Direct observation of dimethyl sulfide trapped by MOF proving efficient removal of sulfur impurities
Morita, Masashi; Yonezu, Akira; Kusaka, Shinpei; Hori, Akihiro; Ma, Yunsheng; Matsuda, Ryotaro; RSC Advances 10 (2020) 4710–4714; doi:10.1039/C9RA09702C

data_7239848
_publ_section_title
;
 Direct observation of dimethyl sulfide trapped by MOF proving efficient
 removal of sulfur impurities
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4710
_journal_page_last               4714
_journal_paper_doi               10.1039/C9RA09702C
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         '0.02(C288 H96 Cu48 O192)'
_chemical_formula_sum            'C6 H2 Cu O4'
_chemical_formula_weight         201.62
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-29 deposited with the CCDC.	2020-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   26.2622(2)
_cell_length_b                   26.2622(2)
_cell_length_c                   26.2622(2)
_cell_measurement_reflns_used    50562
_cell_measurement_temperature    203
_cell_measurement_theta_max      29.4850
_cell_measurement_theta_min      2.5450
_cell_volume                     18113.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      203
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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    -87.00 -36.00   0.50    3.00    --   -3.70 -38.00   0.00  102
  2  \w    -85.00 -11.00   0.50    3.00    --   -3.70 -19.00  90.00  148
  3  \w    -33.00  86.00   0.50    3.00    --   -3.70  38.00 120.00  238
  4  \w    -21.00  17.00   0.50    3.00    --   -3.70  82.00   0.00   76
  5  \w    -93.00  24.00   0.50    3.00    --   -3.70 -57.00-150.00  234
  6  \w    -32.00  22.00   0.50    3.00    --   -3.70  77.00-120.00  108
  7  \w     44.00  69.00   0.50    3.00    --   -3.70  57.00 -30.00   50
  8  \w    -10.00  16.00   0.50    3.00    --   -3.70  57.00 150.00   52
  9  \w     45.00  70.00   0.50    3.00    --   -3.70  38.00-120.00   50
 10  \w    -27.00   1.00   0.50    3.00    --   -3.70 -57.00  90.00   56
 11  \w    -26.00  32.00   0.50    3.00    --   -3.70 -77.00 -60.00  116
 12  \w     47.00  72.00   0.50    3.00    --    4.20  57.00 -60.00   50
 13  \w    -58.00  23.00   0.50    3.00    --    4.20 -57.00  60.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0123962500
_diffrn_orient_matrix_UB_12      0.0067560000
_diffrn_orient_matrix_UB_13      0.0230296500
_diffrn_orient_matrix_UB_21      -0.0089030500
_diffrn_orient_matrix_UB_22      0.0227708000
_diffrn_orient_matrix_UB_23      -0.0114673500
_diffrn_orient_matrix_UB_31      -0.0222809500
_diffrn_orient_matrix_UB_32      -0.0128539000
_diffrn_orient_matrix_UB_33      -0.0082304500
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0073
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            108242
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.386
_diffrn_reflns_theta_min         2.193
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.887
_exptl_crystal_description       block
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         1291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0311P)^2^+13.7746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1227
_reflns_number_total             1291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra09702c2.cif
_cod_data_source_block           exp_1851
_cod_depositor_comments
'Adding full bibliography for 7239846--7239848.cif.'
_cod_original_cell_volume        18113.1(4)
_cod_database_code               7239848
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C003(H003)
;
_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 0.768