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_7248698
_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
'Bi0.5 Br2.14 Cl0.86, Bi0.5 Br1.97 Cl1.03, 2(C9 H9 N), C9 H10 N'
_chemical_formula_sum            'C27 H28 Bi Br4.11 Cl1.89 N3'
_chemical_formula_weight         998.93
_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             2024-03-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                81.087(3)
_cell_angle_beta                 76.125(4)
_cell_angle_gamma                69.233(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4546(10)
_cell_length_b                   13.2860(12)
_cell_length_c                   13.9063(11)
_cell_measurement_reflns_used    1780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.681
_cell_measurement_theta_min      2.321
_cell_volume                     1581.0(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.597
_diffrn_reflns_theta_min         1.644
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.951
_exptl_absorpt_correction_T_max  0.2657
_exptl_absorpt_correction_T_min  0.1630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0906 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.6461. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.559
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         9451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0076P)^2^+3.8193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7008
_reflns_number_total             9451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           pyxk_bibr_4_1_dmso_0m
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_database_code               7248698
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.290
_shelx_estimated_absorpt_t_min   0.218
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Cl0A) = Uanis(Br07)
Uanis(Br08) = Uanis(Cl1A)
Uanis(Cl2A) = Uanis(Br06)
Uanis(Cl3A) = Uanis(Br03)
Uanis(Cl4A) = Uanis(Br04)
Uanis(Cl) = Uanis(Br05)
2. Others
 Sof(Cl0A)=1-FVAR(1)
 Sof(Br07)=FVAR(1)
 Sof(Cl1A)=1-FVAR(2)
 Sof(Br08)=FVAR(2)
 Sof(Cl2A)=1-FVAR(3)
 Sof(Br06)=FVAR(3)
 Sof(Cl3A)=1-FVAR(4)
 Sof(Br03)=FVAR(4)
 Sof(Cl4A)=1-FVAR(5)
 Sof(Br04)=FVAR(5)
 Sof(Cl)=1-FVAR(6)
 Sof(Br05)=FVAR(6)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C1BA(H1BA,H1BB), C9AA(H9AA,H9AB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C18(H18), C3AA(H3AA), C8AA(H8AA), C4(H4), C2AA(H2AA), C4AA(H4AA), C0BA(H0BA),
 C7AA(H7AA), C6AA(H6AA), C1AA(H1AA), C5AA(H5AA), C0AA(H0AA)
;
_shelx_res_checksum              74680
_olex2_submission_special_instructions 'No special instructions were received'