Triple Boron-Cored Chromophores Bearing Discotic 5,11,17-Triazatrinaphthylene-Based Ligands.
Qiu, Feng; Zhang, Fan; Tang, Ruizhi; Fu, Yubin; Wang, Xinyang; Han, Sheng; Zhuang, Xiaodong; Feng, Xinliang; Organic letters 18 (2016) 1398–1401; doi:10.1021/acs.orglett.6b00335

data_1555498
_publ_section_title
;
 Triple Boron-Cored Chromophores Bearing Discotic
 5,11,17-Triazatrinaphthylene-Based Ligands.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1398
_journal_page_last               1401
_journal_paper_doi               10.1021/acs.orglett.6b00335
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C81 H81 B3 N6, C7 H8'
_chemical_formula_sum            'C88 H89 B3 N6'
_chemical_formula_weight         1263.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.552(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8983(7)
_cell_length_b                   28.293(2)
_cell_length_c                   24.5786(19)
_cell_measurement_reflns_used    3382
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      65.1720
_cell_measurement_theta_min      3.8990
_cell_volume                     6838.3(9)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3415
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega  -39.00   29.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2424   38.0000  -90.0000 68

  2 omega   12.00   82.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  -77.0000   30.0000 70

  3 omega   88.00  120.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  -77.0000   30.0000 32

  4 omega   56.00   98.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  -45.0000  150.0000 42

  5 omega   46.00  109.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  -94.0000   30.0000 63

  6 omega   70.00  145.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981   45.0000 -180.0000 75

  7 omega   65.00  150.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981   45.0000  -60.0000 85

  8 omega  135.00  160.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  125.0000   30.0000 25

  9 omega -124.00  -95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2424  -99.0000  -30.0000 29

 10 omega -122.00  -91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2424  -99.0000   30.0000 31

 11 omega -130.00  -56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2424 -178.0000  -90.0000 74
;
_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      0.0489674000
_diffrn_orient_matrix_UB_12      -0.0139280000
_diffrn_orient_matrix_UB_13      0.0596322000
_diffrn_orient_matrix_UB_21      -0.0971709000
_diffrn_orient_matrix_UB_22      0.0366927000
_diffrn_orient_matrix_UB_23      0.0205254000
_diffrn_orient_matrix_UB_31      -0.1126828000
_diffrn_orient_matrix_UB_32      -0.0377519000
_diffrn_orient_matrix_UB_33      -0.0018200000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.1434
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24544
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38029
_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.
;
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         11411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+2.2759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2903
_reflns_number_gt                5825
_reflns_number_total             11411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b00335_si_003.cif
_cod_data_source_block           exp_5886
_cod_original_cell_volume        6838.5(9)
_cod_database_code               1555498
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H59C(0.4) H59D(0.4) H59A(0.6) H59B(0.6) C1(0.6) H1A(0.6) H1B(0.6)
 C5AA(0.6) H5AA(0.6) H5AB(0.6) C6AA(0.6) H6AA(0.6) H6AB(0.6) C3(0.4) H3A(0.4)
 H3B(0.4) C4(0.4) H4A(0.4) H4B(0.4) C321(0.4) H32A(0.4) H32B(0.4) C2(0.6)
 H2A(0.6) H2B(0.6) H2C(0.6) C7(0.4) H7A(0.4) H7B(0.4) H7C(0.4) C1A(0.4)
 H1AA(0.4) H1AB(0.4) C1B(0.6) H1BA(0.6) H1BB(0.6)
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C42(H42A,H42B), C50(H50A,H50B), C57(H57A,
 H57B), C59(H59C,H59D), C59(H59A,H59B), C65(H65A,H65B), C78(H78A,H78B),
 C82(H82A,H82B), C84(H84A,H84B), C90(H90A,H90B), C1(H1A,H1B), C5AA(H5AA,H5AB),
 C6AA(H6AA,H6AB), C3(H3A,H3B), C4(H4A,H4B), C321(H32A,H32B), C1A(H1AA,H1AB),
 C1B(H1BA,H1BB)
3.b Aromatic/amide H refined with riding coordinates:
 C4AA(H4AA), C11(H11), C12(H12), C19(H19), C21(H21), C22(H22), C23(H23),
 C25(H25), C26(H26), C28(H28), C29(H29), C32(H32), C33(H33), C38(H38), C41(H41),
  C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C51(H51), C52(H52),
 C54(H54), C55(H55), C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
  C67(H67), C68(H68), C70(H70), C71(H71), C74(H74), C76(H76), C77(H77),
 C80(H80), C81(H81), C85(H85), C87(H87), C92(H92), C27(H27), C58(H58), C75(H75),
  C79(H79), C88(H88)
3.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C2(H2A,H2B,
 H2C), C7(H7A,H7B,H7C)
;
_olex2_date_sample_data_collection 2014-12-15
_olex2_submission_special_instructions 'No special instructions were received'