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_7248699
_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 I6, 1.5(C18 H18 N2), C3 H7 N O'
_chemical_formula_sum            'C30 H34 Bi I6 N4 O'
_chemical_formula_weight         1436.99
_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             2024-05-13
_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                74.6500(10)
_cell_angle_beta                 87.7940(10)
_cell_angle_gamma                72.9350(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0547(5)
_cell_length_b                   13.7612(6)
_cell_length_c                   13.8907(6)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.36
_cell_volume                     1946.28(15)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker AXS D8 VENTURE PHOTON III C14 IuS 3.0'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46406
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.556
_diffrn_reflns_theta_min         2.116
_exptl_absorpt_coefficient_mu    9.316
_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    2.452
_exptl_crystal_description       block
_exptl_crystal_F_000             1302
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00048(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         12915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0203
_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^)+(0.0022P)^2^+2.1242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12041
_reflns_number_total             12915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           shelx_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_database_code               7248699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.523
_shelx_estimated_absorpt_t_min   0.234
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N101) = Uanis(N111)
Uanis(C113) = Uanis(C101)
Uanis(O101) = Uanis(O111)
Uanis(C111) = Uanis(C103)
Uanis(C102) = Uanis(C112)
3. Others
 Sof(O111)=Sof(N111)=Sof(C111)=Sof(H111)=Sof(C112)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C113)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(O101)=Sof(N101)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C103)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C24(H24A,H24B)
4.b Me refined with riding coordinates:
 C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C112(H11A,H11B,H11C), C113(H11D,
 H11E,H11F)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C26(H26), C27(H27), C101(H101), C111(H111)
;
_shelx_res_checksum              30074
_olex2_submission_special_instructions 'No special instructions were received'