Lanthanoid beta-triketonates: a new class of highly efficient NIR emitters for bright NIR-OLEDs
Brodie L. Reid; Stefano Stagni; Joanna M. Malicka; Massimo Cocchi; Garry S. Hanan; Mark I. Ogden; Massimiliano Massi; Chem.Commun. 50 (2014) 11580–; doi:10.1039/C4cc04961F

data_7115690
_publ_section_title
;
 Lanthanoid beta-triketonates: a new class of highly efficient NIR
 emitters for bright NIR-OLEDs
;
_journal_name_full               Chem.Commun.
_journal_page_first              11580
_journal_paper_doi               10.1039/C4cc04961F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C180 H132 K2 O26 Yb2'
_chemical_formula_sum            'C180 H132 K2 O26 Yb2'
_chemical_formula_weight         3135.13
_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   mixed
_audit_creation_date             2014-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                102.772(4)
_cell_angle_beta                 90.083(4)
_cell_angle_gamma                91.038(4)
_cell_formula_units_Z            1
_cell_length_a                   14.1075(12)
_cell_length_b                   14.4693(12)
_cell_length_c                   17.9695(14)
_cell_measurement_reflns_used    9257
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.598
_cell_measurement_theta_min      2.522
_cell_volume                     3576.6(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            254230
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.375
_diffrn_reflns_theta_min         2.521
_diffrn_source                   'Rotating Anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.494
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1203 before and 0.0870 after correction.
The Ratio of minimum to maximum transmission is 0.6356.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       plates
_exptl_crystal_F_000             1598
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.078
_refine_diff_density_max         2.638
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         13465
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1031P)^2^+6.7909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12372
_reflns_number_total             13465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc04961f2.cif
_cod_data_source_block           brod11_0m
_cod_database_code               7115690
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O501-H501
 0.85 with sigma of 0.01
 C302-C305
 1.5 with sigma of 0.02
 C205-C202
 1.5 with sigma of 0.02
 C204-C217
 1.5 with sigma of 0.02
 C305-C302
 1.3 with sigma of 0.02
 C205-C202
 1.3 with sigma of 0.02
 C501-H501
 1.909817 with sigma of 0.02
 K1-H501
 3.33927 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C501(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C118(H118), C119(H119),
 C120(H120), C121(H121), C122(H122), C206(H206), C207(H207), C208(H208),
 C209(H209), C210(H210), C212(H212), C213(H213), C214(H214), C215(H215),
 C216(H216), C218(H218), C219(H219), C220(H220), C221(H221), C222(H222),
 C306(H306), C307(H307), C308(H308), C309(H309), C310(H310), C312(H312),
 C313(H313), C314(H314), C315(H315), C316(H316), C318(H318), C319(H319),
 C320(H320), C321(H321), C322(H322), C406(H406), C407(H407), C408(H408),
 C409(H409), C410(H410), C412(H412), C413(H413), C414(H414), C415(H415),
 C416(H416), C418(H418), C419(H419), C420(H420), C421(H421), C422(H422)
3.c Idealised Me refined as rotating group:
 C502(H50C,H50D,H50E)
;
_shelx_res_checksum              89321