Mechanistic insights into polyoxometalate self-assembly in organic solvent: conversion of a cyclic polyoxovanadate-ethoxide to its Lindqvist congener.
Meyer, Rachel L.; Love, Robert; Brennessel, William W.; Matson, Ellen M.; Chemical communications (Cambridge, England) 56 (2020) 8607–8610; doi:10.1039/d0cc03464a

data_7126781
_publ_section_title
;
 Mechanistic insights into polyoxometalate self-assembly in organic
 solvent: conversion of a cyclic polyoxovanadate-ethoxide to its Lindqvist
 congener.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8607
_journal_page_last               8610
_journal_paper_doi               10.1039/d0cc03464a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C24 H60 O18 V6'
_chemical_formula_sum            'C24 H60 O18 V6'
_chemical_formula_weight         942.36
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-13
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.36790(10)
_cell_length_b                   16.36790(10)
_cell_length_c                   16.36790(10)
_cell_measurement_reflns_used    11788
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      77.3670
_cell_measurement_theta_min      4.6750
_cell_volume                     4385.09(5)
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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   -121.00 -41.00   0.50    0.34    --  -49.87 -42.00 109.00  160
  2  \w    -65.00 -12.00   0.50    1.37    --  -84.25  42.00 -98.00  106
  3  \w     34.00  85.00   0.50    1.37    --  105.75 -42.00 109.00  102
  4  \w   -121.00 -70.00   0.50    0.34    --  -49.87-125.00 -90.00  102
  5  \w     33.00  82.00   0.50    1.37    --  105.75 -15.00 150.00   98
  6  \w     34.00 109.00   0.50    1.37    --  105.75 -94.00-150.00  150
  7  \w    114.00 173.00   0.50    1.37    --  105.75  30.00 120.00  118
  8  \w     45.00  77.00   0.50    1.37    --  105.75 -15.00   0.00   64
  9  \w     48.00  73.00   0.50    1.37    --  105.75 -45.00-150.00   50
 10  \w     34.00  71.00   0.50    1.37    --  105.75 -30.00 -30.00   74
 11  \w     36.00  71.00   0.50    1.37    --  105.75 -30.00  60.00   70
;
_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      0.0795655000
_diffrn_orient_matrix_UB_12      0.0498470000
_diffrn_orient_matrix_UB_13      -0.0064993000
_diffrn_orient_matrix_UB_21      -0.0105463000
_diffrn_orient_matrix_UB_22      0.0046581000
_diffrn_orient_matrix_UB_23      -0.0933911000
_diffrn_orient_matrix_UB_31      -0.0491286000
_diffrn_orient_matrix_UB_32      0.0797463000
_diffrn_orient_matrix_UB_33      0.0095324000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17780
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.601
_diffrn_reflns_theta_min         4.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52381
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0509P)^2^+2.1606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1482
_reflns_number_total             1567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03464a2.cif
_cod_data_source_block           matrm13
_cod_depositor_comments          'Adding full bibliography for 7126781.cif.'
_cod_original_cell_volume        4385.09(8)
_cod_database_code               7126781
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C96 H240 O72 V24 '
_shelx_estimated_absorpt_t_max   0.301
_shelx_estimated_absorpt_t_min   0.250
_reflns_odcompleteness_completeness 100.00
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              41022
_shelx_fab_checksum              61676
_olex2_submission_original_sample_id matrm13
_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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.713