Synthesis, Spectroscopic, and X-ray Characterization of Rhenium Carbonyl Complexes with Different Silsesquioxanes, as Models That Mimic the Chemical Behavior and the Topology of the Silica Surface
Dragonetti, Claudia; Carlucci, Lucia; D'Alfonso, Giuseppe; Lucenti, Elena; Macchi, Piero; Roberto, Dominique; Sironi, Angelo; Ugo, Renato; Organometallics 28 (2009) 2668–2676; doi:10.1021/om800991s

data_4068629
_publ_section_title
;
 Synthesis, Spectroscopic, and X-ray Characterization of Rhenium Carbonyl
 Complexes with Different Silsesquioxanes, as Models That Mimic the
 Chemical Behavior and the Topology of the Silica Surface
;
_journal_coden_ASTM              ORGND7
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2668
_journal_page_last               2676
_journal_paper_doi               10.1021/om800991s
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C50 H77 O21 Re2 Si8'
_chemical_formula_weight         1611.23
_space_group_IT_number           2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-10-09T18:13:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                111.662(5)
_cell_angle_beta                 99.928(5)
_cell_angle_gamma                96.807(5)
_cell_formula_units_Z            4
_cell_length_a                   16.628(5)
_cell_length_b                   21.022(5)
_cell_length_c                   21.850(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6852(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            79763
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    3.735
_exptl_absorpt_correction_T_max  0.3733
_exptl_absorpt_correction_T_min  0.3642
_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    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3228
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.268
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         19709
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.156
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+34.9511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                13841
_reflns_number_total             19709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800991s_si_001.cif
_cod_data_source_block           6
_cod_database_code               4068629