#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302489.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_4302489
loop_
_publ_author_name
'Robila Belghiche'
'Ouahiba Bechiri'
'Mostefa Abbessi'
'Stéphane Golhen'
'Yann Le Gal'
'Lahcène Ouahab'
_publ_contact_author_address
;Organométalliques et Matériaux Moléculaires
UMR 6226 CNRS-Université de Rennes 1
Sciences Chimiques de Rennes
Avenue Général Leclerc
35042 Rennes Cedex
France
;
_publ_contact_author_email       lahcene.ouahab@univ-rennes1.fr
_publ_contact_author_fax         +33(0)223236840
_publ_contact_author_name        'Lahcène Ouahab'
_publ_contact_author_phone       +33(0)223235659
_publ_section_title
;
2D and 3D Polymeric Wells-Dawson Polyoxometelates: Synthesis, Crystal
Structures, and Cyclic Voltammetry of [(M(H2O)4)x][H6-2xP2W18-nMonO62]
(M = CuII, CoII, NiII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6026
_journal_page_last               6033
_journal_paper_doi               10.1021/ic9003406
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '[Cu(H2O)4]2.5[HP2W18O62],11.33H2O'
_chemical_formula_sum            'Cu2.5 H43.67 O83.33 P2 W18'
_chemical_formula_weight         4907.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   none
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.2890(9)
_cell_length_b                   15.2890(9)
_cell_length_c                   55.9800(10)
_cell_measurement_reflns_used    56784
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.910
_cell_volume                     11332.4(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare al, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            66668
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    28.130
_exptl_crystal_density_diffrn    4.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             12869
_refine_diff_density_max         3.262
_refine_diff_density_min         -4.210
_refine_diff_density_rms         0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         6056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0199P)²+266.2549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                4307
_reflns_number_total             6056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003406_si_001_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'H43.67 Cu2.50 O83.33 P2 W18'
_cod_database_code               4302489
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z'
'-x+y, -x, z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z'
'x-y, x, -z'
'x, x-y, z'
'-x+y, y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.16213(6) 0.83787(6) 0.10674(2) 0.0266(5) Uani 0.834(5) 2 d SP . .
O1 O 0.4274(5) 1.2137(2) -0.03896(10) 0.0203(13) Uani 1 2 d S . .
O2 O 0.3185(3) 1.0028(3) 0.03184(8) 0.0225(9) Uani 1 1 d . . .
O3 O 0.3195(3) 0.9976(4) 0.11026(8) 0.0227(9) Uani 1 1 d . . .
O4 O 0.4264(5) 1.2132(2) 0.18110(10) 0.0232(14) Uani 1 2 d S . .
O5 O 0.6087(2) 1.2173(4) -0.03022(10) 0.0145(11) Uani 1 2 d S . .
O6 O 0.4713(3) 1.1507(3) 0.00526(7) 0.0168(8) Uani 1 1 d . . .
O7 O 0.5161(2) 1.0321(4) 0.03318(10) 0.0152(11) Uani 1 2 d S . .
O8 O 0.4156(4) 1.2078(2) 0.04374(10) 0.0159(11) Uani 1 2 d S . .
O9 O 0.4423(3) 1.0815(3) 0.07127(7) 0.0160(8) Uani 1 1 d . . .
O10 O 0.5162(2) 1.0323(4) 0.10968(10) 0.0157(11) Uani 1 2 d S . .
O11 O 0.4130(4) 1.2065(2) 0.09912(10) 0.0157(11) Uani 1 2 d S . .
O12 O 0.4693(3) 1.1497(3) 0.13721(7) 0.0161(8) Uani 1 1 d . . .
O13 O 0.6085(2) 1.3915(2) 0.17234(10) 0.0163(11) Uani 1 2 d S . .
O14 O 0.6667 1.3333 0.00694(16) 0.0119(18) Uani 1 6 d S . .
O15 O 0.6112(2) 1.2224(4) 0.04354(9) 0.0124(10) Uani 1 2 d S . .
O16 O 0.6112(2) 1.2224(4) 0.09874(10) 0.0135(10) Uani 1 2 d S . .
O17 O 0.6667 1.3333 0.13521(16) 0.0121(18) Uani 1 6 d S . .
O18 O 0.1399(4) 0.8601(4) 0.07315(14) 0.038(2) Uani 0.834(5) 2 d SP . .
O19 O 0.0896(4) 0.9104(4) 0.11472(14) 0.033(2) Uani 0.834(5) 2 d SP . .
O20 O 0.1819(5) 0.8181(5) 0.14080(16) 0.049(3) Uani 0.834(5) 2 d SP . .
O21 O 0.2335(4) 0.7665(4) 0.09696(18) 0.038(2) Uani 0.834(5) 2 d SP . .
P1 P 0.6667 1.3333 0.03549(5) 0.0073(5) Uani 1 6 d S . .
P2 P 0.6667 1.3333 0.10680(6) 0.0092(6) Uani 1 6 d S . .
W1 W 0.51833(2) 1.259165(12) -0.017140(5) 0.01412(7) Uani 1 2 d S . .
W2 W 0.438785(17) 1.098397(17) 0.037091(4) 0.01366(5) Uani 1 1 d . . .
W3 W 0.438083(17) 1.097788(17) 0.104529(4) 0.01334(5) Uani 1 1 d . . .
W4 W 0.51724(2) 1.258621(12) 0.159294(5) 0.01394(7) Uani 1 2 d S . .
O1W O 0.2271(11) 1.1135(6) -0.0092(3) 0.070(7) Uani 0.72(3) 2 d SP . .
O2W O 0.4285(3) 0.8571(7) 0.07678(15) 0.051(2) Uani 1 2 d S . .
O3W O 0.0284(6) 0.3618(6) 0.1667 0.047(2) Uani 1 2 d S . .
O4W O 0.1811(18) 1.0906(9) 0.0767(10) 0.42(3) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
P P 0.1023 0.0942 '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'
H H 0.0000 0.0000 '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
_geom_angle_publ_flag
O21 Cu O18 91.2(4) . . ?
O21 Cu O19 176.9(4) . . ?
O18 Cu O19 85.7(4) . . ?
O21 Cu O20 90.8(5) . . ?
O18 Cu O20 178.0(5) . . ?
O19 Cu O20 92.3(5) . . ?
O21 Cu O3 92.02(12) . 21_665 ?
O18 Cu O3 94.21(11) . 21_665 ?
O19 Cu O3 88.21(12) . 21_665 ?
O20 Cu O3 85.72(11) . 21_665 ?
O21 Cu O3 92.02(12) . . ?
O18 Cu O3 94.21(11) . . ?
O19 Cu O3 88.21(12) . . ?
O20 Cu O3 85.72(11) . . ?
O3 Cu O3 170.6(2) 21_665 . ?
W3 O3 Cu 162.2(3) . . ?
W1 O5 W1 123.3(3) 2_775 . ?
W1 O6 W2 151.7(2) . . ?
W2 O7 W2 123.6(3) 24 . ?
W2 O8 W2 150.8(3) 23_575 . ?
W3 O9 W2 162.6(2) . . ?
W3 O10 W3 123.3(3) 24 . ?
W3 O11 W3 152.7(3) . 23_575 ?
W4 O12 W3 150.7(2) . . ?
W4 O13 W4 123.8(3) . 21_775 ?
P1 O14 W1 124.46(17) . 2_775 ?
P1 O14 W1 124.46(17) . . ?
W1 O14 W1 91.1(2) 2_775 . ?
P1 O14 W1 124.46(17) . 21_775 ?
W1 O14 W1 91.1(2) 2_775 21_775 ?
W1 O14 W1 91.1(2) . 21_775 ?
P1 O15 W2 127.90(16) . . ?
P1 O15 W2 127.90(16) . 24 ?
W2 O15 W2 90.24(19) . 24 ?
P2 O16 W3 128.38(17) . . ?
P2 O16 W3 128.38(17) . 24 ?
W3 O16 W3 90.43(19) . 24 ?
P2 O17 W4 124.27(18) . 2_775 ?
P2 O17 W4 124.27(18) . 21_775 ?
W4 O17 W4 91.4(2) 2_775 21_775 ?
P2 O17 W4 124.27(18) . . ?
W4 O17 W4 91.4(2) 2_775 . ?
W4 O17 W4 91.4(2) 21_775 . ?
O15 P1 O15 111.8(2) 2_775 . ?
O15 P1 O15 111.8(2) 2_775 4_575 ?
O15 P1 O15 111.8(2) . 4_575 ?
O15 P1 O14 107.1(2) 2_775 . ?
O15 P1 O14 107.1(2) . . ?
O15 P1 O14 107.1(2) 4_575 . ?
O16 P2 O16 111.7(2) . 2_775 ?
O16 P2 O16 111.7(2) . 4_575 ?
O16 P2 O16 111.7(2) 2_775 4_575 ?
O16 P2 O17 107.1(2) . . ?
O16 P2 O17 107.1(2) 2_775 . ?
O16 P2 O17 107.1(2) 4_575 . ?
O1 W1 O6 103.8(2) . 23_575 ?
O1 W1 O6 103.8(2) . . ?
O6 W1 O6 85.7(3) 23_575 . ?
O1 W1 O5 99.5(2) . 4_575 ?
O6 W1 O5 89.0(2) 23_575 4_575 ?
O6 W1 O5 156.72(19) . 4_575 ?
O1 W1 O5 99.5(2) . . ?
O6 W1 O5 156.72(19) 23_575 . ?
O6 W1 O5 89.0(2) . . ?
O5 W1 O5 87.0(3) 4_575 . ?
O1 W1 O14 169.1(3) . . ?
O6 W1 O14 84.11(18) 23_575 . ?
O6 W1 O14 84.11(18) . . ?
O5 W1 O14 72.79(18) 4_575 . ?
O5 W1 O14 72.79(18) . . ?
O2 W2 O8 101.0(2) . . ?
O2 W2 O6 98.1(2) . . ?
O8 W2 O6 86.5(2) . . ?
O2 W2 O7 102.3(2) . . ?
O8 W2 O7 156.7(2) . . ?
O6 W2 O7 90.8(2) . . ?
O2 W2 O9 98.4(2) . . ?
O8 W2 O9 87.4(2) . . ?
O6 W2 O9 163.23(18) . . ?
O7 W2 O9 88.7(2) . . ?
O2 W2 O15 175.32(19) . . ?
O8 W2 O15 83.7(2) . . ?
O6 W2 O15 81.72(18) . . ?
O7 W2 O15 73.05(18) . . ?
O9 W2 O15 82.10(17) . . ?
O3 W3 O9 99.1(2) . . ?
O3 W3 O11 102.9(2) . . ?
O9 W3 O11 89.6(2) . . ?
O3 W3 O10 99.3(2) . . ?
O9 W3 O10 90.5(2) . . ?
O11 W3 O10 157.5(2) . . ?
O3 W3 O12 96.97(19) . . ?
O9 W3 O12 163.84(18) . . ?
O11 W3 O12 84.8(2) . . ?
O10 W3 O12 89.0(2) . . ?
O3 W3 O16 172.08(19) . . ?
O9 W3 O16 82.73(18) . . ?
O11 W3 O16 84.8(2) . . ?
O10 W3 O16 72.96(18) . . ?
O12 W3 O16 81.66(18) . . ?
O4 W4 O12 103.2(2) . . ?
O4 W4 O12 103.2(2) . 23_575 ?
O12 W4 O12 86.1(2) . 23_575 ?
O4 W4 O13 99.7(2) . . ?
O12 W4 O13 157.04(19) . . ?
O12 W4 O13 89.0(2) 23_575 . ?
O4 W4 O13 99.7(2) . 2_775 ?
O12 W4 O13 89.0(2) . 2_775 ?
O12 W4 O13 157.04(19) 23_575 2_775 ?
O13 W4 O13 86.7(4) . 2_775 ?
O4 W4 O17 168.8(3) . . ?
O12 W4 O17 84.82(18) . . ?
O12 W4 O17 84.82(18) 23_575 . ?
O13 W4 O17 72.39(19) . . ?
O13 W4 O17 72.39(19) 2_775 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu O21 1.968(9) . ?
Cu O18 1.970(8) . ?
Cu O19 1.973(10) . ?
Cu O20 1.978(9) . ?
Cu O3 2.432(5) 21_665 ?
Cu O3 2.432(5) . ?
O1 W1 1.715(6) . ?
O2 W2 1.707(4) . ?
O3 W3 1.720(4) . ?
O4 W4 1.713(6) . ?
O5 W1 1.933(3) 2_775 ?
O5 W1 1.933(3) . ?
O6 W1 1.910(4) . ?
O6 W2 1.914(4) . ?
O7 W2 1.915(3) 24 ?
O7 W2 1.915(3) . ?
O8 W2 1.9117(15) 23_575 ?
O8 W2 1.9117(15) . ?
O9 W3 1.884(4) . ?
O9 W2 1.935(4) . ?
O10 W3 1.925(3) 24 ?
O10 W3 1.925(3) . ?
O11 W3 1.9076(14) . ?
O11 W3 1.9076(14) 23_575 ?
O12 W4 1.903(4) . ?
O12 W3 1.956(4) . ?
O13 W4 1.942(3) . ?
O13 W4 1.942(3) 21_775 ?
O14 P1 1.598(9) . ?
O14 W1 2.382(5) 2_775 ?
O14 W1 2.382(5) . ?
O14 W1 2.382(5) 21_775 ?
O15 P1 1.537(6) . ?
O15 W2 2.382(4) . ?
O15 W2 2.382(4) 24 ?
O16 P2 1.537(6) . ?
O16 W3 2.387(4) . ?
O16 W3 2.387(4) 24 ?
O17 P2 1.590(9) . ?
O17 W4 2.394(5) 2_775 ?
O17 W4 2.394(5) 21_775 ?
O17 W4 2.394(5) . ?
P1 O15 1.537(6) 2_775 ?
P1 O15 1.537(6) 4_575 ?
P2 O16 1.537(6) 2_775 ?
P2 O16 1.537(6) 4_575 ?
W1 O6 1.910(4) 23_575 ?
W1 O5 1.933(3) 4_575 ?
W4 O12 1.903(4) 23_575 ?
W4 O13 1.942(3) 2_775 ?
