Terahertz time-domain absorption spectra of Cu(I) complexes bearing tetraphosphine ligands: the bridge between the C-Hπ and ππ interactions and photoluminescence properties.
Pan, Xun; Kuang, Xiao-Nan; Zhu, Ning; Wang, Guo; Yang, Yu-Ping; Liu, Jian-Ming; Li, Zhong-Feng; Xin, Xiu-Lan; Han, Hong-Liang; Jin, Qiong-Hua; Ren, Zhi-Gang; Zhang, Jiang-Wei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14941–14950; doi:10.1039/d0dt02542a

data_7705544
_publ_section_title
;
 Terahertz time-domain absorption spectra of Cu(I) complexes bearing
 tetraphosphine ligands: the bridge between the C-H\p and \p\p
 interactions and photoluminescence properties.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14941
_journal_page_last               14950
_journal_paper_doi               10.1039/d0dt02542a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(C41 H38 Cu N3 P2), 2(Cl O4), 1.302(C H2 Cl2), 1.698(C4 H10 O)'
_chemical_formula_sum            'C90.1 H95.59 Cl4.61 Cu2 N6 O9.7 P4'
_chemical_formula_weight         1831.85
_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
_audit_creation_date             2020-08-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-01 deposited with the CCDC.	2020-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                98.591(2)
_cell_angle_beta                 97.338(2)
_cell_angle_gamma                90.613(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5137(4)
_cell_length_b                   14.6165(3)
_cell_length_c                   22.3671(6)
_cell_measurement_reflns_used    7176
_cell_measurement_temperature    108.30(10)
_cell_measurement_theta_max      27.5620
_cell_measurement_theta_min      3.3620
_cell_volume                     4330.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      108.30(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -18.00   19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000   90.0000 37

  2 omega  -11.00   18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000  -30.0000 29

  3 omega    0.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000  -90.0000 26

  4 omega  -24.00   24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000 -150.0000 48

  5 omega  -47.00   34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -57.0000   60.0000 81

  6 omega  -35.00   28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -39.0000  -94.0000 63

  7 omega   59.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   37.0000 -120.0000 27

  8 omega   29.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210   57.0000 -180.0000 25

  9 omega   41.00   88.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  178.0000 -150.0000 47

 10 omega   52.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  178.0000   90.0000 39

 11 omega  -50.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -37.0000  150.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0430376000
_diffrn_orient_matrix_UB_12      -0.0016165000
_diffrn_orient_matrix_UB_13      -0.0152165000
_diffrn_orient_matrix_UB_21      0.0034026000
_diffrn_orient_matrix_UB_22      0.0490703000
_diffrn_orient_matrix_UB_23      0.0047640000
_diffrn_orient_matrix_UB_31      0.0306496000
_diffrn_orient_matrix_UB_32      -0.0006017000
_diffrn_orient_matrix_UB_33      0.0281470000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.995
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         16996
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+10.4154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12502
_reflns_number_total             16996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02542a6.cif
_cod_data_source_block           exp_5403
_cod_depositor_comments
'Adding full bibliography for 7705544--7705547.cif.'
_cod_original_formula_sum        'C90.10 H95.59 Cl4.61 Cu2 N6 O9.70 P4'
_cod_database_code               7705544
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.780
_reflns_odcompleteness_completeness 99.81
_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
2. Restrained distances
 Cl5-C92 = Cl6-C92
 1.754 with sigma of 0.001
 C89-C88 = C90-C91
 1.49 with sigma of 0.001
 O10-C88 = O10-C90
 1.42 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(Cl6) = Uanis(C92) = Uanis(Cl5)
Uanis(C89) = Uanis(C88) = Uanis(O10) = Uanis(C90) = Uanis(C91)
4. Others
 Sof(Cl6)=Sof(Cl5)=Sof(C92)=Sof(H92A)=Sof(H92B)=1-FVAR(1)
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(O10)=Sof(C88)=Sof(H88A)=Sof(H88B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C28(H28A,H28B), C69(H69A,H69B), C70(H70A,
 H70B), C68(H68A,H68B), C87(H87A,H87B), C85(H85A,H85B), C83(H83A,H83B),
 C90(H90A,H90B), C88(H88A,H88B), C92(H92A,H92B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C37(H37), C26(H26), C11(H11), C22(H22), C18(H18), C19(H19),
 C35(H35), C40(H40), C24(H24), C34(H34), C23(H23), C31(H31), C25(H25), C20(H20),
  C33(H33), C16(H16), C38(H38), C41(H41), C12(H12), C8(H8), C17(H17), C9(H9),
 C39(H39), C32(H32), C43(H43), C63(H63), C52(H52), C64(H64), C44(H44), C67(H67),
  C73(H73), C75(H75), C50(H50), C76(H76), C49(H49), C57(H57), C74(H74),
 C82(H82), C53(H53), C60(H60), C61(H61), C59(H59), C58(H58), C65(H65), C66(H66),
  C78(H78), C81(H81), C79(H79), C80(H80), C72(H72)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C86(H86A,H86B,H86C), C84(H84A,H84B,H84C), C89(H89A,H89B,H89C), C91(H91A,
 H91B,H91C)
;
_shelx_res_checksum              90471
_olex2_submission_special_instructions 'No special instructions were received'