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_7034227
_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         'C15 H35 Cl4 Nb O5 Sn '
_chemical_formula_sum            'C15 H35 Cl4 Nb O5 Sn'
_chemical_formula_weight         648.85
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-11-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.382(2)
_cell_length_b                   14.234(2)
_cell_length_c                   9.515(1)
_cell_measurement_reflns_used    5366
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4874
_cell_measurement_theta_min      3.5425
_cell_volume                     2625.0(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16727
_diffrn_reflns_theta_full        26.254
_diffrn_reflns_theta_max         29.499
_diffrn_reflns_theta_min         3.552
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.796
_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    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.1889
_exptl_crystal_size_mid          0.1430
_exptl_crystal_size_min          0.0769
_refine_diff_density_max         2.57
_refine_diff_density_min         -3.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0476
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.0020789
_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:
78.3 94.6 36.8 4.64
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1069
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.1069
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2012
_reflns_number_total             3411
_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   0.0793
_oxford_refine_ls_scale          0.5004(8)
_oxford_reflns_number_all        3411
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr226b in P n m a'
_cod_data_source_file            c5dt00339c2.cif
_cod_data_source_block           SMR226b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 n m a '
_cod_original_formula_sum        'C15 H35 Cl4 Nb O5 Sn '
_cod_database_code               7034227