Synthesis, characterization, and green to orange luminescence properties of copper(i) complexes with 3-bdppmapy ligand-containing phenanthroline and its derivatives
Mou, Wen-Long; Fan, Si-Jie; Wang, Ying-Long; Wang, Guo; Hu, Fu-Zhen; Guo, Gui-Xiong; Han, Hong-Liang; Xin, Xiu-Lan; Liu, Jian-Ming; Yang, Yu-Ping; Li, Zhong-Feng; Jin, Qiong-Hua; CrystEngComm 27 (2025) 2086–2100; doi:10.1039/D4CE01324G

data_7250008
_publ_section_title
;
 Synthesis, characterization, and green to orange luminescence properties
 of copper(i) complexes with 3-bdppmapy ligand-containing phenanthroline
 and its derivatives
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2086
_journal_page_last               2100
_journal_paper_doi               10.1039/D4CE01324G
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C45 H36 Cu N6 P2, Cl O4, C H4 O'
_chemical_formula_sum            'C46 H40 Cl Cu N6 O5 P2'
_chemical_formula_weight         917.77
_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             2022-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2024-10-21 deposited with the CCDC.	2025-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                85.4870(10)
_cell_angle_beta                 82.2100(10)
_cell_angle_gamma                88.5300(10)
_cell_formula_units_Z            2
_cell_length_a                   11.86660(10)
_cell_length_b                   13.4149(2)
_cell_length_c                   13.5834(2)
_cell_measurement_reflns_used    17801
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.0340
_cell_measurement_theta_min      4.4830
_cell_volume                     2135.49(5)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.966
_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    -89.00  20.00   0.50    1.00    --    0.00 -57.00-120.00  218
  2  \w    -13.00  89.00   0.50    1.00    --    0.00  37.00  30.00  204
  3  \w    -13.00  89.00   0.50    1.00    --    0.00  37.00 -30.00  204
  4  \w    -84.00 -17.00   0.50    1.00    --    0.00 -19.00 120.00  134
  5  \w     23.00  88.00   0.50    1.00    --    0.00  57.00  90.00  130
  6  \w    -20.00  15.00   0.50    1.00    --    0.00  57.00  90.00   70
  7  \w    -38.00   2.00   0.50    1.00    --    0.00 -19.00 -60.00   80
  8  \w    145.00 179.00   0.50    1.00    --   94.00  60.00 160.11   68
  9  \w     77.00 136.00   0.50    1.00    --   94.00  60.00 160.11  118
 10  \w      5.00  65.00   0.50    1.00    --   94.00 -82.00   0.00  120
 11  \w     53.00 116.00   0.50    1.00    --   94.00 -82.00 -60.00  126
 12  \w      5.00 121.00   0.50    1.00    --   94.00 -82.00-150.00  232
 13  \w    109.00 169.00   0.50    1.00    --   94.00  45.00 150.00  120
 14  \w      9.00  50.00   0.50    1.00    --   94.00 -45.00-150.00   82
 15  \w      6.00 114.00   0.50    1.00    --   94.00 -61.00-150.00  216
 16  \w      7.00 115.00   0.50    1.00    --   94.00 -61.00  60.00  216
 17  \w     93.00 161.00   0.50    1.00    --   94.00  15.00 120.00  136
 18  \w     46.00 103.00   0.50    1.00    --   94.00 -61.00 -60.00  114
 19  \w      9.00 123.00   0.50    1.00    --   94.00 -82.00  60.00  228
 20  \w     72.00  98.00   0.50    1.00    --   94.00 -82.00   0.00   52
 21  \w     66.00 109.00   0.50    1.00    --   94.00 -82.00 150.00   86
 22  \w     27.00  98.00   0.50    1.00    --   94.00 -15.00-150.00  142
;
_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      0.0201156000
_diffrn_orient_matrix_UB_12      -0.0767576000
_diffrn_orient_matrix_UB_13      0.0865826000
_diffrn_orient_matrix_UB_21      -0.0645347000
_diffrn_orient_matrix_UB_22      -0.0790257000
_diffrn_orient_matrix_UB_23      -0.0458630000
_diffrn_orient_matrix_UB_31      0.1122676000
_diffrn_orient_matrix_UB_32      -0.0337137000
_diffrn_orient_matrix_UB_33      -0.0598317000
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24693
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.447
_diffrn_reflns_theta_min         4.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55652
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0044(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0554P)^2^+0.7823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7821
_reflns_number_total             8414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01324g2.cif
_cod_data_source_block           hfz-99
_cod_depositor_comments
'Adding full bibliography for 7250002--7250009.cif.'
_cod_database_code               7250008
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 P1 Cl1 O1 Cu1'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.640
_reflns_odcompleteness_completeness 99.66
_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.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C)
2.d Idealised tetrahedral OH refined as rotating group:
 O47(H47)
;
_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 2.661
_oxdiff_exptl_absorpt_empirical_full_min 0.546