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_4134583
_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, 2.5(H2 O)'
_chemical_formula_sum            'C26 H21 Mg3 N2 O12.5'
_chemical_formula_weight         634.38
_chemical_name_common            'Mg-CUK-1L Dehydrated'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.220(5)
_cell_length_b                   17.812(4)
_cell_length_c                   10.975(2)
_cell_measurement_reflns_used    1355
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.9190
_cell_measurement_theta_min      3.0700
_cell_volume                     4728.9(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12981
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         6.024
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77978
_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            colorless
_exptl_crystal_density_diffrn    0.891
_exptl_crystal_description       rod
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0992
_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^)+(0.1610P)^2^+22.3368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2669
_refine_ls_wR_factor_ref         0.2883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3169
_reflns_number_total             4158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13793_si_003.cif
_cod_data_source_block           sh17008
_cod_original_cell_volume        4728.8(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C26 H21 Mg3 N2 O12.50'
_cod_database_code               4134583
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              1050
_shelx_hkl_checksum              48756