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_7043493
_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         'C45 H69 N2 O3 V, C4 H10 O'
_chemical_formula_sum            'C49 H79 N2 O4 V'
_chemical_formula_weight         811.08
_chemical_properties_physical
'air-sensitive, moisture-sensitive, paramagnetic'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.824(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   19.6630(7)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.88
_cell_volume                     4594.2(3)
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_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)'
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_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0624
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47432
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.260
_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
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_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_recrystallization_method Et2O
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_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   27.90
_exptl_transmission_factor_min   2.88
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8110
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_refine_ls_restrained_S_all      1.059
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_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^)+(0.0635P)^2^+3.1005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6308
_reflns_number_total             8110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01699a2.cif
_cod_data_source_block           3
_cod_database_code               7043493
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              23481