Synthesis and crystal structure of bis[μ-<i>N</i>,<i>N</i>-bis(2-aminoethyl)ethane-1,2-diamine]bis[<i>N</i>,<i>N</i>-bis(2-aminoethyl)ethane-1,2-diamine]-μ~4~-oxido-hexa-μ~3~-oxido-octa-μ~2~-oxido-tetraoxidotetranickel(II)hexatantalum(V) nonadecahydrate
Krause, Dana-Céline; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section E 77 (2021) 1253–1257; doi:10.1107/S2056989021011531

data_2243988
_publ_section_title
;
 Synthesis and crystal structure of
 bis[\m-<i>N</i>,<i>N</i>-bis(2-aminoethyl)ethane-1,2-diamine]bis[<i>N</i>,<i>N</i>-bis(2-aminoethyl)ethane-1,2-diamine]-\m~4~-oxido-hexa-\m~3~-oxido-octa-\m~2~-oxido-tetraoxidotetranickel(II)hexatantalum(V)
 nonadecahydrate
;
_journal_coeditor_code           WM5616
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1253
_journal_page_last               1257
_journal_paper_doi               10.1107/S2056989021011531
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ni4 Ta6 O19 (C6 H18 N4)4], 19H2 O'
_chemical_formula_moiety         'C24 H72 N16 Ni4 O19 Ta6, 19(H2 O)'
_chemical_formula_sum            'C24 H110 N16 Ni4 O38 Ta6'
_chemical_formula_weight         2551.81
_chemical_name_systematic
'Bis[\m-<i>N</i>,<i>N</i>-bis(2-aminoethyl)ethane-1,2-diamine]bis[<i>N</i>,<i>N</i>-bis(2-aminoethyl)ethane-1,2-diamine]-\m~4~-oxido-hexa-\m~3~-oxido-octa-\m~2~-oxido-tetraoxidotetranickel(II)hexatantalum(V) nonadecahydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                73.7480(10)
_cell_angle_beta                 80.9180(10)
_cell_angle_gamma                80.8420(10)
_cell_formula_units_Z            1
_cell_length_a                   10.50330(10)
_cell_length_b                   12.0980(2)
_cell_length_c                   13.8640(2)
_cell_measurement_reflns_used    37095
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      34.0390
_cell_measurement_theta_min      2.3610
_cell_volume                     1657.75(4)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.878
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.062
_exptl_absorpt_correction_T_max  0.69366
_exptl_absorpt_correction_T_min  0.68613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    2.556
_exptl_crystal_description       needle
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.014
_exptl_crystal_size_rad          0.023
_refine_diff_density_max         2.828
_refine_diff_density_min         -1.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+3.1986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                7404
_reflns_number_total             7897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5616sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1657.76(4)
_cod_database_code               2243988
_shelx_estimated_absorpt_t_min   0.373
_shelx_estimated_absorpt_t_max   0.861
_shelx_hkl_checksum              82084
_shelx_res_checksum              76125
_cod_database_fobs_code 2243988