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_7704071
_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         'C24 H60 Cl1 O18 V6'
_chemical_formula_sum            'C24 H60 Cl O18 V6'
_chemical_formula_weight         977.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-09-07
_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                90
_cell_angle_beta                 107.866(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7617(7)
_cell_length_b                   17.7653(9)
_cell_length_c                   10.9667(7)
_cell_measurement_reflns_used    2544
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      75.6040
_cell_measurement_theta_min      4.9260
_cell_volume                     1995.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (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      223.00(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 0.984
_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     52.00  78.00   0.50    0.05    --   49.62  46.00  20.00   52
  2  \w     81.00 122.00   0.50    0.05    --   49.62  46.00  20.00   82
  3  \w   -154.00-116.00   0.50    0.09    --  -84.25 -46.00-128.00   76
  4  \w    123.00 177.00   0.50    0.09    --  105.75  46.00  20.00  108
  5  \w    116.00 174.00   0.50    0.09    --  105.75  99.00-120.00  116
  6  \w     37.00 106.00   0.50    0.09    --  105.75 -84.00  26.00  138
  7  \w    -84.00 -47.00   0.50    0.05    --  -49.62 -46.00-128.00   74
  8  \w   -119.00 -92.00   0.50    0.05    --  -49.62 -46.00-128.00   54
  9  \w   -121.00 -73.00   0.50    0.05    --  -49.62-125.00 150.00   96
 10  \w     -4.00  21.00   0.50    0.05    --  -49.62  19.00 150.00   50
 11  \w    -14.00  11.00   0.50    0.05    --   49.62 -19.00  30.00   50
 12  \w    100.00 164.00   0.50    0.09    --  105.75  15.00 -60.00  128
 13  \w     48.00  73.00   0.50    0.09    --  105.75 -61.00 -90.00   50
 14  \w     40.00  74.00   0.50    0.09    --  105.75 -61.00-180.00   68
 15  \w     74.00 102.00   0.50    0.09    --  105.75 -94.00 -30.00   56
 16  \w    138.00 174.00   0.50    0.09    --  105.75  15.00   0.00   72
 17  \w     41.00  67.00   0.50    0.09    --  105.75 -61.00 150.00   52
 18  \w    104.00 133.00   0.50    0.09    --  105.75  45.00   0.00   58
 19  \w    151.00 176.00   0.50    0.09    --  105.75  45.00   0.00   50
 20  \w    114.00 153.00   0.50    0.09    --  105.75  30.00-120.00   78
 21  \w     98.00 126.00   0.50    0.09    --  105.75  15.00   0.00   56
 22  \w     51.00  77.00   0.50    0.09    --  105.75 -61.00 -30.00   52
 23  \w     36.00  78.00   0.50    0.09    --  105.75 -61.00-150.00   84
 24  \w     35.00  78.00   0.50    0.09    --  105.75 -61.00  30.00   86
 25  \w   -121.00 -88.00   0.50    0.05    --  -49.87 -46.00-128.00   66
 26  \w   -118.00 -82.00   0.50    0.05    --  -49.87-125.00  30.00   72
 27  \w    -46.00  15.00   0.50    0.05    --  -49.87  46.00  20.00  122
 28  \w    -12.00  13.00   0.50    0.05    --   49.87 -19.00  60.00   50
 29  \w     50.00  80.00   0.50    0.09    --  105.75 -61.00 -60.00   60
 30  \w     49.00  75.00   0.50    0.09    --  105.75 -61.00  60.00   52
 31  \w    111.00 137.00   0.50    0.09    --  105.75  15.00 150.00   52
 32  \w     61.00  88.00   0.50    0.09    --  105.75 -94.00  90.00   54
 33  \w     98.00 170.00   0.50    0.09    --  105.75  30.00  90.00  144
 34  \w     35.00  78.00   0.50    0.09    --  105.75 -61.00  90.00   86
 35  \w    106.00 135.00   0.50    0.09    --  105.75  15.00-180.00   58
 36  \w    150.00 175.00   0.50    0.09    --  105.75  15.00-180.00   50
 37  \w     49.00  75.00   0.50    0.09    --  105.75 -61.00-120.00   52
 38  \w     51.00  77.00   0.50    0.09    --  105.75 -61.00 -90.00   52
 39  \w     37.00  67.00   0.50    0.09    --  105.75 -61.00 120.00   60
 40  \w    100.00 126.00   0.50    0.09    --  105.75  48.00 -62.00   52
 41  \w    -44.00 -16.00   0.50    0.05    --  -49.87  57.00  90.00   56
 42  \w     60.00  87.00   0.50    0.05    --   49.87-125.00 -30.00   54
 43  \w     44.00  71.00   0.50    0.09    --  105.75 -94.00-150.00   54
 44  \w     65.00 105.00   0.50    0.09    --  105.75 -94.00 150.00   80
 45  \w     47.00  73.00   0.50    0.09    --  105.75 -94.00  90.00   52
 46  \w     81.00 106.00   0.50    0.09    --  105.75 -94.00  90.00   50
 47  \w     53.00  79.00   0.50    0.09    --  105.75 -61.00   0.00   52
 48  \w     34.00  59.00   0.50    0.09    --  105.75 -61.00  30.00   50
 49  \w     81.00 106.00   0.50    0.09    --  105.75 -94.00 120.00   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      -0.0753410000
_diffrn_orient_matrix_UB_12      0.0367035000
_diffrn_orient_matrix_UB_13      0.0834140000
_diffrn_orient_matrix_UB_21      0.1277238000
_diffrn_orient_matrix_UB_22      0.0353746000
_diffrn_orient_matrix_UB_23      0.0854730000
_diffrn_orient_matrix_UB_31      -0.0249951000
_diffrn_orient_matrix_UB_32      0.0701525000
_diffrn_orient_matrix_UB_33      -0.0867270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            2173
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.049
_diffrn_reflns_theta_min         4.914
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             1006
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2173
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0712
_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^)+(0.1499P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1400
_reflns_number_total             2173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01077d2.cif
_cod_data_source_block           matbp32
_cod_depositor_comments
'Adding full bibliography for 7704070--7704072.cif.'
_cod_original_cell_volume        1995.5(2)
_cod_database_code               7704071
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.389
_shelx_estimated_absorpt_t_min   0.171
_diffrn_oxdiff_digest_frames
;
016bcaa00497f3789a65e58c5c20f1c1bf0336647ce
;
_diffrn_oxdiff_digest_hkl
;
01bb6dea735aa33a591d9929ed49dc081a30c1
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.641(12)
 0.359(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 V1-O1 \\sim V2-O2
 with sigma of 0.01
 V1-Cl1 \\sim V2-Cl2
 with sigma of 0.01
 O3-C1 \\sim O3-C1' \\sim O6-C7 \\sim O6-C7'
 with sigma of 0.01
 C1-C2 \\sim C1'-C2'
 with sigma of 0.01
 O3-C2 \\sim O3-C2
 with sigma of 0.02
 C7-C8 \\sim C7'-C8'
 with sigma of 0.01
 O6-C8 \\sim O6-C8'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O3 \\sim C1 \\sim C2: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
O4 \\sim C3 \\sim C4: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(C7) = Uanis(C7')
Uanis(C8) = Uanis(C8')
Uanis(O1) = Uanis(Cl1)
Uanis(O2) = Uanis(Cl2)
Uanis(C1) = Uanis(C1')
Uanis(C2) = Uanis(C2')
5. Others
 1*[Sof(O1)+Sof(Cl1)]+1*[Sof(O2)+Sof(Cl2)]=1.66667 with esd of 0.0001
 Sof(Cl1)=0.5*(1-FVAR(2))
 Sof(O1)=0.5*FVAR(2)
 Sof(Cl2)=1-FVAR(2)
 Sof(O2)=FVAR(2)
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(H2'C)=1-FVAR(3)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(3)
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=1-FVAR(4)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(4)
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 H5A(0.5) H5B(0.5) H6B(0.5) H6C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C1'(H1'A,H1'B), C7'(H7'A,
 H7'B)
6.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C2'(H2'A,
 H2'B,H2'C), C8'(H8'A,H8'B,H8'C)
;
_shelx_res_checksum              68760
_olex2_submission_original_sample_id matbp32
_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 2.011
_oxdiff_exptl_absorpt_empirical_full_min 0.631