#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313655.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_4313655
loop_
_publ_author_name
'Richard D. Adams'
'Burjor Captain'
'O-Sung Kwon'
'Shaobin Miao'
_publ_section_title
;
 New Disulfido Molybdenum-Manganese Complexes Exhibit Facile Addition of
 Small Molecules to the Sulfur Atoms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3356
_journal_page_last               3365
_journal_paper_doi               10.1021/ic030034i
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C15 H14 Mn Mo N O5 S2'
_chemical_formula_weight         503.27
_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                 105.0420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4347(5)
_cell_length_b                   19.5193(10)
_cell_length_c                   10.6607(5)
_cell_measurement_reflns_used    3976
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.24
_cell_volume                     1895.99(17)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14467
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0385P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                3854
_reflns_number_total             4713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030034i_06.cif
_cod_data_source_block           sbmomncs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313655
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 0.16998(2) 0.151468(10) 0.007177(17) 0.03668(7) Uani 1 1 d . . .
Mn1 Mn 0.44646(4) 0.18006(2) -0.02032(3) 0.04303(10) Uani 1 1 d . . .
S1 S 0.36484(7) 0.21784(3) 0.15585(5) 0.04029(14) Uani 1 1 d . . .
S2 S 0.24559(7) 0.25136(3) -0.10230(5) 0.03895(14) Uani 1 1 d . . .
O10 O 0.6617(2) 0.07772(13) 0.1135(2) 0.0794(7) Uani 1 1 d . . .
O11 O 0.4795(3) 0.12750(14) -0.2695(2) 0.0968(8) Uani 1 1 d . . .
O12 O 0.6667(2) 0.28744(14) -0.0059(3) 0.1007(9) Uani 1 1 d . . .
O20 O 0.3498(2) 0.02104(10) 0.1232(2) 0.0713(6) Uani 1 1 d . . .
O21 O 0.1611(3) 0.07705(12) -0.2559(2) 0.0833(7) Uani 1 1 d . . .
N1 N 0.2996(2) 0.35149(9) 0.09798(17) 0.0397(4) Uani 1 1 d . . .
C1 C -0.0450(3) 0.21275(16) 0.0041(3) 0.0625(8) Uani 1 1 d . . .
H1 H -0.0606 0.2573 -0.0274 0.075 Uiso 1 1 calc R . .
C2 C 0.0172(3) 0.19509(19) 0.1306(3) 0.0714(9) Uani 1 1 d . . .
H2 H 0.0505 0.2254 0.1991 0.086 Uiso 1 1 calc R . .
C3 C 0.0223(4) 0.1234(2) 0.1391(3) 0.0814(11) Uani 1 1 d . . .
H3 H 0.0606 0.0976 0.2135 0.098 Uiso 1 1 calc R . .
C4 C -0.0420(3) 0.09811(16) 0.0131(4) 0.0750(9) Uani 1 1 d . . .
H4 H -0.0560 0.0523 -0.0107 0.090 Uiso 1 1 calc R . .
C5 C -0.0806(3) 0.15443(17) -0.0690(3) 0.0624(8) Uani 1 1 d . . .
H5 H -0.1233 0.1528 -0.1580 0.075 Uiso 1 1 calc R . .
C6 C 0.2982(2) 0.29226(11) 0.0571(2) 0.0364(5) Uani 1 1 d . . .
C10 C 0.5776(3) 0.11772(15) 0.0632(3) 0.0539(7) Uani 1 1 d . . .
C11 C 0.4652(3) 0.14803(15) -0.1741(3) 0.0607(7) Uani 1 1 d . . .
C12 C 0.5829(3) 0.24457(16) -0.0108(3) 0.0635(8) Uani 1 1 d . . .
C20 C 0.2921(3) 0.07023(13) 0.0804(3) 0.0499(6) Uani 1 1 d . . .
C21 C 0.1698(3) 0.10493(14) -0.1609(3) 0.0539(7) Uani 1 1 d . . .
C50 C 0.2556(3) 0.41270(12) 0.0138(2) 0.0453(6) Uani 1 1 d . . .
C51 C 0.3604(3) 0.42050(14) -0.0724(3) 0.0587(7) Uani 1 1 d . . .
H51A H 0.4594 0.4230 -0.0193 0.088 Uiso 1 1 calc R . .
H51B H 0.3372 0.4617 -0.1229 0.088 Uiso 1 1 calc R . .
H51C H 0.3506 0.3818 -0.1295 0.088 Uiso 1 1 calc R . .
C52 C 0.2727(4) 0.47379(14) 0.1064(3) 0.0683(9) Uani 1 1 d . . .
H52A H 0.2084 0.4682 0.1622 0.103 Uiso 1 1 calc R . .
H52B H 0.2480 0.5152 0.0570 0.103 Uiso 1 1 calc R . .
H52C H 0.3724 0.4763 0.1580 0.103 Uiso 1 1 calc R . .
C53 C 0.0959(3) 0.40681(14) -0.0659(3) 0.0587(7) Uani 1 1 d . . .
H53A H 0.0867 0.3694 -0.1259 0.088 Uiso 1 1 calc R . .
H53B H 0.0668 0.4486 -0.1131 0.088 Uiso 1 1 calc R . .
H53C H 0.0339 0.3988 -0.0088 0.088 Uiso 1 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'
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'
Mn Mn 0.3368 0.7283 '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
C20 Mo1 C21 81.73(11) . . ?
C20 Mo1 C4 92.75(12) . . ?
C21 Mo1 C4 91.18(13) . . ?
C20 Mo1 C3 87.22(12) . . ?
C21 Mo1 C3 125.50(14) . . ?
C4 Mo1 C3 36.10(13) . . ?
C20 Mo1 C5 126.59(11) . . ?
C21 Mo1 C5 86.19(11) . . ?
C4 Mo1 C5 35.56(12) . . ?
C3 Mo1 C5 59.16(11) . . ?
C20 Mo1 C1 145.01(11) . . ?
C21 Mo1 C1 114.67(11) . . ?
C4 Mo1 C1 58.00(11) . . ?
C3 Mo1 C1 57.92(11) . . ?
C5 Mo1 C1 34.35(11) . . ?
C20 Mo1 C2 116.42(12) . . ?
C21 Mo1 C2 143.62(11) . . ?
C4 Mo1 C2 58.52(12) . . ?
C3 Mo1 C2 35.16(12) . . ?
C5 Mo1 C2 57.51(11) . . ?
C1 Mo1 C2 33.86(11) . . ?
C20 Mo1 S1 84.69(8) . . ?
C21 Mo1 S1 129.79(8) . . ?
C4 Mo1 S1 137.71(10) . . ?
C3 Mo1 S1 101.67(11) . . ?
C5 Mo1 S1 138.08(8) . . ?
C1 Mo1 S1 103.83(8) . . ?
C2 Mo1 S1 85.00(8) . . ?
C20 Mo1 S2 127.11(8) . . ?
C21 Mo1 S2 82.46(8) . . ?
C4 Mo1 S2 137.70(10) . . ?
C3 Mo1 S2 140.86(11) . . ?
C5 Mo1 S2 102.15(8) . . ?
C1 Mo1 S2 86.88(8) . . ?
C2 Mo1 S2 105.83(9) . . ?
S1 Mo1 S2 68.274(19) . . ?
C20 Mo1 Mn1 74.70(8) . . ?
C21 Mo1 Mn1 77.19(8) . . ?
C4 Mo1 Mn1 163.86(8) . . ?
C3 Mo1 Mn1 149.06(9) . . ?
C5 Mo1 Mn1 151.00(8) . . ?
C1 Mo1 Mn1 137.17(8) . . ?
C2 Mo1 Mn1 136.16(8) . . ?
S1 Mo1 Mn1 52.600(17) . . ?
S2 Mo1 Mn1 52.614(16) . . ?
C12 Mn1 C10 93.21(13) . . ?
C12 Mn1 C11 93.24(14) . . ?
C10 Mn1 C11 89.90(12) . . ?
C12 Mn1 S1 96.63(10) . . ?
C10 Mn1 S1 98.29(8) . . ?
C11 Mn1 S1 166.77(10) . . ?
C12 Mn1 S2 95.98(9) . . ?
C10 Mn1 S2 167.93(9) . . ?
C11 Mn1 S2 97.35(9) . . ?
S1 Mn1 S2 72.91(2) . . ?
C12 Mn1 Mo1 145.62(9) . . ?
C10 Mn1 Mo1 111.03(9) . . ?
C11 Mn1 Mo1 110.18(10) . . ?
S1 Mn1 Mo1 57.167(17) . . ?
S2 Mn1 Mo1 57.383(17) . . ?
C6 S1 Mn1 85.57(7) . . ?
C6 S1 Mo1 87.67(7) . . ?
Mn1 S1 Mo1 70.233(19) . . ?
C6 S2 Mn1 85.06(7) . . ?
C6 S2 Mo1 86.99(7) . . ?
Mn1 S2 Mo1 70.003(19) . . ?
C6 N1 C50 124.34(19) . . ?
C2 C1 C5 109.3(3) . . ?
C2 C1 Mo1 73.12(17) . . ?
C5 C1 Mo1 70.65(17) . . ?
C1 C2 C3 108.3(3) . . ?
C1 C2 Mo1 73.02(16) . . ?
C3 C2 Mo1 70.08(17) . . ?
C2 C3 C4 106.7(3) . . ?
C2 C3 Mo1 74.77(17) . . ?
C4 C3 Mo1 71.25(17) . . ?
C5 C4 C3 107.4(3) . . ?
C5 C4 Mo1 73.11(17) . . ?
C3 C4 Mo1 72.66(18) . . ?
C1 C5 C4 108.2(3) . . ?
C1 C5 Mo1 75.01(17) . . ?
C4 C5 Mo1 71.34(17) . . ?
N1 C6 S1 125.23(17) . . ?
N1 C6 S2 135.51(18) . . ?
S1 C6 S2 99.20(11) . . ?
O10 C10 Mn1 178.3(2) . . ?
O11 C11 Mn1 178.8(3) . . ?
O12 C12 Mn1 177.7(3) . . ?
O20 C20 Mo1 173.5(2) . . ?
O21 C21 Mo1 175.6(3) . . ?
N1 C50 C51 108.7(2) . . ?
N1 C50 C52 105.74(19) . . ?
C51 C50 C52 109.6(2) . . ?
N1 C50 C53 110.8(2) . . ?
C51 C50 C53 111.8(2) . . ?
C52 C50 C53 109.9(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 C20 1.996(3) . ?
Mo1 C21 2.009(3) . ?
Mo1 C4 2.270(3) . ?
Mo1 C3 2.288(3) . ?
Mo1 C5 2.293(3) . ?
Mo1 C1 2.347(3) . ?
Mo1 C2 2.349(3) . ?
Mo1 S1 2.4613(6) . ?
Mo1 S2 2.4708(6) . ?
Mo1 Mn1 2.7566(5) . ?
Mn1 C12 1.785(3) . ?
Mn1 C10 1.797(3) . ?
Mn1 C11 1.806(3) . ?
Mn1 S1 2.3270(7) . ?
Mn1 S2 2.3308(7) . ?
S1 C6 1.808(2) . ?
S2 C6 1.826(2) . ?
O10 C10 1.143(3) . ?
O11 C11 1.133(3) . ?
O12 C12 1.143(4) . ?
O20 C20 1.139(3) . ?
O21 C21 1.134(3) . ?
N1 C6 1.234(3) . ?
N1 C50 1.487(3) . ?
C1 C2 1.368(4) . ?
C1 C5 1.371(4) . ?
C2 C3 1.402(5) . ?
C3 C4 1.412(5) . ?
C4 C5 1.393(5) . ?
C50 C51 1.523(4) . ?
C50 C52 1.529(3) . ?
C50 C53 1.530(4) . ?
