Air oxidation of divanadium(IV) complexes
Kirk Egdal, Rune; Bond, Andrew D.; McKenzie, Christine J.; Dalton Transactions  (2009) 3833–3839; doi:10.1039/b901633c

data_7001272
_publ_section_title
;
 Air oxidation of divanadium(IV) complexes
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3833
_journal_page_last               3839
_journal_paper_doi               10.1039/b901633c
_journal_year                    2009
_chemical_formula_moiety
;
C36 H41 N6 O5 V2 2+, 2(Cl O4 -), 2(H2 O), C2 H6 O
;
_chemical_formula_sum            'C38 H51 Cl2 N6 O16 V2'
_chemical_formula_weight         1020.63
_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
_cell_angle_alpha                91.023(5)
_cell_angle_beta                 99.366(5)
_cell_angle_gamma                101.768(5)
_cell_formula_units_Z            2
_cell_length_a                   10.740(3)
_cell_length_b                   11.952(3)
_cell_length_c                   17.766(4)
_cell_measurement_reflns_used    1119
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      2.48
_cell_volume                     2199.7(10)
_computing_cell_refinement       'SAINT v.6.36 (Bruker, 2002)'
_computing_data_collection       'SMART v.5.628 (Bruker, 2002)'
_computing_data_reduction        'SAINT v.6.36'
_computing_molecular_graphics    'SHELXTL v.6.10'
_computing_publication_material  'SHELXTL v.6.10'
_computing_structure_refinement  'SHELXTL v.6.10'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source
;
Beamline I711 at the MAX-II storage ring: MAX-Lab, Lund, Sweden
;
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8974
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14402
_diffrn_reflns_theta_full        29.90
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         1.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.05 (Sheldrick, 2002)
Ratio of minimum to maximum apparent transmission: 0.717897
The transmission factors are not real since they include
corrections for beam decay and possibly crystal decay (the
two cannot be distinguished).
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         6271
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2300
_reflns_number_gt                3696
_reflns_number_total             6271
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b901633c.txt
_cod_data_source_block           3
_cod_database_code               7001272