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_7714531
_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), 2(C3 H6 O), 2(H2 O)'
_chemical_formula_sum            'C74 H84 Cl2 Cu2 N12 O12 P4'
_chemical_formula_weight         1655.39
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-05 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                72.490(2)
_cell_angle_beta                 67.577(2)
_cell_angle_gamma                67.012(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8443(3)
_cell_length_b                   13.3701(3)
_cell_length_c                   13.9219(3)
_cell_measurement_reflns_used    31310
_cell_measurement_temperature    297.46(15)
_cell_measurement_theta_max      30.9940
_cell_measurement_theta_min      2.0420
_cell_volume                     2001.86(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.46(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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     -5.00  80.00   0.50    0.60    --    4.92  19.00 -60.00  170
  2  \w     -3.00  68.00   0.50    0.60    --    4.92  19.00  30.00  142
  3  \w      0.00  39.00   0.50    0.60    --    4.92  91.00 110.00   78
  4  \w    -34.00  -1.00   0.50    0.60    --   -5.39  91.00 110.00   66
  5  \w    -18.00  62.00   0.50    0.60    --   -5.39  37.00  90.00  160
  6  \w    -18.00  58.00   0.50    0.60    --   -5.39  19.00-120.00  152
  7  \w    -18.00  70.00   0.50    0.60    --   -5.39  19.00-180.00  176
  8  \w    -25.00  18.00   0.50    0.60    --    4.92 -28.00 -11.00   86
  9  \w    -67.00 -29.00   0.50    0.60    --    4.92 -28.00 -11.00   76
 10  \w    -67.00  18.00   0.50    0.60    --    4.92 -34.00 -64.64  170
 11  \w     -9.00  34.00   0.50    0.60    --    4.92 -91.00  -2.00   86
 12  \w    -42.00  19.00   0.50    0.60    --    4.92 -33.00  57.10  122
 13  \w    -78.00   6.00   0.50    0.60    --   -5.39 -57.00  30.00  168
 14  \w    -34.00   5.00   0.50    0.60    --   -5.39 -91.00  -2.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0001719000
_diffrn_orient_matrix_UB_12      -0.0348891000
_diffrn_orient_matrix_UB_13      -0.0296988000
_diffrn_orient_matrix_UB_21      0.0471935000
_diffrn_orient_matrix_UB_22      0.0149931000
_diffrn_orient_matrix_UB_23      -0.0419518000
_diffrn_orient_matrix_UB_31      0.0415772000
_diffrn_orient_matrix_UB_32      -0.0445892000
_diffrn_orient_matrix_UB_33      0.0222655000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58231
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.806
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9157
_refine_ls_number_restraints     470
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0907P)^2^+0.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7609
_reflns_number_total             9157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03124a2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7714531--7714534.cif.'
_cod_database_code               7714531
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         'C H O N Cu'
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.890
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C7-C10A
 1.5 with sigma of 0.02
 C9A-C7 = C7-C8A
 1.5 with sigma of 0.02
 C9-C7 = C7-C10
 1.5 with sigma of 0.02
 C7-C8
 1.5 with sigma of 0.02
 C37-C36 \\sim C37A-C36A
 with sigma of 0.02
 C36A-C35A \\sim C35-C36
 with sigma of 0.02
 O3A-O2A \\sim O3A-O4A \\sim O3A-O5A \\sim O2A-O4A \\sim O2A-O5A \\sim O4A-O5A
 with sigma of 0.02
 Cl1-O3A \\sim Cl1-O4 \\sim Cl1-O5A \\sim Cl1-O5 \\sim Cl1-O2A \\sim Cl1-O3
\\sim Cl1-O4A \\sim Cl1-O2
 with sigma of 0.02
 O4-O3 \\sim O4-O2 \\sim O4-O5 \\sim O3-O2 \\sim O3-O5 \\sim O2-O5
 with sigma of 0.02
 C37A-C35A \\sim C37-C35
 with sigma of 0.02
 O1-C37 \\sim O1A-C37A
 with sigma of 0.02
3. Restrained planarity
 O1A, C35A, C36A, C37A
 with sigma of 0.1
 O1, C35, C36, C37
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim O1A \\sim C35 \\sim C35A \\sim C36 \\sim C36A \\sim C37 \\sim C37A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Cl1 \\sim O2 \\sim O2A \\sim O3 \\sim O3A \\sim O4 \\sim O4A \\sim O5 \\sim
O5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A)
\\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O3A)
\\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O2A) \\sim Ueq,
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) = Uanis(O7)
5. Rigid body (RIGU) restrains
 C7, C8, C8A, C9, C9A, C10, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O1A, C35, C35A, C36, C36A, C37, C37A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O2, O2A, O3, O3A, O4, O4A, O5, O5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=1-FVAR(2)
 Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=FVAR(2)
 Sof(O1A)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=Sof(C37A)=1-FVAR(3)
 Sof(O1)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=Sof(C37)=FVAR(3)
 Fixed Sof: O6(0.5) H6A(0.5) H6B(0.5) O7(0.5) H7A(0.5) H7B(0.5)
 Fixed X: O7(0.44086)
7.a Riding coordinates:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C36A(H36D,
 H36E,H36F), O6(H6A,H6B), O7(H7A), O7(H7B)
7.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C1(H1), C2(H2), C3(H3A), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C),
 C35A(H35D,H35E,H35F), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              9260
_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 2.031
_oxdiff_exptl_absorpt_empirical_full_min 0.535