Synthesis, structures and properties of metal–organic frameworks prepared using a semi-rigid tricarboxylate linker
Rixson, Daniel; Günay Sezer, Güneş; Alp, Emre; Mahon, Mary F.; Burrows, Andrew D.; CrystEngComm 24 (2022) 863–876; doi:10.1039/D1CE01284C

data_7244152
_publ_section_title
;
 Synthesis, structures and properties of metal--organic frameworks
 prepared using a semi-rigid tricarboxylate linker
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              863
_journal_page_last               876
_journal_paper_doi               10.1039/D1CE01284C
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C20 H20 Cd3 N2 O16, 4(H2 O)'
_chemical_formula_sum            'C20 H28 Cd3 N2 O20'
_chemical_formula_weight         953.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.353(4)
_cell_angle_beta                 75.848(3)
_cell_angle_gamma                70.505(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7777(2)
_cell_length_b                   8.9715(4)
_cell_length_c                   11.4851(4)
_cell_measurement_reflns_used    8998
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3890
_cell_measurement_theta_min      4.1840
_cell_volume                     690.98(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.349
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.292
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2755
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0263P)^2^+0.6327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2639
_reflns_number_total             2755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01284c2.cif
_cod_data_source_block           s18adb28
_cod_depositor_comments
'Adding full bibliography for 7244143--7244152.cif.'
_cod_database_code               7244152
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Colourless Block'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O8-H8B = O8-H8A = O7_$1-H7A_$1 = O7_$1-H7B_$1
 0.98 with sigma of 0.005
 N1-H1
 0.98 with sigma of 0.005
 O9-H9B = O9-H9A
 0.98 with sigma of 0.005
 O10-H10A = O10-H10B
 0.98 with sigma of 0.02
 H10B-H10A
 1.5 with sigma of 0.1
 O10-H10A
 0.98 with sigma of 0.02
 H10A-H10B
 1.52 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'