Unusual cationic rhodathiaboranes: synthesis and characterization of [8,8,8-(H)(PR3)2-9-(Py)-nido-8,7-RhSB9H10](+) and [1,3-μ-(H)-1,1-(PR3)2-3-(Py)-isonido-1,2-RhSB9H8](+).
Calvo, Beatriz; Macías, Ramón; Artigas, Maria Jose; Lahoz, Fernando J.; Oro, Luis A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5121–5133; doi:10.1039/c3dt52018h

data_7029329
_publ_section_title
;
 Unusual cationic rhodathiaboranes: synthesis and characterization of
 [8,8,8-(H)(PR3)2-9-(Py)-nido-8,7-RhSB9H10](+) and
 [1,3-\m-(H)-1,1-(PR3)2-3-(Py)-isonido-1,2-RhSB9H8](+).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5121
_journal_page_last               5133
_journal_paper_doi               10.1039/c3dt52018h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'3 (C26 H38 B9 N P2 Rh S), 3 (C F3 S O3), 5 (C H2 Cl2)'
_chemical_formula_sum            'C86 H124 B27 Cl10 F9 N3 O9 P6 Rh3 S6'
_chemical_formula_weight         2848.16
_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                106.782(4)
_cell_angle_beta                 96.410(4)
_cell_angle_gamma                94.265(4)
_cell_formula_units_Z            2
_cell_length_a                   15.722(3)
_cell_length_b                   17.815(4)
_cell_length_c                   23.470(5)
_cell_measurement_reflns_used    4048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      2.34
_cell_volume                     6215(2)
_computing_cell_refinement       'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ENCIFER
_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 0.966
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0874
_diffrn_reflns_av_sigmaI/netI    0.1892
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52276
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        no-decay
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.9145
_exptl_absorpt_correction_T_min  0.7210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.654
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         29709
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1838
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                14227
_reflns_number_total             29709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52018h.txt
_cod_data_source_block           compnd_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7029329