#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:29:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179113 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/75/4307564.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_4307564
loop_
_publ_author_name
'David W. Aldous'
'Nicholas F. Stephens'
'Philip Lightfoot'
_publ_contact_author_address
;
School of Chemistry
University of St Andrews
St Andrews
Fife
KY16 9ST
UNITED KINGDOM
;
_publ_contact_author_email       PL@ST-ANDREWS.AC.UK
_publ_contact_author_name        'Dr Philip Lightfoot'
_publ_section_title
;
Hydrothermal Vanadium Fluoride Chemistry: Four New V3+ Chain Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3996
_journal_page_last               4001
_journal_paper_doi               10.1021/ic062061p
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C2 H10 F5 N2 V'
_chemical_formula_weight         208.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :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            8
_cell_length_a                   12.837(2)
_cell_length_b                   12.837(2)
_cell_length_c                   7.9502(17)
_cell_measurement_temperature    93(2)
_cell_volume                     1310.1(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6977
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            Green/yellow
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.1000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0309P)²+2.2890P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                583
_reflns_number_total             593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062061p-file001_3.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4307564
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, -z+1/2'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'-y, -x, -z+1/2'
'-x, -y, -z'
'-x-1/2, y, z-1/2'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -z'
'y, x, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.2500 0.7500 0.2500 0.0057(3) Uani 1 4 d S . .
V2 V 0.7500 0.7500 0.23567(8) 0.0057(3) Uani 1 4 d S . .
F1 F 0.25061(10) 0.89865(10) 0.24905(15) 0.0144(4) Uani 1 1 d . . .
F2 F 0.2500 0.7500 0.0000 0.0222(8) Uani 1 4 d S . .
F3 F 0.7500 0.7500 -0.0164(3) 0.0165(7) Uani 1 4 d S . .
F4 F 0.62236(10) 0.82637(10) 0.22968(15) 0.0133(4) Uani 1 1 d . . .
N1 N 0.14639(16) 1.00601(13) 0.4795(2) 0.0121(4) Uani 1 1 d . . .
H1 H 0.1953 0.9551 0.4692 0.018 Uiso 1 1 calc R . .
H2 H 0.1592 1.0439 0.5739 0.018 Uiso 1 1 calc R . .
H3 H 0.1490 1.0484 0.3879 0.018 Uiso 1 1 calc R . .
C1 C 0.04119(17) 0.95786(17) 0.4915(3) 0.0111(5) Uani 1 1 d . . .
H4 H 0.0384 0.9110 0.5904 0.013 Uiso 1 1 calc R . .
H5 H 0.0274 0.9158 0.3896 0.013 Uiso 1 1 calc R . .
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
V1 0.0055(3) 0.0055(3) 0.0061(4) 0.000 0.000 0.0001(2)
V2 0.0056(3) 0.0056(3) 0.0059(4) 0.000 0.000 0.000
F1 0.0179(7) 0.0076(6) 0.0176(7) 0.0004(5) 0.0047(5) 0.0005(5)
F2 0.0302(12) 0.0302(12) 0.0060(14) 0.000 0.000 0.000
F3 0.0219(10) 0.0219(10) 0.0056(13) 0.000 0.000 0.000
F4 0.0098(7) 0.0160(7) 0.0141(6) 0.0037(5) 0.0026(5) 0.0045(5)
N1 0.0111(10) 0.0158(10) 0.0094(9) -0.0005(7) 0.0010(7) -0.0006(7)
C1 0.0115(11) 0.0103(11) 0.0115(11) -0.0005(8) 0.0012(8) 0.0007(10)
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
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
_geom_angle_publ_flag
F1 V1 F1 179.55(7) 8_665 5_455 ?
F1 V1 F1 89.53(7) 8_665 3_565 ?
F1 V1 F1 90.47(7) 5_455 3_565 ?
F1 V1 F1 90.47(7) 8_665 . ?
F1 V1 F1 89.53(7) 5_455 . ?
F1 V1 F1 179.55(7) 3_565 . ?
F1 V1 F2 89.77(4) 8_665 10_656 ?
F1 V1 F2 89.77(4) 5_455 10_656 ?
F1 V1 F2 90.23(4) 3_565 10_656 ?
F1 V1 F2 90.23(4) . 10_656 ?
F1 V1 F2 90.23(4) 8_665 . ?
F1 V1 F2 90.23(4) 5_455 . ?
F1 V1 F2 89.77(4) 3_565 . ?
F1 V1 F2 89.77(4) . . ?
F2 V1 F2 180.0 10_656 . ?
F4 V2 F4 89.964(2) 7_655 . ?
F4 V2 F4 177.14(8) 7_655 6_565 ?
F4 V2 F4 89.964(2) . 6_565 ?
F4 V2 F4 89.964(2) 7_655 3_665 ?
F4 V2 F4 177.14(8) . 3_665 ?
F4 V2 F4 89.964(2) 6_565 3_665 ?
F4 V2 F3 91.43(4) 7_655 10_756 ?
F4 V2 F3 91.43(4) . 10_756 ?
F4 V2 F3 91.43(4) 6_565 10_756 ?
F4 V2 F3 91.43(4) 3_665 10_756 ?
F4 V2 F3 88.57(4) 7_655 . ?
F4 V2 F3 88.57(4) . . ?
F4 V2 F3 88.57(4) 6_565 . ?
F4 V2 F3 88.57(4) 3_665 . ?
F3 V2 F3 180.000(1) 10_756 . ?
V1 F2 V1 180.0 10_655 . ?
V2 F3 V2 180.000(1) 10_755 . ?
C1 N1 H1 109.5 . . ?
C1 N1 H2 109.5 . . ?
H1 N1 H2 109.5 . . ?
C1 N1 H3 109.5 . . ?
H1 N1 H3 109.5 . . ?
H2 N1 H3 109.5 . . ?
N1 C1 C1 110.0(2) . 9_576 ?
N1 C1 H4 109.7 . . ?
C1 C1 H4 109.7 9_576 . ?
N1 C1 H5 109.7 . . ?
C1 C1 H5 109.7 9_576 . ?
H4 C1 H5 108.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 F1 1.9082(13) 8_665 ?
V1 F1 1.9082(13) 5_455 ?
V1 F1 1.9082(13) 3_565 ?
V1 F1 1.9082(13) . ?
V1 F2 1.9876(4) 10_656 ?
V1 F2 1.9876(4) . ?
V2 F4 1.9101(13) 7_655 ?
V2 F4 1.9101(13) . ?
V2 F4 1.9101(13) 6_565 ?
V2 F4 1.9101(13) 3_665 ?
V2 F3 1.971(3) 10_756 ?
V2 F3 2.004(3) . ?
F2 V1 1.9876(4) 10_655 ?
F3 V2 1.971(3) 10_755 ?
N1 C1 1.488(3) . ?
N1 H1 0.9100 . ?
N1 H2 0.9100 . ?
N1 H3 0.9100 . ?
C1 C1 1.519(4) 9_576 ?
C1 H4 0.9900 . ?
C1 H5 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 F1 0.91 2.02 2.654(2) 125.2 .
N1 H2 F4 0.91 1.87 2.775(2) 175.3 14_666
N1 H3 F4 0.91 1.89 2.737(2) 153.9 2_475
