Synthesis and reactions of beta-diketiminate-supported complexes with Mg-Fe or Yb-Fe bonds
Matthew P. Blake; Nikolas Kaltsoyannis; Philip Mountford; Chem.Commun. 49 (2013) 3315–; doi:10.1039/c3cc41360h

data_7109092
_publ_section_title
;
 Synthesis and reactions of beta-diketiminate-supported complexes with
 Mg-Fe or Yb-Fe bonds
;
_journal_name_full               Chem.Commun.
_journal_page_first              3315
_journal_paper_doi               10.1039/c3cc41360h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C88 H124 Fe2 N4 O8 Yb2'
_chemical_formula_sum            'C88 H124 Fe2 N4 O8 Yb2'
_chemical_formula_weight         1823.75
_chemical_name_systematic
;
[Yb(NacNac)(THF)2Fp]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   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                113.800(3)
_cell_angle_beta                 91.1767(19)
_cell_angle_gamma                100.858(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3150(3)
_cell_length_b                   18.4454(6)
_cell_length_c                   21.4837(5)
_cell_measurement_reflns_used    36458
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     4359.8(2)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.986
_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  0.060
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            80462
_diffrn_reflns_theta_full        74.815
_diffrn_reflns_theta_max         77.129
_diffrn_reflns_theta_min         3.676
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.841
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as
contributions to the A and B parts of the calculated structure factors.
PLATON
PLATON, A Multipurpose Crystallographic Tool, A. L. Spek. Utrecht,
the Netherlands, 1998.; A. Spek, J. Appl. Cryst. (2003), 36, 7-13.
SQUEEZE
A. Spek, J. Appl. Cryst. (2003), 36, 7-13;
P. van der Sluis & A. L. Spek, Acta Cryst. (1990). A46, 194-201.
MCE
J. Rohlicek & M. Husak, J. Appl. Cryst. (2007), 40, 600-601.
;
_refine_diff_density_max         1.19
_refine_diff_density_min         -1.05
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         14702
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.0546364
_refine_ls_shift/su_mean         0.0030037
_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:
2.62 -13.7 -2.24 -3.89 -3.73
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0225
_refine_ls_wR_factor_gt          0.0206
_refine_ls_wR_factor_ref         0.0202
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              21
_reflns_limit_k_min              -23
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                15479
_reflns_number_total             18221
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      0.81
_oxford_refine_ls_r_factor_ref   0.0307
_oxford_refine_ls_scale          1.2135(5)
_oxford_reflns_number_all        18150
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3cc41360h.txt
_cod_data_source_block           MPB51
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7109092