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_7044075
_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 Nd4 O124 W29, 12.6667(O)'
_chemical_formula_sum            'H57.3333 K2 Na1.3333 Nd4 O136.6667 W29'
_chemical_formula_weight         8261.92
_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                   35.972(3)
_cell_length_b                   35.972(3)
_cell_length_c                   35.972(3)
_cell_measurement_reflns_used    525
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.24
_cell_measurement_theta_min      2.53
_cell_volume                     46547(7)
_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  0.1104
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            115779
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.087
_diffrn_reflns_theta_max         25.087
_diffrn_reflns_theta_min         1.601
_exptl_absorpt_coefficient_mu    22.866
_exptl_absorpt_correction_T_max  0.1420
_exptl_absorpt_correction_T_min  0.0533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    3.537
_exptl_crystal_description       block
_exptl_crystal_F_000             43072
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.264
_refine_ls_abs_structure_details
;
 Flack x determined using 2655 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0364P)^2^+1703.2975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6028
_reflns_number_total             6885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02471a2.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 Nd12 O410 W87'
_cod_original_formula_weight         24785.76
_cod_original_formula_moiety         '0.25(K24 Na16 Nd48 O1488 W348), 38(O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        46546(13)
_cod_database_code               7044075
_shelx_estimated_absorpt_t_max   0.142
_shelx_estimated_absorpt_t_min   0.053
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O7W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O10W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
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'