Directed Synthesis of the Triangular Mixed-Metal Cluster H2RhRe2Cp*(CO)9: Ligand Fluxionality and Facile Cluster Fragmentation in the Presence of CO, Halogenated Solvents, and Thiols
Huang, Shih-Huang; Watson, William H.; Carrano, Carl J.; Wang, Xiaoping; Richmond, Michael G.; Organometallics 29 (2010) 61–; doi:10.1021/om9007407

data_4067276
_publ_section_title
;
 Directed Synthesis of the Triangular Mixed-Metal Cluster H2RhRe2Cp*(CO)9:
 Ligand Fluxionality and Facile Cluster Fragmentation in the Presence of
 CO, Halogenated Solvents, and Thiols
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              61
_journal_paper_doi               10.1021/om9007407
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C14 H15 O4 Rh3 S2'
_chemical_formula_weight         620.11
_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                 103.347(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4420(11)
_cell_length_b                   23.212(3)
_cell_length_c                   10.2361(14)
_cell_measurement_reflns_used    805
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.63
_cell_volume                     1951.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0887
_diffrn_reflns_av_sigmaI/netI    0.1147
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16833
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  0.6747
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0055P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                2781
_reflns_number_total             4553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9007407_si_003.cif
_cod_data_source_block           w1417m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        1951.7(4)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4067276