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_7711166
_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         'C40 H36 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C42 H36 F6 O6 P2 S2'
_chemical_formula_weight         876.77
_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
_audit_creation_date             2022-06-16
_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                86.981(7)
_cell_angle_beta                 82.275(5)
_cell_angle_gamma                83.804(5)
_cell_formula_units_Z            2
_cell_length_a                   9.1211(19)
_cell_length_b                   12.648(5)
_cell_length_c                   17.550(7)
_cell_measurement_reflns_used    4117
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      22.85
_cell_measurement_theta_min      3.46
_cell_volume                     1993.0(12)
_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      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1444
_diffrn_reflns_av_unetI/netI     0.1314
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32776
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.621
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.7199
_exptl_absorpt_correction_T_min  0.5973
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1275 before and 0.1078 after correction.
The Ratio of minimum to maximum transmission is 0.8297.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4338
_reflns_number_total             6982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02855g2.cif
_cod_data_source_block           fin_a_CCDC1
_cod_original_cell_volume        1993.1(11)
_cod_database_code               7711166
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.991
_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:
 C00W(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00X(H00X), C010(H010),
 C011(H011), C013(H013), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D),
 C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K)
2.c Idealised Me refined as rotating group:
 C00Y(H00C,H00D,H00E)
;
_olex2_submission_special_instructions 'No special instructions were received'