Unusual Metal-Coordinated Zwitterionic P-C-N-C-N-C Phosphido Adducts
Allen T. Ekubo; Mark R. J. Elsegood; Andrew J. Lake; Martin B. Smith; Inorganic Chemistry 49 (2010) 3703–3705; doi:10.1021/ic1002308

data_4315339
_publ_section_title
;
 Unusual Metal-Coordinated Zwitterionic P-C-N-C-N-C Phosphido Adducts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3703
_journal_page_last               3705
_journal_paper_doi               10.1021/ic1002308
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C34 H40 Cl F3 N4 P Pd 1+, Cl 1-'
_chemical_formula_sum            'C34 H40 Cl2 F3 N4 P Pd'
_chemical_formula_weight         769.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.817(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3089(7)
_cell_length_b                   9.5474(4)
_cell_length_c                   23.2240(10)
_cell_measurement_reflns_used    6696
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.44
_cell_volume                     3495.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69430
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34142
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        3
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0406P)^2^+0.6658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                6710
_reflns_number_total             8666
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1002308_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4315339