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_7248695
_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         '1.5(C18 H18 N2), Bi2 I9, C3 H7 N O'
_chemical_formula_sum            'C30 H34 Bi2 I9 N4 O'
_chemical_formula_weight         2026.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2024-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-20 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.466(2)
_cell_angle_beta                 103.2530(10)
_cell_angle_gamma                112.5700(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4022(5)
_cell_length_b                   12.5641(7)
_cell_length_c                   19.9063(10)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.36
_cell_volume                     2298.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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, 2018)'
_computing_structure_solution    'SHELXS-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker AXS D8 VENTURE PHOTON III C14 IuS 3.0'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53186
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.595
_diffrn_reflns_theta_min         2.192
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.719
_exptl_absorpt_correction_T_max  0.182
_exptl_absorpt_correction_T_min  0.032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1786
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.22
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         15231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0
_reflns_number_gt                14053
_reflns_number_total             15231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           shelx_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_database_code               7248695
_shelx_estimated_absorpt_t_max   0.29
_shelx_estimated_absorpt_t_min   0.17
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C24(H24A,H24B)
1.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C5(H5A), C8(H8A), C9(H9A), C11(H11A),
 C12(H12A), C14(H14A), C15(H15A), C16(H16A), C17(H17A), C18(H18A), C19(H19A),
 C20(H20A), C21(H21A), C22(H22A), C23(H23A), C26(H26A), C27(H27A), C101(H10G)
1.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C103(H10D,H10E,H10F)
;
_shelx_res_checksum              55990
_olex2_submission_special_instructions 'No special instructions were received'