Reactions of A Lewis acidic methylene phosphonium cationic adduct with olefins
Miao, linkun; Yeganeh, Amir; Yeung, Jason; Stephan, Douglas W.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02855G

data_7711167
_publ_section_title
;
 Reactions of A Lewis acidic methylene phosphonium cationic adduct with
 olefins
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02855G
_journal_year                    2022
_chemical_formula_moiety         'C30 H32 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H32 F6 O6 P2 S2'
_chemical_formula_weight         752.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-07-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-31 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.509(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8075(11)
_cell_length_b                   19.1511(15)
_cell_length_c                   15.4157(10)
_cell_measurement_reflns_used    6816
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.30
_cell_volume                     3643.5(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1257
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54913
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.742
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1178 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.8899.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       shard
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.879
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+7.8922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4028
_reflns_number_total             6388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02855g2.cif
_cod_data_source_block           fin_a_CCDC2
_cod_original_cell_volume        3643.4(5)
_cod_database_code               7711167
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.982
_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:
 C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C29(H29), C2(H2), C26(H26), C8(H8), C28(H28), C27(H27), C12(H12),
 C3(H3), C6(H6), C4(H4), C11(H11), C10(H10), C24(H24), C9(H9), C5(H5), C23(H23),
  C20(H20), C22(H22), C21(H21)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'