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_4133678
_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         '0.25(C248 H271.99 N96)'
_chemical_formula_sum            'C62 H68 N24'
_chemical_formula_weight         1149.38
_chemical_name_common            'monomer 1'
_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
_audit_creation_date             2019-04-09
_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                   20.5062(13)
_cell_length_b                   35.210(2)
_cell_length_c                   42.652(4)
_cell_measurement_reflns_used    3005
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.987
_cell_measurement_theta_min      2.550
_cell_volume                     30796(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1858
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            58859
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1390 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.3923.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_description       block
_exptl_crystal_F_000             9728
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00031(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6754
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1656P)^2^+105.2766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2578
_refine_ls_wR_factor_ref         0.2713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5502
_reflns_number_total             6754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05232_si_002.cif
_cod_data_source_block           xuanfeng-monomer1_sq
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4133678
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26E,H26F} of C26B, {H25A,H25B} of C25, {H31C,H31D} of
  C31B, {H28A,H28B} of C28C, {H26C,H26D} of C26A, {H26A,H26B} of C26C, {H28C,
  H28D} of C28A, {H20A,H20B} of C20, {H22A,H22B} of C22, {H31A,H31B} of C31A,
  {H23A,H23B} of C23, All C(H,H,H,H) groups, All N(H) groups, All N(H,H,H)
  groups
 At 1.5 times of:
  {H28E,H28F} of C28B
2. Restrained distances
 C30B-C31B
 1.35 with sigma of 0.02
 C26C-C27C
 1.45 with sigma of 0.02
 C26C-C27A
 1.45 with sigma of 0.02
 C27A-C28A
 1.35 with sigma of 0.02
 C30A-C31B
 1.35 with sigma of 0.02
 C30A-C31A
 1.35 with sigma of 0.02
 C27C-C28C
 1.35 with sigma of 0.02
 C27C-C28A
 1.35 with sigma of 0.02
 C26C-C27B
 2.2 with sigma of 0.02
 N11-C27B
 2.35 with sigma of 0.02
 C27B-C28B
 1.33 with sigma of 0.02
 C28B-C26B
 2.35 with sigma of 0.02
 N11-C28B
 3.45 with sigma of 0.02
 C26B-C27B
 1.5 with sigma of 0.02
 N11-C26A
 1.43 with sigma of 0.02
 C26A-C27A
 1.5 with sigma of 0.02
 C28A-C26A
 2.35 with sigma of 0.02
 C26B-C26A
 2.4 with sigma of 0.02
3. Rigid bond restraints
 C30A, C30B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26B, C27B, C28B, C26C, C27C, C28C, C28A, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C27C \\sim C27A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C26C \\sim C27C \\sim C28C \\sim C28A \\sim C27A \\sim C26B \\sim C27B \\sim
C28B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C27B \\sim C28B \\sim C26B \\sim C26C \\sim C27C \\sim C28C \\sim C28A \\sim
C27A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C26A \\sim C27C \\sim C27A \\sim C28A \\sim C28C \\sim C27B \\sim C26B \\sim
C28B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C28B) \\sim Ueq, Uanis(C27B) \\sim Ueq, Uanis(C26C) \\sim Ueq,
Uanis(C27C) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C28C) \\sim Ueq,
Uanis(C28A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31A) \\sim Ueq, Uanis(C31B) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C30B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30A) = Uanis(C30B)
Uanis(C27C) = Uanis(C27A)
Uanis(C28A) = Uanis(C28C) = Uanis(C27A) = Uanis(C27C)
Uanis(C27A) = Uanis(C27C)
Uanis(C27C) = Uanis(C27A) = Uanis(C28C) = Uanis(C28A)
Uanis(C31A) = Uanis(C31B)
Uanis(C31B) = Uanis(C31A)
Uanis(C28A) = Uanis(C28C)
Uanis(C27C) = Uanis(C27A) = Uanis(C27B)
Uanis(C28B) = Uanis(C28A) = Uanis(C28C)
Uanis(C26A) = Uanis(C26B) = Uanis(C26C)
5. Others
 1*[Sof(H11)+Sof(C26C)+Sof(H26A)+Sof(H26B)+Sof(C27C)+Sof(H27C)+Sof(C28C)+
 Sof(H28A)+Sof(H28B)]+1*[Sof(H11A)+Sof(C26A)+Sof(H26C)+Sof(H26D)+Sof(C27A)+
 Sof(H27A)+Sof(C28A)+Sof(H28C)+Sof(H28D)]+1*[Sof(H11B)+Sof(C26B)+Sof(H26E)+
 Sof(H26F)+Sof(C27B)+Sof(H27B)+Sof(C28B)+Sof(H28E)+Sof(H28F)]=1 with esd of
 0.001
 Sof(H11)=Sof(C26C)=Sof(H26A)=Sof(H26B)=Sof(C27C)=Sof(H27C)=Sof(C28C)=
 Sof(H28A)=Sof(H28B)=FVAR(1)
 Sof(H11A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27A)=Sof(C28A)=
 Sof(H28C)=Sof(H28D)=FVAR(2)
 Sof(H11B)=Sof(C26B)=Sof(H26E)=Sof(H26F)=Sof(C27B)=Sof(H27B)=Sof(C28B)=
 Sof(H28E)=Sof(H28F)=FVAR(3)
 Fixed Sof: H29A(0.5) H29B(0.5) H29C(0.5) H29D(0.5) C30A(0.5) H30A(0.5)
 C31A(0.5) H31A(0.5) H31B(0.5) C31B(0.5) H31C(0.5) H31D(0.5) C30B(0.5) H30B(0.5)
6.a Riding coordinates:
 C27B(H27B), C28B(H28E,H28F)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C29(H29A,H29B), C29(H29C,H29D), C20(H20A,H20B), C26C(H26A,
 H26B), C26A(H26C,H26D), C26B(H26E,H26F)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C3(H3), C4(H4), C6(H6), C7(H7),
 C30A(H30A), C21(H21), N10(H10A), N12(H12A), N2(H2), N1(H1), N11(H11),
 N11(H11A), N11(H11B), N9(H9A), C30B(H30B), C24(H24), C27C(H27C), C27A(H27A)
6.d X=CH2 refined with riding coordinates:
 C31A(H31A,H31B), C22(H22A,H22B), C31B(H31C,H31D), C25(H25A,H25B), C28C(H28A,
 H28B), C28A(H28C,H28D)
;
_shelx_res_checksum              98478
_shelx_hkl_checksum              28598
_shelx_fab_checksum              80920
_olex2_submission_special_instructions 'No special instructions were received'