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_4069270
_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_sum            'C38 H59 N2 O V'
_chemical_formula_weight         610.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.550(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6996(11)
_cell_length_b                   16.8433(18)
_cell_length_c                   11.5092(14)
_cell_measurement_reflns_used    873
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.42
_cell_volume                     1782.6(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local program)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
'   0.30 degree frames measured for  30.17 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w 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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13280
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9553
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cleaved
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7586
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                5051
_reflns_number_total             7586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900115v_si_001.cif
_cod_data_source_block           04065
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_database_code               4069270