#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179085 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/47/4304720.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_4304720
loop_
_publ_author_name
'Pabitra Baran Chatterjee'
'Debdas Mandal'
'Anandalok Audhya'
'Ki-Young Choi'
'Akira Endo'
'Muktimoy Chaudhury'
_publ_section_title
;
Reporting a New Class of Divanadium(V) Compounds Connected by an
Unsupported Hydroxo Bridge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3709
_journal_page_last               3718
_journal_paper_doi               10.1021/ic702286h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C40 H45 F6 N4 O9 P V2'
_chemical_formula_weight         972.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3764(8)
_cell_length_b                   12.4181(8)
_cell_length_c                   12.6910(8)
_cell_measurement_reflns_used    5158
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5575
_cell_measurement_theta_min      2.3005
_cell_volume                     2096.5(2)
_computing_cell_refinement       'SMART (Brucker, 1999)'
_computing_data_collection       'SMART (Brucker, 1999)'
_computing_data_reduction        'SAINT-plus (bruker, 1999)'
_computing_molecular_graphics    'Ortep-3 for windows(Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD dffractometer'
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21182
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.9414
_exptl_absorpt_correction_T_min  0.8030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5238
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0606P)²+2.0280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                3514
_reflns_number_total             5238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702286h-file002.cif
_cod_data_source_block           MC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304720
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V -0.49843(4) 0.33624(4) 0.52863(3) 0.03502(15) Uani 1 1 d D . .
P1 P 0.0000 0.5000 0.5000 0.0448(3) Uani 1 2 d S . .
F1 F -0.11178(16) 0.5178(2) 0.44609(18) 0.0793(7) Uani 1 1 d . . .
F2 F 0.03903(19) 0.4982(2) 0.38735(17) 0.0915(8) Uani 1 1 d . . .
F3 F 0.0180(2) 0.62518(19) 0.5052(3) 0.0981(8) Uani 1 1 d . . .
O1 O -0.49189(16) 0.20699(17) 0.53548(15) 0.0461(5) Uani 1 1 d . . .
O2 O -0.63504(14) 0.34668(15) 0.49742(14) 0.0389(4) Uani 1 1 d . . .
O3 O -0.47216(15) 0.37186(17) 0.66817(14) 0.0433(5) Uani 1 1 d . . .
O4 O -0.5000 0.5000 0.5000 0.0280(5) Uani 1 2 d SD . .
HO4 H -0.560(3) 0.494(2) 0.464(5) 0.07(2) Uiso 0.50 1 d PD . .
O5 O -0.7982(2) -0.2031(3) 0.3024(3) 0.0888(9) Uani 1 1 d . . .
N1 N -0.49009(17) 0.33189(17) 0.36743(16) 0.0344(5) Uani 1 1 d . . .
N2 N -0.34626(18) 0.36374(19) 0.51669(17) 0.0378(5) Uani 1 1 d . . .
C1 C -0.6923(2) 0.2872(2) 0.4273(2) 0.0342(6) Uani 1 1 d . . .
C2 C -0.7900(2) 0.2609(2) 0.4459(2) 0.0435(7) Uani 1 1 d . . .
H2 H -0.8148 0.2829 0.5082 0.052 Uiso 1 1 calc R . .
C3 C -0.8499(2) 0.2022(3) 0.3721(3) 0.0523(8) Uani 1 1 d . . .
H3 H -0.9148 0.1840 0.3855 0.063 Uiso 1 1 calc R . .
C4 C -0.8151(3) 0.1696(3) 0.2779(3) 0.0552(8) Uani 1 1 d . . .
H4 H -0.8558 0.1288 0.2292 0.066 Uiso 1 1 calc R . .
C5 C -0.7203(2) 0.1979(3) 0.2572(2) 0.0481(7) Uani 1 1 d . . .
H5 H -0.6978 0.1780 0.1931 0.058 Uiso 1 1 calc R . .
C6 C -0.6564(2) 0.2566(2) 0.3310(2) 0.0366(6) Uani 1 1 d . . .
C7 C -0.5608(2) 0.2933(2) 0.3025(2) 0.0378(6) Uani 1 1 d . . .
H7 H -0.552(2) 0.294(2) 0.232(3) 0.045 Uiso 1 1 d . . .
C8 C -0.3960(2) 0.3703(3) 0.3306(2) 0.0436(7) Uani 1 1 d . . .
H8A H -0.3966 0.4481 0.3240 0.052 Uiso 1 1 calc R . .
H8B H -0.3866 0.3392 0.2623 0.052 Uiso 1 1 calc R . .
C9 C -0.3130(2) 0.3347(3) 0.4133(2) 0.0465(7) Uani 1 1 d . . .
H9A H -0.3025 0.2576 0.4091 0.056 Uiso 1 1 calc R . .
H9B H -0.2506 0.3710 0.4031 0.056 Uiso 1 1 calc R . .
C10 C -0.2852(2) 0.4118(2) 0.5861(2) 0.0411(6) Uani 1 1 d . . .
H10 H -0.219(2) 0.425(3) 0.572(2) 0.049 Uiso 1 1 d . . .
C11 C -0.3081(2) 0.4476(2) 0.6893(2) 0.0374(6) Uani 1 1 d . . .
C12 C -0.2348(2) 0.5031(3) 0.7543(2) 0.0470(7) Uani 1 1 d . . .
H12 H -0.1729 0.5174 0.7301 0.056 Uiso 1 1 calc R . .
C13 C -0.2528(3) 0.5369(3) 0.8539(2) 0.0527(8) Uani 1 1 d . . .
H13 H -0.2037 0.5744 0.8963 0.063 Uiso 1 1 calc R . .
C14 C -0.3442(3) 0.5149(3) 0.8905(2) 0.0504(8) Uani 1 1 d . . .
H14 H -0.3560 0.5375 0.9580 0.061 Uiso 1 1 calc R . .
C15 C -0.4185(2) 0.4598(2) 0.8283(2) 0.0422(6) Uani 1 1 d . . .
H15 H -0.4797 0.4451 0.8539 0.051 Uiso 1 1 calc R . .
C16 C -0.4008(2) 0.4266(2) 0.7272(2) 0.0351(6) Uani 1 1 d . . .
C17 C -0.7887(4) -0.1219(4) 0.3779(4) 0.0910(14) Uani 1 1 d . . .
H17A H -0.7782 -0.0529 0.3450 0.109 Uiso 1 1 calc R . .
H17B H -0.7323 -0.1361 0.4306 0.109 Uiso 1 1 calc R . .
C18 C -0.8841(5) -0.1218(5) 0.4273(5) 0.119(2) Uani 1 1 d . . .
H18A H -0.8810 -0.1720 0.4862 0.143 Uiso 1 1 calc R . .
H18B H -0.8990 -0.0505 0.4527 0.143 Uiso 1 1 calc R . .
C19 C -0.9604(4) -0.1558(5) 0.3411(4) 0.0985(16) Uani 1 1 d . . .
H19A H -0.9904 -0.0941 0.3030 0.118 Uiso 1 1 calc R . .
H19B H -1.0130 -0.1980 0.3684 0.118 Uiso 1 1 calc R . .
C20 C -0.9009(3) -0.2228(4) 0.2714(4) 0.0837(13) Uani 1 1 d . . .
H20A H -0.9159 -0.2986 0.2795 0.100 Uiso 1 1 calc R . .
H20B H -0.9176 -0.2032 0.1977 0.100 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
O1 V1 O3 100.70(10) . . ?
O1 V1 O2 97.44(10) . . ?
O3 V1 O2 106.20(9) . . ?
O1 V1 N1 91.10(9) . . ?
O3 V1 N1 160.97(9) . . ?
O2 V1 N1 86.78(9) . . ?
O1 V1 O4 172.28(7) . . ?
O3 V1 O4 85.95(7) . . ?
O2 V1 O4 84.31(6) . . ?
N1 V1 O4 81.48(6) . . ?
O1 V1 N2 96.85(10) . . ?
O3 V1 N2 86.60(9) . . ?
O2 V1 N2 158.63(9) . . ?
N1 V1 N2 77.13(9) . . ?
O4 V1 N2 79.51(7) . . ?
F2 P1 F2 180.000(1) . 3_566 ?
F2 P1 F3 90.69(16) . 3_566 ?
F2 P1 F3 89.31(16) 3_566 3_566 ?
F2 P1 F3 89.31(16) . . ?
F2 P1 F3 90.69(16) 3_566 . ?
F3 P1 F3 180.0 3_566 . ?
F2 P1 F1 90.14(13) . 3_566 ?
F2 P1 F1 89.86(13) 3_566 3_566 ?
F3 P1 F1 90.78(14) 3_566 3_566 ?
F3 P1 F1 89.22(14) . 3_566 ?
F2 P1 F1 89.86(13) . . ?
F2 P1 F1 90.14(13) 3_566 . ?
F3 P1 F1 89.22(14) 3_566 . ?
F3 P1 F1 90.78(14) . . ?
F1 P1 F1 180.0 3_566 . ?
C1 O2 V1 126.44(17) . . ?
C16 O3 V1 136.19(17) . . ?
V1 O4 V1 180.0 . 3_466 ?
C17 O5 C20 109.5(4) . . ?
C7 N1 C8 121.1(2) . . ?
C7 N1 V1 122.38(18) . . ?
C8 N1 V1 116.41(17) . . ?
C10 N2 C9 119.7(2) . . ?
C10 N2 V1 125.6(2) . . ?
C9 N2 V1 114.36(18) . . ?
O2 C1 C2 120.0(2) . . ?
O2 C1 C6 120.2(2) . . ?
C2 C1 C6 119.7(2) . . ?
C3 C2 C1 119.9(3) . . ?
C2 C3 C4 121.1(3) . . ?
C5 C4 C3 119.5(3) . . ?
C4 C5 C6 121.2(3) . . ?
C5 C6 C1 118.6(3) . . ?
C5 C6 C7 119.4(3) . . ?
C1 C6 C7 121.7(2) . . ?
N1 C7 C6 124.9(2) . . ?
N1 C8 C9 106.0(2) . . ?
N2 C9 C8 106.2(2) . . ?
N2 C10 C11 125.7(3) . . ?
C12 C11 C16 118.8(3) . . ?
C12 C11 C10 119.0(3) . . ?
C16 C11 C10 122.2(3) . . ?
C13 C12 C11 120.9(3) . . ?
C12 C13 C14 119.8(3) . . ?
C13 C14 C15 121.0(3) . . ?
C14 C15 C16 119.4(3) . . ?
O3 C16 C15 119.1(3) . . ?
O3 C16 C11 120.6(2) . . ?
C15 C16 C11 120.3(3) . . ?
O5 C17 C18 105.8(4) . . ?
C19 C18 C17 104.2(5) . . ?
C18 C19 C20 103.1(4) . . ?
O5 C20 C19 107.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.609(2) . ?
V1 O3 1.8233(18) . ?
V1 O2 1.833(2) . ?
V1 N1 2.061(2) . ?
V1 O4 2.0655(5) . ?
V1 N2 2.085(2) . ?
P1 F2 1.573(2) . ?
P1 F2 1.573(2) 3_566 ?
P1 F3 1.573(2) 3_566 ?
P1 F3 1.573(2) . ?
P1 F1 1.593(2) 3_566 ?
P1 F1 1.593(2) . ?
O2 C1 1.335(3) . ?
O3 C16 1.336(3) . ?
O4 V1 2.0655(5) 3_466 ?
O5 C17 1.388(6) . ?
O5 C20 1.410(5) . ?
N1 C7 1.281(4) . ?
N1 C8 1.468(3) . ?
N2 C10 1.284(4) . ?
N2 C9 1.473(3) . ?
C1 C2 1.391(4) . ?
C1 C6 1.411(4) . ?
C2 C3 1.376(4) . ?
C3 C4 1.388(5) . ?
C4 C5 1.367(5) . ?
C5 C6 1.405(4) . ?
C6 C7 1.439(4) . ?
C8 C9 1.511(4) . ?
C10 C11 1.446(4) . ?
C11 C12 1.396(4) . ?
C11 C16 1.400(4) . ?
C12 C13 1.377(4) . ?
C13 C14 1.379(5) . ?
C14 C15 1.384(4) . ?
C15 C16 1.392(4) . ?
C17 C18 1.480(7) . ?
C18 C19 1.478(7) . ?
C19 C20 1.502(7) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 O2 C1 -44.5(2) . . . . ?
O3 V1 O2 C1 -148.0(2) . . . . ?
N1 V1 O2 C1 46.2(2) . . . . ?
O4 V1 O2 C1 127.9(2) . . . . ?
N2 V1 O2 C1 87.1(3) . . . . ?
O1 V1 O3 C16 117.2(3) . . . . ?
O2 V1 O3 C16 -141.7(3) . . . . ?
N1 V1 O3 C16 -10.2(5) . . . . ?
O4 V1 O3 C16 -58.8(3) . . . . ?
N2 V1 O3 C16 20.9(3) . . . . ?
O1 V1 O4 V1 -70(55) . . . 3_466 ?
O3 V1 O4 V1 80(55) . . . 3_466 ?
O2 V1 O4 V1 -173(55) . . . 3_466 ?
N1 V1 O4 V1 -86(55) . . . 3_466 ?
N2 V1 O4 V1 -7(55) . . . 3_466 ?
O1 V1 N1 C7 68.0(2) . . . . ?
O3 V1 N1 C7 -163.3(3) . . . . ?
O2 V1 N1 C7 -29.4(2) . . . . ?
O4 V1 N1 C7 -114.1(2) . . . . ?
N2 V1 N1 C7 164.8(2) . . . . ?
O1 V1 N1 C8 -108.8(2) . . . . ?
O3 V1 N1 C8 19.8(4) . . . . ?
O2 V1 N1 C8 153.8(2) . . . . ?
O4 V1 N1 C8 69.05(19) . . . . ?
N2 V1 N1 C8 -12.06(19) . . . . ?
O1 V1 N2 C10 -114.1(2) . . . . ?
O3 V1 N2 C10 -13.7(2) . . . . ?
O2 V1 N2 C10 114.2(3) . . . . ?
N1 V1 N2 C10 156.3(3) . . . . ?
O4 V1 N2 C10 72.8(2) . . . . ?
O1 V1 N2 C9 73.0(2) . . . . ?
O3 V1 N2 C9 173.3(2) . . . . ?
O2 V1 N2 C9 -58.7(3) . . . . ?
N1 V1 N2 C9 -16.61(19) . . . . ?
O4 V1 N2 C9 -100.16(20) . . . . ?
V1 O2 C1 C2 146.7(2) . . . . ?
V1 O2 C1 C6 -37.4(3) . . . . ?
O2 C1 C2 C3 178.1(3) . . . . ?
C6 C1 C2 C3 2.2(4) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C2 C3 C4 C5 -1.2(5) . . . . ?
C3 C4 C5 C6 2.0(5) . . . . ?
C4 C5 C6 C1 -0.7(4) . . . . ?
C4 C5 C6 C7 -174.4(3) . . . . ?
O2 C1 C6 C5 -177.3(2) . . . . ?
C2 C1 C6 C5 -1.4(4) . . . . ?
O2 C1 C6 C7 -3.8(4) . . . . ?
C2 C1 C6 C7 172.1(3) . . . . ?
C8 N1 C7 C6 -178.2(3) . . . . ?
V1 N1 C7 C6 5.1(4) . . . . ?
C5 C6 C7 N1 -168.3(3) . . . . ?
C1 C6 C7 N1 18.2(4) . . . . ?
C7 N1 C8 C9 -140.4(3) . . . . ?
V1 N1 C8 C9 36.5(3) . . . . ?
C10 N2 C9 C8 -133.1(3) . . . . ?
V1 N2 C9 C8 40.2(3) . . . . ?
N1 C8 C9 N2 -47.0(3) . . . . ?
C9 N2 C10 C11 178.2(3) . . . . ?
V1 N2 C10 C11 5.6(4) . . . . ?
N2 C10 C11 C12 -177.2(3) . . . . ?
N2 C10 C11 C16 4.2(5) . . . . ?
C16 C11 C12 C13 -0.1(4) . . . . ?
C10 C11 C12 C13 -178.8(3) . . . . ?
C11 C12 C13 C14 0.6(5) . . . . ?
C12 C13 C14 C15 -0.4(5) . . . . ?
C13 C14 C15 C16 -0.3(5) . . . . ?
V1 O3 C16 C15 164.2(2) . . . . ?
V1 O3 C16 C11 -17.6(4) . . . . ?
C14 C15 C16 O3 178.9(3) . . . . ?
C14 C15 C16 C11 0.8(4) . . . . ?
C12 C11 C16 O3 -178.7(3) . . . . ?
C10 C11 C16 O3 -0.1(4) . . . . ?
C12 C11 C16 C15 -0.6(4) . . . . ?
C10 C11 C16 C15 178.1(3) . . . . ?
C20 O5 C17 C18 23.5(6) . . . . ?
O5 C17 C18 C19 -31.9(6) . . . . ?
C17 C18 C19 C20 27.2(6) . . . . ?
C17 O5 C20 C19 -5.9(5) . . . . ?
C18 C19 C20 O5 -13.9(6) . . . . ?
