ?
N1A H13A . 0.9100 ?
O1B C1B . 1.302(4) ?
O1B H1B . 0.82(5) ?
O2B C1B . 1.210(4) ?
C1B C2B . 1.499(4) ?
C2B N1B . 1.476(4) ?
C2B H21B . 0.9900 ?
C2B H22B . 0.9900 ?
N1B H11B . 0.9100 ?
N1B H12B . 0.9100 ?
N1B H13B . 0.9100 ?
O1C C1C . 1.322(4) ?
O1C H1C . 0.90(5) ?
O2C C1C . 1.196(4) ?
N1C C2C . 1.477(4) ?
N1C H11C . 0.9100 ?
N1C H12C . 0.9100 ?
N1C H13C . 0.9100 ?
C1C C2C . 1.507(5) ?
C2C H21C . 0.9900 ?
C2C H22C . 0.9900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1A H1A O2A 2_765 0.79(5) 1.85(3) 2.638(4) 171(4) yes
C2A H21A I1 1_655 0.99 3.10 3.669(3) 118.0 yes
C2A H22A I2 . 0.99 3.33 4.271(4) 159.9 yes
N1A H11A I4 2_655 0.91 3.05 3.549(3) 116.0 yes
N1A H11A I5 1_655 0.91 3.27 3.983(3) 137.0 yes
N1A H11A I6 . 0.91 3.04 3.655(3) 126.2 yes
N1A H12A I5 2_655 0.91 2.69 3.588(3) 170.3 yes
N1A H13A I4 . 0.91 2.75 3.605(3) 156.3 yes
O1B H1B O2B 2_665 0.82(4) 1.85(4) 2.667(3) 176(4) yes
C2B H21B I2 . 0.99 3.03 3.976(3) 160.8 yes
C2B H22B I6 1_565 0.99 3.18 3.775(3) 120.2 yes
N1B H11B I3 2_666 0.91 2.82 3.648(3) 151.1 yes
N1B H12B I1 . 0.91 3.11 3.647(3) 119.4 yes
N1B H12B O1A 1_455 0.91 2.49 3.320(4) 151.2 yes
N1B H13B I6 1_565 0.91 2.79 3.528(3) 138.7 yes
O1C H1C I5 2_656 0.90(5) 2.57(3) 3.445(3) 164(4) yes
N1C H11C I1 1_655 0.91 3.09 3.711(3) 126.8 yes
N1C H11C I2 . 0.91 3.13 3.640(3) 117.4 yes
N1C H11C I6 . 0.91 3.31 3.868(3) 121.6 yes
N1C H12C I2 2_766 0.91 3.00 3.779(3) 145.0 yes
N1C H13C I3 . 0.91 2.73 3.628(3) 170.2 yes
C2C H21C I3 1_655 0.99 3.14 4.068(3) 155.9 yes
