A four-coordinate thionitrosyl complex of vanadium
Ba L. Tran; Rick Thompson; Soumya Ghosh; Xinfeng Gao; Chun-Hsing Chen; Mu-Hyun Baik; Daniel J. Mindiola; Chem.Commun. 49 (2013) 2768–; doi:10.1039/c3cc38799b

data_7109020
_publ_section_title
;
 A four-coordinate thionitrosyl complex of vanadium
;
_journal_name_full               Chem.Commun.
_journal_page_first              2768
_journal_paper_doi               10.1039/c3cc38799b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C45 H68 N3 O2 S1 V1'
_chemical_formula_sum            'C45 H68 N3 O2 S V'
_chemical_formula_weight         766.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-08-27
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 107.722(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9142(17)
_cell_length_b                   21.113(3)
_cell_length_c                   18.224(3)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     4366.6(11)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51184
_diffrn_reflns_theta_full        29.542
_diffrn_reflns_theta_max         30.145
_diffrn_reflns_theta_min         1.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.201
_refine_diff_density_max         1.09
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0148
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         12804
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.0012477
_refine_ls_shift/su_mean         0.0000445
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 3.82P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1450
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1450
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10379
_reflns_number_total             12804
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.74
_oxford_diffrn_Wilson_scale      128.58
_oxford_refine_ls_r_factor_ref   0.0607
_oxford_refine_ls_scale          0.09368(2)
_oxford_reflns_number_all        12804
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10089_0m in P2(1)/c'
_cod_data_source_file            c3cc38799b.txt
_cod_data_source_block           10089
_cod_original_cell_volume        4366.7(11)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C45 H68 N3 O2 S1 V1'
_cod_database_code               7109020