Monomers and Polymers of Tripalladium(0) Ditropylium Halides
Frank L. Mulligan; Dominic C. Babbini; Isaac R. Davis; Stephanie K. Hurst; Gary S. Nichol; Inorganic Chemistry 48 (2009) 2708–2710; doi:10.1021/ic8014578

data_4301759
_publ_contact_author             'Dr Stephanie K. Hurst'
_publ_contact_author_email       stephanie.hurst@nau.edu
_publ_contact_author_fax         '+1 928.523.8111'
_publ_contact_author_phone       '+1 (928) 523-6204'
_publ_section_title
;
Monomers and Polymers of Tripalladium(0) Ditropylium Halides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2708
_journal_page_last               2710
_journal_paper_doi               10.1021/ic8014578
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C14 H14 Br3 Pd3 -, C24 H20 P +, C2 H3 N'
_chemical_formula_sum            'C40 H37 Br3 N P Pd3'
_chemical_formula_weight         1121.61
_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                 90.838(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.550(3)
_cell_length_b                   30.138(11)
_cell_length_c                   16.293(6)
_cell_measurement_reflns_used    1905
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.50
_cell_measurement_theta_min      2.50
_cell_volume                     3707(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_sigmaI/netI    0.1048
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19496
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.747
_exptl_absorpt_correction_T_max  0.7973
_exptl_absorpt_correction_T_min  0.2319
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.798
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0000P)^2^+186.2965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                2667
_reflns_number_total             4794
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8014578_si_001_1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301759