A microporous six-fold interpenetrated hydrogen-bonded organic framework for highly selective separation of C2H4/C2H6
Peng Li; Yabing He; Hadi D. Arman; Rajamani Krishna; Hailong Wang; Linhong Weng; Banglin Chen; Chem.Commun. 50 (2014) 13081–; doi:10.1039/C4cc05506C

data_7115824
_publ_section_title
;
 A microporous six-fold interpenetrated hydrogen-bonded organic framework
 for highly selective separation of C2H4/C2H6
;
_journal_name_full               Chem.Commun.
_journal_page_first              13081
_journal_paper_doi               10.1039/C4cc05506C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C61 H48 N20'
_chemical_formula_sum            'C61 H48 N20'
_chemical_formula_weight         1061.19
_chemical_name_systematic        HOF-4
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.606(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.212(6)
_cell_length_b                   7.275(2)
_cell_length_c                   26.666(8)
_cell_measurement_reflns_used    13649
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.3
_cell_volume                     3921(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20646
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1108
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+7.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2139
_reflns_number_gt                4534
_reflns_number_total             6927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05506c2.cif
_cod_data_source_block           HOF-4
_cod_database_code               7115824
_olex2_refinement_description
;
1. Others
 Fixed U12: C1(0)
 Fixed U23: C1(0)
 Fixed Uiso: H3(0.054) H4(0.066) H6(0.053) H7(0.053) H9(0.103) H10(0.113)
 H12(0.086) H13(0.075) H18(0.05) H19(0.052) H21(0.054) H22(0.054) H24(0.072)
 H25(0.074) H27(0.06) H28(0.06) H4A(0.12) H4B(0.12) H5A(0.17) H5B(0.17)
 H9A(0.084) H9B(0.084) H10A(0.067) H10B(0.067)
 Fixed X: C1(0.25) H3(0.3198) H4(0.4045) H6(0.3954) H7(0.3105) H9(0.5135)
 H10(0.5977) H12(0.5269) H13(0.4409) H18(0.1902) H19(0.2228) H21(0.3976)
 H22(0.364) H24(0.2507) H25(0.2856) H27(0.4716) H28(0.4362) H4A(0.8026)
 H4B(0.765) H5A(0.7372) H5B(0.6745) H9A(0.3658) H9B(0.319) H10A(0.5415)
 H10B(0.5538)
 Fixed Y: H3(1.0873) H4(1.2766) H6(1.5374) H7(1.3462) H9(1.3602) H10(1.5434)
 H12(1.9563) H13(1.7783) H18(0.7863) H19(0.5602) H21(0.8172) H22(1.0404)
 H24(0.4171) H25(0.1546) H27(0.2629) H28(0.5263) H4A(1.8881) H4B(1.7121)
 H5A(2.3574) H5B(2.3425) H9A(-0.3804) H9B(-0.2231) H10A(-0.4182) H10B(-0.2664)
 Fixed Z: C1(0.75) H3(0.8389) H4(0.864) H6(0.7312) H7(0.7069) H9(0.8568)
 H10(0.8864) H12(0.8048) H13(0.7807) H18(0.7067) H19(0.6526) H21(0.6383)
 H22(0.693) H24(0.5845) H25(0.5431) H27(0.5856) H28(0.6254) H4A(0.9517)
 H4B(0.9497) H5A(0.8537) H5B(0.8241) H9A(0.4246) H9B(0.4285) H10A(0.5334)
 H10B(0.5698)
;