#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:47:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179424 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/21/4332133.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_4332133
loop_
_publ_author_name
'Ren, Yan-Ping'
'Kong, Xiang-Jian'
'Hu, Xiang-Yang'
'Sun, Meng'
'Long, La-Sheng'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
_publ_section_title
;
 Influence of Steric Hindrance of Organic Ligand on the Structure of
 Keggin-Based Coordination Polymer
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4016
_journal_page_last               4023
_journal_paper_doi               10.1021/ic060004q
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C12 H12 Cu3 N6 O40 P W12'
_chemical_formula_weight         3308.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.4070(14)
_cell_length_b                   18.4070(14)
_cell_length_c                   22.544(3)
_cell_measurement_temperature    123(2)
_cell_volume                     6615.0(11)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24083
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    32.718
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.983
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.997
_refine_diff_density_min         -3.279
_refine_diff_density_rms         0.528
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0440P)²+2032.1438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                1757
_reflns_number_total             1781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060004qsup1.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        6614.9(11)
_cod_original_sg_symbol_H-M      r-3c
_cod_database_code               4332133
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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 0.11773(4) 0.51317(4) -0.33576(3) 0.01103(19) Uani 1 1 d .
W2 W 0.20891(4) 0.63056(4) -0.20675(3) 0.0166(2) Uani 1 1 d .
P1 P 0.3333 0.6667 -0.3333 0.0109(18) Uani 1 6 d S
O1 O 0.3333 0.6667 -0.2639(15) 0.005(3) Uani 0.50 3 d SP
O2 O 0.2685(13) 0.5795(13) -0.3541(9) 0.005(3) Uani 0.50 1 d P
O5 O 0.3094(13) 0.7340(13) -0.1863(10) 0.058(5) Uani 1 1 d U
O6 O 0.0165(9) 0.4401(10) -0.3370(8) 0.042(4) Uani 1 1 d .
O7 O 0.1383(11) 0.5422(10) -0.2534(7) 0.034(3) Uani 1 1 d U
O8 O 0.1460(10) 0.5123(11) -0.4142(7) 0.036(4) Uani 1 1 d U
O9 O 0.1514(10) 0.6149(9) -0.1466(6) 0.028(3) Uani 1 1 d .
O10 O 0.1132(15) 0.6117(10) -0.3466(8) 0.052(6) Uani 1 1 d .
Cu1 Cu 0.08081(19) 0.6667 -0.0833 0.0196(6) Uani 1 2 d S
N1 N 0.1295(9) 0.7670(9) -0.1285(6) 0.012(3) Uani 1 1 d U
C1 C 0.0836(10) 0.7859(10) -0.1638(7) 0.013(3) Uani 1 1 d U
H1A H 0.0242 0.7533 -0.1625 0.016 Uiso 1 1 calc R
C2 C 0.1222(11) 0.8531(11) -0.2027(8) 0.019(3) Uani 1 1 d .
H2A H 0.0887 0.8654 -0.2282 0.023 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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
O6 W1 O8 100.6(8) . . ?
O6 W1 O10 101.9(10) . . ?
O8 W1 O10 91.9(8) . . ?
O6 W1 O10 101.1(10) . 27_554 ?
O8 W1 O10 86.6(7) . 27_554 ?
O10 W1 O10 156.9(14) . 27_554 ?
O6 W1 O7 103.1(8) . . ?
O8 W1 O7 155.9(7) . . ?
O10 W1 O7 87.4(7) . . ?
O10 W1 O7 84.7(7) 27_554 . ?
O6 W1 O2 158.9(8) . . ?
O8 W1 O2 65.6(7) . . ?
O10 W1 O2 94.8(9) . . ?
O10 W1 O2 63.6(8) 27_554 . ?
O7 W1 O2 90.4(7) . . ?
O6 W1 O2 159.9(8) . 26_454 ?
O8 W1 O2 94.3(7) . 26_454 ?
O10 W1 O2 64.0(8) . 26_454 ?
O10 W1 O2 93.1(9) 27_554 26_454 ?
O7 W1 O2 63.8(7) . 26_454 ?
O2 W1 O2 41.2(8) . 26_454 ?
O9 W2 O7 102.1(7) . . ?
O9 W2 O5 100.9(9) . 2_665 ?
O7 W2 O5 90.1(8) . 2_665 ?
O9 W2 O8 100.6(7) . 26_454 ?
O7 W2 O8 88.2(7) . 26_454 ?
O5 W2 O8 158.2(9) 2_665 26_454 ?
O9 W2 O5 100.9(9) . . ?
O7 W2 O5 156.9(9) . . ?
O5 W2 O5 87.4(12) 2_665 . ?
O8 W2 O5 85.8(8) 26_454 . ?
O9 W2 O1 157.2(9) . . ?
O7 W2 O1 95.3(7) . . ?
O5 W2 O1 64.1(8) 2_665 . ?
O8 W2 O1 94.5(7) 26_454 . ?
O5 W2 O1 63.1(8) . . ?
O9 W2 O2 159.1(7) . 26_454 ?
O7 W2 O2 64.6(7) . 26_454 ?
O5 W2 O2 95.4(9) 2_665 26_454 ?
O8 W2 O2 64.4(7) 26_454 26_454 ?
O5 W2 O2 92.9(8) . 26_454 ?
O1 W2 O2 43.7(8) . 26_454 ?
O2 P1 O2 179.997(3) 27_554 3_565 ?
O2 P1 O2 69.1(7) 27_554 . ?
O2 P1 O2 110.9(7) 3_565 . ?
O2 P1 O2 69.1(7) 27_554 2_665 ?
O2 P1 O2 110.9(7) 3_565 2_665 ?
O2 P1 O2 110.9(7) . 2_665 ?
O2 P1 O2 110.9(7) 27_554 25_564 ?
O2 P1 O2 69.1(7) 3_565 25_564 ?
O2 P1 O2 179.997(4) . 25_564 ?
O2 P1 O2 69.1(7) 2_665 25_564 ?
O2 P1 O2 110.9(7) 27_554 26_454 ?
O2 P1 O2 69.1(7) 3_565 26_454 ?
O2 P1 O2 69.1(7) . 26_454 ?
O2 P1 O2 180.0(7) 2_665 26_454 ?
O2 P1 O2 110.9(7) 25_564 26_454 ?
O2 P1 O1 108.0(7) 27_554 25_564 ?
O2 P1 O1 72.0(7) 3_565 25_564 ?
O2 P1 O1 72.0(7) . 25_564 ?
O2 P1 O1 72.0(7) 2_665 25_564 ?
O2 P1 O1 108.0(7) 25_564 25_564 ?
O2 P1 O1 108.0(7) 26_454 25_564 ?
O2 P1 O1 72.0(7) 27_554 . ?
O2 P1 O1 108.0(7) 3_565 . ?
O2 P1 O1 108.0(7) . . ?
O2 P1 O1 108.0(7) 2_665 . ?
O2 P1 O1 72.0(7) 25_564 . ?
O2 P1 O1 72.0(7) 26_454 . ?
O1 P1 O1 179.997(4) 25_564 . ?
P1 O1 O2 52.7(10) . 27_554 ?
P1 O1 O2 52.7(10) . 25_564 ?
O2 O1 O2 87.1(15) 27_554 25_564 ?
P1 O1 O2 52.7(10) . 26_454 ?
O2 O1 O2 87.1(15) 27_554 26_454 ?
O2 O1 O2 87.1(15) 25_564 26_454 ?
P1 O1 W2 122.3(7) . 3_565 ?
O2 O1 W2 132.9(6) 27_554 3_565 ?
O2 O1 W2 69.5(6) 25_564 3_565 ?
O2 O1 W2 129.6(6) 26_454 3_565 ?
P1 O1 W2 122.3(7) . . ?
O2 O1 W2 129.6(6) 27_554 . ?
O2 O1 W2 132.9(6) 25_564 . ?
O2 O1 W2 69.5(6) 26_454 . ?
W2 O1 W2 94.2(9) 3_565 . ?
P1 O1 W2 122.3(7) . 2_665 ?
O2 O1 W2 69.5(6) 27_554 2_665 ?
O2 O1 W2 129.6(6) 25_564 2_665 ?
O2 O1 W2 132.9(6) 26_454 2_665 ?
W2 O1 W2 94.2(9) 3_565 2_665 ?
W2 O1 W2 94.2(9) . 2_665 ?
P1 O2 O2 55.5(3) . 27_554 ?
P1 O2 O2 55.5(4) . 26_454 ?
O2 O2 O2 93.2(16) 27_554 26_454 ?
P1 O2 O1 55.2(10) . 25_564 ?
O2 O2 O1 89.7(9) 27_554 25_564 ?
O2 O2 O1 89.7(9) 26_454 25_564 ?
P1 O2 W1 125.0(11) . . ?
O2 O2 W1 135.9(16) 27_554 . ?
O2 O2 W1 69.5(10) 26_454 . ?
O1 O2 W1 128.7(10) 25_564 . ?
P1 O2 W1 124.8(11) . 27_554 ?
O2 O2 W1 69.3(10) 27_554 27_554 ?
O2 O2 W1 133.0(16) 26_454 27_554 ?
O1 O2 W1 131.4(10) 25_564 27_554 ?
W1 O2 W1 92.7(7) . 27_554 ?
P1 O2 W2 122.0(11) . 27_554 ?
O2 O2 W2 127.3(14) 27_554 27_554 ?
O2 O2 W2 130.7(14) 26_454 27_554 ?
O1 O2 W2 66.8(10) 25_564 27_554 ?
W1 O2 W2 91.6(7) . 27_554 ?
W1 O2 W2 91.3(7) 27_554 27_554 ?
W2 O5 W2 138.3(13) 3_565 . ?
W2 O7 W1 139.5(9) . . ?
W1 O8 W2 138.1(9) . 27_554 ?
W2 O9 Cu1 146.8(8) . . ?
W1 O10 W1 139.1(13) . 26_454 ?
N1 Cu1 N1 178.3(9) 11_564 . ?
N1 Cu1 O9 88.9(6) 11_564 11_564 yes
N1 Cu1 O9 92.3(5) . 11_564 yes
N1 Cu1 O9 92.3(5) 11_564 . yes
N1 Cu1 O9 88.9(6) . . yes
O9 Cu1 O9 85.7(8) 11_564 . yes
C2 N1 C1 118.7(14) 31_564 . yes
C2 N1 Cu1 119.1(11) 31_564 . ?
C1 N1 Cu1 121.7(11) . . ?
N1 C1 C2 120.3(16) . . ?
N1 C2 C1 121.0(16) 31_564 . ?
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 O6 1.666(14) . ?
W1 O8 1.846(17) . ?
W1 O10 1.872(17) . ?
W1 O10 1.906(16) 27_554 ?
W1 O7 1.916(15) . ?
W1 O2 2.44(2) . ?
W1 O2 2.45(2) 26_454 ?
W2 O9 1.654(14) . ?
W2 O7 1.825(16) . ?
W2 O5 1.85(2) 2_665 ?
W2 O8 1.919(16) 26_454 ?
W2 O5 1.93(2) . ?
W2 O1 2.413(18) . ?
W2 O2 2.46(2) 26_454 ?
P1 O2 1.52(2) 27_554 ?
P1 O2 1.52(2) 3_565 ?
P1 O2 1.52(2) . ?
P1 O2 1.52(2) 2_665 ?
P1 O2 1.52(2) 25_564 ?
P1 O2 1.52(2) 26_454 ?
P1 O1 1.57(3) 25_564 ?
P1 O1 1.57(3) . ?
O1 O2 1.81(3) 27_554 ?
O1 O2 1.81(3) 25_564 ?
O1 O2 1.81(3) 26_454 ?
O1 W2 2.413(18) 3_565 ?
O1 W2 2.413(18) 2_665 ?
O2 O2 1.72(3) 27_554 ?
O2 O2 1.72(3) 26_454 ?
O2 O1 1.81(3) 25_564 ?
O2 W1 2.45(2) 27_554 ?
O2 W2 2.46(2) 27_554 ?
O5 W2 1.85(2) 3_565 ?
O8 W2 1.919(16) 27_554 ?
O9 Cu1 2.422(14) . yes
O10 W1 1.906(16) 26_454 yes
Cu1 N1 1.896(13) 11_564 yes
Cu1 N1 1.896(13) . yes
Cu1 O9 2.422(14) 11_564 yes
N1 C2 1.31(2) 31_564 ?
N1 C1 1.33(2) . ?
C1 C2 1.39(2) . ?
C2 N1 1.31(2) 31_564 ?
