Consequences of Electron-Density Manipulations on the X-ray Photoelectron Spectroscopic Properties of Ferrocenyl-β-diketonato Complexes of Manganese(III). Structure of [Mn(FcCOCHCOCH3)3].
Buitendach, Blenerhassitt E.; Erasmus, Elizabeth; Landman, Marilé; Niemantsverdriet, J. W. Hans; Swarts, Jannie C.; Inorganic chemistry 55 (2016) 1992–2000; doi:10.1021/acs.inorgchem.5b02250

data_4346857
_publ_section_title
;
 Consequences of Electron-Density Manipulations on the X-ray Photoelectron
 Spectroscopic Properties of Ferrocenyl-\b-diketonato Complexes of
 Manganese(III). Structure of [Mn(FcCOCHCOCH3)3].
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1992
_journal_page_last               2000
_journal_paper_doi               10.1021/acs.inorgchem.5b02250
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C42 H39 Fe3 Mn O6, 0.471(C6 H4), 0.471(C H3)'
_chemical_formula_sum            'C45.29 H42.29 Fe3 Mn O6'
_chemical_formula_weight         905.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                107.596(2)
_cell_angle_beta                 106.553(2)
_cell_angle_gamma                107.047(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7776(3)
_cell_length_b                   14.1725(5)
_cell_length_c                   14.9765(5)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.72
_cell_volume                     1901.60(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
; <i>ORTEP-3 for Windows</i> (Farrugia, 1997), 
 <i>Mercury</i> (Macrae <i>et al</i>., 2008) 
_computing_publication_material   'SHELXL-2013' 
  
_refine_special_details
The toluene solvent molecule includes an inversionn centre and the methyl group 
is disordered. This site occupancy of the ring atoms converged to 0.94139. The 
one five-membered ring had to be refined using the EADP instruction due to some 
large librations of three atoms in the ring. 
;
_computing_structure_refinement  'SHELXTL-2013, SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66050
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.512
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       needle
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+8.5636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5476
_reflns_number_total             7212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02250_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1901.60(11)
_cod_database_code               4346857
_shelx_estimated_absorpt_t_min   0.582
_shelx_estimated_absorpt_t_max   0.748
_shelxl_version_number           2014-3
_shelx_res_checksum              45528
_shelx_hkl_checksum              73701