Efficient Synthesis of an Unprecedented Enantiopure Hybrid Scorpionate/Cyclopentadienyl by Diastereoselective Nucleophilic Addition to a Fulvene
Honrado, Manuel; Otero, Antonio; Fernández-Baeza, Juan; Sánchez-Barba, Luis F.; Lara-Sánchez, Agust\?ín; Tejeda, Juan; Carrión, Mar\?ía P.; Mart\?ínez-Ferrer, Jaime; Garcés, Andrés; Rodr\?íguez, Ana M.; Organometallics 32 (2013) 3437–; doi:10.1021/om4003279

data_4089516
_publ_section_title
;
 Efficient Synthesis of an Unprecedented Enantiopure Hybrid
 Scorpionate/Cyclopentadienyl by Diastereoselective Nucleophilic Addition
 to a Fulvene
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3437
_journal_paper_doi               10.1021/om4003279
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C28 H38 N4 Zn'
_chemical_formula_sum            'C28 H38 N4 Zn'
_chemical_formula_weight         495.99
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.892(3)
_cell_length_b                   15.484(5)
_cell_length_c                   17.079(6)
_cell_measurement_reflns_used    1317
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      15.679
_cell_measurement_theta_min      2.379
_cell_volume                     2616.0(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1166
_diffrn_reflns_av_sigmaI/netI    0.1257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.8934
_exptl_absorpt_correction_T_min  0.8237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                2815
_reflns_number_total             4600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4003279_si_001.cif
_cod_data_source_block           3
_cod_original_cell_volume        2616.0(16)
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4089516