Oxygen atom transfer with organofunctionalized polyoxovanadium clusters: O-atom vacancy formation with tertiary phosphines and deoxygenation of styrene oxide
Petel, Brittney E.; Meyer, Rachel L.; Brennessel, William W.; Matson, Ellen; Chemical Science  (2019) –; doi:10.1039/C9SC02882J

data_1552111
_publ_section_title
;
 Oxygen atom transfer with organofunctionalized polyoxovanadium clusters:
 O-atom vacancy formation with tertiary phosphines and deoxygenation of
 styrene oxide
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02882J
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H49 O19 P V6'
_chemical_formula_sum            'C25 H49 O19 P V6'
_chemical_formula_weight         990.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-04
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-06 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.004(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0627(8)
_cell_length_b                   10.8304(7)
_cell_length_c                   16.9545(12)
_cell_measurement_reflns_used    9161
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      77.1520
_cell_measurement_theta_min      4.9040
_cell_volume                     1931.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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     32.00  59.00   0.50    5.00    --   49.87  77.00 -60.00   54
  2  \w     41.00  67.00   0.50    5.00    --   49.87  57.00 -60.00   52
  3  \w     85.00 116.00   0.50    5.00    --   49.87  77.00 -30.00   62
  4  \w     90.00 118.00   0.50    5.00    --   49.87  77.00 -90.00   56
  5  \w     96.00 121.00   0.50    5.00    --   49.87  77.00 -60.00   50
  6  \w    121.00 149.00   0.50   20.00    --  105.75 108.00   0.00   56
  7  \w    144.00 173.00   0.50   20.00    --  105.75  77.00 -60.00   58
  8  \w    137.00 167.00   0.50   20.00    --  105.75  61.00   0.00   60
  9  \w    127.00 176.00   0.50   20.00    --  105.75  30.00  60.00   98
 10  \w    107.00 175.00   0.50   20.00    --  105.75  61.00  30.00  136
 11  \w     92.00 138.00   0.50   20.00    --  105.75  61.00 -90.00   92
 12  \w     97.00 171.00   0.50   20.00    --  105.75  61.00 -30.00  148
 13  \w     96.00 132.00   0.50   20.00    --  105.75  61.00   0.00   72
 14  \w     94.00 150.00   0.50   20.00    --  105.75  61.00 -60.00  112
 15  \w     86.00 119.00   0.50   20.00    --  105.75  77.00-120.00   66
 16  \w     85.00 112.00   0.50   20.00    --  105.75  77.00 -60.00   54
 17  \w     86.00 121.00   0.50   20.00    --  105.75  77.00 -30.00   70
 18  \w     86.00 176.00   0.50   20.00    --  105.75  77.00   0.00  180
 19  \w     86.00 178.00   0.50   20.00    --  105.75  77.00 -90.00  184
 20  \w     57.00  94.00   0.50   20.00    --  105.75-108.00 -96.00   74
 21  \w     59.00  87.00   0.50   20.00    --  105.75 -94.00 -30.00   56
 22  \w     61.00 103.00   0.50   20.00    --  105.75 -94.00   0.00   84
 23  \w     39.00 109.00   0.50   20.00    --  105.75 -94.00 -90.00  140
 24  \w     39.00  72.00   0.50   20.00    --  105.75 -30.00 -60.00   66
 25  \w     35.00  71.00   0.50   20.00    --  105.75 -30.00-120.00   72
 26  \w     35.00  88.00   0.50   20.00    --  105.75 -45.00 -60.00  106
 27  \w     52.00  85.00   0.50    5.00    --   49.87  19.00 -60.00   66
 28  \w     31.00  61.00   0.50    5.00    --   49.87  77.00 -90.00   60
 29  \w     33.00  64.00   0.50    5.00    --   49.87  77.00 -30.00   62
 30  \w     37.00  65.00   0.50   20.00    --  105.75 -30.00  60.00   56
 31  \w     39.00  70.00   0.50   20.00    --  105.75 -30.00 120.00   62
 32  \w     23.00  55.00   0.50    5.00    --   49.87-108.00 -96.00   64
 33  \w     36.00  90.00   0.50   20.00    --  105.75 -45.00-120.00  108
 34  \w     39.00  74.00   0.50   20.00    --  105.75 -45.00-150.00   70
 35  \w     36.00  66.00   0.50   20.00    --  105.75 -30.00 -90.00   60
 36  \w    -84.00   1.00   0.50    5.00    --  -49.87 108.00   0.00  170
 37  \w    -73.00 -48.00   0.50   20.00    --  -84.25 108.00   0.00   50
 38  \w    -80.00 -44.00   0.50    5.00    --  -49.87 -38.00  30.00   72
 39  \w    -75.00 -33.00   0.50    5.00    --  -49.87 -77.00  30.00   84
 40  \w    -75.00 -37.00   0.50    5.00    --  -49.87 -57.00 -60.00   76
 41  \w    -89.00 -47.00   0.50    5.00    --  -49.87 -38.00 -30.00   84
 42  \w    -90.00 -65.00   0.50   20.00    --  -84.25 -74.00  -9.24   50
 43  \w    -92.00 -61.00   0.50   20.00    --  -84.25 -82.00  44.11   62
 44  \w    -91.00 -64.00   0.50   20.00    --  -84.25 -83.00  -3.63   54
 45  \w    -88.00 -63.00   0.50   20.00    --  -84.25 -77.00 -30.00   50
 46  \w    -90.00 -63.00   0.50   20.00    --  -84.25 -77.00  21.54   54
 47  \w    -88.00 -63.00   0.50   20.00    --  -84.25 -77.00  30.00   50
 48  \w    -87.00 -62.00   0.50   20.00    --  -84.25 -81.00  19.39   50
 49  \w    -88.00 -63.00   0.50   20.00    --  -84.25 -77.00   0.00   50
 50  \w    -93.00 -66.00   0.50   20.00    --  -84.25 -71.00 -47.41   54
 51  \w    -90.00 -65.00   0.50   20.00    --  -84.25 -73.00 -80.93   50
 52  \w    -90.00 -65.00   0.50   20.00    --  -84.25 -80.00 -63.55   50
 53  \w    -91.00 -66.00   0.50   20.00    --  -84.25 -70.00 -59.15   50
 54  \w    -88.00 -63.00   0.50   20.00    --  -84.25 -77.00 -60.00   50
 55  \w    -88.00 -63.00   0.50   20.00    --  -84.25 -77.00 -90.00   50
 56  \w   -105.00 -80.00   0.50    5.00    --  -49.87 -57.00 -60.00   50
 57  \w    -93.00 -68.00   0.50   20.00    --  -84.25 -66.00 -37.78   50
 58  \w   -114.00 -80.00   0.50    5.00    --  -49.87 -77.00  30.00   68
 59  \w   -131.00-106.00   0.50   20.00    --  -84.25-108.00 -96.00   50
 60  \w   -135.00-110.00   0.50   20.00    --  -84.25 -77.00 -30.00   50
 61  \w   -154.00-129.00   0.50   20.00    --  -84.25 -80.00 -63.55   50
 62  \w   -149.00-124.00   0.50   20.00    --  -84.25 -70.00 -59.15   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1063523000
_diffrn_orient_matrix_UB_12      -0.0259418000
_diffrn_orient_matrix_UB_13      0.0385960000
_diffrn_orient_matrix_UB_21      -0.1002990000
_diffrn_orient_matrix_UB_22      0.0188502000
_diffrn_orient_matrix_UB_23      -0.0852382000
_diffrn_orient_matrix_UB_31      0.0072213000
_diffrn_orient_matrix_UB_32      -0.1387090000
_diffrn_orient_matrix_UB_33      -0.0189734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1184
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27440
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.437
_diffrn_reflns_theta_min         4.202
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.702
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.532
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.011
_refine_diff_density_max         2.028
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7696
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.1213
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1132P)^2^+25.9211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2832
_refine_ls_wR_factor_ref         0.3019
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.957
_reflns_Friedel_fraction_max     0.873
_reflns_number_gt                6053
_reflns_number_total             7696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02882j2.cif
_cod_data_source_block           matbp24
_cod_database_code               1552111
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.056
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O18-C25 \\sim O18-C25'
 with sigma of 0.01
 O13-C20 \\sim O13-C20'
 with sigma of 0.01
 O14-C21 \\sim O14-C21'
 with sigma of 0.01
 O10-C17 \\sim O10-C17'
 with sigma of 0.01
 O9-C16' \\sim O9-C16
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O13 \\sim C20 \\sim C20': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O14 \\sim C21 \\sim C21': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O9 \\sim C16 \\sim C16': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C25 \\sim C25': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
O10 \\sim C17 \\sim C17': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
 Sof(C16')=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17')=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=1-FVAR(3)
 Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 FVAR(3)
 Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(4)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16D,H16E,
 H16F), C16'(H16A,H16B,H16C), C17(H17A,H17B,H17C), C17'(H17D,H17E,H17F),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C20'(H20D,H20E,
 H20F), C21(H21A,H21B,H21C), C21'(H21D,H21E,H21F), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C25'(H25D,H25E,
 H25F)
;
_shelx_res_checksum              2836
_olex2_submission_original_sample_id matbp24
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 12.115
_oxdiff_exptl_absorpt_empirical_full_min 0.222