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_7039566
_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 H60 N12 O18 V4 W2'
_chemical_formula_weight         1280.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                100.764(9)
_cell_angle_beta                 108.148(9)
_cell_angle_gamma                100.314(9)
_cell_formula_units_Z            1
_cell_length_a                   8.4223(7)
_cell_length_b                   10.4091(8)
_cell_length_c                   11.8757(10)
_cell_measurement_temperature    200(2)
_cell_volume                     940.03(16)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13222
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.132
_exptl_absorpt_correction_T_max  0.561
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.738
_refine_diff_density_min         -2.677
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.0154(9)
_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   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0731P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                4084
_reflns_number_total             4352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02282k2.cif
_cod_data_source_block           mr183tt
_cod_depositor_comments
'Adding full bibliography for 7039566--7039567.cif.'
_cod_original_cell_volume        940.03(13)
_cod_database_code               7039566