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_1560209
_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           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-30
_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                 104.3380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.40930(10)
_cell_length_b                   28.89370(10)
_cell_length_c                   17.71090(10)
_cell_measurement_reflns_used    77908
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      77.5250
_cell_measurement_theta_min      2.9850
_cell_volume                     5656.66(7)
_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      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_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    -40.00 -13.00   0.50    0.57    --    0.00 -64.00 131.00   54
  2  \w      7.00  32.00   0.50    0.57    --    0.00  64.00 -92.00   50
  3  \w     27.00  52.00   0.50    2.00    --   82.70 -64.00 131.00   50
  4  \w     89.00 114.00   0.50    2.00    --   82.70  64.00 -92.00   50
  5  \w    -34.00  39.00   0.50    0.57    --    0.00  82.00 -60.00  146
  6  \w     82.00 172.00   0.50    2.00    --   82.70  82.00   0.00  180
  7  \w     56.00 131.00   0.50    2.00    --   82.70  57.00  30.00  150
  8  \w    134.00 160.00   0.50    2.00    --   82.70  57.00  30.00   52
  9  \w     75.00 171.00   0.50    2.00    --   82.70  77.00-120.00  192
 10  \w      8.00 105.00   0.50    2.00    --   82.70 -38.00 120.00  194
 11  \w     61.00 168.00   0.50    2.00    --   82.70  57.00 -30.00  214
 12  \w    -79.00 -52.00   0.50    0.57    --    0.90 -64.00 131.00   54
 13  \w    -27.00  18.00   0.50    0.57    --   -0.90  57.00   0.00   90
 14  \w    -87.00 -48.00   0.50    0.57    --   -0.90 -19.00  90.00   78
 15  \w      3.00  29.00   0.50    0.57    --   -0.90 -82.00 -30.00   52
 16  \w     54.00  80.00   0.50    0.57    --   -0.90  57.00   0.00   52
 17  \w    -88.00 -52.00   0.50    0.57    --   -0.90 -38.00 150.00   72
 18  \w    -35.00  -1.00   0.50    0.57    --   -0.90 -82.00 -30.00   68
 19  \w    -31.00  21.00   0.50    0.57    --   -0.90 -38.00 150.00  104
 20  \w    -42.00   6.00   0.50    0.57    --   -0.90 -19.00  90.00   96
 21  \w    -27.00   2.00   0.50    0.57    --    0.90  82.00 150.00   58
 22  \w     29.00  86.00   0.50    0.57    --    0.90  38.00-120.00  114
 23  \w    -31.00  76.00   0.50    0.57    --    0.90  19.00  60.00  214
 24  \w    -23.00  33.00   0.50    0.57    --    0.90 -19.00 -60.00  112
 25  \w    -18.00  34.00   0.50    0.57    --    0.90  38.00 150.00  104
 26  \w    -87.00 -52.00   0.50    0.57    --    0.90 -19.00 -60.00   70
 27  \w     -4.00  28.00   0.50    0.57    --    0.90 -64.00 131.00   64
 28  \w    -22.00  12.00   0.50    0.57    --    0.90  38.00-120.00   68
 29  \w     80.00 105.00   0.50    2.00    --  105.10  60.00 104.02   50
 30  \w     77.00 103.00   0.50    2.00    --  105.10  66.00-118.84   52
 31  \w     79.00 105.00   0.50    2.00    --  105.10  57.00  90.00   52
 32  \w    134.00 171.00   0.50    2.00    --  105.10  69.00-131.37   74
 33  \w     75.00 101.00   0.50    2.00    --  105.10  71.00  36.16   52
 34  \w     76.00 102.00   0.50    2.00    --  105.10  69.00-131.37   52
 35  \w    136.00 183.00   0.50    2.00    --  105.10  66.00-159.88   94
 36  \w     79.00 105.00   0.50    2.00    --  105.10  57.00 179.42   52
 37  \w     76.00 102.00   0.50    2.00    --  105.10  68.00-175.20   52
 38  \w     83.00 193.00   0.50    2.00    --  105.10  38.00 120.00  220
 39  \w     77.00 103.00   0.50    2.00    --  105.10  67.00 102.79   52
 40  \w     75.00 102.00   0.50    2.00    --  105.10  72.00 -41.47   54
 41  \w     79.00 105.00   0.50    2.00    --  105.10  58.00  81.01   52
 42  \w     79.00 105.00   0.50    2.00    --  105.10  57.00  30.00   52
 43  \w    157.00 183.00   0.50    2.00    --  105.10  61.00 126.01   52
 44  \w     73.00  99.00   0.50    2.00    --  105.10  75.00-124.14   52
 45  \w    148.00 175.00   0.50    2.00    --  105.10  70.00 -81.72   54
 46  \w    118.00 194.00   0.50    2.00    --  105.10  41.00 -54.71  152
 47  \w     75.00 101.00   0.50    2.00    --  105.10  70.00 -81.72   52
 48  \w     19.00  44.00   0.50    2.00    --  105.10 -82.00-150.00   50
 49  \w     82.00 108.00   0.50    2.00    --  105.10  38.00  90.00   52
 50  \w     82.00 114.00   0.50    2.00    --  105.10  41.00 -54.71   64
 51  \w     77.00 103.00   0.50    2.00    --  105.10  66.00-159.88   52
 52  \w     17.00 135.00   0.50    2.00    --  105.10 -82.00  30.00  236
 53  \w     81.00 107.00   0.50    2.00    --  105.10  47.00  59.01   52
 54  \w    136.00 189.00   0.50    2.00    --  105.10  47.00  59.01  106
 55  \w     79.00 114.00   0.50    2.00    --  105.10  57.00-120.00   70
 56  \w     78.00 104.00   0.50    2.00    --  105.10  62.00 163.79   52
 57  \w     78.00 126.00   0.50    2.00    --  105.10  62.00-161.72   96
 58  \w     79.00 106.00   0.50    2.00    --  105.10  66.00 171.32   54
 59  \w     82.00 193.00   0.50    2.00    --  105.10  38.00-180.00  222
 60  \w     79.00 105.00   0.50    2.00    --  105.10  57.00 -90.00   52
 61  \w     77.00 115.00   0.50    2.00    --  105.10  77.00 -60.00   76
 62  \w     82.00 109.00   0.50    2.00    --  105.10  82.00  30.00   54
 63  \w     81.00 107.00   0.50    2.00    --  105.10  51.00 -62.72   52
 64  \w     90.00 129.00   0.50    2.00    --  105.10 -82.00   0.00   78
 65  \w     80.00 155.00   0.50    2.00    --  105.10  30.00 -68.66  150
 66  \w     82.00 116.00   0.50    2.00    --  105.10  46.00  95.06   68
 67  \w    137.00 193.00   0.50    2.00    --  105.10  48.00   3.41  112
 68  \w     47.00  80.00   0.50    2.00    --  105.10 -82.00   0.00   66
 69  \w    142.00 171.00   0.50    2.00    --  105.10  67.00 102.79   58
 70  \w     82.00 108.00   0.50    2.00    --  105.10  38.00-120.00   52
 71  \w     82.00 144.00   0.50    2.00    --  105.10  36.00 171.87  124
 72  \w     79.00 104.00   0.50    2.00    --  105.10  60.00-138.44   50
 73  \w     78.00 104.00   0.50    2.00    --  105.10  61.00 158.86   52
 74  \w     76.00 107.00   0.50    2.00    --  105.10  69.00 -23.99   62
 75  \w     89.00 140.00   0.50    2.00    --  105.10 -82.00  90.00  102
 76  \w     81.00 128.00   0.50    2.00    --  105.10  48.00   3.41   94
 77  \w    115.00 141.00   0.50    2.00    --  105.10  38.00 150.00   52
 78  \w     82.00 107.00   0.50    2.00    --  105.10  38.00 150.00   50
 79  \w     74.00 100.00   0.50    2.00    --  105.10  73.00 117.49   52
 80  \w     73.00  98.00   0.50    2.00    --  105.10  75.00-105.91   50
 81  \w     76.00 101.00   0.50    2.00    --  105.10  69.00 -59.46   50
 82  \w    116.00 142.00   0.50    2.00    --  105.10  69.00 -23.99   52
 83  \w     79.00 105.00   0.50    2.00    --  105.10  58.00  50.53   52
 84  \w     76.00 102.00   0.50    2.00    --  105.10  77.00 120.00   52
 85  \w     74.00 100.00   0.50    2.00    --  105.10  76.00  73.92   52
 86  \w    118.00 194.00   0.50    2.00    --  105.10  76.00  73.92  152
 87  \w     78.00 104.00   0.50    2.00    --  105.10  63.00-178.22   52
 88  \w     75.00 102.00   0.50    2.00    --  105.10  71.00-148.75   54
 89  \w     20.00  85.00   0.50    2.00    --  105.10 -82.00  90.00  130
 90  \w     76.00 135.00   0.50    2.00    --  105.10 -82.00 120.00  118
 91  \w     16.00 140.00   0.50    2.00    --  105.10 -82.00 -90.00  248
 92  \w     51.00 134.00   0.50    2.00    --  105.10 -82.00-150.00  166
 93  \w     78.00 104.00   0.50    2.00    --  105.10  61.00 126.01   52
;
_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      0.0652678000
_diffrn_orient_matrix_UB_12      0.0371872000
_diffrn_orient_matrix_UB_13      -0.0367814000
_diffrn_orient_matrix_UB_21      -0.1209451000
_diffrn_orient_matrix_UB_22      0.0132803000
_diffrn_orient_matrix_UB_23      -0.0566013000
_diffrn_orient_matrix_UB_31      -0.0228789000
_diffrn_orient_matrix_UB_32      0.0358236000
_diffrn_orient_matrix_UB_33      0.0592203000
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            168102
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.891
_diffrn_reflns_theta_min         2.995
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90448
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.338
_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         3.678
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1363
_refine_ls_number_reflns         23733
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0990
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2510
_refine_ls_wR_factor_ref         0.2556
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                22477
_reflns_number_total             23733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc07058k2.cif
_cod_data_source_block           cu-5b-100k
_cod_depositor_comments
;
Adding full bibliography for 1560208--1560210.cif.

2022-05-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C126 H132 Cu6 N18'
_cod_original_formula_sum        'C126 H132 Cu6 N18'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2279.73
_cod_database_code               1560209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.731
_shelx_estimated_absorpt_t_min   0.731
_reflns_odcompleteness_completeness 99.96
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C011(H01A,H01B), C018(H01C,H01D), C01B(H01F,H01G), C01E(H01I,H01J), C022(H02A,
 H02B), C023(H02C,H02D), C028(H02E,H02F), C02F(H02H,H02I), C02G(H02J,H02K),
 C02M(H02Q,H02R), C02Q(H02V,H02W), C02T(H02Z,H), C02X(H2,HC), C02Y(H3,HD),
 C033(H03G,H03H), C036(H03L,H03M), C039(H03N,H03O), C03B(H03Q,H03R), C03H(H03V,
 H03W), C03K(H03Z,HG), C03R(H8,HL), C03S(H9,HM), C03T(H10,HN), C03Z(H16,HS)
2.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C010(H010), C012(H012), C014(H014), C017(H017), C01A(H01E),
 C01C(H01H), C01G(H01K), C01K(H01L), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q), C01T(H01T), C01U(H01U), C025(H025), C027(H027), C02B(H02G),
 C02H(H02L), C02I(H02M), C02N(H02S), C02O(H02T), C02P(H02U), C02R(H02X),
 C02S(H02Y), C02W(H1), C02Z(H4), C030(H030), C034(H034), C037(H037), C038(H038),
  C03A(H03P), C03C(H03S), C03D(H03T), C03E(H03U), C03I(H03X), C03L(H03),
 C03O(H6), C03U(H11), C03V(H12), C03W(H13), C040(H040), C041(H041), C042(H042),
 C043(H043), C044(H044), C045(H045), C046(H046)
2.c Idealised Me refined as rotating group:
 C01R(H01M,H01R,H01S), C01W(H01V,H01W,H01X), C02L(H02N,H02O,H02P), C02V(H02,HA,
 HB), C031(H03A,H03B,H03C), C032(H03D,H03E,H03F), C035(H03I,H03J,H03K),
 C03J(H03Y,HE,HF), C03M(H5,HH,HI), C03P(H7,HJ,HK), C03X(H14,HO,HP), C03Y(H15,HQ,
 HR)
;
_shelx_res_checksum              83190
_shelx_hkl_checksum              29499
_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 1.186
_oxdiff_exptl_absorpt_empirical_full_min 0.888