Expanding molecular transition metal cubane clusters of the form [M(4)(μ(3)-O)(4)](12+): syntheses, spectroscopic and structural characterizations of molecules M(4)(μ(3)-O)(4)(O(2)P(Bn)(2))(4)(O(4)), M = V(V) and W(V).
Maass, John S.; Chen, Zhichao; Zeller, Matthias; Luck, Rudy L.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 11356–11358; doi:10.1039/c1dt11375e

data_7017097
_publ_section_title
;
 Expanding molecular transition metal cubane clusters of the form
 [M(4)(\m(3)-O)(4)](12+): syntheses, spectroscopic and structural
 characterizations of molecules M(4)(\m(3)-O)(4)(O(2)P(Bn)(2))(4)(O(4)), M
 = V(V) and W(V).
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11356
_journal_page_last               11358
_journal_paper_doi               10.1039/c1dt11375e
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C56 H56 O16 P4 W4, 3(C4 H8 O)'
_chemical_formula_sum            'C68 H80 O19 P4 W4'
_chemical_formula_weight         2060.56
_chemical_name_common
;Tetrakisdibenzylphosphinato-octaoxo-
tetratungsten(V).tristetrahydrofuran
;
_chemical_name_systematic
;
Tetrakisdibenzylphosphinato-octaoxo-tetratungsten(V).tristetrahydrofuran
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-06-25T13:09:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.771(4)
_cell_length_b                   22.771(4)
_cell_length_c                   13.107(2)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9615
_cell_measurement_theta_min      2.5299
_cell_measurement_wavelength     0.71073
_cell_volume                     6796(2)
_computing_cell_refinement       'SAINT V7.66A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.336537E-1
_diffrn_orient_matrix_UB_12      0.243559E-1
_diffrn_orient_matrix_UB_13      -0.247442E-1
_diffrn_orient_matrix_UB_21      0.21986E-1
_diffrn_orient_matrix_UB_22      -0.874432E-2
_diffrn_orient_matrix_UB_23      0.642765E-1
_diffrn_orient_matrix_UB_31      0.176827E-1
_diffrn_orient_matrix_UB_32      -0.354818E-1
_diffrn_orient_matrix_UB_33      -0.328259E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17299
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         31.11
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    6.915
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5083
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+16.8014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                4522
_reflns_number_total             5083
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt11375e.txt
_cod_data_source_block           11mz143_0m
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C68 H80 O19 P4 W4 '
_cod_database_code               7017097