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_7219391
_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_formula_moiety
'2(C30 H24 N6 Ni), C6 O13 Ta, Cl, 6(H2 O), 5(O)'
_chemical_formula_sum            'C66 H60 Cl N12 Ni2 O24 Ta'
_chemical_formula_weight         1739.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-15T15:51:06-00:00
_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                 101.2320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8900(3)
_cell_length_b                   13.37190(10)
_cell_length_c                   23.1855(3)
_cell_measurement_reflns_used    30306
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.771
_cell_measurement_theta_min      3.774
_cell_volume                     7264.85(14)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0614041
_diffrn_orient_matrix_UB_12      0.0102085
_diffrn_orient_matrix_UB_13      -0.0352546
_diffrn_orient_matrix_UB_21      0.0218845
_diffrn_orient_matrix_UB_22      -0.0153086
_diffrn_orient_matrix_UB_23      -0.0576488
_diffrn_orient_matrix_UB_31      -0.0084604
_diffrn_orient_matrix_UB_32      -0.1137512
_diffrn_orient_matrix_UB_33      0.0046114
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39712
_diffrn_reflns_theta_full        65
_diffrn_reflns_theta_max         65
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    4.383
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.30906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.59
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.934
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         12352
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.05
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+18.3630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                11711
_reflns_number_total             12352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02516d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7219391--7219393.cif.'
_cod_database_code               7219391