Rhodium and Iridium Phosphinothiolato Complexes. Synthesis and Crystal Structures of Mononuclear [M(cod)(S,P-SC~2~B~10~H~10~PPh~2~)] and Dinuclear [M~2~(CO)~2~(S,P-μ-SC~2~B~10~H~10~PPh~2~)] (M = Rh, Ir) and Their Performance in Catalytic Carbonylation
Lee, Heung-Sae; Bae, Jin-Young; Kim, Dae-Hyun; Kim, Hoon Sik; Kim, Sung-Joon; Cho, Sungil; Ko, Jaejung; Kang, Sang Ook; Organometallics 21 (2002) 210–219; doi:10.1021/om0107789

data_4060799
_publ_section_title
;
Rhodium and Iridium Phosphinothiolato Complexes. Synthesis and Crystal 
Structures of Mononuclear [M(cod)(S,P-SC~2~B~10~H~10~PPh~2~)] and 
Dinuclear [M~2~(CO)~2~(S,P-\m-SC~2~B~10~H~10~PPh~2~)] (M = Rh, Ir) 
and Their Performance in Catalytic Carbonylation
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              210
_journal_page_last               219
_journal_paper_doi               10.1021/om0107789
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C22 H32 B10 Ir P S'
_chemical_formula_weight         659.81
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.366(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6869(10)
_cell_length_b                   11.1010(6)
_cell_length_c                   18.7413(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.39
_cell_measurement_theta_min      11.49
_cell_volume                     2604.3(3)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1988)'
_computing_data_reduction        'Xtal3.2 (Hall & Stewart, 1992)'
_computing_molecular_graphics    'ORTEP3 (Jonson & Burrett, 1998)'
_computing_publication_material  SHELXL-97(Sheldrick,1997)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5376
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        4.47
_diffrn_standards_interval_count 3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.281
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.703
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.703
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                4255
_reflns_number_total             5101
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4060798
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060799