#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:07:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179913 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/08/7020833.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_7020833
loop_
_publ_author_name
'Yang, Lei'
'Huo, Yu'
'Niu, Jingyang'
_publ_section_title
;
 Combination between [B-α-SiW9O34] unit and triangular inorganic Ni6 core
 under hydrothermal conditions: from monomer to rare dimer with malposed
 dodeca-nickel centers.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              364
_journal_page_last               367
_journal_paper_doi               10.1039/c2dt32122j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'H42 Ni6 O56 Si W9'
_chemical_formula_weight         2973.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   constr
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8278(15)
_cell_length_b                   20.7853(16)
_cell_length_c                   12.2101(10)
_cell_measurement_reflns_used    6061
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.93
_cell_volume                     4778.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0764
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24417
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    24.023
_exptl_absorpt_correction_T_max  0.008
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5352
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.627
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0352
_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)+(0.0348P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                3277
_reflns_number_total             4338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32122j.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7020833
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
W1 W 0.27920(3) 0.16159(2) 0.34325(4) 0.02136(14) Uani 1 1 d U
W3 W 0.09948(3) 0.16014(2) 0.35312(4) 0.02269(14) Uani 1 1 d U
W5 W 0.10062(3) 0.33028(2) 0.76217(4) 0.02210(14) Uani 1 1 d U
W7 W 0.19414(3) 0.08156(2) 0.54507(4) 0.02142(14) Uani 1 1 d U
W9 W 0.00537(4) 0.2500 0.57171(6) 0.02407(19) Uani 1 2 d SU
Ni1 Ni 0.27133(10) 0.39695(8) 0.80552(14) 0.0305(4) Uani 1 1 d U
Ni2 Ni 0.26543(12) 0.2500 0.79727(17) 0.0215(5) Uani 1 2 d SU
Ni3 Ni 0.34352(8) 0.17677(8) 0.61613(13) 0.0206(4) Uani 1 1 d U
Ni4 Ni 0.42633(12) 0.2500 0.43693(19) 0.0282(6) Uani 1 2 d SU
Si1 Si 0.1954(2) 0.2500 0.5543(3) 0.0114(9) Uani 1 2 d SU
O1 O 0.1928(4) 0.1859(4) 0.4764(6) 0.0145(17) Uani 1 1 d U
O3 O 0.1255(6) 0.2500 0.6346(8) 0.016(3) Uani 1 2 d SU
O4 O 0.4134(6) 0.2500 0.6021(9) 0.023(3) Uani 1 2 d SU
O5 O 0.1233(4) 0.3872(4) 0.6452(7) 0.025(2) Uani 1 1 d U
O6 O 0.3439(4) 0.1816(4) 0.4480(7) 0.024(2) Uani 1 1 d U
O7 O 0.2671(6) 0.2500 0.6260(9) 0.018(3) Uani 1 2 d SU
O8 O 0.3358(4) 0.3225(4) 0.7805(6) 0.023(2) Uani 1 1 d U
O10 O 0.1920(5) 0.3248(4) 0.8016(6) 0.025(2) Uani 1 1 d U
O12 O 0.0394(4) 0.1879(4) 0.4685(7) 0.028(2) Uani 1 1 d U
O13 O 0.0777(6) 0.2500 0.8333(9) 0.025(3) Uani 1 2 d SU
O15 O 0.2699(6) 0.2500 0.3013(9) 0.026(3) Uani 1 2 d SU
O16 O 0.2652(4) 0.1079(4) 0.6327(7) 0.026(2) Uani 1 1 d U
O17 O 0.0384(5) 0.1332(4) 0.2582(8) 0.038(2) Uani 1 1 d U
O19 O 0.1025(6) 0.2500 0.3155(10) 0.030(3) Uani 1 2 d SU
O21 O 0.3304(5) 0.1329(4) 0.2396(7) 0.035(2) Uani 1 1 d U
O22 O 0.0103(5) 0.3145(4) 0.6806(7) 0.029(2) Uani 1 1 d U
O25 O 0.2562(4) 0.0816(4) 0.4188(7) 0.027(2) Uani 1 1 d U
O26 O 0.1177(5) 0.0849(4) 0.4317(7) 0.029(2) Uani 1 1 d U
O27 O 0.0648(5) 0.3834(4) 0.8543(7) 0.036(2) Uani 1 1 d U
O29 O 0.1892(5) 0.0002(4) 0.5713(7) 0.033(2) Uani 1 1 d U
O30 O 0.1847(5) 0.1498(4) 0.2730(6) 0.027(2) Uani 1 1 d U
O34 O 0.2708(7) 0.2500 0.9681(9) 0.033(3) Uani 1 2 d SU
O35 O -0.0829(7) 0.2500 0.5431(10) 0.034(3) Uani 1 2 d SU
O38 O 0.1981(5) 0.4702(5) 0.8247(8) 0.047(3) Uani 1 1 d U
O39 O 0.4181(5) 0.1025(5) 0.6171(8) 0.045(3) Uani 1 1 d U
O42 O 0.5044(5) 0.1771(5) 0.4451(8) 0.049(3) Uani 1 1 d U
O44 O 0.4332(8) 0.2500 0.2654(12) 0.053(4) Uani 1 2 d SU
O45 O 0.2785(6) 0.3879(5) 0.9735(8) 0.054(3) Uani 1 1 d U
O46 O 0.3514(6) 0.4648(5) 0.8001(9) 0.055(3) Uani 1 1 d U
O2W O 0.1508(13) 0.2500 1.0815(19) 0.122(8) Uani 1 2 d SU
O1W O 0.4757(9) 0.4455(7) 0.9210(13) 0.115(5) Uani 1 1 d U
O3W O 0.0647(9) -0.0298(7) 0.7037(15) 0.130(6) Uani 1 1 d U
O4W O 0.1520(14) 0.0712(12) 0.087(2) 0.078(8) Uani 0.50 1 d PU
O5W O 0.0656(16) -0.0123(14) -0.039(2) 0.103(9) Uani 0.50 1 d PU
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'
Ni Ni 0.3393 1.1124 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
O21 W1 O6 102.9(4) . .
O21 W1 O15 100.9(5) . .
O6 W1 O15 91.7(4) . .
O21 W1 O25 100.3(4) . .
O6 W1 O25 90.6(4) . .
O15 W1 O25 157.5(4) . .
O21 W1 O30 98.3(4) . .
O6 W1 O30 158.8(3) . .
O15 W1 O30 85.5(4) . .
O25 W1 O30 84.3(3) . .
O21 W1 O1 169.0(4) . .
O6 W1 O1 85.9(3) . .
O15 W1 O1 85.1(4) . .
O25 W1 O1 72.7(3) . .
O30 W1 O1 72.9(3) . .
O17 W3 O26 101.3(4) . .
O17 W3 O12 101.5(4) . .
O26 W3 O12 89.0(4) . .
O17 W3 O30 100.4(4) . .
O26 W3 O30 90.9(4) . .
O12 W3 O30 157.6(4) . .
O17 W3 O19 100.0(5) . .
O26 W3 O19 158.5(4) . .
O12 W3 O19 84.2(4) . .
O30 W3 O19 87.8(4) . .
O17 W3 O1 172.6(3) . .
O26 W3 O1 74.2(3) . .
O12 W3 O1 84.4(3) . .
O30 W3 O1 74.1(3) . .
O19 W3 O1 84.9(4) . .
O27 W5 O10 104.0(4) . .
O27 W5 O5 100.3(4) . .
O10 W5 O5 91.5(4) . .
O27 W5 O13 100.0(4) . .
O10 W5 O13 92.2(5) . .
O5 W5 O13 157.7(4) . .
O27 W5 O22 95.6(4) . .
O10 W5 O22 160.3(3) . .
O5 W5 O22 85.3(3) . .
O13 W5 O22 83.8(4) . .
O27 W5 O3 168.2(4) . .
O10 W5 O3 86.6(4) . .
O5 W5 O3 84.2(3) . .
O13 W5 O3 74.1(3) . .
O22 W5 O3 73.8(3) . .
O29 W7 O16 103.2(4) . .
O29 W7 O25 100.5(4) . .
O16 W7 O25 91.4(4) . .
O29 W7 O5 100.1(4) . 8_565
O16 W7 O5 92.0(4) . 8_565
O25 W7 O5 157.8(3) . 8_565
O29 W7 O26 97.1(4) . .
O16 W7 O26 159.6(3) . .
O25 W7 O26 83.3(4) . .
O5 W7 O26 85.9(3) 8_565 .
O29 W7 O1 169.0(3) . .
O16 W7 O1 86.5(3) . .
O25 W7 O1 73.7(3) . .
O5 W7 O1 84.7(3) 8_565 .
O26 W7 O1 73.1(3) . .
O35 W9 O22 101.1(4) . .
O35 W9 O22 101.1(4) . 8_565
O22 W9 O22 90.3(5) . 8_565
O35 W9 O12 101.1(4) . .
O22 W9 O12 157.6(4) . .
O22 W9 O12 88.2(4) 8_565 .
O35 W9 O12 101.1(4) . 8_565
O22 W9 O12 88.2(4) . 8_565
O22 W9 O12 157.6(4) 8_565 8_565
O12 W9 O12 84.8(5) . 8_565
O35 W9 O3 173.1(5) . .
O22 W9 O3 74.2(3) . .
O22 W9 O3 74.2(3) 8_565 .
O12 W9 O3 84.0(3) . .
O12 W9 O3 84.0(3) 8_565 .
O8 Ni1 O45 92.4(4) . .
O8 Ni1 O38 175.4(4) . .
O45 Ni1 O38 89.9(4) . .
O8 Ni1 O46 94.6(4) . .
O45 Ni1 O46 92.7(4) . .
O38 Ni1 O46 89.3(4) . .
O8 Ni1 O16 81.0(3) . 8_565
O45 Ni1 O16 172.0(4) . 8_565
O38 Ni1 O16 96.4(4) . 8_565
O46 Ni1 O16 92.3(4) . 8_565
O8 Ni1 O10 82.9(3) . .
O45 Ni1 O10 90.2(4) . .
O38 Ni1 O10 93.1(4) . .
O46 Ni1 O10 176.3(4) . .
O16 Ni1 O10 84.6(3) 8_565 .
O8 Ni2 O8 96.7(5) 8_565 .
O8 Ni2 O10 83.1(3) 8_565 8_565
O8 Ni2 O10 175.6(3) . 8_565
O8 Ni2 O10 175.6(3) 8_565 .
O8 Ni2 O10 83.1(3) . .
O10 Ni2 O10 96.7(5) 8_565 .
O8 Ni2 O7 83.6(3) 8_565 .
O8 Ni2 O7 83.6(3) . .
O10 Ni2 O7 92.0(3) 8_565 .
O10 Ni2 O7 92.0(3) . .
O8 Ni2 O34 94.0(3) 8_565 .
O8 Ni2 O34 94.0(3) . .
O10 Ni2 O34 90.4(3) 8_565 .
O10 Ni2 O34 90.4(3) . .
O7 Ni2 O34 176.3(5) . .
O4 Ni3 O8 97.3(4) . 8_565
O4 Ni3 O16 175.0(4) . .
O8 Ni3 O16 81.7(3) 8_565 .
O4 Ni3 O6 82.9(4) . .
O8 Ni3 O6 174.9(3) 8_565 .
O16 Ni3 O6 97.7(3) . .
O4 Ni3 O39 96.9(4) . .
O8 Ni3 O39 92.8(4) 8_565 .
O16 Ni3 O39 88.1(4) . .
O6 Ni3 O39 92.3(4) . .
O4 Ni3 O7 84.6(3) . .
O8 Ni3 O7 83.5(4) 8_565 .
O16 Ni3 O7 90.4(3) . .
O6 Ni3 O7 91.4(4) . .
O39 Ni3 O7 176.2(4) . .
O4 Ni4 O44 176.7(5) . .
O4 Ni4 O42 92.1(4) . 8_565
O44 Ni4 O42 90.2(4) . 8_565
O4 Ni4 O42 92.1(4) . .
O44 Ni4 O42 90.2(4) . .
O42 Ni4 O42 91.6(6) 8_565 .
O4 Ni4 O6 81.3(3) . .
O44 Ni4 O6 96.3(4) . .
O42 Ni4 O6 172.8(4) 8_565 .
O42 Ni4 O6 91.4(4) . .
O4 Ni4 O6 81.3(3) . 8_565
O44 Ni4 O6 96.3(4) . 8_565
O42 Ni4 O6 91.4(4) 8_565 8_565
O42 Ni4 O6 172.8(4) . 8_565
O6 Ni4 O6 84.8(4) . 8_565
O7 Si1 O1 110.0(4) . .
O7 Si1 O1 110.0(4) . 8_565
O1 Si1 O1 108.9(6) . 8_565
O7 Si1 O3 110.3(6) . .
O1 Si1 O3 108.8(4) . .
O1 Si1 O3 108.8(4) 8_565 .
Si1 O1 W7 123.3(4) . .
Si1 O1 W1 123.7(4) . .
W7 O1 W1 92.3(3) . .
Si1 O1 W3 125.0(4) . .
W7 O1 W3 91.5(3) . .
W1 O1 W3 91.4(2) . .
Si1 O3 W5 124.1(3) . .
Si1 O3 W5 124.1(3) . 8_565
W5 O3 W5 91.5(4) . 8_565
Si1 O3 W9 124.5(5) . .
W5 O3 W9 91.4(3) . .
W5 O3 W9 91.4(3) 8_565 .
Ni3 O4 Ni3 97.8(5) . 8_565
Ni3 O4 Ni4 99.3(4) . .
Ni3 O4 Ni4 99.3(4) 8_565 .
W5 O5 W7 147.4(5) . 8_565
W1 O6 Ni3 133.6(4) . .
W1 O6 Ni4 127.1(4) . .
Ni3 O6 Ni4 95.7(3) . .
Si1 O7 Ni2 122.1(6) . .
Si1 O7 Ni3 122.9(4) . .
Ni2 O7 Ni3 93.9(4) . .
Si1 O7 Ni3 122.9(4) . 8_565
Ni2 O7 Ni3 93.9(4) . 8_565
Ni3 O7 Ni3 93.0(4) . 8_565
Ni1 O8 Ni2 99.5(4) . .
Ni1 O8 Ni3 101.0(4) . 8_565
Ni2 O8 Ni3 98.9(3) . 8_565
W5 O10 Ni2 132.8(4) . .
W5 O10 Ni1 129.7(4) . .
Ni2 O10 Ni1 93.5(3) . .
W3 O12 W9 153.3(5) . .
W5 O13 W5 119.7(5) 8_565 .
W1 O15 W1 147.2(6) . 8_565
W7 O16 Ni3 133.2(4) . .
W7 O16 Ni1 128.3(4) . 8_565
Ni3 O16 Ni1 95.3(3) . 8_565
W3 O19 W3 152.2(7) . 8_565
W9 O22 W5 120.6(4) . .
W7 O25 W1 120.8(4) . .
W3 O26 W7 121.2(4) . .
W3 O30 W1 121.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O21 1.699(8) .
W1 O6 1.815(8) .
W1 O15 1.916(3) .
W1 O25 1.950(8) .
W1 O30 1.991(8) .
W1 O1 2.355(7) .
W3 O17 1.727(9) .
W3 O26 1.866(8) .
W3 O12 1.898(8) .
W3 O30 1.891(8) .
W3 O19 1.924(3) .
W3 O1 2.375(7) .
W5 O27 1.714(8) .
W5 O10 1.790(9) .
W5 O5 1.903(8) .
W5 O13 1.930(5) .
W5 O22 1.997(9) .
W5 O3 2.330(7) .
W7 O29 1.724(8) .
W7 O16 1.799(8) .
W7 O25 1.935(8) .
W7 O5 1.923(8) 8_565
W7 O26 1.998(9) .
W7 O1 2.326(7) .
W9 O35 1.698(12) .
W9 O22 1.891(8) .
W9 O22 1.891(8) 8_565
W9 O12 1.914(8) .
W9 O12 1.914(8) 8_565
W9 O3 2.389(11) .
Ni1 O8 1.989(8) .
Ni1 O45 2.064(10) .
Ni1 O38 2.067(10) .
Ni1 O46 2.065(10) .
Ni1 O16 2.116(8) 8_565
Ni1 O10 2.117(9) .
Ni2 O8 2.017(8) 8_565
Ni2 O8 2.017(8) .
Ni2 O10 2.081(8) 8_565
Ni2 O10 2.081(8) .
Ni2 O7 2.091(11) .
Ni2 O34 2.088(12) .
Ni3 O4 2.019(8) .
Ni3 O8 2.013(8) 8_565
Ni3 O16 2.065(8) .
Ni3 O6 2.056(8) .
Ni3 O39 2.088(9) .
Ni3 O7 2.098(8) .
Ni4 O4 2.031(11) .
Ni4 O44 2.099(14) .
Ni4 O42 2.112(10) 8_565
Ni4 O42 2.112(10) .
Ni4 O6 2.108(8) .
Ni4 O6 2.108(8) 8_565
Si1 O7 1.609(11) .
Si1 O1 1.637(8) .
Si1 O1 1.637(8) 8_565
Si1 O3 1.641(11) .
O3 W5 2.330(7) 8_565
O4 Ni3 2.019(8) 8_565
O5 W7 1.923(8) 8_565
O7 Ni3 2.098(8) 8_565
O8 Ni3 2.013(8) 8_565
O13 W5 1.930(5) 8_565
O15 W1 1.916(3) 8_565
O16 Ni1 2.116(8) 8_565
O19 W3 1.924(3) 8_565
