#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:57:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179460 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/57/4335799.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_4335799
loop_
_publ_author_name
'Luke A. Wilkinson'
'Laura McNeill'
'Paul A. Scattergood'
'Nathan J. Patmore'
_publ_section_title
;
 Hydrogen Bonding and Electron Transfer between Dimetal Paddlewheel
 Compounds Containing Pendant 2-Pyridone Functional Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9683
_journal_page_last               9691
_journal_paper_doi               10.1021/ic401555g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C32 H20 Mo2 N8 O8, 4(C2 H6 O S)'
_chemical_formula_sum            'C40 H44 Mo2 N8 O12 S4'
_chemical_formula_weight         1148.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.240(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.2138(11)
_cell_length_b                   9.9307(7)
_cell_length_c                   15.6547(11)
_cell_measurement_reflns_used    896
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.552
_cell_measurement_theta_min      2.200
_cell_volume                     2270.8(3)
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(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  0.1632
_diffrn_reflns_av_sigmaI/netI    0.1596
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19305
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_correction_T_min  0.8954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       rod
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4024
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1659
_refine_ls_R_factor_gt           0.0629
_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)+(0.0613P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                1901
_reflns_number_total             4024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401555g_si_002_2.cif
_cod_data_source_block           Mo2(HDON)4(DMSO)2.2DMSO
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.54259(5) 0.03885(7) 0.96338(5) 0.0426(3) Uani 1 1 d . . .
N1 N 0.5536(4) 0.2329(6) 1.0313(4) 0.0438(17) Uani 1 1 d . . .
N2 N 0.6659(5) 0.3247(8) 0.9701(5) 0.074(2) Uani 1 1 d . . .
H1 H 0.6632 0.2490 0.9403 0.088 Uiso 1 1 calc R . .
N3 N 0.4223(5) 0.1098(6) 0.8587(4) 0.0429(17) Uani 1 1 d . . .
N4 N 0.5039(5) 0.2137(7) 0.7701(5) 0.060(2) Uani 1 1 d . . .
H4 H 0.5532 0.1769 0.8059 0.072 Uiso 1 1 calc R . .
O1 O 0.5424(4) -0.1432(5) 0.8958(3) 0.0492(15) Uani 1 1 d . . .
O2 O 0.7831(6) 0.3918(9) 0.9158(6) 0.113(3) Uani 1 1 d . . .
O3 O 0.6627(3) -0.0184(6) 1.0579(4) 0.0523(15) Uani 1 1 d . . .
O4 O 0.5949(5) 0.3132(8) 0.6960(5) 0.101(3) Uani 1 1 d . . .
O5 O 0.6577(4) 0.0850(6) 0.8771(4) 0.0662(18) Uani 1 1 d . . .
C1 C 0.5038(6) 0.2451(8) 1.0907(6) 0.050(2) Uani 1 1 d U . .
C2 C 0.5028(6) 0.3672(9) 1.1390(6) 0.056(2) Uani 1 1 d U . .
H2 H 0.4668 0.3738 1.1795 0.068 Uiso 1 1 calc R . .
C3 C 0.5525(7) 0.4704(11) 1.1267(6) 0.074(3) Uani 1 1 d U . .
H3 H 0.5498 0.5529 1.1566 0.089 Uiso 1 1 calc R . .
C4 C 0.6091(7) 0.4602(10) 1.0702(7) 0.070(3) Uani 1 1 d U . .
C5 C 0.6085(7) 0.3389(10) 1.0239(6) 0.057(2) Uani 1 1 d U . .
C6 C 0.6723(9) 0.5626(11) 1.0548(9) 0.105(4) Uani 1 1 d U . .
H6 H 0.6739 0.6475 1.0832 0.126 Uiso 1 1 calc R . .
C7 C 0.7292(8) 0.5431(14) 1.0018(10) 0.114(5) Uani 1 1 d U . .
H7 H 0.7690 0.6132 0.9946 0.137 Uiso 1 1 calc R . .
C8 C 0.7287(8) 0.4236(12) 0.9597(10) 0.094(4) Uani 1 1 d U . .
C9 C 0.3383(6) 0.0838(8) 0.8723(6) 0.052(2) Uani 1 1 d . . .
C10 C 0.2557(6) 0.1294(9) 0.8128(6) 0.061(3) Uani 1 1 d . . .
H10 H 0.1988 0.1034 0.8217 0.074 Uiso 1 1 calc R . .
C11 C 0.2570(7) 0.2075(10) 0.7453(7) 0.071(3) Uani 1 1 d . . .
H11 H 0.2015 0.2442 0.7089 0.085 Uiso 1 1 calc R . .
C12 C 0.3416(7) 0.2373(9) 0.7266(6) 0.060(3) Uani 1 1 d . . .
C13 C 0.4204(6) 0.1842(8) 0.7863(6) 0.052(2) Uani 1 1 d . . .
C14 C 0.3539(8) 0.3223(10) 0.6554(7) 0.075(3) Uani 1 1 d . . .
H14 H 0.3007 0.3571 0.6139 0.091 Uiso 1 1 calc R . .
C15 C 0.4372(8) 0.3553(11) 0.6443(6) 0.082(3) Uani 1 1 d . . .
H15 H 0.4418 0.4162 0.5989 0.098 Uiso 1 1 calc R . .
C16 C 0.5166(8) 0.2962(11) 0.7022(7) 0.079(3) Uani 1 1 d . . .
S1 S 0.7249(4) -0.0091(6) 0.8415(5) 0.062(2) Uani 0.589(12) 1 d PDU A 1
C17 C 0.7772(17) 0.097(2) 0.7781(14) 0.087(8) Uani 0.589(12) 1 d PDU A 1
H17A H 0.7362 0.1065 0.7178 0.131 Uiso 0.589(12) 1 calc PR A 1
H17B H 0.8351 0.0561 0.7751 0.131 Uiso 0.589(12) 1 calc PR A 1
H17C H 0.7893 0.1852 0.8065 0.131 Uiso 0.589(12) 1 calc PR A 1
C18 C 0.8238(11) 0.005(2) 0.9366(10) 0.098(8) Uani 0.589(12) 1 d PD A 1
H18A H 0.8119 -0.0416 0.9874 0.146 Uiso 0.589(12) 1 calc PR A 1
H18B H 0.8365 0.1003 0.9513 0.146 Uiso 0.589(12) 1 calc PR A 1
H18C H 0.8768 -0.0359 0.9227 0.146 Uiso 0.589(12) 1 calc PR A 1
S1A S 0.7555(6) 0.0463(11) 0.8885(8) 0.077(3) Uani 0.411(12) 1 d PDU A 2
C17A C 0.752(3) 0.052(4) 0.7730(15) 0.103(14) Uiso 0.411(12) 1 d PDU A 2
H17D H 0.7554 0.1460 0.7548 0.154 Uiso 0.411(12) 1 calc PR A 2
H17E H 0.6952 0.0113 0.7371 0.154 Uiso 0.411(12) 1 calc PR A 2
H17F H 0.8046 0.0022 0.7640 0.154 Uiso 0.411(12) 1 calc PR A 2
C18A C 0.7500(16) -0.1323(18) 0.8965(18) 0.084(9) Uani 0.411(12) 1 d PD A 2
H18D H 0.7523 -0.1574 0.9576 0.126 Uiso 0.411(12) 1 calc PR A 2
H18E H 0.8019 -0.1729 0.8804 0.126 Uiso 0.411(12) 1 calc PR A 2
H18F H 0.6926 -0.1648 0.8558 0.126 Uiso 0.411(12) 1 calc PR A 2
S2 S 0.0102(7) 0.2578(11) 0.8803(9) 0.113(4) Uani 0.585(13) 1 d PDU B 3
O6 O 0.1027(10) 0.1910(18) 0.8952(15) 0.150(6) Uani 0.585(13) 1 d PDU B 3
C19 C 0.026(3) 0.416(3) 0.829(3) 0.19(2) Uani 0.585(13) 1 d PDU B 3
H19A H 0.0145 0.4033 0.7653 0.284 Uiso 0.585(13) 1 calc PR B 3
H19B H 0.0883 0.4483 0.8553 0.284 Uiso 0.585(13) 1 calc PR B 3
H19C H -0.0178 0.4824 0.8403 0.284 Uiso 0.585(13) 1 calc PR B 3
C20 C 0.025(4) 0.346(4) 0.985(2) 0.168(18) Uani 0.585(13) 1 d PDU B 3
H20A H 0.0203 0.2815 1.0306 0.253 Uiso 0.585(13) 1 calc PR B 3
H20B H -0.0225 0.4147 0.9774 0.253 Uiso 0.585(13) 1 calc PR B 3
H20C H 0.0855 0.3886 1.0021 0.253 Uiso 0.585(13) 1 calc PR B 3
S2A S 0.0604(14) 0.279(2) 0.9021(17) 0.161(9) Uani 0.415(13) 1 d PDU B 4
O6A O 0.0044(15) 0.153(2) 0.8690(18) 0.151(6) Uani 0.415(13) 1 d PDU B 4
C19A C -0.017(3) 0.403(3) 0.837(2) 0.082(12) Uani 0.415(13) 1 d PDU B 4
H19D H -0.0061 0.4112 0.7783 0.123 Uiso 0.415(13) 1 calc PR B 4
H19E H -0.0057 0.4905 0.8674 0.123 Uiso 0.415(13) 1 calc PR B 4
H19F H -0.0801 0.3753 0.8301 0.123 Uiso 0.415(13) 1 calc PR B 4
C20A C 0.007(5) 0.290(6) 0.992(4) 0.17(2) Uani 0.415(13) 1 d PDU B 4
H20D H 0.0372 0.2275 1.0394 0.252 Uiso 0.415(13) 1 calc PR B 4
H20E H -0.0581 0.2657 0.9693 0.252 Uiso 0.415(13) 1 calc PR B 4
H20F H 0.0121 0.3819 1.0151 0.252 Uiso 0.415(13) 1 calc PR B 4
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'
Mo Mo -1.6832 0.6857 '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'
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
O3 Mo1 O1 90.0(2) . .
O3 Mo1 Mo1 93.69(17) . 3_657
O1 Mo1 Mo1 92.56(16) . 3_657
O3 Mo1 N1 87.8(2) . .
O1 Mo1 N1 175.1(2) . .
Mo1 Mo1 N1 91.92(19) 3_657 .
O3 Mo1 N3 175.4(2) . .
O1 Mo1 N3 91.0(2) . .
Mo1 Mo1 N3 90.7(2) 3_657 .
N1 Mo1 N3 90.8(2) . .
O3 Mo1 O5 80.1(2) . .
O1 Mo1 O5 77.9(2) . .
Mo1 Mo1 O5 168.54(14) 3_657 .
N1 Mo1 O5 97.4(2) . .
N3 Mo1 O5 95.7(2) . .
C1 N1 C5 117.3(8) . .
C1 N1 Mo1 115.5(5) . .
C5 N1 Mo1 127.1(6) . .
C5 N2 C8 124.3(10) . .
C13 N3 C9 115.5(7) . .
C13 N3 Mo1 128.3(6) . .
C9 N3 Mo1 116.0(6) . .
C13 N4 C16 126.0(8) . .
C1 O1 Mo1 121.4(5) 3_657 .
C9 O3 Mo1 121.9(5) 3_657 .
O1 C1 N1 118.6(7) 3_657 .
O1 C1 C2 119.6(9) 3_657 .
N1 C1 C2 121.8(8) . .
C3 C2 C1 119.4(10) . .
C2 C3 C4 121.0(10) . .
C3 C4 C5 118.2(10) . .
C3 C4 C6 127.0(11) . .
C5 C4 C6 114.9(11) . .
N1 C5 N2 118.6(9) . .
N1 C5 C4 122.1(10) . .
N2 C5 C4 119.2(10) . .
C7 C6 C4 123.8(12) . .
C8 C7 C6 119.9(13) . .
O2 C8 C7 124.8(13) . .
O2 C8 N2 117.4(11) . .
C7 C8 N2 117.7(13) . .
O3 C9 N3 117.6(7) 3_657 .
O3 C9 C10 120.4(9) 3_657 .
N3 C9 C10 122.1(9) . .
C11 C10 C9 120.5(10) . .
C10 C11 C12 120.3(10) . .
C13 C12 C11 115.9(9) . .
C13 C12 C14 117.5(9) . .
C11 C12 C14 126.5(9) . .
N3 C13 N4 117.5(8) . .
N3 C13 C12 125.5(9) . .
N4 C13 C12 116.9(9) . .
C15 C14 C12 124.1(9) . .
C14 C15 C16 118.2(10) . .
O4 C16 N4 118.8(10) . .
O4 C16 C15 124.1(10) . .
N4 C16 C15 117.1(10) . .
O5 S1 C17 106.3(9) . .
O5 S1 C18 97.7(7) . .
C17 S1 C18 90.8(11) . .
O5 S1A C18A 101.4(10) . .
O5 S1A C17A 97.2(17) . .
C18A S1A C17A 96.6(18) . .
O6 S2 C20 101(2) . .
O6 S2 C19 102.7(18) . .
C20 S2 C19 89(2) . .
O6A S2A C19A 98.9(19) . .
O6A S2A C20A 89(3) . .
C19A S2A C20A 92(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 2.084(5) .
Mo1 O1 2.095(5) .
Mo1 Mo1 2.1026(15) 3_657
Mo1 N1 2.184(7) .
Mo1 N3 2.203(6) .
Mo1 O5 2.535(6) .
N1 C1 1.360(10) .
N1 C5 1.369(10) .
N2 C5 1.380(11) .
N2 C8 1.410(12) .
N2 O5 2.775(10) .
N3 C13 1.347(10) .
N3 C9 1.377(10) .
N4 C13 1.394(10) .
N4 C16 1.398(11) .
N4 O5 2.778(9) .
O1 C1 1.283(9) 3_657
O2 C8 1.255(13) .
O3 C9 1.274(9) 3_657
O4 C16 1.235(11) .
O5 S1A 1.500(9) .
O5 S1 1.597(7) .
C1 O1 1.283(9) 3_657
C1 C2 1.431(11) .
C2 C3 1.319(12) .
C3 C4 1.401(13) .
C4 C5 1.404(12) .
C4 C6 1.466(15) .
C6 C7 1.370(16) .
C7 C8 1.357(16) .
C9 O3 1.274(9) 3_657
C9 C10 1.414(11) .
C10 C11 1.316(12) .
C11 C12 1.429(12) .
C12 C13 1.401(11) .
C12 C14 1.451(12) .
C14 C15 1.367(12) .
C15 C16 1.419(13) .
S1 C17 1.777(14) .
S1 C18 1.802(14) .
S1A C18A 1.781(16) .
S1A C17A 1.796(17) .
S2 O6 1.514(16) .
S2 C20 1.81(2) .
S2 C19 1.81(2) .
S2A O6A 1.520(19) .
S2A C19A 1.81(2) .
S2A C20A 1.81(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
N1 Mo1 Mo1 O1 1.9(2) 3_657 3_657
O3 Mo1 Mo1 N3 -1.2(2) 3_657 3_657
