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_4133674
_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         'C29 H27 N12 S1'
_chemical_formula_sum            'C29 H27 N12 S'
_chemical_formula_weight         575.68
_chemical_name_common            P7
_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             2019-04-15
_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                   20.1440(3)
_cell_length_b                   34.7052(4)
_cell_length_c                   42.3035(3)
_cell_measurement_reflns_used    26405
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.4140
_cell_measurement_theta_min      1.6160
_cell_volume                     29574.4(6)
_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_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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      0.0301960000
_diffrn_orient_matrix_UB_12      0.0009096000
_diffrn_orient_matrix_UB_13      -0.0027378000
_diffrn_orient_matrix_UB_21      -0.0047407000
_diffrn_orient_matrix_UB_22      -0.0067873000
_diffrn_orient_matrix_UB_23      -0.0133705000
_diffrn_orient_matrix_UB_31      -0.0036722000
_diffrn_orient_matrix_UB_32      0.0164965000
_diffrn_orient_matrix_UB_33      -0.0053227000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61992
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            120127
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        21.836
_diffrn_reflns_theta_max         24.408
_diffrn_reflns_theta_min         1.620
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50443
_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    1.034
_exptl_crystal_description       block
_exptl_crystal_F_000             9632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.733
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9150
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.736
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.1365
_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          0.4046
_refine_ls_wR_factor_ref         0.4231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6742
_reflns_number_total             9150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05232_si_009.cif
_cod_data_source_block           17ck
_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               4133674
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.990
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C28
 1.54 with sigma of 0.02
 C20-C21
 1.54 with sigma of 0.02
 C22-C21
 1.34 with sigma of 0.02
 S1B-C25
 1.82 with sigma of 0.02
 C26-C27
 1.54 with sigma of 0.02
 C24A-C25
 1.54 with sigma of 0.02
 S1B-C24A
 2.96 with sigma of 0.04
 C25-S1B \\sim C25-S1A \\sim C25-S1C
 with sigma of 0.02
 C24A-C23 \\sim C23-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C26: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C25: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1B \\sim S1C: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1B \\sim S1C \\sim S1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
S1B \\sim S1C \\sim C25 \\sim S1A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C27: 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
C24 \\sim C23: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C24A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C24A \\sim 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
 1*[Sof(S1B)]+1*[Sof(S1C)]+1*[Sof(S1A)]=1 with esd of 0.01
 Sof(H23C)=Sof(H23D)=Sof(C24A)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C28(H28A,H28B), C23(H23A,H23B), C23(H23C,H23D), C26(H26A,H26B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N9(H9), C4(H4), C7(H7), C6(H6), C3(H3), N10(H10), N11(H11), C9(H9A),
 C13(H13), C12(H12), C10(H10A), C21(H21)
6.c X=CH2 refined with riding coordinates:
 C22(H22A,H22B)
6.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              26869
_shelx_hkl_checksum              7609
_olex2_submission_special_instructions 'No special instructions were received'