#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:43:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/99/2209958.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_2209958
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)
;
_journal_coeditor_code           NG2042
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1994
_journal_page_last               m1996
_journal_paper_doi               10.1107/S1600536806028832
_journal_volume                  62
_journal_year                    2006
_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          .454E-305
_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
_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    296(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.61
_cell_volume                     1779.74(16)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    XSHELL
_computing_publication_material  XSHELL
_computing_structure_refinement  'XSHELL (Bruker, 2004)'
_computing_structure_solution    'SHELXS97 (Bruker, 2004)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II area-detector'
_diffrn_measurement_method       'φ and ω'
_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    0.0179
_diffrn_reflns_limit_h_max       17
_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       -18
_diffrn_reflns_number            11097
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.753
_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          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.06P)²+1.031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                3214
_reflns_number_total             3461
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2042.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               2209958
_cod_database_fobs_code          2209958
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
Mo Mo1 0.779342(14) 0.82962(2) 1.036562(13) 0.03053(10) Uani d . 1 A 4
S S1 0.68353(6) 0.60908(8) 1.15747(5) 0.05242(19) Uani d . 1 A 4
O O1 0.89699(14) 0.3911(2) 1.00913(13) 0.0464(4) Uani d . 1 A 4
O O2 0.80375(13) 0.63641(19) 0.99676(12) 0.0383(4) Uani d . 1 A 4
O O3 0.68970(12) 0.98848(17) 1.03310(11) 0.0348(3) Uani d . 1 A 4
O O4 0.41534(16) 1.0419(2) 0.84641(16) 0.0531(5) Uani d . 1 A 4
H H4 0.3815 1.0394 0.8791 0.080 Uiso calc R 1 A 4
O O5 0.49277(18) 0.9309(2) 0.67953(13) 0.0590(6) Uani d . 1 A 4
H H5A 0.4585 0.9813 0.6312 0.089 Uiso calc R 1 A 4
O O6 0.85542(14) 0.9214(2) 0.99462(15) 0.0493(5) Uani d . 1 A 4
O O7 0.84674(16) 0.8218(2) 1.16267(14) 0.0502(5) Uani d . 1 A 4
O O8 0.65380(16) 0.6936(2) 1.06084(14) 0.0469(4) Uani d . 1 A 4
N N1 0.64278(15) 0.82189(19) 0.88244(14) 0.0280(4) Uani d . 1 A 4
C C1 0.61624(17) 0.7169(3) 0.82019(16) 0.0306(4) Uani d . 1 A 4
H H1 0.5550 0.7270 0.7628 0.037 Uiso calc R 1 A 4
C C2 0.67332(16) 0.5842(2) 0.83160(15) 0.0293(4) Uani d . 1 A 4
C C3 0.76272(16) 0.5506(2) 0.91730(15) 0.0287(4) Uani d . 1 A 4
C C4 0.81288(17) 0.4179(3) 0.92181(16) 0.0320(5) Uani d . 1 A 4
C C5 0.77712(19) 0.3256(2) 0.84106(18) 0.0350(5) Uani d . 1 A 4
H H5 0.8111 0.2389 0.8442 0.042 Uiso calc R 1 A 4
C C6 0.68987(19) 0.3623(3) 0.75464(17) 0.0379(5) Uani d . 1 A 4
H H6 0.6670 0.3010 0.6998 0.045 Uiso calc R 1 A 4
C C7 0.63803(18) 0.4876(3) 0.75026(17) 0.0358(5) Uani d . 1 A 4
H H7 0.5788 0.5097 0.6931 0.043 Uiso calc R 1 A 4
C C8 0.9577(2) 0.2671(3) 1.0141(2) 0.0594(8) Uani d . 1 A 4
H H8A 0.9193 0.1815 1.0129 0.089 Uiso calc R 1 A 4
H H8B 1.0202 0.2695 1.0747 0.089 Uiso calc R 1 A 4
H H8C 0.9745 0.2666 0.9581 0.089 Uiso calc R 1 A 4
C C9 0.57770(17) 0.9536(2) 0.85891(16) 0.0313(5) Uani d . 1 A 4
C C10 0.64003(19) 1.0618(3) 0.94075(17) 0.0366(5) Uani d . 1 A 4
H H10A 0.6913 1.1086 0.9242 0.044 Uiso calc R 1 A 4
H H10B 0.5943 1.1355 0.9458 0.044 Uiso calc R 1 A 4
C C11 0.47637(18) 0.9147(3) 0.86466(18) 0.0374(5) Uani d . 1 A 4
H H11A 0.4396 0.8417 0.8153 0.045 Uiso calc R 1 A 4
H H11B 0.4907 0.8764 0.9300 0.045 Uiso calc R 1 A 4
C C12 0.55954(19) 1.0198(3) 0.75862(17) 0.0376(5) Uani d . 1 A 4
H H12A 0.5291 1.1150 0.7527 0.045 Uiso calc R 1 A 4
H H12B 0.6251 1.0305 0.7546 0.045 Uiso calc R 1 A 4
C C13 0.7072(3) 0.4302(4) 1.1308(3) 0.0683(9) Uani d . 1 A 4
H H13A 0.6517 0.3991 1.0697 0.102 Uiso calc R 1 A 4
H H13B 0.7115 0.3676 1.1840 0.102 Uiso calc R 1 A 4
H H13C 0.7711 0.4270 1.1244 0.102 Uiso calc R 1 A 4
C C14 0.5640(4) 0.5800(6) 1.1634(4) 0.1000(17) Uani d . 1 A 4
H H14A 0.5345 0.6712 1.1679 0.150 Uiso calc R 1 A 4
H H14B 0.5751 0.5228 1.2210 0.150 Uiso calc R 1 A 4
H H14C 0.5177 0.5302 1.1045 0.150 Uiso calc R 1 A 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
_geom_angle_publ_flag
O7 Mo1 O8 85.34(9) y
O7 Mo1 O3 96.81(8) y
O7 Mo1 O2 101.69(8) y
O7 Mo1 N1 159.84(10) y
O6 Mo1 O8 168.57(8) y
O6 Mo1 O7 105.96(11) y
O6 Mo1 O3 97.58(8) y
O6 Mo1 O2 96.94(9) y
O6 Mo1 N1 93.20(8) y
O5 C12 H12B 109.6 ?
O5 C12 H12A 109.6 ?
O5 C12 C9 110.4(2) ?
O4 C11 H11B 110.0 ?
O4 C11 H11A 110.0 ?
O4 C11 C9 108.3(2) ?
O3 Mo1 O8 82.51(7) y
O3 Mo1 O2 152.29(7) y
O3 C10 H10B 109.8 ?
O3 C10 H10A 109.8 ?
O3 C10 C9 109.58(18) ?
O2 Mo1 O8 78.67(8) y
O2 Mo1 N1 81.72(6) y
O2 C3 C4 117.05(19) ?
O2 C3 C2 123.9(2) ?
O1 C4 C5 124.2(2) ?
O1 C4 C3 115.35(19) ?
N1 Mo1 O8 75.78(7) y
N1 C9 C12 112.81(18) ?
N1 C9 C11 107.90(18) ?
N1 C9 C10 104.88(17) ?
N1 C1 H1 117.2 ?
N1 C1 C2 125.6(2) ?
H12A C12 H12B 108.1 ?
H11A C11 H11B 108.4 ?
H10A C10 H10B 108.2 ?
C9 N1 Mo1 113.05(13) ?
C9 C12 H12B 109.6 ?
C9 C12 H12A 109.6 ?
C9 C11 H11B 110.0 ?
C9 C11 H11A 110.0 ?
C9 C10 H10B 109.8 ?
C9 C10 H10A 109.8 ?
C7 C6 H6 119.8 ?
C7 C6 C5 120.4(2) ?
C7 C2 C1 117.5(2) ?
C6 C7 H7 119.7 ?
C6 C7 C2 120.7(2) ?
C6 C5 H5 120.0 ?
C5 C6 H6 119.8 ?
C5 C4 C3 120.4(2) ?
C4 O1 C8 117.9(2) ?
C4 C5 H5 120.0 ?
C4 C5 C6 120.1(2) ?
C3 O2 Mo1 137.95(15) ?
C3 C2 C7 119.4(2) ?
C3 C2 C1 123.11(19) ?
C2 C7 H7 119.7 ?
C2 C3 C4 119.01(19) ?
C2 C1 H1 117.2 ?
C1 N1 C9 119.42(19) ?
C13 S1 C14 98.6(2) ?
C12 C9 C11 112.26(19) ?
C12 C9 C10 108.06(19) ?
C11 C9 C10 110.69(19) ?
C10 O3 Mo1 116.17(13) ?
C1 N1 Mo1 127.44(15) y
O3 Mo1 N1 74.03(6) y
S1 O8 Mo1 119.74(11) ?
O8 S1 C14 103.78(16) ?
O8 S1 C13 105.81(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 N1 2.289(2) y
Mo1 O2 1.9619(16) y
Mo1 O3 1.9380(15) y
Mo1 O6 1.6958(19) y
Mo1 O7 1.7028(18) y
Mo1 O8 2.345(2) y
S1 O8 1.5270(19) ?
S1 C13 1.769(4) ?
S1 C14 1.771(4) ?
O1 C4 1.363(3) ?
O1 C8 1.423(3) ?
O2 C3 1.333(3) ?
O3 C10 1.419(3) ?
O4 C11 1.422(3) ?
O4 H4 0.8200 ?
O5 C12 1.418(3) ?
O5 H5A 0.8200 ?
N1 C1 1.282(3) ?
N1 C9 1.483(3) ?
C1 C2 1.445(3) ?
C1 H1 0.9300 ?
C2 C3 1.400(3) ?
C2 C7 1.412(3) ?
C3 C4 1.411(3) ?
C4 C5 1.381(3) ?
C5 C6 1.397(4) ?
C5 H5 0.9300 ?
C6 C7 1.363(4) ?
C6 H6 0.9300 ?
C7 H7 0.9300 ?
C8 H8A 0.9600 ?
C8 H8B 0.9600 ?
C8 H8C 0.9600 ?
C9 C12 1.527(3) ?
C9 C11 1.532(3) ?
C9 C10 1.533(3) ?
C10 H10A 0.9700 ?
C10 H10B 0.9700 ?
C11 H11A 0.9700 ?
C11 H11B 0.9700 ?
C12 H12A 0.9700 ?
C12 H12B 0.9700 ?
C13 H13A 0.9600 ?
C13 H13B 0.9600 ?
C13 H13C 0.9600 ?
C14 H14A 0.9600 ?
C14 H14B 0.9600 ?
C14 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
_geom_hbond_publ_flag
C14 H14B O7 2_647 0.96 2.46 3.347(4) 153.6 ?
C11 H11A O7 4_575 0.97 2.57 3.532(3) 169.9 ?
C8 H8A O6 1_545 0.96 2.55 3.480(4) 163.4 ?
O4 H4 O3 3_677 0.82 1.99 2.801(2) 172.7 y
O5 H5A O1 4_575 0.82 2.02 2.835(2) 170.0 y
O5 H5A O2 4_575 0.82 2.51 2.966(2) 116.3 y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139070060
