Structural Evidence of Strong Calcium−π Interactions to Aryl Substituents Stabilized by Coexistent Agostic Bonds to Alkyl Groups
Loh, Claas; Seupel, Susanne; Görls, Helmar; Krieck, Sven; Westerhausen, Matthias; Organometallics 33 (2014) 1480–; doi:10.1021/om500135g

data_4082723
_publ_section_title
;
 Structural Evidence of Strong Calcium&#x2212;\p Interactions to Aryl
 Substituents Stabilized by Coexistent Agostic Bonds to Alkyl Groups
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1480
_journal_paper_doi               10.1021/om500135g
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C27 H42 Li N3 O2'
_chemical_formula_sum            'C27 H42 Li N3 O2'
_chemical_formula_weight         447.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.327(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8728(3)
_cell_length_b                   18.6663(5)
_cell_length_c                   15.3965(3)
_cell_measurement_reflns_used    16254
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.77
_cell_volume                     2693.48(12)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16253
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.8584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                5251
_reflns_number_total             6170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500135g_si_001.cif
_cod_data_source_block           FO5296
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4082723