In situ generated dimethylamine constructs a robust hydrogen-bonded organic framework for selective fluorescence detection
Lai, Xiaoxia; Liu, Xinxin; Yang, Ye; Huang, Jinyan; Song, Shichang; Ren, Shicheng; Liang, Xuexue; Wu, Dongqi; Zhou, Liya; Chen, Peican; CrystEngComm 26 (2024) 1876–1883; doi:10.1039/D4CE00004H

data_7248246
_publ_section_title
;
 In situ generated dimethylamine constructs a robust hydrogen-bonded
 organic framework for selective fluorescence detection
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1876
_journal_page_last               1883
_journal_paper_doi               10.1039/D4CE00004H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C34 H22 N4 O4, C2 H7 N'
_chemical_formula_sum            'C36 H29 N5 O4'
_chemical_formula_weight         595.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-15 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.792(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.466(7)
_cell_length_b                   8.2745(15)
_cell_length_c                   10.0269(18)
_cell_measurement_reflns_used    2654
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.695
_cell_measurement_theta_min      2.255
_cell_volume                     2997.6(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8783
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         2.255
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0408 before and 0.0284 after correction. The Ratio of minimum to maximum transmission is 0.8979. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.038
_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     206
_refine_ls_number_reflns         3403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0631P)^2^+0.9574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2264
_reflns_number_total             3403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00004h2.cif
_cod_data_source_block           230802lxx_0m
_cod_depositor_comments
'Adding full bibliography for 7248245--7248246.cif.'
_cod_original_cell_volume        2997.5(9)
_cod_database_code               7248246
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H3A(0.5)
3.a Riding coordinates:
 N3(H3A)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
  C16(H16)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              21223
_olex2_submission_special_instructions 'No special instructions were received'