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_7107900
_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         'C78 H115 K N2 O8 Si Ta2, 2.5(C5 H12)'
_chemical_formula_sum            'C90.5 H145 K N2 O8 Si2 Ta2'
_chemical_formula_weight         1846.27
_chemical_name_systematic
;
?
;
_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                 94.990(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4755(10)
_cell_length_b                   30.724(2)
_cell_length_c                   22.0497(12)
_cell_measurement_reflns_used    21784
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     9769.3(11)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2009)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2009)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Mercury375R CCD (2x2 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  0.0920
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            101648
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  0.8716
_exptl_absorpt_correction_T_min  0.7190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3836
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         2.662
_refine_diff_density_min         -2.995
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         22455
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+78.5787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1925
_reflns_number_gt                17315
_reflns_number_total             22455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32535g.txt
_cod_data_source_block           '[K(DME)][{(OOO)2Ta2}(NSiMe3)2](pentane)2.5'
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C90.50 H145 K N2 O8 Si2 Ta2'
_cod_database_code               7107900