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_4105536
_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 O8 Pb Zn'
_chemical_formula_weight         1100.79
_chemical_name_systematic
; 
 catena-(di(hexafluoroacetylacetonate)-zinc(II)-
 di(hexafluoroacetylacetonate)-lead(II))
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.3070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.3980(16)
_cell_length_b                   14.4711(13)
_cell_length_c                   23.748(2)
_cell_measurement_reflns_used    8135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.28
_cell_volume                     6036.4(9)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            50446
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.67
_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    6.559
_exptl_absorpt_correction_T_max  0.3848
_exptl_absorpt_correction_T_min  0.2280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Bruker-AXS 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.293
_refine_diff_density_min         -2.004
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         13979
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+29.1052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                10283
_reflns_number_total             13979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109128r_si_002_1.cif
_cod_data_source_block           PbZn(CF3COCHCOCF3)4_(5)
_cod_original_cell_volume        6036.5(9)
_cod_database_code               4105536