Topochemical Synthesis of Single-Crystalline Hydrogen-Bonded Cross-Linked Organic Frameworks and Their Guest-Induced Elastic Expansion.
Jiang, Xuanfeng; Cui, Xunzhe; Duncan, Andrew J. E.; Li, Liang; Hughes, Russell P.; Staples, Richard J.; Alexandrov, Eugeny V.; Proserpio, Davide M.; Wu, Yuyang; Ke, Chenfeng; Journal of the American Chemical Society 141 (2019) 10915–10923; doi:10.1021/jacs.9b05232

data_4133679
_publ_section_title
;
 Topochemical Synthesis of Single-Crystalline Hydrogen-Bonded Cross-Linked
 Organic Frameworks and Their Guest-Induced Elastic Expansion.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10915
_journal_page_last               10923
_journal_paper_doi               10.1021/jacs.9b05232
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C58 H68 N24'
_chemical_formula_sum            'C58 H68 N24'
_chemical_formula_weight         1101.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   20.6068(5)
_cell_length_b                   35.0090(10)
_cell_length_c                   42.3618(10)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.31
_cell_measurement_theta_min      2.70
_cell_volume                     30560.8(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      150.0
_diffrn_detector_type            'pixel array detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            43203
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.075
_diffrn_reflns_theta_min         2.698
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0851 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.9037.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_description       block
_exptl_crystal_F_000             9344
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.002
_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          0.3052
_refine_ls_wR_factor_ref         0.3365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5154
_reflns_number_total             7822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05232_si_003.cif
_cod_data_source_block           sad_sq
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4133679
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-C21
 1.503 with sigma of 0.01
 C22-C21
 1.299 with sigma of 0.01
 C26A-C27A
 1.53 with sigma of 0.01
 N12-H12
 0.91 with sigma of 0.02
 C27B-C26B
 1.53 with sigma of 0.01
 C25A-C24A = C25B-C24B
 1.299 with sigma of 0.01
 C23-C24A
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C23 \\sim C24A \\sim C25A \\sim C24B \\sim C25B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
N11 \\sim C26B \\sim C27B \\sim C26A \\sim C27A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25C)=Sof(H25D)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(H25B)=FVAR(1)
 Sof(H11A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=1-FVAR(2)
 Sof(H11)=Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C27B)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C23(H23C,H23D), C28(H28A,H28B), C26B(H26A,
 H26B), C26A(H26C,H26D)
6.b Me refined with riding coordinates:
 C27B(H27A,H27B,H27C), C27A(H27D,H27E,H27F)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N9(H9), N10(H10), N11(H11), N11(H11A), C3(H3), C4(H4), C6(H6),
  C7(H7), C9(H9A), C10(H10A), C12(H12A), C13(H13), C21(H21), C24A(H24A),
 C24B(H24B)
6.d X=CH2 refined with riding coordinates:
 C22(H22A,H22B), C25A(H25A,H25B), C25B(H25C,H25D)
6.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              22328
_shelx_hkl_checksum              54774
_shelx_fab_checksum              14040
_olex2_submission_special_instructions 'No special instructions were received'