#------------------------------------------------------------------------------
#$Date: 2023-11-06 10:33:12 +0200 (Mon, 06 Nov 2023) $
#$Revision: 287427 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/96/1569659.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_1569659
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(Br3 In0.5), C6 H20 N3, H2 O'
_chemical_formula_sum            'C6 H22 Br6 In N3 O'
_chemical_formula_weight         746.54
_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                94.554(2)
_cell_angle_beta                 108.689(2)
_cell_angle_gamma                109.0060(10)
_cell_formula_units_Z            2
_cell_length_a                   7.8936(3)
_cell_length_b                   11.0840(5)
_cell_length_c                   12.1633(5)
_cell_measurement_reflns_used    7766
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.39
_cell_volume                     932.85(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.541
_diffrn_reflns_theta_min         1.986
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.108
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3201
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1368 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.4290.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.658
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         5694
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0311
_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)+(0.0227P)²+0.1883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4330
_reflns_number_total             5694
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3mh00536d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1569658--1569659.cif.'
_cod_database_code               1569659
_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   0.333
_shelx_estimated_absorpt_t_min   0.333
_olex2_refinement_description
;
1. Others
 Fixed Sof: In1(0.5) In2(0.5)
 Fixed Uiso: H21(0.103) H1(0.045) H2(0.045) H3(0.045) H10(0.036) H11(0.036)
 H18(0.056) H19(0.056) H20(0.056) H4(0.038) H5(0.038) H6(0.04) H7(0.04)
 H8(0.044) H9(0.044) H12(0.037) H13(0.037) H14(0.046) H15(0.046) H16(0.055)
 H17(0.055)
 Fixed X: In1(0) In2(1) H21(0.096901) H1(0.515628) H2(0.645574) H3(0.720895)
 H10(0.4749) H11(0.381919) H18(0.153058) H19(0.219746) H20(0.354238)
 H4(0.566086) H5(0.787303) H6(0.51354) H7(0.736416) H8(0.773391) H9(0.669956)
 H12(0.602572) H13(0.515968) H14(0.297012) H15(0.202991) H16(0.415767)
 H17(0.19486)
 Fixed Y: In1(0) In2(0.5) H21(0.325941) H1(0.255681) H2(0.186898) H3(0.328534)
 H10(0.178907) H11(0.270177) H18(0.239837) H19(0.207346) H20(0.302404)
 H4(0.172835) H5(0.252531) H6(0.369954) H7(0.447187) H8(0.3437) H9(0.442787)
 H12(0.212342) H13(0.320539) H14(0.052654) H15(0.157783) H16(0.121889)
 H17(0.03948)
 Fixed Z: In1(0.5) In2(1) H21(0.230799) H1(0.648789) H2(0.687567) H3(0.710329)
 H10(0.302171) H11(0.273309) H18(-0.096414) H19(-0.188943) H20(-0.081335)
 H4(0.489287) H5(0.555611) H6(0.482291) H7(0.543601) H8(0.37648) H9(0.346771)
 H12(0.15959) H13(0.131555) H14(0.095701) H15(0.078895) H16(-0.058028) H17(-
 0.099699)
;
_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 0.000000 0.500000 0.02245(8) Uani 1 2 d S . P . .
Br1 Br 0.17463(5) 0.25744(3) 0.57066(4) 0.03411(9) Uani 1 1 d . . . . .
Br2 Br 0.29223(5) -0.02643(4) 0.67245(3) 0.03405(9) Uani 1 1 d . . . . .
Br3 Br 0.17109(5) -0.00751(4) 0.34124(3) 0.03122(9) Uani 1 1 d . . . . .
In2 In 1.000000 0.500000 1.000000 0.02474(8) Uani 1 2 d S . P . .
Br4 Br 1.13856(6) 0.76211(4) 1.03042(4) 0.04025(10) Uani 1 1 d . . . . .
Br5 Br 1.07080(5) 0.47787(4) 0.80290(3) 0.03666(10) Uani 1 1 d . . . . .
Br6 Br 1.35931(5) 0.51717(4) 1.12217(4) 0.03513(10) Uani 1 1 d . . . . .
O1 O 0.1646(6) 0.3002(5) 0.2865(4) 0.0684(10) Uani 1 1 d DG . . . .
H21 H 0.096901 0.325941 0.230799 0.103 Uiso 1 1 d G U . . .
H22 H 0.094(10) 0.230(5) 0.304(7) 0.17(4) Uiso 1 1 d D . . . .
N1 N 0.6328(4) 0.2563(3) 0.6592(3) 0.0376(8) Uani 1 1 d . . . . .
H1 H 0.515628 0.255681 0.648789 0.045 Uiso 1 1 calc R U . . .
H2 H 0.645574 0.186898 0.687567 0.045 Uiso 1 1 calc R U . . .
H3 H 0.720895 0.328534 0.710329 0.045 Uiso 1 1 calc R U . . .
N2 N 0.4872(4) 0.2541(3) 0.2783(3) 0.0303(7) Uani 1 1 d . . . . .
H10 H 0.474900 0.178907 0.302171 0.036 Uiso 1 1 calc R U . . .
H11 H 0.381919 0.270177 0.273309 0.036 Uiso 1 1 calc R U . . .
N3 N 0.2511(5) 0.2287(3) -0.1110(3) 0.0463(9) Uani 1 1 d . . . . .
H18 H 0.153058 0.239837 -0.096414 0.056 Uiso 1 1 calc R U . . .
H19 H 0.219746 0.207346 -0.188943 0.056 Uiso 1 1 calc R U . . .
H20 H 0.354238 0.302404 -0.081335 0.056 Uiso 1 1 calc R U . . .
C1 C 0.6600(5) 0.2528(4) 0.5440(3) 0.0320(8) Uani 1 1 d . . . . .
H4 H 0.566086 0.172835 0.489287 0.038 Uiso 1 1 calc R U . . .
H5 H 0.787303 0.252531 0.555611 0.038 Uiso 1 1 calc R U . . .
C2 C 0.6386(6) 0.3673(4) 0.4906(3) 0.0336(8) Uani 1 1 d . . . . .
H6 H 0.513540 0.369954 0.482291 0.040 Uiso 1 1 calc R U . . .
H7 H 0.736416 0.447187 0.543601 0.040 Uiso 1 1 calc R U . . .
C3 C 0.6575(5) 0.3598(4) 0.3706(3) 0.0365(9) Uani 1 1 d . . . . .
H8 H 0.773391 0.343700 0.376480 0.044 Uiso 1 1 calc R U . . .
H9 H 0.669956 0.442787 0.346771 0.044 Uiso 1 1 calc R U . . .
C4 C 0.4957(5) 0.2383(3) 0.1576(3) 0.0308(8) Uani 1 1 d . . . . .
H12 H 0.602572 0.212342 0.159590 0.037 Uiso 1 1 calc R U . . .
H13 H 0.515968 0.320539 0.131555 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3095(6) 0.1360(4) 0.0727(3) 0.0383(9) Uani 1 1 d . . . . .
H14 H 0.297012 0.052654 0.095701 0.046 Uiso 1 1 calc R U . . .
H15 H 0.202991 0.157783 0.078895 0.046 Uiso 1 1 calc R U . . .
C6 C 0.2950(6) 0.1225(4) -0.0546(4) 0.0458(11) Uani 1 1 d . . . . .
H16 H 0.415767 0.121889 -0.058028 0.055 Uiso 1 1 calc R U . . .
H17 H 0.194860 0.039480 -0.099699 0.055 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
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
Br1 In1 Br1 180.0 2_556 . ?
Br1 In1 Br2 89.059(12) 2_556 2_556 ?
Br1 In1 Br2 89.060(12) . . ?
Br1 In1 Br2 90.941(12) . 2_556 ?
Br1 In1 Br2 90.941(13) 2_556 . ?
Br1 In1 Br3 87.371(12) 2_556 . ?
Br1 In1 Br3 92.629(12) 2_556 2_556 ?
Br1 In1 Br3 92.628(12) . . ?
Br1 In1 Br3 87.372(12) . 2_556 ?
Br2 In1 Br2 180.000(16) 2_556 . ?
Br2 In1 Br3 91.822(12) . . ?
Br2 In1 Br3 91.822(12) 2_556 2_556 ?
Br2 In1 Br3 88.178(12) . 2_556 ?
Br2 In1 Br3 88.178(12) 2_556 . ?
Br3 In1 Br3 180.0 . 2_556 ?
Br4 In2 Br4 180.0 2_767 . ?
Br5 In2 Br4 90.771(13) 2_767 2_767 ?
Br5 In2 Br4 89.229(13) 2_767 . ?
Br5 In2 Br4 89.229(13) . 2_767 ?
Br5 In2 Br4 90.771(13) . . ?
Br5 In2 Br5 180.0 2_767 . ?
Br5 In2 Br6 88.821(12) . . ?
Br5 In2 Br6 88.821(12) 2_767 2_767 ?
Br5 In2 Br6 91.179(12) . 2_767 ?
Br5 In2 Br6 91.179(12) 2_767 . ?
Br6 In2 Br4 91.967(12) 2_767 . ?
Br6 In2 Br4 91.967(12) . 2_767 ?
Br6 In2 Br4 88.033(12) 2_767 2_767 ?
Br6 In2 Br4 88.033(12) . . ?
Br6 In2 Br6 180.0 . 2_767 ?
H21 O1 H22 112.3 . . ?
H1 N1 H2 109.5 . . ?
H1 N1 H3 109.5 . . ?
H3 N1 H2 109.5 . . ?
C1 N1 H1 109.5 . . ?
C1 N1 H2 109.5 . . ?
C1 N1 H3 109.5 . . ?
H10 N2 H11 107.5 . . ?
C3 N2 H10 108.5 . . ?
C3 N2 H11 108.5 . . ?
C4 N2 H10 108.5 . . ?
C4 N2 H11 108.5 . . ?
C4 N2 C3 115.3(3) . . ?
H19 N3 H18 109.5 . . ?
H19 N3 H20 109.5 . . ?
H20 N3 H18 109.5 . . ?
C6 N3 H18 109.5 . . ?
C6 N3 H19 109.5 . . ?
C6 N3 H20 109.5 . . ?
N1 C1 H4 109.2 . . ?
N1 C1 H5 109.2 . . ?
N1 C1 C2 112.2(3) . . ?
H4 C1 H5 107.9 . . ?
C2 C1 H4 109.2 . . ?
C2 C1 H5 109.2 . . ?
C1 C2 H6 109.2 . . ?
C1 C2 H7 109.2 . . ?
C1 C2 C3 111.9(3) . . ?
H7 C2 H6 107.9 . . ?
C3 C2 H6 109.2 . . ?
C3 C2 H7 109.2 . . ?
N2 C3 C2 111.7(3) . . ?
N2 C3 H8 109.3 . . ?
N2 C3 H9 109.3 . . ?
C2 C3 H8 109.3 . . ?
C2 C3 H9 109.3 . . ?
H9 C3 H8 107.9 . . ?
N2 C4 H12 109.8 . . ?
N2 C4 H13 109.8 . . ?
N2 C4 C5 109.3(3) . . ?
H12 C4 H13 108.3 . . ?
C5 C4 H12 109.8 . . ?
C5 C4 H13 109.8 . . ?
C4 C5 H14 108.9 . . ?
C4 C5 H15 108.9 . . ?
H14 C5 H15 107.7 . . ?
C6 C5 C4 113.5(3) . . ?
C6 C5 H14 108.9 . . ?
C6 C5 H15 108.9 . . ?
N3 C6 C5 113.4(3) . . ?
N3 C6 H16 108.9 . . ?
N3 C6 H17 108.9 . . ?
C5 C6 H16 108.9 . . ?
C5 C6 H17 108.9 . . ?
H16 C6 H17 107.7 . . ?
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 Br1 2.6590(4) 2_556 ?
In1 Br1 2.6591(4) . ?
In1 Br2 2.6914(4) . ?
In1 Br2 2.6913(4) 2_556 ?
In1 Br3 2.6979(4) 2_556 ?
In1 Br3 2.6979(4) . ?
In2 Br4 2.6970(4) 2_767 ?
In2 Br4 2.6970(4) . ?
In2 Br5 2.6410(4) . ?
In2 Br5 2.6410(4) 2_767 ?
In2 Br6 2.6816(4) . ?
In2 Br6 2.6817(4) 2_767 ?
O1 H21 0.8501 . ?
O1 H22 0.88(2) . ?
N1 H1 0.8900 . ?
N1 H2 0.8900 . ?
N1 H3 0.8900 . ?
N1 C1 1.483(5) . ?
N2 H10 0.8900 . ?
N2 H11 0.8900 . ?
N2 C3 1.496(4) . ?
N2 C4 1.489(4) . ?
N3 H18 0.8900 . ?
N3 H19 0.8900 . ?
N3 H20 0.8900 . ?
N3 C6 1.489(5) . ?
C1 H4 0.9700 . ?
C1 H5 0.9700 . ?
C1 C2 1.503(5) . ?
C2 H6 0.9700 . ?
C2 H7 0.9700 . ?
C3 C2 1.513(5) . ?
C3 H8 0.9700 . ?
C3 H9 0.9700 . ?
C4 H12 0.9700 . ?
C4 H13 0.9700 . ?
C4 C5 1.507(5) . ?
C5 H14 0.9700 . ?
C5 H15 0.9700 . ?
C5 C6 1.506(5) . ?
C6 H16 0.9700 . ?
C6 H17 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 C1 C2 C3 -177.4(3) . . . . ?
N2 C3 C2 C1 70.8(4) . . . . ?
N2 C4 C5 C6 173.9(3) . . . . ?
C3 N2 C4 C5 -175.8(3) . . . . ?
C4 N2 C3 C2 -178.9(3) . . . . ?
C4 C5 C6 N3 -76.5(4) . . . . ?
