A convenient and quantitative route to Sn(iv)-M [M = Ti(iv), Nb(v), Ta(v)] heterobimetallic precursors for dense mixed-metal oxide ceramics.
Mishra, Shashank; Jeanneau, Erwann; Mangematin, Stéphane; Chermette, Henry; Poor Kalhor, Mahboubeh; Bonnefont, Guillaume; Fantozzi, Gilbert; Le Floch, Sylvie; Pailhes, Stéphane; Daniele, Stéphane; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6848–6862; doi:10.1039/c5dt00339c

data_7034226
_publ_section_title
;
 A convenient and quantitative route to Sn(iv)-M [M = Ti(iv), Nb(v),
 Ta(v)] heterobimetallic precursors for dense mixed-metal oxide ceramics.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6848
_journal_page_last               6862
_journal_paper_doi               10.1039/c5dt00339c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C27 H65 Cl3 O10 Sn1 Ti2'
_chemical_formula_sum            'C27 H65 Cl3 O10 Sn Ti2'
_chemical_formula_weight         870.66
_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
_audit_update_record
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.309(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5427(9)
_cell_length_b                   19.876(2)
_cell_length_c                   18.1660(10)
_cell_measurement_reflns_used    9045
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4813
_cell_measurement_theta_min      3.5348
_cell_volume                     4086.8(6)
_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 0.853
_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  0.062
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20371
_diffrn_reflns_theta_full        26.331
_diffrn_reflns_theta_max         29.585
_diffrn_reflns_theta_min         3.548
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.754
_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    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.095
_refine_diff_density_max         2.35
_refine_diff_density_min         -2.18
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9784
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9784
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.0013562
_refine_ls_shift/su_mean         1.8561907
_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:
247. 372. 176. 41.2
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1729
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1729
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                6722
_reflns_number_total             9784
_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   0.0888
_oxford_refine_ls_scale          0.7334(16)
_oxford_reflns_number_all        9784
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr224b in P 1 21/n 1'
_cod_data_source_file            c5dt00339c2.cif
_cod_data_source_block           SMR224b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3086 2015-02-26 13:12:21Z robertas 

 Adding full bibliography for 7034222--7034230.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C27 H65 Cl3 O10 Sn1 Ti2'
_cod_database_code               7034226