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_7717317
_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 Br Cu N3 P3'
_chemical_formula_sum            'C79 H58 Br Cu N3 P3'
_chemical_formula_weight         1285.64
_chemical_name_systematic        123
_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                 96.7570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7946(2)
_cell_length_b                   13.5185(2)
_cell_length_c                   37.9095(6)
_cell_measurement_reflns_used    21657
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4420
_cell_measurement_theta_min      2.3630
_cell_volume                     7020.35(18)
_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 0.994
_diffrn_measured_fraction_theta_max 0.951
_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     50.00  75.00   0.50    0.47    --   47.64  71.00-115.00   50
  2  \w     94.00 162.00   0.50    1.89    --  106.49  15.00-150.00  136
  3  \w     99.00 177.00   0.50    1.89    --  106.49  15.00-180.00  156
  4  \w     95.00 175.00   0.50    1.89    --  106.49  71.00-115.00  160
  5  \w    106.00 138.00   0.50    1.89    --  106.49  15.00   0.00   64
  6  \w    127.00 164.00   0.50    1.89    --  106.49  45.00 120.00   74
  7  \w   -107.00 -28.00   0.50    0.47    --  -47.64 -71.00 113.00  158
  8  \w    -75.00 -50.00   0.50    1.89    --  -86.25  71.00-115.00   50
  9  \w    -49.00 -15.00   0.50    1.89    --  -86.25  45.00  60.00   68
 10  \w    -48.00 -16.00   0.50    1.89    --  -86.25  45.00  90.00   64
 11  \w   -120.00 -95.00   0.50    0.47    --  -47.64-125.00 -60.00   50
 12  \w   -120.00 -81.00   0.50    0.47    --  -47.64-125.00-120.00   78
 13  \w     -3.00  55.00   0.50    0.47    --   47.64 -71.00 113.00  116
 14  \w     39.00  69.00   0.50    1.89    --  106.49 -61.00 150.00   60
 15  \w     34.00  88.00   0.50    1.89    --  106.49 -71.00 113.00  108
 16  \w     39.00  71.00   0.50    1.89    --  106.49 -61.00  30.00   64
 17  \w     40.00  70.00   0.50    1.89    --  106.49 -61.00   0.00   60
 18  \w     47.00  79.00   0.50    1.89    --  106.49 -77.00 -30.00   64
 19  \w     34.00  60.00   0.50    1.89    --  106.49 -61.00 -90.00   52
 20  \w     42.00  68.00   0.50    1.89    --  106.49 -61.00-120.00   52
 21  \w     37.00  71.00   0.50    1.89    --  106.49 -61.00-180.00   68
 22  \w     36.00  62.00   0.50    1.89    --  106.49 -61.00  60.00   52
 23  \w     34.00  60.00   0.50    1.89    --  106.49 -61.00-150.00   52
 24  \w     38.00  70.00   0.50    1.89    --  106.49 -61.00 -30.00   64
 25  \w    -67.00  25.00   0.50    0.47    --  -47.64  71.00-115.00  184
 26  \w     49.00  96.00   0.50    1.89    --  106.49 -94.00-180.00   94
;
_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      -0.0340977000
_diffrn_orient_matrix_UB_12      -0.0910541000
_diffrn_orient_matrix_UB_13      0.0196647000
_diffrn_orient_matrix_UB_21      -0.0984086000
_diffrn_orient_matrix_UB_22      0.0018968000
_diffrn_orient_matrix_UB_23      -0.0238717000
_diffrn_orient_matrix_UB_31      0.0424350000
_diffrn_orient_matrix_UB_32      -0.0685831000
_diffrn_orient_matrix_UB_33      -0.0267707000
_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  0.0671
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            45974
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.830
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51283
_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            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00014(3)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         14089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.1005
_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^)+(0.0433P)^2^+106.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2436
_refine_ls_wR_factor_ref         0.2484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12001
_reflns_number_total             14089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           li-cz-s1-br
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.773
_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.a Aromatic/amide H refined with riding coordinates:
 C68(H68), C70(H70), C30(H30), C45(H45), C71(H71), C27(H27), C37(H37),
 C40(H40), C51(H51), C39(H39), C77(H77), C65(H65), C33(H33), C31(H31), C43(H43),
  C64(H64), C78(H78), C66(H66), C52(H52), C15(H15), C62(H62), C75(H75),
 C57(H57), C41(H41), C63(H63), C48(H48), C42(H42), C36(H36), C21(H21), C55(H55),
  C76(H76), C17(H17), C18(H18), C58(H58), C34(H34), C46(H46), C35(H35),
 C49(H49), C54(H54), C47(H47), C1(H1), C9(H9), C16(H16), C24(H24), C53(H53),
 C60(H60), C12(H12), C59(H59), C22(H22), C23(H23), C5(H5), C11(H11), C10(H10),
 C4(H4), C6(H6)
2.b Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C)
;
_shelx_res_checksum              62366
_shelx_fab_checksum              36634
_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 1.705
_oxdiff_exptl_absorpt_empirical_full_min 0.589