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_7047342
_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_formula_moiety         'C18 H24 As2 Cs2 K5 N6 Ni4 O83 P6 W12, 10(O)'
_chemical_formula_sum            'C18 H60 As2 Cs2 K5 N6 Ni4 O93 P6 W12'
_chemical_formula_weight         5086.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-11
_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                90
_cell_formula_units_Z            8
_cell_length_a                   26.670(2)
_cell_length_b                   29.464(3)
_cell_length_c                   36.519(3)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.08
_cell_measurement_theta_min      2.36
_cell_volume                     28697(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1077
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            145052
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.518
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.346
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1637 before and 0.0696 after correction.
The Ratio of minimum to maximum transmission is 0.3135.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_description       block
_exptl_crystal_F_000             18520
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.594
_refine_diff_density_min         -2.237
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         25465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0762P)^2^+1450.3706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16129
_reflns_number_total             25465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02590h2.cif
_cod_data_source_block           njy1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7047340--7047342.cif.'
_cod_original_cell_volume        28696(4)
_cod_database_code               7047342
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.099
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: Ni4(0.6) Ni5(0.4) K3(0.5) K4(0.5) K5(0.5) K6(0.5) K7(0.5) K8(0.5)
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),
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'