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.
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; Inorganic Chemistry 49 (2010) 977–988; doi:10.1021/ic9017745

data_4314657
_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            'C33 H34 N2 O2 P S3 V'
_chemical_formula_weight         668.10
_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                85.7640(10)
_cell_angle_beta                 83.4080(10)
_cell_angle_gamma                78.4900(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2708(7)
_cell_length_b                   9.7822(7)
_cell_length_c                   18.2902(13)
_cell_measurement_temperature    298(2)
_cell_volume                     1612.4(2)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19285
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9675
_exptl_absorpt_correction_T_min  0.6923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.085
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+0.1248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                5495
_reflns_number_total             7647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9017745_si_003_2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4314657