[(V<sup>IV</sup>O)<sub>2</sub>MII5] (M = Ni, Co) Anderson wheels.
Fraser, Hector W. L.; Payne, Emily H.; Sarkar, Arup; Wilson, Lucinda R. B.; Mitcov, Dmitri; Nichol, Gary S.; Rajaraman, Gopalan; Piligkos, Stergios; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12495–12501; doi:10.1039/d1dt01710a

data_7707797
_publ_section_title
;
 [(V<sup>IV</sup>O)<sub>2</sub>MII5] (M = Ni, Co) Anderson wheels.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12495
_journal_page_last               12501
_journal_paper_doi               10.1039/d1dt01710a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C60 H60 Cl2 N10 Ni5 O12 V2, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C62 H68 Cl4 N10 Ni5 O22 V2'
_chemical_formula_weight         1842.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-23
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-23 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.745(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7800(3)
_cell_length_b                   12.4392(2)
_cell_length_c                   19.0165(4)
_cell_measurement_reflns_used    28878
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.6410
_cell_measurement_theta_min      3.4520
_cell_volume                     3555.16(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_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   -104.00 -57.00   1.00   10.00    --  -17.68-178.00-150.00   47
  2  \w    -92.00  14.00   1.00   10.00    --  -17.68 -77.00 120.00  106
  3  \w    -49.00  56.00   1.00   10.00    --  -17.68  77.00 -30.00  105
  4  \w   -103.00 -55.00   1.00   10.00    --  -17.68 178.00  60.00   48
  5  \w    -12.00  93.00   1.00   10.00    --   19.09  77.00-150.00  105
  6  \w    -12.00  93.00   1.00   10.00    --   19.09  77.00 -60.00  105
  7  \w    -51.00  37.00   1.00   10.00    --   19.09 -38.00 -60.00   88
  8  \w     12.00  91.00   1.00   10.00    --   19.09  38.00 150.00   79
  9  \w     38.00  64.00   1.00   10.00    --   19.09 178.00 -30.00   26
 10  \w    -18.00   9.00   1.00   10.00    --   19.09 -38.00  60.00   27
 11  \w    -19.00  58.00   1.00   10.00    --   19.09 -99.00  60.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0182721000
_diffrn_orient_matrix_UB_12      0.0018205000
_diffrn_orient_matrix_UB_13      0.0297550000
_diffrn_orient_matrix_UB_21      0.0152109000
_diffrn_orient_matrix_UB_22      0.0536453000
_diffrn_orient_matrix_UB_23      0.0076722000
_diffrn_orient_matrix_UB_31      -0.0407720000
_diffrn_orient_matrix_UB_32      0.0191996000
_diffrn_orient_matrix_UB_33      -0.0242909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            90810
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.985
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12777
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0287P)^2^+2.6346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10678
_reflns_number_total             12777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01710a2.cif
_cod_data_source_block           eb17037
_cod_depositor_comments
'Adding full bibliography for 7707796--7707797.cif.'
_cod_database_code               7707797
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C62H68Cl4Ni5N10O22V2 '
_chemical_oxdiff_usercomment     '@ 120 K 845o (ii)'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11-H11
 0.84 with sigma of 0.02
 O7-O8 \\sim O7-O9 \\sim O7-O10 \\sim O8-O9 \\sim O8-O10 \\sim O9-O10 \\sim
O9A-O10A \\sim O9A-O7A \\sim O9A-
 O8A \\sim O10A-O7A \\sim O10A-O8A \\sim O7A-O8A
 with sigma of 0.04
 Cl2-O7 \\sim Cl2-O8 \\sim Cl2-O9 \\sim Cl2-O10 \\sim Cl2-O9A \\sim Cl2-O10A
\\sim Cl2-O7A \\sim Cl2-O8A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O7, O8, O9, O10, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9A, O10A, O7A, O8A, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O9A)=Sof(O10A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              48136
_olex2_date_sample_data_collection 2017-03-17
_olex2_date_sample_submission    2017-03-16
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 845o(ii)
_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 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.804