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_7248702
_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, I, 2(C18 H18 N2), 3[C3NOH7]'
_chemical_formula_sum            'C45 H57 Bi I7 N7 O3'
_chemical_formula_weight         1841.25
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-22 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.690(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3495(14)
_cell_length_b                   14.7084(12)
_cell_length_c                   13.8354(11)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.36
_cell_volume                     3004.2(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20006
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    6.571
_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    2.035
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+8.7703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3189
_reflns_number_total             3441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           shelx_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_database_code               7248702
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.506
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C13-C1 \\sim C12-C1
 with sigma of 0.02
 C8-C00A \\sim C7-C00A
 with sigma of 0.02
 C2A-C007 \\sim C4A-C007
 with sigma of 0.02
 C2-C0 \\sim C4-C0
 with sigma of 0.02
 C1-C007 \\sim C00A-C0
 with sigma of 0.02
 N0-C00A \\sim N1-C1
 with sigma of 0.02
 Bi01-I005 \\sim Bi01-I1
 with sigma of 0.02
 C4A-C2A_$1 \\sim C2A_$1-C007_$1 \\sim C4A_$1-C007_$1 \\sim C4A_$1-C2A
 with sigma of 0.02
 C2-C0 \\sim C4_$1-C2 \\sim C4-C0 \\sim C4-C2_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C0) = Uanis(C007)
Uanis(C4) = Uanis(C4A)
Uanis(C2A) = Uanis(C2)
Uanis(N0) = Uanis(N1)
Uanis(C8) = Uanis(C13)
Uanis(C3) = Uanis(C9)
Uanis(C5) = Uanis(C10)
Uanis(C11) = Uanis(C6)
Uanis(C7) = Uanis(C12)
Uanis(C4A) = Uanis(C4)
Uanis(C2) = Uanis(C2A)
Uanis(C1) = Uanis(C00A)
Uanis(C007) = Uanis(C0)
4. Others
 Sof(I0)=0.5*(1-FVAR(2))
 Sof(I004)=0.5*FVAR(2)
 Sof(I1)=0.5*(1-FVAR(3))
 Sof(I005)=0.5*FVAR(3)
 Fixed Sof: C007(0.5) C00A(0.5) H00A(0.5) H00B(0.5) C8(0.5) H8(0.5) C3(0.5)
 H3(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) N0(0.5) C2(0.5)
 H2(0.5) C4(0.5) H4(0.5) C2A(0.5) H2A(0.5) C4A(0.5) H4A(0.5) C0(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) C13(0.5) H13(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5)
 H11(0.5) C12(0.5) H12(0.5) N1(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C00A(H00A,H00B), C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C5(H5), C6(H6), C7(H7), C2(H2), C4(H4), C2A(H2A), C4A(H4A),
 C13(H13), C9(H9), C10(H10), C11(H11), C12(H12)
5.c Fitted hexagon refined as free rotating group:
 C8(C3,C5,C6,C7,N0), C13(C9,C10,C11,C12,N1)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 250 electrons were 
found in a volume of 882\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C3NOH7] per formula unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35345
_shelx_fab_checksum              83519
_olex2_submission_special_instructions 'No special instructions were received'