Calcium, Strontium, Barium, and Ytterbium Complexes with Cyclooctatetraenyl or Cyclononatetraenyl Ligands1
Marc D. Walter; Gotthelf Wolmershäuser; Helmut Sitzmann; Journal of the American Chemical Society 127 (2005) 17494–17503; doi:10.1021/ja0550071

data_4112076
_publ_section_title
;
 Calcium, Strontium, Barium, and Ytterbium Complexes with
 Cyclooctatetraenyl or Cyclononatetraenyl Ligands1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17494
_journal_page_last               17503
_journal_paper_doi               10.1021/ja0550071
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C42 H66 Ca2'
_chemical_formula_weight         651.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.673(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6021(8)
_cell_length_b                   26.5918(15)
_cell_length_c                   16.0383(11)
_cell_measurement_reflns_used    7491
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.5
_cell_volume                     4010.5(5)
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_collection       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_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  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44377
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.91902
_exptl_absorpt_correction_T_min  0.88259
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'ABST/PLATON 98'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                4018
_reflns_number_total             7614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0550071si20050928_022809.cif
_cod_data_source_block           0229
_cod_database_code               4112076