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#$Date: 2016-03-26 21:12:15 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180470 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/39/7213937.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_7213937
loop_
_publ_author_name
'Guo, Hai-Yang'
'Li, Zhi-Fang'
'Zhao, De-Chuan'
'Hu, Yang-Yang'
'Xiao, Li-Na'
'Cui, Xiao-Bing'
'Guan, Jing-Qi'
'Xu, Ji-Qing'
_publ_section_title
;
 The synthesis and characterization of three organic--inorganic hybrids
 based on different transition metal complexes and {As8V14O42(H2O)}
 clusters
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2251
_journal_paper_doi               10.1039/c3ce42450b
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C80 H66 As8 Cu4 N16 O43 V14'
_chemical_formula_weight         3506.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.369(4)
_cell_length_b                   28.369(4)
_cell_length_c                   14.436(3)
_cell_measurement_temperature    293(2)
_cell_volume                     11618(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0963
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54802
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    4.130
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6816
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6639
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0654
_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)+(0.1184P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2244
_reflns_number_gt                2914
_reflns_number_total             6639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42450b.txt
_cod_data_source_block           k
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7213937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
As1 As 0.53864(3) 0.13636(4) 0.08895(6) 0.0969(4) Uani 1 1 d .
As2 As 0.42636(3) 0.15531(4) 0.08800(6) 0.0949(4) Uani 1 1 d .
V1 V 0.63865(5) 0.22755(5) -0.13393(10) 0.0842(4) Uani 1 1 d .
V2 V 0.59929(5) 0.23303(6) 0.04747(10) 0.0871(5) Uani 1 1 d .
V3 V 0.61201(5) 0.33026(5) -0.12494(9) 0.0815(4) Uani 1 1 d .
V4 V 0.5000 0.2500 0.13447(12) 0.0908(7) Uani 1 2 d S
Cu1 Cu 0.83806(5) 0.41097(5) 0.05944(13) 0.1380(6) Uani 1 1 d .
O1 O 0.60761(18) 0.18673(18) -0.0479(4) 0.0814(14) Uani 1 1 d .
O2 O 0.62270(19) 0.2763(2) -0.0460(4) 0.0852(15) Uani 1 1 d .
O3 O 0.53068(18) 0.1273(2) -0.0303(4) 0.0857(15) Uani 1 1 d .
O4 O 0.6943(2) 0.2200(2) -0.1320(4) 0.1066(19) Uani 1 1 d U
O5 O 0.6379(2) 0.2245(2) 0.1250(5) 0.1076(19) Uani 1 1 d U
O6 O 0.4796(2) 0.1291(2) 0.1276(4) 0.0961(17) Uani 1 1 d U
O7 O 0.5000 0.2500 0.2420(6) 0.110(3) Uani 1 2 d SU
O8 O 0.4441(2) 0.2151(2) 0.0891(4) 0.0922(16) Uani 1 1 d U
O9 O 0.6572(2) 0.3628(2) -0.1262(4) 0.0999(17) Uani 1 1 d U
O10 O 0.54140(19) 0.1987(2) 0.0882(4) 0.0891(15) Uani 1 1 d U
O11 O 0.43222(18) 0.1437(2) -0.0305(4) 0.0846(15) Uani 1 1 d .
N3 N 0.7952(3) 0.3591(3) 0.0981(6) 0.104(2) Uani 1 1 d U
N2 N 0.9055(3) 0.4034(4) 0.0978(7) 0.117(3) Uani 1 1 d U
N4 N 0.8082(3) 0.3993(3) -0.0626(7) 0.114(3) Uani 1 1 d U
N1 N 0.8471(4) 0.4697(4) 0.1331(8) 0.146(3) Uani 1 1 d U
OW1 O 0.5000 0.2500 -0.1250 0.233(11) Uani 1 4 d S
C1 C 0.8134(7) 0.5047(7) 0.1366(13) 0.207(7) Uani 1 1 d U
H1A H 0.7837 0.5011 0.1105 0.248 Uiso 1 1 calc R
C2 C 0.8285(9) 0.5510(8) 0.1876(16) 0.237(9) Uani 1 1 d U
H2A H 0.8105 0.5784 0.1906 0.285 Uiso 1 1 calc R
C3 C 0.8702(7) 0.5458(7) 0.2252(14) 0.205(7) Uani 1 1 d U
H3A H 0.8788 0.5709 0.2631 0.246 Uiso 1 1 calc R
C4 C 0.9040(7) 0.5108(7) 0.2205(12) 0.192(6) Uani 1 1 d U
H4A H 0.9332 0.5138 0.2491 0.230 Uiso 1 1 calc R
C5 C 0.8920(5) 0.4718(4) 0.1713(8) 0.121(4) Uani 1 1 d .
C6 C 0.9233(5) 0.4341(4) 0.1560(7) 0.121(4) Uani 1 1 d .
C7 C 0.9682(5) 0.4322(5) 0.1950(8) 0.123(4) Uani 1 1 d .
H7A H 0.9791 0.4549 0.2361 0.148 Uiso 1 1 calc R
C8 C 0.9948(6) 0.3947(6) 0.1689(10) 0.148(5) Uani 1 1 d .
H8A H 1.0251 0.3923 0.1928 0.177 Uiso 1 1 calc R
C9 C 0.9800(6) 0.3616(7) 0.1116(11) 0.166(6) Uani 1 1 d .
H9A H 0.9986 0.3360 0.0941 0.200 Uiso 1 1 calc R
C10 C 0.9350(5) 0.3681(5) 0.0801(9) 0.144(5) Uani 1 1 d .
H10A H 0.9235 0.3447 0.0411 0.173 Uiso 1 1 calc R
C11 C 0.7871(6) 0.3429(4) 0.1774(10) 0.144(5) Uani 1 1 d .
H11A H 0.8062 0.3541 0.2248 0.173 Uiso 1 1 calc R
C12 C 0.7535(6) 0.3107(6) 0.2032(12) 0.163(6) Uani 1 1 d .
H12A H 0.7510 0.3003 0.2641 0.196 Uiso 1 1 calc R
C13 C 0.7251(5) 0.2950(5) 0.1379(16) 0.162(7) Uani 1 1 d .
H13A H 0.7012 0.2739 0.1526 0.194 Uiso 1 1 calc R
C14 C 0.7309(3) 0.3101(4) 0.0473(13) 0.136(5) Uani 1 1 d .
H14A H 0.7113 0.2991 0.0004 0.163 Uiso 1 1 calc R
C15 C 0.7676(3) 0.3429(3) 0.0278(8) 0.097(3) Uani 1 1 d .
C16 C 0.7788(3) 0.3625(4) -0.0630(9) 0.106(3) Uani 1 1 d .
C17 C 0.7609(5) 0.3447(6) -0.1454(13) 0.160(6) Uani 1 1 d .
H17A H 0.7401 0.3193 -0.1454 0.192 Uiso 1 1 calc R
C18 C 0.7750(6) 0.3663(11) -0.2293(15) 0.214(12) Uani 1 1 d U
H18A H 0.7627 0.3557 -0.2852 0.257 Uiso 1 1 calc R
C19 C 0.8028(6) 0.3981(11) -0.2285(16) 0.215(12) Uani 1 1 d U
H19A H 0.8146 0.4094 -0.2844 0.258 Uiso 1 1 calc R
C20 C 0.8183(4) 0.4191(5) -0.1443(13) 0.148(5) Uani 1 1 d .
H20A H 0.8357 0.4469 -0.1461 0.178 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'
V V 0.3005 0.5294 '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'
As As 0.0499 2.0058 '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
O3 As1 O10 98.4(3) . .
O3 As1 O6 99.8(3) . .
O10 As1 O6 99.2(3) . .
O11 As2 O8 99.4(3) . .
O11 As2 O6 98.9(3) . .
O8 As2 O6 99.0(3) . .
O4 V1 O1 111.3(3) . .
O4 V1 O2 108.5(3) . .
O1 V1 O2 84.2(2) . .
O4 V1 O3 109.6(3) . 16_655
O1 V1 O3 138.8(2) . 16_655
O2 V1 O3 79.3(2) . 16_655
O4 V1 O11 112.2(3) . 16_655
O1 V1 O11 78.5(2) . 16_655
O2 V1 O11 139.2(2) . 16_655
O3 V1 O11 89.9(2) 16_655 16_655
O4 V1 V2 112.3(2) . .
O1 V1 V2 41.97(17) . .
O2 V1 V2 42.75(16) . .
O3 V1 V2 115.99(16) 16_655 .
O11 V1 V2 114.93(16) 16_655 .
O4 V1 V3 112.2(2) . .
O1 V1 V3 116.24(18) . .
O2 V1 V3 38.74(16) . .
O3 V1 V3 40.71(15) 16_655 .
O11 V1 V3 122.15(16) 16_655 .
V2 V1 V3 79.01(5) . .
O4 V1 V3 115.3(2) . 11_665
O1 V1 V3 38.24(17) . 11_665
O2 V1 V3 116.37(16) . 11_665
O3 V1 V3 122.18(18) 16_655 11_665
O11 V1 V3 40.49(15) 16_655 11_665
V2 V1 V3 78.07(5) . 11_665
V3 V1 V3 132.12(7) . 11_665
O5 V2 O1 108.5(3) . .
O5 V2 O2 110.5(3) . .
O1 V2 O2 83.8(2) . .
O5 V2 O10 106.7(3) . .
O1 V2 O10 88.8(2) . .
O2 V2 O10 142.6(2) . .
O5 V2 O8 108.9(3) . 6_554
O1 V2 O8 142.3(2) . 6_554
O2 V2 O8 87.4(2) . 6_554
O10 V2 O8 76.4(2) . 6_554
O5 V2 V1 111.7(3) . .
O1 V2 V1 41.82(15) . .
O2 V2 V1 42.47(17) . .
O10 V2 V1 124.43(18) . .
O8 V2 V1 123.68(18) 6_554 .
O9 V3 O2 110.0(3) . .
O9 V3 O1 109.8(3) . 16_655
O2 V3 O1 140.2(2) . 16_655
O9 V3 O3 106.4(3) . 16_655
O2 V3 O3 79.7(2) . 16_655
O1 V3 O3 89.8(2) 16_655 16_655
O9 V3 O11 107.6(3) . 6_554
O2 V3 O11 89.4(2) . 6_554
O1 V3 O11 78.2(2) 16_655 6_554
O3 V3 O11 146.0(2) 16_655 6_554
O9 V3 V1 111.1(2) . .
O2 V3 V1 38.74(17) . .
O1 V3 V1 122.79(17) 16_655 .
O3 V3 V1 41.15(15) 16_655 .
O11 V3 V1 123.08(17) 6_554 .
O9 V3 V1 111.2(2) . 16_655
O2 V3 V1 122.60(17) . 16_655
O1 V3 V1 37.66(15) 16_655 16_655
O3 V3 V1 122.90(18) 16_655 16_655
O11 V3 V1 40.75(17) 6_554 16_655
V1 V3 V1 137.68(7) . 16_655
O7 V4 O8 109.30(17) . .
O7 V4 O8 109.30(17) . 6_554
O8 V4 O8 141.4(3) . 6_554
O7 V4 O10 109.67(17) . 6_554
O8 V4 O10 77.4(2) . 6_554
O8 V4 O10 89.8(2) 6_554 6_554
O7 V4 O10 109.67(17) . .
O8 V4 O10 89.8(2) . .
O8 V4 O10 77.4(2) 6_554 .
O10 V4 O10 140.7(3) 6_554 .
N4 Cu1 N3 82.2(4) . .
N4 Cu1 N1 132.0(4) . .
N3 Cu1 N1 123.2(4) . .
N4 Cu1 N2 129.5(4) . .
N3 Cu1 N2 115.3(4) . .
N1 Cu1 N2 79.6(5) . .
V1 O1 V2 96.2(2) . .
V1 O1 V3 104.1(3) . 11_665
V2 O1 V3 148.4(3) . 11_665
V3 O2 V1 102.5(3) . .
V3 O2 V2 149.0(3) . .
V1 O2 V2 94.8(2) . .
As1 O3 V3 124.2(3) . 11_665
As1 O3 V1 137.4(3) . 11_665
V3 O3 V1 98.1(2) 11_665 11_665
As1 O6 As2 130.7(4) . .
As2 O8 V4 135.2(3) . .
As2 O8 V2 121.6(3) . 6_554
V4 O8 V2 102.9(3) . 6_554
As1 O10 V4 134.7(3) . .
As1 O10 V2 121.7(3) . .
V4 O10 V2 103.2(3) . .
As2 O11 V3 122.6(3) . 6_554
As2 O11 V1 138.5(3) . 11_665
V3 O11 V1 98.8(2) 6_554 11_665
C11 N3 C15 116.8(10) . .
C11 N3 Cu1 129.7(9) . .
C15 N3 Cu1 113.1(7) . .
C6 N2 C10 112.5(12) . .
C6 N2 Cu1 118.2(10) . .
C10 N2 Cu1 128.9(8) . .
C16 N4 C20 117.3(12) . .
C16 N4 Cu1 113.6(8) . .
C20 N4 Cu1 128.5(10) . .
C1 N1 C5 126.0(14) . .
C1 N1 Cu1 122.2(11) . .
C5 N1 Cu1 111.5(9) . .
N1 C1 C2 115.6(18) . .
C3 C2 C1 110(2) . .
C2 C3 C4 133(2) . .
C5 C4 C3 115.9(19) . .
C4 C5 N1 118.3(15) . .
C4 C5 C6 122.8(14) . .
N1 C5 C6 118.9(10) . .
N2 C6 C7 125.7(14) . .
N2 C6 C5 111.3(13) . .
C7 C6 C5 122.9(11) . .
C8 C7 C6 115.3(13) . .
C9 C8 C7 123.7(18) . .
C8 C9 C10 114.1(19) . .
N2 C10 C9 128.7(15) . .
N3 C11 C12 128.2(14) . .
C13 C12 C11 117.2(17) . .
C12 C13 C14 119.8(14) . .
C13 C14 C15 118.4(13) . .
N3 C15 C14 119.5(12) . .
N3 C15 C16 114.6(9) . .
C14 C15 C16 125.8(10) . .
N4 C16 C17 121.1(14) . .
N4 C16 C15 115.4(9) . .
C17 C16 C15 123.5(12) . .
C16 C17 C18 118.1(18) . .
C19 C18 C17 120(2) . .
C18 C19 C20 122(2) . .
N4 C20 C19 120.8(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O3 1.755(5) .
As1 O10 1.770(6) .
As1 O6 1.776(6) .
As2 O11 1.750(5) .
As2 O8 1.771(6) .
As2 O6 1.779(6) .
V1 O4 1.594(6) .
V1 O1 1.912(5) .
V1 O2 1.932(6) .
V1 O3 2.003(5) 16_655
V1 O11 2.005(6) 16_655
V1 V2 2.851(2) .
V1 V3 3.013(2) .
V1 V3 3.036(2) 11_665
V2 O5 1.585(7) .
V2 O1 1.918(6) .
V2 O2 1.942(5) .
V2 O10 1.998(6) .
V2 O8 2.009(6) 6_554
V3 O9 1.581(6) .
V3 O2 1.932(6) .
V3 O1 1.937(6) 16_655
V3 O3 1.985(5) 16_655
V3 O11 1.995(5) 6_554
V3 V1 3.036(2) 16_655
V4 O7 1.552(9) .
V4 O8 1.980(6) .
V4 O8 1.980(6) 6_554
V4 O10 1.986(6) 6_554
V4 O10 1.986(6) .
Cu1 N4 1.983(10) .
Cu1 N3 1.989(9) .
Cu1 N1 1.992(11) .
Cu1 N2 2.004(10) .
O1 V3 1.937(6) 11_665
O3 V3 1.985(5) 11_665
O3 V1 2.003(5) 11_665
O8 V2 2.009(6) 6_554
O11 V3 1.995(5) 6_554
O11 V1 2.005(6) 11_665
N3 C11 1.256(15) .
N3 C15 1.359(11) .
N2 C6 1.311(12) .
N2 C10 1.330(16) .
N4 C16 1.336(13) .
N4 C20 1.336(16) .
N1 C1 1.38(2) .
N1 C5 1.389(15) .
C1 C2 1.57(2) .
C2 C3 1.31(2) .
C3 C4 1.38(2) .
C4 C5 1.358(19) .
C5 C6 1.407(16) .
C6 C7 1.394(16) .
C7 C8 1.356(18) .
C8 C9 1.322(19) .
C9 C10 1.368(18) .
C11 C12 1.370(19) .
C12 C13 1.32(2) .
C13 C14 1.39(2) .
C14 C15 1.427(15) .
C15 C16 1.459(14) .
C16 C17 1.389(16) .
C17 C18 1.41(3) .
C18 C19 1.20(4) .
C19 C20 1.42(3) .
