A Re(CO)5 Fragment Bonded to a Polyhedral Oligomeric Hydroxysilsesquioxane as a Model which Gives Further Evidence to the Existence of an Unexpected Re(CO)5 Surface Species
Elena Lucenti; Giuseppe D'Alfonso; Piero Macchi; Mario Maranesi; Dominique Roberto; Angelo Sironi; Renato Ugo; Journal of the American Chemical Society 128 (2006) 12054–12055; doi:10.1021/ja0630588

data_4110868
_publ_contact_author             'Macchi, P.'
_publ_contact_author_email       piero.macchi@unimi.it
_publ_section_title
;
 A Re(CO)5 Fragment Bonded to a Polyhedral Oligomeric
 Hydroxysilsesquioxane as a Model which Gives Further Evidence to the
 Existence of an Unexpected Re(CO)5 Surface Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12054
_journal_page_last               12055
_journal_paper_doi               10.1021/ja0630588
_journal_volume                  128
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_sum            'C95 H160 Cl6 O34 Re2 Si16'
_chemical_formula_weight         2880.77
_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_date             2006-07-27T17:25:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.923(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4531(16)
_cell_length_b                   38.667(5)
_cell_length_c                   13.6401(17)
_cell_measurement_temperature    293(2)
_cell_volume                     6567.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            66900
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    2.178
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.7431
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
        Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
        for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
        p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
        A31,146-148) is used with some modification.
;
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_F_000             2956
_refine_diff_density_max         1.603
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.570(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         25399
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+34.8433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.149
_refine_ls_wR_factor_ref         0.1633
_reflns_number_gt                19775
_reflns_number_total             25399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0630588si20060729_065230.cif
_cod_data_source_block           dr6c
_cod_original_cell_volume        6567.2(14)
_cod_database_code               4110868