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_7244150
_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_absolute_configuration syn
_chemical_formula_moiety         'C46.75 H59.25 Cd6 N6.25 O36, 0.6(C3 H7 N O)'
_chemical_formula_sum            'C51.25 H105.75 Cd6 N7.75 O55.5'
_chemical_formula_weight         2393.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-05
_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                 90.9450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.10810(10)
_cell_length_b                   14.3068(2)
_cell_length_c                   23.1617(3)
_cell_measurement_reflns_used    23833
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      72.9320
_cell_measurement_theta_min      3.6940
_cell_volume                     4674.36(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66896
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.074
_diffrn_reflns_theta_min         3.133
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64233
_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    1.700
_exptl_crystal_description       plate
_exptl_crystal_F_000             2399
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.031
_refine_diff_density_max         3.787
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.419(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         17026
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1035P)^2^+25.2960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.834
_reflns_Friedel_fraction_max     0.816
_reflns_number_gt                16197
_reflns_number_total             17026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01284c2.cif
_cod_data_source_block           s19adb23
_cod_depositor_comments
'Adding full bibliography for 7244143--7244152.cif.'
_cod_original_formula_sum        'C51.25 H105.75 Cd6 N7.75 O55.50'
_cod_database_code               7244150
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'Colourless Shard'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.581(13)
 0.419(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 H27A-Cd1
 2.8 with sigma of 0.04
 H27B-Cd1
 2.8 with sigma of 0.04
 H26B-Cd1
 2.8 with sigma of 0.04
 H26A-Cd1
 2.8 with sigma of 0.04
 H28B-Cd1
 2.8 with sigma of 0.04
 H28A-Cd1
 2.8 with sigma of 0.04
 H31B-Cd2
 2.8 with sigma of 0.04
 H31A-Cd2
 2.8 with sigma of 0.04
 H32B-Cd2
 2.8 with sigma of 0.04
 H32A-Cd2
 2.8 with sigma of 0.04
 H30B-Cd2
 2.8 with sigma of 0.04
 H30A-Cd2
 2.8 with sigma of 0.04
 H35B-Cd3
 2.8 with sigma of 0.04
 H35A-Cd3
 2.8 with sigma of 0.04
 H34B-Cd3
 2.8 with sigma of 0.04
 H34A-Cd3
 2.8 with sigma of 0.04
 H38B-Cd4
 2.8 with sigma of 0.04
 H37B-Cd4
 2.8 with sigma of 0.04
 H37A-Cd4
 2.8 with sigma of 0.04
 H36A-Cd4
 2.8 with sigma of 0.04
 H36B-Cd4
 2.8 with sigma of 0.04
 H38A-Cd4
 2.8 with sigma of 0.04
 O26-H26B = O26-H26A = O27-H27B = O27-H27A = O28-H28B = O28-H28A = O32-H32A =
 O32-H32B = O31-H31A = O31-H31B = O30-H30A = O30-H30B = O34-H34B = O34-H34A =
 O35-H35B = O35-H35A = O36-H36A = O36-H36B = O38-H38A = O38-H38B = O37-H37A =
 O37-H37B
 0.98 with sigma of 0.005
 H36A-H36B \\sim H37B-H37A \\sim H35B-H35A \\sim H34A-H34B \\sim H38B-H38A
\\sim H30A-H30B \\sim H31A-
 H31B \\sim H32B-H32A \\sim H26B-H26A \\sim H27A-H27B \\sim H28A-H28B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O29 \\sim N6 \\sim C44 \\sim C45 \\sim C46 \\sim O30: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.005
C42 \\sim O25 \\sim N5 \\sim C41 \\sim C43 \\sim O26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.005
O33 \\sim N7 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.05 and
sigma for terminal atoms of 0.01
O40 \\sim N9 \\sim C53 \\sim C54 \\sim C55: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.005
5. Others
 Fixed Sof: C42(0.7) H42A(0.7) H42B(0.7) H42C(0.7) O25(0.7) O29(0.55) N5(0.7)
 N6(0.55) C41(0.7) H41(0.7) C43(0.7) H43A(0.7) H43B(0.7) H43C(0.7) C44(0.55)
 H44(0.55) C45(0.55) H45A(0.55) H45B(0.55) H45C(0.55) C46(0.55) H46A(0.55)
 H46B(0.55) H46C(0.55) O26(0.3) H26A(0.3) H26B(0.3) O30(0.45) H30A(0.45)
 H30B(0.45) O40(0.6) N9(0.6) C53(0.6) H53(0.6) C54(0.6) H54A(0.6) H54B(0.6)
 H54C(0.6) C55(0.6) H55A(0.6) H55B(0.6) H55C(0.6)
 Fixed Y: Cd1(0.82707)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B), C22(H22A,H22B), C32(H32C,H32D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C7(H7), C10(H10), C14(H14), C17(H17), C20(H20), C24(H24), C27(H27),
 C30(H30), C34(H34), C37(H37), C40(H40), C47(H47), C41(H41), C44(H44), C53(H53)
6.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C)
;
_olex2_submission_special_instructions 'No special instructions were received'