Synthesis and Structure of New Water-Soluble and Stable Tantalum Compound: Ammonium Tetralactatodiperoxo-μ-oxo-ditantalate(V)
Petrykin, Valery; Kakihana, Masato; Yoshioka, Kohtaro; Sasaki, Satoshi; Ueda, Yoshihiro; Tomita, Koji; Nakamura, Yoshiyuki; Shiro, Motoo; Kudo, Akihiko; Inorganic Chemistry 45 (2006) 9251–9256; doi:10.1021/ic060861u

data_4332804
_publ_section_title
;
 Synthesis and Structure of New Water-Soluble and Stable Tantalum
 Compound:&#x00A0; Ammonium Tetralactatodiperoxo-\m-oxo-ditantalate(V)
;
_journal_issue                   23
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9251
_journal_page_last               9256
_journal_paper_doi               10.1021/ic060861u
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C12 H16 O17 Ta2, 4(H4 N), 3(H2 O)'
_chemical_formula_sum            'C12 H38 N4 O20 Ta2'
_chemical_formula_weight         920.34
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 116.30(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.85(2)
_cell_length_b                   9.06(1)
_cell_length_c                   12.32(2)
_cell_measurement_reflns_used    7013
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      3.3
_cell_volume                     1386(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure 2003 (R/MSC, Rigaku, 2003)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure 2003 (R/MSC, Rigaku, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9916
_diffrn_measured_fraction_theta_max 0.9916
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8125
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_exptl_absorpt_coefficient_mu    7.967
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             888.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.16
_refine_diff_density_min         -2.03
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1859 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3990
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                2166
_reflns_number_total             3990
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic060861usup1.cif
_cod_data_source_block           '_kakihana'
_cod_original_cell_volume        1385(3)
_cod_original_formula_sum        'C12 H38 N4 O20 Ta2 '
_cod_database_code               4332804