Formations of mixed-valence oxovanadiumV,IV citrates and homocitrate with N-heterocycle chelated ligand.
Chen, Can-Yu; Zhou, Zhao-Hui; Chen, Hong-Bin; Huang, Pei-Qiang; Tsai, Khi-Rui; Chow, Yuan L.; Inorganic chemistry 47 (2008) 8714–8720; doi:10.1021/ic800553p

data_4338707
_publ_section_title
;
 Formations of mixed-valence oxovanadiumV,IV citrates and homocitrate with
 N-heterocycle chelated ligand.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8714
_journal_page_last               8720
_journal_paper_doi               10.1021/ic800553p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C84 H82 N12 O32 V4'
_chemical_formula_weight         1975.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.442(3)
_cell_angle_beta                 105.709(3)
_cell_angle_gamma                115.186(3)
_cell_formula_units_Z            1
_cell_length_a                   13.0831(5)
_cell_length_b                   13.0996(4)
_cell_length_c                   14.8791(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2072.48(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker Apex CCD diffractomer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16986
_diffrn_reflns_theta_full        60.92
_diffrn_reflns_theta_max         60.92
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    4.507
_exptl_absorpt_correction_T_max  0.4976
_exptl_absorpt_correction_T_min  0.3870
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         6105
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.4305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                5492
_reflns_number_total             6105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cif2.cif
_cod_data_source_block           sad
_cod_original_cell_volume        2072.48(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338707