Interaction of some divalent metal acetylacetonates with Al, Ti, Nb and Ta isopropoxides. Factors influencing the formation and stability of heterometallic alkoxide complexes
Kessler, Vadim G.; Gohil, Suresh; Parola, Stephane; Dalton Transactions  (2003) 544–550; doi:10.1039/b206662a

data_7012002
_publ_section_title
;
 Interaction of some divalent metal acetylacetonates with Al, Ti, Nb
 and Ta isopropoxides. Factors influencing the formation and stability
 of heterometallic alkoxide complexes
;
_journal_coden_ASTM              DTARAF
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              544
_journal_page_last               550
_journal_paper_doi               10.1039/b206662a
_journal_year                    2003
_chemical_formula_sum            'C42 H98 Co2 O14 Ta2'
_chemical_formula_weight         1306.96
_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                83.624(15)
_cell_angle_beta                 78.361(13)
_cell_angle_gamma                68.940(14)
_cell_formula_units_Z            1
_cell_length_a                   9.586(6)
_cell_length_b                   10.551(6)
_cell_length_c                   15.938(10)
_cell_measurement_reflns_used    1202(I>2sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      1.31
_cell_volume                     1472.1(16)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD 1k'
_diffrn_measurement_method       'Bruker SMART'
_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  0.1055
_diffrn_reflns_av_sigmaI/netI    0.3139
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3813
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    4.308
_exptl_absorpt_correction_T_max  0.8134
_exptl_absorpt_correction_T_min  0.0878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             662
_exptl_crystal_size_max          1.10
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.1790
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.981
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1893
_reflns_number_gt                1194
_reflns_number_total             2667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206662a.txt
_cod_data_source_block           cotapr1m
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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 
;
_cod_original_cell_volume        1472.0(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012002