Mono- and Dinuclear Oxovanadium(V)calixarene Complexes and Their Activity as Oxidation Catalysts
Hoppe, Elke; Limberg, Christian; Ziemer, Burkhard; Inorganic Chemistry 45 (2006) 8308–8317; doi:10.1021/ic061106j

data_4332928
_publ_section_title
;
 Mono- and Dinuclear Oxovanadium(V)calixarene Complexes and Their Activity
 as Oxidation Catalysts
;
_journal_issue                   20
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8308
_journal_page_last               8317
_journal_paper_doi               10.1021/ic061106j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C44 H52 O5 V, C24 H20 P, C H2 Cl2'
_chemical_formula_sum            'C69 H74 Cl2 O5 P V'
_chemical_formula_weight         1136.09
_chemical_name_systematic
; 
 Ph~4~P[p-tert-butyl-calix[4]arene tetrahydroxylato oxovanadate(V)] 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.763(3)
_cell_length_b                   12.763(3)
_cell_length_c                   18.722(9)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      13.0
_cell_volume                     3049.7(18)
_computing_cell_refinement       'STADI4-1.06 (Stoe & Cie, 1997)'
_computing_data_collection       'STADI4-1.06 (Stoe & Cie, 1997)'
_computing_data_reduction        'XRED1.08 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Stoe STADI4 diffractometer'
_diffrn_measurement_method       2\Q/\w-scan,ratio=1.0,width(\w)=1.2-1.35\%
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8969
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        5.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_correction_T_min  0.7365
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 North,A.C.T., Phillips,D.C., Mathwes,F.S. (1968). Acta Cryst. A24, 351-359.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0088(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+2.1983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                2445
_reflns_number_total             2995
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic061106jsup5.cif
_cod_data_source_block           hopp8
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4332928