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_7043492
_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         'C37 H58 Cl N2 O3 V'
_chemical_formula_sum            'C37 H58 Cl N2 O3 V'
_chemical_formula_weight         665.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.997(2)
_cell_length_b                   12.560(3)
_cell_length_c                   28.755(6)
_cell_measurement_reflns_used    1373
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.75
_cell_measurement_theta_min      2.60
_cell_volume                     3610.5(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.996
_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  0.1644
_diffrn_reflns_av_unetI/netI     0.1487
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            39525
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.153
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_recrystallization_method pentane
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1270 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3895
_reflns_number_total             6353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01699a2.cif
_cod_data_source_block           6
_cod_original_cell_volume        3610.5(13)
_cod_database_code               7043492
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              5936