#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:34:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179977 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/71/7027172.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_7027172
loop_
_publ_author_name
'Zheng, Li-Min'
'Zhao, Jie-Shou'
'Lii, Kwang-Hwa'
'Zhang, Li-Yi'
'Liu, Yang'
'Xin, Xin-Quan'
_publ_section_title
;
 One- and two-dimensional materials containing vanadium oxide: structures
 and magnetic properties of Cu(dien)V2O6·H2O and Ni(dien)V2O6
 (dien = diethylenetriamine) †
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              939
_journal_paper_doi               10.1039/a808839j
_journal_year                    1999
_chemical_formula_sum            'C4 H13 N3 Ni O6 V2'
_chemical_formula_weight         359.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                101.8070(10)
_cell_angle_beta                 102.8010(10)
_cell_angle_gamma                98.8310(10)
_cell_formula_units_Z            2
_cell_length_a                   7.37700(10)
_cell_length_b                   8.09300(10)
_cell_length_c                   10.23500(10)
_cell_measurement_reflns_used    4094
_cell_measurement_temperature    293(2)
_cell_volume                     570.458(13)
_computing_cell_refinement       'SMART (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens Smart-CCD diffractometer'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5431
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_description       trunk
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0075(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_obs          0.0290
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0376P)²+0.3103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0748
_refine_ls_wR_factor_obs         0.0696
_reflns_number_observed          2104
_reflns_number_total             2460
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808839jsup1.cif
_cod_data_source_block           niv
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.3103P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.3103P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        570.458(12)
_cod_database_code               7027172
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
Ni Ni 0.41875(5) -0.63763(4) 0.35591(3) 0.01584(12) Uani 1 d
V1 V 0.81682(6) -0.85029(6) 0.38879(5) 0.02016(14) Uani 1 d
V2 V 0.73513(6) -1.25950(6) 0.37905(5) 0.01742(13) Uani 1 d
O1 O 0.6774(3) -0.7110(3) 0.3877(2) 0.0274(5) Uani 1 d
O2 O 0.6849(3) -1.0475(3) 0.4055(3) 0.0350(5) Uani 1 d
O3 O 0.8792(3) -0.8850(3) 0.2454(3) 0.0395(6) Uani 1 d
O4 O 0.9765(3) -1.2387(3) 0.4693(3) 0.0376(6) Uani 1 d
O5 O 0.5805(3) -1.3839(2) 0.4371(2) 0.0179(4) Uani 1 d
O6 O 0.7062(4) -1.3418(3) 0.2177(2) 0.0401(6) Uani 1 d
N1 N 0.1761(4) -0.5381(4) 0.3173(3) 0.0234(5) Uani 1 d
N2 N 0.3979(4) -0.6488(3) 0.1490(3) 0.0255(5) Uani 1 d
N3 N 0.2973(4) -0.9023(3) 0.2812(3) 0.0262(5) Uani 1 d
C1 C 0.1837(5) -0.4570(5) 0.2025(4) 0.0352(8) Uani 1 d
C2 C 0.2308(6) -0.5824(7) 0.0911(4) 0.0456(10) Uani 1 d
C3 C 0.3978(6) -0.8276(5) 0.0817(4) 0.0386(8) Uani 1 d
C4 C 0.2668(6) -0.9514(5) 0.1301(4) 0.0452(9) Uani 1 d
H12 H 0.0630(54) -0.4218(48) 0.1638(39) 0.039(10) Uiso 1 d
H1B H 0.1729(49) -0.4665(47) 0.3851(38) 0.026(9) Uiso 1 d
H2A H 0.4921(51) -0.5839(46) 0.1505(36) 0.025(9) Uiso 1 d
H3B H 0.3727(59) -0.9607(53) 0.3213(43) 0.046(12) Uiso 1 d
H32 H 0.5284(57) -0.8414(49) 0.1062(40) 0.041(10) Uiso 1 d
H42 H 0.2799(54) -1.0584(54) 0.0956(41) 0.043(11) Uiso 1 d
H22 H 0.2497(60) -0.5350(56) 0.0163(47) 0.052(12) Uiso 1 d
H3A H 0.2003(56) -0.9259(48) 0.3037(39) 0.033(10) Uiso 1 d
H21 H 0.1170(74) -0.6769(66) 0.0526(52) 0.070(15) Uiso 1 d
H11 H 0.2977(60) -0.3532(55) 0.2360(44) 0.050(12) Uiso 1 d
H41 H 0.1280(82) -0.9511(72) 0.0783(59) 0.097(19) Uiso 1 d
H1A H 0.0596(72) -0.6192(63) 0.2901(51) 0.071(15) Uiso 1 d
H31 H 0.3562(53) -0.8496(49) -0.0150(41) 0.039(10) Uiso 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'
Ni Ni 0.3393 1.1124 '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
O1 Ni N1 172.86(10) . .
O1 Ni N2 93.49(9) . .
N1 Ni N2 82.99(10) . .
O1 Ni O5 91.39(8) . 2_636
N1 Ni O5 92.06(9) . 2_636
N2 Ni O5 175.04(8) . 2_636
O1 Ni N3 86.08(10) . .
N1 Ni N3 99.63(11) . .
N2 Ni N3 83.42(11) . .
O5 Ni N3 97.78(9) 2_636 .
O1 Ni O5 85.23(8) . 1_565
N1 Ni O5 89.07(9) . 1_565
N2 Ni O5 97.52(9) . 1_565
O5 Ni O5 82.02(8) 2_636 1_565
N3 Ni O5 171.29(9) . 1_565
O3 V1 O1 109.69(12) . .
O3 V1 O4 109.57(12) . 2_736
O1 V1 O4 108.31(11) . 2_736
O3 V1 O2 109.76(12) . .
O1 V1 O2 107.61(10) . .
O4 V1 O2 111.86(11) 2_736 .
O6 V2 O5 108.64(11) . .
O6 V2 O4 109.50(13) . .
O5 V2 O4 113.06(10) . .
O6 V2 O2 110.38(13) . .
O5 V2 O2 107.99(10) . .
O4 V2 O2 107.25(11) . .
V1 O1 Ni 154.79(13) . .
V2 O2 V1 129.92(13) . .
V2 O4 V1 154.2(2) . 2_736
V2 O5 Ni 125.65(10) . 2_636
V2 O5 Ni 132.65(10) . 1_545
Ni O5 Ni 97.98(8) 2_636 1_545
C1 N1 Ni 106.3(2) . .
C3 N2 C2 115.5(3) . .
C3 N2 Ni 107.0(2) . .
C2 N2 Ni 109.4(2) . .
C4 N3 Ni 109.3(2) . .
N1 C1 C2 108.0(3) . .
N2 C2 C1 110.7(3) . .
N2 C3 C4 109.8(3) . .
N3 C4 C3 111.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni O1 2.062(2) .
Ni N1 2.066(2) .
Ni N2 2.071(3) .
Ni O5 2.088(2) 2_636
Ni N3 2.101(3) .
Ni O5 2.108(2) 1_565
V1 O3 1.617(2) .
V1 O1 1.639(2) .
V1 O4 1.791(2) 2_736
V1 O2 1.798(2) .
V2 O6 1.602(2) .
V2 O5 1.692(2) .
V2 O4 1.780(2) .
V2 O2 1.790(2) .
O4 V1 1.791(2) 2_736
O5 Ni 2.088(2) 2_636
O5 Ni 2.108(2) 1_545
N1 C1 1.466(4) .
N2 C3 1.469(4) .
N2 C2 1.473(4) .
N3 C4 1.472(5) .
C1 C2 1.503(5) .
C3 C4 1.517(6) .
