#------------------------------------------------------------------------------
#$Date: 2016-03-23 19:51:03 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179427 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332498.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_4332498
loop_
_publ_author_name
'Yan, Bangbo'
'Luo, Junhua'
'Dube, Paul'
'Sefat, Athena S.'
'Greedan, John E.'
'Maggard, Paul A.'
_publ_section_title
;
 Spin-Gap Formation and Thermal Structural Studies in Reduced Hybrid
 Layered Vanadates
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5109
_journal_page_last               5118
_journal_paper_doi               10.1021/ic0604563
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C4 H4 N2 Ni O10 V4'
_chemical_formula_weight         502.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                   14.2372(4)
_cell_length_b                   6.9008(2)
_cell_length_c                   11.5102(3)
_cell_measurement_reflns_used    6465
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      32.14
_cell_measurement_theta_min      2.86
_cell_volume                     1130.85(5)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16407
_diffrn_reflns_theta_full        33.54
_diffrn_reflns_theta_max         33.54
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    4.875
_exptl_absorpt_correction_T_max  0.7586
_exptl_absorpt_correction_T_min  0.3875
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            lustrous
_exptl_crystal_density_diffrn    2.952
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       long
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0206
_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)+(0.0350P)²+1.9239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                1025
_reflns_number_total             1120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604563sup2.cif
_cod_data_source_block           NiPyzV4O10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Cmcm
_cod_database_code               4332498
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+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
Ni1 Ni 0.5000 0.31609(5) 0.7500 0.00685(9) Uani 1 4 d S
V1 V 0.288779(17) 0.36349(3) 0.60384(2) 0.00792(9) Uani 1 1 d .
O1 O 0.40026(7) 0.31578(16) 0.62390(9) 0.0114(2) Uani 1 1 d .
O2 O 0.22372(9) 0.13096(14) 0.57004(10) 0.0126(2) Uani 1 1 d .
O3 O 0.24251(11) 0.3843(2) 0.7500 0.0114(3) Uani 1 2 d S
N1 N 0.5000 0.6152(3) 0.7500 0.0101(4) Uani 1 4 d S
N2 N 0.5000 0.0178(4) 0.7500 0.0096(4) Uani 1 4 d S
C1 C 0.5000 0.7157(3) 0.8484(2) 0.0296(7) Uani 1 2 d S
H1 H 0.5000 0.6557 0.9199 0.044 Uiso 1 2 d SR
H2 H 0.5000 -0.0199 0.5835 0.044 Uiso 1 2 d SR
C2 C 0.5000 -0.0836(4) 0.6532(2) 0.0387(9) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.00698(16) 0.00600(16) 0.00757(16) 0.000 0.000 0.000
V1 0.00889(13) 0.00654(14) 0.00833(13) 0.00074(7) -0.00280(8) -0.00017(7)
O1 0.0102(5) 0.0134(5) 0.0107(5) 0.0002(4) -0.0024(4) 0.0013(4)
O2 0.0217(6) 0.0086(5) 0.0075(5) 0.0020(3) -0.0040(4) -0.0052(4)
O3 0.0128(7) 0.0112(7) 0.0103(7) 0.000 0.000 -0.0013(5)
N1 0.0099(11) 0.0085(10) 0.0118(11) 0.000 0.000 0.000
N2 0.0122(11) 0.0080(10) 0.0087(10) 0.000 0.000 0.000
C1 0.070(2) 0.0080(9) 0.0108(9) 0.0015(8) 0.000 0.000
C2 0.098(3) 0.0092(10) 0.0091(9) 0.0030(8) 0.000 0.000
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 Ni1 O1 91.25(6) 3_656 12_655
O1 Ni1 O1 179.88(6) 3_656 .
O1 Ni1 O1 88.75(6) 12_655 .
O1 Ni1 O1 88.75(6) 3_656 10_557
O1 Ni1 O1 179.88(7) 12_655 10_557
O1 Ni1 O1 91.25(6) . 10_557
O1 Ni1 N2 89.94(3) 3_656 .
O1 Ni1 N2 89.94(3) 12_655 .
O1 Ni1 N2 89.94(3) . .
O1 Ni1 N2 89.94(3) 10_557 .
O1 Ni1 N1 90.06(3) 3_656 .
O1 Ni1 N1 90.06(3) 12_655 .
O1 Ni1 N1 90.06(3) . .
O1 Ni1 N1 90.06(3) 10_557 .
N2 Ni1 N1 180.000(1) . .
O1 V1 O3 103.73(6) . .
O1 V1 O2 109.44(5) . .
O3 V1 O2 94.59(6) . .
O1 V1 O2 108.42(6) . 16
O3 V1 O2 94.55(6) . 16
O2 V1 O2 137.52(4) . 16
O1 V1 O2 103.30(5) . 13_556
O3 V1 O2 152.96(6) . 13_556
O2 V1 O2 76.59(5) . 13_556
O2 V1 O2 76.62(5) 16 13_556
O1 V1 V1 103.60(4) . 4_566
O3 V1 V1 132.84(5) . 4_566
O2 V1 V1 111.30(4) . 4_566
O2 V1 V1 40.16(4) 16 4_566
O2 V1 V1 37.44(3) 13_556 4_566
O1 V1 V1 110.89(4) . 13_556
O3 V1 V1 129.33(5) . 13_556
O2 V1 V1 39.65(4) . 13_556
O2 V1 V1 107.69(4) 16 13_556
O2 V1 V1 36.95(3) 13_556 13_556
V1 V1 V1 72.763(11) 4_566 13_556
V1 O1 Ni1 141.12(7) . .
V1 O2 V1 146.04(7) . 16_545
V1 O2 V1 103.41(5) . 13_556
V1 O2 V1 102.40(5) 16_545 13_556
V1 O3 V1 136.32(9) 10_557 .
C1 N1 C1 117.0(3) . 10_557
C1 N1 Ni1 121.48(14) . .
C1 N1 Ni1 121.48(14) 10_557 .
C2 N2 C2 115.7(3) 10_557 .
C2 N2 Ni1 122.14(14) 10_557 .
C2 N2 Ni1 122.14(14) . .
N1 C1 C2 120.7(2) . 10_567
N2 C2 C1 122.9(2) . 10_547
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0306(11) 3_656
Ni1 O1 2.0306(11) 12_655
Ni1 O1 2.0306(11) .
Ni1 O1 2.0306(11) 10_557
Ni1 N2 2.058(2) .
Ni1 N1 2.064(2) .
V1 O1 1.6373(11) .
V1 O3 1.8124(6) .
V1 O2 1.8931(10) .
V1 O2 1.8948(10) 16
V1 O2 2.0096(12) 13_556
V1 V1 3.0438(5) 4_566
V1 V1 3.0638(5) 13_556
O2 V1 1.8947(10) 16_545
O2 V1 2.0097(12) 13_556
O3 V1 1.8124(6) 10_557
N1 C1 1.328(3) .
N1 C1 1.328(3) 10_557
N2 C2 1.316(3) 10_557
N2 C2 1.316(3) .
C1 C2 1.385(3) 10_567
C2 C1 1.385(3) 10_547
