#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/59/2225941.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_2225941
loop_
_publ_author_name
'Sui, Yan'
'Fang, Xiao-Niu'
'Luo, Qiu-Yan'
'Chen, Hong-Mei'
'Zhou, Meng-Qiang'
_publ_section_title
;
 (Dimethyl
 sulfoxide-κO)[3-hydroxy-2-hydroxymethyl-2-(3-methoxy-2-oxidobenzylideneamino-κ²O²,N)propanolato-κO]dioxomolybdenum(VI).
 Corrigendum
;
_journal_coeditor_code           NG9064
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              e23
_journal_paper_doi               10.1107/S1600536810007476
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mo (C12 H15 N O5) O2 (C2 H6 O S)]'
_chemical_formula_moiety         'C14 H21 Mo N O8 S'
_chemical_formula_sum            'C14 H21 Mo N O8 S'
_chemical_formula_weight         459.32
_chemical_melting_point_gt       454
_chemical_melting_point_lt       456
_chemical_name_systematic
;
(Dimethyl sulfoxide-\kO)[3-hydroxy-2-hydroxymethyl-2-(3-methoxy-2-
oxidobenzylideneamino-κ²O²,N)propanolato-\kO]dioxomolybdenum(VI)
;
_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                 115.3240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3130(7)
_cell_length_b                   9.2596(5)
_cell_length_c                   14.8563(7)
_cell_measurement_reflns_used    11097
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.61
_cell_volume                     1779.74(16)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'APEX2 (Bruker, 2004)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10668
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.9103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                3056
_reflns_number_total             3278
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng9064.cif
_cod_data_source_block           I
_cod_original_cell_volume        1779.74(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2225941
_cod_database_fobs_code          2225941
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.61630(15) 0.7171(2) 0.82021(14) 0.0306(4) Uani d . 1 . .
H H1 0.5551 0.7275 0.7628 0.037 Uiso calc R 1 . .
C C2 0.67331(15) 0.5841(2) 0.83147(14) 0.0296(4) Uani d . 1 . .
C C3 0.76286(15) 0.5507(2) 0.91746(14) 0.0290(4) Uani d . 1 . .
C C4 0.81292(15) 0.4178(2) 0.92185(15) 0.0320(4) Uani d . 1 . .
C C5 0.77698(17) 0.3257(2) 0.84100(16) 0.0353(5) Uani d . 1 . .
H H5 0.8110 0.2390 0.8441 0.042 Uiso calc R 1 . .
C C6 0.69022(17) 0.3620(2) 0.75494(16) 0.0382(5) Uani d . 1 . .
H H6 0.6675 0.3005 0.7002 0.046 Uiso calc R 1 . .
C C7 0.63806(16) 0.4877(2) 0.75039(15) 0.0358(5) Uani d . 1 . .
H H7 0.5788 0.5097 0.6932 0.043 Uiso calc R 1 . .
C C8 0.9572(2) 0.2667(3) 1.0142(2) 0.0606(8) Uani d . 1 . .
H H8A 0.9176 0.1814 1.0104 0.091 Uiso calc R 1 . .
H H8B 1.0184 0.2670 1.0760 0.091 Uiso calc R 1 . .
H H8C 0.9764 0.2679 0.9597 0.091 Uiso calc R 1 . .
C C9 0.57775(15) 0.9537(2) 0.85896(14) 0.0315(4) Uani d . 1 . .
C C10 0.64007(17) 1.0616(2) 0.94075(15) 0.0370(5) Uani d . 1 . .
H H10A 0.6914 1.1084 0.9242 0.044 Uiso calc R 1 . .
H H10B 0.5944 1.1355 0.9457 0.044 Uiso calc R 1 . .
C C11 0.47619(16) 0.9150(2) 0.86463(17) 0.0376(5) Uani d . 1 . .
H H11A 0.4393 0.8422 0.8152 0.045 Uiso calc R 1 . .
H H11B 0.4904 0.8766 0.9300 0.045 Uiso calc R 1 . .
C C12 0.55921(17) 1.0195(2) 0.75826(15) 0.0379(5) Uani d . 1 . .
H H12A 0.5287 1.1146 0.7523 0.045 Uiso calc R 1 . .
H H12B 0.6247 1.0302 0.7542 0.045 Uiso calc R 1 . .
Mo Mo1 0.779330(13) 0.829629(19) 1.036557(12) 0.03081(8) Uani d U 1 A .
N N1 0.64298(13) 0.82184(17) 0.88262(12) 0.0280(3) Uani d . 1 . .
O O1 0.89683(12) 0.39109(19) 1.00918(11) 0.0467(4) Uani d . 1 . .
O O2 0.80380(11) 0.63679(17) 0.99656(10) 0.0384(3) Uani d . 1 . .
O O3 0.68969(11) 0.98850(16) 1.03313(10) 0.0350(3) Uani d . 1 . .
O O4 0.41554(14) 1.0420(2) 0.84657(14) 0.0535(4) Uani d . 1 . .
H H4 0.3791 1.0373 0.8766 0.080 Uiso calc R 1 . .
O O5 0.49290(16) 0.9313(2) 0.67962(12) 0.0589(5) Uani d . 1 . .
H H5A 0.4619 0.9810 0.6300 0.088 Uiso calc R 1 . .
O O6 0.85527(13) 0.92141(19) 0.99470(13) 0.0498(4) Uani d . 1 . .
O O7 0.84674(14) 0.82180(19) 1.16266(12) 0.0506(4) Uani d . 1 . .
O O8 0.65402(13) 0.69377(18) 1.06088(12) 0.0463(4) Uani d U 1 . .
C C13 0.7091(3) 0.4309(4) 1.1317(3) 0.0645(9) Uani d PU 0.9402(18) A 1
H H13D 0.6536 0.3982 1.0710 0.077 Uiso calc PR 0.9402(18) A 1
H H13E 0.7147 0.3685 1.1854 0.077 Uiso calc PR 0.9402(18) A 1
H H13F 0.7727 0.4291 1.1247 0.077 Uiso calc PR 0.9402(18) A 1
C C14 0.5638(3) 0.5787(5) 1.1629(3) 0.0811(10) Uani d PU 0.9402(18) A 1
H H14D 0.5338 0.6697 1.1671 0.097 Uiso calc PR 0.9402(18) A 1
H H14E 0.5749 0.5216 1.2205 0.097 Uiso calc PR 0.9402(18) A 1
H H14F 0.5179 0.5285 1.1040 0.097 Uiso calc PR 0.9402(18) A 1
C C13A 0.662(5) 0.419(7) 1.110(4) 0.056(6) Uani d PU 0.0598(18) A 2
H H13A 0.6969 0.4216 1.0676 0.068 Uiso calc PR 0.0598(18) A 2
H H13B 0.6114 0.3433 1.0892 0.068 Uiso calc PR 0.0598(18) A 2
H H13C 0.7112 0.4022 1.1776 0.068 Uiso calc PR 0.0598(18) A 2
C C14A 0.630(4) 0.631(6) 1.219(4) 0.059(4) Uani d PU 0.0598(18) A 2
H H14A 0.6970 0.5990 1.2657 0.071 Uiso calc PR 0.0598(18) A 2
H H14B 0.5784 0.5938 1.2383 0.071 Uiso calc PR 0.0598(18) A 2
H H14C 0.6276 0.7345 1.2184 0.071 Uiso calc PR 0.0598(18) A 2
S S1 0.68357(6) 0.60903(8) 1.15748(5) 0.0488(2) Uani d PU 0.9402(18) A 1
S S1A 0.6059(10) 0.5697(14) 1.1039(9) 0.060(2) Uani d PU 0.0598(18) A 2
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 125.56(18) ?
N1 C1 H1 . . 117.2 ?
C2 C1 H1 . . 117.2 ?
C3 C2 C7 . . 119.53(19) ?
C3 C2 C1 . . 122.88(18) ?
C7 C2 C1 . . 117.55(18) ?
O2 C3 C2 . . 123.88(18) ?
O2 C3 C4 . . 117.29(17) ?
C2 C3 C4 . . 118.83(18) ?
O1 C4 C5 . . 124.42(19) ?
O1 C4 C3 . . 115.21(17) ?
C5 C4 C3 . . 120.36(19) ?
C4 C5 C6 . . 120.3(2) ?
C4 C5 H5 . . 119.8 ?
C6 C5 H5 . . 119.8 ?
C7 C6 C5 . . 120.31(19) ?
C7 C6 H6 . . 119.8 ?
C5 C6 H6 . . 119.8 ?
C6 C7 C2 . . 120.55(19) ?
C6 C7 H7 . . 119.7 ?
C2 C7 H7 . . 119.7 ?
O1 C8 H8A . . 109.5 ?
O1 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
O1 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
N1 C9 C12 . . 112.79(16) ?
N1 C9 C10 . . 104.78(15) ?
C12 C9 C10 . . 108.35(17) ?
N1 C9 C11 . . 108.02(16) ?
C12 C9 C11 . . 112.00(17) ?
C10 C9 C11 . . 110.68(17) ?
O3 C10 C9 . . 109.68(17) ?
O3 C10 H10A . . 109.7 ?
C9 C10 H10A . . 109.7 ?
O3 C10 H10B . . 109.7 ?
C9 C10 H10B . . 109.7 ?
H10A C10 H10B . . 108.2 ?
O4 C11 C9 . . 108.29(18) ?
O4 C11 H11A . . 110.0 ?
C9 C11 H11A . . 110.0 ?
O4 C11 H11B . . 110.0 ?
C9 C11 H11B . . 110.0 ?
H11A C11 H11B . . 108.4 ?
O5 C12 C9 . . 110.72(18) ?
O5 C12 H12A . . 109.5 ?
C9 C12 H12A . . 109.5 ?
O5 C12 H12B . . 109.5 ?
C9 C12 H12B . . 109.5 ?
H12A C12 H12B . . 108.1 ?
O6 Mo1 O7 . . 105.95(9) ?
O6 Mo1 O3 . . 97.53(7) ?
O7 Mo1 O3 . . 96.80(7) ?
O6 Mo1 O2 . . 96.88(8) ?
O7 Mo1 O2 . . 101.78(7) ?
O3 Mo1 O2 . . 152.32(6) ?
O6 Mo1 N1 . . 93.20(7) ?
O7 Mo1 N1 . . 159.85(8) ?
O3 Mo1 N1 . . 74.06(6) ?
O2 Mo1 N1 . . 81.65(6) ?
O6 Mo1 O8 . . 168.61(7) ?
O7 Mo1 O8 . . 85.31(8) ?
O3 Mo1 O8 . . 82.51(6) ?
O2 Mo1 O8 . . 78.78(7) ?
N1 Mo1 O8 . . 75.82(6) ?
C1 N1 C9 . . 119.23(17) ?
C1 N1 Mo1 . . 127.61(14) ?
C9 N1 Mo1 . . 113.08(12) ?
C4 O1 C8 . . 117.75(18) ?
C3 O2 Mo1 . . 138.18(13) ?
C10 O3 Mo1 . . 116.08(12) ?
C11 O4 H4 . . 109.5 ?
C12 O5 H5A . . 109.5 ?
S1 O8 S1A . . 41.6(5) ?
S1 O8 Mo1 . . 119.88(10) ?
S1A O8 Mo1 . . 158.9(5) ?
S1A C13A H13A . . 109.5 ?
S1A C13A H13B . . 109.5 ?
H13A C13A H13B . . 109.5 ?
S1A C13A H13C . . 109.5 ?
H13A C13A H13C . . 109.5 ?
H13B C13A H13C . . 109.5 ?
S1A C14A H14A . . 109.5 ?
S1A C14A H14B . . 109.5 ?
H14A C14A H14B . . 109.5 ?
S1A C14A H14C . . 109.5 ?
H14A C14A H14C . . 109.5 ?
H14B C14A H14C . . 109.5 ?
O8 S1 C13 . . 106.01(15) ?
O8 S1 C14 . . 103.85(14) ?
C13 S1 C14 . . 98.9(2) ?
C13A S1A O8 . . 111(2) ?
C13A S1A C14A . . 111(3) ?
O8 S1A C14A . . 103(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.282(3) ?
C1 C2 . 1.448(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.403(3) ?
C2 C7 . 1.407(3) ?
C3 O2 . 1.331(2) ?
C3 C4 . 1.411(3) ?
C4 O1 . 1.362(2) ?
C4 C5 . 1.381(3) ?
C5 C6 . 1.390(3) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.369(3) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 O1 . 1.422(3) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 N1 . 1.485(2) ?
C9 C12 . 1.530(3) ?
C9 C10 . 1.531(3) ?
C9 C11 . 1.534(3) ?
C10 O3 . 1.419(2) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 O4 . 1.417(3) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C12 O5 . 1.409(3) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
Mo1 O6 . 1.6937(17) ?
Mo1 O7 . 1.7028(16) ?
Mo1 O3 . 1.9383(14) ?
Mo1 O2 . 1.9602(15) ?
Mo1 N1 . 2.2861(17) ?
Mo1 O8 . 2.3419(17) ?
O4 H4 . 0.8200 ?
O5 H5A . 0.8200 ?
O8 S1 . 1.5280(17) ?
O8 S1A . 1.606(12) ?
C13 S1 . 1.767(4) ?
C13 H13D . 0.9600 ?
C13 H13E . 0.9600 ?
C13 H13F . 0.9600 ?
C14 S1 . 1.772(4) ?
C14 H14D . 0.9600 ?
C14 H14E . 0.9600 ?
C14 H14F . 0.9600 ?
C13A S1A . 1.59(6) ?
C13A H13A . 0.9600 ?
C13A H13B . 0.9600 ?
C13A H13C . 0.9600 ?
C14A S1A . 1.69(5) ?
C14A H14A . 0.9600 ?
C14A H14B . 0.9600 ?
C14A H14C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C10 H10B O4 . 0.97 2.50 2.911(3) 105.3
C1 H1 O5 . 0.93 2.22 2.874(3) 126.5
C14 H14E O7 2_647 0.96 2.45 3.343(4) 153.8
C8 H8A O6 1_545 0.96 2.54 3.475(4) 163.7
C11 H11A O7 4_575 0.97 2.57 3.534(3) 170.0
O5 H5A O1 4_575 0.82 2.02 2.834(2) 175.4
O5 H5A O2 4_575 0.82 2.53 2.970(2) 114.9
O4 H4 O3 3_677 0.82 1.99 2.801(2) 170.9
