A series of luminescent Cu(i) complexes based on the diphosphine ligand and diimine ligand: weak intermolecular interactions, terahertz spectroscopy and photoproperties
Li, Zi-Xi; Kuang, Xiao-Nan; Wang, Guo; Zhu, Ning; Sun, Zhen-Zhou; Han, Hong-Liang; Yang, Yu-Ping; Li, Zhong-Feng; Xin, Xiu-Lan; Jin, Qiong-Hua; Ren, Zhi-Gang; CrystEngComm 23 (2021) 8323–8333; doi:10.1039/D1CE01132D

data_7243754
_publ_section_title
;
 A series of luminescent Cu(i) complexes based on the diphosphine ligand
 and diimine ligand: weak intermolecular interactions, terahertz
 spectroscopy and photoproperties
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              8323
_journal_page_last               8333
_journal_paper_doi               10.1039/D1CE01132D
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C55 H44 Cu N4 P2, B F4, 0.27(C H4 O)'
_chemical_formula_sum            'C55.27 H45.07 B Cu F4 N4 O0.27 P2'
_chemical_formula_weight         981.81
_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     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
;
2021-08-17 deposited with the CCDC.	2021-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0114(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5279(3)
_cell_length_b                   19.7802(4)
_cell_length_c                   16.4881(3)
_cell_measurement_reflns_used    8057
_cell_measurement_temperature    105.2
_cell_measurement_theta_max      29.3208
_cell_measurement_theta_min      2.9850
_cell_volume                     4731.56(16)
_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      105.2
_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  -35.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.8148   77.0000   90.0000 87

  2 omega   30.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273   77.0000    0.0000 59

  3 omega  -23.00    7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -37.0000  120.0000 30

  4 omega  -19.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -77.0000  120.0000 67

  5 omega   -4.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273   37.0000  -90.0000 89
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0466402000
_diffrn_orient_matrix_UB_12      0.0023444000
_diffrn_orient_matrix_UB_13      -0.0104437000
_diffrn_orient_matrix_UB_21      0.0075032000
_diffrn_orient_matrix_UB_22      0.0263029000
_diffrn_orient_matrix_UB_23      0.0288290000
_diffrn_orient_matrix_UB_31      0.0126230000
_diffrn_orient_matrix_UB_32      -0.0242538000
_diffrn_orient_matrix_UB_33      0.0302581000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25470
_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         25.026
_diffrn_reflns_theta_min         2.991
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88572
_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    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             2027
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.053
_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     653
_refine_ls_number_reflns         8355
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0245P)^2^+3.7552P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7010
_reflns_number_total             8355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01132d2.cif
_cod_data_source_block           exp_4284
_cod_depositor_comments
'Adding full bibliography for 7243753--7243757.cif.'
_cod_original_cell_volume        4731.53(15)
_cod_database_code               7243754
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 99.78
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 F3-B1 \\sim F4-B1 \\sim F5-B2 \\sim F6-B2
 with sigma of 0.02
3. Rigid bond restraints
 F5, B2, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F3, B1, F4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(F4)=Sof(F3)=Sof(B1)=1-FVAR(1)
 Sof(B2)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C25(H25A,H25B)
5.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C11(H11), C37(H37), C1(H1), C12(H12), C18(H18), C36(H36), C52(H52),
 C53(H53), C2(H2), C49(H49), C31(H31), C45(H45), C29(H29), C39(H39), C51(H51),
 C46(H46), C28(H28), C17(H17), C43(H43), C42(H42), C24(H24), C10(H10), C34(H34),
  C35(H35), C48(H48), C9(H9), C47(H47), C40(H40), C14(H14), C20(H20), C30(H30),
 C21(H21), C41(H41), C16(H16), C23(H23), C55(H55), C22(H22), C15(H15), C54(H54)
5.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              86105
_shelx_hkl_checksum              33128
_olex2_submission_special_instructions 'No special instructions were received'