Synthesis of an ammelide-based ultra-microporous Cd-MOF for sensitive detection of dichromate ions.
Liang, Linfeng; Ding, Yin-Kang; Yin, Yang; Yang, Feng-Fan; Yang, Jing; Chemical communications (Cambridge, England) 61 (2025) 1834–1837; doi:10.1039/d4cc05516k

data_7134095
_publ_section_title
;
 Synthesis of an ammelide-based ultra-microporous Cd-MOF for sensitive
 detection of dichromate ions.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1834
_journal_page_last               1837
_journal_paper_doi               10.1039/d4cc05516k
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C6 H6 Cd N8 O4, 1[C3H7NO]'
_chemical_formula_sum            'C6 H6 Cd N8 O4'
_chemical_formula_weight         366.59
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-12-11 deposited with the CCDC.	2024-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.7618(2)
_cell_length_b                   12.7618(2)
_cell_length_c                   7.6340(2)
_cell_measurement_reflns_used    13941
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.8420
_cell_measurement_theta_min      2.0460
_cell_volume                     1076.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.958
_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      7.66 119.16   0.50   10.00    --   28.00  59.94 -20.34  223
  2  \w      7.66 119.16   0.50   10.00    --   28.00  59.94  69.66  223
  3  \w      7.66 119.16   0.50   10.00    --   28.00  59.94 159.66  223
  4  \w      7.66 119.16   0.50   10.00    --   28.00  59.94-110.34  223
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17797
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.968
_diffrn_reflns_theta_min         4.553
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       rod
_exptl_crystal_F_000             534
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack x determined using 1522 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         3670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0624P)^2^+0.1325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                3542
_reflns_number_total             3670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05516k2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7134095.cif.'
_cod_database_code               7134095
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N004(H004)
2.b X=CH2 refined with riding coordinates:
 N008(H00A,H00B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 330\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C3H7NO] per Asymmetric Unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;