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_4301762
_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 I2 Pd3, 2 C2 H6 O S'
_chemical_formula_sum            'C18 H26 I2 O2 Pd3 S2'
_chemical_formula_weight         911.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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                   7.7483(9)
_cell_length_b                   17.074(2)
_cell_length_c                   17.804(2)
_cell_measurement_reflns_used    6761
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.35
_cell_volume                     2355.4(5)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10000
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.077
_exptl_absorpt_correction_T_max  0.6177
_exptl_absorpt_correction_T_min  0.2696
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 02/2008; Sheldrick, 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.00036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0170P)^2^+2.4926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0444
_reflns_number_gt                2900
_reflns_number_total             2995
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8014578_si_001_4.cif
_cod_data_source_block           5
_cod_original_cell_volume        2355.3(5)
_cod_database_code               4301762