Bridging Azines in the Coordination Sphere of Low-Valent Vanadocene Derivatives†
Jordan, Markus; Saak, Wolfgang; Haase, Detlev; Beckhaus, Rüdiger; Organometallics 29 (2010) 5859–; doi:10.1021/om100612e

data_4066755
_publ_section_title
;
 Bridging Azines in the Coordination Sphere of Low-Valent Vanadocene
 Derivatives&#x2020;
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5859
_journal_paper_doi               10.1021/om100612e
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C39 H35 B N V'
_chemical_formula_weight         579.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5674(14)
_cell_length_b                   9.8425(5)
_cell_length_c                   15.7720(9)
_cell_measurement_temperature    153(2)
_cell_volume                     3037.6(3)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe,l999)'
_computing_data_reduction        'XRED (Stoe, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24512
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.8424
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED (Stoe, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.767
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5983
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.767
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                4244
_reflns_number_total             5983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100612e_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4066755