An in situ approach to functionalize metal-organic frameworks with tertiary aliphatic amino groups.
Xi, Fu-Gui; Sun, Wei; Dong, Zhi-Yun; Yang, Ning-Ning; Gong, Teng; Gao, En-Qing; Chemical communications (Cambridge, England) 56 (2020) 13177–13180; doi:10.1039/d0cc05568a

data_7127332
_publ_section_title
;
 An in situ approach to functionalize metal-organic frameworks with
 tertiary aliphatic amino groups.
;
_journal_issue                   86
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13177
_journal_page_last               13180
_journal_paper_doi               10.1039/d0cc05568a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C54 H54 N4 O15 Zn4'
_chemical_formula_weight         1260.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 101.016(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3686(14)
_cell_length_b                   25.4298(15)
_cell_length_c                   17.1469(13)
_cell_measurement_reflns_used    3754
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.361
_cell_measurement_theta_min      2.401
_cell_volume                     9573.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1636
_diffrn_reflns_av_unetI/netI     0.1137
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60285
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.005
_diffrn_reflns_theta_min         1.593
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.874
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_platon_squeeze_details
;
TITL 1 in P-1                    New: C2/m
CELL   22.3686   25.4298   17.1469     90.00    101.02     90.00
SPGR C2/m
C101 0.500 0.500 0.500 !       2.78 eA-3
C102 0.507 0.503 0.437 !       2.14 eA-3
C103 0.486 0.392 0.492 !       1.54 eA-3
C104 0.500 0.383 0.002 !       1.38 eA-3
C105 0.500 0.422 0.499 !       1.34 eA-3
C106 0.014 0.065 0.468 !       1.18 eA-3
C107 0.470 0.163 0.061 !       1.14 eA-3
Q108 0.022 0.503 0.734 !       1.14 eA-3
C109 0.431 0.144 0.090 !       1.14 eA-3
C110 0.515 0.172 0.222 !       1.11 eA-3
Q111 0.061 0.503 0.750 !       1.10 eA-3
C112 0.929 0.371 0.030 !       1.10 eA-3
Q113 0.654 0.063 0.939 !       1.09 eA-3
C114 0.070 0.498 0.859 !       1.07 eA-3
C115 0.187 0.178 0.050 !       1.06 eA-3
C116 0.405 0.268 0.756 !       1.04 eA-3
Q117 0.893 0.350 0.031 !       1.03 eA-3
C118 0.712 0.351 0.028 !       1.03 eA-3
C119 0.035 0.134 0.033 !       1.02 eA-3
C120 0.538 0.136 0.933 !       1.02 eA-3
C121 0.126 0.151 0.079 !       1.01 eA-3
C122 0.902 0.502 0.078 !       1.00 eA-3
Q123 0.085 0.039 0.179 !       1.00 eA-3
Q124 0.343 0.091 0.063 !       0.98 eA-3
C125 0.991 0.483 0.789 !       0.98 eA-3
C126 0.336 0.320 0.932 !       0.98 eA-3
Q127 0.057 0.351 0.861 !       0.98 eA-3
Q128 0.015 0.355 0.264 !       0.97 eA-3
C129 0.037 0.357-0.001 !       0.97 eA-3
C130 0.929 0.263 0.768 !       0.97 eA-3
C131 0.435 0.161 0.027 !       0.96 eA-3
Q132 0.918 0.505 0.172 !       0.94 eA-3
C133 0.827 0.137 0.976 !       0.94 eA-3
Q134 0.907 0.432 0.175 !       0.94 eA-3
C135 0.078 0.148 0.053 !       0.93 eA-3
Q136 0.482 0.139 0.220 !       0.93 eA-3
Q137 0.902 0.466 0.158 !       0.92 eA-3
C138 0.456 0.197 0.819 !       0.91 eA-3
C139 0.562 0.257 0.022 !       0.91 eA-3
Q140 0.462 0.027 0.203 !       0.91 eA-3
C141 0.399 0.323 0.935 !       0.90 eA-3
Q142 0.022 0.469 0.267 !       0.90 eA-3
C143 0.006 0.359 0.036 !       0.90 eA-3
C144 0.016 0.361 0.154 !       0.90 eA-3
C145 0.586 0.300 0.109 !       0.89 eA-3
C146 0.429 0.258 0.813 !       0.89 eA-3
Q147 0.054 0.142-0.003 !       0.89 eA-3
C148 0.494 0.279 0.957 !       0.89 eA-3
Q149 0.016 0.464 0.360 !       0.88 eA-3
Q150 0.486 0.102 0.876 !       0.88 eA-3
C151 0.491 0.142 0.119 !       0.88 eA-3
C152 0.907 0.503 0.625 !       0.88 eA-3
Q153 1.002 0.424 0.266 !       0.88 eA-3
Q154 0.924 0.359-0.005 !       0.87 eA-3
C155 0.055 0.295 0.233 !       0.87 eA-3
Q156 0.587 0.304 0.269 !       0.87 eA-3
C157 0.501 0.173 0.970 !       0.86 eA-3
Q158 0.603 0.334 0.500 !       0.86 eA-3
C159 1.000 0.391 0.001 !       0.85 eA-3
Q160 0.157 0.444 0.355 !       0.85 eA-3
Q161 0.482 0.102 0.187 !       0.85 eA-3
C162 0.908 0.216 0.943 !       0.84 eA-3
Q163 0.053 0.501 0.000 !       0.84 eA-3
Q164 0.571 0.257 0.951 !       0.84 eA-3
C165 0.484 0.132 0.780 !       0.84 eA-3
C166 0.562 0.226 0.189 !       0.84 eA-3
C167 0.464 0.090 0.095 !       0.84 eA-3
C168 0.086 0.267 0.989 !       0.84 eA-3
Q169 0.886 0.436 0.115 !       0.83 eA-3
Q170 0.056 0.472 0.344 !       0.83 eA-3
C171 0.057 0.504 0.890 !       0.82 eA-3
C172 0.982 0.382 0.076 !       0.82 eA-3
C173 0.500 0.273 0.002 !       0.82 eA-3
Q174 0.114 0.335 0.937 !       0.81 eA-3
C175 0.047 0.504 0.953 !       0.81 eA-3
C176 0.382 0.314 0.987 !       0.81 eA-3
Q177 0.860 0.500 0.109 !       0.81 eA-3
C178 0.117 0.133 0.030 !       0.80 eA-3
C179 0.025 0.489 0.920 !       0.80 eA-3
Q180 0.540 0.399 0.979 !       0.80 eA-3
C181 0.095 0.237 0.138 !       0.80 eA-3
C182 0.500 0.062 0.004 !       0.80 eA-3
C183 0.243 0.317 0.011 !       0.79 eA-3
C184 0.025 0.504 0.828 !       0.79 eA-3
C185 0.907 0.253 0.971 !       0.79 eA-3
Q186 0.678 0.063 0.514 !       0.78 eA-3
C187 0.007 0.352 0.096 !       0.78 eA-3
C188 0.620 0.297 0.170 !       0.78 eA-3
Q189 0.948 0.337 0.814 !       0.78 eA-3
Q190 0.061 0.475 0.405 !       0.78 eA-3
C191 0.601 0.053 0.933 !       0.78 eA-3
C192 0.890 0.219 0.985 !       0.78 eA-3
C193 0.031 0.202 0.006 !       0.78 eA-3
Q194 0.203 0.179 0.495 !       0.78 eA-3
Q195 0.047 0.498 0.172 !       0.77 eA-3
Q196 0.015 0.496 0.672 !       0.77 eA-3
Q197 0.985 0.305 0.685 !       0.77 eA-3
C198 0.485 0.033 0.093 !       0.77 eA-3
Q199 0.909 0.475 0.217 !       0.77 eA-3
;
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9564
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.0827
_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^)+(0.1359P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.2655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4158
_reflns_number_total             9564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05568a3.cif
_cod_data_source_block           ZnMOF
_cod_depositor_comments          'Adding full bibliography for 7127332.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7127332
_shelx_estimated_absorpt_t_min   0.747
_shelx_estimated_absorpt_t_max   0.747
_shelxl_version_number           2014-3
_shelx_res_checksum              29448
_shelx_hkl_checksum              77791
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              74190