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_7717319
_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         'C72 H53 Cl Cu N2 P3, 3(C H2 Cl2)'
_chemical_formula_sum            'C75 H59 Cl7 Cu N2 P3'
_chemical_formula_weight         1392.84
_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             2022-07-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                106.0020(10)
_cell_angle_beta                 95.2810(10)
_cell_angle_gamma                97.9430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.05020(10)
_cell_length_b                   14.4627(2)
_cell_length_c                   24.4386(3)
_cell_measurement_reflns_used    32628
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      76.1990
_cell_measurement_theta_min      3.2080
_cell_volume                     3350.08(7)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(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 0.960
_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     94.00 178.00   0.50    0.24    --  106.49  45.00-150.00  168
  2  \w     94.00 173.00   0.50    0.24    --  106.49  30.00 -90.00  158
  3  \w     95.00 168.00   0.50    0.24    --  106.49  45.00   0.00  146
  4  \w    117.00 173.00   0.50    0.24    --  106.49  15.00 120.00  112
  5  \w    147.00 173.00   0.50    0.24    --  106.49  61.00 150.00   52
  6  \w     99.00 132.00   0.50    0.24    --  106.49  61.00 150.00   66
  7  \w    106.00 135.00   0.50    0.24    --  106.49 139.00 156.00   58
  8  \w    114.00 139.00   0.50    0.24    --  106.49 130.00 -16.00   50
  9  \w     95.00 127.00   0.50    0.24    --  106.49 125.00 -60.00   64
 10  \w    135.00 177.00   0.50    0.24    --  106.49 125.00 -60.00   84
 11  \w    -26.00  27.00   0.50    0.06    --  -47.70  19.00 -60.00  106
 12  \w    -25.00  26.00   0.50    0.06    --  -47.70  19.00   0.00  102
 13  \w    -26.00  28.00   0.50    0.06    --  -47.70  19.00  60.00  108
 14  \w    -40.00 -15.00   0.50    0.24    --  -86.25  45.00 120.00   50
 15  \w    -18.00   9.00   0.50    0.06    --  -47.70  19.00 150.00   54
 16  \w     37.00  67.00   0.50    0.24    --  106.49 -61.00  60.00   60
 17  \w     34.00  59.00   0.50    0.24    --  106.49 -61.00  90.00   50
 18  \w     41.00  68.00   0.50    0.24    --  106.49 -61.00 120.00   54
 19  \w     36.00  61.00   0.50    0.24    --  106.49 -61.00 150.00   50
 20  \w    -18.00  25.00   0.50    0.06    --   47.70 -19.00 150.00   86
 21  \w     43.00  88.00   0.50    0.24    --  106.49 -77.00 120.00   90
 22  \w     45.00 106.00   0.50    0.24    --  106.49 -77.00   0.00  122
 23  \w     41.00  66.00   0.50    0.24    --  106.49 -61.00 -60.00   50
 24  \w     39.00  68.00   0.50    0.24    --  106.49 -61.00 -90.00   58
 25  \w     39.00  71.00   0.50    0.24    --  106.49 -61.00-120.00   64
 26  \w    121.00 177.00   0.50    0.24    --  106.49 125.00   0.00  112
 27  \w     76.00 104.00   0.50    0.24    --  106.49 -94.00  90.00   56
 28  \w     87.00 122.00   0.50    0.24    --  106.49-139.00  96.00   70
 29  \w     46.00 103.00   0.50    0.06    --   47.70-139.00  96.00  114
 30  \w     67.00 104.00   0.50    0.24    --  106.49 -94.00 -30.00   74
 31  \w     78.00 113.00   0.50    0.24    --  106.49-130.00 -89.00   70
 32  \w     37.00  94.00   0.50    0.06    --   47.70-130.00 -89.00  114
 33  \w     35.00 111.00   0.50    0.24    --  106.49-125.00 -60.00  152
 34  \w     35.00 106.00   0.50    0.24    --  106.49-107.00 -30.34  142
 35  \w     81.00 108.00   0.50    0.24    --  106.49-125.00 120.00   54
 36  \w     35.00  60.00   0.50    0.24    --  106.49-125.00 120.00   50
 37  \w     46.00 107.00   0.50    0.24    --  106.49-104.00 140.18  122
 38  \w     37.00  69.00   0.50    0.24    --  106.49 -94.00  90.00   64
 39  \w     59.00  84.00   0.50    0.24    --  106.49 -94.00  30.00   50
 40  \w    -88.00 -63.00   0.50    0.24    --  -86.25 -77.00 -60.00   50
 41  \w   -104.00 -69.00   0.50    0.24    --  -86.25 -77.00   0.00   70
 42  \w   -104.00 -72.00   0.50    0.24    --  -86.25 -61.00 -30.00   64
 43  \w   -135.00-109.00   0.50    0.24    --  -86.25 -61.00 -30.00   52
 44  \w   -149.00-116.00   0.50    0.24    --  -86.25 -77.00   0.00   66
 45  \w   -159.00-107.00   0.50    0.24    --  -86.25 -77.00 -60.00  104
 46  \w   -115.00 -72.00   0.50    0.06    --  -47.70-130.00 -89.00   86
 47  \w   -137.00 -99.00   0.50    0.24    --  -86.25-130.00 -89.00   76
 48  \w   -102.00 -73.00   0.50    0.06    --  -47.70-139.00  96.00   58
 49  \w   -115.00 -75.00   0.50    0.06    --  -47.70-125.00 120.00   80
 50  \w   -116.00 -90.00   0.50    0.24    --  -86.25-139.00  96.00   52
 51  \w    -76.00 -51.00   0.50    0.06    --  -47.70 139.00 156.00   50
 52  \w    -82.00 -57.00   0.50    0.24    --  -86.25 139.00 156.00   50
 53  \w    -77.00 -52.00   0.50    0.06    --  -47.70 130.00 -16.00   50
 54  \w    -77.00 -52.00   0.50    0.24    --  -86.25 130.00 -16.00   50
 55  \w    -41.00 -16.00   0.50    0.24    --  -86.25 125.00 -60.00   50
;
_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      0.0563992000
_diffrn_orient_matrix_UB_12      -0.0837674000
_diffrn_orient_matrix_UB_13      -0.0397000000
_diffrn_orient_matrix_UB_21      0.0746537000
_diffrn_orient_matrix_UB_22      -0.0184264000
_diffrn_orient_matrix_UB_23      0.0529220000
_diffrn_orient_matrix_UB_31      -0.1251248000
_diffrn_orient_matrix_UB_32      -0.0727492000
_diffrn_orient_matrix_UB_33      0.0023813000
_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  0.1070
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49036
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.603
_diffrn_reflns_theta_min         3.226
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56699
_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    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.338
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1475P)^2^+3.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2272
_refine_ls_wR_factor_ref         0.2362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11664
_reflns_number_total             13539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           wza-s2-cl
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717319
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Cu Cl'
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C73(H73A,H73B), C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C24(H24), C36(H36), C38(H38), C40(H40), C44(H44), C48(H48),
 C50(H50), C54(H54), C58(H58), C60(H60), C62(H62), C64(H64), C66(H66), C68(H68),
  C70(H70), C72(H72), C74(H74), C75(H75), C19(H19), C39(H39), C5(H5), C21(H21),
 C43(H43), C11(H11), C45(H45), C23(H23), C47(H47), C3(H3), C49(H49), C25(H25),
 C51(H51), C13(H13), C53(H53), C27(H27), 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), C69(H69), C35(H35), C71(H71)
;
_shelx_res_checksum              14727
_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 3.508
_oxdiff_exptl_absorpt_empirical_full_min 0.415