#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:17:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178843 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/97/4109786.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_4109786
loop_
_publ_author_name
'Huaqiao Tan'
'Yangguang Li'
'Zhiming Zhang'
'Chao Qin'
'Xinlong Wang'
'Enbo Wang'
'Zhongmin Su'
_publ_section_title
;
 Chiral Polyoxometalate-Induced Enantiomerically 3D Architectures: A New
 Route for Synthesis of High-Dimensional Chiral Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10066
_journal_page_last               10067
_journal_paper_doi               10.1021/ja073153w
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'H26 Mn Mo9 O45 Zn3'
_chemical_formula_weight         1860.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   none
_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            3
_cell_length_a                   15.6460(4)
_cell_length_b                   15.6460(4)
_cell_length_c                   12.5656(7)
_cell_measurement_reflns_used    1479
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.60
_cell_volume                     2663.92(18)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6365
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.527
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.480
_exptl_crystal_description       block
_exptl_crystal_F_000             2637
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.194
_refine_diff_density_min         -2.716
_refine_diff_density_rms         0.366
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(7)
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1479
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0469
_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)+(0.1220P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                1424
_reflns_number_total             1479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073153wsi20070504_093106.cif
_cod_data_source_block           tl1a
_cod_original_cell_volume        2663.91(18)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4109786
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+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-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+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
Mo1 Mo 0.6667 0.53769(6) 0.8333 0.0186(3) Uani 1 2 d S
Mo2 Mo 0.58078(5) 0.38923(5) 1.03340(6) 0.0192(3) Uani 1 1 d .
Mn1 Mn 0.6667 0.3333 0.8333 0.0126(5) Uani 1 6 d S
Zn1 Zn 0.3333 0.24633(18) 1.1667 0.0880(12) Uani 1 2 d S
O1 O 0.5566(4) 0.2674(4) 0.9244(5) 0.0143(10) Uani 1 1 d .
O2 O 0.5523(5) 0.4484(5) 0.9201(5) 0.0222(13) Uani 1 1 d .
O4 O 0.6364(6) 0.4867(6) 1.1213(6) 0.0337(16) Uani 1 1 d .
O3 O 0.7274(6) 0.6328(5) 0.9213(7) 0.0316(16) Uani 1 1 d .
O5 O 0.6667 0.3333 1.0914(8) 0.020(2) Uani 1 3 d S
O6 O 0.4669(5) 0.3134(5) 1.0892(6) 0.0282(14) Uani 1 1 d .
O1W O 0.3333 0.3709(6) 1.1667 0.033(2) Uani 1 2 d SU
O2W O 0.3333 0.1151(5) 1.1667 0.0194(16) Uani 1 2 d SU
O3W O 0.258(2) 0.202(2) 1.018(2) 0.078(7) Uani 0.50 1 d PU
OW1 O 0.8159(10) 0.8159(10) 1.0000 0.063(4) Uiso 1 2 d S
OW2 O 1.0000 1.0000 1.0000 0.076 Uiso 1 6 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
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 O3 107.4(6) 18_656 .
O3 Mo1 O2 97.5(3) 18_656 .
O3 Mo1 O2 100.0(3) . .
O3 Mo1 O2 100.0(3) 18_656 18_656
O3 Mo1 O2 97.5(3) . 18_656
O2 Mo1 O2 150.3(4) . 18_656
O3 Mo1 O1 160.6(3) 18_656 3_665
O3 Mo1 O1 91.3(3) . 3_665
O2 Mo1 O1 73.6(2) . 3_665
O2 Mo1 O1 82.2(3) 18_656 3_665
O3 Mo1 O1 91.3(3) 18_656 17_556
O3 Mo1 O1 160.6(3) . 17_556
O2 Mo1 O1 82.2(3) . 17_556
O2 Mo1 O1 73.6(2) 18_656 17_556
O1 Mo1 O1 70.7(3) 3_665 17_556
O3 Mo1 Mn1 126.3(3) 18_656 .
O3 Mo1 Mn1 126.3(3) . .
O2 Mo1 Mn1 75.15(18) . .
O2 Mo1 Mn1 75.15(18) 18_656 .
O1 Mo1 Mn1 35.33(16) 3_665 .
O1 Mo1 Mn1 35.33(15) 17_556 .
O6 Mo2 O4 103.8(4) . .
O6 Mo2 O2 103.3(3) . .
O4 Mo2 O2 100.9(4) . .
O6 Mo2 O5 103.5(3) . .
O4 Mo2 O5 90.1(3) . .
O2 Mo2 O5 147.6(3) . .
O6 Mo2 O1 89.2(3) . .
O4 Mo2 O1 161.4(3) . .
O2 Mo2 O1 88.6(3) . .
O5 Mo2 O1 73.8(3) . .
O6 Mo2 O1 160.5(3) . 3_665
O4 Mo2 O1 95.5(3) . 3_665
O2 Mo2 O1 75.1(3) . 3_665
O5 Mo2 O1 73.5(3) . 3_665
O1 Mo2 O1 71.3(3) . 3_665
O6 Mo2 Mn1 124.6(2) . .
O4 Mo2 Mn1 130.9(3) . .
O2 Mo2 Mn1 76.8(2) . .
O5 Mo2 Mn1 73.0(3) . .
O1 Mo2 Mn1 35.75(15) . .
O1 Mo2 Mn1 35.83(16) 3_665 .
O1 Mn1 O1 169.6(3) 17_556 2_655
O1 Mn1 O1 86.3(3) 17_556 3_665
O1 Mn1 O1 87.0(3) 2_655 3_665
O1 Mn1 O1 100.6(4) 17_556 .
O1 Mn1 O1 87.0(3) 2_655 .
O1 Mn1 O1 87.0(3) 3_665 .
O1 Mn1 O1 87.0(3) 17_556 16_546
O1 Mn1 O1 100.6(4) 2_655 16_546
O1 Mn1 O1 169.6(3) 3_665 16_546
O1 Mn1 O1 86.3(3) . 16_546
O1 Mn1 O1 87.0(3) 17_556 18_656
O1 Mn1 O1 86.3(3) 2_655 18_656
O1 Mn1 O1 100.6(4) 3_665 18_656
O1 Mn1 O1 169.6(3) . 18_656
O1 Mn1 O1 87.0(3) 16_546 18_656
O1 Mn1 Mo2 128.18(17) 17_556 3_665
O1 Mn1 Mo2 43.94(18) 2_655 3_665
O1 Mn1 Mo2 43.45(16) 3_665 3_665
O1 Mn1 Mo2 90.26(18) . 3_665
O1 Mn1 Mo2 144.54(18) 16_546 3_665
O1 Mn1 Mo2 90.51(18) 18_656 3_665
O1 Mn1 Mo2 43.45(17) 17_556 17_556
O1 Mn1 Mo2 144.54(18) 2_655 17_556
O1 Mn1 Mo2 128.18(17) 3_665 17_556
O1 Mn1 Mo2 90.51(18) . 17_556
O1 Mn1 Mo2 43.94(18) 16_546 17_556
O1 Mn1 Mo2 90.26(17) 18_656 17_556
Mo2 Mn1 Mo2 171.52(2) 3_665 17_556
O1 Mn1 Mo2 144.54(18) 17_556 2_655
O1 Mn1 Mo2 43.45(17) 2_655 2_655
O1 Mn1 Mo2 90.26(17) 3_665 2_655
O1 Mn1 Mo2 43.94(18) . 2_655
O1 Mn1 Mo2 90.51(18) 16_546 2_655
O1 Mn1 Mo2 128.17(17) 18_656 2_655
Mo2 Mn1 Mo2 63.78(2) 3_665 2_655
Mo2 Mn1 Mo2 121.66(3) 17_556 2_655
O1 Mn1 Mo2 90.51(18) 17_556 .
O1 Mn1 Mo2 90.26(17) 2_655 .
O1 Mn1 Mo2 43.94(18) 3_665 .
O1 Mn1 Mo2 43.45(17) . .
O1 Mn1 Mo2 128.18(17) 16_546 .
O1 Mn1 Mo2 144.54(18) 18_656 .
Mo2 Mn1 Mo2 63.78(2) 3_665 .
Mo2 Mn1 Mo2 111.70(3) 17_556 .
Mo2 Mn1 Mo2 63.78(2) 2_655 .
O1 Mn1 Mo2 43.94(18) 17_556 18_656
O1 Mn1 Mo2 128.17(17) 2_655 18_656
O1 Mn1 Mo2 90.51(18) 3_665 18_656
O1 Mn1 Mo2 144.54(18) . 18_656
O1 Mn1 Mo2 90.26(18) 16_546 18_656
O1 Mn1 Mo2 43.45(16) 18_656 18_656
Mo2 Mn1 Mo2 111.70(3) 3_665 18_656
Mo2 Mn1 Mo2 63.78(2) 17_556 18_656
Mo2 Mn1 Mo2 171.52(2) 2_655 18_656
Mo2 Mn1 Mo2 121.66(3) . 18_656
O1 Mn1 Mo2 90.26(17) 17_556 16_546
O1 Mn1 Mo2 90.51(18) 2_655 16_546
O1 Mn1 Mo2 144.54(18) 3_665 16_546
O1 Mn1 Mo2 128.17(17) . 16_546
O1 Mn1 Mo2 43.45(17) 16_546 16_546
O1 Mn1 Mo2 43.94(18) 18_656 16_546
Mo2 Mn1 Mo2 121.66(3) 3_665 16_546
Mo2 Mn1 Mo2 63.78(2) 17_556 16_546
Mo2 Mn1 Mo2 111.70(3) 2_655 16_546
Mo2 Mn1 Mo2 171.52(2) . 16_546
Mo2 Mn1 Mo2 63.78(2) 18_656 16_546
O1W Zn1 O2W 180.000(3) . .
O1W Zn1 O6 89.9(2) . .
O2W Zn1 O6 90.1(2) . .
O1W Zn1 O6 89.8(2) . 12_557
O2W Zn1 O6 90.2(2) . 12_557
O6 Zn1 O6 179.7(4) . 12_557
O1W Zn1 O3W 92.6(8) . .
O2W Zn1 O3W 87.4(8) . .
O6 Zn1 O3W 90.4(8) . .
O6 Zn1 O3W 89.6(8) 12_557 .
O1W Zn1 O3W 92.6(8) . 12_557
O2W Zn1 O3W 87.4(8) . 12_557
O6 Zn1 O3W 89.6(8) . 12_557
O6 Zn1 O3W 90.4(8) 12_557 12_557
O3W Zn1 O3W 174.7(15) . 12_557
Mn1 O1 Mo2 100.8(2) . .
Mn1 O1 Mo1 101.5(2) . 2_655
Mo2 O1 Mo1 153.5(3) . 2_655
Mn1 O1 Mo2 100.2(3) . 2_655
Mo2 O1 Mo2 97.5(2) . 2_655
Mo1 O1 Mo2 92.4(2) 2_655 2_655
Mo2 O2 Mo1 114.7(4) . .
Mo2 O5 Mo2 108.3(3) 2_655 3_665
Mo2 O5 Mo2 108.3(3) 2_655 .
Mo2 O5 Mo2 108.3(3) 3_665 .
Mo2 O6 Zn1 169.6(5) . .
O3W O3W Zn1 116(2) 4_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.710(8) 18_656
Mo1 O3 1.710(8) .
Mo1 O2 1.961(7) .
Mo1 O2 1.961(7) 18_656
Mo1 O1 2.232(5) 3_665
Mo1 O1 2.232(6) 17_556
Mo1 Mn1 3.1974(9) .
Mo2 O6 1.720(7) .
Mo2 O4 1.726(7) .
Mo2 O2 1.870(7) .
Mo2 O5 2.068(4) .
Mo2 O1 2.221(6) .
Mo2 O1 2.237(6) 3_665
Mo2 Mn1 3.1726(7) .
Mn1 O1 1.887(6) 17_556
Mn1 O1 1.887(6) 2_655
Mn1 O1 1.887(6) 3_665
Mn1 O1 1.887(6) .
Mn1 O1 1.887(6) 16_546
Mn1 O1 1.887(6) 18_656
Mn1 Mo2 3.1726(7) 3_665
Mn1 Mo2 3.1726(7) 17_556
Mn1 Mo2 3.1726(7) 2_655
Mn1 Mo2 3.1727(7) 18_656
Mn1 Mo2 3.1727(7) 16_546
Zn1 O1W 1.950(9) .
Zn1 O2W 2.053(8) .
Zn1 O6 2.055(7) .
Zn1 O6 2.055(7) 12_557
Zn1 O3W 2.13(3) .
Zn1 O3W 2.13(3) 12_557
O1 Mo1 2.232(5) 2_655
O1 Mo2 2.237(6) 2_655
O5 Mo2 2.068(4) 2_655
O5 Mo2 2.068(4) 3_665
O3W O3W 1.57(6) 4_557
