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_4066761
_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            'C186 H206 B3 F8 N6 V3'
_chemical_formula_weight         2862.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           158
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   22.8523(11)
_cell_length_b                   22.8523(11)
_cell_length_c                   18.2102(7)
_cell_measurement_temperature    153(2)
_cell_volume                     8235.8(6)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_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 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70703
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9429
_exptl_absorpt_correction_T_min  0.7553
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED (Stoe, 1999)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long needle'
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          1.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                6385
_reflns_number_total             10314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100612e_si_002.cif
_cod_data_source_block           26
_cod_original_sg_symbol_H-M      P3c1
_cod_database_code               4066761