Aminotroponiminate Complexes of the Heavy Alkaline Earth and the Divalent Lanthanide Metals as Catalysts for the Hydroamination/Cyclization Reaction
Datta, Simmi; Gamer, Michael T.; Roesky, Peter W.; Organometallics 27 (2008) 1207–; doi:10.1021/om701014d

data_4070791
_publ_section_title
;
 Aminotroponiminate Complexes of the Heavy Alkaline Earth and the Divalent
 Lanthanide Metals as Catalysts for the Hydroamination/Cyclization
 Reaction
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1207
_journal_paper_doi               10.1021/om701014d
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C27 H53 Eu N3 O2 Si2'
_chemical_formula_sum            'C27 H53 Eu N3 O2 Si2'
_chemical_formula_weight         659.86
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.272(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0714(8)
_cell_length_b                   14.8719(9)
_cell_length_c                   11.2287(9)
_cell_measurement_reflns_used    14759
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.74
_cell_volume                     1674.7(2)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9306
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.6775
_exptl_absorpt_correction_T_min  0.5281
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.327
_exptl_crystal_size_min          0.291
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                5308
_reflns_number_total             5700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701014d-file001.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4070791