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_7244143
_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 H18 Cd2 N2 O14, H2 O'
_chemical_formula_sum            'C20 H20 Cd2 N2 O15'
_chemical_formula_weight         753.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-11
_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                90
_cell_angle_beta                 90.088(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7701(4)
_cell_length_b                   11.5100(3)
_cell_length_c                   29.1745(7)
_cell_measurement_reflns_used    14938
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      30.1010
_cell_measurement_theta_min      3.9110
_cell_volume                     4624.0(2)
_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      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            21531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.343
_diffrn_reflns_theta_min         3.517
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.655
_refine_diff_density_min         -3.605
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+35.2439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5621
_reflns_number_total             6180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01284c2.cif
_cod_data_source_block           e18adb4
_cod_depositor_comments
'Adding full bibliography for 7244143--7244152.cif.'
_cod_database_code               7244143
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Light Brown Tablet'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6 = O12-H12
 0.98 with sigma of 0.005
 N1-H1 = N2-H2
 0.98 with sigma of 0.005
 O15-H15A = O15-H15B
 0.98 with sigma of 0.005
 O14-H14B
 0.98 with sigma of 0.005
 H14B-H14A
 1.55 with sigma of 0.005
 O14-H14A
 0.98 with sigma of 0.005
 H14A-Cd2 = H14B-Cd2
 2.75 with sigma of 0.02
 O13-H13A = O13-H13B
 0.98 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(Cd2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C14(H14), C17(H17), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'