Mechanistic Elucidation of the Formation of the Inverse Ca(I) Sandwich Complex [(thf)~3~Ca(μ-C~6~H~3~-1,3,5-Ph~3~)Ca(thf)~3~]and Stability of Aryl-Substituted Phenylcalcium Complexes
Sven Krieck; Helmar Görls; Matthias Westerhausen; Journal of the American Chemical Society 132 (2010) 12492–12501; doi:10.1021/ja105534w

data_4103018
_publ_contact_author
;
      Matthias Westerhausen
      Institut f\"ur anorganische und analytische Chemie
      Friedrich-Schiller-Universit\"at Jena
      August-Bebel-Str. 2
      07743 Jena
      Germany
;
_publ_contact_author_email       m.we@uni-jena.de
_publ_contact_author_fax         '03641 948 102'
_publ_contact_author_phone       '03641 948 110'
_publ_section_title
;
 Mechanistic Elucidation of the Formation of the Inverse Ca(I) Sandwich
 Complex [(thf)~3~Ca(\m-C~6~H~3~-1,3,5-Ph~3~)Ca(thf)~3~]and Stability of
 Aryl-Substituted Phenylcalcium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12492
_journal_page_last               12501
_journal_paper_doi               10.1021/ja105534w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         '2(C50 H67 Ca2 O7), 2(C24 H18), 7(C4 H8 O)'
_chemical_formula_sum            'C88 H113 Ca2 O10.5'
_chemical_formula_weight         1418.94
_chemical_name_systematic
; 
 ? 
;
_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                 92.546(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.6771(5)
_cell_length_b                   14.9476(4)
_cell_length_c                   22.7395(5)
_cell_measurement_reflns_used    57700
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.01
_cell_volume                     8379.5(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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0895
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57700
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            opalizierend
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         19010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1555P)^2^+3.4072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2772
_reflns_number_gt                10570
_reflns_number_total             19010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105534w_si_001_2.cif
_cod_data_source_block           FO4017
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C88 H113 Ca2 O10.50'
_cod_database_code               4103018