Reductive N–N bond cleavage and coupling of organic azides mediated by chromium(i) and vanadium(i) β-diketiminate
Lin, Kuan-Ming; Wang, Po-Yang; Shieh, Yun-Jen; Chen, Hong-Zhang; Kuo, Ting-Shen; Tsai, Yi-Chou; New Journal of Chemistry 34 (2010) 1737–; doi:10.1039/c0nj00114g

data_7053506
_publ_section_title
;
 Reductive N--N bond cleavage and coupling of organic azides mediated by
 chromium(i) and vanadium(i) \b-diketiminate
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1737
_journal_paper_doi               10.1039/c0nj00114g
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C35 H59 Cr N3 Si2'
_chemical_formula_sum            'C35 H59 Cr N3 Si2'
_chemical_formula_weight         630.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.350(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1132(9)
_cell_length_b                   20.144(2)
_cell_length_c                   20.551(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3772.6(6)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29834
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+3.4899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                5058
_reflns_number_total             6633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00114g.txt
_cod_data_source_block           a7326
_cod_original_cell_volume        3772.7(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7053506