Thermal decomposition of DMSO or DMF solvates: an advanced method for obtaining new hybrid bismuth(iii) halides
Dudko, Ekaterina M.; Buikin, Petr A.; Ilyukhin, Andey B.; Korlyukov, Alexander A.; Dorovatovskii, Pavel V.; Simonenko, Nikolai P.; Kotov, Vitalii Yu.; CrystEngComm 26 (2024) 3490–3500; doi:10.1039/D4CE00279B

data_7248700
_publ_section_title
;
 Thermal decomposition of DMSO or DMF solvates: an advanced method for
 obtaining new hybrid bismuth(iii) halides
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3490
_journal_page_last               3500
_journal_paper_doi               10.1039/D4CE00279B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'Bi Br4.083 Cl1.917, Bi0.5 Br2.207 Cl0.793, Bi0.5 Br2.199 Cl0.801, 6(C9 H9 N)'
_chemical_formula_sum            'C54 H54 Bi2 Br8.49 Cl3.51 N6'
_chemical_formula_weight         2007.85
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                67.593(5)
_cell_angle_beta                 73.276(5)
_cell_angle_gamma                80.529(7)
_cell_formula_units_Z            2
_cell_length_a                   12.790(3)
_cell_length_b                   14.769(4)
_cell_length_c                   19.156(5)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    140
_cell_measurement_theta_max      24.349
_cell_measurement_theta_min      2.166
_cell_volume                     3197.6(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      140
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40876
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.186
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.987
_exptl_absorpt_correction_T_max  0.4926
_exptl_absorpt_correction_T_min  0.2652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1477 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.1532.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1886
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.971
_refine_diff_density_min         -2.588
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         12597
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+35.3205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9665
_reflns_number_total             12597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           pyxk_bibr_4_1_dmso
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_original_cell_volume        3197.5(13)
_cod_database_code               7248700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.290
_olex2_refinement_description
;
1. Restrained distances
 Cl4B-Bi1
 2.7 with sigma of 0.02
 Cl5A-Bi1
 2.7 with sigma of 0.02
 Cl6B-Bi1
 2.7 with sigma of 0.02
2. Restrained planarity
 Cl1A, Cl3A, Cl4B, Cl6B, Bi1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2A) = Uanis(Br2B)
Uanis(Br5) = Uanis(Cl5A)
Uanis(Cl7A) = Uanis(Br7B)
Uanis(Cl) = Uanis(Br)
Uanis(Cl1) = Uanis(Br10)
Uanis(Cl6B) = Uanis(Br6A)
Uanis(Cl9B) = Uanis(Br9A)
Uanis(Br8B) = Uanis(Cl8A)
Uanis(Br2) = Uanis(Cl2)
Uanis(Br3B) = Uanis(Cl3A)
Uanis(Cl4B) = Uanis(Br4A)
Uanis(Br1B) = Uanis(Cl1A)
4. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
 Sof(Cl5A)=1-FVAR(2)
 Sof(Br5)=FVAR(2)
 Sof(Br7B)=1-FVAR(3)
 Sof(Cl7A)=FVAR(3)
 Sof(Br)=1-FVAR(4)
 Sof(Cl)=FVAR(4)
 Sof(Cl1)=1-FVAR(5)
 Sof(Br10)=FVAR(5)
 Sof(Cl6B)=1-FVAR(6)
 Sof(Br6A)=FVAR(6)
 Sof(Br8B)=1-FVAR(7)
 Sof(Cl8A)=FVAR(7)
 Sof(Cl9B)=1-FVAR(8)
 Sof(Br9A)=FVAR(8)
 Sof(Br2)=1-FVAR(9)
 Sof(Cl2)=FVAR(9)
 Sof(Br3B)=1-FVAR(10)
 Sof(Cl3A)=FVAR(10)
 Sof(Cl4B)=1-FVAR(11)
 Sof(Br4A)=FVAR(11)
 Sof(Br1B)=1-FVAR(12)
 Sof(Cl1A)=FVAR(12)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C15(H15A,H15B), C22(H22A,H22B), C33(H33A,H33B), C42(H42A,H42B),
 C49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54)
;
_shelx_res_checksum              8569
_olex2_submission_special_instructions 'No special instructions were received'