Zwitterionic and Cationic Titanium and Vanadium Complexes Having Terminal M−C Multiple Bonds. The Role of the β-Diketiminate Ligand in Formation of Charge-Separated Species
Adhikari, Debashis; Basuli, Falguni; Orlando, Justin H.; Gao, Xinfeng; Huffman, John C.; Pink, Maren; Mindiola, Daniel J.; Organometallics 28 (2009) 4115–; doi:10.1021/om900115v

data_4069272
_publ_section_title
;
 Zwitterionic and Cationic Titanium and Vanadium Complexes Having Terminal
 M&#x2212;C Multiple Bonds. The Role of the \b-Diketiminate Ligand in
 Formation of Charge-Separated Species
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4115
_journal_paper_doi               10.1021/om900115v
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
'(C56 H57 B F15 N2 O V), 2.25 (C7 H8), 0.25 (C6 H14)'
_chemical_formula_sum            'C73.25 H78.5 B F15 N2 O V'
_chemical_formula_weight         1349.63
_chemical_name_systematic
; 
 ? 
;
_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                84.864(2)
_cell_angle_beta                 83.414(2)
_cell_angle_gamma                75.774(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7637(15)
_cell_length_b                   13.1181(16)
_cell_length_c                   21.448(3)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.3
_cell_volume                     3451.0(8)
_computing_cell_refinement       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_collection       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_reduction        'APEX II v.2.2 (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
'0.30 degree frames measured for 50 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30700
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.9665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         13535
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1141P)^2^+0.7081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.2026
_reflns_number_gt                8236
_reflns_number_total             13535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900115v_si_003.cif
_cod_data_source_block           08128
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3451.0(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C73.25 H78.50 B F15 N2 O V'
_cod_database_code               4069272