Lewis Acid Base Chemistry of Bestmann’s Ylide, Ph3PCCO, and its Bulkier Analogue, (Cyclohexyl)3PCCO
Krempner, Clemens; Brar, Amandeep; Unruh, Daniel K.; Aquino, Adelia; Chemical Communications  (2019) –; doi:10.1039/C9CC01239G

data_7123076
_publ_section_title
;
 Lewis Acid Base Chemistry of Bestmann&#x2019;s Ylide, Ph3PCCO, and its
 Bulkier Analogue, (Cyclohexyl)3PCCO
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01239G
_journal_year                    2019
_chemical_formula_sum            'C43 H36 Br N2 O P'
_chemical_formula_weight         707.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-16T16:10:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-11-28 deposited with the CCDC.    2019-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                113.8390(10)
_cell_angle_beta                 90.9690(10)
_cell_angle_gamma                102.4640(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3865(8)
_cell_length_b                   13.6653(10)
_cell_length_c                   14.2202(11)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.41
_cell_volume                     1790.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_unetI/netI     0.032
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31758
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.128
_diffrn_reflns_theta_min         1.576
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.33
_refine_diff_density_rms         0.058
_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     438
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.7488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0
_reflns_number_gt                6810
_reflns_number_total             7925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01239g2.cif
_cod_data_source_block           8
_cod_database_code               7123076
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.852
_shelx_res_checksum              3984
_shelx_hkl_checksum              47534