Microporous Metal-Organic Framework with a Completely Reversed Adsorption Relationship for C<sub>2</sub> Hydrocarbons at Room Temperature.
Sun, Fang-Zhou; Yang, Shan-Qing; Krishna, Rajamani; Zhang, Ying-Hui; Xia, Yu-Pei; Hu, Tong-Liang; ACS applied materials & interfaces  (2020) –; doi:10.1021/acsami.9b22410

data_4517321
_publ_section_title
;
 Microporous Metal-Organic Framework with a Completely Reversed Adsorption
 Relationship for C<sub>2</sub> Hydrocarbons at Room Temperature.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.9b22410
_journal_year                    2020
_chemical_formula_moiety         'C33 H25 Mn2 N O10, C3 H7 N O, C2 H3 N'
_chemical_formula_sum            'C38 H35 Mn2 N3 O11'
_chemical_formula_weight         819.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.62120(10)
_cell_length_b                   13.0997(2)
_cell_length_c                   25.0298(3)
_cell_measurement_reflns_used    12388
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8630
_cell_measurement_theta_min      5.1260
_cell_volume                     3780.71(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -29.00  87.00   0.50    0.50    --    0.00  57.00 -60.00  232
  2  \w    -81.00 -56.00   0.50    0.50    --    0.00 -57.00  60.00   50
  3  \w     13.00  38.00   0.50    0.50    --    0.00  57.00-150.00   50
  4  \w    -47.00  22.00   0.50    0.50    --    0.00 -57.00  60.00  138
  5  \w     11.00 121.00   0.50    0.50    --   95.80 -61.00  60.00  220
  6  \w      6.00 123.00   0.50    0.50    --   95.80 -82.00 -90.00  234
  7  \w    138.00 184.00   0.50    0.50    --   95.80  45.00  60.00   92
  8  \w     71.00 131.00   0.50    0.50    --   95.80  45.00  60.00  120
  9  \w     18.00 120.00   0.50    0.50    --   95.80 -61.00 -90.00  204
 10  \w     45.00 171.00   0.50    0.50    --   95.80   0.00-150.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0918498000
_diffrn_orient_matrix_UB_12      -0.0838625000
_diffrn_orient_matrix_UB_13      0.0028880000
_diffrn_orient_matrix_UB_21      -0.0718745000
_diffrn_orient_matrix_UB_22      0.0733372000
_diffrn_orient_matrix_UB_23      0.0307010000
_diffrn_orient_matrix_UB_31      -0.0651269000
_diffrn_orient_matrix_UB_32      0.0375345000
_diffrn_orient_matrix_UB_33      -0.0538686000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21634
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.497
_diffrn_reflns_theta_min         3.559
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.978
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       stick
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0717P)^2^+5.0409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6803
_reflns_number_total             7496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b22410_si_002.cif
_cod_data_source_block           NUM-7
_cod_database_code               4517321
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011),
 C014(H014), C015(H015), C016(H016), C017(H017), C01A(H01A), C01D(H01H)
2.c Idealised Me refined as rotating group:
 C01B(H01O,H01P,H01Q), C01C(H01B,H01C,H01D), C01E(H01E,H01F,H01G), C01H(H01I,
 H01J,H01K), C01I(H01L,H01M,H01N)
;
_shelx_res_checksum              49949
_shelx_hkl_checksum              70223
_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 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.739