#------------------------------------------------------------------------------
#$Date: 2023-11-06 10:33:12 +0200 (Mon, 06 Nov 2023) $
#$Revision: 287427 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/96/1569658.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_1569658
loop_
_publ_author_name
'Li, Dong-Yang'
'Shang, Yan-Bing'
'Liu, Qi'
'Zhang, Hua-Wu'
'Zhang, Xin-Yue'
'Yue, Cheng-Yang'
'Lei, Xiao-Wu'
_publ_section_title
;
 0D hybrid indium halide as a highly efficient X-ray scintillation and
 ultra-sensitive fluorescent probe.
;
_journal_issue                   11
_journal_name_full               'Materials horizons'
_journal_page_first              5004
_journal_page_last               5015
_journal_paper_doi               10.1039/d3mh00536d
_journal_volume                  10
_journal_year                    2023
_chemical_formula_moiety         '2(Cl3 In0.5), C6 H20 N3, H2 O'
_chemical_formula_sum            'C6 H22 Cl6 In N3 O'
_chemical_formula_weight         479.78
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-30 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                94.6940(10)
_cell_angle_beta                 107.997(2)
_cell_angle_gamma                109.4970(10)
_cell_formula_units_Z            2
_cell_length_a                   7.54750(10)
_cell_length_b                   10.68050(10)
_cell_length_c                   11.8682(2)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    273
_cell_measurement_theta_max      50.698
_cell_measurement_theta_min      4.524
_cell_volume                     839.27(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.173
_diffrn_reflns_theta_min         4.002
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.974
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull light gray'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00278(17)
_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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3389
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0439P)²+0.2819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3295
_reflns_number_total             3389
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3mh00536d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1569658--1569659.cif.'
_cod_database_code               1569658
_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.
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: In1(0.5) In2(0.5)
 Fixed Uiso: H00U(0.085) H1(0.034) H2(0.034) H3(0.034) H19(0.046) H20(0.046)
 H21(0.046) H11(0.032) H13(0.032) H4(0.035) H5(0.035) H6(0.033) H7(0.033)
 H9(0.036) H10(0.036) H14(0.031) H16(0.031) H17(0.039) H18(0.039) H22(0.044)
 H23(0.044) H24(0.055)
 Fixed X: In1(0) In2(1) H00U(0.073937) H1(0.728592) H2(0.51431) H3(0.645024)
 H19(0.356792) H20(0.14709) H21(0.210349) H11(0.37308) H13(0.479123)
 H4(0.505471) H5(0.73628) H6(0.808567) H7(0.581128) H9(0.666417) H10(0.784258)
 H14(0.515913) H16(0.608027) H17(0.189026) H18(0.288095) H22(0.41239)
 H23(0.180223)
 Fixed Y: In1(0.5) In2(1) H00U(0.821328) H1(0.827018) H2(0.753903)
 H3(0.679498) H19(0.805937) H20(0.743895) H21(0.709756) H11(0.765049)
 H13(0.675813) H4(0.868945) H5(0.957105) H6(0.762153) H7(0.670295) H9(0.952464)
 H10(0.855697) H14(0.824289) H16(0.713096) H17(0.651974) H18(0.543844)
 H22(0.615332) H23(0.531424)
 Fixed Z: In1(0.5) In2(1) H00U(0.227207) H1(0.718568) H2(0.652717)
 H3(0.690111) H19(-0.088214) H20(-0.099934) H21(-0.198218) H11(0.272875)
 H13(0.302456) H4(0.485017) H5(0.54695) H6(0.561706) H7(0.491479) H9(0.344368)
 H10(0.374691) H14(0.127337) H16(0.154237) H17(0.073143) H18(0.089739) H22(-
 0.06922) H23(-0.111514)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, 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
In1 In 0.000000 0.500000 0.500000 0.01799(8) Uani 1 2 d S . P . .
Cl4 Cl 0.18155(8) 0.75080(5) 0.57756(5) 0.02945(13) Uani 1 1 d . . . . .
Cl5 Cl 0.17637(8) 0.49675(5) 0.34984(5) 0.02760(13) Uani 1 1 d . . . . .
Cl6 Cl 0.27539(8) 0.46447(5) 0.66468(4) 0.02966(13) Uani 1 1 d . . . . .
In2 In 1.000000 1.000000 1.000000 0.01966(8) Uani 1 2 d S . P . .
Cl1 Cl 1.06980(8) 0.98149(5) 0.80892(5) 0.03187(13) Uani 1 1 d . . . . .
Cl2 Cl 0.64965(8) 0.98463(5) 0.88304(5) 0.03236(14) Uani 1 1 d . . . . .
Cl3 Cl 0.86276(9) 0.74343(5) 0.96579(6) 0.03491(14) Uani 1 1 d . . . . .
O1 O 0.1415(4) 0.7918(2) 0.2823(2) 0.0568(6) Uani 1 1 d DG . . . .
H00U H 0.073937 0.821328 0.227207 0.085 Uiso 1 1 d DG U . . .
N1 N 0.6364(3) 0.75374(19) 0.66390(16) 0.0283(4) Uani 1 1 d . . . . .
H1 H 0.728592 0.827018 0.718568 0.034 Uiso 1 1 calc R U . . .
H2 H 0.514310 0.753903 0.652717 0.034 Uiso 1 1 calc R U . . .
H3 H 0.645024 0.679498 0.690111 0.034 Uiso 1 1 calc R U . . .
N2 N 0.2462(3) 0.7306(2) -0.11815(19) 0.0386(5) Uani 1 1 d . . . . .
H19 H 0.356792 0.805937 -0.088214 0.046 Uiso 1 1 calc R U . . .
H20 H 0.147090 0.743895 -0.099934 0.046 Uiso 1 1 calc R U . . .
H21 H 0.210349 0.709756 -0.198218 0.046 Uiso 1 1 calc R U . . .
N3 N 0.4859(3) 0.75293(18) 0.27725(18) 0.0269(4) Uani 1 1 d . . . . .
H11 H 0.373080 0.765049 0.272875 0.032 Uiso 1 1 calc R U . . .
H13 H 0.479123 0.675813 0.302456 0.032 Uiso 1 1 calc R U . . .
C1 C 0.6389(4) 0.8722(2) 0.4932(2) 0.0293(5) Uani 1 1 d . . . . .
H4 H 0.505471 0.868945 0.485017 0.035 Uiso 1 1 calc R U . . .
H5 H 0.736280 0.957105 0.546950 0.035 Uiso 1 1 calc R U . . .
C2 C 0.6717(4) 0.7551(2) 0.54796(19) 0.0278(4) Uani 1 1 d . . . . .
H6 H 0.808567 0.762153 0.561706 0.033 Uiso 1 1 calc R U . . .
H7 H 0.581128 0.670295 0.491479 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6600(4) 0.8673(2) 0.3694(2) 0.0299(5) Uani 1 1 d . . . . .
H9 H 0.666417 0.952464 0.344368 0.036 Uiso 1 1 calc R U . . .
H10 H 0.784258 0.855697 0.374691 0.036 Uiso 1 1 calc R U . . .
C4 C 0.4957(3) 0.7384(2) 0.15333(19) 0.0254(4) Uani 1 1 d . . . . .
H14 H 0.515913 0.824289 0.127337 0.031 Uiso 1 1 calc R U . . .
H16 H 0.608027 0.713096 0.154237 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3009(4) 0.6305(2) 0.0664(2) 0.0322(5) Uani 1 1 d . . . . .
H17 H 0.189026 0.651974 0.073143 0.039 Uiso 1 1 calc R U . . .
H18 H 0.288095 0.543844 0.089739 0.039 Uiso 1 1 calc R U . . .
C6 C 0.2870(4) 0.6169(2) -0.0646(2) 0.0368(5) Uani 1 1 d . . . . .
H22 H 0.412390 0.615332 -0.069220 0.044 Uiso 1 1 calc R U . . .
H23 H 0.180223 0.531424 -0.111514 0.044 Uiso 1 1 calc R U . . .
H24 H 0.057(4) 0.735(3) 0.308(3) 0.055 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
_geom_angle_publ_flag
Cl4 In1 Cl4 180.0 . 2_566 ?
Cl4 In1 Cl5 87.161(17) 2_566 . ?
Cl4 In1 Cl5 87.161(17) . 2_566 ?
Cl4 In1 Cl5 92.839(17) . . ?
Cl4 In1 Cl5 92.840(17) 2_566 2_566 ?
Cl4 In1 Cl6 88.847(18) . . ?
Cl4 In1 Cl6 91.153(18) . 2_566 ?
Cl4 In1 Cl6 91.153(18) 2_566 . ?
Cl4 In1 Cl6 88.847(18) 2_566 2_566 ?
Cl5 In1 Cl5 180.00(2) . 2_566 ?
Cl6 In1 Cl5 91.958(18) 2_566 2_566 ?
Cl6 In1 Cl5 88.042(18) . 2_566 ?
Cl6 In1 Cl5 88.042(18) 2_566 . ?
Cl6 In1 Cl5 91.958(18) . . ?
Cl6 In1 Cl6 180.0 . 2_566 ?
Cl1 In2 Cl1 180.0 2_777 . ?
Cl1 In2 Cl2 90.349(19) . . ?
Cl1 In2 Cl2 89.651(19) 2_777 . ?
Cl1 In2 Cl2 89.651(19) . 2_777 ?
Cl1 In2 Cl2 90.349(19) 2_777 2_777 ?
Cl1 In2 Cl3 88.58(2) 2_777 2_777 ?
Cl1 In2 Cl3 88.58(2) . . ?
Cl1 In2 Cl3 91.42(2) . 2_777 ?
Cl1 In2 Cl3 91.41(2) 2_777 . ?
Cl2 In2 Cl2 180.0 2_777 . ?
Cl2 In2 Cl3 88.344(19) . . ?
Cl2 In2 Cl3 91.657(19) 2_777 . ?
Cl2 In2 Cl3 88.343(19) 2_777 2_777 ?
Cl2 In2 Cl3 91.656(19) . 2_777 ?
Cl3 In2 Cl3 180.0 2_777 . ?
H00U O1 H24 107.7 . . ?
H1 N1 H3 109.5 . . ?
H2 N1 H1 109.5 . . ?
H2 N1 H3 109.5 . . ?
C2 N1 H1 109.5 . . ?
C2 N1 H2 109.5 . . ?
C2 N1 H3 109.5 . . ?
H19 N2 H20 109.5 . . ?
H21 N2 H19 109.5 . . ?
H21 N2 H20 109.5 . . ?
C6 N2 H19 109.5 . . ?
C6 N2 H20 109.5 . . ?
C6 N2 H21 109.5 . . ?
H13 N3 H11 107.6 . . ?
C3 N3 H11 108.6 . . ?
C3 N3 H13 108.6 . . ?
C4 N3 H11 108.6 . . ?
C4 N3 H13 108.6 . . ?
C4 N3 C3 114.59(18) . . ?
H5 C1 H4 108.0 . . ?
C2 C1 H4 109.3 . . ?
C2 C1 H5 109.3 . . ?
C2 C1 C3 111.57(18) . . ?
C3 C1 H4 109.3 . . ?
C3 C1 H5 109.3 . . ?
N1 C2 C1 111.65(18) . . ?
N1 C2 H6 109.3 . . ?
N1 C2 H7 109.3 . . ?
C1 C2 H6 109.3 . . ?
C1 C2 H7 109.3 . . ?
H7 C2 H6 108.0 . . ?
N3 C3 C1 110.75(18) . . ?
N3 C3 H9 109.5 . . ?
N3 C3 H10 109.5 . . ?
C1 C3 H9 109.5 . . ?
C1 C3 H10 109.5 . . ?
H9 C3 H10 108.1 . . ?
N3 C4 H14 109.8 . . ?
N3 C4 H16 109.8 . . ?
N3 C4 C5 109.23(18) . . ?
H16 C4 H14 108.3 . . ?
C5 C4 H14 109.8 . . ?
C5 C4 H16 109.8 . . ?
C4 C5 H17 108.9 . . ?
C4 C5 H18 108.9 . . ?
C4 C5 C6 113.5(2) . . ?
H17 C5 H18 107.7 . . ?
C6 C5 H17 108.9 . . ?
C6 C5 H18 108.9 . . ?
N2 C6 C5 112.04(19) . . ?
N2 C6 H22 109.2 . . ?
N2 C6 H23 109.2 . . ?
C5 C6 H22 109.2 . . ?
C5 C6 H23 109.2 . . ?
H22 C6 H23 107.9 . . ?
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
In1 Cl4 2.5034(5) . ?
In1 Cl4 2.5034(5) 2_566 ?
In1 Cl5 2.5369(5) 2_566 ?
In1 Cl5 2.5369(5) . ?
In1 Cl6 2.5341(5) . ?
In1 Cl6 2.5341(5) 2_566 ?
In2 Cl1 2.4888(5) . ?
In2 Cl1 2.4888(5) 2_777 ?
In2 Cl2 2.5200(5) 2_777 ?
In2 Cl2 2.5200(5) . ?
In2 Cl3 2.5319(5) 2_777 ?
In2 Cl3 2.5319(5) . ?
O1 H00U 0.8500 . ?
O1 H24 0.879(18) . ?
N1 H1 0.8900 . ?
N1 H2 0.8900 . ?
N1 H3 0.8900 . ?
N1 C2 1.481(3) . ?
N2 H19 0.8900 . ?
N2 H20 0.8900 . ?
N2 H21 0.8900 . ?
N2 C6 1.493(3) . ?
N3 H11 0.8900 . ?
N3 H13 0.8900 . ?
N3 C3 1.496(3) . ?
N3 C4 1.493(3) . ?
C1 H4 0.9700 . ?
C1 H5 0.9700 . ?
C2 C1 1.513(3) . ?
C2 H6 0.9700 . ?
C2 H7 0.9700 . ?
C3 C1 1.525(3) . ?
C3 H9 0.9700 . ?
C3 H10 0.9700 . ?
C4 H14 0.9700 . ?
C4 H16 0.9700 . ?
C4 C5 1.514(3) . ?
C5 H17 0.9700 . ?
C5 H18 0.9700 . ?
C5 C6 1.516(3) . ?
C6 H22 0.9700 . ?
C6 H23 0.9700 . ?
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
N1 C2 C1 C3 -175.76(18) . . . . ?
N3 C3 C1 C2 71.0(2) . . . . ?
N3 C4 C5 C6 174.56(19) . . . . ?
C3 N3 C4 C5 -173.52(18) . . . . ?
C4 N3 C3 C1 -178.84(18) . . . . ?
C4 C5 C6 N2 -75.0(3) . . . . ?
