The loss of CO from [Rh12(μ12-Sn)(CO)27]4−: Synthesis, spectroscopic and structural characterization of the electron-deficient, icosahedral [Rh12(μ12-Sn)(CO)25]4− and [Rh12(μ12-Sn)(CO)26]4− tetra-anions
Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Tiozzo, Cristina; Zacchini, Stefano; Heaton, Brian T.; Iggo, Johnathan A.; Zanello, Piero; Fedi, Serena; Garland, Marc V.; Li, Chuanzhao; Dalton Transactions  (2009) 2217–2223; doi:10.1039/b818944g

data_7000784
_publ_section_title
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 The loss of CO from [Rh12(\m12-Sn)(CO)27]4&#x2212;: Synthesis,
 spectroscopic and structural characterization of the
 electron-deficient, icosahedral [Rh12(\m12-Sn)(CO)25]4&#x2212; and
 [Rh12(\m12-Sn)(CO)26]4&#x2212; tetra-anions
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_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2217
_journal_page_last               2223
_journal_paper_doi               10.1039/b818944g
_journal_year                    2009
_chemical_formula_sum            'C61 H86 N6 O25 Rh12 Sn'
_chemical_formula_weight         2656.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.230(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8773(14)
_cell_length_b                   14.4853(16)
_cell_length_c                   21.568(2)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    97(2)
_cell_measurement_theta_max      28.141
_cell_measurement_theta_min      2.7015
_cell_volume                     3981.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      97(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37552
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   'empirical sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         13983
_refine_ls_number_restraints     367
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                11160
_reflns_number_total             13983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818944g.txt
_cod_data_source_block           p21num
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7000784