#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:46:23 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179989 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/83/7028316.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_7028316
loop_
_publ_author_name
'Hou, Wentao'
'Guo, Jiuyu'
'Xu, Xiao'
'Wang, Zuoxiang'
'Zhang, Deng'
'Wan, Hongxiang'
'Song, You'
'Zhu, Dunru'
'Xu, Yan'
_publ_section_title
;
 Syntheses, structures and properties of two 2-D layered hybrid
 organic-inorganic materials based on different V4O12 building units.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              865
_journal_page_last               871
_journal_paper_doi               10.1039/c3dt52195h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C16 H14 N6 O12 V4 Zn2'
_chemical_formula_weight         816.83
_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                92.394(7)
_cell_angle_beta                 105.807(7)
_cell_angle_gamma                112.067(7)
_cell_formula_units_Z            2
_cell_length_a                   8.466(5)
_cell_length_b                   10.357(6)
_cell_length_c                   15.391(8)
_cell_measurement_reflns_used    1542
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.325
_cell_measurement_theta_min      2.712
_cell_volume                     1187.5(12)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω 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  0.0427
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8794
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    3.574
_exptl_absorpt_correction_T_max  0.6737
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            lightyellow
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4323
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0083P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                1792
_reflns_number_total             4323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52195h.txt
_cod_data_source_block           hwt-7
_cod_original_cell_volume        1187.6(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028316
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
Zn1 Zn 0.74838(5) 0.26632(4) 0.20214(3) 0.01919(14) Uani 1 1 d .
Zn2 Zn 1.25133(6) 0.73344(4) 0.29811(3) 0.01794(14) Uani 1 1 d .
V1 V 0.91681(7) 0.55001(6) 0.39351(4) 0.01512(19) Uani 1 1 d .
V2 V 1.08443(8) 0.45081(6) 0.10671(5) 0.0162(2) Uani 1 1 d .
V3 V 0.51822(7) 0.54644(6) 0.39356(4) 0.0203(2) Uani 1 1 d .
V4 V 1.48091(9) 0.45261(7) 0.10683(5) 0.0212(2) Uani 1 1 d .
N1 N 0.8848(3) 0.1553(3) 0.2917(2) 0.0202(9) Uani 1 1 d U
N2 N 0.5781(3) 0.0583(3) 0.15416(19) 0.0171(10) Uani 1 1 d U
N3 N 0.5225(4) -0.1671(3) 0.1513(2) 0.0273(10) Uani 1 1 d U
H3B H 0.5298 -0.2452 0.1638 0.033 Uiso 1 1 calc R
N4 N 1.1172(4) 0.8470(3) 0.2065(2) 0.0196(9) Uani 1 1 d U
N5 N 1.4211(4) 0.9403(3) 0.3465(2) 0.0255(11) Uani 1 1 d U
N6 N 1.4727(4) 1.1647(3) 0.3471(2) 0.0309(10) Uani 1 1 d U
H6A H 1.4560 1.2377 0.3296 0.037 Uiso 1 1 calc R
C1 C 1.0318(5) 0.2086(4) 0.3624(3) 0.0279(12) Uani 1 1 d U
H1A H 1.0927 0.3061 0.3784 0.033 Uiso 1 1 calc R
C2 C 1.0977(5) 0.1221(4) 0.4134(3) 0.0446(15) Uani 1 1 d U
H2A H 1.1995 0.1640 0.4642 0.054 Uiso 1 1 calc R
C3 C 1.0245(5) -0.0133(4) 0.3937(3) 0.0351(10) Uani 1 1 d U
H3A H 1.0771 -0.0681 0.4263 0.042 Uiso 1 1 calc R
C4 C 0.8584(4) -0.0780(4) 0.3195(2) 0.0250(10) Uani 1 1 d U
H4A H 0.7945 -0.1754 0.3046 0.030 Uiso 1 1 calc R
C5 C 0.8018(4) 0.0138(3) 0.2727(2) 0.0168(9) Uani 1 1 d U
C6 C 0.6380(4) -0.0355(3) 0.1951(3) 0.0218(10) Uani 1 1 d U
C7 C 0.4249(5) -0.0131(4) 0.0845(3) 0.0271(13) Uani 1 1 d U
H7A H 0.3583 0.0281 0.0463 0.033 Uiso 1 1 calc R
C8 C 0.3843(5) -0.1500(4) 0.0792(3) 0.0335(11) Uani 1 1 d U
H8A H 0.2858 -0.2217 0.0372 0.040 Uiso 1 1 calc R
C9 C 0.9671(5) 0.7950(4) 0.1351(3) 0.0299(12) Uani 1 1 d U
H9A H 0.9081 0.6973 0.1200 0.036 Uiso 1 1 calc R
C10 C 0.8941(5) 0.8728(4) 0.0832(3) 0.0326(12) Uani 1 1 d U
H10A H 0.7882 0.8326 0.0346 0.039 Uiso 1 1 calc R
C11 C 0.9946(5) 1.0235(4) 0.1095(3) 0.0308(11) Uani 1 1 d U
H11A H 0.9548 1.0843 0.0762 0.037 Uiso 1 1 calc R
C12 C 1.1412(5) 1.0756(4) 0.1798(3) 0.0220(10) Uani 1 1 d U
H12A H 1.2024 1.1731 0.1958 0.026 Uiso 1 1 calc R
C13 C 1.2080(5) 0.9893(4) 0.2311(3) 0.0218(10) Uani 1 1 d U
C14 C 1.3677(5) 1.0309(4) 0.3083(3) 0.0167(10) Uani 1 1 d U
C15 C 1.5787(5) 1.0236(4) 0.4166(3) 0.0322(15) Uani 1 1 d U
H15A H 1.6533 0.9904 0.4567 0.039 Uiso 1 1 calc R
C16 C 1.6051(5) 1.1669(4) 0.4162(3) 0.0241(10) Uani 1 1 d U
H16A H 1.6966 1.2454 0.4562 0.029 Uiso 1 1 calc R
O1 O 0.5000 0.5000 0.5000 0.0620(19) Uani 1 2 d S
O2 O 1.5000 0.5000 0.0000 0.067(2) Uani 1 2 d S
O3 O 1.5938(3) 0.5932(2) 0.1808(2) 0.0424(11) Uani 1 1 d .
O4 O 0.4056(4) 0.4074(3) 0.3152(2) 0.0367(11) Uani 1 1 d .
O5 O 1.4440(3) 0.6688(2) 0.36600(19) 0.0348(10) Uani 1 1 d U
O6 O 0.5600(3) 0.3302(3) 0.1293(2) 0.0329(10) Uani 1 1 d .
O7 O 1.0000 0.5000 0.5000 0.0298(13) Uani 1 2 d SU
O8 O 1.0000 0.5000 0.0000 0.0304(14) Uani 1 2 d S
O9 O 0.9196(3) 0.3251(2) 0.12880(17) 0.0274(8) Uani 1 1 d U
O10 O 1.0841(3) 0.6760(3) 0.37085(19) 0.0248(9) Uani 1 1 d .
O11 O 1.1756(3) 0.5886(2) 0.18666(17) 0.0313(9) Uani 1 1 d .
O12 O 0.8271(3) 0.4114(3) 0.31311(19) 0.0276(10) Uani 1 1 d .
O13 O 0.7524(3) 0.6133(2) 0.40237(17) 0.0235(8) Uani 1 1 d .
O14 O 1.2424(3) 0.3864(3) 0.09589(19) 0.0253(9) Uani 1 1 d .
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'
Zn Zn 0.2839 1.4301 '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
O9 Zn1 O12 111.22(11) . .
O9 Zn1 O6 98.84(13) . .
O12 Zn1 O6 93.95(12) . .
O9 Zn1 N2 108.36(11) . .
O12 Zn1 N2 138.77(12) . .
O6 Zn1 N2 91.00(11) . .
O9 Zn1 N1 96.50(12) . .
O12 Zn1 N1 86.87(12) . .
O6 Zn1 N1 163.18(11) . .
N2 Zn1 N1 77.60(11) . .
O10 Zn2 O11 112.12(11) . .
O10 Zn2 O5 101.03(13) . .
O11 Zn2 O5 91.58(11) . .
O10 Zn2 N5 108.01(14) . .
O11 Zn2 N5 138.44(14) . .
O5 Zn2 N5 91.03(12) . .
O10 Zn2 N4 97.68(13) . .
O11 Zn2 N4 86.87(12) . .
O5 Zn2 N4 160.35(12) . .
N5 Zn2 N4 77.44(13) . .
O12 V1 O10 109.97(15) . .
O12 V1 O7 108.78(11) . .
O10 V1 O7 109.44(10) . .
O12 V1 O13 110.36(13) . .
O10 V1 O13 110.08(14) . .
O7 V1 O13 108.17(9) . .
O11 V2 O9 110.79(14) . .
O11 V2 O14 110.96(13) . .
O9 V2 O14 109.11(14) . .
O11 V2 O8 109.19(11) . .
O9 V2 O8 109.22(9) . .
O14 V2 O8 107.49(11) . .
O4 V3 O5 109.30(15) . 1_455
O4 V3 O1 109.29(12) . .
O5 V3 O1 112.07(12) 1_455 .
O4 V3 O13 110.04(15) . .
O5 V3 O13 108.78(12) 1_455 .
O1 V3 O13 107.32(9) . .
O3 V4 O6 111.84(15) . 1_655
O3 V4 O2 106.75(12) . .
O6 V4 O2 108.76(13) 1_655 .
O3 V4 O14 111.21(15) . .
O6 V4 O14 111.56(13) 1_655 .
O2 V4 O14 106.42(10) . .
C1 N1 C5 116.5(3) . .
C1 N1 Zn1 128.8(2) . .
C5 N1 Zn1 114.6(2) . .
C7 N2 C6 109.1(3) . .
C7 N2 Zn1 136.1(3) . .
C6 N2 Zn1 114.51(19) . .
C6 N3 C8 106.3(3) . .
C6 N3 H3B 126.9 . .
C8 N3 H3B 126.9 . .
C9 N4 C13 119.3(4) . .
C9 N4 Zn2 129.4(3) . .
C13 N4 Zn2 111.3(2) . .
C14 N5 C15 103.7(3) . .
C14 N5 Zn2 115.4(2) . .
C15 N5 Zn2 140.6(3) . .
C16 N6 C14 108.9(4) . .
C16 N6 H6A 125.5 . .
C14 N6 H6A 125.5 . .
N1 C1 C2 121.3(3) . .
N1 C1 H1A 119.4 . .
C2 C1 H1A 119.4 . .
C3 C2 C1 122.9(4) . .
C3 C2 H2A 118.5 . .
C1 C2 H2A 118.5 . .
C2 C3 C4 118.2(4) . .
C2 C3 H3A 120.9 . .
C4 C3 H3A 120.9 . .
C5 C4 C3 115.2(3) . .
C5 C4 H4A 122.4 . .
C3 C4 H4A 122.4 . .
N1 C5 C4 125.6(3) . .
N1 C5 C6 112.7(3) . .
C4 C5 C6 121.7(3) . .
N3 C6 N2 108.3(3) . .
N3 C6 C5 131.4(3) . .
N2 C6 C5 120.3(3) . .
C8 C7 N2 109.6(4) . .
C8 C7 H7A 125.2 . .
N2 C7 H7A 125.2 . .
C7 C8 N3 106.8(3) . .
C7 C8 H8A 126.6 . .
N3 C8 H8A 126.6 . .
N4 C9 C10 125.4(4) . .
N4 C9 H9A 117.3 . .
C10 C9 H9A 117.3 . .
C9 C10 C11 114.3(4) . .
C9 C10 H10A 122.8 . .
C11 C10 H10A 122.8 . .
C12 C11 C10 120.8(4) . .
C12 C11 H11A 119.6 . .
C10 C11 H11A 119.6 . .
C11 C12 C13 121.9(4) . .
C11 C12 H12A 119.0 . .
C13 C12 H12A 119.0 . .
N4 C13 C12 118.3(3) . .
N4 C13 C14 113.6(4) . .
C12 C13 C14 128.1(3) . .
N5 C14 N6 114.0(3) . .
N5 C14 C13 122.1(3) . .
N6 C14 C13 123.9(4) . .
N5 C15 C16 108.4(4) . .
N5 C15 H15A 125.8 . .
C16 C15 H15A 125.8 . .
N6 C16 C15 105.0(3) . .
N6 C16 H16A 127.5 . .
C15 C16 H16A 127.5 . .
V3 O1 V3 180.000(1) . 2_666
V4 O2 V4 180.00(4) . 2_865
V3 O5 Zn2 152.25(13) 1_655 .
V4 O6 Zn1 151.19(15) 1_455 .
V1 O7 V1 180.0 2_766 .
V2 O8 V2 180.0 . 2_765
V2 O9 Zn1 148.41(16) . .
V1 O10 Zn2 148.73(17) . .
V2 O11 Zn2 167.89(17) . .
V1 O12 Zn1 168.84(18) . .
V1 O13 V3 139.68(14) . .
V2 O14 V4 139.26(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O9 2.008(3) .
Zn1 O12 2.008(3) .
Zn1 O6 2.030(3) .
Zn1 N2 2.054(3) .
Zn1 N1 2.195(3) .
Zn2 O10 1.975(3) .
Zn2 O11 2.017(3) .
Zn2 O5 2.037(3) .
Zn2 N5 2.044(3) .
Zn2 N4 2.221(3) .
V1 O12 1.640(3) .
V1 O10 1.658(3) .
V1 O7 1.7795(10) .
V1 O13 1.780(3) .
V2 O11 1.629(2) .
V2 O9 1.640(2) .
V2 O14 1.745(3) .
V2 O8 1.7810(10) .
V3 O4 1.622(3) .
V3 O5 1.637(3) 1_455
V3 O1 1.7569(11) .
V3 O13 1.801(3) .
V4 O3 1.598(3) .
V4 O6 1.650(3) 1_655
V4 O2 1.7672(12) .
V4 O14 1.828(3) .
N1 C1 1.317(4) .
N1 C5 1.343(4) .
N2 C7 1.354(4) .
N2 C6 1.359(5) .
N3 C6 1.353(4) .
N3 C8 1.448(5) .
N3 H3B 0.8600 .
N4 C9 1.337(5) .
N4 C13 1.360(5) .
N5 C14 1.285(5) .
N5 C15 1.401(5) .
N6 C16 1.311(5) .
N6 C14 1.335(4) .
N6 H6A 0.8600 .
C1 C2 1.388(6) .
C1 H1A 0.9300 .
C2 C3 1.285(5) .
C2 H2A 0.9300 .
C3 C4 1.444(5) .
C3 H3A 0.9300 .
C4 C5 1.366(5) .
C4 H4A 0.9300 .
C5 C6 1.458(4) .
C7 C8 1.321(5) .
C7 H7A 0.9300 .
C8 H8A 0.9300 .
C9 C10 1.353(7) .
C9 H9A 0.9300 .
C10 C11 1.444(5) .
C10 H10A 0.9300 .
C11 C12 1.311(5) .
C11 H11A 0.9300 .
C12 C13 1.392(6) .
C12 H12A 0.9300 .
C13 C14 1.440(5) .
C15 C16 1.416(6) .
C15 H15A 0.9300 .
C16 H16A 0.9300 .
O1 V3 1.7569(11) 2_666
O2 V4 1.7672(12) 2_865
O5 V3 1.637(3) 1_655
O6 V4 1.650(3) 1_455
O7 V1 1.7795(10) 2_766
O8 V2 1.7810(10) 2_765
