# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_author_name A.Mahammad
_publ_contact_author_name 'Mahammad, Ali'
_publ_contact_author_email 'm ali2062@yahoo.com'
data_in73
_database_code_depnum_ccdc_archive 'CCDC 775686'
#TrackingRef '- compound1-c.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C4 H32 Cu2 Mo6 N2 Na4 O42 Te'
_chemical_formula_sum 'C4 H32 Cu2 Mo6 N2 Na4 O42 Te'
_chemical_formula_weight 1702.60
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'
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'
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.1526(5)
_cell_length_b 10.6481(6)
_cell_length_c 14.2288(9)
_cell_angle_alpha 73.573(5)
_cell_angle_beta 78.822(5)
_cell_angle_gamma 78.197(5)
_cell_volume 1006.74(11)
_cell_formula_units_Z 1
_cell_measurement_temperature 120(2)
_cell_measurement_reflns_used 6731
_cell_measurement_theta_min 3.7613
_cell_measurement_theta_max 32.1632
_exptl_crystal_description prism
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.808
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 812
_exptl_absorpt_coefficient_mu 3.720
_exptl_absorpt_correction_T_min 0.31866
_exptl_absorpt_correction_T_max 0.69258
_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_special_details
;
?
;
_diffrn_ambient_temperature 120(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'Enhance (Oxford Diffraction)'
_diffrn_measurement_device_type 'KUMA + CCD'
_diffrn_measurement_method 'rotation method, \w--scan'
_diffrn_detector_area_resol_mean 8.3611
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 6905
_diffrn_reflns_av_R_equivalents 0.0159
_diffrn_reflns_av_sigmaI/netI 0.0144
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 3.78
_diffrn_reflns_theta_max 25.04
_reflns_number_total 3549
_reflns_number_gt 3348
_reflns_threshold_expression >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
C-bound and N-bound H-atoms were included in the riding model approximation
with distances of 0.99 \%A (CH~2~) and 0.92 \%A (NH~2~), and with
U~iso~(H) values of 1.2U~eq~(CH~2~, CH~2~). 12 O-bound H atoms
were refined, with the O---H distances restrained to 0.95(2) \%A and with
U~iso~(H) values of 1.5U~eq~(O~water~).
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3549
_refine_ls_number_parameters 323
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.0265
_refine_ls_R_factor_gt 0.0246
_refine_ls_wR_factor_ref 0.0636
_refine_ls_wR_factor_gt 0.0624
_refine_ls_goodness_of_fit_ref 0.902
_refine_ls_restrained_S_all 0.901
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.5000 0.5000 0.5000 0.00557(9) Uani 1 2 d S . .
Mo1 Mo 0.52633(4) 0.21597(3) 0.44831(2) 0.00654(9) Uani 1 1 d . . .
Mo2 Mo 0.60999(4) 0.47925(3) 0.27046(2) 0.00683(9) Uani 1 1 d . . .
Mo3 Mo 0.41490(4) 0.23364(3) 0.67905(2) 0.00706(9) Uani 1 1 d . . .
Cu Cu 0.05440(6) 0.24697(4) 0.35742(3) 0.00866(11) Uani 1 1 d . . .
O1 O 0.1080(4) 0.2770(3) 0.21258(19) 0.0114(5) Uani 1 1 d . . .
O2 O 0.0691(5) 0.1979(3) 0.0905(2) 0.0212(7) Uani 1 1 d . . .
N3 N 0.0490(5) 0.0641(3) 0.3543(2) 0.0105(6) Uani 1 1 d . . .
H3A H 0.1659 0.0120 0.3661 0.013 Uiso 1 1 calc R . .
H3B H -0.0454 0.0292 0.4027 0.013 Uiso 1 1 calc R . .
C1 C 0.0679(6) 0.1885(4) 0.1794(3) 0.0129(8) Uani 1 1 d . . .
C2 C 0.0094(6) 0.0651(4) 0.2561(3) 0.0135(8) Uani 1 1 d . . .
H2A H -0.1299 0.0644 0.2591 0.016 Uiso 1 1 calc R . .
H2B H 0.0826 -0.0154 0.2366 0.016 Uiso 1 1 calc R . .
O4 O 0.0006(4) 0.2105(3) 0.50460(19) 0.0105(5) Uani 1 1 d D . .
H4V H -0.113(4) 0.243(4) 0.541(3) 0.016 Uiso 1 1 d D . .
H4W H 0.101(5) 0.215(5) 0.536(3) 0.016 Uiso 1 1 d D . .
O5 O 0.0702(4) 0.4368(3) 0.3460(2) 0.0104(5) Uani 1 1 d D . .
H5V H 0.164(5) 0.453(5) 0.378(3) 0.016 Uiso 1 1 d D . .
H5W H -0.048(4) 0.483(4) 0.369(3) 0.016 Uiso 1 1 d D . .
O6 O 0.3837(4) 0.1913(3) 0.37300(19) 0.0098(5) Uani 1 1 d . . .
O7 O 0.6793(4) 0.0718(3) 0.4841(2) 0.0109(5) Uani 1 1 d . . .
O8 O 0.7147(4) 0.3074(2) 0.34731(19) 0.0090(5) Uani 1 1 d . . .
O9 O 0.3321(4) 0.2094(3) 0.56483(19) 0.0096(5) Uani 1 1 d . . .
O10 O 0.6264(4) 0.3195(2) 0.54328(19) 0.0072(5) Uani 1 1 d . . .
O11 O 0.4659(4) 0.4361(3) 0.2047(2) 0.0113(6) Uani 1 1 d . . .
O12 O 0.8151(4) 0.5129(3) 0.18994(19) 0.0109(5) Uani 1 1 d . . .
O13 O 0.4811(4) 0.6616(3) 0.25815(19) 0.0101(5) Uani 1 1 d . . .
O14 O 0.6998(4) 0.5483(3) 0.38989(19) 0.0086(5) Uani 1 1 d . . .
O15 O 0.3939(4) 0.4376(3) 0.41061(18) 0.0074(5) Uani 1 1 d . . .
O16 O 0.2066(4) 0.2078(3) 0.7594(2) 0.0130(6) Uani 1 1 d . . .
O17 O 0.5747(4) 0.0905(3) 0.7094(2) 0.0128(6) Uani 1 1 d . . .
Na1 Na 0.1520(2) 0.49870(15) 0.16337(11) 0.0128(3) Uani 1 1 d . . .
Na2 Na 0.2827(3) 0.78924(18) -0.01495(13) 0.0286(4) Uani 1 1 d . . .
O20 O 0.4293(5) 0.8447(3) -0.1758(2) 0.0198(6) Uani 1 1 d D A .
H20V H 0.477(7) 0.924(3) -0.211(3) 0.030 Uiso 1 1 d D . .
H20W H 0.481(7) 0.780(4) -0.210(4) 0.030 Uiso 1 1 d D . .
O21 O 0.1705(4) 0.7207(3) 0.1577(2) 0.0154(6) Uani 1 1 d D . .
H21V H 0.048(4) 0.745(5) 0.189(3) 0.023 Uiso 1 1 d D . .
H21W H 0.257(6) 0.718(5) 0.199(3) 0.023 Uiso 1 1 d D . .
O22 O 0.2095(6) 0.5707(4) -0.0078(2) 0.0326(8) Uani 1 1 d D . .
H22V H 0.093(5) 0.579(6) -0.031(5) 0.049 Uiso 1 1 d D . .
H22W H 0.290(8) 0.498(4) -0.027(5) 0.049 Uiso 1 1 d D . .
O23 O 0.5950(6) 0.7033(4) 0.0297(3) 0.0378(9) Uani 1 1 d D A .
H23V H 0.705(6) 0.741(6) -0.007(4) 0.057 Uiso 1 1 d D . .
H23W H 0.620(10) 0.719(7) 0.087(3) 0.057 Uiso 1 1 d D . .
O24A O 0.181(3) 1.0187(7) -0.0341(5) 0.048(5) Uani 0.54(3) 1 d P A 1
O24B O 0.301(4) 1.000(2) -0.008(3) 0.127(11) Uani 0.46(3) 1 d P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te 0.00663(17) 0.00451(17) 0.00627(17) -0.00320(13) 0.00041(12) -0.00110(13)
Mo1 0.00719(16) 0.00522(16) 0.00804(17) -0.00376(12) 0.00021(12) -0.00115(12)
Mo2 0.00775(16) 0.00667(17) 0.00677(17) -0.00367(12) 0.00009(12) -0.00101(12)
Mo3 0.00835(17) 0.00546(16) 0.00748(17) -0.00290(12) 0.00057(12) -0.00119(12)
Cu 0.0109(2) 0.0072(2) 0.0088(2) -0.00403(17) -0.00007(17) -0.00175(18)
O1 0.0137(13) 0.0091(13) 0.0113(13) -0.0035(11) 0.0000(11) -0.0023(11)
O2 0.0353(18) 0.0192(15) 0.0113(15) -0.0061(12) -0.0002(13) -0.0090(14)
N3 0.0106(16) 0.0092(15) 0.0110(16) -0.0017(13) -0.0007(13) -0.0018(13)
C1 0.0130(19) 0.0123(19) 0.014(2) -0.0072(16) -0.0004(15) 0.0002(15)
C2 0.018(2) 0.0114(19) 0.0127(19) -0.0046(16) -0.0029(16) -0.0032(16)
O4 0.0089(13) 0.0135(14) 0.0093(13) -0.0046(11) 0.0001(10) -0.0012(11)
O5 0.0090(13) 0.0107(13) 0.0130(13) -0.0056(11) -0.0013(11) -0.0017(11)
O6 0.0093(13) 0.0113(13) 0.0099(13) -0.0045(11) -0.0005(10) -0.0026(10)
O7 0.0102(13) 0.0101(13) 0.0124(14) -0.0044(11) 0.0013(11) -0.0026(11)
O8 0.0094(13) 0.0074(12) 0.0105(13) -0.0037(10) -0.0010(10) -0.0006(10)
O9 0.0087(13) 0.0103(13) 0.0110(13) -0.0051(11) 0.0012(10) -0.0037(10)
O10 0.0077(12) 0.0057(12) 0.0080(12) -0.0031(10) 0.0007(10) 0.0000(10)
O11 0.0136(13) 0.0107(13) 0.0105(13) -0.0044(11) -0.0025(11) -0.0006(11)
O12 0.0111(13) 0.0103(13) 0.0111(13) -0.0034(11) -0.0008(11) -0.0010(11)
O13 0.0106(13) 0.0098(13) 0.0103(13) -0.0045(10) -0.0019(10) 0.0005(10)
O14 0.0065(12) 0.0082(13) 0.0116(13) -0.0039(10) 0.0003(10) -0.0016(10)
O15 0.0069(12) 0.0090(13) 0.0072(12) -0.0045(10) 0.0011(10) -0.0016(10)
O16 0.0140(14) 0.0145(14) 0.0110(13) -0.0055(11) 0.0013(11) -0.0029(11)
O17 0.0141(14) 0.0107(13) 0.0138(14) -0.0052(11) -0.0018(11) 0.0006(11)
Na1 0.0129(8) 0.0124(8) 0.0135(8) -0.0026(6) -0.0017(6) -0.0038(6)
Na2 0.0437(12) 0.0207(9) 0.0180(9) -0.0041(7) 0.0080(8) -0.0107(8)
O20 0.0262(17) 0.0154(15) 0.0167(15) -0.0061(12) 0.0038(13) -0.0051(13)
O21 0.0119(14) 0.0185(15) 0.0159(15) -0.0076(12) -0.0006(11) 0.0004(12)
O22 0.049(2) 0.036(2) 0.0163(16) -0.0095(15) 0.0007(16) -0.0167(18)
O23 0.043(2) 0.046(2) 0.0211(18) 0.0012(17) -0.0045(16) -0.0131(19)
O24A 0.110(12) 0.015(4) 0.013(4) -0.002(3) 0.003(4) -0.010(5)
O24B 0.084(14) 0.088(11) 0.23(2) -0.127(14) 0.103(15) -0.058(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O15 1.922(2) . ?
Te O15 1.922(2) 2_666 ?
Te O10 1.930(3) . ?
Te O10 1.930(2) 2_666 ?
Te O14 1.933(3) . ?
Te O14 1.933(3) 2_666 ?
Mo1 O7 1.703(3) . ?
Mo1 O6 1.718(3) . ?
Mo1 O9 1.940(3) . ?
Mo1 O8 1.955(3) . ?
Mo1 O10 2.257(3) . ?
Mo1 O15 2.307(3) . ?
Mo2 O12 1.710(3) . ?
Mo2 O11 1.721(3) . ?
Mo2 O8 1.931(3) . ?
Mo2 O13 1.947(3) . ?
Mo2 O15 2.269(2) . ?
Mo2 O14 2.272(3) . ?
Mo3 O17 1.709(3) . ?
Mo3 O16 1.713(3) . ?
Mo3 O9 1.932(3) . ?
Mo3 O13 1.938(3) 2_666 ?
Mo3 O14 2.296(3) 2_666 ?
Mo3 O10 2.300(3) . ?
Cu O1 1.967(3) . ?
Cu N3 1.969(3) . ?
Cu O4 1.993(3) . ?
Cu O5 2.006(3) . ?
Cu O6 2.346(3) . ?
Cu O8 2.404(3) 1_455 ?
Cu Na1 3.3359(16) . ?
O1 C1 1.268(5) . ?
O1 Na1 2.333(3) . ?
O2 C1 1.239(5) . ?
O2 Na2 2.886(4) 2_565 ?
N3 C2 1.475(5) . ?
N3 H3A 0.9200 . ?
N3 H3B 0.9200 . ?
C1 C2 1.526(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O4 H4V 0.93(4) . ?
O4 H4W 0.93(4) . ?
O5 Na1 2.476(3) . ?
O5 H5V 0.95(4) . ?
O5 H5W 0.94(4) . ?
O8 Cu 2.404(3) 1_655 ?
O11 Na1 2.347(3) . ?
O12 Na1 2.346(3) 1_655 ?
O13 Mo3 1.938(3) 2_666 ?
O14 Mo3 2.296(3) 2_666 ?
Na1 O22 2.318(4) . ?
Na1 O12 2.346(3) 1_455 ?
Na1 O21 2.373(3) . ?
Na2 O20 2.291(3) . ?
Na2 O24B 2.310(13) . ?
Na2 O24A 2.355(8) . ?
Na2 O23 2.370(5) . ?
Na2 O21 2.382(3) . ?
Na2 O22 2.458(4) . ?
Na2 O2 2.886(4) 2_565 ?
O20 H20V 0.94(5) . ?
O20 H20W 0.93(5) . ?
O21 H21V 0.92(2) . ?
O21 H21W 0.92(2) . ?
O22 H22V 0.94(2) . ?
O22 H22W 0.94(5) . ?
O23 H23V 0.95(5) . ?
O23 H23W 0.93(6) . ?
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
O15 Te O15 180 . 2_666 ?
O15 Te O10 86.22(11) . . ?
O15 Te O10 93.78(11) 2_666 . ?
O15 Te O10 93.78(11) . 2_666 ?
O15 Te O10 86.22(11) 2_666 2_666 ?
O10 Te O10 180 . 2_666 ?
O15 Te O14 85.68(11) . . ?
O15 Te O14 94.32(11) 2_666 . ?
O10 Te O14 94.47(11) . . ?
O10 Te O14 85.53(11) 2_666 . ?
O15 Te O14 94.32(11) . 2_666 ?
O15 Te O14 85.68(11) 2_666 2_666 ?
O10 Te O14 85.53(11) . 2_666 ?
O10 Te O14 94.47(11) 2_666 2_666 ?
O14 Te O14 180 . 2_666 ?
O7 Mo1 O6 107.88(12) . . ?
O7 Mo1 O9 101.56(12) . . ?
O6 Mo1 O9 96.77(12) . . ?
O7 Mo1 O8 96.30(12) . . ?
O6 Mo1 O8 99.43(12) . . ?
O9 Mo1 O8 150.86(11) . . ?
O7 Mo1 O10 94.01(11) . . ?
O6 Mo1 O10 157.69(11) . . ?
O9 Mo1 O10 74.08(10) . . ?
O8 Mo1 O10 81.92(10) . . ?
O7 Mo1 O15 162.27(11) . . ?
O6 Mo1 O15 88.44(11) . . ?
O9 Mo1 O15 82.79(10) . . ?
O8 Mo1 O15 73.64(10) . . ?
O10 Mo1 O15 70.45(9) . . ?
O12 Mo2 O11 105.79(13) . . ?
O12 Mo2 O8 97.93(12) . . ?
O11 Mo2 O8 101.30(12) . . ?
O12 Mo2 O13 97.47(12) . . ?
O11 Mo2 O13 96.70(12) . . ?
O8 Mo2 O13 152.09(11) . . ?
O12 Mo2 O15 162.55(11) . . ?
O11 Mo2 O15 91.33(11) . . ?
O8 Mo2 O15 74.95(10) . . ?
O13 Mo2 O15 83.53(10) . . ?
O12 Mo2 O14 92.93(11) . . ?
O11 Mo2 O14 160.14(11) . . ?
O8 Mo2 O14 82.18(10) . . ?
O13 Mo2 O14 73.91(10) . . ?
O15 Mo2 O14 70.51(9) . . ?
O17 Mo3 O16 105.60(13) . . ?
O17 Mo3 O9 100.52(12) . . ?
O16 Mo3 O9 97.15(12) . . ?
O17 Mo3 O13 97.34(12) . 2_666 ?
O16 Mo3 O13 100.01(12) . 2_666 ?
O9 Mo3 O13 150.85(11) . 2_666 ?
O17 Mo3 O14 159.70(11) . 2_666 ?
O16 Mo3 O14 93.96(11) . 2_666 ?
O9 Mo3 O14 81.99(10) . 2_666 ?
O13 Mo3 O14 73.51(10) 2_666 2_666 ?
O17 Mo3 O10 91.66(11) . . ?
O16 Mo3 O10 161.69(11) . . ?
O9 Mo3 O10 73.22(10) . . ?
O13 Mo3 O10 83.45(10) 2_666 . ?
O14 Mo3 O10 69.61(9) 2_666 . ?
O1 Cu N3 83.44(12) . . ?
O1 Cu O4 178.22(11) . . ?
N3 Cu O4 94.79(12) . . ?
O1 Cu O5 90.85(11) . . ?
N3 Cu O5 174.21(12) . . ?
O4 Cu O5 90.92(11) . . ?
O1 Cu O6 92.42(10) . . ?
N3 Cu O6 90.21(11) . . ?
O4 Cu O6 87.40(10) . . ?
O5 Cu O6 89.07(10) . . ?
O1 Cu O8 89.58(10) . 1_455 ?
N3 Cu O8 91.18(11) . 1_455 ?
O4 Cu O8 90.63(10) . 1_455 ?
O5 Cu O8 89.74(10) . 1_455 ?
O6 Cu O8 177.68(9) . 1_455 ?
O1 Cu Na1 43.29(8) . . ?
N3 Cu Na1 126.65(10) . . ?
O4 Cu Na1 138.47(8) . . ?
O5 Cu Na1 47.61(8) . . ?
O6 Cu Na1 89.63(7) . . ?
O8 Cu Na1 91.03(7) 1_455 . ?
C1 O1 Cu 115.0(2) . . ?
C1 O1 Na1 141.1(3) . . ?
Cu O1 Na1 101.41(11) . . ?
C1 O2 Na2 120.9(3) . 2_565 ?
C2 N3 Cu 109.0(2) . . ?
C2 N3 H3A 109.9 . . ?
Cu N3 H3A 109.9 . . ?
C2 N3 H3B 109.9 . . ?
Cu N3 H3B 109.9 . . ?
H3A N3 H3B 108.3 . . ?
O2 C1 O1 124.3(4) . . ?
O2 C1 C2 119.1(3) . . ?
O1 C1 C2 116.5(3) . . ?
N3 C2 C1 110.0(3) . . ?
N3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N3 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
Cu O4 H4V 126(3) . . ?
Cu O4 H4W 116(3) . . ?
H4V O4 H4W 106(4) . . ?
Cu O5 Na1 95.62(11) . . ?
Cu O5 H5V 117(3) . . ?
Na1 O5 H5V 112(3) . . ?
Cu O5 H5W 112(3) . . ?
Na1 O5 H5W 113(3) . . ?
H5V O5 H5W 106(4) . . ?
Mo1 O6 Cu 135.16(14) . . ?
Mo2 O8 Mo1 114.68(13) . . ?
Mo2 O8 Cu 121.26(12) . 1_655 ?
Mo1 O8 Cu 120.82(12) . 1_655 ?
Mo3 O9 Mo1 115.48(13) . . ?
Te O10 Mo1 102.42(11) . . ?
Te O10 Mo3 102.40(11) . . ?
Mo1 O10 Mo3 91.87(9) . . ?
Mo2 O11 Na1 139.10(15) . . ?
Mo2 O12 Na1 148.31(15) . 1_655 ?
Mo3 O13 Mo2 116.10(13) 2_666 . ?
Te O14 Mo2 101.65(11) . . ?
Te O14 Mo3 102.46(11) . 2_666 ?
Mo2 O14 Mo3 92.36(9) . 2_666 ?
Te O15 Mo2 102.13(11) . . ?
Te O15 Mo1 100.92(11) . . ?
Mo2 O15 Mo1 91.31(9) . . ?
O22 Na1 O1 110.68(13) . . ?
O22 Na1 O12 100.77(13) . 1_455 ?
O1 Na1 O12 76.83(10) . 1_455 ?
O22 Na1 O11 102.19(13) . . ?
O1 Na1 O11 90.19(11) . . ?
O12 Na1 O11 156.45(12) 1_455 . ?
O22 Na1 O21 84.08(12) . . ?
O1 Na1 O21 165.08(12) . . ?
O12 Na1 O21 98.86(11) 1_455 . ?
O11 Na1 O21 88.66(11) . . ?
O22 Na1 O5 175.54(14) . . ?
O1 Na1 O5 72.04(10) . . ?
O12 Na1 O5 76.22(10) 1_455 . ?
O11 Na1 O5 81.15(10) . . ?
O21 Na1 O5 93.09(11) . . ?
O22 Na1 Cu 145.95(11) . . ?
O1 Na1 Cu 35.30(7) . . ?
O12 Na1 Cu 74.35(8) 1_455 . ?
O11 Na1 Cu 83.67(8) . . ?
O21 Na1 Cu 129.86(9) . . ?
O5 Na1 Cu 36.77(6) . . ?
O22 Na1 Na2 43.25(10) . . ?
O1 Na1 Na2 153.38(9) . . ?
O12 Na1 Na2 109.30(9) 1_455 . ?
O11 Na1 Na2 91.14(9) . . ?
O21 Na1 Na2 41.53(8) . . ?
O5 Na1 Na2 134.36(9) . . ?
Cu Na1 Na2 170.33(6) . . ?
O20 Na2 O24B 87.3(7) . . ?
O20 Na2 O24A 86.0(3) . . ?
O24B Na2 O24A 23.9(7) . . ?
O20 Na2 O23 87.27(13) . . ?
O24B Na2 O23 92.7(10) . . ?
O24A Na2 O23 116.5(5) . . ?
O20 Na2 O21 172.69(15) . . ?
O24B Na2 O21 93.0(8) . . ?
O24A Na2 O21 97.3(2) . . ?
O23 Na2 O21 85.42(13) . . ?
O20 Na2 O22 99.64(13) . . ?
O24B Na2 O22 170.6(4) . . ?
O24A Na2 O22 149.4(5) . . ?
O23 Na2 O22 93.99(15) . . ?
O21 Na2 O22 80.92(12) . . ?
O20 Na2 O2 87.77(12) . 2_565 ?
O24B Na2 O2 107.8(10) . 2_565 ?
O24A Na2 O2 83.9(4) . 2_565 ?
O23 Na2 O2 158.60(14) . 2_565 ?
O21 Na2 O2 99.07(11) . 2_565 ?
O22 Na2 O2 66.39(12) . 2_565 ?
O20 Na2 Na1 137.67(10) . . ?
O24B Na2 Na1 134.3(8) . . ?
O24A Na2 Na1 134.5(3) . . ?
O23 Na2 Na1 83.98(11) . . ?
O21 Na2 Na1 41.34(8) . . ?
O22 Na2 Na1 40.25(9) . . ?
O2 Na2 Na1 85.75(8) 2_565 . ?
Na2 O20 H20V 129(3) . . ?
Na2 O20 H20W 121(3) . . ?
H20V O20 H20W 109(5) . . ?
Na1 O21 Na2 97.13(12) . . ?
Na1 O21 H21V 99(3) . . ?
Na2 O21 H21V 126(3) . . ?
Na1 O21 H21W 108(3) . . ?
Na2 O21 H21W 115(3) . . ?
H21V O21 H21W 108(4) . . ?
Na1 O22 Na2 96.49(13) . . ?
Na1 O22 H22V 108(4) . . ?
Na2 O22 H22V 111(4) . . ?
Na1 O22 H22W 104(4) . . ?
Na2 O22 H22W 130(4) . . ?
H22V O22 H22W 106(6) . . ?
Na2 O23 H23V 121(4) . . ?
Na2 O23 H23W 117(4) . . ?
H23V O23 H23W 90(6) . . ?
loop_
_geom_torsion_atom_site_label_1
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_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
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_geom_torsion_publ_flag
N3 Cu O1 C1 17.2(3) . . . . ?
O5 Cu O1 C1 -163.7(3) . . . . ?
O6 Cu O1 C1 107.2(3) . . . . ?
O8 Cu O1 C1 -74.0(3) 1_455 . . . ?
Na1 Cu O1 C1 -165.9(3) . . . . ?
N3 Cu O1 Na1 -176.82(14) . . . . ?
O5 Cu O1 Na1 2.22(12) . . . . ?
O6 Cu O1 Na1 -86.89(11) . . . . ?
O8 Cu O1 Na1 91.95(11) 1_455 . . . ?
O1 Cu N3 C2 -22.1(2) . . . . ?
O4 Cu N3 C2 158.1(2) . . . . ?
O6 Cu N3 C2 -114.5(2) . . . . ?
O8 Cu N3 C2 67.4(2) 1_455 . . . ?
Na1 Cu N3 C2 -24.8(3) . . . . ?
Na2 O2 C1 O1 -114.5(4) 2_565 . . . ?
Na2 O2 C1 C2 63.7(4) 2_565 . . . ?
Cu O1 C1 O2 170.8(3) . . . . ?
Na1 O1 C1 O2 13.0(7) . . . . ?
Cu O1 C1 C2 -7.5(4) . . . . ?
Na1 O1 C1 C2 -165.2(3) . . . . ?
Cu N3 C2 C1 23.5(4) . . . . ?
O2 C1 C2 N3 170.6(3) . . . . ?
O1 C1 C2 N3 -11.1(5) . . . . ?
O1 Cu O5 Na1 -2.06(11) . . . . ?
O4 Cu O5 Na1 177.74(11) . . . . ?
O6 Cu O5 Na1 90.35(10) . . . . ?
O8 Cu O5 Na1 -91.63(10) 1_455 . . . ?
O7 Mo1 O6 Cu 136.83(18) . . . . ?
O9 Mo1 O6 Cu 32.3(2) . . . . ?
O8 Mo1 O6 Cu -123.35(19) . . . . ?
O10 Mo1 O6 Cu -31.7(4) . . . . ?
O15 Mo1 O6 Cu -50.22(19) . . . . ?
O1 Cu O6 Mo1 144.1(2) . . . . ?
N3 Cu O6 Mo1 -132.4(2) . . . . ?
O4 Cu O6 Mo1 -37.6(2) . . . . ?
O5 Cu O6 Mo1 53.3(2) . . . . ?
Na1 Cu O6 Mo1 100.92(19) . . . . ?
O12 Mo2 O8 Mo1 -175.87(13) . . . . ?
O11 Mo2 O8 Mo1 -67.93(15) . . . . ?
O13 Mo2 O8 Mo1 61.2(3) . . . . ?
O15 Mo2 O8 Mo1 20.40(12) . . . . ?
O14 Mo2 O8 Mo1 92.24(13) . . . . ?
O12 Mo2 O8 Cu 24.32(16) . . . 1_655 ?
O11 Mo2 O8 Cu 132.26(14) . . . 1_655 ?
O13 Mo2 O8 Cu -98.6(2) . . . 1_655 ?
O15 Mo2 O8 Cu -139.41(15) . . . 1_655 ?
O14 Mo2 O8 Cu -67.57(13) . . . 1_655 ?
O7 Mo1 O8 Mo2 174.73(14) . . . . ?
O6 Mo1 O8 Mo2 65.37(15) . . . . ?
O9 Mo1 O8 Mo2 -57.5(3) . . . . ?
O10 Mo1 O8 Mo2 -92.10(13) . . . . ?
O15 Mo1 O8 Mo2 -20.19(12) . . . . ?
O7 Mo1 O8 Cu -25.37(15) . . . 1_655 ?
O6 Mo1 O8 Cu -134.72(14) . . . 1_655 ?
O9 Mo1 O8 Cu 102.4(2) . . . 1_655 ?
O10 Mo1 O8 Cu 67.81(13) . . . 1_655 ?
O15 Mo1 O8 Cu 139.72(14) . . . 1_655 ?
O17 Mo3 O9 Mo1 -68.46(16) . . . . ?
O16 Mo3 O9 Mo1 -175.86(14) . . . . ?
O13 Mo3 O9 Mo1 58.4(3) 2_666 . . . ?
O14 Mo3 O9 Mo1 91.13(14) 2_666 . . . ?
O10 Mo3 O9 Mo1 20.09(12) . . . . ?
O7 Mo1 O9 Mo3 70.51(15) . . . . ?
O6 Mo1 O9 Mo3 -179.62(14) . . . . ?
O8 Mo1 O9 Mo3 -56.2(3) . . . . ?
O10 Mo1 O9 Mo3 -20.40(12) . . . . ?
O15 Mo1 O9 Mo3 -92.06(14) . . . . ?
O15 Te O10 Mo1 -0.08(10) . . . . ?
O15 Te O10 Mo1 179.92(10) 2_666 . . . ?
O14 Te O10 Mo1 -85.44(11) . . . . ?
O14 Te O10 Mo1 94.56(11) 2_666 . . . ?
O15 Te O10 Mo3 -94.81(11) . . . . ?
O15 Te O10 Mo3 85.19(11) 2_666 . . . ?
O14 Te O10 Mo3 179.83(10) . . . . ?
O14 Te O10 Mo3 -0.17(10) 2_666 . . . ?
O7 Mo1 O10 Te 171.31(12) . . . . ?
O6 Mo1 O10 Te -19.7(3) . . . . ?
O9 Mo1 O10 Te -87.80(12) . . . . ?
O8 Mo1 O10 Te 75.50(12) . . . . ?
O15 Mo1 O10 Te 0.07(9) . . . . ?
O7 Mo1 O10 Mo3 -85.56(11) . . . . ?
O6 Mo1 O10 Mo3 83.5(3) . . . . ?
O9 Mo1 O10 Mo3 15.33(9) . . . . ?
O8 Mo1 O10 Mo3 178.63(10) . . . . ?
O15 Mo1 O10 Mo3 103.19(10) . . . . ?
O17 Mo3 O10 Te -171.84(12) . . . . ?
O16 Mo3 O10 Te 27.5(4) . . . . ?
O9 Mo3 O10 Te 87.67(12) . . . . ?
O13 Mo3 O10 Te -74.64(12) 2_666 . . . ?
O14 Mo3 O10 Te 0.15(9) 2_666 . . . ?
O17 Mo3 O10 Mo1 85.02(11) . . . . ?
O16 Mo3 O10 Mo1 -75.7(4) . . . . ?
O9 Mo3 O10 Mo1 -15.47(9) . . . . ?
O13 Mo3 O10 Mo1 -177.79(10) 2_666 . . . ?
O14 Mo3 O10 Mo1 -102.99(10) 2_666 . . . ?
O12 Mo2 O11 Na1 -125.4(2) . . . . ?
O8 Mo2 O11 Na1 132.9(2) . . . . ?
O13 Mo2 O11 Na1 -25.7(2) . . . . ?
O15 Mo2 O11 Na1 58.0(2) . . . . ?
O14 Mo2 O11 Na1 34.6(5) . . . . ?
O11 Mo2 O12 Na1 -141.3(3) . . . 1_655 ?
O8 Mo2 O12 Na1 -37.1(3) . . . 1_655 ?
O13 Mo2 O12 Na1 119.5(3) . . . 1_655 ?
O15 Mo2 O12 Na1 27.4(6) . . . 1_655 ?
O14 Mo2 O12 Na1 45.4(3) . . . 1_655 ?
O12 Mo2 O13 Mo3 -72.97(16) . . . 2_666 ?
O11 Mo2 O13 Mo3 -179.94(14) . . . 2_666 ?
O8 Mo2 O13 Mo3 50.0(3) . . . 2_666 ?
O15 Mo2 O13 Mo3 89.47(14) . . . 2_666 ?
O14 Mo2 O13 Mo3 17.94(12) . . . 2_666 ?
O15 Te O14 Mo2 -1.11(10) . . . . ?
O15 Te O14 Mo2 178.89(10) 2_666 . . . ?
O10 Te O14 Mo2 84.74(11) . . . . ?
O10 Te O14 Mo2 -95.26(11) 2_666 . . . ?
O15 Te O14 Mo3 93.97(11) . . . 2_666 ?
O15 Te O14 Mo3 -86.03(11) 2_666 . . 2_666 ?
O10 Te O14 Mo3 179.83(10) . . . 2_666 ?
O10 Te O14 Mo3 -0.17(10) 2_666 . . 2_666 ?
O12 Mo2 O14 Te -173.35(12) . . . . ?
O11 Mo2 O14 Te 25.9(4) . . . . ?
O8 Mo2 O14 Te -75.75(12) . . . . ?
O13 Mo2 O14 Te 89.72(12) . . . . ?
O15 Mo2 O14 Te 1.00(9) . . . . ?
O12 Mo2 O14 Mo3 83.41(11) . . . 2_666 ?
O11 Mo2 O14 Mo3 -77.3(3) . . . 2_666 ?
O8 Mo2 O14 Mo3 -178.98(10) . . . 2_666 ?
O13 Mo2 O14 Mo3 -13.51(9) . . . 2_666 ?
O15 Mo2 O14 Mo3 -102.24(10) . . . 2_666 ?
O10 Te O15 Mo2 -93.66(11) . . . . ?
O10 Te O15 Mo2 86.34(11) 2_666 . . . ?
O14 Te O15 Mo2 1.11(10) . . . . ?
O14 Te O15 Mo2 -178.89(10) 2_666 . . . ?
O10 Te O15 Mo1 0.07(10) . . . . ?
O10 Te O15 Mo1 -179.93(10) 2_666 . . . ?
O14 Te O15 Mo1 94.85(11) . . . . ?
O14 Te O15 Mo1 -85.15(11) 2_666 . . . ?
O12 Mo2 O15 Te 18.2(4) . . . . ?
O11 Mo2 O15 Te -172.77(12) . . . . ?
O8 Mo2 O15 Te 85.88(12) . . . . ?
O13 Mo2 O15 Te -76.18(12) . . . . ?
O14 Mo2 O15 Te -1.00(9) . . . . ?
O12 Mo2 O15 Mo1 -83.3(4) . . . . ?
O11 Mo2 O15 Mo1 85.77(11) . . . . ?
O8 Mo2 O15 Mo1 -15.58(9) . . . . ?
O13 Mo2 O15 Mo1 -177.64(10) . . . . ?
O14 Mo2 O15 Mo1 -102.46(10) . . . . ?
O7 Mo1 O15 Te -30.0(4) . . . . ?
O6 Mo1 O15 Te 172.57(12) . . . . ?
O9 Mo1 O15 Te 75.55(11) . . . . ?
O8 Mo1 O15 Te -87.14(12) . . . . ?
O10 Mo1 O15 Te -0.07(9) . . . . ?
O7 Mo1 O15 Mo2 72.6(4) . . . . ?
O6 Mo1 O15 Mo2 -84.81(11) . . . . ?
O9 Mo1 O15 Mo2 178.17(10) . . . . ?
O8 Mo1 O15 Mo2 15.48(9) . . . . ?
O10 Mo1 O15 Mo2 102.55(10) . . . . ?
C1 O1 Na1 O22 -18.7(4) . . . . ?
Cu O1 Na1 O22 -178.15(13) . . . . ?
C1 O1 Na1 O12 78.0(4) . . . 1_455 ?
Cu O1 Na1 O12 -81.44(12) . . . 1_455 ?
C1 O1 Na1 O11 -121.8(4) . . . . ?
Cu O1 Na1 O11 78.74(12) . . . . ?
C1 O1 Na1 O21 152.7(5) . . . . ?
Cu O1 Na1 O21 -6.8(5) . . . . ?
C1 O1 Na1 O5 157.6(4) . . . . ?
Cu O1 Na1 O5 -1.89(10) . . . . ?
C1 O1 Na1 Cu 159.5(5) . . . . ?
C1 O1 Na1 Na2 -28.9(5) . . . . ?
Cu O1 Na1 Na2 171.66(15) . . . . ?
Mo2 O11 Na1 O22 117.8(2) . . . . ?
Mo2 O11 Na1 O1 -130.9(2) . . . . ?
Mo2 O11 Na1 O12 -75.2(4) . . . 1_455 ?
Mo2 O11 Na1 O21 34.2(2) . . . . ?
Mo2 O11 Na1 O5 -59.1(2) . . . . ?
Mo2 O11 Na1 Cu -96.2(2) . . . . ?
Mo2 O11 Na1 Na2 75.7(2) . . . . ?
Cu O5 Na1 O1 1.82(10) . . . . ?
Cu O5 Na1 O12 82.20(11) . . . 1_455 ?
Cu O5 Na1 O11 -91.27(11) . . . . ?
Cu O5 Na1 O21 -179.43(11) . . . . ?
Cu O5 Na1 Na2 -174.14(8) . . . . ?
O1 Cu Na1 O22 3.1(2) . . . . ?
N3 Cu Na1 O22 7.0(2) . . . . ?
O4 Cu Na1 O22 -177.3(2) . . . . ?
O5 Cu Na1 O22 -173.9(2) . . . . ?
O6 Cu Na1 O22 97.0(2) . . . . ?
O8 Cu Na1 O22 -85.2(2) 1_455 . . . ?
N3 Cu Na1 O1 3.94(17) . . . . ?
O4 Cu Na1 O1 179.59(17) . . . . ?
O5 Cu Na1 O1 -177.00(16) . . . . ?
O6 Cu Na1 O1 93.93(13) . . . . ?
O8 Cu Na1 O1 -88.29(13) 1_455 . . . ?
O1 Cu Na1 O12 89.20(14) . . . 1_455 ?
N3 Cu Na1 O12 93.14(14) . . . 1_455 ?
O4 Cu Na1 O12 -91.20(14) . . . 1_455 ?
O5 Cu Na1 O12 -87.79(13) . . . 1_455 ?
O6 Cu Na1 O12 -176.87(10) . . . 1_455 ?
O8 Cu Na1 O12 0.91(9) 1_455 . . 1_455 ?
O1 Cu Na1 O11 -99.34(14) . . . . ?
N3 Cu Na1 O11 -95.40(14) . . . . ?
O4 Cu Na1 O11 80.26(14) . . . . ?
O5 Cu Na1 O11 83.67(13) . . . . ?
O6 Cu Na1 O11 -5.41(9) . . . . ?
O8 Cu Na1 O11 172.37(9) 1_455 . . . ?
O1 Cu Na1 O21 177.74(17) . . . . ?
N3 Cu Na1 O21 -178.32(16) . . . . ?
O4 Cu Na1 O21 -2.67(18) . . . . ?
O5 Cu Na1 O21 0.74(14) . . . . ?
O6 Cu Na1 O21 -88.33(13) . . . . ?
O8 Cu Na1 O21 89.45(13) 1_455 . . . ?
O1 Cu Na1 O5 177.00(16) . . . . ?
N3 Cu Na1 O5 -179.06(16) . . . . ?
O4 Cu Na1 O5 -3.41(16) . . . . ?
O6 Cu Na1 O5 -89.07(12) . . . . ?
O8 Cu Na1 O5 88.70(12) 1_455 . . . ?
O22 Na1 Na2 O20 -24.2(2) . . . . ?
O1 Na1 Na2 O20 -10.2(3) . . . . ?
O12 Na1 Na2 O20 -109.46(18) 1_455 . . . ?
O11 Na1 Na2 O20 82.44(18) . . . . ?
O21 Na1 Na2 O20 169.1(2) . . . . ?
O5 Na1 Na2 O20 161.15(18) . . . . ?
O22 Na1 Na2 O24B 168.6(13) . . . . ?
O1 Na1 Na2 O24B -177.4(13) . . . . ?
O12 Na1 Na2 O24B 83.4(13) 1_455 . . . ?
O11 Na1 Na2 O24B -84.7(12) . . . . ?
O21 Na1 Na2 O24B 2.0(13) . . . . ?
O5 Na1 Na2 O24B -6.0(13) . . . . ?
O22 Na1 Na2 O24A 134.9(6) . . . . ?
O1 Na1 Na2 O24A 148.9(6) . . . . ?
O12 Na1 Na2 O24A 49.7(6) 1_455 . . . ?
O11 Na1 Na2 O24A -118.4(6) . . . . ?
O21 Na1 Na2 O24A -31.7(6) . . . . ?
O5 Na1 Na2 O24A -39.7(6) . . . . ?
O22 Na1 Na2 O23 -103.46(19) . . . . ?
O1 Na1 Na2 O23 -89.5(2) . . . . ?
O12 Na1 Na2 O23 171.32(13) 1_455 . . . ?
O11 Na1 Na2 O23 3.22(12) . . . . ?
O21 Na1 Na2 O23 89.91(16) . . . . ?
O5 Na1 Na2 O23 81.92(16) . . . . ?
O22 Na1 Na2 O21 166.6(2) . . . . ?
O1 Na1 Na2 O21 -179.4(2) . . . . ?
O12 Na1 Na2 O21 81.41(14) 1_455 . . . ?
O11 Na1 Na2 O21 -86.69(13) . . . . ?
O5 Na1 Na2 O21 -7.99(15) . . . . ?
O1 Na1 Na2 O22 14.0(3) . . . . ?
O12 Na1 Na2 O22 -85.22(17) 1_455 . . . ?
O11 Na1 Na2 O22 106.68(17) . . . . ?
O21 Na1 Na2 O22 -166.6(2) . . . . ?
O5 Na1 Na2 O22 -174.6(2) . . . . ?
O22 Na1 Na2 O2 57.74(17) . . . 2_565 ?
O1 Na1 Na2 O2 71.7(2) . . . 2_565 ?
O12 Na1 Na2 O2 -27.49(11) 1_455 . . 2_565 ?
O11 Na1 Na2 O2 164.41(10) . . . 2_565 ?
O21 Na1 Na2 O2 -108.90(14) . . . 2_565 ?
O5 Na1 Na2 O2 -116.88(13) . . . 2_565 ?
O22 Na1 O21 Na2 -9.16(14) . . . . ?
O1 Na1 O21 Na2 178.9(4) . . . . ?
O12 Na1 O21 Na2 -109.19(12) 1_455 . . . ?
O11 Na1 O21 Na2 93.23(12) . . . . ?
O5 Na1 O21 Na2 174.29(11) . . . . ?
Cu Na1 O21 Na2 173.85(8) . . . . ?
O24B Na2 O21 Na1 -178.6(9) . . . . ?
O24A Na2 O21 Na1 157.8(5) . . . . ?
O23 Na2 O21 Na1 -86.08(14) . . . . ?
O22 Na2 O21 Na1 8.70(13) . . . . ?
O2 Na2 O21 Na1 72.83(12) 2_565 . . . ?
O1 Na1 O22 Na2 -173.35(12) . . . . ?
O12 Na1 O22 Na2 106.79(14) 1_455 . . . ?
O11 Na1 O22 Na2 -78.47(15) . . . . ?
O21 Na1 O22 Na2 8.87(13) . . . . ?
Cu Na1 O22 Na2 -175.26(12) . . . . ?
O20 Na2 O22 Na1 163.72(14) . . . . ?
O24A Na2 O22 Na1 -97.8(4) . . . . ?
O23 Na2 O22 Na1 75.82(16) . . . . ?
O21 Na2 O22 Na1 -8.90(14) . . . . ?
O2 Na2 O22 Na1 -113.03(15) 2_565 . . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 25.04
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.863
_refine_diff_density_min -0.808
_refine_diff_density_rms 0.133
# Attachment '- complex2.cif'
data_gkl017a
_database_code_depnum_ccdc_archive 'CCDC 775687'
#TrackingRef '- complex2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C12 H40 Cu3 N12 O24 Te W6, 6(O)'
_chemical_formula_sum 'C6 H20 Cu1.50 N6 O15 Te0.50 W3'
_chemical_formula_weight 1126.94
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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.5690(12)
_cell_length_b 11.5330(15)
_cell_length_c 13.1650(15)
_cell_angle_alpha 67.370(4)
_cell_angle_beta 85.640(3)
_cell_angle_gamma 72.680(4)
_cell_volume 1145.3(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 3.268
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1019
_exptl_absorpt_coefficient_mu 17.084
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 15207
_diffrn_reflns_av_R_equivalents 0.0290
_diffrn_reflns_av_sigmaI/netI 0.0377
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.94
_diffrn_reflns_theta_max 32.19
_reflns_number_total 7294
_reflns_number_gt 6031
_reflns_threshold_expression >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution ?
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment noref
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7294
_refine_ls_number_parameters 237
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0612
_refine_ls_R_factor_gt 0.0544
_refine_ls_wR_factor_ref 0.1446
_refine_ls_wR_factor_gt 0.1419
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_restrained_S_all 1.051
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
C1 C -0.3091(13) 0.5380(11) 0.6000(9) 0.024(2) Uani 1 1 d . . .
H1A H -0.3020 0.5874 0.6439 0.029 Uiso 1 1 calc R . .
H1B H -0.3998 0.5013 0.6249 0.029 Uiso 1 1 calc R . .
C2 C -0.3381(13) 0.6280(11) 0.4798(9) 0.024(2) Uani 1 1 d . . .
H2A H -0.3634 0.5834 0.4368 0.028 Uiso 1 1 calc R . .
H2B H -0.4290 0.7058 0.4706 0.028 Uiso 1 1 calc R . .
C3 C -0.3251(10) 0.2231(8) -0.1338(7) 0.0094(15) Uani 1 1 d . . .
H3A H -0.4282 0.2258 -0.1617 0.011 Uiso 1 1 calc R . .
H3B H -0.2416 0.2086 -0.1853 0.011 Uiso 1 1 calc R . .
C4 C -0.3399(10) 0.3514(9) -0.1221(7) 0.0121(16) Uani 1 1 d . . .
H4A H -0.2317 0.3601 -0.1175 0.015 Uiso 1 1 calc R . .
H4B H -0.3990 0.4243 -0.1862 0.015 Uiso 1 1 calc R . .
C5 C -0.5614(11) 0.1353(10) 0.2996(7) 0.0150(17) Uani 1 1 d . . .
H5A H -0.6710 0.1289 0.2960 0.018 Uiso 1 1 calc R . .
H5B H -0.5503 0.1527 0.3648 0.018 Uiso 1 1 calc R . .
C6 C -0.4365(10) 0.0062(9) 0.3079(7) 0.0118(16) Uani 1 1 d . . .
H6A H -0.3294 0.0030 0.3301 0.014 Uiso 1 1 calc R . .
H6B H -0.4681 -0.0673 0.3618 0.014 Uiso 1 1 calc R . .
N1 N -0.1541(9) 0.4302(7) 0.6145(6) 0.0118(14) Uani 1 1 d . . .
H1C H -0.1745 0.3620 0.6063 0.014 Uiso 1 1 calc R . .
H1D H -0.1089 0.4022 0.6824 0.014 Uiso 1 1 calc R . .
N2 N -0.1877(8) 0.6640(7) 0.4437(6) 0.0099(13) Uani 1 1 d . . .
H2C H -0.1780 0.7225 0.4707 0.012 Uiso 1 1 calc R . .
H2D H -0.1893 0.7005 0.3697 0.012 Uiso 1 1 calc R . .
N3 N -0.2800(8) 0.1144(7) -0.0230(6) 0.0097(13) Uani 1 1 d . . .
H3C H -0.1726 0.0942 -0.0071 0.012 Uiso 1 1 calc R . .
H3D H -0.3008 0.0423 -0.0229 0.012 Uiso 1 1 calc R . .
N4 N -0.4278(9) 0.3548(7) -0.0216(6) 0.0093(13) Uani 1 1 d . . .
H4C H -0.5339 0.3997 -0.0400 0.011 Uiso 1 1 calc R . .
H4D H -0.3855 0.3972 0.0089 0.011 Uiso 1 1 calc R . .
N5 N -0.5367(9) 0.2438(7) 0.2009(6) 0.0111(14) Uani 1 1 d . . .
N6 N -0.4325(9) 0.0002(7) 0.1979(6) 0.0107(13) Uiso 1 1 d . . .
O1 O -0.1545(6) 0.4064(5) 0.0747(5) 0.0042(10) Uiso 1 1 d . . .
O2 O 0.1625(6) 0.3308(5) 0.0531(4) 0.0035(10) Uiso 1 1 d . . .
O1W O 0.1270(8) 0.1298(7) 0.4854(6) 0.0184(14) Uani 1 1 d . . .
O3 O -0.0084(6) 0.4692(5) -0.1330(4) 0.0034(10) Uiso 1 1 d . . .
O2W O 0.1305(9) -0.1648(7) 0.3783(6) 0.0218(15) Uani 1 1 d . . .
O4 O 0.0118(6) 0.2051(5) -0.0035(4) 0.0036(9) Uiso 1 1 d . . .
O3W O 0.3072(9) 0.8717(7) -0.4776(6) 0.0213(14) Uani 1 1 d . . .
O5 O 0.2940(7) 0.4006(6) -0.1613(5) 0.0063(10) Uiso 1 1 d . . .
O6 O 0.0133(6) 0.2653(5) 0.2557(4) 0.0046(10) Uani 1 1 d . . .
O7 O 0.1762(7) 0.0544(6) 0.1997(5) 0.0061(10) Uiso 1 1 d . . .
O8 O -0.1604(7) 0.1370(6) 0.1836(5) 0.0084(11) Uani 1 1 d . . .
O9 O 0.3231(7) 0.6446(6) -0.2818(5) 0.0100(11) Uani 1 1 d . . .
O10 O 0.1031(7) 0.5615(6) -0.3592(5) 0.0080(11) Uani 1 1 d . . .
O11 O 0.1344(7) 0.2452(6) -0.2081(5) 0.0083(11) Uani 1 1 d . . .
O12 O 0.3510(7) 0.1414(6) -0.0303(5) 0.0081(11) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.5000 0.5000 0.0080(3) Uani 1 2 d S . .
Cu2 Cu -0.41146(12) 0.17329(9) 0.08940(8) 0.00694(19) Uani 1 1 d . . .
Te1 Te 0.0000 0.5000 0.0000 0.00068(13) Uiso 1 2 d S . .
W1 W 0.01059(3) 0.19284(3) 0.14613(2) 0.00271(9) Uiso 1 1 d . . .
W2 W 0.17977(3) 0.27054(3) -0.09306(2) 0.00295(9) Uiso 1 1 d . . .
W3 W 0.16056(3) 0.57735(3) -0.24306(2) 0.00305(9) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.022(5) 0.024(5) 0.019(5) -0.002(4) 0.011(4) -0.005(4)
C2 0.025(5) 0.017(5) 0.021(5) -0.002(4) -0.002(4) -0.002(4)
C3 0.009(3) 0.011(4) 0.009(4) -0.004(3) 0.004(3) -0.006(3)
C4 0.010(4) 0.012(4) 0.011(4) 0.001(3) 0.000(3) -0.006(3)
C5 0.010(4) 0.029(5) 0.012(4) -0.012(4) 0.002(3) -0.008(4)
C6 0.008(4) 0.012(4) 0.008(4) 0.002(3) 0.001(3) -0.002(3)
N1 0.012(3) 0.007(3) 0.010(3) 0.003(3) -0.001(3) -0.002(3)
N2 0.013(3) 0.008(3) 0.006(3) -0.003(3) 0.004(2) 0.000(3)
N3 0.008(3) 0.009(3) 0.012(3) -0.002(3) 0.001(3) -0.004(3)
N4 0.013(3) 0.003(3) 0.012(3) -0.003(3) -0.006(3) 0.000(2)
N5 0.010(3) 0.011(3) 0.014(4) -0.009(3) 0.001(3) -0.001(3)
O1W 0.023(3) 0.015(3) 0.013(3) -0.003(3) -0.003(3) -0.002(3)
O2W 0.037(4) 0.010(3) 0.017(3) -0.003(3) 0.004(3) -0.010(3)
O3W 0.025(3) 0.019(3) 0.015(3) 0.002(3) -0.004(3) -0.009(3)
O6 0.008(2) 0.002(2) 0.003(2) 0.000(2) -0.0020(19) -0.0002(19)
O8 0.011(3) 0.006(3) 0.008(3) 0.000(2) 0.002(2) -0.006(2)
O9 0.015(3) 0.006(3) 0.010(3) -0.002(2) 0.003(2) -0.007(2)
O10 0.012(3) 0.006(3) 0.006(3) -0.003(2) -0.001(2) -0.001(2)
O11 0.012(3) 0.009(3) 0.005(3) -0.003(2) 0.001(2) -0.005(2)
O12 0.005(2) 0.004(2) 0.014(3) -0.002(2) 0.002(2) -0.002(2)
Cu1 0.0096(6) 0.0038(6) 0.0083(6) -0.0006(5) 0.0015(5) -0.0010(5)
Cu2 0.0098(4) 0.0036(4) 0.0063(4) -0.0015(4) -0.0007(3) -0.0006(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 N1 1.490(12) . ?
C1 C2 1.512(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.460(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.496(11) . ?
C3 C4 1.513(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.481(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N5 1.471(12) . ?
C5 C6 1.522(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.473(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 Cu1 2.015(7) . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 Cu1 2.001(7) . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
N3 Cu2 1.996(7) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 Cu2 2.009(7) . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
N5 Cu2 2.032(7) . ?
N6 Cu2 2.009(7) . ?
O1 Te1 1.929(5) . ?
O1 W3 2.290(5) 2_565 ?
O1 W1 2.301(5) . ?
O2 Te1 1.928(5) . ?
O2 W2 2.266(5) . ?
O2 W1 2.284(5) . ?
O3 Te1 1.926(5) . ?
O3 W3 2.262(5) . ?
O3 W2 2.265(5) . ?
O4 W1 1.919(5) . ?
O4 W2 1.933(5) . ?
O5 W2 1.928(6) . ?
O5 W3 1.932(6) . ?
O6 W1 1.930(5) . ?
O6 W3 1.933(5) 2_565 ?
O7 W1 1.732(6) . ?
O8 W1 1.735(6) . ?
O8 Cu2 2.410(6) . ?
O9 W3 1.741(6) . ?
O10 W3 1.731(6) . ?
O11 W2 1.739(6) . ?
O12 W2 1.729(6) . ?
Cu1 N2 2.001(7) 2_566 ?
Cu1 N1 2.015(7) 2_566 ?
Te1 O3 1.926(5) 2_565 ?
Te1 O2 1.928(5) 2_565 ?
Te1 O1 1.929(5) 2_565 ?
W3 O6 1.933(5) 2_565 ?
W3 O1 2.290(5) 2_565 ?
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
N1 C1 C2 109.4(8) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 106.9(8) . . ?
N2 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N2 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 108.4(7) . . ?
N3 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
N3 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N4 C4 C3 109.8(7) . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N5 C5 C6 110.4(7) . . ?
N5 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N5 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N6 C6 C5 106.9(7) . . ?
N6 C6 H6A 110.3 . . ?
C5 C6 H6A 110.3 . . ?
N6 C6 H6B 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.6 . . ?
C1 N1 Cu1 108.3(5) . . ?
C1 N1 H1C 110.0 . . ?
Cu1 N1 H1C 110.0 . . ?
C1 N1 H1D 110.0 . . ?
Cu1 N1 H1D 110.0 . . ?
H1C N1 H1D 108.4 . . ?
C2 N2 Cu1 107.7(6) . . ?
C2 N2 H2C 110.2 . . ?
Cu1 N2 H2C 110.2 . . ?
C2 N2 H2D 110.2 . . ?
Cu1 N2 H2D 110.2 . . ?
H2C N2 H2D 108.5 . . ?
C3 N3 Cu2 108.7(5) . . ?
C3 N3 H3C 110.0 . . ?
Cu2 N3 H3C 110.0 . . ?
C3 N3 H3D 110.0 . . ?
Cu2 N3 H3D 110.0 . . ?
H3C N3 H3D 108.3 . . ?
C4 N4 Cu2 111.8(5) . . ?
C4 N4 H4C 109.3 . . ?
Cu2 N4 H4C 109.3 . . ?
C4 N4 H4D 109.3 . . ?
Cu2 N4 H4D 109.3 . . ?
H4C N4 H4D 107.9 . . ?
C5 N5 Cu2 110.3(5) . . ?
C6 N6 Cu2 106.8(5) . . ?
Te1 O1 W3 101.9(2) . 2_565 ?
Te1 O1 W1 101.9(2) . . ?
W3 O1 W1 91.5(2) 2_565 . ?
Te1 O2 W2 102.0(2) . . ?
Te1 O2 W1 102.6(2) . . ?
W2 O2 W1 92.10(19) . . ?
Te1 O3 W3 103.0(2) . . ?
Te1 O3 W2 102.0(2) . . ?
W3 O3 W2 92.94(19) . . ?
W1 O4 W2 116.5(3) . . ?
W2 O5 W3 116.5(3) . . ?
W1 O6 W3 116.7(3) . 2_565 ?
W1 O8 Cu2 134.8(3) . . ?
N2 Cu1 N2 180.000(1) . 2_566 ?
N2 Cu1 N1 94.9(3) . 2_566 ?
N2 Cu1 N1 85.1(3) 2_566 2_566 ?
N2 Cu1 N1 85.1(3) . . ?
N2 Cu1 N1 94.9(3) 2_566 . ?
N1 Cu1 N1 180.000(1) 2_566 . ?
N3 Cu2 N4 84.4(3) . . ?
N3 Cu2 N6 99.9(3) . . ?
N4 Cu2 N6 171.2(3) . . ?
N3 Cu2 N5 175.7(3) . . ?
N4 Cu2 N5 92.3(3) . . ?
N6 Cu2 N5 83.8(3) . . ?
N3 Cu2 O8 89.1(2) . . ?
N4 Cu2 O8 97.7(2) . . ?
N6 Cu2 O8 90.1(2) . . ?
N5 Cu2 O8 88.6(2) . . ?
O3 Te1 O3 180.0(3) . 2_565 ?
O3 Te1 O2 94.5(2) . 2_565 ?
O3 Te1 O2 85.5(2) 2_565 2_565 ?
O3 Te1 O2 85.5(2) . . ?
O3 Te1 O2 94.5(2) 2_565 . ?
O2 Te1 O2 180.000(1) 2_565 . ?
O3 Te1 O1 94.9(2) . . ?
O3 Te1 O1 85.1(2) 2_565 . ?
O2 Te1 O1 94.3(2) 2_565 . ?
O2 Te1 O1 85.7(2) . . ?
O3 Te1 O1 85.1(2) . 2_565 ?
O3 Te1 O1 94.9(2) 2_565 2_565 ?
O2 Te1 O1 85.7(2) 2_565 2_565 ?
O2 Te1 O1 94.3(2) . 2_565 ?
O1 Te1 O1 180.0(3) . 2_565 ?
O7 W1 O8 105.1(3) . . ?
O7 W1 O4 98.8(2) . . ?
O8 W1 O4 97.0(2) . . ?
O7 W1 O6 97.6(2) . . ?
O8 W1 O6 100.1(2) . . ?
O4 W1 O6 152.2(2) . . ?
O7 W1 O2 95.5(2) . . ?
O8 W1 O2 158.5(2) . . ?
O4 W1 O2 73.5(2) . . ?
O6 W1 O2 82.7(2) . . ?
O7 W1 O1 163.6(2) . . ?
O8 W1 O1 90.4(2) . . ?
O4 W1 O1 84.4(2) . . ?
O6 W1 O1 73.8(2) . . ?
O2 W1 O1 69.79(19) . . ?
O12 W2 O11 104.6(3) . . ?
O12 W2 O5 96.3(2) . . ?
O11 W2 O5 99.9(3) . . ?
O12 W2 O4 100.0(2) . . ?
O11 W2 O4 96.1(2) . . ?
O5 W2 O4 153.5(2) . . ?
O12 W2 O3 157.9(2) . . ?
O11 W2 O3 96.5(2) . . ?
O5 W2 O3 73.3(2) . . ?
O4 W2 O3 84.0(2) . . ?
O12 W2 O2 89.6(2) . . ?
O11 W2 O2 163.9(2) . . ?
O5 W2 O2 85.7(2) . . ?
O4 W2 O2 73.7(2) . . ?
O3 W2 O2 70.5(2) . . ?
O10 W3 O9 105.4(3) . . ?
O10 W3 O5 101.2(3) . . ?
O9 W3 O5 95.6(3) . . ?
O10 W3 O6 96.9(3) . 2_565 ?
O9 W3 O6 99.2(3) . 2_565 ?
O5 W3 O6 152.6(2) . 2_565 ?
O10 W3 O3 93.9(2) . . ?
O9 W3 O3 159.4(2) . . ?
O5 W3 O3 73.3(2) . . ?
O6 W3 O3 85.2(2) 2_565 . ?
O10 W3 O1 161.7(2) . 2_565 ?
O9 W3 O1 91.9(2) . 2_565 ?
O5 W3 O1 82.6(2) . 2_565 ?
O6 W3 O1 74.0(2) 2_565 2_565 ?
O3 W3 O1 69.9(2) . 2_565 ?
_diffrn_measured_fraction_theta_max 0.902
_diffrn_reflns_theta_full 32.19
_diffrn_measured_fraction_theta_full 0.902
_refine_diff_density_max 7.116
_refine_diff_density_min -17.129
_refine_diff_density_rms 0.808
data_IN_10_01d
_database_code_depnum_ccdc_archive 'CCDC 788177'
#TrackingRef '- compound2-c.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C12 H48 Cu3 N12 O24 Te W6, 6(H2 O) '
_chemical_formula_sum 'C12 H60 Cu3 N12 O30 Te W6'
_chemical_formula_weight 2274.04
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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.5534(3)
_cell_length_b 11.5294(4)
_cell_length_c 13.1841(5)
_cell_angle_alpha 67.382(4)
_cell_angle_beta 85.597(3)
_cell_angle_gamma 72.689(3)
_cell_volume 1144.75(7)
_cell_formula_units_Z 1
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 6854
_cell_measurement_theta_min 2.9437
_cell_measurement_theta_max 29.0786
_exptl_crystal_description prism
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.4442
_exptl_crystal_size_mid 0.3394
_exptl_crystal_size_min 0.3022
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 3.299
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1039
_exptl_absorpt_coefficient_mu 16.932
_exptl_absorpt_correction_T_min 0.016
_exptl_absorpt_correction_T_max 0.067
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
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_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window'
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measurement_method '\w scans'
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 5959
_diffrn_reflns_av_R_equivalents 0.0192
_diffrn_reflns_av_sigmaI/netI 0.0134
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.95
_diffrn_reflns_theta_max 25.01
_reflns_number_total 4013
_reflns_number_gt 3947
_reflns_threshold_expression >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Oxygens O3, O6 and O9 were refined anisotropically, but restrained by ISOR
instruction as a tool preventing individual atoms from becoming 'non-
positive-definite'.
C-bound and N-bound H-atoms were included in the riding model approximation
with distances of 0.97 \%A (CH~2~) and 0.90 \%A (NH~2~), and with
U~iso~(H) values of 1.2U~eq~(CH~2~, CH~2~). 6 O-bound H atoms
were refined, with the O---H distances restrained to 0.90(2) \%A and with
U~iso~(H) values of 1.5U~eq~(O~water~).
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4013
_refine_ls_number_parameters 310
_refine_ls_number_restraints 24
_refine_ls_R_factor_all 0.0294
_refine_ls_R_factor_gt 0.0289
_refine_ls_wR_factor_ref 0.0786
_refine_ls_wR_factor_gt 0.0784
_refine_ls_goodness_of_fit_ref 1.264
_refine_ls_restrained_S_all 1.262
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 -0.17989(4) 0.22972(3) 0.59308(2) 0.00717(10) Uani 1 1 d . . .
W2 W -0.16060(4) -0.07756(3) 0.74327(2) 0.00734(10) Uani 1 1 d . . .
W3 W 0.01069(4) -0.30764(3) 0.64633(2) 0.00705(10) Uani 1 1 d . . .
Te1 Te 0.0000 0.0000 0.5000 0.00676(15) Uani 1 2 d S . .
O1 O -0.3522(7) 0.3604(5) 0.5294(5) 0.0135(12) Uani 1 1 d . . .
O2 O -0.1340(7) 0.2549(6) 0.7086(5) 0.0136(12) Uani 1 1 d . . .
O3 O -0.2925(7) 0.0981(5) 0.6627(4) 0.0105(11) Uani 1 1 d U . .
O4 O 0.0088(7) 0.0308(5) 0.6323(4) 0.0101(11) Uani 1 1 d . . .
O5 O -0.1634(7) 0.1690(5) 0.4470(5) 0.0106(11) Uani 1 1 d . . .
O6 O -0.0105(6) 0.2949(5) 0.5042(4) 0.0073(10) Uani 1 1 d U . .
O7 O -0.1034(7) -0.0616(6) 0.8595(5) 0.0138(12) Uani 1 1 d . . .
O8 O -0.3248(7) -0.1431(6) 0.7814(5) 0.0145(12) Uani 1 1 d . . .
O9 O 0.0156(7) -0.2343(5) 0.7559(4) 0.0096(11) Uani 1 1 d U . .
O10 O -0.1537(7) -0.0947(6) 0.5758(5) 0.0115(11) Uani 1 1 d . . .
O11 O 0.1783(7) -0.4477(6) 0.7003(5) 0.0142(12) Uani 1 1 d . . .
O12 O -0.1615(7) -0.3625(5) 0.6843(5) 0.0124(11) Uani 1 1 d . . .
Cu1 Cu -0.41218(11) -0.32708(9) 0.59018(8) 0.0105(2) Uani 1 1 d . . .
Cu2 Cu 0.0000 0.0000 1.0000 0.0111(3) Uani 1 2 d S . .
N1 N -0.5381(8) -0.2573(7) 0.7018(6) 0.0135(14) Uani 1 1 d . . .
H1A H -0.4825 -0.2126 0.7202 0.016 Uiso 1 1 calc R . .
H1B H -0.6363 -0.2015 0.6716 0.016 Uiso 1 1 calc R . .
N2 N -0.4334(8) -0.5005(7) 0.6977(6) 0.0136(14) Uani 1 1 d . . .
H2A H -0.5259 -0.5138 0.6826 0.016 Uiso 1 1 calc R . .
H2B H -0.3473 -0.5667 0.6946 0.016 Uiso 1 1 calc R . .
N3 N -0.2806(8) -0.3852(7) 0.4763(5) 0.0116(13) Uani 1 1 d . . .
H3A H -0.1728 -0.4058 0.4921 0.014 Uiso 1 1 calc R . .
H3B H -0.3017 -0.4570 0.4760 0.014 Uiso 1 1 calc R . .
N4 N -0.4299(8) -0.1449(7) 0.4790(6) 0.0125(14) Uani 1 1 d . . .
H4A H -0.5362 -0.1004 0.4605 0.015 Uiso 1 1 calc R . .
H4B H -0.3881 -0.1020 0.5092 0.015 Uiso 1 1 calc R . .
N5 N -0.1884(8) 0.1646(7) 0.9433(6) 0.0142(14) Uani 1 1 d . . .
H5A H -0.1793 0.2234 0.9700 0.017 Uiso 1 1 calc R . .
H5B H -0.1905 0.2009 0.8693 0.017 Uiso 1 1 calc R . .
N6 N -0.1552(8) -0.0702(7) 1.1157(6) 0.0154(15) Uani 1 1 d . . .
H6A H -0.1744 -0.1394 1.1086 0.019 Uiso 1 1 calc R . .
H6B H -0.1105 -0.0968 1.1835 0.019 Uiso 1 1 calc R . .
C1 C -0.5624(10) -0.3662(9) 0.8021(7) 0.0166(17) Uani 1 1 d . . .
H1C H -0.6724 -0.3729 0.7999 0.020 Uiso 1 1 calc R . .
H1D H -0.5490 -0.3491 0.8670 0.020 Uiso 1 1 calc R . .
C2 C -0.4378(10) -0.4937(8) 0.8078(7) 0.0146(17) Uani 1 1 d . . .
H2C H -0.3305 -0.4967 0.8296 0.017 Uiso 1 1 calc R . .
H2D H -0.4684 -0.5678 0.8617 0.017 Uiso 1 1 calc R . .
C3 C -0.3253(10) -0.2764(9) 0.3663(7) 0.0163(17) Uani 1 1 d . . .
H3C H -0.4281 -0.2740 0.3379 0.020 Uiso 1 1 calc R . .
H3D H -0.2411 -0.2901 0.3150 0.020 Uiso 1 1 calc R . .
C4 C -0.3417(10) -0.1482(8) 0.3790(7) 0.0134(16) Uani 1 1 d . . .
H4C H -0.2337 -0.1390 0.3837 0.016 Uiso 1 1 calc R . .
H4D H -0.4009 -0.0753 0.3151 0.016 Uiso 1 1 calc R . .
C5 C -0.3402(11) 0.1252(9) 0.9813(7) 0.0182(18) Uani 1 1 d . . .
H5C H -0.3638 0.0794 0.9389 0.022 Uiso 1 1 calc R . .
H5D H -0.4325 0.2023 0.9717 0.022 Uiso 1 1 calc R . .
C6 C -0.3119(11) 0.0372(9) 1.1002(7) 0.0215(19) Uani 1 1 d . . .
H6C H -0.3064 0.0874 1.1436 0.026 Uiso 1 1 calc R . .
H6D H -0.4023 -0.0002 1.1249 0.026 Uiso 1 1 calc R . .
O21 O 0.1257(8) -0.3687(6) 0.9873(5) 0.0198(13) Uani 1 1 d D . .
H21V H 0.176(13) -0.442(7) 0.975(9) 0.030 Uiso 1 1 d D . .
H21W H 0.060(11) -0.344(11) 0.928(6) 0.030 Uiso 1 1 d D . .
O22 O -0.1339(8) -0.3323(6) 1.1209(5) 0.0214(13) Uani 1 1 d D . .
H22V H -0.150(14) -0.403(7) 1.177(6) 0.032 Uiso 1 1 d D . .
H22W H -0.055(10) -0.373(10) 1.087(9) 0.032 Uiso 1 1 d D . .
O23 O 0.3079(8) -0.6264(6) 1.0231(5) 0.0206(13) Uani 1 1 d D . .
H23V H 0.284(14) -0.647(11) 0.968(7) 0.031 Uiso 1 1 d D . .
H23W H 0.283(14) -0.695(7) 1.075(7) 0.031 Uiso 1 1 d D . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.00743(16) 0.00630(16) 0.00752(17) -0.00224(12) -0.00044(11) -0.00194(12)
W2 0.00790(16) 0.00701(17) 0.00695(17) -0.00195(12) -0.00057(11) -0.00268(12)
W3 0.00702(16) 0.00633(16) 0.00731(17) -0.00155(12) -0.00111(11) -0.00229(12)
Te1 0.0071(3) 0.0064(3) 0.0067(3) -0.0020(3) -0.0004(3) -0.0025(3)
O1 0.014(3) 0.007(3) 0.017(3) -0.002(2) -0.001(2) -0.002(2)
O2 0.012(3) 0.013(3) 0.011(3) -0.004(2) -0.001(2) 0.001(2)
O3 0.0109(18) 0.0093(18) 0.0117(18) -0.0031(14) 0.0017(14) -0.0052(14)
O4 0.014(3) 0.012(3) 0.005(3) -0.003(2) 0.000(2) -0.005(2)
O5 0.011(3) 0.007(3) 0.012(3) 0.000(2) -0.001(2) -0.003(2)
O6 0.0084(17) 0.0070(17) 0.0087(18) -0.0041(14) 0.0000(14) -0.0037(14)
O7 0.011(3) 0.015(3) 0.012(3) -0.004(2) -0.002(2) 0.000(2)
O8 0.015(3) 0.013(3) 0.015(3) -0.004(2) -0.001(2) -0.005(2)
O9 0.0113(18) 0.0118(18) 0.0079(18) -0.0063(14) -0.0026(14) -0.0021(14)
O10 0.008(3) 0.017(3) 0.011(3) -0.003(2) 0.001(2) -0.009(2)
O11 0.012(3) 0.011(3) 0.016(3) -0.005(2) -0.003(2) 0.002(2)
O12 0.011(3) 0.011(3) 0.012(3) -0.001(2) -0.001(2) -0.002(2)
Cu1 0.0113(5) 0.0088(5) 0.0106(5) -0.0030(4) -0.0007(4) -0.0025(4)
Cu2 0.0101(6) 0.0096(6) 0.0112(7) -0.0018(5) 0.0005(5) -0.0026(5)
N1 0.007(3) 0.015(4) 0.019(4) -0.008(3) -0.002(3) -0.001(3)
N2 0.007(3) 0.015(4) 0.017(4) -0.008(3) 0.002(3) 0.001(3)
N3 0.014(3) 0.010(3) 0.012(3) -0.003(3) -0.004(3) -0.006(3)
N4 0.013(3) 0.009(3) 0.017(3) -0.006(3) -0.005(3) -0.002(3)
N5 0.014(3) 0.015(4) 0.013(3) -0.006(3) 0.000(3) -0.001(3)
N6 0.013(3) 0.016(4) 0.016(4) -0.006(3) 0.001(3) -0.003(3)
C1 0.013(4) 0.024(5) 0.013(4) -0.008(4) -0.002(3) -0.004(3)
C2 0.016(4) 0.014(4) 0.010(4) 0.002(3) -0.002(3) -0.007(3)
C3 0.013(4) 0.023(5) 0.012(4) -0.005(4) 0.001(3) -0.007(3)
C4 0.008(4) 0.012(4) 0.019(4) -0.003(3) -0.003(3) -0.003(3)
C5 0.018(4) 0.014(4) 0.018(4) -0.004(4) 0.002(3) -0.002(3)
C6 0.021(5) 0.018(4) 0.018(5) -0.003(4) 0.004(4) -0.001(4)
O21 0.021(3) 0.021(3) 0.016(3) -0.005(3) -0.005(2) -0.004(3)
O22 0.029(4) 0.014(3) 0.022(3) -0.006(3) 0.002(3) -0.009(3)
O23 0.021(3) 0.021(3) 0.018(3) -0.004(3) -0.001(3) -0.009(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
W1 O1 1.744(5) . ?
W1 O2 1.748(6) . ?
W1 O3 1.933(5) . ?
W1 O6 1.936(5) . ?
W1 O4 2.268(6) . ?
W1 O5 2.270(6) . ?
W2 O7 1.735(6) . ?
W2 O8 1.740(6) . ?
W2 O3 1.916(5) . ?
W2 O9 1.937(5) . ?
W2 O4 2.269(5) . ?
W2 O10 2.287(6) . ?
W3 O12 1.737(6) . ?
W3 O11 1.750(5) . ?
W3 O6 1.933(5) 2_556 ?
W3 O9 1.942(5) . ?
W3 O5 2.293(5) 2_556 ?
W3 O10 2.293(6) . ?
Te1 O4 1.921(5) . ?
Te1 O4 1.921(5) 2_556 ?
Te1 O5 1.929(5) 2_556 ?
Te1 O5 1.929(5) . ?
Te1 O10 1.932(5) 2_556 ?
Te1 O10 1.932(5) . ?
O5 W3 2.293(5) 2_556 ?
O6 W3 1.933(5) 2_556 ?
O12 Cu1 2.409(6) . ?
Cu1 N3 2.009(7) . ?
Cu1 N2 2.009(7) . ?
Cu1 N4 2.015(7) . ?
Cu1 N1 2.031(7) . ?
Cu2 N5 2.008(7) 2_557 ?
Cu2 N5 2.008(7) . ?
Cu2 N6 2.031(7) 2_557 ?
Cu2 N6 2.031(7) . ?
N1 C1 1.486(11) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.480(11) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N3 C3 1.491(11) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C4 1.475(11) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C5 1.489(11) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C6 1.494(11) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.515(12) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.515(12) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.495(12) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
O21 H21V 0.90(9) . ?
O21 H21W 0.90(8) . ?
O22 H22V 0.90(8) . ?
O22 H22W 0.90(11) . ?
O23 H23V 0.90(10) . ?
O23 H23W 0.90(9) . ?
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
O1 W1 O2 104.8(3) . . ?
O1 W1 O3 97.2(2) . . ?
O2 W1 O3 99.4(3) . . ?
O1 W1 O6 99.9(2) . . ?
O2 W1 O6 95.8(2) . . ?
O3 W1 O6 153.3(2) . . ?
O1 W1 O4 157.7(2) . . ?
O2 W1 O4 96.6(2) . . ?
O3 W1 O4 72.9(2) . . ?
O6 W1 O4 83.8(2) . . ?
O1 W1 O5 89.4(2) . . ?
O2 W1 O5 164.0(2) . . ?
O3 W1 O5 85.7(2) . . ?
O6 W1 O5 74.2(2) . . ?
O4 W1 O5 70.37(19) . . ?
O7 W2 O8 105.4(3) . . ?
O7 W2 O3 100.9(2) . . ?
O8 W2 O3 95.2(2) . . ?
O7 W2 O9 96.7(2) . . ?
O8 W2 O9 100.4(3) . . ?
O3 W2 O9 152.5(2) . . ?
O7 W2 O4 94.2(2) . . ?
O8 W2 O4 158.9(2) . . ?
O3 W2 O4 73.1(2) . . ?
O9 W2 O4 84.7(2) . . ?
O7 W2 O10 161.8(2) . . ?
O8 W2 O10 91.9(2) . . ?
O3 W2 O10 83.1(2) . . ?
O9 W2 O10 73.9(2) . . ?
O4 W2 O10 69.67(19) . . ?
O12 W3 O11 105.4(3) . . ?
O12 W3 O6 97.0(2) . 2_556 ?
O11 W3 O6 99.1(2) . 2_556 ?
O12 W3 O9 100.3(2) . . ?
O11 W3 O9 97.5(2) . . ?
O6 W3 O9 151.9(2) 2_556 . ?
O12 W3 O5 158.3(2) . 2_556 ?
O11 W3 O5 95.6(2) . 2_556 ?
O6 W3 O5 73.7(2) 2_556 2_556 ?
O9 W3 O5 82.2(2) . 2_556 ?
O12 W3 O10 90.1(2) . . ?
O11 W3 O10 163.5(2) . . ?
O6 W3 O10 84.4(2) 2_556 . ?
O9 W3 O10 73.7(2) . . ?
O5 W3 O10 69.71(19) 2_556 . ?
O4 Te1 O4 180 . 2_556 ?
O4 Te1 O5 94.4(2) . 2_556 ?
O4 Te1 O5 85.6(2) 2_556 2_556 ?
O4 Te1 O5 85.6(2) . . ?
O4 Te1 O5 94.4(2) 2_556 . ?
O5 Te1 O5 180 2_556 . ?
O4 Te1 O10 95.0(2) . 2_556 ?
O4 Te1 O10 85.0(2) 2_556 2_556 ?
O5 Te1 O10 94.5(2) 2_556 2_556 ?
O5 Te1 O10 85.5(2) . 2_556 ?
O4 Te1 O10 85.0(2) . . ?
O4 Te1 O10 95.0(2) 2_556 . ?
O5 Te1 O10 85.5(2) 2_556 . ?
O5 Te1 O10 94.5(2) . . ?
O10 Te1 O10 180 2_556 . ?
W2 O3 W1 117.3(3) . . ?
Te1 O4 W1 102.2(2) . . ?
Te1 O4 W2 103.2(2) . . ?
W1 O4 W2 92.9(2) . . ?
Te1 O5 W1 101.9(2) . . ?
Te1 O5 W3 102.4(2) . 2_556 ?
W1 O5 W3 91.9(2) . 2_556 ?
W3 O6 W1 115.9(3) 2_556 . ?
W2 O9 W3 116.0(3) . . ?
Te1 O10 W2 102.2(2) . . ?
Te1 O10 W3 102.3(2) . . ?
W2 O10 W3 91.8(2) . . ?
W3 O12 Cu1 134.7(3) . . ?
N3 Cu1 N2 99.9(3) . . ?
N3 Cu1 N4 84.2(3) . . ?
N2 Cu1 N4 170.9(3) . . ?
N3 Cu1 N1 175.8(3) . . ?
N2 Cu1 N1 83.8(3) . . ?
N4 Cu1 N1 92.4(3) . . ?
N3 Cu1 O12 89.6(2) . . ?
N2 Cu1 O12 90.3(2) . . ?
N4 Cu1 O12 97.9(2) . . ?
N1 Cu1 O12 88.6(2) . . ?
N5 Cu2 N5 180 2_557 . ?
N5 Cu2 N6 85.3(3) 2_557 2_557 ?
N5 Cu2 N6 94.7(3) . 2_557 ?
N5 Cu2 N6 94.7(3) 2_557 . ?
N5 Cu2 N6 85.3(3) . . ?
N6 Cu2 N6 180 2_557 . ?
C1 N1 Cu1 110.9(5) . . ?
C1 N1 H1A 109.5 . . ?
Cu1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
Cu1 N1 H1B 109.5 . . ?
H1A N1 H1B 108.0 . . ?
C2 N2 Cu1 106.2(5) . . ?
C2 N2 H2A 110.5 . . ?
Cu1 N2 H2A 110.5 . . ?
C2 N2 H2B 110.5 . . ?
Cu1 N2 H2B 110.5 . . ?
H2A N2 H2B 108.7 . . ?
C3 N3 Cu1 108.9(5) . . ?
C3 N3 H3A 109.9 . . ?
Cu1 N3 H3A 109.9 . . ?
C3 N3 H3B 109.9 . . ?
Cu1 N3 H3B 109.9 . . ?
H3A N3 H3B 108.3 . . ?
C4 N4 Cu1 111.7(5) . . ?
C4 N4 H4A 109.3 . . ?
Cu1 N4 H4A 109.3 . . ?
C4 N4 H4B 109.3 . . ?
Cu1 N4 H4B 109.3 . . ?
H4A N4 H4B 107.9 . . ?
C5 N5 Cu2 106.5(5) . . ?
C5 N5 H5A 110.4 . . ?
Cu2 N5 H5A 110.4 . . ?
C5 N5 H5B 110.4 . . ?
Cu2 N5 H5B 110.4 . . ?
H5A N5 H5B 108.6 . . ?
C6 N6 Cu2 108.3(5) . . ?
C6 N6 H6A 110.0 . . ?
Cu2 N6 H6A 110.0 . . ?
C6 N6 H6B 110.0 . . ?
Cu2 N6 H6B 110.0 . . ?
H6A N6 H6B 108.4 . . ?
N1 C1 C2 109.2(7) . . ?
N1 C1 H1C 109.8 . . ?
C2 C1 H1C 109.8 . . ?
N1 C1 H1D 109.8 . . ?
C2 C1 H1D 109.8 . . ?
H1C C1 H1D 108.3 . . ?
N2 C2 C1 108.4(6) . . ?
N2 C2 H2C 110.0 . . ?
C1 C2 H2C 110.0 . . ?
N2 C2 H2D 110.0 . . ?
C1 C2 H2D 110.0 . . ?
H2C C2 H2D 108.4 . . ?
N3 C3 C4 108.3(7) . . ?
N3 C3 H3C 110.0 . . ?
C4 C3 H3C 110.0 . . ?
N3 C3 H3D 110.0 . . ?
C4 C3 H3D 110.0 . . ?
H3C C3 H3D 108.4 . . ?
N4 C4 C3 110.4(7) . . ?
N4 C4 H4C 109.6 . . ?
C3 C4 H4C 109.6 . . ?
N4 C4 H4D 109.6 . . ?
C3 C4 H4D 109.6 . . ?
H4C C4 H4D 108.1 . . ?
N5 C5 C6 107.7(7) . . ?
N5 C5 H5C 110.2 . . ?
C6 C5 H5C 110.2 . . ?
N5 C5 H5D 110.2 . . ?
C6 C5 H5D 110.2 . . ?
H5C C5 H5D 108.5 . . ?
N6 C6 C5 109.6(7) . . ?
N6 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N6 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.2 . . ?
H21V O21 H21W 87(10) . . ?
H22V O22 H22W 100(10) . . ?
H23V O23 H23W 94(10) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 25.01
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 1.123
_refine_diff_density_min -2.200
_refine_diff_density_rms 0.270