A series of compounds containing various (oxalato)tantalate(v) complex anions ‒ synthesis, properties and the mixed-metal oxide formation via thermal decomposition
Androš, Lidija; Matković-Čalogović, Dubravka; Planinić, Pavica; CrystEngComm 15 (2013) 533–; doi:10.1039/c2ce26391b

data_7208989
_publ_section_title
;
 A series of compounds containing various (oxalato)tantalate(v) complex
 anions -- synthesis, properties and the mixed-metal oxide formation via
 thermal decomposition
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              533
_journal_paper_doi               10.1039/c2ce26391b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C56 H46 N8 Ni O22.5 Ta'
_chemical_formula_weight         1430.67
_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             2012-05-24T16:43:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                76.487(3)
_cell_angle_beta                 86.836(3)
_cell_angle_gamma                72.440(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0511(4)
_cell_length_b                   14.9625(5)
_cell_length_c                   16.2348(5)
_cell_measurement_reflns_used    16714
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.6271
_cell_measurement_theta_min      3.7371
_cell_volume                     2713.33(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0188867663
_diffrn_orient_matrix_UB_12      0.0405181828
_diffrn_orient_matrix_UB_13      0.0184622843
_diffrn_orient_matrix_UB_21      0.0345983218
_diffrn_orient_matrix_UB_22      -0.0267855273
_diffrn_orient_matrix_UB_23      0.0367063281
_diffrn_orient_matrix_UB_31      0.0476515942
_diffrn_orient_matrix_UB_32      0.0158032193
_diffrn_orient_matrix_UB_33      -0.0181752462
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29028
_diffrn_reflns_theta_full        29
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    2.457
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.86511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1438
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.746
_refine_diff_density_min         -2.344
_refine_diff_density_rms         0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         15253
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+23.7529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                12398
_reflns_number_total             15253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26391b.txt
_cod_data_source_block           1
_cod_original_cell_volume        2713.33(15)
_cod_original_formula_sum        'C56 H46 N8 Ni O22.50 Ta'
_cod_database_code               7208989