Multielectron reduction of diazoalkane and azides via reversible cyclometalation in ditantalum complexes
Takashi Kurogi; Yutaka Ishida; Tsubasa Hatanaka; Hiroyuki Kawaguchi; Chem.Commun. 48 (2012) 6809–; doi:10.1039/c2cc32535g

data_7107898
_publ_section_title
;
 Multielectron reduction of diazoalkane and azides via reversible
 cyclometalation in ditantalum complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6809
_journal_paper_doi               10.1039/c2cc32535g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C72 H97 N2 O6 Si Ta2, C16 H40 K O8'
_chemical_formula_sum            'C88 H137 K N2 O14 Si Ta2'
_chemical_formula_weight         1876.09
_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                96.844(2)
_cell_angle_beta                 93.925(3)
_cell_angle_gamma                99.634(3)
_cell_formula_units_Z            2
_cell_length_a                   14.205(2)
_cell_length_b                   14.235(2)
_cell_length_c                   23.253(4)
_cell_measurement_reflns_used    11705
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      3.0268
_cell_volume                     4583.8(12)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Saturn CCD (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            57423
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.502
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_correction_T_min  0.7704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.604
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         20932
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+8.0033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                16081
_reflns_number_total             20932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32535g.txt
_cod_data_source_block           '[K(DME)4][{(OOO)Ta}2(N)(NCH2SiMe3)]'
_cod_original_cell_volume        4583.7(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107898