Crystal disassembly and reassembly of heterometallic NiII‒TaVoxalate compounds
Dubraja, Lidija Androš; Matković-Čalogović, Dubravka; Planinić, Pavica; CrystEngComm 17 (2015) 2021–; doi:10.1039/C4CE02516D

data_7219392
_publ_section_title
;
 Crystal disassembly and reassembly of heterometallic NiII--TaVoxalate
 compounds
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              2021
_journal_paper_doi               10.1039/C4CE02516D
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety
'2(C30 H24 N6 Ni), C6 O13 Ta, Cl, 5(H2 O), 7(O)'
_chemical_formula_sum            'C66 H58 Cl N12 Ni2 O25 Ta'
_chemical_formula_weight         1753.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-22T16:47:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-12-23 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9775(2)
_cell_length_b                   21.8439(2)
_cell_length_c                   22.3074(3)
_cell_measurement_reflns_used    16975
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9064
_cell_measurement_theta_min      4.275
_cell_volume                     7298.25(15)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0324210099
_diffrn_orient_matrix_UB_12      -0.0046915119
_diffrn_orient_matrix_UB_13      -0.0226959463
_diffrn_orient_matrix_UB_21      -0.0266562485
_diffrn_orient_matrix_UB_22      -0.0168396992
_diffrn_orient_matrix_UB_23      0.020442826
_diffrn_orient_matrix_UB_31      -0.0219748095
_diffrn_orient_matrix_UB_32      0.0273635909
_diffrn_orient_matrix_UB_33      0.0086820599
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28815
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         4.29
_exptl_absorpt_coefficient_mu    2.13
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.88321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.801
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         16073
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                13045
_reflns_number_total             16073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02516d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7219391--7219393.cif.'
_cod_database_code               7219392