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_7244149
_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         'C10 H11 N O9 Zn2, H2 O, 2(O)'
_chemical_formula_sum            'C10 H17 N O12 Zn2'
_chemical_formula_weight         473.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 96.871(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4213(3)
_cell_length_b                   19.3205(6)
_cell_length_c                   10.8081(4)
_cell_measurement_reflns_used    5772
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.5550
_cell_measurement_theta_min      4.0880
_cell_volume                     1538.57(10)
_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 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12808
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81256
_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            'light tan'
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0315P)^2^+2.3458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3070
_reflns_number_total             3507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01284c2.cif
_cod_data_source_block           e18adb10
_cod_depositor_comments
'Adding full bibliography for 7244143--7244152.cif.'
_cod_database_code               7244149
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Very light tan block'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H,H,H) groups, All O(H) groups, All O(H,H,H) groups
2. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
 O9-H9
 0.98 with sigma of 0.005
 O8-H8A = O8-H8B = O10-H10B
 0.98 with sigma of 0.005
 O10-H10A
 0.98 with sigma of 0.005
 O7-H7A = O7-H7B
 0.98 with sigma of 0.005
 H7B-H7A
 1.55 with sigma of 0.009
 H8A-H8B
 1.55 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O11A \\sim O12 \\sim O11 \\sim O12A \\sim O11B: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O11A(0.65) O12(0.8) O11(0.25) O12A(0.1) O11B(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'