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_7109094
_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         'C94 H118 Ca2 Fe5 N4 O10'
_chemical_formula_sum            'C94 H118 Ca2 Fe5 N4 O10'
_chemical_formula_weight         1823.39
_chemical_name_systematic
;
[{Ca(NacNac)(THF)}2{Cp4Fe5(CO)8}]
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                73.007(2)
_cell_angle_beta                 86.687(2)
_cell_angle_gamma                63.809(3)
_cell_formula_units_Z            1
_cell_length_a                   11.5470(3)
_cell_length_b                   12.4516(3)
_cell_length_c                   17.7694(6)
_cell_measurement_reflns_used    11064
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     2184.90(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.985
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21630
_diffrn_reflns_theta_full        73.617
_diffrn_reflns_theta_max         76.684
_diffrn_reflns_theta_min         4.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.003
_exptl_absorpt_correction_T_max  0.20
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1526
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.0016213
_refine_ls_shift/su_mean         0.0000711
_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:
13.5 -5.87 8.29 4.22
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0259
_refine_ls_wR_factor_gt          0.0254
_refine_ls_wR_factor_ref         0.0253
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                8365
_reflns_number_total             9075
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.36
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0296
_oxford_refine_ls_scale          4.379(3)
_oxford_reflns_number_all        9039
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3cc41360h.txt
_cod_data_source_block           MPB116
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7109094