Effective oxygen activation on polyoxometalate-based hybrids for epoxidation of alkenes.
Bai, Xue; Zhu, Maochun; Liu, Yifei; Xing, Min; Ji, Xiaoying; Zhang, Ange; Yang, Yanli; Lu, Ying; Liu, Shuxia; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6875–6880; doi:10.1039/d4dt00530a

data_7715709
_publ_section_title
;
 Effective oxygen activation on polyoxometalate-based hybrids for
 epoxidation of alkenes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6875
_journal_page_last               6880
_journal_paper_doi               10.1039/d4dt00530a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'O40 P W12, C18 H20 Co N14 O3, 3(H2 O)'
_chemical_formula_sum            'C18 H27 Co N14 O46 P W12'
_chemical_formula_weight         3471.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2024-01-22 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.403(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0651(8)
_cell_length_b                   18.4692(11)
_cell_length_c                   23.0933(16)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.017
_cell_measurement_theta_min      2.376
_cell_volume                     5562.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66938
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.427
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    25.140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    4.144
_exptl_crystal_description       block
_exptl_crystal_F_000             6120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.081
_exptl_transmission_factor_min   0.015
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         9806
_refine_ls_number_restraints     558
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0149P)^2^+106.9604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7599
_reflns_number_total             9806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00530a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715708--7715709.cif.'
_cod_database_code               7715709
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 13
3. Others
 Fixed Sof: W11(0.82) W11B(0.18)
4.a Riding coordinates:
 O44(H44A,H44B)
4.b Free rotating group:
 O45(H45A,H45B), O46(H46A,H46B)
4.c Rotating group:
 O3(H3A,H3B), O1(H1A,H1B), O2(H2A,H2B)
4.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C17(H17), C11(H11), C18(H18), C12(H12), C8(H8), C9(H9),
 C16(H16), C7(H7), C1(H1), C2(H2), C10(H10), C4(H4)
;
_shelx_res_checksum              79798
_olex2_submission_special_instructions 'No special instructions were received'