#------------------------------------------------------------------------------
#$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $
#$Revision: 858 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1100716.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_1100716
_journal_name_full               Inorg.Chem.
_publ_section_title
;
Synthesis and Characterization of Twin Cubane-type Molybdenum
- Rhodium - Sulfur Cluster, [{Mo3RhCp*S4(H2O)7(O)}2]8+
X-ray structure of [{Mo3RhCp*S4(H2O)7(O)}2](CH3C6H4SO3)8.14H2O
;
loop_
_publ_author_name
'H.Akashi'
'K.Isobe'
'T.Shibahara'
_chemical_formula_sum            'C38 H71 Mo3 O27 Rh S8'
_[local]_cod_chemical_formula_sum_orig 'C38 H71 Mo3 O27 Rh1 S8'
_chemical_formula_moiety         'C38 H71 Mo3 O27 Rh1 S8'
_chemical_formula_weight         1607.17
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
_cell_length_a                   12.2631(8)
_cell_length_b                   15.911(1)
_cell_length_c                   17.389(3)
_cell_angle_alpha                63.704(3)
_cell_angle_beta                 78.688(2)
_cell_angle_gamma                81.038(2)
_cell_volume                     2973.5(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7019
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    93.1
_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1628.00
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.939
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.32
_diffrn_reflns_number            33644
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_theta_max         27.48
_diffrn_measured_fraction_theta_max 0.9861
_diffrn_reflns_theta_full        25.75
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_reflns_number_total             13440
_reflns_number_gt                7661
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1630
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_reflns         11328
_refine_ls_number_parameters     737
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_shift/su_max          0.0000
_refine_diff_density_max         2.61
_refine_diff_density_min         -3.49
_refine_ls_extinction_method     none
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Mo Mo -1.683 0.686
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.125 0.123
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Rh Rh -1.118 0.919
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
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
Rh(1) Rh 0.01465(5) 0.18656(4) 0.63249(4) 0.0137(2) Uani 1.00 1 d . . .
Mo(1) Mo 0.01154(5) 0.37297(5) 0.46407(4) 0.0129(2) Uani 1.00 1 d . . .
Mo(2) Mo 0.21417(5) 0.26746(5) 0.51156(4) 0.0129(2) Uani 1.00 1 d . . .
Mo(3) Mo 0.09712(5) 0.37460(5) 0.59911(4) 0.0128(2) Uani 1.00 1 d . . .
S(1) S 0.1802(1) 0.4324(1) 0.4544(1) 0.0145(5) Uani 1.00 1 d . . .
S(2) S 0.0679(1) 0.2145(1) 0.4839(1) 0.0152(5) Uani 1.00 1 d . . .
S(3) S 0.1808(1) 0.2175(1) 0.6613(1) 0.0146(5) Uani 1.00 1 d . . .
S(4) S -0.0809(1) 0.3395(1) 0.6034(1) 0.0140(5) Uani 1.00 1 d . . .
S(5) S 0.2638(2) 0.7438(1) -0.3246(1) 0.0183(5) Uani 1.00 1 d . . .
S(6) S 0.4775(2) 1.0366(1) -0.3047(1) 0.0173(5) Uani 1.00 1 d . . .
S(7) S 0.2726(2) 0.5643(1) 0.2151(1) 0.0201(5) Uani 1.00 1 d . . .
S(8) S 0.7893(2) 0.7544(1) 0.0996(1) 0.0207(5) Uani 1.00 1 d . . .
O(1) O -0.1446(4) 0.3397(4) 0.4441(4) 0.019(1) Uani 1.00 1 d . . .
O(2) O 0.0514(4) 0.4009(4) 0.3260(3) 0.017(1) Uani 1.00 1 d . . .
O(3) O 0.2997(4) 0.1306(4) 0.5357(4) 0.021(1) Uani 1.00 1 d . . .
O(4) O 0.3796(4) 0.2901(4) 0.5260(4) 0.017(1) Uani 1.00 1 d . . .
O(5) O 0.2991(4) 0.2966(4) 0.3842(3) 0.016(1) Uani 1.00 1 d . . .
O(6) O 0.0346(4) 0.3459(4) 0.7360(3) 0.018(1) Uani 1.00 1 d . . .
O(7) O 0.0538(4) 0.5014(4) 0.5785(3) 0.018(1) Uani 1.00 1 d . . .
O(8) O 0.2472(4) 0.4049(4) 0.6307(3) 0.014(1) Uani 1.00 1 d . . .
O(9) O 0.3114(5) 0.6475(4) -0.3049(4) 0.022(2) Uani 1.00 1 d . . .
O(10) O 0.1630(5) 0.7642(4) -0.3646(4) 0.022(2) Uani 1.00 1 d . . .
O(11) O 0.3454(5) 0.8121(4) -0.3755(4) 0.024(2) Uani 1.00 1 d . . .
O(12) O 0.4824(4) 1.1384(4) -0.3413(4) 0.020(1) Uani 1.00 1 d . . .
O(13) O 0.3790(5) 1.0129(4) -0.3231(4) 0.024(2) Uani 1.00 1 d . . .
O(14) O 0.5801(5) 0.9889(4) -0.3299(4) 0.023(2) Uani 1.00 1 d . . .
O(15) O 0.2910(5) 0.6422(4) 0.2315(4) 0.024(2) Uani 1.00 1 d . . .
O(16) O 0.1525(5) 0.5552(4) 0.2222(4) 0.026(2) Uani 1.00 1 d . . .
O(17) O 0.3288(5) 0.4764(4) 0.2689(4) 0.023(2) Uani 1.00 1 d . . .
O(18) O 0.8458(5) 0.6637(4) 0.1500(4) 0.026(2) Uani 1.00 1 d . . .
O(19) O 0.8394(5) 0.8318(5) 0.0957(4) 0.028(2) Uani 1.00 1 d . . .
O(20) O 0.6681(5) 0.7561(5) 0.1266(4) 0.031(2) Uani 1.00 1 d . . .
O(21) O 0.8788(5) 0.4644(4) 0.2362(4) 0.027(2) Uani 1.00 1 d . . .
O(22) O 0.5859(4) 0.7142(4) 0.2919(4) 0.020(1) Uani 1.00 1 d . . .
O(23) O 0.4229(5) 0.5895(4) 0.3567(4) 0.025(2) Uani 1.00 1 d . . .
O(24) O 0.5550(5) 0.8188(5) -0.3442(4) 0.029(2) Uani 1.00 1 d . . .
O(25) O 0.3088(5) 0.9945(5) -0.5088(4) 0.030(2) Uani 1.00 1 d . . .
O(26) O -0.3330(4) 0.4331(4) 0.4803(4) 0.022(2) Uani 1.00 1 d . . .
O(27) O 0.4871(4) 0.5930(4) -0.4008(4) 0.021(1) Uani 1.00 1 d . . .
C(1) C 0.0185(7) 0.0565(6) 0.7514(5) 0.019(2) Uani 1.00 1 d . . .
C(2) C 0.0155(6) 0.0343(5) 0.6817(5) 0.018(2) Uani 1.00 1 d . . .
C(3) C -0.0895(6) 0.0788(5) 0.6473(5) 0.017(2) Uani 1.00 1 d . . .
C(4) C -0.1475(7) 0.1273(6) 0.6969(5) 0.021(2) Uani 1.00 1 d . . .
C(5) C -0.0794(6) 0.1159(6) 0.7608(5) 0.018(2) Uani 1.00 1 d . . .
C(6) C 0.1037(7) 0.0168(6) 0.8122(6) 0.025(2) Uani 1.00 1 d . . .
C(7) C 0.0961(7) -0.0290(6) 0.6519(6) 0.023(2) Uani 1.00 1 d . . .
C(8) C -0.1360(7) 0.0679(7) 0.5794(6) 0.027(2) Uani 1.00 1 d . . .
C(9) C -0.2611(6) 0.1767(6) 0.6876(6) 0.022(2) Uani 1.00 1 d . . .
C(10) C -0.1072(7) 0.1517(7) 0.8292(6) 0.027(2) Uani 1.00 1 d . . .
C(11) C 0.2223(6) 0.7534(6) -0.2254(5) 0.016(2) Uani 1.00 1 d . . .
C(12) C 0.1269(7) 0.7107(6) -0.1708(6) 0.022(2) Uani 1.00 1 d . . .
C(13) C 0.0969(7) 0.7157(6) -0.0922(6) 0.025(2) Uani 1.00 1 d . . .
C(14) C 0.1572(7) 0.7636(7) -0.0663(6) 0.026(2) Uani 1.00 1 d . . .
C(15) C 0.2515(7) 0.8037(6) -0.1205(5) 0.018(2) Uani 1.00 1 d . . .
C(16) C 0.2839(6) 0.8010(6) -0.2009(5) 0.018(2) Uani 1.00 1 d . . .
C(17) C 0.1206(9) 0.7699(8) 0.0191(6) 0.035(3) Uani 1.00 1 d . . .
C(18) C 0.4632(6) 0.9937(6) -0.1913(5) 0.016(2) Uani 1.00 1 d . . .
C(19) C 0.3765(6) 1.0308(6) -0.1487(5) 0.018(2) Uani 1.00 1 d . . .
C(20) C 0.3582(7) 0.9938(5) -0.0590(5) 0.017(2) Uani 1.00 1 d . . .
C(21) C 0.4305(6) 0.9180(6) -0.0100(5) 0.019(2) Uani 1.00 1 d . . .
C(22) C 0.5175(6) 0.8830(6) -0.0542(6) 0.020(2) Uani 1.00 1 d . . .
C(23) C 0.5350(6) 0.9192(6) -0.1439(6) 0.020(2) Uani 1.00 1 d . . .
C(24) C 0.4092(7) 0.8770(7) 0.0874(6) 0.025(2) Uani 1.00 1 d . . .
C(25) C 0.8070(6) 0.7628(6) -0.0076(5) 0.021(2) Uani 1.00 1 d . . .
C(26) C 0.8315(7) 0.8485(6) -0.0788(6) 0.022(2) Uani 1.00 1 d . . .
C(27) C 0.8388(7) 0.8538(6) -0.1608(6) 0.024(2) Uani 1.00 1 d . . .
C(28) C 0.8221(7) 0.7783(6) -0.1758(6) 0.023(2) Uani 1.00 1 d . . .
C(29) C 0.7963(8) 0.6953(7) -0.1040(6) 0.029(3) Uani 1.00 1 d . . .
C(30) C 0.7886(7) 0.6865(7) -0.0207(6) 0.029(2) Uani 1.00 1 d . . .
C(31) C 0.8323(8) 0.7861(8) -0.2657(7) 0.035(3) Uani 1.00 1 d . . .
C(32) C 0.3305(7) 0.5883(6) 0.1083(6) 0.023(2) Uani 1.00 1 d . . .
C(33) C 0.4292(8) 0.6312(7) 0.0735(6) 0.029(2) Uani 1.00 1 d . . .
C(34) C 0.4798(9) 0.6428(7) -0.0104(7) 0.033(3) Uani 1.00 1 d . . .
C(35) C 0.4344(9) 0.6112(7) -0.0582(6) 0.035(3) Uani 1.00 1 d . . .
C(36) C 0.3336(8) 0.5684(7) -0.0216(6) 0.029(2) Uani 1.00 1 d . . .
C(37) C 0.2816(7) 0.5572(6) 0.0597(6) 0.025(2) Uani 1.00 1 d . . .
C(38) C 0.4899(9) 0.6230(9) -0.1460(7) 0.045(3) Uani 1.00 1 d . . .
H(1) H 0.1589 -0.0223 0.7942 0.030 Uiso 1.00 1 c R . .
H(2) H 0.0684 -0.0191 0.8692 0.030 Uiso 1.00 1 c R . .
H(3) H 0.1376 0.0669 0.8117 0.030 Uiso 1.00 1 c R . .
H(4) H 0.0701 -0.0347 0.6065 0.030 Uiso 1.00 1 c R . .
H(5) H 0.1030 -0.0893 0.6989 0.030 Uiso 1.00 1 c R . .
H(6) H 0.1668 -0.0036 0.6312 0.030 Uiso 1.00 1 c R . .
H(7) H -0.2073 0.1014 0.5724 0.034 Uiso 1.00 1 c R . .
H(8) H -0.1428 0.0032 0.5964 0.034 Uiso 1.00 1 c R . .
H(9) H -0.0874 0.0921 0.5260 0.034 Uiso 1.00 1 c R . .
H(10) H -0.2823 0.2013 0.7296 0.024 Uiso 1.00 1 c R . .
H(11) H -0.3128 0.1336 0.6961 0.024 Uiso 1.00 1 c R . .
H(12) H -0.2607 0.2266 0.6312 0.024 Uiso 1.00 1 c R . .
H(13) H -0.0497 0.1303 0.8646 0.031 Uiso 1.00 1 c R . .
H(14) H -0.1757 0.1291 0.8640 0.031 Uiso 1.00 1 c R . .
H(15) H -0.1142 0.2185 0.8027 0.031 Uiso 1.00 1 c R . .
H(16) H 0.0836 0.6789 -0.1878 0.028 Uiso 1.00 1 c R . .
H(17) H 0.0334 0.6857 -0.0546 0.031 Uiso 1.00 1 c R . .
H(18) H 0.2955 0.8341 -0.1026 0.025 Uiso 1.00 1 c R . .
H(19) H 0.3474 0.8313 -0.2383 0.022 Uiso 1.00 1 c R . .
H(20) H 0.0709 0.8244 0.0107 0.045 Uiso 1.00 1 c R . .
H(21) H 0.1840 0.7738 0.0408 0.045 Uiso 1.00 1 c R . .
H(22) H 0.0838 0.7156 0.0594 0.045 Uiso 1.00 1 c R . .
H(23) H 0.3290 1.0823 -0.1813 0.023 Uiso 1.00 1 c R . .
H(24) H 0.2975 1.0190 -0.0304 0.022 Uiso 1.00 1 c R . .
H(25) H 0.5667 0.8326 -0.0222 0.024 Uiso 1.00 1 c R . .
H(26) H 0.5951 0.8938 -0.1728 0.025 Uiso 1.00 1 c R . .
H(27) H 0.4479 0.9094 0.1070 0.031 Uiso 1.00 1 c R . .
H(28) H 0.4348 0.8123 0.1106 0.031 Uiso 1.00 1 c R . .
H(29) H 0.3315 0.8831 0.1064 0.031 Uiso 1.00 1 c R . .
H(30) H 0.8427 0.9015 -0.0705 0.027 Uiso 1.00 1 c R . .
H(31) H 0.8560 0.9115 -0.2091 0.030 Uiso 1.00 1 c R . .
H(32) H 0.7835 0.6428 -0.1124 0.038 Uiso 1.00 1 c R . .
H(33) H 0.7709 0.6287 0.0274 0.032 Uiso 1.00 1 c R . .
H(34) H 0.7616 0.8066 -0.2853 0.043 Uiso 1.00 1 c R . .
H(35) H 0.8567 0.7264 -0.2657 0.043 Uiso 1.00 1 c R . .
H(36) H 0.8847 0.8304 -0.3029 0.043 Uiso 1.00 1 c R . .
H(37) H 0.4627 0.6528 0.1056 0.035 Uiso 1.00 1 c R . .
H(38) H 0.5472 0.6733 -0.0346 0.038 Uiso 1.00 1 c R . .
H(39) H 0.3004 0.5465 -0.0537 0.035 Uiso 1.00 1 c R . .
H(40) H 0.2129 0.5286 0.0830 0.032 Uiso 1.00 1 c R . .
H(41) H 0.4635 0.6812 -0.1884 0.046 Uiso 1.00 1 c R . .
H(42) H 0.4738 0.5730 -0.1569 0.046 Uiso 1.00 1 c R . .
H(43) H 0.5683 0.6218 -0.1492 0.046 Uiso 1.00 1 c R . .