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_2015072
_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) I (C18 H15 P)]'
_chemical_formula_moiety         'C22 H31 B9 I P Pd S'
_chemical_formula_sum            'C22 H31 B9 I P Pd S'
_chemical_formula_weight         689.12
_chemical_name_systematic
;
4-dimethylsulfido-3-iodo-3-triphenylphosphine-closo-3-pallada-
1,2-dicarbadodecaborane
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.9576(5)
_cell_length_b                   16.8316(10)
_cell_length_c                   30.2015(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      15.97
_cell_measurement_theta_min      9.88
_cell_volume                     5570.2(5)
_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  0.0
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6057
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'(ABSCOR in NRCVAX; Gabe <i>et al.</i>, 1989)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.925
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0367
_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^)+(0.1025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                3546
_reflns_number_total             6057
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1861.cif
_cod_data_source_block           I
_cod_database_code               2015072
_cod_database_fobs_code          2015072