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_4317260
_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_formula_moiety         'C12 H32 Cl4 O6 Sn Ti, C2 H6 O'
_chemical_formula_sum            'C14 H38 Cl4 O7 Sn Ti'
_chemical_formula_weight         626.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-12-18
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 97.526(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6432(7)
_cell_length_b                   17.1750(10)
_cell_length_c                   16.2760(10)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4714
_cell_measurement_theta_min      3.4571
_cell_volume                     2672.4(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_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      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16663
_diffrn_reflns_theta_full        26.350
_diffrn_reflns_theta_max         29.606
_diffrn_reflns_theta_min         3.465
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
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    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.706
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.317
_refine_diff_density_max         1.39
_refine_diff_density_min         -1.32
_refine_ls_extinction_coef       61(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9360
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.0008312
_refine_ls_shift/su_mean         0.0940120
_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: 
 0.184E+04 0.300E+04 0.179E+04 723. 156. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1227
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1227
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4981
_reflns_number_total             6468
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0615
_oxford_refine_ls_scale          2.276(17)
_oxford_reflns_number_all        6468
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr224c in P 1 21/n 1'
_cod_data_source_file            ic102134w_si_002_1.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C14 H38 Cl4 O7 Sn1 Ti1'
_cod_database_code               4317260