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_4106893
_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         'C88 H122 Ca2 Fe2 N4 O8'
_chemical_formula_sum            'C88 H122 Ca2 Fe2 N4 O8'
_chemical_formula_weight         1555.81
_chemical_name_systematic
;
[Ca(LDipp)Fp(THF)2]2
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 109.7630(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.90090(10)
_cell_length_b                   21.4323(2)
_cell_length_c                   16.23550(10)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4224.64(6)
_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       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72250
_diffrn_reflns_theta_full        26.922
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         5.114
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       150(100)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0939
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7604
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.0025050
_refine_ls_shift/su_mean         0.0000395
_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: 
 1.50 1.22 1.58 0.432 0.410 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0436
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0363
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7996
_reflns_number_total             9591
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      6.46
_oxford_refine_ls_r_factor_ref   0.0350
_oxford_refine_ls_scale          0.4227(5)
_oxford_reflns_number_all        9591
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja207487j_si_001_2.cif
_cod_data_source_block           COMPOUND_1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4106893