An inorganic–organic hybrid supramolecular framework based on the γ-[Mo~8~O~26~]^4{-^} cluster and cobalt complex of aspartic acid: X-ray structure and DFT study
Tahmasebi, Morteza; Mirzaei, Masoud; Eshtiagh-Hosseini, Hossein; Mague, Joel T.; Bauzá, Antonio; Frontera, Antonio; Acta Crystallographica Section C 75 (2019) 469–477; doi:10.1107/S2053229619004029

data_2021559
_publ_section_title
;
 An inorganic--organic hybrid supramolecular framework based on the
 \g-[Mo~8~O~26~]^4{-^} cluster and cobalt complex of aspartic acid: X-ray
 structure and DFT study
;
_journal_coeditor_code           JX3036
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              469
_journal_page_last               477
_journal_paper_doi               10.1107/S2053229619004029
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Co2 (C4 H6 N1 O4)2 (Mo8 O26) (H2 O)10], 4H2 O'
_chemical_formula_moiety         'C8 H32 Co2 Mo8 N2 O44, 4(H2 O)'
_chemical_formula_sum            'C8 H40 Co2 Mo8 N2 O48'
_chemical_formula_weight         1817.80
_chemical_name_systematic
;
[Pentaaquacobalt(III)]-\m-aspartato-[\g-octamolybdato]-\m-aspartato-
[pentaaquacobalt(III)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 110.602(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.507(4)
_cell_length_b                   12.853(5)
_cell_length_c                   15.795(6)
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      29.9097
_cell_measurement_theta_min      2.4672
_cell_volume                     2186.7(14)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Bruker, 2016) and
DIAMOND (Macrae <i>et al.</i>,  2008)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41259
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         30.099
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.086
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    2.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.356
_refine_diff_density_min         -1.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0498P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                5156
_reflns_number_total             6170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3036sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2186.6(13)
_cod_database_code               2021559
_cod_database_fobs_code          2021559
_shelx_estimated_absorpt_t_min   0.460
_shelx_estimated_absorpt_t_max   0.728
_shelx_hkl_checksum              23068
_shelx_res_checksum              71489
_shelx_fab_checksum              3723