Twisted [(<i>R</i>~3~P)Pd<i>X</i>] groups above dicarbaborane ligands: 4-dimethylsulfido-3-iodo-3-triphenylphosphine-<i>closo</i>-3-pallada-1,2-dicarbadodecaborane and 3-dimethylphenylphosphine-3-chloro-4-dimethylsulfido-<i>closo</i>-3-pallada-1,2-dicarbadodecaborane
Ferguson, George; Gallagher, John F.; Kennedy, John D.; O'Connell, Donnacha P.; Patterson, Jennifer C.; Spalding, Trevor R.; Acta Crystallographica Section C 61 (2005) m393–m396; doi:10.1107/S0108270105022286

data_2015073
_publ_section_title
;Twisted [(<i>R</i>~3~P)Pd<i>X</i>] groups above dicarbaborane ligands:
 4-dimethylsulfido-3-iodo-3-triphenylphosphine-<i>closo</i>-3-pallada-1,2-dicarbadodecaborane
 and
 3-dimethylphenylphosphine-3-chloro-4-dimethylsulfido-<i>closo</i>-3-pallada-1,2-dicarbadodecaborane
;
_journal_coeditor_code           SK1861
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m393
_journal_page_last               m396
_journal_paper_doi               10.1107/S0108270105022286
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Pd (C4 H16 B9 S) Cl (C8 H11 P1)]'
_chemical_formula_moiety         'C12 H27 B9 Cl P Pd S'
_chemical_formula_sum            'C12 H27 B9 Cl P Pd S'
_chemical_formula_weight         473.54
_chemical_name_systematic
;
3-dimethylphenylphosphine-
3-chloro-4-dimethylsulfido-closo-3-pallada-1,2-dicarbadodecaborane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.567(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8117(8)
_cell_length_b                   9.2670(7)
_cell_length_c                   18.2948(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      16.50
_cell_measurement_theta_min      10.01
_cell_volume                     2157.8(2)
_computing_cell_refinement       'DIFRAC (Gabe & White, 1993)'
_computing_data_collection
'DIFRAC (Gabe & White, 1993) with profile analysis'
_computing_data_reduction
'DATRD2 in NRCVAX94 (Gabe <i>et al.</i>, 1989)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997) in WinGX (Version 1.70.01; Farrugia, 1999)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6506
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'(ABSCOR in NRCVAX; Gabe <i>et al.</i>, 1989)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.514
_refine_ls_extinction_coef       0.00185(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         6265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.6303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                5023
_reflns_number_total             6265
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1861.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015073
_cod_database_fobs_code          2015073