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_4311619
_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            'C3 H18 N9 O8 Ta'
_chemical_formula_weight         489.21
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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                90.00
_cell_angle_beta                 103.08(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.572(3)
_cell_length_b                   10.327(5)
_cell_length_c                   8.874(3)
_cell_measurement_temperature    293(2)
_cell_volume                     765.2(5)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  ' MAR345 image plate '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9258
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    7.236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         3.139
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.089(18)
_refine_ls_extinction_coef       0.081(5)
_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   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1745
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                1700
_reflns_number_total             1745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049639ksi20040702_113325_1.cif
_cod_data_source_block           SD23
_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 n '
_cod_database_code               4311619