Study on the luminescence properties of ionic [Cu(N^N)(P^P)]+ complexes: influence of ligands, counteranions and weak interactions
Li, Zi-Xi; Sun, Zhen-Zhou; Wang, Guo; Yang, Wei; Han, Hong-Liang; Yang, Yu-Ping; Li, Zhong-Feng; Dai, Lixiong; Yao, Yi-Shan; Jin, Qiong-Hua; CrystEngComm  (2022) –; doi:10.1039/D2CE01177H

data_7245716
_publ_section_title
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 Study on the luminescence properties of ionic [Cu(N^N)(P^P)]+ complexes:
 influence of ligands, counteranions and weak interactions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01177H
_journal_year                    2022
_chemical_formula_moiety         'Br, C45 H36 Cu N6 P2, 3(C H4 O)'
_chemical_formula_sum            'C48 H48 Br Cu N6 O3 P2'
_chemical_formula_weight         962.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-05-25 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.3040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.94130(10)
_cell_length_b                   16.47510(10)
_cell_length_c                   21.8307(2)
_cell_measurement_reflns_used    15381
_cell_measurement_temperature    286(6)
_cell_measurement_theta_max      74.0760
_cell_measurement_theta_min      4.3250
_cell_volume                     4579.44(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 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_environment      air
_diffrn_ambient_temperature      286(6)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_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    -15.00  12.00   0.50    0.50    --    0.00  77.00-150.00   54
  2  \w     55.00  89.00   0.50    0.50    --    0.00  82.00 -60.00   68
  3  \w    -29.00  41.00   0.50    0.50    --    0.00  82.00 -60.00  140
  4  \w     41.00  68.00   0.50    0.50    --    0.00  77.00-150.00   54
  5  \w    -89.00 -16.00   0.50    0.50    --    0.00 -77.00 120.00  146
  6  \w     12.00 105.00   0.50    1.00    --   94.00 -30.00   0.00  186
  7  \w      8.00 102.00   0.50    1.00    --   94.00 -15.00 -90.00  188
  8  \w     60.00  87.00   0.50    1.00    --   94.00 -15.00   0.00   54
  9  \w      7.00 102.00   0.50    1.00    --   94.00 -61.00-120.00  190
 10  \w     48.00 113.00   0.50    1.00    --   94.00 -61.00 -30.00  130
 11  \w     66.00 108.00   0.50    1.00    --   94.00 -77.00-180.00   84
 12  \w      6.00 105.00   0.50    1.00    --   94.00 -30.00 -90.00  198
 13  \w     68.00 122.00   0.50    1.00    --   94.00 -82.00-127.33  108
 14  \w     78.00 104.00   0.50    1.00    --   94.00 -82.00-180.00   52
 15  \w     12.00  38.00   0.50    1.00    --   94.00 -82.00-127.33   52
;
_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      0.0896676000
_diffrn_orient_matrix_UB_12      -0.0056452000
_diffrn_orient_matrix_UB_13      -0.0376988000
_diffrn_orient_matrix_UB_21      0.0808955000
_diffrn_orient_matrix_UB_22      0.0140610000
_diffrn_orient_matrix_UB_23      0.0599185000
_diffrn_orient_matrix_UB_31      0.0068967000
_diffrn_orient_matrix_UB_32      -0.0923018000
_diffrn_orient_matrix_UB_33      0.0114607000
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.464
_diffrn_reflns_theta_min         4.117
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28125
_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    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9111
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0980P)^2^+1.5087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7885
_reflns_number_total             9111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01177h2.cif
_cod_data_source_block           zn-769
_cod_database_code               7245716
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu1 Br1 C1 H1 N1 P1'
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.515
_reflns_odcompleteness_completeness 99.88
_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
 C1-O47 = C2-O46 = O3-C48
 1.43 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B)
3.b Aromatic/amide H refined with riding coordinates:
 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), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3A), O46(H46A), 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 2.175
_oxdiff_exptl_absorpt_empirical_full_min 0.528