Tuning of Metal Complex Electronics and Reactivity by Remote Lewis Acid Binding to π-Coordinated Pyridine Diphosphine Ligands
Horak, Kyle T.; VanderVelde, David G.; Agapie, Theodor; Organometallics 34 (2015) 4753–; doi:10.1021/acs.organomet.5b00562

data_4087747
_publ_section_title
;
 Tuning of Metal Complex Electronics and Reactivity by Remote Lewis Acid
 Binding to \p-Coordinated Pyridine Diphosphine Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4753
_journal_paper_doi               10.1021/acs.organomet.5b00562
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C29 H39 N P2 Pd'
_chemical_formula_weight         569.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.464(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6112(7)
_cell_length_b                   17.8635(16)
_cell_length_c                   8.8154(11)
_cell_measurement_temperature    100(2)
_cell_volume                     1337.6(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.1660
_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       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57288
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.810
_diffrn_reflns_theta_min         2.342
_exptl_absorpt_coefficient_mu    0.831
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_refine_diff_density_max         1.534
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details
;
 Flack x determined using 5305 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         22507
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0723P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                14550
_reflns_number_total             22507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00562_si_005.cif
_cod_data_source_block           p14013
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4087747
_shelx_estimated_absorpt_t_min   0.743
_shelx_estimated_absorpt_t_max   0.832
_shelxl_version_number           2013-3
_shelx_res_checksum              87564
_shelx_hkl_checksum              88951