Improved quantum yield in geometrically constrained tetraphenylethylene-based metal–organic frameworks
Stawiasz, Katherine J.; Deneff, Jacob I.; Reyes, Raphael A.; Woods, Toby J.; Rohwer, Lauren E. S.; Valdez, Nichole; Rodriguez, Mark A.; Lawal, Abdul; Moore, Jeffrey S.; Sava Gallis, Dorina F.; CrystEngComm 25 (2023) 2701–2705; doi:10.1039/D3CE00228D

data_7246629
_publ_section_title
;
 Improved quantum yield in geometrically constrained
 tetraphenylethylene-based metal--organic frameworks
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2701
_journal_page_last               2705
_journal_paper_doi               10.1039/D3CE00228D
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
; 
C72 H54 N2 O10 Zn2, 0.5(C5 H11 N O) 
;
_chemical_formula_sum            'C74.5 H59.5 N2.5 O10.5 Zn2'
_chemical_formula_weight         1288.48
_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
_atom_sites_solution_primary     'dual space'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-02-03 deposited with the CCDC.	2023-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                89.7118(11)
_cell_angle_beta                 89.6383(12)
_cell_angle_gamma                82.0544(12)
_cell_formula_units_Z            2
_cell_length_a                   10.4851(5)
_cell_length_b                   17.0154(8)
_cell_length_c                   24.7946(11)
_cell_measurement_reflns_used    76079
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.30
_cell_volume                     4381.0(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX3 V2019.11-0 (Bruker, 2019)'
_computing_data_reduction
; 
SAINT V8.40B, XPREP v2014/2, (Bruker, 2019), SADABS V2016/2 
(Krause et al., 2015) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2019), CrystalMaker v9.2.8 (CrystalMaker, 2016) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2019)'
_computing_structure_refinement  'SHELXL-2018-3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT-2018-2 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ed46qs_sq
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            147139
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.539
_diffrn_reflns_theta_min         1.961
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_id                ed46qs_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -7 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.264
_platon_squeeze_details
;
SQUEEZE identified two distinct void spaces in the P1 cell and removed a total
of 426 electrons from the P1 cell. The electron count is consistent with either
approximately 16 ethanol molecules per unit cell or approximately eight DEF
molecules per unit cell. The most likely solution is a combination of ethanol
and DEF molecules in the void spaces.
;
_refine_diff_density_max         1.350
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.584
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         16274
_refine_ls_number_restraints     1280
_refine_ls_restrained_S_all      1.544
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.1034
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3158
_refine_ls_wR_factor_ref         0.3259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15091
_reflns_number_total             16274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00228d2.cif
_cod_data_source_block           ed46qs_sq
_cod_depositor_comments
'Adding full bibliography for 7246628--7246629.cif.'
_cod_original_formula_sum        'C74.50 H59.50 N2.50 O10.50 Zn2'
_cod_database_code               7246629
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              41330
_shelx_fab_checksum              75479
_platon_squeeze_void_probe_radius 1.20