Using frustrated Lewis pairs to explore C-F bond activation.
Briceno-Strocchia, Alvaro I; Johnstone, Timothy C.; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1319–1324; doi:10.1039/c9dt04588k

data_7703039
_publ_section_title
;
 Using frustrated Lewis pairs to explore C-F bond activation.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1319
_journal_page_last               1324
_journal_paper_doi               10.1039/c9dt04588k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C F3 O3 S, C17 H28 N4 O P'
_chemical_formula_sum            'C18 H28 F3 N4 O4 P S'
_chemical_formula_weight         484.48
_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             2019-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-29 deposited with the CCDC.	2019-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                71.896(5)
_cell_angle_beta                 89.899(5)
_cell_angle_gamma                89.942(6)
_cell_formula_units_Z            4
_cell_length_a                   9.0748(8)
_cell_length_b                   14.7556(14)
_cell_length_c                   17.4680(17)
_cell_measurement_reflns_used    3572
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.45
_cell_volume                     2223.2(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.9914
_diffrn_measured_fraction_theta_max 0.9899
_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  0.1461
_diffrn_reflns_av_unetI/netI     0.2098
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34926
_diffrn_reflns_theta_full        27.5374
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.9266.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4473
_exptl_crystal_description       Shard
_exptl_crystal_F_000             1017.4989
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.7786
_refine_diff_density_min         -0.8350
_refine_diff_density_rms         0.2002
_refine_ls_d_res_high            0.7686
_refine_ls_d_res_low             14.0251
_refine_ls_goodness_of_fit_ref   0.7597
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    80
_refine_ls_number_parameters     581
_refine_ls_number_reflns         10143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.7597
_refine_ls_R_factor_all          0.1458
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0217P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4332
_reflns_number_total             10143
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt04588k2.cif
_cod_data_source_block           ABS012_01m_a
_cod_depositor_comments
'Adding full bibliography for 7703037--7703039.cif.'
_cod_database_code               7703039
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C23(H23a,H23b), C22(H22a,H22b), C2(H2a,H2b), C4(H4a,H4b), C3(H3a,
 H3b), C6(H6a,H6b), C20(H20a,H20b), C21(H21a,H21b), C18(H18a,H18b), C5(H5a,H5b),
  C19(H19a,H19b)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C30(H30), C17(H17), C31(H31), C14(H14), C34(H34), C15(H15),
 C32(H32), C16(H16), C33(H33)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C26(H26a,H26b,H26c),
 C24(H24a,H24b,H24c), C9(H9a,H9b,H9c)
;
_olex2_submission_special_instructions 'No special instructions were received'