Reversible Solid-State Isomerism of Azobenzene-Loaded Large-Pore Isoreticular Mg-CUK-1.
He, Junpeng; Aggarwal, Kanchan; Katyal, Naman; He, Shichao; Chiang, Edward; Dunning, Samuel G.; Reynolds, 3rd, Joseph E; Steiner, Alexander; Henkelman, Graeme; Que, Emily L.; Humphrey, Simon M.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13793

data_4134584
_publ_contact_author             'Dr. Simon M. Humphrey'
_publ_section_title
;
 Reversible Solid-State Isomerism of Azobenzene-Loaded Large-Pore
 Isoreticular Mg-CUK-1.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13793
_journal_year                    2020
_chemical_formula_moiety         'C26 H16 Mg3 N2 O10, 2(C12 H10 N2)'
_chemical_formula_sum            'C50 H36 Mg3 N6 O10'
_chemical_formula_weight         953.78
_chemical_name_common            'Mg-CUK-1L incl. AzB'
_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   geom
_audit_creation_method           'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_cell_angle_alpha                71.410(18)
_cell_angle_beta                 86.86(2)
_cell_angle_gamma                88.896(16)
_cell_formula_units_Z            2
_cell_length_a                   10.937(3)
_cell_length_b                   14.947(3)
_cell_length_c                   15.041(4)
_cell_measurement_reflns_used    1529
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      51.0420
_cell_measurement_theta_min      3.0990
_cell_volume                     2327.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_unetI/netI     0.1874
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7808
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        52.570
_diffrn_reflns_theta_max         52.569
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       rod
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         4937
_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1981
_refine_ls_R_factor_gt           0.1337
_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^)+(0.1500P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3114
_refine_ls_wR_factor_ref         0.3805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2427
_reflns_number_total             4937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13793_si_005.cif
_cod_data_source_block           sh17011
_cod_database_code               4134584
_cell_oxdiff_length_a            15.041(4)
_cell_oxdiff_length_b            18.350(3)
_cell_oxdiff_length_c            18.690(4)
_cell_oxdiff_angle_alpha         72.384(17)
_cell_oxdiff_angle_beta          73.32(2)
_cell_oxdiff_angle_gamma         76.88(2)
_cell_oxdiff_volume              4654(2)
_cell_oxdiff_measurement_reflns_used 1451
_oxdiff_exptl_absorpt_empirical_full_min 0.656
_oxdiff_exptl_absorpt_empirical_full_max 2.137
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              27868
_shelx_hkl_checksum              71957