#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:42:39 +0300 (Fri, 05 May 2023) $
#$Revision: 283349 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/17/7711711.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_7711711
loop_
_publ_author_name
'Lin, Rong-Yan'
'Deng, Lan'
'An, Dong-Li'
'Zhou, Zhao-Hui'
_publ_section_title
;
 Binuclear, tetranuclear and hexadecanuclear thio-oxomolybdenum(V/IV)
 glycolates with selective adsorptions of gases.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              562
_journal_page_last               571
_journal_paper_doi               10.1039/d2dt03324k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C10 H14 Mo2 N4 O9 S, 0.5(H4 O2)'
_chemical_formula_sum            'C10 H16 Mo2 N4 O10 S'
_chemical_formula_weight         576.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1969(3)
_cell_length_b                   23.5561(7)
_cell_length_c                   5.9279(2)
_cell_measurement_reflns_used    3635
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9650
_cell_measurement_theta_min      6.9450
_cell_volume                     1842.79(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00  58.00   0.50    0.60    --  105.19-125.00 150.00   50
  2  ω     78.00 108.00   0.50    0.60    --  105.19-125.00 150.00   60
  3  ω     77.00 119.00   0.50    0.18    --   47.87 169.00  54.00   84
  4  ω     74.00 151.00   0.50    0.60    --  105.19 169.00  54.00  154
  5  ω     41.00  66.00   0.50    0.60    --  105.19 -61.00-150.00   50
  6  ω     49.00  90.00   0.50    0.60    --  105.19-125.00-150.00   82
  7  ω    -24.00   1.00   0.50    0.18    --  -47.87  19.00 120.00   50
  8  ω   -165.00 -95.00   0.50    0.60    --  -99.00-103.00  81.00  140
  9  ω   -166.00 -89.00   0.50    0.60    --  -99.00 -25.00 -97.00  154
 10  ω   -117.00 -92.00   0.50    0.18    --  -47.87 -77.00-120.00   50
 11  ω    -68.00 -26.00   0.50    0.18    --  -47.87 -77.00-120.00   84
 12  ω    -21.00  27.00   0.50    0.18    --  -47.87  19.00-180.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0366929000
_diffrn_orient_matrix_UB_12      0.0450571000
_diffrn_orient_matrix_UB_13      -0.1698069000
_diffrn_orient_matrix_UB_21      0.0101899000
_diffrn_orient_matrix_UB_22      0.0461783000
_diffrn_orient_matrix_UB_23      0.1825961000
_diffrn_orient_matrix_UB_31      0.1103043000
_diffrn_orient_matrix_UB_32      0.0107124000
_diffrn_orient_matrix_UB_33      -0.0735552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6129
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.432
_diffrn_reflns_theta_min         3.753
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0404P)²+6.3158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1720
_reflns_number_total             1873
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03324k2.cif
_cod_data_source_block           exp_329_auto
_cod_depositor_comments
'Adding full bibliography for 7711711--7711714.cif.'
_cod_database_code               7711711
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.362
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1WB(0.5)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C4(H4), C5(H5)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.385
_oxdiff_exptl_absorpt_empirical_full_min 0.811
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.25021(2) 0.69324(2) 0.53022(6) 0.01947(15) Uani 1 1 d . . . . .
S1 S 0.20068(9) 0.750000 0.2275(2) 0.0195(3) Uani 1 2 d S T P . .
O3 O 0.39092(19) 0.67565(12) 0.3243(5) 0.0225(6) Uani 1 1 d . . . . .
H3 H 0.416405 0.697387 0.227383 0.034 Uiso 1 1 calc R U . . .
O1 O 0.3278(3) 0.750000 0.6914(7) 0.0221(8) Uani 1 2 d S T P . .
O1W O 0.4562(3) 0.750000 0.0233(7) 0.0256(9) Uani 1 2 d GS T P . .
H1WA H 0.419245 0.749875 -0.097722 0.038 Uiso 1 2 d G U P . .
H1WB H 0.516383 0.761280 -0.016799 0.038 Uiso 0.5 1 d G U P . .
O2 O 0.1450(2) 0.68387(12) 0.6866(5) 0.0246(6) Uani 1 1 d . . . . .
O4 O 0.3415(2) 0.63640(13) 0.7073(5) 0.0294(7) Uani 1 1 d . . . . .
O5 O 0.4822(2) 0.58642(13) 0.7572(6) 0.0360(8) Uani 1 1 d . . . . .
N1 N 0.2053(2) 0.61558(14) 0.3422(6) 0.0233(7) Uani 1 1 d . . . . .
N2 N 0.1399(3) 0.57795(15) 0.4387(6) 0.0271(8) Uani 1 1 d . . . . .
H2 H 0.110769 0.582682 0.570878 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4302(3) 0.61974(17) 0.6476(7) 0.0253(9) Uani 1 1 d . . . . .
C3 C 0.1259(3) 0.53279(18) 0.3049(8) 0.0322(10) Uani 1 1 d . . . . .
H3A H 0.082888 0.501309 0.334372 0.039 Uiso 1 1 calc R U . . .
C4 C 0.1848(3) 0.5404(2) 0.1188(9) 0.0352(11) Uani 1 1 d . . . . .
H4 H 0.191759 0.515142 -0.005136 0.042 Uiso 1 1 calc R U . . .
C5 C 0.2327(3) 0.5925(2) 0.1461(8) 0.0290(9) Uani 1 1 d . . . . .
H5 H 0.278136 0.609104 0.040892 0.035 Uiso 1 1 calc R U . . .
C1 C 0.4690(3) 0.6430(2) 0.4276(8) 0.0310(10) Uani 1 1 d . . . . .
H1A H 0.529149 0.667195 0.454916 0.037 Uiso 1 1 calc R U . . .
H1B H 0.489201 0.611491 0.326837 0.037 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
S1 Mo1 Mo1 55.00(2) . 7_575 ?
O3 Mo1 Mo1 100.56(7) . 7_575 ?
O3 Mo1 S1 85.41(8) . . ?
O1 Mo1 Mo1 46.32(8) . 7_575 ?
O1 Mo1 S1 97.58(9) . . ?
O1 Mo1 O3 87.63(13) . . ?
O1 Mo1 O4 83.66(12) . . ?
O1 Mo1 N1 163.10(13) . . ?
O2 Mo1 Mo1 97.53(10) . 7_575 ?
O2 Mo1 S1 105.53(10) . . ?
O2 Mo1 O3 161.90(12) . . ?
O2 Mo1 O1 104.76(15) . . ?
O2 Mo1 O4 96.60(13) . . ?
O2 Mo1 N1 87.06(13) . . ?
O4 Mo1 Mo1 129.96(9) . 7_575 ?
O4 Mo1 S1 156.63(9) . . ?
O4 Mo1 O3 71.30(11) . . ?
O4 Mo1 N1 82.98(12) . . ?
N1 Mo1 Mo1 145.40(9) . 7_575 ?
N1 Mo1 S1 90.65(9) . . ?
N1 Mo1 O3 78.30(11) . . ?
Mo1 S1 Mo1 69.99(4) . 7_575 ?
Mo1 O3 H3 125.9 . . ?
C1 O3 Mo1 117.5(2) . . ?
C1 O3 H3 109.5 . . ?
Mo1 O1 Mo1 87.36(16) . 7_575 ?
H1WA O1W H1WB 106.6 . 7_575 ?
H1WA O1W H1WB 106.8 . . ?
H1WB O1W H1WB 35.5 . 7_575 ?
C2 O4 Mo1 125.8(3) . . ?
N2 N1 Mo1 119.6(3) . . ?
C5 N1 Mo1 134.5(3) . . ?
C5 N1 N2 105.8(3) . . ?
N1 N2 H2 124.6 . . ?
C3 N2 N1 110.8(4) . . ?
C3 N2 H2 124.6 . . ?
O4 C2 C1 115.9(4) . . ?
O5 C2 O4 123.9(4) . . ?
O5 C2 C1 120.1(4) . . ?
N2 C3 H3A 126.4 . . ?
N2 C3 C4 107.2(4) . . ?
C4 C3 H3A 126.4 . . ?
C3 C4 H4 126.8 . . ?
C3 C4 C5 106.4(4) . . ?
C5 C4 H4 126.8 . . ?
N1 C5 C4 109.8(4) . . ?
N1 C5 H5 125.1 . . ?
C4 C5 H5 125.1 . . ?
O3 C1 C2 108.9(3) . . ?
O3 C1 H1A 109.9 . . ?
O3 C1 H1B 109.9 . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
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 Mo1 2.6741(6) 7_575 ?
Mo1 S1 2.3312(11) . ?
Mo1 O3 2.260(3) . ?
Mo1 O1 1.936(3) . ?
Mo1 O2 1.684(3) . ?
Mo1 O4 2.085(3) . ?
Mo1 N1 2.222(3) . ?
O3 H3 0.8400 . ?
O3 C1 1.424(5) . ?
O1W H1WA 0.8676 . ?
O1W H1WB 0.8702 . ?
O1W H1WB 0.87(6) 7_575 ?
O4 C2 1.285(5) . ?
O5 C2 1.228(5) . ?
N1 N2 1.364(5) . ?
N1 C5 1.333(5) . ?
N2 H2 0.8800 . ?
N2 C3 1.340(6) . ?
C2 C1 1.505(6) . ?
C3 H3A 0.9500 . ?
C3 C4 1.361(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(7) . ?
C5 H5 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O3 C1 C2 8.8(4) . . . . ?
Mo1 O4 C2 O5 179.5(3) . . . . ?
Mo1 O4 C2 C1 -1.3(5) . . . . ?
Mo1 N1 N2 C3 -177.0(3) . . . . ?
Mo1 N1 C5 C4 175.5(3) . . . . ?
O4 C2 C1 O3 -5.2(5) . . . . ?
O5 C2 C1 O3 174.1(4) . . . . ?
N1 N2 C3 C4 1.1(5) . . . . ?
N2 N1 C5 C4 0.0(5) . . . . ?
N2 C3 C4 C5 -1.1(5) . . . . ?
C3 C4 C5 N1 0.7(5) . . . . ?
C5 N1 N2 C3 -0.7(4) . . . . ?
