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_4340719
_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
'C29 H25 N5 O V, C0.59 F1.76 O1.76 S0.54, 0.41(C F3 O3 S), 0.05(S)'
_chemical_formula_sum            'C30 H25 F3 N5 O4 S V'
_chemical_formula_weight         659.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     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                 90.280(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7910(5)
_cell_length_b                   20.233(1)
_cell_length_c                   15.2867(8)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.7402
_cell_measurement_theta_min      2.3168
_cell_volume                     2719.0(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1142
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.403
_diffrn_reflns_theta_min         1.670
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+29.5374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1980
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3748
_reflns_number_total             5014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5010177_si_003.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 4340719--4340721.cif.'
_cod_original_cell_volume        2719.0(7)
_cod_database_code               4340719
_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. Restrained distances
 F2A-C30A
 1.34 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F2A) = Uanis(O2A) = Uanis(O3A) = Uanis(O4A) = Uanis(C30A) = Uanis(F2) =
Uanis(F3) = Uanis(O2) = Uanis(O3) = Uanis(C30)
Uanis(S1) = Uanis(S1B)
4. Others
 Fixed Sof: S1(0.53687) S1A(0.41313) S1B(0.05) F1(0.58687) F1A(0.41313)
 F2(0.58687) F2A(0.41313) F3(0.58687) F3A(0.41313) O2(0.58687) O2A(0.41313)
 O3(0.58687) O3A(0.41313) O4(0.58687) O4A(0.41313) C30(0.58687) C30A(0.41313)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C26(H26),
  C27(H27), C28(H28)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              99211
_shelx_hkl_checksum              55846