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_7717318
_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 Cl Cu N3 P3'
_chemical_formula_sum            'C79 H58 Cl Cu N3 P3'
_chemical_formula_weight         1241.18
_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                 97.2860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.87700(10)
_cell_length_b                   13.53800(10)
_cell_length_c                   37.2607(3)
_cell_measurement_reflns_used    33906
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4810
_cell_measurement_theta_min      3.2620
_cell_volume                     6943.53(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.967
_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     45.00  92.00   0.50    0.07    --   47.70  44.00  63.00   94
  2  \w     94.00 178.00   0.50    0.28    --  106.49  61.00 120.00  168
  3  \w     93.00 178.00   0.50    0.28    --  106.49  44.00  63.00  170
  4  \w     96.00 140.00   0.50    0.28    --  106.49  30.00-180.00   88
  5  \w     40.00  75.00   0.50    0.28    --  106.49 -94.00 -60.00   70
  6  \w     77.00 104.00   0.50    0.28    --  106.49 -94.00 -60.00   54
  7  \w     53.00 105.00   0.50    0.28    --  106.49 -94.00   0.00  104
  8  \w     35.00  81.00   0.50    0.28    --  106.49 -94.00  30.00   92
  9  \w     56.00 100.00   0.50    0.28    --  106.49 -94.00  60.00   88
 10  \w     40.00 101.00   0.50    0.28    --  106.49 -77.00 150.00  122
 11  \w     44.00  70.00   0.50    0.28    --  106.49 -61.00 150.00   52
 12  \w     34.00  67.00   0.50    0.28    --  106.49 -61.00  60.00   66
 13  \w     36.00  62.00   0.50    0.28    --  106.49 -61.00   0.00   52
 14  \w     40.00  71.00   0.50    0.28    --  106.49 -61.00 -60.00   62
 15  \w     44.00  69.00   0.50    0.28    --  106.49 -61.00 -90.00   50
 16  \w     40.00  82.00   0.50    0.28    --  106.49 -77.00-120.00   84
 17  \w     -9.00  17.00   0.50    0.07    --   47.70 -44.00 -86.00   52
 18  \w     37.00  70.00   0.50    0.28    --  106.49 -61.00-180.00   66
 19  \w    -27.00  28.00   0.50    0.07    --  -47.70  19.00-150.00  110
 20  \w    -43.00 -18.00   0.50    0.28    --  -86.25  45.00-120.00   50
 21  \w    -49.00 -22.00   0.50    0.28    --  -86.25  45.00 -90.00   54
 22  \w    -42.00  24.00   0.50    0.07    --  -47.70  44.00  63.00  132
 23  \w    -49.00 -24.00   0.50    0.28    --  -86.25  44.00  63.00   50
 24  \w   -140.00-115.00   0.50    0.28    --  -86.25 -44.00 -86.00   50
 25  \w   -120.00 -53.00   0.50    0.07    --  -47.70 -44.00 -86.00  134
 26  \w   -111.00 -74.00   0.50    0.07    --  -47.70-125.00-150.00   74
 27  \w   -113.00 -73.00   0.50    0.07    --  -47.70-125.00  60.00   80
;
_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      0.0902214000
_diffrn_orient_matrix_UB_12      -0.0616945000
_diffrn_orient_matrix_UB_13      0.0140884000
_diffrn_orient_matrix_UB_21      0.0390673000
_diffrn_orient_matrix_UB_22      0.0126955000
_diffrn_orient_matrix_UB_23      -0.0366092000
_diffrn_orient_matrix_UB_31      0.0535452000
_diffrn_orient_matrix_UB_32      0.0947359000
_diffrn_orient_matrix_UB_33      0.0141080000
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            52922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.791
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90148
_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    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00010(2)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         14156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0530P)^2^+5.1022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12950
_reflns_number_total             14156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           li-cz-s1-cl
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717318
_shelx_shelxl_version_number     2018/3
_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:
 C12(H12), C51(H51), C54(H54), C67(H67), C10(H10), C25(H25), C34(H34),
 C64(H64), C9(H9), C46(H46), C44(H44), C32(H32), C66(H66), C37(H37), C21(H21),
 C18(H18), C72(H72), C24(H24), C35(H35), C19(H19), C4(H4), C36(H36), C79(H79),
 C39(H39), C1(H1), C60(H60), C49(H49), C15(H15), C31(H31), C43(H43), C65(H65),
 C2(H2), C27(H27), C48(H48), C17(H17), C3(H3), C68(H68), C23(H23), C56(H56),
 C16(H16), C22(H22), C59(H59), C47(H47), C42(H42), C75(H75), C78(H78), C40(H40),
  C41(H41), C74(H74), C30(H30), C77(H77), C73(H73), C28(H28), C58(H58), C29(H29)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              93749
_shelx_fab_checksum              57393
_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 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.785