#------------------------------------------------------------------------------
#$Date: 2017-02-04 15:40:53 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191545 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/71/7227153.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_7227153
loop_
_publ_author_name
'Guo, Hai-Yang'
'Zhang, Ting-Ting'
'Lin, Po-Han'
'Xiao-Zhang, Xiao-Zhang'
'Cui, Xiao-Bing'
'Huo, Qi-Sheng'
'Xu, Ji-Qing'
_publ_section_title
;
 Preparation, structure and characterization of a series of vanadates
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              265
_journal_paper_doi               10.1039/C6CE02205G
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C54 H106 Cl N36 Ni3 O53 V15'
_chemical_formula_weight         3083.42
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-13 deposited with the CCDC.
2016-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.989(2)
_cell_length_b                   14.989(2)
_cell_length_c                   28.467(6)
_cell_measurement_reflns_used    37477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.07
_cell_volume                     5538.8(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            51286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.072
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2798
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.959
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0625
_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)+(0.1050P)²+9.4157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3243
_reflns_number_total             4331
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce02205g2.cif
_cod_data_source_block           shelx_2
_cod_depositor_comments
'Adding full bibliography for 7227152--7227155.cif.'
_cod_original_cell_volume        5539.0(19)
_cod_database_code               7227153
_shelx_shelxl_version_number     2014/7
_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'
'-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'
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
Ni1 Ni 0.6667 0.3333 0.55272(3) 0.0320(3) Uani 1 3 d S T P
V3 V 0.91712(8) 0.42195(8) 0.2500 0.0309(3) Uani 1 2 d S T P
Ni2 Ni 1.0000 0.0000 0.5000 0.0467(4) Uani 1 6 d S T P
V2 V 0.74950(6) 0.17985(6) 0.30877(3) 0.0373(2) Uani 1 1 d . . .
V1 V 0.82311(6) 0.38637(6) 0.34624(3) 0.0325(2) Uani 1 1 d . . .
O7 O 0.8609(2) 0.3171(2) 0.29976(10) 0.0339(7) Uani 1 1 d . . .
O8 O 0.8954(2) 0.4973(2) 0.30115(11) 0.0337(7) Uani 1 1 d . . .
Cl1 Cl 0.6667 0.3333 0.2500 0.0433(6) Uani 1 6 d S T P
O5 O 0.8964(3) 0.4096(3) 0.39052(12) 0.0435(8) Uani 1 1 d . . .
O4 O 0.7458(3) 0.4537(3) 0.35507(11) 0.0384(7) Uani 1 1 d . . .
O3 O 0.7674(4) 0.1422(3) 0.2500 0.0369(10) Uani 1 2 d S T P
O2 O 0.7842(3) 0.1178(3) 0.34396(13) 0.0485(9) Uani 1 1 d . . .
O1 O 1.0392(4) 0.4654(4) 0.2500 0.0482(12) Uani 1 2 d S T P
N3 N 0.7769(3) 0.4528(3) 0.50917(14) 0.0376(9) Uani 1 1 d . . .
N1 N 0.5543(3) 0.2150(3) 0.59600(15) 0.0405(9) Uani 1 1 d . . .
C4 C 0.8829(4) 0.5069(4) 0.51371(19) 0.0484(12) Uani 1 1 d . . .
H4A H 0.9195 0.4996 0.5384 0.058 Uiso 1 1 calc R U .
N2 N 0.4760(5) 0.0934(4) 0.64815(19) 0.0660(15) Uani 1 1 d . . .
H2B H 0.4674 0.0520 0.6708 0.079 Uiso 1 1 calc R U .
N4 N 0.8462(4) 0.5584(4) 0.44930(16) 0.0499(11) Uani 1 1 d . . .
H4B H 0.8515 0.5902 0.4234 0.060 Uiso 1 1 calc R U .
C6 C 0.7581(4) 0.4872(4) 0.46919(18) 0.0455(12) Uani 1 1 d . . .
H6A H 0.6929 0.4647 0.4569 0.055 Uiso 1 1 calc R U .
C3 C 0.4501(5) 0.1756(5) 0.5935(2) 0.0576(15) Uani 1 1 d . . .
H3A H 0.4175 0.1977 0.5727 0.069 Uiso 1 1 calc R U .
C5 C 0.9254(5) 0.5716(5) 0.4771(2) 0.0583(15) Uani 1 1 d . . .
H5A H 0.9952 0.6165 0.4719 0.070 Uiso 1 1 calc R U .
C2 C 0.5670(5) 0.1625(5) 0.6294(2) 0.0612(16) Uani 1 1 d . . .
H2A H 0.6304 0.1718 0.6389 0.073 Uiso 1 1 calc R U .
C1 C 0.4010(5) 0.0997(5) 0.6257(2) 0.0627(16) Uani 1 1 d . . .
H1A H 0.3304 0.0605 0.6311 0.075 Uiso 1 1 calc R U .
N5 N 1.0032(3) 0.1157(3) 0.45788(14) 0.0553(12) Uani 1 1 d G . .
C11 C 1.0577(4) 0.1514(4) 0.41485(16) 0.076(2) Uani 1 1 d G . .
H11A H 1.1009 0.1304 0.4016 0.091 Uiso 1 1 calc R U .
N6 N 1.0345(4) 0.2248(3) 0.39554(14) 0.0772(17) Uani 1 1 d G . .
H6B H 1.0580 0.2577 0.3696 0.093 Uiso 1 1 calc R U .
C12 C 0.9657(4) 0.2345(3) 0.42663(18) 0.0707(18) Uani 1 1 d G . .
H12A H 0.9382 0.2774 0.4225 0.085 Uiso 1 1 calc R U .
C13 C 0.9464(3) 0.1670(4) 0.46516(15) 0.0689(18) Uani 1 1 d G . .
H13A H 0.9040 0.1580 0.4907 0.083 Uiso 1 1 calc R U .
O4W O 0.6561(10) -0.0913(10) 0.2500 0.137(4) Uani 1 2 d S TU P
O3W O 1.0664(9) 0.3179(9) 0.3112(4) 0.181(4) Uani 1 1 d . U .
O2W O 1.2711(17) 0.5910(16) 0.2500 0.160(7) Uani 0.6667 2 d S TU P
O1W O 0.8929(12) 0.0259(13) 0.3035(6) 0.255(7) Uani 1 1 d . U .
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Ni1 N1 89.75(17) 2_655 3_665
N1 Ni1 N1 89.75(17) 2_655 .
N1 Ni1 N1 89.75(17) 3_665 .
N1 Ni1 N3 89.61(16) 2_655 3_665
N1 Ni1 N3 178.80(17) 3_665 3_665
N1 Ni1 N3 91.26(16) . 3_665
N1 Ni1 N3 178.80(16) 2_655 2_655
N1 Ni1 N3 91.26(16) 3_665 2_655
N1 Ni1 N3 89.62(16) . 2_655
N3 Ni1 N3 89.39(16) 3_665 2_655
N1 Ni1 N3 91.26(16) 2_655 .
N1 Ni1 N3 89.62(16) 3_665 .
N1 Ni1 N3 178.80(16) . .
N3 Ni1 N3 89.39(16) 3_665 .
N3 Ni1 N3 89.39(16) 2_655 .
O1 V3 O7 105.66(16) . .
O1 V3 O7 105.67(16) . 10_556
O7 V3 O7 92.23(18) . 10_556
O1 V3 O8 104.42(16) . 10_556
O7 V3 O8 149.88(15) . 10_556
O7 V3 O8 78.36(13) 10_556 10_556
O1 V3 O8 104.42(16) . .
O7 V3 O8 78.36(13) . .
O7 V3 O8 149.88(15) 10_556 .
O8 V3 O8 95.48(18) 10_556 .
O1 V3 V1 114.21(2) . 10_556
O7 V3 V1 122.68(10) . 10_556
O7 V3 V1 39.22(9) 10_556 10_556
O8 V3 V1 39.60(9) 10_556 10_556
O8 V3 V1 125.40(10) . 10_556
O1 V3 V1 114.21(2) . .
O7 V3 V1 39.22(9) . .
O7 V3 V1 122.68(10) 10_556 .
O8 V3 V1 125.40(10) 10_556 .
O8 V3 V1 39.59(9) . .
V1 V3 V1 131.57(5) 10_556 .
N5 Ni2 N5 180.0 8_666 2_645
N5 Ni2 N5 90.34(16) 8_666 9_546
N5 Ni2 N5 89.66(17) 2_645 9_546
N5 Ni2 N5 90.34(16) 8_666 7_756
N5 Ni2 N5 89.66(17) 2_645 7_756
N5 Ni2 N5 90.34(17) 9_546 7_756
N5 Ni2 N5 89.66(17) 8_666 3_765
N5 Ni2 N5 90.34(16) 2_645 3_765
N5 Ni2 N5 180.00(18) 9_546 3_765
N5 Ni2 N5 89.66(16) 7_756 3_765
N5 Ni2 N5 89.67(17) 8_666 .
N5 Ni2 N5 90.33(16) 2_645 .
N5 Ni2 N5 89.67(16) 9_546 .
N5 Ni2 N5 180.0 7_756 .
N5 Ni2 N5 90.33(17) 3_765 .
O2 V2 O3 104.5(2) . .
O2 V2 O7 110.04(17) . .
O3 V2 O7 91.47(17) . .
O2 V2 O8 109.71(17) . 3_665
O3 V2 O8 91.06(18) . 3_665
O7 V2 O8 138.11(14) . 3_665
O2 V2 O4 100.95(18) . 3_665
O3 V2 O4 154.56(17) . 3_665
O7 V2 O4 80.66(13) . 3_665
O8 V2 O4 79.40(13) 3_665 3_665
O2 V2 V1 108.87(15) . .
O3 V2 V1 128.77(14) . .
O7 V2 V1 40.89(9) . .
O8 V2 V1 112.11(10) 3_665 .
O4 V2 V1 39.82(9) 3_665 .
O2 V2 V1 109.80(15) . 3_665
O3 V2 V1 127.32(15) . 3_665
O7 V2 V1 111.95(10) . 3_665
O8 V2 V1 40.21(9) 3_665 3_665
O4 V2 V1 39.19(9) 3_665 3_665
V1 V2 V1 74.84(4) . 3_665
O5 V1 O4 107.09(17) . 3_665
O5 V1 O4 108.48(17) . .
O4 V1 O4 93.4(2) 3_665 .
O5 V1 O7 107.70(17) . .
O4 V1 O7 83.53(14) 3_665 .
O4 V1 O7 142.94(14) . .
O5 V1 O8 107.86(17) . .
O4 V1 O8 144.39(14) 3_665 .
O4 V1 O8 81.94(14) . .
O7 V1 O8 79.64(13) . .
O5 V1 V2 112.04(14) . .
O4 V1 V2 43.27(11) 3_665 .
O4 V1 V2 127.25(11) . .
O7 V1 V2 40.31(9) . .
O8 V1 V2 114.78(10) . .
O5 V1 V2 114.20(14) . 2_655
O4 V1 V2 126.26(11) 3_665 2_655
O4 V1 V2 42.17(11) . 2_655
O7 V1 V2 113.28(10) . 2_655
O8 V1 V2 39.77(10) . 2_655
V2 V1 V2 132.65(4) . 2_655
O5 V1 V3 118.18(14) . .
O4 V1 V3 114.23(11) 3_665 .
O4 V1 V3 112.56(11) . .
O7 V1 V3 39.99(9) . .
O8 V1 V3 40.12(9) . .
V2 V1 V3 75.53(3) . .
V2 V1 V3 74.38(3) 2_655 .
V2 O7 V1 98.80(14) . .
V2 O7 V3 138.77(17) . .
V1 O7 V3 100.79(15) . .
V2 O8 V1 100.02(15) 2_655 .
V2 O8 V3 135.84(17) 2_655 .
V1 O8 V3 100.28(14) . .
V1 O4 V1 142.4(2) 2_655 .
V1 O4 V2 96.91(15) 2_655 2_655
V1 O4 V2 98.64(15) . 2_655
V2 O3 V2 132.5(3) 10_556 .
C6 N3 C4 104.8(4) . .
C6 N3 Ni1 126.7(4) . .
C4 N3 Ni1 128.4(3) . .
C2 N1 C3 104.8(5) . .
C2 N1 Ni1 129.1(4) . .
C3 N1 Ni1 126.0(4) . .
C5 C4 N3 109.9(5) . .
C1 N2 C2 108.7(5) . .
C6 N4 C5 108.2(5) . .
N3 C6 N4 110.8(5) . .
C1 C3 N1 110.6(6) . .
C4 C5 N4 106.4(5) . .
N1 C2 N2 110.9(6) . .
N2 C1 C3 105.0(6) . .
C13 N5 C11 108.0 . .
C13 N5 Ni2 126.5(2) . .
C11 N5 Ni2 125.4(2) . .
N6 C11 N5 108.0 . .
C11 N6 C12 108.0 . .
N6 C12 C13 108.0 . .
N5 C13 C12 108.0 . .
O2W O2W O2W 60.001(6) 3_775 2_755
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.125(4) 2_655
Ni1 N1 2.125(4) 3_665
Ni1 N1 2.125(4) .
Ni1 N3 2.125(4) 3_665
Ni1 N3 2.125(4) 2_655
Ni1 N3 2.125(4) .
V3 O1 1.607(5) .
V3 O7 1.965(3) .
V3 O7 1.965(3) 10_556
V3 O8 1.967(3) 10_556
V3 O8 1.967(3) .
V3 V1 3.0039(10) 10_556
V3 V1 3.0040(10) .
Ni2 N5 2.089(3) 8_666
Ni2 N5 2.089(3) 2_645
Ni2 N5 2.089(3) 9_546
Ni2 N5 2.089(3) 7_756
Ni2 N5 2.089(3) 3_765
Ni2 N5 2.089(3) .
V2 O2 1.619(4) .
V2 O3 1.828(2) .
V2 O7 1.911(3) .
V2 O8 1.928(3) 3_665
V2 O4 2.016(4) 3_665
V2 V1 2.9192(12) .
V2 V1 2.9680(12) 3_665
V1 O5 1.592(3) .
V1 O4 1.883(3) 3_665
V1 O4 1.897(3) .
V1 O7 1.934(3) .
V1 O8 1.946(3) .
V1 V2 2.9680(12) 2_655
O8 V2 1.928(3) 2_655
O4 V1 1.883(3) 2_655
O4 V2 2.016(4) 2_655
O3 V2 1.828(2) 10_556
N3 C6 1.336(6) .
N3 C4 1.382(7) .
N1 C2 1.306(7) .
N1 C3 1.367(7) .
C4 C5 1.347(8) .
N2 C1 1.337(9) .
N2 C2 1.344(8) .
N4 C6 1.338(7) .
N4 C5 1.357(8) .
C3 C1 1.356(8) .
N5 C13 1.4200 .
N5 C11 1.4200 .
C11 N6 1.4200 .
N6 C12 1.4200 .
C12 C13 1.4200 .
O2W O2W 1.82(4) 3_775
O2W O2W 1.82(4) 2_755
