Synthesis, characterization and catalytic epoxidation properties of lanthanide-stabilized peroxoisopolytungstates
Guo, Jipeng; Niu, Yanjun; Song, Lanying; Xu, Qiaofei; Lu, Jingkun; Ma, Pengtao; Zhang, Dongdi; Zhang, Chao; Niu, Jingyang; Wang, Jingping; Dalton Trans.  (2017) –; doi:10.1039/C7DT02471A

data_7044073
_publ_section_title
;
 Synthesis, characterization and catalytic epoxidation properties of
 lanthanide-stabilized peroxoisopolytungstates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02471A
_journal_year                    2017
_chemical_formula_moiety         'K2 Na1.3333 O124 Sm4 W29, 12.6667(O)'
_chemical_formula_sum            'H57.3333 K2 Na1.3333 O136.6667 Sm4 W29'
_chemical_formula_weight         8286.36
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   35.953(5)
_cell_length_b                   35.953(5)
_cell_length_c                   35.953(5)
_cell_measurement_reflns_used    551
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.42
_cell_measurement_theta_min      2.53
_cell_volume                     46474(11)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1578
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            114893
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.086
_diffrn_reflns_theta_max         25.086
_diffrn_reflns_theta_min         1.602
_exptl_absorpt_coefficient_mu    23.076
_exptl_absorpt_correction_T_max  0.0654
_exptl_absorpt_correction_T_min  0.0380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.553
_exptl_crystal_description       block
_exptl_crystal_F_000             43168
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.317
_refine_ls_abs_structure_details
;
 Flack x determined using 2373 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6875
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0484P)^2^+995.6187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5622
_reflns_number_total             6875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02471a3.cif
_cod_data_source_block           njy1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

2024-03-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'H172 K6 Na4 O410 Sm12 W87'
_cod_original_formula_weight         24859.08
_cod_original_formula_moiety         '0.25(K24 Na16 O1488 Sm48 W348), 38(O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        46475(19)
_cod_database_code               7044073
_shelx_estimated_absorpt_t_max   0.065
_shelx_estimated_absorpt_t_min   0.038
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O22) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O8W) \\sim Ueq,
Uanis(O9W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O7W) \\sim Ueq,
Uanis(O10W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
2. Others
 Fixed Sof: O7W(0.5) O8W(0.5) O9W(0.16667) O10W(0.5)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'