Synthesis of Rhodium‒Primary Thioamide Complexes and Their Desulfurization Leading to Rhodium Sulfido Cubane-Type Clusters and Nitriles
Mutoh, Yuichiro; Sakigawara, Masahiro; Niiyama, Ippei; Saito, Shinichi; Ishii, Youichi; Organometallics 33 (2014) 5414–; doi:10.1021/om500714c

data_4084394
_publ_section_title
;
 Synthesis of Rhodium--Primary Thioamide Complexes and Their
 Desulfurization Leading to Rhodium Sulfido Cubane-Type Clusters and
 Nitriles
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5414
_journal_paper_doi               10.1021/om500714c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C72 H72 B F24 Rh4 S4'
_chemical_formula_weight         1943.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 101.209(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.743(2)
_cell_length_b                   15.166(3)
_cell_length_c                   19.650(4)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    123.1500
_cell_measurement_theta_max      27.5126
_cell_measurement_theta_min      3.1422
_cell_volume                     3725.1(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      123.1500
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27852
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQUAB Jacobsen'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1938
_exptl_crystal_size_max          0.4250
_exptl_crystal_size_mid          0.4210
_exptl_crystal_size_min          0.2170
_refine_diff_density_max         2.014
_refine_diff_density_min         -1.956
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+7.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                7298
_reflns_number_total             8511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500714c_si_002.cif
_cod_data_source_block           4BArF_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 

 Adding full bibliography for 4084388--4084398.cif.
;
_cod_original_cell_volume        3724.9(11)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4084394