Photoluminescent chain-of-dimer anion in a novel hybrid halometallate (C<sub>5</sub>H<sub>14</sub>N<sub>2</sub>)<sub>3</sub>{Sb<sub>2</sub>Br<sub>9</sub>}<sub>2</sub>: atypical behavior in one-dimensional anionic systems.
Bykov, Andrei V.; Shestimerova, Tatiana A.; Bykov, Mikhail A.; Gontcharenko, Victoria E.; Lyssenko, Konstantin A.; Metlin, Mikhail T.; Taydakov, Ilya V.; Grigorieva, Anastasia V.; Shevelkov, Andrei V.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1541–1551; doi:10.1039/d4dt02751e

data_7717571
_publ_section_title
;
 Photoluminescent chain-of-dimer anion in a novel hybrid halometallate
 (C<sub>5</sub>H<sub>14</sub>N<sub>2</sub>)<sub>3</sub>{Sb<sub>2</sub>Br<sub>9</sub>}<sub>2</sub>:
 atypical behavior in one-dimensional anionic systems.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1541
_journal_page_last               1551
_journal_paper_doi               10.1039/d4dt02751e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Br18 Sb4, 3(C5 H14 N2)'
_chemical_formula_sum            'C15 H42 Br18 N6 Sb4'
_chemical_formula_weight         2231.92
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-05-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                95.8690(10)
_cell_angle_beta                 105.9410(10)
_cell_angle_gamma                113.3180(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4203(2)
_cell_length_b                   10.0299(3)
_cell_length_c                   15.1993(4)
_cell_measurement_reflns_used    8148
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      36.31
_cell_measurement_theta_min      2.53
_cell_volume                     1231.36(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III Detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13126
_diffrn_reflns_point_group_measured_fraction_full 0.807
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.277
_exptl_absorpt_coefficient_mu    16.794
_exptl_absorpt_correction_T_max  0.0801
_exptl_absorpt_correction_T_min  0.0259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1963 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.3233.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.010
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.780
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.298
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         11085
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0487
_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/[\s^2^(Fo^2^)+(0.0766P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.563
_reflns_Friedel_fraction_full    0.617
_reflns_Friedel_fraction_max     0.557
_reflns_number_gt                8865
_reflns_number_total             11085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02751e2.cif
_cod_data_source_block           qq
_cod_depositor_comments          'Adding full bibliography for 7717571.cif.'
_cod_database_code               7717571
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(3)
 0.46(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.004
Uanis(N2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(N5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C7) = Uanis(C10)
4.a Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N2(H2A,H2B), N5(H5A,H5B), N1(H1A,H1B), C12(H12A,H12B), C1(H1C,
 H1D), C11(H11A,H11B), C2(H2C,H2D), C10(H10A,H10B), C7(H7A,H7B), C14(H14A,H14B),
  C4(H4A,H4B), C3(H3A,H3B), C15(H15A,H15B), C5(H5C,H5D), C13(H13A,H13B), N4(H4C,
 H4D), C6(H6C,H6D), C9(H9A,H9B), C8(H8A,H8B), N3(H3C,H3D)
;
_shelx_res_checksum              73957
_shelx_hkl_checksum              69564
_olex2_submission_special_instructions 'No special instructions were received'