CF3-substituted sulfonium cations as efficient chalcogen bond donors towards cyanometalates
Streit, Tim-Niclas; Gomila, Rosa M.; Sievers, Robin; Frontera, Antonio; Malischewski, Moritz; CrystEngComm 26 (2024) 594–598; doi:10.1039/D3CE01155K

data_7248003
_publ_section_title
;
 CF3-substituted sulfonium cations as efficient chalcogen bond donors
 towards cyanometalates
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              594
_journal_page_last               598
_journal_paper_doi               10.1039/D3CE01155K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C6 Mo0.822 N O5 W0.178, C13 H7 F3 N O2 S, C H2 Cl2'
_chemical_formula_sum            'C20 H9 Cl2 F3 Mo0.822 N2 O7 S W0.178'
_chemical_formula_weight         660.865
_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
_audit_creation_date             2024-01-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                73.180(1)
_cell_angle_beta                 85.274(2)
_cell_angle_gamma                62.991(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1988(4)
_cell_length_b                   10.2849(4)
_cell_length_c                   13.3894(5)
_cell_measurement_reflns_used    9635
_cell_measurement_temperature    105
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.32
_cell_volume                     1195.77(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      105
_diffrn_measured_fraction_theta_full 0.9914
_diffrn_measured_fraction_theta_max 0.9909
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.9914
_diffrn_reflns_Laue_measured_fraction_max 0.9909
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17918
_diffrn_reflns_point_group_measured_fraction_full 0.9914
_diffrn_reflns_point_group_measured_fraction_max 0.9909
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6361
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1073 before and 0.0394 after correction.
The Ratio of minimum to maximum transmission is 0.8536.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear blackish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             645.488
_exptl_crystal_recrystallization_method DCM/Pentane
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.9038
_refine_diff_density_min         -0.6738
_refine_diff_density_rms         0.1257
_refine_ls_d_res_high            0.8298
_refine_ls_d_res_low             9.0714
_refine_ls_goodness_of_fit_ref   1.1098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1098
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+2.8530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -11
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3876
_reflns_number_total             4343
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ce01155k2.cif
_cod_data_source_block           p-1_cellnow
_cod_depositor_comments
'Adding full bibliography for 7248001--7248003.cif.'
_cod_database_code               7248003
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Mo01(0.82222) W1(0.17778)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C1(H1), C12(H12), C11(H11), C5(H5), C3(H3), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'