Synthesis and luminescent properties of three excellent yellow emissive Cu(i) complexes based on the diphosphine ligand and the diimine ligand
Mou, Wen-Long; Gao, Cheng-Jie; Li, Zi-Xi; Fan, Si-Jie; Hou, Chuan-Bin; Zhao, Jing-Tong; Zhang, Shuai; Li, Zhong-Feng; Han, Hong-Liang; Duan, Chun-Bo; Wang, Guo; Jin, Qiong-Hua; CrystEngComm 26 (2024) 2297–2305; doi:10.1039/D4CE00206G

data_7248359
_publ_section_title
;
 Synthesis and luminescent properties of three excellent yellow emissive
 Cu(i) complexes based on the diphosphine ligand and the diimine ligand
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2297
_journal_page_last               2305
_journal_paper_doi               10.1039/D4CE00206G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C46 H36 Cl Cu N2 O P2, C H2 Cl2, C H4 O'
_chemical_formula_sum            'C48 H42 Cl3 Cu N2 O2 P2'
_chemical_formula_weight         910.66
_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
_audit_creation_date             2022-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-09 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.52970(10)
_cell_length_b                   19.3980(2)
_cell_length_c                   15.05820(10)
_cell_measurement_reflns_used    14114
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.9550
_cell_measurement_theta_min      4.4010
_cell_volume                     4468.09(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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      5.00  88.00   0.50    1.00    --    0.00  19.00 150.00  166
  2  \w    -66.00  12.00   0.50    1.00    --    0.00 -37.00   0.00  156
  3  \w     35.00  61.00   0.50    1.00    --    0.00  19.00  90.00   52
  4  \w     -5.00  31.00   0.50    1.00    --    0.00  19.00 -60.00   72
  5  \w    -14.00  19.00   0.50    1.00    --    0.00  37.00  60.00   66
  6  \w     90.00 182.00   0.50    4.00    --   94.00  77.00  90.00  184
  7  \w     75.00 111.00   0.50    4.00    --   94.00 -45.00 -30.00   72
  8  \w     11.00 105.00   0.50    4.00    --   94.00 -15.00 -60.00  188
  9  \w    149.00 183.00   0.50    4.00    --   94.00  45.00-150.00   68
 10  \w     91.00 126.00   0.50    4.00    --   94.00  45.00-150.00   70
 11  \w     25.00 117.00   0.50    4.00    --   94.00 -77.00 -60.00  184
 12  \w     41.00 106.00   0.50    4.00    --   94.00 -30.00 -60.00  130
 13  \w     25.00  87.00   0.50    4.00    --   94.00 -15.00  90.00  124
 14  \w     81.00 107.00   0.50    4.00    --   94.00 -82.00 -90.00   52
 15  \w      5.00  45.00   0.50    4.00    --   94.00 -82.00 -90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0136935000
_diffrn_orient_matrix_UB_12      -0.0727216000
_diffrn_orient_matrix_UB_13      0.0411501000
_diffrn_orient_matrix_UB_21      0.0996409000
_diffrn_orient_matrix_UB_22      0.0083379000
_diffrn_orient_matrix_UB_23      0.0073815000
_diffrn_orient_matrix_UB_31      0.0053266000
_diffrn_orient_matrix_UB_32      0.0308154000
_diffrn_orient_matrix_UB_33      0.0950734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.401
_diffrn_reflns_theta_min         4.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.076
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8854
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1306P)^2^+2.6053P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7585
_reflns_number_total             8854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00206g12.cif
_cod_data_source_block           lzx-148
_cod_depositor_comments
'Adding full bibliography for 7248357--7248359.cif.'
_cod_database_code               7248359
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N O P Cu Cl'
_shelx_estimated_absorpt_t_max   0.514
_shelx_estimated_absorpt_t_min   0.415
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2. Restrained distances
 O2-C48
 1.43 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C32(H32), C2(H2), C21(H21), C23(H23), C22(H22), C36(H36),
 C11(H11), C20(H20), C15(H15), C37(H37), C30(H30), C6(H6), C38(H38), C16(H16),
 C26(H26), C17(H17), C40(H40), C33(H33), C8(H8), C10(H10), C35(H35), C43(H43),
 C3(H3), C41(H41), C34(H34), C5(H5), C9(H9), C28(H28), C27(H27), C45(H45),
 C42(H42), C29(H29), C4(H4), C46(H46)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              14693
_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 1.684
_oxdiff_exptl_absorpt_empirical_full_min 0.604