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_1564900
_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
'0.5(C68 H36 Cu2 O16 S8), C3 H7 N O, 2(C H4.5 N0.5)'
_chemical_formula_sum            'C39 H34 Cu N2 O9 S4'
_chemical_formula_weight         866.51
_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
_atom_sites_solution_primary     dual
_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                 97.5830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1651(9)
_cell_length_b                   34.7043(16)
_cell_length_c                   8.8821(4)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.35
_cell_volume                     5855.9(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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25669
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.604
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_description       neddle-like
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6751
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1463P)^2^+7.6264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5393
_reflns_number_total             6751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03962h2.cif
_cod_data_source_block           CuI_TTFTB
_cod_database_code               1564900
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C21
 2.5 with sigma of 0.02
 C22-O5
 1.2 with sigma of 0.02
 N2-C23
 1.5 with sigma of 0.02
 C23-O5
 2.5 with sigma of 0.02
 C19-C20
 2.5 with sigma of 0.02
 N1-C19 = N1-C20 = N2_$1-C22_$1 = N2_$1-C21_$1
 1.5 with sigma of 0.02
 C20-H1B
 1.9 with sigma of 0.02
 C19-H1B
 1.9 with sigma of 0.02
 H1B-H1A
 1.5 with sigma of 0.02
 O3-H3
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim N2 \\sim C21 \\sim C22 \\sim C23: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N2 \\sim C21 \\sim C22 \\sim N1 \\sim C19 \\sim C20: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O5, N2, C21, C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C21, C22, N1, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: O5(0.5) N2(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5)
 H22(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) N1(0.5) H1A(0.5) C19(0.5)
 H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
6.a Riding coordinates:
 N1(H1A), C19(H19A,H19B,H19C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6), C7(H7), C13(H13), C14(H14), C16(H16), C17(H17),
 C22(H22)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'