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_4133673
_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         'C34 H25 N12 S2'
_chemical_formula_sum            'C34 H25 N12 S2'
_chemical_formula_weight         665.78
_chemical_name_common            HCOF-3
_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             2019-04-08
_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                   20.2514(2)
_cell_length_b                   35.0504(2)
_cell_length_c                   42.5407(2)
_cell_measurement_reflns_used    49222
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.4250
_cell_measurement_theta_min      1.5990
_cell_volume                     30196.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.36a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.36a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.36a (Rigaku OD, 2017)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f      0.00 360.00   0.20    0.10   0.00   0.00   0.00    --  1800
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137907000
_diffrn_orient_matrix_UB_12      0.0023623000
_diffrn_orient_matrix_UB_13      -0.0128591000
_diffrn_orient_matrix_UB_21      -0.0264970000
_diffrn_orient_matrix_UB_22      0.0054291000
_diffrn_orient_matrix_UB_23      -0.0057714000
_diffrn_orient_matrix_UB_31      0.0066632000
_diffrn_orient_matrix_UB_32      0.0166693000
_diffrn_orient_matrix_UB_33      0.0037016000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61992
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            118202
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        21.836
_diffrn_reflns_theta_max         23.999
_diffrn_reflns_theta_min         1.611
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.36a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             11040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.248
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8915
_refine_ls_number_restraints     470
_refine_ls_restrained_S_all      2.275
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.1676
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_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          0.4469
_refine_ls_wR_factor_ref         0.4597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7615
_reflns_number_total             8915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05232_si_005.cif
_cod_data_source_block           10ck
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4133673
_shelx_shelxl_version_number     2018/3
_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
2. Restrained distances
 N2-H2
 0.99 with sigma of 0.02
 H12-N12
 1.01 with sigma of 0.02
 C24B-C25B
 1.54 with sigma of 0.02
 S2B-C25B
 1.82 with sigma of 0.02
 C32B-C32A
 1.54 with sigma of 0.02
 C28-C27
 1.54 with sigma of 0.02
 S1-C28
 1.82 with sigma of 0.02
 C33-S1
 1.82 with sigma of 0.02
 S1-C33
 1.82 with sigma of 0.02
 C33_$2-C34
 1.54 with sigma of 0.02
 C27-C26
 1.54 with sigma of 0.02
 C29-C30
 1.54 with sigma of 0.02
 C30_$3-C31_$3
 1.54 with sigma of 0.02
 C30_$4-C31_$4
 1.54 with sigma of 0.02
 C30-C31
 1.54 with sigma of 0.02
 S2A-C25A
 1.82 with sigma of 0.02
 S2A-C32B
 1.82 with sigma of 0.02
 S2B-C24B
 2.74 with sigma of 0.04
 C32B-C32B_$1
 2.5 with sigma of 0.04
 C27-S1
 2.74 with sigma of 0.04
 S1_$2-C34
 2.74 with sigma of 0.04
 C28-C33
 2.96 with sigma of 0.04
 C33_$2-C33
 2.5 with sigma of 0.04
 C28-C26
 2.5 with sigma of 0.04
 C31_$3-C29_$3
 2.51 with sigma of 0.04
 C31-C29
 2.51 with sigma of 0.04
 C24A-S2A
 2.74 with sigma of 0.04
 C32B-C25A
 2.96 with sigma of 0.04
 H2-C11 \\sim H2-C17
 with sigma of 0.02
 C20-H9 \\sim H9-C16
 with sigma of 0.02
 C14-H1 \\sim C5-H1
 with sigma of 0.02
 C25B-C24B \\sim C24B-C23
 with sigma of 0.02
 C28-S1 \\sim S1-C33
 with sigma of 0.02
 C26-C27 \\sim C27-C28
 with sigma of 0.02
 C19-H12 \\sim H12-C29
 with sigma of 0.02
 C25A-C24A \\sim C24A-C23
 with sigma of 0.02
 S2A-C25A \\sim S2B-C25B
 with sigma of 0.02
 C25B-S2B \\sim C25A-S2A
 with sigma of 0.02
 S2A-C32B \\sim C32B-S2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24B \\sim C25B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C24B \\sim C24A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C32B \\sim S2B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C32A \\sim C32B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C27 \\sim C28: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1 \\sim C33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C33 \\sim C34: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C27 \\sim C26: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S2B \\sim S2A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C25B \\sim C25A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C32B \\sim S2A: 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
 Sof(H23C)=Sof(H23D)=Sof(S2A)=Sof(C24A)=Sof(C25A)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(S2B)=Sof(C24B)=Sof(C25B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C23(H23C,H23D), C29(H29A,H29B), C26(H26A,H26B)
6.b Aromatic/amide H refined with riding coordinates:
 N9(H9), N10(H10), N11(H11), 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)
;
_shelx_res_checksum              23326
_shelx_hkl_checksum              47767
_olex2_submission_special_instructions 'No special instructions were received'