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_1552110
_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         'C30 H51 O19 P V6'
_chemical_formula_sum            'C30 H51 O19 P V6'
_chemical_formula_weight         1052.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-02-03
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.72880(10)
_cell_length_b                   16.00950(10)
_cell_length_c                   18.8692(2)
_cell_measurement_reflns_used    24647
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      77.0820
_cell_measurement_theta_min      3.6100
_cell_volume                     4147.28(6)
_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(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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   -120.00 -55.00   0.50    0.25    --  -49.75 -37.00-174.00  130
  2  \w    -55.00  20.00   0.50    0.25    --  -49.75  37.00 -18.00  150
  3  \w     42.00  91.00   0.50    0.25    --   49.75  37.00 -18.00   98
  4  \w    -22.00  21.00   0.50    0.25    --   49.75 -37.00-174.00   86
  5  \w   -141.00-116.00   0.50    1.01    --  -84.25 -37.00-174.00   50
  6  \w    -54.00 -29.00   0.50    1.01    --  -84.25  37.00 -18.00   50
  7  \w    117.00 143.00   0.50    1.01    --  105.75  37.00 -18.00   52
  8  \w     41.00  67.00   0.50    1.01    --  105.75 -37.00-174.00   52
  9  \w   -121.00 -95.00   0.50    0.25    --  -49.75-125.00 -30.00   52
 10  \w     45.00  95.00   0.50    0.25    --   49.75-125.00-180.00  100
 11  \w     33.00  64.00   0.50    1.01    --  105.75 -15.00   0.00   62
 12  \w     42.00  67.00   0.50    1.01    --  105.75 -30.00  60.00   50
 13  \w     42.00 113.00   0.50    1.01    --  105.75-125.00 120.00  142
 14  \w     38.00  69.00   0.50    1.01    --  105.75 -30.00 150.00   62
 15  \w     99.00 176.00   0.50    1.01    --  105.75  15.00 -90.00  154
 16  \w     41.00  82.00   0.50    1.01    --  105.75 -15.00  60.00   82
 17  \w     87.00 117.00   0.50    1.01    --  105.75 -61.00 -30.00   60
 18  \w     34.00  82.00   0.50    1.01    --  105.75 -15.00-150.00   96
 19  \w     34.00  59.00   0.50    1.01    --  105.75 -45.00 -30.00   50
 20  \w    102.00 169.00   0.50    1.01    --  105.75  30.00  30.00  134
 21  \w     41.00  67.00   0.50    1.01    --  105.75 -94.00   0.00   52
 22  \w     77.00 107.00   0.50    1.01    --  105.75 -94.00   0.00   60
 23  \w     39.00  88.00   0.50    1.01    --  105.75 -45.00  60.00   98
 24  \w     42.00  77.00   0.50    1.01    --  105.75 -15.00 -30.00   70
 25  \w     86.00 178.00   0.50    1.01    --  105.75  77.00  90.00  184
 26  \w     38.00  82.00   0.50    1.01    --  105.75 -15.00 120.00   88
 27  \w     44.00  69.00   0.50    1.01    --  105.75 -45.00  90.00   50
 28  \w     35.00  87.00   0.50    1.01    --  105.75 -45.00   0.00  104
;
_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      0.0936006000
_diffrn_orient_matrix_UB_12      -0.0527281000
_diffrn_orient_matrix_UB_13      -0.0042987000
_diffrn_orient_matrix_UB_21      -0.0567048000
_diffrn_orient_matrix_UB_22      -0.0696502000
_diffrn_orient_matrix_UB_23      -0.0383248000
_diffrn_orient_matrix_UB_31      0.0246259000
_diffrn_orient_matrix_UB_32      0.0403887000
_diffrn_orient_matrix_UB_33      -0.0719797000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38388
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.966
_diffrn_reflns_theta_min         3.621
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29774
_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-brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 3421 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0677P)^2^+2.2501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                8252
_reflns_number_total             8699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02882j2.cif
_cod_data_source_block           matbp25
_cod_database_code               1552110
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.107
_reflns_odcompleteness_completeness 99.92
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              17910
_olex2_submission_original_sample_id matbp25
_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 2.381
_oxdiff_exptl_absorpt_empirical_full_min 0.663