#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:12:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179958 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/52/7025237.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_7025237
loop_
_publ_author_name
'Cui, Feng-Yun'
'Huang, Kun-Lin'
'Ma, Xiao-Yu'
'Li, Cong'
'Han, Zhan-Gang'
'Gao, Yuan-Zhe'
'Liu, Xi'
'Chi, Ying-Nan'
'Hu, Chang-Wen'
_publ_section_title
;
 Transformation from [W6O19]2− to [W6O22]8− stabilized by
 Cu(ii) complexation
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              5080
_journal_paper_doi               10.1039/b926024b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C56 H38 Cl2 Cu2 N18 O19 W6'
_chemical_formula_weight         2568.12
_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                98.0720(10)
_cell_angle_beta                 109.9870(10)
_cell_angle_gamma                117.834(2)
_cell_formula_units_Z            1
_cell_length_a                   12.0461(13)
_cell_length_b                   12.8977(14)
_cell_length_c                   13.7956(13)
_cell_measurement_reflns_used    5542
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.277
_cell_measurement_theta_min      3.402
_cell_volume                     1661.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8798
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    11.134
_exptl_absorpt_correction_T_max  0.4023
_exptl_absorpt_correction_T_min  0.3047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5786
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0331
_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)+(0.0660P)²+0.2457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                4690
_reflns_number_total             5786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926024b.txt
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025237
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
W1 W 0.50462(4) 0.32867(3) 0.52848(3) 0.03966(12) Uani 1 1 d .
W2 W 0.48229(4) 0.54477(3) 0.66086(3) 0.04040(12) Uani 1 1 d .
W3 W 0.25539(3) 0.37295(3) 0.39977(3) 0.03950(11) Uani 1 1 d .
Cu1 Cu 0.63113(10) 0.86566(9) 0.92823(8) 0.0348(2) Uani 1 1 d .
Cl1 Cl 0.7900(2) 1.08456(19) 1.05256(17) 0.0461(5) Uani 1 1 d .
N1 N 0.8934(6) 0.8531(6) 0.9250(5) 0.0336(14) Uani 1 1 d .
H1 H 0.9740 0.8656 0.9358 0.040 Uiso 1 1 calc R
N2 N 0.7277(6) 0.9000(6) 0.8369(5) 0.0314(13) Uani 1 1 d .
N3 N 0.9273(7) 0.9561(6) 0.8091(5) 0.0346(14) Uani 1 1 d .
N4 N 0.4930(7) 0.8810(6) 0.8036(5) 0.0356(14) Uani 1 1 d .
N5 N 0.9495(8) 1.1265(8) 0.6274(7) 0.056(2) Uani 1 1 d .
N6 N 0.7252(7) 0.7818(6) 0.9898(5) 0.0335(14) Uani 1 1 d .
N7 N 0.8920(7) 0.7238(6) 1.0223(6) 0.0448(17) Uani 1 1 d .
N8 N 0.5288(7) 0.7973(6) 1.0142(5) 0.0400(15) Uani 1 1 d .
O1 O 0.5000 0.5000 0.5000 0.0368(17) Uani 1 2 d S
O2 O 0.4879(6) 0.3982(5) 0.6520(4) 0.0443(14) Uani 1 1 d .
O3 O 0.5168(6) 0.3265(5) 0.3934(5) 0.0430(13) Uani 1 1 d .
O4 O 0.3069(6) 0.2603(5) 0.4417(4) 0.0397(13) Uani 1 1 d .
O5 O 0.7000(6) 0.4644(6) 0.6044(5) 0.0507(15) Uani 1 1 d .
O6 O 0.5053(7) 0.2010(6) 0.5491(6) 0.0601(18) Uani 1 1 d .
O7 O 0.2897(6) 0.4346(5) 0.5490(5) 0.0449(14) Uani 1 1 d .
O8 O 0.6827(6) 0.6383(5) 0.7101(4) 0.0448(14) Uani 1 1 d .
O9 O 0.4711(8) 0.5765(6) 0.7791(5) 0.067(2) Uani 1 1 d .
O10 O 0.0756(6) 0.2810(6) 0.3288(6) 0.0605(18) Uani 1 1 d .
C1 C 0.8451(8) 0.9043(7) 0.8558(6) 0.0326(16) Uani 1 1 d .
C2 C 0.8858(8) 1.0053(7) 0.7377(6) 0.0334(17) Uani 1 1 d .
C3 C 0.7634(8) 1.0027(7) 0.7108(6) 0.0381(18) Uani 1 1 d .
H3 H 0.7355 1.0373 0.6604 0.046 Uiso 1 1 calc R
C4 C 0.6851(8) 0.9472(7) 0.7613(6) 0.0337(16) Uani 1 1 d .
C5 C 0.5464(8) 0.9275(7) 0.7384(7) 0.0364(17) Uani 1 1 d .
C6 C 0.4748(10) 0.9520(9) 0.6534(7) 0.052(2) Uani 1 1 d .
H6 H 0.5160 0.9883 0.6111 0.063 Uiso 1 1 calc R
C7 C 0.3399(10) 0.9215(11) 0.6319(8) 0.062(3) Uani 1 1 d .
H7 H 0.2883 0.9355 0.5738 0.074 Uiso 1 1 calc R
C8 C 0.2848(10) 0.8716(10) 0.6961(8) 0.059(3) Uani 1 1 d .
H8 H 0.1937 0.8488 0.6821 0.071 Uiso 1 1 calc R
C9 C 0.3633(10) 0.8548(9) 0.7813(8) 0.053(2) Uani 1 1 d .
H9 H 0.3254 0.8235 0.8270 0.064 Uiso 1 1 calc R
C10 C 0.9787(8) 1.0615(7) 0.6867(6) 0.0358(17) Uani 1 1 d .
C11 C 1.0893(9) 1.0476(8) 0.7035(8) 0.048(2) Uani 1 1 d .
H11 H 1.1052 0.9998 0.7443 0.057 Uiso 1 1 calc R
C12 C 1.1754(10) 1.1060(9) 0.6585(8) 0.056(2) Uani 1 1 d .
H12 H 1.2522 1.0996 0.6694 0.067 Uiso 1 1 calc R
C13 C 1.1485(11) 1.1730(10) 0.5984(9) 0.069(3) Uani 1 1 d .
H13 H 1.2049 1.2119 0.5660 0.083 Uiso 1 1 calc R
C14 C 1.0379(12) 1.1822(11) 0.5864(9) 0.071(3) Uani 1 1 d .
H14 H 1.0221 1.2307 0.5467 0.085 Uiso 1 1 calc R
C15 C 0.8320(8) 0.7842(7) 0.9803(6) 0.0356(17) Uani 1 1 d .
C16 C 0.8321(9) 0.6539(8) 1.0745(8) 0.051(2) Uani 1 1 d .
C17 C 0.7194(9) 0.6438(8) 1.0875(7) 0.047(2) Uani 1 1 d .
H17 H 0.6803 0.5938 1.1242 0.056 Uiso 1 1 calc R
C18 C 0.6670(8) 0.7102(7) 1.0441(6) 0.0386(18) Uani 1 1 d .
C19 C 0.5579(8) 0.7216(7) 1.0593(6) 0.0387(18) Uani 1 1 d .
C20 C 0.4955(10) 0.6653(9) 1.1195(8) 0.056(2) Uani 1 1 d .
H20 H 0.5161 0.6120 1.1486 0.067 Uiso 1 1 calc R
C21 C 0.4022(11) 0.6884(11) 1.1363(8) 0.068(3) Uani 1 1 d .
H21 H 0.3573 0.6496 1.1758 0.082 Uiso 1 1 calc R
C22 C 0.3755(11) 0.7694(10) 1.0943(8) 0.061(3) Uani 1 1 d .
H22 H 0.3146 0.7881 1.1067 0.074 Uiso 1 1 calc R
C23 C 0.4396(10) 0.8216(9) 1.0344(7) 0.052(2) Uani 1 1 d .
H23 H 0.4214 0.8764 1.0061 0.062 Uiso 1 1 calc R
C24 C 0.8925(11) 0.5881(10) 1.1236(11) 0.075(4) Uani 1 1 d .
N9 N 0.8301(12) 0.5134(10) 1.1673(10) 0.104(4) Uani 1 1 d .
C25 C 0.995(2) 0.5901(19) 1.1076(18) 0.161(7) Uani 1 1 d U
H25 H 1.0431 0.6489 1.0808 0.194 Uiso 1 1 calc R
C26 C 1.035(3) 0.498(2) 1.132(2) 0.186(8) Uani 1 1 d U
H26 H 1.0902 0.4811 1.1080 0.223 Uiso 1 1 calc R
C27 C 0.979(2) 0.4428(19) 1.1959(18) 0.158(7) Uani 1 1 d U
H27 H 1.0119 0.3993 1.2311 0.189 Uiso 1 1 calc R
C28 C 0.875(2) 0.4502(16) 1.2089(15) 0.132(6) Uani 1 1 d U
H28 H 0.8356 0.4076 1.2496 0.158 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'
O O 0.0106 0.0060 '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'
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'
Cl Cl 0.1484 0.1585 '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
O6 W1 O5 104.5(3) . .
O6 W1 O4 103.1(3) . .
O5 W1 O4 152.4(2) . .
O6 W1 O3 104.3(3) . .
O5 W1 O3 87.4(3) . .
O4 W1 O3 86.2(2) . .
O6 W1 O2 103.6(3) . .
O5 W1 O2 86.7(3) . .
O4 W1 O2 86.4(2) . .
O3 W1 O2 152.1(2) . .
O6 W1 O1 179.1(2) . .
O5 W1 O1 76.30(17) . .
O4 W1 O1 76.08(15) . .
O3 W1 O1 76.05(16) . .
O2 W1 O1 76.02(16) . .
O9 W2 O7 104.3(3) . .
O9 W2 O3 104.6(3) . 2_666
O7 W2 O3 86.9(2) . 2_666
O9 W2 O2 102.8(3) . .
O7 W2 O2 86.5(3) . .
O3 W2 O2 152.5(2) 2_666 .
O9 W2 O8 103.2(3) . .
O7 W2 O8 152.6(2) . .
O3 W2 O8 86.5(3) 2_666 .
O2 W2 O8 87.2(3) . .
O9 W2 O1 179.0(3) . .
O7 W2 O1 76.28(17) . .
O3 W2 O1 76.16(17) 2_666 .
O2 W2 O1 76.36(16) . .
O8 W2 O1 76.28(16) . .
O10 W3 O4 103.9(3) . .
O10 W3 O8 104.9(3) . 2_666
O4 W3 O8 86.6(2) . 2_666
O10 W3 O7 102.5(3) . .
O4 W3 O7 87.2(2) . .
O8 W3 O7 152.6(2) 2_666 .
O10 W3 O5 103.5(3) . 2_666
O4 W3 O5 152.6(2) . 2_666
O8 W3 O5 86.4(3) 2_666 2_666
O7 W3 O5 87.0(3) . 2_666
O10 W3 O1 178.7(3) . .
O4 W3 O1 76.35(16) . .
O8 W3 O1 76.40(16) 2_666 .
O7 W3 O1 76.20(16) . .
O5 W3 O1 76.29(17) 2_666 .
N2 Cu1 N6 89.6(3) . .
N2 Cu1 N8 168.4(3) . .
N6 Cu1 N8 81.4(3) . .
N2 Cu1 N4 80.5(2) . .
N6 Cu1 N4 153.6(3) . .
N8 Cu1 N4 104.6(3) . .
N2 Cu1 Cl1 90.94(19) . .
N6 Cu1 Cl1 105.06(19) . .
N8 Cu1 Cl1 98.4(2) . .
N4 Cu1 Cl1 99.50(19) . .
C1 N1 C15 129.2(7) . .
C1 N2 C4 117.3(6) . .
C1 N2 Cu1 126.1(5) . .
C4 N2 Cu1 115.3(5) . .
C2 N3 C1 116.9(7) . .
C9 N4 C5 117.4(7) . .
C9 N4 Cu1 130.2(6) . .
C5 N4 Cu1 112.3(5) . .
C14 N5 C10 115.7(8) . .
C15 N6 C18 117.9(6) . .
C15 N6 Cu1 127.6(5) . .
C18 N6 Cu1 114.4(5) . .
C16 N7 C15 114.7(7) . .
C19 N8 C23 117.7(7) . .
C19 N8 Cu1 114.4(5) . .
C23 N8 Cu1 127.8(6) . .
W3 O1 W3 180.0 . 2_666
W3 O1 W2 90.023(13) . 2_666
W3 O1 W2 89.977(13) 2_666 2_666
W3 O1 W2 89.977(13) . .
W3 O1 W2 90.023(13) 2_666 .
W2 O1 W2 180.0 2_666 .
W3 O1 W1 90.005(13) . .
W3 O1 W1 89.995(13) 2_666 .
W2 O1 W1 89.917(12) 2_666 .
W2 O1 W1 90.083(12) . .
W3 O1 W1 89.995(13) . 2_666
W3 O1 W1 90.005(13) 2_666 2_666
W2 O1 W1 90.083(12) 2_666 2_666
W2 O1 W1 89.917(12) . 2_666
W1 O1 W1 180.0 . 2_666
W2 O2 W1 117.5(3) . .
W2 O3 W1 117.9(3) 2_666 .
W3 O4 W1 117.6(3) . .
W1 O5 W3 117.4(3) . 2_666
W2 O7 W3 117.5(3) . .
W2 O8 W3 117.3(3) . 2_666
N2 C1 N3 124.8(7) . .
N2 C1 N1 122.4(7) . .
N3 C1 N1 112.8(7) . .
N3 C2 C3 122.4(7) . .
N3 C2 C10 115.7(7) . .
C3 C2 C10 121.9(7) . .
C4 C3 C2 117.0(7) . .
N2 C4 C3 121.5(7) . .
N2 C4 C5 113.3(7) . .
C3 C4 C5 125.2(7) . .
N4 C5 C6 122.0(8) . .
N4 C5 C4 115.6(7) . .
C6 C5 C4 122.4(8) . .
C5 C6 C7 118.8(9) . .
C8 C7 C6 119.1(8) . .
C7 C8 C9 119.2(9) . .
N4 C9 C8 123.5(9) . .
N5 C10 C11 123.5(8) . .
N5 C10 C2 116.0(7) . .
C11 C10 C2 120.5(7) . .
C10 C11 C12 118.0(9) . .
C13 C12 C11 119.7(9) . .
C12 C13 C14 118.4(9) . .
N5 C14 C13 124.7(9) . .
N6 C15 N7 125.8(7) . .
N6 C15 N1 120.6(6) . .
N7 C15 N1 113.6(7) . .
N7 C16 C17 123.9(7) . .
N7 C16 C24 117.9(9) . .
C17 C16 C24 118.2(9) . .
C18 C17 C16 117.4(8) . .
N6 C18 C17 120.2(8) . .
N6 C18 C19 114.3(7) . .
C17 C18 C19 125.2(8) . .
N8 C19 C20 122.1(8) . .
N8 C19 C18 114.8(7) . .
C20 C19 C18 123.0(8) . .
C21 C20 C19 119.2(9) . .
C20 C21 C22 119.4(9) . .
C23 C22 C21 118.8(10) . .
N8 C23 C22 122.8(9) . .
N9 C24 C25 120.8(12) . .
N9 C24 C16 118.6(11) . .
C25 C24 C16 119.7(12) . .
C24 N9 C28 122.0(15) . .
C24 C25 C26 121(2) . .
C27 C26 C25 110(2) . .
C26 C27 C28 121.7(19) . .
N9 C28 C27 122.1(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O6 1.713(6) .
W1 O5 1.911(6) .
W1 O4 1.918(6) .
W1 O3 1.917(6) .
W1 O2 1.929(6) .
W1 O1 2.3204(4) .
W2 O9 1.692(6) .
W2 O7 1.908(6) .
W2 O3 1.911(5) 2_666
W2 O2 1.911(6) .
W2 O8 1.917(6) .
W2 O1 2.3200(4) .
W3 O10 1.697(6) .
W3 O4 1.913(5) .
W3 O8 1.920(6) 2_666
W3 O7 1.922(6) .
W3 O5 1.922(6) 2_666
W3 O1 2.3128(4) .
Cu1 N2 1.953(6) .
Cu1 N6 1.979(6) .
Cu1 N8 1.995(7) .
Cu1 N4 2.052(6) .
Cu1 Cl1 2.434(2) .
N1 C1 1.358(9) .
N1 C15 1.371(10) .
N2 C1 1.320(10) .
N2 C4 1.351(9) .
N3 C2 1.326(10) .
N3 C1 1.335(10) .
N4 C9 1.341(11) .
N4 C5 1.330(10) .
N5 C14 1.335(12) .
N5 C10 1.331(10) .
N6 C15 1.324(10) .
N6 C18 1.361(10) .
N7 C16 1.335(11) .
N7 C15 1.354(9) .
N8 C19 1.344(10) .
N8 C23 1.352(11) .
O1 W3 2.3128(4) 2_666
O1 W2 2.3200(4) 2_666
O1 W1 2.3204(4) 2_666
O3 W2 1.911(5) 2_666
O5 W3 1.922(6) 2_666
O8 W3 1.920(6) 2_666
C2 C3 1.375(11) .
C2 C10 1.481(10) .
C3 C4 1.359(11) .
C4 C5 1.475(11) .
C5 C6 1.372(11) .
C6 C7 1.388(12) .
C7 C8 1.343(13) .
C8 C9 1.351(12) .
C10 C11 1.372(11) .
C11 C12 1.368(12) .
C12 C13 1.348(14) .
C13 C14 1.349(15) .
C16 C17 1.378(13) .
C16 C24 1.453(12) .
C17 C18 1.372(11) .
C18 C19 1.467(12) .
C19 C20 1.367(11) .
C20 C21 1.371(14) .
C21 C22 1.374(15) .
C22 C23 1.355(12) .
C24 N9 1.286(15) .
C24 C25 1.31(2) .
N9 C28 1.271(17) .
C25 C26 1.52(3) .
C26 C27 1.36(3) .
C27 C28 1.37(3) .
