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_7705546
_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         'C106 H84 Cu2 N6 P4, 2(Cl O4), 3(C H2 Cl2)'
_chemical_formula_sum            'C109 H90 Cl8 Cu2 N6 O8 P4'
_chemical_formula_weight         2146.52
_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                71.4901(12)
_cell_angle_beta                 65.5328(15)
_cell_angle_gamma                64.5233(15)
_cell_formula_units_Z            1
_cell_length_a                   13.6176(3)
_cell_length_b                   13.86960(18)
_cell_length_c                   16.3807(2)
_cell_measurement_reflns_used    8676
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      73.6620
_cell_measurement_theta_min      5.5620
_cell_volume                     2505.37(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 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_temperature      100.01
_diffrn_measured_fraction_theta_full 0.9949
_diffrn_measured_fraction_theta_max 0.9647
_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    -89.00  22.00   0.50    0.50    --    0.00 -57.00  90.00  222
  2  \w    -13.00  42.00   0.50    0.50    --    0.00  19.00-120.00  110
  3  \w    -72.00 -46.00   0.50    0.50    --    0.00 -57.00   0.00   52
  4  \w     41.00  67.00   0.50    0.50    --    0.00  77.00-120.00   52
  5  \w    -17.00  64.00   0.50    0.50    --    0.00  19.00 -30.00  162
  6  \w    -43.00  22.00   0.50    0.50    --    0.00 -57.00   0.00  130
  7  \w     22.00  67.00   0.50    1.50    --   94.60 -82.00 -30.00   90
  8  \w      6.00 118.00   0.50    1.50    --   94.60 -15.00-180.00  224
  9  \w     74.00 126.00   0.50    1.50    --   94.60 -82.00 -90.00  104
 10  \w    128.00 162.00   0.50    1.50    --   94.60  30.00-120.00   68
 11  \w     46.00 126.00   0.50    1.50    --   94.60 -82.00  30.00  160
 12  \w     64.00  99.00   0.50    1.50    --   94.60 -82.00 150.00   70
 13  \w      8.00 126.00   0.50    1.50    --   94.60 -82.00-180.00  236
 14  \w      5.00 112.00   0.50    1.50    --   94.60 -15.00 -60.00  214
 15  \w      7.00 118.00   0.50    1.50    --   94.60 -15.00  60.00  222
 16  \w      5.00 126.00   0.50    1.50    --   94.60 -82.00-120.00  242
 17  \w     22.00 107.00   0.50    1.50    --   94.60 -61.00  30.00  170
 18  \w     53.00  79.00   0.50    1.50    --   94.60 -61.00-180.00   52
 19  \w     84.00 109.00   0.50    1.50    --   94.60 -82.00 -30.00   50
 20  \w     86.00 125.00   0.50    1.50    --   94.60 -82.00  90.00   78
 21  \w     81.00 107.00   0.50    1.50    --   94.60  30.00-120.00   52
 22  \w     19.00  69.00   0.50    1.50    --   94.60 -45.00  90.00  100
 23  \w     29.00  69.00   0.50    1.50    --   94.60 -82.00 -90.00   80
 24  \w     25.00 105.00   0.50    1.50    --   94.60 -30.00 -90.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.9949
_diffrn_reflns_Laue_measured_fraction_max 0.9647
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29293
_diffrn_reflns_point_group_measured_fraction_full 0.9949
_diffrn_reflns_point_group_measured_fraction_max 0.9647
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         74.03
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    3.581
_exptl_absorpt_correction_T_max  0.627
_exptl_absorpt_correction_T_min  0.375
_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_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1102.317
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.7421
_refine_diff_density_min         -0.7716
_refine_diff_density_rms         0.0628
_refine_ls_d_res_high            0.8019
_refine_ls_d_res_low             11.6290
_refine_ls_goodness_of_fit_ref   1.0324
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    83
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9828
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.0293
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0029
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+1.5259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                9057
_reflns_number_total             9828
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt02542a6.cif
_cod_data_source_block           exp_1064
_cod_depositor_comments
'Adding full bibliography for 7705544--7705547.cif.'
_cod_original_cell_volume        2505.36(8)
_cod_original_formula_sum        'C109 Cl8 Cu2 H90 N6 O8 P4 '
_cod_database_code               7705546
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-O2 \\sim Cl1a-O2a
 with sigma of 0.02
 Cl1-O4 \\sim Cl1a-O4a
 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
 O2-O4 \\sim O2a-O4a
 with sigma of 0.04
 O2-O3 \\sim O2a-O3a
 with sigma of 0.04
 O2-O1 \\sim O2a-O1a
 with sigma of 0.04
 O4-O3 \\sim O4a-O3a
 with sigma of 0.04
 O4-O1 \\sim O4a-O1a
 with sigma of 0.04
 O3-O1 \\sim O3a-O1a
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 Cl1, O2, O4, O3, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, Cl1, O2, O4, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1a, O2a, O4a, O3a, O1a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(Cl1a)=Sof(O2a)=Sof(O4a)=Sof(O3a)=Sof(O1a)=1-FVAR(1)
 Sof(Cl1)=Sof(O2)=Sof(O4)=Sof(O3)=Sof(O1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C38(H38a,H38b), C25(H25a,H25b)
5.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C12(H12), C53(H53), C6(H6), C37(H37), C11(H11), C33(H33), C1(H1),
 C2(H2), C14(H14), C7(H7), C27(H27), C50(H50), C44(H44), C18(H18), C15(H15),
 C40(H40), C20(H20), C43(H43), C36(H36), C28(H28), C42(H42), C46(H46), C35(H35),
  C16(H16), C17(H17), C34(H34), C49(H49), C24(H24), C41(H41), C48(H48),
 C30(H30), C23(H23), C31(H31), C29(H29), C47(H47), C21(H21), C22(H22)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;