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_4340720
_publ_section_title
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 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_absolute_configuration unk
_chemical_formula_moiety
'2(C29 H25 N5 O V), 4(C F3 O3 S), 1.5(C4 H6 N2)'
_chemical_formula_sum            'C68 H59 F12 N13 O14 S4 V2'
_chemical_formula_weight         1740.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-07
_audit_creation_method
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8802(5)
_cell_length_b                   22.0171(7)
_cell_length_c                   21.9728(7)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3010
_cell_measurement_theta_min      2.4832
_cell_volume                     7198.7(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.9848
_diffrn_measured_fraction_theta_max 0.9848
_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  0.0234
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46821
_diffrn_reflns_theta_full        25.3474
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.9183
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.6057
_exptl_crystal_description       block
_exptl_crystal_F_000             3558.7201
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.3778
_refine_diff_density_min         -0.4361
_refine_diff_density_rms         0.0443
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.008(14)
_refine_ls_d_res_high            0.8301
_refine_ls_d_res_low             12.3286
_refine_ls_goodness_of_fit_ref   1.0557
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     578
_refine_ls_number_reflns         6732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0557
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+7.5749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.969
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              26
_reflns_limit_k_min              -26
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                6577
_reflns_number_total             6732
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic5010177_si_002.cif
_cod_data_source_block           comopound2
_cod_depositor_comments
'Adding full bibliography for 4340719--4340721.cif.'
_cod_database_code               4340720
_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. Others
 Fixed Sof: F4(0.5) F4A(0.5) F5(0.5) O6(0.5) O7(0.5) O7A(0.5) H2Sa(0.5)
 H2Sb(0.5) H2Sc(0.5) H22a(0.5) H22b(0.5) H22c(0.5) H29a(0.5) H29b(0.5) H29c(0.5)
3.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), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26),
  C31(H31), C32(H32), C33(H33), C34(H34)
3.b Idealised Me refined as rotating group:
 C2S(H2Sa,H2Sb,H2Sc), C4S(H4Sa,H4Sb,H4Sc), C12(H12a,H12b,H12c), C22(H22a,H22b,
 H22c), C29(H29a,H29b,H29c)
;