Fluorinated β-Diketonates of the First Row Divalent Transition Metals: New Approach to the Synthesis of Unsolvated Species
Haitao Zhang; Bo Li; Jinyu Sun; Rodolphe Clérac; Evgeny V. Dikarev; Inorganic Chemistry 47 (2008) 10046–10052; doi:10.1021/ic801320p

data_4306500
_publ_section_title
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Fluorinated \b-Diketonates of the First Row Divalent Transition Metals: New
Approach to the Synthesis of Unsolvated Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10046
_journal_page_last               10052
_journal_paper_doi               10.1021/ic801320p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
;
 Ni3 (C F3 C O C H C O C F3)6
;
_chemical_formula_sum            'C30 H6 F36 Ni3 O12'
_chemical_formula_weight         1418.48
_chemical_melting_point          ?
_chemical_name_systematic
; 
 hexa(hexafluoroacetylacetonate)-trinickel(II,II,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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.619(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.518(2)
_cell_length_b                   16.237(2)
_cell_length_c                   16.842(2)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.03
_cell_volume                     4355.1(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      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.937
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36176
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.42
_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    1.497
_exptl_absorpt_correction_T_max  0.8896
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         10156
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+4.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                8557
_reflns_number_total             10156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801320p_si_001_6.cif
_cod_data_source_block           Ni3(CF3COCHCOCF3)6_(4b)
_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 
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_cod_original_cell_volume        4355.0(10)
_cod_database_code               4306500