Flexible Luminescent MOF: Trapping of Less Stable Conformation of Rotational Isomers, In Situ Guest-Responsive Turn-Off and Turn-On Luminescence and Mechanistic Study.
Khatua, Sajal; Biswas, Protap; ACS applied materials & interfaces  (2020) –; doi:10.1021/acsami.0c02891

data_4517637
_publ_section_title
;
 Flexible Luminescent MOF: Trapping of Less Stable Conformation of
 Rotational Isomers, In Situ Guest-Responsive Turn-Off and Turn-On
 Luminescence and Mechanistic Study.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.0c02891
_journal_year                    2020
_chemical_formula_moiety         'C22 H15.95 Cu I N3 O, C1 Cl4'
_chemical_formula_sum            'C23 H15.95 Cl4 Cu I N3 O'
_chemical_formula_weight         682.57
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.100(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.282(3)
_cell_length_b                   12.4370(14)
_cell_length_c                   17.961(2)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.42
_cell_volume                     5025.6(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      108.77
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21459
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.476
_diffrn_reflns_theta_min         2.041
_exptl_absorpt_coefficient_mu    2.545
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1103 before and 0.0724 after correction. The Ratio of minimum to maximum transmission is 0.6355. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.45
_refine_diff_density_max         2.015
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4644
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+412.9888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4087
_reflns_number_total             4644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1P.cif
_cod_data_source_block           1p
_cod_original_cell_volume        5025.5(10)
_cod_database_code               4517637
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.394
_shelx_estimated_absorpt_t_min   0.330
_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
 Cl2A-C23A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23A) = Uanis(C6)
Uanis(C0AA) = Uanis(C9)
Uanis(C20A) = Uanis(C21A)
Uanis(C19B) = Uanis(C17)
Uanis(C2) = Uanis(C1)
Uanis(C22A) = Uanis(C19A)
Uanis(O1B) = Uanis(O1A)
4. Others
 Fixed Sof: Cl2A(0.4395) Cl3A(0.4395) Cl1A(0.4395) C23A(0.4395) C22A(0.47353)
 H22A(0.47353) H22B(0.47353) H22C(0.47353) H17(0.47353) O1A(0.47353)
 H18(0.47353) C20A(0.47353) C19A(0.47353) H19A(0.47353) C21A(0.47353)
 H21A(0.47353) Cl4A(0.4395) Cl2B(0.5605) Cl1B(0.5605) Cl4B(0.5605) Cl3B(0.5605)
 C0AA(0.5605) O1B(0.52647) C19B(0.52647) H19B(0.52647) C21B(0.52647)
 H21B(0.52647) C20B(0.52647) C22B(0.52647) H22D(0.52647) H22E(0.52647)
 H22F(0.52647)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C23B(H23B), C14(H14), C13(H13), C15(H15), C12(H12), C7(H7), C1(H1),
 C4(H4), C17(H17), C18(H18), C19A(H19A), C21A(H21A), C2(H2), C19B(H19B),
 C21B(H21B)
5.b Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
;
_shelx_res_checksum              88413
_shelx_hkl_checksum              71415
_olex2_submission_special_instructions 'No special instructions were received'