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_4133680
_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         'C30 H34 N12 S'
_chemical_formula_sum            'C30 H34 N12 S'
_chemical_formula_weight         594.75
_chemical_name_common            P5
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-05
_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            32
_cell_length_a                   19.6681(12)
_cell_length_b                   34.306(2)
_cell_length_c                   42.246(2)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.83
_cell_measurement_theta_min      2.49
_cell_volume                     28505(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            59786
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.851
_diffrn_reflns_theta_max         20.851
_diffrn_reflns_theta_min         1.875
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             10048
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         3752
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.995
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.1386
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4079
_refine_ls_wR_factor_ref         0.4218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3138
_reflns_number_total             3752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05232_si_007.cif
_cod_data_source_block           af50m
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4133680
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2-N2
 1.01 with sigma of 0.02
 C22-C21
 1.34 with sigma of 0.02
 C26-C27
 1.54 with sigma of 0.02
 S1-C30
 1.82 with sigma of 0.02
 C25-C24
 1.54 with sigma of 0.02
 C23-C24
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C26 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.07
S1 \\sim C24 \\sim C25 \\sim C30: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C24: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
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
 Fixed Sof: H22A(0.5) H22B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C26(H26A,H26B), C28(H28A,H28B), C24(H24A,
 H24B), C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N9(H9), N10(H10), N11(H11), N12(H12), C3(H3), C4(H4), C6(H6),
 C7(H7), C9(H9A), C10(H10A), C12(H12A), C13(H13), C21(H21)
6.c X=CH2 refined with riding coordinates:
 C22(H22A,H22B)
6.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              88948
_shelx_hkl_checksum              73738
_olex2_submission_special_instructions 'No special instructions were received'