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_7711713
_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 H4 Mo4 O18 S6, 4(C10 H10 N3)'
_chemical_formula_sum            'C44 H44 Mo4 N12 O18 S6'
_chemical_formula_weight         1605.03
_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
_audit_creation_date             2022-06-02
_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                104.9280(10)
_cell_angle_beta                 103.8410(10)
_cell_angle_gamma                98.2450(10)
_cell_formula_units_Z            1
_cell_length_a                   11.1684(2)
_cell_length_b                   11.2139(2)
_cell_length_c                   11.8751(2)
_cell_measurement_reflns_used    8788
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      74.2540
_cell_measurement_theta_min      4.0180
_cell_volume                     1361.60(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.950
_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     84.00 178.00   0.50    0.28    --  107.68  30.00  30.00  188
  2  \w    138.00 174.00   0.50    0.28    --  107.68  45.00 -60.00   72
  3  \w     98.00 178.00   0.50    0.28    --  107.68  45.00 -90.00  160
  4  \w     93.00 124.00   0.50    0.28    --  107.68  45.00 -60.00   62
  5  \w    -28.00  43.00   0.50    0.07    --   43.80 -38.00   0.00  142
  6  \w     38.00  66.00   0.50    0.28    --  107.68 -61.00 150.00   56
  7  \w     34.00  59.00   0.50    0.28    --  107.68 -61.00 120.00   50
  8  \w     49.00  91.00   0.50    0.28    --  107.68 -77.00   0.00   84
  9  \w     34.00  70.00   0.50    0.28    --  107.68 -61.00 -60.00   72
 10  \w     37.00 102.00   0.50    0.28    --  107.68 -77.00-120.00  130
 11  \w     81.00 108.00   0.50    0.28    --  107.68 -94.00 -60.00   54
 12  \w     89.00 115.00   0.50    0.28    --  107.68-125.00 -90.00   52
 13  \w     81.00 111.00   0.50    0.28    --  107.68-125.00 -30.00   60
 14  \w     39.00  70.00   0.50    0.28    --  107.68-125.00 -90.00   62
 15  \w     84.00 116.00   0.50    0.28    --  107.68-125.00  60.00   64
 16  \w     48.00  99.00   0.50    0.28    --  107.68 -94.00 120.00  102
 17  \w     52.00  80.00   0.50    0.28    --  107.68-125.00 120.00   56
 18  \w     91.00 116.00   0.50    0.28    --  107.68-125.00 120.00   50
 19  \w     34.00 102.00   0.50    0.28    --  107.68 -94.00-150.00  136
 20  \w     31.00  91.00   0.50    0.07    --   43.80-125.00 -90.00  120
 21  \w      2.00  40.00   0.50    0.07    --   43.80 -99.00 -30.00   76
 22  \w     53.00  79.00   0.50    0.07    --   43.80 -99.00 -30.00   52
 23  \w    101.00 127.00   0.50    0.28    --  107.68 125.00 -60.00   52
 24  \w     93.00 118.00   0.50    0.28    --  107.68 125.00-150.00   50
 25  \w    144.00 178.00   0.50    0.28    --  107.68 125.00-150.00   68
 26  \w    146.00 178.00   0.50    0.28    --  107.68 125.00 -60.00   64
 27  \w    -24.00  36.00   0.50    0.07    --  -43.80  19.00-180.00  120
 28  \w    -50.00 -16.00   0.50    0.28    --  -90.25  45.00 -30.00   68
 29  \w    -46.00 -15.00   0.50    0.28    --  -90.25  45.00  30.00   62
 30  \w      8.00  36.00   0.50    0.07    --  -43.80  19.00  90.00   56
 31  \w    -37.00  -5.00   0.50    0.07    --  -43.80  38.00  60.00   64
 32  \w    -49.00 -14.00   0.50    0.28    --  -90.25  45.00-180.00   70
 33  \w   -101.00 -21.00   0.50    0.28    --  -90.25  77.00  60.00  160
 34  \w    -51.00 -14.00   0.50    0.28    --  -90.25  45.00   0.00   74
 35  \w    -51.00 -26.00   0.50    0.28    --  -90.25  45.00  60.00   50
 36  \w    -51.00 -16.00   0.50    0.28    --  -90.25  45.00 120.00   70
 37  \w   -143.00 -69.00   0.50    0.28    --  -90.25 -45.00  90.00  148
 38  \w   -161.00-109.00   0.50    0.28    --  -90.25 -61.00  60.00  104
 39  \w   -114.00 -71.00   0.50    0.07    --  -43.80-125.00  90.00   86
 40  \w   -115.00 -74.00   0.50    0.07    --  -43.80-125.00   0.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1082090000
_diffrn_orient_matrix_UB_12      0.0441318000
_diffrn_orient_matrix_UB_13      0.1198380000
_diffrn_orient_matrix_UB_21      0.0174532000
_diffrn_orient_matrix_UB_22      -0.1368580000
_diffrn_orient_matrix_UB_23      -0.0187828000
_diffrn_orient_matrix_UB_31      0.0958157000
_diffrn_orient_matrix_UB_32      0.0234729000
_diffrn_orient_matrix_UB_33      -0.0703768000
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13703
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.830
_diffrn_reflns_theta_min         4.024
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.250
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0329P)^2^+9.5031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5163
_reflns_number_total             5299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03324k2.cif
_cod_data_source_block           exp_1830
_cod_depositor_comments
'Adding full bibliography for 7711711--7711714.cif.'
_cod_database_code               7711713
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'Fe Dy C O N'
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.149
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), N4(H4A), N1(H1), C10(H10), C14(H14), C9(H9), C8(H8), C13(H13),
  C4(H4), C11(H11), C16(H16), C15(H15), C21(H21), C20(H20), C19(H19), C6(H6),
 C7(H7), C22(H22), C23(H23)
;
_shelx_res_checksum              85063
_shelx_hkl_checksum              12602
_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 2.022
_oxdiff_exptl_absorpt_empirical_full_min 0.695