Multistimuli-responsive multicolor solid-state luminescence tuned by NH-dependent switchable hydrogen bonds.
Zhang, Rui; He, Li-Hua; Liu, Sui-Jun; Liao, Jin-Sheng; Wen, He-Rui; Chen, Jing-Lin; Zhao, Feng; Dalton transactions (Cambridge, England : 2003) 53 (2023) 339–345; doi:10.1039/d3dt03124a

data_7714533
_publ_section_title
;
 Multistimuli-responsive multicolor solid-state luminescence tuned by
 NH-dependent switchable hydrogen bonds.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              339
_journal_page_last               345
_journal_paper_doi               10.1039/d3dt03124a
_journal_volume                  53
_journal_year                    2023
_chemical_formula_moiety         'C68 H68 Cu2 N12 P4, 2(Cl O4), 4(C H2 Cl2)'
_chemical_formula_sum            'C72 H76 Cl10 Cu2 N12 O8 P4'
_chemical_formula_weight         1842.994
_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_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-05 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                99.272(4)
_cell_angle_beta                 105.477(4)
_cell_angle_gamma                96.117(4)
_cell_formula_units_Z            1
_cell_length_a                   10.9861(5)
_cell_length_b                   13.9800(6)
_cell_length_c                   16.0424(7)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    297
_cell_measurement_theta_max      29.2930
_cell_measurement_theta_min      2.3030
_cell_volume                     2314.36(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9909
_diffrn_measured_fraction_theta_max 0.9909
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -54.29 148.71   1.00    8.00    --  -16.73  73.91 127.19  203
  2  \w    -54.29 148.71   1.00    8.00    --  -16.73  73.91  25.19  203
  3  \w    -54.29 148.71   1.00    8.00    --  -16.73  73.91 -79.81  203
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0432992000
_diffrn_orient_matrix_UB_12      0.0204050000
_diffrn_orient_matrix_UB_13      0.0208863000
_diffrn_orient_matrix_UB_21      -0.0521910000
_diffrn_orient_matrix_UB_22      -0.0288461000
_diffrn_orient_matrix_UB_23      -0.0341221000
_diffrn_orient_matrix_UB_31      0.0017453000
_diffrn_orient_matrix_UB_32      -0.0382281000
_diffrn_orient_matrix_UB_33      0.0242885000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.9909
_diffrn_reflns_Laue_measured_fraction_max 0.9909
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26563
_diffrn_reflns_point_group_measured_fraction_full 0.9909
_diffrn_reflns_point_group_measured_fraction_max 0.9909
_diffrn_reflns_theta_full        25.0273
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             946.915
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.3786
_refine_diff_density_min         -0.5425
_refine_diff_density_rms         0.1911
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             9.2624
_refine_ls_goodness_of_fit_ref   1.0588
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8082
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.0494
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         -0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1893P)^2^+1.9634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2496
_refine_ls_wR_factor_ref         0.2737
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6454
_reflns_number_total             8082
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03124a2.cif
_cod_data_source_block           1d
_cod_depositor_comments
'Adding full bibliography for 7714531--7714534.cif.'
_cod_database_code               7714533
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C33A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Rigid body (RIGU) restrains
 Cl2, Cl5, C9, Cl3, Cl7, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C17, C17A, C31, C31A, C33, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C17A)=Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(C31A)=Sof(H31d)=Sof(H31e)=
 Sof(H31f)=Sof(C33A)=Sof(H33d)=Sof(H33e)=Sof(H33f)=1-FVAR(1)
 Sof(C17)=Sof(H17a)=Sof(H17b)=Sof(H17c)=Sof(C31)=Sof(H31a)=Sof(H31b)=Sof(H31c)=
 Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(H33c)=FVAR(1)
 Fixed Sof: Cl2(0.5) Cl5(0.5) C9(0.5) H9a(0.5) H9b(0.5) Cl3(0.5) Cl7(0.5)
 C35(0.5) H35a(0.5) H35b(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C35(H35a,H35b), C2(H2a,H2b)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C3(H3a), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C29(H29), C30(H30), C32(H32), C34(H34),
 C36(H36), C37(H37)
4.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C17A(H17d,H17e,H17f), C31(H31a,H31b,H31c), C31A(H31d,
 H31e,H31f), C33(H33a,H33b,H33c), C33A(H33d,H33e,H33f)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.600