Pyrazine dicarboxylate-bridged arsenotungstate: synthesis, characterization, and catalytic activities in epoxidation of olefins and oxidation of alcohols.
Ma, Xinyi; He, Peipei; Xu, Baijie; Lu, Jingkun; Wan, Rong; Wu, Hechen; Wang, Yuan; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12956–12963; doi:10.1039/c9dt02436k

data_7700665
_publ_section_title
;
 Pyrazine dicarboxylate-bridged arsenotungstate: synthesis,
 characterization, and catalytic activities in epoxidation of olefins and
 oxidation of alcohols.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12956
_journal_page_last               12963
_journal_paper_doi               10.1039/c9dt02436k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H4 As6 K16 N4 O238 Pr4 W58, 13(O)'
_chemical_formula_sum            'C12 H4 As6 K16 N4 O251 Pr4 W58'
_chemical_formula_weight         16522.25
_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             2019-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-21 deposited with the CCDC.    2019-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                101.789(5)
_cell_angle_beta                 104.044(4)
_cell_angle_gamma                114.608(4)
_cell_formula_units_Z            1
_cell_length_a                   19.358(5)
_cell_length_b                   21.762(6)
_cell_length_c                   23.710(6)
_cell_measurement_reflns_used    7150
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.16
_cell_volume                     8265(4)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0739
_diffrn_reflns_av_unetI/netI     0.1578
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42561
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.468
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.548
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1409 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.3884. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7142
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.714
_refine_diff_density_min         -3.276
_refine_diff_density_rms         0.539
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1427
_refine_ls_number_reflns         29171
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16656
_reflns_number_total             29171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02436k2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7700665.cif.'
_cod_database_code               7700665
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.166
_shelx_estimated_absorpt_t_min   0.088
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O45) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O73) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq,
Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O35)
\\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(O87) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O38) \\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O56) \\sim Ueq, Uanis(O61)
\\sim Ueq, Uanis(O65) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O69) \\sim Ueq,
Uanis(O34) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O84) \\sim Ueq, Uanis(O85)
\\sim Ueq, Uanis(O89) \\sim Ueq, Uanis(O93) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O107) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O67) \\sim Ueq,
Uanis(O91) \\sim Ueq, Uanis(O100) \\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(O51)
\\sim Ueq, Uanis(O78) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O55)
\\sim Ueq, Uanis(O77) \\sim Ueq, Uanis(O103) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Others
 Fixed Sof: K8(0.5) K9(0.5) K10(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              62121
_shelx_fab_checksum              10396
_olex2_submission_special_instructions 'No special instructions were received'