#------------------------------------------------------------------------------
#$Date: 2022-01-04 04:27:42 +0200 (Tue, 04 Jan 2022) $
#$Revision: 271787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/05/8000562.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_8000562
loop_
_publ_author_name
'Lin, Jiawei'
'Liu, Kunjie'
'Ruan, Hang'
'Sun, Niu'
'Chen, Xin'
'Zhao, Jing'
'Guo, Zhongnan'
'Liu, Quanlin'
'Yuan, Wenxia'
_publ_section_title
;
 Zero-Dimensional Lead-Free Halide with Indirect Optical Gap and Enhanced
 Photoluminescence by Sb Doping.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              198
_journal_page_last               207
_journal_paper_doi               10.1021/acs.jpclett.1c03649
_journal_year                    2021
_chemical_formula_moiety         'Cl6 In, 3(C7 H8 N3), H2 O'
_chemical_formula_sum            'C21 H26 Cl6 In N9 O'
_chemical_formula_weight         748.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.1380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9918(4)
_cell_length_b                   11.8909(4)
_cell_length_c                   17.0091(5)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.504
_cell_measurement_theta_min      2.714
_cell_volume                     2926.93(15)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.496
_diffrn_reflns_theta_min         2.105
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0724 before and 0.0593 after correction. The Ratio of minimum to maximum transmission is 0.8324. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0396(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0415P)²+1.1035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5769
_reflns_number_total             6055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jz1c03649_si_002.cif
_cod_data_source_block           mo_20210429_bkd_ljw_1_2_0m
_cod_database_code               8000562
_shelx_shelxl_version_number     2014/7
_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   0.543
_shelx_estimated_absorpt_t_min   0.465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1C,H1D)
2.b Aromatic/amide H refined with riding coordinates:
 N9(H9), N3(H3), N8(H8), N6(H6A), N2(H2), N5(H5A), C20(H20), C17(H17),
 C19(H19), C6(H6), C13(H13), C10(H10), C18(H18), C3(H3A), C5(H5), C12(H12),
 C4(H4), C11(H11)
2.c X=CH2 refined with riding coordinates:
 N7(H7A,H7B), N1(H1A,H1B), N4(H4A,H4B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.30159(2) 0.50104(2) 0.61458(2) 0.02756(8) Uani 1 1 d . . . . .
Cl1 Cl 0.12753(3) 0.53445(4) 0.54370(3) 0.03946(12) Uani 1 1 d . . . . .
Cl3 Cl 0.46826(3) 0.45713(4) 0.67749(3) 0.04106(12) Uani 1 1 d . . . . .
Cl4 Cl 0.33654(4) 0.70767(4) 0.64011(3) 0.04330(12) Uani 1 1 d . . . . .
Cl2 Cl 0.26685(3) 0.29798(4) 0.58430(3) 0.04465(13) Uani 1 1 d . . . . .
Cl6 Cl 0.33091(4) 0.52719(5) 0.47784(3) 0.04276(12) Uani 1 1 d . . . . .
Cl5 Cl 0.26405(4) 0.49236(4) 0.74820(3) 0.04575(14) Uani 1 1 d . . . . .
N9 N 0.08566(10) 0.26390(13) 0.28036(9) 0.0353(3) Uani 1 1 d . . . . .
H9 H 0.0367 0.2212 0.2619 0.042 Uiso 1 1 calc R . . . .
N3 N -0.04137(11) 0.86496(14) 0.34796(9) 0.0389(3) Uani 1 1 d . . . . .
H3 H -0.0830 0.8924 0.3059 0.047 Uiso 1 1 calc R . . . .
N8 N 0.18014(11) 0.38601(14) 0.35336(9) 0.0400(4) Uani 1 1 d . . . . .
H8 H 0.2035 0.4364 0.3910 0.048 Uiso 1 1 calc R . . . .
N6 N 0.57247(11) 0.17674(15) 0.50527(10) 0.0426(4) Uani 1 1 d . . . . .
H6A H 0.6122 0.1863 0.4758 0.051 Uiso 1 1 calc R . . . .
N7 N 0.03882(13) 0.35375(19) 0.38669(12) 0.0561(5) Uani 1 1 d . . . . .
H7A H -0.0139 0.3168 0.3758 0.067 Uiso 1 1 calc R . . . .
H7B H 0.0520 0.4027 0.4269 0.067 Uiso 1 1 calc R . . . .
O1 O -0.12395(13) 0.26369(19) 0.28879(15) 0.0772(6) Uani 1 1 d . . . . .
H1C H -0.1514 0.2027 0.2710 0.116 Uiso 1 1 d G . . . .
H1D H -0.1572 0.3191 0.2672 0.116 Uiso 1 1 d G . . . .
N2 N 0.03735(12) 0.74709(15) 0.43662(10) 0.0462(4) Uani 1 1 d . . . . .
H2 H 0.0560 0.6839 0.4627 0.055 Uiso 1 1 calc R . . . .
C21 C 0.16319(12) 0.26752(15) 0.24926(10) 0.0324(3) Uani 1 1 d . . . . .
N5 N 0.45507(12) 0.20274(15) 0.55543(11) 0.0476(4) Uani 1 1 d . . . . .
H5A H 0.4050 0.2322 0.5647 0.057 Uiso 1 1 calc R . . . .
C15 C 0.09806(13) 0.33581(16) 0.34265(11) 0.0375(4) Uani 1 1 d . . . . .
C16 C 0.22260(12) 0.34592(16) 0.29571(10) 0.0348(4) Uani 1 1 d . . . . .
C1 C -0.03306(13) 0.75673(17) 0.36937(12) 0.0402(4) Uani 1 1 d . . . . .
N1 N -0.08205(14) 0.67267(18) 0.32968(13) 0.0569(5) Uani 1 1 d . . . . .
H1A H -0.1251 0.6856 0.2844 0.068 Uiso 1 1 calc R . . . .
H1B H -0.0717 0.6036 0.3485 0.068 Uiso 1 1 calc R . . . .
C14 C 0.57589(13) 0.09128(16) 0.56177(12) 0.0402(4) Uani 1 1 d . . . . .
C7 C 0.02557(13) 0.92762(17) 0.40212(11) 0.0366(4) Uani 1 1 d . . . . .
C20 C 0.18398(14) 0.21070(16) 0.18568(11) 0.0394(4) Uani 1 1 d . . . . .
H20 H 0.1434 0.1563 0.1545 0.047 Uiso 1 1 calc R . . . .
N4 N 0.47351(14) 0.32953(18) 0.45440(14) 0.0622(5) Uani 1 1 d . . . . .
H4A H 0.4232 0.3671 0.4552 0.075 Uiso 1 1 calc R . . . .
H4B H 0.5068 0.3502 0.4212 0.075 Uiso 1 1 calc R . . . .
C2 C 0.07613(13) 0.85232(18) 0.45860(11) 0.0397(4) Uani 1 1 d . . . . .
C8 C 0.49905(12) 0.2424(2) 0.50278(12) 0.0442(5) Uani 1 1 d . . . . .
C9 C 0.50054(14) 0.10744(17) 0.59356(12) 0.0428(4) Uani 1 1 d . . . . .
C17 C 0.30576(13) 0.37339(19) 0.27953(13) 0.0450(4) Uani 1 1 d . . . . .
H17 H 0.3462 0.4281 0.3106 0.054 Uiso 1 1 calc R . . . .
C19 C 0.26760(15) 0.2376(2) 0.16985(13) 0.0497(5) Uani 1 1 d . . . . .
H19 H 0.2849 0.2007 0.1265 0.060 Uiso 1 1 calc R . . . .
C6 C 0.04522(17) 1.0412(2) 0.40653(14) 0.0489(5) Uani 1 1 d . . . . .
H6 H 0.0098 1.0930 0.3684 0.059 Uiso 1 1 calc R . . . .
C13 C 0.63744(19) 0.00451(18) 0.58781(17) 0.0520(6) Uani 1 1 d . . . . .
H13 H 0.6893 -0.0063 0.5664 0.062 Uiso 1 1 calc R . . . .
C10 C 0.48301(19) 0.0363(2) 0.65198(15) 0.0591(6) Uani 1 1 d . . . . .
H10 H 0.4314 0.0469 0.6738 0.071 Uiso 1 1 calc R . . . .
C18 C 0.32650(15) 0.3168(2) 0.21575(14) 0.0520(5) Uani 1 1 d . . . . .
H18 H 0.3831 0.3328 0.2029 0.062 Uiso 1 1 calc R . . . .
C3 C 0.14934(15) 0.8877(2) 0.52167(13) 0.0569(6) Uani 1 1 d . . . . .
H3A H 0.1839 0.8364 0.5607 0.068 Uiso 1 1 calc R . . . .
C5 C 0.11861(17) 1.0758(2) 0.46880(14) 0.0576(6) Uani 1 1 d . . . . .
H5 H 0.1346 1.1533 0.4732 0.069 Uiso 1 1 calc R . . . .
C12 C 0.6198(2) -0.0660(2) 0.64672(16) 0.0635(6) Uani 1 1 d . . . . .
H12 H 0.6611 -0.1264 0.6666 0.076 Uiso 1 1 calc R . . . .
C4 C 0.16968(19) 1.0012(2) 0.52501(17) 0.0608(7) Uani 1 1 d . . . . .
H4 H 0.2200 1.0285 0.5670 0.073 Uiso 1 1 calc R . . . .
C11 C 0.5449(2) -0.0513(2) 0.67708(16) 0.0675(7) Uani 1 1 d . . . . .
H11 H 0.5348 -0.1028 0.7166 0.081 Uiso 1 1 calc R . . . .
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'
Cl Cl 0.1484 0.1585 '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
Cl3 In1 Cl1 176.223(16) . . ?
Cl3 In1 Cl4 89.446(17) . . ?
Cl4 In1 Cl1 93.955(16) . . ?
Cl2 In1 Cl1 85.534(16) . . ?
Cl2 In1 Cl3 91.012(16) . . ?
Cl2 In1 Cl4 178.018(17) . . ?
Cl2 In1 Cl6 90.360(18) . . ?
Cl6 In1 Cl1 87.053(17) . . ?
Cl6 In1 Cl3 91.449(17) . . ?
Cl6 In1 Cl4 87.701(18) . . ?
Cl5 In1 Cl1 89.472(18) . . ?
Cl5 In1 Cl3 92.275(19) . . ?
Cl5 In1 Cl4 88.255(17) . . ?
Cl5 In1 Cl2 93.654(18) . . ?
Cl5 In1 Cl6 174.474(18) . . ?
C21 N9 H9 125.6 . . ?
C15 N9 H9 125.6 . . ?
C15 N9 C21 108.85(15) . . ?
C1 N3 H3 125.2 . . ?
C1 N3 C7 109.67(16) . . ?
C7 N3 H3 125.2 . . ?
C15 N8 H8 125.5 . . ?
C15 N8 C16 109.06(15) . . ?
C16 N8 H8 125.5 . . ?
C14 N6 H6A 125.4 . . ?
C8 N6 H6A 125.4 . . ?
C8 N6 C14 109.21(17) . . ?
H7A N7 H7B 120.0 . . ?
C15 N7 H7A 120.0 . . ?
C15 N7 H7B 120.0 . . ?
H1C O1 H1D 109.5 . . ?
C1 N2 H2 125.3 . . ?
C1 N2 C2 109.44(16) . . ?
C2 N2 H2 125.3 . . ?
C16 C21 N9 106.21(15) . . ?
C20 C21 N9 131.50(17) . . ?
C20 C21 C16 122.28(17) . . ?
C8 N5 H5A 125.2 . . ?
C8 N5 C9 109.50(17) . . ?
C9 N5 H5A 125.2 . . ?
N9 C15 N8 109.05(16) . . ?
N7 C15 N9 125.33(18) . . ?
N7 C15 N8 125.61(18) . . ?
C21 C16 N8 106.83(15) . . ?
C17 C16 N8 131.57(17) . . ?
C17 C16 C21 121.58(17) . . ?
N3 C1 N2 108.13(18) . . ?
N1 C1 N3 126.30(19) . . ?
N1 C1 N2 125.5(2) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C9 C14 N6 106.34(17) . . ?
C13 C14 N6 132.1(2) . . ?
C13 C14 C9 121.6(2) . . ?
C2 C7 N3 106.44(18) . . ?
C6 C7 N3 131.93(17) . . ?
C6 C7 C2 121.62(19) . . ?
C21 C20 H20 121.9 . . ?
C21 C20 C19 116.15(18) . . ?
C19 C20 H20 121.9 . . ?
H4A N4 H4B 120.0 . . ?
C8 N4 H4A 120.0 . . ?
C8 N4 H4B 120.0 . . ?
C7 C2 N2 106.31(17) . . ?
C3 C2 N2 132.32(19) . . ?
C3 C2 C7 121.4(2) . . ?
N5 C8 N6 108.6(2) . . ?
N4 C8 N6 125.5(2) . . ?
N4 C8 N5 125.9(2) . . ?
C14 C9 N5 106.30(18) . . ?
C10 C9 N5 132.2(2) . . ?
C10 C9 C14 121.5(2) . . ?
C16 C17 H17 121.9 . . ?
C18 C17 C16 116.17(19) . . ?
C18 C17 H17 121.9 . . ?
C20 C19 H19 119.2 . . ?
C18 C19 C20 121.54(19) . . ?
C18 C19 H19 119.2 . . ?
C7 C6 H6 121.6 . . ?
C5 C6 C7 116.8(2) . . ?
C5 C6 H6 121.6 . . ?
C14 C13 H13 121.7 . . ?
C14 C13 C12 116.6(2) . . ?
C12 C13 H13 121.7 . . ?
C9 C10 H10 121.8 . . ?
C9 C10 C11 116.4(2) . . ?
C11 C10 H10 121.8 . . ?
C17 C18 C19 122.27(19) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C2 C3 H3A 121.6 . . ?
C4 C3 C2 116.8(2) . . ?
C4 C3 H3A 121.6 . . ?
C6 C5 H5 119.1 . . ?
C6 C5 C4 121.9(2) . . ?
C4 C5 H5 119.1 . . ?
C13 C12 H12 119.1 . . ?
C11 C12 C13 121.9(3) . . ?
C11 C12 H12 119.1 . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.5(2) . . ?
C5 C4 H4 119.2 . . ?
C10 C11 H11 119.0 . . ?
C12 C11 C10 122.0(2) . . ?
C12 C11 H11 119.0 . . ?
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 Cl1 2.6035(4) . ?
In1 Cl3 2.5029(4) . ?
In1 Cl4 2.5261(5) . ?
In1 Cl2 2.4953(5) . ?
In1 Cl6 2.4967(5) . ?
In1 Cl5 2.4821(5) . ?
N9 H9 0.8800 . ?
N9 C21 1.398(2) . ?
N9 C15 1.336(2) . ?
N3 H3 0.8800 . ?
N3 C1 1.334(3) . ?
N3 C7 1.389(3) . ?
N8 H8 0.8800 . ?
N8 C15 1.337(2) . ?
N8 C16 1.386(2) . ?
N6 H6A 0.8800 . ?
N6 C14 1.390(3) . ?
N6 C8 1.341(3) . ?
N7 H7A 0.8800 . ?
N7 H7B 0.8800 . ?
N7 C15 1.320(2) . ?
O1 H1C 0.8498 . ?
O1 H1D 0.8497 . ?
N2 H2 0.8800 . ?
N2 C1 1.344(3) . ?
N2 C2 1.389(3) . ?
C21 C16 1.385(2) . ?
C21 C20 1.378(3) . ?
N5 H5A 0.8800 . ?
N5 C8 1.329(3) . ?
N5 C9 1.392(3) . ?
C16 C17 1.384(3) . ?
C1 N1 1.317(3) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
C14 C9 1.387(3) . ?
C14 C13 1.378(3) . ?
C7 C2 1.385(3) . ?
C7 C6 1.380(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.387(3) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C8 1.316(3) . ?
C2 C3 1.385(3) . ?
C9 C10 1.381(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.385(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.376(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.384(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(4) . ?
C18 H18 0.9500 . ?
C3 H3A 0.9500 . ?
C3 C4 1.382(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.380(4) . ?
C12 H12 0.9500 . ?
C12 C11 1.365(4) . ?
C4 H4 0.9500 . ?
C11 H11 0.9500 . ?
