#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:26:27 +0100 (jue 07 de nov de 2019) $
#$Revision: 223785 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/99/7049963.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_7049963
loop_
_publ_author_name
'Mulkapuri, Sateesh'
'Kurapati, Sathish Kumar'
'Das, Samar K.'
_publ_section_title
;
 Carbonate encapsulation from dissolved atmospheric CO₂ into a
 polyoxovanadate capsule.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8773
_journal_page_last               8781
_journal_paper_doi               10.1039/c9dt01103j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C H0 N6 Na6 O73 V15'
_chemical_formula_sum            'C H0 N6 Na6 O73 V15'
_chemical_formula_weight         2166.11
_chemical_name_systematic        'Compound 1'
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   None
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-02-17 deposited with the CCDC.    2019-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.9910(6)
_cell_length_b                   12.9910(6)
_cell_length_c                   23.1099(12)
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.21
_cell_measurement_theta_min      2.14
_cell_volume                     3377.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            79029
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.266
_diffrn_reflns_theta_min         2.527
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2086
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.384
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 2140 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         5165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0285
_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)+(0.0416P)²+3.2475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4927
_reflns_number_total             5165
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01103j2.cif
_cod_data_source_block           SKD13_a
_cod_depositor_comments          'Adding full bibliography for 7049963.cif.'
_cod_original_cell_volume        3377.6(4)
_cod_database_code               7049963
_shelx_shelxl_version_number     2018/1
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
V2 V -0.01375(3) -0.16956(3) 0.62993(2) 0.00704(7) Uani 1 1 d . . .
V3 V 0.22617(4) -0.02012(4) 0.67903(2) 0.00995(8) Uani 1 1 d . . .
V1 V -0.02619(5) -0.26293(5) 0.750000 0.00746(9) Uani 1 2 d S T P
Na1 Na -0.333333 -0.666667 0.68030(8) 0.0146(3) Uani 1 3 d S T P
Na3 Na 0.333333 -0.333333 0.54267(8) 0.0138(3) Uani 1 3 d S T P
Na2 Na 0.333333 -0.333333 0.68147(8) 0.0166(4) Uani 1 3 d S T P
O7 O 0.2874(2) -0.0232(2) 0.750000 0.0090(4) Uani 1 2 d S T P
O8 O 0.28949(16) 0.15091(16) 0.68204(7) 0.0105(3) Uani 1 1 d . . .
O1 O -0.0696(3) -0.1122(3) 0.750000 0.0219(6) Uani 1 2 d S T P
O3 O 0.08810(15) -0.17415(15) 0.68932(7) 0.0090(3) Uani 1 1 d . . .
O10 O -0.2364(2) -0.4987(2) 0.62038(9) 0.0187(4) Uani 1 1 d . . .
O16 O 0.000000 0.000000 0.500000 0.045(2) Uani 1 6 d S T P
O12 O 0.22637(18) -0.28654(19) 0.61255(9) 0.0185(4) Uani 1 1 d . . .
O2 O -0.0306(2) -0.3911(2) 0.750000 0.0135(4) Uani 1 2 d S T P
O5 O 0.11775(17) -0.00932(15) 0.62317(8) 0.0116(3) Uani 1 1 d . . .
O6 O 0.31323(17) -0.03854(18) 0.63477(8) 0.0139(3) Uani 1 1 d . . .
O11 O 0.1718(3) -0.4348(3) 0.750000 0.0194(5) Uani 1 2 d S T P
O14 O -0.0072(2) -0.4621(2) 0.63092(11) 0.0237(4) Uani 1 1 d . . .
O4 O -0.01320(17) -0.23703(16) 0.57089(8) 0.0139(3) Uani 1 1 d . . .
O9 O -0.1808(3) -0.6358(3) 0.750000 0.0182(5) Uani 1 2 d S T P
O13 O 0.1708(2) -0.4803(2) 0.48527(11) 0.0236(4) Uani 1 1 d . . .
O15 O 0.000000 -0.4098(2) 0.500000 0.0223(6) Uani 1 2 d S T P
N1 N 0.2140(3) -0.0588(2) 0.51259(11) 0.0217(4) Uani 1 1 d . . .
C1 C 0.000000 0.000000 0.750000 0.0121(9) Uani 1 6 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'
Na Na 0.0362 0.0249 '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'
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
O4 V2 O5 109.53(9) . 3
O4 V2 O3 113.15(9) . .
O5 V2 O3 137.08(8) 3 .
O4 V2 O5 105.90(9) . .
O5 V2 O5 92.06(11) 3 .
O3 V2 O5 80.78(8) . .
O4 V2 O8 107.87(9) . 3
O5 V2 O8 81.69(8) 3 3
O3 V2 O8 81.29(7) . 3
O5 V2 O8 145.81(8) . 3
O4 V2 V3 112.94(7) . .
O5 V2 V3 123.15(6) 3 .
O3 V2 V3 39.80(5) . .
O5 V2 V3 41.18(6) . .
O8 V2 V3 117.39(5) 3 .
O4 V2 V3 117.92(7) . 3
O5 V2 V3 41.03(6) 3 3
O3 V2 V3 110.55(5) . 3
O5 V2 V3 122.91(6) . 3
O8 V2 V3 40.83(5) 3 3
V3 V2 V3 128.88(2) . 3
O4 V2 V1 124.95(7) . .
O5 V2 V1 108.87(6) 3 .
O3 V2 V1 39.48(5) . .
O5 V2 V1 110.54(6) . .
O8 V2 V1 42.91(5) 3 .
V3 V2 V1 74.706(15) . .
V3 V2 V1 72.696(15) 3 .
O6 V3 O7 102.61(10) . .
O6 V3 O3 106.26(9) . .
O7 V3 O3 93.21(9) . .
O6 V3 O8 105.19(9) . .
O7 V3 O8 92.99(10) . .
O3 V3 O8 145.71(8) . .
O6 V3 O5 99.96(9) . .
O7 V3 O5 157.43(9) . .
O3 V3 O5 80.01(7) . .
O8 V3 O5 81.44(7) . .
O6 V3 V2 104.14(7) . .
O7 V3 V2 131.05(8) . .
O3 V3 V2 39.98(5) . .
O8 V3 V2 117.96(6) . .
O5 V3 V2 40.23(5) . .
O6 V3 V2 109.40(7) . 2
O7 V3 V2 129.72(8) . 2
O3 V3 V2 112.92(6) . 2
O8 V3 V2 42.07(5) . 2
O5 V3 V2 39.53(5) . 2
V2 V3 V2 76.814(19) . 2
O2 V1 O3 103.35(8) . 4_556
O2 V1 O3 103.35(8) . .
O3 V1 O3 92.18(10) 4_556 .
O2 V1 O8 99.73(8) . 3
O3 V1 O8 156.71(8) 4_556 3
O3 V1 O8 79.40(7) . 3
O2 V1 O8 99.73(8) . 6_556
O3 V1 O8 79.41(7) 4_556 6_556
O3 V1 O8 156.71(8) . 6_556
O8 V1 O8 99.83(10) 3 6_556
O2 V1 O1 165.98(13) . .
O3 V1 O1 86.24(8) 4_556 .
O3 V1 O1 86.24(8) . .
O8 V1 O1 71.67(7) 3 .
O8 V1 O1 71.67(7) 6_556 .
O2 V1 V2 112.249(12) . .
O3 V1 V2 123.76(6) 4_556 .
O3 V1 V2 39.03(5) . .
O8 V1 V2 41.44(5) 3 .
O8 V1 V2 131.73(5) 6_556 .
O1 V1 V2 68.973(16) . .
O2 V1 V2 112.248(12) . 4_556
O3 V1 V2 39.03(5) 4_556 4_556
O3 V1 V2 123.77(5) . 4_556
O8 V1 V2 131.73(5) 3 4_556
O8 V1 V2 41.44(5) 6_556 4_556
O1 V1 V2 68.974(16) . 4_556
V2 V1 V2 135.30(2) . 4_556
O10 Na1 O10 88.77(9) 3_545 .
O10 Na1 O10 88.77(9) 3_545 2_445
O10 Na1 O10 88.77(9) . 2_445
O10 Na1 O9 88.44(8) 3_545 .
O10 Na1 O9 102.92(8) . .
O10 Na1 O9 167.91(9) 2_445 .
O10 Na1 O9 102.92(8) 3_545 3_545
O10 Na1 O9 167.91(9) . 3_545
O10 Na1 O9 88.44(8) 2_445 3_545
O9 Na1 O9 80.73(9) . 3_545
O10 Na1 O9 167.91(9) 3_545 2_445
O10 Na1 O9 88.44(8) . 2_445
O10 Na1 O9 102.92(8) 2_445 2_445
O9 Na1 O9 80.73(9) . 2_445
O9 Na1 O9 80.73(9) 3_545 2_445
O10 Na1 Na1 126.13(7) 3_545 4_556
O10 Na1 Na1 126.13(7) . 4_556
O10 Na1 Na1 126.13(7) 2_445 4_556
O9 Na1 Na1 48.40(6) . 4_556
O9 Na1 Na1 48.40(6) 3_545 4_556
O9 Na1 Na1 48.40(6) 2_445 4_556
O12 Na3 O12 79.63(9) . 3_655
O12 Na3 O12 79.63(9) . 2_545
O12 Na3 O12 79.63(9) 3_655 2_545
O12 Na3 O13 87.37(8) . 3_655
O12 Na3 O13 100.48(8) 3_655 3_655
O12 Na3 O13 166.78(9) 2_545 3_655
O12 Na3 O13 100.48(8) . .
O12 Na3 O13 166.78(9) 3_655 .
O12 Na3 O13 87.37(8) 2_545 .
O13 Na3 O13 92.72(10) 3_655 .
O12 Na3 O13 166.78(9) . 2_545
O12 Na3 O13 87.37(8) 3_655 2_545
O12 Na3 O13 100.48(8) 2_545 2_545
O13 Na3 O13 92.72(10) 3_655 2_545
O13 Na3 O13 92.72(10) . 2_545
O12 Na3 Na2 47.68(6) . .
O12 Na3 Na2 47.68(6) 3_655 .
O12 Na3 Na2 47.68(6) 2_545 .
O13 Na3 Na2 123.32(7) 3_655 .
O13 Na3 Na2 123.32(7) . .
O13 Na3 Na2 123.32(7) 2_545 .
O12 Na2 O12 80.23(9) . 3_655
O12 Na2 O12 80.23(9) . 2_545
O12 Na2 O12 80.23(9) 3_655 2_545
O12 Na2 O11 101.08(8) . 3_655
O12 Na2 O11 96.80(8) 3_655 3_655
O12 Na2 O11 176.54(9) 2_545 3_655
O12 Na2 O11 96.80(8) . .
O12 Na2 O11 176.55(9) 3_655 .
O12 Na2 O11 101.08(8) 2_545 .
O11 Na2 O11 81.98(9) 3_655 .
O12 Na2 O11 176.54(9) . 2_545
O12 Na2 O11 101.08(8) 3_655 2_545
O12 Na2 O11 96.80(8) 2_545 2_545
O11 Na2 O11 81.98(9) 3_655 2_545
O11 Na2 O11 81.98(9) . 2_545
O12 Na2 Na2 131.93(6) . 4_556
O12 Na2 Na2 131.93(6) 3_655 4_556
O12 Na2 Na2 131.93(6) 2_545 4_556
O11 Na2 Na2 49.24(6) 3_655 4_556
O11 Na2 Na2 49.24(6) . 4_556
O11 Na2 Na2 49.24(6) 2_545 4_556
O12 Na2 Na3 48.07(6) . .
O12 Na2 Na3 48.07(6) 3_655 .
O12 Na2 Na3 48.07(6) 2_545 .
O11 Na2 Na3 130.76(6) 3_655 .
O11 Na2 Na3 130.76(6) . .
O11 Na2 Na3 130.76(6) 2_545 .
Na2 Na2 Na3 180.0 4_556 .
V3 O7 V3 127.12(14) 4_556 .
V3 O8 V2 97.10(8) . 2
V3 O8 V1 123.88(9) . 2
V2 O8 V1 95.65(8) 2 2
C1 O1 V1 129.80(19) . .
V3 O3 V2 100.22(8) . .
V3 O3 V1 138.15(9) . .
V2 O3 V1 101.49(8) . .
Na2 O12 Na3 84.25(8) . .
V2 O5 V2 146.26(11) 2 .
V2 O5 V3 99.44(8) 2 .
V2 O5 V3 98.59(8) . .
Na2 O11 Na2 81.52(12) 4_556 .
Na1 O9 Na1 83.19(12) . 4_556
O1 C1 O1 120.000(1) 3 .
O1 C1 O1 120.002(1) 3 2
O1 C1 O1 120.0 . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V2 O4 1.6236(18) .
V2 O5 1.9067(18) 3
V2 O3 1.9280(17) .
V2 O5 1.9287(18) .
V2 O8 1.9952(18) 3
V2 V3 2.9530(6) .
V2 V3 2.9550(6) 3
V2 V1 3.0002(4) .
V3 O6 1.6290(19) .
V3 O7 1.8318(11) .
V3 O3 1.9206(17) .
V3 O8 1.9469(19) .
V3 O5 1.9665(19) .
V1 O2 1.637(3) .
V1 O3 1.9464(17) 4_556
V1 O3 1.9465(17) .
V1 O8 2.0527(18) 3
V1 O8 2.0527(18) 6_556
V1 O1 2.293(3) .
Na1 O10 2.349(2) 3_545
Na1 O10 2.349(2) .
Na1 O10 2.349(2) 2_445
Na1 O9 2.426(3) .
Na1 O9 2.426(3) 3_545
Na1 O9 2.426(3) 2_445
Na1 Na1 3.221(4) 4_556
Na3 O12 2.399(2) .
Na3 O12 2.399(2) 3_655
Na3 O12 2.399(2) 2_545
Na3 O13 2.415(3) 3_655
Na3 O13 2.415(3) .
Na3 O13 2.415(3) 2_545
Na3 Na2 3.208(3) .
Na2 O12 2.384(3) .
Na2 O12 2.384(3) 3_655
Na2 O12 2.384(3) 2_545
Na2 O11 2.426(3) 3_655
Na2 O11 2.426(3) .
Na2 O11 2.426(3) 2_545
Na2 Na2 3.167(4) 4_556
O1 C1 1.275(3) .
N1 N1 1.446(5) 8_556
