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_1552109
_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_formula_moiety         'C20 H47 O19 P V6'
_chemical_formula_sum            'C20 H47 O19 P V6'
_chemical_formula_weight         928.18
_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     dual
_audit_creation_date             2018-10-11
_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                 92.6080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.3410(3)
_cell_length_b                   10.76690(10)
_cell_length_c                   20.2152(2)
_cell_measurement_reflns_used    22439
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.5760
_cell_measurement_theta_min      2.6810
_cell_volume                     7249.32(12)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_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    -56.00  21.00   0.50    0.68    --  -49.75  38.00 -90.00  154
  2  \w    -57.00  21.00   0.50    0.68    --  -49.75  38.00-180.00  156
  3  \w    -70.00 -45.00   0.50    0.68    --  -49.75 118.00-146.00   50
  4  \w     75.00 100.00   0.50    0.68    --   49.75 160.00   5.00   50
  5  \w     51.00  76.00   0.50    0.68    --   49.75-118.00 126.00   50
  6  \w   -108.00 -83.00   0.50    0.68    --  -49.75-160.00 -25.00   50
  7  \w   -110.00 -85.00   0.50    0.68    --  -49.75-118.00 126.00   50
  8  \w   -116.00 -70.00   0.50    0.68    --  -49.75-125.00 150.00   92
  9  \w   -118.00 -90.00   0.50    0.68    --  -49.75-125.00 -90.00   56
 10  \w   -116.00 -71.00   0.50    0.68    --  -49.75-125.00-180.00   90
 11  \w    -74.00 -49.00   0.50    2.71    --  -84.25 118.00-146.00   50
 12  \w   -140.00-115.00   0.50    2.71    --  -84.25-118.00 126.00   50
 13  \w   -121.00 -96.00   0.50    2.71    --  -84.25-160.00 -25.00   50
 14  \w    116.00 160.00   0.50    2.71    --  105.75 160.00   5.00   88
 15  \w    116.00 143.00   0.50    2.71    --  105.75 118.00-146.00   54
 16  \w    109.00 135.00   0.50    2.71    --  105.75  15.00 -90.00   52
 17  \w     59.00  90.00   0.50    2.71    --  105.75 -45.00 -60.00   62
 18  \w     47.00  77.00   0.50    2.71    --  105.75 -15.00 -30.00   60
 19  \w     38.00  72.00   0.50    2.71    --  105.75 -30.00   0.00   68
 20  \w     34.00  74.00   0.50    2.71    --  105.75 -15.00  30.00   80
 21  \w     61.00  94.00   0.50    2.71    --  105.75 -77.00  90.00   66
 22  \w     72.00 113.00   0.50    2.71    --  105.75-118.00 126.00   82
 23  \w     81.00 107.00   0.50    2.71    --  105.75 -94.00 150.00   52
 24  \w     36.00 125.00   0.50    2.71    --  105.75 -77.00 120.00  178
 25  \w     56.00  90.00   0.50    2.71    --  105.75 -45.00 150.00   68
 26  \w     46.00  71.00   0.50    2.71    --  105.75 -15.00 120.00   50
 27  \w     35.00  90.00   0.50    2.71    --  105.75 -45.00  90.00  110
 28  \w     35.00  60.00   0.50    2.71    --  105.75 -94.00 150.00   50
 29  \w     35.00  78.00   0.50    2.71    --  105.75 -45.00 120.00   86
 30  \w     34.00  68.00   0.50    2.71    --  105.75 -30.00  30.00   68
 31  \w     36.00  63.00   0.50    2.71    --  105.75 -30.00 -30.00   54
 32  \w     37.00  68.00   0.50    2.71    --  105.75 -30.00 -60.00   62
 33  \w     37.00  63.00   0.50    2.71    --  105.75 -15.00 -90.00   52
 34  \w     34.00  69.00   0.50    2.71    --  105.75 -15.00-120.00   70
 35  \w     43.00  82.00   0.50    2.71    --  105.75 -45.00-180.00   78
 36  \w     70.00  95.00   0.50    2.71    --  105.75-160.00 -25.00   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      -0.0451381000
_diffrn_orient_matrix_UB_12      0.0193998000
_diffrn_orient_matrix_UB_13      -0.0163977000
_diffrn_orient_matrix_UB_21      0.0075969000
_diffrn_orient_matrix_UB_22      -0.0079249000
_diffrn_orient_matrix_UB_23      -0.0744919000
_diffrn_orient_matrix_UB_31      -0.0066025000
_diffrn_orient_matrix_UB_32      -0.1415533000
_diffrn_orient_matrix_UB_33      0.0018881000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34073
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.865
_diffrn_reflns_theta_min         2.653
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14089
_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            red-green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       needle
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+13.3859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6869
_reflns_number_total             7553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02882j2.cif
_cod_data_source_block           matbp16
_cod_database_code               1552109
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.088
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 O9-C11' \\sim O9-C11
 with sigma of 0.01
 O11-C13' \\sim O11-C13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O9 \\sim C11 \\sim C11': within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C13 \\sim C13': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
4. Others
 Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
 Sof(C13')=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(2)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C11'(H11D,H11E,H11F), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C13'(H13D,H13E,H13F), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              48821
_olex2_submission_original_sample_id matbp16
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.961
_oxdiff_exptl_absorpt_empirical_full_min 0.499