3d Early Transition Metal Complexes Supported by a New Sterically Demanding Aryloxide Ligand
Keith Searles; Ba L. Tran; Maren Pink; Chun-Hsing Chen; Daniel J. Mindiola; Inorganic Chemistry 52 (2013) 11126–11135; doi:10.1021/ic401363p

data_4336187
_publ_section_title
;
 3d Early Transition Metal Complexes Supported by a New Sterically
 Demanding Aryloxide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11126
_journal_page_last               11135
_journal_paper_doi               10.1021/ic401363p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C80 H82 Cl O4 V, 3(C4 H8 O)'
_chemical_formula_sum            'C92 H106 Cl O7 V'
_chemical_formula_weight         1410.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.921(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.298(2)
_cell_length_b                   15.8883(14)
_cell_length_c                   23.727(2)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.17
_cell_volume                     7899.3(12)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2010)'
_computing_publication_material  'SHELXTL (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
'0.50 degree frames measured for 25 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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62328
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.9548
_exptl_absorpt_correction_T_min  0.9192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       prism
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         17889
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0665P)^2^+3.6895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                11348
_reflns_number_total             17889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401363p_si_003.cif
_cod_data_source_block           11042
_cod_original_cell_volume        7899.1(12)
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_database_code               4336187