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_7244148
_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 ad
_chemical_formula_moiety         'C10 H9.4 Cu N O7.2'
_chemical_formula_sum            'C10 H9.4 Cu N O7.2'
_chemical_formula_weight         322.32
_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     iterative
_audit_creation_date             2018-08-24
_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                 97.117(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.9056(5)
_cell_length_b                   9.7392(10)
_cell_length_c                   11.4649(14)
_cell_measurement_reflns_used    1701
_cell_measurement_temperature    150.1(4)
_cell_measurement_theta_max      27.1300
_cell_measurement_theta_min      4.1640
_cell_volume                     543.53(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      150.1(4)
_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 0.995
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2564
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.690
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       plate
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.564
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2564
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0517P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                2093
_reflns_number_total             2564
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9814\% 
 around [0.96 -0.00 -0.28] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            d1ce01284c2.cif
_cod_data_source_block           e18adb3
_cod_depositor_comments
'Adding full bibliography for 7244143--7244152.cif.'
_cod_original_formula_sum        'C10 H9.40 Cu N O7.20'
_cod_database_code               7244148
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Green-Blue Plate'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.787(3)
 0.213(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
3. Restrained distances
 N1-H1
 0.98 with sigma of 0.005
 O7-H7B = O7-H7A = O6-H6
 0.98 with sigma of 0.005
4. Others
 Fixed Sof: O8(0.2) H8A(0.2) H8B(0.2)
 Fixed Uiso: H1(0.07)
5.a Rotating group:
 O8(H8A,H8B)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2