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_7711711
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     33.00  58.00   0.50    0.60    --  105.19-125.00 150.00   50
  2  \w     78.00 108.00   0.50    0.60    --  105.19-125.00 150.00   60
  3  \w     77.00 119.00   0.50    0.18    --   47.87 169.00  54.00   84
  4  \w     74.00 151.00   0.50    0.60    --  105.19 169.00  54.00  154
  5  \w     41.00  66.00   0.50    0.60    --  105.19 -61.00-150.00   50
  6  \w     49.00  90.00   0.50    0.60    --  105.19-125.00-150.00   82
  7  \w    -24.00   1.00   0.50    0.18    --  -47.87  19.00 120.00   50
  8  \w   -165.00 -95.00   0.50    0.60    --  -99.00-103.00  81.00  140
  9  \w   -166.00 -89.00   0.50    0.60    --  -99.00 -25.00 -97.00  154
 10  \w   -117.00 -92.00   0.50    0.18    --  -47.87 -77.00-120.00   50
 11  \w    -68.00 -26.00   0.50    0.18    --  -47.87 -77.00-120.00   84
 12  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0404P)^2^+6.3158P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              30969
_shelx_hkl_checksum              63498
_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