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_7034230
_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         'C12 H32 Cl4 Nb1 O6 Sn1'
_chemical_formula_sum            'C12 H32 Cl4 Nb O6 Sn'
_chemical_formula_weight         625.79
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-11-19
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record
;
2010-11-25 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3200(10)
_cell_length_b                   19.198(2)
_cell_length_c                   14.026(2)
_cell_measurement_reflns_used    4908
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.5459
_cell_measurement_theta_min      3.4073
_cell_volume                     2413.8(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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      110
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.884
_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  0.065
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10336
_diffrn_reflns_theta_full        26.353
_diffrn_reflns_theta_max         29.610
_diffrn_reflns_theta_min         3.414
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.386
_exptl_crystal_size_min          0.211
_refine_diff_density_max         2.21
_refine_diff_density_min         -2.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9174
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3001
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.0002955
_refine_ls_shift/su_mean         0.0000299
_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:
0.267E+04 0.436E+04 0.256E+04 986. 210.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1759
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1759
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2209
_reflns_number_total             3001
_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   0.0978
_oxford_refine_ls_scale          1.94(2)
_oxford_reflns_number_all        3001
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr268b in C 2/c'
_cod_data_source_file            c5dt00339c2.cif
_cod_data_source_block           smr268b
_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_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C12 H32 Cl4 Nb1 O6 Sn1'
_cod_database_code               7034230
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE O ( 2,X'S) H ( 2,X'S)
RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S)
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S)
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S)
RIDE C ( 2,X'S) H ( 23,X'S) H ( 22,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;