#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316018.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_4316018
loop_
_publ_author_name
'Guangfeng Hou'
'Lihua Bi'
'Bao Li'
'Lixin Wu'
_publ_section_title
;
 Reaction Controlled Assemblies of Polyoxotungstates (-molybdates) and
 Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6474
_journal_page_last               6483
_journal_paper_doi               10.1021/ic1001495
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C42 H42 Cu3 N12 O40 P W12'
_chemical_formula_sum            'C42 H42 Cu3 N12 O40 P W12'
_chemical_formula_weight         3782.58
_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                102.340(15)
_cell_angle_beta                 109.300(16)
_cell_angle_gamma                105.490(17)
_cell_formula_units_Z            1
_cell_length_a                   12.029(6)
_cell_length_b                   12.671(5)
_cell_length_c                   13.429(5)
_cell_measurement_reflns_used    14902
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.05
_cell_volume                     1756.0(13)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.1196
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13125
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.569
_exptl_absorpt_correction_T_max  0.2065
_exptl_absorpt_correction_T_min  0.1677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1687
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.135
_refine_diff_density_min         -3.088
_refine_diff_density_rms         0.407
_refine_ls_extinction_coef       0.00217(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0619
_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)+(0.0000P)²+27.8581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                5126
_reflns_number_total             5858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1001495_si_002_4.cif
_cod_data_source_block           Compound-4
_cod_database_code               4316018
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
C1 C 0.667(3) 0.536(2) 0.539(3) 0.096(11) Uani 1 1 d . . .
H1 H 0.5887 0.4844 0.4840 0.116 Uiso 1 1 calc R . .
C2 C 0.6902(18) 0.6510(18) 0.5891(16) 0.050(5) Uani 1 1 d . . .
H2 H 0.6333 0.6891 0.5767 0.060 Uiso 1 1 calc R . .
C3 C 0.8137(19) 0.6964(16) 0.661(2) 0.061(7) Uani 1 1 d . . .
H3 H 0.8596 0.7724 0.7092 0.074 Uiso 1 1 calc R . .
C4 C 0.985(2) 0.6072(19) 0.6989(19) 0.063(6) Uani 1 1 d U . .
H4A H 1.0297 0.6226 0.6520 0.076 Uiso 1 1 calc R . .
H4B H 0.9807 0.5315 0.7056 0.076 Uiso 1 1 calc R . .
C5 C 1.0558(18) 0.6979(14) 0.8121(18) 0.048(5) Uani 1 1 d . . .
C6 C 1.1468(19) 0.8027(16) 0.8300(19) 0.052(5) Uani 1 1 d . . .
H6 H 1.1661 0.8189 0.7720 0.063 Uiso 1 1 calc R . .
C7 C 1.2087(17) 0.8837(15) 0.9395(17) 0.042(4) Uani 1 1 d . . .
H7 H 1.2699 0.9539 0.9520 0.050 Uiso 1 1 calc R . .
C8 C 1.1839(15) 0.8650(13) 1.0310(18) 0.042(5) Uani 1 1 d . . .
C9 C 1.0945(16) 0.7561(14) 1.0068(16) 0.043(5) Uani 1 1 d . . .
H9 H 1.0750 0.7378 1.0640 0.051 Uiso 1 1 calc R . .
C10 C 1.0346(15) 0.6754(15) 0.9016(17) 0.046(5) Uani 1 1 d . . .
H10 H 0.9779 0.6032 0.8901 0.055 Uiso 1 1 calc R . .
C11 C 1.2467(16) 0.9551(16) 1.1438(16) 0.045(4) Uani 1 1 d . . .
H11A H 1.3156 0.9384 1.1913 0.054 Uiso 1 1 calc R . .
H11B H 1.2821 1.0304 1.1375 0.054 Uiso 1 1 calc R . .
C12 C 1.157(2) 0.9364(18) 1.2868(19) 0.063(6) Uani 1 1 d U . .
H12 H 1.2199 0.9201 1.3360 0.076 Uiso 1 1 calc R . .
C13 C 1.054(3) 0.941(2) 1.298(2) 0.084(9) Uani 1 1 d . . .
H13 H 1.0308 0.9306 1.3561 0.101 Uiso 1 1 calc R . .
C14 C 0.988(2) 0.9638(16) 1.2059(17) 0.051(5) Uani 1 1 d . . .
H14 H 0.9100 0.9710 1.1913 0.061 Uiso 1 1 calc R . .
C15 C 0.9498(17) 0.2340(14) 0.5198(19) 0.053(6) Uani 1 1 d . . .
H15 H 1.0252 0.2906 0.5746 0.064 Uiso 1 1 calc R . .
C16 C 0.937(2) 0.1303(18) 0.4514(15) 0.050(5) Uani 1 1 d . . .
H16 H 1.0031 0.1062 0.4494 0.060 Uiso 1 1 calc R . .
C17 C 0.815(2) 0.0699(16) 0.3886(17) 0.050(5) Uani 1 1 d . . .
H17 H 0.7802 -0.0049 0.3374 0.059 Uiso 1 1 calc R . .
C18 C 0.6138(16) 0.1072(14) 0.3667(16) 0.040(4) Uani 1 1 d . . .
H18A H 0.5756 0.0524 0.2913 0.048 Uiso 1 1 calc R . .
H18B H 0.5955 0.1766 0.3631 0.048 Uiso 1 1 calc R . .
C19 C 0.5566(16) 0.0547(15) 0.4377(14) 0.036(4) Uani 1 1 d . . .
C20 C 0.5361(17) 0.1180(14) 0.5192(16) 0.046(5) Uani 1 1 d . . .
H20 H 0.5586 0.1977 0.5341 0.056 Uiso 1 1 calc R . .
C21 C 0.5192(19) -0.0649(15) 0.4177(18) 0.054(6) Uani 1 1 d . . .
H21 H 0.5310 -0.1109 0.3611 0.064 Uiso 1 1 calc R . .
Cu1 Cu 0.7907(3) 0.3706(2) 0.5306(3) 0.0750(10) Uani 1 1 d . . .
Cu2 Cu 1.0000 1.0000 1.0000 0.0390(7) Uani 1 2 d S . .
N1 N 0.7641(15) 0.5083(15) 0.5739(18) 0.066(6) Uani 1 1 d . . .
N2 N 0.8572(15) 0.6071(13) 0.6476(16) 0.056(5) Uani 1 1 d . . .
N3 N 1.1586(14) 0.9587(13) 1.1945(11) 0.044(4) Uani 1 1 d . . .
N4 N 1.0497(14) 0.9749(11) 1.1379(13) 0.039(3) Uani 1 1 d . . .
N5 N 0.8326(14) 0.2395(12) 0.4936(14) 0.043(4) Uani 1 1 d . . .
N6 N 0.7507(13) 0.1367(11) 0.4123(12) 0.037(3) Uani 1 1 d . . .
O1 O 0.7121(12) 0.3467(9) 0.3153(11) 0.047(3) Uani 1 1 d . . .
O2 O 0.4772(14) 0.3414(14) 0.1952(13) 0.078(5) Uani 1 1 d U . .
O3 O 0.5986(13) 0.2682(15) 0.0837(13) 0.078(5) Uani 1 1 d U . .
O4 O 0.2198(12) 0.2030(9) 0.1181(10) 0.042(3) Uani 1 1 d . . .
O5 O 0.3530(13) 0.2004(14) -0.0138(13) 0.076(5) Uani 1 1 d U . .
O6 O 0.4713(12) 0.0649(10) -0.0997(13) 0.055(4) Uani 1 1 d . . .
O7 O 0.4931(17) 0.3910(15) 0.0405(15) 0.019(4) Uani 0.50 1 d PU . .
O8 O 0.6096(11) 0.2774(11) -0.1083(13) 0.054(4) Uani 1 1 d . . .
O9 O 0.7956(15) 0.4764(11) -0.0035(12) 0.066(4) Uani 1 1 d U . .
O10 O 0.1896(16) 0.3089(11) -0.0418(13) 0.070(5) Uani 1 1 d . . .
O11 O 0.3801(17) 0.4700(15) 0.0203(17) 0.027(5) Uani 0.50 1 d PU . .
O12 O 0.4952(14) 0.4045(12) -0.0860(14) 0.008(3) Uani 0.50 1 d PU . .
O13 O 0.3915(17) 0.4631(13) -0.1052(18) 0.021(4) Uani 0.50 1 d PU . .
O14 O 0.3650(12) 0.2044(10) -0.2007(12) 0.052(3) Uani 1 1 d U . .
O15 O 0.7436(12) 0.3582(13) -0.2294(11) 0.058(4) Uani 1 1 d . . .
O16 O 0.6883(15) 0.5545(11) -0.1618(11) 0.062(4) Uani 1 1 d U . .
O17 O 0.4998(11) 0.3512(10) -0.2659(12) 0.050(3) Uani 1 1 d . . .
O18 O 0.1997(14) 0.3118(11) -0.2360(14) 0.062(4) Uani 1 1 d . . .
O19 O 0.0052(11) 0.3658(10) -0.1928(14) 0.063(5) Uani 1 1 d . . .
O20 O 0.2169(14) 0.5266(11) -0.1859(13) 0.059(4) Uani 1 1 d . . .
O21 O 0.3368(14) 0.4542(11) -0.2981(14) 0.065(5) Uani 1 1 d . . .
O22 O 0.2493(14) 0.2154(12) -0.4140(12) 0.068(5) Uani 1 1 d . . .
P1 P 0.5000 0.5000 0.0000 0.0258(13) Uani 1 2 d S . .
W1 W 0.64488(6) 0.39571(6) 0.21548(6) 0.0358(2) Uani 1 1 d . . .
W2 W 0.30872(6) 0.29922(6) 0.08171(6) 0.0393(2) Uani 1 1 d . . .
W3 W 0.48207(6) 0.20516(5) -0.06583(6) 0.0335(2) Uani 1 1 d . . .
W4 W 0.16422(5) 0.40888(5) -0.12901(6) 0.0312(2) Uani 1 1 d . . .
W5 W 0.32995(6) 0.30735(5) -0.28134(5) 0.02554(19) Uani 1 1 d . . .
W6 W 0.66674(6) 0.40437(5) -0.15435(6) 0.0295(2) Uani 1 1 d . . .
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'
Cu Cu 0.3201 1.2651 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 113(2) . . ?
N1 C1 H1 123.3 . . ?
C2 C1 H1 123.3 . . ?
C3 C2 C1 105(2) . . ?
C3 C2 H2 127.5 . . ?
C1 C2 H2 127.5 . . ?
C2 C3 N2 105.6(18) . . ?
C2 C3 H3 127.2 . . ?
N2 C3 H3 127.2 . . ?
N2 C4 C5 109.9(15) . . ?
N2 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
N2 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C10 C5 C6 119.2(19) . . ?
C10 C5 C4 119.5(17) . . ?
C6 C5 C4 121(2) . . ?
C5 C6 C7 117.6(19) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
C8 C7 C6 124.2(16) . . ?
C8 C7 H7 117.9 . . ?
C6 C7 H7 117.9 . . ?
C9 C8 C7 114.7(17) . . ?
C9 C8 C11 122.9(17) . . ?
C7 C8 C11 122.4(15) . . ?
C10 C9 C8 122.1(18) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C5 122.1(16) . . ?
C9 C10 H10 118.9 . . ?
C5 C10 H10 118.9 . . ?
N3 C11 C8 111.3(13) . . ?
N3 C11 H11A 109.4 . . ?
C8 C11 H11A 109.4 . . ?
N3 C11 H11B 109.4 . . ?
C8 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 N3 110(2) . . ?
C13 C12 H12 124.8 . . ?
N3 C12 H12 124.8 . . ?
C12 C13 C14 105(2) . . ?
C12 C13 H13 127.7 . . ?
C14 C13 H13 127.7 . . ?
N4 C14 C13 113(2) . . ?
N4 C14 H14 123.6 . . ?
C13 C14 H14 123.6 . . ?
N5 C15 C16 108.0(16) . . ?
N5 C15 H15 126.0 . . ?
C16 C15 H15 126.0 . . ?
C17 C16 C15 108.7(18) . . ?
C17 C16 H16 125.7 . . ?
C15 C16 H16 125.7 . . ?
C16 C17 N6 107.5(17) . . ?
C16 C17 H17 126.2 . . ?
N6 C17 H17 126.2 . . ?
N6 C18 C19 111.4(16) . . ?
N6 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
N6 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C21 117.2(17) . . ?
C20 C19 C18 122.8(16) . . ?
C21 C19 C18 120.0(15) . . ?
C19 C20 C21 120.8(16) . 2_656 ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 2_656 . ?
C19 C21 C20 122.0(14) . 2_656 ?
C19 C21 H21 119.0 . . ?
C20 C21 H21 119.0 2_656 . ?
N1 Cu1 N5 175.0(7) . . ?
N1 Cu1 O1 95.8(8) . . ?
N5 Cu1 O1 85.9(6) . . ?
N4 Cu2 N4 180.000(5) . 2_777 ?
C1 N1 N2 104.8(18) . . ?
C1 N1 Cu1 132.1(16) . . ?
N2 N1 Cu1 122.8(13) . . ?
N1 N2 C3 111.1(17) . . ?
N1 N2 C4 119.0(14) . . ?
C3 N2 C4 129.9(17) . . ?
C12 N3 N4 110.5(17) . . ?
C12 N3 C11 130.1(19) . . ?
N4 N3 C11 119.0(14) . . ?
C14 N4 N3 101.8(17) . . ?
C14 N4 Cu2 130.2(15) . . ?
N3 N4 Cu2 127.9(11) . . ?
C15 N5 N6 105.8(12) . . ?
C15 N5 Cu1 128.2(11) . . ?
N6 N5 Cu1 124.4(11) . . ?
C17 N6 N5 109.9(15) . . ?
C17 N6 C18 128.0(15) . . ?
N5 N6 C18 122.0(13) . . ?
W1 O1 Cu1 146.4(6) . . ?
W1 O2 W2 140.3(10) . . ?
W3 O3 W1 139.1(10) . . ?
W3 O5 W2 140.2(9) . . ?
P1 O7 O12 51.5(8) . . ?
P1 O7 O13 50.1(9) . 2_665 ?
O12 O7 O13 86.1(12) . 2_665 ?
P1 O7 W3 125.4(9) . . ?
O12 O7 W3 73.9(7) . . ?
O13 O7 W3 136.1(10) 2_665 . ?
P1 O7 W1 123.9(9) . . ?
O12 O7 W1 136.4(10) . . ?
O13 O7 W1 73.8(9) 2_665 . ?
W3 O7 W1 94.1(6) . . ?
P1 O7 W2 119.6(9) . . ?
O12 O7 W2 129.2(11) . . ?
O13 O7 W2 129.0(9) 2_665 . ?
W3 O7 W2 92.8(6) . . ?
W1 O7 W2 92.4(6) . . ?
W6 O8 W3 142.1(7) . . ?
W4 O9 W6 140.0(9) 2_665 . ?
W2 O10 W4 141.7(8) . . ?
P1 O11 O12 54.0(7) . 2_665 ?
P1 O11 O13 52.6(8) . . ?
O12 O11 O13 91.2(12) 2_665 . ?
P1 O11 W6 126.5(10) . 2_665 ?
O12 O11 W6 72.5(7) 2_665 2_665 ?
O13 O11 W6 137.5(13) . 2_665 ?
P1 O11 W4 123.6(12) . . ?
O12 O11 W4 134.2(13) 2_665 . ?
O13 O11 W4 71.1(10) . . ?
W6 O11 W4 92.2(6) 2_665 . ?
P1 O11 W2 122.0(11) . . ?
O12 O11 W2 131.6(13) 2_665 . ?
O13 O11 W2 125.8(10) . . ?
W6 O11 W2 92.0(6) 2_665 . ?
W4 O11 W2 90.7(6) . . ?
P1 O12 O13 56.4(9) . . ?
P1 O12 O11 57.5(7) . 2_665 ?
O13 O12 O11 95.3(12) . 2_665 ?
P1 O12 O7 58.2(8) . . ?
O13 O12 O7 93.4(12) . . ?
O11 O12 O7 92.2(12) 2_665 . ?
P1 O12 W5 126.9(9) . . ?
O13 O12 W5 70.5(9) . . ?
O11 O12 W5 134.2(12) 2_665 . ?
O7 O12 W5 130.8(9) . . ?
P1 O12 W6 125.7(8) . . ?
O13 O12 W6 134.3(11) . . ?
O11 O12 W6 68.1(7) 2_665 . ?
O7 O12 W6 128.0(10) . . ?
W5 O12 W6 90.6(5) . . ?
P1 O13 O12 57.0(9) . . ?
P1 O13 O11 56.6(10) . . ?
O12 O13 O11 95.8(15) . . ?
P1 O13 O7 57.0(9) . 2_665 ?
O12 O13 O7 94.0(12) . 2_665 ?
O11 O13 O7 89.0(12) . 2_665 ?
P1 O13 W5 129.1(9) . . ?
O12 O13 W5 72.0(8) . . ?
O11 O13 W5 135.9(11) . . ?
O7 O13 W5 133.0(11) 2_665 . ?
P1 O13 W4 125.3(11) . . ?
O12 O13 W4 137.1(11) . . ?
O11 O13 W4 68.8(8) . . ?
O7 O13 W4 124.2(9) 2_665 . ?
W5 O13 W4 91.3(6) . . ?
W3 O14 W5 140.4(7) . . ?
W6 O16 W2 140.8(8) . 2_665 ?
W6 O17 W5 140.4(8) . . ?
W5 O18 W4 140.9(8) . . ?
W4 O20 W1 141.4(8) . 2_665 ?
W1 O21 W5 140.5(9) 2_665 . ?
O13 P1 O13 180.0(13) . 2_665 ?
O13 P1 O12 113.4(9) . 2_665 ?
O13 P1 O12 66.6(9) 2_665 2_665 ?
O13 P1 O12 66.6(9) . . ?
O13 P1 O12 113.4(9) 2_665 . ?
O12 P1 O12 180.000(2) 2_665 . ?
O13 P1 O11 70.9(11) . . ?
O13 P1 O11 109.1(11) 2_665 . ?
O12 P1 O11 68.5(8) 2_665 . ?
O12 P1 O11 111.5(8) . . ?
O13 P1 O11 109.1(11) . 2_665 ?
O13 P1 O11 70.9(11) 2_665 2_665 ?
O12 P1 O11 111.5(8) 2_665 2_665 ?
O12 P1 O11 68.5(8) . 2_665 ?
O11 P1 O11 180.0(12) . 2_665 ?
O13 P1 O7 107.1(9) . . ?
O13 P1 O7 72.9(9) 2_665 . ?
O12 P1 O7 109.7(9) 2_665 . ?
O12 P1 O7 70.3(9) . . ?
O11 P1 O7 74.5(10) . . ?
O11 P1 O7 105.5(10) 2_665 . ?
O13 P1 O7 72.9(9) . 2_665 ?
O13 P1 O7 107.1(9) 2_665 2_665 ?
O12 P1 O7 70.3(9) 2_665 2_665 ?
O12 P1 O7 109.7(9) . 2_665 ?
O11 P1 O7 105.5(10) . 2_665 ?
O11 P1 O7 74.5(10) 2_665 2_665 ?
O7 P1 O7 180.0(5) . 2_665 ?
O1 W1 O2 101.8(7) . . ?
O1 W1 O21 102.5(6) . 2_665 ?
O2 W1 O21 89.3(6) . 2_665 ?
O1 W1 O20 102.9(6) . 2_665 ?
O2 W1 O20 155.3(8) . 2_665 ?
O21 W1 O20 86.1(5) 2_665 2_665 ?
O1 W1 O3 101.2(7) . . ?
O2 W1 O3 87.4(6) . . ?
O21 W1 O3 156.3(8) 2_665 . ?
O20 W1 O3 87.1(6) 2_665 . ?
O1 W1 O7 158.2(6) . . ?
O2 W1 O7 64.8(7) . . ?
O21 W1 O7 94.7(6) 2_665 . ?
O20 W1 O7 91.4(7) 2_665 . ?
O3 W1 O7 62.7(7) . . ?
O4 W2 O10 102.3(7) . . ?
O4 W2 O5 100.9(6) . . ?
O10 W2 O5 90.2(7) . . ?
O4 W2 O16 104.0(6) . 2_665 ?
O10 W2 O16 85.8(6) . 2_665 ?
O5 W2 O16 155.1(7) . 2_665 ?
O4 W2 O2 102.7(7) . . ?
O10 W2 O2 154.9(7) . . ?
O5 W2 O2 86.9(6) . . ?
O16 W2 O2 86.5(6) 2_665 . ?
O4 W2 O7 156.4(6) . . ?
O10 W2 O7 94.5(7) . . ?
O5 W2 O7 62.3(6) . . ?
O16 W2 O7 93.6(6) 2_665 . ?
O2 W2 O7 62.2(7) . . ?
O4 W2 O11 159.7(6) . . ?
O10 W2 O11 63.6(7) . . ?
O5 W2 O11 94.0(7) . . ?
O16 W2 O11 62.3(6) 2_665 . ?
O2 W2 O11 91.7(7) . . ?
O7 W2 O11 43.9(6) . . ?
O6 W3 O3 102.5(8) . . ?
O6 W3 O14 101.2(6) . . ?
O3 W3 O14 156.2(7) . . ?
O6 W3 O8 103.1(6) . . ?
O3 W3 O8 89.7(6) . . ?
O14 W3 O8 86.5(6) . . ?
O6 W3 O5 102.4(7) . . ?
O3 W3 O5 87.7(6) . . ?
O14 W3 O5 85.7(7) . . ?
O8 W3 O5 154.2(7) . . ?
O6 W3 O7 159.7(7) . . ?
O3 W3 O7 63.5(7) . . ?
O14 W3 O7 93.2(6) . . ?
O8 W3 O7 91.8(6) . . ?
O5 W3 O7 64.2(6) . . ?
O19 W4 O9 102.8(7) . 2_665 ?
O19 W4 O20 101.6(8) . . ?
O9 W4 O20 88.4(6) 2_665 . ?
O19 W4 O10 103.7(8) . . ?
O9 W4 O10 87.0(6) 2_665 . ?
O20 W4 O10 154.7(7) . . ?
O19 W4 O18 101.8(6) . . ?
O9 W4 O18 155.5(7) 2_665 . ?
O20 W4 O18 86.2(5) . . ?
O10 W4 O18 87.7(6) . . ?
O19 W4 O11 160.4(7) . . ?
O9 W4 O11 63.3(6) 2_665 . ?
O20 W4 O11 92.1(7) . . ?
O10 W4 O11 63.7(7) . . ?
O18 W4 O11 92.9(6) . . ?
O19 W4 O13 159.4(7) . . ?
O9 W4 O13 93.4(6) 2_665 . ?
O20 W4 O13 65.8(6) . . ?
O10 W4 O13 89.6(7) . . ?
O18 W4 O13 62.6(6) . . ?
O11 W4 O13 40.2(6) . . ?
O22 W5 O18 102.1(7) . . ?
O22 W5 O17 102.4(6) . . ?
O18 W5 O17 155.4(6) . . ?
O22 W5 O21 102.8(8) . . ?
O18 W5 O21 86.1(5) . . ?
O17 W5 O21 86.6(5) . . ?
O22 W5 O14 101.8(7) . . ?
O18 W5 O14 89.9(6) . . ?
O17 W5 O14 87.1(5) . . ?
O21 W5 O14 155.4(7) . . ?
O22 W5 O13 161.8(8) . . ?
O18 W5 O13 64.4(6) . . ?
O17 W5 O13 91.3(6) . . ?
O21 W5 O13 65.7(7) . . ?
O14 W5 O13 90.7(6) . . ?
O22 W5 O12 160.7(7) . . ?
O18 W5 O12 92.4(6) . . ?
O17 W5 O12 64.3(5) . . ?
O21 W5 O12 90.7(6) . . ?
O14 W5 O12 65.2(5) . . ?
O13 W5 O12 37.4(6) . . ?
O15 W6 O16 102.5(7) . . ?
O15 W6 O8 103.0(7) . . ?
O16 W6 O8 154.6(6) . . ?
O15 W6 O17 101.6(6) . . ?
O16 W6 O17 88.9(6) . . ?
O8 W6 O17 86.8(5) . . ?
O15 W6 O9 103.8(7) . . ?
O16 W6 O9 87.5(6) . . ?
O8 W6 O9 85.7(6) . . ?
O17 W6 O9 154.5(7) . . ?
O15 W6 O11 160.6(6) . 2_665 ?
O16 W6 O11 64.2(7) . 2_665 ?
O8 W6 O11 91.0(6) . 2_665 ?
O17 W6 O11 92.5(6) . 2_665 ?
O9 W6 O11 63.4(7) . 2_665 ?
O15 W6 O12 160.0(6) . . ?
O16 W6 O12 91.2(6) . . ?
O8 W6 O12 64.6(5) . . ?
O17 W6 O12 63.7(6) . . ?
O9 W6 O12 91.2(6) . . ?
O11 W6 O12 39.3(5) 2_665 . ?
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 1.28(3) . ?
C1 C2 1.37(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.35(3) . ?
C2 H2 0.9300 . ?
C3 N2 1.37(2) . ?
C3 H3 0.9300 . ?
C4 N2 1.46(3) . ?
C4 C5 1.49(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C10 1.38(3) . ?
C5 C6 1.39(2) . ?
C6 C7 1.41(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.41(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.40(2) . ?
C8 C11 1.49(2) . ?
C9 C10 1.37(2) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 N3 1.44(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.31(3) . ?
C12 N3 1.33(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.37(4) . ?
C13 H13 0.9300 . ?
C14 N4 1.36(2) . ?
C14 H14 0.9300 . ?
C15 N5 1.36(2) . ?
C15 C16 1.37(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.33(3) . ?
C16 H16 0.9300 . ?
C17 N6 1.35(2) . ?
C17 H17 0.9300 . ?
C18 N6 1.46(2) . ?
C18 C19 1.51(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.35(2) . ?
C19 C21 1.40(2) . ?
C20 C21 1.41(3) 2_656 ?
C20 H20 0.9300 . ?
C21 C20 1.41(3) 2_656 ?
C21 H21 0.9300 . ?
Cu1 N1 1.864(17) . ?
Cu1 N5 1.876(14) . ?
Cu1 O1 2.647(14) . ?
Cu2 N4 1.873(16) . ?
Cu2 N4 1.873(16) 2_777 ?
N1 N2 1.34(2) . ?
N3 N4 1.37(2) . ?
N5 N6 1.362(18) . ?
O1 W1 1.657(15) . ?
O2 W1 1.853(14) . ?
O2 W2 1.935(17) . ?
O3 W3 1.868(16) . ?
O3 W1 1.923(13) . ?
O4 W2 1.665(10) . ?
O5 W3 1.894(12) . ?
O5 W2 1.903(12) . ?
O6 W3 1.695(12) . ?
O7 P1 1.581(19) . ?
O7 O12 1.75(2) . ?
O7 O13 1.80(2) 2_665 ?
O7 W3 2.423(16) . ?
O7 W1 2.43(2) . ?
O7 W2 2.507(17) . ?
O8 W6 1.886(13) . ?
O8 W3 1.889(13) . ?
O9 W4 1.862(14) 2_665 ?
O9 W6 1.928(15) . ?
O10 W2 1.852(17) . ?
O10 W4 1.917(16) . ?
O11 P1 1.519(16) . ?
O11 O12 1.68(2) 2_665 ?
O11 O13 1.72(3) . ?
O11 W6 2.453(16) 2_665 ?
O11 W4 2.49(2) . ?
O11 W2 2.52(2) . ?
O12 P1 1.457(14) . ?
O12 O13 1.59(2) . ?
O12 O11 1.68(2) 2_665 ?
O12 W5 2.493(16) . ?
O12 W6 2.521(14) . ?
O13 P1 1.45(2) . ?
O13 O7 1.80(2) 2_665 ?
O13 W5 2.471(17) . ?
O13 W4 2.524(17) . ?
O14 W3 1.888(14) . ?
O14 W5 1.910(13) . ?
O15 W6 1.693(10) . ?
O16 W6 1.878(14) . ?
O16 W2 1.919(13) 2_665 ?
O17 W6 1.894(13) . ?
O17 W5 1.895(12) . ?
O18 W5 1.868(10) . ?
O18 W4 1.921(11) . ?
O19 W4 1.688(12) . ?
O20 W4 1.874(13) . ?
O20 W1 1.903(12) 2_665 ?
O21 W1 1.899(13) 2_665 ?
O21 W5 1.905(13) . ?
O22 W5 1.685(13) . ?
P1 O13 1.45(2) 2_665 ?
P1 O12 1.457(14) 2_665 ?
P1 O11 1.519(16) 2_665 ?
P1 O7 1.581(19) 2_665 ?
W1 O21 1.899(13) 2_665 ?
W1 O20 1.903(12) 2_665 ?
W2 O16 1.919(13) 2_665 ?
W4 O9 1.862(14) 2_665 ?
W6 O11 2.453(16) 2_665 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11B O4 0.97 2.53 3.32(2) 138.6 1_666
C17 H17 O14 0.93 2.52 3.43(2) 165.6 2_655
C18 H18A O6 0.97 2.47 3.42(2) 166.2 2_655
C18 H18B O1 0.97 2.57 3.26(2) 128.0 .
C9 H9 O19 0.93 2.65 3.56(2) 166.3 2_666
C15 H15 O18 0.93 2.61 3.36(3) 137.6 1_656
C16 H16 O22 0.93 2.68 3.32(3) 127.0 1_656
