#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327456.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_4327456
loop_
_publ_author_name
'Yangguang Li'
'Na Hao'
'Enbo Wang'
'Mei Yuan'
'Changwen Hu'
'Ninghai Hu'
'Hengqing Jia'
_publ_section_title
;
 New High-Dimensional Networks Based on Polyoxometalate and Crown Ether
 Building Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2729
_journal_page_last               2735
_journal_paper_doi               10.1021/ic026172+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C80 H133 As Mo12 N7 Na3 O72'
_chemical_formula_weight         3640.10
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            2
_cell_length_a                   15.7435(17)
_cell_length_b                   15.7435(17)
_cell_length_c                   30.042(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.04
_cell_measurement_theta_min      4.79
_cell_volume                     6448.5(18)
_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  'siemens P4 dffractometer'
_diffrn_measurement_method       '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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9722
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_T_max  0.5967
_exptl_absorpt_correction_T_min  0.4213
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3870
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0713P)²+51.2657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                2454
_reflns_number_total             3870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0261722B_3.cif
_cod_data_source_block           l118
_cod_original_cell_volume        6448.5(17)
_cod_database_code               4327456
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo -0.81234(6) 0.25142(6) 0.50573(3) 0.0422(3) Uani 1 1 d .
Mo2 Mo -0.97795(6) 0.14123(6) 0.59704(3) 0.0431(3) Uani 1 1 d .
As As -1.0000 0.0000 0.5000 0.0289(5) Uani 1 6 d S
O1 O -1.0000 0.0000 0.5554(6) 0.029(4) Uani 0.50 3 d SP
O2 O -0.8890(8) 0.0817(8) 0.4812(4) 0.034(3) Uani 0.50 1 d P
O3 O -0.7288(5) 0.3684(5) 0.5047(3) 0.066(2) Uani 1 1 d .
O4 O -0.7408(8) 0.1911(7) 0.5105(3) 0.091(3) Uani 1 1 d .
O5 O -0.8556(6) 0.2320(8) 0.5628(3) 0.085(3) Uani 1 1 d .
O6 O -0.9591(6) 0.2089(6) 0.6412(3) 0.064(2) Uani 1 1 d .
O7 O -1.0411(5) 0.1820(8) 0.5600(3) 0.091(3) Uani 1 1 d .
O8 O -1.0825(5) 0.0236(5) 0.6133(4) 0.092(4) Uani 1 1 d .
O9 O -0.0877(9) 0.3223(8) 0.7500 0.065(3) Uani 1 2 d S
O10 O -0.0669(6) 0.4257(5) 0.6720(3) 0.066(2) Uani 1 1 d .
O11 O -0.0059(6) 0.6110(6) 0.6716(3) 0.071(2) Uani 1 1 d .
O12 O 0.0467(9) 0.7153(8) 0.7500 0.074(4) Uani 1 2 d S
O13 O -0.8188(11) 0.5007(12) 0.6618(5) 0.151(6) Uani 1 1 d .
N1 N -0.8596(9) 0.5252(10) 0.5933(5) 0.090(4) Uani 1 1 d .
C1 C -0.0465(10) 0.3062(9) 0.7102(3) 0.064(3) Uani 1 1 d .
H1A H -0.0585 0.2395 0.7097 0.064 Uiso 1 1 calc R
H1B H 0.0238 0.3507 0.7095 0.064 Uiso 1 1 calc R
C2 C -0.0929(10) 0.3236(9) 0.6712(4) 0.063(3) Uani 1 1 d .
H2A H -0.0696 0.3091 0.6440 0.063 Uiso 1 1 calc R
H2B H -0.1636 0.2818 0.6726 0.063 Uiso 1 1 calc R
C3 C -0.0969(9) 0.4591(9) 0.6373(4) 0.054(3) Uani 1 1 d .
C4 C -0.1531(10) 0.4012(10) 0.6031(5) 0.080(4) Uani 1 1 d .
H4 H -0.1749 0.3344 0.6032 0.080 Uiso 1 1 calc R
C5 C -0.1782(11) 0.4434(12) 0.5673(5) 0.095(5) Uani 1 1 d .
H5 H -0.2163 0.4043 0.5439 0.095 Uiso 1 1 calc R
C6 C -0.1459(11) 0.5421(12) 0.5675(5) 0.085(4) Uani 1 1 d .
H6 H -0.1617 0.5701 0.5440 0.085 Uiso 1 1 calc R
C7 C -0.0902(10) 0.5999(10) 0.6024(5) 0.073(4) Uani 1 1 d .
H7 H -0.0699 0.6664 0.6029 0.073 Uiso 1 1 calc R
C8 C -0.0646(9) 0.5585(8) 0.6367(4) 0.055(3) Uani 1 1 d .
C9 C 0.0358(11) 0.7155(9) 0.6716(5) 0.078(4) Uani 1 1 d .
H9A H -0.0154 0.7322 0.6744 0.078 Uiso 1 1 calc R
H9B H 0.0709 0.7430 0.6440 0.078 Uiso 1 1 calc R
C10 C 0.1028(10) 0.7541(9) 0.7093(4) 0.081(4) Uani 1 1 d .
H10A H 0.1523 0.7348 0.7070 0.081 Uiso 1 1 calc R
H10B H 0.1356 0.8252 0.7094 0.081 Uiso 1 1 calc R
C11 C -0.8296(19) 0.553(2) 0.6388(8) 0.162(11) Uani 1 1 d .
H11 H -0.8190 0.6124 0.6496 0.162 Uiso 1 1 calc R
C12 C -0.864(2) 0.592(2) 0.5671(10) 0.27(2) Uani 1 1 d .
H12A H -0.8020 0.6319 0.5528 0.271 Uiso 1 1 calc R
H12B H -0.8802 0.6330 0.5848 0.271 Uiso 1 1 calc R
H12C H -0.9140 0.5592 0.5448 0.271 Uiso 1 1 calc R
C13 C -0.8856(19) 0.4367(15) 0.5783(11) 0.26(2) Uani 1 1 d .
H13A H -0.9513 0.4066 0.5668 0.257 Uiso 1 1 calc R
H13B H -0.8829 0.3975 0.6021 0.257 Uiso 1 1 calc R
H13C H -0.8416 0.4416 0.5550 0.257 Uiso 1 1 calc R
Na Na -0.0257(6) 0.5248(5) 0.7500 0.075(2) Uani 1 2 d S
OW1 O -0.202(2) 0.475(2) 0.7500 0.103(9) Uani 0.56 2 d SP
OW1' O -0.146(2) 0.571(2) 0.7500 0.104(12) Uani 0.44 2 d SP
OW2 O 0.1285(11) 0.5452(13) 0.7500 0.116(6) Uani 1 2 d S
OW3 O -0.3333 0.3333 0.6940(11) 0.209(13) Uiso 1 3 d S
N2 N -1.0000 0.0000 0.7500 0.142(15) Uiso 1 6 d S
C14 C -0.915(4) 0.061(6) 0.7500 0.13(3) Uiso 0.33 2 d SPD
C15 C -0.813(4) 0.106(4) 0.7500 0.068(15) Uiso 0.33 2 d SPD
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'
As As 0.0499 2.0058 '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'
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
O3 Mo1 O4 103.4(5) . .
O3 Mo1 O5 103.3(4) . .
O4 Mo1 O5 96.7(4) . .
O3 Mo1 O4 100.1(4) . 9_566
O4 Mo1 O4 154.5(6) . 9_566
O5 Mo1 O4 87.4(3) . 9_566
O3 Mo1 O7 98.7(4) . 8_446
O4 Mo1 O7 86.1(3) . 8_446
O5 Mo1 O7 156.5(5) . 8_446
O4 Mo1 O7 80.6(4) 9_566 8_446
O3 Mo1 O2 156.5(4) . 9_566
O4 Mo1 O2 97.8(5) . 9_566
O5 Mo1 O2 63.9(4) . 9_566
O4 Mo1 O2 61.4(4) 9_566 9_566
O7 Mo1 O2 92.6(4) 8_446 9_566
O3 Mo1 O2 154.8(4) . .
O4 Mo1 O2 62.8(4) . .
O5 Mo1 O2 99.4(5) . .
O4 Mo1 O2 91.6(4) 9_566 .
O7 Mo1 O2 61.1(4) 8_446 .
O2 Mo1 O2 47.2(5) 9_566 .
O6 Mo2 O7 102.8(5) . .
O6 Mo2 O8 102.8(5) . .
O7 Mo2 O8 98.5(4) . .
O6 Mo2 O5 98.9(4) . .
O7 Mo2 O5 86.2(3) . .
O8 Mo2 O5 156.1(4) . .
O6 Mo2 O8 98.9(4) . 3_345
O7 Mo2 O8 156.0(5) . 3_345
O8 Mo2 O8 86.3(4) . 3_345
O5 Mo2 O8 80.5(3) . 3_345
O6 Mo2 O2 155.4(4) . 9_566
O7 Mo2 O2 63.8(4) . 9_566
O8 Mo2 O2 99.7(5) . 9_566
O5 Mo2 O2 61.3(4) . 9_566
O8 Mo2 O2 92.2(4) 3_345 9_566
O6 Mo2 O1 156.2(5) . .
O7 Mo2 O1 98.9(5) . .
O8 Mo2 O1 64.2(4) . .
O5 Mo2 O1 92.0(4) . .
O8 Mo2 O1 62.0(4) 3_345 .
O2 Mo2 O1 46.7(5) 9_566 .
O2 As O2 70.9(4) 8_446 3_345
O2 As O2 70.9(4) 8_446 .
O2 As O2 109.1(4) 3_345 .
O2 As O2 109.1(4) 8_446 7_356
O2 As O2 70.9(4) 3_345 7_356
O2 As O2 180.000(2) . 7_356
O2 As O2 109.1(4) 8_446 9_566
O2 As O2 180.0(4) 3_345 9_566
O2 As O2 70.9(4) . 9_566
O2 As O2 109.1(4) 7_356 9_566
O2 As O2 180.0(8) 8_446 2_465
O2 As O2 109.1(4) 3_345 2_465
O2 As O2 109.1(4) . 2_465
O2 As O2 70.9(4) 7_356 2_465
O2 As O2 70.9(4) 9_566 2_465
O2 As O1 70.2(4) 8_446 .
O2 As O1 109.8(4) 3_345 .
O2 As O1 109.8(4) . .
O2 As O1 70.2(4) 7_356 .
O2 As O1 70.2(4) 9_566 .
O2 As O1 109.8(4) 2_465 .
O2 As O1 109.8(4) 8_446 7_356
O2 As O1 70.2(4) 3_345 7_356
O2 As O1 70.2(4) . 7_356
O2 As O1 109.8(4) 7_356 7_356
O2 As O1 109.8(4) 9_566 7_356
O2 As O1 70.2(4) 2_465 7_356
O1 As O1 180.000(2) . 7_356
As O1 Mo2 121.1(4) . 3_345
As O1 Mo2 121.1(4) . .
Mo2 O1 Mo2 95.7(5) 3_345 .
As O1 Mo2 121.1(4) . 2_465
Mo2 O1 Mo2 95.7(5) 3_345 2_465
Mo2 O1 Mo2 95.7(5) . 2_465
As O2 Mo1 121.8(6) . 8_446
As O2 Mo2 121.4(6) . 8_446
Mo1 O2 Mo2 96.2(4) 8_446 8_446
As O2 Mo1 119.8(6) . .
Mo1 O2 Mo1 95.7(4) 8_446 .
Mo2 O2 Mo1 95.6(4) 8_446 .
Mo1 O4 Mo1 139.8(5) . 8_446
Mo1 O5 Mo2 138.4(5) . .
Mo2 O7 Mo1 139.4(6) . 9_566
Mo2 O8 Mo2 138.1(6) . 2_465
C1 O9 C1 112.0(11) 10_557 .
C1 O9 Na 105.4(7) 10_557 .
C1 O9 Na 105.4(7) . .
C3 O10 C2 117.4(9) . .
C3 O10 Na 118.1(7) . .
C2 O10 Na 120.4(6) . .
C8 O11 C9 118.4(10) . .
C8 O11 Na 120.0(7) . .
C9 O11 Na 117.1(8) . .
C10 O12 C10 114.7(14) 10_557 .
C10 O12 Na 107.8(7) 10_557 .
C10 O12 Na 107.8(7) . .
C13 N1 C12 121(3) . .
C13 N1 C11 121(2) . .
C12 N1 C11 117(2) . .
O9 C1 C2 108.5(9) . .
O10 C2 C1 107.6(10) . .
O10 C3 C4 123.8(11) . .
O10 C3 C8 116.7(11) . .
C4 C3 C8 119.5(11) . .
C3 C4 C5 119.8(13) . .
C6 C5 C4 119.6(14) . .
C5 C6 C7 120.2(13) . .
C8 C7 C6 119.7(13) . .
O11 C8 C3 115.3(10) . .
O11 C8 C7 123.6(11) . .
C3 C8 C7 121.0(12) . .
O11 C9 C10 107.4(11) . .
O12 C10 C9 108.5(11) . .
O13 C11 N1 120(3) . .
OW2 Na OW1' 157.4(10) . .
OW2 Na OW1 171.0(9) . .
OW1' Na OW1 31.6(9) . .
OW2 Na O12 90.9(6) . .
OW1' Na O12 66.5(8) . .
OW1 Na O12 98.1(8) . .
OW2 Na O11 94.8(3) . .
OW1' Na O11 75.4(4) . .
OW1 Na O11 89.4(4) . .
O12 Na O11 62.8(2) . .
OW2 Na O11 94.8(3) . 10_557
OW1' Na O11 75.4(4) . 10_557
OW1 Na O11 89.4(4) . 10_557
O12 Na O11 62.8(2) . 10_557
O11 Na O11 124.8(5) . 10_557
OW2 Na O10 90.7(3) . .
OW1' Na O10 100.4(5) . .
OW1 Na O10 84.8(4) . .
O12 Na O10 120.0(2) . .
O11 Na O10 57.3(2) . .
O11 Na O10 173.8(4) 10_557 .
OW2 Na O10 90.7(3) . 10_557
OW1' Na O10 100.4(5) . 10_557
OW1 Na O10 84.8(4) . 10_557
O12 Na O10 120.0(2) . 10_557
O11 Na O10 173.8(4) . 10_557
O11 Na O10 57.3(2) 10_557 10_557
O10 Na O10 119.9(4) . 10_557
OW2 Na O9 84.4(5) . .
OW1' Na O9 118.3(9) . .
OW1 Na O9 86.6(7) . .
O12 Na O9 175.3(5) . .
O11 Na O9 117.5(2) . .
O11 Na O9 117.5(2) 10_557 .
O10 Na O9 60.2(2) . .
O10 Na O9 60.2(2) 10_557 .
OW1' OW1 Na 68.9(19) . .
OW1 OW1' Na 79.5(19) . .
C14 N2 C14 120.000(19) . 3_345
C14 N2 C14 120.00(10) . 2_465
C14 N2 C14 120.00(12) 3_345 2_465
N2 C14 C15 161(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.643(7) .
Mo1 O4 1.807(7) .
Mo1 O5 1.813(8) .
Mo1 O4 2.006(8) 9_566
Mo1 O7 2.015(8) 8_446
Mo1 O2 2.396(12) 9_566
Mo1 O2 2.433(11) .
Mo2 O6 1.634(7) .
Mo2 O7 1.811(8) .
Mo2 O8 1.825(8) .
Mo2 O5 2.014(8) .
Mo2 O8 2.017(8) 3_345
Mo2 O2 2.412(13) 9_566
Mo2 O1 2.421(10) .
As O2 1.667(12) 8_446
As O2 1.667(12) 3_345
As O2 1.667(12) .
As O2 1.667(12) 7_356
As O2 1.667(12) 9_566
As O2 1.667(12) 2_465
As O1 1.663(19) .
As O1 1.663(19) 7_356
O1 Mo2 2.421(10) 3_345
O1 Mo2 2.421(10) 2_465
O2 Mo1 2.396(12) 8_446
O2 Mo2 2.412(13) 8_446
O4 Mo1 2.006(8) 8_446
O7 Mo1 2.015(8) 9_566
O8 Mo2 2.017(8) 2_465
O9 C1 1.442(12) 10_557
O9 C1 1.442(12) .
O9 Na 2.829(13) .
O10 C3 1.353(12) .
O10 C2 1.447(13) .
O10 Na 2.709(9) .
O11 C8 1.370(13) .
O11 C9 1.434(13) .
O11 Na 2.657(9) .
O12 C10 1.453(13) 10_557
O12 C10 1.453(13) .
O12 Na 2.623(14) .
O13 C11 1.14(2) .
N1 C13 1.32(2) .
N1 C12 1.35(2) .
N1 C11 1.44(3) .
C1 C2 1.476(15) .
C3 C4 1.367(17) .
C3 C8 1.382(15) .
C4 C5 1.418(18) .
C5 C6 1.37(2) .
C6 C7 1.378(19) .
C7 C8 1.382(16) .
C9 C10 1.456(17) .
Na OW2 2.284(17) .
Na OW1' 2.35(3) .
Na OW1 2.47(3) .
Na O11 2.657(9) 10_557
Na O10 2.709(9) 10_557
OW1 OW1' 1.32(4) .
N2 C14 1.20(6) .
N2 C14 1.20(6) 3_345
N2 C14 1.20(6) 2_465
C14 C15 1.39(2) .
