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_7717322
_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 Cu I N4 P3, C H2 Cl2'
_chemical_formula_sum            'C87 H65 Cl2 Cu I N4 P3'
_chemical_formula_weight         1520.68
_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             2023-07-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-07-30 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                98.9400(10)
_cell_angle_beta                 100.9360(10)
_cell_angle_gamma                97.5010(10)
_cell_formula_units_Z            2
_cell_length_a                   10.38730(10)
_cell_length_b                   15.8741(2)
_cell_length_c                   24.5313(3)
_cell_measurement_reflns_used    28256
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.6200
_cell_measurement_theta_min      2.8390
_cell_volume                     3869.47(8)
_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 0.962
_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     92.00 129.00   0.50    0.91    --  106.49  61.00  60.00   74
  2  \w    153.00 178.00   0.50    0.91    --  106.49  61.00  60.00   50
  3  \w    112.00 154.00   0.50    0.91    --  106.49  45.00 150.00   84
  4  \w     83.00 178.00   0.50    0.91    --  106.49  78.00 157.00  190
  5  \w    135.00 177.00   0.50    0.91    --  106.49  30.00 120.00   84
  6  \w     95.00 120.00   0.50    0.23    --   47.70  78.00 157.00   50
  7  \w     46.00  72.00   0.50    0.23    --   47.70  78.00 157.00   52
  8  \w     93.00 177.00   0.50    0.91    --  106.49  15.00  90.00  168
  9  \w    134.00 166.00   0.50    0.91    --  106.49  30.00-120.00   64
 10  \w    104.00 129.00   0.50    0.91    --  106.49  30.00-120.00   50
 11  \w     36.00 162.00   0.50    0.91    --  106.49   0.00  30.00  252
 12  \w    -70.00  23.00   0.50    0.23    --  -47.70  78.00 157.00  186
 13  \w    -26.00  28.00   0.50    0.23    --  -47.70  19.00 150.00  108
 14  \w    -23.00  27.00   0.50    0.23    --  -47.70  19.00 -90.00  100
 15  \w    -26.00  25.00   0.50    0.23    --   47.70 -19.00 -60.00  102
 16  \w     34.00  60.00   0.50    0.91    --  106.49 -61.00-180.00   52
 17  \w     21.00  61.00   0.50    0.23    --   47.70 -78.00  32.00   80
 18  \w     41.00  68.00   0.50    0.91    --  106.49 -61.00  60.00   54
 19  \w     55.00  97.00   0.50    0.91    --  106.49 -78.00  32.00   84
 20  \w    -85.00 -14.00   0.50    0.23    --  -47.70 125.00 -60.00  142
 21  \w     35.00  62.00   0.50    0.91    --  106.49 -77.00 -60.00   54
 22  \w     42.00  67.00   0.50    0.91    --  106.49 -61.00-150.00   50
 23  \w    123.00 174.00   0.50    0.91    --  106.49 125.00  90.00  102
 24  \w     34.00 107.00   0.50    0.91    --  106.49-115.00 150.10  146
 25  \w     40.00  84.00   0.50    0.23    --   47.70-125.00 120.00   88
 26  \w     53.00 108.00   0.50    0.91    --  106.49-110.00  58.17  110
 27  \w     54.00 111.00   0.50    0.91    --  106.49-125.00   0.00  114
 28  \w     36.00  86.00   0.50    0.91    --  106.49 -94.00 -90.00  100
 29  \w     67.00  99.00   0.50    0.91    --  106.49 -94.00-120.00   64
 30  \w     40.00 107.00   0.50    0.91    --  106.49-104.00-141.33  134
 31  \w     37.00 105.00   0.50    0.91    --  106.49-125.00-180.00  136
 32  \w     71.00 111.00   0.50    0.91    --  106.49-125.00-120.00   80
 33  \w     35.00  78.00   0.50    0.91    --  106.49-125.00 -90.00   86
 34  \w   -106.00 -25.00   0.50    0.23    --  -47.70 -78.00  32.00  162
 35  \w   -135.00-110.00   0.50    0.91    --  -86.25 -78.00  32.00   50
 36  \w     40.00 105.00   0.50    0.91    --  106.49-125.00  60.00  130
 37  \w     85.00 110.00   0.50    0.91    --  106.49-125.00  30.00   50
 38  \w     45.00  72.00   0.50    0.91    --  106.49-125.00  30.00   54
 39  \w     82.00 111.00   0.50    0.91    --  106.49-125.00 150.00   58
 40  \w     46.00  74.00   0.50    0.91    --  106.49-125.00 150.00   56
 41  \w   -142.00 -97.00   0.50    0.91    --  -86.25 -94.00  90.00   90
 42  \w    -50.00 -16.00   0.50    0.91    --  -86.25  78.00 157.00   68
 43  \w    -50.00 -20.00   0.50    0.91    --  -86.25  45.00 -30.00   60
 44  \w    -44.00 -15.00   0.50    0.91    --  -86.25  45.00 -60.00   58
;
_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      0.0884097000
_diffrn_orient_matrix_UB_12      -0.0704127000
_diffrn_orient_matrix_UB_13      0.0046094000
_diffrn_orient_matrix_UB_21      0.0431076000
_diffrn_orient_matrix_UB_22      0.0158446000
_diffrn_orient_matrix_UB_23      -0.0547764000
_diffrn_orient_matrix_UB_31      0.1173954000
_diffrn_orient_matrix_UB_32      0.0686487000
_diffrn_orient_matrix_UB_33      0.0348491000
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53253
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.790
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49493
_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    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         15702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+7.0211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14170
_reflns_number_total             15702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           cz-s2-i
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717322
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Cu I'
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C83(H83A,H83B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C18(H18), C22(H22), C26(H26), C32(H32), C36(H36), C38(H38),
 C40(H40), C44(H44), C46(H46), C50(H50), C54(H54), C56(H56), C58(H58), C62(H62),
  C66(H66), C74(H74), C82(H82), C84(H84), C86(H86), C11(H11), C23(H23),
 C47(H47), C3(H3), C25(H25), C13(H13), C53(H53), C27(H27), C55(H55), 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), C9(H9), C73(H73),
 C37(H37), C19(H19), C77(H77), C39(H39), C79(H79), C5(H5), C81(H81), C41(H41),
 C21(H21), C85(H85), C43(H43)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C75(H75A,H75B,H75C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65887
_shelx_fab_checksum              94272
_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.676