A pendant phosphorus Lewis acid: route to a palladium-benzoyl derived phosphorane.
Firth, Kelly F.; Möbus, Juri; Stephan, Douglas W.; Chemical communications (Cambridge, England) 52 (2016) 13967–13970; doi:10.1039/c6cc08561j

data_7125298
_publ_section_title
;
 A pendant phosphorus Lewis acid: route to a palladium-benzoyl derived
 phosphorane.
;
_journal_issue                   97
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13967
_journal_page_last               13970
_journal_paper_doi               10.1039/c6cc08561j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C55 H44 Br F O P3 Pd, 1.5(C H2 Cl2), C F3 O3 S'
_chemical_formula_sum            'C57.5 H47 Br Cl3 F4 O4 P3 Pd S'
_chemical_formula_weight         1295.58
_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   geom
_audit_creation_date             2016-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-17 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.688(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2329(9)
_cell_length_b                   20.4798(13)
_cell_length_c                   19.1729(11)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.26
_cell_volume                     5550.6(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.999
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50319
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         2.137
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0624 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.9177.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12780
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0367P)^2^+3.7844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9642
_reflns_number_total             12780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08561j2.cif
_cod_data_source_block           pre
_cod_original_formula_sum        'C57.50 H47 Br Cl3 F4 O4 P3 Pd S'
_cod_database_code               7125298
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C1B, S1B, F1B, F2B, F3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(S1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(C1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=1-
 FVAR(1)
 Sof(S1C)=Sof(O1C)=Sof(O2C)=Sof(O3C)=Sof(C1C)=Sof(F2C)=Sof(F1C)=Sof(F3C)=FVAR(1)
 Fixed Sof: Cl22(0.5) C51(0.5) H51A(0.5) H51B(0.5) Cl21(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B)
4.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C48(H48), C47(H47),
 C46(H46), C45(H45), C44(H44), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C24(H24), C23(H23),
  C22(H22), C21(H21), C30(H30), C29(H29), C28(H28), C27(H27), C26(H26),
 C902(H902), C903(H903), C904(H904), C905(H905), C906(H906)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'