Single electron transfer (SET) activity of the dialkyl-amido sodium zincate [(TMEDA)*Na(m-TMP)(m-tBu)Zn(tBu)] towards TEMPO and chalcone
David Armstrong; Liam Balloch; James Crawford; Ben Fleming; Lorna Hogg; A.R. Kennedy; Jan Klett; Stuart Robertson; Samantha Orr; Charles T. O'Hara; Chem. Commun. 48 (2012) 1541–; doi:10.1039/c1cc12869h

data_7107264
_publ_section_title
;
 Single electron transfer (SET) activity of the dialkyl-amido sodium
 zincate [(TMEDA)*Na(m-TMP)(m-tBu)Zn(tBu)] towards TEMPO and chalcone
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              1541
_journal_paper_doi               10.1039/c1cc12869h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C68 H110 N6 Na2 O2 Zn2'
_chemical_formula_weight         1220.34
_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                102.420(7)
_cell_angle_beta                 105.102(6)
_cell_angle_gamma                91.831(6)
_cell_formula_units_Z            2
_cell_length_a                   11.9774(7)
_cell_length_b                   15.1883(13)
_cell_length_c                   20.8913(16)
_cell_measurement_reflns_used    5807
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.1695
_cell_measurement_theta_min      2.8580
_cell_volume                     3567.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       'omega scans'
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.3100
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31018
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.725
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         12537
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      0.722
_refine_ls_R_factor_all          0.1577
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                4451
_reflns_number_total             12537
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc12869h.txt
_cod_data_source_block           jksam2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107264