Monocarbaborane anion chemistry. An interesting encapsulation of the Pd2I2{P(C6H4-4-Me)3}4]2+ cation by a pair of [PhCB9H4I(C6H4Me)4]??? anions
Franken, Andreas; Kilner, Colin A.; Thornton-Pett, Mark; Kennedy, John D.; Chemical Communications  (2002) 2048–; doi:10.1039/b205697f

data_7114022
_publ_section_title
;
 Monocarbaborane anion chemistry. An interesting encapsulation of the
 Pd2I2{P(C6H4-4-Me)3}4]2+ cation by a pair of [PhCB9H4I(C6H4Me)4]???
 anions
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2048
_journal_paper_doi               10.1039/b205697f
_journal_year                    2002
_chemical_formula_sum            'C77 H79 B9 Cl0.25 I1.75 P2 Pd'
_chemical_formula_weight         1500.97
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.2970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.23370(10)
_cell_length_b                   19.1946(2)
_cell_length_c                   28.6687(3)
_cell_measurement_temperature    150(2)
_cell_volume                     7830.57(13)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 1997)
XSeed (Barbour, 2001)
;
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60090
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.8794
_exptl_absorpt_correction_T_min  0.6990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         15331
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.615
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+11.1714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                11947
_reflns_number_total             15331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205697f.txt
_cod_data_source_block           afx10a
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7114022