#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180007 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/01/7030123.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_7030123
loop_
_publ_author_name
'Wu, Xiao-Yuan'
'Zhang, Qi-Kai'
'Kuang, Xiao-Fei'
'Yang, Wen-bin'
'Yu, Rong-Min'
'Lu, Can-Zhong'
_publ_section_title
;
 Two hybrid polyoxometalate-pillared metal-organic frameworks.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11783
_journal_page_last               11787
_journal_paper_doi               10.1039/c2dt30920c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H32 Cu5 N30 O44 Si W12, 4(H2 O)'
_chemical_formula_sum            'C36 H40 Cu5 N30 O48 Si W12'
_chemical_formula_weight         4212.97
_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
_cell_angle_alpha                104.904(8)
_cell_angle_beta                 111.632(6)
_cell_angle_gamma                105.607(2)
_cell_formula_units_Z            1
_cell_length_a                   12.195(10)
_cell_length_b                   13.489(11)
_cell_length_c                   14.276(12)
_cell_measurement_reflns_used    2101
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4449
_cell_measurement_theta_min      2.7710
_cell_volume                     1929(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Mercury2
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0773
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14945
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    19.287
_exptl_absorpt_correction_T_max  0.1133
_exptl_absorpt_correction_T_min  0.1133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1897
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.904
_refine_diff_density_min         -2.854
_refine_diff_density_rms         0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         8720
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0940
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0091P)²+149.1118P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                7051
_reflns_number_total             8720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30920c.txt
_cod_data_source_block           a_833800
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7030123
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
Si1 Si -0.5000 0.0000 -0.5000 0.0214(17) Uani 1 2 d S
W1 W -0.35316(11) -0.06191(9) -0.27041(8) 0.0356(3) Uani 1 1 d .
W2 W -0.78300(10) -0.05100(9) -0.46902(9) 0.0374(3) Uani 1 1 d .
W3 W -0.51954(13) -0.14510(8) -0.75405(9) 0.0439(3) Uani 1 1 d .
W4 W -0.80162(9) -0.19737(8) -0.72336(8) 0.0297(2) Uani 1 1 d .
W5 W -0.65603(9) -0.25759(7) -0.49204(8) 0.0288(2) Uani 1 1 d .
W6 W -0.37518(12) -0.20641(9) -0.52617(9) 0.0444(3) Uani 1 1 d .
Cu1 Cu -0.1505(3) -0.0563(2) 0.0306(2) 0.0268(6) Uani 1 1 d .
Cu2 Cu 0.0326(3) 0.4510(2) 0.1261(2) 0.0294(6) Uani 1 1 d .
Cu3 Cu -0.5000 -0.5000 0.0000 0.0378(11) Uani 1 2 d S
O1 O -0.634(3) -0.096(2) -0.535(2) 0.018(6) Uani 0.50 1 d PU
O2 O -0.399(2) 0.057(2) -0.363(2) 0.014(5) Uani 0.50 1 d PU
O3 O -0.512(2) 0.101(2) -0.538(2) 0.016(5) Uani 0.50 1 d PU
O4 O -0.420(2) -0.058(2) -0.558(2) 0.015(5) Uani 0.50 1 d PU
O5 O -0.743(2) -0.177(2) -0.4495(15) 0.061(6) Uani 1 1 d .
O6 O -0.5184(18) -0.175(2) -0.3452(17) 0.067(7) Uani 1 1 d U
O7 O -0.2843(16) -0.0922(17) -0.1602(15) 0.046(5) Uani 1 1 d .
O8 O -0.221(3) 0.0683(19) -0.243(2) 0.072(7) Uani 1 1 d U
O9 O -0.308(2) -0.140(2) -0.3706(18) 0.068(7) Uani 1 1 d .
O10 O -0.759(3) 0.084(2) -0.4893(19) 0.090(8) Uani 1 1 d U
O11A O -0.674(3) 0.047(3) -0.309(3) 0.026(7) Uani 0.50 1 d P
O11B O -0.627(3) 0.031(2) -0.334(2) 0.024(7) Uani 0.50 1 d P
O12 O -0.576(2) -0.0296(19) -0.781(2) 0.076(7) Uani 1 1 d U
O13 O -0.5275(17) -0.2082(14) -0.8742(15) 0.040(4) Uani 1 1 d .
O14 O -0.689(2) -0.2254(17) -0.779(2) 0.063(6) Uani 1 1 d U
O15A O -0.441(3) -0.247(3) -0.687(3) 0.027(7) Uani 0.50 1 d P
O15B O -0.492(4) -0.222(3) -0.665(3) 0.039(9) Uani 0.50 1 d P
O16 O -0.943(2) -0.2936(16) -0.8267(17) 0.064(7) Uani 1 1 d .
O17 O -0.760(2) -0.287(2) -0.6391(19) 0.067(6) Uani 1 1 d U
O18 O -0.732(2) -0.3776(18) -0.4830(19) 0.065(6) Uani 1 1 d U
O19 O -0.5369(19) -0.289(2) -0.5362(16) 0.070(8) Uani 1 1 d .
O20 O -0.314(2) -0.3056(17) -0.5344(17) 0.053(5) Uani 1 1 d .
O21 O -0.915(2) -0.078(2) -0.454(2) 0.071(7) Uani 1 1 d .
O22 O -0.851(2) -0.126(2) -0.6210(18) 0.066(7) Uani 1 1 d .
OW1 O -0.0107(17) 0.4886(18) 0.2479(16) 0.051(5) Uani 1 1 d .
HW1B H 0.0509 0.5521 0.2920 0.061 Uiso 1 1 d R
HW1A H -0.0738 0.5070 0.2242 0.061 Uiso 1 1 d R
OW2 O 0.0017(18) 0.0114(19) 0.2302(17) 0.055(6) Uani 1 1 d .
HW2A H 0.0226 0.0773 0.2743 0.066 Uiso 1 1 d R
HW2B H 0.0698 -0.0002 0.2418 0.066 Uiso 1 1 d R
OW3 O 0.027(4) 0.223(3) 0.358(3) 0.129(13) Uani 1 1 d .
HW3A H -0.0129 0.1802 0.3792 0.155 Uiso 1 1 d R
HW3B H 0.1072 0.2501 0.4015 0.155 Uiso 1 1 d R
OW4 O -0.043(4) 0.400(4) 0.392(3) 0.147(16) Uani 1 1 d .
HW4A H -0.0330 0.4296 0.3479 0.176 Uiso 1 1 d R
HW4B H -0.0211 0.3448 0.3825 0.176 Uiso 1 1 d R
N1 N -0.2001(18) -0.2000(17) 0.1425(16) 0.032(5) Uani 1 1 d .
N2 N -0.255(2) -0.1877(19) 0.0423(17) 0.039(5) Uani 1 1 d .
N3 N -0.3655(19) -0.2751(16) -0.0211(17) 0.032(5) Uani 1 1 d .
N4 N -0.3854(18) -0.3467(15) 0.0251(16) 0.028(4) Uani 1 1 d U
C5 C -0.282(3) -0.2971(18) 0.126(2) 0.034(6) Uani 1 1 d .
C6 C -0.267(2) -0.3560(18) 0.1991(19) 0.026(5) Uani 1 1 d .
N7 N -0.3626(18) -0.4613(15) 0.1515(15) 0.027(4) Uani 1 1 d U
C8 C -0.353(3) -0.528(2) 0.208(2) 0.038(6) Uani 1 1 d .
H8A H -0.4159 -0.6006 0.1772 0.046 Uiso 1 1 calc R
C9 C -0.251(3) -0.488(2) 0.311(3) 0.046(7) Uani 1 1 d .
H9A H -0.2487 -0.5340 0.3492 0.055 Uiso 1 1 calc R
C10 C -0.151(3) -0.382(3) 0.360(3) 0.069(11) Uani 1 1 d .
H10A H -0.0812 -0.3584 0.4284 0.082 Uiso 1 1 calc R
C11 C -0.161(2) -0.313(2) 0.301(2) 0.041(6) Uani 1 1 d .
H11A H -0.0987 -0.2410 0.3293 0.049 Uiso 1 1 calc R
N12 N 0.1344(17) 0.5121(15) 0.0575(16) 0.026(4) Uani 1 1 d .
N13 N 0.1239(19) 0.5402(15) -0.0261(16) 0.028(4) Uani 1 1 d .
N14 N 0.2332(19) 0.5615(18) -0.037(2) 0.045(6) Uani 1 1 d .
N15 N 0.3167(18) 0.5466(15) 0.0456(17) 0.030(4) Uani 1 1 d .
C16 C 0.257(2) 0.518(2) 0.102(2) 0.030(5) Uani 1 1 d U
C17 C 0.299(2) 0.4905(17) 0.1989(17) 0.021(4) Uani 1 1 d U
C18 C 0.415(2) 0.497(2) 0.256(2) 0.037(6) Uani 1 1 d .
H18A H 0.4820 0.5300 0.2423 0.044 Uiso 1 1 calc R
C19 C 0.438(3) 0.453(3) 0.340(2) 0.047(7) Uani 1 1 d .
H19A H 0.5182 0.4535 0.3788 0.056 Uiso 1 1 calc R
C20 C 0.341(3) 0.413(2) 0.359(3) 0.054(8) Uani 1 1 d .
H20A H 0.3523 0.3798 0.4093 0.065 Uiso 1 1 calc R
C21 C 0.226(2) 0.4177(19) 0.309(2) 0.031(5) Uani 1 1 d .
H21A H 0.1634 0.3960 0.3300 0.037 Uiso 1 1 calc R
N22 N 0.2039(18) 0.4556(16) 0.2248(16) 0.030(4) Uani 1 1 d .
N23 N -0.0216(17) 0.2633(13) 0.0550(16) 0.025(4) Uani 1 1 d .
N24 N 0.0663(15) 0.2384(13) 0.0273(14) 0.018(3) Uani 1 1 d U
N25 N 0.0515(17) 0.1353(14) 0.0145(16) 0.025(4) Uani 1 1 d .
N26 N -0.0488(17) 0.0884(13) 0.0293(14) 0.020(4) Uani 1 1 d .
C27 C -0.0960(18) 0.1686(16) 0.0534(16) 0.017(4) Uani 1 1 d U
C28 C -0.199(2) 0.1429(18) 0.0780(19) 0.027(5) Uani 1 1 d U
N29 N -0.238(2) 0.0374(17) 0.0766(18) 0.034(5) Uani 1 1 d .
C30 C -0.330(3) 0.011(2) 0.107(2) 0.047(7) Uani 1 1 d U
H30A H -0.3564 -0.0603 0.1087 0.057 Uiso 1 1 calc R
C31 C -0.388(4) 0.078(3) 0.137(3) 0.074(13) Uani 1 1 d .
H31A H -0.4457 0.0570 0.1639 0.089 Uiso 1 1 calc R
C32 C -0.355(3) 0.179(3) 0.125(3) 0.053(8) Uani 1 1 d U
H32A H -0.4001 0.2235 0.1341 0.063 Uiso 1 1 calc R
C33 C -0.257(3) 0.215(2) 0.100(2) 0.041(6) Uani 1 1 d .
H33A H -0.2300 0.2850 0.0972 0.050 Uiso 1 1 calc 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
O1 Si1 O1 180.000(4) 2_454 .
O1 Si1 O3 65.4(13) 2_454 .
O1 Si1 O3 114.6(13) . .
O1 Si1 O3 114.6(13) 2_454 2_454
O1 Si1 O3 65.4(13) . 2_454
O3 Si1 O3 180.000(7) . 2_454
O1 Si1 O2 67.0(13) 2_454 .
O1 Si1 O2 113.0(13) . .
O3 Si1 O2 108.0(13) . .
O3 Si1 O2 72.0(13) 2_454 .
O1 Si1 O2 113.0(13) 2_454 2_454
O1 Si1 O2 67.0(13) . 2_454
O3 Si1 O2 72.0(13) . 2_454
O3 Si1 O2 108.0(13) 2_454 2_454
O2 Si1 O2 180.000(6) . 2_454
O1 Si1 O4 108.6(13) 2_454 2_454
O1 Si1 O4 71.4(13) . 2_454
O3 Si1 O4 72.8(13) . 2_454
O3 Si1 O4 107.2(13) 2_454 2_454
O2 Si1 O4 75.3(12) . 2_454
O2 Si1 O4 104.7(12) 2_454 2_454
O1 Si1 O4 71.4(13) 2_454 .
O1 Si1 O4 108.6(13) . .
O3 Si1 O4 107.2(13) . .
O3 Si1 O4 72.8(13) 2_454 .
O2 Si1 O4 104.7(12) . .
O2 Si1 O4 75.3(12) 2_454 .
O4 Si1 O4 180.0(17) 2_454 .
O7 W1 O12 101.0(12) . 2_454
O7 W1 O6 101.3(10) . .
O12 W1 O6 86.3(10) 2_454 .
O7 W1 O8 102.6(11) . .
O12 W1 O8 87.4(10) 2_454 .
O6 W1 O8 156.0(12) . .
O7 W1 O9 102.0(11) . .
O12 W1 O9 157.0(12) 2_454 .
O6 W1 O9 90.2(9) . .
O8 W1 O9 86.7(10) . .
O7 W1 O2 155.6(9) . .
O12 W1 O2 64.3(10) 2_454 .
O6 W1 O2 97.2(10) . .
O8 W1 O2 59.4(10) . .
O9 W1 O2 93.8(10) . .
O7 W1 O3 156.8(9) . 2_454
O12 W1 O3 93.6(11) 2_454 2_454
O6 W1 O3 61.4(10) . 2_454
O8 W1 O3 96.0(10) . 2_454
O9 W1 O3 65.1(10) . 2_454
O2 W1 O3 47.6(9) . 2_454
O21 W2 O22 102.2(12) . .
O21 W2 O10 102.9(13) . .
O22 W2 O10 88.2(10) . .
O21 W2 O11B 113.7(13) . .
O22 W2 O11B 143.9(12) . .
O10 W2 O11B 87.3(11) . .
O21 W2 O5 99.7(11) . .
O22 W2 O5 88.9(8) . .
O10 W2 O5 157.3(12) . .
O11B W2 O5 81.9(11) . .
O21 W2 O11A 90.5(13) . .
O22 W2 O11A 166.8(13) . .
O10 W2 O11A 85.5(11) . .
O11B W2 O11A 24.3(11) . .
O5 W2 O11A 92.5(10) . .
O21 W2 O4 156.8(11) . 2_454
O22 W2 O4 94.8(10) . 2_454
O10 W2 O4 61.5(11) . 2_454
O11B W2 O4 52.2(12) . 2_454
O5 W2 O4 96.3(10) . 2_454
O11A W2 O4 72.1(12) . 2_454
O21 W2 O1 156.0(11) . .
O22 W2 O1 63.2(9) . .
O10 W2 O1 95.8(12) . .
O11B W2 O1 81.7(12) . .
O5 W2 O1 63.0(9) . .
O11A W2 O1 106.0(11) . .
O4 W2 O1 47.1(9) 2_454 .
O13 W3 O11B 111.6(12) . 2_454
O13 W3 O15B 113.2(13) . .
O11B W3 O15B 93.4(15) 2_454 .
O13 W3 O14 101.9(9) . .
O11B W3 O14 146.1(13) 2_454 .
O15B W3 O14 77.3(15) . .
O13 W3 O12 100.0(10) . .
O11B W3 O12 82.5(13) 2_454 .
O15B W3 O12 145.5(15) . .
O14 W3 O12 87.1(9) . .
O13 W3 O11A 90.3(10) . 2_454
O11B W3 O11A 23.0(11) 2_454 2_454
O15B W3 O11A 94.6(15) . 2_454
O14 W3 O11A 167.3(12) . 2_454
O12 W3 O11A 94.4(11) . 2_454
O13 W3 O15A 92.3(12) . .
O11B W3 O15A 89.0(14) 2_454 .
O15B W3 O15A 25.0(14) . .
O14 W3 O15A 94.6(12) . .
O12 W3 O15A 167.0(12) . .
O11A W3 O15A 81.1(12) 2_454 .
O13 W3 O4 155.3(9) . .
O11B W3 O4 52.1(12) 2_454 .
O15B W3 O4 56.5(12) . .
O14 W3 O4 97.5(10) . .
O12 W3 O4 96.1(10) . .
O11A W3 O4 69.8(11) 2_454 .
O15A W3 O4 70.9(11) . .
O13 W3 O2 153.7(9) . 2_454
O11B W3 O2 85.8(12) 2_454 2_454
O15B W3 O2 84.0(14) . 2_454
O14 W3 O2 61.1(9) . 2_454
O12 W3 O2 61.6(9) . 2_454
O11A W3 O2 108.7(11) 2_454 2_454
O15A W3 O2 108.1(11) . 2_454
O4 W3 O2 51.0(8) . 2_454
O16 W4 O14 100.3(12) . .
O16 W4 O8 104.2(11) . 2_454
O14 W4 O8 88.3(9) . 2_454
O16 W4 O22 102.3(12) . .
O14 W4 O22 157.4(11) . .
O8 W4 O22 86.4(9) 2_454 .
O16 W4 O17 98.4(10) . .
O14 W4 O17 88.4(10) . .
O8 W4 O17 157.4(11) 2_454 .
O22 W4 O17 88.1(9) . .
O16 W4 O2 158.2(11) . 2_454
O14 W4 O2 65.1(10) . 2_454
O8 W4 O2 61.1(11) 2_454 2_454
O22 W4 O2 93.2(11) . 2_454
O17 W4 O2 97.3(10) . 2_454
O16 W4 O1 156.3(11) . .
O14 W4 O1 94.5(10) . .
O8 W4 O1 94.5(11) 2_454 .
O22 W4 O1 64.2(10) . .
O17 W4 O1 63.4(9) . .
O2 W4 O1 45.4(9) 2_454 .
O18 W5 O5 97.5(12) . .
O18 W5 O17 101.1(11) . .
O5 W5 O17 89.8(9) . .
O18 W5 O19 103.4(12) . .
O5 W5 O19 159.1(12) . .
O17 W5 O19 86.9(10) . .
O18 W5 O6 100.7(11) . .
O5 W5 O6 86.6(9) . .
O17 W5 O6 158.2(11) . .
O19 W5 O6 88.8(8) . .
O18 W5 O3 159.1(11) . 2_454
O5 W5 O3 94.8(10) . 2_454
O17 W5 O3 95.7(10) . 2_454
O19 W5 O3 65.0(10) . 2_454
O6 W5 O3 63.2(10) . 2_454
O18 W5 O1 157.6(11) . .
O5 W5 O1 66.3(10) . .
O17 W5 O1 65.1(10) . .
O19 W5 O1 93.7(11) . .
O6 W5 O1 93.9(11) . .
O3 W5 O1 43.0(9) 2_454 .
O20 W6 O15B 112.4(14) . .
O20 W6 O10 101.3(12) . 2_454
O15B W6 O10 93.6(13) . 2_454
O20 W6 O9 99.4(10) . .
O15B W6 O9 147.2(14) . .
O10 W6 O9 87.6(11) 2_454 .
O20 W6 O19 100.0(11) . .
O15B W6 O19 79.0(15) . .
O10 W6 O19 158.7(12) 2_454 .
O9 W6 O19 88.1(9) . .
O20 W6 O15A 89.6(12) . .
O15B W6 O15A 26.6(13) . .
O10 W6 O15A 85.0(12) 2_454 .
O9 W6 O15A 169.4(12) . .
O19 W6 O15A 96.0(12) . .
O20 W6 O4 156.9(10) . .
O15B W6 O4 57.5(12) . .
O10 W6 O4 61.5(11) 2_454 .
O9 W6 O4 95.4(10) . .
O19 W6 O4 98.1(10) . .
O15A W6 O4 74.3(11) . .
O20 W6 O3 154.5(9) . 2_454
O15B W6 O3 83.1(14) . 2_454
O10 W6 O3 97.6(12) 2_454 2_454
O9 W6 O3 64.4(9) . 2_454
O19 W6 O3 61.9(9) . 2_454
O15A W6 O3 109.1(11) . 2_454
O4 W6 O3 48.6(9) . 2_454
N2 Cu1 N25 92.5(8) . 2
N2 Cu1 N29 93.4(8) . .
N25 Cu1 N29 174.1(7) 2 .
N2 Cu1 N26 173.9(8) . .
N25 Cu1 N26 93.2(7) 2 .
N29 Cu1 N26 80.9(7) . .
N2 Cu1 O7 100.3(7) . .
N25 Cu1 O7 90.1(7) 2 .
N29 Cu1 O7 89.5(8) . .
N26 Cu1 O7 81.9(6) . .
N13 Cu2 OW1 90.9(8) 2_565 .
N13 Cu2 N12 92.8(7) 2_565 .
OW1 Cu2 N12 145.0(8) . .
N13 Cu2 N22 173.5(8) 2_565 .
OW1 Cu2 N22 92.5(8) . .
N12 Cu2 N22 81.3(7) . .
N13 Cu2 N23 100.7(7) 2_565 .
OW1 Cu2 N23 109.2(8) . .
N12 Cu2 N23 104.3(7) . .
N22 Cu2 N23 83.4(7) . .
N7 Cu3 N7 180.0(11) . 2_445
N7 Cu3 N4 82.4(7) . .
N7 Cu3 N4 97.6(7) 2_445 .
N7 Cu3 N4 97.6(7) . 2_445
N7 Cu3 N4 82.4(7) 2_445 2_445
N4 Cu3 N4 180.000(2) . 2_445
Si1 O1 O3 57.9(12) . 2_454
Si1 O1 O2 59.4(12) . 2_454
O3 O1 O2 98.1(17) 2_454 2_454
Si1 O1 W5 124.8(15) . .
O3 O1 W5 66.9(12) 2_454 .
O2 O1 W5 134.5(16) 2_454 .
Si1 O1 W4 122.7(14) . .
O3 O1 W4 133.4(17) 2_454 .
O2 O1 W4 63.3(11) 2_454 .
W5 O1 W4 95.2(9) . .
Si1 O1 W2 119.8(14) . .
O3 O1 W2 129.0(16) 2_454 .
O2 O1 W2 125.3(15) 2_454 .
W5 O1 W2 93.3(9) . .
W4 O1 W2 93.0(9) . .
Si1 O2 O1 53.6(11) . 2_454
Si1 O2 W4 124.9(14) . 2_454
O1 O2 W4 71.3(12) 2_454 2_454
Si1 O2 W1 119.9(12) . .
O1 O2 W1 136.7(15) 2_454 .
W4 O2 W1 99.1(9) 2_454 .
Si1 O2 W3 115.6(12) . 2_454
O1 O2 W3 128.0(15) 2_454 2_454
W4 O2 W3 96.6(9) 2_454 2_454
W1 O2 W3 94.5(9) . 2_454
Si1 O3 O1 56.7(12) . 2_454
Si1 O3 W5 126.8(14) . 2_454
O1 O3 W5 70.1(12) 2_454 2_454
Si1 O3 W1 120.5(13) . 2_454
O1 O3 W1 135.1(17) 2_454 2_454
W5 O3 W1 95.4(9) 2_454 2_454
Si1 O3 W6 118.2(14) . 2_454
O1 O3 W6 130.0(16) 2_454 2_454
W5 O3 W6 95.5(9) 2_454 2_454
W1 O3 W6 92.6(9) 2_454 2_454
Si1 O4 W6 120.4(13) . .
Si1 O4 W2 121.7(13) . 2_454
W6 O4 W2 98.2(9) . 2_454
Si1 O4 W3 118.1(13) . .
W6 O4 W3 96.1(9) . .
W2 O4 W3 96.9(9) 2_454 .
W5 O5 W2 136.9(13) . .
W1 O6 W5 139.0(14) . .
W1 O7 Cu1 157.6(11) . .
W1 O8 W4 139.8(16) . 2_454
W1 O9 W6 137.7(13) . .
W2 O10 W6 138.6(17) . 2_454
O11B O11A W2 71(3) . .
O11B O11A W3 55(3) . 2_454
W2 O11A W3 120.8(16) . 2_454
O11A O11B W3 102(4) . 2_454
O11A O11B W2 84(4) . .
W3 O11B W2 152.8(18) 2_454 .
W1 O12 W3 139.6(14) 2_454 .
W4 O14 W3 137.0(13) . .
O15B O15A W6 70(3) . .
O15B O15A W3 60(3) . .
W6 O15A W3 117.6(15) . .
O15A O15B W3 95(4) . .
O15A O15B W6 84(4) . .
W3 O15B W6 142(2) . .
W5 O17 W4 135.7(13) . .
W5 O19 W6 137.3(14) . .
W2 O22 W4 139.2(13) . .
Cu2 OW1 HW1B 101.2 . .
Cu2 OW1 HW1A 105.3 . .
HW1B OW1 HW1A 101.6 . .
HW2A OW2 HW2B 108.7 . .
HW3A OW3 HW3B 108.2 . .
HW4A OW4 HW4B 108.4 . .
C5 N1 N2 104(2) . .
N3 N2 N1 106.2(19) . .
N3 N2 Cu1 137.4(16) . .
N1 N2 Cu1 116.3(16) . .
N2 N3 N4 112.5(19) . .
N3 N4 C5 104.1(18) . .
N3 N4 Cu3 144.7(16) . .
C5 N4 Cu3 111.0(14) . .
N1 C5 N4 113(2) . .
N1 C5 C6 127(2) . .
N4 C5 C6 120(2) . .
N7 C6 C11 124(2) . .
N7 C6 C5 113(2) . .
C11 C6 C5 123(2) . .
C8 N7 C6 118(2) . .
C8 N7 Cu3 127.5(17) . .
C6 N7 Cu3 114.3(14) . .
N7 C8 C9 120(2) . .
N7 C8 H8A 120.2 . .
C9 C8 H8A 120.2 . .
C8 C9 C10 123(3) . .
C8 C9 H9A 118.3 . .
C10 C9 H9A 118.3 . .
C9 C10 C11 117(3) . .
C9 C10 H10A 121.7 . .
C11 C10 H10A 121.7 . .
C6 C11 C10 118(3) . .
C6 C11 H11A 121.1 . .
C10 C11 H11A 121.1 . .
N13 N12 C16 103.5(18) . .
N13 N12 Cu2 142.5(15) . .
C16 N12 Cu2 113.5(16) . .
N12 N13 N14 112.2(19) . .
N12 N13 Cu2 124.3(14) . 2_565
N14 N13 Cu2 123.5(16) . 2_565
N15 N14 N13 106(2) . .
C16 N15 N14 107.0(19) . .
N15 C16 N12 111(2) . .
N15 C16 C17 132(2) . .
N12 C16 C17 117(2) . .
C18 C17 N22 122(2) . .
C18 C17 C16 125(2) . .
N22 C17 C16 112.8(18) . .
C17 C18 C19 119(2) . .
C17 C18 H18A 120.4 . .
C19 C18 H18A 120.4 . .
C20 C19 C18 117(3) . .
C20 C19 H19A 121.3 . .
C18 C19 H19A 121.3 . .
C19 C20 C21 123(3) . .
C19 C20 H20A 118.5 . .
C21 C20 H20A 118.5 . .
C20 C21 N22 119(2) . .
C20 C21 H21A 120.6 . .
N22 C21 H21A 120.6 . .
C17 N22 C21 119.1(19) . .
C17 N22 Cu2 115.4(14) . .
C21 N22 Cu2 125.2(15) . .
C27 N23 N24 106.0(15) . .
C27 N23 Cu2 139.5(15) . .
N24 N23 Cu2 112.3(12) . .
N25 N24 N23 110.3(16) . .
N24 N25 N26 108.4(17) . .
N24 N25 Cu1 126.5(14) . 2
N26 N25 Cu1 125.0(13) . 2
N25 N26 C27 107.3(15) . .
N25 N26 Cu1 141.7(14) . .
C27 N26 Cu1 111.0(13) . .
N23 C27 N26 107.9(17) . .
N23 C27 C28 133(2) . .
N26 C27 C28 119.2(17) . .
N29 C28 C33 123(2) . .
N29 C28 C27 112.7(19) . .
C33 C28 C27 124(2) . .
C30 N29 C28 116(2) . .
C30 N29 Cu1 128.4(18) . .
C28 N29 Cu1 116.0(15) . .
N29 C30 C31 126(3) . .
N29 C30 H30A 116.9 . .
C31 C30 H30A 116.9 . .
C30 C31 C32 116(3) . .
C30 C31 H31A 122.1 . .
C32 C31 H31A 122.1 . .
C33 C32 C31 121(3) . .
C33 C32 H32A 119.6 . .
C31 C32 H32A 119.6 . .
C28 C33 C32 118(3) . .
C28 C33 H33A 121.0 . .
C32 C33 H33A 121.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.59(3) 2_454
Si1 O1 1.59(3) .
Si1 O3 1.61(3) .
Si1 O3 1.61(3) 2_454
Si1 O2 1.70(3) .
Si1 O2 1.70(3) 2_454
Si1 O4 1.71(3) 2_454
Si1 O4 1.71(3) .
W1 O7 1.700(16) .
W1 O12 1.84(2) 2_454
W1 O6 1.86(2) .
W1 O8 1.87(2) .
W1 O9 1.886(19) .
W1 O2 2.37(3) .
W1 O3 2.44(3) 2_454
W2 O21 1.66(2) .
W2 O22 1.87(2) .
W2 O10 1.87(2) .
W2 O11B 1.90(3) .
W2 O5 1.95(2) .
W2 O11A 2.00(3) .
W2 O4 2.33(3) 2_454
W2 O1 2.48(3) .
W3 O13 1.660(18) .
W3 O11B 1.73(3) 2_454
W3 O15B 1.84(4) .
W3 O14 1.91(2) .
W3 O12 1.93(2) .
W3 O11A 2.07(4) 2_454
W3 O15A 2.11(3) .
W3 O4 2.39(3) .
W3 O2 2.45(3) 2_454
W4 O16 1.663(18) .
W4 O14 1.89(2) .
W4 O8 1.90(2) 2_454
W4 O22 1.912(19) .
W4 O17 1.95(2) .
W4 O2 2.28(3) 2_454
W4 O1 2.42(3) .
W5 O18 1.70(2) .
W5 O5 1.854(19) .
W5 O17 1.87(2) .
W5 O19 1.89(2) .
W5 O6 1.91(2) .
W5 O3 2.33(3) 2_454
W5 O1 2.38(3) .
W6 O20 1.695(18) .
W6 O15B 1.88(4) .
W6 O10 1.89(2) 2_454
W6 O9 1.91(2) .
W6 O19 1.92(2) .
W6 O15A 1.99(3) .
W6 O4 2.33(3) .
W6 O3 2.46(3) 2_454
Cu1 N2 1.97(2) .
Cu1 N25 1.980(19) 2
Cu1 N29 1.99(2) .
Cu1 N26 2.020(16) .
Cu1 O7 2.435(17) .
Cu2 N13 1.97(2) 2_565
Cu2 OW1 1.98(2) .
Cu2 N12 1.99(2) .
Cu2 N22 2.016(19) .
Cu2 N23 2.272(16) .
Cu3 N7 2.009(18) .
Cu3 N7 2.009(18) 2_445
Cu3 N4 2.014(18) .
Cu3 N4 2.014(18) 2_445
O1 O3 1.73(4) 2_454
O1 O2 1.82(4) 2_454
O2 O1 1.82(4) 2_454
O2 W4 2.28(2) 2_454
O2 W3 2.45(3) 2_454
O3 O1 1.73(4) 2_454
O3 W5 2.33(3) 2_454
O3 W1 2.44(3) 2_454
O3 W6 2.46(3) 2_454
O4 W2 2.33(3) 2_454
O8 W4 1.90(2) 2_454
O10 W6 1.89(2) 2_454
O11A O11B 0.83(3) .
O11A W3 2.07(3) 2_454
O11B W3 1.73(3) 2_454
O12 W1 1.84(2) 2_454
O15A O15B 0.90(4) .
OW1 HW1B 0.8497 .
OW1 HW1A 0.8500 .
OW2 HW2A 0.8499 .
OW2 HW2B 0.8501 .
OW3 HW3A 0.8501 .
OW3 HW3B 0.8499 .
OW4 HW4A 0.8497 .
OW4 HW4B 0.8500 .
N1 C5 1.32(3) .
N1 N2 1.41(3) .
N2 N3 1.31(3) .
N3 N4 1.32(2) .
N4 C5 1.35(3) .
C5 C6 1.46(3) .
C6 N7 1.37(3) .
C6 C11 1.37(3) .
N7 C8 1.35(3) .
C8 C9 1.37(4) .
C8 H8A 0.9300 .
C9 C10 1.39(4) .
C9 H9A 0.9300 .
C10 C11 1.41(4) .
C10 H10A 0.9300 .
C11 H11A 0.9300 .
N12 N13 1.32(3) .
N12 C16 1.36(3) .
N13 N14 1.36(3) .
N13 Cu2 1.97(2) 2_565
N14 N15 1.35(3) .
N15 C16 1.33(3) .
C16 C17 1.47(3) .
C17 C18 1.31(3) .
C17 N22 1.35(3) .
C18 C19 1.43(4) .
C18 H18A 0.9300 .
C19 C20 1.32(4) .
C19 H19A 0.9300 .
C20 C21 1.34(4) .
C20 H20A 0.9300 .
C21 N22 1.39(3) .
C21 H21A 0.9300 .
N23 C27 1.34(2) .
N23 N24 1.36(2) .
N24 N25 1.31(2) .
N25 N26 1.34(2) .
N25 Cu1 1.980(19) 2
N26 C27 1.38(3) .
C27 C28 1.40(3) .
C28 N29 1.37(3) .
C28 C33 1.38(3) .
N29 C30 1.34(3) .
C30 C31 1.37(4) .
C30 H30A 0.9300 .
C31 C32 1.39(4) .
C31 H31A 0.9300 .
C32 C33 1.38(4) .
C32 H32A 0.9300 .
C33 H33A 0.9300 .
