Linear and Nonlinear Two-Coordinate Vanadium Complexes: Synthesis, Characterization, and Magnetic Properties of V(II) Amides
Jessica N. Boynton; Jing-Dong Guo; James C. Fettinger; Christopher E. Melton; Shigeru Nagase; Philip P. Power; Journal of the American Chemical Society 135 (2013) 10720–10728; doi:10.1021/ja403244w

data_4120140
_publ_section_title
;
 Linear and Nonlinear Two-Coordinate Vanadium Complexes: Synthesis,
 Characterization, and Magnetic Properties of V(II) Amides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10720
_journal_page_last               10728
_journal_paper_doi               10.1021/ja403244w
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C72 H100 N2 V'
_chemical_formula_sum            'C72 H100 N2 V'
_chemical_formula_weight         1044.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 104.2210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4038(3)
_cell_length_b                   17.0341(3)
_cell_length_c                   24.8449(5)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      72.09
_cell_measurement_theta_min      3.94
_cell_volume                     6319.3(2)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2012.2-0) (Bruker, 2012)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_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      190(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Duo APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31143
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         2.959
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             2276
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11146
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+1.8250P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10320
_reflns_number_total             11146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403244w_si_002.cif
_cod_data_source_block           JB34FMI
_cod_database_code               4120140
_shelx_estimated_absorpt_t_min   0.675
_shelx_estimated_absorpt_t_max   0.877
_shelxl_version_number           2012-9
_shelx_res_checksum              8429