Syntheses and structures of chiral rhenium-containing phosphonium salts and phosphines with ReCH<sub>2</sub>P̈Ar<sub>2</sub> or ReCH(R)P̈Ar<sub>2</sub> linkages; enantioselective catalysis of intramolecular Morita-Baylis-Hillman and Rauhut-Currier reactions.
Seidel, Florian O.; O'Brien, Michael J; Hampel, Frank; Gladysz, John A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10071–10084; doi:10.1039/d5dt01102g

data_7718847
_publ_section_title
;
 Syntheses and structures of chiral rhenium-containing phosphonium salts
 and phosphines with ReCH<sub>2</sub>P&#x308;Ar<sub>2</sub> or
 ReCH(R)P&#x308;Ar<sub>2</sub> linkages; enantioselective catalysis of
 intramolecular Morita-Baylis-Hillman and Rauhut-Currier reactions.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10071
_journal_page_last               10084
_journal_paper_doi               10.1039/d5dt01102g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C38 H37 N O3 P2 Re, F6 P'
_chemical_formula_sum            'C38 H37 F6 N O3 P3 Re'
_chemical_formula_weight         948.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-02-11
_audit_creation_method
;
Olex2 1.5-ac7-013
(compiled 2025.01.02 svn.rf662f148 for Rigaku Oxford Diffraction, GUI svn.r7109)
;
_audit_update_record
;
2025-02-11 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.260(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7618(3)
_cell_length_b                   15.3419(5)
_cell_length_c                   19.2417(5)
_cell_measurement_reflns_used    8286
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     3737.13(18)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Olex2 1.5-ac7-013 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-013 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15168
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         2.434
_exptl_absorpt_coefficient_mu    3.448
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_correction_T_min  0.5455
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.221
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00073(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5972
_reflns_number_total             8537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01102g2.cif
_cod_data_source_block           fls02
_cod_depositor_comments
'Adding full bibliography for 7718847--7718848.cif.'
_cod_database_code               7718847
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.545
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 P1(H1)
2.b Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.d Me refined with riding coordinates:
 C24A(H24A,H24B,H24C), C34A(H34A,H34B,H34C)
2.e Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C35(H35),
 C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
;
_shelx_res_checksum              55011
_shelx_hkl_checksum              26073
_olex2_submission_special_instructions 'No special instructions were received'