#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209000.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_7209000
loop_
_publ_author_name
'Zhang, Tian-Zhan'
'Zhang, Zhi-Ming'
'Lu, Ying'
'Fu, Hai'
'Wang, En-Bo'
_publ_section_title
;
 Expansion of sodalite-type metal--organic frameworks with heterometallic
 metal--oxo cluster and its cation exchange property
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              459
_journal_paper_doi               10.1039/c2ce26400e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C16.5 H17.5 N1.5 Na O9.5 V'
_chemical_formula_weight         462.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   20.463(4)
_cell_length_b                   20.463(4)
_cell_length_c                   27.880(7)
_cell_measurement_reflns_used    20457
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      1.36
_cell_volume                     10110(4)
_computing_cell_refinement       auto
_computing_data_collection       auto
_computing_data_reduction        auto
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20457
_diffrn_reflns_theta_full        27.70
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4266
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                3559
_reflns_number_total             5212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26400e.txt
_cod_data_source_block           1
_cod_original_cell_volume        10111(3)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C16.50 H17.50 N1.50 Na O9.50 V'
_cod_database_code               7209000
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
V1 V 0.411901(18) 0.098582(18) 0.120184(12) 0.01830(10) Uani 1 1 d .
Na1 Na 0.39915(5) 0.28033(5) 0.13472(3) 0.0308(2) Uani 1 1 d .
C1 C 0.24457(12) -0.12733(12) 0.03103(7) 0.0293(5) Uani 1 1 d .
H1A H 0.2879 -0.1014 0.0125 0.035 Uiso 1 1 calc R
C2 C 0.30926(11) -0.03094(11) 0.09438(7) 0.0235(4) Uani 1 1 d .
C3 C 0.11975(12) -0.23163(12) 0.04161(7) 0.0289(5) Uani 1 1 d .
H3A H 0.0782 -0.2750 0.0298 0.035 Uiso 1 1 calc R
C4 C 0.18264(11) -0.19122(11) 0.01253(7) 0.0274(5) Uani 1 1 d .
C5 C 0.24282(11) -0.10159(11) 0.07675(7) 0.0266(5) Uani 1 1 d .
C6 C 0.58324(11) 0.17007(11) 0.11739(7) 0.0229(4) Uani 1 1 d .
C7 C 0.58875(11) 0.29575(11) 0.12075(8) 0.0245(5) Uani 1 1 d .
H7A H 0.5363 0.2703 0.1204 0.029 Uiso 1 1 calc R
C8 C 0.62643(11) 0.25484(10) 0.12099(8) 0.0234(5) Uani 1 1 d .
C9 C 0.05044(12) -0.25286(12) 0.11917(7) 0.0273(5) Uani 1 1 d .
C10 C 0.17916(11) -0.14134(11) 0.10508(7) 0.0279(5) Uani 1 1 d .
H10A H 0.1772 -0.1235 0.1354 0.033 Uiso 1 1 calc R
C11 C 0.11823(11) -0.20784(11) 0.08820(7) 0.0261(5) Uani 1 1 d .
C12 C 0.18459(12) -0.21324(12) -0.03856(7) 0.0270(5) Uani 1 1 d .
O1 O 0.61340(8) 0.13323(8) 0.12818(6) 0.0351(4) Uani 1 1 d .
O2 O 0.30009(7) 0.01197(8) 0.12355(5) 0.0260(3) Uani 1 1 d .
O3 O 0.51607(7) 0.14182(7) 0.09999(5) 0.0259(3) Uani 1 1 d .
O4 O 0.37403(8) -0.01170(8) 0.07976(5) 0.0274(3) Uani 1 1 d .
O5 O 0.40076(8) 0.15778(8) 0.15147(5) 0.0290(3) Uani 1 1 d .
O6 O 0.05621(7) -0.22687(8) 0.16159(5) 0.0281(3) Uani 1 1 d .
O7 O -0.00501(9) -0.30924(9) 0.10290(6) 0.0487(5) Uani 1 1 d .
O8 O 0.12235(8) -0.26754(8) -0.05443(5) 0.0300(3) Uani 1 1 d .
O9 O 0.24333(9) -0.17899(9) -0.06147(5) 0.0400(4) Uani 1 1 d .
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'
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'
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
O5 V1 O3 110.70(7) . .
O5 V1 O6 99.67(7) . 14
O3 V1 O6 85.02(6) . 14
O5 V1 O8 100.41(7) . 12
O3 V1 O8 87.29(6) . 12
O6 V1 O8 159.92(6) 14 12
O5 V1 O2 96.21(6) . .
O3 V1 O2 153.09(6) . .
O6 V1 O2 90.61(6) 14 .
O8 V1 O2 87.89(6) 12 .
O5 V1 O4 155.71(6) . .
O3 V1 O4 93.44(5) . .
O6 V1 O4 84.55(6) 14 .
O8 V1 O4 77.41(6) 12 .
O2 V1 O4 59.68(5) . .
O5 V1 C2 126.25(7) . .
O3 V1 C2 122.93(6) . .
O6 V1 C2 88.79(6) 14 .
O8 V1 C2 79.89(6) 12 .
O2 V1 C2 30.26(6) . .
O4 V1 C2 29.50(6) . .
O5 V1 Na1 54.90(5) . 13
O3 V1 Na1 156.33(5) . 13
O6 V1 Na1 79.91(4) 14 13
O8 V1 Na1 112.57(5) 12 13
O2 V1 Na1 45.95(4) . 13
O4 V1 Na1 103.10(4) . 13
C2 V1 Na1 75.14(5) . 13
O7 Na1 O9 92.63(7) 2 12
O7 Na1 O1 110.85(7) 2 3_665
O9 Na1 O1 86.65(6) 12 3_665
O7 Na1 O2 82.77(6) 2 13
O9 Na1 O2 175.39(6) 12 13
O1 Na1 O2 95.10(6) 3_665 13
O7 Na1 O5 132.75(7) 2 .
O9 Na1 O5 74.66(5) 12 .
O1 Na1 O5 113.48(6) 3_665 .
O2 Na1 O5 108.40(6) 13 .
O7 Na1 O5 76.65(6) 2 13
O9 Na1 O5 116.31(6) 12 13
O1 Na1 O5 156.04(6) 3_665 13
O2 Na1 O5 62.56(5) 13 13
O5 Na1 O5 69.60(5) . 13
O7 Na1 V1 68.30(5) 2 13
O9 Na1 V1 140.33(5) 12 13
O1 Na1 V1 132.13(5) 3_665 13
O2 Na1 V1 37.30(3) 13 13
O5 Na1 V1 92.79(4) . 13
O5 Na1 V1 27.71(3) 13 13
C5 C1 C4 120.99(19) . .
O4 C2 O2 119.27(18) . .
O4 C2 C5 120.61(18) . .
O2 C2 C5 120.08(18) . .
O4 C2 V1 64.36(10) . .
O2 C2 V1 55.15(9) . .
C5 C2 V1 171.65(15) . .
C4 C3 C11 120.78(19) . .
C1 C4 C3 118.78(19) . .
C1 C4 C12 119.15(18) . .
C3 C4 C12 122.05(18) . .
C1 C5 C10 119.73(18) . .
C1 C5 C2 119.22(18) . .
C10 C5 C2 121.04(18) . .
O1 C6 O3 124.58(18) . .
O1 C6 C8 120.38(18) . .
O3 C6 C8 114.93(17) . .
C8 C7 C8 120.72(19) 3_665 .
C7 C8 C7 119.28(19) 2_655 .
C7 C8 C6 119.90(17) 2_655 .
C7 C8 C6 120.63(18) . .
O7 C9 O6 125.53(19) . .
O7 C9 C11 120.05(18) . .
O6 C9 C11 114.41(18) . .
C5 C10 C11 120.08(19) . .
C10 C11 C3 119.48(18) . .
C10 C11 C9 120.60(18) . .
C3 C11 C9 119.90(18) . .
O9 C12 O8 125.6(2) . .
O9 C12 C4 119.27(19) . .
O8 C12 C4 115.13(17) . .
C6 O1 Na1 151.66(14) . 2_655
C2 O2 V1 94.59(11) . .
C2 O2 Na1 158.62(13) . 13
V1 O2 Na1 96.75(5) . 13
C6 O3 V1 141.02(13) . .
C2 O4 V1 86.14(12) . .
V1 O5 Na1 135.82(8) . .
V1 O5 Na1 97.38(6) . 13
Na1 O5 Na1 110.40(5) . 13
C9 O6 V1 130.94(13) . 15_445
C9 O7 Na1 134.15(14) . 3
C12 O8 V1 128.73(13) . 11
C12 O9 Na1 137.11(16) . 11
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.5988(14) .
V1 O3 1.9385(14) .
V1 O6 1.9836(14) 14
V1 O8 2.0048(14) 12
V1 O2 2.0808(14) .
V1 O4 2.2836(14) .
V1 C2 2.527(2) .
V1 Na1 3.4097(10) 13
Na1 O7 2.3044(17) 2
Na1 O9 2.3082(18) 12
Na1 O1 2.3433(17) 3_665
Na1 O2 2.4678(16) 13
Na1 O5 2.5674(17) .
Na1 O5 2.8131(17) 13
Na1 V1 3.4097(10) 13
C1 C5 1.386(3) .
C1 C4 1.387(3) .
C2 O4 1.247(2) .
C2 O2 1.278(2) .
C2 C5 1.488(3) .
C3 C4 1.391(3) .
C3 C11 1.393(3) .
C4 C12 1.500(3) .
C5 C10 1.387(3) .
C6 O1 1.227(2) .
C6 O3 1.290(2) .
C6 C8 1.506(3) .
C7 C8 1.379(3) 3_665
C7 C8 1.393(3) .
C8 C7 1.379(3) 2_655
C9 O7 1.231(2) .
C9 O6 1.278(2) .
C9 C11 1.497(3) .
C10 C11 1.390(3) .
C12 O9 1.225(2) .
C12 O8 1.280(2) .
O1 Na1 2.3433(17) 2_655
O2 Na1 2.4678(16) 13
O5 Na1 2.8131(17) 13
O6 V1 1.9837(14) 15_445
O7 Na1 2.3044(17) 3
O8 V1 2.0048(14) 11
O9 Na1 2.3082(18) 11
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 636.4 14.4
2 -0.010 0.485 -0.012 3234.6 73.1
3 0.333 0.667 0.667 637.2 14.5
4 0.667 0.333 0.333 637.1 14.5
