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_4120142
_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         'C96 H104 Li2 N4 O4 V2'
_chemical_formula_sum            'C96 H104 Li2 N4 O4 V2'
_chemical_formula_weight         1493.59
_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
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 107.291(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6799(6)
_cell_length_b                   20.8049(11)
_cell_length_c                   15.9520(8)
_cell_measurement_reflns_used    3469
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.03
_cell_measurement_theta_min      8.03
_cell_volume                     4018.0(4)
_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      90(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker 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  0.0394
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9991
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.903
_diffrn_reflns_theta_min         8.220
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.7142
_exptl_absorpt_correction_T_min  0.4005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       Trapezoid
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.393
_exptl_crystal_size_min          0.213
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0653
_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^)+(0.1222P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5846
_reflns_number_total             7200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403244w_si_004.cif
_cod_data_source_block           jb55tw411
_cod_database_code               4120142
_shelx_estimated_absorpt_t_min   0.433
_shelx_estimated_absorpt_t_max   0.632
_shelxl_version_number           2012-9
_shelx_res_checksum              47518