A five coordinate PdII complex stable in solution and in the solid state
Martin Broring; Carsten D. Brandt; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b305547g

data_7103873
_publ_section_title
;
A five coordinate PdII complex stable in solution and in the solid state
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b305547g
_journal_year                    2003
_chemical_formula_sum            'C63 H59 B F24 N3 P Pd'
_chemical_formula_weight         1462.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 104.331(1)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   12.9944(11)
_cell_length_b                   20.5527(17)
_cell_length_c                   25.0962(21)
_cell_measurement_reflns_used    5435
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      56.667
_cell_measurement_theta_min      4.459
_cell_volume                     6493.9(9)
_computing_cell_refinement       'SMART-NT V5.6'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SMART-NT V5.6'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex with D8-Goniometer'
_diffrn_measurement_method       '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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66958
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS2.0 (Sheldrick 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         13271
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+2.4109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                10167
_reflns_number_total             13271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305547g.txt
_cod_data_source_block           cb21cb
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7103873