Highly near-IR emissive ytterbium(iii) complexes with unprecedented quantum yields
Hu, Ji-Yun; Ning, Yingying; Meng, Yin-Shan; Zhang, Jing; Wu, Zhuo-Yan; Gao, Song; Zhang, Jun-Long; Chem. Sci. 8 (2017) 2702–; doi:10.1039/C6SC05021B

data_1545047
_publ_section_title
;
 Highly near-IR emissive ytterbium(iii) complexes with unprecedented
 quantum yields
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2702
_journal_paper_doi               10.1039/C6SC05021B
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C55 D18 Co F8 H25 N4 O9 P3 Yb'
_chemical_formula_sum            'C55 H25 Co D18 F8 N4 O9 P3 Yb'
_chemical_formula_weight         1398.92
_chemical_name_systematic
;
 ?
;
_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             2016-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-08-27 deposited with the CCDC.
2017-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                72.8693(19)
_cell_angle_beta                 73.873(2)
_cell_angle_gamma                77.720(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2948(3)
_cell_length_b                   14.0793(3)
_cell_length_c                   16.6204(4)
_cell_measurement_reflns_used    18644
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      30.0650
_cell_measurement_theta_min      3.4110
_cell_volume                     2614.22(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3914
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega    6.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -131.0000  -43.1593 68

  2 omega    7.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -133.0000   54.6193 69

  3 omega  -73.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628    0.0000   60.0000 173

  4 omega  -13.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   38.0000  150.0000 101

  5 omega  -12.00   89.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   38.0000 -120.0000 101

  6 omega   29.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -125.0000 -165.3238 42

  7 omega  -20.00   27.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000  -60.0000 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0135563000
_diffrn_orient_matrix_UB_12      0.0292475000
_diffrn_orient_matrix_UB_13      0.0306009000
_diffrn_orient_matrix_UB_21      -0.0574751000
_diffrn_orient_matrix_UB_22      -0.0094297000
_diffrn_orient_matrix_UB_23      0.0117323000
_diffrn_orient_matrix_UB_31      0.0139345000
_diffrn_orient_matrix_UB_32      -0.0435024000
_diffrn_orient_matrix_UB_33      0.0321255000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39776
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         2.722
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.278
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.2537
_exptl_crystal_size_mid          0.1366
_exptl_crystal_size_min          0.0816
_refine_diff_density_max         12.480
_refine_diff_density_min         -3.451
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         11924
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+45.1004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.1999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10320
_reflns_number_total             11924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05021b2.cif
_cod_data_source_block           1_160123
_cod_depositor_comments
'Adding full bibliography for 1545045--1545047.cif.'
_cod_database_code               1545047
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C55 H25 D18 Co1 F8 N4 O9 P3 Yb1'
_reflns_odcompleteness_completeness 99.85
_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
2. Uiso/Uaniso restraints and constraints
Uanis(F24) \\sim Ueq, Uanis(F16) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C1AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq,
Uanis(C143) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma
of 0.2 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C0AA)
\\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C90) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3AA(H3AA), C20(H20), C30(H30), C37(H37), C48(H48), C53(H53), C55(H55),
 C76(H76), C78(H78), C79(H79), C83(H83), C86(H86), C88(H88), C91(H91), C97(H97),
  C99(H99), C102(H102), C109(H109), C122(H122), C125(H125), C132(H132),
 C143(H143), C0AA(H0AA), C1AA(H1AA), C2AA(H2AA)
3.b Idealised Me refined as rotating group:
 C9(D9A,D9B,D9C), C12(D12A,D12B,D12C), C13(D13A,D13B,D13C), C14(D14A,D14B,
 D14C), C15(D15A,D15B,D15C), C17(D17A,D17B,D17C)
;
_olex2_submission_special_instructions 'No special instructions were received'