Isolation and characterisation of the mixed-metal alkyl amide [(TMEDA)Na(mu-Bu)(mu-TMP)Mg(TMP)], an unexpected chelate-trapped intermediate in the formation of inverse crowns.
Hevia, Eva; Gallagher, Daniel J.; Kennedy, Alan R.; Mulvey, Robert E.; O'Hara, Charles T; Talmard, Christine; Chemical communications (Cambridge, England)  (2004) 2422–2423; doi:10.1039/b410293b

data_7113382
_publ_section_title
;
 Isolation and characterisation of the mixed-metal alkyl amide
 [(TMEDA)Na(mu-Bu)(mu-TMP)Mg(TMP)], an unexpected chelate-trapped
 intermediate in the formation of inverse crowns.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2422
_journal_page_last               2423
_journal_paper_doi               10.1039/b410293b
_journal_year                    2004
_chemical_formula_sum            'C28 H61 Mg N4 Na'
_chemical_formula_weight         501.11
_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                97.037(3)
_cell_angle_beta                 106.436(4)
_cell_angle_gamma                96.617(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2664(6)
_cell_length_b                   10.9478(7)
_cell_length_c                   15.3294(8)
_cell_measurement_reflns_used    87615
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.00
_cell_volume                     1619.62(17)
_computing_data_collection       'Denzo & Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi 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  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23255
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0788P)^2^+0.8739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                5441
_reflns_number_total             6474
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b410293b.txt
_cod_data_source_block           grem124
_cod_original_cell_volume        1619.62(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113382