Synthesis and X-ray structure of the [{Fe3(CO)9(micro3-O)}2H]3- trianion: dimerization of a metal carbonyl cluster via formation of an exceptionally short hydrogen bond.
Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Zazzaroni, Enrico; Dalton transactions (Cambridge, England : 2003)  (2007) 2644–2651; doi:10.1039/b703628k

data_7005613
_publ_section_title
;
 Synthesis and X-ray structure of the [{Fe3(CO)9(micro3-O)}2H]3-
 trianion: dimerization of a metal carbonyl cluster via formation of an
 exceptionally short hydrogen bond.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2644
_journal_page_last               2651
_journal_paper_doi               10.1039/b703628k
_journal_year                    2007
_chemical_formula_sum            'C22 H9 Cs3 Fe6 O21'
_chemical_formula_weight         1343.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           166
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.0952(3)
_cell_length_b                   13.0952(3)
_cell_length_c                   18.5660(10)
_cell_measurement_reflns_used    5555
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.263
_cell_measurement_theta_min      2.8355
_cell_volume                     2757.23(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0082
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10703
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    5.312
_exptl_absorpt_correction_T_max  0.5926
_exptl_absorpt_correction_T_min  0.4318
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         837
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.550
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0296P)^2^+5.7606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                772
_reflns_number_total             837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703628k.txt
_cod_data_source_block           r-3m
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               7005613