Designing luminescent diimine-Cu(i)–phosphine complexes by tuning N-ligand and counteranions: correlation of weak interactions, luminescence and THz absorption spectra
Sun, Zhen-Zhou; Zhu, Ning; Pan, Xun; Hu, Fu-Zhen; Wang, Guo; Yang, Yu-Ping; Qiu, Qi-Ming; Li, Zhong-Feng; Xin, Xiu-Lan; Liu, Jian-Ming; Li, Xiao-Qi; Jin, Qiong-Hua; Ren, Zhi-Gang; Zhou, Qing-Li; CrystEngComm  (2022) –; doi:10.1039/D1CE01574E

data_7244261
_publ_section_title
;
 Designing luminescent diimine-Cu(i)--phosphine complexes by tuning
 N-ligand and counteranions: correlation of weak interactions,
 luminescence and THz absorption spectra
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01574E
_journal_year                    2022
_chemical_formula_moiety         'C43 H36 Cu N4 P2, B F4'
_chemical_formula_sum            'C43 H36 B Cu F4 N4 P2'
_chemical_formula_weight         821.05
_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     direct
_audit_creation_date             2019-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-02 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                88.298(2)
_cell_angle_beta                 73.809(3)
_cell_angle_gamma                87.479(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5699(5)
_cell_length_b                   12.5429(3)
_cell_length_c                   13.6715(4)
_cell_measurement_reflns_used    6188
_cell_measurement_temperature    106.7
_cell_measurement_theta_max      29.3135
_cell_measurement_theta_min      3.1296
_cell_volume                     1903.16(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      106.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -44.00   13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.9711   77.0000  150.0000 57

  2 omega   -8.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       21.2836   77.0000   90.0000 38

  3 omega  -51.00   41.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       21.2836  -37.0000   60.0000 92

  4 omega   -5.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       21.2836   77.0000  -30.0000 91

  5 omega  -46.00   50.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       21.2836  -77.0000 -150.0000 96
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0627954000
_diffrn_orient_matrix_UB_12      0.0077348000
_diffrn_orient_matrix_UB_13      -0.0118767000
_diffrn_orient_matrix_UB_21      0.0094944000
_diffrn_orient_matrix_UB_22      -0.0537784000
_diffrn_orient_matrix_UB_23      0.0143335000
_diffrn_orient_matrix_UB_31      0.0068919000
_diffrn_orient_matrix_UB_32      -0.0159116000
_diffrn_orient_matrix_UB_33      -0.0507255000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12067
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0262P)^2^+1.0842P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6025
_reflns_number_total             6711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01574e2.cif
_cod_data_source_block           exp_4283
_cod_original_cell_volume        1903.17(12)
_cod_database_code               7244261
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.739
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 F3, B1, F4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F5, B2, F6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
B1 \\sim F3 \\sim F4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F5 \\sim B2 \\sim F6: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Sof(F6)=Sof(F5)=Sof(B2)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(B1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C25(H25), C39(H39), C16(H16), C17(H17), C3(H3), C24(H24), C11(H11),
 C1(H1), C8(H8), C43(H43), C2(H2), C34(H34), C35(H35), C41(H41), C31(H31),
 C12(H12), C30(H30), C27(H27), C18(H18), C37(H37), C9(H9), C10(H10), C21(H21),
 C36(H36), C22(H22), C40(H40), C19(H19), C42(H42), C23(H23), C29(H29), C28(H28)
;
_shelx_res_checksum              19273
_shelx_hkl_checksum              80085
_olex2_submission_special_instructions 'No special instructions were received'