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_7717320
_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 Br Cu N2 P3, C H2 Cl2'
_chemical_formula_sum            'C73 H55 Br Cl2 Cu N2 P3'
_chemical_formula_weight         1267.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-24
_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                90
_cell_angle_beta                 94.0320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.31050(10)
_cell_length_b                   16.27350(10)
_cell_length_c                   37.9409(2)
_cell_measurement_reflns_used    32887
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5100
_cell_measurement_theta_min      2.3460
_cell_volume                     6350.27(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 2014/5 (Sheldrick, 2014)'
_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 0.995
_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     51.00  76.00   0.50    0.06    --   47.70  65.00 -94.00   50
  2  \w     97.00 123.00   0.50    0.26    --  106.49  30.00-150.00   52
  3  \w    101.00 177.00   0.50    0.26    --  106.49  15.00-180.00  152
  4  \w    147.00 174.00   0.50    0.26    --  106.49  30.00-150.00   54
  5  \w     89.00 154.00   0.50    0.26    --  106.49  65.00 -94.00  130
  6  \w     97.00 161.00   0.50    0.26    --  106.49  15.00  30.00  128
  7  \w     36.00  94.00   0.50    0.06    --   47.70-125.00 120.00  116
  8  \w    -44.00 -18.00   0.50    0.26    --  -86.25  45.00  90.00   52
  9  \w    -46.00 -14.00   0.50    0.26    --  -86.25  45.00  60.00   64
 10  \w    -63.00  22.00   0.50    0.06    --  -47.70  65.00 -94.00  170
 11  \w    -51.00 -25.00   0.50    0.26    --  -86.25  45.00-120.00   52
 12  \w    -67.00 -19.00   0.50    0.26    --  -86.25  65.00 -94.00   96
 13  \w    -65.00 -39.00   0.50    0.06    --  -47.70 -65.00 129.00   52
 14  \w   -119.00 -75.00   0.50    0.06    --  -47.70-125.00 -60.00   88
 15  \w   -159.00-116.00   0.50    0.26    --  -86.25 -94.00-150.00   86
 16  \w   -159.00-103.00   0.50    0.26    --  -86.25-125.00 -30.00  112
 17  \w   -138.00-113.00   0.50    0.26    --  -86.25 -65.00 129.00   50
 18  \w   -113.00 -69.00   0.50    0.06    --  -47.70 -65.00 129.00   88
 19  \w     35.00  85.00   0.50    0.26    --  106.49 -77.00 -30.00  100
 20  \w     34.00 105.00   0.50    0.26    --  106.49 -77.00 120.00  142
 21  \w     34.00  74.00   0.50    0.26    --  106.49 -65.00 129.00   80
 22  \w     37.00  71.00   0.50    0.26    --  106.49 -61.00  60.00   68
 23  \w     44.00  71.00   0.50    0.26    --  106.49 -61.00 -30.00   54
 24  \w     37.00  62.00   0.50    0.26    --  106.49 -61.00 -90.00   50
 25  \w     43.00 105.00   0.50    0.26    --  106.49 -77.00-150.00  124
 26  \w     35.00  60.00   0.50    0.26    --  106.49 -61.00-180.00   50
 27  \w    140.00 169.00   0.50    0.26    --  106.49 125.00  60.00   58
 28  \w     95.00 122.00   0.50    0.26    --  106.49 125.00  60.00   54
 29  \w      2.00  27.00   0.50    0.06    --   47.70 -65.00 129.00   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      -0.0762370000
_diffrn_orient_matrix_UB_12      0.0679350000
_diffrn_orient_matrix_UB_13      -0.0207531000
_diffrn_orient_matrix_UB_21      -0.0713034000
_diffrn_orient_matrix_UB_22      0.0213564000
_diffrn_orient_matrix_UB_23      0.0331501000
_diffrn_orient_matrix_UB_31      0.1074431000
_diffrn_orient_matrix_UB_32      0.0623759000
_diffrn_orient_matrix_UB_33      0.0112675000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            52968
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.704
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48555
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.653
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0433P)^2^+6.3430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11760
_reflns_number_total             12814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02469a2.cif
_cod_data_source_block           xw-s2-br
_cod_depositor_comments
'Adding full bibliography for 7717316--7717322.cif.'
_cod_database_code               7717320
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.462
_shelx_estimated_absorpt_t_min   0.311
_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:
 C73(H73A,H73B)
2.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C45(H45), C18(H18), C30(H30), C6(H6), C20(H20), C71(H71), C38(H38),
 C62(H62), C58(H58), C42(H42), C2(H2), C5(H5), C50(H50), C57(H57), C36(H36),
 C40(H40), C59(H59), C56(H56), C29(H29), C26(H26), C39(H39), C24(H24), C12(H12),
  C8(H8), C32(H32), C33(H33), C63(H63), C41(H41), C21(H21), C10(H10), C70(H70),
 C51(H51), C3(H3), C53(H53), C9(H9), C69(H69), C68(H68), C17(H17), C27(H27),
 C22(H22), C35(H35), C28(H28), C34(H34), C52(H52), C4(H4), C11(H11), C23(H23),
 C65(H65), C64(H64), C14(H14), C16(H16), C15(H15)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93629
_shelx_fab_checksum              84611
_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 1.977
_oxdiff_exptl_absorpt_empirical_full_min 0.691