Intermolecular C‒H bond activation of benzene and pyridines by a vanadium(iii) alkylidene including a stepwise conversion of benzene to a vanadium-benzyne complex
Andino, José G.; Kilgore, Uriah J.; Pink, Maren; Ozarowski, Andrew; Krzystek, J.; Telser, Joshua; Baik, Mu-Hyun; Mindiola, Daniel J.; Chemical Science 1 (2010) 351–; doi:10.1039/c0sc00201a

data_1515812
_publ_section_title
;
 Intermolecular C--H bond activation of benzene and pyridines by a
 vanadium(iii) alkylidene including a stepwise conversion of benzene to a
 vanadium-benzyne complex
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              351
_journal_paper_doi               10.1039/c0sc00201a
_journal_volume                  1
_journal_year                    2010
_chemical_formula_moiety         'C38 H50 N P2 V'
_chemical_formula_sum            'C38 H50 N P2 V'
_chemical_formula_weight         633.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.1601(5)
_cell_length_b                   19.1808(5)
_cell_length_c                   20.2261(5)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      2.3
_cell_volume                     7045.3(3)
_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      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'0.30 degree frames measured for 0.3 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            137251
_diffrn_reflns_theta_full        17.19
_diffrn_reflns_theta_max         17.19
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.9979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.011
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.003
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+2.9754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                8869
_reflns_number_total             10771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00201a.txt
_cod_data_source_block           09510
_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_sg_symbol_H-M      Pbca
_cod_database_code               1515812