Site-selective halogenation of mixed-valent vanadium oxide clusters.
Maiola, Michela L.; Petel, Brittney E.; Brennessel, William W.; Matson, Ellen M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16184–16192; doi:10.1039/d0dt01077d

data_7704072
_publ_section_title
;
 Site-selective halogenation of mixed-valent vanadium oxide clusters.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16184
_journal_page_last               16192
_journal_paper_doi               10.1039/d0dt01077d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C25 H60 F3 O21 S V6'
_chemical_formula_sum            'C25 H60 F3 O21 S V6'
_chemical_formula_weight         1091.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-14
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-03-12 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                83.447(2)
_cell_angle_beta                 77.638(2)
_cell_angle_gamma                64.530(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7375(2)
_cell_length_b                   11.6187(3)
_cell_length_c                   19.2768(4)
_cell_measurement_reflns_used    14744
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5050
_cell_measurement_theta_min      2.3940
_cell_volume                     2120.16(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_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     -5.00  20.00   0.50    1.11    --  -49.62  19.00  60.00   50
  2  \w     -5.00  24.00   0.50    1.11    --  -49.62  19.00   0.00   58
  3  \w     -3.00  22.00   0.50    1.11    --  -49.62  19.00 -30.00   50
  4  \w     -5.00  22.00   0.50    1.11    --  -49.62  19.00  30.00   54
  5  \w    -31.00  20.00   0.50    1.11    --  -49.62  38.00 -60.00  102
  6  \w    -77.00 -52.00   0.50    1.11    --  -49.62 131.00-106.00   50
  7  \w    -63.00 -37.00   0.50    1.11    --  -49.62 138.00  69.00   52
  8  \w    -21.00   7.00   0.50    1.11    --   49.62 -19.00-120.00   56
  9  \w    -23.00   2.00   0.50    1.11    --   49.62 -19.00 -60.00   50
 10  \w    -22.00  10.00   0.50    1.11    --   49.62 -19.00   0.00   64
 11  \w    -21.00  11.00   0.50    1.11    --   49.62 -19.00  90.00   64
 12  \w    -23.00  11.00   0.50    1.11    --   49.62 -19.00 150.00   68
 13  \w     64.00 102.00   0.50    1.11    --   49.62-138.00   7.00   76
 14  \w     39.00  82.00   0.50    1.11    --   49.62-131.00-176.00   86
 15  \w    -97.00 -71.00   0.50    1.11    --  -49.62-131.00-176.00   52
 16  \w   -100.00 -75.00   0.50    1.11    --  -49.62-125.00-120.00   50
 17  \w    -97.00 -70.00   0.50    1.11    --  -49.62-138.00   7.00   54
 18  \w   -116.00 -78.00   0.50    1.11    --  -49.62-125.00  90.00   76
 19  \w    -40.00 -13.00   0.50    4.44    --  -84.25  45.00-120.00   54
 20  \w    -77.00 -52.00   0.50    4.44    --  -84.25 131.00-106.00   50
 21  \w   -111.00 -86.00   0.50    4.44    --  -84.25-138.00   7.00   50
 22  \w   -137.00-112.00   0.50    4.44    --  -84.25-131.00-176.00   50
 23  \w     36.00  72.00   0.50    4.44    --  105.75 -61.00 120.00   72
 24  \w     93.00 120.00   0.50    4.44    --  105.75 -77.00 120.00   54
 25  \w     82.00 121.00   0.50    4.44    --  105.75-138.00   7.00   78
 26  \w    102.00 127.00   0.50    4.44    --  105.75 -77.00   0.00   50
 27  \w     73.00 105.00   0.50    4.44    --  105.75 -94.00 -30.00   64
 28  \w     81.00 106.00   0.50    4.44    --  105.75-125.00  30.00   50
 29  \w     62.00 106.00   0.50    4.44    --  105.75 -94.00  30.00   88
 30  \w     52.00  97.00   0.50    4.44    --  105.75-125.00  90.00   90
 31  \w     42.00  72.00   0.50    4.44    --  105.75-125.00  30.00   60
 32  \w     35.00  72.00   0.50    4.44    --  105.75 -77.00   0.00   74
 33  \w     36.00  79.00   0.50    4.44    --  105.75 -61.00 -60.00   86
 34  \w     50.00  96.00   0.50    4.44    --  105.75 -77.00-120.00   92
 35  \w     90.00 116.00   0.50    4.44    --  105.75 -77.00-180.00   52
 36  \w     78.00 116.00   0.50    4.44    --  105.75-131.00-176.00   76
 37  \w     86.00 111.00   0.50    4.44    --  105.75-125.00-150.00   50
 38  \w     61.00 108.00   0.50    4.44    --  105.75-107.00-146.36   94
 39  \w     38.00  74.00   0.50    4.44    --  105.75 -61.00-180.00   72
 40  \w     45.00  70.00   0.50    4.44    --  105.75 -61.00-120.00   50
 41  \w     39.00 106.00   0.50    4.44    --  105.75 -94.00-120.00  134
 42  \w     37.00  77.00   0.50    4.44    --  105.75 -61.00   0.00   80
 43  \w     35.00 106.00   0.50    4.44    --  105.75 -94.00 -60.00  142
 44  \w     98.00 132.00   0.50    4.44    --  105.75  15.00  60.00   68
 45  \w    135.00 174.00   0.50    4.44    --  105.75  15.00  60.00   78
 46  \w    131.00 172.00   0.50    4.44    --  105.75  61.00  60.00   82
 47  \w    133.00 159.00   0.50    4.44    --  105.75  30.00   0.00   52
 48  \w    104.00 177.00   0.50    4.44    --  105.75  61.00  90.00  146
 49  \w    123.00 175.00   0.50    4.44    --  105.75  30.00 150.00  104
 50  \w    117.00 142.00   0.50    4.44    --  105.75 138.00  69.00   50
 51  \w     93.00 121.00   0.50    4.44    --  105.75  61.00  60.00   56
 52  \w     99.00 125.00   0.50    4.44    --  105.75  30.00   0.00   52
 53  \w     98.00 170.00   0.50    4.44    --  105.75  45.00 -60.00  144
 54  \w    110.00 135.00   0.50    4.44    --  105.75 131.00-106.00   50
 55  \w    100.00 161.00   0.50    4.44    --  105.75  61.00-120.00  122
 56  \w     98.00 157.00   0.50    4.44    --  105.75  45.00-150.00  118
 57  \w    102.00 168.00   0.50    4.44    --  105.75  15.00-150.00  132
 58  \w     35.00  73.00   0.50    4.44    --  105.75 -94.00-180.00   76
 59  \w     43.00 111.00   0.50    4.44    --  105.75-125.00 120.00  136
 60  \w     35.00 109.00   0.50    4.44    --  105.75-125.00 150.00  148
 61  \w     38.00  74.00   0.50    4.44    --  105.75 -77.00 120.00   72
;
_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      0.0552496000
_diffrn_orient_matrix_UB_12      -0.0845891000
_diffrn_orient_matrix_UB_13      0.0639640000
_diffrn_orient_matrix_UB_21      -0.1123075000
_diffrn_orient_matrix_UB_22      0.1030430000
_diffrn_orient_matrix_UB_23      0.0509996000
_diffrn_orient_matrix_UB_31      -0.1023482000
_diffrn_orient_matrix_UB_32      -0.0617297000
_diffrn_orient_matrix_UB_33      0.0023527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35608
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.893
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       plate
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.894
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         8882
_refine_ls_number_restraints     371
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1428P)^2^+2.5673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7347
_reflns_number_total             8882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01077d2.cif
_cod_data_source_block           matbp43
_cod_depositor_comments
'Adding full bibliography for 7704070--7704072.cif.'
_cod_database_code               7704072
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.205
_diffrn_oxdiff_digest_frames
;
014878adda3c364841cb3ba0bf1bca630000029f921
;
_diffrn_oxdiff_digest_hkl
;
017d77738b2d5980851873bbc9b03b7591b65d
;
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-S1 \\sim O1-S1'
 with sigma of 0.01
 S1-O20 \\sim S1-O21 \\sim S1'-O20' \\sim S1'-O21'
 with sigma of 0.01
 S1-C25 \\sim S1'-C25'
 with sigma of 0.01
 C25-F1 \\sim C25-F2 \\sim C25-F3 \\sim C25'-F1' \\sim C25'-F2' \\sim C25'-F3'
 with sigma of 0.01
 O10-C7 \\sim O10-C7'
 with sigma of 0.01
 C7-C8 \\sim C7'-C8'
 with sigma of 0.01
 O10-C8 \\sim O10-C8'
 with sigma of 0.02
 O13-C13 \\sim O13-C13'
 with sigma of 0.01
 C13-C14 \\sim C13'-C14'
 with sigma of 0.01
 O13-C14 \\sim O13-C14'
 with sigma of 0.02
 O15-C17 \\sim O15-C17'
 with sigma of 0.01
 C17-C18 \\sim C17'-C18'
 with sigma of 0.01
 O15-C18 \\sim O15-C18'
 with sigma of 0.02
 O16-C19 \\sim O16-C19'
 with sigma of 0.01
 C19-C20 \\sim C19'-C20'
 with sigma of 0.01
 O16-C20 \\sim O16-C20'
 with sigma of 0.02
 O17-C21 \\sim O17-C21'
 with sigma of 0.01
 C21-C22 \\sim C21'-C22'
 with sigma of 0.01
 O17-C22 \\sim O17-C22'
 with sigma of 0.02
 O18-C23 \\sim O18-C23'
 with sigma of 0.01
 C23-C24 \\sim C23'-C24'
 with sigma of 0.01
 O18-C24 \\sim O18-C24'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.4A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S1, O20, O21, C25, F1, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1', O20', O21', C25', F1', F2', F3'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1')=Sof(O20')=Sof(O21')=Sof(C25')=Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(S1)=Sof(O20)=Sof(O21)=Sof(C25)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
 Sof(C13')=Sof(H13C)=Sof(H13D)=Sof(C14')=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(3)
 Sof(C17')=Sof(H17C)=Sof(H17D)=Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(4)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(4)
 Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(5)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(5)
 Sof(C21')=Sof(H21C)=Sof(H21D)=Sof(C22')=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(6)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(6)
 Sof(C23')=Sof(H23C)=Sof(H23D)=Sof(C24')=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(7)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(7)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B), C7'(H7'A,H7'B), C13'(H13C,H13D), C17'(H17C,
 H17D), C19'(H19C,H19D), C21'(H21C,H21D), C23'(H23C,H23D)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C8'(H8'A,H8'B,H8'C), C14'(H14D,H14E,H14F), C18'(H18D,H18E,H18F),
 C20'(H20D,H20E,H20F), C22'(H22D,H22E,H22F), C24'(H24D,H24E,H24F)
;
_shelx_res_checksum              69896
_olex2_submission_original_sample_id matbp43
_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 2.223
_oxdiff_exptl_absorpt_empirical_full_min 0.401