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_1560208
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-05
_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                75.096(7)
_cell_angle_beta                 83.457(7)
_cell_angle_gamma                84.935(7)
_cell_formula_units_Z            8
_cell_length_a                   9.7333(10)
_cell_length_b                   27.941(2)
_cell_length_c                   42.675(4)
_cell_measurement_reflns_used    1249
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      17.3570
_cell_measurement_theta_min      3.8630
_cell_volume                     11121.3(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_details
;
  1 omega    1.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -        8.1402 -131.0000  -79.0000 68

  2 omega  -19.00   68.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.3745   38.0000  150.0000 87

  3 omega  -80.00   18.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.3745  -57.0000    0.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0059536000
_diffrn_orient_matrix_UB_12      0.0190208000
_diffrn_orient_matrix_UB_13      -0.0145198000
_diffrn_orient_matrix_UB_21      0.0037900000
_diffrn_orient_matrix_UB_22      -0.0181696000
_diffrn_orient_matrix_UB_23      -0.0090623000
_diffrn_orient_matrix_UB_31      -0.0731504000
_diffrn_orient_matrix_UB_32      -0.0008652000
_diffrn_orient_matrix_UB_33      0.0023574000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3024
_diffrn_reflns_av_unetI/netI     0.9050
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            72260
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.063
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       needle
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         43243
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.5885
_refine_ls_R_factor_gt           0.1609
_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^)+(0.0202P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2386
_refine_ls_wR_factor_ref         0.4138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5062
_reflns_number_total             43243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc07058k2.cif
_cod_data_source_block           140210a
_cod_depositor_comments
;
Adding full bibliography for 1560208--1560210.cif.

2022-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C252 H264 Cu12 N36'
_cod_original_formula_weight         4559.46
_cod_original_formula_moiety         '4(C63 H66 Cu3 N9)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        11121.5(18)
_cod_database_code               1560208
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Cu I'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.943
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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. Restrained distances
 C36-C37
 1.3 with sigma of 0.02
 C246-C247
 1.3 with sigma of 0.02
 C142-C141
 1.3 with sigma of 0.02
 C30-N18
 1.5 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C04T(H04A,H04B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C49(H49A,H49B),
 C50(H50A,H50B), C61(H61A,H61B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
  C72(H72A,H72B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,
 H93B), C111(H11D,H11E), C112(H11F,H11G), C113(H11H,H11I), C114(H11J,H11K),
 C195(H19G,H19H), C196(H19I,H19J), C197(H19K,H19L), C198(H19M,H19N), C216(H21G,
 H21H), C217(H21I,H21J), C218(H21K,H21L), C219(H21M,H21N), C237(H23G,H23H),
 C238(H23I,H23J), C239(H23K,H23L), C240(H24A,H24B), C132(H13D,H13E), C133(H13F,
 H13G), C134(H13H,H13I), C135(H13J,H13K), C153(H15D,H15E), C154(H15F,H15G),
 C155(H15H,H15I), C156(H15J,H15K), C174(H17D,H17E), C175(H17F,H17G), C176(H17H,
 H17I), C177(H17J,H17K)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C15(H15), C14(H14), C18(H18), C21(H21), C20(H20),
 C19(H19), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C38(H38), C39(H39),
  C40(H40), C52(H52), C53(H53), C54(H54), C55(H55), C58(H58), C59(H59),
 C60(H60), C62(H62), C74(H74), C75(H75), C76(H76), C77(H77), C84(H84), C83(H83),
  C82(H82), C81(H81), C97(H97), C96(H96), C95(H95), C98(H98), C104(H104),
 C103(H103), C102(H102), C101(H101), C115(H115), C116(H116), C117(H117),
 C118(H118), C122(H122), C123(H123), C124(H124), C125(H125), C199(H199),
 C200(H200), C201(H201), C202(H202), C206(H206), C207(H207), C208(H208),
 C209(H209), C221(H221), C224(H224), C223(H223), C222(H222), C227(H227),
 C228(H228), C229(H229), C230(H230), C242(H242), C243(H243), C244(H244),
 C245(H245), C248(H248), C249(H249), C250(H250), C251(H251), C138(H138),
 C137(H137), C140(H140), C139(H139), C145(H145), C144(H144), C143(H143),
 C146(H146), C158(H158), C159(H159), C160(H160), C161(H161), C166(H166),
 C167(H167), C164(H164), C165(H165), C182(H182), C181(H181), C180(H180),
 C179(H179), C186(H186), C187(H187), C188(H188), C189(H189)
3.c Fitted pentagon refined as free rotating group:
 N12(C23,C24,C25,N11), C4(N13,N14,C2,C3), N1(N2,C107,C108,C109), N4(C88,C87,
 C86,N3), N5(N6,C65,C66,C67), N33(C212,C213,C214,N32), C233(N30,N31,C235,C234),
 N21(N22,C151,C150,C149), N23(N24,C170,C171,C172), C130(C129,C128,N19,N20)
3.d Fitted hexagon refined as free rotating group:
 C12(C11,C10,C15,C14,C13), C18(C17,C16,C21,C20,C19), C31(C32,C33,C34,C35,C36),
 C41(C42,C37,C38,C39,C40), C51(C52,C53,C54,C55,C56), C57(C58,C59,C60,C62,C63),
 C74(C75,C76,C77,C78,C73), C79(C84,C83,C82,C81,C80), C97(C96,C95,C94,C99,C98),
 C105(C104,C103,C102,C101,C100), C119(C120,C115,C116,C117,C118), C126(C121,C122,
 C123,C124,C125), C204(C199,C200,C201,C202,C203), C210(C205,C206,C207,C208,
 C209), C221(C220,C225,C224,C223,C222), C227(C228,C229,C230,C226,C231),
 C241(C242,C243,C244,C245,C246), C247(C248,C249,C250,C251,C252), C138(C137,C136,
 C141,C140,C139), C145(C144,C143,C142,C147,C146), C162(C157,C158,C159,C160,
 C161), C166(C167,C168,C163,C164,C165), C178(C183,C182,C181,C180,C179),
 C185(C186,C187,C188,C189,C184)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C),
 C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C64(H64A,H64B,H64C), C68(H68A,H68B,
 H68C), C85(H85A,H85B,H85C), C89(H89A,H89B,H89C), C106(H10A,H10B,H10C),
 C110(H11A,H11B,H11C), C190(H19A,H19B,H19C), C194(H19D,H19E,H19F), C211(H21A,
 H21B,H21C), C215(H21D,H21E,H21F), C232(H23A,H23B,H23C), C236(H23D,H23E,H23F),
 C127(H12A,H12B,H12C), C131(H13A,H13B,H13C), C148(H14A,H14B,H14C), C152(H15A,
 H15B,H15C), C169(H16A,H16B,H16C), C173(H17A,H17B,H17C)
;
_shelx_res_checksum              74190
_shelx_hkl_checksum              68061
_olex2_submission_special_instructions 'No special instructions were received'