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_7715708
_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         '2(O40 P W12), C36 H40 Mn2 N28 O6, 7(H2 O)'
_chemical_formula_sum            'C36 H56 Mn2 N28 O93 P2 W24'
_chemical_formula_weight         6953.30
_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             2024-01-13
_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                 93.494(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1218(3)
_cell_length_b                   18.3926(4)
_cell_length_c                   23.5962(6)
_cell_measurement_reflns_used    10495
_cell_measurement_temperature    297
_cell_measurement_theta_max      28.6490
_cell_measurement_theta_min      2.5170
_cell_volume                     5684.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -82.82  13.18   1.20    8.00    --   -4.01 -59.25  20.08   80
  2  \w    -82.82  13.18   1.20    8.00    --   -4.01 -59.25 164.08   80
  3  \w    -82.82  13.18   1.20    8.00    --   -4.01 -59.25  92.08   80
  4  \w    -82.82  13.18   1.20    8.00    --   -4.01 -59.25 -51.92   80
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000964000
_diffrn_orient_matrix_UB_12      0.0302333000
_diffrn_orient_matrix_UB_13      0.0186404000
_diffrn_orient_matrix_UB_21      -0.0111211000
_diffrn_orient_matrix_UB_22      0.0234355000
_diffrn_orient_matrix_UB_23      -0.0234405000
_diffrn_orient_matrix_UB_31      -0.0530248000
_diffrn_orient_matrix_UB_32      -0.0048680000
_diffrn_orient_matrix_UB_33      0.0030743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83380
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.395
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.534
_exptl_absorpt_correction_T_max  0.02549
_exptl_absorpt_correction_T_min  0.00609
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.061
_exptl_crystal_description       prism
_exptl_crystal_F_000             6132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         2.298
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         11775
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0372P)^2^+118.6884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9059
_reflns_number_total             11775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00530a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715708--7715709.cif.'
_cod_database_code               7715708
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.244
_shelx_estimated_absorpt_t_min   0.120
_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. Restrained distances
 Mn1-H2A \\sim Mn1-H2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim O9 \\sim O9A \\sim O17 \\sim O17A \\sim O35 \\sim O35A \\sim O37 \\sim
O37A \\sim O38: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O9A)=Sof(O17A)=Sof(O35A)=Sof(O37A)=1-FVAR(1)
 Sof(O9)=Sof(O17)=Sof(O35)=Sof(O37)=FVAR(1)
 Fixed Sof: O23(0.5) H23A(0.5) H23B(0.5)
5.a Riding coordinates:
 O2(H2A,H2B), O41(H41A,H41B), O43(H43A,H43B), O11(H11A,H11B), O23(H23A,H23B),
 O25(H25A,H25B), O45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C10(H10), C2(H2), C17(H17), C11(H11), C1(H1), C3(H3),
 C7(H7), C13(H13), C14(H14), C19(H19), C21(H21), C22(H22)
5.c Fitted hexagon refined as free rotating group:
 N1(C12,C4,C8,C6,C10), N20(C2,C9,C17,C23,C11)
;
_shelx_res_checksum              18635
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.564
_oxdiff_exptl_absorpt_empirical_full_min 0.446