#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:49:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179492 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/89/4338946.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_4338946
loop_
_publ_author_name
'Cotton, F. Albert'
'Li, Zhong'
'Liu, Chun Y.'
'Murillo, Carlos A.'
_publ_section_title
;
 Enhancement in electronic communication upon replacement of Mo-O by Mo-S
 bonds in tetranuclear clusters of the type [Mo2]2(mu-E-E)2 (E = O or S).
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9294
_journal_page_last               9302
_journal_paper_doi               10.1021/ic701303k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[Mo2(C15H15N2O2)2]2(C6H4S2)2,(CH2Cl2)'
_chemical_formula_sum            'C74 H72 Cl4 Mo4 N8 O8 S4'
_chemical_formula_weight         1855.20
_chemical_name_common            '[Mo2(DAniF)2]2(C6H4S2)2,(CH2Cl2)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                118.909(6)
_cell_angle_beta                 94.175(6)
_cell_angle_gamma                103.173(6)
_cell_formula_units_Z            1
_cell_length_a                   10.365(4)
_cell_length_b                   15.036(5)
_cell_length_c                   15.210(5)
_cell_measurement_reflns_used    1713
_cell_measurement_temperature    213(2)
_cell_volume                     1973.4(12)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'None (area detector data)'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.1434
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9624
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.7699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       niddle
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.754
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0730P)²+6.0825P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1943
_reflns_number_gt                2844
_reflns_number_total             5127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701303k.cif
_cod_data_source_block           xl
_cod_database_code               4338946
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Mo1 Mo -0.03554(11) 1.03734(9) -0.35055(9) 0.0280(4) Uani 1 1 d .
Mo2 Mo 0.12136(11) 1.14190(9) -0.36480(9) 0.0286(4) Uani 1 1 d .
S1 S -0.2234(3) 0.9818(3) -0.4993(3) 0.0312(9) Uani 1 1 d .
S2 S 0.0324(3) 1.1476(3) -0.5203(3) 0.0320(9) Uani 1 1 d .
N1 N -0.1075(10) 1.1624(9) -0.2505(9) 0.038(3) Uani 1 1 d .
N2 N 0.0558(10) 1.2743(8) -0.2695(8) 0.032(3) Uani 1 1 d .
N3 N 0.0931(11) 1.0435(8) -0.2326(8) 0.033(3) Uani 1 1 d .
N4 N 0.2592(10) 1.1591(9) -0.2454(8) 0.035(3) Uani 1 1 d .
O1 O -0.5267(10) 1.0705(9) -0.0684(9) 0.062(3) Uani 1 1 d .
O2 O 0.2817(11) 1.6576(8) -0.2555(10) 0.079(4) Uani 1 1 d .
O3 O -0.0537(11) 0.7463(9) -0.1074(9) 0.069(3) Uani 1 1 d .
O4 O 0.7746(9) 1.4567(8) -0.0992(7) 0.049(3) Uani 1 1 d .
C1 C -0.2406(8) 1.0929(6) -0.5087(6) 0.026(3) Uani 1 1 d G
C2 C -0.3665(7) 1.1106(7) -0.5052(7) 0.037(4) Uani 1 1 d G
H2A H -0.4390 1.0639 -0.5002 0.045 Uiso 1 1 calc R
C3 C -0.3853(7) 1.1973(7) -0.5091(7) 0.052(4) Uani 1 1 d G
H3A H -0.4705 1.2093 -0.5068 0.063 Uiso 1 1 calc R
C4 C -0.2781(10) 1.2664(6) -0.5166(8) 0.055(4) Uani 1 1 d G
H4A H -0.2908 1.3251 -0.5192 0.066 Uiso 1 1 calc R
C5 C -0.1522(8) 1.2488(6) -0.5200(7) 0.049(4) Uani 1 1 d G
H5A H -0.0797 1.2955 -0.5251 0.058 Uiso 1 1 calc R
C6 C -0.1334(7) 1.1620(7) -0.5161(7) 0.036(4) Uani 1 1 d G
C10 C -0.0510(13) 1.2589(11) -0.2313(9) 0.028(3) Uani 1 1 d .
H10A H -0.0856 1.3151 -0.1917 0.034 Uiso 1 1 calc R
C11 C -0.2142(7) 1.1447(7) -0.1992(6) 0.027(3) Uani 1 1 d G
C12 C -0.1987(7) 1.2052(6) -0.0932(6) 0.031(3) Uani 1 1 d G
H12A H -0.1187 1.2614 -0.0530 0.037 Uiso 1 1 calc R
C13 C -0.3015(9) 1.1825(7) -0.0466(5) 0.041(4) Uani 1 1 d G
H13A H -0.2910 1.2234 0.0251 0.049 Uiso 1 1 calc R
C14 C -0.4198(7) 1.0993(7) -0.1060(7) 0.037(4) Uani 1 1 d G
C15 C -0.4353(7) 1.0388(6) -0.2121(6) 0.043(4) Uani 1 1 d G
H15A H -0.5153 0.9825 -0.2523 0.051 Uiso 1 1 calc R
C16 C -0.3325(9) 1.0615(7) -0.2587(5) 0.050(4) Uani 1 1 d G
H16A H -0.3430 1.0206 -0.3304 0.060 Uiso 1 1 calc R
C17 C -0.5144(17) 1.1316(14) 0.0397(12) 0.072(6) Uani 1 1 d .
H17A H -0.5959 1.1044 0.0577 0.109 Uiso 1 1 calc R
H17B H -0.5025 1.2055 0.0606 0.109 Uiso 1 1 calc R
H17C H -0.4366 1.1266 0.0744 0.109 Uiso 1 1 calc R
C21 C 0.1147(8) 1.3770(6) -0.2604(7) 0.034(3) Uani 1 1 d G
C22 C 0.0375(7) 1.4433(7) -0.2547(8) 0.047(4) Uani 1 1 d G
H22A H -0.0543 1.4249 -0.2517 0.057 Uiso 1 1 calc R
C23 C 0.0960(9) 1.5368(7) -0.2536(8) 0.061(5) Uani 1 1 d G
H23A H 0.0438 1.5817 -0.2497 0.074 Uiso 1 1 calc R
C24 C 0.2318(10) 1.5641(6) -0.2581(8) 0.054(5) Uani 1 1 d G
C25 C 0.3091(7) 1.4978(7) -0.2637(8) 0.055(5) Uani 1 1 d G
H25A H 0.4009 1.5163 -0.2668 0.066 Uiso 1 1 calc R
C26 C 0.2505(8) 1.4043(7) -0.2649(8) 0.048(4) Uani 1 1 d G
H26A H 0.3028 1.3595 -0.2687 0.057 Uiso 1 1 calc R
C27 C 0.4043(18) 1.6732(13) -0.2901(14) 0.075(6) Uani 1 1 d .
H27A H 0.4279 1.7419 -0.2853 0.113 Uiso 1 1 calc R
H27B H 0.3919 1.6173 -0.3610 0.113 Uiso 1 1 calc R
H27C H 0.4766 1.6712 -0.2475 0.113 Uiso 1 1 calc R
C30 C 0.2192(13) 1.1017(11) -0.2028(10) 0.033(3) Uani 1 1 d .
H30A H 0.2797 1.1030 -0.1527 0.040 Uiso 1 1 calc R
C31 C 0.0559(9) 0.9687(6) -0.1974(7) 0.038(4) Uani 1 1 d G
C32 C -0.0636(9) 0.9593(7) -0.1621(8) 0.050(4) Uani 1 1 d G
H32A H -0.1178 1.0026 -0.1591 0.060 Uiso 1 1 calc R
C33 C -0.1028(8) 0.8858(8) -0.1312(8) 0.068(5) Uani 1 1 d G
H33A H -0.1836 0.8794 -0.1073 0.082 Uiso 1 1 calc R
C34 C -0.0227(9) 0.8217(7) -0.1357(8) 0.046(4) Uani 1 1 d G
C35 C 0.0967(9) 0.8311(7) -0.1710(8) 0.053(4) Uani 1 1 d G
H35A H 0.1509 0.7878 -0.1740 0.063 Uiso 1 1 calc R
C36 C 0.1360(7) 0.9046(7) -0.2019(7) 0.046(4) Uani 1 1 d G
H36A H 0.2168 0.9110 -0.2258 0.055 Uiso 1 1 calc R
C37 C -0.175(2) 0.7333(16) -0.0752(17) 0.107(8) Uani 1 1 d .
H37A H -0.1872 0.6781 -0.0580 0.161 Uiso 1 1 calc R
H37B H -0.2501 0.7130 -0.1300 0.161 Uiso 1 1 calc R
H37C H -0.1736 0.7998 -0.0151 0.161 Uiso 1 1 calc R
C41 C 0.3925(6) 1.2349(6) -0.2034(7) 0.035(4) Uani 1 1 d G
C42 C 0.4735(8) 1.2393(6) -0.2710(5) 0.043(4) Uani 1 1 d G
H42A H 0.4422 1.1914 -0.3421 0.052 Uiso 1 1 calc R
C43 C 0.6008(8) 1.3146(7) -0.2334(6) 0.038(4) Uani 1 1 d G
H43A H 0.6556 1.3175 -0.2791 0.045 Uiso 1 1 calc R
C44 C 0.6471(7) 1.3854(6) -0.1283(7) 0.032(3) Uani 1 1 d G
C45 C 0.5661(9) 1.3811(7) -0.0607(5) 0.040(4) Uani 1 1 d G
H45A H 0.5974 1.4290 0.0105 0.048 Uiso 1 1 calc R
C46 C 0.4388(8) 1.3058(7) -0.0982(6) 0.038(4) Uani 1 1 d G
H46A H 0.3840 1.3029 -0.0525 0.046 Uiso 1 1 calc R
C47 C 0.8268(15) 1.5210(12) 0.0076(12) 0.062(5) Uani 1 1 d .
H47A H 0.9161 1.5686 0.0209 0.093 Uiso 1 1 calc R
H47B H 0.8333 1.4762 0.0359 0.093 Uiso 1 1 calc R
H47C H 0.7668 1.5626 0.0395 0.093 Uiso 1 1 calc R
Cl2 Cl 0.7625(12) 1.5706(6) -0.3921(8) 0.247(6) Uani 1 1 d .
Cl1 Cl 0.6519(9) 1.7111(13) -0.4262(11) 0.287(8) Uani 1 1 d .
C1S C 0.786(3) 1.666(2) -0.419(2) 0.147(10) Uani 1 1 d .
H1SA H 0.8145 1.6405 -0.4845 0.177 Uiso 1 1 calc R
H1SB H 0.8612 1.7266 -0.3660 0.177 Uiso 1 1 calc R
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'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 '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
Mo2 Mo1 N3 91.7(3) . .
Mo2 Mo1 N1 92.2(3) . .
N3 Mo1 N1 95.1(4) . .
Mo2 Mo1 S2 105.82(9) . 2_574
N3 Mo1 S2 92.2(3) . 2_574
N1 Mo1 S2 160.3(3) . 2_574
Mo2 Mo1 S1 102.14(10) . .
N3 Mo1 S1 164.6(3) . .
N1 Mo1 S1 91.1(3) . .
S2 Mo1 S1 77.63(11) 2_574 .
Mo1 Mo2 N4 92.4(3) . .
Mo1 Mo2 N2 91.8(3) . .
N4 Mo2 N2 95.4(4) . .
Mo1 Mo2 S1 103.06(10) . 2_574
N4 Mo2 S1 92.3(3) . 2_574
N2 Mo2 S1 162.9(3) . 2_574
Mo1 Mo2 S2 106.70(9) . .
N4 Mo2 S2 160.0(3) . .
N2 Mo2 S2 90.1(3) . .
S1 Mo2 S2 77.79(12) 2_574 .
C1 S1 Mo2 115.7(3) . 2_574
C1 S1 Mo1 112.1(3) . .
Mo2 S1 Mo1 95.02(12) 2_574 .
C6 S2 Mo1 114.0(3) . 2_574
C6 S2 Mo2 109.3(3) . .
Mo1 S2 Mo2 95.13(12) 2_574 .
C10 N1 C11 119.2(10) . .
C10 N1 Mo1 119.3(9) . .
C11 N1 Mo1 121.4(7) . .
C10 N2 C21 120.2(11) . .
C10 N2 Mo2 119.0(9) . .
C21 N2 Mo2 120.1(7) . .
C30 N3 C31 116.8(11) . .
C30 N3 Mo1 119.6(9) . .
C31 N3 Mo1 122.4(8) . .
C30 N4 C41 118.3(11) . .
C30 N4 Mo2 118.6(9) . .
C41 N4 Mo2 123.0(8) . .
C14 O1 C17 116.5(11) . .
C24 O2 C27 117.7(11) . .
C34 O3 C37 116.5(11) . .
C44 O4 C47 115.1(10) . .
C2 C1 C6 120.0 . .
C2 C1 S1 117.2(5) . .
C6 C1 S1 122.8(5) . .
C1 C2 C3 120.0 . .
C2 C3 C4 120.0 . .
C5 C4 C3 120.0 . .
C4 C5 C6 120.0 . .
C5 C6 C1 120.0 . .
C5 C6 S2 116.2(5) . .
C1 C6 S2 123.8(5) . .
N1 C10 N2 117.5(12) . .
C12 C11 C16 120.0 . .
C12 C11 N1 121.9(7) . .
C16 C11 N1 118.1(7) . .
C11 C12 C13 120.0 . .
C14 C13 C12 120.0 . .
O1 C14 C13 124.8(8) . .
O1 C14 C15 115.2(8) . .
C13 C14 C15 120.0 . .
C14 C15 C16 120.0 . .
C15 C16 C11 120.0 . .
C22 C21 C26 120.0 . .
C22 C21 N2 122.1(7) . .
C26 C21 N2 117.7(7) . .
C21 C22 C23 120.0 . .
C24 C23 C22 120.0 . .
O2 C24 C25 123.7(8) . .
O2 C24 C23 116.3(8) . .
C25 C24 C23 120.0 . .
C24 C25 C26 120.0 . .
C25 C26 C21 120.0 . .
N3 C30 N4 117.6(13) . .
C32 C31 C36 120.0 . .
C32 C31 N3 119.3(7) . .
C36 C31 N3 120.7(7) . .
C31 C32 C33 120.0 . .
C34 C33 C32 120.0 . .
O3 C34 C33 124.2(7) . .
O3 C34 C35 115.8(7) . .
C33 C34 C35 120.0 . .
C36 C35 C34 120.0 . .
C35 C36 C31 120.0 . .
C42 C41 C46 120.0 . .
C42 C41 N4 118.4(7) . .
C46 C41 N4 121.5(7) . .
C43 C42 C41 120.0 . .
C42 C43 C44 120.0 . .
O4 C44 C45 124.7(7) . .
O4 C44 C43 115.3(7) . .
C45 C44 C43 120.0 . .
C44 C45 C46 120.0 . .
C45 C46 C41 120.0 . .
Cl2 C1S Cl1 117.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 Mo2 2.0926(16) .
Mo1 N3 2.107(11) .
Mo1 N1 2.109(11) .
Mo1 S2 2.522(4) 2_574
Mo1 S1 2.530(4) .
Mo2 N4 2.100(11) .
Mo2 N2 2.120(11) .
Mo2 S1 2.520(3) 2_574
Mo2 S2 2.523(4) .
S1 C1 1.791(7) .
S1 Mo2 2.520(3) 2_574
S2 C6 1.782(7) .
S2 Mo1 2.522(4) 2_574
N1 C10 1.309(15) .
N1 C11 1.447(11) .
N2 C10 1.313(15) .
N2 C21 1.460(11) .
N3 C30 1.299(15) .
N3 C31 1.454(12) .
N4 C30 1.325(16) .
N4 C41 1.438(12) .
O1 C14 1.362(11) .
O1 C17 1.421(17) .
O2 C24 1.362(11) .
O2 C27 1.425(17) .
O3 C34 1.378(11) .
O3 C37 1.393(17) .
O4 C44 1.379(10) .
O4 C47 1.408(16) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C2 C3 1.3900 .
C3 C4 1.3900 .
C4 C5 1.3900 .
C5 C6 1.3900 .
C11 C12 1.3900 .
C11 C16 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C14 C15 1.3900 .
C15 C16 1.3900 .
C21 C22 1.3900 .
C21 C26 1.3900 .
C22 C23 1.3900 .
C23 C24 1.3900 .
C24 C25 1.3900 .
C25 C26 1.3900 .
C31 C32 1.3900 .
C31 C36 1.3900 .
C32 C33 1.3900 .
C33 C34 1.3900 .
C34 C35 1.3900 .
C35 C36 1.3900 .
C41 C42 1.3900 .
C41 C46 1.3900 .
C42 C43 1.3900 .
C43 C44 1.3900 .
C44 C45 1.3900 .
C45 C46 1.3900 .
Cl2 C1S 1.64(2) .
Cl1 C1S 1.70(3) .
