Synthesis and Characterization of VV(3,6-DBSQ)(3,6-DBCat)2, a d0 Metal Complex with Dioxygenase Catalytic Activity
Aimee M. Morris; Cortlandt G. Pierpont; Richard G. Finke; Inorganic Chemistry 48 (2009) 3496–3498; doi:10.1021/ic802122q

data_4301951
_publ_section_title
;
Synthesis and Characterization of VV(3,6-DBSQ)(3,6-DBCat)2, a d0 Metal
Complex with Dioxygenase Catalytic Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3496
_journal_page_last               3498
_journal_paper_doi               10.1021/ic802122q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C43 H64 O7 V'
_chemical_formula_weight         743.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :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            8
_cell_length_a                   19.9969(17)
_cell_length_b                   23.740(2)
_cell_length_c                   18.1741(16)
_cell_measurement_reflns_used    3222
_cell_measurement_temperature    296(2)
_cell_volume                     8627.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14529
_diffrn_reflns_theta_full        23.53
_diffrn_reflns_theta_max         23.53
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.9826
_exptl_absorpt_correction_T_min  0.9080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
PLATON SQUEEZE was used to correct for a disordered methanol solvate molecule 
located about the inversion center (0, 0.25, 0.25). 
;
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0545P)^2^+5.9333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                2234
_reflns_number_total             3222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802122q_si_002.cif
_cod_data_source_block           rf110r_0m
_cod_original_cell_volume        8627.8(13)
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4301951