New Class of Single-Source Precursors for the Synthesis of Main Group-Transition Metal Oxides: Heterobimetallic Pb-Mn β-Diketonates
Haitao Zhang; Jen-Hsien Yang; Roman V. Shpanchenko; Artem M. Abakumov; Joke Hadermann; Rodolphe Clérac; Evgeny V. Dikarev; Inorganic Chemistry 48 (2009) 8480–8488; doi:10.1021/ic901107s

data_4303100
_publ_section_title
;
New Class of Single-Source Precursors for the Synthesis of Main
Group-Transition Metal Oxides: Heterobimetallic Pb-Mn \b-Diketonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8480
_journal_page_last               8488
_journal_paper_doi               10.1021/ic901107s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
;
C30 H6 F36 Mn2 O12 Pb
;
_chemical_formula_sum            'C30 H6 F36 Mn2 O12 Pb'
_chemical_formula_weight         1559.42
_chemical_melting_point          ?
_chemical_name_systematic
; 
 hexa(hexafluoroacetylacetonate)-dimanganese(II)-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                117.96(3)
_cell_angle_beta                 97.64(3)
_cell_angle_gamma                107.01(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5223(19)
_cell_length_b                   12.124(2)
_cell_length_c                   12.224(2)
_cell_measurement_reflns_used    5680
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.36
_cell_volume                     1129.4(7)
_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 0.902
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9816
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.22
_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    4.474
_exptl_absorpt_correction_T_max  0.8413
_exptl_absorpt_correction_T_min  0.5534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS 2003)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.517
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5038
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0612P)^2^+0.0943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                4570
_reflns_number_total             5038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901107s_si_002_2.cif
_cod_data_source_block           PbMn2(CF3COCHCOCF3)6_(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1129.4(4)
_cod_database_code               4303100