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_4301761
_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 Br2 Pd2, 2 C2 H6 O S'
_chemical_formula_sum            'C18 H26 Br2 O2 Pd3 S2'
_chemical_formula_weight         817.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.969(4)
_cell_length_b                   7.4951(19)
_cell_length_c                   17.292(5)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.40
_cell_volume                     2199.3(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_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, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11636
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    6.263
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.0759
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.041(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3626
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.004
_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^+20.6061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                3117
_reflns_number_total             3626
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8014578_si_001_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        2199.2(10)
_cod_database_code               4301761