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_7017096
_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 V4, 4(H2 O)'
_chemical_formula_sum            'C56 H64 O20 P4 V4'
_chemical_formula_weight         1384.75
_chemical_name_common
;Tetrakisdibenzylphosphinato-octaoxo-
tetravanadium(V).tetrahydrate
;
_chemical_name_systematic
;
Tetrakisdibenzylphosphinato-octaoxo-tetravanadium(V).tetrahydrate
;
_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             2011-06-25T13:18:59-00:00
_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                   22.306(4)
_cell_length_b                   22.306(4)
_cell_length_c                   12.824(2)
_cell_measurement_reflns_used    4266
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4582
_cell_measurement_theta_min      2.5827
_cell_measurement_wavelength     0.71073
_cell_volume                     6380.7(19)
_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)'
_computing_structure_solution    'SIR-2004 (Altomare et al, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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      0.224517E-2
_diffrn_orient_matrix_UB_12      0.446448E-1
_diffrn_orient_matrix_UB_13      -0.5928E-2
_diffrn_orient_matrix_UB_21      -0.195418E-2
_diffrn_orient_matrix_UB_22      -0.331127E-2
_diffrn_orient_matrix_UB_23      -0.776944E-1
_diffrn_orient_matrix_UB_31      -0.44732E-1
_diffrn_orient_matrix_UB_32      0.238545E-2
_diffrn_orient_matrix_UB_33      0.309666E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22239
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.46
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4828
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+5.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.102
_reflns_number_gt                3503
_reflns_number_total             4828
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt11375e.txt
_cod_data_source_block           10mz512_0m
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7017096