Pargyline-phosphine copper(I) clusters with tunable emission for light-emitting devices.
Huang, Qiu-Qin; Lin, Yan-Yan; Wang, Yu-Ling; Qi, Jia Yuan; Fu, FengFu; Wei, Qiao-Hua; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5844–5850; doi:10.1039/d4dt00022f

data_7715267
_publ_section_title
;
 Pargyline-phosphine copper(I) clusters with tunable emission for
 light-emitting devices.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5844
_journal_page_last               5850
_journal_paper_doi               10.1039/d4dt00022f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C112 H104 Cu6 N8 P4, 2(F6 P), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C112.5 H105 Cl Cu6 F12 N8 P6'
_chemical_formula_weight         2399.55
_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             2024-01-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-20 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                74.6580(10)
_cell_angle_beta                 78.7900(10)
_cell_angle_gamma                72.0250(10)
_cell_formula_units_Z            2
_cell_length_a                   14.51350(10)
_cell_length_b                   14.80280(10)
_cell_length_c                   26.8559(2)
_cell_measurement_reflns_used    67411
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9650
_cell_measurement_theta_min      2.0380
_cell_volume                     5252.41(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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     -9.00  80.00   0.50    0.33    --    6.80  57.00 -30.00  178
  2  \w    -18.00  26.00   0.50    0.33    --    6.80 -99.00-180.00   88
  3  \w    -66.00  31.00   0.50    0.33    --    6.80 -77.00-150.00  194
  4  \w    -18.00  41.00   0.50    0.33    --    6.80 -99.00  60.00  118
  5  \w    -18.00  29.00   0.50    0.33    --   -5.24 -99.00  90.00   94
  6  \w    -20.00  69.00   0.50    0.33    --   -5.24  38.00-120.00  178
  7  \w    -18.00  29.00   0.50    0.33    --   -5.24 -99.00-120.00   94
  8  \w    -81.00  10.00   0.50    0.33    --   -5.24 -19.00  60.00  182
  9  \w    -21.00  68.00   0.50    0.33    --   -5.24  57.00  30.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            113448
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.741
_exptl_absorpt_coefficient_mu    1.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             2450
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1635
_refine_ls_number_reflns         24051
_refine_ls_number_restraints     874
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+11.3986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20246
_reflns_number_total             24051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00022f2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 7715265--7715267.cif.'
_cod_original_cell_volume        5252.41(8)
_cod_original_formula_sum        'C112.50 H105 Cl Cu6 F12 N8 P6'
_cod_database_code               7715267
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.947
_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
 Cl1-Cl2
 2.6 with sigma of 0.01
 C87-N3 = N3-C91A
 1.4 with sigma of 0.01
 N8A-C115 = N8-C106
 1.4 with sigma of 0.02
 C106-C114 = C115-C108
 1.45 with sigma of 0.02
 N8A-C108 = N8-C114
 2.4 with sigma of 0.02
 C1B-C1C = C1C-C1A
 1.4 with sigma of 0.02
 C1C-C98
 2.8 with sigma of 0.02
 N8-C107 = C116-N8A
 1.4 with sigma of 0.02
 Cl4-C117 \\sim C117-Cl3
 with sigma of 0.02
 Cl2-C2A \\sim C2A-Cl1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim C2A \\sim Cl1 \\sim Cl4 \\sim Cl3 \\sim C117: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
P5 \\sim F9 \\sim F7 \\sim F4 \\sim F5 \\sim F2 \\sim F11 \\sim F7A \\sim F11A
\\sim F5A \\sim F9A \\sim F2A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N3 \\sim C87 \\sim C91 \\sim C99A \\sim F3 \\sim C98 \\sim C99 \\sim C100 \\sim
C104 \\sim C103 \\sim C101 \\sim C102 \\sim C105 \\sim C1A \\sim C1B \\sim C1C
\\sim C1D: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C91 \\sim C91A \\sim N3 \\sim C87A \\sim C87 \\sim C99A \\sim C99: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C107 \\sim C47 \\sim C47A \\sim N8 \\sim N8A \\sim C106 \\sim C109 \\sim C113
\\sim C110 \\sim C112 \\sim C108 \\sim C114 \\sim C1E \\sim C1F \\sim C1G \\sim
C111 \\sim C1I \\sim C1H \\sim C115 \\sim C45A \\sim C45 \\sim C20: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N8 \\sim N8A \\sim C107 \\sim C116: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F12 \\sim F12A \\sim P2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C21 \\sim C89 \\sim C89A \\sim C21A \\sim C23 \\sim C93 \\sim C95 \\sim C93A
\\sim C23A \\sim C95A \\sim C73: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Sof(C93A)=Sof(H93A)=Sof(C95A)=Sof(H95A)=Sof(C23A)=Sof(H23A)=Sof(C89A)=
 Sof(H89A)=Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(C21)=Sof(H21)=Sof(C89)=Sof(H89)=Sof(C23)=Sof(H23)=Sof(C93)=Sof(H93)=
 Sof(C95)=Sof(H95)=FVAR(1)
 Sof(Cu5A)=1-FVAR(2)
 Sof(Cu5)=FVAR(2)
 Fixed Sof: F12(0.5) F3(0.5) F7(0.5) F2(0.5) C87(0.5) H87A(0.5) H87B(0.5)
 C45(0.5) F9(0.5) C91(0.5) H91A(0.5) H91B(0.5) H91C(0.5) F5(0.5) C47(0.5)
 H47A(0.5) H47B(0.5) F11(0.5) C45A(0.5) C47A(0.5) H47C(0.5) H47D(0.5) N8(0.5)
 N8A(0.5) F7A(0.5) F11A(0.5) F5A(0.5) F9A(0.5) F2A(0.5) C99(0.5) H99A(0.5)
 H99B(0.5) C100(0.5) H100(0.5) C104(0.5) H104(0.5) C103(0.5) H103(0.5)
 C101(0.5) H101(0.5) C102(0.5) H102(0.5) C99A(0.5) H99C(0.5) H99D(0.5)
 C105(0.5) H105(0.5) C1A(0.5) H1AA(0.5) C1B(0.5) H1BA(0.5) C1C(0.5) H1C(0.5)
 C1D(0.5) H1D(0.5) C106(0.5) H10A(0.5) H10B(0.5) C107(0.5) H10C(0.5) H10D(0.5)
 H10E(0.5) C109(0.5) H109(0.5) C113(0.5) H113(0.5) C110(0.5) H110(0.5)
 C112(0.5) H112(0.5) C108(0.5) C114(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5)
 C1G(0.5) H1G(0.5) C111(0.5) H111(0.5) C1I(0.5) H1I(0.5) C1H(0.5) H1H(0.5)
 C91A(0.5) H91D(0.5) H91E(0.5) H91F(0.5) C87A(0.5) H87C(0.5) H87D(0.5) F3A(0.5)
 F12A(0.5) C115(0.5) H11A(0.5) H11B(0.5) C116(0.5) H11C(0.5) H11D(0.5)
 H11E(0.5) Cl2(0.25) Cl1(0.25) C2A(0.25) H2AA(0.25) H2AB(0.25) Cl3(0.25)
 Cl4(0.25) C117(0.25) H11F(0.25) H11G(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C51(H51A,H51B), C13(H13A,H13B), C87(H87A,H87B),
 C47(H47A,H47B), C47A(H47C,H47D), C99(H99A,H99B), C99A(H99C,H99D), C106(H10A,
 H10B), C87A(H87C,H87D), C115(H11A,H11B), C2A(H2AA,H2AB), C117(H11F,H11G)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C18(H18), C24(H24), C26(H26), C30(H30), C32(H32),
 C36(H36), C40(H40), C42(H42), C44(H44), C54(H54), C56(H56), C60(H60), C64(H64),
  C70(H70), C72(H72), C78(H78), C80(H80), C82(H82), C84(H84), C86(H86),
 C88(H88), C92(H92), C94(H94), C96(H96), C97(H97), C49(H49), C53(H53), C27(H27),
  C55(H55), C7(H7), C57(H57), C29(H29), C59(H59), C15(H15), C61(H61), C31(H31),
 C63(H63), C65(H65), C33(H33), C67(H67), C17(H17), C69(H69), C35(H35), C71(H71),
  C9(H9), C37(H37), C75(H75), C19(H19), C77(H77), C39(H39), C79(H79), C5(H5),
 C81(H81), C41(H41), C83(H83), C21(H21), C85(H85), C43(H43), C11(H11), C89(H89),
  C23(H23), C93(H93), C95(H95), C3(H3), C93A(H93A), C95A(H95A), C23A(H23A),
 C89A(H89A), C21A(H21A), C100(H100), C104(H104), C103(H103), C101(H101),
 C102(H102), C105(H105), C1A(H1AA), C1B(H1BA), C1C(H1C), C1D(H1D), C109(H109),
 C113(H113), C110(H110), C112(H112), C1E(H1E), C1F(H1F), C1G(H1G), C111(H111),
 C1I(H1I), C1H(H1H)
5.c Fitted hexagon refined as free rotating group:
 C114(C1E,C1F,C1G,C111,C1I)
5.d Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C25(H25A,H25B,H25C), C91(H91A,H91B,H91C), C107(H10C,H10D,
 H10E), C91A(H91D,H91E,H91F), C116(H11C,H11D,H11E)
;
_shelx_res_checksum              62493
_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
;