Unexpectedly High Barriers to M‒P Rotation in Tertiary Phobane Complexes: PhobPR Behavior That Is Commensurate withtBu2PR
Lister, Julia M.; Carreira, Monica; Haddow, Mairi F.; Hamilton, Alex; McMullin, Claire L.; Orpen, A. Guy; Pringle, Paul G.; Stennett, Tom E.; Organometallics 33 (2014) 702–; doi:10.1021/om400980e

data_4082498
_publ_section_title
;
 Unexpectedly High Barriers to M--P Rotation in Tertiary Phobane
 Complexes: PhobPR Behavior That Is Commensurate withtBu2PR
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              702
_journal_paper_doi               10.1021/om400980e
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H46 Cl2 P2 Pd'
_chemical_formula_sum            'C24 H46 Cl2 P2 Pd'
_chemical_formula_weight         573.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.289(3)
_cell_angle_beta                 103.064(3)
_cell_angle_gamma                96.625(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7650(3)
_cell_length_b                   7.8175(4)
_cell_length_c                   11.0564(5)
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.91
_cell_volume                     641.25(5)
_computing_cell_refinement       'Apex II (Bruker, 2008)'
_computing_data_collection       'Apex II (Bruker, 2008)'
_computing_data_reduction        'SAINT V7.68A (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6756
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.501
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+6.9991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                2689
_reflns_number_total             2914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400980e_si_002.cif
_cod_data_source_block           4a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082498