Coordination-Bond-Directed Synthesis of Hydrogen-bonded Organic Frameworks from Metal–Organic Frameworks as Templates
Su, Jian; Yuan, Shuai; Cheng, Yi-Xun; Yang, Zhi-Mei; Zuo, Jing-Lin; Chemical Science  (2021) –; doi:10.1039/D1SC03962H

data_1564902
_publ_section_title
;
 Coordination-Bond-Directed Synthesis of Hydrogen-bonded Organic
 Frameworks from Metal--Organic Frameworks as Templates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03962H
_journal_year                    2021
_chemical_formula_moiety         'C34 H20 O8 S4'
_chemical_formula_sum            'C34 H20 O8 S4'
_chemical_formula_weight         684.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-09-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-15 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.997(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.495(10)
_cell_length_b                   34.798(16)
_cell_length_c                   8.801(5)
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.34
_cell_volume                     6116(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART'
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.1337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21673
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.525
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5606
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1327 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.7521.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2902
_reflns_number_total             6285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03962h2.cif
_cod_data_source_block           TTFTB_HOF
_cod_database_code               1564902
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O4-H4A
 0.86 with sigma of 0.02
 H4A-C18
 1.81 with sigma of 0.02
 H4A-O3
 2.4 with sigma of 0.02
3. Rigid bond restraints
 O4, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C4(H4), C17(H17), C13(H13), C3(H3), C14(H14), C16(H16)
4.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'