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_7248694
_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         '2(C18 H18 N2), Bi Br6, 3(C2 H6 O S), Br'
_chemical_formula_sum            'C42 H54 Bi Br7 N4 O3 S3'
_chemical_formula_weight         1527.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_Int_Tables_number      12
_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                90
_cell_angle_beta                 125.2900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.5194(9)
_cell_length_b                   14.5925(9)
_cell_length_c                   13.2748(7)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.36
_cell_volume                     2612.0(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22807
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.543
_diffrn_reflns_theta_min         2.056
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.889
_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    1.942
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.65
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0
_reflns_number_gt                4043
_reflns_number_total             4494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_database_code               7248694
_shelx_estimated_absorpt_t_max   0.224
_shelx_estimated_absorpt_t_min   0.176
_olex2_refinement_description
;
1. Restrained distances
 S101-O101
 1.54 with sigma of 0.01
 S101-C101 = S101-C102
 1.78 with sigma of 0.01
 O101-C101 = O101-C102
 2.6 with sigma of 0.02
 C101-C102
 2.8 with sigma of 0.02
 S201-O201
 1.54 with sigma of 0.01
 S201-C201 = S201-C202
 1.78 with sigma of 0.01
 O201-C201 = O201-C202
 2.6 with sigma of 0.02
 C201-C202
 2.8 with sigma of 0.02
 S211-O211
 1.54 with sigma of 0.01
 S211-C211 = S211-C212
 1.78 with sigma of 0.01
 O211-C211 = O211-C212
 2.6 with sigma of 0.02
 C211-C212
 2.8 with sigma of 0.02
2. Others
 Uiso(S201)=Uiso(O201)=Uiso(C201)=Uiso(C202)=Uiso(S211)=Uiso(O211)=Uiso(C211)=
 Uiso(C212)=FVAR(1)
 Fixed Sof: S101(0.5) O101(0.5) C101(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C102(0.5) H10D(0.5) H10E(0.5) H10F(0.5) S201(0.2) O201(0.2) C201(0.2)
 H20A(0.2) H20B(0.2) H20C(0.2) C202(0.2) H20D(0.2) H20E(0.2) H20F(0.2)
 S211(0.05) O211(0.05) C211(0.05) H21A(0.05) H21B(0.05) H21C(0.05) C212(0.05)
 H21D(0.05) H21E(0.05) H21F(0.05)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.b Me refined with riding coordinates:
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C201(H20A,H20B,H20C), C202(H20D,
 H20E,H20F), C211(H21A,H21B,H21C), C212(H21D,H21E,H21F)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C5(H5A), C8(H8A), C9(H9A)
;
_shelx_res_checksum              95776
_olex2_submission_special_instructions 'No special instructions were received'