#------------------------------------------------------------------------------
#$Date: 2016-08-26 16:26:54 +0300 (Fri, 26 Aug 2016) $
#$Revision: 186026 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/91/7119173.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_7119173
loop_
_publ_author_name
'Jian-Zhen Liao'
'Chen Wu'
'Xiao-Yuan Wu'
'Shui-Quan Deng'
'Can-Zhong Lu'
_publ_section_title
;
 Exceptional photosensitivity of a polyoxometalate-based charge-transfer
 hybrid material
;
_journal_name_full               Chem.Commun.
_journal_page_first              7394
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C64 H60 F3 N12 O52 P W12 Zn2'
_chemical_formula_sum            'C64 H60 F3 N12 O52 P W12 Zn2'
_chemical_formula_weight         4254.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-03-30 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.5965(3)
_cell_length_b                   19.5965(3)
_cell_length_c                   16.0780(3)
_cell_measurement_reflns_used    8879
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.6740
_cell_measurement_theta_min      2.6480
_cell_volume                     6174.32(18)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18135
_diffrn_reflns_theta_full        74.48
_diffrn_reflns_theta_max         74.48
_diffrn_reflns_theta_min         5.29
_exptl_absorpt_coefficient_mu    21.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3868
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.570
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6320
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0255P)²+26.3051P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                5155
_reflns_number_total             6320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc02711c2.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 4624 2016-04-14 12:54:50Z antanas 
;
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7119173
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.688401(13) 0.364213(13) 0.844065(14) 0.01423(7) Uani 1 1 d U . .
W2 W 0.633612(12) 0.198393(13) 0.843794(14) 0.01395(7) Uani 1 1 d U . .
W3 W 0.577582(13) 0.309211(14) 0.993694(14) 0.01543(8) Uani 1 1 d U . .
Zn1 Zn 0.2500 0.2500 0.59339(9) 0.0150(3) Uani 1 4 d SU . .
Zn2 Zn 0.2500 0.2500 0.84311(10) 0.0232(3) Uani 1 4 d SU . .
P1 P 0.7500 0.2500 1.0000 0.0118(5) Uani 1 4 d SU . .
F1 F 0.2500 0.2500 0.4487(6) 0.058(2) Uani 1 4 d SU . .
F2 F 0.2500 0.2500 0.7200(4) 0.0286(16) Uani 1 4 d SU . .
F3 F 0.2500 0.2500 0.9789(6) 0.068(3) Uani 1 4 d SU . .
N1 N 0.2541(3) 0.3573(3) 0.5908(3) 0.0286(12) Uani 1 1 d U . .
N2 N 0.2540(3) 0.5710(3) 0.6020(3) 0.0264(12) Uani 1 1 d U . .
N3 N 0.4141(3) 0.3979(3) 0.8443(4) 0.0421(15) Uani 1 1 d U . .
O1 O 0.1374(3) 0.5678(2) 0.6171(3) 0.0353(11) Uani 1 1 d U . .
O2 O 0.3688(3) 0.5737(2) 0.5824(3) 0.0342(11) Uani 1 1 d U . .
O3 O 0.3366(2) 0.3149(2) 0.8381(3) 0.0381(11) Uani 1 1 d U . .
O4 O 0.7240(2) 0.1725(2) 0.8150(2) 0.0257(10) Uani 1 1 d U . .
O5 O 0.5859(2) 0.1575(2) 0.7709(2) 0.0290(10) Uani 1 1 d U . .
O6 O 0.5639(2) 0.2430(2) 0.9085(2) 0.0275(10) Uani 1 1 d U . .
O7 O 0.6487(2) 0.2851(2) 0.7919(2) 0.0252(9) Uani 1 1 d U . .
O8 O 0.5874(2) 0.2359(2) 1.0706(2) 0.0256(10) Uani 1 1 d U . .
O9 O 0.6897(2) 0.2708(2) 0.9451(2) 0.0211(9) Uani 1 1 d U . .
O10 O 0.6317(2) 0.3604(2) 1.0710(2) 0.0258(9) Uani 1 1 d U . .
O11 O 0.6758(2) 0.4260(2) 0.7718(3) 0.0322(11) Uani 1 1 d U . .
O12 O 0.6066(2) 0.3713(2) 0.9077(2) 0.0268(10) Uani 1 1 d U . .
O13 O 0.4972(2) 0.3373(3) 1.0124(2) 0.0357(12) Uani 1 1 d U . .
C1 C 0.2195(4) 0.3946(3) 0.5346(4) 0.0325(16) Uani 1 1 d U . .
H1 H 0.1942 0.3715 0.4928 0.039 Uiso 1 1 calc R . .
C2 C 0.2193(4) 0.4646(3) 0.5351(4) 0.0348(16) Uani 1 1 d U . .
H2 H 0.1955 0.4898 0.4938 0.042 Uiso 1 1 calc R . .
C3 C 0.2552(4) 0.4978(3) 0.5984(4) 0.0296(15) Uani 1 1 d U . .
C4 C 0.2906(3) 0.4604(3) 0.6562(4) 0.0285(14) Uani 1 1 d U . .
H4 H 0.3163 0.4824 0.6985 0.034 Uiso 1 1 calc R . .
C5 C 0.2881(3) 0.3901(3) 0.6513(4) 0.0319(15) Uani 1 1 d U . .
H5 H 0.3112 0.3640 0.6923 0.038 Uiso 1 1 calc R . .
C6 C 0.1894(3) 0.6021(3) 0.6100(4) 0.0253(14) Uani 1 1 d U . .
C7 C 0.1885(3) 0.6779(3) 0.6067(3) 0.0240(14) Uani 1 1 d U . .
C8 C 0.2506(3) 0.7140(3) 0.6067(3) 0.0212(13) Uani 1 1 d U . .
C9 C 0.3139(3) 0.6800(3) 0.6038(3) 0.0238(14) Uani 1 1 d U . .
C10 C 0.3163(3) 0.6053(3) 0.5959(4) 0.0252(14) Uani 1 1 d U . .
C11 C 0.3742(3) 0.7166(3) 0.6050(3) 0.0244(14) Uani 1 1 d U . .
H11 H 0.4167 0.6933 0.6040 0.029 Uiso 1 1 calc R . .
C12 C 0.3728(3) 0.7885(3) 0.6076(4) 0.0269(14) Uani 1 1 d U . .
H12 H 0.4143 0.8135 0.6099 0.032 Uiso 1 1 calc R . .
C13 C 0.3565(4) 0.3699(4) 0.8686(4) 0.0349(16) Uani 1 1 d U . .
C14 C 0.3173(5) 0.4061(4) 0.9346(5) 0.055(2) Uani 1 1 d U . .
H14A H 0.2723 0.3849 0.9407 0.082 Uiso 1 1 calc R . .
H14B H 0.3118 0.4541 0.9191 0.082 Uiso 1 1 calc R . .
H14C H 0.3421 0.4031 0.9875 0.082 Uiso 1 1 calc R . .
C15 C 0.4553(4) 0.3638(5) 0.7798(6) 0.059(2) Uani 1 1 d U . .
H15A H 0.4333 0.3209 0.7637 0.089 Uiso 1 1 calc R . .
H15B H 0.5010 0.3543 0.8018 0.089 Uiso 1 1 calc R . .
H15C H 0.4591 0.3936 0.7311 0.089 Uiso 1 1 calc R . .
C16 C 0.4431(5) 0.4614(4) 0.8771(6) 0.061(2) Uani 1 1 d U . .
H16A H 0.4142 0.4784 0.9223 0.092 Uiso 1 1 calc R . .
H16B H 0.4452 0.4955 0.8326 0.092 Uiso 1 1 calc R . .
H16C H 0.4891 0.4526 0.8982 0.092 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 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O11 W1 O12 101.2(2) . .
O11 W1 O8 102.0(2) . 6_667
O12 W1 O8 89.31(18) . 6_667
O11 W1 O4 103.35(19) . 3_655
O12 W1 O4 155.47(17) . 3_655
O8 W1 O4 85.70(17) 6_667 3_655
O11 W1 O7 102.5(2) . .
O12 W1 O7 87.28(18) . .
O8 W1 O7 155.37(17) 6_667 .
O4 W1 O7 87.34(18) 3_655 .
O11 W1 O9 171.91(18) . .
O12 W1 O9 72.93(15) . .
O8 W1 O9 83.65(15) 6_667 .
O4 W1 O9 82.65(16) 3_655 .
O7 W1 O9 72.03(15) . .
O5 W2 O10 101.94(19) . 8_657
O5 W2 O4 102.64(19) . .
O10 W2 O4 86.26(17) 8_657 .
O5 W2 O7 101.70(19) . .
O10 W2 O7 156.35(17) 8_657 .
O4 W2 O7 89.25(18) . .
O5 W2 O6 101.30(19) . .
O10 W2 O6 88.04(18) 8_657 .
O4 W2 O6 156.04(17) . .
O7 W2 O6 86.70(18) . .
O5 W2 O9 171.37(18) . .
O10 W2 O9 83.69(15) 8_657 .
O4 W2 O9 84.11(16) . .
O7 W2 O9 72.76(15) . .
O6 W2 O9 72.13(15) . .
O13 W3 O8 102.9(2) . .
O13 W3 O6 102.6(2) . .
O8 W3 O6 88.11(18) . .
O13 W3 O10 103.2(2) . .
O8 W3 O10 85.32(18) . .
O6 W3 O10 154.18(17) . .
O13 W3 O12 101.4(2) . .
O8 W3 O12 155.72(17) . .
O6 W3 O12 87.47(18) . .
O10 W3 O12 88.34(18) . .
O13 W3 O9 171.62(16) . .
O8 W3 O9 83.37(15) . .
O6 W3 O9 71.81(15) . .
O10 W3 O9 82.63(15) . .
O12 W3 O9 72.57(15) . .
F2 Zn1 N1 91.13(15) . 3
F2 Zn1 N1 91.13(15) . 2
N1 Zn1 N1 89.978(7) 3 2
F2 Zn1 N1 91.13(15) . .
N1 Zn1 N1 177.7(3) 3 .
N1 Zn1 N1 89.978(6) 2 .
F2 Zn1 N1 91.13(15) . 4
N1 Zn1 N1 89.978(6) 3 4
N1 Zn1 N1 177.7(3) 2 4
N1 Zn1 N1 89.978(7) . 4
F2 Zn1 F1 180.000(2) . .
N1 Zn1 F1 88.87(15) 3 .
N1 Zn1 F1 88.87(15) 2 .
N1 Zn1 F1 88.87(15) . .
N1 Zn1 F1 88.87(15) 4 .
F2 Zn2 O3 87.82(14) . 3
F2 Zn2 O3 87.82(14) . .
O3 Zn2 O3 175.6(3) 3 .
F2 Zn2 O3 87.82(14) . 2
O3 Zn2 O3 89.917(11) 3 2
O3 Zn2 O3 89.917(11) . 2
F2 Zn2 O3 87.82(14) . 4
O3 Zn2 O3 89.917(11) 3 4
O3 Zn2 O3 89.917(11) . 4
O3 Zn2 O3 175.6(3) 2 4
F2 Zn2 F3 180.000(3) . .
O3 Zn2 F3 92.18(14) 3 .
O3 Zn2 F3 92.18(14) . .
O3 Zn2 F3 92.18(14) 2 .
O3 Zn2 F3 92.18(14) 4 .
O9 P1 O9 109.40(14) . 8_657
O9 P1 O9 109.40(14) . 6_667
O9 P1 O9 109.6(3) 8_657 6_667
O9 P1 O9 109.6(3) . 3_655
O9 P1 O9 109.40(14) 8_657 3_655
O9 P1 O9 109.40(14) 6_667 3_655
Zn2 F2 Zn1 180.0 . .
C5 N1 C1 118.5(6) . .
C5 N1 Zn1 118.9(4) . .
C1 N1 Zn1 122.4(4) . .
C10 N2 C6 125.7(5) . .
C10 N2 C3 117.6(6) . .
C6 N2 C3 116.7(5) . .
C13 N3 C16 125.4(7) . .
C13 N3 C15 119.4(6) . .
C16 N3 C15 115.2(6) . .
C13 O3 Zn2 138.9(5) . .
W2 O4 W1 151.0(2) . 3_655
W3 O6 W2 126.6(2) . .
W2 O7 W1 125.9(2) . .
W3 O8 W1 152.1(2) . 8_657
P1 O9 W2 125.6(2) . .
P1 O9 W1 126.1(2) . .
W2 O9 W1 89.26(12) . .
P1 O9 W3 126.2(2) . .
W2 O9 W3 89.31(13) . .
W1 O9 W3 88.44(13) . .
W2 O10 W3 151.8(2) 6_667 .
W1 O12 W3 126.0(2) . .
N1 C1 C2 122.7(6) . .
C1 C2 C3 117.9(6) . .
C4 C3 C2 120.0(6) . .
C4 C3 N2 121.0(6) . .
C2 C3 N2 119.1(6) . .
C3 C4 C5 118.4(6) . .
N1 C5 C4 122.4(6) . .
O1 C6 N2 121.3(6) . .
O1 C6 C7 122.7(6) . .
N2 C6 C7 116.0(5) . .
C12 C7 C8 121.1(6) 3_565 .
C12 C7 C6 119.4(6) 3_565 .
C8 C7 C6 119.4(6) . .
C9 C8 C8 119.2(7) . 3_565
C9 C8 C7 121.7(6) . .
C8 C8 C7 119.2(7) 3_565 .
C11 C9 C8 120.5(6) . .
C11 C9 C10 119.4(6) . .
C8 C9 C10 120.1(6) . .
O2 C10 N2 120.4(6) . .
O2 C10 C9 123.2(6) . .
N2 C10 C9 116.4(6) . .
C9 C11 C12 120.2(6) . .
C7 C12 C11 119.8(6) 3_565 .
O3 C13 N3 120.8(7) . .
O3 C13 C14 122.1(7) . .
N3 C13 C14 117.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O11 1.695(4) .
W1 O12 1.906(4) .
W1 O8 1.910(4) 6_667
W1 O4 1.919(4) 3_655
W1 O7 1.926(4) .
W1 O9 2.448(4) .
W2 O5 1.701(4) .
W2 O10 1.897(4) 8_657
W2 O4 1.900(4) .
W2 O7 1.916(4) .
W2 O6 1.926(4) .
W2 O9 2.424(4) .
W3 O13 1.696(5) .
W3 O8 1.905(4) .
W3 O6 1.907(4) .
W3 O10 1.917(4) .
W3 O12 1.927(4) .
W3 O9 2.449(4) .
Zn1 F2 2.036(7) .
Zn1 N1 2.105(5) 3
Zn1 N1 2.105(5) 2
Zn1 N1 2.105(5) .
Zn1 N1 2.105(5) 4
Zn1 F1 2.326(10) .
Zn2 F2 1.979(7) .
Zn2 O3 2.123(5) 3
Zn2 O3 2.123(5) .
Zn2 O3 2.123(5) 2
Zn2 O3 2.123(5) 4
Zn2 F3 2.183(10) .
P1 O9 1.531(4) .
P1 O9 1.531(4) 8_657
P1 O9 1.531(4) 6_667
P1 O9 1.531(4) 3_655
N1 C5 1.342(8) .
N1 C1 1.346(8) .
N2 C10 1.397(8) .
N2 C6 1.411(8) .
N2 C3 1.437(8) .
N3 C13 1.315(9) .
N3 C16 1.466(10) .
N3 C15 1.474(10) .
O1 C6 1.225(8) .
O2 C10 1.219(7) .
O3 C13 1.246(8) .
O4 W1 1.919(4) 3_655
O8 W1 1.910(4) 8_657
O10 W2 1.897(4) 6_667
C1 C2 1.372(9) .
C2 C3 1.397(9) .
C3 C4 1.371(9) .
C4 C5 1.381(9) .
C6 C7 1.487(8) .
C7 C12 1.371(9) 3_565
C7 C8 1.409(9) .
C8 C9 1.408(8) .
C8 C8 1.412(12) 3_565
C9 C11 1.382(9) .
C9 C10 1.472(8) .
C11 C12 1.409(9) .
C12 C7 1.371(9) 3_565
C13 C14 1.490(10) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.133 0.344 0.500 1942 466 ' '
