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_7717321
_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         'C86 H63 Br Cu N4 P3'
_chemical_formula_sum            'C86 H63 Br Cu N4 P3'
_chemical_formula_weight         1388.76
_chemical_name_systematic        0.11
_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
_audit_creation_date             2023-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-02 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.8150(10)
_cell_angle_beta                 100.9750(10)
_cell_angle_gamma                97.9910(10)
_cell_formula_units_Z            2
_cell_length_a                   10.35530(10)
_cell_length_b                   16.0837(3)
_cell_length_c                   24.9522(2)
_cell_measurement_reflns_used    30073
_cell_measurement_temperature    293
_cell_measurement_theta_max      75.8990
_cell_measurement_theta_min      2.8040
_cell_volume                     3983.40(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_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   -119.00 -45.00   0.50    0.40    --  -47.70 -51.00  46.00  148
  2  \w    -43.00  25.00   0.50    0.40    --  -47.70  51.00-167.00  136
  3  \w    -13.00  58.00   0.50    0.40    --   47.70 -51.00  46.00  142
  4  \w     58.00  88.00   0.50    0.40    --   47.70  51.00-167.00   60
  5  \w   -156.00-104.00   0.50    1.61    --  -86.25 -51.00  46.00  104
  6  \w    -54.00 -17.00   0.50    1.61    --  -86.25  51.00-167.00   74
  7  \w     93.00 178.00   0.50    1.61    --  106.49  51.00-167.00  170
  8  \w   -118.00 -73.00   0.50    0.40    --  -47.70-125.00   0.00   90
  9  \w    -25.00  28.00   0.50    0.40    --  -47.70  19.00 -60.00  106
 10  \w   -116.00 -73.00   0.50    0.40    --  -47.70-125.00-180.00   86
 11  \w     60.00  95.00   0.50    0.40    --   47.70-125.00  90.00   70
 12  \w    -49.00 -15.00   0.50    1.61    --  -86.25  45.00  30.00   68
 13  \w    -69.00 -15.00   0.50    1.61    --  -86.25  61.00-120.00  108
 14  \w   -133.00-107.00   0.50    1.61    --  -86.25 -94.00-180.00   52
 15  \w    -70.00 -26.00   0.50    1.61    --  -86.25  61.00   0.00   88
 16  \w    -48.00 -16.00   0.50    1.61    --  -86.25  45.00 -90.00   64
 17  \w   -133.00 -72.00   0.50    1.61    --  -86.25 -15.00  60.00  122
 18  \w     35.00 106.00   0.50    1.61    --  106.49 -77.00 -90.00  142
 19  \w     35.00  70.00   0.50    1.61    --  106.49 -61.00  60.00   70
 20  \w     38.00  68.00   0.50    1.61    --  106.49 -61.00   0.00   60
 21  \w    122.00 174.00   0.50    1.61    --  106.49  30.00 -30.00  104
 22  \w     48.00 109.00   0.50    1.61    --  106.49-125.00  30.00  122
 23  \w     79.00 111.00   0.50    1.61    --  106.49-125.00  60.00   64
 24  \w     68.00 110.00   0.50    1.61    --  106.49-125.00 150.00   84
 25  \w     34.00  68.00   0.50    1.61    --  106.49 -61.00  30.00   68
 26  \w    147.00 175.00   0.50    1.61    --  106.49 125.00-180.00   56
 27  \w     96.00 135.00   0.50    1.61    --  106.49 125.00-180.00   78
 28  \w     40.00  66.00   0.50    1.61    --  106.49 -77.00 150.00   52
 29  \w     78.00 104.00   0.50    1.61    --  106.49 -77.00 150.00   52
 30  \w     93.00 177.00   0.50    1.61    --  106.49  15.00 -60.00  168
 31  \w     98.00 138.00   0.50    1.61    --  106.49  15.00 150.00   80
 32  \w    145.00 172.00   0.50    1.61    --  106.49  15.00 150.00   54
 33  \w     38.00  99.00   0.50    1.61    --  106.49 -94.00 -60.00  122
 34  \w     70.00 111.00   0.50    1.61    --  106.49-125.00 -90.00   82
 35  \w     95.00 139.00   0.50    1.61    --  106.49 125.00  30.00   88
 36  \w     98.00 124.00   0.50    1.61    --  106.49  30.00   0.00   52
 37  \w    147.00 172.00   0.50    1.61    --  106.49  30.00   0.00   50
 38  \w     38.00  63.00   0.50    1.61    --  106.49-125.00 -90.00   50
 39  \w     74.00 108.00   0.50    1.61    --  106.49-110.00 -25.88   68
 40  \w     40.00  65.00   0.50    1.61    --  106.49-110.00 -25.88   50
 41  \w     73.00 107.00   0.50    1.61    --  106.49-103.00 130.76   68
 42  \w     53.00 104.00   0.50    1.61    --  106.49-105.00 103.12  102
 43  \w     39.00 104.00   0.50    1.61    --  106.49 -94.00-120.00  130
 44  \w     34.00  92.00   0.50    1.61    --  106.49 -77.00   0.00  116
 45  \w     41.00  66.00   0.50    1.61    --  106.49 -61.00  90.00   50
 46  \w     40.00 104.00   0.50    1.61    --  106.49 -94.00 150.00  128
 47  \w     82.00 107.00   0.50    1.61    --  106.49-105.00-120.59   50
 48  \w     43.00  69.00   0.50    1.61    --  106.49 -61.00-150.00   52
;
_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      -0.1183257000
_diffrn_orient_matrix_UB_12      0.0384971000
_diffrn_orient_matrix_UB_13      0.0159721000
_diffrn_orient_matrix_UB_21      -0.0955115000
_diffrn_orient_matrix_UB_22      -0.0829590000
_diffrn_orient_matrix_UB_23      -0.0286088000
_diffrn_orient_matrix_UB_31      0.0228358000
_diffrn_orient_matrix_UB_32      -0.0354948000
_diffrn_orient_matrix_UB_33      0.0547293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57274
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.681
_diffrn_reflns_theta_min         2.814
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25038
_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    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         16170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+0.6010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13530
_reflns_number_total             16170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           1217-cz-s2
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717321
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Si Br P'
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.792
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C4(H4), C9(H9), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C26(H26), C30(H30), C31(H31), C33(H33), C36(H36), C39(H39), C40(H40), C41(H41),
  C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
  C75(H75), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86)
2.b Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C78(H78A,H78B,H78C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70156
_shelx_fab_checksum              65299
_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 3.898
_oxdiff_exptl_absorpt_empirical_full_min 0.429