Zirconium-Substituted Isopolytungstates: Structural Models for Zirconia-Supported Tungsten Catalysts
Carabineiro, Hugo; Villanneau, Richard; Carrier, Xavier; Herson, Patrick; Lemos, Francisco; Ramôa Ribeiro, Fernando; Proust, Anna; Che, Michel; Inorganic Chemistry 45 (2006) 1915–1923; doi:10.1021/ic051941l

data_4331968
_publ_section_title
;
 Zirconium-Substituted Isopolytungstates:&#x00A0; Structural Models for
 Zirconia-Supported Tungsten Catalysts
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1915
_journal_page_last               1923
_journal_paper_doi               10.1021/ic051941l
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
'2(N1 C4 H12)+, (C4 H14 O21 S2 W5 Zr1)2-,(C2 H6 O1 S1)'
_chemical_formula_sum            'C14 H44 N2 O22 S3 W5 Zr'
_chemical_formula_weight         1699.17
_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             05-10-18
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 91.245(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0093(7)
_cell_length_b                   21.946(2)
_cell_length_c                   15.1748(18)
_cell_measurement_reflns_used    238
_cell_measurement_temperature    295
_cell_measurement_theta_max      23
_cell_measurement_theta_min      4
_cell_volume                     3665.5(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT. Nonius (1997-2001).'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26745
_diffrn_reflns_theta_full        29.403
_diffrn_reflns_theta_max         30.003
_diffrn_reflns_theta_min         1.632
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.151
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.079
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.75
_refine_diff_density_min         -1.40
_refine_ls_extinction_coef       21(3)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0912
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5508
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000937
_refine_ls_structure_factor_coef F
_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: 
2.07 -0.716 1.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0609
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0402
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5508
_reflns_number_total             5508
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic051941lsup1.cif
_cod_data_source_block           1c_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C14 H44 N2 O22 S3 W5 Zr1'
_cod_database_code               4331968