Heterobimetallic Complexes Containing Ca-Fe or Yb-Fe Bonds: Synthesis and Molecular and Electronic Structures of [M{CpFe(CO)2}2(THF)3]2 (M = Ca or Yb)
Matthew P. Blake; Nikolas Kaltsoyannis; Philip Mountford; Journal of the American Chemical Society 133 (2011) 15358–15361; doi:10.1021/ja207487j

data_4106895
_publ_contact_author
;
 Prof P. Mountford           
 Chemistry Research Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
 Heterobimetallic Complexes Containing Ca-Fe or Yb-Fe Bonds: Synthesis and
 Molecular and Electronic Structures of [M{CpFe(CO)2}2(THF)3]2 (M = Ca or
 Yb)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15358
_journal_page_last               15361
_journal_paper_doi               10.1021/ja207487j
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C52 H68 Fe4 O14 Yb2, 1.5 (C4 H8 O1)'
_chemical_formula_sum            'C58 H80 Fe4 O15.5 Yb2'
_chemical_formula_weight         1594.73
_chemical_name_systematic
;
YbFp2(THF)3
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                106.9250(6)
_cell_angle_beta                 102.6480(5)
_cell_angle_gamma                99.4417(6)
_cell_formula_units_Z            1
_cell_length_a                   10.17420(10)
_cell_length_b                   11.04280(10)
_cell_length_c                   15.7031(2)
_cell_measurement_reflns_used    6727
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1597.11(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12770
_diffrn_reflns_theta_full        26.904
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         5.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.843
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.34
_refine_diff_density_min         -0.83
_refine_ls_extinction_coef       63(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0766
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6715
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.0015538
_refine_ls_shift/su_mean         0.0000250
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.894 -0.251 0.578 -0.117 0.119 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0277
_refine_ls_wR_factor_gt          0.0266
_refine_ls_wR_factor_ref         0.0264
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6828
_reflns_number_total             7241
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.69
_oxford_diffrn_Wilson_scale      4.60
_oxford_refine_ls_r_factor_ref   0.0249
_oxford_refine_ls_scale          0.4803(5)
_oxford_reflns_number_all        7241
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja207487j_si_001_4.cif
_cod_data_source_block           COMPOUND_2_Yb
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C58 H80 Fe4 O15.50 Yb2'
_cod_database_code               4106895