#------------------------------------------------------------------------------
#$Date: 2019-09-30 11:59:06 +0300 (Mon, 30 Sep 2019) $
#$Revision: 218930 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/42/7234242.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_7234242
loop_
_publ_author_name
'Yanfen Liang'
'Suzhi Li'
'Donghui Yang'
'Pengtao Ma'
'Jingyang Niu'
'Jingping Wang'
_publ_section_title
;
 Controllable assembly of multicarboxylic acids functionalized
 heteropolyoxomolybdates and allochroic properties
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              4632
_journal_page_last               4639
_journal_paper_doi               10.1039/C5TC00297D
_journal_volume                  3
_journal_year                    2015
_chemical_formula_sum            'C24 H57 Mo12 N8 O63.5 Te2'
_chemical_formula_weight         2880.2052
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.8647(11)
_cell_length_b                   20.8647(11)
_cell_length_c                   16.3866(10)
_cell_measurement_reflns_used    7721
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.57
_cell_volume                     6177.9(6)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10669
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  0.5888
_exptl_absorpt_correction_T_min  0.3592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4266
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.468
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2463
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0483
_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)+(0.0866P)²+53.9184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1359
_reflns_number_gt                2361
_reflns_number_total             2463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            J-Mater-Chem-C-2015-3-4632.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

data item '_symmetry_cell_setting' value 'Hexagonal' was changed to
'hexagonal' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      R32
_cod_database_code               7234242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -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'
'y+2/3, x+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+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'
'y+1/3, x+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 1.0000 1.0000 0.76568(5) 0.0459(3) Uani 1 3 d S . .
Mo1 Mo 0.91704(5) 0.80672(5) 0.71336(5) 0.0518(3) Uani 1 1 d . . .
Mo2 Mo 0.80787(5) 0.88209(5) 0.71100(7) 0.0588(3) Uani 1 1 d . . .
O1 O 0.8937(6) 0.7202(5) 0.7480(7) 0.085(3) Uani 1 1 d . . .
O2 O 0.9312(4) 0.8030(4) 0.6119(5) 0.0625(18) Uani 1 1 d . . .
O3 O 1.0183(4) 0.8643(4) 0.7494(5) 0.0604(18) Uani 1 1 d . . .
O4 O 0.8189(4) 0.7953(4) 0.7098(5) 0.062(2) Uani 1 1 d . . .
O5 O 0.9044(7) 0.8268(6) 0.8509(5) 0.084(3) Uani 1 1 d . . .
O6 O 0.9274(4) 0.9183(4) 0.7070(4) 0.0485(14) Uani 1 1 d . . .
O7 O 0.8048(4) 0.8953(5) 0.6089(5) 0.0664(19) Uani 1 1 d . . .
O8 O 0.7160(5) 0.8407(5) 0.7387(8) 0.091(3) Uani 1 1 d . . .
O9 O 0.8298(7) 0.8744(6) 0.8509(6) 0.086(3) Uani 1 1 d . . .
C1 C 0.8585(12) 0.8452(10) 0.8821(8) 0.102(6) Uani 1 1 d D . .
C2 C 0.8623(10) 0.8302(10) 0.9715(8) 0.109 Uiso 1 1 d D . .
H2A H 0.8368 0.7770 0.9797 0.131 Uiso 1 1 calc R . .
H2B H 0.9138 0.8493 0.9861 0.131 Uiso 1 1 calc R . .
C3 C 0.6667 0.6920(9) 0.8333 0.085(7) Uani 1 2 d S . .
H3A H 0.6667 0.7366 0.8333 0.102 Uiso 1 2 calc SR . .
C4 C 0.6971(8) 0.6085(8) 0.8077(10) 0.080(4) Uani 1 1 d . . .
H4A H 0.7221 0.5856 0.7871 0.096 Uiso 1 1 calc R . .
C5 C 0.9368(4) 0.9368(4) 0.5000 0.123 Uiso 0.80 2 d SPD . .
N1 N 0.7121(6) 0.6776(6) 0.7943(8) 0.074(3) Uani 1 1 d . . .
H1A H 0.7474 0.7087 0.7635 0.088 Uiso 1 1 calc R . .
N2 N 1.0000 0.9367(4) 0.5000 0.118(14) Uiso 0.67 2 d SPD A 1
C6 C 1.0000 0.958(8) 0.5000 0.11(4) Uiso 0.20 2 d SP . 2
O1W O 0.7425(6) 0.9544(6) 0.8949(7) 0.091(3) Uiso 1 1 d . . .
O2W O 1.0000 0.7473(5) 0.5000 0.058(2) Uiso 1 2 d S . .
O3W O 0.9623(12) 0.7222(12) 0.4785(13) 0.085(5) Uiso 0.50 1 d P . .
O4W O 0.9852(14) 0.6667 0.6667 0.153(8) Uiso 1 2 d S . .
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'
Mo Mo -1.6832 0.6857 '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'
Te Te -0.5308 1.6751 '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'
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
O6 Te1 O6 96.2(3) . 2_765
O6 Te1 O6 96.2(3) . 3_675
O6 Te1 O6 96.2(3) 2_765 3_675
O2 Mo1 O1 103.9(5) . .
O2 Mo1 O3 99.6(4) . .
O1 Mo1 O3 101.6(5) . .
O2 Mo1 O4 99.4(4) . .
O1 Mo1 O4 98.8(4) . .
O3 Mo1 O4 147.7(3) . .
O2 Mo1 O6 94.3(3) . .
O1 Mo1 O6 160.5(4) . .
O3 Mo1 O6 81.9(3) . .
O4 Mo1 O6 70.9(3) . .
O2 Mo1 O5 173.3(4) . .
O1 Mo1 O5 82.6(4) . .
O3 Mo1 O5 77.2(4) . .
O4 Mo1 O5 81.0(4) . .
O6 Mo1 O5 79.5(3) . .
O7 Mo2 O8 102.6(5) . .
O7 Mo2 O3 100.1(4) . 3_675
O8 Mo2 O3 102.2(4) . 3_675
O7 Mo2 O4 100.0(4) . .
O8 Mo2 O4 99.0(4) . .
O3 Mo2 O4 146.7(4) 3_675 .
O7 Mo2 O6 92.5(3) . .
O8 Mo2 O6 163.5(5) . .
O3 Mo2 O6 81.6(3) 3_675 .
O4 Mo2 O6 71.3(3) . .
O7 Mo2 O9 172.1(4) . .
O8 Mo2 O9 85.1(5) . .
O3 Mo2 O9 76.4(3) 3_675 .
O4 Mo2 O9 80.1(4) . .
O6 Mo2 O9 80.1(3) . .
Mo2 O3 Mo1 142.9(5) 2_765 .
Mo2 O4 Mo1 119.8(4) . .
C1 O5 Mo1 126.8(9) . .
Te1 O6 Mo2 123.6(3) . .
Te1 O6 Mo1 122.4(3) . .
Mo2 O6 Mo1 97.9(3) . .
C1 O9 Mo2 129.0(9) . .
O9 C1 O5 129.0(12) . .
O9 C1 C2 128.9(14) . .
O5 C1 C2 101.4(13) . .
C2 C2 C1 115.6(15) 4_557 .
C2 C2 H2A 108.4 4_557 .
C1 C2 H2A 108.4 . .
C2 C2 H2B 108.4 4_557 .
C1 C2 H2B 108.4 . .
H2A C2 H2B 107.4 . .
N1 C3 N1 106.6(16) . 17_656
N1 C3 H3A 126.7 . .
N1 C3 H3A 126.7 17_656 .
N1 C4 C4 105.2(7) . 17_656
N1 C4 H4A 127.4 . .
C4 C4 H4A 127.4 17_656 .
C6 C5 C6 81(10) 3_675 .
C6 C5 N2 100(9) 3_675 .
C6 C5 N2 20(9) . .
C6 C5 N2 20(9) 3_675 3_675
C6 C5 N2 100(9) . 3_675
N2 C5 N2 120.1(5) . 3_675
C3 N1 C4 111.5(11) . .
C3 N1 H1A 124.3 . .
C4 N1 H1A 124.3 . .
C5 N2 C5 119.9(5) 2_765 .
C5 C6 C5 159(10) 2_765 .
C5 C6 C6 50(9) 2_765 2_765
C5 C6 C6 110(9) . 2_765
C5 C6 C6 110(8) 2_765 3_675
C5 C6 C6 50(9) . 3_675
C6 C6 C6 60.000(10) 2_765 3_675
O3W O2W O3W 161(4) 5_766 .
O2W O3W O3W 9.6(19) . 5_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 O6 1.882(7) .
Te1 O6 1.882(7) 2_765
Te1 O6 1.882(7) 3_675
Mo1 O2 1.697(8) .
Mo1 O1 1.715(9) .
Mo1 O3 1.928(8) .
Mo1 O4 1.941(8) .
Mo1 O6 2.230(7) .
Mo1 O5 2.331(8) .
Mo2 O7 1.702(8) .
Mo2 O8 1.724(9) .
Mo2 O3 1.922(8) 3_675
Mo2 O4 1.936(8) .
Mo2 O6 2.216(7) .
Mo2 O9 2.360(10) .
O3 Mo2 1.922(8) 2_765
O5 C1 1.30(2) .
O9 C1 1.16(2) .
C1 C2 1.510(10) .
C2 C2 1.490(10) 4_557
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N1 1.298(16) .
C3 N1 1.298(16) 17_656
C3 H3A 0.9300 .
C4 N1 1.332(18) .
C4 C4 1.38(3) 17_656
C4 H4A 0.9300 .
C5 C6 1.16(3) 3_675
C5 C6 1.16(3) .
C5 N2 1.320(7) .
C5 N2 1.320(7) 3_675
N1 H1A 0.8600 .
N2 C5 1.320(7) 2_765
C6 C5 1.16(3) 2_765
C6 C6 1.5(3) 2_765
C6 C6 1.5(3) 3_675
O2W O3W 0.78(2) 5_766
O2W O3W 0.78(2) .
O3W O3W 1.53(4) 5_766
