Small, beautiful and magnetically exotic: {V4W2}- and {V4W4}-type polyoxometalates.
Rasmussen, Maren; Näther, Christian; van Leusen, Jan; Warzok, Ulrike; Schalley, Christoph A.; Kögerler, Paul; Bensch, Wolfgang; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10519–10522; doi:10.1039/c6dt02282k

data_7039567
_publ_section_title
;
 Small, beautiful and magnetically exotic: {V4W2}- and {V4W4}-type
 polyoxometalates.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10519
_journal_page_last               10522
_journal_paper_doi               10.1039/c6dt02282k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C16 H64 N12 O26 V4 W4'
_chemical_formula_weight         1779.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-21 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.296(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1608(7)
_cell_length_b                   12.6983(7)
_cell_length_c                   27.5889(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      52
_cell_measurement_theta_min      4
_cell_volume                     4521.3(4)
_computing_cell_refinement       'X-Area (STOE)'
_computing_data_collection       'X-Area (STOE)'
_computing_data_reduction        'X-Area (STOE)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26122
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.015
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    2.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.013
_refine_diff_density_min         -2.368
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       0.00039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         8769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                7083
_reflns_number_total             8769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02282k2.cif
_cod_data_source_block           mr222tt
_cod_depositor_comments
'Adding full bibliography for 7039566--7039567.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7039567