Self-Assembly of High-Nuclearity Metal Clusters: Programmed Expansion of a Metallasiloxane Cage to an Octacopper(II) Cluster
Gian Luca Abbati; Andrea Cornia; Andrea Caneschi; Antonio Costantino Fabretti; Cecilia Mortalò; Inorganic Chemistry 43 (2004) 4540–4542; doi:10.1021/ic049898+

data_4327437
_publ_contact_author_address
;     Universit\'a di Modena and Reggio Emilia
      Dipartimento di Chimica 
      Via G. Campi, 183
      I-41100, Modena
      Italy
;
_publ_contact_author_email       'abbati@unimore.it, acornia@unimore.it'
_publ_contact_author_name        'Abbati, Gian Luca - Cornia, Andrea'
_publ_contact_author_phone       '++39 059 2055030, ++39 059 2055032'
_publ_section_title
;
 Self-Assembly of High-Nuclearity Metal Clusters: Programmed Expansion of
 a Metallasiloxane Cage to an Octacopper(II) Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4540
_journal_page_last               4542
_journal_paper_doi               10.1021/ic049898+
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
;
 (C102 H136 Cu8 N10 O28 Si12 2+), 2(Cl1 O4 1-), (C1 H4 O1)
;
_chemical_formula_sum            'C103 H140 Cl2 Cu8 N10 O37 Si12'
_chemical_formula_weight         3026.56
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.7658(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   16.8490(3)
_cell_length_b                   22.2966(4)
_cell_length_c                   17.2508(3)
_cell_measurement_reflns_used    380
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71069
_cell_volume                     6458.3(2)
_computing_cell_refinement       'SAINT (Siemens Inc., 1995)'
_computing_data_collection       'SMART (Siemens Inc., 1993)'
_computing_data_reduction        'SAINT (Siemens Inc., 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SIEMENS/SMART CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_wavelength_id  1
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85127
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_T_max  0.6101
_exptl_absorpt_correction_T_min  0.4027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens Inc., 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             3108
_exptl_crystal_id                1
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1193
_refine_ls_number_reflns         18857
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+1.1375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                14299
_reflns_number_total             18857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0498982Bsi20040126_112043.cif
_cod_data_source_block           cu8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4327437