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_4121137
_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            'C31 H26 Cl N3 O2 Pd S'
_chemical_formula_weight         646.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5864(4)
_cell_length_b                   16.0764(4)
_cell_length_c                   12.5172(4)
_cell_measurement_reflns_used    6926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.77
_cell_measurement_theta_min      4.26
_cell_volume                     2734.01(14)
_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 0.997
_diffrn_measured_fraction_theta_max 0.981
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17591
_diffrn_reflns_theta_full        66.00
_diffrn_reflns_theta_max         69.48
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    7.365
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4517
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.001
_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^+9.4026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                3837
_reflns_number_total             4517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408770u_si_002_5.cif
_cod_data_source_block           q28c_Pd(Le)(CEES)
_cod_database_code               4121137