Preparation of an Isocyano-β-diketone via its Metal Complexes, by Use of Metal Ions as Protecting Groups
Yixun Zhang; Andrew W. Maverick; Inorganic Chemistry 48 (2009) 10512–10518; doi:10.1021/ic900202e

data_4303548
_publ_section_title
;
Preparation of an Isocyano-\b-diketone via its Metal Complexes, by Use of
Metal Ions as Protecting Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10512
_journal_page_last               10518
_journal_paper_doi               10.1021/ic900202e
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'local laboratory'
_chemical_formula_moiety         'C36 H30 Al N3 O6, 0.58(C6 H14)'
_chemical_formula_sum            'C39.48 H38.12 Al N3 O6'
_chemical_formula_weight         677.59
_chemical_name_common            Al(acphNC)3.(C6H14)0.58
_chemical_name_systematic
;
 Tris(3-(4-isocyanophenyl)-2,4-pentanedionato)aluminum
 0.58-hexane solvate
;
_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                107.653(6)
_cell_angle_beta                 97.532(6)
_cell_angle_gamma                94.569(7)
_cell_formula_units_Z            2
_cell_length_a                   7.4327(10)
_cell_length_b                   13.510(2)
_cell_length_c                   20.657(4)
_cell_measurement_reflns_used    8304
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     1943.8(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w and \f scans '
_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  0.097
_diffrn_reflns_av_sigmaI/netI    0.217
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33734
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.4
_diffrn_reflns_theta_min         2.8
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
58 electrons corresponds to 1.16 hexane molecules per cell (0.58 per
Al complex). This solvent is included in the formula, FW, density, etc.,
but is not included in the model coordinates.
;
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.25
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         8704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.197
_refine_ls_R_factor_gt           0.069
_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^)+(0.0828P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.153
_refine_ls_wR_factor_ref         0.185
_reflns_number_gt                3067
_reflns_number_total             8704
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic900202e_si_001_8.cif
_cod_data_source_block           compound_14
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4303548