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_4133677
_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 H25 N12'
_chemical_formula_sum            'C30 H25 N12'
_chemical_formula_weight         553.58
_chemical_name_common            HCOF-4
_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                   20.8296(2)
_cell_length_b                   35.3105(3)
_cell_length_c                   42.4936(2)
_cell_measurement_reflns_used    45753
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.4240
_cell_measurement_theta_min      1.5510
_cell_volume                     31254.2(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61992
_diffrn_reflns_av_R_equivalents  0.2481
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            96529
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        21.836
_diffrn_reflns_theta_max         22.498
_diffrn_reflns_theta_min         1.598
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35451
_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    0.941
_exptl_crystal_description       block
_exptl_crystal_F_000             9247
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7684
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      2.015
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.1761
_refine_ls_shift/su_max          0.247
_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          0.4285
_refine_ls_wR_factor_ref         0.4405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6692
_reflns_number_total             7684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05232_si_006.cif
_cod_data_source_block           9ck
_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               4133677
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.998
_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 C(H,H,H,H,H,
  H) groups, All N(H) groups
2. Restrained distances
 C39-C6AA
 1.54 with sigma of 0.02
 C4-C39
 1.54 with sigma of 0.02
 C00X-C2 \\sim C00X-C1AA \\sim C00X-C3AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C39 \\sim C6AA: 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(H00F)+Sof(H00I)+Sof(C1AA)]+1*[Sof(H00D)+Sof(H00E)+Sof(C2)]+1*
 [Sof(H00J)+Sof(H00L)+Sof(C3AA)]=1 with esd of 0.01
 Sof(H1BC)=Sof(H1BD)=Sof(C3)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C0AA)=FVAR(1)
 Sof(H00F)=Sof(H00I)=Sof(C1AA)=FVAR(2)
 Sof(H00D)=Sof(H00E)=Sof(C2)=FVAR(3)
 Sof(H00J)=Sof(H00L)=Sof(C3AA)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00C), C00X(H00F,H00I), C00X(H00D,H00E), C00X(H00J,H00L), C00Y(H00P,
 H00Q), C1(H1AA,H1AB), C1(H1BC,H1BD)
6.b Aromatic/amide H refined with riding coordinates:
 N001(H001), N00B(H00B), C00G(H00G), C00H(H00H), N00K(H00K), C00M(H00M),
 N00N(H00N), C00O(H00O), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00Z(H00Z)
6.c X=CH2 refined with riding coordinates:
 C010(H01A,H01B)
;
_shelx_res_checksum              37725
_shelx_hkl_checksum              20603
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.831
_oxdiff_exptl_absorpt_empirical_full_min 0.348