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_4082728
_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         '2(C50 H74 Ca N6 O2), 5(C7 H8)'
_chemical_formula_sum            'C67.5 H94 Ca N6 O2'
_chemical_formula_weight         1061.57
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.915(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3575(4)
_cell_length_b                   20.7250(5)
_cell_length_c                   21.1401(4)
_cell_measurement_reflns_used    34509
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.27
_cell_volume                     6285.2(3)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34509
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         14312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0322P)^2^+7.5757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                10744
_reflns_number_total             14312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500135g_si_001.cif
_cod_data_source_block           FO4981
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C67.50 H94 Ca N6 O2'
_cod_database_code               4082728