Formaldehyde recognition through aminal formation in a luminescent metal–organic framework
Li, Jia-Li; Xiong, Xiao; Luo, Dong; Wei, Yu-Bai; Lu, Weigang; Li, Dan; Chemical Communications  (2022) –; doi:10.1039/D2CC02041F

data_7130093
_publ_section_title
;
 Formaldehyde recognition through aminal formation in a luminescent
 metal--organic framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02041F
_journal_year                    2022
_chemical_formula_moiety         'C24 H14 N10 O10 Zn4, 2(H2 O)'
_chemical_formula_sum            'C24 H18 N10 O12 Zn4'
_chemical_formula_weight         899.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-03 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.49970(10)
_cell_length_b                   19.64560(10)
_cell_length_c                   32.3093(2)
_cell_measurement_reflns_used    40677
_cell_measurement_temperature    99.99(17)
_cell_measurement_theta_max      77.5210
_cell_measurement_theta_min      3.1520
_cell_volume                     12377.15(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(17)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -23.00   2.00   0.50    5.75    --   -0.90 -82.00-180.00   50
  2  \w    -25.00  14.00   0.50    5.75    --   -0.90  82.00-180.00   78
  3  \w    -38.00  28.00   0.50    5.75    --   -0.90 -82.00 -30.00  132
  4  \w     18.00  89.00   0.50    5.75    --    0.90  38.00 -90.00  142
  5  \w    -31.00  37.00   0.50    5.75    --    0.90  82.00 120.00  136
  6  \w    -87.00  32.00   0.50    5.75    --    0.90 -19.00 -30.00  238
  7  \w     16.00 132.00   0.50   22.99    --  105.10 -57.00 120.00  232
  8  \w     28.00 100.00   0.50   22.99    --  105.10 -38.00 -90.00  144
  9  \w     17.00 140.00   0.50   22.99    --  105.10 -82.00 120.00  246
 10  \w     59.00 140.00   0.50   22.99    --  105.10 -82.00 -90.00  162
 11  \w     54.00  79.00   0.50   22.99    --  105.10 -82.00   0.00   50
 12  \w     88.00 123.00   0.50   22.99    --  105.10 -82.00   0.00   70
 13  \w     26.00 138.00   0.50   22.99    --  105.10 -19.00-150.00  224
 14  \w     82.00 120.00   0.50   22.99    --  105.10  82.00-120.00   76
 15  \w     92.00 138.00   0.50   22.99    --  105.10 -77.00 -60.00   92
 16  \w     42.00  70.00   0.50   22.99    --  105.10 -82.00  90.00   56
 17  \w     16.00 137.00   0.50   22.99    --  105.10 -19.00 -30.00  242
 18  \w     89.00 114.00   0.50   22.99    --  105.10 -82.00-180.00   50
 19  \w     19.00  77.00   0.50   22.99    --  105.10 -77.00 -60.00  116
 20  \w    101.00 128.00   0.50   22.99    --  105.10 -82.00  60.00   54
 21  \w     42.00 168.00   0.50   22.99    --  105.10   0.00 -90.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0173179000
_diffrn_orient_matrix_UB_12      0.0560554000
_diffrn_orient_matrix_UB_13      -0.0316611000
_diffrn_orient_matrix_UB_21      -0.0290147000
_diffrn_orient_matrix_UB_22      0.0447598000
_diffrn_orient_matrix_UB_23      0.0350323000
_diffrn_orient_matrix_UB_31      0.0714139000
_diffrn_orient_matrix_UB_32      0.0317195000
_diffrn_orient_matrix_UB_33      0.0065543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            123274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.776
_diffrn_reflns_theta_min         2.735
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_description       plate
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.875
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         13122
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0940P)^2^+15.2499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11318
_reflns_number_total             13122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02041f2.cif
_cod_data_source_block           JNU-105-(NH2)2
_cod_database_code               7130093
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn C H O N '
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C4-C6
 2.315 with sigma of 0.002
 N2-C4
 1.49 with sigma of 0.002
 N2-C5
 2.557 with sigma of 0.002
 N2-C3
 2.432 with sigma of 0.002
 N2-C7
 4.258 with sigma of 0.002
 C2-N2
 3.723 with sigma of 0.002
2. Uiso/Uaniso restraints and constraints
O7 \\sim O12 \\sim O1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(O12) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.1
Uanis(C11) = Uanis(C10)
Uanis(C11) = Uanis(C10) = Uanis(C5) = Uanis(C2)
Uanis(N5) = Uanis(C22) = Uanis(C21)
Uanis(N3) = Uanis(N1) = Uanis(N2)
3. Others
 Fixed Sof: C11(0.25) H11(0.25) C10(0.25) C9(0.25) H9A(0.25) C8(0.25) H8(0.25)
 C3(0.75) H3(0.75) C7(0.75) H7(0.75) C6(0.75) H6(0.75) C4(0.75) N2(0.5)
 H2A(0.5) H2B(0.5) N1(0.5) H1A(0.5) H1B(0.5)
4.a Riding coordinates:
 O1(H1C), O1(H1D), O12(H12A), O12(H12B)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N9(H9), C24(H24), C20(H20), C11(H11), C9(H9A), C8(H8), C16(H16),
 C14(H14), C3(H3), C13(H13), C7(H7), C6(H6)
4.c Fitted hexagon refined as free rotating group:
 C2(C11,C10,C5,C9,C8)
4.d X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N2(H2A,H2B), N1(H1A,H1B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44853
_shelx_fab_checksum              45620
_platon_squeeze_void_probe_radius 1.20
_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 2.275
_oxdiff_exptl_absorpt_empirical_full_min 0.576