Chemical Mustard Containment Using Simple Palladium Pincer Complexes: The Influence of Molecular Walls
Qi-Qiang Wang; Rowshan Ara Begum; Victor W. Day; Kristin Bowman-James; Journal of the American Chemical Society 135 (2013) 17193–17199; doi:10.1021/ja408770u

data_4121135
_publ_section_title
;
 Chemical Mustard Containment Using Simple Palladium Pincer Complexes: The
 Influence of Molecular Walls
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17193
_journal_page_last               17199
_journal_paper_doi               10.1021/ja408770u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C23 H20 N4 O4 Pd'
_chemical_formula_weight         522.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 130.9280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.9568(12)
_cell_length_b                   17.9591(10)
_cell_length_c                   14.4943(8)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.90
_cell_measurement_theta_min      3.72
_cell_volume                     4121.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optics'
_diffrn_radiation_source         'Bruker MicroStar microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16319
_diffrn_reflns_theta_full        66.00
_diffrn_reflns_theta_max         69.40
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    7.607
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       'Rectangular parallelepiped'
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00071(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         3728
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0400P)^2^+27.4270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3727
_reflns_number_total             3728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408770u_si_002_3.cif
_cod_data_source_block           q35c_Pd(Lc)(CH3CN)
_cod_database_code               4121135