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_7707688
_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, B F4'
_chemical_formula_sum            'C44 H36 B Cu F4 N6 P2'
_chemical_formula_weight         861.08
_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             2017-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2020-09-23 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                94.161(2)
_cell_angle_beta                 94.741(2)
_cell_angle_gamma                108.746(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9379(2)
_cell_length_b                   12.2840(2)
_cell_length_c                   19.3667(4)
_cell_measurement_reflns_used    13562
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.5840
_cell_measurement_theta_min      4.5780
_cell_volume                     1995.55(7)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.961
_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    -18.00  89.00   0.50    0.50    --    0.00  19.00   0.00  214
  3  \w    -18.00  89.00   0.50    0.50    --    0.00  19.00  90.00  214
  4  \w    -89.00  22.00   0.50    0.50    --    0.00 -57.00   0.00  222
  5  \w    -89.00  17.00   0.50    0.50    --    0.00 -37.00   0.00  212
  6  \w     78.00 104.00   0.50    1.00    --   94.60 -82.00   0.00   52
  7  \w     82.00 108.00   0.50    1.00    --   94.60 -82.00-150.00   52
  8  \w      7.00  33.00   0.50    1.00    --   94.60 -82.00   0.00   52
  9  \w     10.00 118.00   0.50    1.00    --   94.60 -61.00 -60.00  216
 10  \w      9.00 104.00   0.50    1.00    --   94.60 -15.00 150.00  190
 11  \w     21.00 126.00   0.50    1.00    --   94.60 -82.00 -60.00  210
 12  \w     38.00  88.00   0.50    1.00    --   94.60 -30.00   0.00  100
 13  \w     25.00 117.00   0.50    1.00    --   94.60 -61.00 150.00  184
 14  \w     59.00  85.00   0.50    1.00    --   94.60 -82.00-120.00   52
 15  \w     63.00 112.00   0.50    1.00    --   94.60 -82.00  60.00   98
 16  \w     81.00 158.00   0.50    1.00    --   94.60  30.00 150.00  154
 17  \w     38.00 111.00   0.50    1.00    --   94.60 -61.00  30.00  146
 18  \w     14.00  40.00   0.50    1.00    --   94.60 -82.00  60.00   52
 19  \w     83.00 183.00   0.50    1.00    --   94.60  30.00 120.00  200
 20  \w     38.00 126.00   0.50    1.00    --   94.60 -82.00 150.00  176
 21  \w     77.00 184.00   0.50    1.00    --   94.60  15.00  60.00  214
;
_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      0.0761937000
_diffrn_orient_matrix_UB_12      -0.0240188000
_diffrn_orient_matrix_UB_13      -0.0654152000
_diffrn_orient_matrix_UB_21      -0.0821700000
_diffrn_orient_matrix_UB_22      0.0724225000
_diffrn_orient_matrix_UB_23      -0.0405427000
_diffrn_orient_matrix_UB_31      0.1448996000
_diffrn_orient_matrix_UB_32      0.1091488000
_diffrn_orient_matrix_UB_33      0.0227919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22029
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.240
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58504
_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_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1490P)^2^+0.6810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6279
_reflns_number_total             7820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01023a2.cif
_cod_data_source_block           zn-445
_cod_depositor_comments
'Adding full bibliography for 7707686--7707690.cif.'
_cod_database_code               7707688
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H30 Cu1 F3 S1 O3 N6 P2'
_reflns_odcompleteness_completeness 99.50
_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, All N(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:
 N3(H3), C10(H10), C38(H38), C9(H9), C1(H1), C34(H34), C8(H8), C44(H44),
 C18(H18), C3(H3A), C37(H37), C2(H2), C35(H35), C42(H42), C21(H21), C27(H27),
 C25(H25), C15(H15), C13(H13), C43(H43), C28(H28), C40(H40), C16(H16), C17(H17),
  C31(H31), C23(H23), C24(H24), C22(H22), C36(H36), C41(H41), C29(H29), C30(H30)
;
_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 3.068
_oxdiff_exptl_absorpt_empirical_full_min 0.208