Homo- and Heterobimetallic NiobiumV and TantalumV Peroxo-tartrate Complexes and Their Use as Molecular Precursors for Nb-Ta Mixed Oxides
Daisy Bayot; Bernard Tinant; Michel Devillers; Inorganic Chemistry 44 (2005) 1554–1562; doi:10.1021/ic0484250

data_4308654
_publ_contact_author_name        'Michel Devillers'
_publ_section_title
;
Homo- and Heterobimetallic NiobiumV and TantalumV Peroxo-tartrate Complexes
and Their Use as Molecular Precursors for Nb-Ta Mixed Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1554
_journal_page_last               1562
_journal_paper_doi               10.1021/ic0484250
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C6.5 H24.5 N7.5 Nb O14'
_chemical_formula_weight         524.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.747(7)
_cell_length_b                   15.608(5)
_cell_length_c                   12.295(4)
_cell_measurement_temperature    110(2)
_cell_volume                     3789(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  ' MAR345 image plate '
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24145
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.0099(6)
_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   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+39.2658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                3825
_reflns_number_total             3879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484250si20041110_015529_2.cif
_cod_data_source_block           db102bt_1b
_cod_original_sg_symbol_H-M      ' C 2/c '
_cod_original_formula_sum        'C6.50 H24.50 N7.50 Nb O14'
_cod_database_code               4308654