Stable "Inverse" Sandwich Complex with Unprecedented Organocalcium(I): Crystal Structures of [(thf)2Mg(Br)-C6H2-2,4,6-Ph3] and [(thf)3Ca{μ-C6H3-1,3,5-Ph3}Ca(thf)3]
Sven Krieck; Helmar Görls; Lian Yu; Markus Reiher; Matthias Westerhausen; Journal of the American Chemical Society 131 (2009) 2977–2985; doi:10.1021/ja808524y

data_4103969
_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
;
 Stable "Inverse" Sandwich Complex with Unprecedented Organocalcium(I):
 Crystal Structures of [(thf)2Mg(Br)-C6H2-2,4,6-Ph3] and
 [(thf)3Ca{\m-C6H3-1,3,5-Ph3}Ca(thf)3]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2977
_journal_page_last               2985
_journal_paper_doi               10.1021/ja808524y
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C48 H66 Ca2 O6'
_chemical_formula_sum            'C48 H66 Ca2 O6'
_chemical_formula_weight         819.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.3116(16)
_cell_length_b                   14.3116(16)
_cell_length_c                   13.612(2)
_cell_measurement_reflns_used    13247
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      3.22
_cell_volume                     2414.5(5)
_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      183(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13247
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.1057
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1856P)^2^+2.9345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2877
_refine_ls_wR_factor_ref         0.3328
_reflns_number_gt                1293
_reflns_number_total             1901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808524y_si_001_1.cif
_cod_data_source_block           FO3333
_cod_original_sg_symbol_Hall     -P6c
_cod_database_code               4103969