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_7711714
_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         'C44 H50 Mo16 N24 Na2 O46'
_chemical_formula_sum            'C44 H50 Mo16 N24 Na2 O46'
_chemical_formula_weight         3232.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 121.411(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.6195(7)
_cell_length_b                   13.79520(10)
_cell_length_c                   20.6277(3)
_cell_measurement_reflns_used    14923
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.4490
_cell_measurement_theta_min      2.3750
_cell_volume                     10593.5(3)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.952
_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     -4.00  22.00   0.50    1.30    --    0.00  50.00 -39.00   52
  2  \w     29.00  71.00   0.50    1.30    --    0.00  50.00 -39.00   84
  3  \w   -169.00-122.00   0.50    6.00    --  -96.86 -50.00 174.00   94
  4  \w    -53.00 -25.00   0.50    6.00    --  -96.86  50.00 -39.00   56
  5  \w     85.00 152.00   0.50    6.00    --   96.86  50.00 -39.00  134
  6  \w     27.00  59.00   0.50    6.00    --   96.86 -50.00 174.00   64
  7  \w    -16.00  29.00   0.50    1.30    --    0.00 -99.00  60.00   90
  8  \w    -54.00  12.00   0.50    1.30    --    0.00 -50.00 174.00  132
  9  \w   -168.00 -85.00   0.50    6.00    --  -96.86 -57.00 120.00  166
 10  \w    -63.00 -28.00   0.50    6.00    --  -96.86  57.00 -90.00   70
 11  \w    -64.00 -26.00   0.50    6.00    --  -96.86  57.00  90.00   76
 12  \w    -62.00 -26.00   0.50    6.00    --  -96.86  57.00 150.00   72
 13  \w    -64.00 -39.00   0.50    6.00    --  -96.86  57.00   0.00   50
 14  \w    -64.00 -36.00   0.50    6.00    --  -96.86  57.00 120.00   56
 15  \w    -63.00 -26.00   0.50    6.00    --  -96.86  57.00  60.00   74
 16  \w     25.00  62.00   0.50    6.00    --   96.86 -99.00 150.00   74
 17  \w     30.00  60.00   0.50    6.00    --   96.86 -57.00 150.00   60
 18  \w    133.00 158.00   0.50    6.00    --   96.86  57.00-120.00   50
 19  \w     88.00 115.00   0.50    6.00    --   96.86 125.00-180.00   54
 20  \w    139.00 164.00   0.50    6.00    --   96.86 125.00-180.00   50
 21  \w     42.00  67.00   0.50    6.00    --   96.86 -57.00 120.00   50
 22  \w     37.00  64.00   0.50    6.00    --   96.86 -57.00-120.00   54
 23  \w     75.00 104.00   0.50    6.00    --   96.86 -99.00 150.00   58
 24  \w     25.00  70.00   0.50    6.00    --   96.86 -99.00  60.00   90
 25  \w     83.00 121.00   0.50    6.00    --   96.86  57.00-120.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0373286000
_diffrn_orient_matrix_UB_12      0.0258446000
_diffrn_orient_matrix_UB_13      -0.0139645000
_diffrn_orient_matrix_UB_21      0.0177524000
_diffrn_orient_matrix_UB_22      0.0628161000
_diffrn_orient_matrix_UB_23      0.0723499000
_diffrn_orient_matrix_UB_31      -0.0017137000
_diffrn_orient_matrix_UB_32      0.0886525000
_diffrn_orient_matrix_UB_33      -0.0472264000
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30981
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.073
_diffrn_reflns_theta_min         2.374
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59787
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       plate
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.587
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10101
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0469
_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/[\s^2^(Fo^2^)+(0.0893P)^2^+15.5338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8156
_reflns_number_total             10101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03324k2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7711711--7711714.cif.'
_cod_database_code               7711714
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C44H50Mo16N24O44
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.301
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N12(H12), C7(H7), C15(H15), C6(H6A), C14(H14), C16(H16A), C8(H8),
 C13(H13), C5(H5), C11(H11), C9(H9), C10(H10), C12(H12A), C17(H17), C22(H22),
 C18(H18), C19(H19), C21(H21), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13403
_shelx_hkl_checksum              63778
_shelx_fab_checksum              85427
_platon_squeeze_void_probe_radius 1.20
_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 1.663
_oxdiff_exptl_absorpt_empirical_full_min 0.704