Stepwise construction of coordinative linkages and dynamic covalent linkages for a porous metal-organic framework.
Peng, Shuyin; Sun, Yuqian; Li, Qingqing; Jiang, Zhongwen; Rao, Yin; Wu, Yichen; Li, Qiaowei; Chemical communications (Cambridge, England) 60 (2024) 1488–1491; doi:10.1039/d3cc05650c

data_7132593
_publ_section_title
;
 Stepwise construction of coordinative linkages and dynamic covalent
 linkages for a porous metal-organic framework.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1488
_journal_page_last               1491
_journal_paper_doi               10.1039/d3cc05650c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C12 H9 Ag3 N6 O3'
_chemical_formula_sum            'C12 H9 Ag3 N6 O3'
_chemical_formula_weight         608.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-14 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   45.975(3)
_cell_length_b                   37.787(3)
_cell_length_c                   3.7540(3)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      52.39
_cell_measurement_theta_min      4.40
_cell_volume                     6521.7(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            24166
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        52.377
_diffrn_reflns_theta_max         52.377
_diffrn_reflns_theta_min         3.916
_diffrn_source_current           2.86
_diffrn_source_power             0.19994259999999997
_diffrn_source_voltage           69.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.676
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.3975
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1579 before and 0.0858 after correction.
The Ratio of minimum to maximum transmission is 0.5298.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_description       block
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.868
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.214
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2751
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0573P)^2^+144.0138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.677
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                2544
_reflns_number_total             2751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05650c2.cif
_cod_data_source_block           Ag3(PyCA)3
_cod_depositor_comments
;
          Adding full bibliography for 7132593.cif.

2025-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H72 Ag24 N48 O24'
_cod_original_formula_weight         4870.89
_cod_original_formula_moiety         '8(C12 H9 Ag3 N6 O3)'
_cod_original_formula_units_Z            2
_cod_database_code               7132593
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.244
_shelx_estimated_absorpt_t_min   0.201
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(4)
 0.06(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C1-C2
 1.43 with sigma of 0.01
 C2-C1
 1.43 with sigma of 0.005
 C6-C5
 1.43 with sigma of 0.005
 C10-C9
 1.43 with sigma of 0.005
4. Rigid bond restraints
 C1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C8(H8), C4(H4), C5(H5), C11(H11), C12(H12), C9(H9), C3(H3)
;
_shelx_res_checksum              27831
_shelx_hkl_checksum              32929
_olex2_submission_special_instructions 'No special instructions were received'