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_7705547
_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
'C82 H68 Cu2 N10 P4, 2(Cl O4), 0.5[CH2Cl2], 1[CH2Cl2]'
_chemical_formula_sum            'C83.5 H71 Cl5 Cu2 N10 O8 P4'
_chemical_formula_weight         1770.806
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2020-09-10
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-09-24 deposited with the CCDC.	2020-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                72.522(2)
_cell_angle_beta                 74.290(2)
_cell_angle_gamma                80.072(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2249(4)
_cell_length_b                   14.9229(4)
_cell_length_c                   21.7760(6)
_cell_measurement_reflns_used    11021
_cell_measurement_temperature    108.30(10)
_cell_measurement_theta_max      29.2740
_cell_measurement_theta_min      3.6730
_cell_volume                     3926.6(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-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 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_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_details
;
  1 omega  -11.00   26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000  -30.0000 37

  2 omega  -12.00   32.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335  -57.0000   60.0000 44

  3 omega  -47.00   34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335  -57.0000  -60.0000 81

  4 omega  -25.00   12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000 -180.0000 37

  5 omega  -12.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210   19.0000 -150.0000 57

  6 omega   10.00   43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335   57.0000 -120.0000 33

  7 omega   60.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335   57.0000 -120.0000 25

  8 omega   36.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335  178.0000 -150.0000 55

  9 omega   46.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335  178.0000  150.0000 27

 10 omega  -79.00  -20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -57.0000 -120.0000 59

 11 omega  -48.00   21.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335  -57.0000   30.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.9975
_diffrn_reflns_Laue_measured_fraction_max 0.9977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44896
_diffrn_reflns_point_group_measured_fraction_full 0.9975
_diffrn_reflns_point_group_measured_fraction_max 0.9977
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90448
_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    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1822.387
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.8186
_refine_diff_density_min         -0.4829
_refine_diff_density_rms         0.0932
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.7329
_refine_ls_goodness_of_fit_ref   1.0468
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    130
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         15415
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.0410
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.7681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                12615
_reflns_number_total             15415
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt02542a6.cif
_cod_data_source_block           exp_5400
_cod_depositor_comments
'Adding full bibliography for 7705544--7705547.cif.'
_cod_original_cell_volume        3926.60(19)
_cod_original_formula_sum        'C83.5 Cl5 Cu2 H71 N10 O8 P4 '
_cod_database_code               7705547
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2-O7 \\sim Cl2A-O7A
 with sigma of 0.02
 Cl2-O6 \\sim Cl2A-O6A
 with sigma of 0.02
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 O6-O8 \\sim O6A-O8A
 with sigma of 0.04
 Cl2-O8 \\sim Cl2A-O8A
 with sigma of 0.02
 Cl2-O5 \\sim Cl2A-O5A
 with sigma of 0.02
 O6-O5 \\sim O6A-O5A
 with sigma of 0.04
 O5-O8 \\sim O5A-O8A
 with sigma of 0.04
 O7-O6 \\sim O7A-O6A
 with sigma of 0.04
 O7-O5 \\sim O7A-O5A
 with sigma of 0.04
 O3-O1 \\sim O3A-O1A
 with sigma of 0.04
 Cl1-O2 \\sim Cl1A-O2A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1A-O3A
 with sigma of 0.02
 Cl1-O1 \\sim Cl1A-O1A
 with sigma of 0.02
 O4-O1 \\sim O4A-O1A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O3-O2 \\sim O3A-O2A
 with sigma of 0.04
 O4-O2 \\sim O4A-O2A
 with sigma of 0.04
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 Cl1-O4 \\sim Cl1A-O4A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O8, Cl2, O7, O6, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2A, O7A, O6A, O5A, O8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3A, Cl1A, O4A, O1A, O2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1A, O3A, O4A, O1A, O2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: Cl2(0.85) O7(0.85) O6(0.85) O5(0.85) O8(0.85) O6A(0.15) Cl2A(0.15)
 O7A(0.15) O5A(0.15) O8A(0.15) Cl1(0.93) O3(0.93) O4(0.93) O1(0.93) O2(0.93)
 Cl1A(0.07) O3A(0.07) O4A(0.07) O1A(0.07) O2A(0.07)
5.a Secondary CH2 refined with riding coordinates:
 C41(H41a,H41b), C81(H81a,H81b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,
 H56b), C82(H82a,H82b)
5.b Aromatic/amide H refined with riding coordinates:
 C80(H80), C24(H24), C61(H61), C1(H1), C65(H65), C22(H22), C29(H29), C68(H68),
 C62(H62), C64(H64), C66(H66), C58(H58), C53(H53), C28(H28), C60(H60), C17(H17),
  C74(H74), C71(H71), C44(H44), C77(H77), C3(H3), C70(H70), C33(H33), C45(H45),
 C10(H10), C15(H15), C43(H43), C52(H52), C67(H67), C2(H2), C46(H46), C49(H49),
 C13(H13), C79(H79), C23(H23), C8(H8), C47(H47), C50(H50), C27(H27), C72(H72),
 C14(H14), C59(H59), C78(H78), C16(H16), C9(H9), C32(H32), C76(H76), C51(H51),
 C37(H37), C38(H38), C31(H31), C30(H30), C73(H73), C36(H36), C39(H39), C40(H40)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 119 electrons were 
found in a volume of 395\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 0.5[CH2Cl2], 1[CH2Cl2] per Formula Unit 
which account for 126 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'