#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:44:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180234 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/20/7112004.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_7112004
loop_
_publ_author_name
'Mariyatra B. Mahimaidoss'
'Sergey A. Krasnikov'
'Lukas Reck'
'Camelia I. Onet'
'John M. Breen'
'Nianyong Zhu'
'Bartosz Marzec'
'Igor V. Shvets'
'Wolfgang Schmitt'
_publ_section_title
;
 Homologous size-extension of hybrid vanadate capsules - solid state
 structures, solution stability and surface deposition
;
_journal_name_full               Chem.Commun.
_journal_page_first              2265
_journal_paper_doi               10.1039/c3cc48541b
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C56 H122 N6 Na6 O84 P8 V10'
_chemical_formula_sum            'C56 H122 N6 Na6 O84 P8 V10'
_chemical_formula_weight         3118.69
_chemical_name_systematic
;

 ?

;
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4314(6)
_cell_length_b                   12.4314(6)
_cell_length_c                   43.467(4)
_cell_measurement_reflns_used    7647
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4023
_cell_measurement_theta_min      2.1586
_cell_volume                     6717.4(8)
_computing_cell_refinement       SAINT
_computing_data_collection       'SMART APEX software'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX I CCD'
_diffrn_measurement_method       'omega or psi scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            86381
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         0.937
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.875436
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.383
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

 w=1/[σ²(Fo²)+(0.1807P)²+21.3835P]

 where P=(Fo²+2Fc²)/3

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2647
_refine_ls_wR_factor_ref         0.2810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3406
_reflns_number_total             4259
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3cc48541b.txt
_cod_data_source_block           V10O18L'4
_cod_original_cell_volume        6717.4(9)
_cod_database_code               7112004
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;

The symmetry employed for this shelxl refinement is uniquely defined

by the following loop, which should always be used as a source of

symmetry information in preference to the above space-group names.

They are only intended as comments.

;
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.59981(6) 0.68394(6) 0.81043(2) 0.0230(3) Uani 1 1 d . . . . .
V2 V 0.5000 0.5000 0.77976(3) 0.0186(3) Uani 1 4 d S T P . .
P3 P 0.40826(10) 0.80311(10) 0.84814(3) 0.0226(3) Uani 1 1 d . . . . .
C1 C 0.4083(5) 0.8211(4) 0.88912(9) 0.0408(15) Uani 1 1 d DG . . . .
C2 C 0.5002(5) 0.8528(8) 0.90492(13) 0.034(3) Uiso 0.3333 1 d DG . P A 1
H2 H 0.5643 0.8688 0.8939 0.041 Uiso 0.3333 1 calc R U P A 1
C3 C 0.4984(6) 0.8612(9) 0.93680(13) 0.036(3) Uiso 0.3333 1 d DG . P A 1
H3 H 0.5612 0.8829 0.9476 0.043 Uiso 0.3333 1 calc R U P A 1
C4 C 0.4046(7) 0.8378(6) 0.95289(9) 0.086(4) Uani 1 1 d DG . . A .
C5 C 0.3127(6) 0.8060(10) 0.93709(14) 0.038(4) Uiso 0.3333 1 d DG . P A 1
H5 H 0.2486 0.7901 0.9481 0.045 Uiso 0.3333 1 calc R U P A 1
C6 C 0.3146(5) 0.7977(9) 0.90520(13) 0.033(3) Uiso 0.3333 1 d DG . P A 1
H6 H 0.2518 0.7760 0.8944 0.040 Uiso 0.3333 1 calc R U P A 1
C2' C 0.5076(11) 0.7942(12) 0.9052(3) 0.035(3) Uiso 0.3333 1 d D . P A 2
H2' H 0.5706 0.7710 0.8947 0.042 Uiso 0.3333 1 calc R U P A 2
C3' C 0.5031(13) 0.8054(15) 0.9376(4) 0.052(5) Uiso 0.3333 1 d D . P A 2
H3' H 0.5656 0.7913 0.9496 0.063 Uiso 0.3333 1 calc R U P A 2
C5' C 0.3198(14) 0.8665(19) 0.9370(4) 0.058(5) Uiso 0.3333 1 d D . P A 2
H5' H 0.2554 0.8910 0.9465 0.069 Uiso 0.3333 1 calc R U P A 2
C6' C 0.3303(12) 0.8587(14) 0.9061(3) 0.038(4) Uiso 0.3333 1 d D . P A 2
H6' H 0.2705 0.8853 0.8948 0.045 Uiso 0.3333 1 calc R U P A 2
C3" C 0.4456(18) 0.9203(16) 0.9369(4) 0.076(7) Uiso 0.3333 1 d D . P A 3
H3" H 0.4690 0.9857 0.9460 0.092 Uiso 0.3333 1 calc R U P A 3
C2" C 0.4501(14) 0.8998(13) 0.9060(4) 0.054(5) Uiso 0.3333 1 d D . P A 3
H2" H 0.4902 0.9511 0.8946 0.065 Uiso 0.3333 1 calc R U P A 3
C6" C 0.336(2) 0.759(2) 0.9065(5) 0.075(8) Uiso 0.3333 1 d D . P A 3
H6" H 0.2903 0.7091 0.8964 0.090 Uiso 0.3333 1 calc R U P A 3
C5" C 0.332(2) 0.769(3) 0.9381(6) 0.094(10) Uiso 0.3333 1 d D . P A 3
H5" H 0.2807 0.7297 0.9497 0.112 Uiso 0.3333 1 calc R U P A 3
C7 C 0.4025(13) 0.8410(9) 0.98589(16) 0.113(5) Uani 1 1 d . . . . .
O1 O 0.6500(3) 0.7651(3) 0.78560(9) 0.0316(8) Uani 1 1 d . . . . .
O2 O 0.4602(2) 0.6363(2) 0.79387(7) 0.0199(6) Uani 1 1 d . . . . .
O3 O 0.5000 0.5000 0.74267(14) 0.0267(14) Uani 1 4 d S T P . .
O4 O 0.7067(3) 0.6668(3) 0.84248(7) 0.0280(8) Uani 1 1 d . . . . .
O5 O 0.5247(3) 0.7772(3) 0.83983(8) 0.0287(8) Uani 1 1 d . . . . .
O6 O 0.3684(3) 0.9044(3) 0.83285(8) 0.0315(8) Uani 1 1 d . . . . .
O7 O 0.5000 1.0000 0.78903(11) 0.0290(10) Uani 1 2 d S T P . .
O8 O 0.3457(6) 0.3847(5) 0.6882(2) 0.096(3) Uani 1 1 d . . . . .
O9 O 0.3480(7) 0.5492(7) 0.5958(3) 0.136(4) Uani 1 1 d . . . . .
O10 O 0.7196(4) 1.0633(4) 0.75558(11) 0.0519(12) Uiso 1 1 d . . . . .
O11 O 0.2888(4) 0.0886(3) 0.85621(14) 0.0549(13) Uani 1 1 d . . . . .
O12 O 0.175(6) 1.050(6) 1.0000 0.33(4) Uiso 0.5 2 d S . P . .
O13 O 0.5000 0.5000 0.6291(18) 0.53(5) Uiso 1 4 d S . P . .
Na1 Na 0.59574(17) 0.90426(17) 0.7500 0.0343(7) Uani 1 2 d S T P . .
Na2 Na 0.5000 0.5000 0.68522(14) 0.0633(16) Uani 1 4 d S T P . .
N1 N 0.5000 0.5000 0.8492(2) 0.066(4) Uani 1 4 d S T P . .
N2 N 0.5000 0.5000 0.8749(3) 0.170(13) Uani 1 4 d S T P . .
N3 N 0.5000 0.5000 0.9027(3) 0.095(6) Uani 1 4 d S T P . .
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'
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'
Na Na 0.0362 0.0249 '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'
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 O4 106.62(18) . .
O1 V1 O5 104.57(18) . .
O4 V1 O5 85.58(15) . .
O1 V1 O2 106.63(16) . .
O4 V1 O2 146.52(15) . .
O5 V1 O2 89.82(14) . .
O1 V1 O2 103.62(17) . 4_565
O4 V1 O2 90.27(14) . 4_565
O5 V1 O2 151.52(15) . 4_565
O2 V1 O2 78.28(18) . 4_565
O1 V1 V2 110.52(14) . .
O4 V1 V2 122.21(11) . .
O5 V1 V2 123.88(11) . .
O2 V1 V2 39.12(9) . .
O2 V1 V2 39.18(9) 4_565 .
O3 V2 O2 109.16(10) . 4_565
O3 V2 O2 109.16(10) . 3_655
O2 V2 O2 141.68(19) 4_565 3_655
O3 V2 O2 109.16(10) . 2_665
O2 V2 O2 83.82(6) 4_565 2_665
O2 V2 O2 83.82(6) 3_655 2_665
O3 V2 O2 109.16(10) . .
O2 V2 O2 83.82(6) 4_565 .
O2 V2 O2 83.82(6) 3_655 .
O2 V2 O2 141.69(19) 2_665 .
O3 V2 V1 117.13(3) . .
O2 V2 V1 42.14(9) 4_565 .
O2 V2 V1 116.24(10) 3_655 .
O2 V2 V1 116.58(10) 2_665 .
O2 V2 V1 41.69(10) . .
O3 V2 V1 117.13(3) . 4_565
O2 V2 V1 41.69(9) 4_565 4_565
O2 V2 V1 116.58(10) 3_655 4_565
O2 V2 V1 42.14(10) 2_665 4_565
O2 V2 V1 116.24(10) . 4_565
V1 V2 V1 78.00(2) . 4_565
O3 V2 V1 117.13(3) . 2_665
O2 V2 V1 116.24(10) 4_565 2_665
O2 V2 V1 42.14(9) 3_655 2_665
O2 V2 V1 41.69(10) 2_665 2_665
O2 V2 V1 116.58(10) . 2_665
V1 V2 V1 125.74(6) . 2_665
V1 V2 V1 78.00(2) 4_565 2_665
O3 V2 V1 117.13(3) . 3_655
O2 V2 V1 116.58(10) 4_565 3_655
O2 V2 V1 41.69(9) 3_655 3_655
O2 V2 V1 116.24(10) 2_665 3_655
O2 V2 V1 42.14(10) . 3_655
V1 V2 V1 78.00(2) . 3_655
V1 V2 V1 125.74(6) 4_565 3_655
V1 V2 V1 78.00(2) 2_665 3_655
O6 P3 O5 112.6(2) . .
O6 P3 O4 112.4(2) . 3_655
O5 P3 O4 111.9(2) . 3_655
O6 P3 C1 109.5(2) . .
O5 P3 C1 105.1(2) . .
O4 P3 C1 104.8(2) 3_655 .
C2 C1 C6 120.0 . .
C2" C1 C6" 110.9(14) . .
C6' C1 C2' 116.1(10) . .
C6' C1 P3 127.3(8) . .
C2" C1 P3 129.8(10) . .
C2 C1 P3 121.7(4) . .
C6 C1 P3 118.2(3) . .
C6" C1 P3 117.7(11) . .
C2' C1 P3 116.6(7) . .
C3 C2 C1 120.0 . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C2 C3 C4 120.0 . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.0 . .
C3" C4 C5" 118.3(16) . .
C5' C4 C7 120.3(12) . .
C3" C4 C7 120.3(11) . .
C5 C4 C7 119.1(8) . .
C3 C4 C7 120.8(8) . .
C5" C4 C7 117.7(13) . .
C5' C4 C3' 121.0(11) . .
C7 C4 C3' 118.7(11) . .
C4 C5 C6 120.0 . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 C1 120.0 . .
C5 C6 H6 120.0 . .
C1 C6 H6 120.0 . .
C3' C2' C1 114.9(13) . .
C3' C2' H2' 122.6 . .
C1 C2' H2' 122.6 . .
C2' C3' C4 121.0(14) . .
C2' C3' H3' 119.5 . .
C4 C3' H3' 119.5 . .
C4 C5' C6' 115.2(16) . .
C4 C5' H5' 122.4 . .
C6' C5' H5' 122.4 . .
C1 C6' C5' 131.3(15) . .
C1 C6' H6' 114.4 . .
C5' C6' H6' 114.4 . .
C4 C3" C2" 112.5(18) . .
C4 C3" H3" 123.7 . .
C2" C3" H3" 123.7 . .
C1 C2" C3" 131.6(19) . .
C1 C2" H2" 114.2 . .
C3" C2" H2" 114.2 . .
C5" C6" C1 121(2) . .
C5" C6" H6" 119.7 . .
C1 C6" H6" 119.7 . .
C6" C5" C4 119(2) . .
C6" C5" H5" 120.4 . .
C4 C5" H5" 120.4 . .
C7 C7 C4 178.1(7) 10_557 .
V1 O1 Na1 140.6(2) . .
V2 O2 V1 99.19(14) . .
V2 O2 V1 98.68(14) . 3_655
V1 O2 V1 137.04(16) . 3_655
V2 O3 Na2 180.0 . .
P3 O4 V1 135.7(2) 4_565 .
P3 O5 V1 136.9(2) . .
Na1 O7 Na1 89.55(19) 2_675 .
O7 Na1 O7 90.46(19) . 7_456
O7 Na1 O1 92.35(12) . .
O7 Na1 O1 161.80(9) 7_456 .
O7 Na1 O1 161.80(9) . 8_666
O7 Na1 O1 92.35(12) 7_456 8_666
O1 Na1 O1 90.6(2) . 8_666
O7 Na1 O10 81.09(12) . .
O7 Na1 O10 88.97(13) 7_456 .
O1 Na1 O10 109.23(16) . .
O1 Na1 O10 80.99(15) 8_666 .
O7 Na1 O10 88.97(13) . 8_666
O7 Na1 O10 81.09(12) 7_456 8_666
O1 Na1 O10 80.99(15) . 8_666
O1 Na1 O10 109.23(16) 8_666 8_666
O10 Na1 O10 165.9(3) . 8_666
O7 Na1 Na1 45.23(9) . 2_675
O7 Na1 Na1 45.23(9) 7_456 2_675
O1 Na1 Na1 134.71(11) . 2_675
O1 Na1 Na1 134.71(11) 8_666 2_675
O10 Na1 Na1 82.95(13) . 2_675
O10 Na1 Na1 82.95(13) 8_666 2_675
O8 Na2 O8 173.8(5) . 2_665
O8 Na2 O8 89.84(3) . 4_565
O8 Na2 O8 89.83(3) 2_665 4_565
O8 Na2 O8 89.83(3) . 3_655
O8 Na2 O8 89.83(3) 2_665 3_655
O8 Na2 O8 173.8(5) 4_565 3_655
O8 Na2 O13 93.1(3) . .
O8 Na2 O13 93.1(3) 2_665 .
O8 Na2 O13 93.1(3) 4_565 .
O8 Na2 O13 93.1(3) 3_655 .
O8 Na2 O3 86.9(3) . .
O8 Na2 O3 86.9(3) 2_665 .
O8 Na2 O3 86.9(3) 4_565 .
O8 Na2 O3 86.9(3) 3_655 .
O13 Na2 O3 180.0 . .
N1 N2 N3 180.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.604(4) .
V1 O4 1.937(3) .
V1 O5 1.962(4) .
V1 O2 1.970(3) .
V1 O2 1.984(3) 4_565
V1 V2 2.9232(10) .
V2 O3 1.612(6) .
V2 O2 1.868(3) 4_565
V2 O2 1.868(3) 3_655
V2 O2 1.868(3) 2_665
V2 O2 1.868(3) .
V2 V1 2.9232(10) 4_565
V2 V1 2.9232(10) 2_665
V2 V1 2.9232(10) 3_655
P3 O6 1.508(4) .
P3 O5 1.527(4) .
P3 O4 1.538(4) 3_655
P3 C1 1.795(4) .
C1 C6' 1.307(12) .
C1 C2" 1.330(13) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C1 C6" 1.403(14) .
C1 C2' 1.456(12) .
C2 C3 1.3900 .
C2 H2 0.9500 .
C3 C4 1.3900 .
C3 H3 0.9500 .
C4 C5' 1.310(13) .
C4 C3" 1.340(14) .
C4 C5 1.3900 .
C4 C5" 1.397(15) .
C4 C7 1.435(8) .
C4 C3' 1.450(13) .
C5 C6 1.3900 .
C5 H5 0.9500 .
C6 H6 0.9500 .
C2' C3' 1.419(13) .
C2' H2' 0.9500 .
C3' H3' 0.9500 .
C5' C6' 1.351(13) .
C5' H5' 0.9500 .
C6' H6' 0.9500 .
C3" C2" 1.366(14) .
C3" H3" 0.9500 .
C2" H2" 0.9500 .
C6" C5" 1.382(14) .
C6" H6" 0.9500 .
C5" H5" 0.9500 .
C7 C7 1.227(14) 10_557
O1 Na1 2.417(4) .
O2 V1 1.984(3) 3_655
O3 Na2 2.497(9) .
O4 P3 1.538(4) 4_565
O7 Na1 2.390(4) 2_675
O7 Na1 2.390(4) .
O8 Na2 2.398(7) .
O10 Na1 2.518(5) .
O13 Na2 2.44(8) .
Na1 O7 2.390(4) 7_456
Na1 O1 2.417(4) 8_666
Na1 O10 2.518(5) 8_666
Na1 Na1 3.366(6) 2_675
Na2 O8 2.398(7) 2_665
Na2 O8 2.398(7) 4_565
Na2 O8 2.398(7) 3_655
N1 N2 1.116(18) .
N2 N3 1.212(18) .
