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_4120143
_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         'C48 H52 N2 V'
_chemical_formula_sum            'C48 H52 N2 V'
_chemical_formula_weight         707.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                76.054(2)
_cell_angle_beta                 84.829(2)
_cell_angle_gamma                83.592(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3263(4)
_cell_length_b                   11.5802(6)
_cell_length_c                   18.5814(8)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      70.02
_cell_measurement_theta_min      2.46
_cell_volume                     1931.31(16)
_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 0.953
_diffrn_measured_fraction_theta_max 0.952
_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  0.0188
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12749
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         2.455
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.4031
_exptl_absorpt_correction_T_min  0.2482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       Block
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.707
_exptl_crystal_size_mid          0.583
_exptl_crystal_size_min          0.328
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0962P)^2^+1.0575P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6547
_reflns_number_total             6723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403244w_si_005.cif
_cod_data_source_block           jb59fmi
_cod_database_code               4120143
_shelx_estimated_absorpt_t_min   0.281
_shelx_estimated_absorpt_t_max   0.506
_shelxl_version_number           2012-6
_shelx_res_checksum              44691