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_4315393
_publ_contact_author             'Professor Stephanie Hurst'
_publ_contact_author_email       stephanie.hurst@nau.edu
_publ_section_title
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 Effect of Pnictogen Ligand Substitution on a Tripalladium Ditropylium
 Core
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_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         '5 C32 H59 P3 Pd3 2+, 10 B F4 -, 9 C H2 Cl2'
_chemical_formula_sum            'C169 H313 B10 Cl18 F40 P15 Pd15'
_chemical_formula_weight         5911.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.523(5)
_cell_angle_beta                 81.124(5)
_cell_angle_gamma                88.128(5)
_cell_formula_units_Z            2
_cell_length_a                   15.047(6)
_cell_length_b                   17.647(7)
_cell_length_c                   43.937(17)
_cell_measurement_reflns_used    4849
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.23
_cell_volume                     11473(8)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 1999)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0975
_diffrn_reflns_av_sigmaI/netI    0.1770
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            52503
_diffrn_reflns_theta_full        20.92
_diffrn_reflns_theta_max         20.92
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  0.7697
_exptl_absorpt_correction_T_min  0.5932
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5916
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.731
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       0.0048(2)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2406
_refine_ls_number_reflns         24033
_refine_ls_number_restraints     1291
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1682
_refine_ls_R_factor_gt           0.1061
_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^)+(0.1708P)^2^+76.2706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2657
_refine_ls_wR_factor_ref         0.3207
_reflns_number_gt                13694
_reflns_number_total             24033
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100151x_si_001_1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        11473(7)
_cod_database_code               4315393