Straightforward Synthesis of Bench-Stable Heteroatom-Centered Difluoromethylated Entities via the Controlled Nucleophilic Transfer from Activated TMSCHF2
Miele, Margherita; Castoldi, Laura; Simeone, Xenia; Holzer, Wolfgang; Pace, Vittorio; Chemical Communications  (2022) –; doi:10.1039/D2CC00886F

data_7129928
_publ_section_title
;
 Straightforward Synthesis of Bench-Stable Heteroatom-Centered
 Difluoromethylated Entities via the Controlled Nucleophilic Transfer from
 Activated TMSCHF2
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00886F
_journal_year                    2022
_chemical_formula_moiety         'C19 H16 F2 Sn'
_chemical_formula_sum            'C19 H16 F2 Sn'
_chemical_formula_weight         401.01
_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     direct
_audit_creation_date             2022-01-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-06 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                78.2253(17)
_cell_angle_beta                 84.6029(10)
_cell_angle_gamma                79.0665(9)
_cell_formula_units_Z            4
_cell_length_a                   9.4404(2)
_cell_length_b                   9.7492(2)
_cell_length_c                   18.7631(4)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      30.047
_cell_measurement_theta_min      2.167
_cell_volume                     1657.11(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 (Bruker, 2021)'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62306
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.130
_diffrn_reflns_theta_min         2.167
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.555
_exptl_absorpt_correction_T_max  0.6042
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0612 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.9457.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.380
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.1494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7641
_reflns_number_total             9756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00886f2.cif
_cod_data_source_block           mami803_p-1
_cod_database_code               7129928
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.800
_shelx_res_checksum              86334