#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:59:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179434 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/31/4333184.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4333184
loop_
_publ_author_name
'Kong, Xiang-Jian'
'Ren, Yan-Ping'
'Zheng, Pei-Qing'
'Long, Yu-Xiang'
'Long, La-Sheng'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
_publ_section_title
;
 Construction of Polyoxometalates-Based Coordination Polymers through
 Direct Incorporation between Polyoxometalates and the Voids in a 2D
 Network
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10702
_journal_page_last               10711
_journal_paper_doi               10.1021/ic061664y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C42 H56 Cu4 N14 O40 Si W12'
_chemical_formula_weight         3885.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.319(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.385(3)
_cell_length_b                   18.976(4)
_cell_length_c                   12.221(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3673.9(12)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13640
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    19.943
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.404
_refine_diff_density_min         -3.156
_refine_diff_density_rms         0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.008
_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+621.1714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                3346
_reflns_number_total             3520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061664ysup1.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3673.7(12)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4333184
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
W1 W 0.44319(6) 0.59196(5) 0.20233(8) 0.0361(3) Uani 1 1 d .
W2 W 0.70959(7) 0.5000 0.03452(10) 0.0249(3) Uani 1 2 d S
W3 W 0.5000 0.68513(6) 0.0000 0.0446(4) Uani 1 2 d S
W4 W 0.65263(5) 0.59152(5) 0.23670(8) 0.0361(3) Uani 1 1 d .
Si1 Si 0.5000 0.5000 0.0000 0.041(3) Uani 1 4 d S
O1 O 0.598(2) 0.5000 0.093(3) 0.022(4) Uani 0.50 2 d SP
O2 O 0.5189(15) 0.5686(13) 0.087(2) 0.022(4) Uani 0.50 1 d P
O3 O 0.564(2) 0.5000 -0.064(3) 0.022(4) Uani 0.50 2 d SP
O5 O 0.673(2) 0.5000 0.302(2) 0.064(8) Uani 1 2 d S
O6 O 0.5000 0.7741(11) 0.0000 0.059(8) Uani 1 2 d S
O7 O 0.6035(12) 0.6649(15) 0.128(2) 0.103(10) Uani 1 1 d .
O8 O 0.4463(12) 0.6669(15) 0.103(2) 0.105(11) Uani 1 1 d .
O9 O 0.3378(15) 0.5673(9) 0.0813(16) 0.075(7) Uani 1 1 d .
O10 O 0.7145(15) 0.5684(9) 0.1475(16) 0.065(6) Uani 1 1 d .
O11 O 0.8128(15) 0.5000 0.054(3) 0.053(7) Uani 1 2 d S
O12 O 0.7265(12) 0.6333(10) 0.3542(17) 0.059(5) Uani 1 1 d .
O13 O 0.4151(10) 0.6392(9) 0.2968(14) 0.048(4) Uani 1 1 d .
O14 O 0.445(2) 0.5000 0.259(2) 0.081(10) Uani 1 2 d S
O15 O 0.5616(12) 0.5985(15) 0.280(2) 0.103(10) Uani 1 1 d .
Cu1 Cu 0.2421(3) 0.8232(2) -0.2545(3) 0.0612(10) Uani 1 1 d .
N1 N 0.2456(13) 0.7824(9) -0.4034(15) 0.039(5) Uani 1 1 d .
C1 C 0.3180(13) 0.7745(11) -0.4107(18) 0.031(4) Uani 1 1 d .
C2 C 0.3233(16) 0.7426(12) -0.508(2) 0.041(5) Uani 1 1 d .
H2A H 0.3766 0.7382 -0.5118 0.050 Uiso 1 1 calc R
C3 C 0.401(2) 0.7969(19) -0.317(3) 0.081(10) Uani 1 1 d .
H3A H 0.3920 0.8191 -0.2506 0.122 Uiso 1 1 calc R
H3B H 0.4270 0.8308 -0.3515 0.122 Uiso 1 1 calc R
H3C H 0.4373 0.7557 -0.2874 0.122 Uiso 1 1 calc R
N2 N 0.2462(11) 0.7791(10) -0.1053(16) 0.037(4) Uani 1 1 d .
C4 C 0.2988(15) 0.8017(12) 0.001(2) 0.042(5) Uani 1 1 d .
H4A H 0.3370 0.8383 0.0043 0.050 Uiso 1 1 calc R
C5 C 0.3019(14) 0.7754(14) 0.108(2) 0.044(6) Uani 1 1 d .
C6 C 0.3587(19) 0.8055(14) 0.219(2) 0.058(8) Uani 1 1 d .
H6A H 0.3879 0.8457 0.2031 0.088 Uiso 1 1 calc R
H6B H 0.4001 0.7700 0.2658 0.088 Uiso 1 1 calc R
H6C H 0.3268 0.8215 0.2646 0.088 Uiso 1 1 calc R
N3 N 0.2628(15) 0.9288(12) -0.2707(17) 0.052(6) Uani 1 1 d .
C7 C 0.2028(16) 0.9655(16) -0.359(2) 0.054(7) Uani 1 1 d .
C8 C 0.3224(17) 0.9626(14) -0.191(2) 0.052(7) Uani 1 1 d .
H8A H 0.3675 0.9377 -0.1312 0.063 Uiso 1 1 calc R
C9 C 0.134(4) 0.938(3) -0.461(5) 0.17(3) Uani 1 1 d .
H9A H 0.1020 0.9771 -0.5120 0.256 Uiso 1 1 calc R
H9B H 0.0973 0.9103 -0.4352 0.256 Uiso 1 1 calc R
H9C H 0.1560 0.9080 -0.5072 0.256 Uiso 1 1 calc R
N4 N 0.923(5) 0.5000 0.404(6) 0.23(5) Uani 1 2 d S
C10 C 0.847(4) 0.5000 0.538(4) 0.19(5) Uani 1 2 d S
H10A H 0.8610 0.5000 0.6244 0.283 Uiso 1 2 calc SR
H10B H 0.8136 0.4578 0.5013 0.283 Uiso 0.50 1 calc PR
H10C H 0.8136 0.5422 0.5013 0.283 Uiso 0.50 1 calc PR
C11 C 0.929(5) 0.5000 0.518(5) 0.12(3) Uani 1 2 d S
C12 C 1.001(3) 0.5000 0.400(5) 0.20(6) Uani 1 2 d S
H12A H 0.9999 0.5000 0.3214 0.241 Uiso 1 2 calc SR
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'
Si Si 0.0817 0.0704 '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'
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
O13 W1 O14 102.0(12) . .
O13 W1 O9 102.0(9) . .
O14 W1 O9 85.7(10) . .
O13 W1 O15 100.7(11) . .
O14 W1 O15 91.3(13) . .
O9 W1 O15 157.2(12) . .
O13 W1 O8 97.6(11) . .
O14 W1 O8 160.2(14) . .
O9 W1 O8 87.6(10) . .
O15 W1 O8 87.6(9) . .
O13 W1 O2 155.4(9) . .
O14 W1 O2 96.7(13) . .
O9 W1 O2 95.0(10) . .
O15 W1 O2 62.8(10) . .
O8 W1 O2 65.3(10) . .
O13 W1 O3 157.8(10) . 5_665
O14 W1 O3 64.7(11) . 5_665
O9 W1 O3 60.9(11) . 5_665
O15 W1 O3 97.4(13) . 5_665
O8 W1 O3 95.8(12) . 5_665
O2 W1 O3 46.6(9) . 5_665
O11 W2 O9 102.6(11) . 5_665
O11 W2 O9 102.6(11) . 2_655
O9 W2 O9 88.5(11) 5_665 2_655
O11 W2 O10 99.9(10) . .
O9 W2 O10 157.4(11) 5_665 .
O9 W2 O10 87.5(8) 2_655 .
O11 W2 O10 99.9(10) . 6_565
O9 W2 O10 87.5(8) 5_665 6_565
O9 W2 O10 157.4(11) 2_655 6_565
O10 W2 O10 87.8(11) . 6_565
O11 W2 O3 158.9(13) . .
O9 W2 O3 63.3(9) 5_665 .
O9 W2 O3 63.3(9) 2_655 .
O10 W2 O3 95.2(10) . .
O10 W2 O3 95.2(10) 6_565 .
O11 W2 O1 156.7(13) . .
O9 W2 O1 94.0(10) 5_665 .
O9 W2 O1 94.0(10) 2_655 .
O10 W2 O1 64.2(9) . .
O10 W2 O1 64.2(9) 6_565 .
O3 W2 O1 44.4(12) . .
O6 W3 O7 101.8(9) . 2_655
O6 W3 O7 101.8(9) . .
O7 W3 O7 156.4(19) 2_655 .
O6 W3 O8 100.6(9) . .
O7 W3 O8 87.3(11) 2_655 .
O7 W3 O8 88.4(9) . .
O6 W3 O8 100.6(9) . 2_655
O7 W3 O8 88.4(9) 2_655 2_655
O7 W3 O8 87.3(11) . 2_655
O8 W3 O8 158.9(18) . 2_655
O6 W3 O2 156.1(6) . 2_655
O7 W3 O2 62.3(10) 2_655 2_655
O7 W3 O2 95.3(11) . 2_655
O8 W3 O2 96.5(11) . 2_655
O8 W3 O2 63.3(10) 2_655 2_655
O6 W3 O2 156.1(6) . .
O7 W3 O2 95.3(11) 2_655 .
O7 W3 O2 62.3(10) . .
O8 W3 O2 63.3(10) . .
O8 W3 O2 96.5(11) 2_655 .
O2 W3 O2 47.8(12) 2_655 .
O12 W4 O15 99.4(12) . .
O12 W4 O7 102.7(12) . .
O15 W4 O7 87.4(9) . .
O12 W4 O10 100.8(9) . .
O15 W4 O10 159.8(12) . .
O7 W4 O10 88.1(9) . .
O12 W4 O5 97.5(11) . .
O15 W4 O5 89.0(11) . .
O7 W4 O5 159.8(13) . .
O10 W4 O5 88.5(9) . .
O12 W4 O2 157.3(9) . .
O15 W4 O2 63.0(11) . .
O7 W4 O2 64.3(11) . .
O10 W4 O2 97.3(9) . .
O5 W4 O2 96.5(11) . .
O12 W4 O1 155.5(10) . .
O15 W4 O1 97.9(13) . .
O7 W4 O1 95.3(12) . .
O10 W4 O1 62.9(10) . .
O5 W4 O1 65.5(10) . .
O2 W4 O1 47.1(10) . .
O3 Si1 O3 180.000(3) 5_665 .
O3 Si1 O1 66.1(18) 5_665 5_665
O3 Si1 O1 113.9(18) . 5_665
O3 Si1 O1 113.9(18) 5_665 .
O3 Si1 O1 66.1(18) . .
O1 Si1 O1 180.000(5) 5_665 .
O3 Si1 O2 109.1(11) 5_665 5_665
O3 Si1 O2 70.9(11) . 5_665
O1 Si1 O2 70.8(11) 5_665 5_665
O1 Si1 O2 109.2(11) . 5_665
O3 Si1 O2 70.9(11) 5_665 .
O3 Si1 O2 109.1(11) . .
O1 Si1 O2 109.2(11) 5_665 .
O1 Si1 O2 70.8(11) . .
O2 Si1 O2 180.0(19) 5_665 .
O3 Si1 O2 109.1(11) 5_665 2_655
O3 Si1 O2 70.9(11) . 2_655
O1 Si1 O2 70.8(11) 5_665 2_655
O1 Si1 O2 109.2(11) . 2_655
O2 Si1 O2 106.0(17) 5_665 2_655
O2 Si1 O2 74.0(17) . 2_655
O3 Si1 O2 70.9(11) 5_665 6_565
O3 Si1 O2 109.1(11) . 6_565
O1 Si1 O2 109.2(11) 5_665 6_565
O1 Si1 O2 70.8(11) . 6_565
O2 Si1 O2 74.0(17) 5_665 6_565
O2 Si1 O2 106.0(17) . 6_565
O2 Si1 O2 180.0(10) 2_655 6_565
Si1 O1 O3 56.4(16) . .
Si1 O1 W2 124.2(19) . .
O3 O1 W2 67.7(16) . .
Si1 O1 W4 120.1(11) . .
O3 O1 W4 131.5(8) . .
W2 O1 W4 95.8(10) . .
Si1 O1 W4 120.1(11) . 6_565
O3 O1 W4 131.5(8) . 6_565
W2 O1 W4 95.8(10) . 6_565
W4 O1 W4 94.0(13) . 6_565
Si1 O2 W1 122.4(13) . .
Si1 O2 W4 122.0(13) . .
W1 O2 W4 97.0(9) . .
Si1 O2 W3 119.1(13) . .
W1 O2 W3 94.8(9) . .
W4 O2 W3 94.9(9) . .
Si1 O3 O1 57.5(16) . .
Si1 O3 W2 125.3(19) . .
O1 O3 W2 67.8(16) . .
Si1 O3 W1 120.1(11) . 5_665
O1 O3 W1 131.6(8) . 5_665
W2 O3 W1 95.3(10) . 5_665
Si1 O3 W1 120.1(11) . 2_655
O1 O3 W1 131.6(8) . 2_655
W2 O3 W1 95.3(10) . 2_655
W1 O3 W1 93.3(12) 5_665 2_655
W4 O5 W4 134.8(16) 6_565 .
W4 O7 W3 138.2(16) . .
W3 O8 W1 136.3(14) . .
W2 O9 W1 139.9(14) 5_665 .
W2 O10 W4 136.8(12) . .
W1 O14 W1 137.3(18) 6_565 .
W4 O15 W1 137.0(16) . .
N2 Cu1 N1 132.1(7) . .
N2 Cu1 N3 123.9(7) . .
N1 Cu1 N3 102.5(7) . .
C1 N1 C2 118.2(18) . 7_564
C1 N1 Cu1 119.8(16) . .
C2 N1 Cu1 121.7(17) 7_564 .
N1 C1 C2 121(2) . .
N1 C1 C3 125(2) . .
C2 C1 C3 114(2) . .
N1 C2 C1 120(2) 7_564 .
C4 N2 C5 117(2) . 7_565
C4 N2 Cu1 121.2(18) . .
C5 N2 Cu1 121.7(16) 7_565 .
N2 C4 C5 124(2) . .
N2 C5 C4 119(2) 7_565 .
N2 C5 C6 121(2) 7_565 .
C4 C5 C6 120(2) . .
C8 N3 C7 118(2) . .
C8 N3 Cu1 123(2) . .
C7 N3 Cu1 118.1(16) . .
C7 C7 N3 121.1(14) 6_575 .
C7 C7 C9 111(3) 6_575 .
N3 C7 C9 127(4) . .
N3 C8 C8 120.5(17) . 6_575
C11 N4 C12 112(7) . .
C12 C11 N4 119(7) 5_766 .
C12 C11 C10 123(5) 5_766 .
N4 C11 C10 119(6) . .
C11 C12 N4 129(6) 5_766 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O13 1.684(15) .
W1 O14 1.874(11) .
W1 O9 1.879(19) .
W1 O15 1.88(2) .
W1 O8 1.88(2) .
W1 O2 2.33(2) .
W1 O3 2.40(2) 5_665
W2 O11 1.71(2) .
W2 O9 1.831(16) 5_665
W2 O9 1.831(16) 2_655
W2 O10 1.871(15) .
W2 O10 1.871(15) 6_565
W2 O3 2.32(3) .
W2 O1 2.32(3) .
W3 O6 1.69(2) .
W3 O7 1.88(2) 2_655
W3 O7 1.88(2) .
W3 O8 1.88(2) .
W3 O8 1.88(2) 2_655
W3 O2 2.42(2) 2_655
W3 O2 2.42(2) .
W4 O12 1.680(17) .
W4 O15 1.87(2) .
W4 O7 1.87(2) .
W4 O10 1.872(18) .
W4 O5 1.881(11) .
W4 O2 2.33(2) .
W4 O1 2.37(2) .
Si1 O3 1.60(3) 5_665
Si1 O3 1.60(3) .
Si1 O1 1.62(3) 5_665
Si1 O1 1.62(3) .
Si1 O2 1.63(2) 5_665
Si1 O2 1.63(2) .
Si1 O2 1.63(2) 2_655
Si1 O2 1.63(2) 6_565
O1 O3 1.75(5) .
O1 W4 2.37(2) 6_565
O3 W1 2.40(2) 5_665
O3 W1 2.40(2) 2_655
O5 W4 1.881(11) 6_565
O9 W2 1.831(16) 5_665
O14 W1 1.874(11) 6_565
Cu1 N2 1.98(2) .
Cu1 N1 2.001(17) .
Cu1 N3 2.06(2) .
N1 C1 1.31(3) .
N1 C2 1.33(3) 7_564
C1 C2 1.37(3) .
C1 C3 1.48(4) .
C2 N1 1.33(3) 7_564
N2 C4 1.31(3) .
N2 C5 1.32(3) 7_565
C4 C5 1.38(3) .
C5 N2 1.32(3) 7_565
C5 C6 1.43(4) .
N3 C8 1.26(3) .
N3 C7 1.34(4) .
C7 C7 1.31(6) 6_575
C7 C9 1.43(6) .
C8 C8 1.42(5) 6_575
N4 C11 1.35(7) .
N4 C12 1.37(8) .
C10 C11 1.55(8) .
C11 C12 1.22(7) 5_766
C12 C11 1.22(7) 5_766
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
C10 H10B O5 0.98 2.77 3.21(6) 107.9
