#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320271.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_4320271
loop_
_publ_author_name
'Maxim N. Sokolov'
'Alexander V.Virovets'
'Danil N. Dybtsev'
'Elena V. Chubarova'
'Vladimir P.Fedin'
'Dieter Fenske'
_publ_contact_author
;
        Prof. Valdimir P.Fedin
        Institute of Inorganic Chemistry SD RAS
        Ak.Lavrentiev prosp. 3
        Novosibirsk 630090
        Russia
;
_publ_contact_author_email       cluster@che.nsk.su
_publ_contact_author_fax         '007 3832 344489'
_publ_contact_author_phone       none
_publ_section_title
;
 Phosphorous Acid and Arsenious Acid as Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4816
_journal_page_last               4817
_journal_paper_doi               10.1021/ic015520p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural
'(Mo3 S4 Cl3 (H2 O)6 Pd (P (O H)3))2 (C36 H36 N24 O12) Cl2 . 20(H2 O)'
_chemical_formula_sum            'C36 H106 Cl8 Mo6 N24 O50 P2 Pd2 S8'
_chemical_formula_weight         3065.91
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
 Bis(tetra(mu3-thio)(phosporoustrihydroxo)trichlorohexaaquatrimolybdenum
palladium) cucurbituril dichloride dodecahydrate
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.669(6)
_cell_length_b                   21.669(6)
_cell_length_c                   21.669(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    212(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      15
_cell_volume                     10175(5)
_computing_cell_refinement       'STOE STADI4 software'
_computing_data_collection       'STOE STADI4 software'
_computing_data_reduction        'XRED (STOE)'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      212(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'STOE STADI4 Diffractometer'
_diffrn_measurement_method       θ/2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       -1
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            3953
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XRED (STOE)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0599
_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)+(0.0667P)²+105.1865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                2832
_reflns_number_total             3953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015520p_s1_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4320271
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.23763(2) 0.23763(2) 0.23763(2) 0.0250(2) Uani 1 3 d S . .
Mo1 Mo 0.22753(3) 0.12353(3) 0.17513(3) 0.02444(19) Uani 1 1 d . . .
S1 S 0.12950(8) 0.12950(8) 0.12950(8) 0.0289(7) Uani 1 3 d S . .
S2 S 0.27979(8) 0.21072(9) 0.14109(9) 0.0268(4) Uani 1 1 d . . .
Cl11 Cl 0.33111(9) 0.08466(9) 0.20593(10) 0.0361(5) Uani 1 1 d . . .
O12M O 0.2551(3) 0.0789(3) 0.0881(3) 0.0376(13) Uani 1 1 d . . .
O13M O 0.2044(3) 0.0250(3) 0.1934(3) 0.0393(14) Uani 1 1 d . . .
P1 P 0.29781(10) 0.29781(10) 0.29781(10) 0.0420(9) Uani 1 3 d S . .
O1 O 0.3680(5) 0.2923(8) 0.2825(7) 0.149(6) Uani 1 1 d . . .
C111 C 0.1792(4) -0.0296(5) -0.1478(4) 0.045(2) Uani 1 1 d . . .
H111 H 0.2145 -0.0457 -0.1719 0.045 Uiso 1 1 calc R . .
C112 C 0.1520(4) 0.0281(5) -0.1774(4) 0.042(2) Uani 1 1 d . . .
H112 H 0.1751 0.0406 -0.2147 0.042 Uiso 1 1 calc R . .
C11 C 0.1842(4) 0.0506(4) -0.0767(4) 0.0365(19) Uani 1 1 d . . .
O11 O 0.1929(3) 0.0796(3) -0.0296(3) 0.0469(16) Uani 1 1 d . . .
C12 C 0.0770(4) -0.0481(4) -0.1754(4) 0.040(2) Uani 1 1 d . . .
O12 O 0.0290(3) -0.0764(3) -0.1841(3) 0.0484(16) Uani 1 1 d . . .
N11 N 0.1279(3) -0.0730(4) -0.1473(4) 0.0424(18) Uani 1 1 d . . .
N12 N 0.0890(4) 0.0098(4) -0.1918(4) 0.0427(18) Uani 1 1 d . . .
N13 N 0.1566(4) 0.0736(4) -0.1286(3) 0.0418(18) Uani 1 1 d . . .
N14 N 0.1985(3) -0.0092(4) -0.0868(4) 0.0411(17) Uani 1 1 d . . .
C11B C 0.2309(4) -0.0469(5) -0.0450(5) 0.047(2) Uani 1 1 d . . .
H11A H 0.2534 -0.0204 -0.0160 0.047 Uiso 1 1 calc R . .
H11B H 0.2614 -0.0711 -0.0679 0.047 Uiso 1 1 calc R . .
C12B C 0.1357(4) -0.1386(5) -0.1366(4) 0.045(2) Uani 1 1 d . . .
H12A H 0.1055 -0.1611 -0.1617 0.045 Uiso 1 1 calc R . .
H12B H 0.1769 -0.1507 -0.1507 0.045 Uiso 1 1 calc R . .
Cl1 Cl 0.572(2) 0.460(2) 0.391(2) 0.37(2) Uiso 0.33 1 d P . .
O1W O 0.4829(5) 0.3204(5) 0.3282(5) 0.104(4) Uani 1 1 d . . .
O2W1 O 0.3186(10) -0.0547(10) 0.1708(10) 0.084(6) Uiso 0.50 1 d P . .
O2W2 O 0.2890(10) -0.0660(9) 0.1893(9) 0.076(5) Uiso 0.50 1 d P . .
O3W1 O 0.3702(10) -0.0038(10) 0.0666(10) 0.099(6) Uiso 0.50 1 d P . .
O3W2 O 0.3696(17) 0.0731(18) 0.0264(17) 0.180(14) Uiso 0.50 1 d P . .
O4W O 0.0517(9) 0.0309(12) 0.0107(9) 0.045(5) Uani 0.33 1 d P . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 '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
_geom_angle_publ_flag
Mo1 Pd1 Mo1 58.42(3) 5 . no
Mo1 Pd1 Mo1 58.42(3) 5 9 no
Mo1 Pd1 Mo1 58.42(3) . 9 no
S2 Pd1 Mo1 98.73(5) 9 5 no
S2 Pd1 Mo1 52.42(5) . 5 no
S2 Pd1 Mo1 52.29(5) 5 5 no
S2 Pd1 Mo1 52.42(5) 9 . no
S2 Pd1 Mo1 52.29(5) . . no
S2 Pd1 Mo1 98.73(5) 5 . no
S2 Pd1 Mo1 52.29(5) 9 9 no
S2 Pd1 Mo1 98.73(5) . 9 no
S2 Pd1 Mo1 52.42(5) 5 9 no
S2 Pd1 S2 102.74(6) 9 . no
S2 Pd1 S2 102.74(6) 9 5 no
S2 Pd1 S2 102.74(6) . 5 no
P1 Pd1 Mo1 145.699(16) . 5 no
P1 Pd1 Mo1 145.699(16) . . no
P1 Pd1 Mo1 145.699(16) . 9 no
P1 Pd1 S2 115.57(5) . 9 no
P1 Pd1 S2 115.57(5) . . no
P1 Pd1 S2 115.57(5) . 5 no
Mo1 Mo1 Pd1 60.788(13) 5 . no
Mo1 Mo1 Pd1 60.788(13) 9 . no
Mo1 Mo1 Mo1 60.0 5 9 no
S1 Mo1 Pd1 102.93(6) . . no
S1 Mo1 Mo1 53.98(4) . 5 no
S1 Mo1 Mo1 53.98(4) . 9 no
S1 Mo1 Cl11 161.46(7) . . no
S2 Mo1 Pd1 53.36(5) . . no
S2 Mo1 Pd1 53.32(5) 9 . no
S2 Mo1 Mo1 53.69(5) . 5 no
S2 Mo1 Mo1 101.35(5) 9 5 no
S2 Mo1 Mo1 101.49(5) . 9 no
S2 Mo1 Mo1 53.52(5) 9 9 no
S2 Mo1 S1 105.23(6) . . no
S2 Mo1 S1 105.06(6) 9 . no
S2 Mo1 S2 104.64(9) . 9 no
S2 Mo1 Cl11 85.45(7) . . no
S2 Mo1 Cl11 86.28(7) 9 . no
Cl11 Mo1 Pd1 95.61(5) . . no
Cl11 Mo1 Mo1 139.12(6) . 5 no
Cl11 Mo1 Mo1 139.75(6) . 9 no
O12M Mo1 Pd1 140.66(16) . . no
O12M Mo1 Mo1 97.08(16) . 5 no
O12M Mo1 Mo1 138.74(16) . 9 no
O12M Mo1 S1 84.76(17) . . no
O12M Mo1 S2 87.32(17) . . no
O12M Mo1 S2 161.52(17) . 9 no
O12M Mo1 Cl11 80.59(17) . . no
O12M Mo1 O13M 78.0(2) . . no
O13M Mo1 Pd1 140.34(16) . . no
O13M Mo1 Mo1 139.61(16) . 5 no
O13M Mo1 Mo1 97.54(17) . 9 no
O13M Mo1 S1 85.64(16) . . no
O13M Mo1 S2 160.97(18) . . no
O13M Mo1 S2 87.02(17) . 9 no
O13M Mo1 Cl11 80.27(17) . . no
Mo1 S1 Mo1 72.04(8) 5 . no
Mo1 S1 Mo1 72.04(8) 5 9 no
Mo1 S1 Mo1 72.04(8) . 9 no
Mo1 S2 Pd1 74.35(6) . . no
Mo1 S2 Pd1 74.25(6) 5 . no
Mo1 S2 Mo1 72.79(6) . 5 no
O1 P1 Pd1 113.3(5) . . no
O1 P1 Pd1 113.3(5) 9 . no
O1 P1 Pd1 113.3(5) 5 . no
O1 P1 O1 105.4(6) . 9 no
O1 P1 O1 105.4(6) . 5 no
O1 P1 O1 105.4(6) 9 5 no
N11 C111 C112 103.7(7) . . no
N14 C111 C112 104.2(7) . . no
N14 C111 N11 114.2(8) . . no
N12 C112 C111 103.3(7) . . no
N13 C112 C111 103.0(7) . . no
N13 C112 N12 114.0(7) . . no
O11 C11 N13 124.9(9) . . no
O11 C11 N14 126.6(9) . . no
N14 C11 N13 108.5(7) . . no
O12 C12 N11 123.7(9) . . no
O12 C12 N12 126.8(10) . . no
N12 C12 N11 109.5(8) . . no
C12 N11 C111 110.9(8) . . no
C12 N11 C12B 123.4(7) . . no
C12B N11 C111 123.0(8) . . no
C112 N12 C11B 124.7(8) . 21 no
C12 N12 C112 112.4(8) . . no
C12 N12 C11B 121.7(8) . 21 no
C11 N13 C112 112.4(8) . . no
C11 N13 C12B 123.8(8) . 21 no
C12B N13 C112 123.6(8) 21 . no
C11 N14 C111 111.8(8) . . no
C11 N14 C11B 124.6(8) . . no
C11B N14 C111 123.5(8) . . no
N14 C11B N12 114.2(7) . 17 no
N13 C12B N11 114.1(7) 17 . no
O4W O4W O4W 60.000(5) 5 9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Mo1 2.8276(12) 5 no
Pd1 Mo1 2.8276(12) . yes
Pd1 Mo1 2.8276(12) 9 no
Pd1 S2 2.356(2) 9 no
Pd1 S2 2.356(2) . yes
Pd1 S2 2.356(2) 5 no
Pd1 P1 2.259(4) . yes
Mo1 Mo1 2.7599(13) 5 yes
Mo1 Mo1 2.7599(13) 9 no
Mo1 S1 2.347(2) . yes
Mo1 S2 2.323(2) . yes
Mo1 S2 2.328(2) 9 yes
Mo1 Cl11 2.489(2) . yes
Mo1 O12M 2.203(6) . yes
Mo1 O13M 2.228(6) . yes
S1 Mo1 2.347(2) 5 no
S1 Mo1 2.347(2) 9 no
S2 Mo1 2.328(2) 5 no
P1 O1 1.561(12) . yes
P1 O1 1.561(12) 9 no
P1 O1 1.561(12) 5 no
C111 C112 1.523(14) . no
C111 N11 1.456(11) . no
C111 N14 1.454(11) . no
C112 N12 1.456(11) . no
C112 N13 1.449(11) . no
C11 O11 1.214(10) . no
C11 N13 1.367(11) . no
C11 N14 1.350(12) . no
C12 O12 1.223(10) . no
C12 N11 1.371(12) . no
C12 N12 1.330(12) . no
N11 C12B 1.449(13) . no
N12 C11B 1.459(13) 21 no
N13 C12B 1.429(12) 21 no
N14 C11B 1.407(13) . no
C11B N12 1.459(13) 17 no
C12B N13 1.429(12) 17 no
Cl1 O3W1 1.73(5) 3_655 no
O2W1 O2W2 0.79(2) . no
O3W1 Cl1 1.73(5) 3_645 no
O4W O4W 1.09(3) 5 no
O4W O4W 1.09(3) 9 no
