Air-Stable Pd(R-allyl)LCl (L= Q-Phos, P(t-Bu)3, etc.) Systems for C-C/N Couplings: Insight into the Structure-Activity Relationship and Catalyst Activation Pathway
Carin C. C. Johansson Seechurn; Sébastien L. Parisel; Thomas J. Colacot; Journal of Organic Chemistry 76 (2011) 7918–7932; doi:10.1021/jo2013324

data_4026618
_publ_section_title
;
 Air-Stable Pd(R-allyl)LCl (L= Q-Phos, P(t-Bu)3, etc.) Systems for C-C/N
 Couplings: Insight into the Structure-Activity Relationship and Catalyst
 Activation Pathway
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7918
_journal_page_last               7932
_journal_paper_doi               10.1021/jo2013324
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C51 H52 Cl Fe P Pd, 0.125(C4 H10 O)'
_chemical_formula_sum            'C51.5 H53.25 Cl Fe O0.125 P Pd'
_chemical_formula_weight         902.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.514(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.0455(6)
_cell_length_b                   12.5496(2)
_cell_length_c                   19.7679(3)
_cell_measurement_reflns_used    86132
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.00
_cell_volume                     8548.1(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_sigmaI/netI    0.1147
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41654
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             3738
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         11069
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.109
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+25.2954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                6887
_reflns_number_total             11069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2013324_si_002.cif
_cod_data_source_block           jm0802
_cod_depositor_comments
;

2025-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1805.72
_cod_original_formula_moiety         'C103 H106.50 Cl2 Fe2 O0.25 P2 Pd2'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C103 H106.50 Cl2 Fe2 O0.25 P2 Pd2'
_cod_database_code               4026618