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_7718848
_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         'C40 H43 N3 O P2 Re, F6 P'
_chemical_formula_sum            'C40 H43 F6 N3 O P3 Re'
_chemical_formula_weight         974.88
_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
_atom_sites_solution_primary     direct
_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                 91.0330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.84610(10)
_cell_length_b                   16.04480(10)
_cell_length_c                   21.0727(2)
_cell_measurement_reflns_used    9467
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     4004.60(6)
_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  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17865
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         2.137
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  0.6439
_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+1.8277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7965
_reflns_number_total             9169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01102g2.cif
_cod_data_source_block           fls01
_cod_depositor_comments
'Adding full bibliography for 7718847--7718848.cif.'
_cod_database_code               7718848
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.565
_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 Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Me refined with riding coordinates:
 C54B(H54A,H54B,H54C), C54A(H54D,H54E,H54F), C64B(H64A,H64B,H64C), C64A(H64D,
 H64E,H64F)
2.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C52(H52), C53(H53), C55(H55), C56(H56), C62(H62), C63(H63), C65(H65), C66(H66)
;
_shelx_res_checksum              79982
_shelx_hkl_checksum              11305
_olex2_submission_special_instructions 'No special instructions were received'