A Well-Defined Terminal Vanadium(III) Oxo Complex.
King, Amanda E.; Nippe, Michael; Atanasov, Mihail; Chantarojsiri, Teera; Wray, Curtis A.; Bill, Eckhard; Neese, Frank; Long, Jeffrey R.; Chang, Christopher J.; Inorganic chemistry 53 (2014) 11388–11395; doi:10.1021/ic5010177

data_4340721
_publ_section_title
;
 A Well-Defined Terminal Vanadium(III) Oxo Complex.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11388
_journal_page_last               11395
_journal_paper_doi               10.1021/ic5010177
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C31 H28 N6 V, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C37 H34 F6 N8 O6 S2 V'
_chemical_formula_weight         915.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     heavy
_audit_creation_date             2014-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4713)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8446(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5042(7)
_cell_length_b                   15.8420(9)
_cell_length_c                   20.147(1)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3770
_cell_measurement_theta_min      2.2978
_cell_volume                     3990.5(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24131
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.377
_diffrn_reflns_theta_min         1.635
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+3.7271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5554
_reflns_number_total             7305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5010177_si_001.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 4340719--4340721.cif.'
_cod_original_cell_volume        3990.5(7)
_cod_database_code               4340721
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4A) = Uanis(O5A) = Uanis(O5) = Uanis(O6A) = Uanis(O6)
Uanis(C32) = Uanis(C32A)
3. Others
 Fixed Sof: F4(0.7436) F4A(0.2564) F5(0.7436) F5A(0.2564) F6(0.7436)
 F6A(0.2564) O4(0.7436) O4A(0.2564) O5(0.7436) O5A(0.2564) O6(0.7436)
 O6A(0.2564) F1(0.64753) F1A(0.35247) F2(0.64753) F2A(0.35247) F3(0.64753)
 F3A(0.35247) O3(0.64753) O3A(0.35247) C32(0.64753) C32A(0.35247)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C4S(H4SA,H4SB,
 H4SC), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              2903
_shelx_hkl_checksum              25820