Fluorinated Heterometallic β-Diketonates as Volatile Single-Source Precursors for the Synthesis of Low-Valent Mixed-Metal Fluorides
Anantharamulu Navulla; Alexander A. Tsirlin; Artem M. Abakumov; Roman V. Shpanchenko; Haitao Zhang; Evgeny V. Dikarev; Journal of the American Chemical Society 133 (2011) 692–694; doi:10.1021/ja109128r

data_4105539
_publ_contact_author_address
;
Department of Chemistry
University at Albany
1400 Washington ave
Albany NY 12222
USA
;
_publ_contact_author_email       dikarev@albany.edu
_publ_contact_author_fax         518-442-3462
_publ_contact_author_name
;
Dikarev, Evgeny V.
;
_publ_contact_author_phone       518-442-4401
_publ_section_title
;
 Fluorinated Heterometallic \b-Diketonates as Volatile Single-Source
 Precursors for the Synthesis of Low-Valent Mixed-Metal Fluorides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              692
_journal_page_last               694
_journal_paper_doi               10.1021/ja109128r
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
;
 C20 H4 F24 Fe O8 Pb
;
_chemical_formula_sum            'C20 H4 F24 Fe O8 Pb'
_chemical_formula_weight         1091.27
_chemical_name_systematic
; 
 catena-(di(hexafluoroacetylacetonate)-iron(II)-
 di(hexafluoroacetylacetonate)-lead(II))
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.8960(10)
_cell_angle_beta                 66.6400(10)
_cell_angle_gamma                64.3160(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4406(6)
_cell_length_b                   12.3702(7)
_cell_length_c                   13.5820(8)
_cell_measurement_reflns_used    5357
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.29
_cell_volume                     1523.87(15)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13373
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    6.184
_exptl_absorpt_correction_T_max  0.8362
_exptl_absorpt_correction_T_min  0.5768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Bruker-AXS 2003)
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.708
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6847
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+6.5964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                6316
_reflns_number_total             6847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109128r_si_002_4.cif
_cod_data_source_block           PbFe(CF3COCHCOCF3)4_(4)
_cod_database_code               4105539