[(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_7707796
_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 Co5 N10 O12 V2, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C62 H68 Cl4 Co5 N10 O22 V2'
_chemical_formula_weight         1843.59
_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                 106.591(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7439(9)
_cell_length_b                   12.4867(5)
_cell_length_c                   18.9773(12)
_cell_measurement_reflns_used    7290
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.7330
_cell_measurement_theta_min      3.2540
_cell_volume                     3575.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.997
_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    -20.00  33.00   1.00   20.00    --   -7.39 -99.00  60.00   53
  2  \w    -20.00  33.00   1.00   20.00    --   -7.39 -99.00 120.00   53
  3  \w    -28.00  87.00   1.00   20.00    --    8.80  19.00   0.00  115
  4  \w    -19.00  25.00   1.00   20.00    --    8.80  19.00-150.00   44
  5  \w    -60.00  31.00   1.00   20.00    --    8.80 -57.00-180.00   91
  6  \w     24.00  49.00   1.00   20.00    --    8.80 -99.00-120.00   25
;
_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      -0.0301715000
_diffrn_orient_matrix_UB_12      -0.0243918000
_diffrn_orient_matrix_UB_13      0.0166203000
_diffrn_orient_matrix_UB_21      0.0301563000
_diffrn_orient_matrix_UB_22      0.0086393000
_diffrn_orient_matrix_UB_23      0.0352342000
_diffrn_orient_matrix_UB_31      -0.0196977000
_diffrn_orient_matrix_UB_32      0.0505705000
_diffrn_orient_matrix_UB_33      0.0019878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34729
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.079
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0794 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.8091. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             1870
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6772
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0586P)^2^+9.8593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4998
_reflns_number_total             6772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01710a2.cif
_cod_data_source_block           eb17019
_cod_depositor_comments
'Adding full bibliography for 7707796--7707797.cif.'
_cod_database_code               7707796
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 N10 O10 Co Cl V'
_chemical_oxdiff_usercomment     '@ 120 K 808o'
_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
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B)
3.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)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              17330
_olex2_date_sample_data_collection 2017-01-20
_olex2_date_sample_submission    2017-01-16
_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 808o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.722