#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:32:37 +0100 (vie 25 de mar de 2016) $
#$Revision: 179795 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/91/7009124.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_7009124
loop_
_publ_author_name
'Davies, Sian C.'
'Hughes, David L.'
'Richards, Raymond L.'
'Sanders, J. Roger'
_publ_section_title
;
 Molybdenum and tungsten complexes of the N(CH2CH2S)33− (NS3)
 ligand with oxide, sulfide, diazenide, hydrazide and nitrosyl
 co-ligands
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              719
_journal_paper_doi               10.1039/a908777j
_journal_year                    2000
_chemical_formula_moiety         'C6 H12 Mo N2 O S3'
_chemical_formula_structural     '[Mo{N(CH2CH2S)3}(NO)]'
_chemical_formula_sum            'C6 H12 Mo N2 O S3'
_chemical_formula_weight         320.3
_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     'automated Patterson'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.410(9)
_cell_angle_beta                 101.230(10)
_cell_angle_gamma                96.569(10)
_cell_formula_units_Z            4
_cell_length_a                   10.5200(13)
_cell_length_b                   13.435(2)
_cell_length_c                   7.9567(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1095.3(2)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992) '
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; ω/θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6811
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        3.16
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.733
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       prisms
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.464
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment
;
 Coordinates were located in idealised positions and subsequently allowed to
 refine freely.  All isotropic thermal displacement parameters were allowed
 to refine freely.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_obs          0.0294
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+0.1104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0774
_refine_ls_wR_factor_obs         0.0708
_reflns_number_observed          5078
_reflns_number_total             6366
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908777j.txt
_cod_data_source_block           ray22
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.1104P] 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^)+(0.0346P)^2^+0.1104P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P-1  (no. 2)'
_cod_database_code               7009124
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.20839(2) 0.205287(15) 0.08789(3) 0.02643(6) Uani 1 d . .
S1 S -0.00611(6) 0.23360(5) 0.03807(10) 0.03606(14) Uani 1 d . .
C14 C 0.0076(3) 0.3695(2) 0.0669(4) 0.0358(6) Uani 1 d . .
H14A H 0.0004(28) 0.3962(22) -0.0477(40) 0.032(8) Uiso 1 d . .
H14B H -0.0695(28) 0.3806(21) 0.1105(38) 0.029(7) Uiso 1 d . .
C41 C 0.1309(3) 0.4094(2) 0.1922(4) 0.0319(5) Uani 1 d . .
H41A H 0.1442(27) 0.4879(21) 0.2048(37) 0.031(7) Uiso 1 d . .
H41B H 0.1262(32) 0.3879(26) 0.3093(48) 0.052(10) Uiso 1 d . .
S2 S 0.33306(7) 0.24127(6) -0.11729(10) 0.0419(2) Uani 1 d . .
C24 C 0.3831(3) 0.3752(3) -0.0772(4) 0.0438(7) Uani 1 d . .
H24A H 0.4716(31) 0.3862(23) -0.0100(41) 0.035(8) Uiso 1 d . .
H24B H 0.3939(33) 0.3970(27) -0.1783(49) 0.050(10) Uiso 1 d . .
C42 C 0.2837(3) 0.4250(2) -0.0035(4) 0.0384(6) Uani 1 d . .
H42A H 0.3132(30) 0.4957(25) 0.0346(42) 0.040(8) Uiso 1 d . .
H42B H 0.2028(32) 0.4274(24) -0.0917(43) 0.042(9) Uiso 1 d . .
S3 S 0.30797(7) 0.18944(5) 0.36980(9) 0.03692(15) Uani 1 d . .
C34 C 0.3432(3) 0.3208(2) 0.4437(3) 0.0351(5) Uani 1 d . .
H34A H 0.2674(28) 0.3321(22) 0.4987(38) 0.031(7) Uiso 1 d . .
H34B H 0.4222(31) 0.3220(24) 0.5223(43) 0.041(9) Uiso 1 d . .
C43 C 0.3603(3) 0.3900(2) 0.2985(4) 0.0357(6) Uani 1 d . .
H43A H 0.3686(26) 0.4622(21) 0.3391(36) 0.026(7) Uiso 1 d . .
H43B H 0.4448(30) 0.3787(23) 0.2625(41) 0.038(8) Uiso 1 d . .
N4 N 0.2494(2) 0.37159(15) 0.1484(3) 0.0268(4) Uani 1 d . .
N5 N 0.1761(2) 0.0751(2) 0.0305(3) 0.0370(5) Uani 1 d . .
O5 O 0.1554(3) -0.0105(2) -0.0168(3) 0.0625(7) Uani 1 d . .
Mo2 Mo 0.78802(2) 0.293524(15) 0.47728(3) 0.02717(6) Uani 1 d . .
S6 S 1.00362(6) 0.26887(5) 0.54238(10) 0.03777(15) Uani 1 d . .
C69 C 0.9931(3) 0.1337(2) 0.5647(4) 0.0371(6) Uani 1 d . .
H69A H 1.0042(32) 0.1043(25) 0.4608(45) 0.047(9) Uiso 1 d . .
H69B H 1.0763(29) 0.1226(23) 0.6532(41) 0.036(8) Uiso 1 d . .
C96 C 0.8702(3) 0.0922(2) 0.6234(4) 0.0324(5) Uani 1 d . .
H96A H 0.8569(28) 0.0134(23) 0.6182(39) 0.036(8) Uiso 1 d . .
H96B H 0.8765(33) 0.1181(26) 0.7453(48) 0.053(10) Uiso 1 d . .
S7 S 0.68420(7) 0.30945(5) 0.70485(9) 0.03682(15) Uani 1 d . .
C79 C 0.6515(3) 0.1779(2) 0.7591(4) 0.0357(6) Uani 1 d . .
H79A H 0.7257(32) 0.1672(25) 0.8530(44) 0.045(9) Uiso 1 d . .
H79B H 0.5795(34) 0.1709(26) 0.7922(47) 0.051(10) Uiso 1 d . .
C97 C 0.6394(3) 0.1074(2) 0.6062(4) 0.0338(5) Uani 1 d . .
H97A H 0.6376(39) 0.0349(32) 0.6404(55) 0.075(13) Uiso 1 d . .
H97B H 0.5557(28) 0.1139(21) 0.5248(38) 0.028(7) Uiso 1 d . .
S8 S 0.66693(7) 0.25430(6) 0.20641(9) 0.0416(2) Uani 1 d . .
C89 C 0.6208(3) 0.1196(2) 0.2176(4) 0.0420(6) Uani 1 d . .
H89A H 0.5242(36) 0.1089(27) 0.2353(46) 0.054(10) Uiso 1 d . .
H89B H 0.6144(38) 0.0899(30) 0.1069(54) 0.068(12) Uiso 1 d . .
C98 C 0.7197(3) 0.0719(2) 0.3467(4) 0.0382(6) Uani 1 d . .
H98A H 0.6860(35) 0.0030(29) 0.3635(49) 0.058(11) Uiso 1 d . .
H98B H 0.8038(29) 0.0710(22) 0.3007(39) 0.034(8) Uiso 1 d . .
N9 N 0.7509(2) 0.12728(15) 0.5164(3) 0.0263(4) Uani 1 d . .
N10 N 0.8170(3) 0.4234(2) 0.4350(3) 0.0400(5) Uani 1 d . .
O10 O 0.8363(3) 0.5083(2) 0.3970(3) 0.0681(8) Uani 1 d . .
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'
Mo Mo -1.6832 0.6857 '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'
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
N5 Mo1 N4 177.46(9) . . ?
N5 Mo1 S1 95.43(8) . . ?
N4 Mo1 S1 84.52(5) . . ?
N5 Mo1 S3 97.52(8) . . ?
N4 Mo1 S3 84.75(6) . . ?
S1 Mo1 S3 116.73(3) . . ?
N5 Mo1 S2 93.81(8) . . ?
N4 Mo1 S2 84.05(5) . . ?
S1 Mo1 S2 120.38(3) . . ?
S3 Mo1 S2 120.10(3) . . ?
C14 S1 Mo1 101.88(9) . . ?
C41 C14 S1 111.5(2) . . ?
C41 C14 H14A 114.7(17) . . ?
S1 C14 H14A 105.8(18) . . ?
C41 C14 H14B 111.3(17) . . ?
S1 C14 H14B 103.9(17) . . ?
H14A C14 H14B 108.9(24) . . ?
N4 C41 C14 111.9(2) . . ?
N4 C41 H41A 110.5(15) . . ?
C14 C41 H41A 113.0(15) . . ?
N4 C41 H41B 106.9(20) . . ?
C14 C41 H41B 110.7(20) . . ?
H41A C41 H41B 103.3(25) . . ?
C24 S2 Mo1 101.62(10) . . ?
C42 C24 S2 111.5(2) . . ?
C42 C24 H24A 114.8(19) . . ?
S2 C24 H24A 109.9(18) . . ?
C42 C24 H24B 114.1(23) . . ?
S2 C24 H24B 103.5(24) . . ?
H24A C24 H24B 102.2(28) . . ?
N4 C42 C24 111.7(2) . . ?
N4 C42 H42A 106.6(19) . . ?
C24 C42 H42A 113.6(18) . . ?
N4 C42 H42B 109.1(19) . . ?
C24 C42 H42B 110.4(19) . . ?
H42A C42 H42B 105.2(26) . . ?
C34 S3 Mo1 101.21(9) . . ?
C43 C34 S3 111.7(2) . . ?
C43 C34 H34A 114.1(17) . . ?
S3 C34 H34A 103.8(17) . . ?
C43 C34 H34B 110.1(20) . . ?
S3 C34 H34B 103.1(20) . . ?
H34A C34 H34B 113.4(26) . . ?
N4 C43 C34 112.2(2) . . ?
N4 C43 H43A 109.1(16) . . ?
C34 C43 H43A 110.3(16) . . ?
N4 C43 H43B 109.8(18) . . ?
C34 C43 H43B 107.8(18) . . ?
H43A C43 H43B 107.6(23) . . ?
C42 N4 C43 110.0(2) . . ?
C42 N4 C41 109.3(2) . . ?
C43 N4 C41 109.3(2) . . ?
C42 N4 Mo1 109.7(2) . . ?
C43 N4 Mo1 108.9(2) . . ?
C41 N4 Mo1 109.66(15) . . ?
O5 N5 Mo1 176.4(2) . . ?
N10 Mo2 N9 177.05(9) . . ?
N10 Mo2 S6 95.49(9) . . ?
N9 Mo2 S6 84.54(5) . . ?
N10 Mo2 S8 93.36(8) . . ?
N9 Mo2 S8 84.10(6) . . ?
S6 Mo2 S8 120.36(3) . . ?
N10 Mo2 S7 97.81(8) . . ?
N9 Mo2 S7 84.79(5) . . ?
S6 Mo2 S7 116.91(3) . . ?
S8 Mo2 S7 119.97(3) . . ?
C69 S6 Mo2 101.78(9) . . ?
C96 C69 S6 111.9(2) . . ?
C96 C69 H69A 114.3(21) . . ?
S6 C69 H69A 108.4(21) . . ?
C96 C69 H69B 112.0(17) . . ?
S6 C69 H69B 104.5(17) . . ?
H69A C69 H69B 105.0(26) . . ?
N9 C96 C69 112.0(2) . . ?
N9 C96 H96A 107.5(16) . . ?
C69 C96 H96A 111.9(16) . . ?
N9 C96 H96B 107.3(19) . . ?
C69 C96 H96B 107.8(20) . . ?
H96A C96 H96B 110.3(26) . . ?
C79 S7 Mo2 100.94(9) . . ?
C97 C79 S7 112.2(2) . . ?
C97 C79 H79A 112.8(19) . . ?
S7 C79 H79A 104.4(19) . . ?
C97 C79 H79B 107.8(25) . . ?
S7 C79 H79B 107.7(24) . . ?
H79A C79 H79B 111.9(31) . . ?
N9 C97 C79 112.3(2) . . ?
N9 C97 H97A 106.0(23) . . ?
C79 C97 H97A 112.0(24) . . ?
N9 C97 H97B 109.9(16) . . ?
C79 C97 H97B 109.1(17) . . ?
H97A C97 H97B 107.4(27) . . ?
C89 S8 Mo2 102.04(10) . . ?
C98 C89 S8 111.6(2) . . ?
C98 C89 H89A 116.3(20) . . ?
S8 C89 H89A 107.6(20) . . ?
C98 C89 H89B 109.7(24) . . ?
S8 C89 H89B 108.4(24) . . ?
H89A C89 H89B 102.7(30) . . ?
N9 C98 C89 112.0(2) . . ?
N9 C98 H98A 108.7(23) . . ?
C89 C98 H98A 109.7(22) . . ?
N9 C98 H98B 108.9(17) . . ?
C89 C98 H98B 109.4(17) . . ?
H98A C98 H98B 108.1(27) . . ?
C97 N9 C98 109.7(2) . . ?
C97 N9 C96 109.3(2) . . ?
C98 N9 C96 109.2(2) . . ?
C97 N9 Mo2 109.1(2) . . ?
C98 N9 Mo2 109.9(2) . . ?
C96 N9 Mo2 109.56(15) . . ?
O10 N10 Mo2 176.1(2) . . ?
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 N5 1.782(2) . ?
Mo1 N4 2.257(2) . ?
Mo1 S1 2.2900(7) . ?
Mo1 S3 2.3058(8) . ?
Mo1 S2 2.3063(8) . ?
S1 C14 1.824(3) . ?
C14 C41 1.514(4) . ?
C14 H14A 0.97(3) . ?
C14 H14B 0.97(3) . ?
C41 N4 1.498(3) . ?
C41 H41A 1.05(3) . ?
C41 H41B 0.99(4) . ?
S2 C24 1.824(3) . ?
C24 C42 1.510(4) . ?
C24 H24A 0.97(3) . ?
C24 H24B 0.88(4) . ?
C42 N4 1.493(3) . ?
C42 H42A 0.99(3) . ?
C42 H42B 1.00(3) . ?
S3 C34 1.830(3) . ?
C34 C43 1.514(4) . ?
C34 H34A 1.01(3) . ?
C34 H34B 0.94(3) . ?
C43 N4 1.495(3) . ?
C43 H43A 1.01(3) . ?
C43 H43B 1.01(3) . ?
N5 O5 1.191(3) . ?
Mo2 N10 1.782(2) . ?
Mo2 N9 2.257(2) . ?
Mo2 S6 2.2890(8) . ?
Mo2 S8 2.3036(8) . ?
Mo2 S7 2.3099(7) . ?
S6 C69 1.819(3) . ?
C69 C96 1.509(4) . ?
C69 H69A 0.95(4) . ?
C69 H69B 1.04(3) . ?
C96 N9 1.499(3) . ?
C96 H96A 1.05(3) . ?
C96 H96B 1.02(4) . ?
S7 C79 1.832(3) . ?
C79 C97 1.514(4) . ?
C79 H79A 0.99(3) . ?
C79 H79B 0.84(4) . ?
C97 N9 1.489(3) . ?
C97 H97A 1.01(4) . ?
C97 H97B 1.00(3) . ?
S8 C89 1.827(3) . ?
C89 C98 1.515(4) . ?
C89 H89A 1.05(4) . ?
C89 H89B 0.95(4) . ?
C98 N9 1.497(3) . ?
C98 H98A 0.97(4) . ?
C98 H98B 1.02(3) . ?
N10 O10 1.188(3) . ?
