Solid State and Aqueous Solution Characterization of Rectangular Tetranuclear VIV/V-p-Semiquinonate/Hydroquinonate Complexes Exhibiting a Proton Induced Electron Transfer
Chryssoula Drouza; Anastasios D. Keramidas; Inorganic Chemistry 47 (2008) 7211–7224; doi:10.1021/ic800569t

data_4305583
_publ_section_title
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Solid State and Aqueous Solution Characterization of Rectangular
Tetranuclear VIV/V-p-Semiquinonate/Hydroquinonate Complexes Exhibiting a
Proton Induced Electron Transfer
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7211
_journal_page_last               7224
_journal_paper_doi               10.1021/ic800569t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C37 H66 N13 Na O34 V4'
_chemical_formula_weight         1463.78
_chemical_name_systematic
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 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 101.404(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3035(11)
_cell_length_b                   10.9657(5)
_cell_length_c                   28.3894(15)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1288
_cell_measurement_theta_min      3.1540
_cell_volume                     5890.7(5)
_computing_cell_refinement
;
'Mon Jun 05 18:53:59 2006'
;
_computing_data_collection
;
'Mon Jun 05 18:53:59 2006'
;
_computing_data_reduction
;
'Mon Jun 05 18:53:59 2006'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            87133
_diffrn_reflns_theta_full        31.28
_diffrn_reflns_theta_max         31.28
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.94139
_exptl_absorpt_correction_T_min  0.87518
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Mon Jun 05 18:53:59 2006'
;
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.14090
_exptl_crystal_size_mid          0.09630
_exptl_crystal_size_min          0.04378
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00000(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         18002
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          5.486
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                10604
_reflns_number_total             18002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800569t-file002_3.cif
_cod_data_source_block           vbiqna26
_cod_database_code               4305583