Heteroleptic mononuclear Cu(I) halide complexes containing carbazolyl substituted phenyl diphosphine and monophosphine: structures and photophysical and electroluminescent properties.
Chen, Zhun; Xu, Wei; Zhu, Ruiqin; Liu, Li; Zhong, Xin-Xin; Li, Fa-Bao; Zhou, Guijiang; Qin, Hai-Mei; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19299–19313; doi:10.1039/d4dt02469a

data_7717316
_publ_section_title
;
 Heteroleptic mononuclear Cu(I) halide complexes containing carbazolyl
 substituted phenyl diphosphine and monophosphine: structures and
 photophysical and electroluminescent properties.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19299
_journal_page_last               19313
_journal_paper_doi               10.1039/d4dt02469a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C79 H58 Cu I N3 P3'
_chemical_formula_sum            'C79 H58 Cu I N3 P3'
_chemical_formula_weight         1332.63
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-07-17 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.79570(10)
_cell_length_b                   13.57050(10)
_cell_length_c                   38.2006(4)
_cell_measurement_reflns_used    34459
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5230
_cell_measurement_theta_min      3.2620
_cell_volume                     7107.68(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_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    -79.00 -38.00   0.50    0.43    --  -86.25  91.00 -61.00   82
  2  \w    -76.00   9.00   0.50    0.11    --  -47.70  91.00 -61.00  170
  3  \w    100.00 178.00   0.50    0.43    --  106.49  30.00-120.00  156
  4  \w    101.00 178.00   0.50    0.43    --  106.49  91.00 -61.00  154
  5  \w     95.00 156.00   0.50    0.43    --  106.49  30.00  30.00  122
  6  \w    -51.00 -26.00   0.50    0.43    --  -86.25  45.00 120.00   50
  7  \w    -27.00  22.00   0.50    0.11    --  -47.70  19.00-150.00   98
  8  \w   -138.00-100.00   0.50    0.43    --  -86.25 -30.00-150.00   76
  9  \w   -118.00 -86.00   0.50    0.11    --  -47.70-125.00 -90.00   64
 10  \w   -140.00-113.00   0.50    0.43    --  -86.25 -91.00-174.00   54
 11  \w   -119.00 -79.00   0.50    0.11    --  -47.70-125.00 -60.00   80
 12  \w   -118.00 -73.00   0.50    0.11    --  -47.70-125.00 -30.00   90
 13  \w   -117.00 -73.00   0.50    0.11    --  -47.70-125.00  60.00   88
 14  \w     38.00 106.00   0.50    0.43    --  106.49 -77.00-120.00  136
 15  \w     52.00  92.00   0.50    0.43    --  106.49 -77.00-150.00   80
 16  \w     34.00  71.00   0.50    0.43    --  106.49 -61.00 -60.00   74
 17  \w     34.00  59.00   0.50    0.43    --  106.49 -61.00 -30.00   50
 18  \w     34.00  66.00   0.50    0.43    --  106.49 -61.00  30.00   64
 19  \w     44.00  71.00   0.50    0.43    --  106.49 -61.00  60.00   54
 20  \w     37.00  67.00   0.50    0.43    --  106.49 -61.00  90.00   60
 21  \w     60.00 101.00   0.50    0.43    --  106.49-125.00  30.00   82
 22  \w    -16.00  29.00   0.50    0.11    --   47.70 -91.00-174.00   90
 23  \w     34.00  71.00   0.50    0.43    --  106.49-125.00-180.00   74
 24  \w     63.00 101.00   0.50    0.43    --  106.49 -91.00-174.00   76
 25  \w     34.00  97.00   0.50    0.43    --  106.49 -94.00-150.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286647000
_diffrn_orient_matrix_UB_12      0.0492482000
_diffrn_orient_matrix_UB_13      -0.0336996000
_diffrn_orient_matrix_UB_21      -0.0598187000
_diffrn_orient_matrix_UB_22      0.0918360000
_diffrn_orient_matrix_UB_23      0.0076389000
_diffrn_orient_matrix_UB_31      0.0906559000
_diffrn_orient_matrix_UB_32      0.0450730000
_diffrn_orient_matrix_UB_33      0.0212868000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            53829
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.826
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.000074(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         14432
_refine_ls_number_restraints     768
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+11.3393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13252
_reflns_number_total             14432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           li-cz-s1-i
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717316
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N3, C67A, C77A, C37, C73A, C39, C65A, C65, C69A, C19, C75A, C33, N3A, C73,
 C33A, C67, C17A, C75, C35A, C17, C37A, C77, C19A, C69, C39A, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C67A \\sim C77A \\sim C37 \\sim C73A \\sim C39 \\sim C65A \\sim C65
\\sim C69A \\sim C19 \\sim C75A \\sim C33 \\sim N3A \\sim C73 \\sim C33A \\sim
C67 \\sim C17A \\sim C75 \\sim C35A \\sim C17 \\sim C37A \\sim C77 \\sim C19A
\\sim C69 \\sim C39A \\sim C35: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 N3, C37, C39, C65, C19, C33, C73, C67, C75, C17, C77, C69, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N3A, C37A, C39A, C65A, C19A, C33A, C73A, C67A, C75A, C17A, C77A, C69A, C35A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(N3A)=Sof(C65A)=Sof(H65A)=Sof(C33A)=Sof(H33A)=Sof(C67A)=Sof(H67A)=
 Sof(C17A)=Sof(H17A)=Sof(C69A)=Sof(C35A)=Sof(C73A)=Sof(H73A)=Sof(C37A)=
 Sof(C75A)=Sof(C19A)=Sof(H19A)=Sof(C77A)=Sof(H77A)=Sof(C39A)=Sof(H39A)=1-FVAR(1)
 Sof(N3)=Sof(C65)=Sof(H65)=Sof(C33)=Sof(H33)=Sof(C67)=Sof(H67)=Sof(C17)=
 Sof(H17)=Sof(C69)=Sof(C35)=Sof(C73)=Sof(H73)=Sof(C37)=Sof(C75)=Sof(C19)=
 Sof(H19)=Sof(C77)=Sof(H77)=Sof(C39)=Sof(H39)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12), C20(H20), C22(H22), C24(H24), C28(H28), C34(H34), C38(H38),
 C40(H40), C44(H44), C46(H46), C48(H48), C52(H52), C54(H54), C56(H56), C62(H62),
  C68(H68), C70(H70), C72(H72), C74(H74), C76(H76), C78(H78), C79(H79), C5(H5),
 C41(H41), C21(H21), C43(H43), C11(H11), C23(H23), C47(H47), C3(H3), C25(H25),
 C51(H51), C13(H13), C53(H53), C55(H55), C7(H7), C57(H57), C29(H29), C59(H59),
 C15(H15), C61(H61), C31(H31), C63(H63), C2(H2), C65(H65), C33(H33), C67(H67),
 C17(H17), C71(H71), C9(H9), C73(H73), C19(H19), C77(H77), C39(H39), C65A(H65A),
  C33A(H33A), C67A(H67A), C17A(H17A), C73A(H73A), C19A(H19A), C77A(H77A),
 C39A(H39A)
6.b Fitted hexagon refined as free rotating group:
 C65(C33,C67,C17,C69,C35), C73(C37,C75,C19,C77,C39), C65A(C33A,C67A,C17A,C69A,
 C35A), C73A(C37A,C75A,C19A,C77A,C39A)
6.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70295
_shelx_fab_checksum              84968
_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 1.352
_oxdiff_exptl_absorpt_empirical_full_min 0.775