Coordination of o-benzosemiquinonate, o-iminobenzosemiquinonate, 4,4′-di-tert-butyl-2,2′-bipyridine and 1,10-phenanthroline anion radicals to oxidovanadium(iv)
Shit, Madhusudan; Maity, Suvendu; Bera, Sachinath; Weyhermüller, Thomas; Ghosh, Prasanta; New J. Chem. 40 (2016) 10305–; doi:10.1039/C6NJ02220K

data_7055827
_publ_section_title
;
 Coordination of o-benzosemiquinonate, o-iminobenzosemiquinonate,
 4,4&#x2032;-di-tert-butyl-2,2&#x2032;-bipyridine and 1,10-phenanthroline
 anion radicals to oxidovanadium(iv)
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              10305
_journal_paper_doi               10.1039/C6NJ02220K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C25 H18 N5 O5 V'
_chemical_formula_sum            'C25 H18 N5 O5 V'
_chemical_formula_weight         519.38
_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-2013
_audit_update_record
;
2016-10-18 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8584(5)
_cell_length_b                   16.1145(6)
_cell_length_c                   22.9607(9)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.63
_cell_volume                     5127.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            78927
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.924
_diffrn_source                   Mo
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 3537 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         11180
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0413P)^2^+1.4506P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8993
_reflns_number_total             11180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02220k2.cif
_cod_data_source_block           3_SQ
_cod_depositor_comments
'Adding full bibliography for 7055826--7055828.cif.'
_cod_database_code               7055827
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2013-2
_shelx_res_checksum              65786
_shelx_fab_checksum              76158