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_7043494
_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_formula_moiety         'C37 H58 Cl N2 O2 V, C4 H10 O'
_chemical_formula_sum            'C41 H68 Cl N2 O3 V'
_chemical_formula_weight         723.36
_chemical_properties_physical
'air-sensitive, moisture-sensitive, paramagnetic'
_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                 100.892(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3330(8)
_cell_length_b                   8.3560(4)
_cell_length_c                   17.3390(9)
_cell_measurement_reflns_used    10777
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.88
_cell_volume                     2039.22(18)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22024
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_min         2.392
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_recrystallization_method EtO2
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 3067 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         10555
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                8284
_reflns_number_total             10555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01699a2.cif
_cod_data_source_block           2
_cod_database_code               7043494
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              28112