New High-Nuclearity Carbonyl and Carbonyl-Substituted Rhodium Clusters and Their Relationships with Polyicosahedral Carbonyl-Substituted Palladium- and Gold-Thiolates
Dmitriy S. Dolzhnikov; Maria C. Iapalucci; Giuliano Longoni; Cristina Tiozzo; Stefano Zacchini; Cristina Femoni; Inorganic Chemistry 51 (2012) 11214–11216; doi:10.1021/ic3011508

data_4330817
_publ_section_title
;
 New High-Nuclearity Carbonyl and Carbonyl-Substituted Rhodium Clusters
 and Their Relationships with Polyicosahedral Carbonyl-Substituted
 Palladium- and Gold-Thiolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11214
_journal_page_last               11216
_journal_paper_doi               10.1021/ic3011508
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C96 H118 N5 O50 Rh33'
_chemical_formula_weight         5537.98
_chemical_name_systematic
; 
 ? 
;
_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                 91.0730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3097(16)
_cell_length_b                   27.097(3)
_cell_length_c                   33.126(3)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.190
_cell_measurement_theta_min      2.294
_cell_volume                     13740(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCANS'
_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  0.3120
_diffrn_reflns_av_sigmaI/netI    0.2428
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            130145
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_T_max  0.6954
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   'empirical SADABS'
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    2.677
_exptl_crystal_description       PRISMATIC
_exptl_crystal_F_000             10456
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1657
_refine_ls_number_reflns         24177
_refine_ls_number_restraints     728
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.2425
_refine_ls_R_factor_gt           0.0823
_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^)+(0.0953P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2574
_reflns_number_gt                8678
_reflns_number_total             24177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3011508_si_002_2.cif
_cod_data_source_block           p21n
_cod_database_code               4330817