#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:47:49 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185344 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/95/7039566.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_7039566
loop_
_publ_author_name
'Rasmussen, Maren'
'Näther, Christian'
'van Leusen, Jan'
'Warzok, Ulrike'
'Schalley, Christoph A.'
'Kögerler, Paul'
'Bensch, Wolfgang'
_publ_section_title
;
 Small, beautiful and magnetically exotic: {V4W2}- and {V4W4}-type
 polyoxometalates.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10519
_journal_page_last               10522
_journal_paper_doi               10.1039/c6dt02282k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C16 H60 N12 O18 V4 W2'
_chemical_formula_weight         1280.22
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-21 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                100.764(9)
_cell_angle_beta                 108.148(9)
_cell_angle_gamma                100.314(9)
_cell_formula_units_Z            1
_cell_length_a                   8.4223(7)
_cell_length_b                   10.4091(8)
_cell_length_c                   11.8757(10)
_cell_measurement_temperature    200(2)
_cell_volume                     940.03(16)
_computing_cell_refinement       'X-Area (STOE)'
_computing_data_collection       'X-Area (STOE)'
_computing_data_reduction        'X-Area (STOE)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13222
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.132
_exptl_absorpt_correction_T_max  0.561
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.738
_refine_diff_density_min         -2.677
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.0154(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0347
_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)+(0.0731P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                4084
_reflns_number_total             4352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02282k2.cif
_cod_data_source_block           mr183tt
_cod_depositor_comments
'Adding full bibliography for 7039566--7039567.cif.'
_cod_original_cell_volume        940.03(13)
_cod_database_code               7039566
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.880792(19) 0.610865(14) 0.965727(13) 0.00962(10) Uani 1 1 d . . .
V1 V 0.66247(10) 0.47935(7) 0.69765(6) 0.01123(16) Uani 1 1 d . . .
V2 V 1.14914(10) 0.55600(7) 0.83460(7) 0.01150(16) Uani 1 1 d . . .
O1 O 0.6477(4) 0.5240(3) 0.8604(3) 0.0130(6) Uani 1 1 d . . .
O2 O 0.9030(4) 0.5362(3) 0.8003(3) 0.0113(6) Uani 1 1 d . . .
O3 O 1.1171(4) 0.6099(3) 1.0146(3) 0.0100(6) Uani 1 1 d . . .
O4 O 0.8960(5) 0.7804(3) 0.9633(3) 0.0185(7) Uani 1 1 d . . .
O5 O 0.8462(4) 0.6118(3) 1.1100(3) 0.0148(6) Uani 1 1 d . . .
O6 O 0.6175(5) 0.6019(4) 0.6354(3) 0.0197(7) Uani 1 1 d . . .
O7 O 1.1624(5) 0.5120(4) 0.7002(3) 0.0186(7) Uani 1 1 d . . .
N1 N 0.3952(5) 0.3666(4) 0.6241(4) 0.0171(8) Uani 1 1 d . . .
H1N H 0.3278 0.4240 0.6377 0.021 Uiso 1 1 calc R . .
H2N H 0.3627 0.3332 0.5406 0.021 Uiso 1 1 calc R . .
C1 C 0.3634(7) 0.2530(5) 0.6797(5) 0.0224(10) Uani 1 1 d . . .
H1A H 0.2452 0.1943 0.6340 0.027 Uiso 1 1 calc R . .
H1B H 0.3747 0.2880 0.7660 0.027 Uiso 1 1 calc R . .
C2 C 0.4949(7) 0.1740(5) 0.6738(5) 0.0226(10) Uani 1 1 d . . .
H2A H 0.4907 0.1072 0.7229 0.027 Uiso 1 1 calc R . .
H2B H 0.4685 0.1244 0.5878 0.027 Uiso 1 1 calc R . .
N2 N 0.6687(5) 0.2672(4) 0.7222(4) 0.0147(7) Uani 1 1 d . . .
H3N H 0.7165 0.2656 0.8028 0.018 Uiso 1 1 d R . .
C3 C 0.7895(7) 0.2166(5) 0.6686(5) 0.0202(9) Uani 1 1 d . . .
H3A H 0.7732 0.1184 0.6610 0.024 Uiso 1 1 calc R . .
H3B H 0.9103 0.2632 0.7223 0.024 Uiso 1 1 calc R . .
C4 C 0.7531(8) 0.2441(5) 0.5423(4) 0.0232(10) Uani 1 1 d . . .
H4A H 0.8467 0.2286 0.5118 0.028 Uiso 1 1 calc R . .
H4B H 0.6430 0.1818 0.4835 0.028 Uiso 1 1 calc R . .
N3 N 0.7421(6) 0.3859(4) 0.5515(4) 0.0206(8) Uani 1 1 d . . .
H4N H 0.6658 0.3893 0.4780 0.025 Uiso 1 1 calc R . .
H5N H 0.8488 0.4375 0.5616 0.025 Uiso 1 1 calc R . .
N11 N 1.4120(5) 0.6297(4) 0.9498(4) 0.0157(7) Uani 1 1 d . . .
H11N H 1.4284 0.6026 1.0211 0.019 Uiso 1 1 calc R . .
H12N H 1.4794 0.5938 0.9112 0.019 Uiso 1 1 calc R . .
C11 C 1.4664(7) 0.7797(5) 0.9799(5) 0.0233(10) Uani 1 1 d . . .
H11A H 1.5927 0.8105 1.0006 0.028 Uiso 1 1 calc R . .
H11B H 1.4382 0.8196 1.0515 0.028 Uiso 1 1 calc R . .
C12 C 1.3714(7) 0.8239(5) 0.8692(5) 0.0228(10) Uani 1 1 d . . .
H12A H 1.3981 0.9238 0.8882 0.027 Uiso 1 1 calc R . .
H12B H 1.4068 0.7904 0.7995 0.027 Uiso 1 1 calc R . .
N12 N 1.1843(5) 0.7667(4) 0.8376(4) 0.0160(8) Uani 1 1 d . . .
H13N H 1.1516 0.8159 0.8955 0.019 Uiso 1 1 d R . .
C13 C 1.0727(7) 0.7872(5) 0.7225(5) 0.0214(10) Uani 1 1 d . B .
H13A H 0.9506 0.7497 0.7116 0.026 Uiso 1 1 calc R . .
H13B H 1.0956 0.7349 0.6532 0.026 Uiso 1 1 calc R . .
C14 C 1.0961(8) 0.9340(5) 0.7158(6) 0.0283(12) Uani 1 1 d . . .
H14A H 1.0789 0.9896 0.7862 0.034 Uiso 0.80 1 calc PR A 1
H14B H 1.2139 0.9713 0.7178 0.034 Uiso 0.80 1 calc PR A 1
H14C H 1.2105 0.9645 0.7095 0.034 Uiso 0.20 1 d PR A 2
H14D H 1.0079 0.9360 0.6387 0.034 Uiso 0.20 1 d PR A 2
N13 N 0.9700(9) 0.9350(6) 0.6030(6) 0.0299(13) Uani 0.80 1 d P B 1
H14N H 0.8672 0.9197 0.6164 0.045 Uiso 0.80 1 d PR B 1
H15N H 1.0013 1.0199 0.5923 0.045 Uiso 0.80 1 d PR B 1
N13' N 1.086(4) 1.025(3) 0.808(3) 0.041(7) Uiso 0.20 1 d P B 2
O8 O 0.7889(6) 1.0137(4) 0.9171(4) 0.0342(9) Uani 1 1 d . . .
H1O H 0.8541 1.0891 0.9614 0.051 Uiso 1 1 d R . .
H2O H 0.8299 0.9489 0.9341 0.051 Uiso 1 1 d R . .
O9 O 0.6387(7) 0.8747(4) 0.6685(4) 0.0404(11) Uani 1 1 d . . .
H3O H 0.7017 0.9168 0.7409 0.061 Uiso 1 1 d R . .
H4O H 0.6391 0.7971 0.6786 0.061 Uiso 1 1 d 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'
N N 0.0061 0.0033 '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'
V V 0.3005 0.5294 '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
O4 W1 O5 101.03(15) . .
O4 W1 O3 100.49(16) . .
O5 W1 O3 99.96(14) . .
O4 W1 O1 102.61(16) . .
O5 W1 O1 96.56(15) . .
O3 W1 O1 148.34(14) . .
O4 W1 O2 99.78(15) . .
O5 W1 O2 159.06(14) . .
O3 W1 O2 78.39(13) . .
O1 W1 O2 76.60(13) . .
O4 W1 O3 174.76(14) . 2_767
O5 W1 O3 76.56(12) . 2_767
O3 W1 O3 75.54(13) . 2_767
O1 W1 O3 82.36(12) . 2_767
O2 W1 O3 82.88(12) . 2_767
O4 W1 V1 98.60(12) . .
O5 W1 V1 134.27(11) . .
O3 W1 V1 116.45(9) . .
O1 W1 V1 38.62(10) . .
O2 W1 V1 38.70(9) . .
O3 W1 V1 86.30(7) 2_767 .
O6 V1 O2 107.31(16) . .
O6 V1 O1 106.91(17) . .
O2 V1 O1 78.76(13) . .
O6 V1 N1 92.26(17) . .
O2 V1 N1 159.40(15) . .
O1 V1 N1 89.61(14) . .
O6 V1 N3 93.25(18) . .
O2 V1 N3 87.22(15) . .
O1 V1 N3 158.08(16) . .
N1 V1 N3 98.29(17) . .
O6 V1 N2 161.37(16) . .
O2 V1 N2 87.16(14) . .
O1 V1 N2 87.06(14) . .
N1 V1 N2 75.20(15) . .
N3 V1 N2 75.39(15) . .
O6 V1 W1 106.42(12) . .
O2 V1 W1 41.81(9) . .
O1 V1 W1 37.69(9) . .
N1 V1 W1 126.94(11) . .
N3 V1 W1 128.55(13) . .
N2 V1 W1 92.18(10) . .
O7 V2 O2 104.05(16) . .
O7 V2 O5 102.15(16) . 2_767
O2 V2 O5 94.65(14) . 2_767
O7 V2 N11 102.16(18) . .
O2 V2 N11 152.73(15) . .
O5 V2 N11 87.06(15) 2_767 .
O7 V2 N12 94.04(17) . .
O2 V2 N12 90.37(15) . .
O5 V2 N12 161.30(15) 2_767 .
N11 V2 N12 80.37(16) . .
O7 V2 O3 177.08(16) . .
O2 V2 O3 73.28(12) . .
O5 V2 O3 77.06(12) 2_767 .
N11 V2 O3 80.65(14) . .
N12 V2 O3 87.22(13) . .
W1 O1 V1 103.68(15) . .
V1 O2 V2 154.64(18) . .
V1 O2 W1 99.49(14) . .
V2 O2 W1 105.81(14) . .
W1 O3 V2 101.48(13) . .
W1 O3 W1 104.46(13) . 2_767
V2 O3 W1 89.92(11) . 2_767
W1 O5 V2 116.35(17) . 2_767
C1 N1 V1 112.5(3) . .
N1 C1 C2 107.7(4) . .
N2 C2 C1 109.5(4) . .
C2 N2 C3 113.1(4) . .
C2 N2 V1 112.4(3) . .
C3 N2 V1 109.4(3) . .
N2 C3 C4 108.4(4) . .
N3 C4 C3 109.3(4) . .
C4 N3 V1 116.9(3) . .
C11 N11 V2 111.0(3) . .
N11 C11 C12 108.1(4) . .
N12 C12 C11 107.5(4) . .
C13 N12 C12 114.6(4) . .
C13 N12 V2 112.1(3) . .
C12 N12 V2 106.9(3) . .
N12 C13 C14 115.0(4) . .
N13' C14 N13 109.0(15) . .
N13' C14 C13 118.1(14) . .
N13 C14 C13 107.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O4 1.752(3) .
W1 O5 1.824(3) .
W1 O3 1.894(3) .
W1 O1 1.910(3) .
W1 O2 2.052(3) .
W1 O3 2.356(3) 2_767
W1 V1 3.0355(8) .
V1 O6 1.633(4) .
V1 O2 1.924(3) .
V1 O1 1.950(3) .
V1 N1 2.157(4) .
V1 N3 2.176(4) .
V1 N2 2.289(4) .
V2 O7 1.620(3) .
V2 O2 1.948(3) .
V2 O5 1.981(3) 2_767
V2 N11 2.116(4) .
V2 N12 2.152(4) .
V2 O3 2.219(3) .
O3 W1 2.356(3) 2_767
O5 V2 1.981(3) 2_767
N1 C1 1.482(6) .
C1 C2 1.504(8) .
C2 N2 1.474(6) .
N2 C3 1.479(6) .
C3 C4 1.528(7) .
C4 N3 1.481(6) .
N11 C11 1.486(6) .
C11 C12 1.510(8) .
C12 N12 1.480(6) .
N12 C13 1.476(6) .
C13 C14 1.525(7) .
C14 N13' 1.34(3) .
C14 N13 1.430(8) .
