Preparation, characterization, and catalytic performances of a pyrazine dicarboxylate-bridging rare-earth-containing polytungstoarsenate aggregate for selective oxidation of thiophenes and deep desulfurization of model fuels.
Niu, Yanjun; Xu, Qiaofei; Wang, Yuan; Li, Zhao; Lu, Jingkun; Ma, Pengtao; Zhang, Chao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9677–9684; doi:10.1039/c8dt01243a

data_7046699
_publ_section_title
;
 Preparation, characterization, and catalytic performances of a pyrazine
 dicarboxylate-bridging rare-earth-containing polytungstoarsenate
 aggregate for selective oxidation of thiophenes and deep desulfurization
 of model fuels.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9677
_journal_page_last               9684
_journal_paper_doi               10.1039/c8dt01243a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C12 H4 As3 Ce4 K6 N4 O136 W29, 11(O)'
_chemical_formula_sum            'C12 H4 As3 Ce4 K6 N4 O147 W29'
_chemical_formula_weight         8907.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-03-09 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                96.152(2)
_cell_angle_beta                 104.376(2)
_cell_angle_gamma                116.764(2)
_cell_formula_units_Z            2
_cell_length_a                   19.533(2)
_cell_length_b                   20.652(2)
_cell_length_c                   25.774(3)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.22
_cell_volume                     8699.6(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.1360
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44392
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.716
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.914
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1509 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.3992.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.400
_exptl_crystal_description       block
_exptl_crystal_F_000             7742
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         4.600
_refine_diff_density_min         -5.501
_refine_diff_density_rms         0.572
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         30618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1041P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18044
_reflns_number_total             30618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01243a2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7046699.cif.'
_cod_original_cell_volume        8699.8(17)
_cod_database_code               7046699
_shelx_estimated_absorpt_t_max   0.097
_shelx_estimated_absorpt_t_min   0.046
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: K6(0.5) K7(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C8(H8)
;
_shelx_shelxl_version_number     2018/1
_olex2_submission_special_instructions 'No special instructions were received'