Separation of C2/C1 hydrocarbons through gate-opening effect in a microporous metal‒organic framework
Lin, Rong-Guang; Li, Libo; Lin, Rui-Biao; Arman, Hadi; Chen, Banglin; CrystEngComm  (2017) –; doi:10.1039/C7CE01766A

data_7229462
_publ_section_title
;
 Separation of C2/C1 hydrocarbons through gate-opening effect in a
 microporous metal--organic framework
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01766A
_journal_year                    2017
_chemical_formula_moiety         'C12 H8 Mn N2 O4, C H4 O'
_chemical_formula_sum            'C13 H12 Mn N2 O5'
_chemical_formula_weight         331.19
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-07-14 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.700(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0292(3)
_cell_length_b                   13.5724(3)
_cell_length_c                   10.3629(4)
_cell_measurement_reflns_used    7694
_cell_measurement_temperature    98
_cell_measurement_theta_max      40.4640
_cell_measurement_theta_min      2.1050
_cell_volume                     1364.43(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      98.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -68.00  55.00   0.50   30.00    --  -35.00  70.00  90.00  246
  2  \w    -68.00  31.00   0.50   30.00    --  -35.00  70.00 270.00  198
  3  \w    -72.00 -34.00   0.50   30.00    --  -35.00   0.00  90.00   76
  4  \w    -56.00 -20.00   0.50   30.00    --  -35.00  70.00   0.00   72
  5  \w   -125.00 -91.00   0.50   30.00    --  -35.00   0.00 180.00   68
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724 (2x2 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0073163000
_diffrn_orient_matrix_UB_12      -0.0486174000
_diffrn_orient_matrix_UB_13      0.0259690000
_diffrn_orient_matrix_UB_21      -0.0354470000
_diffrn_orient_matrix_UB_22      -0.0186075000
_diffrn_orient_matrix_UB_23      -0.0633825000
_diffrn_orient_matrix_UB_31      0.0635028000
_diffrn_orient_matrix_UB_32      -0.0047851000
_diffrn_orient_matrix_UB_33      -0.0177348000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8858
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2455
_reflns_number_total             2678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01766a2.cif
_cod_data_source_block           cd1570
_cod_database_code               7229462
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Mn1 C12 H10 N2'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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,H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O5A(0.5) H5A(0.5) O5B(0.5) H5B(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 H13D(0.5) H13E(0.5) H13F(0.5)
3.a Riding coordinates:
 O5A(H5A), O5B(H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C13(H13D,H13E,H13F)
;
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.886