#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314656.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_4314656
loop_
_publ_author_name
'Shengfa Ye'
'Frank Neese'
'Andrew Ozarowski'
'Dmitry Smirnov'
'J. Krzystek'
'Joshua Telser'
'Ju-Hsiou Liao'
'Chen-Hsiung Hung'
'Wei-Chen Chu'
'Yi-Feng Tsai'
'Rong-Chin Wang'
'Kun-Yuan Chen'
'Hua-Fen Hsu'
_publ_section_title
;
 Family of V(III)-Tristhiolato Complexes Relevant to Functional Models of
 Vanadium Nitrogenase: Synthesis and Electronic Structure Investigations
 by Means of High-Frequency and -Field Electron Paramagnetic Resonance
 Coupled to Quantum Chemical Computations.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              977
_journal_page_last               988
_journal_paper_doi               10.1021/ic9017745
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C25 H24 N2 P S3 V'
_chemical_formula_weight         530.03
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.462(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6066(15)
_cell_length_b                   21.519(4)
_cell_length_c                   13.877(3)
_cell_measurement_reflns_used    108
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.529
_cell_measurement_theta_min      -23.529
_cell_volume                     2527.4(8)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  'Wingx publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       'phi-Omega scan'
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15482
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_correction_T_min  0.8406
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1035P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1932
_reflns_number_gt                2978
_reflns_number_total             5967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9017745_si_003_1.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2527.3(8)
_cod_database_code               4314656
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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
C1 C 0.8910(8) 0.2517(4) 0.6410(5) 0.098(2) Uani 1 1 d . . .
H1 H 0.8544 0.2857 0.6718 0.118 Uiso 1 1 calc R . .
C2 C 1.0073(8) 0.2539(4) 0.5877(5) 0.099(2) Uani 1 1 d . . .
H2 H 1.0628 0.2886 0.5726 0.119 Uiso 1 1 calc R . .
C3 C 0.9189(6) 0.1584(3) 0.5941(5) 0.088(2) Uani 1 1 d . . .
H3 H 0.9103 0.1159 0.5825 0.105 Uiso 1 1 calc R . .
C4 C 1.1395(8) 0.1753(4) 0.5043(6) 0.130(3) Uani 1 1 d . . .
H4A H 1.1497 0.2052 0.4545 0.195 Uiso 1 1 calc R . .
H4B H 1.1040 0.1365 0.4740 0.195 Uiso 1 1 calc R . .
H4C H 1.2401 0.1696 0.5463 0.195 Uiso 1 1 calc R . .
C5 C 0.6674(6) 0.1066(2) 0.9437(3) 0.0493(11) Uani 1 1 d . . .
C6 C 0.7299(6) 0.0845(2) 1.0365(4) 0.0629(13) Uani 1 1 d . . .
H6 H 0.8389 0.0805 1.0551 0.076 Uiso 1 1 calc R . .
C7 C 0.6343(8) 0.0683(2) 1.1014(4) 0.0682(15) Uani 1 1 d . . .
H7 H 0.6801 0.0544 1.1635 0.082 Uiso 1 1 calc R . .
C8 C 0.4730(7) 0.0722(2) 1.0771(4) 0.0579(13) Uani 1 1 d . . .
C9 C 0.4090(6) 0.0939(2) 0.9838(3) 0.0518(11) Uani 1 1 d . . .
H9 H 0.2998 0.0971 0.9658 0.062 Uiso 1 1 calc R . .
C10 C 0.5028(5) 0.11097(18) 0.9168(3) 0.0437(10) Uani 1 1 d . . .
C11 C 0.3667(8) 0.0549(3) 1.1490(4) 0.0847(19) Uani 1 1 d . . .
H11A H 0.3179 0.0918 1.1688 0.127 Uiso 1 1 calc R . .
H11B H 0.4284 0.0354 1.2055 0.127 Uiso 1 1 calc R . .
H11C H 0.2864 0.0267 1.1182 0.127 Uiso 1 1 calc R . .
C12 C 0.3670(5) 0.0585(2) 0.6464(3) 0.0473(11) Uani 1 1 d . . .
C13 C 0.3077(5) 0.08297(18) 0.7263(3) 0.0422(10) Uani 1 1 d . . .
C14 C 0.1666(5) 0.0588(2) 0.7486(3) 0.0470(11) Uani 1 1 d . . .
H14 H 0.1269 0.0752 0.8012 0.056 Uiso 1 1 calc R . .
C15 C 0.0853(5) 0.0111(2) 0.6941(4) 0.0519(11) Uani 1 1 d . . .
C16 C 0.1467(6) -0.0124(2) 0.6162(4) 0.0618(13) Uani 1 1 d . . .
H16 H 0.0934 -0.0443 0.5790 0.074 Uiso 1 1 calc R . .
C17 C 0.2856(6) 0.0105(2) 0.5919(4) 0.0580(12) Uani 1 1 d . . .
H17 H 0.3242 -0.0064 0.5392 0.070 Uiso 1 1 calc R . .
C18 C -0.0642(6) -0.0148(2) 0.7206(5) 0.0772(17) Uani 1 1 d . . .
H18A H -0.1007 0.0124 0.7666 0.116 Uiso 1 1 calc R . .
H18B H -0.0433 -0.0552 0.7495 0.116 Uiso 1 1 calc R . .
H18C H -0.1437 -0.0181 0.6626 0.116 Uiso 1 1 calc R . .
C19 C 0.3838(5) 0.2656(2) 0.7717(3) 0.0501(11) Uani 1 1 d . . .
C20 C 0.3208(5) 0.21224(18) 0.8087(3) 0.0440(10) Uani 1 1 d . . .
C21 C 0.1932(5) 0.2182(2) 0.8551(3) 0.0513(11) Uani 1 1 d . . .
H21 H 0.1515 0.1826 0.8787 0.062 Uiso 1 1 calc R . .
C22 C 0.1240(6) 0.2753(2) 0.8679(4) 0.0592(13) Uani 1 1 d . . .
C23 C 0.1912(6) 0.3266(2) 0.8320(4) 0.0690(15) Uani 1 1 d . . .
H23 H 0.1498 0.3657 0.8410 0.083 Uiso 1 1 calc R . .
C24 C 0.3152(6) 0.3224(2) 0.7843(4) 0.0661(15) Uani 1 1 d . . .
H24 H 0.3545 0.3582 0.7597 0.079 Uiso 1 1 calc R . .
C25 C -0.0147(7) 0.2812(3) 0.9172(5) 0.0876(19) Uani 1 1 d . . .
H25A H -0.0058 0.3188 0.9551 0.131 Uiso 1 1 calc R . .
H25B H -0.0183 0.2462 0.9596 0.131 Uiso 1 1 calc R . .
H25C H -0.1097 0.2825 0.8688 0.131 Uiso 1 1 calc R . .
N1 N 0.8336(5) 0.1912(2) 0.6433(3) 0.0697(12) Uani 1 1 d . . .
N2 N 1.0236(4) 0.1979(2) 0.5627(3) 0.0609(11) Uani 1 1 d . . .
P1 P 0.43134(13) 0.14161(5) 0.79550(8) 0.0403(3) Uani 1 1 d . . .
S1 S 0.79536(14) 0.12816(7) 0.86240(10) 0.0637(4) Uani 1 1 d . . .
S2 S 0.54016(15) 0.08785(6) 0.61014(9) 0.0606(4) Uani 1 1 d . . .
S3 S 0.54733(16) 0.26332(6) 0.71059(12) 0.0685(4) Uani 1 1 d . . .
V1 V 0.64937(9) 0.16419(4) 0.71799(6) 0.0501(3) 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 110.3(7) . . ?
N2 C2 C1 104.3(6) . . ?
N1 C3 N2 107.3(6) . . ?
C6 C5 C10 118.2(4) . . ?
C6 C5 S1 119.9(4) . . ?
C10 C5 S1 121.9(3) . . ?
C7 C6 C5 121.3(5) . . ?
C8 C7 C6 121.7(5) . . ?
C7 C8 C9 117.5(5) . . ?
C7 C8 C11 121.9(5) . . ?
C9 C8 C11 120.6(5) . . ?
C10 C9 C8 122.1(5) . . ?
C9 C10 C5 119.2(4) . . ?
C9 C10 P1 125.4(4) . . ?
C5 C10 P1 115.4(3) . . ?
C17 C12 C13 119.2(4) . . ?
C17 C12 S2 118.4(4) . . ?
C13 C12 S2 122.4(3) . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 P1 114.7(3) . . ?
C14 C13 P1 126.1(3) . . ?
C15 C14 C13 121.6(4) . . ?
C16 C15 C14 118.1(4) . . ?
C16 C15 C18 121.3(4) . . ?
C14 C15 C18 120.6(4) . . ?
C15 C16 C17 121.9(5) . . ?
C16 C17 C12 120.0(4) . . ?
C24 C19 C20 118.3(4) . . ?
C24 C19 S3 118.7(4) . . ?
C20 C19 S3 123.0(3) . . ?
C21 C20 C19 119.2(4) . . ?
C21 C20 P1 126.9(3) . . ?
C19 C20 P1 113.7(3) . . ?
C20 C21 C22 122.5(4) . . ?
C23 C22 C21 116.3(5) . . ?
C23 C22 C25 121.5(5) . . ?
C21 C22 C25 122.2(5) . . ?
C24 C23 C22 122.8(5) . . ?
C23 C24 C19 120.8(5) . . ?
C3 N1 C1 105.1(5) . . ?
C3 N1 V1 130.5(5) . . ?
C1 N1 V1 124.4(4) . . ?
C2 N2 C3 113.1(6) . . ?
C2 N2 C4 125.5(6) . . ?
C3 N2 C4 121.4(6) . . ?
C10 P1 C13 107.93(19) . . ?
C10 P1 C20 107.8(2) . . ?
C13 P1 C20 111.59(19) . . ?
C10 P1 V1 109.44(15) . . ?
C13 P1 V1 109.80(14) . . ?
C20 P1 V1 110.19(15) . . ?
C5 S1 V1 109.75(16) . . ?
C12 S2 V1 109.51(16) . . ?
C19 S3 V1 109.53(15) . . ?
N1 V1 S1 100.32(12) . . ?
N1 V1 S3 92.11(14) . . ?
S1 V1 S3 119.69(7) . . ?
N1 V1 S2 97.53(14) . . ?
S1 V1 S2 114.82(6) . . ?
S3 V1 S2 121.62(6) . . ?
N1 V1 P1 175.08(14) . . ?
S1 V1 P1 83.57(5) . . ?
S3 V1 P1 83.31(5) . . ?
S2 V1 P1 83.44(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
C1 C2 1.349(9) . ?
C1 N1 1.395(8) . ?
C2 N2 1.270(8) . ?
C3 N1 1.298(7) . ?
C3 N2 1.366(7) . ?
C4 N2 1.477(7) . ?
C5 C6 1.387(6) . ?
C5 C10 1.401(6) . ?
C5 S1 1.775(5) . ?
C6 C7 1.371(7) . ?
C7 C8 1.370(7) . ?
C8 C9 1.393(6) . ?
C8 C11 1.518(7) . ?
C9 C10 1.387(6) . ?
C10 P1 1.809(4) . ?
C12 C17 1.393(6) . ?
C12 C13 1.403(6) . ?
C12 S2 1.774(5) . ?
C13 C14 1.407(6) . ?
C13 P1 1.810(4) . ?
C14 C15 1.386(6) . ?
C15 C16 1.382(6) . ?
C15 C18 1.508(6) . ?
C16 C17 1.390(7) . ?
C19 C24 1.383(6) . ?
C19 C20 1.406(6) . ?
C19 S3 1.771(5) . ?
C20 C21 1.376(6) . ?
C20 P1 1.820(4) . ?
C21 C22 1.393(6) . ?
C22 C23 1.380(7) . ?
C22 C25 1.485(7) . ?
C23 C24 1.358(7) . ?
N1 V1 2.127(4) . ?
P1 V1 2.3763(13) . ?
S1 V1 2.2981(16) . ?
S2 V1 2.3045(16) . ?
S3 V1 2.3021(16) . ?
