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_7243756
_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         'Br, C55 H44 Cu N4 P2, 2(C H4 O)'
_chemical_formula_sum            'C57 H52 Br Cu N4 O2 P2'
_chemical_formula_weight         1030.41
_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                 105.9070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.90440(10)
_cell_length_b                   19.1935(2)
_cell_length_c                   21.5471(3)
_cell_measurement_reflns_used    46871
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.6220
_cell_measurement_theta_min      4.3200
_cell_volume                     4734.71(9)
_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      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    -31.00  89.00   0.50    0.50    --    0.00  82.00-120.00  240
  2  \w    -89.00  22.00   0.50    0.50    --    0.00 -57.00 -90.00  222
  3  \w    -17.00  89.00   0.50    0.50    --    0.00  37.00 -30.00  212
  4  \w    -17.00  89.00   0.50    0.50    --    0.00  37.00 -60.00  212
  5  \w    -17.00  89.00   0.50    0.50    --    0.00  37.00 150.00  212
  6  \w      7.00  69.00   0.50    1.50    --   94.60 -61.00  90.00  124
  7  \w     26.00  70.00   0.50    1.50    --   94.60 -45.00-150.00   88
  8  \w     80.00 106.00   0.50    1.50    --   94.60 -82.00-150.00   52
  9  \w     53.00 125.00   0.50    1.50    --   94.60 -82.00 -60.00  144
 10  \w     48.00  75.00   0.50    1.50    --   94.60 -82.00  60.00   54
 11  \w     12.00 111.00   0.50    1.50    --   94.60 -30.00-150.00  198
 12  \w      7.00  38.00   0.50    1.50    --   94.60 -82.00 -60.00   62
 13  \w      5.00 105.00   0.50    1.50    --   94.60 -61.00 150.00  200
 14  \w     78.00 107.00   0.50    1.50    --   94.60 -82.00   0.00   58
 15  \w     99.00 172.00   0.50    1.50    --   94.60  59.00-164.78  146
 16  \w      6.00 117.00   0.50    1.50    --   94.60 -61.00 -60.00  222
 17  \w    109.00 173.00   0.50    1.50    --   94.60  45.00-180.00  128
 18  \w      6.00 124.00   0.50    1.50    --   94.60 -82.00 150.00  236
 19  \w      6.00  99.00   0.50    1.50    --   94.60 -82.00  90.00  186
 20  \w      6.00  58.00   0.50    1.50    --   94.60 -82.00   0.00  104
 21  \w     95.00 165.00   0.50    1.50    --   94.60  53.00 137.38  140
;
_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      -0.0439965000
_diffrn_orient_matrix_UB_12      0.0550848000
_diffrn_orient_matrix_UB_13      -0.0529946000
_diffrn_orient_matrix_UB_21      0.0211260000
_diffrn_orient_matrix_UB_22      0.0574556000
_diffrn_orient_matrix_UB_23      0.0518202000
_diffrn_orient_matrix_UB_31      0.1255318000
_diffrn_orient_matrix_UB_32      0.0097195000
_diffrn_orient_matrix_UB_33      -0.0055114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53574
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.052
_diffrn_reflns_theta_min         3.866
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64735
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.287
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.097
_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     608
_refine_ls_number_reflns         9462
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0674P)^2^+11.8708P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9102
_reflns_number_total             9462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01132d2.cif
_cod_data_source_block           zn-567
_cod_depositor_comments
'Adding full bibliography for 7243753--7243757.cif.'
_cod_database_code               7243756
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'Cu1 Br1 C1 H1 N1 P1'
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.350
_reflns_odcompleteness_completeness 99.78
_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
 O2-C57
 1.43 with sigma of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C36(H36), C40(H40), C8(H8), C41(H41), C11(H11), C32(H32), C30(H30),
 C27(H27), C49(H49), C55(H55), C18(H18), C35(H35), C42(H42), C1(H1), C26(H26),
 C24(H24), C20(H20), C12(H12), C23(H23), C14(H14), C33(H33), C2(H2), C21(H21),
 C45(H45), C46(H46), C29(H29), C22(H22), C51(H51), C17(H17), C34(H34), C48(H48),
  C47(H47), C43(H43), C15(H15), C28(H28), C52(H52), C16(H16), C54(H54), C53(H53)
3.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C56(H56A,H56B,H56C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O1(H1A)
;
_shelx_res_checksum              13666
_shelx_hkl_checksum              18610
_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 4.324
_oxdiff_exptl_absorpt_empirical_full_min 0.319