Radical reactions of diamine bis(phenolate) vanadium(III) complexes. Solid state binding of O2 to form a vanadium(V) peroxo complex
Barroso, Sonia; Coelho, Ana M.; Adão, Pedro; Calhorda, Maria Jose; Martins, Ana M.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01699A

data_7043497
_publ_section_title
;
 Radical reactions of diamine bis(phenolate) vanadium(III) complexes.
 Solid state binding of O2 to form a vanadium(V) peroxo complex
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01699A
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C40 H65 N2 O4 V'
_chemical_formula_sum            'C40 H65 N2 O4 V'
_chemical_formula_weight         688.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.875(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5180(11)
_cell_length_b                   23.5210(10)
_cell_length_c                   21.8270(10)
_cell_measurement_reflns_used    8434
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.19
_cell_volume                     7823.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48637
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.108
_diffrn_reflns_theta_max         25.108
_diffrn_reflns_theta_min         1.979
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 6772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1713
_refine_ls_number_reflns         24927
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                18919
_reflns_number_total             24927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01699a2.cif
_cod_data_source_block           8
_cod_database_code               7043497
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              91301
_shelx_fab_checksum              69947