A novel octanuclear nickel(II)‒molybdenum(VI) heterometallic cluster based on the salicylhydroxamate ligand
Dou, Ming-Yu; Lu, Jing; Acta Crystallographica Section C 72 (2016) 161–165; doi:10.1107/S2053229616000243

data_2020405
_publ_section_title
;
 A novel octanuclear nickel(II)--molybdenum(VI) heterometallic cluster
 based on the salicylhydroxamate ligand
;
_journal_coeditor_code           QS3051
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              161
_journal_page_last               165
_journal_paper_doi               10.1107/S2053229616000243
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Mo2 Ni6 (C7 H4 N O3)2 (C2 H3 O2)4 O6 (O H)2 (C5 H5 N)8], H2 O'
_chemical_formula_moiety         'C31 H32 Mo1 N5  Ni3 O11.5'
_chemical_formula_sum            'C62 H64 Mo2 N10 Ni6 O23'
_chemical_formula_weight         1861.38
_chemical_name_systematic
'Di-\m~3~-acetato-di-\m~2~-acetato-di-\m~3~-hydroxido-di-\m~3~-oxido-tetraoxidooctakis(pyridine-\k<i>N</i>)bis(\m~5~-salicylhydroxamato)hexanickel(II)dimolybdenum(VI) dihydrate'
_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_method           SHELXL-97
_cell_angle_alpha                111.551(7)
_cell_angle_beta                 95.979(7)
_cell_angle_gamma                98.854(6)
_cell_formula_units_Z            1
_cell_length_a                   10.5079(8)
_cell_length_b                   12.7461(9)
_cell_length_c                   14.5850(13)
_cell_measurement_reflns_used    6238
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.74
_cell_volume                     1767.6(3)
_computing_cell_refinement
;
SMART (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11408
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.987
_exptl_absorpt_correction_T_max  0.5871
_exptl_absorpt_correction_T_min  0.4366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                4334
_reflns_number_total             6238
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3051sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020405.cif.'
_cod_original_cell_volume        1767.6(2)
_cod_database_code               2020405
_cod_database_fobs_code          2020405