A Metal-Organic Framework as a Flask: Photophysics of Confined Chromophores with a Benzylidene Imidazolinone Core
Dolgopolova, Ekaterina A.; Moore, Thomas; Ejegbavwo, Otega; Pellechia, Perry J.; Smith, Mark D.; Shustova, Natalia; Chem. Commun.  (2017) –; doi:10.1039/C7CC02253K

data_7120186
_publ_section_title
;
 A Metal-Organic Framework as a Flask: Photophysics of Confined
 Chromophores with a Benzylidene Imidazolinone Core
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02253K
_journal_year                    2017
_chemical_formula_moiety
'2(C13 H11.5 N2 O3), 0.83(C H4 O), 0.83(H2 O), 0.29(O)'
_chemical_formula_sum            'C26.82 H28.56 N4 O7.95'
_chemical_formula_weight         534.12
_chemical_name_systematic        pCOOH-BI
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                106.072(2)
_cell_angle_beta                 97.728(2)
_cell_angle_gamma                95.999(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2557(4)
_cell_length_b                   12.9984(6)
_cell_length_c                   14.6568(8)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.51
_cell_volume                     1301.56(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54527
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.755
_diffrn_reflns_theta_max         27.756
_diffrn_reflns_theta_min         2.510
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1655 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.9744.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0603P)^2^+0.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4682
_reflns_number_total             6129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02253k2.cif
_cod_data_source_block           ead2cooh
_cod_database_code               7120186
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.955
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1S-H1S
 0.85 with sigma of 0.02
 O2S-H2SA = O2S-H2SB
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O3S) = Uiso(O4S)
4. Others
 Sof(O1S)=Sof(H1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=FVAR(1)
 Sof(O2S)=Sof(H2SA)=Sof(H2SB)=FVAR(2)
 Fixed Sof: H3A(0.5) H2B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C8A(H8A), C9A(H9A), C11A(H11A), C12A(H12A), C6B(H6B), C8B(H8B),
 C9B(H9B), C11B(H11B), C12B(H12B)
5.b Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,
 H5BC), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              91988
_olex2_submission_special_instructions 'No special instructions were received'