#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:59:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179874 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/70/7017096.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7017096
loop_
_publ_author_name
'Maass, John S.'
'Chen, Zhichao'
'Zeller, Matthias'
'Luck, Rudy L.'
_publ_section_title
;
 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).
;
_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       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω 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/[σ²(Fo²)+(0.0448P)²+5.6540P] where P=(Fo²+2Fc²)/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     >2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O10 O 0.0263(4) -0.0300(6) 0.9832(6) 0.079(3) Uani 0.277(4) 1 d P
O20 O 0.1602(6) -0.2709(3) 0.7773(6) 0.044(4) Uani 0.201(7) 1 d P
O30 O 0.0112(4) -0.1836(6) 0.8872(8) 0.236(8) Uani 0.522(7) 1 d P
V1 V -0.030017(14) 0.195879(13) 0.51982(3) 0.01826(9) Uani 1 1 d .
O1 O -0.03415(6) 0.18969(6) 0.39740(12) 0.0234(3) Uani 1 1 d .
O2 O 0.04627(6) 0.22173(6) 0.54049(11) 0.0195(3) Uani 1 1 d .
O3 O -0.11450(6) 0.18088(6) 0.55609(11) 0.0198(3) Uani 1 1 d .
O4 O -0.01110(6) 0.11349(6) 0.55626(11) 0.0207(3) Uani 1 1 d .
P1 P 0.02739(2) 0.08896(2) 0.64562(4) 0.01845(11) Uani 1 1 d .
C1 C -0.02034(9) 0.05926(9) 0.74631(17) 0.0245(4) Uani 1 1 d .
H1A H 0.0052 0.0426 0.8024 0.029 Uiso 1 1 calc R
H1B H -0.0438 0.0926 0.7767 0.029 Uiso 1 1 calc R
C2 C -0.06332(9) 0.01104(9) 0.71069(16) 0.0236(4) Uani 1 1 d .
C3 C -0.11831(9) 0.02607(10) 0.66867(18) 0.0276(4) Uani 1 1 d .
H3 H -0.1286 0.0671 0.6598 0.033 Uiso 1 1 calc R
C4 C -0.15889(10) -0.01815(11) 0.63918(19) 0.0330(5) Uani 1 1 d .
H4 H -0.1968 -0.0073 0.6111 0.04 Uiso 1 1 calc R
C5 C -0.14398(11) -0.07773(11) 0.65076(19) 0.0351(5) Uani 1 1 d .
H5 H -0.172 -0.108 0.6319 0.042 Uiso 1 1 calc R
C6 C -0.08853(11) -0.09360(10) 0.6896(2) 0.0346(5) Uani 1 1 d .
H6 H -0.0779 -0.1347 0.6952 0.042 Uiso 1 1 calc R
C7 C -0.04829(10) -0.04960(9) 0.72043(19) 0.0302(5) Uani 1 1 d .
H7 H -0.0104 -0.0607 0.7482 0.036 Uiso 1 1 calc R
C8 C 0.07245(8) 0.02957(8) 0.59303(16) 0.0199(4) Uani 1 1 d .
H8A H 0.0459 0.0021 0.5537 0.024 Uiso 1 1 calc R
H8B H 0.1011 0.0472 0.5426 0.024 Uiso 1 1 calc R
C9 C 0.10754(8) -0.00696(8) 0.67133(15) 0.0187(4) Uani 1 1 d .
C10 C 0.10558(9) -0.06903(9) 0.66538(17) 0.0246(4) Uani 1 1 d .
H10 H 0.0826 -0.0877 0.6121 0.03 Uiso 1 1 calc R
C11 C 0.13674(10) -0.10431(10) 0.73618(19) 0.0323(5) Uani 1 1 d .
H11 H 0.1352 -0.1468 0.7307 0.039 Uiso 1 1 calc R
C12 C 0.16996(10) -0.07790(11) 0.81466(18) 0.0332(5) Uani 1 1 d .
H12 H 0.1911 -0.102 0.8634 0.04 Uiso 1 1 calc R
C13 C 0.17210(10) -0.01616(11) 0.82173(18) 0.0316(5) Uani 1 1 d .
H13 H 0.1947 0.0023 0.8758 0.038 Uiso 1 1 calc R
C14 C 0.14148(9) 0.01907(9) 0.75039(17) 0.0253(4) Uani 1 1 d .
H14 H 0.1437 0.0615 0.7555 0.03 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 V1 O2 103.16(7) . .
O1 V1 O2 102.31(7) . 2
O2 V1 O2 81.41(6) . 2
O1 V1 O4 99.74(7) . .
O2 V1 O4 93.54(6) . .
O2 V1 O4 157.95(6) 2 .
O1 V1 O3 99.44(7) . .
O2 V1 O3 156.33(6) . .
O2 V1 O3 87.06(5) 2 .
O4 V1 O3 89.44(5) . .
O1 V1 O2 177.40(6) . 15_556
O2 V1 O2 79.43(6) . 15_556
O2 V1 O2 78.08(5) 2 15_556
O4 V1 O2 79.89(5) . 15_556
O3 V1 O2 77.99(5) . 15_556
O1 V1 V1 96.02(5) . 2
O2 V1 V1 42.94(4) . 2
O2 V1 V1 40.83(4) 2 2
O4 V1 V1 136.22(4) . 2
O3 V1 V1 127.78(4) . 2
O2 V1 V1 85.95(3) 15_556 2
V1 O2 V1 96.23(6) . 2
V1 O2 V1 102.00(6) . 16_556
V1 O2 V1 99.73(6) 2 16_556
P1 O3 V1 130.03(8) 15_556 .
P1 O4 V1 129.73(8) . .
O3 P1 O4 113.73(7) 16_556 .
O3 P1 C8 108.24(8) 16_556 .
O4 P1 C8 107.24(9) . .
O3 P1 C1 108.67(9) 16_556 .
O4 P1 C1 109.66(9) . .
C8 P1 C1 109.22(9) . .
C2 C1 P1 114.85(15) . .
C2 C1 H1A 108.6 . .
P1 C1 H1A 108.6 . .
C2 C1 H1B 108.6 . .
P1 C1 H1B 108.6 . .
H1A C1 H1B 107.5 . .
C3 C2 C7 118.84(19) . .
C3 C2 C1 120.57(18) . .
C7 C2 C1 120.59(19) . .
C2 C3 C4 120.8(2) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C5 C4 C3 119.8(2) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 120.2(2) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C5 C6 C7 120.1(2) . .
C5 C6 H6 120 . .
C7 C6 H6 120 . .
C6 C7 C2 120.2(2) . .
C6 C7 H7 119.9 . .
C2 C7 H7 119.9 . .
C9 C8 P1 116.00(14) . .
C9 C8 H8A 108.3 . .
P1 C8 H8A 108.3 . .
C9 C8 H8B 108.3 . .
P1 C8 H8B 108.3 . .
H8A C8 H8B 107.4 . .
C10 C9 C14 118.26(18) . .
C10 C9 C8 119.02(17) . .
C14 C9 C8 122.71(17) . .
C9 C10 C11 120.9(2) . .
C9 C10 H10 119.5 . .
C11 C10 H10 119.5 . .
C12 C11 C10 120.2(2) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C13 C12 C11 119.4(2) . .
C13 C12 H12 120.3 . .
C11 C12 H12 120.3 . .
C12 C13 C14 120.3(2) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C13 C14 C9 120.80(19) . .
C13 C14 H14 119.6 . .
C9 C14 H14 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O10 O20 1.345(14) 12_557
O20 O10 1.345(14) 11_657
V1 O1 1.5786(16) .
V1 O2 1.8161(13) .
V1 O2 1.8919(13) 2
V1 O4 1.9427(13) .
V1 O3 1.9697(13) .
V1 O2 2.4392(15) 15_556
V1 V1 2.7610(8) 2
O2 V1 1.8919(13) 2
O2 V1 2.4392(15) 16_556
O3 P1 1.5258(14) 15_556
O4 P1 1.5328(14) .
P1 O3 1.5258(14) 16_556
P1 C8 1.7944(19) .
P1 C1 1.800(2) .
C1 C2 1.512(3) .
C1 H1A 0.99 .
C1 H1B 0.99 .
C2 C3 1.381(3) .
C2 C7 1.399(3) .
C3 C4 1.391(3) .
C3 H3 0.95 .
C4 C5 1.378(3) .
C4 H4 0.95 .
C5 C6 1.380(4) .
C5 H5 0.95 .
C6 C7 1.388(3) .
C6 H6 0.95 .
C7 H7 0.95 .
C8 C9 1.512(3) .
C8 H8A 0.99 .
C8 H8B 0.99 .
C9 C10 1.387(3) .
C9 C14 1.392(3) .
C10 C11 1.388(3) .
C10 H10 0.95 .
C11 C12 1.382(3) .
C11 H11 0.95 .
C12 C13 1.381(3) .
C12 H12 0.95 .
C13 C14 1.386(3) .
C13 H13 0.95 .
C14 H14 0.95 .
