An Elastic Hydrogen-Bonded Cross-Linked Organic Framework for Effective Iodine Capture in Water.
Lin, Yunxiao; Jiang, Xuanfeng; Kim, Samuel T.; Alahakoon, Sampath B.; Hou, Xisen; Zhang, Zhiyun; Thompson, Christina M.; Smaldone, Ronald A.; Ke, Chenfeng; Journal of the American Chemical Society 139 (2017) 7172–7175; doi:10.1021/jacs.7b03204

data_4126046
_publ_section_title
;
 An Elastic Hydrogen-Bonded Cross-Linked Organic Framework for Effective
 Iodine Capture in Water.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7172
_journal_page_last               7175
_journal_paper_doi               10.1021/jacs.7b03204
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '2(C4 H8 O2), C62 H52 N24'
_chemical_formula_sum            'C70 H68 N24 O4'
_chemical_formula_weight         1309.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.517(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.945(2)
_cell_length_b                   26.364(5)
_cell_length_c                   15.094(3)
_cell_measurement_reflns_used    4631
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.18
_cell_volume                     4701.0(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4466
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.483
_diffrn_reflns_theta_min         1.364
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0508 before and 0.0381 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0568 before and 0.0427 after correction.
 The Ratio of minimum to maximum transmission is 0.90.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 23893 reflections, Rint = 0.0450
 (6752 with I > 3sig(I), Rint = 0.0241)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.1103
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3367
_refine_ls_wR_factor_ref         0.3706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2333
_reflns_number_total             4465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03204_si_002.cif
_cod_data_source_block           ck516at
_cod_depositor_comments          'Adding full bibliography for 4126046.cif.'
_cod_original_cell_volume        4700.9(14)
_cod_database_code               4126046
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 C14-C15 = C14A-C15A
 0.01 with sigma of 1.22
 C15-C16 = C15A-C16A
 0.01 with sigma of 1.12
3. Same fragment restrains
{C11, C12, C13} sigma for 1-2: 0.01, 1-3: 0.03
as
{C14, C15, C16}
{C11, C12, C13} sigma for 1-2: 0.01, 1-3: 0.03
as
{C14A, C15A, C16A}
4. Others
 Fixed Sof: H6A(0.5) H6B(0.5) C3(0.5) H3(0.5) C3A(0.5) H3A(0.5) C4(0.5)
 H4(0.5) C4A(0.5) H4A(0.5) C6(0.5) H6(0.5) C6A(0.5) H6AA(0.5) C7(0.5) H7(0.5)
 C7A(0.5) H7A(0.5) C14(0.6) H14A(0.6) H14B(0.6) C15(0.6) C16(0.6) H16(0.6)
 C14A(0.4) H14C(0.4) H14D(0.4) C15A(0.4) C16A(0.4) H16A(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C11(H11A,H11B), C14(H14A,H14B), C14A(H14C,H14D)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N5(H5), N6(H6A), N6(H6B), C3(H3), C3A(H3A), C4(H4), C4A(H4A), C6(H6),
 C6A(H6AA), C7(H7), C7A(H7A)
5.c :
 C13(H13), C16(H16), C16A(H16A)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'