#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:45:17 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180275 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/61/7116187.cif $
#------------------------------------------------------------------------------
#
# 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_7116187
loop_
_publ_author_name
'Adonin, Sergey A.'
'Izarova, Natalya V.'
'Besson, Claire'
'Abramov, Pavel A.'
'Santiago-Schübel, Beatrix'
'Kögerler, Paul'
'Fedin, Vladimir P.'
'Sokolov, Maxim N.'
_publ_section_title
;
 An Ir(IV)-containing polyoxometalate.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1222
_journal_page_last               1225
_journal_paper_doi               10.1039/c4cc09271f
_journal_volume                  51
_journal_year                    2014
_chemical_formula_sum            'H54 Ir Na6 O50 W6'
_chemical_formula_weight         2287.67
_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   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.449(2)
_cell_angle_beta                 106.127(2)
_cell_angle_gamma                105.317(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9995(2)
_cell_length_b                   11.2653(2)
_cell_length_c                   12.4259(3)
_cell_measurement_reflns_used    13324
_cell_measurement_temperature    119.95(10)
_cell_measurement_theta_max      30.9570
_cell_measurement_theta_min      3.2850
_cell_volume                     1058.86(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22392
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    19.555
_exptl_absorpt_correction_T_max  0.5561
_exptl_absorpt_correction_T_min  0.0457
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1041
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.616
_refine_diff_density_min         -2.630
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0338
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                3940
_reflns_number_total             4264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09271f3.cif
_cod_data_source_block           Na-IrW6
_cod_original_cell_volume        1058.86(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ir1 Ir 0.0000 0.5000 0.0000 0.00766(14) Uani 1 2 d S
W1 W 0.33543(3) 0.55402(3) 0.22248(2) 0.01199(14) Uani 1 1 d .
W2 W 0.20772(3) 0.80133(3) 0.23832(2) 0.01106(13) Uani 1 1 d .
W3 W 0.13609(4) 0.25724(3) -0.00392(3) 0.01241(14) Uani 1 1 d .
O1T1 O 0.3516(7) 0.4771(5) 0.3249(5) 0.0201(11) Uani 1 1 d .
O12 O 0.2496(6) 0.6800(5) 0.3139(4) 0.0139(11) Uani 1 1 d .
O1T2 O 0.5396(6) 0.6672(5) 0.2702(5) 0.0229(12) Uani 1 1 d .
O13 O 0.3410(6) 0.4179(5) 0.0840(5) 0.0149(11) Uani 1 1 d .
O2T1 O 0.4113(6) 0.9162(5) 0.2884(5) 0.0167(10) Uani 1 1 d .
O2T2 O 0.1286(7) 0.8828(5) 0.3392(5) 0.0188(11) Uani 1 1 d .
O23 O 0.1022(6) 0.8341(5) 0.0972(4) 0.0143(10) Uani 1 1 d .
O3T1 O 0.1599(7) 0.1784(5) 0.0955(5) 0.0229(12) Uani 1 1 d .
O3T2 O 0.2035(7) 0.1758(5) -0.1141(5) 0.0212(11) Uani 1 1 d .
O112 O 0.2322(7) 0.6401(5) 0.1023(5) 0.0124(11) Uani 1 1 d .
O113 O 0.0756(7) 0.4104(5) 0.1074(5) 0.0121(11) Uani 1 1 d .
O123 O -0.0540(7) 0.6328(5) 0.1207(5) 0.0123(11) Uani 1 1 d .
Na1 Na 0.8229(3) 0.4570(3) 0.3758(2) 0.0218(7) Uani 1 1 d .
Na2 Na 0.6184(4) 0.1440(3) 0.1315(3) 0.0242(7) Uani 1 1 d .
Na3 Na 0.2245(5) 1.1754(4) 0.4690(4) 0.0492(10) Uani 1 1 d .
O1W O 0.5732(7) 0.2755(6) 0.0120(5) 0.0229(12) Uiso 1 1 d .
O2W O 0.7438(6) 0.5265(5) 0.2092(5) 0.0214(11) Uiso 1 1 d .
O3W O 0.9021(7) 0.3060(6) 0.2361(5) 0.0274(13) Uiso 1 1 d .
O4W O 0.6778(7) 0.0080(6) -0.0264(5) 0.0220(12) Uiso 1 1 d .
O5W O 0.5411(7) 0.2808(6) 0.2813(5) 0.0260(13) Uiso 1 1 d .
O6W O 1.0974(9) 0.6265(7) 0.4724(6) 0.0385(16) Uiso 1 1 d .
O7W O 0.4794(7) 1.1760(5) 0.4496(5) 0.0237(11) Uiso 1 1 d .
O8W O 0.2974(7) 1.4070(6) 0.5096(5) 0.0280(13) Uiso 1 1 d .
O9W O 0.0633(7) 1.1159(6) 0.2644(5) 0.0310(13) Uiso 1 1 d .
O10W O 0.6932(10) 0.0134(8) 0.2442(7) 0.0513(18) Uiso 1 1 d .
O11W O -0.0401(13) 1.1420(11) 0.4733(9) 0.025(2) Uiso 0.50 1 d P
O12W O 0.166(2) 1.1228(19) 0.6135(16) 0.076(5) Uiso 0.50 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
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
O113 Ir1 O113 180.0 . 2_565
O113 Ir1 O112 97.6(2) . 2_565
O113 Ir1 O112 82.4(2) 2_565 2_565
O113 Ir1 O112 82.4(2) . .
O113 Ir1 O112 97.6(2) 2_565 .
O112 Ir1 O112 180.0 2_565 .
O113 Ir1 O123 83.0(2) . 2_565
O113 Ir1 O123 97.0(2) 2_565 2_565
O112 Ir1 O123 81.8(2) 2_565 2_565
O112 Ir1 O123 98.2(2) . 2_565
O113 Ir1 O123 97.0(2) . .
O113 Ir1 O123 83.0(2) 2_565 .
O112 Ir1 O123 98.3(2) 2_565 .
O112 Ir1 O123 81.8(2) . .
O123 Ir1 O123 179.999(1) 2_565 .
O1T2 W1 O1T1 104.0(3) . .
O1T2 W1 O13 95.2(2) . .
O1T1 W1 O13 100.0(2) . .
O1T2 W1 O12 99.0(2) . .
O1T1 W1 O12 92.7(2) . .
O13 W1 O12 158.1(2) . .
O1T2 W1 O112 92.7(2) . .
O1T1 W1 O112 159.8(2) . .
O13 W1 O112 89.6(2) . .
O12 W1 O112 73.21(19) . .
O1T2 W1 O113 162.4(2) . .
O1T1 W1 O113 91.3(2) . .
O13 W1 O113 73.2(2) . .
O12 W1 O113 88.9(2) . .
O112 W1 O113 74.4(2) . .
O1T2 W1 W3 128.68(18) . .
O1T1 W1 W3 89.01(17) . .
O13 W1 W3 33.52(15) . .
O12 W1 W3 130.25(15) . .
O112 W1 W3 89.35(14) . .
O113 W1 W3 41.39(13) . .
O2T1 W2 O2T2 104.3(2) . .
O2T1 W2 O23 98.6(2) . .
O2T2 W2 O23 99.1(2) . .
O2T1 W2 O12 100.6(2) . .
O2T2 W2 O12 96.3(2) . .
O23 W2 O12 151.6(2) . .
O2T1 W2 O112 94.9(2) . .
O2T2 W2 O112 159.8(2) . .
O23 W2 O112 83.8(2) . .
O12 W2 O112 73.89(19) . .
O2T1 W2 O123 164.1(2) . .
O2T2 W2 O123 89.7(2) . .
O23 W2 O123 71.20(19) . .
O12 W2 O123 85.2(2) . .
O112 W2 O123 72.3(2) . .
O3T1 W3 O3T2 103.5(3) . .
O3T1 W3 O13 100.9(2) . .
O3T2 W3 O13 94.4(2) . .
O3T1 W3 O23 99.3(2) . 2_565
O3T2 W3 O23 99.0(2) . 2_565
O13 W3 O23 152.3(2) . 2_565
O3T1 W3 O113 95.3(2) . .
O3T2 W3 O113 159.7(2) . .
O13 W3 O113 74.3(2) . .
O23 W3 O113 85.2(2) 2_565 .
O3T1 W3 O123 166.3(2) . 2_565
O3T2 W3 O123 88.5(2) . 2_565
O13 W3 O123 84.6(2) . 2_565
O23 W3 O123 71.79(19) 2_565 2_565
O113 W3 O123 73.8(2) . 2_565
O3T1 W3 W1 91.82(18) . .
O3T2 W3 W1 127.94(18) . .
O13 W3 W1 33.51(15) . .
O23 W3 W1 127.49(14) 2_565 .
O113 W3 W1 42.58(15) . .
O123 W3 W1 85.84(13) 2_565 .
W2 O12 W1 111.7(2) . .
W1 O1T2 Na3 123.9(3) . 2_676
W1 O13 W3 113.0(2) . .
W2 O2T2 Na3 127.2(3) . .
W2 O23 W3 119.7(2) . 2_565
Ir1 O112 W1 102.2(2) . .
Ir1 O112 W2 105.7(2) . .
W1 O112 W2 97.8(2) . .
Ir1 O113 W3 104.5(2) . .
Ir1 O113 W1 101.0(2) . .
W3 O113 W1 96.0(2) . .
Ir1 O123 W3 98.7(2) . 2_565
Ir1 O123 W2 100.2(2) . .
W3 O123 W2 94.0(2) 2_565 .
O6W Na1 O6W 88.2(3) . 2_766
O6W Na1 O3W 91.7(2) . .
O6W Na1 O3W 91.9(2) 2_766 .
O6W Na1 O2W 92.9(2) . .
O6W Na1 O2W 175.3(3) 2_766 .
O3W Na1 O2W 83.47(19) . .
O6W Na1 O8W 95.5(2) . 2_676
O6W Na1 O8W 92.9(2) 2_766 2_676
O3W Na1 O8W 171.4(2) . 2_676
O2W Na1 O8W 91.5(2) . 2_676
O6W Na1 O5W 178.4(2) . .
O6W Na1 O5W 90.2(2) 2_766 .
O3W Na1 O5W 88.8(2) . .
O2W Na1 O5W 88.7(2) . .
O8W Na1 O5W 84.2(2) 2_676 .
O6W Na1 Na1 44.31(18) . 2_766
O6W Na1 Na1 43.88(18) 2_766 2_766
O3W Na1 Na1 92.52(18) . 2_766
O2W Na1 Na1 137.00(19) . 2_766
O8W Na1 Na1 95.88(18) 2_676 2_766
O5W Na1 Na1 134.12(19) . 2_766
O6W Na1 Na2 135.93(19) . .
O6W Na1 Na2 95.3(2) 2_766 .
O3W Na1 Na2 44.35(16) . .
O2W Na1 Na2 80.77(15) . .
O8W Na1 Na2 128.01(18) 2_676 .
O5W Na1 Na2 44.66(15) . .
Na1 Na1 Na2 124.22(14) 2_766 .
O6W Na1 Na3 73.75(19) . 2_676
O6W Na1 Na3 110.68(19) 2_766 2_676
O3W Na1 Na3 152.24(18) . 2_676
O2W Na1 Na3 74.03(15) . 2_676
O8W Na1 Na3 29.01(16) 2_676 2_676
O5W Na1 Na3 106.45(17) . 2_676
Na1 Na1 Na3 93.02(12) 2_766 2_676
Na2 Na1 Na3 142.32(11) . 2_676
O4W Na2 O3W 92.5(2) . .
O4W Na2 O5W 176.1(3) . .
O3W Na2 O5W 90.3(2) . .
O4W Na2 O10W 87.3(3) . .
O3W Na2 O10W 89.2(3) . .
O5W Na2 O10W 95.6(2) . .
O4W Na2 O1W 87.5(2) . .
O3W Na2 O1W 86.3(2) . .
O5W Na2 O1W 89.9(2) . .
O10W Na2 O1W 172.9(3) . .
O4W Na2 O4W 90.3(2) . 2_655
O3W Na2 O4W 175.9(2) . 2_655
O5W Na2 O4W 86.8(2) . 2_655
O10W Na2 O4W 93.9(2) . 2_655
O1W Na2 O4W 90.9(2) . 2_655
O4W Na2 Na2 46.11(15) . 2_655
O3W Na2 Na2 138.5(2) . 2_655
O5W Na2 Na2 130.9(2) . 2_655
O10W Na2 Na2 90.9(2) . 2_655
O1W Na2 Na2 88.91(19) . 2_655
O4W Na2 Na2 44.18(15) 2_655 2_655
O4W Na2 Na1 136.91(18) . .
O3W Na2 Na1 45.05(16) . .
O5W Na2 Na1 45.48(15) . .
O10W Na2 Na1 97.2(2) . .
O1W Na2 Na1 83.38(15) . .
O4W Na2 Na1 131.74(17) 2_655 .
Na2 Na2 Na1 171.36(17) 2_655 .
O12W Na3 O11W 60.0(6) . .
O12W Na3 O9W 132.5(6) . .
O11W Na3 O9W 78.8(3) . .
O12W Na3 O8W 114.4(5) . .
O11W Na3 O8W 94.9(3) . .
O9W Na3 O8W 90.0(2) . .
O12W Na3 O7W 118.7(5) . .
O11W Na3 O7W 172.0(4) . .
O9W Na3 O7W 98.7(2) . .
O8W Na3 O7W 92.7(2) . .
O12W Na3 O2T2 84.0(5) . .
O11W Na3 O2T2 91.2(3) . .
O9W Na3 O2T2 73.8(2) . .
O8W Na3 O2T2 161.2(2) . .
O7W Na3 O2T2 80.8(2) . .
O12W Na3 O1T2 60.2(5) . 2_676
O11W Na3 O1T2 104.8(3) . 2_676
O9W Na3 O1T2 162.8(3) . 2_676
O8W Na3 O1T2 73.0(2) . 2_676
O7W Na3 O1T2 79.9(2) . 2_676
O2T2 Na3 O1T2 122.45(19) . 2_676
O12W Na3 Na1 88.4(5) . 2_676
O11W Na3 Na1 68.5(3) . 2_676
O9W Na3 Na1 97.95(19) . 2_676
O8W Na3 Na1 29.94(16) . 2_676
O7W Na3 Na1 119.5(2) . 2_676
O2T2 Na3 Na1 159.37(17) . 2_676
O1T2 Na3 Na1 68.63(14) 2_676 2_676
Na2 O3W Na1 90.6(2) . .
Na2 O4W Na2 89.7(2) . 2_655
Na2 O5W Na1 89.9(2) . .
Na1 O6W Na1 91.8(3) . 2_766
Na3 O8W Na1 121.1(3) . 2_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 O113 1.994(5) .
Ir1 O113 1.994(5) 2_565
Ir1 O112 1.996(5) 2_565
Ir1 O112 1.996(5) .
Ir1 O123 2.022(5) 2_565
Ir1 O123 2.022(5) .
W1 O1T2 1.741(5) .
W1 O1T1 1.747(5) .
W1 O13 1.932(5) .
W1 O12 1.987(5) .
W1 O112 2.157(5) .
W1 O113 2.193(6) .
W1 W3 3.2225(4) .
W2 O2T1 1.738(5) .
W2 O2T2 1.742(5) .
W2 O23 1.945(5) .
W2 O12 1.944(5) .
W2 O112 2.163(5) .
W2 O123 2.293(5) .
W3 O3T1 1.735(5) .
W3 O3T2 1.745(5) .
W3 O13 1.933(5) .
W3 O23 1.923(5) 2_565
W3 O113 2.142(5) .
W3 O123 2.283(5) 2_565
O1T2 Na3 2.950(7) 2_676
O2T2 Na3 2.928(7) .
O23 W3 1.923(5) 2_565
O123 W3 2.283(5) 2_565
Na1 O6W 2.366(7) .
Na1 O6W 2.385(7) 2_766
Na1 O3W 2.424(7) .
Na1 O2W 2.430(6) .
Na1 O8W 2.429(7) 2_676
Na1 O5W 2.442(6) .
Na1 Na1 3.412(5) 2_766
Na1 Na2 3.424(4) .
Na1 Na3 4.169(5) 2_676
Na2 O4W 2.365(6) .
Na2 O3W 2.394(7) .
Na2 O5W 2.407(6) .
Na2 O10W 2.426(8) .
Na2 O1W 2.437(6) .
Na2 O4W 2.446(6) 2_655
Na2 Na2 3.394(6) 2_655
Na3 O12W 2.213(19) .
Na3 O11W 2.329(12) .
Na3 O9W 2.318(7) .
Na3 O8W 2.360(7) .
Na3 O7W 2.371(7) .
Na3 O1T2 2.950(7) 2_676
Na3 Na1 4.169(5) 2_676
O4W Na2 2.446(6) 2_655
O6W Na1 2.385(7) 2_766
O8W Na1 2.429(7) 2_676
