Expanding Heteroscorpionates. Facile Synthesis of New Hybrid Scorpionate/Cyclopentadienyl Ligands and Their Lithium and Group 4 Metal Compounds: A Combined Experimental and Density Functional Theory Study
Otero, Antonio; Fernández-Baeza, Juan; Antiñolo, Antonio; Tejeda, Juan; Lara-Sánchez, Agustín; Sánchez-Barba, Luis F.; Sánchez-Molina, Margarita; Rodríguez, Ana M.; Bo, Carles; Urbano-Cuadrado, Manuel; Organometallics 26 (2007) 4310–; doi:10.1021/om7003942

data_4083689
_publ_section_title
;
 Expanding Heteroscorpionates. Facile Synthesis of New Hybrid
 Scorpionate/Cyclopentadienyl Ligands and Their Lithium and Group 4 Metal
 Compounds:&#x00A0; A Combined Experimental and Density Functional Theory
 Study
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4310
_journal_paper_doi               10.1021/om7003942
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C33 H37 Li N4 O'
_chemical_formula_weight         512.61
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 115.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.576(3)
_cell_length_b                   11.509(4)
_cell_length_c                   17.059(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2940.8(13)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q 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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.3565
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5290
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.3313
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                1542
_reflns_number_total             5107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7003942-file002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2940.8(12)
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4083689