Ferrocenyl-Passivated Nanoclusters: Synthesis of [Cu20Se6(Se2fc)4(PR2R‘)10] and [Cu40Se12(Se2fc)8(PPh3)9]
Wallbank, Andrew I.; Borecki, Aneta; Taylor, Nicholas J.; Corrigan, John F.; Organometallics 24 (2005) 788–; doi:10.1021/om049238c

data_4075727
_publ_section_title
;
 Ferrocenyl-Passivated Nanoclusters:&#x00A0; Synthesis of
 [Cu20Se6(Se2fc)4(PR2R&#x2018;)10] and [Cu40Se12(Se2fc)8(PPh3)9]
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              788
_journal_paper_doi               10.1021/om049238c
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C212 H246 Cu20 Fe4 O8 P10 Se14'
_chemical_formula_weight         5831.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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_creation_method           SHELXL-97
_cell_angle_alpha                79.948(1)
_cell_angle_beta                 89.293(1)
_cell_angle_gamma                63.643(1)
_cell_formula_units_Z            1
_cell_length_a                   17.6298(4)
_cell_length_b                   18.2844(3)
_cell_length_c                   19.0130(5)
_cell_measurement_temperature    200(2)
_cell_volume                     5392.7(2)
_computing_cell_refinement       'Nonius Collect'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'Nonius Collect'
_computing_molecular_graphics    Schakal
_computing_publication_material  Schakal
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.1537
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28154
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.674
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle plate'
_exptl_crystal_F_000             2892
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         18927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                10076
_reflns_number_total             18927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049238csi20050120_102422.cif
_cod_data_source_block           complex1a
_cod_database_code               4075727