#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:02:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178546 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/53/4065378.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_4065378
loop_
_publ_author_name
'Arias-Ugarte, Renzo'
'Sharma, Hemant K.'
'Metta-Magaña, Alejandro J.'
'Pannell, Keith H.'
_publ_section_title
;
 Mo(CO)6-Catalyzed Reduction ofN,N-Dimethylthioformamide by Silanes,
 Germanes, and Stannanes (R3EH) To Produce Trimethylamine and Group 14
 Thioethers (R3E--S--ER3)
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6506
_journal_paper_doi               10.1021/om200753t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C8 H7 Mo N O5 S'
_chemical_formula_weight         325.15
_chemical_name_common            Pentacarbonyl-thioformamide-Molibdenum
_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'
_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                 109.022(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6872(15)
_cell_length_b                   12.8629(18)
_cell_length_c                   9.7035(14)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.56
_cell_volume                     1261.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2112
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.8715
_exptl_absorpt_correction_T_min  0.8172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.394
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.394
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0434
_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)+(0.1126P)²+0.2523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2131
_reflns_number_gt                1598
_reflns_number_total             2112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200753t_si_002.cif
_cod_data_source_block           306ra4sa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               4065378
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_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 0.25234(6) 0.12176(4) 0.44078(7) 0.0449(4) Uani 1 1 d .
S1 S 0.0714(2) 0.12453(12) 0.1876(3) 0.0549(6) Uani 1 1 d .
O1 O 0.4798(8) 0.1204(4) 0.7398(9) 0.098(3) Uani 1 1 d .
O2 O 0.0488(7) 0.1041(4) 0.6175(9) 0.085(2) Uani 1 1 d .
O3 O 0.2606(7) -0.1238(5) 0.4340(8) 0.092(3) Uani 1 1 d .
O4 O 0.4693(8) 0.1284(4) 0.2834(9) 0.101(3) Uani 1 1 d .
O5 O 0.2550(7) 0.3687(5) 0.4446(7) 0.091(3) Uani 1 1 d .
N1 N -0.1903(7) 0.1252(3) 0.0961(8) 0.0521(17) Uani 1 1 d .
C1 C 0.3970(11) 0.1209(5) 0.6285(13) 0.067(3) Uani 1 1 d .
C2 C 0.1199(10) 0.1128(5) 0.5538(10) 0.056(2) Uani 1 1 d .
C3 C 0.2562(7) -0.0371(6) 0.4353(8) 0.058(2) Uani 1 1 d .
C4 C 0.3895(10) 0.1262(5) 0.3359(11) 0.060(2) Uani 1 1 d .
C5 C 0.2510(6) 0.2813(7) 0.4425(7) 0.056(2) Uani 1 1 d .
C6 C -0.0799(8) 0.1228(4) 0.2018(9) 0.050(2) Uani 1 1 d .
H6 H -0.0851 0.1199 0.2955 0.060 Uiso 1 1 calc R
C7 C -0.1935(11) 0.1307(7) -0.0559(11) 0.082(3) Uani 1 1 d .
H7A H -0.1493 0.1928 -0.0701 0.123 Uiso 1 1 calc R
H7B H -0.2838 0.1319 -0.1191 0.123 Uiso 1 1 calc R
H7C H -0.1495 0.0710 -0.0780 0.123 Uiso 1 1 calc R
C8 C -0.3172(9) 0.1212(5) 0.1207(13) 0.074(3) Uani 1 1 d .
H8A H -0.3031 0.1178 0.2235 0.111 Uiso 1 1 calc R
H8B H -0.3652 0.0608 0.0740 0.111 Uiso 1 1 calc R
H8C H -0.3673 0.1825 0.0810 0.111 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0381(5) 0.0457(5) 0.0478(6) 0.0011(2) 0.0098(4) -0.0003(2)
S1 0.0434(12) 0.0690(13) 0.0504(14) 0.0011(8) 0.0125(11) -0.0006(8)
O1 0.071(5) 0.119(7) 0.072(6) -0.008(4) -0.018(5) 0.002(4)
O2 0.085(5) 0.095(4) 0.095(5) -0.013(3) 0.056(5) -0.030(3)
O3 0.105(7) 0.050(5) 0.116(8) -0.003(3) 0.029(6) 0.007(3)
O4 0.073(5) 0.130(7) 0.116(7) 0.034(4) 0.052(5) 0.025(3)
O5 0.136(9) 0.052(5) 0.098(7) 0.000(3) 0.054(7) -0.002(3)
N1 0.040(4) 0.051(4) 0.057(5) -0.007(3) 0.005(4) -0.003(2)
C1 0.061(6) 0.060(5) 0.070(7) -0.005(4) 0.010(6) -0.002(3)
C2 0.057(5) 0.050(4) 0.057(6) -0.005(3) 0.017(5) -0.009(3)
C3 0.057(5) 0.050(5) 0.065(6) -0.001(4) 0.017(4) 0.003(3)
C4 0.057(5) 0.061(5) 0.066(6) 0.010(3) 0.026(5) 0.011(3)
C5 0.059(5) 0.054(5) 0.054(5) 0.007(3) 0.019(4) 0.002(3)
C6 0.054(5) 0.050(4) 0.049(5) 0.001(3) 0.020(5) -0.005(3)
C7 0.064(7) 0.113(9) 0.056(7) -0.008(4) 0.001(6) 0.009(4)
C8 0.042(5) 0.091(7) 0.088(8) 0.002(4) 0.020(6) -0.001(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'
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
C1 Mo1 C4 89.2(4)
C1 Mo1 C3 90.1(3)
C4 Mo1 C3 89.5(3)
C1 Mo1 C2 88.6(4)
C4 Mo1 C2 177.3(3)
C3 Mo1 C2 88.9(3)
C1 Mo1 C5 90.2(2)
C4 Mo1 C5 89.1(2)
C3 Mo1 C5 178.5(3)
C2 Mo1 C5 92.5(3)
C1 Mo1 S1 177.0(3)
C4 Mo1 S1 87.8(3)
C3 Mo1 S1 90.2(2)
C2 Mo1 S1 94.3(3)
C5 Mo1 S1 89.36(18)
C6 S1 Mo1 111.5(3)
C6 N1 C8 122.1(7)
C6 N1 C7 121.2(8)
C8 N1 C7 116.8(8)
O1 C1 Mo1 178.6(10)
O2 C2 Mo1 177.4(7)
O3 C3 Mo1 178.7(7)
O4 C4 Mo1 177.1(9)
O5 C5 Mo1 177.6(6)
N1 C6 S1 126.6(7)
N1 C6 H6 116.7
S1 C6 H6 116.7
N1 C7 H7A 109.5
N1 C7 H7B 109.5
H7A C7 H7B 109.5
N1 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
N1 C8 H8A 109.5
N1 C8 H8B 109.5
H8A C8 H8B 109.5
N1 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 C1 1.968(12)
Mo1 C4 2.039(9)
Mo1 C3 2.044(8)
Mo1 C2 2.058(9)
Mo1 C5 2.052(9)
Mo1 S1 2.584(3)
S1 C6 1.667(8)
O1 C1 1.152(13)
O2 C2 1.129(11)
O3 C3 1.117(9)
O4 C4 1.128(11)
O5 C5 1.125(10)
N1 C6 1.287(11)
N1 C8 1.453(11)
N1 C7 1.466(12)
C6 H6 0.9300
C7 H7A 0.9600
C7 H7B 0.9600
C7 H7C 0.9600
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
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
C1 Mo1 S1 C6 -172(4)
C4 Mo1 S1 C6 -179.5(3)
C3 Mo1 S1 C6 91.0(3)
C2 Mo1 S1 C6 2.0(3)
C5 Mo1 S1 C6 -90.4(3)
C4 Mo1 C1 O1 178(100)
C3 Mo1 C1 O1 -93(23)
C2 Mo1 C1 O1 -4(23)
C5 Mo1 C1 O1 89(23)
S1 Mo1 C1 O1 170(20)
C1 Mo1 C2 O2 -68(18)
C4 Mo1 C2 O2 -32(22)
C3 Mo1 C2 O2 22(18)
C5 Mo1 C2 O2 -159(18)
S1 Mo1 C2 O2 112(18)
C1 Mo1 C3 O3 -21(31)
C4 Mo1 C3 O3 69(31)
C2 Mo1 C3 O3 -109(31)
C5 Mo1 C3 O3 82(34)
S1 Mo1 C3 O3 156(31)
C1 Mo1 C4 O4 2(12)
C3 Mo1 C4 O4 -88(12)
C2 Mo1 C4 O4 -34(16)
C5 Mo1 C4 O4 93(12)
S1 Mo1 C4 O4 -178(100)
C1 Mo1 C5 O5 48(15)
C4 Mo1 C5 O5 -41(15)
C3 Mo1 C5 O5 -55(22)
C2 Mo1 C5 O5 136(15)
S1 Mo1 C5 O5 -129(15)
C8 N1 C6 S1 178.7(4)
C7 N1 C6 S1 -0.5(8)
Mo1 S1 C6 N1 178.9(4)
