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#$Date: 2016-03-25 14:55:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179906 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/02/7020200.cif $
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#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7020200
loop_
_publ_author_name
'Choujaa, Hamid'
'Johnson, Andrew L.'
'Kociok-Köhn, Gabriele'
'Molloy, Kieran C.'
_publ_section_title
;
 The synthesis of W-O-W μ-oxo clusters by hydrolysis of tungsten
 aminoalkoxides and their structural characterisation.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11393
_journal_page_last               11401
_journal_paper_doi               10.1039/c2dt30966a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C40 H96 N12 O14 W4'
_chemical_formula_sum            'C40 H96 N12 O14 W4'
_chemical_formula_weight         1704.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.9274(2)
_cell_length_b                   24.9274(2)
_cell_length_c                   9.68370(10)
_cell_measurement_reflns_used    55569
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     6017.21(9)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
DENZO-SCALEPACK Z. Otwinowski and W. Minor, "
Processing of X-ray Diffraction Data Collected in Oscillation Mode ",
Methods in Enzymology, Volume 276: Macromolecular Crystallography,
part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
'WinGX publication routines, Farrugia,
L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
SHELXL97 -Program for Crystal Structure Analysis (Release 97-2).
Sheldrick, G.M., Institut für Anorganische Chemie der Universität,
Tammanstrasse 4, D-3400 Göttingen, Germany, 1998
;
_computing_structure_solution
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '323 1.7 degree images with 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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            71613
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         5.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.685
_exptl_absorpt_correction_T_max  0.6999
_exptl_absorpt_correction_T_min  0.2496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00064(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0321P)²+14.8729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                3988
_reflns_number_total             4370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30966a.txt
_cod_data_source_block           shelxl7
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7020200
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.048107(4) 0.195231(4) 0.482470(11) 0.01927(6) Uani 1 1 d .
O1 O 0.11679(8) 0.16689(8) 0.5311(2) 0.0227(4) Uani 1 1 d .
O2 O 0.03261(9) 0.14981(9) 0.3549(2) 0.0279(4) Uani 1 1 d .
O3 O 0.0000 0.2500 0.4220(3) 0.0217(5) Uani 1 2 d S
O4 O 0.01102(8) 0.17320(8) 0.6276(2) 0.0217(4) Uani 1 1 d .
N1 N 0.10919(10) 0.24394(10) 0.3475(3) 0.0236(5) Uani 1 1 d .
N2 N 0.22456(11) 0.14312(11) 0.6807(3) 0.0310(6) Uani 1 1 d .
N3 N 0.24086(11) 0.14790(11) 0.3260(3) 0.0306(5) Uani 1 1 d .
C1 C 0.16885(11) 0.18169(12) 0.4846(3) 0.0223(5) Uani 1 1 d .
C2 C 0.16343(11) 0.23627(12) 0.4111(3) 0.0250(5) Uani 1 1 d .
H2A H 0.1700 0.2654 0.4785 0.030 Uiso 1 1 calc R
H2B H 0.1911 0.2389 0.3381 0.030 Uiso 1 1 calc R
C3 C 0.10740(14) 0.22392(15) 0.2032(3) 0.0333(7) Uani 1 1 d .
H3A H 0.0721 0.2316 0.1632 0.050 Uiso 1 1 calc R
H3B H 0.1137 0.1851 0.2025 0.050 Uiso 1 1 calc R
H3C H 0.1352 0.2418 0.1486 0.050 Uiso 1 1 calc R
C4 C 0.09847(13) 0.30264(12) 0.3407(3) 0.0299(6) Uani 1 1 d .
H4A H 0.1272 0.3203 0.2885 0.045 Uiso 1 1 calc R
H4B H 0.0972 0.3174 0.4344 0.045 Uiso 1 1 calc R
H4C H 0.0640 0.3089 0.2946 0.045 Uiso 1 1 calc R
C5 C 0.20668(12) 0.19118(12) 0.6075(3) 0.0278(6) Uani 1 1 d .
H5A H 0.2388 0.2106 0.5737 0.033 Uiso 1 1 calc R
H5B H 0.1883 0.2149 0.6744 0.033 Uiso 1 1 calc R
C6 C 0.18299(15) 0.12071(16) 0.7686(4) 0.0393(8) Uani 1 1 d .
H6A H 0.1720 0.1475 0.8369 0.059 Uiso 1 1 calc R
H6B H 0.1969 0.0889 0.8161 0.059 Uiso 1 1 calc R
H6C H 0.1520 0.1105 0.7119 0.059 Uiso 1 1 calc R
C7 C 0.27164(16) 0.15597(18) 0.7647(4) 0.0446(9) Uani 1 1 d .
H7A H 0.2618 0.1823 0.8354 0.067 Uiso 1 1 calc R
H7B H 0.2998 0.1709 0.7056 0.067 Uiso 1 1 calc R
H7C H 0.2849 0.1233 0.8094 0.067 Uiso 1 1 calc R
C8 C 0.18858(12) 0.13613(12) 0.3902(3) 0.0265(6) Uani 1 1 d .
H8A H 0.1916 0.1027 0.4450 0.032 Uiso 1 1 calc R
H8B H 0.1617 0.1299 0.3166 0.032 Uiso 1 1 calc R
C9 C 0.23916(15) 0.14598(17) 0.1763(4) 0.0419(8) Uani 1 1 d .
H9A H 0.2748 0.1540 0.1392 0.063 Uiso 1 1 calc R
H9B H 0.2134 0.1725 0.1423 0.063 Uiso 1 1 calc R
H9C H 0.2281 0.1101 0.1464 0.063 Uiso 1 1 calc R
C10 C 0.28192(17) 0.1104(2) 0.3751(5) 0.0634(14) Uani 1 1 d .
H10A H 0.2737 0.0743 0.3414 0.095 Uiso 1 1 calc R
H10B H 0.2824 0.1104 0.4763 0.095 Uiso 1 1 calc R
H10C H 0.3171 0.1216 0.3403 0.095 Uiso 1 1 calc R
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 W1 O4 104.41(10) . .
O2 W1 O3 96.29(10) . .
O4 W1 O3 97.90(9) . .
O2 W1 O1 97.76(9) . .
O4 W1 O1 99.05(9) . .
O3 W1 O1 154.51(6) . .
O2 W1 O4 170.53(9) . 16_556
O4 W1 O4 85.06(8) . 16_556
O3 W1 O4 82.11(7) . 16_556
O1 W1 O4 80.54(8) . 16_556
O2 W1 N1 94.96(10) . .
O4 W1 N1 160.45(9) . .
O3 W1 N1 82.34(7) . .
O1 W1 N1 75.36(9) . .
O4 W1 N1 75.58(8) 16_556 .
C1 O1 W1 130.03(17) . .
W1 O3 W1 144.29(16) 3 .
W1 O4 W1 139.66(11) . 14_556
C3 N1 C4 106.4(2) . .
C3 N1 C2 111.8(2) . .
C4 N1 C2 107.8(2) . .
C3 N1 W1 109.32(19) . .
C4 N1 W1 114.66(18) . .
C2 N1 W1 106.93(17) . .
C6 N2 C5 112.4(3) . .
C6 N2 C7 109.3(3) . .
C5 N2 C7 109.6(3) . .
C9 N3 C10 108.9(3) . .
C9 N3 C8 112.9(3) . .
C10 N3 C8 110.8(3) . .
O1 C1 C5 110.7(2) . .
O1 C1 C8 106.8(2) . .
C5 C1 C8 112.2(2) . .
O1 C1 C2 107.2(2) . .
C5 C1 C2 106.0(2) . .
C8 C1 C2 113.9(2) . .
N1 C2 C1 112.4(2) . .
N1 C2 H2A 109.1 . .
C1 C2 H2A 109.1 . .
N1 C2 H2B 109.1 . .
C1 C2 H2B 109.1 . .
H2A C2 H2B 107.8 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N2 C5 C1 115.9(2) . .
N2 C5 H5A 108.3 . .
C1 C5 H5A 108.3 . .
N2 C5 H5B 108.3 . .
C1 C5 H5B 108.3 . .
H5A C5 H5B 107.4 . .
N2 C6 H6A 109.5 . .
N2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N3 C8 C1 112.7(2) . .
N3 C8 H8A 109.0 . .
C1 C8 H8A 109.0 . .
N3 C8 H8B 109.0 . .
C1 C8 H8B 109.0 . .
H8A C8 H8B 107.8 . .
N3 C9 H9A 109.5 . .
N3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N3 C10 H10A 109.5 . .
N3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O2 1.719(2) .
W1 O4 1.770(2) .
W1 O3 1.9091(9) .
W1 O1 1.911(2) .
W1 O4 2.2443(19) 16_556
W1 N1 2.345(2) .
O1 C1 1.422(3) .
O3 W1 1.9091(9) 3
O4 W1 2.2443(19) 14_556
N1 C3 1.485(4) .
N1 C4 1.489(4) .
N1 C2 1.498(4) .
N2 C6 1.453(5) .
N2 C5 1.462(4) .
N2 C7 1.464(4) .
N3 C9 1.451(5) .
N3 C10 1.465(5) .
N3 C8 1.473(4) .
C1 C5 1.537(4) .
C1 C8 1.539(4) .
C1 C2 1.541(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
