Novel Heteroleptic Heterobimetallic Alkoxide Complexes as Facile Single-Source Precursors for Ta5+ Doped TiO2-SnO2 Nanoparticles
Shashank Mishra; Erwann Jeanneau; Marie-Hélène Berger; Jean-François Hochepied; Stéphane Daniele; Inorganic Chemistry 49 (2010) 11184–11189; doi:10.1021/ic102134w

data_4317261
_publ_contact_author_address
;Universit\'e Claude Bernard Lyon 1
IRCELYON
2 avenue A. Einstein
69626 Villeurbanne C\'edex
France.
;
_publ_contact_author_email       mishrashashank74@rediffmail.com
_publ_contact_author_fax         '(+33) 472445399'
_publ_contact_author_name        'Dr. Shashank Mishra'
_publ_contact_author_phone       '(+33) 472445329'
_publ_section_title
;
 Novel Heteroleptic Heterobimetallic Alkoxide Complexes as Facile
 Single-Source Precursors for Ta5+ Doped TiO2-SnO2 Nanoparticles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11184
_journal_page_last               11189
_journal_paper_doi               10.1021/ic102134w
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H40 Cl4 O6 Sn Ti '
_chemical_formula_sum            'C16 H40 Cl4 O6 Sn Ti'
_chemical_formula_weight         636.86
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-06-10
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 106.034(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6599(8)
_cell_length_b                   14.9929(10)
_cell_length_c                   10.1380(9)
_cell_measurement_reflns_used    11054
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5041
_cell_measurement_theta_min      3.4169
_cell_volume                     1411.2(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15378
_diffrn_reflns_theta_full        26.877
_diffrn_reflns_theta_max         29.535
_diffrn_reflns_theta_min         3.424
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.628
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.5247
_exptl_crystal_size_mid          0.5051
_exptl_crystal_size_min          0.4000
_refine_diff_density_max         0.97
_refine_diff_density_min         -1.80
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9632
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.0006447
_refine_ls_shift/su_mean         0.0000495
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.158E+04 0.232E+04 0.120E+04 288. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0710
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0710
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3252
_reflns_number_total             3682
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0461
_oxford_refine_ls_scale          4.94(5)
_oxford_reflns_number_all        3682
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr258 in P 1 21 1'
_cod_data_source_file            ic102134w_si_002_2.cif
_cod_data_source_block           complex_3
_cod_original_sg_symbol_H-M      'P 21/m '
_cod_original_formula_sum        'C16 H40 Cl4 O6 Sn Ti '
_cod_database_code               4317261