Synthesis, Reactivity, and Electronic Structure of [n]Vanadoarenophanes: An Experimental and Theoretical Study
Holger Braunschweig; Martin Kaupp; Christopher J. Adams; Thomas Kupfer; Krzysztof Radacki; Sandra Schinzel; Journal of the American Chemical Society 130 (2008) 11376–11393; doi:10.1021/ja802034p

data_4108230
_publ_contact_author_address
; Institut fuer Anorganische Chemie
Universitaet Wuerzburg
Am Hubland
97074 Wuerzburg, Germany
;
_publ_contact_author_email       H.Braunschweig@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-8884623
_publ_contact_author_name        'Prof. Dr. Holger Braunschweig'
_publ_contact_author_phone       +49-931-8885260
_publ_section_title
;
 Synthesis, Reactivity, and Electronic Structure of [n]Vanadoarenophanes:
 An Experimental and Theoretical Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11376
_journal_page_last               11393
_journal_paper_doi               10.1021/ja802034p
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C48 H68 Li4 O6 V2, C4 H8 O'
_chemical_formula_sum            'C52 H76 Li4 O7 V2'
_chemical_formula_weight         942.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                93.159(4)
_cell_angle_beta                 90.694(4)
_cell_angle_gamma                93.629(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1225(7)
_cell_length_b                   12.4870(8)
_cell_length_c                   19.2872(12)
_cell_measurement_reflns_used    9033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      2.29
_cell_volume                     2429.0(3)
_computing_cell_refinement       'Saint+ ver. 7.12A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 1.0-27 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.12A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62805
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2004/1 (Brucker Nonius 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         14700
_refine_ls_number_restraints     975
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+4.1261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                9790
_reflns_number_total             14700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802034p-file004.cif
_cod_data_source_block           Kr092
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               4108230