New Chemistry of the Triply Bonded Divanadium (V24+) Unit and Reduction to an Unprecedented V23+ Core
F. Albert Cotton; Elizabeth A. Hillard; Carlos A. Murillo; Xiaoping Wang; Inorganic Chemistry 42 (2003) 6063–6070; doi:10.1021/ic034646e

data_4314292
_publ_section_title
;
 New Chemistry of the Triply Bonded Divanadium (V24+) Unit and Reduction
 to an Unprecedented V23+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6063
_journal_page_last               6070
_journal_paper_doi               10.1021/ic034646e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C55 H53 Cl12 Li N6 O4 V1'
_chemical_formula_sum            'C55 H53 Cl12 Li N6 O4 V'
_chemical_formula_weight         1345.31
_chemical_melting_point          ?
_chemical_name_systematic
;
 tetrakis(THF)lithium-tris-3,5-dichlorophenylformamdinate vanadium(II)
;
_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                98.4680(10)
_cell_angle_beta                 96.0810(10)
_cell_angle_gamma                105.7370(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0014(7)
_cell_length_b                   15.9750(10)
_cell_length_c                   18.9046(12)
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22.289
_cell_measurement_theta_min      2.204
_cell_volume                     3125.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELTXL v5.05 (Siemens, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART area detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14877
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         'none(area detector data)'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.8294
_exptl_absorpt_correction_T_min  0.7193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+0.5518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                5424
_reflns_number_total             8151
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic034646esi20030610_035606_8.cif
_cod_data_source_block           footnote_compound
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C55 H53 Cl12 Li N6 O4 V1'
_cod_database_code               4314292