Mixed Ruthenium-Rhodium Carbonyl Cluster Complexes. Synthesis of the Anions [Ru3Rh(CO)13]- and [RuRh3(CO)12]- and Crystal Structures of Their [N(PPh3)2]+ Salts 1
Alessandro Fumagalli; Mascia Bianchi; Maria Carlotta Malatesta; Gianfranco Ciani; Massimo Moret; Angelo Sironi; Inorganic Chemistry 37 (1998) 1324–1328; doi:10.1021/ic970862+

data_4327672
_publ_section_title
;
 Mixed Ruthenium-Rhodium Carbonyl Cluster Complexes. Synthesis of the
 Anions [Ru3Rh(CO)13]- and [RuRh3(CO)12]- and Crystal Structures of Their
 [N(PPh3)2]+ Salts 1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1324
_journal_page_last               1328
_journal_paper_doi               10.1021/ic970862+
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C49 H30 N O13 P2 Rh Ru3'
_chemical_formula_weight         1308.80
_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
_cell_angle_alpha                110.53(1)
_cell_angle_beta                 99.79(2)
_cell_angle_gamma                91.85(2)
_cell_formula_units_Z            2
_cell_length_a                   9.827(2)
_cell_length_b                   14.911(2)
_cell_length_c                   18.735(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2520.9(8)
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_method       'w scan'
_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  0.0112
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8800
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        3%
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.060
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.026
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.026
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_obs          0.0342
_refine_ls_shift/esd_max         0.052
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.0557P)^2^+3.7112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0983
_refine_ls_wR_factor_obs         0.0926
_reflns_number_observed          7257
_reflns_number_total             7272
_reflns_observed_criterion       I>3s(I)
_cod_data_source_file            ic9708622B_1.cif
_cod_data_source_block           fu6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w=1/[s^2^(Fo^2^)+(0.0557P)^2^+3.7112P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[s^2^(Fo^2^)+(0.0557P)^2^+3.7112P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2520.9(7)
_cod_database_code               4327672
_exptl_absorpt_correction_nazim  3
_diffrn_measurement_domega       '1.0 + 0.35 tan q'
_diffrn_measurement_rtime        60