Binuclear, tetranuclear and hexadecanuclear thio-oxomolybdenum(V/IV) glycolates with selective adsorptions of gases.
Lin, Rong-Yan; Deng, Lan; An, Dong-Li; Zhou, Zhao-Hui; Dalton transactions (Cambridge, England : 2003) 52 (2023) 562–571; doi:10.1039/d2dt03324k

data_7711712
_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         'C4 H7 Mo2 O9 S2, C10 H10 N3'
_chemical_formula_sum            'C14 H17 Mo2 N3 O9 S2'
_chemical_formula_weight         627.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-17
_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                74.526(3)
_cell_angle_beta                 85.918(3)
_cell_angle_gamma                89.947(3)
_cell_formula_units_Z            2
_cell_length_a                   6.8529(3)
_cell_length_b                   10.7593(4)
_cell_length_c                   14.1435(6)
_cell_measurement_reflns_used    4419
_cell_measurement_temperature    230
_cell_measurement_theta_max      71.6790
_cell_measurement_theta_min      3.2400
_cell_volume                     1002.31(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (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_temperature      230
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00  64.00   1.00    2.50    --    0.00-178.00 -60.00   29
  2  \w    -64.00 -37.00   1.00    2.50    --    0.00 -57.00-120.00   27
  3  \w     37.00  76.00   1.00    2.50    --    0.00-178.00 150.00   39
  4  \w     -6.00  24.00   1.00    2.50    --    0.00 -57.00-120.00   30
  5  \w   -125.00 -81.00   1.00   10.00    --  -57.00 -61.00 120.00   44
  6  \w   -131.00-106.00   1.00   10.00    --  -57.00 -95.00 -60.00   25
  7  \w    -57.00 -32.00   1.00   10.00    --  -57.00 -61.00 150.00   25
  8  \w    -66.00 -34.00   1.00   10.00    --  -57.00 -61.00 120.00   32
  9  \w    -76.00   8.00   1.00   10.00    --  -57.00  61.00 -90.00   84
 10  \w   -117.00  -4.00   1.00   10.00    --  -57.00 126.00 -90.00  113
 11  \w   -119.00 -87.00   1.00   10.00    --  -57.00 -95.00  60.00   32
 12  \w   -114.00 -81.00   1.00   10.00    --  -57.00 -95.00 -90.00   33
 13  \w     32.00 119.00   1.00   10.00    --   57.00  61.00 150.00   87
 14  \w    -10.00  82.00   1.00   10.00    --   57.00 -61.00   0.00   92
 15  \w     90.00 151.00   1.00   17.50    --  114.00  50.00  30.00   61
 16  \w     85.00 116.00   1.00   17.50    --  114.00-112.00 -30.00   31
 17  \w     93.00 130.00   1.00   17.50    --  114.00 -50.00 -90.00   37
 18  \w     60.00  86.00   1.00   17.50    --  114.00 -50.00 -90.00   26
 19  \w     81.00 140.00   1.00   17.50    --  114.00 -38.00   0.00   59
 20  \w     43.00 144.00   1.00   17.50    --  114.00 -38.00-150.00  101
 21  \w    124.00 176.00   1.00   17.50    --  114.00 -12.00-150.00   52
 22  \w     40.00  98.00   1.00   17.50    --  114.00 -12.00-150.00   58
 23  \w    152.00 177.00   1.00   17.50    --  114.00  77.00  90.00   25
 24  \w    109.00 139.00   1.00   17.50    --  114.00 -64.00  60.00   30
 25  \w     89.00 172.00   1.00   17.50    --  114.00  50.00-120.00   83
 26  \w     47.00  81.00   1.00   17.50    --  114.00-112.00 -30.00   34
 27  \w    130.00 156.00   1.00   17.50    --  114.00  50.00-180.00   26
 28  \w     44.00  93.00   1.00   17.50    --  114.00 -64.00  60.00   49
 29  \w     41.00  75.00   1.00   17.50    --  114.00 -38.00   0.00   34
 30  \w     87.00 115.00   1.00   17.50    --  114.00-112.00-120.00   28
 31  \w     44.00  81.00   1.00   17.50    --  114.00-112.00-120.00   37
 32  \w     68.00 106.00   1.00   17.50    --  114.00-112.00  90.00   38
 33  \w    121.00 172.00   1.00   17.50    --  114.00  25.00 120.00   51
 34  \w     73.00  98.00   1.00   17.50    --  114.00  25.00 120.00   25
 35  \w     44.00  85.00   1.00   17.50    --  114.00 -77.00 120.00   41
 36  \w    100.00 146.00   1.00   17.50    --  114.00 -77.00 120.00   46
 37  \w     43.00  69.00   1.00   17.50    --  114.00 -92.00  60.00   26
 38  \w     90.00 115.00   1.00   17.50    --  114.00 -92.00  60.00   25
 39  \w     81.00 116.00   1.00   17.50    --  114.00-112.00-180.00   35
 40  \w    106.00 177.00   1.00   17.50    --  114.00 112.00 120.00   71
 41  \w     53.00  92.00   1.00   17.50    --  114.00 -92.00-180.00   39
 42  \w     45.00 133.00   1.00   17.50    --  114.00 -25.00  90.00   88
 43  \w     68.00  94.00   1.00   17.50    --  114.00-112.00  60.00   26
 44  \w     73.00 105.00   1.00   17.50    --  114.00 -77.00-150.00   32
 45  \w    124.00 149.00   1.00   17.50    --  114.00 178.00-180.00   25
 46  \w    106.00 132.00   1.00   17.50    --  114.00 -92.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0024246000
_diffrn_orient_matrix_UB_12      0.0237834000
_diffrn_orient_matrix_UB_13      0.1027655000
_diffrn_orient_matrix_UB_21      0.1774786000
_diffrn_orient_matrix_UB_22      0.0928021000
_diffrn_orient_matrix_UB_23      -0.0348098000
_diffrn_orient_matrix_UB_31      -0.1389507000
_diffrn_orient_matrix_UB_32      0.1135903000
_diffrn_orient_matrix_UB_33      -0.0327229000
_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  0.0807
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7558
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.588
_diffrn_reflns_theta_min         3.251
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.952
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+4.3590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.2167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3214
_reflns_number_total             3887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03324k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7711711--7711714.cif.'
_cod_database_code               7711712
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.095
_reflns_odcompleteness_completeness 94.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 Mo2-H4
 2.923871 with sigma of 0.02
 C3-H4
 1.882004 with sigma of 0.02
 Mo2-H9A \\sim Mo2-H9B
 with sigma of 0.02
3.a Free rotating group:
 O9(H9A,H9B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C6(H6), C9(H9), C8(H8), C11(H11), C7(H7), C12(H12), C14(H14),
 C13(H13)
;
_shelx_res_checksum              51918
_shelx_hkl_checksum              91781
_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 3.179
_oxdiff_exptl_absorpt_empirical_full_min 0.485