#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:36:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180345 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/14/7201411.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_7201411
loop_
_publ_author_name
'Ali, Mahammad'
'Dutta, Daipayan'
'Biswas, Surajit'
'Marek, Jaromir'
'Jana, Atish Dipankar'
_publ_section_title
;
 The first crystallographic observation of up to the third hydration
 layer of Cu(II) ion in an unusual ‘water-cation layer’
 templated by an Anderson polyoxometallate
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2608
_journal_paper_doi               10.1039/b910732k
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety
'2(C36 H24 Cu N6), Mo6 O24 Te, Cu H12 O6, 27(H2 O) '
_chemical_formula_sum            'C72 H114 Cu3 Mo6 N12 O57 Te'
_chemical_formula_weight         2953.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           163
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   17.2848(6)
_cell_length_b                   17.2848(6)
_cell_length_c                   19.2560(11)
_cell_measurement_reflns_used    25262
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.1316
_cell_measurement_theta_min      2.7176
_cell_volume                     4982.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM4 + CCD'
_diffrn_measurement_method       'rotation method, ω--scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0079
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37123
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.04437
_exptl_absorpt_correction_T_min  0.94010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2954
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.645
_refine_diff_density_min         -3.151
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+45.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                2580
_reflns_number_total             2951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910732k.txt
_cod_data_source_block           in72
_cod_database_code               7201411
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
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
Te Te 0.0000 0.0000 0.5000 0.02374(15) Uani 1 6 d S . .
Mo Mo 0.14285(2) 0.21653(2) 0.50397(2) 0.03205(11) Uani 1 1 d . . .
Cu1 Cu 0.3333 0.6667 0.45534(6) 0.0720(4) Uani 1 3 d S . .
Cu2 Cu 0.0000 0.0000 0.2500 0.0418(4) Uani 1 6 d S . .
O7 O 0.20505(19) 0.1671(2) 0.45226(17) 0.0353(8) Uani 1 1 d . . .
O8 O 0.02193(17) 0.10333(18) 0.44658(16) 0.0299(7) Uani 1 1 d D . .
O9 O 0.2148(2) 0.2674(2) 0.57181(19) 0.0444(10) Uani 1 1 d . . .
O10 O 0.1654(2) 0.2991(2) 0.44508(19) 0.0476(10) Uani 1 1 d D . .
N1 N 0.2315(4) 0.5541(4) 0.5095(3) 0.0771(17) Uani 1 1 d . . .
C2 C 0.2381(5) 0.5153(5) 0.5680(4) 0.087(2) Uani 1 1 d . . .
H2 H 0.2935 0.5419 0.5920 0.104 Uiso 1 1 calc R . .
C3 C 0.1659(5) 0.4367(4) 0.5946(4) 0.081(2) Uani 1 1 d . . .
H3 H 0.1732 0.4103 0.6355 0.097 Uiso 1 1 calc R . .
C4 C 0.0863(5) 0.3989(4) 0.5622(4) 0.076(2) Uani 1 1 d . . .
H4 H 0.0376 0.3463 0.5810 0.091 Uiso 1 1 calc R . .
C5 C 0.0742(5) 0.4354(4) 0.5020(3) 0.0689(18) Uani 1 1 d . . .
C6 C 0.1503(5) 0.5150(4) 0.4768(3) 0.0694(18) Uani 1 1 d . . .
C7 C 0.1415(5) 0.5586(4) 0.4169(3) 0.0681(18) Uani 1 1 d . . .
C8 C 0.0582(5) 0.5230(4) 0.3839(3) 0.0711(18) Uani 1 1 d . . .
C9 C 0.0533(5) 0.5723(5) 0.3284(3) 0.081(2) Uani 1 1 d . . .
H9 H -0.0016 0.5513 0.3044 0.097 Uiso 1 1 calc R . .
C10 C 0.1252(5) 0.6492(5) 0.3087(3) 0.085(2) Uani 1 1 d . . .
H10 H 0.1207 0.6830 0.2716 0.101 Uiso 1 1 calc R . .
C11 C 0.2066(5) 0.6793(5) 0.3429(4) 0.087(2) Uani 1 1 d . . .
H11 H 0.2574 0.7329 0.3276 0.105 Uiso 1 1 calc R . .
N12 N 0.2155(4) 0.6353(4) 0.3963(3) 0.0758(17) Uani 1 1 d . . .
C13 C -0.0083(5) 0.4010(4) 0.4650(4) 0.074(2) Uani 1 1 d . . .
H13 H -0.0587 0.3473 0.4806 0.089 Uiso 1 1 calc R . .
C14 C -0.0163(5) 0.4420(4) 0.4095(4) 0.076(2) Uani 1 1 d . . .
H14 H -0.0722 0.4173 0.3864 0.091 Uiso 1 1 calc R . .
O1 O -0.0964(3) -0.0990(3) 0.30866(19) 0.0583(11) Uani 1 1 d D . .
H1W H -0.104(3) -0.097(3) 0.3556(7) 0.070 Uiso 1 1 d D . .
H1V H -0.1553(8) -0.110(2) 0.3012(15) 0.070 Uiso 1 1 d D . .
O2 O 0.1152(4) 0.3454(4) 0.3233(3) 0.108(2) Uani 1 1 d D . .
H2V H 0.1366(17) 0.333(2) 0.3636(12) 0.130 Uiso 1 1 d D . .
H2W H 0.0540(9) 0.322(6) 0.311(4) 0.38(11) Uiso 1 1 d D . .
O4 O 0.11770(19) 0.2354(4) 0.2500 0.0519(14) Uani 1 2 d SD . .
H4W H 0.1161(18) 0.2696(12) 0.2856(13) 0.062 Uiso 1 1 d D . .
O6 O 0.2228(4) 0.1885(4) 0.3133(3) 0.109(3) Uani 1 1 d D . .
H6V H 0.183(3) 0.1247(10) 0.309(5) 0.131 Uiso 1 1 d D . .
H6W H 0.1831(9) 0.2031(15) 0.295(2) 0.131 Uiso 1 1 d D . .
O5 O 0.3434(3) 0.2781(4) 0.2117(2) 0.0915(19) Uani 1 1 d D . .
H5W H 0.3070(16) 0.243(3) 0.2467(12) 0.110 Uiso 1 1 d D . .
H5V H 0.318(3) 0.252(3) 0.1691(9) 0.110 Uiso 1 1 d D . .
O3 O 0.5238(3) 0.3391(4) 0.2213(3) 0.102(2) Uani 1 1 d D . .
H3V H 0.573(2) 0.385(3) 0.242(3) 0.122 Uiso 0.50 1 d PD . .
H3W H 0.4635(8) 0.322(3) 0.223(4) 0.122 Uiso 1 1 d D . .
H3X H 0.5286(16) 0.2929(11) 0.240(3) 0.122 Uiso 0.50 1 d PD . .
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O8 Te O8 180.00(15) 2 8_556 ?
O8 Te O8 85.83(13) 2 7_556 ?
O8 Te O8 94.17(12) 8_556 7_556 ?
O8 Te O8 85.83(12) 2 9_556 ?
O8 Te O8 94.17(12) 8_556 9_556 ?
O8 Te O8 94.17(12) 7_556 9_556 ?
O8 Te O8 94.17(12) 2 3 ?
O8 Te O8 85.83(12) 8_556 3 ?
O8 Te O8 85.83(12) 7_556 3 ?
O8 Te O8 180.00(16) 9_556 3 ?
O8 Te O8 94.17(12) 2 . ?
O8 Te O8 85.83(13) 8_556 . ?
O8 Te O8 180.00(19) 7_556 . ?
O8 Te O8 85.83(12) 9_556 . ?
O8 Te O8 94.17(12) 3 . ?
O10 Mo O9 105.85(16) . . ?
O10 Mo O7 100.80(16) . 9_556 ?
O9 Mo O7 97.10(16) . 9_556 ?
O10 Mo O7 94.69(17) . . ?
O9 Mo O7 101.38(16) . . ?
O7 Mo O7 151.61(15) 9_556 . ?
O10 Mo O8 162.99(15) . 8_556 ?
O9 Mo O8 88.66(14) . 8_556 ?
O7 Mo O8 85.82(11) 9_556 8_556 ?
O7 Mo O8 73.35(11) . 8_556 ?
O10 Mo O8 97.02(14) . . ?
O9 Mo O8 156.60(13) . . ?
O7 Mo O8 73.40(12) 9_556 . ?
O7 Mo O8 81.25(12) . . ?
O8 Mo O8 69.65(15) 8_556 . ?
N1 Cu1 N1 98.10(19) 3_565 . ?
N1 Cu1 N1 98.1(2) 3_565 2_665 ?
N1 Cu1 N1 98.10(19) . 2_665 ?
N1 Cu1 N12 90.3(2) 3_565 . ?
N1 Cu1 N12 77.5(2) . . ?
N1 Cu1 N12 171.1(3) 2_665 . ?
N1 Cu1 N12 77.5(2) 3_565 3_565 ?
N1 Cu1 N12 171.1(3) . 3_565 ?
N1 Cu1 N12 90.3(2) 2_665 3_565 ?
N12 Cu1 N12 94.7(2) . 3_565 ?
N1 Cu1 N12 171.1(3) 3_565 2_665 ?
N1 Cu1 N12 90.3(2) . 2_665 ?
N1 Cu1 N12 77.5(2) 2_665 2_665 ?
N12 Cu1 N12 94.7(2) . 2_665 ?
N12 Cu1 N12 94.7(2) 3_565 2_665 ?
O1 Cu2 O1 89.5(2) 5 2 ?
O1 Cu2 O1 177.8(3) 5 3 ?
O1 Cu2 O1 92.10(14) 2 3 ?
O1 Cu2 O1 92.10(14) 5 6 ?
O1 Cu2 O1 177.8(3) 2 6 ?
O1 Cu2 O1 86.4(2) 3 6 ?
O1 Cu2 O1 86.4(2) 5 . ?
O1 Cu2 O1 92.10(14) 2 . ?
O1 Cu2 O1 92.10(14) 3 . ?
O1 Cu2 O1 89.5(2) 6 . ?
O1 Cu2 O1 92.10(14) 5 4 ?
O1 Cu2 O1 86.4(2) 2 4 ?
O1 Cu2 O1 89.5(2) 3 4 ?
O1 Cu2 O1 92.10(14) 6 4 ?
O1 Cu2 O1 177.8(3) . 4 ?
Mo O7 Mo 117.18(16) 8_556 . ?
Te O8 Mo 102.58(12) . 9_556 ?
Te O8 Mo 101.84(13) . . ?
Mo O8 Mo 91.76(11) 9_556 . ?
C2 N1 C6 117.5(6) . . ?
C2 N1 Cu1 128.8(5) . . ?
C6 N1 Cu1 113.6(4) . . ?
N1 C2 C3 122.1(7) . . ?
N1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C4 C3 C2 120.0(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 121.2(6) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C13 125.1(6) . . ?
C4 C5 C6 116.4(6) . . ?
C13 C5 C6 118.5(6) . . ?
N1 C6 C7 117.6(6) . . ?
N1 C6 C5 122.8(6) . . ?
C7 C6 C5 119.5(6) . . ?
N12 C7 C8 123.6(6) . . ?
N12 C7 C6 117.0(6) . . ?
C8 C7 C6 119.4(6) . . ?
C9 C8 C7 116.2(6) . . ?
C9 C8 C14 124.1(7) . . ?
C7 C8 C14 119.7(6) . . ?
C10 C9 C8 120.8(7) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 119.7(7) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
N12 C11 C10 122.2(7) . . ?
N12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 N12 C7 117.4(6) . . ?
C11 N12 Cu1 128.9(5) . . ?
C7 N12 Cu1 113.7(5) . . ?
C14 C13 C5 121.8(6) . . ?
C14 C13 H13 119.1 . . ?
C5 C13 H13 119.1 . . ?
C13 C14 C8 121.1(7) . . ?
C13 C14 H14 119.5 . . ?
C8 C14 H14 119.5 . . ?
Cu2 O1 H1W 126(3) . . ?
Cu2 O1 H1V 115.2(17) . . ?
H1W O1 H1V 90(4) . . ?
H2V O2 H2W 126(4) . . ?
H6V O6 H6W 94(4) . . ?
H5W O5 H5V 109(3) . . ?
H3V O3 H3W 132(5) . . ?
H3V O3 H3X 98(5) . . ?
H3W O3 H3X 106(4) . . ?
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
Te O8 1.927(3) 2 ?
Te O8 1.927(3) 8_556 ?
Te O8 1.927(3) 7_556 ?
Te O8 1.927(3) 9_556 ?
Te O8 1.927(3) 3 ?
Te O8 1.927(3) . ?
Mo O10 1.709(4) . ?
Mo O9 1.713(3) . ?
Mo O7 1.917(3) 9_556 ?
Mo O7 1.949(4) . ?
Mo O8 2.288(3) 8_556 ?
Mo O8 2.308(3) . ?
Cu1 N1 2.133(5) 3_565 ?
Cu1 N1 2.133(5) . ?
Cu1 N1 2.133(5) 2_665 ?
Cu1 N12 2.152(6) . ?
Cu1 N12 2.152(6) 3_565 ?
Cu1 N12 2.152(6) 2_665 ?
Cu2 O1 2.032(4) 5 ?
Cu2 O1 2.032(4) 2 ?
Cu2 O1 2.032(4) 3 ?
Cu2 O1 2.032(4) 6 ?
Cu2 O1 2.032(4) . ?
Cu2 O1 2.032(4) 4 ?
O7 Mo 1.917(3) 8_556 ?
O8 Mo 2.288(3) 9_556 ?
N1 C2 1.344(9) . ?
N1 C6 1.369(9) . ?
C2 C3 1.404(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.345(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(10) . ?
C4 H4 0.9500 . ?
C5 C13 1.429(10) . ?
C5 C6 1.431(9) . ?
C6 C7 1.428(9) . ?
C7 N12 1.361(8) . ?
C7 C8 1.404(10) . ?
C8 C9 1.395(10) . ?
C8 C14 1.435(9) . ?
C9 C10 1.343(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.399(11) . ?
C10 H10 0.9500 . ?
C11 N12 1.332(9) . ?
C11 H11 0.9500 . ?
C13 C14 1.327(10) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
O1 H1W 0.918(13) . ?
O1 H1V 0.950(13) . ?
O2 H2V 0.93(3) . ?
O2 H2W 0.95(6) . ?
O4 H4W 0.916(15) . ?
O6 H6V 0.969(13) . ?
O6 H6W 0.913(14) . ?
O5 H5W 0.915(15) . ?
O5 H5V 0.935(15) . ?
O3 H3V 0.92(2) . ?
O3 H3W 0.93(3) . ?
O3 H3X 0.921(15) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1W O8 0.918(13) 1.771(12) 2.683(5) 172(4) 2
O1 H1V O4 0.950(13) 1.647(16) 2.524(6) 152(3) 2
O2 H2V O10 0.93(3) 1.83(3) 2.754(7) 174(2) .
O2 H2W O5 0.95(6) 1.86(6) 2.813(8) 178(11) 5
O3 H3W O5 0.93(3) 1.83(3) 2.753(8) 170(7) .
O3 H3V O3 0.92(2) 1.70(2) 2.614(10) 176(7) 4_665
O3 H3X O3 0.921(15) 1.973(15) 2.889(12) 173(2) 6
O4 H4W O2 0.916(15) 1.504(15) 2.386(8) 160(3) .
O5 H5W O6 0.915(15) 1.81(3) 2.710(7) 167(5) .
O5 H5V O9 0.935(15) 2.03(3) 2.956(6) 171(5) 10
O6 H6W O4 0.913(14) 1.722(15) 2.629(7) 172(4) .
O6 H6V O1 0.969(13) 1.870(14) 2.836(7) 174(7) 2
