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_7707686
_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         'C45 H36 Cu N6 P2, B F4'
_chemical_formula_sum            'C45 H36 B Cu F4 N6 P2'
_chemical_formula_weight         873.09
_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                93.6821(8)
_cell_angle_beta                 95.5889(8)
_cell_angle_gamma                106.8124(9)
_cell_formula_units_Z            2
_cell_length_a                   8.79421(9)
_cell_length_b                   11.97329(12)
_cell_length_c                   20.23452(19)
_cell_measurement_reflns_used    18161
_cell_measurement_temperature    132.98(10)
_cell_measurement_theta_max      73.6760
_cell_measurement_theta_min      4.2620
_cell_volume                     2020.28(4)
_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_environment      N~2~
_diffrn_ambient_temperature      132.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_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  90.00  222
  2  \w    -89.00  18.00   0.50    0.50    --    0.00 -19.00 120.00  214
  3  \w    -89.00  18.00   0.50    0.50    --    0.00 -19.00 150.00  214
  4  \w    -89.00  -3.00   0.50    0.50    --    0.00 -57.00-120.00  172
  5  \w    -34.00  14.00   0.50    0.50    --    0.00 -37.00 -90.00   96
  6  \w      9.00  40.00   0.50    0.50    --   94.60 -61.00 120.00   62
  7  \w     33.00 100.00   0.50    0.50    --   94.60 -61.00-120.00  134
  8  \w      7.00 126.00   0.50    0.50    --   94.60 -82.00   0.00  238
  9  \w     75.00 183.00   0.50    0.50    --   94.60  45.00  90.00  216
 10  \w     36.00 124.00   0.50    0.50    --   94.60 -82.00-120.00  176
 11  \w     12.00 118.00   0.50    0.50    --   94.60 -61.00   0.00  212
 12  \w     16.00 116.00   0.50    0.50    --   94.60 -15.00 120.00  200
 13  \w     49.00 125.00   0.50    0.50    --   94.60 -82.00 150.00  152
 14  \w     72.00 125.00   0.50    0.50    --   94.60 -82.00  60.00  106
 15  \w      6.00 106.00   0.50    0.50    --   94.60 -30.00 120.00  200
 16  \w      5.00  40.00   0.50    0.50    --   94.60 -82.00  60.00   70
 17  \w     63.00  89.00   0.50    0.50    --   94.60 -61.00 120.00   52
 18  \w      8.00  45.00   0.50    0.50    --   94.60 -82.00 150.00   74
 19  \w     77.00 103.00   0.50    0.50    --   94.60 -82.00 -60.00   52
 20  \w     65.00 120.00   0.50    0.50    --   94.60  77.00 -50.20  110
 21  \w     84.00 123.00   0.50    0.50    --   94.60 -82.00  90.00   78
 22  \w    108.00 183.00   0.50    0.50    --   94.60  34.00  63.43  150
;
_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      0.0237664000
_diffrn_orient_matrix_UB_12      -0.0756422000
_diffrn_orient_matrix_UB_13      0.0566339000
_diffrn_orient_matrix_UB_21      -0.1808181000
_diffrn_orient_matrix_UB_22      -0.0645643000
_diffrn_orient_matrix_UB_23      -0.0096991000
_diffrn_orient_matrix_UB_31      0.0270231000
_diffrn_orient_matrix_UB_32      -0.0913659000
_diffrn_orient_matrix_UB_33      -0.0510508000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23983
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.967
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77361
_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    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.3290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7558
_reflns_number_total             7930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01023a2.cif
_cod_data_source_block           20171208-2
_cod_depositor_comments
'Adding full bibliography for 7707686--7707690.cif.'
_cod_database_code               7707686
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H30 N8 P8 Cu1 B1 F4 O1'
_reflns_odcompleteness_completeness 99.57
_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
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C37(H37), C41(H41), C22(H22), C43(H43), C30(H30), C42(H42),
 C10(H10), C31(H31), C32(H32), C45(H45), C44(H44), C16(H16), C18(H18), C25(H25),
  C9(H9), C26(H26), C29(H29), C19(H19), C8(H8), C2(H2), C38(H38), C39(H39),
 C23(H23), C13(H13), C17(H17), C14(H14), C1(H1), C35(H35), C36(H36), C3(H3),
 C24(H24)
;
_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 1.463
_oxdiff_exptl_absorpt_empirical_full_min 0.734