#------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/01/4300127.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_4300127
loop_
_publ_author_name
'Booyong S. Lim'
'James P. Donahue'
'R. H. Holm'
_publ_contact_author             R.H.Holm
_publ_contact_author_address
;
   R.H.Holm
   Dept. of Chemistry and Chemical Biology 
   Harvard University 
   Cambridge, MA 02138
   USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_section_title
;
Synthesis and Structures of Bis(dithiolene)molybdenum Complexes Related to
the Active Sites of the DMSO Reductase Enzyme Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              263
_journal_page_last               273
_journal_paper_doi               10.1021/ic9908672
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C31 H55 Mo N S5'
_chemical_formula_weight         698.00
_chemical_name_systematic
; 
 [Mo(SC6H2-2,4,6-Pri3)(S2C2Me2)2](Et4N)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.3419(2)
_cell_length_b                   15.3984(3)
_cell_length_c                   15.1147(2)
_cell_measurement_temperature    213(2)
_cell_volume                     7538.62(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15838
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.644
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       bar
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_obs          0.0316
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0767
_refine_ls_wR_factor_obs         0.0711
_reflns_number_observed          3606
_reflns_number_total             4942
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0350P)^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^)+(0.0350P)^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_original_cell_volume        7538.6(2)
_cod_database_code               4300127
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.180677(9) 0.24617(2) 0.66732(2) 0.03798(11) Uani 1 d . .
S1 S 0.15119(3) 0.37674(6) 0.60292(7) 0.0478(3) Uani 1 d . .
S2 S 0.15543(3) 0.28028(7) 0.78220(7) 0.0554(3) Uani 1 d . .
S3 S 0.23222(3) 0.27584(6) 0.61232(7) 0.0448(3) Uani 1 d . .
S4 S 0.23612(3) 0.18797(7) 0.79674(7) 0.0514(3) Uani 1 d . .
S5 S 0.13596(3) 0.14186(6) 0.56684(7) 0.0515(3) Uani 1 d . .
N1 N 0.27581(9) 0.4653(2) 0.9671(2) 0.0455(8) Uani 1 d . .
C1 C 0.12075(11) 0.4129(3) 0.6643(3) 0.0547(11) Uani 1 d . .
C2 C 0.12272(11) 0.3707(3) 0.7422(3) 0.0613(12) Uani 1 d . .
C5 C 0.09384(13) 0.4906(3) 0.6206(4) 0.086(2) Uani 1 d . .
H3A H 0.09799(13) 0.5093(3) 0.5645(4) 0.130 Uiso 1 calc R .
H3B H 0.10099(13) 0.5369(3) 0.6669(4) 0.130 Uiso 1 calc R .
H3C H 0.06539(13) 0.4751(3) 0.6023(4) 0.130 Uiso 1 calc R .
C6 C 0.09860(14) 0.3946(3) 0.8022(4) 0.096(2) Uani 1 d . .
H4A H 0.10516(14) 0.3545(3) 0.8550(4) 0.144 Uiso 1 calc R .
H4B H 0.06956(14) 0.3920(3) 0.7626(4) 0.144 Uiso 1 calc R .
H4C H 0.10582(14) 0.4524(3) 0.8271(4) 0.144 Uiso 1 calc R .
C3 C 0.27920(10) 0.2306(2) 0.6925(3) 0.0450(9) Uani 1 d . .
C4 C 0.28110(10) 0.1931(2) 0.7728(3) 0.0500(10) Uani 1 d . .
C7 C 0.31573(11) 0.2429(2) 0.6658(3) 0.0629(11) Uani 1 d . .
H7A H 0.30689(11) 0.2717(2) 0.6045(3) 0.094 Uiso 1 calc R .
H7B H 0.32726(11) 0.1874(2) 0.6619(3) 0.094 Uiso 1 calc R .
H7C H 0.33624(11) 0.2777(2) 0.7142(3) 0.094 Uiso 1 calc R .
C8 C 0.31945(11) 0.1542(3) 0.8505(3) 0.0795(14) Uani 1 d . .
H8A H 0.31262(11) 0.1310(3) 0.9012(3) 0.119 Uiso 1 calc R .
H8B H 0.34012(11) 0.1984(3) 0.8763(3) 0.119 Uiso 1 calc R .
H8C H 0.32987(11) 0.1086(3) 0.8232(3) 0.119 Uiso 1 calc R .
C9 C 0.08545(10) 0.1858(2) 0.5409(3) 0.0452(9) Uani 1 d . .
C10 C 0.06723(10) 0.2419(2) 0.4624(3) 0.0470(9) Uani 1 d . .
C11 C 0.02929(10) 0.2789(3) 0.4488(3) 0.0530(11) Uani 1 d . .
H11A H 0.01701(10) 0.3169(3) 0.3974(3) 0.064 Uiso 1 calc R .
C12 C 0.00935(11) 0.2615(3) 0.5084(3) 0.0602(11) Uani 1 d . .
C13 C 0.02716(11) 0.2023(3) 0.5828(3) 0.0619(12) Uani 1 d . .
H13A H 0.01350(11) 0.1888(3) 0.6223(3) 0.074 Uiso 1 calc R .
C14 C 0.06467(11) 0.1626(3) 0.6000(3) 0.0543(11) Uani 1 d . .
C15 C 0.08648(11) 0.2594(3) 0.3903(3) 0.0557(11) Uani 1 d . .
H15A H 0.11652(11) 0.2588(3) 0.4263(3) 0.067 Uiso 1 calc R .
C16 C 0.07510(13) 0.3472(3) 0.3388(3) 0.0838(15) Uani 1 d . .
H16A H 0.08844(13) 0.3530(3) 0.2949(3) 0.126 Uiso 1 calc R .
H16B H 0.08400(13) 0.3931(3) 0.3856(3) 0.126 Uiso 1 calc R .
H16C H 0.04572(13) 0.3504(3) 0.3036(3) 0.126 Uiso 1 calc R .
C17 C 0.07563(13) 0.1851(3) 0.3170(3) 0.093(2) Uani 1 d . .
H17A H 0.08777(13) 0.1960(3) 0.2715(3) 0.139 Uiso 1 calc R .
H17B H 0.04618(13) 0.1812(3) 0.2834(3) 0.139 Uiso 1 calc R .
H17C H 0.08614(13) 0.1314(3) 0.3500(3) 0.139 Uiso 1 calc R .
C18 C 0.08107(12) 0.0935(3) 0.6778(3) 0.0704(13) Uani 1 d . .
H18A H 0.11123(12) 0.0985(3) 0.7054(3) 0.084 Uiso 1 calc R .
C19 C 0.06765(13) 0.1039(4) 0.7610(3) 0.100(2) Uani 1 d . .
H19A H 0.07927(13) 0.0578(4) 0.8068(3) 0.150 Uiso 1 calc R .
H19B H 0.03807(13) 0.1015(4) 0.7368(3) 0.150 Uiso 1 calc R .
H19C H 0.07712(13) 0.1588(4) 0.7920(3) 0.150 Uiso 1 calc R .
C20 C 0.0707(2) 0.0035(3) 0.6318(4) 0.108(2) Uani 1 d . .
H20A H 0.0796(2) -0.0005(3) 0.5798(4) 0.162 Uiso 1 calc R .
H20B H 0.0414(2) -0.0057(3) 0.6075(4) 0.162 Uiso 1 calc R .
H20C H 0.0845(2) -0.0399(3) 0.6794(4) 0.162 Uiso 1 calc R .
C21 C -0.03044(12) 0.3086(3) 0.4957(3) 0.0743(14) Uani 1 d . .
H21A H -0.03882(12) 0.3431(3) 0.4364(3) 0.089 Uiso 1 calc R .
C22 C -0.06511(13) 0.2462(4) 0.4834(5) 0.125(2) Uani 1 d . .
H22A H -0.06895(13) 0.2077(4) 0.4306(5) 0.188 Uiso 1 calc R .
H22B H -0.09008(13) 0.2782(4) 0.4703(5) 0.188 Uiso 1 calc R .
H22C H -0.05835(13) 0.2131(4) 0.5415(5) 0.188 Uiso 1 calc R .
C23 C -0.02303(14) 0.3710(4) 0.5784(4) 0.108(2) Uani 1 d . .
H23A H -0.00084(14) 0.4096(4) 0.5841(4) 0.162 Uiso 1 calc R .
H23B H -0.01591(14) 0.3389(4) 0.6373(4) 0.162 Uiso 1 calc R .
H23C H -0.04765(14) 0.4041(4) 0.5661(4) 0.162 Uiso 1 calc R .
C24 C 0.29923(12) 0.3817(3) 0.9798(3) 0.0673(12) Uani 1 d . .
H24A H 0.28230(12) 0.3409(3) 0.9312(3) 0.081 Uiso 1 calc R .
H24B H 0.30360(12) 0.3576(3) 1.0425(3) 0.081 Uiso 1 calc R .
C25 C 0.34101(14) 0.3893(3) 0.9727(4) 0.108(2) Uani 1 d . .
H25A H 0.35376(14) 0.3331(3) 0.9816(4) 0.162 Uiso 1 calc R .
H25B H 0.35844(14) 0.4282(3) 1.0217(4) 0.162 Uiso 1 calc R .
H25C H 0.33709(14) 0.4114(3) 0.9103(4) 0.162 Uiso 1 calc R .
C26 C 0.23529(11) 0.4422(3) 0.9725(3) 0.0594(11) Uani 1 d . .
H26A H 0.24095(11) 0.4203(3) 1.0367(3) 0.071 Uiso 1 calc R .
H26B H 0.22268(11) 0.3955(3) 0.9272(3) 0.071 Uiso 1 calc R .
C27 C 0.20436(13) 0.5157(3) 0.9511(4) 0.089(2) Uani 1 d . .
H27A H 0.17972(13) 0.4948(3) 0.9563(4) 0.134 Uiso 1 calc R .
H27B H 0.19773(13) 0.5369(3) 0.8869(4) 0.134 Uiso 1 calc R .
H27C H 0.21604(13) 0.5618(3) 0.9967(4) 0.134 Uiso 1 calc R .
C28 C 0.29979(12) 0.5314(2) 1.0447(2) 0.0551(11) Uani 1 d . .
H28A H 0.32357(12) 0.5502(2) 1.0330(2) 0.066 Uiso 1 calc R .
H28B H 0.28232(12) 0.5818(2) 1.0374(2) 0.066 Uiso 1 calc R .
C29 C 0.31459(13) 0.5007(3) 1.1472(3) 0.0791(14) Uani 1 d . .
H29A H 0.32918(13) 0.5468(3) 1.1900(3) 0.119 Uiso 1 calc R .
H29B H 0.33272(13) 0.4519(3) 1.1564(3) 0.119 Uiso 1 calc R .
H29C H 0.29136(13) 0.4836(3) 1.1608(3) 0.119 Uiso 1 calc R .
C30 C 0.26924(12) 0.5084(2) 0.8719(2) 0.0537(10) Uani 1 d . .
H30A H 0.25528(12) 0.5634(2) 0.8681(2) 0.064 Uiso 1 calc R .
H30B H 0.29597(12) 0.5207(2) 0.8709(2) 0.064 Uiso 1 calc R .
C31 C 0.24458(13) 0.4553(3) 0.7848(3) 0.0744(13) Uani 1 d . .
H31A H 0.24169(13) 0.4866(3) 0.7275(3) 0.112 Uiso 1 calc R .
H31B H 0.21776(13) 0.4439(3) 0.7842(3) 0.112 Uiso 1 calc R .
H31C H 0.25850(13) 0.4013(3) 0.7870(3) 0.112 Uiso 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'
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'
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
S1 Mo1 S2 82.71(4) . . ?
S1 Mo1 S4 141.42(4) . . ?
S2 Mo1 S4 84.49(4) . . ?
S1 Mo1 S3 87.94(3) . . ?
S2 Mo1 S3 144.73(4) . . ?
S4 Mo1 S3 81.93(3) . . ?
S1 Mo1 S5 104.61(4) . . ?
S2 Mo1 S5 106.32(4) . . ?
S4 Mo1 S5 113.90(4) . . ?
S3 Mo1 S5 108.95(4) . . ?
C1 S1 Mo1 108.75(14) . . ?
C2 S2 Mo1 108.74(15) . . ?
C3 S3 Mo1 109.48(13) . . ?
C4 S4 Mo1 109.56(13) . . ?
C9 S5 Mo1 103.71(12) . . ?
C24 N1 C26 106.2(3) . . ?
C24 N1 C30 111.4(3) . . ?
C26 N1 C30 111.4(3) . . ?
C24 N1 C28 111.4(3) . . ?
C26 N1 C28 111.3(3) . . ?
C30 N1 C28 105.3(3) . . ?
C2 C1 C5 125.5(4) . . ?
C2 C1 S1 119.1(3) . . ?
C5 C1 S1 115.4(3) . . ?
C1 C2 C6 124.8(4) . . ?
C1 C2 S2 119.3(3) . . ?
C6 C2 S2 115.9(4) . . ?
C4 C3 C7 124.4(3) . . ?
C4 C3 S3 119.5(3) . . ?
C7 C3 S3 116.0(3) . . ?
C3 C4 C8 125.8(3) . . ?
C3 C4 S4 119.2(3) . . ?
C8 C4 S4 114.9(3) . . ?
C10 C9 C14 120.9(3) . . ?
C10 C9 S5 119.8(3) . . ?
C14 C9 S5 119.4(3) . . ?
C11 C10 C9 117.9(3) . . ?
C11 C10 C15 120.0(3) . . ?
C9 C10 C15 122.0(3) . . ?
C12 C11 C10 122.6(3) . . ?
C11 C12 C13 118.3(3) . . ?
C11 C12 C21 120.9(4) . . ?
C13 C12 C21 120.7(4) . . ?
C14 C13 C12 122.1(4) . . ?
C13 C14 C9 118.1(3) . . ?
C13 C14 C18 119.6(4) . . ?
C9 C14 C18 122.2(3) . . ?
C10 C15 C16 114.8(3) . . ?
C10 C15 C17 109.4(3) . . ?
C16 C15 C17 110.6(4) . . ?
C19 C18 C14 114.8(4) . . ?
C19 C18 C20 112.0(4) . . ?
C14 C18 C20 109.6(4) . . ?
C22 C21 C23 111.7(4) . . ?
C22 C21 C12 112.1(4) . . ?
C23 C21 C12 110.6(4) . . ?
N1 C24 C25 115.1(3) . . ?
N1 C26 C27 115.6(3) . . ?
C29 C28 N1 116.1(3) . . ?
C31 C30 N1 114.2(3) . . ?
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
Mo1 S1 2.2944(10) . ?
Mo1 S2 2.3078(10) . ?
Mo1 S4 2.3243(9) . ?
Mo1 S3 2.3301(9) . ?
Mo1 S5 2.3375(10) . ?
S1 C1 1.769(4) . ?
S2 C2 1.755(4) . ?
S3 C3 1.761(4) . ?
S4 C4 1.768(4) . ?
S5 C9 1.799(3) . ?
N1 C24 1.500(4) . ?
N1 C26 1.509(4) . ?
N1 C30 1.516(4) . ?
N1 C28 1.528(4) . ?
C1 C2 1.322(5) . ?
C1 C5 1.507(5) . ?
C2 C6 1.518(5) . ?
C3 C4 1.321(5) . ?
C3 C7 1.510(5) . ?
C4 C8 1.517(5) . ?
C9 C10 1.399(5) . ?
C9 C14 1.410(5) . ?
C10 C11 1.394(5) . ?
C10 C15 1.522(5) . ?
C11 C12 1.374(5) . ?
C12 C13 1.387(5) . ?
C12 C21 1.525(5) . ?
C13 C14 1.387(5) . ?
C14 C18 1.519(5) . ?
C15 C16 1.531(5) . ?
C15 C17 1.532(5) . ?
C18 C19 1.519(5) . ?
C18 C20 1.529(6) . ?
C21 C22 1.508(6) . ?
C21 C23 1.514(6) . ?
C24 C25 1.527(6) . ?
C26 C27 1.515(5) . ?
C28 C29 1.500(5) . ?
C30 C31 1.498(5) . ?
