Structure-Directing Effects in the Supramolecular Intercluster Compound [Au9(PPh3)8]2[V10O28H3]2: Long-Range versus Short-Range Bonding Interactions
Martin Schulz-Dobrick; Martin Jansen; Inorganic Chemistry 46 (2007) 4380–4382; doi:10.1021/ic700434x

data_4308293
_publ_contact_author_address
;MPI for Solid State Research
Heisenbergstr. 1
70569 Stuttgart
Germany
;
_publ_contact_author_email       m.jansen@fkf.mpg.de
_publ_contact_author_name        'Martin Jansen'
_publ_section_title
;
Structure-Directing Effects in the Supramolecular Intercluster Compound
[Au9(PPh3)8]2[V10O28H3]2: Long-Range versus Short-Range Bonding
Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4380
_journal_page_last               4382
_journal_paper_doi               10.1021/ic700434x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'2(Au9P8C144H120), 2(V10O28H3), 2(CH2Cl2), 3(C2H3N)'
_chemical_formula_sum            'C296 H253 Au18 Cl4 N3 O56 P16 V20'
_chemical_formula_weight         9949.53
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.654(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.510(2)
_cell_length_b                   33.749(3)
_cell_length_c                   46.872(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     35606(6)
_computing_cell_refinement       'SMART32 (Bruker AXS)'
_computing_data_collection       'SMART32 (Bruker AXS)'
_computing_data_reduction        'SMART32 (Bruker AXS)'
_computing_molecular_graphics    'Diamond 3.0b (Crystal-Impact, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'AXS Bruker, SMART APEX'
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            309758
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    8.040
_exptl_absorpt_correction_T_max  0.6893
_exptl_absorpt_correction_T_min  0.1965
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
' SADABS, G.M. Sheldrick, Bruker AXS Inc., Madison, WI (1998).'
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             18752
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         4.020
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3634
_refine_ls_number_reflns         81832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                59781
_reflns_number_total             81832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700434x-file001.cif
_cod_data_source_block           Au9V10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308293