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_7125297
_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         'C54 H44 Br F2 P3 Pd, 1.5(C6 H6)'
_chemical_formula_sum            'C63 H53 Br F2 P3 Pd'
_chemical_formula_weight         1127.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2016-08-07
_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                98.543(2)
_cell_angle_beta                 90.489(2)
_cell_angle_gamma                118.142(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2250(5)
_cell_length_b                   12.6710(5)
_cell_length_c                   19.4112(8)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.57
_cell_volume                     2611.30(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38726
_diffrn_reflns_theta_full        27.5806
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0345 after correction.
The Ratio of minimum to maximum transmission is 0.9438.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4337
_exptl_crystal_description       block
_exptl_crystal_F_000             1148.4935
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.4758
_refine_diff_density_min         -1.1381
_refine_diff_density_rms         0.0952
_refine_ls_d_res_high            0.7675
_refine_ls_d_res_low             11.0045
_refine_ls_goodness_of_fit_ref   1.0313
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    106
_refine_ls_number_parameters     630
_refine_ls_number_reflns         12045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0313
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+1.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10300
_reflns_number_total             12045
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc08561j2.cif
_cod_data_source_block           KF002_0m
_cod_database_code               7125297
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
;
_olex2_submission_special_instructions 'No special instructions were received'