#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:54:05 +0300 (Fri, 05 May 2023) $
#$Revision: 283385 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/23/7062391.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_7062391
loop_
_publ_author_name
'Jin, Shuya'
'Wei, Qilin'
'Peng, Hui'
'Ke, Bao'
'Lin, Wenchao'
'He, Bin'
'Zhong, Xianci'
'Zou, Bingsuo'
_publ_section_title
;
 Boosting the broadband orange emission in organic--inorganic hybrid
 (DPG)3InBr6via antimony doping
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8249
_journal_page_last               8257
_journal_paper_doi               10.1039/D3NJ01019H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'Br6 In1, 3(C13 H14 N3)'
_chemical_formula_sum            'C39 H42 Br6 In N9'
_chemical_formula_weight         1231.09
_chemical_name_systematic
'tris(N,N'-Diphenylquanidinum) hexabromoindium(iii)'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-04 deposited with the CCDC.	2023-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.613(3)
_cell_length_b                   16.613
_cell_length_c                   14.280(2)
_cell_measurement_reflns_used    2505
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.700
_cell_measurement_theta_min      2.452
_cell_volume                     3413.1(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON 100'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_min         3.171
_diffrn_source                   TXS
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.826
_exptl_absorpt_correction_T_max  0.0469
_exptl_absorpt_correction_T_min  0.0180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0335 after correction.
The Ratio of minimum to maximum transmission is 0.3838.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             1794
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0288
_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)+(0.0363P)²+6.5891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1332
_reflns_number_total             1740
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj01019h2.cif
_cod_data_source_block           220901h_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7062391.cif.
;
_cod_original_cell_volume        3413.1(13)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7062391
_shelx_shelxl_version_number     2019/2
_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   0.593
_shelx_estimated_absorpt_t_min   0.518
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2. Others
 Fixed Sof: C7(0.5) N2(0.5) H2(0.5) N1(0.5) H1(0.5) C9(0.5) H9(0.5) C8(0.5)
 C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5) C10(0.5) H10(0.5)
 N3(0.5) H3A(0.5) H3B(0.5) C6(0.5) C5(0.5) H5(0.5) C4(0.5) H4(0.5) C3(0.5)
 H3(0.5) C2(0.5) H2A(0.5) C1(0.5) H1A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C9(H9), C13(H13), C12(H12), C11(H11), C10(H10), C5(H5),
 C4(H4), C3(H3), C2(H2A), C1(H1A)
3.b Fitted hexagon refined as free rotating group:
 C9(C8,C13,C12,C11,C10), C6(C5,C4,C3,C2,C1)
3.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.333333 0.666667 0.666667 0.04717(16) Uani 1 6 d S T P . .
Br1 Br 0.26847(2) 0.51289(2) 0.56199(2) 0.05789(14) Uani 1 1 d . . . . .
C7 C 0.4981(16) 0.5114(11) 0.5039(13) 0.050(2) Uani 0.5 1 d . . P A -1
N2 N 0.4694(5) 0.4886(5) 0.5907(5) 0.0692(17) Uani 0.5 1 d . . P A -1
H2 H 0.457499 0.527138 0.621924 0.083 Uiso 0.5 1 calc R U P A -1
N1 N 0.5067(5) 0.5910(4) 0.4704(5) 0.0712(17) Uani 0.5 1 d . . P A -1
H1 H 0.493395 0.623262 0.510096 0.085 Uiso 0.5 1 calc R U P A -1
C9 C 0.5294(4) 0.3926(5) 0.6539(6) 0.076(2) Uani 0.5 1 d G . P A -1
H9 H 0.588557 0.433471 0.627399 0.092 Uiso 0.5 1 calc R U P A -1
C8 C 0.4555(5) 0.4080(4) 0.6390(4) 0.0593(18) Uani 0.5 1 d G . P A -1
C13 C 0.3690(4) 0.3482(6) 0.6778(7) 0.091(4) Uani 0.5 1 d G . P A -1
H13 H 0.318492 0.358666 0.667553 0.110 Uiso 0.5 1 calc R U P A -1
C12 C 0.3564(6) 0.2730(6) 0.7315(8) 0.120(6) Uani 0.5 1 d G . P A -1
H12 H 0.297264 0.232079 0.758058 0.144 Uiso 0.5 1 calc R U P A -1
C11 C 0.4303(7) 0.2576(5) 0.7465(7) 0.109(4) Uani 0.5 1 d G . P A -1
H11 H 0.421682 0.206188 0.783234 0.130 Uiso 0.5 1 calc R U P A -1
C10 C 0.5168(6) 0.3174(6) 0.7077(7) 0.086(3) Uani 0.5 1 d G . P A -1
H10 H 0.567328 0.306882 0.717905 0.103 Uiso 0.5 1 calc R U P A -1
N3 N 0.5157(5) 0.4576(4) 0.4490(5) 0.0608(15) Uani 0.5 1 d . . P A -1
H3A H 0.508113 0.404548 0.470376 0.073 Uiso 0.5 1 calc R U P A -1
H3B H 0.534855 0.474893 0.391170 0.073 Uiso 0.5 1 calc R U P A -1
C6 C 0.5337(5) 0.6290(4) 0.3812(4) 0.0617(18) Uani 0.5 1 d G . P A -1
C5 C 0.6214(6) 0.6556(7) 0.3457(7) 0.098(5) Uani 0.5 1 d G . P A -1
H5 H 0.660515 0.637793 0.377221 0.118 Uiso 0.5 1 calc R U P A -1
C4 C 0.6520(6) 0.7081(8) 0.2642(8) 0.111(5) Uani 0.5 1 d G . P A -1
H4 H 0.711904 0.726199 0.239932 0.133 Uiso 0.5 1 calc R U P A -1
C3 C 0.5948(7) 0.7341(7) 0.2181(6) 0.115(5) Uani 0.5 1 d G . P A -1
H3 H 0.615635 0.769957 0.162371 0.138 Uiso 0.5 1 calc R U P A -1
C2 C 0.5071(7) 0.7075(8) 0.2536(5) 0.105(4) Uani 0.5 1 d G . P A -1
H2A H 0.467977 0.725310 0.222098 0.126 Uiso 0.5 1 calc R U P A -1
C1 C 0.4765(4) 0.6550(7) 0.3351(5) 0.084(3) Uani 0.5 1 d G . P A -1
H1A H 0.416585 0.636905 0.359388 0.100 Uiso 0.5 1 calc R U P A -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'
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'
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 3_565 15_556 ?
Br1 In1 Br1 91.859(12) 14_456 13_566 ?
Br1 In1 Br1 88.140(13) 14_456 . ?
Br1 In1 Br1 88.140(13) 2_665 13_566 ?
Br1 In1 Br1 88.139(13) 15_556 . ?
Br1 In1 Br1 91.862(13) 2_665 . ?
Br1 In1 Br1 180.0 13_566 . ?
Br1 In1 Br1 91.861(16) 3_565 2_665 ?
Br1 In1 Br1 91.863(17) 15_556 14_456 ?
Br1 In1 Br1 91.862(13) 3_565 . ?
Br1 In1 Br1 180.0 2_665 14_456 ?
Br1 In1 Br1 88.140(17) 15_556 2_665 ?
Br1 In1 Br1 88.136(13) 3_565 13_566 ?
Br1 In1 Br1 91.863(13) 15_556 13_566 ?
Br1 In1 Br1 88.136(17) 3_565 14_456 ?
N2 C7 N1 117.5(10) . . ?
N2 C7 N3 122.3(11) . . ?
N3 C7 N1 120.1(14) . . ?
C7 N2 H2 116.8 . . ?
C7 N2 C8 126.4(7) . . ?
C8 N2 H2 116.8 . . ?
C7 N1 H1 115.8 . . ?
C7 N1 C6 128.4(9) . . ?
C6 N1 H1 115.8 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C8 N2 120.5(6) . . ?
C9 C8 C13 120.0 . . ?
C13 C8 N2 119.3(6) . . ?
C8 C13 H13 120.0 . . ?
C8 C13 C12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C13 C12 C11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C7 N3 H3A 120.0 . . ?
C7 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C5 C6 N1 121.8(6) . . ?
C5 C6 C1 120.0 . . ?
C1 C6 N1 117.3(6) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C3 C2 C1 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C6 C1 H1A 120.0 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 H1A 120.0 . . ?
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 Br1 2.6775(4) 3_565 ?
In1 Br1 2.6776(5) 14_456 ?
In1 Br1 2.6775(5) 2_665 ?
In1 Br1 2.6775(4) . ?
In1 Br1 2.6776(3) 13_566 ?
In1 Br1 2.6774(4) 15_556 ?
C7 N2 1.314(19) . ?
C7 N1 1.346(15) . ?
C7 N3 1.326(14) . ?
N2 H2 0.8800 . ?
N2 C8 1.419(9) . ?
N1 H1 0.8800 . ?
N1 C6 1.393(8) . ?
C9 H9 0.9500 . ?
C9 C8 1.3900 . ?
C9 C10 1.3900 . ?
C8 C13 1.3900 . ?
C13 H13 0.9500 . ?
C13 C12 1.3900 . ?
C12 H12 0.9500 . ?
C12 C11 1.3900 . ?
C11 H11 0.9500 . ?
C11 C10 1.3900 . ?
C10 H10 0.9500 . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
C6 C5 1.3900 . ?
C6 C1 1.3900 . ?
C5 H5 0.9500 . ?
C5 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C3 1.3900 . ?
C3 H3 0.9500 . ?
C3 C2 1.3900 . ?
C2 H2A 0.9500 . ?
C2 C1 1.3900 . ?
C1 H1A 0.9500 . ?
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
C7 N2 C8 C9 61.5(16) . . . . ?
C7 N2 C8 C13 -123.6(15) . . . . ?
C7 N1 C6 C5 -62.4(16) . . . . ?
C7 N1 C6 C1 128.8(14) . . . . ?
N2 C7 N1 C6 -178.6(12) . . . . ?
N2 C8 C13 C12 -174.9(7) . . . . ?
N1 C7 N2 C8 179.8(11) . . . . ?
N1 C6 C5 C4 -168.5(7) . . . . ?
N1 C6 C1 C2 169.0(7) . . . . ?
C9 C8 C13 C12 0.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C8 C13 C12 C11 0.0 . . . . ?
C13 C12 C11 C10 0.0 . . . . ?
C12 C11 C10 C9 0.0 . . . . ?
C10 C9 C8 N2 174.9(7) . . . . ?
C10 C9 C8 C13 0.0 . . . . ?
N3 C7 N2 C8 2(3) . . . . ?
N3 C7 N1 C6 -1(3) . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C5 C6 C1 C2 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C4 C3 C2 C1 0.0 . . . . ?
C3 C2 C1 C6 0.0 . . . . ?
C1 C6 C5 C4 0.0 . . . . ?
