Modification of [8,8,8-(H)(PPh3)2-9-(Py)-nido-8,7-RhSB9H9], Py = NC5H5, with Monodentate Phosphines: Reactivity and Mechanistic Insights
Calvo, Beatriz; Álvarez, Álvaro; Macías, Ramón; García-Orduña, Pilar; Lahoz, Fernando J.; Oro, Luis A.; Organometallics 31 (2012) 2986–; doi:10.1021/om2009205

data_4077876
_publ_section_title
;
 Modification of [8,8,8-(H)(PPh3)2-9-(Py)-nido-8,7-RhSB9H9], Py = NC5H5,
 with Monodentate Phosphines: Reactivity and Mechanistic Insights
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2986
_journal_paper_doi               10.1021/om2009205
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C26 H37 B9 N P2 Rh S, C H2 Cl2'
_chemical_formula_sum            'C27 H39 B9 Cl2 N P2 Rh S'
_chemical_formula_weight         742.69
_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                87.299(2)
_cell_angle_beta                 69.5940(10)
_cell_angle_gamma                81.4180(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8930(11)
_cell_length_b                   12.0718(12)
_cell_length_c                   14.3942(14)
_cell_measurement_reflns_used    219
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.9045
_cell_measurement_theta_min      2.268
_cell_volume                     1754.1(3)
_computing_cell_refinement       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker Kappa APEX DUO CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19013
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.9428
_exptl_absorpt_correction_T_min  0.7984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.377
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                6398
_reflns_number_total             8827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2009205_si_001.cif
_cod_data_source_block           compound_10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4077876