Simultaneously Enhancing Efficiency and Lifetime of Ultralong Organic Phosphorescence Materials by Molecular Self-Assembly.
Bian, Lifang; Shi, Huifang; Wang, Xuan; Ling, Kun; Ma, Huili; Li, Mengping; Cheng, Zhichao; Ma, Chaoqun; Cai, Suzhi; Wu, Qi; Gan, Nan; Xu, Xiangfei; An, Zhongfu; Huang, Wei; Journal of the American Chemical Society 140 (2018) 10734–10739; doi:10.1021/jacs.8b03867

data_4132426
_publ_section_title
;
 Simultaneously Enhancing Efficiency and Lifetime of Ultralong Organic
 Phosphorescence Materials by Molecular Self-Assembly.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10734
_journal_page_last               10739
_journal_paper_doi               10.1021/jacs.8b03867
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C8 H5 O4, 2(H2 O), C3 H7 N6'
_chemical_formula_sum            'C11 H16 N6 O6'
_chemical_formula_weight         328.30
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                95.341(7)
_cell_angle_beta                 105.299(7)
_cell_angle_gamma                97.970(8)
_cell_formula_units_Z            2
_cell_length_a                   7.076(2)
_cell_length_b                   9.231(3)
_cell_length_c                   12.242(4)
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.25
_cell_volume                     756.8(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_number            3475
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.656
_diffrn_reflns_theta_min         2.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1205 before and 0.0374 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1191 before and 0.0373 after correction.
 The Ratio of minimum to maximum transmission is 0.84.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 8027 reflections, Rint = 0.0309
 (4747 with I > 3sig(I), Rint = 0.0256)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.067
_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     223
_refine_ls_number_reflns         3475
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0851P)^2^+0.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2217
_reflns_number_total             3475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03867_si_001.cif
_cod_data_source_block           zz
_cod_database_code               4132426
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5C = O5-H5B
 0.86 with sigma of 0.02
3.a Free rotating group:
 O6(H6C,H6D), O5(H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C4(H4)
3.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B), N1(H1A,H1B), N3(H3A,H3B)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'