In Situ Visualization of Assembly and Photonic Signal Processing in a Triplet Light-Harvesting Nanosystem.
Sun, Meng-Jia; Liu, Yingying; Yan, Yaming; Li, Rui; Shi, Qiang; Zhao, Yong Sheng; Zhong, Yu-Wu; Yao, Jiannian; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b12519

data_4127215
_publ_section_title
;
 In Situ Visualization of Assembly and Photonic Signal Processing in a
 Triplet Light-Harvesting Nanosystem.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12519
_journal_year                    2018
_chemical_formula_moiety         'C30 H23 Ir N5, F6 P'
_chemical_formula_sum            'C30 H23 F6 Ir N5 P'
_chemical_formula_weight         790.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.887(2)
_cell_length_b                   15.832(3)
_cell_length_c                   32.699(7)
_cell_measurement_reflns_used    10614
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.2462
_cell_volume                     5636.1(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            19241
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.354
_diffrn_source                   Confocal
_exptl_absorpt_coefficient_mu    4.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       plate
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6392
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0138P)^2^+37.2269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4880
_reflns_number_total             6392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12519_si_002.cif
_cod_data_source_block           mx5838b
_cod_original_cell_volume        5636(2)
_cod_database_code               4127215
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C25A-C24A = C30-C29 = C28-C25A = C29-C28 = C27-C26 = C29A-C26 = C25-C24 = C24-
 C23
 1.38 with sigma of 0.001
 N3-C28 = N2-C30 = N4-C27 = N4-C23
 1.34 with sigma of 0.001
 N3A-C26 = N4-C30A
 1.34 with sigma of 0.001
 C24A-C23A = C25A-C24A = C28-C25A = C28-C27A
 1.38 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
N3 \\sim C28 \\sim C29 \\sim C30 \\sim C27A \\sim C24A \\sim C25A \\sim C23A
\\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim N3A \\sim C29A \\sim C30A \\sim
C23: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N3) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C27A)
\\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C23A) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N4)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(H26A)=Sof(H28A)=Sof(N3A)=Sof(C27A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=Sof(C30A)=Sof(H30A)=Sof(C29A)=Sof(H29A)=Sof(C23A)=Sof(H23A)=1-FVAR(1)
 Sof(N3)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(H26)=
 Sof(C27)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C26(H26A), C28(H28), C28(H28A), C29(H29),
 C30(H30), C24A(H24A), C25A(H25A), C30A(H30A), C29A(H29A), C23A(H23A)
;
_shelx_res_checksum              51588
_shelx_hkl_checksum              44892
_olex2_submission_special_instructions 'No special instructions were received'