#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:53:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179429 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/26/4332687.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332687
loop_
_publ_author_name
'Uchida, Sayaka'
'Kawamoto, Ryosuke'
'Mizuno, Noritaka'
_publ_section_title
;
 Recognition of Small Polar Molecules with an Ionic Crystal of
 α-Keggin-Type Polyoxometalate with a Macrocation
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5136
_journal_page_last               5144
_journal_paper_doi               10.1021/ic060684x
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C6 H44 B Cr3 O72 Rb4 W12'
_chemical_formula_weight         3983.30
_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_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                   24.680(10)
_cell_length_b                   16.137(5)
_cell_length_c                   17.281(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.30
_cell_measurement_theta_min      17.44
_cell_volume                     6882(5)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure 
Corporation, 1993)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure 
Corporation, 1993)
;
_computing_data_reduction
;
teXsan (Molecular Structure Corporation, 1995)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type
;
RIGAKU four-cricle automatic X-ray diffractometer
;
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2719
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10375
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -8.5
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    23.352
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3167
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7076
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.511
_refine_diff_density_min         -3.168
_refine_diff_density_rms         0.512
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         10375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.2496
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0444P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                3879
_reflns_number_total             10375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060684xsup3.cif
_cod_data_source_block           '__3a'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'psiscan' changed to
'psi-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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4332687
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, 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_calc_flag
_atom_site_refinement_flags
W1 W 0.47810(4) 0.13709(5) 0.31248(6) 0.0279(2) Uani 1 d .
W2 W 0.50458(4) 0.13711(5) 0.12369(6) 0.0296(2) Uani 1 d .
W3 W 0.58379(4) 0.03409(5) 0.24393(7) 0.0280(2) Uani 1 d .
W4 W 0.56744(7) 0.2500 0.44504(9) 0.0303(4) Uani 1 d S
W5 W 0.67292(4) 0.14752(5) 0.37534(6) 0.0298(2) Uani 1 d .
W6 W 0.70133(4) 0.14683(5) 0.16808(6) 0.0260(2) Uani 1 d .
W7 W 0.62111(7) 0.2500 0.04888(9) 0.0269(3) Uani 1 d S
Rb1 Rb 0.65798(13) 0.01699(15) 0.56944(16) 0.0424(7) Uani 1 d .
Rb2 Rb 0.70194(14) 0.04571(17) -0.06052(18) 0.0553(8) Uani 1 d .
Cr1 Cr 0.63222(15) 0.14807(19) 0.7520(2) 0.0248(8) Uani 1 d .
Cr2 Cr 0.5185(2) 0.2500 0.7757(3) 0.0264(13) Uani 1 d S
B B 0.5906(19) 0.2500 0.240(4) 0.047(14) Uani 1 d S
O1 O 0.4213(7) 0.1008(10) 0.3579(11) 0.042(5) Uani 1 d .
O2 O 0.4647(8) 0.0982(12) 0.0500(11) 0.050(5) Uani 1 d .
O3 O 0.5982(7) -0.0694(8) 0.2467(11) 0.033(4) Uani 1 d .
O4 O 0.5433(12) 0.2500 0.5357(14) 0.043(7) Uani 1 d S
O5 O 0.7147(8) 0.0829(9) 0.4248(10) 0.041(5) Uani 1 d .
O6 O 0.7537(8) 0.0812(9) 0.1463(10) 0.041(5) Uani 1 d .
O7 O 0.6206(13) 0.2500 -0.0496(17) 0.053(8) Uani 1 d S
O8 O 0.4548(7) 0.1199(9) 0.2077(10) 0.035(4) Uani 1 d .
O9 O 0.5191(7) 0.0377(8) 0.3054(10) 0.036(5) Uani 1 d .
O10 O 0.5407(6) 0.0357(8) 0.1526(9) 0.026(4) Uani 1 d .
O11 O 0.4590(10) 0.2500 0.3021(14) 0.033(6) Uani 1 d S
O12 O 0.4825(11) 0.2500 0.1228(13) 0.031(6) Uani 1 d S
O13 O 0.5217(8) 0.1700(8) 0.3968(9) 0.035(4) Uani 1 d .
O14 O 0.6212(8) 0.1671(8) 0.4574(9) 0.036(4) Uani 1 d .
O15 O 0.7067(12) 0.2500 0.4024(15) 0.039(7) Uani 1 d S
O16 O 0.6239(7) 0.0705(8) 0.3332(10) 0.031(4) Uani 1 d .
O17 O 0.6448(6) 0.0706(8) 0.1829(10) 0.026(4) Uani 1 d .
O18 O 0.7076(8) 0.1517(8) 0.2790(9) 0.035(4) Uani 1 d .
O19 O 0.7412(9) 0.2500 0.1639(13) 0.022(5) Uani 1 d S
O20 O 0.6757(6) 0.1679(10) 0.0657(9) 0.030(4) Uani 1 d .
O21 O 0.5675(7) 0.1699(9) 0.0690(9) 0.030(4) Uani 1 d .
O22 O 0.5550(6) 0.1721(8) 0.2357(9) 0.025(4) Uani 1 d .
O23 O 0.6175(10) 0.2500 0.3239(13) 0.026(6) Uani 1 d S
O24 O 0.6351(10) 0.2500 0.1818(16) 0.034(6) Uani 1 d S
O31 O 0.5928(8) 0.2500 0.7588(15) 0.022(5) Uani 1 d S
O32 O 0.6758(6) 0.0419(8) 0.7405(10) 0.027(4) Uani 1 d .
O33 O 0.4349(12) 0.2500 0.7929(18) 0.063(9) Uani 1 d S
O34 O 0.5821(8) 0.0983(10) 0.6757(10) 0.039(5) Uani 1 d .
O35 O 0.5048(8) 0.1662(9) 0.6968(10) 0.040(5) Uani 1 d .
O36 O 0.5953(8) 0.0951(10) 0.8408(11) 0.045(5) Uani 1 d .
O37 O 0.5200(7) 0.1645(9) 0.8602(10) 0.035(4) Uani 1 d .
O38 O 0.6752(7) 0.1802(9) 0.6590(9) 0.031(4) Uani 1 d .
O39 O 0.6912(7) 0.1814(10) 0.8256(10) 0.035(4) Uani 1 d .
C1 C 0.5343(11) 0.1156(14) 0.6603(14) 0.030(6) Uiso 1 d .
C2 C 0.5528(11) 0.1103(14) 0.8765(15) 0.033(6) Uiso 1 d .
C3 C 0.6849(14) 0.2500 0.627(2) 0.029(8) Uiso 1 d S
C4 C 0.7074(19) 0.2500 0.848(3) 0.048(11) Uiso 1 d S
OW1 O 0.6546(7) -0.0855(10) 0.8305(12) 0.049(5) Uani 1 d .
OW2 O 0.3817(10) 0.0227(15) -0.0317(12) 0.075(8) Uani 1 d .
OW3 O 0.5566(10) -0.0029(13) 0.4735(13) 0.066(7) Uani 1 d .
OW4 O 0.7798(9) 0.0848(18) 0.750(2) 0.125(12) Uani 1 d .
OW5 O 0.8030(11) 0.1335(13) -0.0324(16) 0.094(9) Uani 1 d .
OW6 O 0.7896(12) 0.1000(16) 0.5764(17) 0.106(10) Uani 1 d .
OW7 O 0.8394(18) 0.2500 0.087(3) 0.125(17) Uani 1 d S
OW8 O 0.8155(18) 0.2500 0.312(3) 0.13(2) Uani 1 d S
OW9 O 0.4216(15) 0.2500 0.9499(14) 0.072(10) Uani 1 d S
OW10 O 0.8089(16) 0.2500 0.498(2) 0.098(14) Uani 1 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
