Pressure-induced phosphorescence enhancement and piezochromism of a carbazole-based cyclic trinuclear Cu(i) complex
Xie, Mo; Chen, Xiao-Ru; Wu, Kun; Lu, Zhou; Wang, Kai; Li, Nan; Wei, Rong-Jia; Zhan, Shun-Ze; Ning, Guo-Hong; Zou, Bo; Li, Dan; Chemical Science 12 (2021) 4425–4431; doi:10.1039/D0SC07058K

data_1560210
_publ_section_title
;
 Pressure-induced phosphorescence enhancement and piezochromism of a
 carbazole-based cyclic trinuclear Cu(i) complex
;
_journal_issue                   12
_journal_name_full               'Chemical Science'
_journal_page_first              4425
_journal_page_last               4431
_journal_paper_doi               10.1039/D0SC07058K
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C63 H66 Cu3 N9'
_chemical_formula_sum            'C63 H66 Cu3 N9'
_chemical_formula_weight         1139.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-11 deposited with the CCDC.	2021-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9899(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.52641(11)
_cell_length_b                   29.1085(3)
_cell_length_c                   17.85854(17)
_cell_measurement_reflns_used    19752
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      74.7580
_cell_measurement_theta_min      3.9340
_cell_volume                     5814.11(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -76.00 -35.00   0.50    1.50    --   -0.90 -57.00-120.00   82
  2  \w    -12.00  15.00   0.50    1.50    --   -0.90 -57.00-120.00   54
  3  \w    -33.00  39.00   0.50    1.50    --    0.90  82.00 -30.00  144
  4  \w    -31.00  37.00   0.50    1.50    --    0.90  82.00  60.00  136
  5  \w    -28.00  45.00   0.50    1.50    --    0.90  77.00 -90.00  146
  6  \w    -26.00  21.00   0.50    1.50    --    0.90  82.00-150.00   94
  7  \w    -29.00  -3.00   0.50    1.50    --    0.90  77.00  30.00   52
  8  \w     19.00  44.00   0.50    1.50    --    0.90  77.00  30.00   50
  9  \w     68.00  97.00   0.50    6.00    --  105.10 -82.00 120.00   58
 10  \w     76.00 102.00   0.50    6.00    --  105.10 -82.00 -60.00   52
 11  \w     17.00 138.00   0.50    6.00    --  105.10 -19.00-150.00  242
 12  \w     87.00 113.00   0.50    6.00    --  105.10 -82.00 -30.00   52
 13  \w     82.00 187.00   0.50    6.00    --  105.10  38.00-150.00  210
 14  \w     28.00 140.00   0.50    6.00    --  105.10 -82.00 150.00  224
 15  \w     16.00 124.00   0.50    6.00    --  105.10 -57.00 -90.00  216
 16  \w    104.00 194.00   0.50    6.00    --  105.10  38.00-180.00  180
 17  \w     49.00  76.00   0.50    6.00    --  105.10 -82.00-150.00   54
 18  \w     18.00 139.00   0.50    6.00    --  105.10 -82.00 -90.00  242
 19  \w    134.00 194.00   0.50    6.00    --  105.10  82.00-150.00  120
 20  \w     82.00 107.00   0.50    6.00    --  105.10 -82.00-150.00   50
 21  \w    141.00 192.00   0.50    6.00    --  105.10  19.00 -60.00  102
 22  \w     65.00 123.00   0.50    6.00    --  105.10 -82.00  60.00  116
 23  \w     35.00  60.00   0.50    6.00    --  105.10 -82.00  60.00   50
 24  \w    111.00 136.00   0.50    6.00    --  105.10 -82.00 120.00   50
 25  \w     16.00  72.00   0.50    6.00    --  105.10 -57.00  90.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0037157000
_diffrn_orient_matrix_UB_12      -0.0197926000
_diffrn_orient_matrix_UB_13      -0.0793704000
_diffrn_orient_matrix_UB_21      -0.1226481000
_diffrn_orient_matrix_UB_22      0.0218531000
_diffrn_orient_matrix_UB_23      -0.0357869000
_diffrn_orient_matrix_UB_31      0.0626980000
_diffrn_orient_matrix_UB_32      0.0439361000
_diffrn_orient_matrix_UB_33      -0.0179671000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61630
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.972
_diffrn_reflns_theta_min         3.966
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         12209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0968P)^2^+1.3283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8933
_reflns_number_total             12209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc07058k2.cif
_cod_data_source_block           cu-5b-293k
_cod_depositor_comments
'Adding full bibliography for 1560208--1560210.cif.'
_cod_database_code               1560210
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu C H N'
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.737
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C3AA(0.5) H3AA(0.5) H3AB(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
 H32D(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C35(0.5)
 H35A(0.5) H35B(0.5) C36(0.5) H36A(0.5) H36B(0.5) H37C(0.5) H37D(0.5) H37A(0.5)
 H37B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 C56(0.5) H56A(0.5) H56B(0.5) C57(0.5) H57A(0.5) H57B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C32(H32A,H32B), C32(H32C,H32D), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37C,H37D), C37(H37A,H37B), C51(H51A,H51B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,
 H56B), C57(H57A,H57B)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29),
 C30(H30), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47),
  C48(H48), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
 C67(H67), C68(H68)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              68660
_shelx_hkl_checksum              37325
_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 1.080
_oxdiff_exptl_absorpt_empirical_full_min 0.953