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_7047341
_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
'0.25(C72 H96 As8 K32 N24 Ni16 O344 P24 W48), 7(O)'
_chemical_formula_sum            'C18 H58 As2 K8 N6 Ni4 O93 P6 W12'
_chemical_formula_weight         4936.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.887(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.181(6)
_cell_length_b                   18.465(5)
_cell_length_c                   34.868(12)
_cell_measurement_reflns_used    7154
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.43
_cell_volume                     14355(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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  0.1038
_diffrn_reflns_av_unetI/netI     0.1280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35144
_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         1.214
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.927
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1561 before and 0.0948 after correction.
The Ratio of minimum to maximum transmission is 0.3552.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_description       block
_exptl_crystal_F_000             9040
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         3.952
_refine_diff_density_min         -2.816
_refine_diff_density_rms         0.561
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         12735
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0882
_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^)+(0.1566P)^2^+408.9906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8402
_reflns_number_total             12735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02590h2.cif
_cod_data_source_block           njy1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7047340--7047342.cif.'
_cod_original_cell_volume        14356(7)
_cod_database_code               7047341
_shelx_estimated_absorpt_t_max   0.188
_shelx_estimated_absorpt_t_min   0.103
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(K1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Others
 Fixed Sof: Ni3(0.5) K4(0.5) K5(0.5) O1W(0.5)
4.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'