#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311898.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_4311898
loop_
_publ_author_name
'Trevor W. Hayton'
'Brian O. Patrick'
'Peter Legzdins'
_publ_section_title
;
 New Details Concerning the Reactions of Nitric Oxide with Vanadium
 Tetrachloride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7227
_journal_page_last               7233
_journal_paper_doi               10.1021/ic0491534
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C14 H24 Cl5 N V0.5'
_chemical_formula_weight         409.06
_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                107.333(3)
_cell_angle_beta                 93.278(3)
_cell_angle_gamma                114.325(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0570(12)
_cell_length_b                   9.2441(13)
_cell_length_c                   13.1457(15)
_cell_measurement_reflns_used    6688
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.55
_cell_volume                     936.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type  'Rigaku/ ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3788
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7412
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             423
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0363
_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)+(0.0679P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                3249
_reflns_number_total             3788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0491534si20040629_045244.cif
_cod_data_source_block           pl236
_cod_original_formula_sum        'C14 H24 Cl5 N V0.50'
_cod_database_code               4311898
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1512(2) 0.3775(2) 0.76377(15) 0.0218(4) Uani 1 1 d . . .
H1B H 0.1699 0.3207 0.6945 0.026 Uiso 1 1 calc R . .
H1A H 0.1517 0.3145 0.8109 0.026 Uiso 1 1 calc R . .
C8 C 0.4935(2) 0.4383(3) 0.73450(14) 0.0230(4) Uani 1 1 d . . .
C7 C 0.4535(2) 0.5376(3) 0.83302(15) 0.0268(4) Uani 1 1 d . . .
H7B H 0.5452 0.6506 0.8638 0.032 Uiso 1 1 calc R . .
H7A H 0.4462 0.4841 0.8870 0.032 Uiso 1 1 calc R . .
C3 C 0.2748(2) 0.6534(3) 0.92404(15) 0.0265(4) Uani 1 1 d . . .
H3B H 0.3763 0.7579 0.9574 0.032 Uiso 1 1 calc R . .
H3A H 0.1867 0.6839 0.9116 0.032 Uiso 1 1 calc R . .
C12 C 0.6220(2) 0.4232(3) 0.57812(17) 0.0376(5) Uani 1 1 d . . .
H12 H 0.6725 0.4726 0.5293 0.045 Uiso 1 1 calc R . .
C5 C 0.2994(3) 0.6497(3) 0.73765(17) 0.0301(4) Uani 1 1 d . . .
H5A H 0.1927 0.6494 0.7249 0.036 Uiso 1 1 calc R . .
H5B H 0.3144 0.5881 0.6683 0.036 Uiso 1 1 calc R . .
C2 C -0.0186(2) 0.3702(3) 0.74509(16) 0.0275(4) Uani 1 1 d . . .
H2A H -0.0370 0.4306 0.8124 0.041 Uiso 1 1 calc R . .
H2B H -0.1014 0.2540 0.7187 0.041 Uiso 1 1 calc R . .
H2C H -0.0250 0.4213 0.6923 0.041 Uiso 1 1 calc R . .
C9 C 0.4666(2) 0.2741(3) 0.72109(17) 0.0305(4) Uani 1 1 d . . .
H9 H 0.4134 0.2224 0.7682 0.037 Uiso 1 1 calc R . .
C13 C 0.5726(2) 0.5125(3) 0.66241(17) 0.0303(4) Uani 1 1 d . . .
H13 H 0.5924 0.6228 0.6709 0.036 Uiso 1 1 calc R . .
C10 C 0.5189(3) 0.1868(3) 0.6375(2) 0.0408(5) Uani 1 1 d . . .
H10 H 0.5014 0.0772 0.6292 0.049 Uiso 1 1 calc R . .
C11 C 0.5959(3) 0.2611(3) 0.56703(18) 0.0394(6) Uani 1 1 d . . .
H11 H 0.6308 0.2018 0.5114 0.047 Uiso 1 1 calc R . .
C4 C 0.2364(3) 0.5597(3) 1.00295(16) 0.0345(5) Uani 1 1 d . . .
H4A H 0.1313 0.4609 0.9736 0.052 Uiso 1 1 calc R . .
H4B H 0.2323 0.6327 1.0710 0.052 Uiso 1 1 calc R . .
H4C H 0.3212 0.5260 1.0145 0.052 Uiso 1 1 calc R . .
C6 C 0.4331(3) 0.8319(3) 0.7760(2) 0.0496(6) Uani 1 1 d . . .
H6A H 0.4083 0.8997 0.8370 0.074 Uiso 1 1 calc R . .
H6C H 0.4372 0.8754 0.7178 0.074 Uiso 1 1 calc R . .
H6B H 0.5382 0.8361 0.7975 0.074 Uiso 1 1 calc R . .
C14 C 0.9901(3) 0.8938(3) 0.63546(19) 0.0396(5) Uani 1 1 d . . .
N1 N 0.29443(17) 0.55465(19) 0.81392(12) 0.0189(3) Uani 1 1 d . . .
Cl1 Cl 0.08669(6) 0.25651(6) 0.13621(4) 0.02802(14) Uani 1 1 d . . .
Cl2 Cl 0.24187(5) 0.10854(6) -0.06686(4) 0.02879(14) Uani 1 1 d . . .
Cl3 Cl -0.12885(6) 0.08218(6) -0.11154(4) 0.03017(14) Uani 1 1 d . . .
Cl4 Cl 0.81384(7) 0.87861(8) 0.56133(5) 0.04312(17) Uani 1 1 d . . .
Cl5 Cl 1.04683(8) 0.73800(9) 0.56304(5) 0.04811(18) Uani 1 1 d . . .
V1 V 0.0000 0.0000 0.0000 0.02049(13) Uani 1 2 d S . .
H14A H 0.969(3) 0.885(3) 0.697(2) 0.025 Uiso 1 1 d . . .
H14B H 1.080(3) 0.999(3) 0.6529(18) 0.025 Uiso 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'
Cl Cl 0.1484 0.1585 '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
C2 C1 N1 115.39(16) . . ?
C9 C8 C13 118.79(17) . . ?
C9 C8 C7 119.18(18) . . ?
C13 C8 C7 121.70(19) . . ?
C8 C7 N1 116.31(14) . . ?
C4 C3 N1 114.89(16) . . ?
C11 C12 C13 119.7(2) . . ?
N1 C5 C6 115.87(19) . . ?
C8 C9 C10 120.1(2) . . ?
C12 C13 C8 120.6(2) . . ?
C11 C10 C9 120.5(2) . . ?
C10 C11 C12 120.30(19) . . ?
Cl4 C14 Cl5 111.38(13) . . ?
C5 N1 C1 108.44(14) . . ?
C5 N1 C7 112.31(15) . . ?
C1 N1 C7 108.19(14) . . ?
C5 N1 C3 108.45(15) . . ?
C1 N1 C3 111.86(14) . . ?
C7 N1 C3 107.63(13) . . ?
Cl1 V1 Cl1 180.00(3) 2 . ?
Cl1 V1 Cl3 89.67(2) 2 . ?
Cl1 V1 Cl3 90.33(2) . . ?
Cl1 V1 Cl3 90.33(2) 2 2 ?
Cl1 V1 Cl3 89.67(2) . 2 ?
Cl3 V1 Cl3 180.00(2) . 2 ?
Cl1 V1 Cl2 89.597(18) 2 . ?
Cl1 V1 Cl2 90.403(18) . . ?
Cl3 V1 Cl2 89.43(2) . . ?
Cl3 V1 Cl2 90.57(2) 2 . ?
Cl1 V1 Cl2 90.403(18) 2 2 ?
Cl1 V1 Cl2 89.597(18) . 2 ?
Cl3 V1 Cl2 90.57(2) . 2 ?
Cl3 V1 Cl2 89.43(2) 2 2 ?
Cl2 V1 Cl2 180.00(4) . 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
C1 C2 1.513(2) . ?
C1 N1 1.519(2) . ?
C8 C9 1.387(3) . ?
C8 C13 1.393(3) . ?
C8 C7 1.507(2) . ?
C7 N1 1.527(2) . ?
C3 C4 1.508(3) . ?
C3 N1 1.529(2) . ?
C12 C11 1.377(4) . ?
C12 C13 1.388(3) . ?
C5 N1 1.509(2) . ?
C5 C6 1.517(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.369(4) . ?
C14 Cl4 1.753(2) . ?
C14 Cl5 1.759(3) . ?
Cl1 V1 2.2849(5) . ?
Cl2 V1 2.3479(5) . ?
Cl3 V1 2.2995(5) . ?
V1 Cl1 2.2849(5) 2 ?
V1 Cl3 2.2995(5) 2 ?
V1 Cl2 2.3479(5) 2 ?
