<i>cyclo</i>-Tetra-μ-oxido-tetrakis[(acetylacetonato-κ^2^<i>O</i>,<i>O</i>')bis(ethanolato-κ<i>O</i>)niobium(V)]
Herbst, Leandra; Visser, Hendrik G.; Roodt, Andreas; Muller, Theunis J.; Acta Crystallographica Section E 67 (2011) m1669–m1670; doi:10.1107/S1600536811044138

data_2232551
_publ_section_title
;
 <i>cyclo</i>-Tetra-\m-oxido-tetrakis[(acetylacetonato-\k^2^<i>O</i>,<i>O</i>')bis(ethanolato-\k<i>O</i>)niobium(V)]
;
_journal_coeditor_code           BG2426
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1669
_journal_page_last               m1670
_journal_paper_doi               10.1107/S1600536811044138
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Nb4 (C2 H5 O)8 (C5 H7 O2)4 O4]'
_chemical_formula_moiety         'C36 H68 Nb4 O20'
_chemical_formula_sum            'C36 H68 Nb4 O20'
_chemical_formula_weight         1192.54
_chemical_name_systematic
;
<i>cyclo</i>-Tetra-\m-oxido-tetrakis[(acetylacetonato-
\k^2^<i>O</i>,<i>O</i>')bis(ethanolato-\k<i>O</i>)niobium(V)]
;
_space_group_IT_number           14
_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_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 136.982(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.907(5)
_cell_length_b                   12.662(5)
_cell_length_c                   21.354(5)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.68
_cell_volume                     2565.3(16)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker X8 APEXII 4K Kappa CCD
;
_diffrn_measurement_method       '\f and \w 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  0.0322
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42149
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.432
_refine_diff_density_min         -1.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+4.1146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                5355
_reflns_number_total             6191
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2426.cif
_cod_data_source_block           I
_cod_original_cell_volume        2565.4(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C36 H68 Nb4 O20 '
_cod_database_code               2232551
_cod_database_fobs_code          2232551