#------------------------------------------------------------------------------
#$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/53/2005332.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005332
loop_
_publ_author_name
'Coffey, T. A.'
'Forster, G. D.'
'Hogarth, G.'
_publ_section_title
;Tris(<i>N</i>,<i>N</i>-diethyldithiocarbamato-<i>S</i>,<i>S</i>')(thionitrosyl-<i>N</i>)molybdenum(III),
 [Mo(\h^2^-S~2~CNEt~2~)~3~(NS)]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2157
_journal_page_last               2159
_journal_paper_doi               10.1107/S010827019600707X
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Mo (C5 H10 N1 S2)3 (N S)]'
_chemical_formula_sum            'C15 H30 Mo N4 S7'
_chemical_formula_weight         586.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.35(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.686(3)
_cell_length_b                   17.512(4)
_cell_length_c                   15.470(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     2607.9(13)
_computing_cell_refinement       'Nicolet R3 software'
_computing_data_collection       'Nicolet R3 software'
_computing_data_reduction        'XDISK (Siemens, 1991)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet R3m/V'
_diffrn_measurement_method       \w-2\q
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4869
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type
'empirical based on \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.41
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.979
_refine_ls_goodness_of_fit_obs   1.006
_refine_ls_hydrogen_treatment    'H atoms fixed'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.006
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_obs          0.0410
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0318P)^2^ + 5.4597P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1033
_refine_ls_wR_factor_obs         0.0858
_reflns_number_observed          3395
_reflns_number_total             4588
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    bm1082.cif
_[local]_cod_data_source_block   str426
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_cod_original_cell_volume        2608.0(12)
_cod_database_code               2005332
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mo(1) 0.0500(2) 0.0499(2) 0.0479(2) 0.0022(2) 0.0061(2) 0.0005(2)
S(1) 0.0675(7) 0.0544(7) 0.0532(6) -0.0133(6) 0.0098(5) 0.0080(5)
S(2) 0.0660(7) 0.0516(7) 0.0555(7) -0.0106(6) 0.0074(5) 0.0084(5)
S(3) 0.0541(7) 0.0669(8) 0.0601(7) 0.0048(6) 0.0132(5) 0.0058(6)
S(4) 0.0700(8) 0.0649(8) 0.0509(6) 0.0167(6) 0.0158(6) 0.0087(5)
S(5) 0.0620(8) 0.0861(10) 0.0681(8) 0.0132(7) 0.0204(6) 0.0136(7)
S(6) 0.0611(7) 0.0723(8) 0.0671(8) 0.0152(6) 0.0056(6) 0.0077(6)
S(7) 0.0720(8) 0.0547(7) 0.0725(8) 0.0004(6) 0.0061(6) -0.0081(6)
N(1) 0.058(2) 0.064(2) 0.045(2) -0.008(2) 0.006(2) 0.003(2)
N(2) 0.066(2) 0.074(3) 0.052(2) 0.019(2) 0.009(2) 0.001(2)
N(3) 0.050(2) 0.076(3) 0.094(3) 0.004(2) 0.014(2) -0.012(3)
N(4) 0.053(2) 0.051(2) 0.046(2) 0.008(2) 0.006(2) 0.001(2)
C(1) 0.051(2) 0.054(3) 0.049(2) -0.006(2) 0.007(2) 0.004(2)
C(2) 0.087(4) 0.077(4) 0.055(3) -0.020(3) 0.010(3) -0.004(3)
C(3) 0.134(6) 0.082(4) 0.103(5) 0.006(4) 0.043(4) -0.011(4)
C(4) 0.066(3) 0.080(3) 0.047(2) -0.010(3) 0.013(2) 0.012(2)
C(5) 0.071(4) 0.093(4) 0.084(4) -0.007(3) 0.006(3) 0.033(3)
C(6) 0.054(3) 0.060(3) 0.051(2) 0.008(2) 0.004(2) -0.005(2)
C(7) 0.074(4) 0.091(4) 0.078(4) 0.027(3) 0.016(3) 0.003(3)
C(8) 0.066(8) 0.116(12) 0.115(12) -0.003(8) 0.008(7) -0.026(10)
C(8A) 0.100(17) 0.13(3) 0.11(2) 0.04(2) 0.003(14) -0.016(19)
C(9) 0.084(4) 0.077(4) 0.051(3) 0.026(3) 0.004(3) 0.006(3)
C(10) 0.124(5) 0.064(4) 0.079(4) 0.021(4) 0.017(4) 0.001(3)
C(11) 0.057(3) 0.063(3) 0.071(3) 0.004(2) 0.001(2) -0.004(2)
C(12) 0.059(3) 0.070(4) 0.116(5) 0.007(3) 0.004(3) -0.019(3)
C(13) 0.095(5) 0.084(4) 0.120(5) 0.000(4) -0.008(4) -0.011(4)
C(14) 0.069(4) 0.108(5) 0.121(5) 0.015(4) 0.039(4) -0.001(4)
C(15) 0.150(7) 0.132(7) 0.104(5) 0.034(6) 0.040(5) 0.003(5)
loop_
_atom_site_label
_atom_site_occupancy
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Mo(1) 1 0.80339(4) 0.08735(2) 0.78350(2) 0.04920(13) Uani d . Mo
S(1) 1 0.69624(13) -0.01498(7) 0.67330(8) 0.0581(3) Uani d . S
S(2) 1 0.82794(13) 0.12681(7) 0.63188(8) 0.0576(3) Uani d . S
S(3) 1 1.03111(12) 0.02744(7) 0.75338(8) 0.0598(3) Uani d . S
S(4) 1 0.88101(13) -0.01402(7) 0.89206(7) 0.0612(3) Uani d . S
S(5) 1 0.62514(14) 0.07494(9) 0.88920(9) 0.0710(4) Uani d . S
S(6) 1 0.58578(13) 0.16167(8) 0.73554(8) 0.0670(3) Uani d . S
S(7) 1 0.96146(14) 0.24365(7) 0.86763(9) 0.0665(3) Uani d . S
N(1) 1 0.7292(4) 0.0278(2) 0.5100(2) 0.0554(9) Uani d . N
N(2) 1 1.1049(4) -0.0924(2) 0.8574(2) 0.0637(10) Uani d . N
N(3) 1 0.3874(4) 0.1504(3) 0.8441(3) 0.0730(12) Uani d . N
N(4) 1 0.8881(4) 0.1682(2) 0.8324(2) 0.0501(9) Uani d . N
C(1) 1 0.7468(4) 0.0430(3) 0.5943(3) 0.0514(10) Uani d . C
C(2) 1 0.6710(6) -0.0451(3) 0.4768(3) 0.0725(14) Uani d . C
H(2A) 1 0.6180(6) -0.0373(3) 0.4213(3) 0.080 Uiso d R H
H(2B) 1 0.6098(6) -0.0647(3) 0.5163(3) 0.080 Uiso d R H
C(3) 1 0.7823(8) -0.1024(4) 0.4668(4) 0.104(2) Uani d . C
H(3A) 1 0.7429(8) -0.1500(4) 0.4453(4) 0.080 Uiso d R H
H(3B) 1 0.8427(8) -0.0829(4) 0.4268(4) 0.080 Uiso d R H
H(3C) 1 0.8344(8) -0.1105(4) 0.5225(4) 0.080 Uiso d R H
C(4) 1 0.7700(5) 0.0827(3) 0.4456(3) 0.0639(13) Uani d . C
H(4A) 1 0.7955(5) 0.0555(3) 0.3958(3) 0.080 Uiso d R H
H(4B) 1 0.8495(5) 0.1109(3) 0.4704(3) 0.080 Uiso d R H
C(5) 1 0.6548(6) 0.1367(3) 0.4163(4) 0.083(2) Uani d . C
H(5A) 1 0.6838(6) 0.1720(3) 0.3744(4) 0.080 Uiso d R H
H(5B) 1 0.5758(6) 0.1084(3) 0.3907(4) 0.080 Uiso d R H
H(5C) 1 0.6303(6) 0.1643(3) 0.4660(4) 0.080 Uiso d R H
C(6) 1 1.0205(5) -0.0347(3) 0.8377(3) 0.0553(11) Uani d . C
C(7) 1 1.2142(6) -0.1127(4) 0.8029(4) 0.080(2) Uani d . C
H(7A) 1 1.1908(6) -0.0925(4) 0.7455(4) 0.080 Uiso d R H
H(7B) 1 1.2184(6) -0.1674(4) 0.7986(4) 0.080 Uiso d R H
C(8) 0.65 1.3437(16) -0.0741(8) 0.8287(11) 0.100(4) Uani d P C
H(8A) 0.65 1.4109(16) -0.0906(8) 0.7915(11) 0.080 Uiso d PR H
H(8B) 0.65 1.3129(16) -0.0235(8) 0.8125(11) 0.080 Uiso d PR H
H(8C) 0.65 1.3852(16) -0.0740(8) 0.8880(11) 0.080 Uiso d PR H
C(8A) 0.35 1.356(4) -0.1165(16) 0.851(2) 0.114(11) Uani d P C
H(8AD) 0.35 1.3986(35) -0.1515(16) 0.8938(23) 0.080 Uiso d PR H
H(8AA) 0.35 1.4120(35) -0.1118(16) 0.8043(23) 0.080 Uiso d PR H
H(8AB) 0.35 1.3462(35) -0.0675(16) 0.8776(23) 0.080 Uiso d PR H
C(9) 1 1.0784(6) -0.1468(3) 0.9256(3) 0.0712(14) Uani d . C
H(9A) 1 1.0427(6) -0.1202(3) 0.9727(3) 0.080 Uiso d R H
H(9B) 1 1.1641(6) -0.1709(3) 0.9479(3) 0.080 Uiso d R H
C(10) 1 0.9760(7) -0.2076(3) 0.8916(4) 0.089(2) Uani d . C
H(10A) 1 0.9600(7) -0.2429(3) 0.9369(4) 0.080 Uiso d R H
H(10B) 1 0.8901(7) -0.1834(3) 0.8700(4) 0.080 Uiso d R H
H(10C) 1 1.0125(7) -0.2345(3) 0.8450(4) 0.080 Uiso d R H
C(11) 1 0.5140(5) 0.1319(3) 0.8256(3) 0.0644(13) Uani d . C
C(12) 1 0.2970(6) 0.1991(3) 0.7830(4) 0.082(2) Uani d . C
H(12A) 1 0.2013(6) 0.1877(3) 0.7881(4) 0.080 Uiso d R H
H(12B) 1 0.3150(6) 0.1874(3) 0.7247(4) 0.080 Uiso d R H
C(13) 1 0.3225(7) 0.2819(4) 0.7992(5) 0.101(2) Uani d . C
H(13A) 1 0.2633(7) 0.3118(4) 0.7583(5) 0.080 Uiso d R H
H(13B) 1 0.3032(7) 0.2938(4) 0.8572(5) 0.080 Uiso d R H
H(13C) 1 0.4179(7) 0.2935(4) 0.7932(5) 0.080 Uiso d R H
C(14) 1 0.3356(6) 0.1246(4) 0.9248(4) 0.097(2) Uani d . C
H(14A) 1 0.3816(6) 0.0776(4) 0.9422(4) 0.080 Uiso d R H
H(14B) 1 0.2377(6) 0.1145(4) 0.9144(4) 0.080 Uiso d R H
C(15) 1 0.3617(9) 0.1800(5) 0.9965(5) 0.127(3) Uani d . C
H(15A) 1 0.3280(9) 0.1607(5) 1.0483(5) 0.080 Uiso d R H
H(15B) 1 0.4597(9) 0.1895(5) 1.0075(5) 0.080 Uiso d R H
H(15C) 1 0.3145(9) 0.2268(5) 0.9795(5) 0.080 Uiso d R H
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_publ_flag
N(4) Mo(1) S(2) 95.36(11) ?
N(4) Mo(1) S(4) 100.98(12) ?
S(2) Mo(1) S(4) 141.17(4) ?
N(4) Mo(1) S(5) 96.35(12) ?
S(2) Mo(1) S(5) 141.53(5) ?
S(4) Mo(1) S(5) 71.29(5) ?
N(4) Mo(1) S(6) 92.64(12) ?
S(2) Mo(1) S(6) 75.06(5) ?
S(4) Mo(1) S(6) 138.09(5) ?
S(5) Mo(1) S(6) 67.90(5) yes
N(4) Mo(1) S(3) 92.19(12) ?
S(2) Mo(1) S(3) 76.41(5) ?
S(4) Mo(1) S(3) 68.05(4) yes
S(5) Mo(1) S(3) 139.33(5) ?
S(6) Mo(1) S(3) 151.38(4) ?
N(4) Mo(1) S(1) 164.62(11) yes
S(2) Mo(1) S(1) 69.29(4) yes
S(4) Mo(1) S(1) 91.12(5) ?
S(5) Mo(1) S(1) 96.51(5) ?
S(6) Mo(1) S(1) 84.43(5) ?
S(3) Mo(1) S(1) 83.50(5) ?
C(1) S(1) Mo(1) 86.2(2) ?
C(1) S(2) Mo(1) 89.67(15) ?
C(6) S(3) Mo(1) 89.8(2) ?
C(6) S(4) Mo(1) 90.9(2) ?
C(11) S(5) Mo(1) 90.5(2) ?
C(11) S(6) Mo(1) 90.3(2) ?
C(1) N(1) C(2) 121.6(4) ?
C(1) N(1) C(4) 121.4(4) ?
C(2) N(1) C(4) 117.0(4) ?
C(6) N(2) C(9) 120.8(4) ?
C(6) N(2) C(7) 121.6(4) ?
C(9) N(2) C(7) 116.7(4) ?
C(11) N(3) C(14) 121.2(5) ?
C(11) N(3) C(12) 119.7(5) ?
C(14) N(3) C(12) 119.1(4) ?
S(7) N(4) Mo(1) 174.8(2) yes
N(1) C(1) S(1) 124.8(3) ?
N(1) C(1) S(2) 120.4(3) ?
S(1) C(1) S(2) 114.8(2) ?
N(1) C(2) C(3) 111.6(5) ?
N(1) C(4) C(5) 111.8(4) ?
N(2) C(6) S(4) 123.7(4) ?
N(2) C(6) S(3) 125.2(4) ?
S(4) C(6) S(3) 111.0(3) ?
C(8) C(7) N(2) 112.8(8) ?
C(8) C(7) C(8A) 32.6(12) ?
N(2) C(7) C(8A) 113.9(15) ?
C(8A) C(8) C(7) 77.(3) ?
C(8) C(8A) C(7) 71.(3) ?
N(2) C(9) C(10) 111.6(4) ?
N(3) C(11) S(5) 124.0(4) ?
N(3) C(11) S(6) 124.8(4) ?
S(5) C(11) S(6) 111.2(3) ?
N(3) C(12) C(13) 112.2(5) ?
N(3) C(14) C(15) 113.0(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mo(1) N(4) 1.765(4) yes
Mo(1) S(2) 2.4817(14) yes
Mo(1) S(4) 2.5016(13) yes
Mo(1) S(5) 2.5152(15) yes
Mo(1) S(6) 2.5182(14) yes
Mo(1) S(3) 2.5320(13) yes
Mo(1) S(1) 2.6083(14) yes
S(1) C(1) 1.703(4) ?
S(2) C(1) 1.734(5) ?
S(3) C(6) 1.710(5) ?
S(4) C(6) 1.707(5) ?
S(5) C(11) 1.700(5) ?
S(6) C(11) 1.706(5) ?
S(7) N(4) 1.568(4) yes
N(1) C(1) 1.324(5) ?
N(1) C(2) 1.465(6) ?
N(1) C(4) 1.469(5) ?
N(2) C(6) 1.314(6) ?
N(2) C(9) 1.467(6) ?
N(2) C(7) 1.468(6) ?
N(3) C(11) 1.330(6) ?
N(3) C(14) 1.466(7) ?
N(3) C(12) 1.486(7) ?
C(2) C(3) 1.494(8) ?
C(4) C(5) 1.495(7) ?
C(7) C(8) 1.44(2) ?
C(7) C(8A) 1.49(3) ?
C(8) C(8A) 0.82(3) ?
C(9) C(10) 1.509(8) ?
C(12) C(13) 1.487(8) ?
C(14) C(15) 1.475(9) ?