Spectroscopic and Structural Characterizations of Novel Water-Soluble Tetraperoxo and Diperoxo[polyaminocarboxylato bis(N-oxido)]tantalate(V) Complexes
Daisy Bayot; Bernard Tinant; Michel Devillers; Inorganic Chemistry 43 (2004) 5999–6005; doi:10.1021/ic049639k

data_4311620
_publ_section_title
;
 Spectroscopic and Structural Characterizations of Novel Water-Soluble
 Tetraperoxo and Diperoxo[polyaminocarboxylato bis(N-oxido)]tantalate(V)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5999
_journal_page_last               6005
_journal_paper_doi               10.1021/ic049639k
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C13 H36 N11 O17.68 Ta'
_chemical_formula_weight         810.32
_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                99.79
_cell_angle_beta                 102.85
_cell_angle_gamma                93.66
_cell_formula_units_Z            2
_cell_length_a                   11.091(3)
_cell_length_b                   11.436(3)
_cell_length_c                   11.762(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1425.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  ' MAR345 image plate '
_diffrn_radiation_monochromator  'Zr filtered'
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12664
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.556
_refine_diff_density_min         -2.240
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.0239(12)
_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   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.7819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                5426
_reflns_number_total             5473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049639ksi20040702_113325_2.cif
_cod_data_source_block           DB195
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      ' P -1'
_cod_database_code               4311620