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_4106894
_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 Ca2 Fe4 O14, O C4 H8'
_chemical_formula_sum            'C56 H76 Ca2 Fe4 O15'
_chemical_formula_weight         1292.76
_chemical_name_systematic
;
[CaFp2(THF)3]2
;
_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     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                106.883(5)
_cell_angle_beta                 102.239(4)
_cell_angle_gamma                99.551(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1473(5)
_cell_length_b                   11.0410(6)
_cell_length_c                   15.6119(8)
_cell_measurement_reflns_used    5475
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     1586.54(16)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15620
_diffrn_reflns_theta_full        73.532
_diffrn_reflns_theta_max         76.596
_diffrn_reflns_theta_min         4.314
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.092
_exptl_absorpt_correction_T_max  0.16
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.76
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1597
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.0003599
_refine_ls_shift/su_mean         0.0000188
_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: 
 46.6 41.6 45.2 29.8 8.58 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0443
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0401
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5051
_reflns_number_total             6555
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.20
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0588
_oxford_refine_ls_scale          4.959(11)
_oxford_reflns_number_all        6529
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja207487j_si_001_3.cif
_cod_data_source_block           COMPOUND_2_Ca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4106894