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_7130094
_publ_section_title
;
 Formaldehyde recognition through aminal formation in a luminescent
 metal--organic framework
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02041F
_journal_year                    2022
_chemical_formula_moiety         'C25 H14 N10 O10 Zn4, 2(H2 O)'
_chemical_formula_sum            'C25 H18 N10 O12 Zn4'
_chemical_formula_weight         911.97
_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
_audit_creation_date             2022-01-12
_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                   19.6175(6)
_cell_length_b                   19.741(2)
_cell_length_c                   32.3260(19)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.3960
_cell_measurement_theta_min      3.5150
_cell_volume                     12518.9(15)
_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, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            40469
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.654
_diffrn_reflns_theta_min         3.176
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69712
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_description       plate
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.400
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         12424
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1118P)^2^+21.0361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10391
_reflns_number_total             12424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02041f2.cif
_cod_data_source_block           JNU-105-(NH)2CH2
_cod_original_cell_volume        12519.1(17)
_cod_database_code               7130094
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Restrained distances
 N36-C94
 1.45 with sigma of 0.005
 N95-C25
 1.45 with sigma of 0.005
 N95-C69
 1.48 with sigma of 0.005
 C69-N36
 1.48 with sigma of 0.005
 C12-N39
 1.45 with sigma of 0.005
 N72-C14
 1.45 with sigma of 0.005
 N39-C6
 1.48 with sigma of 0.005
 C6-N72
 1.48 with sigma of 0.005
 N36-C1AA
 2.4 with sigma of 0.01
 N36-C9
 2.4 with sigma of 0.01
 C4-N95
 2.4 with sigma of 0.01
 N95-C34
 2.4 with sigma of 0.01
 N95-N36
 2.6 with sigma of 0.01
 C69-C94
 2.6 with sigma of 0.01
 C69-C25
 2.6 with sigma of 0.01
 C6-C14
 2.6 with sigma of 0.01
 C6-C12
 2.6 with sigma of 0.01
 N39-N72
 2.6 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C2) = Uanis(C94) = Uanis(C1AA) = Uanis(C8) = Uanis(C14) = Uanis(C83) =
Uanis(N36) = Uanis(N95) = Uanis(N39) = Uanis(N72)
Uanis(C1) = Uanis(C34) = Uanis(C25) = Uanis(C85) = Uanis(C59) = Uanis(C12) =
Uanis(C32)
Uanis(C4) = Uanis(C69) = Uanis(C6)
3. Others
 Fixed Sof: C5(0.75) H5(0.75) C2AA(0.75) H2AA(0.75) C7(0.75) H7(0.75) C8(0.75)
 H8(0.75) C11(0.75) H11(0.75) C12(0.75) C14(0.75) C0AA(0.75) H0AA(0.75)
 C34(0.25) H34(0.25) C25(0.25) C85(0.25) H85(0.25) C59(0.25) H59(0.25)
 C94(0.25) C83(0.25) H83(0.25) C32(0.25) H32(0.25) C1AA(0.25) H1AA(0.25)
 C6(0.75) H6A(0.75) H6B(0.75) N36(0.25) H36(0.25) N39(0.75) H39(0.75) N95(0.25)
 H95(0.25) C69(0.25) H69A(0.25) H69B(0.25) N72(0.75) H72(0.75)
4.a Riding coordinates:
 O1(H1B), O1(H1A), O2(H2B), O2(H2A), N36(H36), N95(H95)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C69(H69A,H69B)
4.c Aromatic/amide H refined with riding coordinates:
 N00J(H00J), N00L(H00L), C00T(H00T), C00U(H00U), C5(H5), C2AA(H2AA), C7(H7),
 C8(H8), C11(H11), C0AA(H0AA), C34(H34), C85(H85), C59(H59), C83(H83), C32(H32),
  C1AA(H1AA), N39(H39), N72(H72)
4.d Fitted hexagon refined as free rotating group:
 C34(C25,C4,C85,C59,C1), C94(C9,C83,C32,C2,C1AA)
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_shelx_res_checksum              57296
_shelx_fab_checksum              28559
_olex2_submission_special_instructions 'No special instructions were received'