#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/25/2232551.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2232551
loop_
_publ_author_name
'Herbst, Leandra'
'Visser, Hendrik G.'
'Roodt, Andreas'
'Muller, Theunis J.'
_publ_section_title
;
 cyclo-Tetra-μ-oxido-tetrakis[(acetylacetonato-κ²O,O')bis(ethanolato-κO)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
;
cyclo-Tetra-μ-oxido-tetrakis[(acetylacetonato-
κ²O,O')bis(ethanolato-κO)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       'φ and ω 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/[σ²(Fo²)+(0.0310P)²+4.1146P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4871(3) 0.5567(3) 0.2203(2) 0.0376(6) Uani d . 1 . .
C C2 0.5266(3) 0.6468(3) 0.2724(2) 0.0440(7) Uani d . 1 . .
H H2 0.4807 0.7098 0.2414 0.053 Uiso calc R 1 . .
C C3 0.6286(3) 0.6484(2) 0.3664(2) 0.0377(6) Uani d . 1 . .
C C4 0.3652(4) 0.5634(3) 0.1170(2) 0.0635(11) Uani d . 1 . .
H H4A 0.3966 0.544 0.0908 0.095 Uiso calc R 1 . .
H H4B 0.3295 0.6344 0.0993 0.095 Uiso calc R 1 . .
H H4C 0.2918 0.5161 0.0952 0.095 Uiso calc R 1 . .
C C5 0.6564(5) 0.7475(3) 0.4162(3) 0.0597(10) Uani d . 1 . .
H H5A 0.6275 0.7376 0.445 0.09 Uiso calc R 1 . .
H H5B 0.6043 0.8049 0.3732 0.09 Uiso calc R 1 . .
H H5C 0.7553 0.7635 0.462 0.09 Uiso calc R 1 . .
C C6 0.4762(4) 0.3502(4) 0.3446(3) 0.0611(10) Uani d . 1 . .
H H6A 0.4608 0.283 0.3581 0.073 Uiso calc R 1 . .
H H6B 0.4148 0.3529 0.2791 0.073 Uiso calc R 1 . .
C C7 0.4382(5) 0.4360(5) 0.3696(4) 0.0893(17) Uani d . 1 . .
H H7A 0.3415 0.4284 0.336 0.134 Uiso calc R 1 . .
H H7B 0.4506 0.5027 0.3548 0.134 Uiso calc R 1 . .
H H7C 0.4976 0.4331 0.4342 0.134 Uiso calc R 1 . .
C C8 0.7632(4) 0.2881(3) 0.2822(3) 0.0485(8) Uani d U 1 . .
H H8A 0.8199 0.3423 0.2892 0.058 Uiso calc R 1 A 3
H H8B 0.6702 0.2895 0.2191 0.058 Uiso calc R 1 A 3
C C10 1.0999(3) 0.4854(3) 0.3539(2) 0.0402(7) Uani d . 1 . .
C C11 1.1829(4) 0.5716(3) 0.3770(3) 0.0494(8) Uani d . 1 . .
H H11 1.2651 0.5589 0.3937 0.059 Uiso calc R 1 . .
C C12 1.1506(4) 0.6763(3) 0.3769(2) 0.0468(8) Uani d . 1 . .
C C13 1.1348(4) 0.3772(3) 0.3489(3) 0.0571(9) Uani d . 1 . .
H H13A 1.0784 0.36 0.2861 0.086 Uiso calc R 1 . .
H H13B 1.116 0.3276 0.3729 0.086 Uiso calc R 1 . .
H H13C 1.2328 0.3739 0.3844 0.086 Uiso calc R 1 . .
C C14 1.2474(5) 0.7644(4) 0.4018(3) 0.0672(12) Uani d . 1 . .
H H14A 1.3141 0.7374 0.4039 0.101 Uiso calc R 1 . .
H H14B 1.2967 0.7925 0.4609 0.101 Uiso calc R 1 . .
H H14C 1.1926 0.8194 0.3566 0.101 Uiso calc R 1 . .
C C15 0.9542(5) 0.8296(3) 0.4372(3) 0.0672(11) Uani d . 1 . .
H H15A 1.0526 0.81 0.4879 0.081 Uiso calc R 1 . .
H H15B 0.921 0.8503 0.4625 0.081 Uiso calc R 1 . .
C C16 0.9434(7) 0.9182(4) 0.3908(4) 0.103(2) Uani d . 1 . .
H H16A 0.8466 0.9396 0.3416 0.155 Uiso calc R 1 . .
H H16B 0.9777 0.8989 0.3665 0.155 Uiso calc R 1 . .
H H16C 0.9986 0.9755 0.4333 0.155 Uiso calc R 1 . .
O O1 0.81776(19) 0.51714(15) 0.36184(13) 0.0296(4) Uani d . 1 B .
O O2 0.54526(19) 0.46715(16) 0.25306(13) 0.0342(4) Uani d . 1 C .
O O3 0.7048(2) 0.56870(15) 0.41852(13) 0.0323(4) Uani d . 1 C .
O O4 0.6178(2) 0.35591(17) 0.39197(14) 0.0351(4) Uani d . 1 C .
O O5 0.90700(18) 0.40537(14) 0.51497(12) 0.0290(4) Uani d . 1 . .
O O6 0.7517(2) 0.31023(15) 0.34129(13) 0.0322(4) Uani d U 1 C .
O O7 0.9881(2) 0.49253(17) 0.33447(14) 0.0362(4) Uani d . 1 . .
O O8 1.0433(2) 0.70416(18) 0.35616(16) 0.0434(5) Uani d . 1 . .
O O9 0.8765(2) 0.74043(15) 0.38001(14) 0.0386(5) Uani d . 1 . .
O O10 0.7637(2) 0.62579(19) 0.22326(14) 0.0458(5) Uani d U 1 . .
Nb Nb1 0.74205(2) 0.422519(18) 0.394088(15) 0.02353(7) Uani d . 1 . .
Nb Nb2 0.90559(2) 0.611158(19) 0.352545(16) 0.02815(7) Uani d . 1 . .
C C17A 0.7186(18) 0.6351(11) 0.1421(9) 0.075(4) Uani d PDU 0.399(12) B 1
H H17A 0.7289 0.7091 0.1364 0.09 Uiso calc PR 0.399(12) B 1
H H17B 0.618 0.6213 0.0954 0.09 Uiso calc PR 0.399(12) B 1
C C18A 0.7686(18) 0.5806(10) 0.1159(9) 0.088(5) Uani d PDU 0.399(12) B 1
H H18A 0.6919 0.5624 0.0521 0.132 Uiso calc PR 0.399(12) B 1
H H18B 0.8142 0.5173 0.1519 0.132 Uiso calc PR 0.399(12) B 1
H H18C 0.8352 0.6235 0.1253 0.132 Uiso calc PR 0.399(12) B 1
C C17B 0.7207(17) 0.5822(11) 0.1469(7) 0.145(7) Uani d PDU 0.601(12) B 2
H H17C 0.7969 0.5989 0.1545 0.174 Uiso calc PR 0.601(12) B 2
H H17D 0.7274 0.5067 0.1572 0.174 Uiso calc PR 0.601(12) B 2
C C18B 0.6150(15) 0.5917(14) 0.0646(7) 0.184(8) Uani d PDU 0.601(12) B 2
H H18D 0.5957 0.6654 0.049 0.276 Uiso calc PR 0.601(12) B 2
H H18E 0.5366 0.5595 0.0484 0.276 Uiso calc PR 0.601(12) B 2
H H18F 0.6292 0.5578 0.0317 0.276 Uiso calc PR 0.601(12) B 2
C C9A 0.828(3) 0.1850(12) 0.3022(14) 0.068(4) Uani d PU 0.53(5) C 3
H H9A1 0.9206 0.1841 0.3642 0.102 Uiso calc PR 0.53(5) C 3
H H9A2 0.8335 0.1718 0.2608 0.102 Uiso calc PR 0.53(5) C 3
H H9A3 0.7713 0.1312 0.2948 0.102 Uiso calc PR 0.53(5) C 3
C C9B 0.885(4) 0.218(3) 0.330(2) 0.076(7) Uani d PU 0.47(5) C 4
H H9B1 0.9691 0.2514 0.3856 0.114 Uiso calc PR 0.47(5) C 4
H H9B2 0.8959 0.2052 0.2909 0.114 Uiso calc PR 0.47(5) C 4
H H9B3 0.8706 0.1524 0.3442 0.114 Uiso calc PR 0.47(5) C 4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 C1 C2 . . 124.8(3)
O2 C1 C4 . . 116.1(3)
C2 C1 C4 . . 119.1(3)
C3 C2 C1 . . 124.3(3)
C3 C2 H2 . . 117.9
C1 C2 H2 . . 117.9
O3 C3 C2 . . 124.9(3)
O3 C3 C5 . . 114.9(3)
C2 C3 C5 . . 120.3(3)
C1 C4 H4A . . 109.5
C1 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C1 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C3 C5 H5A . . 109.5
C3 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C3 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
O4 C6 C7 . . 112.7(3)
O4 C6 H6A . . 109.1
C7 C6 H6A . . 109.1
O4 C6 H6B . . 109.1
C7 C6 H6B . . 109.1
H6A C6 H6B . . 107.8
C6 C7 H7A . . 109.5
C6 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
C6 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
O6 C8 C9A . . 111.3(7)
O6 C8 C9B . . 109.2(9)
O6 C8 H8A . . 109.4
C9A C8 H8A . . 109.4
C9B C8 H8A . . 85.6
O6 C8 H8B . . 109.4
C9A C8 H8B . . 109.4
C9B C8 H8B . . 131.4
H8A C8 H8B . . 108
O7 C10 C11 . . 123.6(3)
O7 C10 C13 . . 115.1(3)
C11 C10 C13 . . 121.4(3)
C10 C11 C12 . . 124.2(3)
C10 C11 H11 . . 117.9
C12 C11 H11 . . 117.9
O8 C12 C11 . . 124.2(3)
O8 C12 C14 . . 115.9(4)
C11 C12 C14 . . 119.8(3)
C10 C13 H13A . . 109.5
C10 C13 H13B . . 109.5
H13A C13 H13B . . 109.5
C10 C13 H13C . . 109.5
H13A C13 H13C . . 109.5
H13B C13 H13C . . 109.5
C12 C14 H14A . . 109.5
C12 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C12 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
O9 C15 C16 . . 113.7(4)
O9 C15 H15A . . 108.8
C16 C15 H15A . . 108.8
O9 C15 H15B . . 108.8
C16 C15 H15B . . 108.8
H15A C15 H15B . . 107.7
C15 C16 H16A . . 109.5
C15 C16 H16B . . 109.5
H16A C16 H16B . . 109.5
C15 C16 H16C . . 109.5
H16A C16 H16C . . 109.5
H16B C16 H16C . . 109.5
Nb2 O1 Nb1 . . 170.20(11)
C1 O2 Nb1 . . 129.84(19)
C3 O3 Nb1 . . 132.58(19)
C6 O4 Nb1 . . 144.2(2)
Nb1 O5 Nb2 . 3_766 177.29(11)
C8 O6 Nb1 . . 142.3(2)
C10 O7 Nb2 . . 133.4(2)
C12 O8 Nb2 . . 129.8(2)
C15 O9 Nb2 . . 139.6(2)
C17A O10 Nb2 . . 153.1(7)
C17B O10 Nb2 . . 140.8(5)
O5 Nb1 O6 . . 101.06(9)
O5 Nb1 O4 . . 99.35(9)
O6 Nb1 O4 . . 96.49(9)
O5 Nb1 O1 . . 97.11(8)
O6 Nb1 O1 . . 87.74(8)
O4 Nb1 O1 . . 161.86(8)
O5 Nb1 O3 . . 92.12(8)
O6 Nb1 O3 . . 163.72(8)
O4 Nb1 O3 . . 90.68(9)
O1 Nb1 O3 . . 81.13(8)
O5 Nb1 O2 . . 171.80(8)
O6 Nb1 O2 . . 86.33(8)
O4 Nb1 O2 . . 83.19(9)
O1 Nb1 O2 . . 79.48(8)
O3 Nb1 O2 . . 80.01(8)
O1 Nb2 O9 . . 102.78(9)
O1 Nb2 O10 . . 98.99(10)
O9 Nb2 O10 . . 97.89(10)
O1 Nb2 O5 . 3_766 93.52(8)
O9 Nb2 O5 . 3_766 90.28(8)
O10 Nb2 O5 . 3_766 163.13(9)
O1 Nb2 O7 . . 93.03(8)
O9 Nb2 O7 . . 162.89(9)
O10 Nb2 O7 . . 85.90(10)
O5 Nb2 O7 3_766 . 82.15(8)
O1 Nb2 O8 . . 169.64(8)
O9 Nb2 O8 . . 84.44(9)
O10 Nb2 O8 . . 87.20(10)
O5 Nb2 O8 3_766 . 78.88(8)
O7 Nb2 O8 . . 79.06(9)
O10 C17A C18A . . 126.0(13)
O10 C17A H17A . . 105.8
C18A C17A H17A . . 105.8
O10 C17A H17B . . 105.8
C18A C17A H17B . . 105.8
H17A C17A H17B . . 106.2
C18B C17B O10 . . 133.5(13)
C18B C17B H17C . . 103.8
O10 C17B H17C . . 103.8
C18B C17B H17D . . 103.8
O10 C17B H17D . . 103.8
H17C C17B H17D . . 105.4
C17B C18B H18D . . 109.5
C17B C18B H18E . . 109.5
H18D C18B H18E . . 109.5
C17B C18B H18F . . 109.5
H18D C18B H18F . . 109.5
H18E C18B H18F . . 109.5
C8 C9A H9A1 . . 109.5
C8 C9A H9A2 . . 109.5
C8 C9A H9A3 . . 109.5
C8 C9B H9B1 . . 109.5
C8 C9B H9B2 . . 109.5
C8 C9B H9B3 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O2 . 1.266(4)
C1 C2 . 1.396(5)
C1 C4 . 1.509(4)
C2 C3 . 1.370(4)
C2 H2 . 0.93
C3 O3 . 1.286(3)
C3 C5 . 1.501(4)
C4 H4A . 0.96
C4 H4B . 0.96
C4 H4C . 0.96
C5 H5A . 0.96
C5 H5B . 0.96
C5 H5C . 0.96
C6 O4 . 1.412(4)
C6 C7 . 1.468(6)
C6 H6A . 0.97
C6 H6B . 0.97
C7 H7A . 0.96
C7 H7B . 0.96
C7 H7C . 0.96
C8 O6 . 1.411(4)
C8 C9A . 1.460(15)
C8 C9B . 1.476(16)
C8 H8A . 0.97
C8 H8B . 0.97
C10 O7 . 1.287(4)
C10 C11 . 1.390(5)
C10 C13 . 1.484(5)
C11 C12 . 1.398(5)
C11 H11 . 0.93
C12 O8 . 1.258(4)
C12 C14 . 1.514(5)
C13 H13A . 0.96
C13 H13B . 0.96
C13 H13C . 0.96
C14 H14A . 0.96
C14 H14B . 0.96
C14 H14C . 0.96
C15 O9 . 1.415(4)
C15 C16 . 1.429(6)
C15 H15A . 0.97
C15 H15B . 0.97
C16 H16A . 0.96
C16 H16B . 0.96
C16 H16C . 0.96
O1 Nb2 . 1.8173(19)
O1 Nb1 . 2.0196(19)
O2 Nb1 . 2.197(2)
O3 Nb1 . 2.089(2)
O4 Nb1 . 1.894(2)
O5 Nb1 . 1.8204(19)
O5 Nb2 3_766 2.0145(19)
O6 Nb1 . 1.8793(19)
O7 Nb2 . 2.090(2)
O8 Nb2 . 2.201(2)
O9 Nb2 . 1.880(2)
O10 C17A . 1.349(12)
O10 C17B . 1.377(11)
O10 Nb2 . 1.893(2)
Nb2 O5 3_766 2.0145(19)
C17A C18A . 1.357(15)
C17A H17A . 0.97
C17A H17B . 0.97
C18A H18A . 0.96
C18A H18B . 0.96
C18A H18C . 0.96
C17B C18B . 1.219(12)
C17B H17C . 0.97
C17B H17D . 0.97
C18B H18D . 0.96
C18B H18E . 0.96
C18B H18F . 0.96
C9A H9A1 . 0.96
C9A H9A2 . 0.96
C9A H9A3 . 0.96
C9B H9B1 . 0.96
C9B H9B2 . 0.96
C9B H9B3 . 0.96
