#------------------------------------------------------------------------------
#$Date: 2021-07-24 02:49:55 +0300 (Sat, 24 Jul 2021) $
#$Revision: 267727 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/05/8000521.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_8000521
loop_
_publ_author_name
'Wei, Qilin'
'Chang, Tong'
'Zeng, Ruosheng'
'Cao, Sheng'
'Zhao, Jialong'
'Han, Xinxin'
'Wang, Lishuang'
'Zou, Bingsuo'
_publ_section_title
;
 Self-Trapped Exciton Emission in a Zero-Dimensional
 (TMA)₂SbCl₅·DMF Single Crystal and Molecular
 Dynamics Simulation of Structural Stability.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              7091
_journal_page_last               7099
_journal_paper_doi               10.1021/acs.jpclett.1c02119
_journal_year                    2021
_chemical_formula_moiety         'Cl5 Sb, C3 H7 N O, 2(C3 H10 N)'
_chemical_formula_sum            'C9 H27 Cl5 N3 O Sb'
_chemical_formula_weight         492.33
_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             2020-08-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1372(3)
_cell_length_b                   17.9515(7)
_cell_length_c                   12.0858(5)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.01
_cell_volume                     1982.32(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32396
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         2.031
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0548 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.3986.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0266
_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)+(0.0322P)²+4.4803P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3900
_reflns_number_total             4037
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jz1c02119_si_002.cif
_cod_data_source_block           mo_0819_2_0m
_cod_database_code               8000521
_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   0.820
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 O1(H1)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c), C9(H9a,
 H9b,H9c), C5(H5a,H5b,H5c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c)
;
_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 0.25355(2) 0.63438(2) 0.23903(2) 0.02389(7) Uani 1 1 d . . . . .
Cl1 Cl 0.02735(8) 0.54823(4) 0.20445(6) 0.03039(15) Uani 1 1 d . . . . .
Cl2 Cl 0.22800(8) 0.60643(4) 0.43287(6) 0.03223(16) Uani 1 1 d . . . . .
Cl3 Cl 0.47720(8) 0.71905(4) 0.29101(6) 0.03276(16) Uani 1 1 d . . . . .
Cl4 Cl 0.08058(8) 0.75429(4) 0.27958(6) 0.03258(16) Uani 1 1 d . . . . .
Cl5 Cl 0.42600(8) 0.52392(4) 0.22089(6) 0.03327(16) Uani 1 1 d . . . . .
O1 O 0.7615(2) 0.78817(12) 0.49401(18) 0.0330(5) Uani 1 1 d . . . . .
N1 N 0.7586(3) 0.87677(14) 0.3594(2) 0.0280(5) Uani 1 1 d . . . . .
C1 C 0.7569(4) 0.89442(19) 0.2420(2) 0.0341(7) Uani 1 1 d . . . . .
H1A H 0.845331 0.922526 0.223391 0.051 Uiso 1 1 calc R U . . .
H1B H 0.670244 0.924469 0.224421 0.051 Uiso 1 1 calc R U . . .
H1C H 0.754032 0.848168 0.198929 0.051 Uiso 1 1 calc R U . . .
C2 C 0.7623(3) 0.80703(17) 0.3948(3) 0.0289(6) Uani 1 1 d . . . . .
H2A H 0.765912 0.768651 0.340738 0.035 Uiso 1 1 calc R U . . .
C3 C 0.7557(4) 0.93886(17) 0.4361(3) 0.0316(6) Uani 1 1 d . . . . .
H3A H 0.856178 0.953489 0.455093 0.047 Uiso 1 1 calc R U . . .
H3B H 0.704290 0.924014 0.503459 0.047 Uiso 1 1 calc R U . . .
H3C H 0.704749 0.981041 0.401685 0.047 Uiso 1 1 calc R U . . .
N2 N 0.2659(3) 0.82850(14) 0.4712(2) 0.0289(5) Uani 1 1 d . . . . .
H2 H 0.238574 0.793180 0.410461 0.035 Uiso 1 1 calc R U . . .
C4 C 0.3522(4) 0.89010(17) 0.4216(3) 0.0336(7) Uani 1 1 d . . . . .
H4A H 0.389910 0.922514 0.480488 0.050 Uiso 1 1 calc R U . . .
H4B H 0.289263 0.919097 0.371613 0.050 Uiso 1 1 calc R U . . .
H4C H 0.434162 0.869267 0.379970 0.050 Uiso 1 1 calc R U . . .
C6 C 0.3560(4) 0.78680(19) 0.5536(3) 0.0438(8) Uani 1 1 d . . . . .
H6A H 0.442497 0.766191 0.517274 0.066 Uiso 1 1 calc R U . . .
H6B H 0.297837 0.746144 0.584835 0.066 Uiso 1 1 calc R U . . .
H6C H 0.386927 0.820608 0.613032 0.066 Uiso 1 1 calc R U . . .
C9 C 0.1284(4) 0.8569(2) 0.5205(3) 0.0471(9) Uani 1 1 d . . . . .
H9A H 0.152081 0.891724 0.580492 0.071 Uiso 1 1 calc R U . . .
H9B H 0.071880 0.815075 0.550069 0.071 Uiso 1 1 calc R U . . .
H9C H 0.070468 0.882598 0.463612 0.071 Uiso 1 1 calc R U . . .
N3 N 0.7510(3) 0.63542(14) 0.5168(2) 0.0281(5) Uani 1 1 d . . . . .
H3 H 0.743958 0.690619 0.506964 0.034 Uiso 1 1 calc R U . . .
C5 C 0.6033(4) 0.60771(19) 0.5461(3) 0.0378(7) Uani 1 1 d . . . . .
H5A H 0.534104 0.619605 0.486313 0.057 Uiso 1 1 calc R U . . .
H5B H 0.571293 0.631600 0.614706 0.057 Uiso 1 1 calc R U . . .
H5C H 0.606937 0.553611 0.556716 0.057 Uiso 1 1 calc R U . . .
C7 C 0.8011(4) 0.60330(19) 0.4107(3) 0.0386(7) Uani 1 1 d . . . . .
H7A H 0.810931 0.549172 0.418263 0.058 Uiso 1 1 calc R U . . .
H7B H 0.896062 0.624850 0.391298 0.058 Uiso 1 1 calc R U . . .
H7C H 0.729480 0.614632 0.352275 0.058 Uiso 1 1 calc R U . . .
C8 C 0.8580(4) 0.6210(2) 0.6068(3) 0.0404(8) Uani 1 1 d . . . . .
H8A H 0.829245 0.648636 0.673141 0.061 Uiso 1 1 calc R U . . .
H8B H 0.955378 0.637288 0.583610 0.061 Uiso 1 1 calc R U . . .
H8C H 0.860125 0.567585 0.623379 0.061 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'
Cl Cl 0.1484 0.1585 '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'
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
Cl1 Sb1 Cl3 175.32(2) . . ?
Cl1 Sb1 Cl4 92.13(2) . . ?
Cl2 Sb1 Cl1 87.10(2) . . ?
Cl2 Sb1 Cl3 88.24(3) . . ?
Cl2 Sb1 Cl4 85.90(3) . . ?
Cl2 Sb1 Cl5 89.23(3) . . ?
Cl3 Sb1 Cl4 87.18(2) . . ?
Cl5 Sb1 Cl1 90.84(2) . . ?
Cl5 Sb1 Cl3 89.45(2) . . ?
Cl5 Sb1 Cl4 174.15(2) . . ?
C2 N1 C1 121.4(3) . . ?
C2 N1 C3 121.4(3) . . ?
C3 N1 C1 117.2(2) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 N1 124.6(3) . . ?
O1 C2 H2A 117.7 . . ?
N1 C2 H2A 117.7 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 N2 H2 107.8 . . ?
C4 N2 C6 110.6(3) . . ?
C6 N2 H2 107.8 . . ?
C9 N2 H2 107.8 . . ?
C9 N2 C4 111.1(3) . . ?
C9 N2 C6 111.6(3) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 N3 H3 107.6 . . ?
C7 N3 H3 107.6 . . ?
C7 N3 C5 111.3(3) . . ?
C8 N3 H3 107.6 . . ?
C8 N3 C5 111.3(3) . . ?
C8 N3 C7 111.2(3) . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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 Cl1 2.6123(7) . ?
Sb1 Cl2 2.4090(7) . ?
Sb1 Cl3 2.6191(7) . ?
Sb1 Cl4 2.7175(7) . ?
Sb1 Cl5 2.5433(7) . ?
O1 C2 1.246(4) . ?
N1 C1 1.454(4) . ?
N1 C2 1.323(4) . ?
N1 C3 1.450(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N2 H2 1.0000 . ?
N2 C4 1.487(4) . ?
N2 C6 1.489(4) . ?
N2 C9 1.485(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N3 H3 1.0000 . ?
N3 C5 1.484(4) . ?
N3 C7 1.482(4) . ?
N3 C8 1.479(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
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
C1 N1 C2 O1 -178.7(3) . . . . ?
C3 N1 C2 O1 1.1(5) . . . . ?
