Probing the Limits of Alkaline Earth-Transition Metal Bonding: An Experimental and Computational Study.
Blake, Matthew P.; Kaltsoyannis, Nikolas; Mountford, Philip; Journal of the American Chemical Society 137 (2015) 12352–12368; doi:10.1021/jacs.5b07866

data_4124577
_publ_section_title
;
 Probing the Limits of Alkaline Earth-Transition Metal Bonding: An
 Experimental and Computational Study.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12352
_journal_page_last               12368
_journal_paper_doi               10.1021/jacs.5b07866
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C108 H180 Co4 O18 P4 Yb2'
_chemical_formula_sum            'C108 H180 Co4 O18 P4 Yb2'
_chemical_formula_weight         2472.32
_chemical_name_systematic
;
Yb{Co(CO)3(PCy3)}2(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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                83.045(2)
_cell_angle_beta                 88.3797(18)
_cell_angle_gamma                79.8875(16)
_cell_formula_units_Z            1
_cell_length_a                   11.18582(19)
_cell_length_b                   14.3086(3)
_cell_length_c                   18.1682(5)
_cell_measurement_reflns_used    18102
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     2841.57(11)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28290
_diffrn_reflns_theta_full        73.875
_diffrn_reflns_theta_max         76.953
_diffrn_reflns_theta_min         3.159
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.390
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.86
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10542
_refine_ls_number_restraints     226
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.0026455
_refine_ls_shift/su_mean         0.0000252
_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: 
 15.8 -0.282 11.3 4.80 -0.972 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0378
_refine_ls_wR_factor_gt          0.0371
_refine_ls_wR_factor_ref         0.0368
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                10895
_reflns_number_total             11778
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      0.16
_oxford_refine_ls_r_factor_ref   0.0336
_oxford_refine_ls_scale          2.808(3)
_oxford_reflns_number_all        11734
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5b07866_si_002.cif
_cod_data_source_block           compound_24
_cod_original_cell_volume        2841.57(12)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4124577