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_4105537
_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_sum            'C20 H4 F24 Ni O8 Pb'
_chemical_formula_weight         1094.13
_chemical_name_systematic
; 
 catena-(di(hexafluoroacetylacetonate)-nickel(II)-
 di(hexafluoroacetylacetonate)-lead(II))
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4611(16)
_cell_length_b                   12.6354(11)
_cell_length_c                   13.6823(11)
_cell_measurement_reflns_used    8295
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.38
_cell_volume                     3162.4(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.936
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13167
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.96
_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    6.096
_exptl_absorpt_correction_T_max  0.7925
_exptl_absorpt_correction_T_min  0.3345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Bruker-AXS 2003)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.298
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.911
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3676
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0538
_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^)+(0.1009P)^2^+15.6121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1516
_reflns_number_gt                3164
_reflns_number_total             3676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109128r_si_002_2.cif
_cod_data_source_block           PbNi(CF3COCHCOCF3)4_(1)
_cod_database_code               4105537