Vanadyl C and N-capped tris(phenolate) complexes: influence of pro-catalyst geometry on catalytic activity.
Carl Redshaw; Sophie H. Dale; Mark R.J. Elsegood; Damien M. Hamden; Sadahiko Matsuura; Shigekazu Matsui; Michael Rowan; Chemical Communications  (2006) –; doi:10.1039/b606897a

data_7101337
_publ_section_title
;
Vanadyl C and N-capped tris(phenolate) complexes:
influence of pro-catalyst geometry on catalytic activity.
;
_journal_issue                   31
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b606897a
_journal_year                    2006
_chemical_formula_sum            'C52 H73 N O3'
_chemical_formula_weight         760.11
_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                116.865(2)
_cell_angle_beta                 116.214(2)
_cell_angle_gamma                91.421(3)
_cell_formula_units_Z            2
_cell_length_a                   14.452(2)
_cell_length_b                   14.819(3)
_cell_length_c                   14.999(3)
_cell_measurement_reflns_used    1797
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      3.63
_cell_volume                     2467.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8464
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12956
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        6
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10, Sheldrick, G.M., (2003)'
_exptl_crystal_colour            yellow/green
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.026(4)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0776
_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^)+(0.1006P)^2^+1.7153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2253
_reflns_number_gt                4298
_reflns_number_total             6318
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b606897a.txt
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101337