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_7130092
_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         'C48 H24 N16 O20 Zn8'
_chemical_formula_sum            'C48 H24 N16 O20 Zn8'
_chemical_formula_weight         1667.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-21
_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                   32.3895(2)
_cell_length_b                   27.4040(2)
_cell_length_c                   28.0141(2)
_cell_measurement_reflns_used    50361
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.2730
_cell_measurement_theta_min      2.6930
_cell_volume                     24865.4(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73414
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        63.348
_diffrn_reflns_theta_max         63.348
_diffrn_reflns_theta_min         2.728
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72135
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.891
_exptl_crystal_description       plate
_exptl_crystal_F_000             6592
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.622
_refine_diff_density_min         -3.170
_refine_diff_density_rms         0.264
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.568
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         19263
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.568
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.1133
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3070
_refine_ls_wR_factor_ref         0.3107
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.904
_reflns_Friedel_fraction_max     0.904
_reflns_number_gt                18810
_reflns_number_total             19263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02041f2.cif
_cod_data_source_block           JNU-105
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7130092
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(5)
 0.45(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
C27 \\sim C26 \\sim C25 \\sim C24: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
Uanis(C37) = Uanis(N8) = Uanis(C38) = Uanis(O11) = Uanis(N7) = Uanis(C35) =
Uanis(C36) = Uanis(N5) = Uanis(C34) = Uanis(N6)
Uanis(C37) = Uanis(O12) = Uanis(N8) = Uanis(C38) = Uanis(O11) = Uanis(N7) =
Uanis(N6) = Uanis(C34) = Uanis(N5) = Uanis(C35) = Uanis(C36)
Uanis(N3) = Uanis(C32) = Uanis(O10) = Uanis(N4) = Uanis(C31) = Uanis(C30) =
Uanis(C33) = Uanis(O9) = Uanis(C29) = Uanis(N1) = Uanis(O20) = Uanis(C14)
Uanis(C17) = Uanis(C16) = Uanis(C19) = Uanis(C1) = Uanis(C9) = Uanis(C15) =
Uanis(C8)
Uanis(C43) = Uanis(O13) = Uanis(C40) = Uanis(N9) = Uanis(C39) = Uanis(N10) =
Uanis(C41) = Uanis(N12) = Uanis(C42) = Uanis(O14) = Uanis(N11) = Uanis(N13) =
Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(N16) = Uanis(N15)
Uanis(C17) = Uanis(N10) = Uanis(C39) = Uanis(N9) = Uanis(C40) = Uanis(C41) =
Uanis(N12) = Uanis(C42) = Uanis(N11) = Uanis(C43) = Uanis(O13) = Uanis(O14) =
Uanis(N13) = Uanis(C46) = Uanis(C47) = Uanis(N16) = Uanis(C48) = Uanis(N15) =
Uanis(C45) = Uanis(C44)
Uanis(C18) = Uanis(O19) = Uanis(O18) = Uanis(C10)
Uanis(O5) = Uanis(O17) = Uanis(O18) = Uanis(O19) = Uanis(O16) = Uanis(O8)
Uanis(N1) = Uanis(N14)
4.a Aromatic/amide H refined with riding coordinates:
 C29(H29), N11(H11), N16(H16), C12(H12), C13(H13), C9(H9), C10(H10), C39(H39),
 C6(H6), C7(H7), C3(H3), C4(H4), C24(H24), C25(H25), C27(H27), C28(H28), N8(H8),
  C34(H34), C44(H44), C18(H18), C19(H19), C21(H21), C16(H16A), N3(H3A)
4.b Fitted hexagon refined as free rotating group:
 N12(C42,N11,C43,C40,C41), C11(C12,C13,C8,C9,C10), C6(C7,C2,C3,C4,C5), C23(C24,
 C25,C26,C27,C28), C36(C37,N8,C38,N7,C35), C17(C18,C19,C20,C21,C16), C33(C30,
 C31,N4,C32,N3)
;
_shelx_res_checksum              21852
_shelx_fab_checksum              90106
_olex2_submission_special_instructions 'No special instructions were received'