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_7243757
_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         'I, C55 H44 Cu N4 P2, C H4 O'
_chemical_formula_sum            'C56 H48 Cu I N4 O P2'
_chemical_formula_weight         1045.36
_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             2021-07-05
_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                 94.1090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.35360(10)
_cell_length_b                   20.0276(2)
_cell_length_c                   16.8454(2)
_cell_measurement_reflns_used    20243
_cell_measurement_temperature    132.99(10)
_cell_measurement_theta_max      73.6630
_cell_measurement_theta_min      4.1820
_cell_volume                     4830.07(8)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      132.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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    -26.00   0.00   0.50    0.50    --    0.00 -37.00-150.00   52
  2  \w    -87.00 -28.00   0.50    0.50    --    0.00 -37.00-150.00  118
  3  \w    -89.00 -19.00   0.50    0.50    --    0.00 -37.00 -90.00  140
  4  \w    -43.00   8.00   0.50    0.50    --    0.00 -37.00 -30.00  102
  5  \w    111.00 181.00   0.50    2.00    --   94.60  61.00  30.00  140
  6  \w     42.00 125.00   0.50    2.00    --   94.60 -82.00 -90.00  166
  7  \w     80.00 107.00   0.50    2.00    --   94.60 -82.00-150.00   54
  8  \w     14.00 111.00   0.50    2.00    --   94.60 -30.00 -60.00  194
  9  \w      5.00 117.00   0.50    2.00    --   94.60 -61.00 -90.00  224
 10  \w     25.00  79.00   0.50    2.00    --   94.60 -45.00 -30.00  108
 11  \w     11.00  77.00   0.50    2.00    --   94.60 -77.00-120.00  132
 12  \w     78.00 182.00   0.50    2.00    --   94.60  30.00 120.00  208
;
_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      0.0132483000
_diffrn_orient_matrix_UB_12      -0.0517383000
_diffrn_orient_matrix_UB_13      -0.0659087000
_diffrn_orient_matrix_UB_21      -0.0064230000
_diffrn_orient_matrix_UB_22      0.0560146000
_diffrn_orient_matrix_UB_23      -0.0628280000
_diffrn_orient_matrix_UB_31      0.1066029000
_diffrn_orient_matrix_UB_32      0.0098474000
_diffrn_orient_matrix_UB_33      0.0110555000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29402
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.818
_diffrn_reflns_theta_min         3.434
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32120
_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    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+8.2746P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9126
_reflns_number_total             9504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01132d2.cif
_cod_data_source_block           20171208-1
_cod_depositor_comments
'Adding full bibliography for 7243753--7243757.cif.'
_cod_database_code               7243757
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C20 H35 N6 P4 Cu1'
_reflns_odcompleteness_completeness 99.79
_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:
 C44(H44A,H44B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C11(H11), C14(H14), C2(H2), C12(H12), C9(H9), C30(H30),
 C18(H18), C46(H46), C53(H53), C24(H24), C38(H38), C26(H26), C55(H55), C54(H54),
  C42(H42), C20(H20), C15(H15), C36(H36), C16(H16), C32(H32), C40(H40),
 C51(H51), C21(H21), C47(H47), C17(H17), C23(H23), C39(H39), C52(H52), C33(H33),
  C29(H29), C27(H27), C41(H41), C22(H22), C49(H49), C28(H28), C35(H35),
 C48(H48), C34(H34)
2.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              83877
_shelx_hkl_checksum              74432
_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 2.166
_oxdiff_exptl_absorpt_empirical_full_min 0.451