P(v) dications: carbon-based Lewis acid initiators for hydrodefluorination.
Waked, Alexander E.; Chitnis, Saurabh S.; Stephan, Douglas W.; Chemical communications (Cambridge, England) 55 (2019) 8971–8974; doi:10.1039/c9cc04010b

data_7125379
_publ_section_title
;
 P(v) dications: carbon-based Lewis acid initiators for
 hydrodefluorination.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8971
_journal_page_last               8974
_journal_paper_doi               10.1039/c9cc04010b
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C27 H16 Cl4 N3 O2 P, 2(C F3 O3 S)'
_chemical_formula_sum            'C29 H16 Cl4 F6 N3 O8 P S2'
_chemical_formula_weight         885.37
_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             2019-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-24 deposited with the CCDC.	2019-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                95.710(8)
_cell_angle_beta                 99.202(8)
_cell_angle_gamma                112.242(8)
_cell_formula_units_Z            2
_cell_length_a                   8.7656(13)
_cell_length_b                   10.8058(15)
_cell_length_c                   19.768(3)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.57
_cell_volume                     1684.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      150.15
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9955
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22897
_diffrn_reflns_theta_full        25.0276
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0523 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.9591.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7455
_exptl_crystal_description       shard
_exptl_crystal_F_000             890.4428
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.4513
_refine_diff_density_min         -0.4037
_refine_diff_density_rms         0.0907
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             7.9517
_refine_ls_goodness_of_fit_ref   1.0498
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0498
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.1587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                4826
_reflns_number_total             5919
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc04010b2.cif
_cod_data_source_block           tri_a
_cod_original_cell_volume        1684.4(4)
_cod_database_code               7125379
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
;
_olex2_submission_special_instructions 'No special instructions were received'