Metal effects on ligand non-innocence in Group 5 complexes of the redox-active [ONO] pincer ligand.
Hananouchi, Steven; Krull, Brandon T.; Ziller, Joseph W.; Furche, Filipp; Heyduk, Alan F.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17991–18000; doi:10.1039/c4dt02259a

data_7032940
_publ_section_title
;
 Metal effects on ligand non-innocence in Group 5 complexes of the
 redox-active [ONO] pincer ligand.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17991
_journal_page_last               18000
_journal_paper_doi               10.1039/c4dt02259a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C31.5 H44 Cl3 N O2 V'
_chemical_formula_weight         625.96
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 91.0821(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.5015(8)
_cell_length_b                   22.5812(19)
_cell_length_c                   31.221(3)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.25
_cell_volume                     6697.4(10)
_computing_cell_refinement       'Bruker SAINT, v7.68a'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT, v7.68a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18750
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.586
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker TWINABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       plate
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         18750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+10.1485P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12680
_reflns_number_total             18750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02259a2.cif
_cod_data_source_block           afh346
_cod_depositor_comments
;Adding full bibliography for 7032938--7032941.cif.

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_cell_volume        6697.3(10)
_cod_original_formula_sum        'C31.50 H44 Cl3 N O2 V'
_cod_database_code               7032940
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2012-9
_shelx_res_checksum              53568
_shelx_hkl_checksum              19320