Polyoxotungstates incorporated organophosphonate and nickel: synthesis, characterization and efficient catalysis for epoxidation of allylic alcohols.
Xu, Qiaofei; Li, Yingguang; Ban, Ran; Li, Zhao; Han, Xiao; Ma, Pengtao; Singh, Vikram; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13479–13486; doi:10.1039/c8dt02590h

data_7047340
_publ_section_title
;
 Polyoxotungstates incorporated organophosphonate and nickel: synthesis,
 characterization and efficient catalysis for epoxidation of allylic
 alcohols.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13479
_journal_page_last               13486
_journal_paper_doi               10.1039/c8dt02590h
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety
'0.33(C54 H72 As6 K42 N18 Ni9 O276 P18 W36), 4(O)'
_chemical_formula_sum            'C18 H24 As2 K14 N6 Ni3 O96 P6 W12'
_chemical_formula_weight         5125.82
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-06-23 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.6407(11)
_cell_length_b                   22.6407(11)
_cell_length_c                   19.7106(10)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.31
_cell_volume                     8750.0(7)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45446
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         1.038
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.507
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1683 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.4971.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.918
_exptl_crystal_description       block
_exptl_crystal_F_000             7008
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.286
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.270
_refine_ls_abs_structure_details
;
 Flack x determined using 3881 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         10385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0449P)^2^+169.1959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9330
_reflns_number_total             10385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02590h2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
'Adding full bibliography for 7047340--7047342.cif.'
_cod_original_cell_volume        8750.0(10)
_cod_database_code               7047340
_shelx_estimated_absorpt_t_max   0.195
_shelx_estimated_absorpt_t_min   0.088
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: K4(0.5) K5(0.5) K6(0.5) K7(0.5) K8(0.5) K9(0.5) K10(0.5) K11(0.5)
 K12(0.5) K13(0.5) K14(0.6) K15(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'