#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/54/4505451.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_4505451
loop_
_publ_author_name
'Tan, Huaqiao'
'Li, Yangguang'
'Chen, Weilin'
'Yan, Aixue'
'Liu, Ding'
'Wang, Enbo'
_publ_section_title
;
 A Series of [MnMo9O32]6--Based Solids: Homochiral Transferred from
 Adjacent Polyoxoanions to One-, Two-, and Three-Dimensional Frameworks
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1111
_journal_paper_doi               10.1021/cg2004936
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'H23 Mn Mo9 Ni3 O43.5'
_chemical_formula_weight         1813.71
_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                   15.706(2)
_cell_length_b                   15.706(2)
_cell_length_c                   12.462(3)
_cell_measurement_reflns_used    1356
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.41
_cell_volume                     2662.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1561
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8568
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.089
_exptl_absorpt_correction_T_max  0.571
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2574
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.838
_refine_diff_density_min         -2.804
_refine_diff_density_rms         0.390
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(19)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1356
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+97.4019P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                1032
_reflns_number_total             1356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2004936_si_002.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      R32
_cod_original_formula_sum        'H23 Mn Mo9 Ni3 O43.50'
_cod_database_code               4505451
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
Mn1 Mn 1.0000 1.0000 1.0000 0.0163(14) Uani 1 6 d S
Mo2 Mo 1.20349(13) 1.0000 1.0000 0.0232(5) Uani 1 2 d S
Mo3 Mo 0.91334(12) 1.05499(11) 1.20151(13) 0.0226(4) Uani 1 1 d .
O4 O 0.9332(9) 0.8909(9) 0.9088(10) 0.017(2) Uani 1 1 d U
O3 O 1.2987(12) 1.0605(11) 0.9113(13) 0.038(4) Uani 1 1 d .
O2 O 1.1146(10) 0.8864(11) 0.9117(11) 0.027(3) Uani 1 1 d .
O5 O 0.9673(13) 1.1513(10) 1.2885(11) 0.039(4) Uani 1 1 d .
O1 O 0.7983(12) 0.9798(12) 1.2551(13) 0.037(4) Uani 1 1 d .
OW2 O 0.6667 0.7824(10) 1.3333 0.016(3) Uani 1 2 d SU
OW1 O 0.6667 1.0360(10) 1.3333 0.023(4) Uani 1 2 d SU
O6 O 1.0000 1.0000 1.260(2) 0.033(6) Uani 1 3 d S
OW3 O 0.743(4) 0.945(4) 1.485(4) 0.021(11) Uani 0.25 1 d PU
OW5 O 1.474(4) 1.141(4) 0.8333 0.16(2) Uiso 1 2 d S
OW4 O 1.6667 1.3333 0.8333 0.12(3) Uiso 1 6 d S
Ni1 Ni 0.6667 0.9132(5) 1.3333 0.109(3) Uani 1 2 d SU
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'
Mo Mo -1.6832 0.6857 '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'
Ni Ni 0.3393 1.1124 '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 Mn1 O4 168.2(7) . 5_677
O4 Mn1 O4 87.2(5) . 2_765
O4 Mn1 O4 101.5(7) 5_677 2_765
O4 Mn1 O4 85.3(7) . 4_557
O4 Mn1 O4 87.2(5) 5_677 4_557
O4 Mn1 O4 168.2(7) 2_765 4_557
O4 Mn1 O4 87.2(5) . 3_675
O4 Mn1 O4 85.3(7) 5_677 3_675
O4 Mn1 O4 87.2(5) 2_765 3_675
O4 Mn1 O4 101.5(7) 4_557 3_675
O4 Mn1 O4 101.5(7) . 6_767
O4 Mn1 O4 87.2(5) 5_677 6_767
O4 Mn1 O4 85.3(7) 2_765 6_767
O4 Mn1 O4 87.2(5) 4_557 6_767
O4 Mn1 O4 168.2(7) 3_675 6_767
O4 Mn1 Mo3 43.8(4) . 5_677
O4 Mn1 Mo3 127.3(4) 5_677 5_677
O4 Mn1 Mo3 90.5(3) 2_765 5_677
O4 Mn1 Mo3 90.4(4) 4_557 5_677
O4 Mn1 Mo3 43.8(4) 3_675 5_677
O4 Mn1 Mo3 145.2(4) 6_767 5_677
O4 Mn1 Mo3 145.2(4) . 3_675
O4 Mn1 Mo3 43.8(4) 5_677 3_675
O4 Mn1 Mo3 90.4(4) 2_765 3_675
O4 Mn1 Mo3 90.5(4) 4_557 3_675
O4 Mn1 Mo3 127.3(4) 3_675 3_675
O4 Mn1 Mo3 43.8(4) 6_767 3_675
Mo3 Mn1 Mo3 171.02(6) 5_677 3_675
O4 Mn1 Mo3 43.8(4) . 4_557
O4 Mn1 Mo3 145.2(4) 5_677 4_557
O4 Mn1 Mo3 43.8(4) 2_765 4_557
O4 Mn1 Mo3 127.3(4) 4_557 4_557
O4 Mn1 Mo3 90.5(3) 3_675 4_557
O4 Mn1 Mo3 90.4(3) 6_767 4_557
Mo3 Mn1 Mo3 64.00(5) 5_677 4_557
Mo3 Mn1 Mo3 121.79(6) 3_675 4_557
O4 Mn1 Mo3 90.5(3) . 6_767
O4 Mn1 Mo3 90.4(4) 5_677 6_767
O4 Mn1 Mo3 43.8(4) 2_765 6_767
O4 Mn1 Mo3 145.2(4) 4_557 6_767
O4 Mn1 Mo3 43.8(4) 3_675 6_767
O4 Mn1 Mo3 127.3(4) 6_767 6_767
Mo3 Mn1 Mo3 64.00(5) 5_677 6_767
Mo3 Mn1 Mo3 111.24(6) 3_675 6_767
Mo3 Mn1 Mo3 64.00(5) 4_557 6_767
O4 Mn1 Mo3 127.3(4) . .
O4 Mn1 Mo3 43.8(4) 5_677 .
O4 Mn1 Mo3 145.2(4) 2_765 .
O4 Mn1 Mo3 43.8(4) 4_557 .
O4 Mn1 Mo3 90.4(3) 3_675 .
O4 Mn1 Mo3 90.5(3) 6_767 .
Mo3 Mn1 Mo3 111.24(6) 5_677 .
Mo3 Mn1 Mo3 64.00(5) 3_675 .
Mo3 Mn1 Mo3 171.02(6) 4_557 .
Mo3 Mn1 Mo3 121.79(6) 6_767 .
O4 Mn1 Mo3 90.4(3) . 2_765
O4 Mn1 Mo3 90.5(3) 5_677 2_765
O4 Mn1 Mo3 127.3(4) 2_765 2_765
O4 Mn1 Mo3 43.8(4) 4_557 2_765
O4 Mn1 Mo3 145.2(4) 3_675 2_765
O4 Mn1 Mo3 43.8(4) 6_767 2_765
Mo3 Mn1 Mo3 121.79(6) 5_677 2_765
Mo3 Mn1 Mo3 64.00(5) 3_675 2_765
Mo3 Mn1 Mo3 111.24(6) 4_557 2_765
Mo3 Mn1 Mo3 171.02(6) 6_767 2_765
Mo3 Mn1 Mo3 64.00(5) . 2_765
O3 Mo2 O3 106.9(11) 5_677 .
O3 Mo2 O2 97.9(7) 5_677 .
O3 Mo2 O2 99.7(7) . .
O3 Mo2 O2 99.7(7) 5_677 5_677
O3 Mo2 O2 97.9(7) . 5_677
O2 Mo2 O2 150.2(8) . 5_677
O3 Mo2 O4 91.9(7) 5_677 6_767
O3 Mo2 O4 160.4(6) . 6_767
O2 Mo2 O4 82.7(5) . 6_767
O2 Mo2 O4 72.9(5) 5_677 6_767
O3 Mo2 O4 160.4(6) 5_677 2_765
O3 Mo2 O4 91.9(7) . 2_765
O2 Mo2 O4 72.9(5) . 2_765
O2 Mo2 O4 82.7(5) 5_677 2_765
O4 Mo2 O4 70.2(7) 6_767 2_765
O3 Mo2 Mn1 126.5(6) 5_677 .
O3 Mo2 Mn1 126.5(6) . .
O2 Mo2 Mn1 75.1(4) . .
O2 Mo2 Mn1 75.1(4) 5_677 .
O4 Mo2 Mn1 35.1(3) 6_767 .
O4 Mo2 Mn1 35.1(3) 2_765 .
O5 Mo3 O1 104.3(8) . .
O5 Mo3 O2 100.0(7) . 4_557
O1 Mo3 O2 102.4(7) . 4_557
O5 Mo3 O6 90.4(8) . .
O1 Mo3 O6 105.0(6) . .
O2 Mo3 O6 147.2(8) 4_557 .
O5 Mo3 O4 95.7(7) . 5_677
O1 Mo3 O4 159.9(6) . 5_677
O2 Mo3 O4 74.5(6) 4_557 5_677
O6 Mo3 O4 73.6(6) . 5_677
O5 Mo3 O4 161.3(7) . 4_557
O1 Mo3 O4 89.4(6) . 4_557
O2 Mo3 O4 89.2(5) 4_557 4_557
O6 Mo3 O4 73.5(6) . 4_557
O4 Mo3 O4 70.9(7) 5_677 4_557
O5 Mo3 Mn1 130.9(6) . .
O1 Mo3 Mn1 124.4(5) . .
O2 Mo3 Mn1 76.9(4) 4_557 .
O6 Mo3 Mn1 72.9(7) . .
O4 Mo3 Mn1 35.6(3) 5_677 .
O4 Mo3 Mn1 35.6(3) 4_557 .
Mn1 O4 Mo2 102.2(5) . 3_675
Mn1 O4 Mo3 100.7(5) . 5_677
Mo2 O4 Mo3 93.0(4) 3_675 5_677
Mn1 O4 Mo3 100.6(5) . 4_557
Mo2 O4 Mo3 152.5(6) 3_675 4_557
Mo3 O4 Mo3 97.6(5) 5_677 4_557
Mo3 O2 Mo2 115.5(8) 4_557 .
Mo3 O1 Ni1 169.5(10) . .
Mo3 O6 Mo3 108.3(7) 2_765 3_675
Mo3 O6 Mo3 108.3(7) 2_765 .
Mo3 O6 Mo3 108.3(7) 3_675 .
OW3 OW3 Ni1 115(4) 5_678 .
OW1 Ni1 O1 89.7(5) . 18_657
OW1 Ni1 O1 89.7(5) . .
O1 Ni1 O1 179.3(10) 18_657 .
OW1 Ni1 OW2 180.000(11) . .
O1 Ni1 OW2 90.3(5) 18_657 .
O1 Ni1 OW2 90.3(5) . .
OW1 Ni1 OW3 92.4(14) . .
O1 Ni1 OW3 90.1(14) 18_657 .
O1 Ni1 OW3 89.9(14) . .
OW2 Ni1 OW3 87.6(14) . .
OW1 Ni1 OW3 92.4(14) . 18_657
O1 Ni1 OW3 89.9(14) 18_657 18_657
O1 Ni1 OW3 90.1(14) . 18_657
OW2 Ni1 OW3 87.6(14) . 18_657
OW3 Ni1 OW3 175(3) . 18_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 1.880(13) .
Mn1 O4 1.880(13) 5_677
Mn1 O4 1.880(13) 2_765
Mn1 O4 1.880(13) 4_557
Mn1 O4 1.880(13) 3_675
Mn1 O4 1.880(13) 6_767
Mn1 Mo3 3.1750(16) 5_677
Mn1 Mo3 3.1750(16) 3_675
Mn1 Mo3 3.1750(16) 4_557
Mn1 Mo3 3.1750(16) 6_767
Mn1 Mo3 3.1750(16) .
Mn1 Mo3 3.1750(16) 2_765
Mo2 O3 1.715(15) 5_677
Mo2 O3 1.715(15) .
Mo2 O2 1.963(15) .
Mo2 O2 1.963(15) 5_677
Mo2 O4 2.217(12) 6_767
Mo2 O4 2.217(11) 2_765
Mo3 O5 1.702(12) .
Mo3 O1 1.724(15) .
Mo3 O2 1.855(14) 4_557
Mo3 O6 2.076(10) .
Mo3 O4 2.234(12) 5_677
Mo3 O4 2.236(12) 4_557
O4 Mo2 2.217(11) 3_675
O4 Mo3 2.234(12) 5_677
O4 Mo3 2.236(12) 4_557
O2 Mo3 1.855(14) 4_557
O1 Ni1 2.039(14) .
OW2 Ni1 2.055(18) .
OW1 Ni1 1.929(18) .
O6 Mo3 2.076(10) 2_765
O6 Mo3 2.076(10) 3_675
OW3 OW3 1.54(10) 5_678
OW3 Ni1 2.15(5) .
Ni1 O1 2.039(14) 18_657
Ni1 OW3 2.15(5) 18_657
