Effect of Pnictogen Ligand Substitution on a Tripalladium Ditropylium Core
Dominic C. Babbini; Frank L. Mulligan; Hannah R. Schulhauser; Tara C. Sweigart; Gary S. Nichol; Stephanie K. Hurst; Inorganic Chemistry 49 (2010) 4307–4312; doi:10.1021/ic100151x

data_4315394
_publ_contact_author             'Professor Stephanie Hurst'
_publ_contact_author_email       stephanie.hurst@nau.edu
_publ_section_title
;
 Effect of Pnictogen Ligand Substitution on a Tripalladium Ditropylium
 Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4307
_journal_page_last               4312
_journal_paper_doi               10.1021/ic100151x
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C68 H59 P3 Pd3 2 +, 2 B F4 -'
_chemical_formula_sum            'C68 H59 B2 F8 P3 Pd3'
_chemical_formula_weight         1461.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 96.119(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9823(9)
_cell_length_b                   27.0746(15)
_cell_length_c                   30.441(2)
_cell_measurement_reflns_used    3395
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.61
_cell_measurement_theta_min      2.20
_cell_volume                     12277.7(13)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34243
_diffrn_reflns_theta_full        21.65
_diffrn_reflns_theta_max         21.65
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1; Sheldrick, 1996'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
One disordered BF4- removed.
;
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         5456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                3659
_reflns_number_total             5456
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100151x_si_001_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4315394