#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:29:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179113 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/75/4307562.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_4307562
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_moiety         'C10 H8 F3 N2 V'
_chemical_formula_sum            'C10 H8 F3 N2 V'
_chemical_formula_weight         264.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 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            2
_cell_length_a                   3.797(4)
_cell_length_b                   10.769(7)
_cell_length_c                   11.312(6)
_cell_measurement_reflns_used    3009
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.6
_cell_volume                     462.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART 1K CCD Diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'SRS Daresbury Laboratories'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6709
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3009
_diffrn_reflns_theta_full        32.87
_diffrn_reflns_theta_max         32.87
_diffrn_reflns_theta_min         2.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0435P)²+0.7195P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                713
_reflns_number_total             839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062061p-file001_1.cif
_cod_data_source_block           4
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        462.6(6)
_cod_original_sg_symbol_H-M      ' I 2 2 2'
_cod_database_code               4307562
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -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+1/2'
'-x+1/2, y+1/2, -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 0.5000 1.0000 0.5000 0.01545(18) Uani 1 4 d S . .
F1 F 0.5000 0.82896(15) 0.5000 0.0207(4) Uani 1 2 d S . .
F2 F 0.0000 1.0000 0.5000 0.0258(6) Uani 1 4 d S . .
N1 N 0.5000 1.0000 0.68820(18) 0.0118(4) Uani 1 2 d S . .
C1 C 0.5000 1.0000 0.9346(2) 0.0126(5) Uani 1 2 d S . .
C2 C 0.3908(6) 0.8960(2) 0.8714(2) 0.0138(4) Uani 1 1 d . . .
H2 H 0.3182 0.8246 0.9108 0.017 Uiso 1 1 calc R . .
C3 C 0.3917(6) 0.9002(2) 0.7497(2) 0.0143(4) Uani 1 1 d . . .
H3 H 0.3139 0.8309 0.7081 0.017 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 0.0226(4) 0.0136(3) 0.0102(3) 0.000 0.000 0.000
F1 0.0298(10) 0.0154(8) 0.0170(8) 0.000 -0.0002(17) 0.000
F2 0.0148(12) 0.0419(16) 0.0207(12) 0.000 0.000 0.000
N1 0.0104(9) 0.0140(9) 0.0109(9) 0.000 0.000 0.0004(14)
C1 0.0113(11) 0.0148(11) 0.0118(11) 0.000 0.000 0.000(2)
C2 0.0157(9) 0.0117(10) 0.0138(9) 0.0014(8) 0.0008(8) -0.0025(7)
C3 0.0145(9) 0.0149(10) 0.0136(9) -0.0007(8) 0.0001(7) -0.0029(8)
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'
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 180.0 . 2_675 ?
F1 V1 F2 90.0 2_675 . ?
F2 V1 N1 90.0 1_655 3_576 ?
F1 V1 N1 90.0 . . ?
N1 V1 N1 180.0 3_576 . ?
V1 F2 V1 180.0 1_455 . ?
C3 N1 C3 117.7(3) 2_675 . ?
C3 N1 V1 121.14(13) . . ?
C2 C1 C2 118.2(2) . 2_675 ?
C2 C1 C1 120.92(12) 2_675 3_577 ?
C3 C2 C1 119.1(2) . . ?
C1 C2 H2 120.5 . . ?
N1 C3 C2 123.0(2) . . ?
N1 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
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 1.8419(16) . ?
V1 F2 1.899(2) . ?
V1 N1 2.129(2) 3_576 ?
N1 C3 1.344(3) 2_675 ?
C1 C2 1.392(3) 2_675 ?
C1 C1 1.479(5) 3_577 ?
C2 C3 1.378(3) . ?
C2 H2 0.9300 . ?
