#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:04:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179466 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/63/4336377.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_4336377
loop_
_publ_author_name
'Henry S. La Pierre'
'Stefan G. Minasian'
'Mark Abubekerov'
'Stosh A. Kozimor'
'David K. Shuh'
'Tolek Tyliszczak'
'John Arnold'
'Robert G. Bergman'
'F. Dean Toste'
_publ_section_title
;
 Vanadium Bisimide Bonding Investigated by X-ray Crystallography, 51V and
 13C Nuclear Magnetic Resonance Spectroscopy, and V L3,2-Edge X-ray
 Absorption Near-Edge Structure Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11650
_journal_page_last               11660
_journal_paper_doi               10.1021/ic4020543
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         VCl(Py)2(NtBu)2
_chemical_formula_sum            'C18 H28 Cl N4 V'
_chemical_formula_weight         386.83
_chemical_name_common            VCl(Py)2(NtBu)2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   9.504(2)
_cell_length_b                   18.182(4)
_cell_length_c                   23.174(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.41
_cell_volume                     4004.5(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SUPERFLIP
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            134969
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.7017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0325
_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)+(0.0318P)²+4.3756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                3074
_reflns_number_total             3692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4020543_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4004.7(15)
_cod_database_code               4336377
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
C1 C 0.4855(2) 0.51406(11) 0.16127(8) 0.0198(4) Uani 1 1 d .
C2 C 0.4329(2) 0.58746(11) 0.13651(10) 0.0263(5) Uani 1 1 d .
H2A H 0.4764 0.5961 0.0997 0.039 Uiso 1 1 calc R
H2B H 0.4568 0.6266 0.1625 0.039 Uiso 1 1 calc R
H2C H 0.3326 0.5855 0.1318 0.039 Uiso 1 1 calc R
C3 C 0.4143(3) 0.49906(13) 0.21930(9) 0.0312(5) Uani 1 1 d .
H3A H 0.3145 0.4952 0.2138 0.047 Uiso 1 1 calc R
H3B H 0.4342 0.5387 0.2454 0.047 Uiso 1 1 calc R
H3C H 0.4496 0.4539 0.2351 0.047 Uiso 1 1 calc R
C4 C 0.6451(2) 0.51802(13) 0.16946(10) 0.0286(5) Uani 1 1 d .
H4A H 0.6895 0.5262 0.1328 0.043 Uiso 1 1 calc R
H4B H 0.6783 0.4726 0.1856 0.043 Uiso 1 1 calc R
H4C H 0.6677 0.5578 0.1951 0.043 Uiso 1 1 calc R
C5 C 0.5110(2) 0.25265(11) 0.17210(9) 0.0218(4) Uani 1 1 d .
C6 C 0.5435(4) 0.29775(15) 0.22562(11) 0.0515(8) Uani 1 1 d .
H6A H 0.6175 0.3320 0.2172 0.077 Uiso 1 1 calc R
H6B H 0.5728 0.2656 0.2562 0.077 Uiso 1 1 calc R
H6C H 0.4608 0.3241 0.2373 0.077 Uiso 1 1 calc R
C7 C 0.3886(3) 0.19980(16) 0.18390(13) 0.0482(7) Uani 1 1 d .
H7A H 0.3671 0.1728 0.1494 0.072 Uiso 1 1 calc R
H7B H 0.3073 0.2274 0.1957 0.072 Uiso 1 1 calc R
H7C H 0.4146 0.1662 0.2140 0.072 Uiso 1 1 calc R
C8 C 0.6398(3) 0.20723(13) 0.15525(11) 0.0363(6) Uani 1 1 d .
H8A H 0.6206 0.1809 0.1202 0.054 Uiso 1 1 calc R
H8B H 0.6610 0.1729 0.1855 0.054 Uiso 1 1 calc R
H8C H 0.7187 0.2393 0.1495 0.054 Uiso 1 1 calc R
C9 C 0.6747(2) 0.45205(11) 0.02468(8) 0.0176(4) Uani 1 1 d .
H9 H 0.6243 0.4934 0.0361 0.021 Uiso 1 1 calc R
C10 C 0.8007(2) 0.46211(11) -0.00401(8) 0.0195(4) Uani 1 1 d .
H10 H 0.8349 0.5092 -0.0109 0.023 Uiso 1 1 calc R
C11 C 0.8750(2) 0.40106(11) -0.02230(9) 0.0210(4) Uani 1 1 d .
H11 H 0.9606 0.4062 -0.0414 0.025 Uiso 1 1 calc R
C12 C 0.8193(2) 0.33204(11) -0.01161(9) 0.0200(4) Uani 1 1 d .
H12 H 0.8660 0.2901 -0.0242 0.024 Uiso 1 1 calc R
C13 C 0.6936(2) 0.32617(11) 0.01789(8) 0.0184(4) Uani 1 1 d .
H13 H 0.6573 0.2795 0.0250 0.022 Uiso 1 1 calc R
C14 C 0.1358(2) 0.30644(11) 0.10348(9) 0.0212(4) Uani 1 1 d .
H14 H 0.1851 0.2642 0.0934 0.025 Uiso 1 1 calc R
C15 C -0.0074(2) 0.30108(12) 0.11249(9) 0.0241(5) Uani 1 1 d .
H15 H -0.0534 0.2563 0.1083 0.029 Uiso 1 1 calc R
C16 C -0.0811(2) 0.36369(12) 0.12796(9) 0.0240(5) Uani 1 1 d .
H16 H -0.1776 0.3617 0.1344 0.029 Uiso 1 1 calc R
C17 C -0.0087(2) 0.42916(12) 0.13365(9) 0.0231(5) Uani 1 1 d .
H17 H -0.0558 0.4720 0.1440 0.028 Uiso 1 1 calc R
C18 C 0.1343(2) 0.43002(11) 0.12377(8) 0.0203(4) Uani 1 1 d .
H18 H 0.1824 0.4743 0.1278 0.024 Uiso 1 1 calc R
N1 N 0.45272(17) 0.45514(9) 0.12096(7) 0.0181(4) Uani 1 1 d .
N2 N 0.47281(17) 0.30014(9) 0.12427(7) 0.0190(4) Uani 1 1 d .
N3 N 0.62122(17) 0.38514(9) 0.03690(7) 0.0167(3) Uani 1 1 d .
N4 N 0.20738(17) 0.36994(9) 0.10862(7) 0.0181(4) Uani 1 1 d .
Cl1 Cl 0.32893(5) 0.35791(3) -0.01026(2) 0.01914(12) Uani 1 1 d .
V1 V 0.42804(3) 0.375196(18) 0.085583(14) 0.01533(10) Uani 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
N1 C1 C3 109.78(17)
N1 C1 C4 109.05(16)
C3 C1 C4 109.73(18)
N1 C1 C2 109.28(16)
C3 C1 C2 109.83(17)
C4 C1 C2 109.15(18)
C1 C2 H2A 109.5
C1 C2 H2B 109.5
H2A C2 H2B 109.5
C1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
C1 C3 H3A 109.5
C1 C3 H3B 109.5
H3A C3 H3B 109.5
C1 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C1 C4 H4A 109.5
C1 C4 H4B 109.5
H4A C4 H4B 109.5
C1 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
N2 C5 C6 110.70(18)
N2 C5 C8 109.07(17)
C6 C5 C8 109.7(2)
N2 C5 C7 108.63(18)
C6 C5 C7 110.3(2)
C8 C5 C7 108.4(2)
C5 C6 H6A 109.5
C5 C6 H6B 109.5
H6A C6 H6B 109.5
C5 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
C5 C7 H7A 109.5
C5 C7 H7B 109.5
H7A C7 H7B 109.5
C5 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
C5 C8 H8A 109.5
C5 C8 H8B 109.5
H8A C8 H8B 109.5
C5 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
N3 C9 C10 123.16(18)
N3 C9 H9 118.4
C10 C9 H9 118.4
C9 C10 C11 118.96(19)
C9 C10 H10 120.5
C11 C10 H10 120.5
C10 C11 C12 118.52(19)
C10 C11 H11 120.7
C12 C11 H11 120.7
C13 C12 C11 119.33(19)
C13 C12 H12 120.3
C11 C12 H12 120.3
N3 C13 C12 122.81(18)
N3 C13 H13 118.6
C12 C13 H13 118.6
N4 C14 C15 123.09(19)
N4 C14 H14 118.5
C15 C14 H14 118.5
C14 C15 C16 118.7(2)
C14 C15 H15 120.7
C16 C15 H15 120.7
C17 C16 C15 118.8(2)
C17 C16 H16 120.6
C15 C16 H16 120.6
C18 C17 C16 119.0(2)
C18 C17 H17 120.5
C16 C17 H17 120.5
N4 C18 C17 123.00(19)
N4 C18 H18 118.5
C17 C18 H18 118.5
C1 N1 V1 167.73(15)
C5 N2 V1 161.83(15)
C13 N3 C9 117.19(17)
C13 N3 V1 122.49(13)
C9 N3 V1 120.32(13)
C18 N4 C14 117.40(17)
C18 N4 V1 121.99(14)
C14 N4 V1 120.38(13)
N1 V1 N2 113.83(8)
N1 V1 N3 93.64(7)
N2 V1 N3 97.51(7)
N1 V1 N4 93.03(7)
N2 V1 N4 94.45(7)
N3 V1 N4 162.60(6)
N1 V1 Cl1 127.55(6)
N2 V1 Cl1 118.57(6)
N3 V1 Cl1 82.14(5)
N4 V1 Cl1 81.05(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.455(2)
C1 C3 1.530(3)
C1 C4 1.531(3)
C1 C2 1.536(3)
C2 H2A 0.9600
C2 H2B 0.9600
C2 H2C 0.9600
C3 H3A 0.9600
C3 H3B 0.9600
C3 H3C 0.9600
C4 H4A 0.9600
C4 H4B 0.9600
C4 H4C 0.9600
C5 N2 1.451(3)
C5 C6 1.519(3)
C5 C8 1.528(3)
C5 C7 1.533(3)
C6 H6A 0.9600
C6 H6B 0.9600
C6 H6C 0.9600
C7 H7A 0.9600
C7 H7B 0.9600
C7 H7C 0.9600
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
C9 N3 1.348(3)
C9 C10 1.382(3)
C9 H9 0.9300
C10 C11 1.383(3)
C10 H10 0.9300
C11 C12 1.384(3)
C11 H11 0.9300
C12 C13 1.380(3)
C12 H12 0.9300
C13 N3 1.348(2)
C13 H13 0.9300
C14 N4 1.346(3)
C14 C15 1.380(3)
C14 H14 0.9300
C15 C16 1.384(3)
C15 H15 0.9300
C16 C17 1.381(3)
C16 H16 0.9300
C17 C18 1.379(3)
C17 H17 0.9300
C18 N4 1.341(3)
C18 H18 0.9300
N1 V1 1.6852(17)
N2 V1 1.6873(17)
N3 V1 2.1626(17)
N4 V1 2.1662(17)
Cl1 V1 2.4329(7)
