A new application of terahertz time-domain absorption spectra in luminescent complexes: characterization of the C-Hπ weak interactions in Cu(I) complexes.
Sun, Zhen-Zhou; Zhu, Ning; Pan, Xun; Wang, Guo; Li, Zhong-Feng; Xin, Xiu-Lan; Han, Hong-Liang; Feng, Yue-Bing; Jin, Qiong-Hua; Yang, Yu-Ping; Yang, Wei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10214–10224; doi:10.1039/d1dt01023a

data_7707687
_publ_section_title
;
 A new application of terahertz time-domain absorption spectra in
 luminescent complexes: characterization of the C-H\p weak interactions in
 Cu(I) complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10214
_journal_page_last               10224
_journal_paper_doi               10.1039/d1dt01023a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C44 H36 Cu N6 P2, C F3 O3 S, C H4 O'
_chemical_formula_sum            'C46 H40 Cu F3 N6 O4 P2 S'
_chemical_formula_weight         955.38
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-09-23 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                96.339(2)
_cell_angle_beta                 95.3140(10)
_cell_angle_gamma                102.620(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8200(2)
_cell_length_b                   13.0493(4)
_cell_length_c                   19.3364(3)
_cell_measurement_reflns_used    15936
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6000
_cell_measurement_theta_min      4.6520
_cell_volume                     2142.78(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 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.964
_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    -22.00  89.00   0.50    0.50    --    0.00  57.00 -60.00  222
  2  \w    -89.00  29.00   0.50    0.50    --    0.00 -77.00 -30.00  236
  3  \w    -89.00  17.00   0.50    0.50    --    0.00 -37.00  90.00  212
  4  \w     -7.00  68.00   0.50    0.50    --    0.00  37.00  60.00  150
  5  \w     15.00  61.00   0.50    0.50    --   94.60 -61.00 -30.00   92
  6  \w     36.00 122.00   0.50    0.50    --   94.60 -82.00 150.00  172
  7  \w     14.00  40.00   0.50    0.50    --   94.60 -82.00   0.00   52
  8  \w     95.00 122.00   0.50    0.50    --   94.60 -82.00-120.00   54
  9  \w     79.00 171.00   0.50    0.50    --   94.60  30.00 -60.00  184
 10  \w      5.00  46.00   0.50    0.50    --   94.60 -61.00 150.00   82
 11  \w     49.00 104.00   0.50    0.50    --   94.60 -61.00 150.00  110
 12  \w    110.00 182.00   0.50    0.50    --   94.60  30.00-180.00  144
 13  \w     63.00 103.00   0.50    0.50    --   94.60  82.00  90.00   80
 14  \w     79.00 184.00   0.50    0.50    --   94.60  30.00 -90.00  210
 15  \w     72.00 126.00   0.50    0.50    --   94.60 -82.00  90.00  108
 16  \w     15.00  59.00   0.50    0.50    --   94.60 -82.00  90.00   88
 17  \w     34.00 118.00   0.50    0.50    --   94.60 -61.00 -90.00  168
 18  \w     14.00  41.00   0.50    0.50    --   94.60 -82.00-120.00   54
 19  \w     63.00 117.00   0.50    0.50    --   94.60 -61.00 -30.00  108
 20  \w     16.00 126.00   0.50    0.50    --   94.60 -82.00 -90.00  220
 21  \w     70.00 126.00   0.50    0.50    --   94.60 -82.00   0.00  112
 22  \w     71.00 110.00   0.50    0.50    --   94.60  61.00 150.00   78
 23  \w    101.00 126.00   0.50    0.50    --   94.60 -82.00-180.00   50
 24  \w     88.00 184.00   0.50    0.50    --   94.60  30.00-150.00  192
;
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23257
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.952
_diffrn_reflns_theta_min         3.932
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54726
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.752
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+3.5461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7407
_reflns_number_total             8379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01023a2.cif
_cod_data_source_block           zn-555
_cod_depositor_comments
'Adding full bibliography for 7707686--7707690.cif.'
_cod_database_code               7707687
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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:
 C32(H32A,H32B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C9(H9), C7(H7), C1(H1), C34(H34), C8(H8), C3(H3), C2(H2), C13(H13),
 C21(H21), C27(H27), C38(H38), C22(H22), C17(H17), C25(H25), C37(H37), C24(H24),
  C42(H42), C14(H14), C36(H36), C23(H23), C35(H35), C44(H44), C40(H40),
 C16(H16), C15(H15), C43(H43), C28(H28), C41(H41), C29(H29), C31(H31), C30(H30)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_shelx_res_checksum              47604
_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
;