Direct structural evidence of commensurate-to-incommensurate transition of hydrocarbon adsorption in a microporous metal organic framework
Banerjee, Debasis; Wang, Hao; Gong, Qihan; Plonka, Anna M.; Jagiello, Jacek; Wu, Haohan; Woerner, William R.; Emge, Thomas J.; Olson, David H.; Parise, John B.; Li, Jing; Chem. Sci. 7 (2016) 759–; doi:10.1039/C5SC03685B

data_1540447
_publ_section_title
;
 Direct structural evidence of commensurate-to-incommensurate transition
 of hydrocarbon adsorption in a microporous metal organic framework
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              759
_journal_paper_doi               10.1039/C5SC03685B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C14 H8 Ca O6 S, 0.18(C4 H10)'
_chemical_formula_sum            'C14.72 H9.79 Ca O6 S'
_chemical_formula_weight         354.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-28 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.691(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6884(5)
_cell_length_b                   5.5643(2)
_cell_length_c                   22.8159(10)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      33.5160
_cell_measurement_theta_min      3.5970
_cell_volume                     1458.14(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4962
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
  1 omega   34.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8714  179.0000  -90.0000 75

  2 omega   -3.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8714   37.0000   60.0000 98

  3 omega -110.00  -56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8089 -179.0000 -180.0000 54

  4 omega  -95.00    6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8089  -57.0000   30.0000 101

  5 omega  -20.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8714   19.0000  -60.0000 121

  6 omega   -3.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8714   37.0000 -180.0000 78

  7 omega -110.00  -56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8089 -179.0000  -30.0000 54

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0569898000
_diffrn_orient_matrix_UB_12      -0.0078427000
_diffrn_orient_matrix_UB_13      -0.0172249000
_diffrn_orient_matrix_UB_21      -0.0119169000
_diffrn_orient_matrix_UB_22      0.1183569000
_diffrn_orient_matrix_UB_23      0.0087325000
_diffrn_orient_matrix_UB_31      0.0206387000
_diffrn_orient_matrix_UB_32      0.0466906000
_diffrn_orient_matrix_UB_33      -0.0250416000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26543
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.845
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4776
_reflns_number_total             5563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03685b2.cif
_cod_data_source_block           CaSDB_butane
_cod_depositor_comments
'Adding full bibliography for 1540441--1540447.cif.'
_cod_database_code               1540447
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              22839