Luminescent cyclic trinuclear coinage metal complexes with aggregation-induced emission (AIE) performance.
Tian, Yuan; Wang, Zhao-Yang; Zang, Shuang-Quan; Li, Dan; Mak, Thomas C. W.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2275–2279; doi:10.1039/c8dt04898c

data_7048521
_publ_section_title
;
 Luminescent cyclic trinuclear coinage metal complexes with
 aggregation-induced emission (AIE) performance.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2275
_journal_page_last               2279
_journal_paper_doi               10.1039/c8dt04898c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C96 H81 Cu3 N6, 1.05(C H Cl3), 0.95(C Cl3)'
_chemical_formula_sum            'C98 H82.05 Cl6 Cu3 N6'
_chemical_formula_weight         1747.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-05 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7328(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.61574(16)
_cell_length_b                   52.1775(11)
_cell_length_c                   17.2889(3)
_cell_measurement_reflns_used    21043
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.0300
_cell_measurement_theta_min      3.1250
_cell_volume                     8493.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.993
_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    -59.00  -1.00   0.50    0.50    --    0.00 -57.00   0.00  116
  2  \w     16.00  41.00   0.50    0.50    --    0.00  38.00  30.00   50
  3  \w    -88.00  29.00   0.50    0.50    --    0.00 -57.00-120.00  234
  4  \w     72.00 132.00   0.50    1.00    --   97.60 -82.00-120.00  120
  5  \w     83.00 123.00   0.50    1.00    --   97.60 -82.00 -60.00   80
  6  \w     62.00 183.00   0.50    1.00    --   97.60  77.00 150.00  242
  7  \w     70.00 100.00   0.50    1.00    --   97.60 -61.00-150.00   60
  8  \w      8.00  65.00   0.50    1.00    --   97.60 -61.00-150.00  114
  9  \w    136.00 161.00   0.50    1.00    --   97.60  82.00-120.00   50
 10  \w     10.00 135.00   0.50    1.00    --   97.60 -82.00-150.00  250
 11  \w     75.00 141.00   0.50    1.00    --   97.60  82.00  30.00  132
 12  \w    136.00 161.00   0.50    1.00    --   97.60  45.00-180.00   50
 13  \w     76.00 172.00   0.50    1.00    --   97.60  77.00  90.00  192
;
_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      -0.0948262000
_diffrn_orient_matrix_UB_12      0.0208532000
_diffrn_orient_matrix_UB_13      0.0254258000
_diffrn_orient_matrix_UB_21      -0.1031959000
_diffrn_orient_matrix_UB_22      -0.0207967000
_diffrn_orient_matrix_UB_23      0.0174063000
_diffrn_orient_matrix_UB_31      0.0844526000
_diffrn_orient_matrix_UB_32      -0.0019717000
_diffrn_orient_matrix_UB_33      0.0856616000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44209
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.494
_diffrn_reflns_theta_min         2.744
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             3604
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         15225
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+17.3526P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12846
_reflns_number_total             15225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04898c2.cif
_cod_data_source_block           hy
_cod_depositor_comments
'Adding full bibliography for 7048520--7048522.cif.'
_cod_database_code               7048521
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 97.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.04
_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
 Cl2A-Cl3A \\sim Cl3A-Cl4A
 with sigma of 0.01
 Cl2A-Cl4A \\sim Cl4A-Cl3A
 with sigma of 0.01
 Cl2-C3BA \\sim Cl3-C3BA \\sim Cl1-C3BA
 with sigma of 0.01
 Cl2-C3BA \\sim Cl2A-C5AA \\sim Cl3A-C5AA \\sim Cl3-C3BA \\sim Cl1-C3BA \\sim
Cl4A-C5AA
 with sigma of 0.01
 Cl1A-C0BA \\sim Cl6B-C4BA \\sim Cl0A-C4BA \\sim Cl1B-C4BA \\sim Cl1B-C0BA
\\sim Cl5A-C0BA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl4A \\sim Cl2A \\sim Cl3A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Cl2 \\sim Cl3 \\sim Cl1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Cl3 \\sim Cl2A \\sim Cl1 \\sim Cl4A \\sim Cl2 \\sim Cl3A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Cl1A \\sim Cl6B \\sim Cl1B \\sim Cl0A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C5AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) \\sim Ueq, Uanis(Cl3A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C0BA) \\sim Ueq, Uanis(Cl5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl0A(0.95) Cl6B(0.8) Cl1(0.95) Cl2(0.95) Cl3(0.95) C4BA(0.9)
 H4BA(0.9) C3BA(0.95) Cl1A(0.2) Cl3A(0.05) Cl4A(0.05) Cl2A(0.05) C5AA(0.05)
 H5AA(0.05) Cl5A(0.05) C0BA(0.1) H0BA(0.1)
5.a Ternary CH refined with riding coordinates:
 C4BA(H4BA), C5AA(H5AA), C0BA(H0BA)
5.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C80(H80A,H80B), C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C4AA(H4AA), C6AA(H6AA), C8AA(H8AA), C9AA(H9AA), C21(H21),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C53(H53), C56(H56), C57(H57),
 C59(H59), C60(H60), C62(H62), C63(H63), C65(H65), C67(H67), C68(H68), C69(H69),
  C71(H71), C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), C81(H81),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C1(H1), C2(H2), C3(H3),
 C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C0AA(H0AA)
5.d Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C87(H87A,H87B,H87C), C8(H8A,H8B,H8C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              12852
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.234