New discovery in crystallography: correlation of terahertz time-domain spectra with crystal structures and photoluminescence properties of mononuclear/binuclear diimine‒Cu(i)-phosphine complexes
Zhu, Ning; Wang, Guo; Lin, Sen; Li, Zhong-Feng; Xin, Xiu-Lan; Yang, Yu-Ping; Liu, Min; Jin, Qiong-Hua; CrystEngComm 21 (2019) 4275–; doi:10.1039/C9CE00729F

data_7232908
_publ_section_title
;
 New discovery in crystallography: correlation of terahertz time-domain
 spectra with crystal structures and photoluminescence properties of
 mononuclear/binuclear diimine--Cu(i)-phosphine complexes
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4275
_journal_paper_doi               10.1039/C9CE00729F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C50 H36 Cu N4 O P2, C F3 O3 S, C H4 O, C O'
_chemical_formula_sum            'C53 H36 Cu F3 N4 O6 P2 S'
_chemical_formula_weight         1039.40
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                83.046(4)
_cell_angle_beta                 77.092(5)
_cell_angle_gamma                70.657(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6980(7)
_cell_length_b                   12.5061(5)
_cell_length_c                   19.6636(10)
_cell_measurement_reflns_used    5554
_cell_measurement_temperature    104.2
_cell_measurement_theta_max      29.4259
_cell_measurement_theta_min      3.1441
_cell_volume                     2416.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      104.2
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -5.00   56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   77.0000  -60.0000 61

  2 omega   -5.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   77.0000   60.0000 37

  3 omega    8.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   37.0000 -180.0000 44

  4 omega  -43.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -37.0000   30.0000 74

  5 omega  -42.00   23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -37.0000  -60.0000 65

  6 omega  -31.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -89.0000 -165.0000 83
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0701387000
_diffrn_orient_matrix_UB_12      0.0073432000
_diffrn_orient_matrix_UB_13      0.0103748000
_diffrn_orient_matrix_UB_21      0.0006132000
_diffrn_orient_matrix_UB_22      -0.0209422000
_diffrn_orient_matrix_UB_23      -0.0320584000
_diffrn_orient_matrix_UB_31      0.0147914000
_diffrn_orient_matrix_UB_32      -0.0559364000
_diffrn_orient_matrix_UB_33      0.0154057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17728
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.150
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.708
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0855P)^2^+5.6155P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8014
_reflns_number_total             9498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00729f2.cif
_cod_data_source_block           exp_3956
_cod_depositor_comments
'Adding full bibliography for 7232899--7232908.cif.'
_cod_database_code               7232908
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.787
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C28(H28), C44(H44), C35(H35), C34(H34), C29(H29), C50(H50),
 C37(H37), C1(H1), C19(H19), C18(H18), C10(H10), C17(H17), C8(H8), C16(H16),
 C22(H22), C41(H41), C36(H36), C20(H20), C3(H3), C43(H43), C31(H31), C26(H26),
 C42(H42), C40(H40), C46(H46), C25(H25), C2(H2), C24(H24), C48(H48), C14(H14),
 C49(H49), C9(H9), C13(H13), C47(H47), C23(H23)
2.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              43940
_olex2_submission_special_instructions 'No special instructions were received'