#------------------------------------------------------------------------------
#$Date: 2025-01-06 13:49:34 +0200 (Mon, 06 Jan 2025) $
#$Revision: 297108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/95/7249565.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_7249565
loop_
_publ_author_name
'Shentseva, Irina A.'
'Usoltsev, Andrey N.'
'Korobeynikov, Nikita A.'
'Sokolov, Maxim N.'
'Adonin, Sergey A.'
_publ_section_title
;
 One-dimensional heterometallic Bi/Ag and Sb/Ag bromometalates(iii):
 structures, thermal stability and optical properties
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              6823
_journal_page_last               6827
_journal_paper_doi               10.1039/D4CE01083C
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'Ag Bi Br6, C10 H16 N4'
_chemical_formula_sum            'C10 H16 Ag Bi Br6 N4'
_chemical_formula_weight         988.58
_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   geom
_audit_creation_date             2024-08-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-26 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                96.3480(10)
_cell_angle_beta                 105.4260(10)
_cell_angle_gamma                108.2370(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9539(3)
_cell_length_b                   11.8928(4)
_cell_length_c                   12.5004(4)
_cell_measurement_reflns_used    5809
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.78
_cell_volume                     1058.08(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16378
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         1.729
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    20.559
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0477 after correction.
The Ratio of minimum to maximum transmission is 0.5812.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.103
_exptl_crystal_description       plank
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.828
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0326
_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)+(0.0191P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5252
_reflns_number_total             6428
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce01083c2.cif
_cod_data_source_block           is434_a
_cod_depositor_comments
'Adding full bibliography for 7249564--7249566.cif.'
_cod_database_code               7249565
_shelx_shelxl_version_number     2017/1
_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   0.578
_shelx_estimated_absorpt_t_min   0.148
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N4(H4), C1(H1), C9(H9), C3(H3), N1(H1A), C10(H10), C8(H8)
;
_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
Bi2 Bi 0.500000 1.000000 0.500000 0.01290(6) Uani 1 2 d S . P . .
Bi1 Bi 1.000000 1.500000 1.000000 0.01282(6) Uani 1 2 d S . P . .
Ag1 Ag 0.66392(7) 1.24068(5) 0.76189(4) 0.03737(12) Uani 1 1 d . . . . .
Br6 Br 0.53295(7) 0.87396(4) 0.67914(4) 0.01870(10) Uani 1 1 d . . . . .
Br4 Br 0.32625(7) 1.13376(5) 0.60939(5) 0.02203(11) Uani 1 1 d . . . . .
Br3 Br 0.87024(7) 1.23930(4) 0.96677(5) 0.02219(11) Uani 1 1 d . . . . .
Br2 Br 0.68026(7) 1.47771(5) 0.81699(4) 0.02220(11) Uani 1 1 d . . . . .
Br5 Br 0.85459(6) 1.18704(4) 0.61861(4) 0.01790(10) Uani 1 1 d . . . . .
Br1 Br 1.21107(6) 1.49145(4) 0.84990(4) 0.01759(10) Uani 1 1 d . . . . .
N2 N 0.1206(5) 0.4114(4) 0.4330(3) 0.0164(8) Uani 1 1 d . . . . .
N3 N -0.1962(5) -0.0921(3) 0.0989(3) 0.0159(8) Uani 1 1 d . . . . .
C2 C 0.3532(7) 0.5315(5) 0.5823(5) 0.0238(11) Uani 1 1 d . . . . .
H2 H 0.449797 0.562048 0.653379 0.029 Uiso 1 1 calc R U . . .
N4 N -0.3871(6) -0.2747(4) 0.0330(4) 0.0224(9) Uani 1 1 d . . . . .
H4 H -0.444141 -0.352557 0.027648 0.027 Uiso 1 1 calc R U . . .
C1 C 0.1536(7) 0.5240(4) 0.4169(4) 0.0173(10) Uani 1 1 d . . . . .
H1 H 0.087740 0.547514 0.353395 0.021 Uiso 1 1 calc R U . . .
C9 C -0.4346(7) -0.2106(5) -0.0471(5) 0.0252(12) Uani 1 1 d . . . . .
H9 H -0.532246 -0.241110 -0.117759 0.030 Uiso 1 1 calc R U . . .
C3 C 0.2450(7) 0.4150(5) 0.5359(4) 0.0225(11) Uani 1 1 d . . . . .
H3 H 0.252581 0.347269 0.567997 0.027 Uiso 1 1 calc R U . . .
C4 C -0.0277(7) 0.3027(4) 0.3556(4) 0.0193(10) Uani 1 1 d . . . . .
H4A H -0.107753 0.327621 0.294867 0.023 Uiso 1 1 calc R U . . .
H4B H -0.106573 0.259074 0.398087 0.023 Uiso 1 1 calc R U . . .
C5 C 0.0489(7) 0.2174(4) 0.3017(4) 0.0186(10) Uani 1 1 d . . . . .
H5A H 0.122209 0.258796 0.255454 0.022 Uiso 1 1 calc R U . . .
H5B H 0.133029 0.194381 0.361907 0.022 Uiso 1 1 calc R U . . .
C6 C -0.1100(6) 0.1046(4) 0.2273(4) 0.0174(10) Uani 1 1 d . . . . .
H6A H -0.184124 0.064683 0.273800 0.021 Uiso 1 1 calc R U . . .
H6B H -0.193025 0.128300 0.167149 0.021 Uiso 1 1 calc R U . . .
C7 C -0.0415(7) 0.0155(4) 0.1726(5) 0.0235(11) Uani 1 1 d . . . . .
H7A H 0.034778 0.055736 0.127215 0.028 Uiso 1 1 calc R U . . .
H7B H 0.039233 -0.009778 0.232589 0.028 Uiso 1 1 calc R U . . .
N1 N 0.2956(6) 0.5978(4) 0.5059(4) 0.0192(9) Uani 1 1 d . . . . .
H1A H 0.345061 0.676905 0.514561 0.023 Uiso 1 1 calc R U . . .
C10 C -0.3146(7) -0.0951(5) -0.0056(4) 0.0212(11) Uani 1 1 d . . . . .
H10 H -0.312161 -0.028456 -0.041423 0.025 Uiso 1 1 calc R U . . .
C8 C -0.2427(7) -0.2020(4) 0.1195(5) 0.0221(11) Uani 1 1 d . . . . .
H8 H -0.182624 -0.225095 0.185224 0.027 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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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'
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
Br6 Bi2 Br6 180.00(2) 2_676 . ?
Br6 Bi2 Br4 90.687(14) 2_676 . ?
Br6 Bi2 Br4 89.313(14) . . ?
Br6 Bi2 Br4 89.313(14) 2_676 2_676 ?
Br6 Bi2 Br4 90.687(14) . 2_676 ?
Br6 Bi2 Br5 91.574(14) . . ?
Br6 Bi2 Br5 88.427(14) 2_676 . ?
Br6 Bi2 Br5 91.573(14) 2_676 2_676 ?
Br6 Bi2 Br5 88.427(14) . 2_676 ?
Br4 Bi2 Br4 180.0 . 2_676 ?
Br4 Bi2 Br5 91.036(15) . 2_676 ?
Br4 Bi2 Br5 91.035(15) 2_676 . ?
Br4 Bi2 Br5 88.965(15) . . ?
Br4 Bi2 Br5 88.965(15) 2_676 2_676 ?
Br5 Bi2 Br5 180.0 . 2_676 ?
Br3 Bi1 Br3 180.0 2_787 . ?
Br2 Bi1 Br3 90.963(15) 2_787 . ?
Br2 Bi1 Br3 89.036(15) 2_787 2_787 ?
Br2 Bi1 Br3 89.037(15) . . ?
Br2 Bi1 Br3 90.964(15) . 2_787 ?
Br2 Bi1 Br2 179.999(18) . 2_787 ?
Br1 Bi1 Br3 90.135(14) 2_787 2_787 ?
Br1 Bi1 Br3 89.864(14) 2_787 . ?
Br1 Bi1 Br3 89.865(14) . 2_787 ?
Br1 Bi1 Br3 90.136(14) . . ?
Br1 Bi1 Br2 91.557(15) . . ?
Br1 Bi1 Br2 88.444(15) . 2_787 ?
Br1 Bi1 Br2 91.556(15) 2_787 2_787 ?
Br1 Bi1 Br2 88.443(15) 2_787 . ?
Br1 Bi1 Br1 180.0 2_787 . ?
Br4 Ag1 Br2 102.31(2) . . ?
Br4 Ag1 Br5 95.26(2) . . ?
Br3 Ag1 Br4 142.69(3) . . ?
Br3 Ag1 Br2 95.46(2) . . ?
Br3 Ag1 Br5 104.35(2) . . ?
Br5 Ag1 Br2 119.10(2) . . ?
Ag1 Br4 Bi2 84.931(18) . . ?
Ag1 Br3 Bi1 85.195(17) . . ?
Ag1 Br2 Bi1 83.629(17) . . ?
Ag1 Br5 Bi2 82.780(16) . . ?
C1 N2 C3 108.5(4) . . ?
C1 N2 C4 125.1(4) . . ?
C3 N2 C4 126.3(4) . . ?
C10 N3 C7 125.3(4) . . ?
C8 N3 C7 126.0(4) . . ?
C8 N3 C10 108.7(4) . . ?
C3 C2 H2 126.9 . . ?
C3 C2 N1 106.1(4) . . ?
N1 C2 H2 126.9 . . ?
C9 N4 H4 125.2 . . ?
C8 N4 H4 125.2 . . ?
C8 N4 C9 109.7(4) . . ?
N2 C1 H1 126.1 . . ?
N2 C1 N1 107.7(4) . . ?
N1 C1 H1 126.1 . . ?
N4 C9 H9 126.9 . . ?
C10 C9 N4 106.2(5) . . ?
C10 C9 H9 126.9 . . ?
N2 C3 H3 126.1 . . ?
C2 C3 N2 107.8(4) . . ?
C2 C3 H3 126.1 . . ?
N2 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
N2 C4 C5 112.6(4) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 C4 110.1(4) . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 C5 112.4(4) . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
N3 C7 C6 112.0(4) . . ?
N3 C7 H7A 109.2 . . ?
N3 C7 H7B 109.2 . . ?
C6 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C2 N1 H1A 125.1 . . ?
C1 N1 C2 109.8(4) . . ?
C1 N1 H1A 125.1 . . ?
N3 C10 H10 126.4 . . ?
C9 C10 N3 107.1(4) . . ?
C9 C10 H10 126.4 . . ?
N3 C8 N4 108.3(4) . . ?
N3 C8 H8 125.8 . . ?
N4 C8 H8 125.8 . . ?
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
Bi2 Br6 2.8294(5) 2_676 ?
Bi2 Br6 2.8295(5) . ?
Bi2 Br4 2.8654(5) 2_676 ?
Bi2 Br4 2.8654(5) . ?
Bi2 Br5 2.8671(5) . ?
Bi2 Br5 2.8672(5) 2_676 ?
Bi1 Br3 2.8869(5) 2_787 ?
Bi1 Br3 2.8870(5) . ?
Bi1 Br2 2.8497(5) 2_787 ?
Bi1 Br2 2.8497(5) . ?
Bi1 Br1 2.8442(5) . ?
Bi1 Br1 2.8442(5) 2_787 ?
Ag1 Br4 2.6584(7) . ?
Ag1 Br3 2.6538(7) . ?
Ag1 Br2 2.7806(7) . ?
Ag1 Br5 2.7771(7) . ?
N2 C1 1.331(6) . ?
N2 C3 1.385(6) . ?
N2 C4 1.470(6) . ?
N3 C7 1.466(6) . ?
N3 C10 1.381(6) . ?
N3 C8 1.317(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.344(7) . ?
C2 N1 1.380(6) . ?
N4 H4 0.8800 . ?
N4 C9 1.370(6) . ?
N4 C8 1.322(7) . ?
C1 H1 0.9500 . ?
C1 N1 1.334(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.351(7) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.519(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.517(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.512(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 H1A 0.8800 . ?
C10 H10 0.9500 . ?
C8 H8 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
N2 C1 N1 C2 -1.2(5) . . . . ?
N2 C4 C5 C6 177.4(4) . . . . ?
N4 C9 C10 N3 0.3(6) . . . . ?
C1 N2 C3 C2 0.4(6) . . . . ?
C1 N2 C4 C5 114.5(5) . . . . ?
C9 N4 C8 N3 0.9(6) . . . . ?
C3 N2 C1 N1 0.5(5) . . . . ?
C3 N2 C4 C5 -67.7(6) . . . . ?
C3 C2 N1 C1 1.4(6) . . . . ?
C4 N2 C1 N1 178.7(4) . . . . ?
C4 N2 C3 C2 -177.7(4) . . . . ?
C4 C5 C6 C7 -179.3(4) . . . . ?
C5 C6 C7 N3 -178.8(4) . . . . ?
C7 N3 C10 C9 178.7(4) . . . . ?
C7 N3 C8 N4 -179.1(4) . . . . ?
N1 C2 C3 N2 -1.1(6) . . . . ?
C10 N3 C7 C6 72.3(6) . . . . ?
C10 N3 C8 N4 -0.6(6) . . . . ?
C8 N3 C7 C6 -109.4(5) . . . . ?
C8 N3 C10 C9 0.2(6) . . . . ?
C8 N4 C9 C10 -0.7(6) . . . . ?
