New Fe-Ta and Co-Ta oxalate complexes: structural characterization and thermal behaviour – formation of mixed-metal oxides
Androš, Lidija; Juric, Marijana; Popović, Jasminka; Planinic, Pavica; RSC Advances  (2014) –; doi:10.1039/C4RA05855K

data_7217311
_publ_section_title
;
 New Fe-Ta and Co-Ta oxalate complexes: structural characterization and
 thermal behaviour -- formation of mixed-metal oxides
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA05855K
_journal_year                    2014
_chemical_formula_sum            'C44 H31 Co N6 O14 Ta'
_chemical_formula_weight         1107.63
_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_date             2014-07-16T12:40:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.147(5)
_cell_angle_beta                 92.156(5)
_cell_angle_gamma                109.194(5)
_cell_formula_units_Z            2
_cell_length_a                   11.538(5)
_cell_length_b                   12.683(5)
_cell_length_c                   15.657(5)
_cell_measurement_reflns_used    14957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9205
_cell_measurement_theta_min      3.0045
_cell_volume                     2031.0(14)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0881678
_diffrn_orient_matrix_UB_12      -0.1166826
_diffrn_orient_matrix_UB_13      -0.0716441
_diffrn_orient_matrix_UB_21      0.0453824
_diffrn_orient_matrix_UB_22      0.0483899
_diffrn_orient_matrix_UB_23      -0.0763666
_diffrn_orient_matrix_UB_31      0.1032171
_diffrn_orient_matrix_UB_32      -0.0528599
_diffrn_orient_matrix_UB_33      -0.0049407
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54179
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20185
_diffrn_reflns_theta_full        76.1
_diffrn_reflns_theta_max         76.1
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    8.781
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.58261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.948
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.035
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.2474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                7551
_reflns_number_total             8389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra05855k2.cif
_cod_data_source_block           new
_cod_database_code               7217311