#------------------------------------------------------------------------------
#$Date: 2022-01-04 04:27:16 +0200 (Tue, 04 Jan 2022) $
#$Revision: 271786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/05/8000561.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_8000561
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         'Br5 Sb, 2(C7 H8 N3)'
_chemical_formula_sum            'C14 H16 Br5 N6 Sb'
_chemical_formula_weight         789.63
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.667(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3309(6)
_cell_length_b                   15.6212(10)
_cell_length_c                   14.2713(9)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      3.01
_cell_volume                     2182.0(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43994
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         2.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.433
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0992 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.3514. 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    2.404
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0212
_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)+(0.0252P)²+0.6449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3841
_reflns_number_total             4421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jz1c03649_si_004.cif
_cod_data_source_block           mo_0416_10_0m
_cod_database_code               8000561
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5A), N6(H6A), N3(H3), C3(H3A), C6(H6), C13(H13), C5(H5), C4(H4),
 C12(H12), C10(H10), C11(H11)
2.b X=CH2 refined with riding coordinates:
 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
Sb1 Sb 0.63155(2) 0.43085(2) 0.43847(2) 0.03133(6) Uani 1 1 d . . . . .
Br1 Br 0.70257(3) 0.26537(2) 0.46178(2) 0.03807(8) Uani 1 1 d . . . . .
Br2 Br 0.54195(3) 0.61066(2) 0.42689(2) 0.04082(8) Uani 1 1 d . . . . .
Br3 Br 0.39508(3) 0.39195(2) 0.26245(2) 0.04204(8) Uani 1 1 d . . . . .
Br5 Br 0.76777(4) 0.45275(2) 0.31375(3) 0.04648(9) Uani 1 1 d . . . . .
Br4 Br 0.84728(3) 0.47795(2) 0.58854(3) 0.04535(9) Uani 1 1 d . . . . .
N2 N 0.3601(3) 0.19719(17) 0.39946(19) 0.0397(6) Uani 1 1 d . . . . .
H2 H 0.3866 0.2510 0.4068 0.048 Uiso 1 1 calc R . . . .
N5 N 0.1096(3) 0.33097(17) 0.5599(2) 0.0407(6) Uani 1 1 d . . . . .
H5A H 0.1294 0.3843 0.5498 0.049 Uiso 1 1 calc R . . . .
N6 N 0.0799(3) 0.21545(17) 0.6343(2) 0.0417(6) Uani 1 1 d . . . . .
H6A H 0.0768 0.1799 0.6814 0.050 Uiso 1 1 calc R . . . .
N3 N 0.2725(3) 0.07736(17) 0.3295(2) 0.0425(6) Uani 1 1 d . . . . .
H3 H 0.2327 0.0394 0.2838 0.051 Uiso 1 1 calc R . . . .
N1 N 0.2666(3) 0.1961(2) 0.2257(2) 0.0546(8) Uani 1 1 d . . . . .
H1A H 0.2249 0.1668 0.1718 0.066 Uiso 1 1 calc R . . . .
H1B H 0.2874 0.2503 0.2214 0.066 Uiso 1 1 calc R . . . .
N4 N 0.1522(3) 0.3387(2) 0.7328(2) 0.0556(8) Uani 1 1 d . . . . .
H4A H 0.1533 0.3116 0.7871 0.067 Uiso 1 1 calc R . . . .
H4B H 0.1750 0.3931 0.7354 0.067 Uiso 1 1 calc R . . . .
C1 C 0.2981(3) 0.1588(2) 0.3129(3) 0.0418(7) Uani 1 1 d . . . . .
C8 C 0.1163(3) 0.2976(2) 0.6474(2) 0.0408(7) Uani 1 1 d . . . . .
C2 C 0.3762(3) 0.1386(2) 0.4765(2) 0.0380(7) Uani 1 1 d . . . . .
C3 C 0.4366(4) 0.1457(2) 0.5773(3) 0.0442(7) Uani 1 1 d . . . . .
H3A H 0.4756 0.1979 0.6077 0.053 Uiso 1 1 calc R . . . .
C9 C 0.0664(3) 0.2682(2) 0.4869(2) 0.0378(7) Uani 1 1 d . . . . .
C14 C 0.0473(3) 0.1947(2) 0.5345(2) 0.0381(7) Uani 1 1 d . . . . .
C7 C 0.3192(3) 0.0621(2) 0.4318(3) 0.0398(7) Uani 1 1 d . . . . .
C6 C 0.3203(3) -0.0107(2) 0.4865(3) 0.0456(8) Uani 1 1 d . . . . .
H6 H 0.2815 -0.0629 0.4562 0.055 Uiso 1 1 calc R . . . .
C13 C 0.0021(4) 0.1199(2) 0.4842(3) 0.0531(9) Uani 1 1 d . . . . .
H13 H -0.0124 0.0697 0.5171 0.064 Uiso 1 1 calc R . . . .
C5 C 0.3808(4) -0.0040(2) 0.5877(3) 0.0512(9) Uani 1 1 d . . . . .
H5 H 0.3836 -0.0529 0.6279 0.061 Uiso 1 1 calc R . . . .
C4 C 0.4373(4) 0.0721(2) 0.6320(3) 0.0517(9) Uani 1 1 d . . . . .
H4 H 0.4777 0.0740 0.7019 0.062 Uiso 1 1 calc R . . . .
C12 C -0.0212(4) 0.1214(3) 0.3833(3) 0.0621(11) Uani 1 1 d . . . . .
H12 H -0.0501 0.0706 0.3457 0.075 Uiso 1 1 calc R . . . .
C10 C 0.0414(4) 0.2706(3) 0.3863(3) 0.0507(9) Uani 1 1 d . . . . .
H10 H 0.0543 0.3213 0.3536 0.061 Uiso 1 1 calc R . . . .
C11 C -0.0030(4) 0.1962(3) 0.3362(3) 0.0616(11) Uani 1 1 d . . . . .
H11 H -0.0220 0.1954 0.2665 0.074 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'
Br Br -0.2901 2.4595 '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'
Sb Sb -0.5866 1.5461 '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 Sb1 Br2 174.825(12) . . ?
Br1 Sb1 Br3 91.504(11) . . ?
Br2 Sb1 Br3 89.366(11) . . ?
Br5 Sb1 Br1 91.434(12) . . ?
Br5 Sb1 Br2 93.718(12) . . ?
Br5 Sb1 Br3 85.814(13) . . ?
Br5 Sb1 Br4 90.980(14) . . ?
Br4 Sb1 Br1 92.376(12) . . ?
Br4 Sb1 Br2 87.048(11) . . ?
Br4 Sb1 Br3 175.028(13) . . ?
C1 N2 C2 109.5(3) . . ?
C8 N5 C9 109.4(3) . . ?
C8 N6 C14 109.3(3) . . ?
C1 N3 C7 109.0(3) . . ?
N3 C1 N2 109.0(3) . . ?
N1 C1 N2 125.1(3) . . ?
N1 C1 N3 125.9(3) . . ?
N6 C8 N5 108.5(3) . . ?
N4 C8 N5 126.1(3) . . ?
N4 C8 N6 125.4(3) . . ?
C3 C2 N2 132.0(3) . . ?
C3 C2 C7 122.0(3) . . ?
C7 C2 N2 106.0(3) . . ?
C2 C3 C4 116.1(3) . . ?
C14 C9 N5 106.2(3) . . ?
C10 C9 N5 132.0(3) . . ?
C10 C9 C14 121.8(3) . . ?
C9 C14 N6 106.5(3) . . ?
C13 C14 N6 131.5(3) . . ?
C13 C14 C9 122.0(3) . . ?
C2 C7 N3 106.5(3) . . ?
C6 C7 N3 131.9(3) . . ?
C6 C7 C2 121.6(3) . . ?
C7 C6 C5 116.6(3) . . ?
C14 C13 C12 116.6(4) . . ?
C6 C5 C4 121.8(3) . . ?
C5 C4 C3 121.9(3) . . ?
C13 C12 C11 120.8(4) . . ?
C11 C10 C9 116.3(4) . . ?
C10 C11 C12 122.4(4) . . ?
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
Sb1 Br1 2.6785(4) . ?
Sb1 Br2 2.9455(4) . ?
Sb1 Br3 2.9528(4) . ?
Sb1 Br5 2.6209(4) . ?
Sb1 Br4 2.6533(4) . ?
N2 C1 1.338(4) . ?
N2 C2 1.399(4) . ?
N5 C8 1.334(4) . ?
N5 C9 1.396(4) . ?
N6 C8 1.334(4) . ?
N6 C14 1.394(4) . ?
N3 C1 1.336(4) . ?
N3 C7 1.404(4) . ?
N1 C1 1.316(4) . ?
N4 C8 1.321(4) . ?
C2 C3 1.377(5) . ?
C2 C7 1.394(4) . ?
C3 C4 1.388(5) . ?
C9 C14 1.380(4) . ?
C9 C10 1.375(5) . ?
C14 C13 1.373(5) . ?
C7 C6 1.377(5) . ?
C6 C5 1.382(5) . ?
C13 C12 1.381(6) . ?
C5 C4 1.385(5) . ?
C12 C11 1.392(6) . ?
C10 C11 1.366(6) . ?
