Synthesis and reactivity of donor stabilized thionylium (SO2+) dications
Andrews, Ryan; De Backere, John; Stephan, Douglas W.; Chemical Communications  (2022) –; doi:10.1039/D2CC04129D

data_7130587
_publ_section_title
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 Synthesis and reactivity of donor stabilized thionylium (SO2+) dications
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04129D
_journal_year                    2022
_chemical_formula_moiety         '2(C F3 O3 S), C15 H11 N3 O S'
_chemical_formula_sum            'C17 H11 F6 N3 O7 S3'
_chemical_formula_weight         579.481
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2022-07-14
_audit_creation_method
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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2022-07-14 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 128.183(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7305(11)
_cell_length_b                   8.0563(3)
_cell_length_c                   22.7955(9)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      38.58
_cell_measurement_theta_min      2.67
_cell_volume                     4291.7(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9979
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            89990
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9979
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         41.40
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.7046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0446 before and 0.0419 after correction.
The Ratio of minimum to maximum transmission is 0.9419.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       SHARD
_exptl_crystal_F_000             2341.129
_refine_diff_density_max         0.8848
_refine_diff_density_min         -0.8190
_refine_diff_density_rms         0.1021
_refine_ls_d_res_high            0.5374
_refine_ls_d_res_low             6.5504
_refine_ls_goodness_of_fit_ref   1.0089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     428
_refine_ls_number_reflns         14445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0089
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+2.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              43
_reflns_limit_h_min              -55
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              0
_reflns_number_gt                11023
_reflns_number_total             14445
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cc04129d2.cif
_cod_data_source_block           JRD016_0m_a
_cod_database_code               7130587
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: F009(0.75) O00D(0.5) F00I(0.75) C010(0.75) F0AA(0.75) O1(0.5)
 F1(0.25) F2(0.25) C3(0.25) O5(0.5) O7(0.5) F10(0.25) O2(0.5) O3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C00S(H00S)
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_olex2_submission_special_instructions 'No special instructions were received'