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_7053505
_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         'C47 H63 Cr N6 O'
_chemical_formula_sum            'C47 H63 Cr N6 O'
_chemical_formula_weight         780.03
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.496(2)
_cell_angle_beta                 90.870(2)
_cell_angle_gamma                91.470(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8881(5)
_cell_length_b                   12.8734(5)
_cell_length_c                   16.1682(8)
_cell_measurement_reflns_used    25734
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     2182.58(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.1372
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27281
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.8957
_exptl_absorpt_correction_T_min  0.8868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.0850
_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^)+(0.1166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1980
_refine_ls_wR_factor_ref         0.2268
_reflns_number_gt                4194
_reflns_number_total             7841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00114g.txt
_cod_data_source_block           7790
_cod_database_code               7053505